Abstract: ABSTRACT A Ternary Insecticidal Composition, and a Process of Preparation thereof A ternary Insecticidal composition comprising N'-tert-butyl-N'-(3,5-dimethylbenzoyl)-3-methoxy-2-methylbenzohydrazide, 3-[benzoyl(methyl)amino]-N-[2-bromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)-6-(trifluoromethyl)phenyl]-2-fluorobenzamide, at least one more compound selected from group of insecticides, and agrochemically acceptable excipients; and a process of preparing said composition. Moreover, the said composition demonstrates high efficacy and insect pests and mite resistance management or delays resistance development through engaging multiple modes of action. Further, the insecticidal composition provides plant tolerance against insects-pests, mites, and abiotic stress as well as the preparation method of the insecticidal composition provides stable and non-phytotoxic formulation. The insecticidal composition of present invention is environmentally safe and improves overall health, yield and vigor of the treated plant and provides complete protection to the crop plants.
DESC:FORM 2
THE PATENTS ACT 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10 and rule 13)
1. TITLE OF THE INVENTION: “A Ternary Insecticidal Composition, and a Process of Preparation thereof”
2. APPLICANT:
(a) Name : RAJDHANI PETROCHEMICALS PRIVATE LIMITED
(b) Nationality : INDIAN
(c) Address : 6, LALITA COMPLEX, RASALA ROAD, NAVRANGPURA, AHMEDABAD-380009 Gujarat, India
PROVISIONAL
The following specification describes the invention. þCOMPLETE
The following specification particularly describes the invention and the manner in which it is to be performed.
FIELD OF INVENTION
The present invention relates to a ternary insecticidal composition comprising N'-tert-butyl-N'-(3,5-dimethylbenzoyl)-3-methoxy-2-methylbenzohydrazide, 3-[benzoyl(methyl)amino]-N-[2-bromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)-6-(trifluoromethyl)phenyl]-2-fluorobenzamide, at least one more compound selected from group of insecticides, and agrochemically acceptable excipients; and a process of preparing said composition. Furthermore, the present invention relates to an insecticidal composition that increases plant tolerance against harmful pests and mites and improves overall health and vigor of the treated plant. The present invention further provides an insecticidal combination comprising aversive agent and at least one insecticide which is useful against harmful pests in plants.
BACKGROUND OF THE INVENTION
The protection of crops and its produce from insect pest damage is essential in agriculture produce enhancement. Chemical control using various chemicals and formulations is an important tool in agriculture for the prevention and control of pests. Insecticides of many types and groups are reported in the literature and a large number are in use, commercially, for control of pests in agriculture. Each year insects, plant pathogens, and weeds, destroy more than 40% of all food production. This loss occurs despite the application of insecticides and the use of a wide array of nonchemical controls, such as crop rotations, and biological controls.
Sucking pests have become quite serious from seedling stage, their heavy infestation at times reduces the crop yield to a great extent. Among the sap feeders leafhoppers commonly known as Jassids is one of the most abundant groups of plant feeding insects in the world. The problem of pest resistance in agricultural production is a global problem, and it has always been the focus of attention of agricultural science and technology workers.
With the continuous use of chemical pesticides to control pests year after year, the increase in the use of pesticides and the unscientific use of pesticides, etc., the resistance to pests has become increasingly serious, and the types of pests that have developed resistance have increased. At the same time, the high-intensity use of pesticides has led to a series of problems such as excessive pesticide residues in agricultural products, environmental pollution, and increased costs for farmers to use drugs, which is not conducive to the sustainable development of agriculture.
Insecticides are used to control a wide variety of insect pests. Diamides insecticides are a relatively new group of insecticides and include insecticides such as flubendiamide, a highly potent lepidoptericide and chlorantraniliprole and its analogue cyantraniliprole. Chlorantraniliprole and cyantraniliprole are anthranilic diamide insecticidal compounds which exhibit larvicidal activity as orally ingested toxicants which target and disrupt the Ca2+ balance and Ryanodine receptor. Benzoylphenyl urea insecticides are known in the art to be active against insect larvae and eggs. Benzoylphenyl urea insecticides are known to inhibit chitin biosynthesis in larvae and eggs of insecticides.
The combination of diamide and benzoylphenyl urea insecticides are known in the art, for example from WO2003015519A1 (Lahm) teaches combinations of diamide insecticides in combination with insecticides such as benzoylphenyl urea insecticides such as Novaluron. However, the spectrum of the combination is not broad enough to control the pest pressure seen in present times.
There is therefore a need in the art for combinations of methoxyfenozide, broflanilide compound with a specific insecticide that helps improve spectrum. With crop tolerances decreasing, lower use rates being imposed, and resistance increasingly observed, there is a need for a combination of actives that allows for broader spectrum of disease control that combines curative and preventive actives and has a lower dosage.
Insecticides are used to control a wide variety of insect pests. Diamides insecticides are a relatively new group of insecticides and include insecticides such as flubendiamide, a highly potent lepidoptericide and chlorantraniliprole and its analogue cyantraniliprole. Evolution of diamide can be studied in article published Pest Manag Sci.2013 January; 69(1):7-14.
Chlorantraniliprole and cyantraniliprole are anthranilic diamide Insecticidal compounds which exhibit larvicidal activity as orally ingested toxicants which target and disrupt the Ca2+ balance and Ryanodine receptor. Fungicides are an integral and important tool yielded by farmers to control diseases, as well as to improve yields and quality of the crops. There are various fungicides that have been developed over the years with many desirable attributes such as specificity, systemicity, curative and eradicant action and high activity at low use rates.
Various classes of fungicides are also known in the art, such as Quinone outside inhibitors (QoIs), ergosterol-biosynthesis inhibitors, and fungicides that act on multiple sites. Dithiocarbamates are multi-site fungicides. These fungicides are used for broad-spectrum disease control in more than crops. Mancozeb is especially important for controlling devastating and fast spreading diseases such as Phytophthora infestans, Venturia inaequalis etc. Dithiocarbamate fungicides, especially mancozeb, are particularly useful for disease control because of their broad spectrum of activity, high tolerance by crop plants, and general usefulness for controlling fungal plant diseases not controlled by active compounds that act on only a single target site in the fungus.
The mixing of insecticides with fungicides results in incompatibility of physical nature and may also alter efficacy of the active ingredients. Hence, an attempt has been made to know the compatibility of fungicides with insecticides and their influence of insecticides on the bio efficacy of fungicides against cabbage leaf spot when applied as mixtures under laboratory condition. U.S. Pat. No. 7,696,232 B2 discloses composition comprising chlorantaniliprole and other actives which includes fungicides.
There is therefore a need in the art for combinations of insecticidal compounds with combination of methoxyfenozide, broflanilide that helps improve spectrum. With crop tolerances decreasing, lower use rates being imposed, and resistance increasingly observed, there is a need for a combination of active composition that allows for broader spectrum of disease control that combines curative and preventive actives and has a lower dosage. The long-term use of a single insecticide makes the resistance stronger, the dosage continues to increase, and the environmental pollution is aggravated. The active ingredients known from the literature have certain disadvantages such as insufficient control efficacy, restriction of its use due to the appearance of drug-resistant pathogenic fungi, phytotoxicity and contamination to plants, or toxicity to human beings, beasts, fishes, and the like. Hence, there is a long felt need to develop novel and effective insecticidal combinations for controlling the harmful pests in plants that demonstrate high efficacy, are environmentally safe and can be advantageously formulated.
Therefore, there is a need to provide an insecticidal composition which overcomes some of the existing problems and can be prepared easily without much complex manufacturing process. The combination of these two agents with compound selected from a group of insecticides can effectively solve this problem. Through many indoor bioassays and field drug efficacy tests, it is found that the combined application of methoxyfenozide, broflanilide compound with a specific insecticide has synergistic effect, can reduce the dosage of drugs, delay resistance, and is safe for the environment. The present inventors have surprisingly developed an effective insecticidal combination which ameliorates the aforesaid shortcomings of the prior art.
OBJECT OF THE INVENTION
The principal object of the present invention is to provide a ternary insecticidal composition and a process of preparation thereof.
Another object of the present invention is to provide a ternary insecticidal composition comprising bioactive amounts of N'-tert-butyl-N'-(3,5-dimethylbenzoyl)-3-methoxy-2-methylbenzohydrazide, 3-[benzoyl(methyl)amino]-N-[2-bromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)-6-(trifluoromethyl)phenyl]-2-fluorobenzamide, one compound selected from insecticide group, and agrochemically acceptable excipients; and method of preparation thereof.
Another object of the present invention is to provide a ternary insecticidal composition for preventing and controlling the harmful pests in crops.
Yet another object of the present invention is to provide a ternary insecticidal composition with synergistic effect, which can delay resistance and reduce usage.
Further object of the present invention is to provide a ternary insecticidal composition demonstrating high efficacy and to provide complete protection to crop plants against insect-pests, mites, fungal and bacterial diseases.
Yet another object of the present invention is to provide a ternary insecticidal composition which improves overall health, yield, and vigor of the treated plant.
Further object of the present invention is to provide a ternary insecticidal composition which can be easily formulated.
Yet another object of the present invention is to provide a ternary insecticidal composition which increases plant tolerance against insect, pests, mites, and fungal and bacterial diseases and abiotic stress.
Further object of the present invention is to provide a ternary insecticidal composition within a certain range, has high safety, and is environmentally friendly.
Another object of the present invention is to provide a combination that causes late senescence to the crop to which it is applied thereby resulting in an increasing yield of the crop.
SUMMARY OF THE INVENTION
The present invention provides a ternary insecticidal composition comprising bioactive amounts of (A) N'-tert-butyl-N'-(3,5-dimethylbenzoyl)-3-methoxy-2-methylbenzohydrazide; (B) 3-[benzoyl(methyl)amino]-N-[2-bromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)-6-(trifluoromethyl)phenyl]-2-fluorobenzamide; (C) at least one or more compounds selected from a group of insecticide; and agrochemically acceptable excipients.
The formulation for the ternary pesticidal composition is selected from Capsule suspension (CS), Dispersible concentrate (DC), Emulsifiable concentrate (EC), Emulsion, water in oil (EO), Emulsion, oil in water (EW), Micro-emulsion (ME), Oil dispersion (OD), Oil miscible flowable concentrate (oil miscible suspension (OF), Oil miscible liquid (OL), Suspension concentrate (SC), Suspo-emulsion (SE), Soluble concentrate (SL), Water dispersible granule (WG or WDG), Water soluble granule (SG), Water soluble powder (SP), Wettable powder (WP), A mixed formulation of CS and SC (ZC), A mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW), Granule (GR) for soil application includes controlled release granules (CR), Jambo balls or bags (bags in water soluble pouch).
The process for preparing the present combination of insecticidal composition can be modified accordingly by any person skilled in the art based on the knowledge of the manufacturing the formulation. However, all such variation and modification is still covered by the scope of present invention.
The present invention can be formulated and is environmentally safe and is used for controlling harmful insects-pests and parasitic mites in plants, and demonstrates high 5 efficacy, and acts for disease resistance management or to delay disease resistance development through engaging multiple modes of action and increases plant tolerance against insect-pests and mites, and fungal and bacterial diseases, abiotic stress and improves overall health and vigor of the treated plant.
DETAILED DESCRIPTION OF THE INVENTION
Before explaining the present invention in detail, it is to be understood that the invention is not limited in its application to the details of the parts illustrated. The invention is capable of other embodiments, as described above and of being practiced or carried out in a variety of ways. It is to be understood that the phraseology and terminology employed herein is for the purpose of description and not to limitation. The invention may have various embodiments and they may be performed as described in the following pages of the complete specification.
The terms and words used in the following description are not limited to the bibliographical meanings, but, are merely used by the inventors to enable a clear and consistent understanding of the invention. Accordingly, it should be apparent to those skilled in the art that the following description of exemplary embodiments of the present invention are provided for illustration purpose only and not for the purpose of limiting the scope of the invention.
It is to be understood that the singular forms "a," "an," and "the" include plural reference unless the context clearly dictates otherwise.
Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments and/or in combination with or instead of the features of the other embodiments.
It should be emphasized that the term "comprises/comprising" when used in this specification is taken to specify the presence of stated features, steps or components but does not preclude the presence or addition of one or more other features, steps, components or groups thereof.
The term 'plants' as used herein, refers to all physical parts of a plant, including seeds, seedlings, saplings, roots, tubers, stems, stalks, foliage and fruits. The term "plant" is to be understood as including wild type plants and plants, which have been modified by either conventional breeding, or mutagenesis or genetic engineering, or by a combination thereof.
The term "crop" refers to both, growing and harvested crops.
The term "insects" as used herein, includes all organisms in the class "Insecta."
The term “fungi” as used herein, includes all organisms in the class of “Fungi.”
The term "animal pest" includes arthropods, gastropods, and nematodes. Preferred animal pests according to the invention are arthropods, preferably insects and arachnids, in particular insects. Insects, which are of particular relevance for crops, are typically referred to as crop insect pests.
The term "insecticidal" as used herein, refers to the ability of an insecticide and/or fungicide to increase mortality or inhibit growth rate of insects.
The term "pesticidal" as used herein, refers to the ability of an insecticide and/or fungicide to increase mortality or inhibit growth rate of pests.
To "control" or "controlling" pests means to inhibit, through a toxic effect, the ability of pests to survive, grow, feed, and/or reproduce, or to limit pest related damage or loss in crop plants. To "control" pests may or may not mean killing the pests, although it preferably means killing the pests.
The term "health of a plant" or "plant health" is defined as a condition of the plant and/or its products. As a result of the improved health, yield, plant vigor, quality and tolerance to abiotic or biotic stress are increased.
"Yield" is to be understood as any plant product of economic value that is produced by the plant such as grains, fruits in the proper sense, vegetables, nuts, grains, seeds, wood (e.g. in the case of silviculture plants) or even flowers (e.g. in the case of gardening plants, ornamentals).
"Increased yield" of a plant, in particular of an agricultural, silvicultural and/or horticultural plant means that the yield of a product of the respective plant is increased by a measurable amount over the yield of the same product of the plant produced under the same conditions, but without the application of the composition according to the invention.
The present invention provides a ternary insecticidal composition comprising:
1. Compound A: N'-tert-butyl-N'-(3,5-dimethylbenzoyl)-3-methoxy-2-methylbenzohydrazide
2. Compound B: 3-[benzoyl(methyl)amino]-N-[2-bromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)-6-(trifluoromethyl)phenyl]-2-fluorobenzamide
3. at least one or more compound selected from group of insecticide, with the following mass percentage of the composition:
Sr.No Ingredient Concentration Range (w/w %)
1 Compound A 10 to 50
2 Compound B 1 to 10
3 Compound C 1 to 40
Compound A - Methoxyfenozide is a type of specific phenylhydrazine insecticide with low toxicity. It is a carbohydrazide that is hydrazine in which the amino hydrogens have been replaced by 3-methoxy-2-methylbenzoyl, 3,5-dimethylbenzoyl, and tert-butyl groups respectively. It has a role as an environmental contaminant, a xenobiotic and an insecticide. It is a carbohydrazide and a monomethoxybenzene. It is functionally related to a N'-benzoyl-N-(tert-butyl)benzohydrazide. It has highly selective insecticidal activity against Lepidoptera pests, mainly with contact action and certain systemic action. The medicine belongs to biomimetic molting hormones. After the pests eat the medicine, they will produce a molt reaction and begin to molt. The inability to completely molt will cause the larvae to dehydrate, starve and die. The mechanism of action of this drug is opposite to that of the agent that inhibits the molt of the pest, and it can be used to control the pest throughout the larval stage.
Structural Formula:
It is mainly used to control the larvae of Lepidoptera pests. The target pests include: noctuid moth, diamondback moth, white butterfly, cabbage armyworm, cabbage borer, tobacco hornworm, spodoptera, mealworm, Spodoptera chrysalis, Spodoptera mint, Armyworm, Spodoptera moth, Spodoptera spp., Silk borer, Corn borer, Kapok worm, Grass moth, Night small tortrix, Solanum stalk moth, Leaf roller Borer, small tumbler moth, long tobacco tumbler moth, color tumbler moth, brown striped tumbler moth, hazel apple, yellow tumbler moth, stone winter moth, brown tumbler moth, peak spot moth, flower wing moth, night borer, grape berry Moth, leaf tobacco wing spot borer, long-haired tortrix.
Compound B includes Broflanilide, it is a benzamide obtained by formal condensation of the carboxy group of 3-[benzoyl(methyl)amino]-2- fluorobenzoic acid with the amino group of 2-bromo-4-(1,1,1,2,3,3,3- heptafluoropropan-2-yl)-6-(trifluoromethyl)aniline. An insecticide that exhibits high larvicidal activity against Spodoptera litura and is effective against pests with resistance to cyclodienes and fipronil. It has a role as an agrochemical and a GABA (Gamma-Aminobutyric Acid) antagonist. It is a member of benzamides, a member of monofluorobenzenes, an organofluorine insecticide, a member of bromobenzenes and a member of (trifluoromethyl) benzenes.
Structural Formula:
It is mainly used to control Lepidoptera, Coleoptera, termites, mosquitoes and other pests on green leafy vegetables, perennial crops and grains.
Compound C is selected from group consisting of
C1 diafenthiuron, 1-tert-butyl-3-[4-phenoxy-2,6-di(propan-2-yl)phenyl]thiourea,
C2 hexythiazox, (4S,5S)-5-(4-chlorophenyl)-N-cyclohexyl-4-methyl-2-oxo-1,3-thiazolidine-3-carboxamide,
C3 beta cyfluthrin, [(R)-cyano-(4-fluoro-3-phenoxyphenyl)methyl] (1S)-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropane-1-carboxylate
C4 spiromesifen, [2-oxo-3-(2,4,6-trimethylphenyl)-1-oxaspiro[4.4]non-3-en-4-yl] 3,3-dimethylbutanoate,
C5 acetamiprid, N-[(6-chloropyridin-3-yl)methyl]-N'-cyano-N-methylethanimidamide,
C6 pyriproxyfen, 2-[1-(4-phenoxyphenoxy)propan-2-yloxy]pyridine,
C7 spirotetramat, [3-(2,5-dimethylphenyl)-8-methoxy-2-oxo-1-azaspiro[4.5]dec-3-en-4-yl] ethyl carbonate,
C8 chlrofenapyr, 4-bromo-2-(4-chlorophenyl)-1-(ethoxymethyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile,
C9 deltamethrin, [(S)-cyano-(3-phenoxyphenyl)methyl] (1R,3R)-3-(2,2-dibromoethenyl)-2,2-dimethylcyclopropane-1-carboxylate,
The present invention optionally comprises agrochemically acceptable excipients including, but not limited to, dispersing agents, antifreezing agent, anti-foam agent, wetting agents, suspension aid and carriers, anti-microbial agent, thickener, colorants, quick coating agent or sticking agents (also referred to as “stickers” or “binders”),polymers, disintegrating agent, oil additive, buffering agent, and solvents.
However, those skilled in the art will appreciate that it is possible to utilize additional agrochemically acceptable excipients without departing from the scope of the present invention. The agrochemically acceptable excipient can be in the range from 0.1% to 99% of the total weight of the composition.
The amount of a composition according to the invention to be applied, will depend on various factors, such as the subject of the treatment, such as, for example plants, soil or seeds; the type of treatment, such as, for example spraying, dusting or seed dressing; the purpose of the treatment, such as, for example prophylactic or therapeutic disease control; in case of disease control or the application time. This amount of the combinations of the present invention to be applied can be readily deduced by a skilled agronomist.
The combination of the present invention is formulated in a manner which suits the specific application. The formulation is selected from Capsule suspension (CS), Dispersible concentrate (DC), Emulsifiable concentrate (EC), Emulsion, water in oil (EO), Emulsion, oil in water (EW), Micro-emulsion (ME), Oil dispersion (OD), Oil miscible flowable concentrate (oil miscible suspension (OF), Oil miscible liquid (OL), Suspension concentrate (SC), Suspo-emulsion (SE), Soluble concentrate (SL), Water dispersible granule (WG or WDG), Water soluble granule (SG), Water soluble powder (SP), Wettable powder (WP), A mixed formulation of CS and SC (ZC), A mixed formulation of CS and SE (ZE), a mixed formulation of CS and EW (ZW), Granule (GR) for soil application includes controlled release granules (CR), Jambo balls or bags (bags in water soluble pouch).
More particularly, the composition is selected from Oil dispersion (OD), Suspension Concentrate (SC), Suspo-emulsion (SE), Wettable Granule (WG), and a mixed formulation of capsule suspension CS and SC (ZC).
The inactive excipients used in various formulations are as follows:
A. Lists of inactive excipients used in Oil dispersion (OD) formulation:
The Oil Dispersion formulation (OD) of the present invention comprises agrochemically acceptable excipients including, but not limited to, wetting agent(s), wetting-spreading-penetrating agent(s), emulsifying agent(s), dispersing agent(s), stabilizer(s), antifoaming agent(s), antifreezing agent(s), solvent(s), and co solvent(s).
The Wetting agent of OD is selected from, but not limited to, ethylene oxide/propylene oxide block copolymer, polyarylphenyl ether phosphate, ethoxylated fatty alcohol, sodium dioctyl sulfosuccinate, sodium lauryl sulfate and sodium dodecyl benzene sulfonate, alkyldiphenyl sulfonates, sodium isopropyl naphthalene sulfonate, alkylnaphthalene sulfonate or mixture thereof.
The Wetting-spreading-penetrating agent of OD is selected from, but not limited to, Organosilicone surfactants includes trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, heptamethyl trisiloxane, Polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, may or may not be in modified form, may be liquid or powder form or mixture thereof.
The Emulsifying agent of OD is selected from, but not limited to, castor oil ethoxylates, alcohol ethoxylates, fatty acid ethoxylates, sorbitan ester ethoxylates, sulphosuccinate, calcium salts of dodecylbenzene sulphonate, alkylammonium salts of alkylbenzene sulphonate, alkylsulphosuccinate salts, ethylene oxide-propylene oxide block copolymers, ethoxylated alkylamines, ethoxylated alkyl phenols, polyoxyethylene sorbitan monolaurate, polyxyethylene sobitol hexaoleate, ethoxylated sorbiton ester or mixture thereof.
The Dispersing agent of OD is selected from, but not limited to, alkyl sulfonates, alkyl benzene sulfonates, alkyl aryl sulfonates, alkylphenolalkoxylates, tristyrylphenol ethoxylates, natural or synthetic fatty ethoxylate alcohols, natural or synthetic fatty acid alkoxylates, natural or synthetic fatty alcohols alkoxylates, alkoxylated alcohols (such as n-butyl alcohol poly glycol ether), block copolymers (such as ethylene oxide-propylene oxide block copolymers and ethylene oxide-butylene oxide block copolymers), fatty acid-polyalkylene glycol condensates, polyamine-fatty acid condensates, polyester condensates, salts of polyolefin condensates, sodium ligno sulfonate, sodium ploycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycolether-phosphate, oleyl-polyglycolether with ethylene oxide, tallow fattyamine polyethylene oxide, nonylphenol polyglycolether with 9-10 moles ethylene oxide or mixture thereof.
The Stabilizers/Rheology modifier of OD is selected from, but not limited to, hectorite clay, aluminium magnesium silicate, bentonite clay, silica, attapulgite clay or mixture thereof.
The Antifoaming agent of OD is selected from, but not limited to, silicone oil, silicone compound, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound, silicone antifoam emulsion, dimethylsiloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified polydimethylsiloxane or mixture thereof.
The Anti-freezing agent of OD is selected from, but not limited to, ethylene glycol, propane diols, glycerine or the urea, glycol (Monoethylene glycol, Diethylene glycol, Polypropylene glycol, Polyethylene glycol), glycerine, urea, magnesium sulfate heptahydrate, sodium chloride etc; Preservative-1,2-benzisothiazolin-3(2H)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenylphenate, 5-chloro-2-methyl-4-isothiazolin-3-one & 2-methyl-4-isothiazolin-3-one or mixture thereof.
The Solvent of OD is selected from, but not limited to, as solvent for the present formulation is selected from and not limited to vegetable oil (plant, seed or tree) or its alkylated or ethoxylated or esterified. The alkylated vegetable oil may be methylated vegetable oil or ethylated vegetable oil. The vegetable oils include olive oil, kapok oil, castor oil, papaya oil, camellia oil, sesame oil, corn oil, rice bran oil, cotton seed oil, soybean oil, groundnut oil, rapeseed-mustard oil, linseed oil, tung oil, sunflower oil, safflower oil, coconut oil. The alkyl ester of vegetable oils includes methyl ester, ethyl ester, propyl ester or butyl ester of vegetable oils. Some of the examples are methylated seed oil, polyalkyleneoxide modified polydimethylsiloxane alkylphenol ethoxylate, rapeseed oil methyl ester, rapeseed oil ethyl ester, rapeseed oil propyl esters, rapeseed oil butyl esters, soybean oil methyl ester, soybean oil ethyl ester, soybean oil propyl ester, soybean oil butyl ester, castor oil methyl ester, castor oil ethyl ester, castor oil propyl ester, castor oil butyl ester, cotton seed oil methyl ester, cotton seed oil ethyl ester, cotton seed oil butyl ester, cotton seed oil propyl ester, tall oil fatty acids esters-tallow methyl ester, tallow ethyl ester, tallow propyl ester, bio-diesel, mineral oil (aromatic solvents, isoparaffin, base solvent), fatty acid amides (e.g. C1 -C3 amines, alkylamines or alkanolamines with C6–C18 carboxylic acids), fatty acids, alkyl esters of fatty acids, methyl and ethyl oleate, methyl and ethyl soyate, alkyl benzenes and alkylnaphthalenes, polyalkylene glycol ethers, fatty acid diesters, fatty alkylamides and diamides, dialkylene carbonates, ketones and alcohols may be used as solo or mixture thereof.
The Co-solvent of OD is selected from, but not limited to, Cyclohexanone, Acetophenone, NMP, Dimethyl sulfoxide, Benzyl alcohol, Butanol, N-octanol, N-Propanol, 2-ethyl hexanol, Tetrahydro furfuryl alcohol, Isophorone, Fatty acid dimethyl amide, 2-hexylethyl lactate, Propylene carbonate or mixture thereof.
Manufacturing process for Oil dispersion (OD) formulation:
Part A-Preparation of the liquid premix (OD)
Step 1: The vegetable oil or solvent or both are charged into a vessel with an anchor stirrer.
Step 2: The emulsifier(s) and dispersing agent(s) are added under stirring condition until all the ingredients get completely dissolved.
Part B-Preparation of the slurry (OD)
Step 1: The liquid premix is charged into a second vessel which is equipped with a cooling and heating device of a high shear stirrer.
Step 2: The active ingredients are added and homogenized thoroughly. The mixture is pre-milled and a particle size distribution is achieved by the final milling, practised along with a bead mill as required by the specification.
Part C-Preparation of the thickener gel (OD)
Step 1: The vegetable/plant/seed oil or solvent is charged to the vessel which is
equipped with a high shear stirrer.
Step 2: The thickener(s) is/are gradually added throughout by mixing and maintaining high-shear. The stirring is continued until thoroughly mixed.
Step 3: The thickener activating agent(s) is/are added under stirring condition.
Further, the gel is allowed to get swell whilst maintaining the mixing.
Part D-Preparation of the final formulation (OD)
Step 1: The thickener gel is added and the mixture is dispersed by using a high shear stirrer.
Step 2: The recommended wetting and spreading agent(s) or adjuvant(s) (silicone or non-silicone based) are finally added to this formulation and dispersed by using high shear stirrer.
Step 3: The finished formulation is checked with specification.
Step 4: The material is packed in its required package sizes when approved.
B. Lists of inactive excipients used in Suspension Concentrate (SC) formulation:
The Suspension Concentrate formulation (SC) of the present invention comprises agrochemically acceptable excipients including, but not limited to, wetting agent(s), wetting-spreading-penetrating agent(s), dispersing agent(s), suspending agent(s), antifoaming agent(s), antifreezing agent(s), preservative(s), thickener(s) and humectants(s).
The Wetting agent of SC is selected from, but not limited to, ethylene oxide/propylene oxide (EO/PO) block copolymer, poly aryl phenyl ether phosphate, polyalkoxylated butyl ether, ethoxylated fatty alcohol, sodium dioctyl sulfosuccinate, sodium lauryl sulfate and sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonates, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate. Ethoxylated alcohol includes natural fatty alcohol (lauryl alcohol ethoxylate, lauryl alcohol alkoxylate), synthetic alcohol ethoxylate (tridecyl alcohol ethoxylate, 2-ethyl hexanol, 2-propylheptanol, isodecyl alcohol or mixture thereof.
The Wetting-spreading-penetrating agent of SC is selected from, but not limited to, trisiloxane ethoxylate, heptamethyl trisiloxane, modified form includes polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, polyalkyleneoxide modified trisiloxane, polyalkyleneoxide modified polydimethylsiloxane, may be liquid or powder form and methylated seed oil or mixture thereof.
The Dispersing agent of SC is selected from, but not limited to, Naphthalenesulfonic acid, sodium salt condensate with formaldehyde, alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium ligno sulfonate, sodium polycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propylene oxide-ethylene oxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycol ether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycol ether-phosphate, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, nonylphenol polyglycol ether with 9-10 moles ethylene oxide, Polymethyl methacrylate-polyethylene glycol graft copolymer, Ethylene-propylene oxide block copolymer or mixture thereof.
The Suspending agent of SC is selected from, but not limited to, aluminium magnesium silicate, bentonite clay, silica, attapulgite clay or mixture thereof.
The Antifoaming agent of SC is selected from, but not limited to, silicone antifoam emulsion, dimethyl siloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids or mixture thereof.
The Anti-freezing agent of SC is selected from, but not limited to, ethylene glycol, propane diols, glycerin or the urea, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol), glycerin, urea, magnesium sulfate heptahydrate, sodium chloride or mixture thereof.
The Preservatives of SC is selected from, but not limited to, 1,2-benzisothiazolin-3(2H)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenyl phenate, 5-chloro-2-methyl-4-isothiazolin-3-one & 2-methyl-4-isothiazolin-3-one or mixture thereof.
The Thickeners of SC is selected from, but not limited to, xanthan gum, PVK, carboxymethyl celluloses, polyvinyl alcohols, gelatin, sodium carboxymethylcellulose, hydroxyethyl cellulose, sodium polyacrylate, modified starch, acacia gum or mixture thereof.
The Humectant of SC is selected from, but not limited to, urea, humic acid, glycerol, lactose or mixture thereof.
Manufacturing process for Suspension Concentrate (SC) formulation:
Step 1: Gel preparation: A required quantity of water is charged to a vessel which is equipped with a high shear stirrer whilst the agitation is initiated. A required amount of preservative(s) is/are added and mixed to form a homogenous mixture. A required amount of thickener(s) is/are added and mixed vigorously to achieve wetness.
Step 2: A required quantity of water is charged to a vessel which is equipped with a bulk agitator and a high shear homogenizer; initiated the agitation. Further, a required amount of an anti freezing agent(s) is/are added and mixed to achieve uniformity. Moreover, the antifoaming agent(s) is/are added whilst ensuring that it is well dispersed. The wetting and dispersing agent(s) is/are added and mixed to achieve uniformity whilst ensuring that the dispersing agent(s) is/are fully dispersed.
Step 3: The active ingredients are added and the agitation of the vessel contents are continued until all the compounds get dissolved. The pre-mix is milled through a colloid mill and subsequently through a dyno mill to meet the specified particle size.
Step 4: The remaining antifoaming agent(s) is/are added to this SC mill base to a vessel which is equipped with the bulk agitator and mixed to achieve uniformity. The required amount of 2% aqueous pre-gel and suspending agent(s) is/are added and the agitation is continued until the formulation is homogeneous and has reached the target viscosity.
Step 5: The final product is submitted for QC’s approval.
Step 6: The material is packed in its required package sizes when received approval.
C. Lists of inactive excipient used in Suspo Emulsion (SE) formulation:
The Suspo Emulsion (SE) of the present invention comprises agrochemically acceptable excipients including, but not limited to, solvent(s), emulsifier(s), stabilizer(s), antifreezing agent(s), antifoaming agent(s), suspending agent(s), wetting agent(s), wetting spreading- penetrating agent(s), preservative(s), thickener(s), dispersing agent(s), buffering agent(s) and humectants(s).
The Solvent of SE is selected from, but not limited to, water, water soluble alcohols and dihydroxy alcohol ethers. Water soluble alcohol or lower alcohol (1-4 carbon atoms) includes-methanol, ethanol, n-propanol, isopropanol, n-butanol, tert-butanol. Macromolecular alcohol includes polyethylene glycol, sorbitol, glucitol etc., dihydroxy alcohol ethers includes dihydroxy alcohol alkyl ether or dihydroxy alcohol aryl ethers. The examples of dihydroxy alcohol alkyl ether include ethylene glycol methyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, di-propylene glycol methyl ether, ethylene glycol ethyl ether, diethylene glycol ethyl ether, propylene glycol ethyl ether, di-propylene glycol ethyl ether, etc. The examples of dihydroxy alcohol aryl ethers include ethylene glycol phenyl ether, 5 diethylene glycol phenyl ether, propylene glycol phenyl ether, di-propylene glycol phenyl ether, and the like. Any of the mentioned solvent can be used either alone or in combinations thereof. Hyrdocarbons includes n-pentane, hexane(s), cyclohexane, methylcyclohexane, heptane, isooctane, benzene, toluene, xylene(s), isophorone and ester solvents such as methyloleate, dimethylamide and morpholineamide derivatives of C6-C16 fatty acids, and mono-alkylene carbonates such as ethylene carbonate, propylene carbonate and butylene carbonates, dimethylsulfoxide (DMSO), 2-ethylhexanol and n-butanol, n-alkylpyrrolidones, fatty acid dimethyl esters, fatty acid esters, dibasic esters, aromatic hydrocarbons and/or aliphatic hydrocarbons, one or more dimethylamides, such as C8-dimethylamide, C10-dimethylamide, C12-dimethylamide, ethylene glycol, propylene glycol, polyalkylene glycols, aromatic hydrocarbons, methylpyrrolidinone (NMP); dimethylformamide (DMF); dimethylisosorbide (DMI); isophorone; acetophenone; 1,3-dimethyl-2-imidazolidonone; lactate esters; dimethyl and diethylcarbonates; alcohols including methanol; ethanol; iso-propanol; n-propanol; n-butanol; iso-butanol; and tert-butanol; Methyl L-lactate, 2-Ethylhexyl L-lactate, Ethyl L-lactate, n-Butyl L-lactate, Octyl phenol ethoxylates, aromatic solvent C9 mixture thereof.
The Emulsifier of SE is selected from, but not limited to, Emulsifiers containing salts of dodecylbenzene sulphonate, e.g. Ca-salts or amine salts, and sulphonates of other C11-C16 alkylbenzenes, alkylether sulphates, alkylphenoletherphosphates and ester phosphates; non-ionic surfactants such as alkoxylated alcohols and alkylphenols, ethoxylated fatty acids, ethoxylated vegetable oils, e.g. ethoxylated castor oil, fatty acid esters, e.g. of sorbitol, and their ethoxylated derivatives, ethoxylated amines, and condensates of glycerol; and catanionic emulsifiers such as a cationic amine, optionally in combination with an alkylsulphonate or ether sulphonate or ether phosphate, alkoxylated alcohols; alkoxylated alkylphenols; ethoxylated fatty acids; ethoxylated vegetable oils; ethoxylated tristyrylphenol (tristyrlphenol with 16 moles EO), tristyrylphenol-polyglycolether-phosphate, fatty acid esters of sorbitol and ethoxylated derivatives thereof; ethoxylated amines and condensates of glycerol; sulfonated alkylbenzenes in the range C11-C16 and salts thereof; alkylether sulphates; alkyletherphosphates; alkylphenoletherphosphates; or combinations thereof; salts of phosphate esters of ethoxylated tristyrylphenol; salts of sulphated ethers of ethoxylated tristyrylphenol; or a catanionic system, wherein a cationic amine is present in combination with an alkylsulphonate, an alkylethersulphonate, an ether sulphate, or an ether phosphate such as an alkyletherphosphate, nonylphenol polyethoxy ethanols, castor oil polyglycol ethers, polyadducts of ethylene oxide and polypropylene, tributyl phenoxy polyethoxy ethanol, octyl phenoxy polyethoxy ethanol, polyarylphenyl anionic ether sulfate, ammonium salt or mixture thereof.
The Stabilizer of SE is selected from, but not limited to, butylated hydroxytoluene (BHT) and epoxidized soybean oil (ESBO), Epichlorhydrin or mixture thereof.
The Anti-freezing agent is selected from, but not limited to, ethylene glycol, propane diols, glycerine or the urea, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol), glycerine, urea, magnesium sulfate heptahydrate, sodium chloride or mixture thereof.
The Antifoaming agent of SE is selected from, but not limited to, silicone oil, silicone compound, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound, silicone antifoam emulsion, dimethylsiloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified polydimethylsiloxane or mixture thereof.
The Suspending agent of SE is selected from, but not limited to, aluminum magnesium silicate, bentonite clay, silica, silicone dioxide, attapulgite clay or mixture thereof.
The Wetting agent of SE is selected from, but not limited to, Ethylene oxide/propylene oxide block copolymer, Polyarylphenyl ether phosphate, Ethoxylated Fatty Alcohol, Sodium dioctyl sulfosuccinate, sodium lauryl sulphate and sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonates, sodium isopropyl naphthalene sulfonate, Alkyl naphthalene sulfonate, Octyl phenol ethoxylate, alkyl phenol ethoxylate or mixture thereof.
The Wetting-spreading-penetrating agent of SE is selected from, but not limited to, Organosilicone surfactants includes trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, heptamethyl trisiloxane, Polyalkyleneoxide modified heptamethyl trisiloxane, heptamethyl trisiloxane ethoxylate, polyether modified polysiloxane, 10 mole ethylene oxide adduct of octylphenol, may or may not be in modified form, may be liquid or powder form or mixture thereof.
The Preservatives of SE is selected from, but not limited to, propionic acid and its sodium salt, sorbic acid and its sodium or potassium salt, benzoic acid and its sodium salt, p-hydroxy benzoic acid sodium salt; methyl p-hydroxy benzoate; and biocide such as sodium benzoate, 1,2-benzisothiazoline-3-one, 2-methyl-4-isothiazolin-3-one, 5-chloro-2- methyl-4-isothiazolin-3-one, potassium sorbate, para hydroxy benzoates or mixtures thereof.
The Thickeners of SE is selected from, but not limited to, Thickening, gelling, and anti-settling agents generally fall into two categories, namely water-insoluble particulates and water-soluble polymers. It is possible to produce suspension concentrate formulations using clays and silicas. Examples of these types of materials, include, but are limited to, montmorillonite, e.g. bentonite; magnesium aluminum silicate; and attapulgite. Water-soluble polysaccharides have been used as thickening-gelling agents for many years. The types of polysaccharides most commonly used are natural extracts of seeds and 15 seaweeds are synthetic derivatives of cellulose or mixtures thereof. Examples of these types of materials include, but are not limited to, guar gum; locust bean gum; carrageenam; xanthan gum; alginates; methyl cellulose; sodium carboxymethyl cellulose (SCMC); hydroxyethyl cellulose (HEC) or mixtures thereof. Other types of anti-settling agents are based on modified starches, polyacrylates, polyvinyl 20 alcohol and polyethylene oxide or mixture thereof.
The Dispersing agent of SE is selected from, but not limited to, polyesters, polyamides, poly- carbonates, polyurea and polyurethanes, acrylic polymers, acrylic graft copolymer, styrene copolymers, butadiene copolymers, polysaccharides such as starch and cellulose derivatives, vinylalcohol, vinylacetate and vinylpyrrolidone polymers and copolymers, polyethers, epoxy, phenolic and melamine resins, polyolefins and define copolymers and mixtures thereof. Examples of preferred polymers are acrylate polymers such as poly(methacrylate), poly(ethyl methacrylate), poly(methylmethacrylate), acrylate copoylmers and styrene-acrylic copolymers as defined herein below, poly(styrene-co maleic anhydride), cellulosic polymers such as ethyl cellulose, cellulose acetate, cellulose acetatebutyrate, acetylated mono, di, and triglycerides, poly(vinylpyrrolidone), vinyl acetate polymers and copolymers, poly(alkylene glycol), styrene butadiene copolymers, poly(orthoesters), alkyd resins, and mixtures of two or more of these. Polymers that are biodegradable are also useful in the present invention. As used herein, a polymer is biodegradable if is not water soluble, but is degraded over a period of several weeks when placed in an application environment. Examples of biodegradable polymers that are useful in the present invention include biodegradable polyesters, starch, polylactic acid starch blends, polylactic acid, poly(lactic acid-glycolic acid) copolymers, polydioxanone, cellulose esters, ethyl cellulose, cellulose acetate butyrate, starch esters, starch esteraliphatic polyester blends, modified corn starch, polycaprolactone, poly(namylmethacrylate), wood rosin, polyanhydrides, polyvinylalcohol, polyhydroxybutyratevalerate, biodegradable aliphatic polyesters, and polyhydroxybutyrate or mixtures thereof. The examples of dispersing agents are alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium salt of alkyl naphthalene sulfonate, sodium ligno sulfonate, sodium ploycarboxylate, EO/PO block copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycolether-phosphate, oleyl-polyglycolether with ethylene oxide, tallow fattyamine polyethylene oxide, nonylphenol polyglycolether with 9-10 moles ethylene oxide, butyl Polyalkylene oxide block copolymer or mixture thereof.
The Buffering agent of SE is selected from, but not limited to, calcium hydroxyapatite, Potassium Dihydrogen Phosphate, Sodium Hydroxide, carbonated apatite, calcium carbonate, sodium bicarbonate, tricalcium phosphate, calcium phosphates, carbonated calcium phosphates, amine monomers, lactate dehydrogenase and magnesium hydroxide or mixture thereof.
The Humectant of SE is selected from, but not limited to, urea, humic acid, glycerol, lactose or mixture thereof.
Manufacturing process for Suspo Emulsion (SE) formulation:
Step 1: Gel preparation: A required quantity of water is charged to a vessel which is equipped with a high shear stirrer whilst the agitation is initiated. The required amount of preservative(s) is/are added and mixed to achieve homogeneity. Further, a required amount of thickener(s) is/are added and mixed vigorously to achieve full wetness.
Step 2: Oil phase: The solvent(s) is/are charged into the vessel and then the active is slowly added and if required, it is heated for 50°C so that the active ingredients can be dissolved in the solvent and followed by addition of emulsifier(s).
Step 3: The agitation is initiated when a required quantity of water is charged to a vessel which is equipped with a bulk agitator and a high shear homogenizer. A required amount of anti freezing agent(s) is/are added and mixed to achieve a uniform mixture. The antifoaming agent(s) is/are added and ensured that it is well dispersed. The wetting and dispersing agent(s) is/are added and mixed to achieve uniform mixture and ensured that the dispersing agent is fully dispersed.
Step 4: The active ingredients are added in the vessel and agitated till entire compounds get dissolved. The pre-mix is milled through a colloid mill and subsequently through a dyno mill to achieve a specified particle size.
Step 5: The remaining antifoaming agent(s) is/are added in the mill base to a vessel which is equipped with bulk agitator and mixed to achieve uniformity.
Step 6: An addition of an oil phase in an aqueous phase is performed and stirred for 30 minutes by using homogenizer.
Step 7: A required amount of aqueous pre-gel and suspending agent(s) are added. A homogenous mixture and a target viscosity are achieved by continuous agitation.
Step 8: The final product is submitted for QC’s approval.
Step 9: The material is packed in its required package sizes when approved.
D. Lists of inactive excipient used in WG (Wettable Granule)/WDG (Water
Dispersible Granule) formulation:
The wettable granule/ water dispersible granule formulation (WG/WDG) of the present invention comprises agrochemically acceptable excipients including, but not limited to, dispersing agent(s), wetting agent(s), antifoaming agent(s), carrier(s), disintegrating agent(s) and humectants(s).
The Dispersing agents of WG/WDG is selected from, but not limited to, alkylnaphthalene sulfonate sodium salt, sodium polycarboxylate, naphthalene sulfonic acid, sodium salt condensates with formaldehyde, polyalcoxylated alkylphenol, naphthalene sulfonic acid formaldehyde condensate, methyl naphthalene-formaldehyde-condensate sodium salt, naphthalene condensates, lignosulfonates, polyacrylates and phosphate esters, calcium lignosulfonate, lignin sulfonate sodium salt, modified sodium lignosulphonate, modified polyacrylate copolymer or mixture thereof.
The Wetting agents of WG/WDG is selected from, but not limited to, sodium N-methyl-N-oleoyl taurate, alkylated naphthalene sulfonate, sodium salt, mixture of isomers of dibutyl naphthalene sulphonic acid sodium salt, sodium di-isopropyl naphthalene sulphonate, sodium Lauryl sulfate, dioctyl sulfate, alkyl naphthalene sulfonates, phosphate esters, sulphosuccinates and non-ionic such as tridecyl alcohol ethoxylate, alkyl or alkaryl sulfonates such as alkylbenzene sulfonates, alpha olefin sulfonate and alkyl naphthalene sulfonates, ethoxylated or non-ethoxylated alkyl or alkaryl carboxylates, alkyl or alkaryl phosphate esters, alkyl polysaccharide, di or mono alkyl sulfosuccinate derivatives, alpha olefin sulfonates, alkyl naphthalene sulfonates, dialkyl sulphosuccinates, butyl, dibutyl, isopropyl and di-isopropyl naphthalene sulfonate salts, C12 alkyl benzene sulfonate or C10-C16 alkyl benzene sulfonate, organosilicons surfactants includes trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, trisiloxane heptamethyl, Polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, may or may not be in modified form, may be liquid or powder form or mixture thereof.
The Antifoaming agent of WG/WDG is selected from, but not limited to, polydimethylsiloxane.
The Carrier of WG/WDG is selected from, but not limited to, china clay, silica, lactose anhydrous, ammonium sulfate, sodium sulfate anhydrous, corn starch, urea, EDTA, urea formaldehyde resin, diatomaceous earth, kaolin, bentonite, kieselguhr, fuller's earth, attapulgite clay, bole, loess, talc, chalk, dolomite, limestone, lime, calcium carbonate, powdered magnesia, magnesium oxide, magnesium sulphate, sodium chloride, gypsum, calcium sulphate, pyrophyllite, silicates and silica gels; fertilizers such as, for example, ammonium sulphate, ammonium phosphate, ammonium nitrate and urea; natural products of vegetable origin such as, for example, grain meals and flours, bark meals, wood meals, nutshell meals and cellulosic powders; and synthetic polymeric materials such as, for example, ground or powdered plastics and resins, bentonites, zeolites, titanium dioxide, iron oxides and hydroxides, aluminium oxides and hydroxides, or organic materials such as bagasse, charcoal, or synthetic organic polymers or mixture thereof.
The Disintegrating agent of WG/WDG is selected from, but not limited to, citric acid, succinic acid or the sodium bicarbonate or mixture thereof.
The Humectant of WG/WDG is selected from, but not limited to, urea, humic acid, glycerol, lactose or mixture thereof.
Manufacturing process for Wettable granule/ Water Dispersible Granule (WG/ WDG):
Step 1: An exact weight of active ingredients is considered and a required quantity of binder(s) and surfactant(s) is/are added in the blender and mixed to achieve a complete homogenization.
Step 2: The homogenized mixture is milled to achieve required wet sieve and post blended to attain homogeneity.
Step 3: The above described homogenous material is passed through an extruder for granulation to achieve granular of require size.
Step 4: The wet granules are transferred through fluidized bed drier to remove excess moisture.
Step 5: The wet granules are further transferred to vibro shifter and further graded using vibrator screens.
Step 6: The final material is collected from the vibro shifter into drum.
Step 7: The sample is sent to QC for an approval.
Step 8: The material is transferred into the different size of drums when received an approval from QC.
E. List of inactive excipients used in the ZC formulation [mixed formulation of CS+SC]:
The mixed formulation (ZC) is a mixture of Capsule Suspension (CS) and Suspension Concentrates (SC). The mixed formulation (ZC) of the present invention comprises agrochemically acceptable excipients including, but not limited to, wall forming material(s) 1, wall forming material(s) 2, dispersing agent(s), wetting agent(s), wetting-spreading-penetrating agent(s), solvent(s), thickner(s), suspending agent(s), antifoaming agent(s), antifreezing agent(s), preservative(s) and buffering agent(s). Since the excipients for SC are the same, only the excipients for CS are listed here.
The Wall forming material 1 of ZC is selected from, but not limited to, Tetramethylene diisocyanate, pentamethylene diisocyanate, hexamethylene diisocyanate, toluene diisocyanate, 4,4-diphenylmethene diisocyanate (MDI), polymethylene polyphenylene isocyanate, 2,4,4’-diphenyl ether tri-isocyanate, 3,3’-dimethyl-4,4’-diphenyl diisocyanate, 3,3’-dimethoxy-4,4’-diphenyl diisocyanate, 1,5-naphthylene diisocyanate and 4,4’4"-triphenylmethane tri-isocyanate, toluene diisocyanate or polymethylene polyphenylisocyanate, polyurethane comprising of polyfunctional iso cyanate and a polyamine in polarized form or mixture thereof.
The Wall forming material 2 of ZC is selected from, but not limited to, Diethylene triamine, Ammonia, hexamine, ethylenediamine, propylene-1,3-diamine, tetramethylenediamine, pentamethylenediamine, 1,6-hexamethylenediamine, diethylenetriamine, triethylenetetramine, tetra ethylene pentamine, pentaethylenehexamine, 4,9-dioxadodecane-1, 12-diamine, 1,3- phenylenediamine, 2,4- and 2,6-toluenediamine and 4,4’-diaminodiphenylmethane, 1,3-phenylenediamine, 2,4- and 2,6-toluenediamine, 4,4'-diaminodiphenylmethane, 1,5-diaminonaphthalene, 1,3,5-triaminobenzene, 2,4,6-triaminotoluene, 1,3,6-triaminonaphthalene, 2,4,4'-triaminodiphenyl ether, 3,4,5-triamino-1,2,4-triazole and 1,4,5,8-tetraminoanthraquinone or mixture thereof.
The Dispersing agents of ZC is selected from, but not limited to, Ethoxylated lignosulfonic acid salts, lignosulfonic acid salts, oxidized lignins, lignin salts, salts of styrenemaleic anhydride copolymers, polyvinyl alcohol, salts of partial esters of styrene-maleic anhydride copolymers, partial salts of polyacrylic acid and partial salts of polyacrylic acid terpolymers. the surfactant is lignosulfonate of calcium or sodium or mixtures thereof or a modified kraft lignin with a high sulfonic acid group , dibutylnaphthalenesulfonic acid ,fatty acids, alkyl- and alkylarylsulfonates, alkyl sulfates, lauryl ether sulfates and fatty alcohol sulfates, and salts of sulfated hexa-, hepta- and octadecanols and of fatty alcohol glycol ethers, condensates of sulfonated naphthalene and its derivatives with formaldehyde, condensates of naphthalene or of the naphthalenesulfonic acids with phenol and formaldehyde, polyoxyethylene octylphenol ether, ethoxylated isooctyl-, octyl- or nonylphenol, alkyl phenyl polyglycol ethers, tributyl phenyl polyglycol ethers, alkyl aryl polyether alcohols, is tridecyl alcohol, fatty alcohol/ethylene oxide condensates, ethoxylated castor oil, polyoxyethylene alkyl ethers or polyoxypropylene alkyl ethers, lauryl alcohol polyglycol ether acetate, sorbitol esters, lignin-sulphite waste liquors, and proteins, denatured proteins, polysaccharides , ammonium salts of sulfonates, sulfates, phosphates or carboxylates, alkylarylsulfonates, diphenyl sulfonates, alpha-olefin sulfonates, sulfonates of fatty acids and oils, sulfonates of ethoxylated alkylphenols, sulfonates of condensed naphthalene, sulfonates of dodecyl- and tridecyl benzenes, sulfonates of naphthalene and alkylnaphthalenes, sulfosuccinates or sulfosuccinates, alkoxylates, N-alkylated fatty acid amides, amine oxides, esters or sugar-based surfactants, alkylphenols, amines (e.g. tallow amine), amides, aryl phenols, fatty acids or fatty acid esters which have been alkoxylated. Ethylene oxide and/or propylene oxide may be employed for the alkoxylation, preferably ethylene oxide, polyethylene oxide and polypropylene oxide, polyacids or polybases, acrylic graft polymer or mixture thereof.
The Wetting agent of ZC is selected from, but not limited to, Ethylene oxide/propylene oxide block copolymer, Polyarylphenyl ether phosphate, Ethoxylated Fatty Alcohol, Sodium dioctyl sulfosuccinate, sodium lauryl sulphate and sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonates, sodium isopropyl naphthalene sulfonate, Alkyl naphthalene sulfonate, Octyl phenol ethoxylate, alkyl phenol ethoxylate or mixture thereof.
The Wetting-spreading-penetrating agent of ZC is selected from, but not limited to, Organosilicone surfactants includes trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, heptamethyl trisiloxane, Polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane, 10 mole ethylene oxide adduct of octylphenol, may or may not be in modified form, may be liquid or powder form or mixture thereof.
The Solvent of ZC is selected from, but not limited to, Hydrocarbon solvent such an aliphatic, cyclic and aromatic hydrocarbons (e.g. toluene, xylene, paraffin, tetrahydronaphthalene, alkylated naphthalene or their derivatives, mineral oil fractions of medium to high boiling point (such as kerosene, diesel oil, coal tar oils)); a vegetable oil such as corn oil, rapeseed oil; a fatty acid ester such as C1-C10-alkylester of a C10-C22-fatty acid; or, methyl- or ethyl esters of vegetable oils such as rapeseed oil methyl ester or corn oil methyl ester, acetophenone, 2-Heptanon , 3-heptanone, 2-hexanone, 5-methyl-2-hexanone , 5-methyl-3-heptanone, 3-methyl-2-hexanone , 4-methyl-2-hexanone, 2-methyl-3-hexanone, 4-methyl-3-hexanone , 5-methyl-3-hexanone , 3-ethyl-2-pentanone , 3,3-dimethyl-2-pentanone , 3,4-dimethyl-2-pentanone, 4,4-dimethyl-2-pentanone , 2,2-dimethyl-3-pentanone , 2,4-dimethyl-3-pentanone, 2-octanone , 2,5-dimethyl-3-hexanone , 2,2-dimethyl-3-hexanone , 3,3-dimethyl-2-hexanone, 3,4-dimethyl-2-hexanone, 4,4-dimethyl-3-hexanone , 3-ethyl-4-methyl-2-pentanone , 2-methyl-3-heptanone, 2-methyl-4-heptanone, 3-methyl-2-heptanone, 3-methyl-4-heptanone, 5-methyl-3-heptanone, 6-methyl-2-heptanone , 6-methyl-3-heptanone, 3-octanone, 4-octanone, 2,2,4-trimethyl-3-pentanone , 3-ethyl-3-methyl-2-pentanone, 5-methyl-2-heptanone, isoprene or mixture thereof.
The Thickener of ZC is selected from, but not limited to, Xanthan gum ,Carboxy methyl cellulose, Attapulgite clay, Bentonite clay or mixture thereof.
The Suspending agent of ZC is selected from, but not limited to, Aluminium Magnesium Silicate, Bentonite clay, Silica, Attapulgite clay or mixture thereof.
The Antifoaming agent of ZC is selected from, but not limited to, silicone oil, silicone compound, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound, Silicone antifoam emulsion, Dimethyl siloxane, Polydimethyl siloxane, Vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified polydimethylsiloxane or mixture thereof.
The Antifreezing agent of ZC is selected from, but not limited to, ethylene glycol, propane diols, glycerine or the urea, Glycol (Monoethylene glycol, Diethylene glycol, Polypropylene glycol, Polyethylene glycol), Glycerine, Urea, Magnesium sulphate heptahydrate, sodium chloride or mixture thereof.
The Preservative of ZC is selected from, but not limited to, 1,2-benzisothiazolin-3(2H)-one, sodium salt, Sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, Formaldehyde, Sodium o-phenyl phenate, 5-chloro-2-methyl-4-isothiazolin-3-one & 2-methyl-4-isothiazolin-3-one or mixture thereof.
The Buffering agent of ZC is selected from, but not limited to, Sodium hydroxide, potassium hydroxide, acetic acid, sulphuric acid, hydrochloric acid, ortho phosphoric acid, ammonium hydroxide or mixture thereof.
The Emulsifier of ZC is selected from, but not limited to,Alkylbenzene sulfonate calcium salts, Tristyrylphenol polyethoxyester phosphate or mixture thereof.
Manufacturing process for Capsule Suspension (CS):
Step 1-Aqueous Phase-Charge water to a stainless-steel vessel equipped with a high speed stirrer. Under agitation, add the wetting agent, dispersing agent 1and dispersing agent 2 into the vessel. Now add 50% quantity of antifoam to avoid foam generation in this vessel.
Step 2-Organic Phase-Charge heavy aromatic hydrocarbons solvent into second stainless-steel reactor. Then, slowly add melted active ingredient into the reactor. Afterwards, charge wall forming material 1 material to the reactor. Continue mixing. Cool the reactor contents to room temperature.
Step 3-Start the high shear disperser of aqueous phase and charge the ‘Organic Solution’ into the ‘Aqueous Phase Solution’ under gravity in specific rate so that required particle size can be achieved and continue to shear for 30 min. Then, start heating the reactor to around 50 °C and stir the formulation under slow rpm for 3-4 hours so that Polymerization reaction gets completed.
Step 4-Now add wall forming material 2 so that residual wall forming material 1 can be consumed and stir for 1 more hour at the same temperature and if required add half quantity of antifoam to remove foam generating due to CO2 during reaction.
Step 5-After the wall polymerization reaction, increase the agitator to high speed. Add the rest half quantity of antifoam to the formulation. Under slight vacuum, allow the mixture to de-gas for approximately 30 minutes to remove CO2 from the solution. Add the linear polysaccharide, preservative and in last freezing agent and mix for some minutes. Add buffering agent for pH adjustment and mix well.
Step 6-Final product is sent for QC approval.
Step 7-After approval, material is packed in required pack sizes.
EXAMPLES
The present invention has been described with reference to specific embodiment which is merely illustrative and not intended to limit the scope of the invention as defined in the present complete specification.
Biological Examples:
The synergistic pesticide action of the inventive mixtures can be demonstrated by the experiments below. A synergistic effect exists wherever the action of a combination (ready-mix) or tank mix of active ingredient is greater than the sum of the action of each of the components alone. Therefore, a synergistically effective amount or an effective amount of a synergistic composition or combination is an amount that exhibits greater pesticide activity than the sum of the pesticide activities of the individual components.
In the field of agriculture, it is often understood that the term “synergy” is as defined by Colby S.R. in an article entitled “ Calculation of the synergistic and antagonistic responses of herbicide combinations” published in the journal Weeds, 1967, 15, p.20-22, incorporated herein by reference in its entirety. The action expected for a given combination of two or three active components can be calculated as follows:
The objective of the present studies was to study the synergism and benefits of present compositions.
Example 1: Bio efficacy against insect-pests infesting chilli crop.
Crop : Chilli
Number of Treatments: 12
Plot size : 42 sq.m. (m2)
Crop stage : 67 days after transplanting.
Method of application: foliar spray with battery operated backpack sprayer.
Water volume : 460 liter per hectare
Observation Methods:
Thrips (mixed infestation of Scirtothrips dorsalis and Thrips parvispinus): Count the number of live thrips by shaking the twigs on black piece of paper. Record the observations from 3 twigs per plant and 10 plants per plot on 7 and 14 DAA (days after application). Calculate thrips control (%) as observed control and apply Colby’s formula to calculate synergism.
Whitefly (Bemisia tabaci): Count the number of live whitefly per leaf, three leaves per plant. Record the observations from 10 per plot on 7th DAA (days after application). Calculate whitefly control (%) as observed control and apply Colby’s formula to calculate
Fruit borer (Helicoverpa armigera) larvae: Count the number of live larvae per plant. Record observations from 10 plants per plot, calculate larval control (%) by using given Formula.
Healthy Fruit count: Count the number of healthy marketable fruits per plant. Record the observations from 10 plants per plot and calculate increase (%) in healthy marketable fruits over UTC (untreated check).
Composition of Compound A 14% + Compound B 1.44% + Compound C1 20% SC
[T1 of Ex. 1]
Chemical composition Function percent (% w/w)
Compound A a.i. Compound A 14.00
Compound B a.i. Compound B 1.44
Compound C1 a.i. Compound C1 20.00
Methylated seed oil, polyalkyleneoxide modified trisiloxane Super wetting-spreading-penetrating agent 5.00
Polymethyl methacrylate-polyethylene glycol graft copolymer Dispersing agent I 3.00
Ethylene-propylene oxide block copolymer Dispersing agent II 1.50
Sodium naphthalene sulphonate formaldehyde condensates Dispersing agent III 0.50
Fatty Alcohol Ethoxylate Wetting agent 2.00
Aluminum magnesium silicate Suspending agent 0.50
Polydimethylsiloxane Anti foaming agent 0.30
1,2-Benzisothiazol-3(2H)-one Preservative 0.20
1,2-Polypropylene glycol Anti freezing agent 5.00
Xanthan gum Thickener 0.20
Diluent water 46.36
Total 100.00
Active ingredient on 100% purity basis
Storage Stability: Composition of Compound A 14% + Compound B 1.44% + Compound C1 20% SC
[T1 of Ex. 1]
Laboratory storage stability for 14 days [T1 of Ex. 1]
Parameters Specification Initial At 54±2 0C At 0±2 0C
Compound A content ( %, w/w) 13.30 to 14.70 14.20 14.19 14.20
Compound B content (%, w/w) 1.37 to 1.58 1.51 1.50 1.51
Compound C1 content (%, w/w) 19.00 to 21.00 20.24 20.23 20.24
Compound A suspensibility (%) 80 94.45 94.39 94.45
Compound B suspensibility (%) 80 92.42 92.38 92.42
Compound C1 suspensibility (%) 80 95.12 95.08 95.12
pH range (1% aq. Suspension) 5.0 to 8.0 6.75 6.77 6.75
Pourability (%) 95 98.45 98.44 98.45
Specific gravity 1.05-1.15 1.08 1.08 1.08
Viscosity at spindle no.62,20 rpm 350-800 cps 490 494 494
Particle size (micron) D50<3, D90<10 1.8,6.1 1.9,6.2 1.8,6.1
Persistent foam ml (after 1 minute) max. 60 Nil Nil Nil
Room temperature storage stability up to 12 months [T1 of Ex. 1]
Parameters Specification 1 month 6 month 12 month
Compound A content ( %, w/w) 13.30 to 14.70 14.20 14.19 14.18
Compound B content (%, w/w) 1.37 to 1.58 1.51 1.50 1.50
Compound C1 content (%, w/w) 19.00 to 21.00 20.24 20.23 20.22
Compound A suspensibility (%) 80 94.45 94.44 94.44
Compound B suspensibility (%) 80 92.42 92.41 92.40
Compound C1 suspensibility (%) 80 95.12 95.10 95.08
pH range (1% aq. Suspension) 5.0 to 8.0 6.75 6.76 6.77
Pourability (%) 95 98.45 98.44 98.42
Specific gravity 1.05-1.15 1.08 1.08 1.08
Viscosity at spindle no.62,20 rpm 350-800 cps 490 492 494
Particle size (micron) D50<3, D90<10 1.8,6.1 1.9,6.2 1.9,6.2
Persistent foam ml (after 1 minute) max. 60 Nil Nil Nil
The Composition of Compound A 14% + Compound B 1.44% + Compound C1 20% SC meets the all inhouse specifications for storage stability studies in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).
Manufacturing process for 100 kg batch of Compound A 14% + Compound B 1.44% + Compound C1 20% SC [T1 of Ex. 1]
Step 1: Preparation of 2% Gum Solution: Xanthan gum (2.0 kg) and 1,2-benzisothiazoline-3-one (2.0 kg) was charged into water (96 kg) and homogenized. It was made 12 to 18 hours prior to use.
Step 2: DM water (36.36 kg) and 1,2-propylene glycol (5 kg) was charged into designated vessel and mixed thoroughly.
Step 3: Half quantity of Polydimethylsiloxane (0.15 kg) was added and mixed well.
Step 3: Sodium naphthalene sulphonate formaldehyde condensates (0.5 kg), Ethylene-propylene oxide block copolymer (1.5 kg) and Aluminum magnesium silicate (0.5 kg) were added into the vessel having water and the contents were homogenised for 45 to 60 minutes using high shear homogeniser.
Step 4: Then Compound A (14 kg), Compound B (1.44 kg) and Compound C1 (20 kg) was added to this premix slowly and homogenised to get uniform slurry ready for grinding.
Step 5: Before grinding half the quantity of Polydimethylsiloxane (0.15 kg) was added and then material was subjected to grinding in Dyno mill till desired particle size is achieved.
Step 6: The remaining Polydimethyl siloxane (0.15 kg) antifoam was added after grinding process completes and before sampling for in process analysis.
Step 7: Finally 2% Xanthum gum solution (10 kg) and Methylated seed oil, polyalkyleneoxide modified trisiloxane (5 kg) was added to this formulation and homogenized for 30 minutes.
Step 8: Final formulation was sent to QC for quality check.
Table 1: Treatment details [Ex1]
S.No. Treatment compositions Rate (ml or g per hectare) gram actives per hectare
T1 Compound A 14%+ Compound B 1.44%+ Compound C1 20% SC 1250 175+18+250
T2 Compound A 17.5%+ Compound B 1.8%+ Compound C6 7.5% SE 1000 175+18+75
T3 Compound B 1.8%+ Compound C1 25% SC 1000 18+250
T4 Compound B 1.8%+ Compound C6 7.5% SE 1000 18+75
T5 Compound A 17.5%+ Compound C1 25% SC 1000 175+250
T6 Compound A 17.5%+ Compound C6 7.5% SE 1000 175+75
T7 Compound A 28%+ Compound B2.88% SC 625 175+18
T8 Compound A 24% SC 729.17 175
T9 Compound B 30% SC 60 18
T10 Compound C 50% WP 500 250
T11 Compound C6 10% EC 750 75
T12 Untreated Check (UTC) - -
T1 and T2 are present compositions, whereas T3 to T7 are known formulations.
Table 2a: Thrips, whitefly and fruit borer larval control in chilli crop
S.No. Thrips control (%) Whitefly control (%) Fruit borer larval control (%)
Observed Expected Ratio Observed Expected Ratio Observed Expected Ratio
T1 100.0 86.9 1.15 98.8 80.6 1.23 100.0 94.6 1.06
T2 99.2 79.2 1.25 96.5 78.1 1.24 100.0 94.4 1.06
T3 85.8 85.3 1.01 79.4 78.8 1.01 80.6 81.0 0.99
T4 77.2 76.7 1.01 77.8 76.0 1.02 78.8 80.0 0.98
T5 60.6 61.2 0.99 78.4 77.9 1.01 75.7 76.5 0.99
T6 39.5 38.3 1.03 76.5 75.0 1.02 74.9 75.3 1.00
T7 70.3 69.9 1.01 17.4 20.0 0.87 94.2 93.6 1.01
T8 10.8 - - 8.6 - - 71.8 - -
T9 66.3 - - 12.5 - - 77.2 - -
T10 56.5 - - 75.8 - - 16.7 - -
T11 30.8 - - 72.6 - - 12.3 - -
T12 0.0 - - 0.0 - - 0.0 - -
Table 2b: chilly fruit yield.
Treatment Number Number of healthy fruits per plant Increase (%) in fruits over UTC
T1 42.7 135.9
T2 41.9 131.5
T3 36.8 103.3
T4 36.3 100.6
T5 35.5 96.1
T6 35.1 93.9
T7 35.9 98.3
T8 28.7 58.6
T9 33.2 83.4
T10 28.5 57.5
T11 26.7 47.5
T12 18.1 0.0
Conclusion: The present compositions (T1 and T2) provide complete protection against fruit borer larvae, shows synergism between Thrips, whitefly and fruit borer larval and also produces higher number (>131%) of green chilly fruits per plant as compared to UTC (T12). Particularly, the thrips control observed T1 and T2 were 100% and 99.2% respectively and expected were T1-86.9% and 79.2%. While, the whitefly control observed T1 and T2 were 98.8% and 96.5% respectively and expected were 80.6% for T1 78.1% for T2. The fruit borer larvae control observed T1 and T2 were 100% whereas the pod borer larval control observed were (T1) 94.6% followed by (T2) 94.4%. Moreover, the colby’s ratio was found to be >1 which shows strong synergism, when compared with known combinations and market products.
Example 2: Insect-pests control in brinjal crop.
Crop : Okra
Number of Treatments: 12
Plot size : 45 sq.m.
Crop age : 82 days after transplanting.
Method of application : foliar spray with battery operated backpack sprayer.
Water volume : 500 liter per hectare
Observation Methods:
Shoot and Fruit borer (Leucinoides orbonalis) control (%): Count the number of healthy and infested fruits per plant, record observations from 10 plants per plot, calculate shoot & fruit borer damage (%) and recalculate reduction shoot & fruit borer damage.
Fruit count: Count the number of healthy fruits (marketable) per plant, record the observations from 10 plants per plot.
Composition of Compound A 15% + Compound B 1.5% + Compound C4 10% OD
[T1 of Ex. 2]
Chemical composition Function Percent
(% w/w)
Compound A a.i. Compound A 15.00
Compound B a.i. Compound B 1.50
Compound C4 a.i. Compound C4 10.00
Polyoxyethylene sorbitol hexaoleate Oil Emulsifier 10.00
Salts of polyolefin condensates Non-Aqueous dispersant 2.50
Ethoxylated sorbitan ester Co-Emulsifier 8.50
Bentonite clay Rheology modifier 1.50
Styrene acrylic polymer Aqueous dispersant 1.50
Methylated seed oil Oil continuous phase 49.50
Total 100.00
Active ingredient on 100% purity basis
Storage Stability: Compound A 15%+ Compound B 1.5%+ Compound C4 10% OD
[T1 of Ex. 2]
Laboratory storage stability for 14 days [T1 of Ex. 2]
Parameters Specifications Initial At 54±2 0C At 0±2 0C
Compound A a.i. 14.25 to 15.75 15.22 15.21 15.22
Compound B a.i. 1.43 to 1.65 1.57 1.56 1.57
Compound C4 a.i. 9.50 to 10.50 10.19 10.18 10.19
Compound A suspensibility (%) 80 97.89 98.10 97.89
Compound B suspensibility (%) 80 92.82 98.50 92.82
Compound C4 suspensibility (%) 80 95.65 98.10 95.65
pH range (1% aq. Suspension) 5.0 to 8.0 6.92 7.05 6.92
Pourability (%) 95 98.27 98.10 98.27
Specific gravity 1.00-1.10 1.03 1.03 1.03
Viscosity at spindle no.62,20 rpm 350-800 cps 510 520 510
Particle size (micron) D50<3, D90<10 2.1,8.0 2.1,8.2 2.1,8.0
Persistent foam ml (after 1 minute) max. 60 Nil Nil Nil
Room temperature storage stability up to 12 months [T1 of Ex. 2]
Parameters Specifications Initial 1 month 6 month 12 month
Compound A a.i. 14.25 to 15.75 15.22 15.21 15.21 15.2
Compound B a.i. 1.43 to 1.65 1.57 1.57 1.56 1.56
Compound C4 a.i. 9.50 to 10.50 10.19 10.19 10.18 10.17
Compound A suspensibility (%) 80 97.89 97.87 97.85 97.79
Compound B suspensibility (%) 80 92.82 92.81 92.78 92.72
Compound C4suspensibility (%) 80 95.65 95.61 95.57 95.52
pH range (1% aq. Suspension) 5.0 to 8.0 6.92 6.92 6.93 6.93
Pourability (%) 95 98.27 98.26 98.24 98.19
Specific gravity 1.00-1.10 1.03 1.03 1.03 1.03
Viscosity at spindle no. 62, 20 rpm 350-800 cps 510 512 514 517
Particle size (micron) D50<3, D90<10 2.1,8.0 2.1,8.0 2.1,8.1 2.2,8.2
Persistent foam in ml (after 1 minute) max. 60 Nil Nil Nil Nil
The composition of Compound A 15%+ Compound B 1.5%+ Compound C4 10% OD meets the all inhouse specifications for storage stability studies in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).
Manufacturing Process for 100 kg batch of Compound A 15%+Compound B 1.5%+ Compound C4 10% OD
Step 1: Preparation of 15% Bentonite clay solution: Bentonite clay (15 kg) is added into Methylated seed oil (85 kg) and homogenized till it gets completely dissolved. It was made 12 to 18 hours prior to use.
Step 2: Preparation of OD Premix
Step 3: Methylated seed oil (41.5 kg) was charged into a designated vessel for OD production.
Step 4: Polyoxyethylene sorbitol hexa oleate (10 kg), Styrene acrylic polymer (1.5 kg), Ethoxylated sorbitan ester (8.5 kg), salts of polyolefin condensates (2.5 kg) were added and the contents were homogenized for 45 to 60 minutes using high shear homogeniser
Step 5: Compound A (15 kg), Compound B (1.5 kg), Compound C4 (10 kg) were added into this premix and homogenized for 30 to 45 minutes.
Step 6: 15% Bentonite clay solution (10 kg) was added after milling to avoid foaming.
Step 7: The final formulation was sent to QC for quality check.
Table 3: Treatment details
S.No. Treatment compositions Rate (ml per hectare) gram actives per hectare
T1 Compound A 15%+Compound B 1.5%+Compound C4 10% OD 1000 150+15+100
T2 Compound A 15%+ Compound B 1.5%+ Compound C7 8% OD 1000 150+15+80
T3 Compound B 3%+ Compound C4 20% OD 500 15+100
T4 Compound B 3%+ Compound C7 16% OD 500 15+80
T5 Compound A 15%+ Compound C4 10% OD 1000 150+100
T6 Compound A15%+ Compound C7 8% OD 1000 150+80
T7 Compound A 30%+ Compound B 3% SC 500 150+!5
T8 Compound A 24% SC 625 150
T9 Compound B 30% SC 50 15
T10 Compound C4 24% SC 416.67 100
T11 Compound C7 15% OD 533.33 80
T12 Untreated Check (UTC) - -
T1 and T2 are present compositions, whereas T3 to T7 are known formulations.
Table 4: Control of shoot & fruit borer in brinjal crop.
S.No. Shoot & Fruit borer control Number of healthy fruits Increase (%) in fruits over UTC (Untreated Check)
Observed Expected Ratio
T1 98.7 90.2 1.09 65.6 101.2
T2 99.3 90.9 1.09 66.1 102.8
T3 74.2 76.2 0.97 54.9 68.4
T4 75.6 78.1 0.97 55.2 69.3
T5 65.2 68.9 0.95 49.6 52.1
T6 67.4 71.3 0.95 50.7 55.5
T7 85.3 87.0 0.98 57.9 77.6
T8 58.7 - - 44.2 35.6
T9 68.5 - - 46.5 42.6
T10 24.6 - - 39.6 21.5
T11 30.4 - - 40.1 23.0
T12 0.0 32.6 0.0
Conclusion: Among the various compositions as shown in Table 2 treatment number T1 and T2 are considered to be present inventive compositions which showed excellent synergism and effectiveness for Shoot & Fruit borer control. Particularly, the Shoot & Fruit borer control for T1 to T2 were observed were (T1) 98.7% followed by (T2) 99.3%. Moreover, the colby’s ratio was found to be >1 which shows strong synergism, when compared with known combinations and market products. Also there was percentage increase in fruits over UTC for both T1-(101.2%) and T2-(102.8%). The present compositions (T1 and T2) provide synergistic control of shoot & fruit in terms of damage.
Example 3: Looper control in Tea.
Crop : Tea
Number of Treatments: 12
Plot size : 70 sq.m.
Method of application: foliar spray with battery operated backpack sprayer.
Water volume : 500 liter per hectare
Observation Methods:
Looper control (%): Count the number of live larvae per bush, record the observations from 10 bushes per plant. Record the observations on 10th DAA and calculate looper control (%).
Composition of Compound A 20% + Compound B 2.5% + Compound C2 3% SE
[T1 of Ex. 3]
Chemical composition Function Percent
(% w/w)
Compound A a.i. Compound A 20.00
Compound B a.i. Compound B 2.50
Compound C2 a.i. Compound C 3.00
Polyarylphenyl anionic ether sulfate, ammonium salt Emulsifier-2 1.50
C9- dimethylamide Aromatic solvent 10.00
Acrylic graft copolymer Dispersing agent I 3.00
Butyl Polyalkylene Oxide block copolymer Dispersing agent II 4.50
Aluminum magnesium silicate Suspending agent 0.50
Polydimethylsiloxane Anti-foaming agent 0.20
1,2-benzisothiazolin-3(2H)-one Preservative 0.15
1,2-Polypropylene glycol Anti-freezing agent 5.00
Xanthan gum Thickener 0.15
Diluent water 49.50
Total 100.00
Active ingredient on 100% purity basis
Storage stability-Compound A 20%+Compound B 2.5%+Compound C2 3% SE [T1 of Ex. 3]
Laboratory storage stability for 14 days [T1 of Ex. 3]
Parameters Specifications Initial At 54±2 0C At 0±2 0C
Compound A a.i. 19.00 to 21.00 20.23 20.22 20.23
Compound B a.i. 2.38 to 2.75 2.57 2.56 2.57
Compound C2a.i. 2.85 to 3.30 3.13 3.12 3.13
Compound A suspensibility (%) 80 94.23 94.21 94.23
Compound B suspensibility (%) 80 91.85 91.82 91.85
Compound C2 suspensibility (%) 80 92.45 92.42 92.45
pH range (1% aq. Suspension) 5.0 to 8.0 6.78 6.79 6.78
Pourability (%) 95 98.75 98.73 98.75
Specific gravity 1.05-1.10 1.07 1.07 1.07
Viscosity at spindle no.62,20 rpm 350-800 cps 480 482 480
Particle size (micron) D50<3, D90<10 2.2,7.2 2.3,7.4 2.2,7.2
Persistent foam ml (after 1 minute) max. 60 Nil Nil Nil
Room temperature storage stability up to 12 months [T5 of Ex. 3]
Parameters Specification Initial 1 month 6 month 12 month
Compound A a.i. 19.00 to 21.00 20.23 20.23 20.22 20.22
Compound B a.i. 2.38 to 2.75 2.57 2.57 2.57 2.56
Compound C2 a.i. 2.85 to 3.30 3.13 3.13 3.13 3.12
Compound A suspensibility (%) 80 94.23 94.23 94.21 94.18
Compound B suspensibility (%) 80 91.85 91.85 91.79 91.67
Compound C2 suspensibility (%) 80 92.45 92.45 92.42 92.39
pH range (1% aq. Suspension) 5.0 to 8.0 6.78 6.78 6.79 6.79
Pourability (%) 95 98.75 98.75 98.74 98.72
Specific gravity 1.05-1.10 1.07 1.07 1.07 1.07
Viscosity at spindle no. 62, 20 rpm 350-800 cps 480 480 482 485
Particle size (micron) D50<3, D90<10 2.2,7.2 2.2,7.2 2.3,7.2 2.3,7.3
Persistent foam in ml (after 1 minute) max. 60 Nil Nil Nil Nil
The composition of Compound A 20%+ Compound B 2.5%+Compound C2 3% SE meets the all inhouse specifications for storage stability studies in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).
Manufacturing process for 100 kg batch of Compound A 20%+Compound B 2.5%+ Compound C2 3% SE
Step 1: Preparation of 2% Gum Solution: Xanthan gum (2kg) and 1,2-benzisothiazoline-3-one (2 kg) were charged into water (96 kg) and homogenized. It was made 12 to 18 hours prior to use.
Step 2: EC premix- Aromatic solvent C-9 (10 kg) was added into other vessel having slow stirring. Now Compound C2 (3 kg), Butyl Polyalkylene Oxide block copolymer (4.5 kg) was added and mixed properly for 30 to 45 minutes.
Step 3: DM water (42 kg) and 1,2-propylene glycol (5 kg) was charged into designated vessel and mix thoroughly.
Step 4: Aluminum magnesium silicate (0.5 kg), Acrylic graft copolymer (3 kg), Polyarylphenyl anionic ether sulfate, ammonium salt (1.5 kg) and Polydimethylsiloxane (0.1 kg) were added into the vessel having water and the contents were homogenised for 45 to 60 minutes using high shear homogeniser.
Step 5: Then Compound A (20 kg) and Compound B (2.5 kg) were added to this premix slowly and homogenised to get uniform slurry ready for grinding.
Step 6: Before grinding, half the quantity of antifoam was added and then material was subjected to grinding in Dyno mill till desired particle size was achieved.
Step 7: The remaining Polydimethyl siloxane antifoam (0.1 kg) was added after grinding process completes and before sampling for in process analysis.
Step 8: The EC premix was mixed to this milled slurry under slow stirring and homogenized for 30 to 45 minutes.
Step 9: Finally 2% gum solution (7.5 kg) was added to this formulation and send to QC for quality check.
Table 5: Treatment details.
S.No. Treatment compositions Rate (ml or g per hectare) gram actives per hectare
T1 Compound A 20%+Compound B 2.5%+Compound C2 3% SC 800 160+20+24
T2 Compound A 20%+Compound B 2.5%+ Compound C8 8% SC 800 160+20+64
T3 Compound B 5%+ Compound C2 6% SE 400 20+24
T4 Compound B 5%+ Compound C8 16% SC 400 20+64
T5 Compound A 20%+ Compound C2 3% SC 800 160+24
T6 Compound A 20%+ Compound C8 8% SC 800 160+64
T7 Compound A 25.6%+ Compound B 3.2% SC 625 160+20
T8 Compound A 24% SC 666.67 160
T9 Compound B 30% SC 66.67 20
T10 Compound C2 5% EC 480.00 24
T11 Compound C8 24% SC 266.67 64
T12 Untreated Check (UTC) - -
T1 and T2 are present compositions, whereas T3 to T7 are known formulations.
Table 6: Looper larvae control in Tea.
S.No. Looper control (%) at 10 DAA
Observed Expected Ratio
T1 100.0 90.0 1.11
T2 100.0 93.1 1.07
T3 73.8 73.2 1.01
T4 82.2 81.4 1.01
T5 71.4 70.4 1.01
T6 80.4 79.4 1.01
T7 88.2 87.5 1.01
T8 62.8 - -
T9 66.3 - -
T10 20.5 - -
T11 44.7 - -
T12 0.0 - -
The present compositions (T1 and T2) provide synergistic control of tea looper larvae on 10th DAA.
Conclusion: Among the various compositions as shown in Table 5 treatment number T1 and T2 are considered to be present inventive compositions which showed excellent synergism and effectiveness against looper larvae control for T1 to T2 observed were 100% whereas, the looper larvae control expected were (T1) 90.0% followed by (T2) 93.1% . Moreover, the colby’s ratio was found to be >1 which shows strong synergism, when compared with known combinations and market products.
Example 4: Pod borer larval control in red gram.
Crop : Red gram
Treatments : 12
Crop age : 105 days after sowing.
Spray water volume : 500 liters per hectare.
Method of Application: Foliar spray with battery operated knapsack sprayer fitted with hollow cone nozzle.
Observation Methods:
Pod borer (Helicoverpa armigera) larval control (%): Count the number of live larvae per plant. Record observations from 10 plants per plot on 14th days after application.
Composition of Compound A 20% + Compound B 2.5% + Compound C3 3% ZC
[T2 of Ex. 4]
Chemical composition Function percent (% w/w)
Compound A a.i. Compound A 20.00
Compound B a.i. Compound B 2.50
Compound C3 a.i. Compound C 3.00
Mixture of heavy aromatic hydrocarbons Solvent 5.00
4,4'-diphenylmethane diisocyanate Wall Forming Material - I 0.25
Diethylene triamine Wall Forming Material - II 0.15
Alkylbenzene sulfonate calcium salts Emulsifier-I 0.12
Tristyrylphenol polyethoxyester phosphate Emulsifier-II 3.50
Acrylic graft copolymer Dispersing agent I 2.50
Sodium naphthalene sulphonate formaldehyde condensate Dispersing agent II 0.16
Aluminium magnesium silicate Suspending agent 1.50
Polydimethylsiloxane Anti foaming agent 0.30
1,2-benzisothiazolin-3(2H)-one Preservative 0.20
1,2-Polypropylene glycol Anti freezing agent 5.00
Xanthan gum Thickener 0.20
Diluent water 55.62
Total 100.00
Active ingredient on 100% purity basis
Storage stability-Compound A 20%+Compound B 2.5%+Compound C3 3% ZC
[T2 of Ex. 4]
Laboratory storage stability for 14 days [T2 of Ex. 4]
Parameters Specifications Initial At 54±2 0C At 0±2 0C
Compound A a.i. (%) 19.00 to 21.00 20.31 20.30 20.31
Compound B a.i. (%) 2.38 to 2.75 2.61 2.6 2.61
Compound C3 a.i. (%) 2.85 to 3.30 3.16 3.15 3.16
Compound B suspensibility (%) 80 91.85 91.66 91.85
Compound A suspensibility (%) 80 95.68 95.61 95.68
Compound C3 suspensibility (%) 80 92.12 91.98 92.12
pH range (1% aq. Suspension) 5.0 to 8.0 6.70 6.71 6.70
Pourability (%) 95 98.87 98.85 98.87
Specific gravity 1.05-1.10 1.06 1.06 1.06
Viscosity at spindle no.62,20 rpm 350-800 cps 410 417 410
Particle size (micron) D50<3, D90<10 1.8,6.1 1.9,6.2 1.8,6.1
Persistent foam ml (after 1 minute) max. 60 Nil Nil Nil
Room temperature storage stability up to 12 months
[T2 of Ex. 4]
Parameters Specifications Initial 1 month 6 month 12 month
Compound A a.i. (%) 19.00 to 21.00 20.31 20.31 20.3 20.3
Compound B a.i. (%) 2.38 to 2.75 2.61 2.61 2.60 2.59
Compound C3 a.i. (%) 2.85 to 3.30 3.16 3.16 3.16 3.15
Compound B suspensibility (%) 80 91.85 91.85 91.81 91.75
Compound A suspensibility (%) 80 95.68 95.68 95.59 95.49
Compound C3 suspensibility (%) 80 92.12 92.12 92.05 91.89
pH range (1% aq. Suspension) 5.0 to 8.0 6.70 6.70 6.71 6.71
Pourability (%) 95 98.87 98.87 98.83 98.79
Specific gravity 1.05-1.10 1.06 1.06 1.06 1.06
Viscosity at spindle no.62,20 rpm 350-800 cps 410 410 412 418
Particle size (micron) D50<3, D90<10 1.8,6.1 1.8,6.1 1.8,6.2 1.9,6.3
Persistent foam ml (after 1 minute) max. 60 Nil Nil nil nil
The composition of Compound A 20%+Compound B 2.5%+Compound C3 3% ZC meets the all inhouse specifications for storage stability studies in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).
Manufacturing process for 100 kg batch of Compound A 20%+Compound B 2.5%+Compound C3 3% ZC
Step 1: Preparation of 2% Gum Solution: Xanthan gum (2kg) and 1,2-benzisothiazoline-3-one (2 kg) were charged into water (96 kg) and homogenized. It was made 12 to 18 hours prior to use.
Step 2: Preparation of CS premix: Mixture of heavy aromatic carbon (5 kg) was added into other vessel having slow stirring. The Compound C3 (3 kg) and of Alkylbenzene sulfonate calcium salts (0.12 kg), 4,4'-diphenylmethane diisocyanate (0.25 kg) were added and mixed properly for 30 to 45 minutes.
Step 3: This premix was added with water (15 kg) and Sodium naphthalene sulphonate formaldehyde condensate (0.16 kg) under high stirring and then Diethylene triamine (0.15 kg) was added and stirred at 50 degree for 3 hours and finally 2% Gum solution (2 kg) was added.
Step 4: DM water (30.62 kg) and 1,2-propylene glycol (5 kg) was charged into designated vessel and mixed thoroughly.
Step 5: Aluminum magnesium silicate (1.5 kg), Acrylic graft copolymer (2.5 kg), Tristyrylphenol polyethoxyester phosphate (3.5 kg) and Polydimethylsiloxane (0.1 kg) were added into the vessel having water and the contents were homogenized for 45 to 60 minutes using high shear homogeniser.
Step 6: Then Compound A (20 kg) and Compound B (2.5 kg) were added to this premix slowly and homogenised to get uniform slurry ready for grinding.
Step 7: Before grinding half the quantity of antifoam was added and then material was subjected to grinding in Dyno mill till desired particle size was achieved.
Step 8: The remaining Polydimethyl siloxane antifoam (0.1 kg) was added after grinding process completes and before sampling for in process analysis.
Step 9: The CS premix was mixed to this milled slurry under slow stirring and homogenized for 30 to 45 minutes.
Step 10: Finally 2% xanthan gum solution (10 kg) was added to this formulation and then sent to QC for quality check.
Table 7: Treatment details
S.No. Treatment compositions Rate (ml or g per hectare) gram actives per hectare
T1 Compound A 20%+Compound B 2.5%+Compound C9 3% SE 800 160+20+24
T2 Compound A 20%+ Compound B 2.5%+ Compound C3 3% ZC 800 160+20+24
T3 Compound B 5%+ Compound C9 6% SE 400 20+24
T4 Compound B 2.5%+ Compound C3 3% ZC 800 20+64
T5 Compound A 20%+ Compound C9 3% SE 800 160+24
T6 Compound A 20%+ Compound C3 3% ZC 800 160+24
T7 Compound A 25.6%+ Compound B 3.2% SC 625 160+20
T8 Compound A 24% SC 666.67 160
T9 Compound B 30% SC 66.67 20
T10 Compound C9 11% EC 218.18 24
T11 Compound C3 2.5% SC 960.00 24
T12 Untreated Check (UTC) - -
T1 and T2 are present compositions, whereas T3 to T7 are known formulations.
Table 8: Pod borer larval control in red gram.
S.No. pod borer larval control (%)
Observed Expected Ratio
T1 100.0 95.2 1.05
T2 100.0 94.6 1.06
T3 85.2 86.5 0.98
T4 83.5 84.7 0.99
T5 78.8 80.8 0.98
T6 76.2 78.3 0.97
T7 89.4 91.2 0.98
T8 64.7 - -
T9 75.2 - -
T10 45.6 - -
T11 38.4 - -
T12 0.0 - -
The present compositions (T1 and T2) provide synergistic control of red gram pod borer larvae on 7th DAA.
Conclusion: Among the various compositions as shown in Table 6 treatment number T1 and T2 are considered to be present inventive compositions which showed excellent synergism and effectiveness against red gram. The looper larvae control expected were (T1) 95.2% followed by (T2) 94.6% . Moreover, the colby’s ratio was found to be >1 which shows strong synergism, when compared with known combinations and market products.
Example 5: Composition of Compound A 30%+Compound B 3%+Compound C5 6% WG
Composition of Compound A 30% + Compound B 3% + Compound C5 6% WG
Chemical composition Function Percent
(% w/w)
Compound A a.i. Compound A 30.00
Compound B a.i. Compound B 3.00
Compound C5 a.i. Compound C 6.00
Modified Sodium lignosulphonate Dispersing agent I 5.00
Modified polyacrylate copolymer Dispersing agent II 4.00
Sodium isopropyl naphthalene sulfonate Wetting agent 5.00
Polydimethylsiloxane Antifoaming agent 1.00
Sodium sulfate anhydrous Carrier 10.00
China clay Carrier 36.00
Total 100.00
Storage Stability: Compound A 30%+Compound B 3%+Compound C5 6% WG
Laboratory storage stability for 14 days
Parameters Specifications Initial At 54±2 0C At 0±2 0C
Compound A a.i. (%) 28.50 to 31.50 30.24 30.23 30.24
Compound B a.i. (%) 2.85 to 3.30 3.13 3.12 3.13
Compound C5 a.i. (%) 5.70 to 6.60 6.19 6.18 6.19
Compound A suspensibility (%) 70 98.45 98.41 98.45
Compound B suspensibility (%) 70 94.78 94.74 94.78
Compound C5 suspensibility (%) 70 98.80 98.78 98.80
pH range (1% aq. Suspension) 5 to 9 7.50 7.51 7.50
Wettability Max 60 s 25 27 25
Wet Sieve(45 micron) Mini 98.5% 99.57 99.54 99.57
Bulk Density 0.45-0.85 0.5 0.5 0.5
Moisture Content Max 2.0% 1.4 1.2 1.4
Persistent foam ml (after 1 minute) max. 60 Nil Nil Nil
Room temperature storage stability up to 12 months
Parameters Specifications Initial 1 month 6 month 12 month
Compound A a.i. 28.50 to 31.50 30.24 30.24 30.23 30.22
Compound B a.i. 2.85 to 3.30 3.13 3.13 3.12 3.10
Compound C5 a.i. 5.70 to 6.60 6.19 6.19 6.18 6.16
Compound A suspensibility (%) 70 98.45 98.44 98.40 98.34
Compound B suspensibility (%) 70 94.78 94.77 94.72 94.68
Compound C5suspensibility (%) 70 98.80 98.80 98.78 98.65
pH range (1% aq. Suspension) 5 to 9 7.50 7.51 7.51 7.52
Wettability Max 60 s 25 25 26 27
Wet Sieve(45 micron) Mini 98.5% 99.57 99.57 99.56 99.54
Bulk Density 0.45-0.85 0.5 0.5 0.5 0.5
Moisture Content Max 2.0% 1.4 1.4 1.4 1.3
Persistent foam ml (after 1 minute) max. 60 Nil Nil Nil Nil
The composition of Compound A 30%+ Compound B 3%+ Compound C5 6% WG meets the all inhouse specifications for storage stability studies in laboratory (at 54±2 C & At 0±2 C for 14 days) and room temperature (for 12 months).
Manufacturing process for 100 kg batch of Compound A 30%+Compound B 3%+Compound C5 6% WG
Step 1: China clay (36 kg), Sodium sulphate anhydrous (10 kg), silicone antifoam (0.5 kg), Sodium isopropyl naphthalene sulfonate (5 kg), Modified polyacrylate copolymer (4 kg) and Modified Sodium lignosulphonate blend (5 kg) was charged into a premix blender and homogenized for 30 minutes
Step 2: The Compound A (30 kg), Compound B (3 kg) and Compound C5 (6 kg) was Charged and again homogenized for 30 minutes and now this Pre-blended material is then grinded through Jet mill/ air classifier mills. Finely grinded material was blended in post blender till it becomes homogeneous. (for approx 1.5 hr)
Step 3: Finely grinded powder is mixed with water (10 kg) having silicone antifoam (0.5 kg) to form extrudable dough.
Step 4: Dough was passed through extruder to get granules of required size.
Step 5: Wet granules are passed through fluidized bed drier to remove extra water (10 kg) added and further graded using vibrating screens.
Step 6: Final product was sent for QC approval.
Step 7: After approval the material was packed in required pack sizes.
The process for preparing the present novel synergistic composition can be modified accordingly by any person skilled in the art based on the knowledge of the manufacturing the formulation. However, all such variation and modification are still covered by the scope of present invention.
Application to the seeds is carried out before sowing, either directly on the seeds or after having pre germinated the latter. Suitable application methods include inter alia soil treatment, seed treatment, furrow application, and foliar application. Soil treatment methods include drenching the soil, drip irrigation (drip application onto the soil), dipping roots, tubers or bulbs, or soil injection. Seed treatment techniques include seed dressing, seed coating, seed dusting, seed soaking, and seed pelleting. In furrow applications typically include the steps of making a furrow in cultivated land, seeding the furrow with seeds, applying the insecticidal active composition to the furrow, and closing the furrow. Foliar application refers to the application of the insecticidal active composition to plant foliage, e.g., through spray equipment.
The rates of application vary within wide limits and depend on the nature of the soil, the method of application, the crop plant, the insect pest to be controlled, the prevailing climatic conditions, and other factors governed by the method of application, the time of application and the target crop.
The present invention is suitable for use in protecting crops, plants, and plant propagation materials, such as seeds, or sailor water, in which the plants are growing, from attack or infestation by pests. Therefore, the present invention also relates to a plant protection method, which comprises contacting crops, plants, plant propagation materials, such as seeds, or soil or water, in which the plants are growing, to be protected from attack or infestation by insect pests, with an insecticidal effective amount of the present invention.
The present invention is also suitable for use in combating or controlling pests. Therefore, the present invention also relates to a method of combating or controlling insects-pests and plant parasitic mites, their habitat, breeding ground, or food supply, or the crops, plants, plant propagation materials, such as seeds, or soil, or the area, material or environment in which the insect pests or mites grow, with an insecticidal effective amount of the present invention.
The lists of crops on which the insecticidal composition of the present invention is used include, but not limited to GMO (Genetically Modified Organism) and Non GMO traits, hybrids and conventional varieties of Cotton (Gossypium spp.), Paddy (Oryza sativa), Wheat (Triticum aestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), Oat (Avena sativa), Pearl millet (Pennisetum glaucum), Sugarcane (Saccharum officinarum), Sugarbeet (Beta vulgaris), Soybean (Glycin max), Groundnut/Peanut (Arachis hypogaea), Sunflower (Helianthus annuus), Mustard (Brassica juncea), Rape seed (Brassica napus), Sesame (Sesamum indicum), Green gram (Vigna radiata), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Cowpea (Vigna unguiculata), Red gram (Cajanus cajan), French bean (Phaseolus vulgaris), Indian bean (Lablab purpureus), Horse gram (Macrotyloma uniflorum), Field pea (Pisum sativum), Cluster bean (Cyamopsis tetragonoloba), Lentils (Lens culinaris), Brinjal (Solanum melongena), Cabbage (Brassica oleracea var. capitata), Cauliflower (Brassica oleracea var. botrytis), Okra (Abelmoschus esculentus), Onion (Allium cepa L.), Tomato (Solanum lycopersicun), Potato (Solanum tuberosum), Sweet potato (Ipomoea batatas), Chilly (Capsicum annum), Bell pepper (Capsicum annum), Garlic (Allium sativum), Cucumber (Cucumis sativus), Muskmelons (Cucumis melo), Watermelon (Citrullus lanatus), Bottle gourd (Lagenaria siceraria), Bitter gourd (Momordica charantia), Radish (Raphanus sativus), Carrot (Dacus carota subsp. sativus), Turnip (Brassica raparapa), Apple (Melus domestica), Banana (Musa spp.), Citrus groups (Citrus spp.), Grape (Vitis vinifera), Guava (Psidium guajava), Mango (Mangifera indica), Papaya (Carica papaya), Pineapple (Ananas comosus), Pomegranate (Punicagranatum), Sapota (Manilkara zapota), Tea (Camellia sinensis), Coffea (Coffea Arabica), Turmeric (Curcuma longa), Ginger (Zingiber officinale), Cumin (Cuminum cyminum), Black Pepper (Piper nigrum), Mentha (Mentha spp.), Rose (Rosa spp.), Jasmine (Jasminum spp.), Marigold (Tagetes spp.), Common daisy (Bellis perennis), Dahlia (Dahlia hortnesis), Gerbera (Gerberajamesonii), Carnation (Dianthus caryophyllus).
Crops are to be understood as also including those crops which have been rendered tolerant to herbicides or classes of herbicides (e.g. ALS-, GS-, EPSPS-, PPO-, ACCase - and HPPD-inhibitors) by conventional methods of breeding or by genetic engineering. An example of a crop that has been rendered tolerant to imidazolinones, e.g., imazamox, by conventional methods of breeding is Clearfield® summer rape (canola). Crops that have been rendered tolerant to herbicides by genetic engineering methods include, but not limited to, glyphosate- and glufosinate-resistant maize varieties commercially available under the trade names RoundupReady® and LibertyLink®.
Crops are also to be understood as being those which have been rendered resistant to harmful insects by genetic engineering methods, for example Bt maize (resistant to European corn borer), Bt cotton (resistant to cotton boll weevil) and Bt potatoes (resistant to Colorado beetle). Bt maize includes Bt 176 maize hybrids of NK® (Syngenta Seeds). The Bt toxin is a protein that is formed naturally by Bacillusthuringiensis soil bacteria. EP-A-451 878, EP-A-374 753, WO 93/07278, WO 95/34656, WO 03/052073 and EP-A-427 529 describe such toxins or transgenic plants able to synthesize such toxins. Transgenic plants comprising one or more genes that code for an insecticidal resistance and express one or more toxins are KnockOut® (maize), Yield Gard® (maize), NuCOTIN33B® (cotton), Bollgard® (cotton), NewLeaf® (potatoes), NatureGard® and Protexcta®. Plant crops or seed material thereof can be both resistant to herbicides and, at the same time, resistant to insect feeding (“stacked” transgenic events). For example, seed can have the ability to express an insecticidal Cry3 protein while at the same time being tolerant to glyphosate.
Crops are also to be understood to include those which are obtained by conventional methods of breeding or genetic engineering and contain so-called output traits (e.g., improved storage stability, higher nutritional value, and improved flavor).
Other useful plants include turf grass for example in golf-courses, lawns, parks and roadsides, or grown commercially for sod and ornamental plants such as flowers or bushes.
The insecticidal composition of the present invention can be used to control insect pests and plant parasitic mites. The major insects-pests belong to the order Hemiptera, for example, but not limited to rice leafhopper/green leaf hopper (GLH) (Nephotettixnigropictus), rice brown plant hopper (BPH) (Nilaparvatalugen), rice backed plant hopper (WBPH) (Sogatellafurcifera), Apple Mealy bug (Phenococcusaceris), bean aphid (Aphisfabae), black citrus aphid (Toxopteraaurantii), citrus black scale (Saissetiaoleae), cabbage aphid (Brevicorynebrassicae), (Lipaphiserysimi), citrus red scale (Aonidiellaaurantii), yellow scale (Aonidiella citrine), citrus mealybug (Planococcuscitri), corn leaf aphid (Rhopalosiphummaidis), aphid (Aphis gossypii), jassid(Amrascabiguttula), mealy bug (Planococcus spp. and Pseudococcus spp.), cotton stainer (Dysdercussuturellus), whitefly (Bemisiatabaci), cowpea aphid (Aphis crassivora), grain aphid (Sitobionavenae), golden glow aphid (Uroleucon spp.), grape mealybug (Pseudococcus maritimus), green peach aphid (Myzuspersicae), greenhouse whitefly (Trialeurodesvaporariorum), papaya mealy bug (Pracoccusmarginatus), pea aphid (Acyrthosiphonpisum), sugarcane mealybug (Saccharicoccussacchari), potato aphid (Myzuspersicae), potato leaf hopper (Empoasca fabae), cotton whitefly (Bemisiatabaci), tarnished plant bug (Lygus lineolaris), wooly apple aphid (Eriosomalanigerum), and mango hopper (Amritodusatkinsoni, Idioscopus spp.); order Lepidoptera, for example, but not limited to army worm (Mythimnaunipuncta), asiatic rice borer (Chilo suppressalis), bean pod borer (Maruca vitrata), beet armyworm (Spodoptera exigua), black cutworm (Agrotisipsilon), bollworm (Helicoverpaarmigera), cabbage looper (Trichoplusiani), codling moth (Cydiapomonella), croton caterpillar (Acheajanata), diamond backmoth (Plutellaxylostella), cabbage worm (Pieris rapae), pink bollworm (Pectinophoragossypiella), sugarcane borer (Diatraeasaccharalis), sugarcane early shoot borer (Chilo infuscatellus) tobacco budworm (Heliothisvirescens), tomato fruitworm(Helicoverpazea), velvet bean caterpillar (Anticarsiagemmatalis), yellow stem borer (Scirpophagaincertulas), spotted bollworm (Eariasvittella), rice leaf-folder (Cnaphalocrocismedinalis), pink stem borer (Sesamia spp.), tobacco leaf-eating caterpillar (Spodopteralitura); brinjal fruit and shoot borer (Leucinodesorbonalis), bean pod borer (Maruca vitrata, Maruca testulalis), armyworm (Mythimna separata), cotton pinkbollworm(Pectinophoragossypiella), citrus leaf-miner (Phyllocnistiscitrella), cabbage butterfly (Pierisbras-sicae), diamond backmoth (Plutellaxylostella), paddy stem borer (Scirpophagaexcerptallis, Scirpophagaincertulas, Scirpophagainnotata), wheat stem borer (Sesamiainferens, Sitotrogacerealella, Spilosomaobliqua), fall armyworm (Spodopterafrugiperda, Spodoptera littoralis, Spodoptera litura, Trichoplusiani, Tryporyzanivella, Tryporyzaincertulas, Tuta absoluta); from the order Coleoptera, for example,but not limited to apple twig borer (Amphicerus spp.), corn root worm (Diabroticavirgifera), cucumber beetle (diabroticabalteata), boll weevil (Anthonomusgrandis), grape flea beetle (Alticachalybea), grape root worm (Fidia viticola), grape trunk borer (Clytoleptusalbofasciatus), radish flea beetle (Phyllotretaarmoraciae), maize weevil (Sitophilus zeamais), northern corn rootworm (Diabroticabarberi), rice water weevil (Lissorhoptrusoryzophilus, Anthonomus grandis, Bruchuslentis, Diabroticasemipunctata, Diabroticavirgifera, Dicladispaarmigera, Epilachnavarivestis), and various species of white grubs (Holotrichia bicolor, Holotrichiaconsanguinea, Holotrichia serrata, Leptinotarsa decemlineata, Phyllotretachrysocephala, Popillia japonica); from the order Orthoptera, for example, but not limited toGryllotalpa spp., Locusta spp., and Schistocerca spp.; from the order Thysanoptera, for example, but not limited to Frankliniella spp., Thrips palmi, Thrips tabaciand Scirtothrips dorsalis; termites (Isoptera),for example, but not limited toCalotermesflavicollis, Coptotermesformosanus, Heterotermes aureus, Leucotermesflavipes, Microtermesobesi, Odontotermesobesus, Reticulitermes flavipes, and Termes natalensis; from the order Heteroptera, for example, but not limited to Dysdercus spp., and Leptocorisa spp., to the order Hymenoptera, for example, but not limited toSolenopsis spp.; to the order Diptera, for example, but not limited to Antherigonasoccata, Dacus spp., Liriomyza spp., and Melanagromyza spp.
The plant parasites from the order Acarina, for example, Aceriamangiferae, Brevipalpus spp., Eriophyes spp., Oligonychusmangiferus, Oligonychuspunicae, Panonychuscitri, Panonychusulmi, Polyphagotarsonemus latus, Tarsonemus spp., Tetranychusurticae, and Tetranychuscinnabarinus;
The present invention has been described with reference to specific embodiment which is merely illustrative and not intended to limit the scope of the invention as defined in the present complete specification.
Dated this on 3rd day of February, 2025 ,CLAIMS:We Claim:
1. A ternary insecticidal composition comprising:
A. Compound A: 10 to 50 w/w% of N'-tert-butyl-N'-(3,5-dimethylbenzoyl)-3-methoxy-2-methylbenzohydrazide;
B. Compound B: 1 to 10 w/w% of 3-[benzoyl(methyl)amino]-N-[2-bromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)-6-(trifluoromethyl)phenyl]-2-fluorobenzamide
C. Compound C: 1 to 40 w/w% of at least one compound selected from group of insecticides and agrochemically acceptable excipients.
2. The ternary insecticidal composition comprising as claimed in claim 1, wherein the insecticides for compound C is selected from the group consisting of
C1, 1-tert-butyl-3-[4-phenoxy-2,6-di(propan-2-yl)phenyl]thiourea,
C2, (4S,5S)-5-(4-chlorophenyl)-N-cyclohexyl-4-methyl-2-oxo-1,3-thiazolidine-3-carboxamide,
C3, [(R)-cyano-(4-fluoro-3-phenoxyphenyl)methyl] (1S)-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropane-1-carboxylate
C4, [2-oxo-3-(2,4,6-trimethylphenyl)-1-oxaspiro[4.4]non-3-en-4-yl] 3,3-dimethylbutanoate,
C5, N-[(6-chloropyridin-3-yl)methyl]-N'-cyano-N-methylethanimidamide,
C6, 2-[1-(4-phenoxyphenoxy)propan-2-yloxy]pyridine,
C7, [3-(2,5-dimethylphenyl)-8-methoxy-2-oxo-1-azaspiro[4.5]dec-3-en-4-yl] ethyl carbonate,
C8, 4-bromo-2-(4-chlorophenyl)-1-(ethoxymethyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile,
C9, [(S)-cyano-(3-phenoxyphenyl)methyl] (1R,3R)-3-(2,2-dibromoethenyl)-2,2-dimethylcyclopropane-1-carboxylate,
3. The composition as claimed in claim 1, wherein the agrochemically acceptable excipients are selected from the group consisting of wetting-spreading-penetrating agent(s), dispersing agent(s), suspending agent(s), anti freezing agent(s), thickener(s),preservative(s), emulsifier(s), anti foaming agent(s), buffering agent(s),rheology modifier(s), wetting agent(s), carrier(s) and solvent(s).
4. The composition as claimed in claim 1, wherein the composition is in the form of oil dispersion (OD), suspension concentrate (SC), suspo emulsion (SE), wettable granule (WG) and mixed formulation (ZC).
5. The composition as claimed in claim 3, wherein the emulsifying agent for oil dispersion (OD) is selected from castor oil ethoxylates, alcohol ethoxylates, fatty acid ethoxylates, sorbitan ester ethoxylates, sulphosuccinate, calcium salts of dodecylbenzene sulphonate, alkylammonium salts of alkylbenzene sulphonate, alkylsulphosuccinate salts, ethylene oxide-propylene oxide block copolymers, ethoxylated alkylamines, ethoxylated alkyl phenols, polyoxyethylene sorbitan monolaurate, polyxyethylene sobitol hexaoleate, ethoxylated sorbiton ester and mixture thereof.
6. The composition as claimed in claim 3, wherein the dispersing agent for oil dispersion (OD) is selected from alkyl sulfonates, alkyl benzene sulfonates, alkyl aryl sulfonates, alkylphenolalkoxylates, tristyrylphenol ethoxylates, natural or synthetic fatty ethoxylate alcohols, natural or synthetic fatty acid alkoxylates, natural or synthetic fatty alcohols alkoxylates, alkoxylated alcohols (such as n-butyl alcohol poly glycol ether), block copolymers (such as ethylene oxide-propylene oxide block copolymers and ethylene oxide-butylene oxide block copolymers), fatty acid-polyalkylene glycol condensates, polyamine-fatty acid condensates, polyester condensates, salts of polyolefin condensates, sodium ligno sulfonate, sodium ploycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycolether-phosphate, oleyl-polyglycolether with ethylene oxide, tallow fattyamine polyethylene oxide, nonylphenol polyglycolether with 9-10 moles ethylene oxide and mixture thereof.
7. The composition as claimed in claim 3, wherein the stabilizers/rheology modifier for oil dispersion (OD) is selected from hectorite clay, aluminium magnesium silicate, bentonite clay, silica, attapulgite clay and mixture thereof.
8. The composition as claimed in claim 3, wherein the solvent for oil dispersion (OD) is selected from vegetable oil its alkylated or ethoxylated or esterified form, the alkylated vegetable oil, methylated vegetable oil, ethylated vegetable oil, the vegetable oils, olive oil, kapok oil, castor oil, papaya oil, camellia oil, sesame oil, corn oil, rice bran oil, cotton seed oil, soybean oil, groundnut oil, rapeseed-mustard oil, linseed oil, tung oil, sunflower oil, safflower oil, coconut oil, the alkyl ester of vegetable oils, methyl ester, ethyl ester, propyl ester, butyl ester of vegetable oils, methylated seed oil, polyalkyleneoxide modified polydimethylsiloxane alkylphenol ethoxylate, rapeseed oil methyl ester, rapeseed oil ethyl ester, rapeseed oil propyl esters, rapeseed oil butyl esters, soybean oil methyl ester, soybean oil ethyl ester, soybean oil propyl ester, soybean oil butyl ester, castor oil methyl ester, castor oil ethyl ester, castor oil propyl ester, castor oil butyl ester, cotton seed oil methyl ester, cotton seed oil ethyl ester, cotton seed oil butyl ester, cotton seed oil propyl ester, tall oil fatty acids esters-tallow methyl ester, tallow ethyl ester, tallow propyl ester, bio-diesel, mineral oil, aromatic solvents, isoparaffin, base solvent, fatty acid amides, C1-C3 amines, alkylamines, alkanolamines with C6-C18 carboxylic acids, fatty acids, alkyl esters of fatty acids, methyl oleate, ethyl oleate, methyl soyate, ethyl soyate, alkyl benzenes, alkylnaphthalenes, polyalkylene glycol ethers, fatty acid diesters, fatty alkylamides, diamides, dialkylene carbonates, ketones, alcohols, cyclohexanone, acetophenone, NMP, dimethyl sulfoxide, benzyl alcohol, butanol, N-octanol, N-propanol, 2-ethyl hexanol, tetrahydro furfuryl alcohol, isophorone, fatty acid dimethyl amide, 2-hexylethyl lactate, propylene carbonate and mixtures thereof.
9. The composition as claimed in claim 3, the wetting spreading-penetrating agent(s) for suspension concentrate (SC) is selected from, ethylene oxide/propylene oxide (EO/PO) block copolymer, poly aryl phenyl ether phosphate, polyalkoxylated butyl ether, ethoxylated fatty alcohol, sodium dioctyl sulfosuccinate, sodium lauryl sulfate and sodium dodecyl benzene sulfonate, alkyl diphenyl sulfonates, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate. Ethoxylated alcohol includes natural fatty alcohol (lauryl alcohol ethoxylate, lauryl alcohol alkoxylate), synthetic alcohol ethoxylate (tridecyl alcohol ethoxylate, 2-ethyl hexanol, 2-propylheptanol, isodecyl alcohol, methylated seed oil, polyakyleneoxide modified trisiloxane, trisiloxane ethoxylate, heptamethyl trisiloxane, modified polyalkyleneoxide, modified heptamethyl trisiloxane, polyether modified polysiloxane, polyalkyleneoxide modified trisiloxane, polyalkyleneoxide modified polydimethylsiloxane, liquid or powder form and mixture thereof.
10. The composition as claimed in claim 3, wherein the dispersing agent for suspension concentrate (SC) is selected from, naphthalene sulfonic acid, sodium salt condensate with formaldehyde, alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium ligno sulfonate, sodium polycarboxylate, EO/PO based copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propylene oxide-ethylene oxide-copolymer, polyethylene glycol 2,4,6-tristyrylphenyl ether, tristyrylphenol-polyglycol ether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycol ether-phosphate, oleyl-polyglycol ether with ethylene oxide, tallow fatty amine polyethylene oxide, nonylphenol polyglycol ether with 9-10 moles ethylene oxide, Polymethyl methacrylate-polyethylene glycol graft copolymer, Ethylene-propylene oxide block copolymer or mixture thereof.
11. The composition as claimed in claim 3, wherein the suspending agent for suspension concentrate (SC) is selected from, aluminium magnesium silicate, bentonite clay, silica, attapulgite clay or mixture thereof.
12. The composition as claimed in claim 3, wherein the antifoaming agent for cuspension concentrate (SC) is selected from, silicone antifoam emulsion, dimethyl siloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids or mixture thereof.
13. The composition as claimed in claim 3, wherein the anti-freezing agent for suspension concentrate (SC) is selected from, ethylene glycol, propane diols, glycerin or the urea, glycol (monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol), glycerin, urea, magnesium sulfate heptahydrate, sodium chloride or mixture thereof.
14. The composition as claimed in claim 3, wherein the preservatives for suspension concentrate (SC) is selected from, 1,2-benzisothiazolin-3(2H)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenyl phenate, 5-chloro-2-methyl-4-isothiazolin-3-one & 2-methyl-4-isothiazolin-3-one or mixture thereof.
15. The composition as claimed in claim 3, wherein the thickeners for suspension concentrate (SC) is selected from, xanthan gum, PVK, carboxymethyl celluloses, polyvinyl alcohols, gelatin, sodium carboxymethylcellulose, hydroxyethyl cellulose, sodium polyacrylate, modified starch, acacia gum or mixture thereof.
16. The composition as claimed in claim 3, wherein the solvent for suspo emulsion (SE) is selected from water, water soluble alcohols and dihydroxy alcohol ethers, water soluble alcohol or lower alcohol -1 to 4 carbon atoms, methanol, ethanol, n-propanol, isopropanol, n-butanol, tert-butanol, macromolecular alcohol, polyethylene glycol, sorbitol, glucitol, dihydroxy alcohol ethers, dihydroxy alcohol alkyl ether, dihydroxy alcohol aryl ethers, dihydroxy alcohol alkyl ether, ethylene glycol methyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, di-propylene glycol methyl ether, ethylene glycol ethyl ether, diethylene glycol ethyl ether, propylene glycol ethyl ether, dipropylene glycol ethyl ether, dihydroxy alcohol aryl ethers includes ethylene glycol phenyl ether, 5 diethylene glycol phenyl ether, propylene glycol phenyl ether, di-propylene glycolphenyl ether, aromatic solvent C-9, hyrdocarbons, n-pentane, hexanes, cyclohexane, methylcyclohexane, heptane, isooctane, benzene, toluene, xylenes, isophorone, ester solvents, methyloleate, dimethylamide, morpholineamide derivatives of C6-C16 fatty acids, mono-alkylene carbonates, ethylene carbonate, propylene carbonate, butylene carbonates, dimethylsulfoxide (DMSO), 2-ethylhexanol, nbutanol, n-alkylpyrrolidones, fatty acid dimethyl esters, fatty acid esters, dibasic esters, aromatic hydrocarbons, aliphatic hydrocarbons, one or more dimethylamides, C8-dimethylamide, C10-dimethylamide, C12-dimethylamide, ethylene glycol, propylene glycol, polyalkylene glycols, aromatic hydrocarbons, methylpyrrolidinone (NMP), dimethylformamide (DMF), dimethylisosorbide (DMI), isophorone, acetophenone, 1,3- dimethyl-2-imidazolidonone, lactate esters, dimethyl, diethylcarbonates, alcohols including methanol, ethanol, iso-propanol, n-propanol, n-butanol, iso-butanol, tert-butanol, methyl L-lactate, 2-ethylhexyl L-lactate, ethyl L-lactate, n-butyl L-lactate, octyl phenol ethoxylates or mixture thereof.
17. The composition as claimed in claim 3, wherein the emulsifier for suspo emulsion (SE) is selected from salts of dodecylbenzene sulphonate, Ca-salts, amine salts, sulphonates of other C11-C16 alkylbenzenes, alkylether sulphates, alkylphenoletherphosphates, ester phosphates, non-ionic surfactants, alkoxylated alcohols, alkylphenols, ethoxylated fatty acids, ethoxylated vegetable oils, ethoxylated castor oil, fatty acid esters, sorbitol, their ethoxylated derivatives, ethoxylated amines, condensates of glycerol, catanionic emulsifiers, cationic amine, alkylsulphonate, ether sulphonate, ether phosphate, alkoxylated alcohols, alkoxylated alkylphenols, ethoxylated fatty acids, ethoxylated vegetable oils, ethoxylated tristyrylphenol tristyrlphenol with 16 moles EO, tristyrylphenol-polyglycoletherphosphate, fatty acid esters of sorbitol, ethoxylated derivatives thereof, ethoxylated amines, condensates of glycerol, sulfonated alkylbenzenes in the range C11-C16, salts thereof, alkylether sulphates, alkyletherphosphates, alkylphenoletherphosphates, salts of phosphate esters of ethoxylated tristyrylphenol, salts of sulphated ethers of ethoxylated tristyrylphenol, catanionic system, alkylsulphonate, alkylethersulphonate, ether sulphate, ether phosphate, alkyletherphosphate, nonylphenol polyethoxyethanols, castor oil polyglycol ethers, poly adducts of ethylene oxide, poly adducts of polypropylene, tributyl phenoxy polyethoxy ethanol, octyl phenoxy polyethoxy ethano, polyarylphenyl anionic ether sulphate, ammonium salts and mixture thereof.
18. The composition as claimed in claim 3, wherein the anti-freezing agent for suspo emulsion (SE) is selected from selected from ethylene glycol, propane diols, glycol, monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol, glycerine, urea, magnesium sulfate heptahydrate, sodium chloride and mixture thereof.
19. The composition as claimed in claim 3, wherein the antifoaming agent for suspo emulsion (SE) is selected from silicone oil, silicone compound, C10~C20 saturated fat acid compounds, C8~C10 aliphatic alcohols compound, silicone antifoam emulsion, dimethylsiloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified and mixture thereof.
20. The composition as claimed in claim 3, wherein the suspending agent for suspo emulsion (SE) is selected from aluminum magnesium silicate, bentonite clay, silica, silicone dioxide, attapulgite clay or mixture thereof.
21. The composition as claimed in claim 3, wherein the preservatives for suspo emulsion (SE) is selected from propionic acid its sodium salt, sorbic acid-its sodium salt, potassium salt, benzoic acid-its sodium salt, p-hydroxy benzoic acid sodium salt, methyl p-hydroxy benzoate, biocide, sodium benzoate, 1,2-benzisothiazoline(2H)- 3-one, 2 methyl-4-isothiazolin-3-one,5-chloro-2-methyl-4-isothiazolin-3-one, potassium sorbate, parahydroxy benzoates and mixture thereof.
22. The composition as claimed in claim 3, wherein the thickeners for suspo emulsion (SE) is selected from is selected from thickening, gelling, and anti-settling agents generally fall into two categories is selected from, but not limited to, water-insoluble particulates and watersoluble polymers, clays, silicas, montmorillonite, bentonite, magnesium aluminum silicate, attapulgite, water-soluble polysaccharides, natural extracts of seeds, seaweeds, synthetic derivatives of cellulose, guar gum, locust bean gum, carrageenam, xanthan gum, alginates, methyl cellulose, sodium carboxymethyl cellulose (SCMC), hydroxyethyl cellulose (HEC), modified starches, polyacrylates, polyvinyl alcohol, polyethylene oxide or mixtures thereof.
23. The composition as claimed in claim 3, wherein the dispersing agent for suspo emulsion (SE) is selected from butyl polyalkylene oxide block copolymer, polyesters, polyamides, polycarbonates, polyurea, polyurethanes, acrylic polymers, acrylic graft copolymer, styrene copolymers, butadiene copolymers, polysaccharides, starch, cellulose derivatives, vinylalcohol, vinylacetate, vinylpyrrolidone polymers, copolymers, polyethers, epoxy, phenolic, melamine resins, polyolefins, define copolymers, acrylate polymers, polymethacrylate, polyethyl methacrylate, polymethylmethacrylate, acrylate copoylmers, styrene-acrylic copolymers, polystyrene-co maleic anhydride, cellulosic polymers, ethyl cellulose, cellulose acetate, cellulose acetate butyrate, acetylated mono, di, triglycerides, polyvinylpyrrolidone, vinyl acetate polymer, vinyl acetate copolymers, polyalkylene glycol, styrene butadiene copolymers, polyorthoesters, alkyd resins, mixtures of two or more of these, polymers, biodegradable polymers, biodegradable polyesters, starch, polylactic acid starch blends, polylactic acid, polylactic acid-glycolic acidits copolymers, polydioxanone, cellulose esters, ethyl cellulose, cellulose acetate butyrate, starch esters, starch esteraliphatic polyester blends, modified corn starch, polycaprolactone, polynamyl methacrylate, wood rosin, polyanhydrides, polyvinylalcohol, polyhydroxybutyratevalerate, biodegradable aliphatic polyesters, polyhydroxybutyrate, alkylated naphthalene sulfonate, sodium salt, sodium salt of naphthalene sulfonate condensate, sodium salt of alkyl naphthalene sulfonate, sodium lingo sulfonate, sodium ploycarboxylate, EO/PO block copolymer, phenol sulfonate, sodium methyl oleoyl taurate, styrene acrylic acid copolymer, propyleneoxide-ethyleneoxide-copolymer, polyethylene glycol 2,4,6- tristyrylphenyl ether, tristyrylphenol-polyglycolether-phosphate, tristyrylphenole with 16 moles EO, tristyrylphenol-polyglycoletherphosphate, oleyl-polyglycolether with ethylene oxide, tallow fattyamine polyethylene oxide, nonylphenol polyglycolether with 9-10 moles ethylene oxide and mixture thereof.
24. The composition as claimed in claim 3, wherein the wall forming material for mixed formulation (ZC) is selected from, tetramethylene diisocyanate, pentamethylene diisocyanate, hexamethylene diisocyanate, toluene diisocyanate, 4,4-diphenylmethenediisocyanate (MDI), polymethylene polyphenylene isocyanate, 2,4,4’-diphenyl ether tri-isocyanate, 3,3’-dimethyl-4,4’-diphenyl diisocyanate, 3,3’-dimethoxy-4,4’-diphenyl diisocyanate, 1,5- naphthylene diisocyanate, 4,4’4"-triphenylmethane tri-isocyanate, toluene diisocyanate, polymethylene polyphenylisocyanate, polyurethane comprising of polyfunctional isocyanate, a polyamine in polarized form, diethylene triamine, Ammonia, hexamine, ethylenediamine, propylene-1,3-diamine, tetramethylenediamine, pentamethylenediamine, 1,6- hexamethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, 4,9-dioxadodecane-1, 12- diamine, 1,3-phenylenediamine, 2,4-toluenediamine, 2,6-toluenediamine, 4,4’-diaminodiphenylmethane, 1,3-phenylenediamine, 1,5- diaminonaphthalene, 1,3,5-triaminobenzene, 2,4,6-triaminotoluene, 1,3,6- triaminonaphthalene, 2,4,4'-triaminodiphenyl ether, 3,4,5-triamino-1,2,4- triazole, 1,4,5 ,5,8-tetraminoanthraquinone or mixture thereof.
25. The composition as claimed in claim 3, wherein the dispersing agents for mixed formulation (ZC) is selected from, ethoxylated lignosulfonic acid salts, lignosulfonic acid salts, oxidized lignins, lignin salts, salts of styrenemaleic anhydride copolymers, polyvinyl alcohol, salts of partial esters of styrene-maleic anhydride copolymers, partial salts of polyacrylic acid, partial salts of polyacrylic acid terpolymers, lignosulfonate of calcium, sodium, a modified kraft lignin with a high sulfonic acid group , dibutylnaphthalenesulfonic acid, fatty acids, alkyl-alkylarylsulfonates, alkyl sulfates, lauryl ether sulfates, fatty alcohol sulfates, salts of sulfated hexa, heptadecanols, octadecanols, fatty alcohol glycol ethers, condensates of sulfonated naphthalene-its derivatives with formaldehyde, condensates of naphthalene, naphthalenesulfonic acids with phenol, naphthalenesulfonic acids with formaldehyde, polyoxyethylene octylphenol ether, ethoxylated isooctyl, octyl- nonylphenol, alkyl phenyl polyglycol ethers, tributyl phenyl polyglycol ethers, alkyl aryl polyether alcohols, tridecyl alcohol, fatty alcohol/ethylene oxide condensates, ethoxylated castor oil, polyoxyethylene alkyl ethers, polyoxypropylene alkyl ethers, lauryl alcohol polyglycol ether acetate, sorbitol esters, lignin-sulphite waste liquors, proteins, denatured proteins, polysaccharides, ammonium salts of sulfonates, sulfates, phosphates, carboxylates, alkylarylsulfonates, diphenyl sulfonates, alpha-olefin sulfonates, sulfonates of fatty acids, oils, sulfonates of ethoxylated alkylphenols, sulfonates of condensed naphthalene, sulfonates of dodecyl-tridecyl benzenes, sulfonates of naphthalene, alkylnaphthalenes, sulfosuccinates, alkoxylates, N-alkylated fatty acid amides, amine oxides, esters, sugar-based surfactants, alkylphenols, amines, tallow amine, amides, aryl phenols, fatty acids, fatty acid esters, alkoxylated ethylene oxide, propylene oxide, ethylene oxide, polyethylene oxide, polypropylene oxide, polyacids, polybases, sodium naphthalene sulphonate formaldehyde condensates, acrylic graft copolymer and mixture thereof.
26. A ternary insecticidal composition as claimed in claim 3, wherein the solvent for mixed formulation (ZC) is selected from, hydrocarbon solvent such as an aliphatic, cyclic, aromatic hydrocarbons, toluene, xylene, paraffin, tetrahydronaphthalene, alkylated naphthalene, their derivatives, mineral oil fractions of medium to high boiling point such as kerosene, diesel oil, coal tar oils, a vegetable oil such as corn oil, rapeseed oil, a fatty acid ester such as C1-C10-alkylester of a C10-C22-fatty acid, methyl-ethyl esters of vegetable oils such as rapeseed oil methyl ester, corn oil methyl ester, acetophenone, 2-heptanon, 3-heptanone, 2- hexanone, 5-methyl-2-hexanone , 5-methyl-3-heptanone, 3-methyl-2-hexanone, 4-methyl-2-hexanone, 2-methyl-3-hexanone, 4-methyl-3-hexanone, 5-methyl-3-hexanone, 3-ethyl-2-pentanone, 3,3-dimethyl-2-pentanone, 3,4-dimethyl-2-pentanone, 4,4-dimethyl-2-pentanone, 2,2-dimethyl-3-pentanone , 2,4-dimethyl-3-pentanone, 2-octanone, 2,5-dimethyl-3-hexanone, 2,2-dimethyl-3-hexanone, 3,3-dimethyl-2-hexanone, 3,4-dimethyl-2-hexanone, 4,4-dimethyl-3-hexanone, 3-ethyl-4-methyl-2-pentanone, 2-methyl-3-heptanone, 2-methyl-4-heptanone, 3-methyl-2-heptanone, 3-methyl-4-heptanone, 5-methyl-3-heptanone, 6-methyl-2-heptanone, 6-methyl-3-heptanone, 3-octanone, 4-octanone, 2,2,4-trimethyl-3-pentanone, 3-ethyl-3-methyl-2-pentanone, 5-methyl-2-heptanone, isoprene or mixture thereof.
27. The composition as claimed in claim 3, wherein the thickener for mixed formulation (ZC) is selected from, xanthan gum ,carboxy methyl cellulose, attapulgite clay, bentonite clay or mixture thereof.
28. The composition as claimed in claim 3, wherein the suspending agent for mixed formulation (ZC) is selected from, aluminium magnesium silicate, bentonite clay, silica, attapulgite clay or mixture thereof.
29. The composition as claimed in claim 3, wherein the antifoaming agent for mixed formulation (ZC) is selected from, silicone oil, silicone compound, C10~C20 saturated fat acid compounds or C8~C10 aliphatic alcohols compound, silicone antifoam emulsion, dimethyl siloxane, polydimethyl siloxane, vegetable oil based antifoam, tallow based fatty acids, polyalkyleneoxide modified polydimethylsiloxane or mixture thereof.
30. The composition as claimed in claim 3, wherein the antifreezing agent for mixed formulation (ZC) is selected from, ethylene glycol, propane diols, glycerine, urea, glycol, monoethylene glycol, diethylene glycol, polypropylene glycol, polyethylene glycol, magnesium sulphateheptahydrate, sodium chloride and mixture thereof.
31. The composition as claimed in claim 3, wherein the preservative for mixed formulation (ZC) is selected from, 1,2-benzisothiazolin-3(2h)-one, sodium salt, sodium benzoate, 2-bromo-2-nitropropane-1,3-diol, formaldehyde, sodium o-phenyl phenate, 5-chloro-2-methyl-4-isothiazolin-3-one & 2-methyl-4-isothiazolin-3-one or mixture thereof.
32. The composition as claimed in claim 3, wherein the emulsifier for mixed formulation (ZC) is selected from, alkylbenzene sulfonate calcium salts, tristyrylphenol polyethoxyester phosphate or mixture thereof.
33. The composition as claimed in claim 3, wherein the dispersing agent for wettable granule (WG) is selected from alkylnaphthalene sulfonate sodium salt, alkylnaphthalene sulfonate, modified polyacrylate copolymer, sodium polycarboxylate, naphthalenesulfonic acid, sodium salt condensates with formaldehyde, polyalcoxylated alkylphenol, naphthalenesulfonic acid formaldehyde condensate, methylnaphthalene-formaldehyde-condensate sodium salt, naphthalene condensates, lignosulfonates, polyacrylates, phosphate esters, calcium lignosulfonate, lignin sulfonate sodium salt, modified sodium lignosulphonate, modified polyacrylate copolymer and mixture thereof.
34. The composition as claimed in claim 3, wherein the carrier for wettable granule (WG) is selected from china clay, silica, lactose anhydrous, ammonium sulfate, sodium sulfate anhydrous, corn starch, urea, EDTA, urea formaldehyde resin, diatomaceous earth, kaolin, bentonite, kieselguhr, fuller's earth, attapulgite clay, bole, loess, talc, chalk, dolomite, limestone, lime, calcium carbonate, powdered magnesia, magnesium oxide, magnesium sulphate, sodium chloride, gypsum, calcium sulphate, pyrophyllite, silicates, silica gels, fertilizers, ammonium sulphate, ammonium phosphate, ammonium nitrate and urea, natural products of vegetable, grain meals, flours, bark meals, wood meals, nutshell meals, cellulosic powders, synthetic polymeric materials, groundpowdered plastics, resins, bentonites, zeolites, titanium dioxide, iron oxides, hydroxides, aluminium oxides, hydroxides, organic materials such as bagasse, charcoal, synthetic organic polymers or mixture thereof.
35. The composition as claimed in claim 3, wherein the wetting agent for wettable granule (WG) is selected from sodium N-methyl-N-oleoyl taurate, alkylated naphthalene sulfonate, sodium salt, mixture of isomers of dibutylnaphthalene sulphonic acid sodium salt, sodium di-isopropylnaphthalenesulphonate, sodium isopropyl naphthalene sulphonate, sodium lauryl sulfate, dioctyl sulfate, alkyl naphthalene sulfonates, phosphate esters, sulphosuccinates, non-ionic, tridecyl alcohol ethoxylate, alkyl-alkaryl sulfonates, alkylbenzene sulfonates, alpha olefin sulfonate, alkyl naphthalene sulfonates, ethoxylated, non-ethoxylated alkyl, alkaryl carboxylates, alkyl, alkaryl phosphate esters, alkyl polysaccharide, di, mono alkyl sulfosuccinate derivatives, alpha olefin sulfonates, alkyl naphthalene sulfonates, dialkyl sulphosuccinates, butyl, dibutyl, isopropyl, di-isopropyl naphthalene sulfonate salts, C12 alkyl benzene sulfonate, C10-C16 alkyl benzene sulfonate, organosilicons surfactants, trisiloxane ethoxylate, polydimethylsiloxane, polyoxyethylene methyl polysiloxane, polyoxyalkylene methyl polysiloxane, polyether polymethyl siloxane copolymer, trisiloxaneheptamethyl, polyalkyleneoxide modified heptamethyl trisiloxane, polyether modified polysiloxane and mixture thereof.
36. The composition as claimed in claim 3, wherein the antifoaming agent for wettable granule (WG) is selected from polydimethylsiloxane.
| # | Name | Date |
|---|---|---|
| 1 | 202421008020-STATEMENT OF UNDERTAKING (FORM 3) [06-02-2024(online)].pdf | 2024-02-06 |
| 2 | 202421008020-PROVISIONAL SPECIFICATION [06-02-2024(online)].pdf | 2024-02-06 |
| 3 | 202421008020-POWER OF AUTHORITY [06-02-2024(online)].pdf | 2024-02-06 |
| 4 | 202421008020-FORM FOR SMALL ENTITY(FORM-28) [06-02-2024(online)].pdf | 2024-02-06 |
| 5 | 202421008020-FORM FOR SMALL ENTITY [06-02-2024(online)].pdf | 2024-02-06 |
| 6 | 202421008020-FORM 1 [06-02-2024(online)].pdf | 2024-02-06 |
| 7 | 202421008020-EVIDENCE FOR REGISTRATION UNDER SSI(FORM-28) [06-02-2024(online)].pdf | 2024-02-06 |
| 8 | 202421008020-EVIDENCE FOR REGISTRATION UNDER SSI [06-02-2024(online)].pdf | 2024-02-06 |
| 9 | 202421008020-DECLARATION OF INVENTORSHIP (FORM 5) [06-02-2024(online)].pdf | 2024-02-06 |
| 10 | 202421008020-FORM-26 [15-04-2024(online)].pdf | 2024-04-15 |
| 11 | 202421008020-FORM-9 [03-02-2025(online)].pdf | 2025-02-03 |
| 12 | 202421008020-CORRESPONDENCE-OTHERS [03-02-2025(online)].pdf | 2025-02-03 |
| 13 | 202421008020-COMPLETE SPECIFICATION [03-02-2025(online)].pdf | 2025-02-03 |
| 14 | 202421008020-MSME CERTIFICATE [04-02-2025(online)].pdf | 2025-02-04 |
| 15 | 202421008020-FORM28 [04-02-2025(online)].pdf | 2025-02-04 |
| 16 | 202421008020-FORM 18A [04-02-2025(online)].pdf | 2025-02-04 |
| 17 | 202421008020-Request Letter-Correspondence [15-02-2025(online)].pdf | 2025-02-15 |
| 18 | 202421008020-Covering Letter [15-02-2025(online)].pdf | 2025-02-15 |
| 19 | 202421008020-FER.pdf | 2025-06-20 |
| 20 | 202421008020-FORM 3 [27-06-2025(online)].pdf | 2025-06-27 |
| 21 | 202421008020-OTHERS [30-07-2025(online)].pdf | 2025-07-30 |
| 22 | 202421008020-FER_SER_REPLY [30-07-2025(online)].pdf | 2025-07-30 |
| 23 | 202421008020-CLAIMS [30-07-2025(online)].pdf | 2025-07-30 |
| 24 | 202421008020-US(14)-HearingNotice-(HearingDate-18-11-2025).pdf | 2025-10-17 |
| 25 | 202421008020-Correspondence to notify the Controller [14-11-2025(online)].pdf | 2025-11-14 |
| 1 | 202421008020_SearchStrategyNew_E_strategyE_20-06-2025.pdf |