Abstract: ABSTRACT NON AQUEOUS WATER DISPERSIBLE GRANULAR FORMULATION OF AN INSECTICIDE The present invention relates to non-aqueous water dispersible granules (WDG) formulation of an insecticide, preferably Pymetrozine. The present invention also relates to non-aqueous water dispersible granules (WDG) formulation of Pymetrozine comprising alcohol as solvent for granulation. The present invention also relates to an efficient process for the preparation of non-aqueous water dispersible granules of Pymetrozine. The present invention also relates to use of non-aqueous water dispersible granules (WDG) formulation of Pymetrozine as insecticides for application to plants.
DESC:FORM 2
THE PATENTS ACT 1970
(SECTION 39 OF 1970)
&
THE PATENT RULES, 2003
COMPLETE SPECIFICATION
(SECTION 10)
NON AQUEOUS WATER DISPERSIBLE GRANULAR FORMULATION OF AN INSECTICIDE
We, COROMANDEL INTERNATIONAL LIMITED,
a company incorporated under the companies act, 1956 having address at Coromandel House, Sardar Patel Road, Secunderabad, Telangana- 500003, India
The following specification describes and ascertains the nature of this invention and the manner in which it is to be performed:
FIELD OF THE INVENTION
The present invention relates to non-aqueous water dispersible granules (WDG) formulation of an insecticide, preferably Pymetrozine.
The present invention also relates to non-aqueous water dispersible granules (WDG) formulation of Pymetrozine comprising alcohol as solvent for granulation.
The present invention also relates to an efficient process for the preparation of non-aqueous water dispersible granules of Pymetrozine.
The present invention also relates to use of non-aqueous water dispersible granules (WDG) formulation of Pymetrozine as insecticides for application to plants.
BACKGROUND OF THE INVENTION
Pymetrozine is an active ingredient from a chemical class (pyridine azomethines). Pymetrozine has been determined to be of low acute toxicity to humans, birds, aquatic organisms, mammals, and bees. Pymetrozine is not mutagenic. It produced some neurotoxic effects, but the frequency and magnitude were low. Pymetrozine is not expected to pose a risk of contaminating groundwater. Pymetrozine is considered as a replacement for organophosphate (OP) pesticides used for the same use patterns. Pymetrozine products are approved under the brand name of ENDEAVOR® which is a water dispersible granule.
Pymetrozine is azomethine insecticide suitable for use in integrated crop management to control aphids and other plant sucking pests. Use of Pymetrozine controls aphids and whitefly in vegetables, potatoes, ornamentals, cotton, deciduous and citrus fruit, tobacco and hops; both juvenile and adult stages are susceptible. It is plant-systemic and readily taken up by leaves and roots and translocated throughout the plant. Plants are immediately protected upon application because insect feeding stops soon after ingestion of Pymetrozine.
An agrochemical compound is applied for its use after it has been formulated into various formulations such as a dust, granules, a wettable powder, an emulsifiable concentrate, SC (a suspension concentrate), EW (an emulsion in the form of an oil-in-water). Among these formulations, the dust and the granules are applied as such or by means of an applicator, whereas, the emulsifiable concentrate, the wettable powder, the SC or the EW is first diluted often with water or other liquid to prepare a liquid formulation containing a predetermined concentration of the active ingredient, and then the liquid formulation is applied by spraying it.
Water-based formulations are considered much more environmentally benign and safe, as they produce no dust and include little or no aromatic solvent. Microparticulate Pymetrozine can be suspended in water at relatively high concentrations to produce a suspension concentrate. Suspension concentrates can overcome the problems with dust of wettable powders, and can provide a number of additional advantages, such as ease of pouring and measuring. However, it can be difficult to prepare suspension concentrate formulations that are storage stable, e.g., with respect to thickening and particle agglomeration, especially for active ingredients having high water solubility such as Pymetrozine.
US 4,931,439 A claims Pymetrozine compound and composition for controlling insects and arachnids. The patent also claims salts of active compound with organic or inorganic acids together with suitable carrier or adjuvants.
US 6,784,176 B2 claims Pymetrozine dihydrate compound and process for preparation of non- solvated (water free) pesticidally active compounds. This patent also discloses the pesticidal formulations, especially granulates, which contain from 3 to 5% by weight, or those which contain from 30 to 50% by weight of pymetrozine. Equally preferred are water-dispersible powders, which contain from 25 to 50% by weight of pymetrozine. Also preferred are pesticidal formulations, in particular granulates, which contain from 8 to 40% by weight, preferably from 8 to 20% by weight, especially from 8 to 14% by weight, of water. Equally preferred are pesticidal formulations, in particular granulates, which contain from 40 to 60% by weight of pymetrozine, especially 50% by weight of pymetrozine. Also preferred are wettable powders which contain from 6 to 20% by weight, especially from 8 to 12% by weight, of water, and from 20 to 30% by weight of pymetrozine, especially 25% by weight of pymetrozine.
CN 10642096 A discloses a Pymetrozine oil suspension formulation composition characterized in that the composition by weight is 5-50 %, wetting agent 1-3 %, dispersant 2-5%, emulsifier 5-15 %, solvent topping up to 100 %.
CN 102524267 A discloses a Pymetrozine suspension formulation comprising vegetable oil and derivatives thereof, characterized in that the composition of the suspension is by weight
Pymetrozine 1 to 50 %
Vegetable oil and its derivatives 1-40 %
Wetting agent 0.5 to 10 %
Dispersant 0.5 to 10 %
Emulsifier 2 to 15 %
Thickener 0.05 % to 5 %
Defoamer 0.05 % to 5%
Antifreeze 1 to 10 %
Preservatives 0.1 to 10 %
Water up to 100 %
CN 103210929 A claims a Pymetrozine aqueous emulsion, characterized in that the components are expressed in weight percent :Pymetrozine1-20 %, solvent 5-20 %, co-solvent 5-15 %, emulsifier 4-15 %, stabilizer 1-5 %, dispersant 0.5 to 2 %, antifreeze 1-5 % and the rest is deionized water.
IN 201721017913 discloses a novel stable crystalline modification III of Pymetrozine and a process for preparation thereof. The present invention further discloses the use of the said stable crystalline modification of Pymetrozine for preparing crop protection composition using water as solvent for granulation for controlling insects.
There remains a need for Pymetrozine formulations that can address these shortcomings.
OBJECTIVE OF THE INVENTION
The main objective of the present invention is to provide non-aqueous water dispersible granules (WDG) formulation of insecticide, preferably Pymetrozine.
In another objective of the present invention is to provide non-aqueous water dispersible granules (WDG) formulation of Pymetrozine comprising alcohol as solvent for granulation.
Still another objective of the present invention is to provide efficient process for the preparation of non-aqueous water dispersible granules of Pymetrozine.
Still another objective of the present invention is to provide use of non-aqueous water dispersible granules (WDG) formulation of Pymetrozine as insecticides for application to plants.
SUMMARY OF THE INVENTION
Accordingly, the present invention provides non-aqueous water dispersible granules (WDG) composition of insecticide preferably Pymetrozine.
In another embodiment, the present invention provides an efficient process for the preparation of non-aqueous water dispersible granules of Pymetrozine.
In yet another embodiment, the present invention provides a water dispersible granulation method using alcohol as solvent.
In yet another embodiment, the present invention provides a composition of water dispersible granules, wherein the composition comprises:
a) Pymetrozine technical,
b) wetting agent,
c) dispersing agents,
d) disintegrating agent,
e) alcohol as solvent, and
f) inert fillers.
In yet another embodiment of the present invention provides a process for preparing water dispersible granule, wherein the process comprises the steps of:
a) pre-blending of Pymetrozine with wetting agent, dispersing agent, disintegrating agent, and inert filler,
b) micronizing pre-blended mixture in air jet mill to get the desired particle size,
c) preparing the dough by employing an alcohol, and
d) extruding using an extruder and drying under vacuum to obtain water dispersible granules.
In yet another embodiment of the present invention provides the non-aqueous water dispersible granules (WDG) formulation of Pymetrozine as insecticides for application to plants.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides composition of non aqueous water dispersible granules of Pymetrozine, the characteristics of which show advantage preparation especially in the production and handling of pesticidal mixtures, particularly granulates.
The formulations i.e. agents, preparations or compositions which contain an active ingredient is Pymetrozine.
The present invention describes one or more solid and/or liquid formulation excipients. The composition of the present invention is produced for example in a manner known per se, by intimately mixing and/or grinding the active ingredient of Pymetrozine with the formulation excipients, such as solvents or solid carriers.
Alternatively, a new preparation method, consisting of addition of the solvating agent during the formulation procedure, thus forms the solvate during the formulation process.
In another important variant of this method, the solvating agent can be added in excess, and removed again at the end for example by evaporation to give the desired value.
In the case of certain mixtures, this procedure can significantly simplify the production process.
The preparations of the present water dispersible granules formulations are shown in table-1 and were prepared step wise as given below:
Step 1: Pre- blending:
50.0 parts by weight of Pymetrozine technical,
2.0 parts by weight of wetting agent,
4.0 parts by weight of dispersing agent-1,
6.0 parts by weight of dispersing agent-2,
10.0 parts by weight of disintegrating agent,
remaining quantity of fillers are preloaded in pre blender and mix the contents to homogenous mixture and check the uniformity.
Step 2: Air-Jet milling of WP
The pre-blended material of step -01 was air jet milled to particle size less than 10microns at pressure of minimum 6.0kg/cm2. Check the particle size analysis by doing sieve test using 500mesh sieve and the desired particle size is achieved. Collect the material from the post blender.
Step 3:
The post blend material is made to dough by adding an alcohol and the dough is subjected to extrusion using basket extruder and the granules achieved are subjected to drying and sample sent for analysis.
All the raw materials are premixed in a ribbon blender and blended with a binder. The mixture is subsequently mixed with 25 to 30% by weight of alcohol and granulated using basket extruder. The granules are dried on a commercial continuous drier, at 70°C.After drying to residual moisture of 1-3% the granulate obtained is sieved to a defined grain size.
Surface-active compounds (surfactants) may additionally be used for preparing the formulations. Depending on the type of active ingredient of Pymetrozine to be formulated, suitable surface-active compound are non-ionic, cationic and/or anionic surfactants and surfactant mixtures having good dispersing and wetting properties.
The concentration of Pymetrozine used in the insecticidal and acaricidal formulations according to the invention is from 0.1 to 99% by weight, preferably from 1 to 95% by weight, preferably from 0.1 to 94% and most preferably from 0.1 to 90% by weight.
The concentration of surfactant used in the insecticidal and acaricidal formulations according to the invention is from 0 to 50% by weight, preferably from 0.1 to 50%, preferably from 0 to 30% by weight and most preferably from 0.1 to 25% by weight.
The concentration of solvent used in the insecticidal and acaricidal formulations according to the invention is from 5 to 40% by weight.
The concentration of solid or liquid formulation excipient used in the insecticidal and acaricidal formulations according to the invention is from 1 to 99.9% by weight, preferably from 5 to 99.8% by weight, preferably from 1 to 94.9% by weight and most preferably from 5 to 90% by weight.
The concentration of Pymetrozine used in the pesticidal formulations, in particular granulates according to the invention is from 40 to 60% by weight and most preferably from 50% by weight.
The concentration of solvent used in the pesticidal formulations, in particular granulates according to the invention is from 1 to 50% by weight, preferably from 5 to 40% by weight and most preferably from 10 to 30% by weight.
When specifying the amount of water content, the fact that the formulation excipients themselves often have a certain residual content of water must be taken into consideration. In general, the measured contents are 1 to 5% by weight higher than those calculated. Hereinbefore and hereinafter, a formulation of Pymetrozine that is essentially free of water or of low water content is understood to be a pesticidal mixture containing at most 3% by weight of water based on the total mixture.
The compound Pymetrozine is usually applied to the plants or the locus thereof in concentrations of 0.001 to 1.0 kg/ha, preferably 0.1 to 0.6 kg/ha. The concentration required to achieve the desired action can be determined by experimentation. It will depend on the type of action, the development stage of the cultivated plant and of the pest, as well as on the application (locus, time, method), and as a result of these variables can vary over a wide range. As with the type of compositions, the methods of application such as spraying, atomising, dusting, wetting, scattering or pouring, are selected in accordance with the intended objectives and the prevailing circumstances.
The wetting agent is a compound that facilitates rapid wetting of the powder when added to the water. The wetting agent employed in the formulation composition is selected from the group consisting of non-ionic surfactants, anionic surfactant and a mixture of anionic and non-ionic surfactant and polymeric surfactant.
The non-ionic surfactants are selected from alkoxylates, N-alkylated fatty acid amides, aminoxides, esters, block polymers or sugar-based surfactants. Examples of alkoxylates are compounds such as alcohols, alkylphenols, amines, amides, arylphenols, fatty acids or fatty acid esters which have been alkoxylated. Ethylene oxide and/or propylene oxide, preferably ethylene oxide, may be applied for the alkoxylation reaction. Examples of N-alkylated fatty acid amides are fatty acid glucamides or fatty acid alkanolamides. Examples of esters are fatty acid esters, glycerol esters, or monoglycerides. Examples of sugar-based surfactants are sorbitans, ethoxylated sorbitans, sucrose and glucose esters or alkylpolyglucosides. Suitable block polymers are block polymers of the A-B or of the A-B-A type comprising blocks of polyethylene oxide and polypropylene oxide or of the A-B-C type comprising alkanol, polyethylene oxide and polypropylene oxide. Preferred nonionic surfactants are alkoxylates such as alcohols, alkylphenols, amines, amides, arylphenols, fatty acids or fatty acid esters which have been ethoxylated.Most preferred non-ionic surfactants are alcohol alkoxylate and fatty alcohol ethoxylates.
The anionic surfactants are selected from the group of alkali metal, alkaline-earth metal or ammonium salts of sulfonates, sulfates, phosphates or carboxylates and EO-PO polymeric and acrylate polymeric surfactant. Examples of sulfonates are alkylarylsulfonates, diphenylsulfonates, alpha-olefinsulfonates, sulfonates of fatty acids and oils, sulfonates of ethoxylated alkylphenols, condensed naphthalenesulfonates, sulfonates of dodecyl- and tridecylbenzenes, sulfonates of naphthalenes and alkylnaphthalenes, sulfosuccinates or sulfosuccinamates. Examples of sulfates are sulfates of fatty acids and oils, of ethoxylated alkylphenols, of alcohols, of ethoxylated alcohols, or of fatty acid esters. Examples of phosphates are phosphate esters. Examples of carboxylates are alkyl carboxylates and carboxylated alcohol or alkylphenol ethoxylates. Preferred anionic surfactants are alkali metal, alkaline-earth metal or ammonium salts of sulfonates, such as alkylarylsulfonates, diphenylsulfonates, alpha-olefinsulfonates, sulfonates of fatty acids and oils, sulfonates of ethoxylated alkylphenols, condensed naphthalenesulfonates, sulfonates of dodecyl- and tridecylbenzenes, sulfonate of naphthalenes and alkylnaphthalenes, sulfosuccinates or sulfosuccinamates.Most preferred anionic surfactants are alkyl naphthalene sulfonate condensate, sodium lauryl sulphate and sodium dodecyl benzene sulfonate, EO-PO polymeric and acrylate polymeric surfactant.
The present invention employs surfactant that are selected from following list of surfactant:
Surfactant A: Sodium lignosulphonate (Borresperse NA),
Surfactant B: Sulfonated naphthalene condensate, sodium salt (Lomar D from Cognis),
Surfactant C: Sodium alkyl naphthalene sulphonate (Morwet IP from Akzonobel),
Surfactant D: Modified Sodium Lignosulphonate,
Surfactant E: Blend of polymeric surfactants (Huntsman),
Surfactant F: Blend of EO-PO polymeric surfactant,
Surfactant G: Sodium alkyl naphthalene sulfonate, formaldehyde condensate (MorwetD-450 from Akzonobel),
Surfactant H: Polycondensate of naphthalenesulphonic acid sodium salt, Surfactant I: Sodium dibutyl naphthalene sulphonate,
Surfactant J: Alkyl naphthalene sulfonate (Sellogen DFL),
Surfactant K: Sodium alkyl naphthalene sulfonate,
Surfactant L: Blend of sodium salt of fatty alcohol sulfate and sodium naphthalene, Sulphonate formaldehyde condensate (Jeemol DW),
Surfactant M: Blend of dialkyl naphthalene sulphonic acid and alcohol sulfate(Jeemol WP),
Surfactant N: Alcohol ethoxylates and fatty alcohol ethoxylate (Jeemol DML),
Surfactant O: Blend of naphthalene sulfonic acid formaldehyde condensate and dioctyl Sulfosuccinate (Jeemol CI),
Surfactant P: Sulfonated aromatic polymer, sodium salt (Morwet D 425),
Surfactant Q: Calcium Lignosulphonate,
Surfactant R: Polyalkyl naphthalene sulphonate (Supragil MNS- 90, Supragil WP) and
Surfactant S: Ligno sulfonic acid, sodium salt sulfomethylated.
The surfactants that are used in the present invention can be used as wetting and dispersing agents.
As wettable/ wetting agent used in the present invention are selected from alpha olefin sulfonates, sodium lauryl sulphate, polyoxyalkylene alkyl ether, polyoxyalkylene alkyl ether, polyoxyalkylene alkyl phenyl ether sulfonates, dialkylsuccinate, polyalkyl naphthalene sulphonate etc. The wetting agent is used in an amount of 0.5 to 5%, more preferably 1 to 4% of the total weight of the composition.
The dispersing agent is a compound which ensures that the particles remain suspended in water. The dispersing agent can be ionic or non ionic or a mixture of such surface active agents or graft co-polymer dispersant.
The dispersing agent are selected from group comprising sodium lignosulphonates; sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenol ethoxylate phosphate esters; aliphatic alcohol ethoxylates; alky ethoxylates; EO-PO block copolymers; and graft copolymers,polycarboxylates, alkyl naphthalene sulfonates, phenol sulphonic acid condensates, lignosulphonates, methyl oleyltaurates and poly vinyl alcohols. Preferred dispersing agents are polycarboxylates, alkyl naphthalene sulfonates, phenol sulphonic acid condensates, lignosulphonates, methyl oleyltaurates and poly vinyl alcohols. The dispersing agent is present in the composition in a range of about 0.5 to 6%, more preferably 2 to 6% of the total weight of the composition.
The disintegrating agents as used in the present invention are selected from microcrystalline cellulose, crosslinked PVP, ammonium sulphate, sodium sulphate, sodium citrate, polycarboxylates, sodium phenylsulphonates, sodium bicarbonate, magnesium sulphate, sodium starch glycolate, sodium lignin sulfonate, sodium lauryl sulfate, combinations of carbonates with solid acids, agar, starch, hydroxypropylstarch, sodium alginate, carboxymethyl starch ether, gum arabic, gum tragacanth, gelatin, casein, crystalline cellulose, carboxymethylcellulose calcium, Tween, Pluronic, sodium laurate, carboxylic resins, ammonium sulfate, potassium chloride, sodium chloride, urea, anionic surfactants, calcium chloride, magnesium chloride, aluminum chloride, glucose, lactose, sodium glutamate, sodium inosinate, dextrin, blend of sulphonates (Sodium, calcium, potassium, magnesium or mixture thereof). Preferred disintegrating agents are microcrystalline cellulose, crosslinked PVP, ammonium sulphate, sodium sulphate, sodium citrate, polycarboxylates, sodium phenylsulphonates, sodium bicarbonate, magnesium sulphate and blend of sulphonates (Sodium, calcium, potassium, magnesium or mixture thereof). The disintegrating agent is used in an amount of 1 to 20%, more preferably 5 to 10% of the total weight of the composition.
Optionally use of binding agents used in the present invention are selected from starch, maltodextrins, carboxymethyl cellulose, polyvinyl pyrrolidone, polyvinyl alcohol, polyvinyl acetate copolymers, polyacrylate, gelatine, polyacrylamide, oligosaccharides, lecithin, sodium starch glycolate, and a mixture thereof. The binding agent is used in an amount of 0 to 5%, more preferably 0 to 2% of the total weight of the composition.
The alcohol as used in the present invention is selected fromC1 to C4alkanolsselected from methanol, ethanol, n-propanol, isopropanol (isopropyl alcohol), n-Butanol, t-Butanol or iso-butanol, amyl alcohol, methyl amyl alcohol, cyclohexanol, 2-ethylhexanol, furfuryl alcohol, tetrahydrofurfuryl alcohol and d-limonene acetonitrile, toluene, dichloromethane, dichloroethane, Tetrahydrofuran (THF), 2- Methyltetrahydrofuran (2-Me-THF), Dimethoxyethane (DME), 1,4-dioxane, acetone, ethyl acetate, Methyl tert-butyl ether (MTBE), Di-isopropyl ether (DIPE), ethylene glycol (EG), diethylene glycol (DEG), poly polyethylene glycol 400 (PEG 400), propylene glycol (PG), alkanolamides, ethoxylated alkanolamides, ethylene bisamides and glycerol or mixture thereof. Preferred alcohols are methanol, ethanol, n-propanol, isopropanol (isopropyl alcohol), n-Butanol, t-Butanol or iso-butanol, acetonitrile, toluene, dichloromethane, dichloroethane, Tetrahydrofuran (THF), 2- Methyltetrahydrofuran (2-Me-THF), Dimethoxyethane (DME), 1,4-dioxane, acetone, ethyl acetate, Methyl tert-butyl ether (MTBE), Di-isopropyl ether (DIPE), ethylene glycol (EG), diethylene glycol (DEG), poly polyethylene glycol 400 (PEG 400), propylene glycol (PG) and glycerol or mixture thereof.
The inert fillers as used in the present invention are includes but are not limited to natural minerals such as calcite, talc, china clay series, and montmorillonite or attapulgite clays including various forms of Bentonite, Kaolin; lactose, starches, calcium carbonate, calcium sulphate, calcium phosphate, sodium tripoly phosphate (STPP), woodflours, activated carbon, sugars, diatomaceous earth, cereal flours, fine-grain inorganic solids, and the like. Clays and inorganic solids which may be used include calcium bentonite, perlite, mica, vermiculite, silicas, quartz powder, montmorillonite and mixtures thereof. Sugars which may be useful include dextrin and maltodextrin. Cereal flours include wheat flour, oat flour and barley flour and a mixture thereof. Preferred inert fillers are lactose anhydrous and china clay. Highly disperse silica or highly disperse absorptive polymers may also be used to improve physical properties.
The main advantage of the formulation described here are improved suspension ability in the spray liquor and improved dispersibility.
Pymetrozine 50WDG prepared by this novel process (Non aqueous) was evaluated in the field for its bio-efficacy against brown plant hopper (BPH) in rice. The results were quite promising in reducing the population of brown plant hopper without any phytotoxicity symptoms and produced good yield when compared to existing Pymetrozine 50WDG formulations.
EXAMPLES
Example 1:
The unit of each value below is “% w/w” i. e. the percentage by weight, relative to the weight of the total composition unless otherwise specified. The compositions contemplated by each of the Examples 1-3 that are tabulated in Table 1 are formulated as a water dispersible granules (WDG) formulation.
Table 1: Pesticide compositions:
Component Function Examples Examples
Examples 1
(% w/w) Examples 2 (gm)
Pymetrozine **A.I (Purity 99.1%) 50.45 504.5
Sodium salt of sulfonated naphthalene formaldehyde condensate 2.0 20.0
Condensed methylnaphthalene sulphonate, Sodium salt 4.0 40.0
Blend of non-ionic and sodium lignosulphonate 6.0 60.0
Ammonium sulphate 10.0 100.0
Lactose anhydrous (Filler) 18.55 185.5
Chinaclay(Filler) 9.0 90.0
Total 100 1000
**A.I = Active ingredient
Table 2: Pesticide compositions (with binding agent):
Component Function Examples Examples
Examples 3
(% w/w) Examples 4(gm)
Pymetrozine **A.I (Purity 99.1%) 50.45 504.5
Sodium salt of sulfonatednaphthalene formaldehyde condensate 2.0 20.0
Condensed methylnaphthalene sulphonate, Sodium salt 4.0 40.0
Blend of non-ionic and sodium lignosulphonate 2.0 20.0
1-vinyl-2-pyrrolidine,-vinyl acetate polymer 1.0 10.0
Ammonium sulphate 10.0 100.0
Lactose anhydrous (Filler) 10.0 100.0
Chinaclay(Filler) 20.55 205.5
Total 100 1000
**A.I = Active ingredient
,CLAIMS:We claim:
1. A non-aqueous water dispersible granules (WDG) composition of insecticide.
2. The composition as claimed in claim 1, wherein insecticide is Pymetrozine.
3. The composition as claimed in claim 2, wherein the composition comprises:
a) Pymetrozine technical,
b) wetting agent,
c) dispersing agents,
d) disintegrating agent,
e) alcohol as solvent, and
f) inert fillers.
4. The composition as claimed in claim 3, wherein Pymetrozine used in the pesticidal formulations, in particular granulates is from 40 to 60% by weight and most preferably from 50% by weight.
5. The composition as claimed in claim 3, wherein the wetting agent is selected from the group consisting of non-ionic surfactants, anionic surfactant and a mixture of anionic and non-ionic surfactant and polymeric surfactant.
6. The composition as claimed in claim 5, wherein the wetting agent is preferably selected from alpha olefin sulfonates, sodium lauryl sulphate, polyoxyalkylene alkyl ether, polyoxyalkylene alkyl ether, polyoxyalkylene alkyl phenyl ether sulfonates, dialkylsuccinate, polyalkyl naphthalene sulphonate.
7. The composition as claimed in claim 6, wherein the wetting agent is used in an amount of 0.5 to 5%, more preferably 1 to 4% of the total weight of the composition.
8. The composition as claimed in claim 3, wherein the dispersing agent is selected from group comprising sodium lignosulphonates; sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenol ethoxylate phosphate esters; aliphatic alcohol ethoxylates; alky ethoxylates; EO-PO block copolymers; and graft copolymers, polycarboxylates, alkyl naphthalene sulfonates, phenol sulphonic acid condensates, lignosulphonates, methyl oleyltaurates and poly vinyl alcohols.
9. The composition as claimed in claim 8, wherein the dispersing agent is preferably selected from group comprising polycarboxylates, alkyl naphthalene sulfonates, phenol sulphonic acid condensates, lignosulphonates, methyl oleyltaurates and poly vinyl alcohols.
10. The composition as claimed in claim 9, wherein the dispersing agent is used in an amount of 0.5 to 6%, more preferably 2 to 6% of the total weight of the composition.
11. The composition as claimed in claim 3, wherein the disintegrating agent is selected from group comprising microcrystalline cellulose, crosslinked PVP, ammonium sulphate, sodium sulphate, sodium citrate, polycarboxylates, sodium phenylsulphonates, sodium bicarbonate, magnesium sulphate, sodium starch glycolate, sodium lignin sulfonate, sodium lauryl sulfate, combinations of carbonates with solid acids, agar, starch, hydroxypropyl starch, sodium alginate, carboxymethyl starch ether, gum arabic, gum tragacanth, gelatin, casein, crystalline cellulose, carboxymethylcellulose calcium, Tween, Pluronic, sodium laurate, carboxylic resins, ammonium sulfate, potassium chloride, sodium chloride, urea, anionic surfactants, calcium chloride, magnesium chloride, aluminum chloride, glucose, lactose, sodium glutamate, sodium inosinate, dextrin, blend of sulphonates (sodium, calcium, potassium, magnesium or mixture thereof).
12. The composition as claimed in claim 11, wherein the disintegrating agent is preferably selected from group comprising microcrystalline cellulose, crosslinked PVP, ammonium sulphate, sodium sulphate, sodium citrate, polycarboxylates, sodium phenylsulphonates, sodium bicarbonate, magnesium sulphate and blend of sulphonates (Sodium, calcium, potassium, magnesium or mixture thereof).
13. The composition as claimed in claim 12, wherein the disintegrating agent is used in an amount of 1 to 20%, more preferably 5 to 10% of the total weight of the composition.
14. The composition as claimed in claim 3, wherein the alcohol is selected from group comprising C1 to C4 alkanols selected from methanol, ethanol, n-propanol, isopropanol (isopropyl alcohol), n-Butanol, t-Butanol or iso-butanol, amyl alcohol, methyl amyl alcohol, cyclohexanol, 2-ethylhexanol, furfuryl alcohol, tetrahydrofurfuryl alcohol and d-limonene acetonitrile, toluene, dichloromethane, dichloroethane, Tetrahydrofuran (THF), 2-methyltetrahydrofuran (2-Me-THF), Dimethoxyethane (DME), 1,4-dioxane, acetone, ethyl acetate, Methyl tert-butyl ether (MTBE), Di-isopropyl ether (DIPE), ethylene glycol (EG), diethylene glycol (DEG), poly polyethylene glycol 400 (PEG 400), propylene glycol (PG), alkanolamides, ethoxylated alkanolamides, ethylene bisamides and glycerol or mixture thereof.
15. The composition as claimed in claim 14, wherein the alcohol is preferably selected from group comprising are methanol, ethanol, n-propanol, isopropanol (isopropyl alcohol), n-Butanol, t-Butanol or iso-butanol, acetonitrile, toluene, dichloromethane, dichloroethane, Tetrahydrofuran (THF), 2-methyltetrahydrofuran (2-Me-THF), Dimethoxyethane (DME), 1,4-dioxane, acetone, ethyl acetate, Methyl tert-butyl ether (MTBE), Di-isopropyl ether (DIPE), ethylene glycol (EG), diethylene glycol (DEG), poly polyethylene glycol 400 (PEG 400), propylene glycol (PG) and glycerol or mixture thereof.
16. The composition as claimed in claim 15, wherein the alcohol is used in an amount 1 to 50% by weight, preferably from 5 to 40% by weight and most preferably from 10 to 30% by weight.
17. The composition as claimed in claim 3, optionally contains binding agent selected from starch, maltodextrins, carboxymethyl cellulose, polyvinyl pyrrolidone, polyvinyl alcohol, polyvinyl acetate copolymers, polyacrylate, gelatine, polyacrylamide, oligosaccharides, lecithin, sodium starch glycolate, and a mixture thereof.
18. The composition as claimed in claim 17, the binding agent is used in an amount of 0 to 5%, more preferably 0 to 2% of the total weight of the composition.
19. The composition as claimed in claim 3, wherein the water dispersible granulation is prepared by a process using alcohol as solvent.
20. The process as claimed in claim 19, wherein the process comprising the steps of:
a) pre-blending of Pymetrozine with wetting agent, dispersing agent, disintegrating agent, and inert filler,
b) micronizing pre-blended mixture in air jet mill to get the desired particle size,
c) preparing the dough by employing an alcohol, and
d) extruding using an extruder and drying under vacuum to obtain water dispersible granules.
21. The composition as claimed in claim 1, wherein the non-aqueous water dispersible granules (WDG) formulation of Pymetrozine is used as insecticides for application to plants.
Dated this Twenty Eighth (28th) day of May, 2019.
__________________________________
Dr. S. Padmaja
Agent for the Applicant
IN/PA/883
| # | Name | Date |
|---|---|---|
| 1 | 201941011739-FORM-27 [20-09-2024(online)].pdf | 2024-09-20 |
| 1 | 201941011739-PROVISIONAL SPECIFICATION [26-03-2019(online)].pdf | 2019-03-26 |
| 2 | 201941011739-POWER OF AUTHORITY [26-03-2019(online)].pdf | 2019-03-26 |
| 2 | 201941011739-RELEVANT DOCUMENTS [13-07-2023(online)].pdf | 2023-07-13 |
| 3 | 201941011739-IntimationOfGrant26-07-2022.pdf | 2022-07-26 |
| 3 | 201941011739-FORM 1 [26-03-2019(online)].pdf | 2019-03-26 |
| 4 | 201941011739-Proof of Right (MANDATORY) [03-04-2019(online)].pdf | 2019-04-03 |
| 4 | 201941011739-PatentCertificate26-07-2022.pdf | 2022-07-26 |
| 5 | Correspondence by Agent_Form 1_Power of Attorney_08-04-2019.pdf | 2019-04-08 |
| 5 | 201941011739-AMMENDED DOCUMENTS [15-07-2022(online)].pdf | 2022-07-15 |
| 6 | 201941011739-FORM-9 [28-05-2019(online)].pdf | 2019-05-28 |
| 6 | 201941011739-FORM 13 [15-07-2022(online)].pdf | 2022-07-15 |
| 7 | 201941011739-MARKED COPIES OF AMENDEMENTS [15-07-2022(online)].pdf | 2022-07-15 |
| 7 | 201941011739-FORM 3 [28-05-2019(online)].pdf | 2019-05-28 |
| 8 | 201941011739-ENDORSEMENT BY INVENTORS [28-05-2019(online)].pdf | 2019-05-28 |
| 8 | 201941011739-CLAIMS [31-01-2022(online)].pdf | 2022-01-31 |
| 9 | 201941011739-COMPLETE SPECIFICATION [28-05-2019(online)].pdf | 2019-05-28 |
| 9 | 201941011739-COMPLETE SPECIFICATION [31-01-2022(online)].pdf | 2022-01-31 |
| 10 | 201941011739-CORRESPONDENCE [31-01-2022(online)].pdf | 2022-01-31 |
| 10 | 201941011739-FORM 18 [03-06-2021(online)].pdf | 2021-06-03 |
| 11 | 201941011739-FER.pdf | 2021-10-17 |
| 11 | 201941011739-FER_SER_REPLY [31-01-2022(online)].pdf | 2022-01-31 |
| 12 | 201941011739-FORM 3 [31-01-2022(online)].pdf | 2022-01-31 |
| 12 | 201941011739-OTHERS [31-01-2022(online)].pdf | 2022-01-31 |
| 13 | 201941011739-FORM 3 [31-01-2022(online)].pdf | 2022-01-31 |
| 13 | 201941011739-OTHERS [31-01-2022(online)].pdf | 2022-01-31 |
| 14 | 201941011739-FER.pdf | 2021-10-17 |
| 14 | 201941011739-FER_SER_REPLY [31-01-2022(online)].pdf | 2022-01-31 |
| 15 | 201941011739-CORRESPONDENCE [31-01-2022(online)].pdf | 2022-01-31 |
| 15 | 201941011739-FORM 18 [03-06-2021(online)].pdf | 2021-06-03 |
| 16 | 201941011739-COMPLETE SPECIFICATION [28-05-2019(online)].pdf | 2019-05-28 |
| 16 | 201941011739-COMPLETE SPECIFICATION [31-01-2022(online)].pdf | 2022-01-31 |
| 17 | 201941011739-ENDORSEMENT BY INVENTORS [28-05-2019(online)].pdf | 2019-05-28 |
| 17 | 201941011739-CLAIMS [31-01-2022(online)].pdf | 2022-01-31 |
| 18 | 201941011739-MARKED COPIES OF AMENDEMENTS [15-07-2022(online)].pdf | 2022-07-15 |
| 18 | 201941011739-FORM 3 [28-05-2019(online)].pdf | 2019-05-28 |
| 19 | 201941011739-FORM-9 [28-05-2019(online)].pdf | 2019-05-28 |
| 19 | 201941011739-FORM 13 [15-07-2022(online)].pdf | 2022-07-15 |
| 20 | Correspondence by Agent_Form 1_Power of Attorney_08-04-2019.pdf | 2019-04-08 |
| 20 | 201941011739-AMMENDED DOCUMENTS [15-07-2022(online)].pdf | 2022-07-15 |
| 21 | 201941011739-Proof of Right (MANDATORY) [03-04-2019(online)].pdf | 2019-04-03 |
| 21 | 201941011739-PatentCertificate26-07-2022.pdf | 2022-07-26 |
| 22 | 201941011739-IntimationOfGrant26-07-2022.pdf | 2022-07-26 |
| 22 | 201941011739-FORM 1 [26-03-2019(online)].pdf | 2019-03-26 |
| 23 | 201941011739-RELEVANT DOCUMENTS [13-07-2023(online)].pdf | 2023-07-13 |
| 23 | 201941011739-POWER OF AUTHORITY [26-03-2019(online)].pdf | 2019-03-26 |
| 24 | 201941011739-PROVISIONAL SPECIFICATION [26-03-2019(online)].pdf | 2019-03-26 |
| 24 | 201941011739-FORM-27 [20-09-2024(online)].pdf | 2024-09-20 |
| 1 | 201941011739E_09-08-2021.pdf |
| 1 | Document2E_09-08-2021.pdf |
| 2 | 201941011739E_09-08-2021.pdf |
| 2 | Document2E_09-08-2021.pdf |