DESC:Technical Field of the Invention:
The present invention relates to a process for preparation of a water dispersible granule composition comprising microcapsule containing agrochemical active ingredients for agricultural, public health, industrial and forestry use.

More particularly, the present invention relates to a process for preparation of water dispersible granule composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C, selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer; wherein said process comprises preparation of encapsulated suspension initially, followed by conversion of encapsulated suspension into water dispersible granules by spray drying. The said process improves formulation quality with mean particle size and provides a flowable formulation with enhanced stability, dispersibility and suspensibility.

The present invention also relates to water dispersible granule composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C prepared by said process; wherein said process provides enhanced stability, suspensibility and dispersibility to the composition under low as well as high temperature conditions throughout its storage period.

Background and Prior art of the Invention:
In recent years, one of the major concerns is the storage of agrochemicals. Agrochemicals, when stored in bulk storage systems pose significant environmental risks. The actives in agrochemicals deteriorate with environmental conditions and are vulnerable to high or freezing temperatures, high humidity and sunlight conditions. The high temperatures can change the chemistry of actives by expansion. Freezing temperature can result in separation of active ingredients from solvents or emulsifiers, or inactivation of emulsifiers, which may lead to crystallization or coagulation. High humidity and exposure to sunlight conditions causes breakdown or dissolve and release the actives in agrochemicals thereby making them ineffective and unusable.
Microencapsulation is one of the effective techniques used to reduce the effect of environmental conditions over the actives in agrochemicals. It has been used to protect the actives from environmental hazards such as humidity, light or heat. The unique advantage of microencapsulation lies in that the core material is completely coated and isolated from external environment. Microencapsulation would not affect the properties of core active, therefore it is very suitable for improving the stability and sustainability of active.

Active ingredients are encapsulated for a variety of reasons, including protection of the ingredient from degradation during processing and storage, timed release of the ingredient, prevention of premature reactions, prevention of unwanted reactions catalyzed by minerals, emulsification, and precise delivery of the ingredient during usage.

In agriculture, water dispersible granules (WDG) are widely accepted form for active agents. WDGs are formulated in many different ways depending on the physico-chemical properties of the active ingredient and the manufacturing equipment available. WDGs to be applied after disintegration and have uniform dispersion upon dilution in water. WDGs are becoming popular because they are easy to handle, non-dusty, have better stability and other processing benefits. The WDG formulations can easily be measured and diluted at the time of application. It provides fast dispersion in water for spray applications. These formulations minimize the risk of inhalation, contamination of non-target area as posed in application of conventional wettable powder compositions.

Some of the insecticides such as alpha-cypermethrin, lambda-cyhalothrin, bifenthrin, deltamethrin, cypermethrin, and the like exhibit itching to the applicator while field application. However, when such actives are encapsulated within a polymeric shell wall and converted into a WDG, these problems of itching are not faced by the applicator, since applicator is not directly exposed to the chemical. There are no dust and inhalation hazards to the applicator during handling of these formulations. WDG formulations are solid and contain very little or no solvent, hence no problem of toxicity or flammability due to solvents. These formulations do not contain any organic solvents, thus making it safer for the crop as well as for the environment.

There are some difficulties in formulating low melting point agricultural active ingredient into water dispersible granules such as active tends to melt or soften when exposed to high temperature or long storage conditions, thus resulting into final product having low suspensibility and sustainability. Hence, it is necessary to avoid raising the temperature of the active above its melting point and should be kept in physical state to prevent the active from becoming too soft and flowing too freely or making it very difficult to reduce to discrete particles.

Currently actives with lower melting points are formulated into emulsifiable concentrate (EC) formulations, which consists of petroleum solvents such as Xylene, Toulene, etc., however these formulations are known to cause phytotoxicity to crops and to environment, due to use of solvent at very high concentration. Wettable powder (WP) formulations with lower melting point actives can also be formulated, however these formulations are not considered to be very safe due to dusting problem. These are also very difficult to transport as they occupy more space due to low bulk density.

There are some patent literatures that discloses about water dispersible granules with low melting point actives. EP0252896 is directed to a process for preparing a water-dispersible granule comprising: (a) forming an aqueous suspension comprising discrete microcapsules containing at least one water-insoluble pesticide within a polymeric shell wall suspended in an aqueous liquid; and (b) forming droplets of said aqueous suspension and spray drying said droplets to form essentially spherical water-dispersible granules which are from about 150 to about 850 microns in diameter and which contain up to about 8.0% moisture, wherein each water-dispersible granule is an aggregation of said microcapsules. However, formulations prepared from aqueous suspensions exhibit long term stability issues.

US5846903 discloses and claims a process for preparation of water dispersible granules comprising low melting point pesticides, the process comprises milling the active substance with a first portion of a finely divided filler to give a finely divided mixture and then blending a second portion of a finely divided filler and a surfactant with the finely divided mixture, wetting the blend with water and then granulating the blend. However, the process for preparation of WDG disclosed in US’903 involves single active pesticidal ingredient and multiple process steps which makes said process commercially not viable. Also, the process for preparation of water dispersible granules of US’903 involves extrusion process that has some limitations such as variation in size of product, impurities on the surface, fluid is under high pressure/high pressure hence difficult to attain and high initial cost setup.

US5665678 discloses and claims an aqueous, stable pesticidal suspension that comprises low melting temperature pesticide active ingredient having melting point in the range from about 30°C to about 130°C, a nucleating agent having a melting point in the range from about 30° to about 130° and having a chain length in the range from about 3 to about 30 and a porous carrier; wherein the nucleating agents provides effective nucleation of a supercooled pesticide active (or a mixture of pesticide actives), and subsequent rapid crystallization of the pesticide active, for preparation of WP, WG, SC, etc. However, the pesticidal suspension disclosed in US’678 is of single active ingredient and is silent on active ingredient with melting point below 30°C.

US6419942 discloses and claims a process for production of a water-dispersible composition containing a microencapsulated pesticide, said process comprising; (a) preparing an aqueous suspension comprising microcapsules containing at least one water-insoluble pesticide enclosed within a polymeric shell suspended in an aqueous medium containing a water-soluble polymer; and (b) spray-drying the aqueous suspension of step (a) to produce a water-dispersible composition comprising said microcapsules in a matrix comprising the water-soluble polymer, wherein the water-soluble polymer comprises from about 4 to about 15 weight percent of the water-dispersible composition. However, the water dispersible composition comprising microcapsules disclosed in US’942 has particle size range of approximately 20-80 microns. Thus composition having such a larger particle size fails to exhibit higher field efficacy.

The water dispersible granules disclosed in the art comprises a solo active ingredient from pesticides. In general, the disease controlling activity is very limited in a single or solo ingredient formulations/composition thereby disease control is narrow and there is always chances of run of deterrents. The main concern with the repeated use of active belongs to any insecticides/ pesticides/ herbicides/ fungicides in solo ingredient formulations is the development of resistance by the causing organism for that particular active and at the end one has to apply more concentrated formulation of agrochemicals. The formulation with high amount of agrochemical when applied on the field may result in toxicity to human beings as well as have bad effects on the environment.

Thus, there is a requirement of agrochemical composition combining more than one active ingredient that reduce the need for multiple individual applications while providing better disease/insect/weed controlling activity. Another requirement also includes composition of combination of more than one active ingredients having synergistic effect which can be extensively applied in the field of agricultural for controlling wide spectra of disease/insect/weed which also exhibits good physical and chemical stability.

Further to reduce the risk of development of resistant strains, mixtures of different active compounds can employed for controlling harmful insects or pests or fungus or any other pathogens. It is possible to ensure successful control over a relatively long period of time by combining active compounds having different mechanisms of action.

Object of the Invention:
The inventors of the present invention addresses the stability related problems of low melting point actives and drawbacks of solo/single ingredient formulations in the art and provides a solution to these problems by preparing a water dispersible granule composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting points. The present process comprises encapsulating the active ingredient within a polymeric shell wall which avoid raising of the temperature of active above its melting point and further process which involves conversion of encapsulated suspension into water dispersible granules by spray drying improves formulation quality with mean particle size thereby providing a flowable formulation with enhanced stability, dispersibility and suspensibility. Thus, this becomes the main object of present invention.

Another object of the present invention is to provide water dispersible granule composition prepared by present process; wherein said process provides enhanced stability, suspensibility and dispersibility to the composition under low as well as high temperature conditions throughout its storage period.

Another object of the present invention is to provide water dispersible granule composition prepared by present process comprising microcapsule which is encapsulated with polymeric shell wall that provides controlled release of actives in the field thereby achieving higher efficacy for longer period of time and higher yield.

Another object of the present invention is to also addresses the problems where extrusion granulation as such is not practical and provides a solution of process wherein the active ingredients is formulated into capsule suspension which is further spray dried to convert into water dispersible granules. The said process improves the formulation quality with mean particle size and provides a flowable formulation with enhanced stability, dispersibility and suspensibility.

Yet another object of the present invention is to provide a process for preparation of water dispersible granule composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting points, which is more cost effective, safer to use, user friendly and environmental friendly.

Summary of the Invention:
In accordance with the above objective, in a preferred aspect, the present invention describes a process for preparation of water dispersible granules composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C; wherein said process comprises preparation of encapsulated suspension initially, followed by conversion of encapsulated suspension into water dispersible granules by spray drying.

In another preferred aspect, the present invention describes a process for preparation of water dispersible granule composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C; wherein, the said process improves the formulation quality with mean particle size and provides a flowable formulation with enhanced stability, dispersibility and suspensibility.

In another aspect, the present invention describes a process for preparation of water dispersible granule composition comprising microcapsules having particle size (D90) maintained between 0.1 micron to 25 micron.

In another aspect, the present invention describes agrochemical active ingredients that are selected from pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticide, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator, flowering inducer and mixtures thereof.

In another aspect, the present invention describes a water dispersible granules composition comprising microcapsule containing at least two or more active ingredients having low melting point of less than 120°C; wherein the active ingredients are encapsulated within a polymeric shell wall that provides controlled release of actives for longer period thereby improving crop health and increasing crop yield.

In another aspect, the present invention describes a water dispersible granule composition prepared with agrochemically active excipients/adjuvants selected from suspending agent, emulsifying agent, dispersing agent, stabilizer, thickeners, wetting agent, coating agent, solvent, fillers, pH adjusting agent and the like.

In another aspect, the present invention describes a water dispersible granule composition comprising microcapsule prepared by said process; wherein the said process provides enhanced stability, suspensibility and dispersibility to the composition under low as well as high temperature conditions throughout its storage period.

In yet another aspect, the present invention describes a process for preparation of water dispersible granules comprising microcapsules that stored under as low as -20°C to as high as +54°C temperature conditions.

In yet another aspect, the present invention describes a process for preparation of water dispersible granules comprising microcapsule for agricultural, public health, industrial and forestry use.

In yet another aspect, the present invention describes variety of crops on which a water dispersible granule composition comprising microcapsule prepared by present process can be applied that include pulses, oil seeds, cereals, legumes, all field crops, horticulture pastures, forestry and non-crop lands.

In yet another aspect, the present invention describes a method of controlling infestation/diseases/weed, improving crop health and increasing crop yield by applying minimum doses of water dispersible granule composition comprising microcapsule prepared by present process and achieving maximum control of disease/infestation/weeds.

In yet another aspect, the present invention describes a water dispersible granule composition comprising microcapsule prepared by present process that exhibits higher/enhanced field efficacy, good physical and chemical properties, good release properties, fine particle size distribution, improved stability, dispersibility and suspensibility even at extended storage under any temperature condition.

Detailed Description of the Invention:
The present invention will now be described in detail in connection with certain embodiments, so that various aspects thereof may be fully understood and appreciated.

Reference phrases:
The phrase “low melting point agrochemical active ingredients” used in the present invention refers to the active ingredients having melting point in the range of -20°C to 120°C.

The phrases "composition" and "formulation" can be used interchangeably in the present invention to denote a composition for agricultural use or an agricultural dosage form formulation.

The phrase “suspensibility” used in the present invention refers to degree of suspension of actives in the solution for a defined period.

The phrase “dispersibility” used in the present invention refers to uniform distribution of particles in the solution.

The phrase “Dry Capsule (DC)” used in the present invention refers to composition/formulation of present invention which involves preparation of encapsulated suspension initially and conversion of the same into water dispersible granules by spray drying.

In one embodiment, the present invention discloses a process for preparation of water dispersible granule composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C; wherein said process comprises preparation of encapsulated suspension initially, followed by conversion of encapsulated suspension into water dispersible granules by spray drying. The said process improves formulation quality with mean particle size and provides a flowable formulation with enhanced stability, dispersibility and suspensibility.

In another embodiment, the present invention discloses a process for preparation of water dispersible granule composition by conversion of capsule suspension (CS) into water dispersible granules (WDG) by spray drying. The prepared water dispersible granule composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator, flowering inducer or mixture thereof.

In a preferred embodiment, the present invention discloses a process for preparation of water dispersible granule composition comprising microcapsule that mainly comprises two stages:-
(i) preparation of encapsulated suspension comprising at least two or more active ingredients having low melting point of less than 120°C; wherein said preparation comprises organic phase, aqueous phase, encapsulation phase and curing phase;
and
(ii) conversion of encapsulated suspension into water dispersible granule by spray drying.

Stage 1: Preparation of encapsulated suspension comprising low melting point active ingredients
a) Preparation of Organic Phase:
The Organic phase comprises of at least two or more agrochemical active ingredients having low melting point of less than 120°C selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer and solvent and encapsulating polymer-1.
The preparation of organic phase includes dissolving the agrochemical active ingredients having low melting point of less than 120°C in solvent and maintaining the temperature of 60°C followed by adding encapsulating polymer-1 and mixing well to get clear solution.

b) Preparation of Aqueous Phase:
The Aqueous phase comprise emulsifying agent, suspending agent and DM (demineralized) water. The preparation of aqueous phase includes mixing emulsifying agent and suspending agent along with DM water followed by heating and maintaining the temperature of 60°C. The said mixture is subjected to high-speed homogenizer and increasing the speed to desired rpm.

c) Encapsulation and Curing Phase:
The encapsulation and curing phase comprises organic phase, aqueous phase and encapsulating polymer-2. The process includes addition of organic phase of step (a) into aqueous phase of step (b) to obtain oil-in-water emulsion; and achieving the particle size to be less than 25 micron. Reducing the rpm and adding encapsulating polymer-2; mixing and curing at the temperature of 60°C for 2 hours followed by cooling the slurry to room temperature and adding stabilizer to obtain stable encapsulated suspension formulation.

Stage 2: Conversion of encapsulated suspension (CS) into water dispersible granules (WDG)
Mixing encapsulated suspension of above stage 1 with additional excipients viz., dispersing agents, wetting agents, stabilizers, thickeners, fillers and pH adjuster to make up the volume of suspension to 100% (total solid basis). Spraying the suspension under temperature range between 40°C-60°C to get granules that are further sieved to obtain the desired water dispersible granules.

Accordingly, in another preferred embodiment, a process for preparation of water dispersible granule composition comprising microcapsule comprises the steps of;
a) preparing an organic phase by dissolving at least two or more agrochemical active ingredients having low melting point of less than 120°C in solvent and maintaining the temperature of 60°C followed by adding encapsulating polymer-1 and mixing well to form clear solution;
b) preparing an aqueous phase by mixing emulsifying agent and suspending agent along with DM water followed by heating and maintaining the temperature of 60°C;
c) subjecting aqueous phase of step (b) to high-speed homogenizer and increasing the speed to 500-5000 rpm;
d) adding organic phase of step (a) into aqueous phase of step (c) to obtain oil-in-water emulsion and achieving the particle size to be less than 25 micron;
e) reducing the rpm and adding encapsulating polymer-2 to step (d); mixing and curing the temperature of 60°C for 2 hours followed by cooling the slurry at room temperature and adding stabilizer to obtain stable encapsulated suspension formulation;
f) mixing encapsulated suspension of step (e) with additional excipients viz., dispersing agents, wetting agents, stabilizers, thickeners, fillers and pH adjuster to make up the volume of suspension to 100% (total solid basis); and
g) spraying the suspension of step (f) under temperature range between 40°C-60°C to get granules that are further sieved to obtain the desired water dispersible granules.

In yet another preferred embodiment, the present invention discloses a water dispersible granules composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer; that exhibits enhanced stability, suspensibility and dispersibility under low as well as high temperature conditions throughout its storage period.

In yet another preferred embodiment, the present invention discloses a water dispersible granules comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer; that are encapsulated within polymeric shell wall which provide controlled release of actives for a longer period of time, thereby resulting in higher crop yield.

The low melting point agrochemical active ingredient that include insecticides are selected from Acynonapyr, Alanycarb, Benfuracarb, Bifenthrin, Cadusafos, Carbosulfan, Chlorpyrifos, Cyanophos, Cyfluthrin, ?-Cyhalothrin, Cypermethrin, Deltamethrin, Dimethoate, Esfenvalerate, Ethion, Etofenprox, Fenitrothion, Fenobucarb, Fenpropathrin, Fenvalerate, Flupyradifurone, Flupyrimin, Fluvalinate, Indoxacarb, Isoxathion, Malathion, Methidathion, Methomyl, Nitenpyram, Oxazosulfyl, Permethrin, Profenofos, Propargite, Prothiofos, Pyrethrins, Pyridalyl, Pyriproxyfen, Quinalphos, Silafluofen, Tebufenpyrad, Tefluthrin and the like.

The low melting point agrochemical active ingredient that include herbicides are selected from Benfluralin, Benfuresate, Clethodim, Clodinafop-propargyl, Napropamide, Pendimethalin, Prosulfocarb, Pyraflufen-ethyl, Quizalofop-ethyl, S-metolachlor, Sulfentrazone, Triclopyr, Trifluralin and the like.

The low melting point agrochemical active ingredient that include fungicides are selected from Azoxystrobin,, Cyflufenamid, Cyprodinil, Difenoconazole, Diflumetorim, Fenoxanil, Hexaconazole, Imibenconazole, Inpyrfluxam, Ipconazole, Iprobenfos, Isoprothiolane, Myclobutanil, Picoxystrobin, Propiconazole, Pyraclostrobin, Tebuconazole, Tetraconazole, Trifloxystrobin, Triflumizole and the like.

The low melting point agrochemical active ingredient that include plant growth regulators (PGR) are selected from Chlorpropham, Triacontanol and the like.

The agrochemical active ingredient is present in an amount ranging from 0.1% to 80% by weight.

The present water dispersible granules composition comprising microcapsule also comprises agrochemically acceptable excipients/adjuvants that includes suspending agent, emulsifying agent, dispersing agent, stabilizer, wetting agent, coating agent, solvent, thickeners, fillers, pH adjusting agent and the like, which is present in an amount ranges from 0.1% to 70% by weight.

The encapsulating polymer-1 used in the process as well as in the composition is selected from isocyanates such as polymethylene polyphenylene isocyanate (PMPPI), hexamethylene diisocyanate (HMDI), Napthalene diisocyanate, Methylene bis-cyclohexylisocyanate, isophorone diisocyanate (IPDI) or 4,4' methylenebis (cyclohexyl isocyanate), polyphenylisocyanate, Polymethylene polyphenylisocyanate, Toulene diisocyanate, and/or trimers of HMDI or IPDI, isomers of tolylene diisocyanate, isomers and derivatives of phenylene diisocyanate, isomers and derivatives of biphenylene diisocyanates, methylene diphenyl diisocyanate (MDI), polymeric polyisocyanates, biurets and blocked polyisocyanates, and the like; and is present in an amount ranges from 0.1 to 10%.

The encapsulating polymer-2 used in the process as well as in the composition is selected from polyamines such as diethylenetriamine, ethylenediamine, triethylenetetraamine, 1,4-diaminobutane, 1,5-diaminopentane, 1,4-Benzenediamine, Benzylamine, Ethyl amine, Butylamine, Propylamine, Isopropyamine, 1-methylbutylamine, Tert-butylamine, Cyclo-hexylamine, Phenylamine, 2-Pentanamine, 2-methylaniline, Hexamethylenediamine and the like; and is present in an amount ranging from 0.1 to 10%.

The emulsifying agents used in the process as well as in the composition is selected from acrylic polymer/copolymer, polyvinyl alcohol, Polyvinyl pyrolidone, EO-PO block copolymer, ethoxylated and ethopropoxylated alcohols and nonyl phenols, ethoxylated tristeryl phenol, ethoxylated tristeryl phenol phosphates, Tristyreneated phenol ethoxylate ethoxylated, 15 Polycarboxylate sodium, nonylphenol ethoxylate and ethopropoxylated castor oil, calcium alkyl benzene sulfonates and the like; and is present in an amount ranging from 0.1 to 15%.

The suspending agents used in the process as well as in the composition is selected from sodium salt of Napthalene formaldehyde condensate, sodium ligno sulphonate, potassium polycarboxylate and the like; and is present in an amount ranging from 2 to 15%.

The solvents used in the process as well as in the composition is selected from Naptha, aromatic chlorinated hydrocarbons, chlorinated maleic hydrocarbons, ketones, long chain esters and mixtures thereof, (commercially available as Solvesso 100, Solvesso 150, Solvesso 200, Solvesso 150ND, Solvesso 200ND, Aromatic 200, Hydrosol A 200, Hydrosol A 230/270, Caromax 20, Caromax 28, Aromat K 150, Aromat K 200, Shellsol A 150, Shellsol A 100, Fin FAS-TX 150, Fin FAST-TX 200, Xylene, Cyclohexane, Cyclopentane, Pentane, Hexane, Heptane, octane, nonane, decane, isooctane, benzene, 2- Methylpentane, 3-Methylpentane, 2-Methylhexane, 3-Methylhexane, 2-methylbutane, 2,3-Dimethylpentane, Methycyclopentane, Methylcyclohexane, 2,4 Dimethylpentane, aromatics such as benzene, toluene, cyclohexane, 1-Pentene, 2-Pentene, 1-Hexene, 1-Heptene, Cyclohexene, Ethylvinylether, Propylether, Isopropylether, petroleum distillates, petroleum ether, and the like, Butylvinylether, Butylethylether, 1,2 - Epoxybutane, Furan, Tetrahydropyran, 1-Butanal, 2-methylpropanal, 2-Pentanone, 3-Pentanone, Fluorbenzene, Hexafluorobenzene, Ethylformate, Propylformate, Isopropylformate, Ethylacetate, Methylacrylate, Ethylacrylate, Methyl-methacrylate, Dichloromethane, Tetramethylsilane, substituted aromatics such as chlorobenzene, benzaldehyde, xylenes and the like; and is present in an amount ranging from 5 to 30%.

The dispersing agents used in the process as well as in the composition is selected from naphthalene sulfonic acid, sodium salt condensed with formaldehyde, polyalcoxylated alkylphenol, naphthalene sulfonic acid formaldehyde condensate, methyl naphtaline-formaldehyde-condensate sodium salt, naphthalene condensates, lignosulfonates, polyacrylates and phosphate esters, calcium lignosulfonate, lignin sulfonate sodium salt, Sodium lingo sulphonate, and the like; and is present in an amount ranging from 2 to 15%.
The wetting agents used in the process as well as in the composition is selected from sodium N-methyl-N-oleoyl taurate, alkylated naphthalene sulfonate, sodium salt, mixture of isomers of dibutyl naphthalene sulphonic acid sodium salt, sodium isopropyl naphthalene sulphonate, sodium lauryl sulfate, alpha olifin sulphate, sodium salt of napthalene sulphate, dioctyl sulfate, alkyl naphthalene sulfonates, phosphate esters, sulphosuccinates and non-ionic such as tridexyl 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 alkyaryl phosphate esters, alkyl polysaccharide, di or mono alkyl sulfosuccinate derivatives, alpha olefin sulfonates, alkyl naphthalene sulfonates, dialkyl sulphosuccinates, butyl, dibutyl, isopropyl and diisopropyl naphthalene sulfonate salts, C12 alkyl benzene sulfonate or C10-C16 alkyl benzene sulfonate and the like; and is present in an amount ranging from 1 to 5%.

The stabilizers used in the process as well as in the composition is selected from polysaccharide, 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 and the like; and is present in an amount ranges from 0.1 to 2%.

The thickening agent/thickener used in the process as well as in the composition is selected from colloidal silica, precipitated silica, bentonite, aluminum silicate, calcium sulfonate, clay, talc and the like; and is present in an amount ranges from 1 to 10%.

The fillers used in the process as well as in the composition are selected from china clay, lactose, dextrin and the like; and is present in an amount ranging from 5 to 50%.

The pH adjusting agent used in the process as well as in the composition is selected from citric acid, acetic acid, sodium acetate and the like; and is present in an amount ranging from 0.5 to 2%.

In another preferred embodiment, the present invention discloses a water dispersible granules composition comprising microcapsule containing active ingredients in the range of 0.1% to 80%; encapsulating polymer in the range of 0.1 to 10%; emulsifying agent in the range of 0.1 to 15%; suspending agent in the range of 2 to 15%; solvent in the range of 5 to 30%; dispersing agent in the range of 2 to 15%; wetting agent in the range of 1 to 5%; stabilizer in the range of 0.1 to 2%; thickener in the range of 1 to 10%; fillers in the range of 5 to 50% and pH adjusting agent in the range of 0.5 to 2% by weight of the total composition.

In yet another preferred embodiment, the present invention discloses a water dispersible granules composition comprising microcapsule containing at least two or more agrochemical active ingredients selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer; wherein said combination is of active ingredients having melting point below 100°C.

In yet another preferred embodiment, the present invention discloses a water dispersible granules composition comprising microcapsule containing at least two or more agrochemical active ingredients selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer; wherein said combination is of active ingredients having melting point above 100°C.

In yet another preferred embodiment, the present invention discloses a water dispersible granules composition comprising microcapsule containing at least two or more agrochemical active ingredients selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer; wherein said combination is of active ingredients having melting point below 100°C and above 100°C.

In yet another embodiment, the microcapsules of the present composition is prepared by encapsulating the agrochemical active ingredient within shell wall made up of polyisocynates polyamides, polyols, polyesters, polysulfonamide, polyurethanes, polythioester, polyphosphonamide, polyiminourea, polyurea, polysiloxane, polyamine, aminoplast resins, polycarbonates or mixtures thereof.

In yet another embodiment, the shell wall of microcapsule is prepared from isocynate and amine that encapsulates the agrochemical active ingredient having low melting point of less than 120°C.

In yet another embodiment, the present invention discloses a water dispersible granules comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer; that are encapsulated within the polymeric shell wall which provides controlled release of actives, thereby resulting in higher crop yield.

In yet another embodiment, different ratio of isocynates and amines are adjusted to encapsulate the active ingredient which resulted into achieving controlled release of active ingredients for a longer period of time in the field.

In yet another embodiment, the particle size (D90) of microcapsule is maintained between 0.1 micron to 25 micron.

In yet another embodiment, the present invention describes a water dispersible granule composition comprising microcapsules containing at least two or more agrochemical active ingredients having low melting point of less than 120°C selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer; that exhibits enhanced stability, suspensibility and dispersibility under low as well as high temperature conditions ranging from -20°C to +54°C throughout its storage period.

In yet another embodiment, the present invention describes a process for preparation of water dispersible granules comprising microcapsule and composition thereof for agricultural, public health, industrial and forestry use.
In yet another embodiment, the present invention describes variety of crops on which a water dispersible granule composition comprising microcapsule prepared by present process can be applied that include pulses, oil seeds, cereals, legumes, all field crops, horticulture pastures, forestry and non-crop lands.

In yet another embodiment, the present invention describes a method of controlling infestation/diseases/weed, improving crop health and increasing crop yield by applying minimum doses of water dispersible granule composition prepared by present process and achieving maximum control of disease/infestation/weeds.

In yet another embodiment, the present invention describes a method of controlling infestation/diseases/weed, improving crop health and increasing crop yield by applying in the field the present water dispersible granules composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer.

In yet another embodiment, the present invention describes a process for preparation of water dispersible granule comprising microcapsule and composition thereof that exhibits higher/enhanced field efficacy, good physical and chemical properties, good release properties, fine particle size distribution, improved stability and suspensibility even at extended storage under any temperature condition.

Examples:
Some examples illustrating the embodiments of the present invention are provided; however, these are exemplary only and should not be regarded as limiting the elements of the present invention.

Example 1: Process for preparation of Water dispersible granule of present invention
a) preparing an organic phase by dissolving at least two or more agrochemical active ingredients having low melting point of less than 120°C in solvent and maintaining the temperature of 60°C followed by adding encapsulating polymer-1 and mixing well to form clear solution;
b) preparing an aqueous phase by mixing emulsifying agent and suspending agent along with DM water followed by heating and maintaining the temperature of 60°C;
c) subjecting aqueous phase of step (b) to high-speed homogenizer and increasing the speed to 500-5000 rpm;
d) adding organic phase of step (a) into aqueous phase of step (c) to obtain oil-in-water emulsion and achieving the particle size to be less than 25 micron;
e) reducing the rpm and adding encapsulating polymer-2 to step (d); mixing and curing at the temperature of 60°C for 2 hours followed by cooling the slurry at room temperature and adding stabilizer to obtain stable encapsulated suspension formulation;
f) mixing encapsulated suspension of step (e) with additional excipients viz., dispersing agents, wetting agents, stabilizers, thickeners, fillers and pH adjuster to make up the volume of suspension to 100% (total solid basis); and
g) spraying the suspension of step (f) under temperature range between 40°C-60°C to get granules that are further sieved to obtain the desired water dispersible granules.

Example 2: Composition 1 –
Difenconazole + Trifloxystrobin (Fungicide + Fungicide) DC
Sr. No. Ingredients Quantity (%) Role / Function
1. Difenconazole (76°C M.P.) 15 Active ingredient
2. Trifloxystrobin (72°C M.P.) 35 Active ingredient
3. Acrylic polymer 5 Emulsifying agent
4. Solvent Naptha 10 Solvent
5. Polymethylene polyphenylisocyanate 1.5 Encapsulating polymer-1
6. Diethylenetriamine 0.5 Encapsulating polymer-2
7. Citric Acid 0.5 pH adjusting agent
8. Sodium Ligno sulphonate 5 Suspending agent
9. Sodium Lauryl sulphates 3 Wetting agent
10. Polysaccharide 0.1 Stabilizer
11. China clay 24.4 Filler
Total 100
M.P.-Melting Point
Example 3: Process for preparation of Water dispersible granules (Composition 1) of Difenconazole + Trifloxystrobin (Fungicide + Fungicide)
a) Preparing an organic phase by dissolving 15gm of Difenconazole and 35gm of Trifloxystrobin in 10gm of solvent Naphtha and maintaining the temperature of 60°C followed by addition of 1.5gm of Polymethylenepolyphenylisocyanate and mixing well to form clear solution;
b) preparing aqueous phase by mixing 5gm of acrylic copolymer and 5gm of sodium ligno sulphonate along with 100ml of DM water followed by heating and maintaining the temperature of 60°C;
c) subjecting the aqueous phase of step (c) to high-speed homogenizer and increasing the speed to 500 to 5000rpm;
d) adding organic phase of step (b) into aqueous phase of step (d) to obtain oil-in-water emulsion; and achieving the particle size to be less than 25 micron;
e) reducing the rpm and adding 0.5gm of diethylenetriamine to step (e) followed by mixing and curing at the temperature of 60°C for 2 hours followed by cooling the slurry to room temperature and adding polysaccharides to obtain stable capsule suspension;
f) mixing encapsulated suspension of step (e) with additional excipients viz., 3gm of sodium lauryl sulphates, 15gm of sodium sulphate, 0.5gm of citric acid and 9.5gm of china clay to make up the volume of suspension to 100% (total solid basis); and
g) spraying the suspension of step (f) under temperature range between 40°C-60°C to get granules that are further sieve to obtain the desired water dispersible granules.

Example 4: Composition 2 –
Chlorpyrifos + Cypermethrin (Insecticide + Insecticide) DC
Sr. No. Ingredients Quantity (%) Role / Function
1. Chlorpyrifos (42°C M.P.) 50 Active ingredient
2. Cypermethrin (83°C M.P.) 5 Active ingredient
3. Acrylic polymer 2 Emulsifying agent
4. Solvent Naptha 10 Solvent
5. Polymethylene polyphenylisocyanate 3.5 Encapsulating polymer-1
6. Diethylenetriamine 1.2 Encapsulating polymer-2
7. Citric Acid 0.5 pH adjusting agent
8. Sodium Ligno sulphonate 5 Suspending agent
9. Sodium Lauryl sulphates 5 Wetting agent
10. Polysaccharide 0.1 Stabilizer
11. China clay 17.7 Filler
Total 100
M.P.-Melting Point

Example 5: Composition 3 –
Pyraclostrobin + Propargite (Fungicide + Insecticide) DC
Sr. No. Ingredients Quantity (%) Role / Function
1. Pyraclostrobin (65°C M.P.) 10 Active ingredient
2. Propargite (?25°C M.P.) 10 Active ingredient
3. Polyvinyl alcohol 2.5 Emulsifying agent
4. Toulene diisocyanate 1 Encapsulating polymer-1
5. Ethylenediamine 0.5 Encapsulating polymer-2
6. Citric acid 0.5 pH adjusting agent
7. Sodium salt of Napthalene formaldehyde condensate 10 Suspending agent
8. Alpha olifin sulphate 5 Wetting agent
9. Precipitated silica 5 Thickening agent
10. Lactose 55.5 Filler
Total 100
M.P.-Melting Point

Example 6: Composition 4 –
Bifenthrin + Chlorpyrifos + Tricontanol (Insecticide + Insecticide + PGR) DC
Sr. No. Ingredients Quantity (%) Role / Function
1. Bifenthrin (69°C M.P.) 5 Active ingredient
2. Chlorpyrifos (42°C M.P.) 20 Active ingredient
3. Tricontanol (87°C M.P.) 0.1 Active ingredient
4. EO-PO Block Copolymer 5 Emulsifying agent
5. Solvent Naptha 10 Solvent
6. Hexamethylene diisocyanate 3 Encapsulating polymer-1
7. Triethylene tetraamine 1 Encapsulating polymer-2
8. Citric acid 0.5 pH adjusting agent
9. Potassium Polycarboxylate 20 Suspending agent
10. Sodium salt of napthalene sulphate 5 Wetting agent
11. Dextrin 30.4 Filler
Total 100
M.P.-Melting Point

Example 7: Composition 5 –
Propiconazole + Picoxystrobin (Fungicide + Fungicide) DC
Sr. No. Ingredients Quantity (%) Role / Function
1. Propiconazole (?25°C M.P.) 40 Active ingredient
2. Picoxystrobin (75°C M.P.) 15 Active ingredient
3. Acrylic polymer 2.5 Emulsifying agent
4. Solvent Naptha 5 Solvent
5. Polymethylene polyphenylisocyanate 1.5 Encapsulating polymer-1
6. Diethylenetriamine 0.5 Encapsulating polymer-2
7. Citric Acid 0.5 pH adjusting agent
8. Sodium Ligno sulphonate 10 Suspending agent
9. Sodium Lauryl sulphates 5 Wetting agent
10. Polysaccharide 0.1 Stabilizer
11. China clay 14.9 Filler
Total 100
M.P.-Melting Point

Example 8: Composition 6 –
Azoxystrobin + Hexaconazole (Fungicide + Fungicide) DC
Sr. No. Ingredients Quantity (%) Role / Function
1. Azoxystrobin (116°C M.P.) 25 Active ingredient
2. Hexaconazole (111°C M.P.) 5 Active ingredient
3. Acrylic polymer 3 Emulsifying agent
4. Solvent Naptha 20 Solvent
5. Polymethylene polyphenylisocyanate 2.5 Encapsulating polymer-1
6. Diethylenetriamine 0.7 Encapsulating polymer-2
7. Citric Acid 0.5 pH adjusting agent
8. Sodium Ligno sulphonate 15 Suspending agent
9. Sodium Lauryl sulphates 10 Wetting agent
10. Polysaccharide 0.1 Stabilizer
11. China clay 18.9 Filler
Total 100
M.P.-Melting Point
Example 9: Composition 7 –
Pyriproxyfen + Tebuconazole (Insecticide + Fungicide) DC
Sr. No. Ingredients Quantity (%) Role / Function
1. Pyriproxyfen (46°C M.P.) 25 Active ingredient
2. Tebuconazole (102°C M.P.) 1.5 Active ingredient
3. Acrylic polymer 5 Emulsifying agent
4. Solvent Naptha 20 Solvent
5. Polymethylene polyphenylisocyanate 2.5 Encapsulating polymer-1
6. Diethylenetriamine 0.5 Encapsulating polymer-2
7. Citric Acid 0.5 pH adjusting agent
8. Sodium Ligno sulphonate 10 Suspending agent
9. Sodium Lauryl sulphates 5 Wetting agent
10. Polysaccharide 0.1 Stabilizer
11. China clay 19.9 Filler
Total 100
M.P.-Melting Point

Example 10: Composition 8 –
Propargite + Ethion (Insecticide + Insecticide) DC
Sr. No. Ingredients Quantity (%) Role / Function
1. Propergite (<25°C M.P.) 15 Active ingredient
2. Ethion (-13°C M.P.) 5 Active ingredient
3. Acrylic polymer 5 Emulsifying agent
4. Solvent Naptha 20 Solvent
5. Polymethylene polyphenylisocyanate 2.5 Encapsulating polymer-1
6. Diethylenetriamine 1 Encapsulating polymer-2
7. Citric Acid 1 pH adjusting agent
8. Sodium Ligno sulphonate 15 Suspending agent
9. Sodium Lauryl sulphates 5 Wetting agent
10. Polysaccharide 0.1 Stabilizer
11. China clay 30.4 Filler
Total 100
M.P.-Melting Point

The dry capsule (DC) Composition 2 to Composition 8 given in above Example 4 to Example 10 is prepared as per the process steps provided in Example 1 above.

Experimental Data:

Example 11: Suspensibility and Dispersibility Study Comparison @ 14 days - Dry Capsule (DC) formulations VS. Direct WDG formulations
The suspensibility and dispersibility of Dry Capsule (present formulations) and Direct WDG are tested for 14 days under low as well as high temperature conditions and observations are provided in below Table 1:
Table 1:
Sr.
No. Product Description Formulation Type Suspensibility Observation for 14 days Dispersibility Observation for 14 days
Initial ATS at
-20°C ATS at 54°C Initial ATS at -20°C ATS at 54°C
1. Difenoconazole 15% + Trifloxystrobin 35% Direct WDG 80.33% 80.25% 79.54% 81.37% 81.42% 81.23%
Difenoconazole 15% + Trifloxystrobin 35% Dry Capsule 85.89% 85.65% 82.72% 87.72% 88.01% 87.69%
2. Pyraclostrobin 10% + Propargite 10% Direct WDG 82.14% 82.19% 79.18% 80.94% 80.92% 80.55%
Pyraclostrobin 10% + Propargite 10% Dry Capsule 86.77% 86.69% 84.32% 86.71% 86.75% 86.44%
3. Pyriproxyfen 25% + Tebuconazole 1.5% Direct WDG 78.43% 78.22% 75.36% 81.33% 81.38% 81.05%
Pyriproxyfen 25% + Tebuconazole 1.5% Dry Capsule 86.24% 86.26% 84.87% 86.04% 86.11% 85.99%
4. Propiconazole 40% + Picoxystrobin 15% Direct WDG 79.98% 79.45% 77.75% 78.82% 78.95% 78.88%
Propiconazole 40% + Picoxystrobin 15% Dry Capsule 84.81% 84.84% 83.59% 84.72% 84.84% 84.67%
5. Azoxystrobin 25% + Hexaconazole 5% Direct WDG 82.45% 82.13% 80.01% 78.16% 78.27% 78.09%
Azoxystrobin 25% + Hexaconazole 5% Dry Capsule 86.47% 86.44% 85.10% 85.06% 85.16% 85.07%
• Dry Capsule – Formulation prepared by process of present invention that involves preparation of encapsulated suspension and conversion of the same into water dispersible granules by spray drying.
• Direct WDG – Formulation that involves preparation of slurry without encapsulating the active ingredient and converting it into WDG by spray drying.
• ATS – Accelerated Temperature Stability

It is observed from above Table 1 that even after 14 days of ATS at low and high temperatures, the formulation of dry capsule prepared by present process (WDG through CS) provides enhanced suspensibility and dispersibility as compared to formulations of WDG that are prepared directly (without encapsulation). Thus the dry capsule formulation prepared by present process improves formulation quality with mean particle size and uniform particle distribution and provides flowable formulation with enhanced stability, dispersibility and suspensibility.

Example 12: Suspensibility and Dispersibility Study Comparison upto 30 months - Dry Capsule (DC) Formulation VS. Direct WDG
The suspensibility and dispersibility of Dry Capsule (present formulations) and Direct WDG are tested for a period of 30 months and observations are provided in below Table 2:
Table 2:

Test Observation
3 Months 6 Months 9 Months 12 Months 18 Months 24 Months 30 Months
WDG DC WDG DC WDG DC WDG DC WDG DC WDG DC WDG DC
Difenoconazole 15% + Trifloxystrobin 35%
Suspensibility (% by w/w) 80.33 85.89 80.11 85.8 80.23 84.96 79.86 85.34 79.88 85.22 80.4 85.38 80.07 85.13
Dispersibility (% by w/w) 81.37 87.72 80.98 87.56 81.02 87.55 81.22 86.73 80.54 87.19 81.91 87.43 81.34 87.2
Pyraclostrobin 10% + Propargite 10%
Suspensibility (% by w/w) 82.14 86.77 81.99 87.02 82.04 86.86 82.15 86.91 82.17 87.11 82.09 87.23 82.26 87.31
Dispersibility (% by w/w) 80.94 86.71 81.00 86.72 80.83 87.08 81.16 87.03 81.31 87.27 81.42 87.30 80.99 87.09
Pyriproxyfen 25% + Tebuconazole 1.5%
Suspensibility (% by w/w) 78.43 86.24 78.12 87.61 78.33 86.95 78.51 87.41 78.27 87.34 78.39 87.19 78.41 87.37
Dispersibility (% by w/w) 81.33 86.04 80.79 86.57 81.24 86.78 81.04 86.84 81.15 86.91 80.88 87.01 81.21 86.95
Propiconazole 40% + Picoxystrobin 15%
Suspensibility (% by w/w) 79.98 84.81 80.21 84.88 79.94 85.26 80.05 85.3 80.11 85.11 80.02 84.99 81.21 85.43
Dispersibility (% by w/w) 78.82 84.72 78.74 85.07 78.96 85.11 78.91 84.83 79.15 84.27 79.05 84.56 78.99 84.64
Azoxystrobin 25% + Hexaconazole 5%
Suspensibility (% by w/w) 82.45 86.47 82.39 85.83 82.49 85.79 82.18 86.22 82.07 86.36 82.44 86.24 82.31 85.99
Dispersibility (% by w/w) 78.16 85.06 78.52 85.01 78.25 86.1 78.19 85.49 78.33 85.37 78.41 85.68 78.33 85.77

It is observed from above Table 2, that the DC formulation (WDG through CS) of the present invention exhibits enhanced suspensiblity and dispersibility throughout its storage period as compare to WDG (prepared directly without encapsulation), thus demonstrate improvement in terms of formulation quality.

Example 13: Synergy data: Dry Capsule (DC) Formulations VS. Solo / Marketed Formulations
The suspensibility of present Dry Capsule formulations and solo formulations / marketed products are tested for 14 days under low as well as high temperature conditions and observations are provided in below Table 3.
Table 3:
Sr.
No. Product Description Suspensibility Observation for 14 days
Initial ATS at -20°C ATS at 54°C
1. Difenoconazole 15% +
Trifloxystrobin 35% DC Present Dry Capsule 85.89% 85.65% 82.72%
Trifloxystrobin 50% WG Marketed Product 79.15% 79.20% 74.54%
Difenoconazole 10% WG Marketed Product 75.82% 76.09% 75.47%
2. Pyraclostrobin 10% + Propargite 10% DC Present Dry Capsule 86.77% 86.69% 84.32%
Propargite 30% WG Marketed Product 72.94% 72.88% 71.22%
Pyraclostrobin 20% WG Marketed Product 78.13% 78.09% 74.23%
3. Pyriproxyfen 25% + Tebuconazole 1.5% DC Present Dry Capsule 86.24% 86.26% 84.87%
Pyriproxyfen8% WG Solo formulation 76.48% 76.54% 75.21%
Tebuconazole 25% WG Marketed Product 76.45% 76.32% 71.23%
4. Bifenthrin 5% + Chlorpyrifos 20% + Triacontanol 0.1% DC Present Dry Capsule 85.13% 85.00% 78.45%
Bifenthrin 10% WG Solo formulation 78.24% 79.4% 77.58%
Chlorpyriphos5% WG Solo formulation 77.26% 77.24% 75.63%
Triacontanol 1.5% WG Solo formulation 79.44% 79.39% 78.58%
5. Propiconazole 40% + Picoxystrobin 15% DC Present Dry Capsule 84.81% 84.84% 83.59%
Propiconazole 50% WG Marketed Product 71.94% 72.11% 70.55%
Picoxystrobin50% WG Solo formulation 81.67% 81.74% 80.55%
6. Azoxystrobin 25% + Hexaconazole 5% DC Present Dry Capsule 86.47% 86.44% 85.10%
Azoxystrobin 50% WG Marketed Product 80.37% 80.27% 79.29%
Hexaconazole 75% WG Marketed Product 78.27% 78.19% 73.69%
7. Chlorpyrifos 50% + Cypermethrin 5% DC Present Dry Capsule 81.82% 81.34% 75.78%
Chlorpyrifos 75% WG Marketed Product 77.83% 77.90% 75.61%
Cypermethrin25% WG Solo formulation 76.44% 76.31% 74.11%
Solo formulation – Prepared in-house for comparison

It is observed from above Table 3 that, the suspensibility of DC formulations of the present invention are higher as compared to solo formulations / marketed products. Hence it is clear that the water dispersible granular composition of the present invention exhibits synergy over solo compositions.

,CLAIMS:We Claim,

1. A process for preparation of water dispersible granule composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C; wherein said process comprises preparation of encapsulated suspension initially, followed by conversion of encapsulated suspension into water dispersible granules by spray drying.

2. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 1; wherein preparation of encapsulated suspension and conversion of encapsulated suspension into water dispersible granules comprising the steps of;
(a) preparing an organic phase by dissolving at least two or more agrochemical active ingredients having low melting point of less than 120°C in solvent and maintaining the temperature of 60°C followed by adding encapsulating polymer-1 and mixing well to form clear solution;
(b) preparing an aqueous phase by mixing emulsifying agent and suspending agent along with DM water followed by heating and subjecting to high speed homogenizer;
(c) adding organic phase of step (a) into aqueous phase of step (b) to obtain oil-in-water emulsion and achieving the particle size to be less than 25 micron;
(d) adding encapsulating polymer-2 to step (c) and mixing and curing the temperature of 60°C followed by cooling the slurry and adding stabilizer to obtain stable encapsulated suspension;
(e) adding agrochemically acceptable excipients/adjuvants selected from dispersing agents, wetting agents, stabilizers, thickeners, fillers and pH adjuster to step (d) to make up the volume of suspension to 100% (total solid basis); and
(f) spraying the suspension of step (e) under temperature between 40°C-60°C to get granules that are further sieved to obtain desired water dispersible granules.

3. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 1 and 2; wherein at least two or more agrochemical active ingredient having low melting point of less than 120°C are selected from insecticides, pesticides, herbicides, fungicides, acaricides, nematicides, miticide, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator, flowering inducer and mixtures thereof.

4. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 3; wherein the insecticides with melting point less than 120°C are selected from Acynonapyr, Alanycarb, Benfuracarb, Bifenthrin, Cadusafos, Carbosulfan, Chlorpyrifos, Cyanophos, Cyfluthrin, ?-Cyhalothrin, Cypermethrin, Deltamethrin, Dimethoate, Esfenvalerate, Ethion, Etofenprox, Fenitrothion, Fenobucarb, Fenpropathrin, Fenvalerate, Flupyradifurone, Flupyrimin, Fluvalinate, Indoxacarb, Isoxathion, Malathion, Methidathion, Methomyl, Nitenpyram, Oxazosulfyl, Permethrin, Profenofos, Propargite, Prothiofos, Pyrethrins, Pyridalyl, Pyriproxyfen, Quinalphos, Silafluofen, Tebufenpyrad and Tefluthrin.

5. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 3; wherein the herbicides with melting point less than 120°C are selected from Benfluralin, Benfuresate, Clethodim, Clodinafop-propargyl, Napropamide, Pendimethalin, Prosulfocarb, Pyraflufen-ethyl, Quizalofop-ethyl, S-metolachlor, Sulfentrazone, Triclopyr and Trifluralin.

6. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 3; wherein the fungicides with melting point less than 120°C are selected from Azoxystrobin,, Cyflufenamid, Cyprodinil, Difenoconazole, Diflumetorim, Fenoxanil, Hexaconazole, Imibenconazole, Inpyrfluxam, Ipconazole, Iprobenfos, Isoprothiolane, Myclobutanil, Picoxystrobin, Propiconazole, Pyraclostrobin, Tebuconazole, Tetraconazole, Trifloxystrobin and Triflumizole.

7. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 3; wherein the plant growth regulators (PGR) with melting point less than 120°C are selected from Chlorpropham and Triacontanol.

8. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the encapsulating polymer-1 are selected from isocyanates such as polymethylene polyphenylene isocyanate (PMPPI), hexamethylene diisocyanate (HMDI), Napthalene diisocyanate, Methylene bis-cyclohexylisocyanate, isophorone diisocyanate (IPDI) or 4,4' methylenebis (cyclohexyl isocyanate), polyphenylisocyanate, Polymethylene polyphenylisocyanate, Toulene diisocyanate, and/or trimers of HMDI or IPDI, isomers of tolylene diisocyanate, isomers and derivatives of phenylene diisocyanate, isomers and derivatives of biphenylene diisocyanates, methylene diphenyl diisocyanate (MDI), polymeric polyisocyanates, biurets and blocked polyisocyanates; present in an amount of 0.1 to 10%.

9. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the encapsulating polymer-2 are selected from polyamines such as diethylenetriamine, ethylenediamine, triethylenetetraamine, 1,4-diaminobutane, 1,5-diaminopentane, 1,4-Benzenediamine, Benzylamine, Ethyl amine, Butylamine, Propylamine, Isopropyamine, 1-methylbutylamine, Tert-butylamine, Cyclo-hexylamine, Phenylamine, 2-Pentanamine, 2-methylaniline and Hexamethylenediamine; present in an amount of 0.1 to 10%.

10. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the emulsifying agent are selected from acrylic polymer/copolymer, polyvinyl alcohol, Polyvinyl pyrolidone, EO-PO block copolymer, ethoxylated and ethopropoxylated alcohols and nonyl phenols, ethoxylated tristeryl phenol, ethoxylated tristeryl phenol phosphates, Tristyreneated phenol ethoxylate ethoxylated, 15 Polycarboxylate sodium, nonylphenol ethoxylate and ethopropoxylated castor oil and calcium alkyl benzene sulfonates; present in an amount ranging from 0.1 to 15%.

11. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the suspending agent are selected from sodium salt of Napthalene formaldehyde condensate, sodium ligno sulphonate and potassium polycarboxylate; present in an amount ranging from 2 to 15%.

12. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the solvent are selected from naptha, aromatic chlorinated hydrocarbons, chlorinated maleic hydrocarbons, ketones, long chain esters and mixtures thereof, (commercially available as Solvesso 100, Solvesso 150, Solvesso 200, Solvesso 150ND, Solvesso 200ND, Aromatic 200, Hydrosol A 200, Hydrosol A 230/270, Caromax 20, Caromax 28, Aromat K 150, Aromat K 200, Shellsol A 150, Shellsol A 100, Fin FAS-TX 150, Fin FAST-TX 200, Xylene, Cyclohexane, Cyclopentane, Pentane, Hexane, Heptane, octane, nonane, decane, isooctane, benzene, 2- Methylpentane, 3-Methylpentane, 2-Methylhexane, 3-Methylhexane, 2-methylbutane, 2,3-Dimethylpentane, Methycyclopentane, Methylcyclohexane, 2,4 Dimethylpentane, aromatics such as benzene, toluene, cyclohexane, 1-Pentene, 2-Pentene, 1-Hexene, 1-Heptene, Cyclohexene, Ethylvinylether, Propylether, Isopropylether, petroleum distillates, petroleum ether, and the like, Butylvinylether, Butylethylether, 1,2 - Epoxybutane, Furan, Tetrahydropyran, 1-Butanal, 2-methylpropanal, 2-Pentanone, 3-Pentanone, Fluorbenzene, Hexafluorobenzene, Ethylformate, Propylformate, Isopropylformate, Ethylacetate and Methylacrylate; present in an amount of 5 to 30%.

13. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the dispersing agents are selected from naphthalene sulfonic acid, sodium salt condensed with formaldehyde, polyalcoxylated alkylphenol, naphthalene sulfonic acid formaldehyde condensate, methyl naphtaline-formaldehyde-condensate sodium salt, naphthalene condensates, sodium lignosulfonates, polyacrylates/Acrylic copolymer and phosphate esters, polyvinyl alcohol, calcium lignosulfonate, lignin sulfonate sodium salt, Sodium lingo sulphonate, and the like; and are present in an amount of 2 to 15%.

14. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the wetting agents are selected from sodium N-methyl-N-oleoyl taurate, alkylated naphthalene sulfonate, sodium salt, mixture of isomers of dibutyl naphthalene sulphonic acid sodium salt, sodium isopropyl naphthalene sulphonate, ethylene oxide/propylene oxide block copolymer, sodium lauryl sulfate, alpha olifin sulphate, sodium salt of napthalene sulphate, dioctyl sulfate, alkyl naphthalene sulfonates, phosphate esters, sulphosuccinates and non-ionic such as tridexyl 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 alkyaryl phosphate esters, alkyl polysaccharide, di or mono alkyl sulfosuccinate derivatives, alpha olefin sulfonates, alkyl naphthalene sulfonates, dialkyl sulphosuccinates, butyl, dibutyl, isopropyl and diisopropyl 25 naphthalene sulfonate salts, C12 alkyl benzene sulfonate or C10-C16 alkyl benzene sulfonate; present in an amount of 1 to 5%.

15. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the stabilizers are selected from polysaccharide, 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; present in an amount of 0.1 to 2%.

16. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the thickening agent/thickener are selected from colloidal silica, precipitated silica, bentonite, aluminum silicate, calcium sulfonate, clay, talc; present in an amount of 1 to 10%.

17. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the fillers are selected from china clay, lactose, dextrin; present in an amount of 5 to 50%.

18. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 2; wherein the pH adjuster is selected from citric acid, acetic acid, sodium acetate; present in an amount of 0.5 to 2%.

19. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 1 and 2; wherein the particle size (D90) of microcapsule is maintained between 0.1 micron to 25 micron.

20. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 1 and 2; wherein said granules are encapsulated within polymeric shell wall which provides controlled release of actives.

21. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 20; wherein said polymeric shell wall comprises mixture of isocynates with amines.

22. The process for preparation of water dispersible granule composition comprising microcapsule as claimed in claim 1 and 2; wherein the said composition exhibits enhanced stability, suspensibility and dispersibility under low as -20°C and under high as +54°C temperature conditions throughout its storage period.

23. A water dispersible granule composition comprising microcapsule containing at least two or more agrochemical active ingredients having low melting point of less than 120°C selected from combination of pesticides, insecticides, herbicides, fungicides, acaricides, nematicides, miticides, plant growth regulators (PGR), plant growth promoter, plant growth retardant, root growth stimulator or flowering inducer; along with agrochemically acceptable excipients/adjuvants.

24. The water dispersible granule composition comprises microcapsule as claimed in claim 23; wherein said agrochemically acceptable excipients/adjuvants includes suspending agent, emulsifying agent, dispersing agent, stabilizer, thickeners, wetting agent, coating agent, solvent, fillers and pH adjusting agent.

25. The water dispersible granule composition comprise microcapsule as claimed in claim 23 and 24; wherein said composition comprises at least two or more agrochemical active ingredients in the range of 0.1% to 80%; encapsulating polymer in the range of 0.1 to 10%; emulsifying agent in the range of 0.1 to 15%; suspending agent in the range of 2 to 15%; solvent in the range of 5 to 30%; dispersing agent in the range of 2 to 15%; wetting agent in the range of 1 to 5%; 15 stabilizer in the range of 0.1 to 5%; thickener in the range of 1 to 10%; fillers in the range of 5 to 50% and pH adjusting agent in the range of 0.5 to 2% by weight of the total composition.

26. The water dispersible granule composition comprise microcapsule as claimed in claim 23 to 25; wherein said composition exhibits enhanced stability, suspensibility and dispersibility under low as well as high temperature conditions ranging from -20°C to +54°C throughout its storage period.

27. The water dispersible granule composition comprises microcapsule as claimed in claim 23 to 25; wherein said composition comprises combination of at least two or more agrochemical active ingredients having melting point below 100°C.

28. The water dispersible granule composition comprises microcapsule as claimed in claim 23 to 25; wherein said composition comprises combination of at least two or more agrochemical active ingredients having melting point above 100°C.

29. The water dispersible granule composition comprise microcapsule as claimed in claim 23 to 25; wherein said composition comprises combination of at least two or more agrochemical active ingredients having melting point below 100°C and above 100°C.

30. A method of controlling nfestation/diseases/weed, improving crop health and increasing crop yield by applying water dispersible granule composition comprising microcapsule as claimed in claim 23 to 29 on varieties of crops include pulses, oil seeds, cereals, legumes, all field crops, horticulture pastures, forestry and non-crop lands.