DESC:
FORM 2
THE PATENTS ACT, 1970
(39 OF 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10; rule 13)

1. Title of the invention – DEFOLIATING COMPOSITION COMPRISING THIDIAZURON

2. Applicant(s)

(a) NAME : GSP CROP SCIENCE PVT. LTD

(b) NATIONALITY: An Indian Company

(c) ADDRESS: 404, Lalita Complex, 352/3 Rasala Road, Navrangpura,
Ahmedabad-380009, Gujarat, India

3. PREAMBLE TO THE DESCRIPTION

The following specification particularly describes the invention and the manner in which it is to be performed:

FIELD OF THE INVENTION:
The present invention relates to a defoliating composition. In particular, the present invention relates to a defoliating composition comprising A) Thidiazuron B) at least one herbicide agent C) at least one Herbicide of sulphonyl urea class and one or more inactive excipient and its use. However, it will be appreciated that the invention is not limited to this particular field of use.

BACKGROUND OF THE INVENTION

Defoliation is the shedding of cotton leaves that naturally occurs when leaves become physiologically mature. Leaf shedding (abscission) results from activity of special cells at the base of the leaf petiole where it joins the stem. This area is called the "abscission layer." Defoliation may be induced by a light frost, insect damage, disease, drought or mineral deficiency. It can also be artificially achieved by the use of certain chemicals called "defoliants" or harvest aids. In situations where canopies are dense and there are significant numbers of green bolls that need to be opened, two applications are often required. Planning a two-pass approach, especially in lush, irrigated cotton as opposed to getting less than desirable results such as stuck leaves or poor defoliation from a single application attempt is recommended. The goal of the first application is to remove as much foliage as possible exposing the unopened bolls without causing desiccation. The second harvest aid application will require additional defoliant to finish removing lower canopy leaves but, more importantly, an adequate boll opener to stimulate boll opening.

Desiccation is drying of plant tissues due to disruption of cell membranes and rapid loss of moisture which often results in "stuck leaves.” Product selection and
application rates are adjusted to match environmental conditions as they change during the harvest season in order to reduce occurrence of leaf desiccation.

Defoliation also promotes mechanical harvesting as it prevents boll rot, eliminates the main source of stain and trash, increases air movement through the crop canopy, improves lint grades, removes leaves, faster and more efficient picker operation, reduces moisture , manages maturity by allowing earlier harvest which facilitates quicker drying, thus allowing picker to begin earlier in the day, storage in modules

Because of the large number of possible influencing factors, there is virtually no individual active compound which, combined the desired properties for different requirements, in particular with regard to the harmful plants and the climatic zones in itself. Then there is the constant need to achieve the effect with lower defoliating agent application rates. A lower application rate reduces not only the required for the application amount of a chemical substance, but usually reduces the amount of composition or formulation auxiliaries required. Both reduce the economic expense and improve the ecological compatibility of the defoliating treatment.

Thidiazuron was first disclosed in US US3883547 and chemically known as 1-Phenyl-3-(1,2,3-thiadiazol-5-yl)urea and having chemical structure as below;

Thidiazuron is Urea plant growth regulator having cytokinin activity. Thidiazuron has gained a considerable attention during past decades due to its efficient role in plant cell and tissue culture. Wide array of physiological responses were observed in response to Thidiazuron application in different plant species. Thidiazuron has shown both auxin and cytokinin like effects, although, chemically, it is totally different from commonly used auxins and cytokinins. A number of biological (physiological and biochemical) events in cells are induced or enhanced by Thidiazuron, but the mode of action of Thidiazuron is yet unknown. However, varieties of underlying mechanisms were revealed by reports showing how morphogenic events were induced by application of Thidiazuron. Other reports showed that Thidiazuron may modify endogenous plant growth regulators, either directly or indirectly and produce reactions in cell/tissue, necessary for its division/regeneration. Other possibilities include modification in cell membrane, energy levels, nutrient absorption, transport and assimilation, etc.

US7981838 describes mixtures of thidiazuron and diuron in a mixture with compounds from the group of the N-phenylsulfonyl(het)arylamides have synergistic effects.

Mixtures of thidiazuron and diuron are commercially available, for example, under the name Dropp Ultra® (Bayer Crop Science). Such mixtures are described, for example, in U.S. Pat. No. 4,613,354 A.

US8349767 discloses an aqueous composition including a synergist combination of thidiazuron and diuron. The invention is also directed to a method of treating plants with an aqueous composition including a synergistic mixture of thidiazuron and diuron as a defoliant and without the use of organic solvents.

Indian patent application IN 4364/CHENP/2008 describes a mixture, comprising (A) thidiazuron or thidiazuron and diuron, and (B) one or more compounds from the group of the benzofurans, preferably benfuresate and/or ethofumesate, is suitable for use as a defoliant and/or a composition for reducing regrowth, in particular in crops of cotton.

Still there is a need for a herbicidal composition which overcomes some of the existing problems and can be prepared easily without much complex manufacturing process.

Inventors of the present invention have surprisingly found that defoliating composition comprising defoliating composition comprising A) Thidiazuron B) at least one herbicide agent C) at least one Herbicide of sulphonyl urea class and one or more inactive excipient described herein in can provide solution to the above mentioned problems.

SUMMARY OF THE INVENTION

Accordingly, in a first aspect of the present invention provides a defoliating composition comprising A) Thidiazuron B) at least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil C) at least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl and one or more inactive excipient.

Accordingly, in a second aspect, the present invention provides a method of preparing defoliating composition comprising A) Thidiazuron B) at least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil C) at least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl and one or more inactive excipient.

Accordingly, in a third aspect, the present invention composition according to the invention are suitable in particular for use as defoliants in crops of cotton, due, for example, to rapid action and/or increased activity or lower application rates provides a method of defoliation which promotes mechanical harvesting and reduce its cost.

DETAILED DESCRIPTION OF THE INVENTION

The present invention is directed to a defoliating composition and a method for treating plants using the said composition. The present invention is particularly directed to a defoliating composition comprising A) Thidiazuron B) at least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil C) at least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl and one or more inactive excipient.

According to one aspect of the present invention the synergistic effect is obtained using defoliating composition of the present invention comprising A) Thidiazuron B) at least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil C) at least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl and one or more inactive excipient.

"Effective amounts” as mentioned herein means that amount which, when applied treatment of crops, is sufficient to effect such treatment.

The term “formulation” and “composition” as used herein conveys the same meaning and can be used interchangeably.

The biochemical mechanisms underlying Thidiazuron-induced regeneration in plant cells have not been clearly elucidated. Exposure of leaf explants of Echinacea purpurea to a medium containing Thidiazuron results in undifferentiated cell proliferation and differentiated growth as mixed shoot organogenesis and somatic embryogenesis. The current studies were undertaken to determine the potential roles of auxin, indoleamines, and ion signaling in the dedifferentiation and redifferentiation of plant cells. E. purpurea leaf explants were found to contain auxin and the related indoleamine neurotransmitters, melatonin, and serotonin. The levels of these endogenous indoleamines were increased by exposure to Thidiazuron associated with the induction of regeneration. The auxin-transport inhibitor 2,3,5-triiodobenzoic acid and auxin action inhibitor, p-chlorophenoxyisobutyric acid decreased the Thidiazuron -induced regeneration but increased concentrations of endogenous serotonin and melatonin. As well, inhibitors of calcium and sodium transport significantly reduced Thidiazuron-induced morphogenesis while increasing endogenous indoleamine content. These data indicate that Thidiazuron -induced regeneration is the manifestation of a metabolic cascade that includes an initial signaling event, accumulation, and transport of endogenous plant signals such as auxin and melatonin, a system of secondary messengers, and a concurrent stress response.

The defoliating composition of the present invention can be prepared in various formulations, for example in the form of a dustable powder (DP), a gel, a wettable powder (WP), a granule (GR) (such as an emulsifiable granule (EG) or more particularly a water-dispersible granule (WG)), a water-dispersible tablet (WT), an emulsifiable concentrate (EC), a micro- emulsifiable concentrate, an oil-in-water emulsion (EW), an oil flowable (e.g. a spreading oil (SO)), an aqueous dispersion (e.g. aqueous suspension concentrate (SC)), an oily dispersion (OD), a suspo-emulsion (SE), a capsule suspension (CS), a soluble liquid, a water-soluble concentrate (with water or a water-miscible organic solvent as carrier), an impregnated polymer film, or jumbo formulation.

As per preferred embodiment, the composition of the present invention is in the form of Water dispersible Granules (WG), Suspension concentrate (SC) and Wettable powders (WP).

Defoliating composition of the present invention have several advantages over the use of a single defoliating agent including (a) an improvement in crop safety by using minimum doses of selected defoliant applied in combination rather than a single high dose of one defoliant and (b) prevents boll rot, (c) high synergistic action in defoliation due to combination (d) Uniform lead drop and boll opening (e) improves lint grades and lint harvest, (f) reduces moisture , manages maturity by allowing earlier harvest which facilitates quicker drying thus increasing efficacy against adverse weather conditions.

For application of defoliating composition of the present invention, hollow cone nozzles are superior to air induction nozzles as they improve foliar coverage using ground application equipment. Two equally spaced hollow cone nozzles per row will give adequate coverage. Spray pressure, ground speed and nozzle size should be matched appropriately in order to apply the desired spray volume in accordance with label instructions. The amount of water used as a carrier in each defoliation application should not be lower than 50 lit per acre for aerial applications and 100 lit per acre by ground.

Further during the defoliating treatment few other things needs to be keep in check are a) Do not defoliate all cotton at one time b) Defoliants should be applied 10 to 14 days prior to anticipated harvest date c) Leaf drop should start in about four days and be complete in about 10 days d) Rain three to four hours after application of a defoliant does not lessen the effectiveness of most chemicals with the exception of thidiazuron, which requires a 24 hour rain-free period.

A) Thidiazuron B) at least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil C) at least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl are present in composition are present in ratio as described below;

Component A B C

Active Thidiazuron Diuron Metsulfuron Methyl
Thidiazuron Diuron Chlorimuron Ethyl
Thidiazuron Paraquat Dichloride Metsulfuron methyl
Thidiazuron Paraquat Dichloride Chlorimuron methyl
Thidiazuron Ethephon Metsulfuron Methyl
Thidiazuron Ethephon Chlorimuron Ethyl
Thidiazuron Carfentrazone Metsulfuron methyl
Thidiazuron Carfentrazone Chlorimuron methyl
Thidiazuron Sulfentrazone Metsulfuron Methyl
Thidiazuron Sulfentrazone Chlorimuron Ethyl
Thidiazuron Pyraflufen Metsulfuron methyl
Thidiazuron Pyraflufen Chlorimuron methyl
Thidiazuron Fluthiacet Metsulfuron Methyl
Thidiazuron Fluthiacet Chlorimuron Ethyl
Thidiazuron Flumiclorac Metsulfuron methyl
Thidiazuron Flumiclorac Chlorimuron methyl
Thidiazuron Cyclanilide Metsulfuron Methyl
Thidiazuron Cyclanilide Chlorimuron Ethyl
Thidiazuron Saflufenacil Metsulfuron methyl
Thidiazuron Saflufenacil Chlorimuron methyl
Concentration 1 to 30% 1 to 60% 0.05 to 10%

In another embodiment of the present invention the above said defoliating composition is effective for defoliation for crops selected from Cotton (GMO and Non GMO), Jute, Soybean (GMO and Non GMO), Green gram, Black gram and Red gram.

As per one embodiment the defoliating composition of the present invention is very effective in cotton.

As per one embodiment, the preferred composition and combinations are selected from below list;
Active Ingredient 1 Active Ingredient 2 Active Ingredient 3 A.I. (%) in formulation Formulation Strength (%) Preferred formulation type Formulation per Hectare (ml)
A.I. 1 A.I. 2 A.I. 3
Thidiazuron Diuron Metsulfuron Methyl 12 6 0.4 18.4 SC 250
Thidiazuron Diuron Metsulfuron Methyl 24 12 0.8 36.8 WG 125
Thidiazuron Diuron Chlorimuron Ethyl 12 6 0.4 18.4 SC 250
Thidiazuron Ethephon Metsulfuron Methyl 2.5 30 0.05 32.55 SC 2000
Thidiazuron Ethephon Metsulfuron Methyl 5 60 0.1 65.1 WG 1000
Thidiazuron Ethephon Chlorimuron Ethyl 2.5 30 0.05 32.55 SC 2000
Thidiazuron Cyclanilide Metsulfuron Methyl 10 15 0.2 25.2 SC 500
Thidiazuron Cyclanilide Chlorimuron Ethyl 10 15 0.2 25.2 SC 500
Thidiazuron Cyclanilide Metsulfuron Methyl 20 30 0.4 50.4 WG 250
Thidiazuron Carfentrazone Ethyl Chlorimuron Ethyl 20 8 0.4 28.4 WG 250
Thidiazuron Sulfentrazone Metsulfuron Methyl 20 8 0.4 28.4 WG 250

The defoliating composition of the present invention comprises of A) Thidiazuron B) at least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil C) at least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl and one or more inactive excipient. Tthe inactive excipients are to be selected from including but not limited to dispersant, anti-freezing agent, anti-foam agent, wetting agent, suspension aid, anti-microbial agent, thickener, quick coating agent or sticking agents (also referred to as “stickers” or “binders”) and buffering agent.

A dispersant is a substance which adsorbs onto the surface of particles and helps to preserve the state of dispersion of the particles and prevents them from re-aggregating. Dispersants are added to agrochemical formulations to facilitate dispersion and suspension during manufacture, and to ensure the particles re-disperse into water in a spray tank. They are widely used in wettable powders, suspension concentrates and water-dispersible granules. Surfactants that are used as dispersants have the ability to adsorb strongly onto a particle surface and provide a charged or steric barrier to re-aggregation of particles. The most commonly used surfactants are anionic, non-ionic, or mixtures of the two types. For wettable powder formulations, the most common dispersants are sodium lignosulphonates. For suspension concentrates, very good adsorption and stabilization are obtained using polyelectrolytes, such as sodium naphthalene sulphonate formaldehyde condensates. Tristyrylphenolethoxylate phosphate esters are also used. Nonionics such as alkylarylethylene oxide condensates and EO-PO block copolymers are sometimes combined with anionics as dispersants for suspension concentrates. In recent years, new types of very high molecular weight polymeric surfactants have been developed as dispersants. These have very long hydrophobic ‘backbones’ and a large number of ethylene oxide chains forming the ‘teeth’ of a ‘comb’ surfactant. These high molecular weight polymers can give very good long-term stability to suspension concentrates because the hydrophobic backbones have many anchoring points onto the particle surfaces. Examples of dispersants used herein include but not limited to sodium lignosulphonates; sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenolethoxylate phosphate esters; aliphatic alcohol ethoxylates; alky ethoxylates; EO-PO block copolymers; and graft copolymers or mixtures thereof.

Anti-freezing agent as used herein can be selected from the group consisting of polyethylene glycols, methoxypolyethylene glycols, polypropylene glycols, polybutylene glycols, glycerin and ethylene glycol.

Water-based formulations often cause foam during mixing operations in production. In order to reduce the tendency to foam, anti-foam agents are often added either during the production stage or before filling into bottles. Generally, there are two types of anti-foam agents, namely silicones and non-silicones. Silicones are usually aqueous emulsions of dimethyl polysiloxane while the non-silicone anti-foam agents are water-insoluble oils, such as octanol and nonanol, or silica. In both cases, the function of the anti-foam agent is to displace the surfactant from the air-water interface.

A wetting agent is a substance that when added to a liquid increases the spreading or penetration power of the liquid by reducing the interfacial tension between the liquid and the surface on which it is spreading. Wetting agents are used for two main functions in agrochemical formulations: during processing and manufacture to increase the rate of wetting of powders in water to make concentrates for soluble liquids or suspension concentrates; and during mixing of a product with water in a spray tank or other vessel to reduce the wetting time of wettable powders and to improve the penetration of water into water-dispersible granules. Examples of wetting agents used in wettable powder, suspension concentrate, and water-dispersible granule formulations include but not limited to sodium lauryl sulphate; sodium dioctylsulphosuccinate; alkyl phenol ethoxylates; and aliphatic alcohol ethoxylates and the salts thereof which are standard in agricultureor mixtures thereof.

Suspension aid in the present description denotes a natural or synthetic, organic or inorganic material with which the active substance is combined in order to facilitate its application to the plant, to the seeds or to the soil. This carrier is hence generally inert, and it must be agriculturally acceptable, in particular to the plant being treated. The carrier may be solid (clays, natural or synthetic silicates, silica, resins, waxes, solid fertilizers, and the like or mixtures thereof) or liquid (water, alcohols, ketones, petroleum fractions, aromatic or paraffinic hydrocarbons, chlorinated hydrocarbons, liquefied gases, and the like or mixtures thereof).

Biocides / Microorganisms cause spoilage of formulated products. Therefore anti-microbial agents are used to eliminate or reduce their effect. Examples of such agents include, but are not limited to: propionic acid and its sodium salt; sorbic acid and its sodium or potassium salts; benzoic acid and its sodium salt; p-hydroxy benzoic acid sodium salt; methyl p-hydroxy benzoate; and biocide such as sodium benzoate, 1,2-benzisothiazoline-3-one, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, potassium sorbate, parahydroxy benzoates or mixtures thereof.

Thickeners or gelling agents are used mainly in the formulation of suspension concentrates, emulsions and suspo-emulsions to modify the rheology or flow properties of the liquid and to prevent separation and settling of the dispersed particles or droplets. Thickening, gelling, and anti-settling agents generally fall into two categories, namely water-insoluble particulates and water-soluble polymers. It is possible to produce suspension concentrate formulations using clays and silicas. Examples of these types of materials, include, but are limited to, montmorillonite, e.g. bentonite; magnesium aluminum silicate; and attapulgite. Water-soluble polysaccharides have been used as thickening-gelling agents for many years. The types of polysaccharides most commonly used are natural extracts of seeds and seaweeds are synthetic derivatives of cellulose or mixtures thereof. Examples of these types of materials include, but are not limited to, guar gum; locust bean gum; carrageenam; xanthan gum; alginates; methyl cellulose; sodium carboxymethyl cellulose (SCMC); hydroxyethyl cellulose (HEC) or mixtures thereof. Other types of anti-settling agents are based on modified starches, polyacrylates, polyvinyl alcohol and polyethylene oxide or mixtures.

The quick coating agent can be a conventionally available sticker, for example polyesters, polyamides, poly- carbonates, polyurea and polyurethanes, acrylate polymers and copolymers, styrene copolymers, butadiene copolymers, polysaccharides such as starch and cellulose derivatives, vinylalcohol, vinylacetate and vinylpyrrolidone polymers and copolymers, polyethers, epoxy, phenolic and melamine resins, polyolefins and define copolymersand mixtures thereof. Examples of preferred polymers are acrylate polymers such as poly(methacrylate), poly(ethyl methacrylate), poly(methylmethacrylate), acrylate copoylmers and styrene-acrylic copolymers as defined herein below, poly(styrene-co maleic anhydride), cellulosic polymers such as ethyl cellulose, cellulose acetate, cellulose acetatebutyrate, acetylated mono, di, and triglycerides, poly(vinylpyrrolidone), vinyl acetate polymers and copolymers, poly(alkylene glycol), styrene butadiene copolymers, poly(orthoesters), alkyd resins, and mixtures of two or more of these. Polymers that are biodegradable are also useful in the present invention. As used herein, a polymer is biodegradable if is not water soluble, but is degraded over a period of several weeks when placed in an application environment. Examples of biodegradable polymers that are useful in the present invention include biodegradable polyesters, starch, polylactic acid starch blends, polylactic acid, poly(lactic acid-glycolic acid) copolymers, polydioxanone, cellulose esters, ethyl cellulose, cellulose acetate butyrate, starch esters, starch esteraliphatic polyester blends, modified corn starch, polycaprolactone, poly(namylmethacrylate), wood rosin, polyanhydrides, polyvinylalcohol, polyhydroxybutyratevalerate, biodegradable aliphatic polyesters, and polyhydroxybutyrate or mixtures thereof.

Buffering agent as used herein is selected from group consisting of calcium hydroxyapatite, Potassium Dihydrogen Phosphate, Sodium Hydroxide, carbonated apatite, calcium carbonate, sodium bicarbonate, tricalcium phosphate, calcium phosphates, carbonated calcium phosphates, amine monomers, lactate dehydrogenase and magnesium hydroxide.

The solvent for the formulation of the present invention may include water, water-soluble alcohols and dihydroxy alcohol ethers. The water-soluble alcohol which can be used in the present invention may be lower alcohols or water-soluble macromolecular alcohols. The term "lower alcohol", as used herein, represents an alcohol having 1-4 carbon atoms, such as methanol, ethanol, n-propanol, isopropanol, n-butanol, tert-butanol, etc. Macromolecular alcohol is not limited, as long as it may be dissolved in water in a suitable amount range, e.g., polyethylene glycol, sorbitol, glucitol, etc. The examples of suitable dihydroxy alcohol ethers used in the present invention may be dihydroxy alcohol alkyl ethers or dihydroxy alcohol aryl ethers. The examples of dihydroxy alcohol alkyl ether include ethylene glycol methyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether, ethylene glycol ethyl ether, diethylene glycol ethyl ether, propylene glycol ethyl ether, dipropylene glycol ethyl ether, etc. The examples of dihydroxy alcohol aryl ethers include ethylene glycol phenyl ether, diethylene glycol phenyl ether, propylene glycol phenyl ether, dipropylene glycol phenyl ether, and the like. Any of the above mentioned solvent can be used either alone or in combination thereof.

Water Dispersible granules (WG) can be applied after disintegration and dispersion in water. Water dispersible granules can be formed by a) agglomeration, b) spray drying, or c) extrusion techniques.

WG formulations offer a number of advantages in packaging, ease of handling and safety. The WG are preferably of uniform size and which are free flowing, low dusting and readily disperse in water to form a homogenous solution of very small particles which may pass through conventional spray nozzles. Ideally WG formulations when dispersed in water under gentle agitation for five minutes have residues of less than 0.01% on a 150 µm sieve screen and less than 0.5% on a 53 µm screen. The granules can usually be measured accurately by volume which is convenient for the end user.

The defoliating composition of the present invention offers the benefits listed below compared to conventional formulation or individual formulations available in market;
• Promote defoliation of mature and juvenile foliage in cotton.
• Reduce terminal growth of cotton plant.
• Accelerate opening of mature boll.
• Potential to promote crop earliness, better boll retention by keeping vegetative and reproductive growth in harmony to enhance seed cotton yield.
• Promote earlier harvest and enhances the potential for high quality, higher yield of lint.
• Cost and labor in case of manual picking as complete harvest will be done in one or maximum two picking.
• Facilitate mechanical harvesting.
• Application can be done on desi cotton, american cotton, hybrid cotton, genetically modified cotton, herbicide tolerant cotton, insect resistant cotton.
The process for preparing the present composition can be modified accordingly by any person skilled in the art based on the knowledge of the manufacturing the formulation. However all such variation and modification is still covered by the scope of present invention.

EXAMPLES
Example 1: Thidiazuron 12% + Diuron 6% + Metsulfuron Methyl 0.4% SC
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 12.0
Diuron a.i. 6.0
Metsulfuron Methyl a.i. 0.4
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
Trisiloxane ethoxylate 2.0
Water QS
TOTAL 100.0

Procedure:
Step 1 Gum Solution should be made 12-18 hour prior to use. Take required quantity of water, biocide, and defoamer and homogenize, then slowly add gum powder to it and stir till complete dissolution.
Step 2 Charge required quantity of DM water need to be taken in designated vessel for Suspension concentrate production.
Step 3 Add required quantity of Wetting agent, antifreeze, dispersing agent & suspending agents and homogenize the contents for 45 – 60 minutes using high shear homogenizer.
Step 4 Then add technical and other remaining adjuvants excluding ‘thickener’ are added to it and homogenized to get uniform slurry ready for grinding.
Step 5 Before grinding half the quantity of antifoam was added and then material was subjected to grinding in Dyno mill till desired particle size is achieved.
Step 6 Half quantity of the antifoam was added after grinding process completes and before sampling for in process analysis.
Step 7 Finally add gum solution to this formulation and send to QC for quality check.

Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description White to Off White colour flowable liquid Complies Complies Complies
Thidiazuron content percent by mass 11.4 to 12.6 12.15 12.02 12.15
Diuron content percent by mass 5.7 to 6.6 6.20 6.13 6.20
Metsulfuron Methyl content percent by mass 0.38 to 0.44 0.43 0.41 0.43
Thidiazuron suspensibility percent mini. 80 94.55 92.47 94.05
Diuron suspensibility percent mini. 80 97.01 93.15 96.55
Metsulfuron Methyl suspensibility percent mini. 80 96.90 94.01 95.75
pH range (1% aq. Suspension) 5.5 to7.5 7.07 7.09 7.07
Pourability 95 % min 98.50 97.70 97.60
Specific gravity 1.05 – 1.15 1.07 1.08 1.07
Viscosity at spindle no.62, 20 rpm 350 -800 cps 510 530 535
Particle size (micron) D50 <3, D90 <10 2.2, 7.9 2.4, 8.5 2.7, 8.5
Persistent foam ml (after 1 minute) max. 60 3 5 5

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description White to Off White colour flowable liquid Complies Complies Complies Complies
Thidiazuron content percent by mass 11.4 to 12.6 12.15 12.14 12.11 12.05
Diuron content percent by mass 5.7 to 6.6 6.19 6.18 6.16 6.13
Metsulfuron Methyl content percent by mass 0.38 to 0.44 0.43 0.43 0.43 0.42
Thidiazuron suspensibility percent mini. 80 94.96 94.87 94.60 94.55
Diuron suspensibility percent mini. 80 96.96 96.51 96.27 95.58
Metsulfuron Methyl suspensibility percent mini. 80 96.86 96.75 96.53 95.81
pH range (1% aq. Suspension) 5.5 to7.5 7.07 7.07 7.08 7.09
Pourability 95 % min 98.50 98.40 97.20 96.80
Specific gravity 1.05 – 1.15 1.07 1.07 1.08 1.08
Viscosity at spindle no.62, 20 rpm 350 -800 cps 510 515 518 526
Particle size (micron) D50 <3, D90 <10 2.2, 8 2.2, 8.1 2.3, 8.2 2.4, 8.5
Persistent foam ml (after 1 minute) max. 60 3 3 5 5

Example 2: Thidiazuron 12% + Diuron 6% + Chlorimuron Ethyl 0.4% SC
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 12.0
Diuron a.i. 6.0
Chlorimuron Ethyl a.i. 0.4
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
Trisiloxane ethoxylate 2.0
Water QS
TOTAL 100.0

Procedure: As per Example 1
Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description White to Off White colour flowable liquid Complies Complies Complies
Thidiazuron content percent by mass 11.4 to 12.6 12.08 12.05 12.07
Diuron content percent by mass 5.7 to 6.6 6.12 6.03 6.12
Chlorimuron Ethyl content percent by mass 0.42 to 0.44 0.42 0.41 0.42
Thidiazuron suspensibility percent mini. 80 95.50 92.58 93.55
Diuron suspensibility percent mini. 80 94.00 92.14 93.75
Chlorimuron Ethyl suspensibility percent mini. 80 95.45 95.06 95.41
pH range (1% aq. Suspension) 5.5 to7.5 7.05 7.08 7.05
Pourability 95 % min 98.50 97.70 97.60
Specific gravity 1.05 – 1.15 1.07 1.08 1.07
Viscosity at spindle no.62, 20 rpm 350 -800 cps 505 530 535
Particle size (micron) D50 <3, D90 <10 2.2, 7.9 2.4, 8.5 2.7, 8.5
Persistent foam ml (after 1 minute) max. 60 3 10 5

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description White to Off White colour flowable liquid Complies Complies Complies Complies
Thidiazuron content percent by mass 11.4 to 12.6 12.08 12.07 12.07 12.06
Diuron content percent by mass 5.7 to 6.6 6.12 6.12 6.07 6.05
Chlorimuron Ethyl content percent by mass 0.38 to 0.44 0.42 0.42 0.41 0.41
Thidiazuron suspensibility percent mini. 80 95.10 94.85 94.72 94.50
Diuron suspensibility percent mini. 80 93.85 93.70 93.55 92.87
Chlorimuron Ethyl suspensibility percent mini. 80 95.05 94.98 94.80 94.71
pH range (1% aq. Suspension) 5.5 to7.5 7.05 7.05 7.07 7.08
Pourability 95 % min 98.40 98.40 97.20 96.80
Specific gravity 1.05 – 1.15 1.07 1.07 1.08 1.08
Viscosity at spindle no.62, 20 rpm 350 -800 cps 505 510 514 518
Particle size (micron) D50 <3, D90 <10 2.2, 8 2.2, 8.1 2.3, 8.2 2.4, 8.5
Persistent foam ml (after 1 minute) max. 60 3 3 5 8

Example 3: Thidiazuron 2.5% + Ethephon 30% + Metsulfuron Methyl 0.05% SC
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 2.5
Ethephon a.i. 30.0
Metsulfuron Methyl a.i. 0.05
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Polyalkoxylated butyl ether 1.0
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
Trisiloxane ethoxylate 2.0
Water QS
TOTAL 100.0

Procedure: As per Example 1
Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description White to Off White colour flowable liquid Complies Complies Complies
Thidiazuron content percent by mass 2.375 to 2.75 2.55 2.51 2.55
Ethephon content percent by mass 28.5 to 31.5 30.30 30.21 30.29
Metsulfuron Methyl content percent by mass 0.0475 to 0.055 0.053 0.051 0.053
Thidiazuron suspensibility percent mini. 80 98.91 97.07 98.71
Ethephon suspensibility percent mini. 80 97.05 95.49 96.51
Metsulfuron Methyl suspensibility percent mini. 80 96.93 95.08 95.76
pH range (1% aq. Suspension) 5.5 to7.5 7.10 7.19 7.11
Pourability 95 % min 98.50 97.70 97.60
Specific gravity 1.05 – 1.15 1.08 1.09 1.08
Viscosity at spindle no.62, 20 rpm 350 -800 cps 530 550 555
Particle size (micron) D50 <3, D90 <10 2.2, 7.9 2.4, 8.5 2.7, 8.5
Persistent foam ml (after 1 minute) max. 60 3 8 5

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description White to Off White colour flowable liquid Complies Complies Complies Complies
Thidiazuron content percent by mass 2.375 to 2.75 2.54 2.54 2.53 2.51
Ethephon content percent by mass 28.5 to 31.5 30.28 30.26 30.25 30.22
Metsulfuron Methyl content percent by mass 0.0475 to 0.055 0.053 0.053 0.052 0.051
Thidiazuron suspensibility percent mini. 80 97.90 97.76 97.70 97.51
Ethephon suspensibility percent mini. 80 96.92 96.52 96.12 95.49
Metsulfuron Methyl suspensibility percent mini. 80 96.84 96.68 96.65 95.41
pH range (1% aq. Suspension) 5.5 to7.5 7.10 7.11 7.12 7.15
Pourability 95 % min 98.50 98.40 97.20 96.80
Specific gravity 1.05 – 1.15 1.08 1.08 1.08 1.09
Viscosity at spindle no.62, 20 rpm 350 -800 cps 530 533 536 540
Particle size (micron) D50 <3, D90 <10 2.2, 8 2.2, 8.1 2.3, 8.2 2.4, 8.6
Persistent foam ml (after 1 minute) max. 60 2 3 5 8

Example 4: Thidiazuron 2.5% + Ethephon 30% + Chlorimuron Ethyl 0.05% SC
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 2.5
Ethephon a.i. 30.0
Chlorimuron Ethyl a.i. 0.05
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Polyalkoxylated butyl ether 1.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
Trisiloxane ethoxylate 2.0
Water QS
TOTAL 100.0

Procedure: As per Example 1

Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description White to Off White colour flowable liquid Complies Complies Complies
Thidiazuron content percent by mass 2.375 to 2.75 2.59 2.51 2.58
Ethephon content percent by mass 28.5 to 31.5 30.25 30.18 30.25
Chlorimuron Ethyl content percent by mass 0.0475 to 0.055 0.054 0.052 0.053
Thidiazuron suspensibility percent mini. 80 95..65 93.51 95.50
Ethephon suspensibility percent mini. 80 97.01 95.50 96.55
Chlorimuron Ethyl suspensibility percent mini. 80 96.95 95.06 95.75
pH range (1% aq. Suspension) 5.5 to7.5 6.97 6.95 6.97
Pourability 95 % min 98.60 97.70 97.60
Specific gravity 1.05 – 1.15 1.07 1.08 1.07
Viscosity at spindle no.62, 20 rpm 350 -800 cps 560 580 580
Particle size (micron) D50 <3, D90 <10 2.2, 7.9 2.5, 8.9 2.7, 8.5
Persistent foam ml (after 1 minute) max. 60 3 10 5

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description White to Off White colour flowable liquid Complies Complies Complies Complies
Thidiazuron content percent by mass 2.375 to 2.75 2.58 2.56 2.55 2.52
Ethephon content percent by mass 28.5 to 31.5 30.24 30.22 30.21 30.19
Chlorimuron Ethyl content percent by mass 0.0475 to 0.055 0.054 0.054 0.054 0.053
Thidiazuron suspensibility percent mini. 80 95.17 94.82 94.75 94.62
Ethephon suspensibility percent mini. 80 96.95 96.50 96.25 95.50
Chlorimuron Ethyl suspensibility percent mini. 80 96.85 96.71 96.51 95.81
pH range (1% aq. Suspension) 5.5 to7.5 6.97 6.97 6.97 6.95
Pourability 95 % min 98.60 98.40 97.20 96.80
Specific gravity 1.05 – 1.15 1.07 1.07 1.08 1.08
Viscosity at spindle no.62, 20 rpm 350 -800 cps 560 561 564 569
Particle size (micron) D50 <3, D90 <10 2.2, 8 2.2, 8.1 2.3, 8.2 2.5, 8.9
Persistent foam ml (after 1 minute) max. 60 3 3 8 10

Example 5: Thidiazuron 10% + Cyclanilide 15% + Metsulfuron Methyl 0.2% SC
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 10.0
Cyclanilide a.i. 15.0
Metsulfuron Methyl a.i. 0.2
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
Trisiloxane ethoxylate 2.0
Water QS
TOTAL 100.0

Procedure: As per Example 1
Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description White to Off White colour flowable liquid Complies Complies Complies
Thidiazuron content percent by mass 9.5 to 10.5 10.18 10.05 10.16
Cyclanilide content percent by mass 14.25 to 15.75 15.32 15.18 15.30
Metsulfuron Methyl content percent by mass 0.19 to 0.22 0.21 0.20 0.21
Thidiazuron suspensibility percent mini. 80 95.14 91.88 95.05
Cyclanilide suspensibility percent mini. 80 97.01 95.50 96.55
Metsulfuron Methyl suspensibility percent mini. 80 95.15 92.17 94.76
pH range (1% aq. Suspension) 5.5 to7.5 7.02 7.01 7.02
Pourability 95 % min 98.50 97.70 97.60
Specific gravity 1.05 – 1.15 1.06 1.07 1.07
Viscosity at spindle no.62, 20 rpm 350 -800 cps 505 530 535
Particle size (micron) D50 <3, D90 <10 2.2, 7.9 2.4, 8.5 2.7, 8.5
Persistent foam ml (after 1 minute) max. 60 5 10 5

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description White to Off White colour flowable liquid Complies Complies Complies Complies
Thidiazuron content percent by mass 9.5 to 10.5 10.17 10.16 10.14 10.11
Cyclanilide content percent by mass 14.25 to 15.75 15.32 15.31 15.30 15.24
Metsulfuron Methyl content percent by mass 0.19 to 0.22 0.21 0.21 0.21 0.20
Thidiazuron suspensibility percent mini. 80 94.75 94.56 94.14 93.45
Cyclanilide suspensibility percent mini. 80 96.95 96.50 96.25 95.50
Metsulfuron Methyl suspensibility percent mini. 80 95.05 94.58 94.45 94.41
pH range (1% aq. Suspension) 5.5 to7.5 7.02 7.02 7.02 7.01
Pourability 95 % min 98.50 98.40 97.20 96.80
Specific gravity 1.05 – 1.15 1.06 1.06 1.06 1.07
Viscosity at spindle no.62, 20 rpm 350 -800 cps 505 513 516 526
Particle size (micron) D50 <3, D90 <10 2.2, 8 2.2, 8.1 2.3, 8.2 2.6, 8.3
Persistent foam ml (after 1 minute) max. 60 5 5 5 10

Example 6: Thidiazuron 10% + Cyclanilide 15% + Chlorimuron Ethyl 0.2% SC
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 10.0
Cyclanilide a.i. 15.0
Chlorimuron Ethyl a.i. 0.2
Ethoxylated Fatty Alcohol 2.0
Acrylic graft copolymer 3.0
Alkylated naphtalene sulfonate, sodium salt 0.5
Silicone antifoam 0.5
1,2-benzisothiazolin-3-one 0.20
Mono Ethylene Glycol 5.0
Polysaccharides 0.15
Trisiloxane ethoxylate 2.0
Water QS
TOTAL 100.0

Procedure: As per Example 1
Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description White to Off White colour flowable liquid Complies Complies Complies
Thidiazuron content percent by mass 9.5 to 10.5 10.08 10.02 10.07
Cyclanilide content percent by mass 14.25 to 15.75 15.12 15.05 15.12
Chlorimuron Ethyl content percent by mass 0.19 to 0.22 0.21 0.20 0.21
Thidiazuron suspensibility percent mini. 80 98.95 97.05 98.69
Cyclanilide suspensibility percent mini. 80 97.01 95.50 96.55
Chlorimuron Ethyl suspensibility percent mini. 80 96.95 95.06 95.75
pH range (1% aq. Suspension) 5.5 to7.5 6.98 7.01 6.98
Pourability 95 % min 98.50 97.70 97.60
Specific gravity 1.05 – 1.15 1.06 1.07 1.07
Viscosity at spindle no.62, 20 rpm 350 -800 cps 505 535 550
Particle size (micron) D50 <3, D90 <10 2.2, 7.9 2.4, 8.5 2.7, 8.5
Persistent foam ml (after 1 minute) max. 60 2 5 5

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description White to Off White colour flowable liquid Complies Complies Complies Complies
Thidiazuron content percent by mass 9.5 to 10.5 10.08 10.07 10.06 10.03
Cyclanilide content percent by mass 14.25 to 15.75 15.11 15.09 15.08 15.05
Chlorimuron Ethyl content percent by mass 0.19 to 0.22 0.21 0.21 0.21 0.20
Thidiazuron suspensibility percent mini. 80 97.91 97.78 97.71 97.55
Cyclanilide suspensibility percent mini. 80 96.95 96.50 96.25 95.50
Chlorimuron Ethyl suspensibility percent mini. 80 96.85 96.71 96.51 95.81
pH range (1% aq. Suspension) 5.5 to7.5 6.98 6.98 6.98 7.01
Pourability 95 % min 98.50 98.40 97.20 96.80
Specific gravity 1.05 – 1.15 1.06 1.06 1.06 1.07
Viscosity at spindle no.62, 20 rpm 350 -800 cps 505 508 512 532
Particle size (micron) D50 <3, D90 <10 2.2, 8 2.2, 8.1 2.3, 8.2 2.4, 8.3
Persistent foam ml (after 1 minute) max. 60 2 3 3 5

Example 7: Thidiazuron 24 % + Diuron 12 % + Metsulfuron Methyl 0.8 % WG
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 24.0
Diuron a.i. 12.0
Metsulfuron Methyl a.i. 0.8
Alkylated naphthalene sulfonate, sodium salt 7.0
Polyacrylate polymer sodium salt 3.0
Sodium alkyl naphthalene sulfonate blend 2.0
Silicone antifoam 1.0
Lactose 10.0
Corn starch 20.0
China Clay QS
TOTAL 100.0

Procedure:
Step 1 Charge the required quantity of filler, wetting agent, dispersing agent, and suspending agent, & technical in premixing blender for homogenization for 30 minutes.
Step 2 Pre-blended material is then grinded through Jet mill/ air classifier mills. Finely grinded material is blended in post blender till it becomes homogeneous. (for approx 1.5 hr)
Step 3 Finely grinded powder is mixed with required quantity of water to form extrudable dough.
Step 4 Dough is passed through extruder to get granules of required size.
Step 5 Wet granules are passed through Fluidized bed drier and further graded using vibrating screens.
Step 6 Final product is sent for QC approval.
Step 7 After approval material is packed in required pack sizes.

Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Off white colour granules Complies Complies Complies
Thidiazuron content percent by mass 22.8 to 25.2 24.16 24.04 24.15
Diuron content percent by mass 11.4 to 12.6 12.08 12.01 12.07
Metsulfuron content percent by mass 0.76 to 0.88 0.85 0.81 0.84
Thidiazuron suspensibility percent min. 70 91.50 90.15 91.48
Diuron suspensibility percent min. 70 93.54 91.17 93.14
Metsulfuron suspensibility percent min. 70 92.14 90.25 92.02
pH range (1% aq. Suspension) 5.5 to7.5 7.03 7.01 7.03
Wettability sec. max. 60 9 10 10
Wet Sieve(45 micron ) percent by mass min. 98.5 99.6 99.3 99.5
Bulk density (g/ml) 0.45 to 0.75 0.48 0.48 0.48
Moisture content percent by mass max. Max. 2.0% 1.6 0.8 1

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description Off white colour granules Complies Complies Complies Complies
Thidiazuron content percent by mass 22.8 to 25.2 24.15 24.14 24.12 24.06
Diuron content percent by mass 11.4 to 12.6 12.08 12.06 12.04 12.02
Metsulfuron content percent by mass 0.76 to 0.88 0.85 0.85 0.83 0.82
Thidiazuron suspensibility percent min. 70 91.42 91.25 91.05 90.54
Diuron suspensibility percent min. 70 93.38 92.98 92.65 92.05
Metsulfuron suspensibility percent min. 70 92.01 91.96 91.74 91.23
pH range (1% aq. Suspension) 5.5 to7.5 7.03 7.03 7.02 7.01
Wettability sec. max. 60 9 9 10 10
Wet Sieve(45 micron ) percent by mass min. 98.5 99.6 99.5 99.5 99.4
Bulk density (g/ml) 0.45 to 0.75 0.48 0.48 0.48 0.48
Moisture content percent by mass max. Max. 2.0% 1.6 1.6 1.4 1.2

Example 8: Thidiazuron 5% + Ethephon 60% + Metsulfuron Methyl 0.1 % WG
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 5.0
Ethephon a.i. 60.0
Metsulfuron Methyl a.i. 0.1
Alkylated naphthalene sulfonate, sodium salt 8.0
Polyacrylate polymer sodium salt 3.0
Sodium alkyl naphthalene sulfonate blend 2.0
Silicone antifoam 1.0
Lactose 5.0
Corn starch 10.0
China Clay QS
TOTAL 100.0

Procedure: As per Example 7
Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Off white colour granules Complies Complies Complies
Thidiazuron content percent by mass 4.75 to 5.5 5.20 5.04 5.20
Ethephon content percent by mass 57 to 63 60.51 60.23 60.48
Metsulfuron content percent by mass 0.095 to 0.11 0.11 0.10 0.10
Thidiazuron suspensibility percent min. 70 94.58 92.14 94.51
Ethephon suspensibility percent min. 70 95.11 93.19 95.05
Metsulfuron suspensibility percent min. 70 93.63 91.15 93.52
pH range (1% aq. Suspension) 5.5 to7.5 6.99 6.95 6.98
Wettability sec. max. 60 9 10 10
Wet Sieve(45 micron ) percent by mass min. 98.5 99.6 99.3 99.5
Bulk density (g/ml) 0.45 to 0.75 0.51 0.51 0.51
Moisture content percent by mass max. Max. 2.0% 1.6 0.8 1

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description Off white colour granules Complies Complies Complies Complies
Thidiazuron content percent by mass 4.75 to 5.5 5.19 5.17 5.16 5.07
Ethephon content percent by mass 57 to 63 60.49 60.46 60.41 60.30
Metsulfuron content percent by mass 0.095 to 0.11 0.11 0.11 0.11 0.10
Thidiazuron suspensibility percent min. 70 94.51 94.14 93.95 93.52
Ethephon suspensibility percent min. 70 95.02 94.85 94.19 93.0
Metsulfuron suspensibility percent min. 70 93.56 93.51 93.45 93.24
pH range (1% aq. Suspension) 5.5 to7.5 6.99 6.99 6.97 6.95
Wettability sec. max. 60 9 9 10 10
Wet Sieve(45 micron ) percent by mass min. 98.5 99.6 99.5 99.5 99.4
Bulk density (g/ml) 0.45 to 0.75 0.51 0.51 0.51 0.51
Moisture content percent by mass max. Max. 2.0% 1.6 1.6 1.4 0.8

Example 9: Thidiazuron 20% + Cyclanilide 30% + Metsulfuron Methyl 0.4 % WG
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 20.0
Cyclanilide a.i. 30.0
Metsulfuron Methyl a.i. 0.4
Alkylated naphthalene sulfonate, sodium salt 6.0
Polyacrylate polymer sodium salt 3.0
Sodium alkyl naphthalene sulfonate blend 2.0
Silicone antifoam 1.0
Lactose 5.0
Corn starch 15.0
China Clay QS
TOTAL 100.0

Procedure: As per Example 7
Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Off white colour granules Complies Complies Complies
Thidiazuron content percent by mass 19 to 21 20.52 20.11 20.49
Cyclanilide content percent by mass 28.5 to 31.5 30.30 30.05 30.28
Metsulfuron content percent by mass 0.38 to 0.44 0.42 0.40 0.42
Thidiazuron suspensibility percent min. 70 94.54 92.10 94.55
Cyclanilide suspensibility percent min. 70 95.13 93.11 95.10
Metsulfuron suspensibility percent min. 70 93.33 91.11 93.30
pH range (1% aq. Suspension) 5.5 to7.5 6.92 6.90 6.92
Wettability sec. max. 60 8 9 9
Wet Sieve(45 micron ) percent by mass min. 98.5 99.6 99.3 99.5
Bulk density (g/ml) 0.45 to 0.75 0.51 0.51 0.51
Moisture content percent by mass max. Max. 2.0% 1 0.8 1

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description Off white colour granules Complies Complies Complies Complies
Thidiazuron content percent by mass 19 to 21 20.51 20.48 20.46 20.22
Cyclanilide content percent by mass 28.5 to 31.5 30.28 30.27 30.26 30.08
Metsulfuron content percent by mass 0.38 to 0.44 0.42 0.42 0.41 0.40
Thidiazuron suspensibility percent min. 70 94.11 93.75 93.65 92.86
Cyclanilide suspensibility percent min. 70 95.05 94.83 94.71 94.38
Metsulfuron suspensibility percent min. 70 93.12 92.86 92.81 91.65
pH range (1% aq. Suspension) 5.5 to7.5 6.92 6.92 6.91 6.90
Wettability sec. max. 60 8 8 8 9
Wet Sieve(45 micron ) percent by mass min. 98.5 99.6 99.5 99.5 99.4
Bulk density (g/ml) 0.45 to 0.75 0.51 0.51 0.51 0.51
Moisture content percent by mass max. Max. 2.0% 1 1 0.8 0.8

Example 10: Thidiazuron 20% + Carfentrazone Ethyl 8% + Chlorimuron Ethyl 0.4 % WG
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 20.0
Carfentrazone Ethyl a.i. 8.0
Chlorimuron Ethyl a.i. 0.4
Alkylated naphthalene sulfonate, sodium salt 7.0
Polyacrylate polymer sodium salt 2.0
Sodium alkyl naphthalene sulfonate blend 1.0
Silicone antifoam 1.0
Lactose 10.0
Corn starch 20.0
China Clay QS
TOTAL 100.0

Procedure:
Step 1 Charge required quantity of DM water need to be taken in designated vessel for production.
Step 2 Add required quantity of Wetting agent, dispersing agent, antifoam & suspending agents and homogenize the contents for 45 – 60 minutes using high shear homogenizer.
Step 3 Add required quantity technical and homogenized to get uniform slurry ready for grinding.
Step 4 Now material is subjected to grinding in Bead mill till desired particle size is achieved.
Step 5 After grinding process completes the material is sprayed at required temperature.
Step 6 After completion of spray drying process material is collected and sent for QC department approval.
Step 7 After approval material is packed in required pack sizes.

Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Off white colour granules Complies Complies Complies
Thidiazuron content percent by mass 19 to 21 20.12 20.01 20.10
Carfentrazone Ethyl content percent by mass 7.6 to 8.8 8.16 8.12 8.00
Chlorimuron Ethyl content percent by mass 0.38 to 0.44 0.43 0.41 0.42
Thidiazuron suspensibility percent min. 70 92.25 91.55 92.16
Carfentrazone Ethyl suspensibility percent min. 70 94.25 91.26 94.24
Chlorimuron Ethyl suspensibility percent min. 70 94.18 92.15 94.08
pH range (1% aq. Suspension) 5.5 to7.5 7.05 7.08 7.05
Wettability sec. max. 60 10 11 10
Wet Sieve(45 micron ) percent by mass min. 98.5 99.6 99.3 99.5
Bulk density (g/ml) 0.45 to 0.75 0.48 0.48 0.48
Moisture content percent by mass max. Max. 2.0% 1.6 0.8 1

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description Off white colour granules Complies Complies Complies Complies
Thidiazuron content percent by mass 19 to 21 20.12 20.11 20.10 20.03
Carfentrazone Ethyl content percent by mass 7.6 to 8.8 8.16 8.15 8.13 8.12
Chlorimuron Ethyl content percent by mass 0.38 to 0.44 0.43 0.43 0.42 0.41
Thidiazuron suspensibility percent min. 70 92.05 92.01 91.85 91.52
Carfentrazone Ethyl suspensibility percent min. 70 94.02 94.01 93.90 93.50
Chlorimuron Ethyl suspensibility percent min. 70 94.16 94.03 93..01 92.42
pH range (1% aq. Suspension) 5.5 to7.5 7.05 7.06 7.06 7.08
Wettability sec. max. 60 10 10 11 11
Wet Sieve(45 micron ) percent by mass min. 98.5 99.6 99.5 99.5 99.4
Bulk density (g/ml) 0.45 to 0.75 0.48 0.48 0.48 0.48
Moisture content percent by mass max. Max. 2.0% 1.6 1.6 1 0.8

Example 11: Thidiazuron 20% + Sulfentrazone 8% + Metsulfuron Methyl 0.4 % WG
Chemical Composition Percent (% w/w)
Thidiazuron a.i. 20.0
Sulfentrazone a.i. 8.0
Metsulfuron Methyl a.i. 0.4
Alkylated naphthalene sulfonate, sodium salt 7.0
Polyacrylate polymer sodium salt 2.0
Sodium alkyl naphthalene sulfonate blend 1.0
Silicone antifoam 1.0
Lactose 10.0
Corn starch 20.0
China Clay QS
TOTAL 100.0

Procedure: As per Example 10
Stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Off white colour granules Complies Complies Complies
Thidiazuron content percent by mass 19 to 21 20.45 20.35 20.42
Sulfentrazone content percent by mass 7.6 to 8.8 8.25 8.05 8.24
Metsulfuron content percent by mass 0.38 to 0.44 0.42 0.41 0.42
Thidiazuron suspensibility percent min. 70 95.52 93.14 94.56
Sulfentrazone suspensibility percent min. 70 94.23 92.17 94.02
Metsulfuron suspensibility percent min. 70 93.14 91.12 93.05
pH range (1% aq. Suspension) 5.5 to7.5 7.03 7.01 7.05
Wettability sec. max. 60 9 11 10
Wet Sieve(45 micron ) percent by mass min. 98.5 99.7 99.1 99.5
Bulk density (g/ml) 0.45 to 0.75 0.49 0.49 0.49
Moisture content percent by mass max. Max. 2.0% 1.2 0.8 1

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 months 24 months
Description Off white colour granules Complies Complies Complies Complies
Thidiazuron content percent by mass 19 to 21 20.45 20.43 20.41 20.35
Sulfentrazone content percent by mass 7.6 to 8.8 8.25 8.24 8.23 8.15
Metsulfuron content percent by mass 0.38 to 0.44 0.42 0.42 0.42 0.40
Thidiazuron suspensibility percent min. 70 95.11 95.01 94.56 93.16
Sulfentrazone suspensibility percent min. 70 94.02 93.60 93.50 93.01
Metsulfuron suspensibility percent min. 70 93.05 92.15 92.02 91.62
pH range (1% aq. Suspension) 5.5 to7.5 7.03 7.03 7.02 7.01
Wettability sec. max. 60 9 9 10 11
Wet Sieve(45 micron ) percent by mass min. 98.5 99.7 99.5 99.5 99.2
Bulk density (g/ml) 0.45 to 0.75 0.49 0.49 0.49 0.49
Moisture content percent by mass max. Max. 2.0% 1.6 1.6 1.4 0.8

Example 12: Bio efficacy trials
The synergistic pesticide action of the composition of present invention can be demonstrated by the experiments below. A synergistic effect exists wherever the action of a combination (tank mix or ready-mix) of active ingredient is greater than the sum of the action of each of the components alone. Therefore a synergistically effective amount or an effective amount of a synergistic composition or combination is an amount that exhibits greater pesticide activity than the sum of the pesticide activities of the individual components. In the field of agriculture, it is often understood that the term “synergy” is as defined by Colby S.R. in an article entitled “ Calculation of the synergistic and antagonistic responses of herbicide combinations” published in the journal Weeds, 1967, 15, p.20-22, incorporated herein by reference in its entirety. The action expected for a given combination of two active components can be calculated as follows:
Colby’s Formula:

To study the synergistic effect of thidiazuron, diuron and one more active ingredient selected from metsulfuron methyl or Chlorimuron ethyl, various sets of experiments were conducted in cotton crop.
Trial 1
Field studies were conducted to determine the synergistic effect as defoliants and ball opening in cotton crop. Various tank mixtures like, Thidiazuron+ Diuron+ Metsulfuron methyl, Thidiazuron+ Diuron+ Chlorimuron ethyl, Thidiazuron+ Ethephon+ Metsulfuron methyl, Thidiazuron+ Cyclanilide+ Metsulfuron methyl were evaluated on cotton crop as a harvesting aid. Cotton is one of the most important fiber crops of India. Cotton harvesting in India is mainly done through hand picking. This manual cotton plucking is involving huge cultivation cost and also it’s a time consuming, required multiple picking (average 4 picking) and producing poor quality lint due to physical mixing of dried foliage and cotton straw. To reduce the cotton cultivation cost, to save time and to produce quality lint, chemical defoliant and boll opener plays an important role. Even the mechanical harvesting requires one time boll opening and defoliation. So to facilitate hand picking and also mechanical harvesting, the mixtures of different active ingredients had been tried to accelerate leaf drop and boll opening.
The experiment was conducted during kharif season 2016 at farmer field in middle Gujarat area. Soil was sandy loam with normal pH and well drain. The experiment comprises 3 sets of treatments (as 3 different trials). Sowing was done in 2nd week of June (after onset of rain). All the required standard agronomic practices were followed including inter culturing, fertilizer application, weed control and insect-pest control.
Details of Experiment:
a) Experiment design : Randomized Block Design
b) Replication : Three
c) Treatments : Twelve (Including untreated check)
d) Plot size : 50 sq. m.
e) Spacing : 90 cm x 60 cm
f) Test Crop & Variety : Cotton, Bt variety
g) Time of application : 150 DAS (Days After Sowing)
h) Spray method : Manually operated knap sack sprayer, using 300
liter per hectare water volume
Evaluation Method:
1) Leaf drop: Observed the entire plot and record the % leaf drop visually from 0 to 100%. The observation should be made at 10 days after application.
2) Open Boll: Count the number of open boll (including crack boll) and total number of boll per plant. Record the observations from 10 plants per plot at 20 Days after application (20 DAA).
Table 1 Leaf drop and Open boll in cotton crop
Treatments Dose (g or ml/l water) % Leaf drop at 10 DAA* Average number of open boll per plant at 20 DAA*
Obs.Value Cal.Value Ratio
Untreated Check 0.0 43.3
Thidiazuron 24% SC 0.416 53.7 51.8
Diuron 80% SC 0.062 43.3 49.4
Metsulfuron Methyl 20% WG 0.016 30.3 44.3
Chlorimuron Ethyl 25% WP 0.013 33.3 45.2
Thidiazuron 24% SC + Diuron 80% SC 0.416+0.062 60.3 73.7 0.82 55.6
Thidiazuron 24% SC + Metsulfuron Methyl 20% WG 0.416+0.016 63.7 67.7 0.94 51.8
Thidiazuron 24% SC + Chlorimuron Ethyl 25% WP 0.416+0.013 63.7 69.1 0.92 52.1
Diuron 80% SC + Metsulfuron Methyl 20% WG 0.062+0.016 52.3 60.5 0.87 50.3
Diuron 80% SC + Chlorimuron Ethyl 25% WP 0.062+0.013 50.7 62.2 0.81 50.8
Thidiazuron 24% SC+Diuron 80% SC + Metsulfuron Methyl 20% WG 0.416+0.062+0.016 91.7 81.7 1.12 66.4
Thidiazuron 24% SC+Diuron 80% SC + Chlorimuron Ethyl 25% WP 0.416+0.062+0.013 92.3 82.5 1.12 65.8
DAA- Days after Application.

The results of above experiment shows that mixture of Thidiazuron+Diuron+Metsulfuron methyl and Thidiazuron+Diuron+Chlorimuron ethyl are synergistic in terms of leaf drop and boll opening compared to Thidiazuron+Diuron and other treatment. The highest lead drop (> 90%) and open boll has been observed in this inventive mixture of Thidiazuron+Diuron+Metsulfuron methyl and Thidiazuron+Diuron+Chlorimuron ethyl compared to the untreated and solo applications as well as mixtures of two active ingredients.

Table 2 Leaf drop and Open boll in cotton crop
Treatments Dose (g or ml/l water) % Leaf drop at 10 DAA Average number of open boll per plant at 20 DAA
Obs.Value Cal.Value Ratio
Untreated Check (water spray) 41.2
Thidiazuron 24% SC 0.693 60.3 53.7
Ethephon 39% SL 5.128 53.7 52.7
Metsulfuron Methyl 20% WG 0.016 33.3 42.8
Chlorimuron Ethyl 25% WP 0.013 36.8 41.3
Thidiazuron 24% SC + Ethephon 39% SL 0.693+5.128 77.7 81.6 0.95 59.3
Thidiazuron 24% SC + Metsulfuron Methyl 20% WG 0.693+0.016 68.3 73.5 0.93 55.3
Thidiazuron 24% SC + Chlorimuron Ethyl 25% WP 0.693+0.013 66.7 74.9 0.89 54.3
Ethephon 39% SL + Metsulfuron Methyl 20% WG 5.128+0.016 65.7 69.1 0.95 53.3
Ethephon 39% SL + Chlorimuron Ethyl 25% WP 5.128+0.013 66.7 70.7 0.94 52.8
Thidiazuron 24% SC+Ethephon 39% SL + Metsulfuron Methyl 20% WG 0.693+5.128+0.016 97.7 87.7 1.11 68.3
Thidiazuron 24% SC + Ethephon 39% SL+Chlorimuron Ethyl 25% WP 0.693+5.128+0.013 97.7 88.4 1.11 66.5

The inventive composition of Thidiazuron+Ethephon+Metsulfuron methyl and Thidiazuron+Ethephon+Chlorimuron ethyl provides highest leaf drop (>97%) and highest number of open boll compared to untreated, solo application and mixtures of two active ingredients.

Table 3 Leaf drop and Open boll in cotton crop
Treatments Dose (g or ml/l water) % Leaf drop at 10 DAA Average number of open boll per plant at 20 DAA
Obs.Value Cal.Value Ratio
Untreated Check (water spray) - 40.6
Thidiazuron 24% SC 0.667 55.4 51.3
Cyclanilide 18% SC 0.556 32.7 38.8
Metsulfuron Methyl 20% WG 0.020 26.7 41.3
Chlorimuron Ethyl 25% WP 0.016 23.3 38.6
Thidiazuron 24% SC + Cyclanilide 18% SC 0.667+0.556 65.3 69.95 0.93 54.3
Thidiazuron 24% SC + Metsulfuron Methyl 20% WG 0.667+0.020 58.8 67.27 0.87 52.8
Thidiazuron 24% SC + Chlorimuron Ethyl 25% WP 0.667+0.016 56.7 65.78 0.86 52.5
Cyclanilide 18% SC + Metsulfuron Methyl 20% WG 0.556+0.020 47.7 50.63 0.94 43.6
Cyclanilide 18% SC + Chlorimuron Ethyl 25% WP 0.556+0.016 46.3 48.38 0.96 42.8
Thidiazuron 24% SC+Cyclanilide 18% SC+Metsulfuron Methyl 20% WG 0.667+0.556+0.020 86.3 77.96 1.11 67.7
Thidiazuron 24% SC+Cyclanilide 18% SC+Chlorimuron Ethyl 25% WP 0.667+0.556+0.016 84.7 76.96 1.10 65.3

The highest lead drop (>84%) and highest number of open boll was obtained in the treatment of Thidiazuron +Cyclanilide + Metsulfuron methyl and Thidiazuron+ Cyclanilide+ Chlorimuron ethyl. The synergism between Thidiazuron+ Cyclanilide+ Metsulfuron methyl and Thidiazuron+ Cyclanilide+ Chlorimuron ethyl was clearly evident from field trial observations.
,CLAIMS:
We claim;
[CLAIM 1]. A defoliating composition comprising A) Thidiazuron B) at least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil C) at least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl and one or more inactive excipient.

[CLAIM 2]. The defoliating composition as claimed in claim 1 wherein
I. A) Thidiazuron is in range of 1-30%;
II. B) at least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil is in range of 1-60%; and
III. C) at least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl is in range of 0.05-10%.

[CLAIM 3]. The defoliating composition as claimed in claim 1 wherein most preferred compositions are selected from:
a) Thidiazuron + Diuron+ Metsulfuron Methyl;
b) Thidiazuron + Diuron+ Chlorimuron Ethyl;
c) Thidiazuron + Ethephon+ Metsulfuron Methyl;
d) Thidiazuron + Ethephon+ Chlorimuron Ethyl;
e) Thidiazuron +Cyclanilide+ Metsulfuron Methyl;
f) Thidiazuron + Cyclanilide+ Chlorimuron Ethyl;
g) Thidiazuron + Carfentrazone Ethyl+ Chlorimuron Ethyl;
h) Thidiazuron + Sulfentrazone+ Metsulfuron Methyl;

[CLAIM 4]. The defoliating composition as claimed in claim 1 or 2, wherein inactive excipients are selected from the group consisting of dispersant, anti-freezing agent, anti-foam agent, wetting agent, suspension aid, anti-microbial agent, thickener, quick coating agent or sticking agents and buffering agent.

[CLAIM 5]. The defoliating composition as claimed in claim 1 -4, wherein the formulations comprises of dustable powder (DP), a wettable powder (WP), a granule (GR) such as an emulsifiable granule (EG) or more particularly a water-dispersible granule (WG), an aqueous dispersion (aqueous suspension concentrate (SC), an oily dispersion (OD), a suspo-emulsion (SE) and a capsule suspension (CS).

[CLAIM 6]. The defoliating composition as claimed in claim 5, wherein the preferable formulations are Water dispersible Granules (WG), Suspension concentrate (SC) and Wettable powders (WP).

[CLAIM 7]. The defoliating composition as claimed in claim 6, wherein suspension concentrate (SC) formulation comprises:
a) Thidiazuron in range of 1-30%;
b) At least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil in range of 1-60%;
c) At least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl in range of 0.05-10% and ;
d) one or more inactive excipients selected from wetting agent, Filler, Absorbent, Emulsifier, Dispersants, Stabilizers, Anti-caking and Free-flow agent.

[CLAIM 8]. The defoliating composition as claimed in claim 6, wherein Water dispersible granules (WG) comprises:
e) Thidiazuron in range of 1-30%;
f) At least one herbicide agent selected from Diuron, Paraquat Dichloride, Ethephon, Carfentrazone, Sulfentrazone, Pyraflufen, Fluthiacet, Flumiclorac, Cyclanilide and Saflufenacil in range of 1-60%;
g) At least one Herbicide of sulphonyl urea class selected from Metsulfuron Methyl and Chlorimuron Ethyl in range of 0.05-10% and ;
h) one or more inactive excipients selected from wetting agent, Filler, Absorbent, Emulsifier, Dispersants, Stabilizers, Anti-caking and Free-flow agent.

[CLAIM 9]. The defoliating composition as claimed in claim in any of the preceding claims, wherein the effective amount in defoliating composition is from about 50 ml to 2500 ml/per hectare.

[CLAIM 10]. The defoliating composition as claimed in claim in any of the preceding claims, wherein the said composition is effective for defoliation for crops selected from Cotton (GMO and Non GMO), Jute, Soybean (GMO and Non GMO), Green gram, Black gram and Red gram