DESC:FORM 2

THE PATENTS ACT 1970
(SECTION 39 OF 1970)

&
THE PATENT RULES, 2003

COMPLETE SPECIFICATION
(SECTION 10 and RULE 13)

INSECTICIDAL OIL DISPERSION COMPOSITION AND ITS PREPARATION PROCESS

We, COROMANDEL INTERNATIONAL LIMITED,
an Indian company incorporated under Companies Act of 1956, having its principal place of business at Coromandel House, Sardar Patel Road, Secunderabad – 500 003, Telangana, India.

The following specification particularly describes the invention and the manner in which it is to be performed:
FIELD OF INVENTION
The present invention relates to composition of insecticidal oil dispersion.

The present invention specifically relates to composition of insecticidal oil dispersion comprising Pymetrozine and other agrochemical auxiliaries.

The present invention more specifically relates to composition of insecticidal oil dispersion comprising Pymetrozine, one or more dispersing agents, one or more emulsifiers, one or more rheology modifiers and one or more oil adjuvants.

The present invention also relates to process for the preparation of Pymetrozine oil dispersion composition comprising the steps of adding, stirring, milling, collecting, homogenizing and packaging.

BACKGROUND OF INVENTION
Pymetrozine (CGA 215944) is a new insecticide, highly active and specific against sucking insect pests. Pymetrozine is the only representative of the pyridine azomethines, a new class of insecticides, and is currently being developed worldwide for control of aphids and whiteflies in field crops, vegetables, ornamentals, cotton, hop, deciduous fruit, and citrus, and of the brown planthopper, Nilaparvata lugens (Staol), in rice. The compound appears to have great promise in integrated pest management (IPM) programs due to its high degree of selectivity, low mammalian toxicity, and safety to birds, fish and non target arthropods.

Pymetrozine is a new insecticide from a chemical class pyridine azomethines, not previously used as a pesticide. The mode of action of Pymetrozine in insects has not been precisely determined biochemically, but it may involve effects on neuroregulation or nerve-muscle interaction. Physiologically, it appears to act by preventing these insects from inserting their stylus into the plant tissue.
The chemical name of Pymetrozine is 6-methyl-4-[(E)-(pyridin-3-ylmethylene)amino]-4,5-dihydro-2H-[1,2,4]-triazin-3-one. Pymetrozine has a chemical formula of C10H11N5O and a molecular mass of 217.23 g/mol. It has a structural formula of:

Pymetrozine was discovered and marketed by Ciba-Geigy/Syngenta Crop Protection Limited with the trade names Fulfill, Relay, Sterling, Plenum, Chess etc.

Oil dispersion is a non-aqueous suspension concentrate. It combines a very good biological efficacy with an environmental friendly formulation. The active ingredient is dispersed in oils or methylated crop oils. The main features are no aromatic solvent, non-aqueous formulation, non-flammable and low volatility, higher efficiency no labeling issue.

US Patent No. 4,931,439 A claims Pymetrozine compound and composition for controlling insects and arachnids. This patent also claims salts of active compound with organic or inorganic acids together with suitable carrier or adjuvants.

CN Patent No. 102017958 B discloses insecticidal composition containing Pymetrozine and propylene glycol alginate and the application thereof. The insecticidal composition can prevent hemiptera pests on crops and particularly can be used for preventing paddy delphacidae and wheat aphids, and the effect of the insecticidal composition is significantly higher than that of single agent.

CN Patent No. 102283193 B discloses preparation method which comprises the following steps of: adding water into 10 to 60 parts of Pymetrozine, 1 to 30 parts of dispersant, 0.1 to 10 parts of stabilizer, 0.1 to 10 parts of thickener, 0.1 to 10 parts of defoaming agent, 0.1 to 10 parts of anti-freezing agent and 0.1 to 10 parts of other auxiliary agents till complementing to 100 weight parts, performing ball milling for 2 to 3 hours in a ball mill till the suspension particle diameter of the materials is 1 to 3 microns, filtering, and thus obtaining the pymetrozine suspension.

CN Publication No. 102524267 A discloses a Pymetrozine suspension formulation comprising vegetable oil and derivatives thereof, characterized in that the composition comprises Pymetrozine 1 to 50%, vegetable oil and its derivatives 1-40 %, wetting agent 0.5 to 10%, dispersant 0.5 to 10%, emulsifier 2 to 15%, thickener 0.05 to 5%, defoamer 0.05 to 5%, antifreeze 1 to 10%, preservatives 0.1 to 10% and water up to 100%.

CN Patent No. 102726418 B discloses suspension seed coating agent comprising 5-60 parts of pymetrozine, 3-30 parts of dispersant, 0.1-10 parts of stabilizer, 0.1-10 parts of film-forming agent, 0.1-10 parts of antifoaming agent, 1-10 parts of antifreeze, 0.1-10 parts of penetrant, 0.2-10 parts of preservative, 0.5-10 parts of dye, add water to make up to 100 parts.

CN Patent No. 104054701 B discloses pymetrozine suspension comprising 5% to 35% of pymetrozine technical, 5% to 30% of dispersant, 1% to 5% of wetting agent, 0.01% to 5% of thickener, 0.1% to 3% of defoamer, 1% to 10% of antifreezing agent, 0% to 5% pH modulator and water.

CN Publication No. 10642096 A discloses a Pymetrozine oil suspension formulation composition characterized in that the composition by weight is 5-50%, wetting agent 1-3 %, dispersant 2-5%, emulsifier 5-15 %, solvent topping up to 100%.

US Patent No. 8,298,990 B2 discloses oil dispersion of improved stability consisting essentially of a) an aprotic organic solvent; b) a polymer or oligomer capable of hydrogen bonding; c) a dispersed active ingredient; d) a clay or silica rheology modifier; and e) at least one surfactant. It discloses insecticides as agrochemical active ingredient.

US Patent No. 9,226,507 B2 discloses composition for producing emulsifiable pesticide solutions comprising (a) water miscible organic solvent selected from the group consisting of glycol ether, a glycerol formal, dimethylsulfoxide, gamma-butyrolactone and mixtures thereof, (b) an alkoxylated alcohol, (c) a pesticidal active ingredient. It also discloses Pymetrozine as pesticidal active ingredient.

US Patent No. 9,635,852 B2 discloses composition including Pymetrozine in particulate form; a first polymeric dispersing agent, the first polymeric dispersing agent being a copolymer of (a) a maleic acid monomer and (b) a hydrophobic monomer; and a second polymeric dispersing agent, the second polymeric dispersing agent being a copolymer of (a) a (meth)acrylic acid monomer, an ethylenically unsaturated dicarboxylic acid monomer or a combination thereof, (b) a (meth)acrylamido alkyl or aryl sulfonate monomer; and (c) a third monomer selected from one or more of vinylic compounds, (meth)acrylic esters, vinyl acetate, and substituted (meth)acrylamides.

The prior art references relates to different compositions of Pymetrozine. None of the prior art references discloses composition containing Pymetrozine with specific excipients used in the present invention and its preparation process.

The inventors of the present invention provide composition of insecticidal oil dispersion comprising Pymetrozine, dispersing agents, rheology modifiers, emulsifiers and oil adjuvant. The inventors of the present invention also provide Pymetrozine oil dispersion produced using process of present invention is having advantage over Pymetrozine 50% WG formulation that has good sticking property, penetration and rain fasting properties, saves operational cost by milling the material, where as in WG we need planetary mixer and extruder for making granules, the oil dispersion requires low dosage is required and gives equivalent efficacy or more compared to Pymetrozine 50% WG and overall, it is an industrially and economically feasible process.

OBJECTIVE OF INVENTION
The main objective of the present invention is to provide composition of insecticidal oil dispersion having good sticking property, penetration and rain fasting properties.

Another objective of the present invention is to provide composition of insecticidal oil dispersion comprising Pymetrozine and other agrochemical auxiliaries.

Another objective of the present invention is to provide composition of insecticidal oil dispersion comprising Pymetrozine, one or more dispersing agents, one or more emulsifiers, one or more rheology modifiers and one or more oil adjuvants.

Another objective of the present invention is to process for the preparation of Pymetrozine oil dispersion composition comprising the steps of adding, stirring, milling, collecting, homogenizing and packaging.

In yet another objective of the present invention is to provide Pymetrozine oil dispersion as insecticide for application to plants.

SUMMARY OF INVENTION
Accordingly, the present invention provides a composition of insecticidal oil dispersion comprising Pymetrozine and other agrochemical auxiliaries.
One embodiment of the present invention provides a composition of insecticidal oil dispersion comprising Pymetrozine, one or more dispersing agents, one or more emulsifiers, one or more rheology modifiers and one or more oil adjuvants.

One embodiment of the present invention provides a composition of insecticidal oil dispersion comprising Pymetrozine, calcium alkyl benzene sulphonate, castor oil ethoxylate, ethoxylate of alkyl polyethylene glycol ether, organic derivative of a hectorite clay, fumed silica and oil.

Another embodiment of the present invention provides a process for the preparation of Pymetrozine oil dispersion composition comprising the steps of adding, stirring, milling, collecting, homogenizing and packaging.

Another embodiment of the present invention provides a composition of Pymetrozine oil dispersion provides good sticking property, penetration and rain fasting properties, saves operational cost by milling the material, requires low dose compare to water dispersible granules, industrially and economically feasible process.

Yet another embodiment of the present invention provides a composition of insecticidal oil dispersion comprising:
(a) Pymetrozine in the range of 20% to 50% (w/w),
(b) dispersing agents in the range of 3% to 10% (w/w),
(c) emulsifiers in the range of 1% to 20% (w/w),
(d) rheology modifiers in the range of 0.1% to 5% (w/w), and
(e) oil adjuvant in the range of 40% to 80% (w/w).

Yet another embodiment of the present invention provides a composition of insecticidal oil dispersion comprising:
(a) Pymetrozine in the range of 20% to 50% (w/w),
(b) calcium alkyl benzene sulphonate in the range of 3% to 10% (w/w),
(c) castor oil ethoxylate in the range of 1% to 10% (w/w),
(d) ethoxylate of alkyl polyethylene glycol ether in the range of 1% to 10% (w/w),
(e) organic derivative of a hectorite clay in the range of 0.1% to 3%,
(f) fumed silica in the range of 0.1% to 3% (w/w), and
(g) oil in the range of 40% to 80% (w/w).

Yet another embodiment of the present invention provides a composition of insecticidal oil dispersion comprising:
(a) Pymetrozine in the range of 20% to 50% (w/w),
(b) calcium alkyl benzene sulphonate in the range of 3% to 10% (w/w),
(c) tri-sec-butylphenol polyglycol ether in the range of 1% to 10% (w/w),
(d) polyoxyethylene sorbitol ester in the range of 1% to 10% (w/w),
(e) organic derivative of a hectorite clay in the range of 0.1% to 3%,
(f) fumed silica in the range of 0.1% to 3% (w/w), and
(g) oil in the range of 40% to 80% (w/w).

In yet another embodiment, the present invention provides a process for the preparation of insecticidal oil dispersion composition, wherein the process comprising steps of:
(a) charging oil adjuvant in high shear disperser and stirring followed by heating to 45-50°C,
(b) charging rheology modifier under stirring,
(c) charging dispersing agent and emulsifiers,
(d) adding Pymetrozine to the obtained homogenized solution in small portions over a period of ~ 1 hour under continuous stirring,
(e) charging rheology modifier under stirring for 30 min,
(f) milling the obtained mixture for 4 hours till the desired particle size distribution is achieved and cooling the contents to room temperature,
(g) transferring the milled material into a separate vessel and continue stirring at room temperature over a period of 2 hours, and
(h) packaging the obtained oil dispersion into the drum.

In yet another embodiment, the present invention provides a process for the preparation of insecticidal oil dispersion composition, wherein the process comprising steps of:
(a) charging oil in the high shear disperser and start stirring followed by heating to 40-45°C.
(b) charging organic derivative of a hectorite clay under stirring,
(c) charging calcium alkyl benzene sulphonate, castor oil ethoxylate and ethoxylate of alkyl polyethylene glycol ether and stirring the mixture for hominization,
(d) adding Pymetrozine to the obtained homogenized solution in small portions over a period of ~ 1 hour under continuous stirring,
(e) charging fumed silica under stirring for 30 min,
(f) milling the obtained mixture for 4 hours till the desired particle size distribution is achieved and cooling the contents to room temperature,
(g) transferring the milled material into a separate vessel and continue stirring at room temperature over a period of 2 hours, and
(h) packaging the obtained oil dispersion into the drum.

In yet another embodiment, the present invention provides a process for the preparation of insecticidal oil dispersion composition, wherein the process comprising steps of:
(a) charging oil in the high shear disperser and start stirring followed by heating to 40-45°C.
(b) charging organic derivative of a hectorite clay under stirring,
(c) charging calcium alkyl benzene sulphonate, tri-sec-butylphenol polyglycol ether, polyoxyethylene sorbitol ester and stirring the mixture for hominization,
(d) adding Pymetrozine to the obtained homogenized solution in small portions over a period of ~ 1 hour under continuous stirring,
(e) charging fumed silica under stirring for 30 min,
(f) milling the obtained mixture for 4 hours till the desired particle size distribution is achieved and cooling the contents to room temperature,
(g) transferring the milled material into a separate vessel and continue stirring at room temperature over a period of 2 hours, and
(h) packaging the obtained oil dispersion into the drum.

DETAILED DESCRIPTION OF THE INVENTION
The term "comprising", which is synonymous with "including", "containing", or "characterized by" here is defined as being inclusive or open-ended, and does not exclude additional, unrecited elements or method steps, unless the context clearly requires otherwise.

The present invention provides a composition of insecticidal oil dispersion comprising Pymetrozine, one or more dispersing agents, one or more emulsifiers, one or more rheology modifiers and one or more oil adjuvants.

One embodiment of the present invention provides a composition of insecticidal oil dispersion comprising Pymetrozine, calcium alkyl benzene sulphonate, castor oil ethoxylate, ethoxylate of alkyl polyethylene glycol ether, organic derivative of a hectorite clay, fumed silica and methyl soyate oil.

An oil dispersion (OD) formulation is a solid active ingredient dispersed in oil. The oil can vary from paraffinic to aromatic solvent types and vegetable oil or methylated seed oils. Ideally the active ingredient is uniformly suspended in the oil phase.

Insecticidal agent used in the composition of the present invention includes Pymetrozine.

The concentration of Pymetrozine used in the insecticidal oil dispersion is from 20% to 50% (w/w). Preferably used concentration of Pymetrozine is 20% to 30% (w/w) of the total weight of the composition.

Dispersing agent used in the composition of the present invention includes but not limited to ethylene oxide-propylene oxide block polymers, alkylphenol polyglycol ethers, tristryrylphenol polyglycol ethers, phosphated or sulphated derivatives of these, calcium alkyl benzene sulphonate in 2-ethylhexanol (CALSOGEN 4814), n-C12 alkyl benzene sulfonate calcium salt phosphate ester (SOPHROPHOR FLR), n-C12 alkyl benzene sulfonate calcium salt, n-C12 alkyl benzene sulfonate calcium salt (PHENYLSULFONAT CAL) and calcium dodecyl benzene sulphonated (RHODOCAL 60 BER).

The concentration of dispersing agent used in the insecticidal oil dispersion is from 1% to 10% (w/w). Preferably used concentration of dispersing agent is 3% to 8% of the total weight of the composition.

Emulsifier used in the composition of the present invention includes but not limited to nonionic, anionic, cationic and amphoteric emulsifiers, or a blend of two or more emulsifiers. Preferably used emulsifiers include aliphatic amine alkoxylates, polyoxyethyleneglycerol fatty acid esters, castor oil alkoxylates, fatty acid alkoxylates, fatty acid amide alkoxylates, fatty acid polydiethanolamides, lanolin ethoxylates, fatty acid polyglycol esters, isoforms tridecyl alcohol, fatty acid amides, alkyl polyglycosides, castor oil ethoxylate with 36 mole EO (EMULSOGEN 360), castor oil ethoxylate with 36 mole EO (ATLOX 4853B), tri-sec-butylphenol polyglycol ether with 4 EO (SAPOGENAT T 040), ethoxylate of alkyl polyethylene glycol ether (LUTENSOL TO 5), EO/PO butyl ether (Ethylene 500 LQ), polyoxyethylene sorbitol ester (TWEEN 20) or its combinations thereof.

The concentration of emulsifiers used in the insecticidal oil dispersion is from 1% to 20% (w/w). Preferably used concentration of emulsifiers is 1% to 10% (w/w).

Rheology modifiers used in the composition of the present invention includes but not limited to organic derivative of a hectorite clay (like BENTONE 38, BENTONE 27, BENTONE 1000), xanthan gum, vegetable oil derivatives such as blend of vegetable oil base (SURFOM ESP 8105), guar gum, locust bean gum, carrageenan, alginates, methyl cellulose, carboxyethyl sodium carboxymethylcellulose, hydroxyethylcellulose, modified starches; other polysaccharides and modified polysaccharides, polyethylene alcohol, glycerol alkyl resins and cellulose derivatives, natural oils, mineral oils such as kyros oil and the fumed silicas such as AEROSIL R974, AEROSIL 200, AEROSIL 972, AEROSIL R816, AEROSIL 300 etc. Preferably used rheology modifiers are BENTONE 38, BENTONE 27, BENTONE 1000, AEROSIL R-816, AEROSIL 200, AEROSIL 300, AEROSIL R-816 AND AEROSIL R-972.

The concentration of rheology modifiers used in the insecticidal oil dispersion is from 0.1% to 5% (w/w). Preferably used concentration of rheology modifiers 0.1% to 1% of the total weight of the composition.

Oil adjuvant used in the composition of the present invention includes but not limited to methyl soyate oil, rapeseed oil, olive oil, castor oil, rape oil, corn oil, cottonseed oil, sunflower oil, mineral oil, paraffin oil, palm methyl ester oil. Preferably used oil adjuvant is methyl soyate oil, sunflower oil, mineral oil, paraffin oil, palm methyl ester oil.

The concentration of oil adjuvant used in the insecticidal oil dispersion is from 40% to 80% (w/w). Preferably used concentration of dispersing agent is 55% to 65% (w/w) of the total weight of the composition.

The present invention is to provide a composition of Pymetrozine oil dispersion with good sticking property, penetration and rain fasting properties, saves operational cost by milling the material, requires low dose compare to water dispersible granules, industrially and economically feasible process.

The present invention is to provide process for the preparation of Pymetrozine oil dispersion comprising the steps of adding, stirring, milling, collecting, homogenizing and packaging.

The following examples describes the nature of the invention and are given only for the purpose of illustrating the present invention in more detail and are not limitative and relate to solutions, which have been particularly effective on bench scale.

Example 1
S.No Ingredients Quantity (% w/w)
1. Pymetrozine tech @ 98 % (b) 25% 25.51
2. Calcium alkyl benzene sulphonate in 2-ethylhexanol (CALSOGEN 4814) 5.0
3. Castor oil ethoxylate with 36 mole EO (EMULSOGEN 360) 5.0
4. Ethoxylate of alkyl polyethylene glycol ether (LUTENSOL TO 5) 2.0
5. Organic derivative of a hectorite clay (BENTONE 38) 0.4
6. Fumed silica (AEROSIL R-816) 0.5
7. Methyl soyate oil 61.59
Total 100

Manufacturing process:
Specified quantity of Methyl soyate oil with the moisture content of NMT 0.1% was charged in the moisture free cleaned high shear disperser, stirred and heated to 40-45°C. Specified quantity of Organic derivative of a hectorite clay (BENTONE 38) was added and stirred. Calcium alkyl benzene sulphonate in 2-ethylhexanol (CALSOGEN 4814), Castor oil ethoxylate with 36 mole EO (EMULSOGEN 360) and Ethoxylate of alkyl polyethylene glycol ether (LUTENSOL TO 5) were added after every 15-20 min of interval. Pymetrozine Technical was added to the obtained homogenized solution at a temperature <50°C in small portions over a period of ~1h under continuous stirring. Specified quantity of fumed silica (AEROSIL-R-816) was added and stirred for 30 min. Obtained mixture was milled to attain the desired particle size distribution (D90 should be ~15 micron), milled further for ~4 hr and cooled the contents to room temperature. Obtained milled materials were transferred into separate vessel and stirred continuously at room temperature over a period of 2 hrs. Obtained oil dispersion was packaged in drum.

Example 2
S.No Ingredients Quantity (% w/w)
1. Pymetrozine tech @ 98 % (b) 25% 25.51
2. N-C12 alkyl benzene sulfonate calcium salt phosphate ester (SOPHROPHOR FLR) 5.0
3. Castor oil ethoxylate with 36 mole EO (ATLOX 4853B) 5.0
4. Ethylene oxide/propylene oxide butyl ether ( ETHYLAN NS 500 LQ) 2.0
5. Organic derivative of a hectorite clay (BENTONE 38) 0.4
6. Fumed silica (AEROSIL 200) 0.5
7. Sunflower oil 61.59
Total 100

Manufacturing process:
Specified quantity of Sunflower oil with the moisture content of NMT 0.1% was charged in the moisture free cleaned high shear disperser, stirred and heated to 40-45°C. Specified quantity of Organic derivative of hectorite clay (BENTONE 38) was added and stirred. N-C12 alkyl benzene sulfonate calcium salt phosphate ester (SOPHROPHOR FLR), Castor oil ethoxylate with 36 mole EO (ATLOX 4853B), Ethylene oxide/propylene oxide butyl ether ( ETHYLAN NS 500 LQ) were added after every 15-20 min of interval. Pymetrozine Technical was added to the obtained homogenized solution at a temperature <50°C in small portions over a period of ~1h under continuous stirring. Specified quantity of Fumed silica (AEROSIL 200) was added and stirred for 30 min. Obtained mixture was milled to attain the desired particle size distribution (D90 should be ~15 micron), milled further for ~4 hr and cooled the contents to room temperature. Obtained milled materials were transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Obtained oil dispersion was packaged in drum.

Example 3
S.No Ingredients Quantity (% w/w)
1. Pymetrozine tech @ 98 % (b) 25% 25.51
2. N-C12 alkyl benzene sulfonate calcium salt (PHENYLSULFONAT CAL) 5.0
3. Tri-sec-butylphenol polyglycol ether with 4 EO (SAPOGENAT T 040) 5.0
4. Polyoxyethylene sorbitol ester (TWEEN 20) 2.0
5. Organic derivative of a hectorite clay (BENTONE 27) 0.4
6. Fumed silica (AEROSIL 300) 0.5
7. Mineral oil 61.59
Total 100

Manufacturing process:
Specified quantity of Mineral oil with the moisture content of NMT 0.1% was charged in the moisture free cleaned high shear disperser, stirred and heated to 40-45°C. Specified quantity of Organic derivative of a hectorite clay (BENTONE 27) was added and stirred. N-C12 alkyl benzene sulfonate calcium salt (PHENYLSULFONAT CAL), Tri-sec-butylphenol polyglycol ether with 4 EO (SAPOGENAT T 040), Polyoxyethylene sorbitol ester (TWEEN 20) were added after every 15-20 min of interval. Pymetrozine technical was added to the obtained homogenized solution at a temperature <50°C in small portions over a period of ~1 h under continuous stirring. Specified quantity of Fumed silica (AEROSIL 300) was added and stirred for 30 min. Obtained mixture was milled to attain the desired particle size distribution (D90 should be ~15 micron), milled further for ~4 hr and cooled the contents to room temperature. Obtained milled materials were transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Obtained oil dispersion was packaged in drum.

Example 4
S.No Ingredients Quantity (% w/w)
1. Pymetrozine tech @ 98 % (b) 25% 25.51
2. Calcium alkyl benzene sulphonate in 2-ethylhexanol (CALSOGEN 4814) 5.0
3. Castor oil ethoxylate with 36 mole EO (EMULSOGEN 360) 5.0
4. Ethoxylate of alkyl polyethylene glycol ether (LUTENSOL TO 5) 2.0
5. Organic derivative of a hectorite clay (BENTONE 38) 0.4
6. Fumed silica (AEROSIL R-816) 0.5
7. Paraffin oil 61.59
Total 100

Manufacturing process:
Specified quantity of Paraffin oil with the moisture content of NMT 0.1% was charged in the moisture free cleaned high shear disperser, stirred and heated to 40-45°C. Specified quantity of Organic derivative of a hectorite clay (BENTONE 38) was added and stirred. Calcium alkyl benzene sulphonate in 2-ethylhexanol (CALSOGEN 4814), Castor oil ethoxylate with 36 mole EO (EMULSOGEN 360), Ethoxylate of alkyl polyethylene glycol ether (LUTENSOL TO 5) were added after every 15-20 min of interval. Pymetrozine technical was added to the obtained homogenized solution at a temperature <50°C in small portions over a period of ~1h under continuous stirring. Specified quantity of Fumed silica (AEROSIL R-816) was added and stirred for 30 min. Obtained mixture was milled to attain the desired particle size distribution (D90 should be ~15 micron), milled further for ~4 hr and cooled the contents to room temperature. Obtained milled materials were transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Obtained oil dispersion was packaged in drum.

Example 5
S.No Ingredients Quantity (% w/w)
1. Pymetrozine tech @ 98 % (b) 25% 25.51
2. Calcium dodecyl benzene sulphonated (RODHOCAL 60BER) 5.0
3. Castor oil ethoxylate (EMULSOGEN EL 360) 5.0
4. Ethoxylate of alkyl polyethylene glycol ether (LUTENSOL TO 5) 2.0
5. Organic derivative of a hectorite clay (BENTONE 1000) 0.4
6. fumed silica (AEROSIL R-972) 0.5
7. Palm methyl ester oil 61.59
Total 100

Manufacturing process:
Specified quantity of Palm methyl ester oil with the moisture content of NMT 0.1% was charged in the moisture free cleaned high shear disperser, stirred and heated to 40-45°C. Specified quantity of Organic derivative of a hectorite clay (BENTONE 1000) was added and stirred. Calcium dodecyl benzene sulphonated (RODHOCAL 60BER), Castor oil ethoxylate (EMULSOGEN EL 360) and Ethoxylate of alkyl polyethylene glycol ether (LUTENSOL TO 5) were added after every 15-20 min of interval. Pymetrozine Technical was added to the obtained homogenized solution at a temperature <50°C in small portions over a period of ~1h under continuous stirring. Specified quantity of Fumed silica (AEROSIL R-972) was added and stirred for 30 min. Obtained mixture was milled to attain the desired particle size distribution (D90 should be ~15 micron), milled further for ~4 hr and cooled the contents to room temperature. Obtained milled materials were transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Obtained oil dispersion was packaged in drum.

Field efficacy trials of Pymetrozine oil dispersion

Trial 1 Rice trial- Brown Planthopper (BPH)

The brown plant hopper, Nilaparvata lugens is a plant hopper species that feeds on rice plants. These insects are among the most important pests of rice, which is the major staple crop for about half the world's population. BPH nymphs and adults congregate at the base of the plant above the water level. Affected plant dries up and gives a scorched appearance called “hopper burn”. Circular patches of drying and lodging of matured plant. It is vector of grassy stunt, ragged stunt and wilted stunt diseases. Ovipositional marks exposing the plant to fungal and bacterial infections

The field trials were conducted to evaluate the efficacy of innovative product Pymetrozine 25% OD versus the existing Pymetrozine 50% WG formulations against BPH in rice trials were conducted in randomized block design with net plot size of 5m x 6m. Rice crop was raised with all standard agronomic practices. Spraying was done with manual operated backpack sprayer with 500 liter of water spray volume per hectare at 45 days after sowing. The observations were recorded by counting the no. of BPH insects per hill. The observations were recorded before spraying and 10 DAA (days after application).

Table 1: BPH control in Rice

Compositions
Dose Gram Active/ha % Insect Control at 10 DAA % Insect Control at 14 DAA
BPH BPH
Pymetrozine 25 % OD 150 GAH 99.5 98.0
Pymetrozine 50 % WG 150 GAH 92.0 89.0
OD Oil dispersion, WG Wettable granule, DAA Days after application

The trial result shows there is a difference between the efficacy of two formulations. Pymetrozine 25% OD provides excellent and longer duration control as compared to existing Pymetrozine 50 % WG Formulations against brown plant hopper in rice.

Trial 2 Rice trial- White Backed Planthopper (WBPH)

The white backed planthopper, Sogata furcifera is a planthopper species that feeds on rice plants. These insects are among the most important pests of rice, which is the major staple crop for about half the world's population. BPH can also transmit Rice Ragged Stunt and rice Grassy Stunt diseases. White backed plant hopper is more abundant during the early stage of the growth of rice crop, especially in nurseries. Rice is more sensitive to attack at the tillering phase than at the boot and heading stages.

The field trials were conducted to evaluate the efficacy of innovative product Pymetrozine 25% OD versus the existing Pymetrozine 50% WG formulations against WBPH in rice. Trials were conducted in randomized block design with net plot size of 5m x 6m. Rice crop was raised with all standard agronomic practices. Spraying was done with manual operated backpack sprayer with 500 liter of water spray volume per hectare at 45 days after sowing. The observations were recorded by counting the no. of BPH insects per hill. The observations were recorded before spraying and 10 DAA (days after application).

Table 2: WBPH control in Rice

Compositions
Dose Gram Active/ha % Insect Control at 10 DAA % Insect Control at 14 DAA
BPH BPH
Pymetrozine 25 % OD 150 GAH 99.0 97.5
Pymetrozine 50 % WG 150 GAH 93.0 88.0
OD Oil dispersion, WG Wettable granule, DAA Days after application

The trial result shows there is a difference between the efficacy of two formulations. Pymetrozine 25% OD provides excellent and longer duration control as compared to existing Pymetrozine 50 % WG formulations against white backed plant hopper in rice.
,CLAIMS:1. A composition of insecticidal oil dispersion comprising Pymetrozine, dispersing agents, emulsifiers, rheology modifiers and oil adjuvants.

2. The composition as claimed in claim 1, wherein said dispersing agents are one or more of ethylene oxide-propylene oxide block polymers, alkylphenol polyglycol ethers, tristryrylphenol polyglycol ethers, phosphated or sulphated derivatives of these, calcium alkyl benzene sulphonate in 2-ethylhexanol, n-C12 alkyl benzene sulfonate calcium salt phosphate ester, n-C12 alkyl benzene sulfonate calcium salt, n-C12 alkyl benzene sulfonate calcium salt and calcium dodecyl benzene sulphonated, wherein the concentration of dispersing agents is in the range of 1% to 10% w/w of total weight of composition.

3. The composition as claimed in claim 1, wherein said emulsifiers are one or more of aliphatic amine alkoxylates, polyoxyethyleneglycerol fatty acid esters, castor oil alkoxylates, fatty acid alkoxylates, fatty acid amide alkoxylates, fatty acid polydiethanolamides, lanolin ethoxylates, fatty acid polyglycol esters, isoforms tridecyl alcohol, fatty acid amides, alkyl polyglycosides, castor oil ethoxylate with 36 mole EO, castor oil ethoxylate with 36 mole EO, tri-sec-butylphenol polyglycol ether with 4 EO, ethoxylate of alkyl polyethylene glycol ether, EO/PO butyl ether, polyoxyethylene sorbitol ester, wherein the concentration of emulsifiers is in the range of 1% to 20% w/w of total weight of composition.

4. The composition as claimed in claim 1, wherein said rheology modifiers are one or more of organic derivative of a hectorite clay, xanthan gum, blend of vegetable oil base, guar gum, locust bean gum, carrageenan, alginates, methyl cellulose, carboxyethyl sodium carboxymethylcellulose, hydroxyethylcellulose, modified starches, polysaccharides, modified polysaccharides, polyethylene alcohol, glycerol alkyl resins, cellulose derivatives, natural oils, mineral oils, kyros oil, and fumed silicas, wherein the concentration of rheology modifiers is in the range of 0.1% to 5% w/w of total weight of composition.

5. The composition as claimed in claim 1, wherein said oil adjuvants are one or more of methyl soyate oil, rapeseed oil, olive oil, castor oil, rape oil, corn oil, cottonseed oil, sunflower oil, mineral oil, paraffin oil and palm methyl ester oil wherein the concentration of oil adjuvants is in the range of 0.1% to 5% w/w of total weight of composition.

6. The composition as claimed in claims 1 - 5, wherein said composition comprising:
(a) Pymetrozine in the range of 20% to 50% (w/w),
(b) calcium alkyl benzene sulphonate in the range of 3% to 10% (w/w),
(c) castor oil ethoxylate in the range of 1% to 10% (w/w),
(d) ethoxylate of alkyl polyethylene glycol ether in the range of 1% to 10% (w/w),
(e) organic derivative of a hectorite clay in the range of 0.1% to 3%,
(f) fumed silica in the range of 0.1% to 3% (w/w), and
(g) oil in the range of 40% to 80% (w/w).

7. The composition as claimed in claims 1 - 5, wherein said composition comprising:
(a) Pymetrozine in the range of 20% to 50% (w/w),
(b) calcium alkyl benzene sulphonate in the range of 3% to 10% (w/w),
(c) tri-sec-butylphenol polyglycol ether in the range of 1% to 10% (w/w),
(d) polyoxyethylene sorbitol ester in the range of 1% to 10% (w/w),
(e) organic derivative of a hectorite clay in the range of 0.1% to 3%,
(f) fumed silica in the range of 0.1% to 3% (w/w), and
(g) oil in the range of 40% to 80% (w/w).

8. The process for the preparation of composition as claimed in claim 1, wherein the process comprising steps of:
(a) charging oil adjuvant in high shear disperser and stirring followed by heating to 45-50°C,
(b) charging rheology modifier under stirring,
(c) charging dispersing agent and emulsifiers,
(d) adding Pymetrozine to the obtained homogenized solution in small portions over a period of ~ 1 hour under continuous stirring,
(e) charging rheology modifier under stirring for 30 min,
(f) milling the obtained mixture for 4 hours till the desired particle size distribution is achieved and cooling the contents to room temperature,
(g) transferring the milled material into a separate vessel and continue stirring at room temperature over a period of 2 hours, and
(h) packaging the obtained oil dispersion into the drum.

9. The process for the preparation of composition as claimed in claim 6, wherein the process comprising steps of:
(a) charging oil in the high shear disperser and start stirring followed by heating to 40-45°C,
(b) charging Organic derivative of a hectorite clay under stirring,
(c) charging calcium alkyl benzene sulphonate, castor oil ethoxylate and ethoxylate of alkyl polyethylene glycol ether and stirring the mixture for hominization,
(d) adding Pymetrozine to the obtained homogenized solution in small portions over a period of ~ 1 hour under continuous stirring,
(e) charging fumed silica under stirring for 30 min,
(f) milling the obtained mixture for 4 hours till the desired particle size distribution is achieved and cooling the contents to room temperature,
(g) transferring the milled material into a separate vessel and continue stirring at room temperature over a period of 2 hours, and
(h) packaging the obtained oil dispersion into the drum.

10. The process for the preparation of composition as claimed in claim 7, wherein the process comprising steps of:
(a) charging oil in the high shear disperser and start stirring followed by heating to 40-45°C,
(b) charging organic derivative of a hectorite clay under stirring,
(c) charging calcium alkyl benzene sulphonate, tri-sec-butylphenol polyglycol ether, polyoxyethylene sorbitol ester and stirring the mixture for hominization,
(d) adding Pymetrozine to the obtained homogenized solution in small portions over a period of ~ 1 hour under continuous stirring,
(e) charging fumed silica under stirring for 30 min,
(f) milling the obtained mixture for 4 hours till the desired particle size distribution is achieved and cooling the contents to room temperature,
(g) transferring the milled material into a separate vessel and continue stirring at room temperature over a period of 2 hours, and
(h) packaging the obtained oil dispersion into the drum.