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: Reduced-risk pesticidal formulation
2. APPLICANT(S):

(a) Name: Excel Crop Care Limited
(b) Nationality: Indian Company
(c) Address:
184-87 S.V. Road,
Jogeshwari (West), Mumbai 400 102, Maharashtra, India.
3. PREAMBLE TO THE DESCRIPTION
The following complete specification particularly describes the invention and the manner in which it is to be performed.

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FIELD OF INVENTIION
This invention relates to a reduced-risk pesticidal formulation comprising an insecticide active ingredient, wetting agents, dispersing agents, antifoaming agents and other inert substances, and the method of preparation of the said formulation.
BACKGROUND AND PRIOR ART
6,7,8,9,10-10-Hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide is a broad-spectrum insecticide used for control of a large variety of insects and mites in horticultural and agricultural crops such as cotton, cereals, oilseeds, fruits, vegetables etc. The said insecticide has a number of important advantages in that it is inexpensive, is less toxic to beneficial insects, and it is useful in resistance management. However, it is toxic to some non-target species such as fish. The risk factor varies, depending on the type of formulation used and characteristics thereof.
Various formulations of the said active ingredient have been reported in
the prior art.
US4804399 discloses a suspension concentrate formulation comprising in addition to the active ingredient, the alkali metal salt of a sulfosuccinic monoester and an alkali metal salt of a lignosulfonic acid in a mixture with a swellable alkaline earth metal silicate. However, this formulation is relatively viscous.
US5753591 describes liquid formulations in the form of aqueous suspension concentrates which comprise a surfactant combination of a

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phosphoric ester based on an ethoxylated alkylphenol and an ethoxylated alkylaryl- and alcohol phosphate ester.
US6294570 describes a microcapsule dispersions in which the dispersed microcapsules comprise active ingredient, an organic solvent or solvent mixture and a capsule-forming material based on isocyanate prepolymers and the aqueous phase which represents the dispersion medium comprises surfactants, a water-soluble inorganic salt and formulation aids.
IL46324 describes ultra-low volume formulation. However, such type of formulations have a very high tendency to drift.
Thus, there is a need for a safer formulation for 6,7,8,9,10-10-
hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-
benzodioxathiepin-3-oxide.
OBJECTS OF INVENTION
The main object of this invention is to provide a relatively safe formulation of the insecticide 6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide.
Another object of the invention is to provide a solvent-free formulation of the said insecticide.
Still another object of the invention is to provide a granular non-dusting and non-staining formulation of the said insecticide.
Another object of the present invention is to provide a formulation which disintegrate and disperse easily in water.

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A further object of the invention is to provide a formulation which is easy to store, handle and use.
A further object of the invention is to provide an effective means to control pests and to minimize the risk to users and to prevent environmental contamination.
Another object of the invention is to provide a method of preparation of the said formulation.
DETAILED DESCRIPTION OF THE INVENTION
This invention provides a novel formulation of the insecticide 6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide in form of water-dispersible granules having several advantages like ease of handling and reduced dusting. These are environmentally desirable characteristics. Moreover, the granules are free flowing, disintegrate and disperse easily in water to form uniform suspension.
The water-dispersible granules of the present invention can be prepared by mixing appropriate amount of active ingredient and inert substances, pulverizing, followed by subjecting the pulverized material to air jet milling to get desired particle size, adding adjuvants, mixing and moistening to appropriate water content and extruding the material to obtain granules of suitable size, and drying the said granules in fluidized bed dryer. The suspensibility and dispersibility of the product obtained were determined by CIPAC method.

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The active ingredient used in the formulation of present invention is the
insecticide 6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-
methano-2,4,3-benzodioxathiepin-3-oxide. In addition to the active ingredient, other components like dispersing agents such as sodium polycarboxylate, hereinafter referred to as Adjuvant A, potassium polycarboxylate hereinafter referred to as adjuvant E; emulsifying agents such as ethoxylated steryl phenols such as ethoxylated tristeryl phenol hereinafter referred to as Adjuvant B; wetting agents like salts of dialkyl sulfosuccinate such as dioctyl sulfosuccinate sodium salt hereinafter referred to as Adjuvant C, sodium lauryl sulfate hereinafter referred to as Adjuvant F, dialkyl naphthalene sulfonate sodium salt hereinafter referred to as Adjuvant J; disintegrating agents such as l-ethenyl-2-pyrrolidinone homopolymer hereinafter referred to as Adjuvant D, sodium starch glycolate hereinafter referred to as Adjuvant G, microcrystalline cellulose hereinafter referred to as Adjuvant H; Kaolin hereinafter referred to as Adjuvant I etc. have been used.
Example 1:
6,7,8,9,10-10-hexachloro-1,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide 50 wt% and adjuvant I 35 wt% were mixed, pulverized and air-jet milled. To this mixture, adjuvant A & B 5.0 wt% each, adjuvant C 2.0 wt% and adjuvant D 3.0 wt% were added. 24 wt% of water was added. The material was then subjected to extrusion to obtain granules of dimensions 0.5-2.0 mm length x 0.5-1.0 mm width. The granules were dried in fluidized bed dryer at around 50°C. The suspensibility and dispersibility of the product was 84.0% and 89.3% respectively.

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The efficacy of the product against gram pod borer is given in the
following Table.

Dose gm/lit Av. No. of larve survived /plant % Pod damage Yield q/ha
3 Days 5 Days 10 Days
1.0 0.40 0.33 0.40 8.17 13.03
2.0 0.53 0.33 0.27 7.54 16.62
3.0 0.53 0.27 0.20 4.50 18.35
5.0 0.60 0.28 0.20 3.85 22.94
control 0.47 0.83 1.0 11.40 11.84
Example 2
6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide 50 wt% and adjuvant I 35 wt% were mixed, pulverized and air-jet milled. To this mixture, adjuvant B & E 5.0 wt% each, adjuvant C 2.0 wt% and adjuvant D 3.0 wt% were added. 17.0 wt% water was added. The material was then subjected to extrusion to obtain granules of dimensions 0.5-2.0 mm length x 0.5-1.0 mm width. The granules were dried in fluidized bed dryer at around 50°C. The suspensibility and dispersibility of the product was 77.8% and 77.2% respectively.
Example 3
6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide 50 wt% and adjuvant I 35 wt% were mixed, pulverized and air-jet milled. To this mixture, adjuvant E 8.0 wt%, adjuvant J 5.0 wt% and adjuvant B 2.0 wt% were added. 14.0 wt%

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water was added. The material was then subjected to extrusion to obtain granules of dimensions 0.5-2.0 mm length x 0.5-1.0 mm width. The granules were dried in fluidized bed dryer at around 50°C. The suspensibility and dispersibility of the product was 85.7% and 84.7% respectively.
Example 4
6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide 50 wt% and adjuvant I 35 wt% were mixed, pulverized and air-jet milled. To this mixture, adjuvant E 5.0 wt%, adjuvant B 3.0 wt%, adjuvant J 2.0 wt%, adjuvant G 5.0 wt% were added. 15.0 wt% water was added. The material was then subjected to extrusion to obtain granules of dimensions 0.5-2.0 mm length x 0.5-1.0 mm width. The granules were dried in fluidized bed dryer at around 50°C. The suspensibility and dispersibility of the product was 67.9% and 41.3% respectively.
Example 5
6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide 50 wt% and adjuvant I 29.4 wt% were mixed, pulverized and air-jet milled. To this mixture, adjuvant A 5.0 wt%, adjuvants B 8s C 3.8 wt% each and adjuvant H 8.0 wt% were added. 16.0 wt% water was added. The material was then subjected to extrusion to obtain granules of dimensions 0.5-2.0 mm length x 0.5-1.0 mm width. The granules were dried in fluidized bed dryer at around 50°C. The suspensibility and dispersibility of the product was 72.0% and 79.0% respectively.

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Example 6
6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide 50 wt% and adjuvant I 35 wt% were mixed, pulverized and air-jet milled. To this mixture, adjuvant A & B 5.0 wt% each, adjuvant F 3.0 wt% and adjuvant B 2.0 wt% were added. 11.5 wt% water was added. The material was then subjected to extrusion to obtain granules of dimensions 0.5-2.0 mm length x 0.5-1.0 mm width. The granules were dried in fluidized bed dryer at around 50°C. The suspensibility and dispersibility of the product was 84.5% and 84.0% respectively.

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WE CLAIM:
1. A water dispersible granular pesticidal formulation comprising 25-75 wt% of 6,7,8,9,10- 10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide as the active ingredient, 3-20 wt% dispersing agent(s), 2-15 wt% disintegrating agent(s), 0.5-10 wt% emulsifying agent(s), 0.5-15 wt% wetting agent(s) and 5-50 wt% filler material.
2. A pesticidal formulation of claim 1 which is prepared by (a) mixing 6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide and filler (b) pulverizing (c) subjecting the pulverized material to particle size reduction by a method such as air jet milling (d) adding adjuvants (e) moistening the mixture (f) extruding the material to obtain granules (g) drying the said granules
3. A pesticidal formulation as claimed in claim 1 8& prepared as in claim 2, wherein the particle size of the material as described in claim 2(c)is such that more than 75% of the particles are below 4-8 microns, preferably 5-7 microns and most preferably below 6 microns.
4. The process of claims 2, wherein the amount of water added for moistening is from 10-30 wt%, more preferably 14-16 wt%.
5. A pesticidal formulation as claimed in claim 1, wherein the dispersing agent is selected from the class of alkali metal polycarboxylate, preferably sodium or potassium poly carboxylate, and most preferably sodium polycarboxylate

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6. A pesticidal formulation as claimed in claim 1, wherein the disintegrating agent is selected from the class of alkenyl pyrrolidinone homopolymer, preferably l-ethenyl-2-pyrrolidinone homopolymer
7. A pesticidal formulation as claimed in claim 1, wherein the disintegrating agent is alkali salt of starch glycolate, preferably sodium starch glycolate.
8. A pesticidal formulation as claimed in claim 1, wherein the disintegrating agent is microcrystalline cellulose.
9. A pesticidal formulation as claimed in claim 1, wherein the emulsifying agent used is ethoxylated steryl phenol, more preferably ethoxylated tristeryl phenol, most preferably ethoxylated tristeryl phenol 40 EO.
10. A pesticidal formulation as claimed in claim 1, wherein the wetting agent used is alkali salt of dialkyl sulfosuccinate, preferably sodium dialkyl sulfosuccinate, most preferably sodium dioctyl sulfosuccinate.
11. A pesticidal formulation as claimed in claim 1, wherein the wetting agent used is sodium lauryl sulfate.
12. A pesticidal formulation as claimed in claim 1, wherein the wetting agent used is alkali salt of dialkyl naphthalene sulfonate.
13. A pesticidal formulation as claimed in claim 1, wherein the filler material is selected from talc, bentonite, silica, lime, kaolin,

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chalk, clay, dolomite, diatomaceous earth, attaclay or kieselguhr, preferably silica and kaolin and most preferably kaolin.
14. A process for preparing water-dispersible granular formulation comprising the steps of (a) mixing 25-75 wt% 6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin-3-oxide and 5-50 wt% filler (b) pulverizing (c) subjecting the pulverized material to particle size reduction by any method such as air jet milling (d) adding 3-20 wt% dispersing agent(s), 2-15 wt% disintegrating agent(s), 0.5-10 wt% emulsifying agent(s), 0.5-15 wt% wetting agent(s) (e) moistening the mixture (f) extruding the material to obtain granules (g) drying the said granules
15. The process of claim 2 85 14, wherein the said granules are dried in a fluidized bed dryer at 25-75°C.

ABSTRACT
This invention relates to a reduced-risk pesticidal formulation and the method of preparation thereof. The formulation comprises 6,7,8,9,10-10-hexachloro-l,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxa'thiepin-3-oxide as an insecticide active ingredient, wetting agents, dispersing agents, antifoaming agents and other inert substances. The formulation of this invention is safer than conventional formulations of the same insecticide, is effective for control of the target pests and it is also storage-stable.
3 1 MAR 2005