FORM2
THE PATENTS ACT, 1970
(39 of l970)
&
The Patents Rules, 2006
COMPLETE SPECIFICATION
(See section 10; rule 13)
1. Title of the invention. -"Ecofriendly Water Dispersible Granular formulation and
manufacturing process for Sulfur"
2. Applicant(s)
(a) NAME : CROP LIFE SCIENCE LIMITED
(b) NATIONALITY: INDIAN
(c) ADDRESS : 209, "PRIMATE" Near Judges Bunglow Cross Road,
Bodakdev,Ahmedabad -380 015, Gujarat, India
3. PREAMBLE TO THE DESCRIPTION
The following specification particularly describes the invention and the manner in which it is to be performed:

Ecofriendly Water Dispersible Granular formulation and manufacturing process for Sulfur
Field of the invention:
The present invention relates to a water dispersible granular formulation of sulfur. More particularly, the present invention relates to a water dispersible granular formulation of sulfur and its manufacturing process.
Background and prior art:
Sulfur formulations are used as a broad spectrum fungicide and acaricide. It is used for the control of powdery mildew and scab on Grapes, Cowpea, Guar, Pea, Cumin, Apple, Mango, Cereals crops, Vegetables and Oilseed crops.
Sulfur product is usually available in different formulation viz.; Wettable Powder, Flowable, Dusts, granules and colloidal formulations. Sulfur is naturally present in the soil as both organic and inorganic forms. However, sulfur is not bioavailable to the plants in its organic form. There is a continuous need in the art for a sulfur composition that apart from its pesticidal properties, also makes sulfur bioavailable to the plants.
WO2008084495, to Deepak Pranjivandas Shah et al., discloses an agricultural composition comprising sulfur and at least one dispersing agent. The disclosed composition further comprises a wetting agent, binding agent, fillers and organic additives. The disclosed compositions are non-specific formulation type and could be formulated as water dispersible granules, wettable powders, dusting powders, suspension concentrates, tablets, liquids and oil suspensions.
WO2009003350 discloses a sulfur-based, chemical soil-corrective or conditioner for agricultural use in the form of pellets. The disclosed product contains fly sulfur powder, at least 3 % by weight of an inert compound selected from the group consisting of clay, bentonite, kaolin and mixtures thereof, and at least 0.5 % by weight of a wetting agent. The components are mixed with one another, then subjected to wet extrusion and next to drying, so as to obtain mechanically strong pellets which are porous and suitable to be very easily disaggregated when they are in contact with soil moisture.
GB2292140 discloses a method for producing sulfur compositions. The disclosed method comprises including an aqueous solution of a binding material to a granular or pulverulent

material produced by feeding the mixture of sulfur particles and inert or filler material between counter-rotating synchronous rollers where pressure is applied to form material of suitable size. A metallic soap may be added to the mixture to act as a release agent. The disclosed process leads to granular or pulverulent mixtures containing particles of sulfur.
US6749659 discloses a fertilizer granule comprising an elemental sulfur; swelling clay matrix, and at least one additional fertilizer material incorporated into said matrix. This disclosure is directed towards preparation of controlled release fertilizer granules but does not envisage a particularly high loading of elemental sulfur useful for pesticidal applications.
There has been a gradual shift in the art towards water dispersible granular formulations. These are formulations in granule form providing ready dispersibilty in water forming a suspension or a solution. These formulations are advantageous in avoiding a solvent, are non dusty, easily wettable, are free flowing and afford cheaper packaging. However, achieving a high dispersibility and quick wetting of such formulations with a high active content loading remains a challenge in the art. Water dispersible granular formulations also have an inherent disadvantage of comprising a higher amount of wetting and dispersing agents since the easy and quick formation of a suspension after dilution of the granules with water is crucial. However, this leads to an escalation of the formulation cost.
The present inventors have surprisingly found a selective relative proportion of the wetting and dispersing agents to facilitate a high loading of sulfur active ingredient.
Objects of the invention:
The present invention achieves at least one, preferably all, of the following mentioned advantages of the present invention.
One object of the present invention is to provide a high loaded water dispersible granular formulation of sulfur.
Another object of the present invention is to provide a water dispersible granular formulation of sulfur which is ecofriendly and higher bioeffectiveness.
Yet another object of the present invention is to provide a water dispersible granular formulation of sulfur which is compatible with fertilizers.

Summary of the invention
In one aspect, the present invention provides a water dispersible granular formulation comprising:
(a) sulfur in an amount of about 50% to about 95% by weight of the formulation;
(b) a first dispersing agent present in an amount of about 0.5% to about 15% by weight of the formulation, said dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene, ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates;
(c) a second dispersing agent present in an amount of about 0.5% to about 15% by total weight of the formulation, said second dispersing agent being selected from alkali or alkaline earth metal salts of lignosulfonate; and
(d) a wetting agent present in an amount of about 0.5% to about 15% by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; and
wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.545:0.5-15:0.5-15.
In another aspect, the present invention provides a process for the preparation of a water dispersible granular formulation comprising:
(a) admixing (i) sulfur in an amount of about 50% to about 95% by weight of the formulation; (ii) a first dispersing agent in an amount of about 0.5% to about 15% by weight of the formulation, said dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene, ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates; (iii) a second dispersing agent an amount of about 0.5% to about 15% by total weight of the formulation, said second dispersing agent being selected from alkali or alkaline earth

metal salts of lignosulfonate; and (iv) a wetting agent in an amount of about 0.5% to about 15% by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.5-15:0.5-15:0.5-15.; with a required quantity of water to form a slurry;
(b) wet grinding the slurry obtained in step (a) to a predetermined particle size;
(c) granulating the ground slurry of step (b); and
(d) sieving the granules obtaining to a predetermined particle size.
Detailed description of the invention
The present inventors have surprisingly found that it is possible to achieve a high loading of sulfur in the presence of a selective combination of a first dispersing agent, a second dispersing agent and a wetting agent present in a ratio of about 0.5-15:0.5-15:0.5-15..
Therefore, in one aspect, the present invention provides a water dispersible granular formulation comprising:
(a) sulfur in an amount of about 50% to about 95% by weight of the formulation;
(b) a first dispersing agent present in an amount of about 1% to about 10% by weight of the formulation, said dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene, ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates;
(c) a second dispersing agent present in an amount of about 0.5% to about 15% by total weight of the formulation, said second dispersing agent being selected from alkali or alkaline earth metal salts of lignosulfonate; and
(d) a wetting agent present in an amount of about 0.5 to about 15% by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; and

wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.5-15: 0.5-15: 0.5-15.
In an embodiment, sulfur active ingredient is present in an amount of about 80% by weight of the formulation.
In another embodiment, the first dispersing agent is present in an amount of about 0.5 -15 % by weight of the formulation.
In another embodiment, the first dispersing agent is selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene and ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates.
In another embodiment, the first dispersing agent is sodium salt of naphthalene condensate sulfonate.
In an embodiment, the second dispersing agent is present in an amount of about 0.5 -15% by total weight of the formulation.
In yet another embodiment, the second dispersing agent is sodium lignosulfonate.
In an embodiment, the first dispersing agent, the second dispersing agent and the wetting agent is present in a ratio of about 0.5-15: 0.5-15: 0.5-15..
Therefore, in a preferred embodiment, the present invention provides a water dispersible granular formulation comprising:
(a) sulfur in an amount of about 80% by weight of the formulation;
(b) a first dispersing agent present in an amount of about 0.5 - 15% by weight of the formulation, said first dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene and ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates;
(c) a second dispersing agent present in an amount of about 0.5 - 15% by total weight of the formulation, said second dispersing agent being sodium lignosulfonate; and

(d) a wetting agent present in an amount of about 0.5 - 15%by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; and
wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.5-15: 0.5-15: 0.5-15.
In another aspect, the present invention provides a process for the preparation of a water dispersible granular formulation comprising;
(a) admixing (i) sulfur in an amount of about 50% to about 95% by weight of the formulation; (ii) a first dispersing agent in an amount of about 0.5% to about 15% by weight of the formulation, said dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene, ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates; (iii) a second dispersing agent an amount of about 0.5% to about 15% by total weight of the formulation, said second dispersing agent being selected from alkali or alkaline earth metal salts of lignosulfonate; and (iv) a wetting agent in an amount of about 0.5% to about 15% by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.5-15:0.5-15:0.5-15; with a required quantity of water to form a slurry;
(b) wet grinding the slurry obtained in step (a) to a predetermined particle size;
(c) granulating the ground slurry of step (b); and
(d) sieving the granules obtaining to a predetermined particle size.
In an embodiment, the desired quantities of sulfur, first dispersing agent, second dispersing agent and wetting agent are admixed to obtain a homogenous blend.

In another embodiment, sulfur active ingredient is blended in an amount of about 80% by weight of the formulation.
In another embodiment, the first dispersing agent is blended in an amount of about 0.5-15% by weight of the formulation.
In another embodiment, the first dispersing agent is selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene and ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates.
In another embodiment, the first dispersing agent is sodium salt of naphthalene condensate sulfonate.
In an embodiment, the second dispersing agent is blended in an amount of about 0.5% to about 15%o by total weight of the formulation.
In yet another embodiment, the second dispersing agent is sodium lignosulfonate.
In an embodiment, the first dispersing agent, the second dispersing agent and the wetting agent is blended in a ratio of about 0.5 -15:0.5-15:0.5-15
In an embodiment, the quantity of water used to prepare the slurry is not particularly limiting and may be conveniently selected by a skilled artisan.
In an embodiment, the blend obtained in step(a) is wet grinded to reduce the particles to a predetermined particle size.
The choice of the wet grinding apparatus is not particularly limiting and may be conveniently selected by a skilled artisan from roll crushers, hammer mills, shredders and other similar devices which are conventionally known in the art.
In an embodiment, the blend particles are wet grinded to a particle size between 1.0 microns to about 40.0 microns.
In an embodiment, the wet grinded slurry is preferably granulated by using a conventionally known dryer with granulator machine. The granulated material is

thereafter sieved to obtain particles having a predetermined particle size of between 0.05 mm to about 1.5 mm.
The sieved particulate material is then packed into suitable bags for commerce.
Therefore, in one preferred embodiment, the present invention also provides a process for the preparation of a water dispersible granular formulation comprising:
(a) blending (i) sulfur in an amount of about 80% by weight of the formulation; (ii) a first dispersing agent in an amount of about 0.5% to about 15% by weight of the formulation, said first dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene and ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates; (iii) a second dispersing agent in an amount of about 0.5% to about 15% by total weight of the formulation, said second dispersing agent being sodium lignosulfonate; and (iv) a wetting agent in an amount of about 0.5% to about 15% by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.5 -15:0.5-15:0.5-15; with a required quantity of water to form a slurry;
(b) wet grinding the slurry obtained in step (a) to a particle size between 1.0 microns to about 40.0 microns;
(c) granulating the ground slurry of step (b);
(d) sieving the granules obtaining to a particle size between 0.05 mm to about 1.5 mm; and
(e) packing the granules into suitable bags.

Example:
80 g of sulfur active ingredient of about 99.0% purity was taken and blended with 0.5 - 15.0 g naphthalene sulfonate, 0.5 - 15.0 sodium lignosulfonate and 0.5 ~ 15.0g of sodium formaldehyde naphthalene condensate in a reactor. An appropriate amount of water was added and mixture blended for about 1 hour to make a slurry. The slurry was wet grinded to a desired particle size. The slurry was passed through a granulator to prepare granules of desired particle size. The granules were passed through a sieve to segregate particles of a uniform size and collected and packed. The composition details were as hereunder:

Component Name Content (% w/w)
Active ingredient Sulfur 80.00
Inert Ingredients Napthelene condensate 0.5-15%
Sodium Lignosulfonate 0.5-15%
Formaledehyde condensate 0.5-15%
Total 100.00%
Advantages of one or more embodiments of the invention
The formulation enabled a high loading of sulfur active ingredient with superior
dispersibility, Wettability & Suspensibility.
The formulation has enhanced bioefficacy for control of diseases caused by various
fungus and mites on different crops
The formulation enables control wide spectrum of fungal diseases on various crops.
The formulation is compatible with conventional fertilizers.
The formulation was found to be an effective fungicide.
The invention has been described above with reference to the specific examples. It should be noted that the example appended above illustrates rather than limits the invention and that those skilled in the art will be able to design many alternative embodiments without departing from the scope of the appended claims. Other than in the operating examples provided hereinbefore or where otherwise indicated, all numbers expressing quantities of ingredients or reaction conditions are to be understood as being modified in all instances by the term "about".

We Claim:
1. A water dispersible granular formulation comprising:
(a) sulfur in an amount of about 50% to about 95% by weight of the formulation;
(b) a first dispersing agent present in an amount of about 0.5% to about 15% by weight of the formulation, said dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene, ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates;
(c) a second dispersing agent present in an amount of about 0.5% to about 15% by total weight of the formulation, said second dispersing agent being selected from alkali or alkaline earth metal salts of lignosulfonate; and
(d) a wetting agent present in an amount of about 0.5% to about 15% by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; and
wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.5-15:0.5-15:0.5-15.
2. The formulation as claimed in claim 1, wherein the first dispersing agent, the second dispersing agent and the wetting agent are present in a ratio of about 0.5-15 : 0.5-15 : 0.5-15.
3. The formulation as claimed in claim 1 or claim 2, wherein the sulfur active ingredient is present in an amount of about 80% by weight of the formulation.
4. The formulation as claimed in any one of the preceding claims, wherein the first dispersing agent is present in an amount of about 0.5% - 15% by weight of the formulation.
5. The formulation as claimed in any one of the preceding claims, wherein the first dispersing agent is selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene

and ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates.
6. The formulation as claimed in claim 5, wherein the first dispersing agent is sodium salt of naphthalene condensate sulfonate.
7. The formulation as claimed in any one of the preceding claims, wherein the second dispersing agent is present in an amount of about 0.5% - 15% by total weight of the formulation.
8. The formulation as claimed in any one of the preceding claims, wherein the second dispersing agent is sodium lignosulfonate.
9. A water dispersible granular formulation comprising:

(a) sulfur in an amount of about 80% by weight of the formulation;
(b) a first dispersing agent present in an amount of about 0.5% -15% by weight of the formulation, said first dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene and ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates;
(c) a second dispersing agent present in an amount of about 0.5% - 15% by total weight of the formulation, said second dispersing agent being sodium lignosulfonate; and
(d) a wetting agent present in an amount of about 0.5% - 15%by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; and wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.5-15: 0.5-15: 0.5 -15.
10. A process for the preparation of a water dispersible granular formulation, said process
comprising:
(a) admixing (i) sulfur in an amount of about 85% to about 95% by weight of the formulation; (ii) a first dispersing agent in an amount of about 0.5% to about 15% by weight of the formulation, said dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of

condensed naphthalene, alkali or alkaline earth metal salts of sulfonated naphthalene, ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates; (iii) a second dispersing agent an amount of about 0.5% to about 15% by total weight of the formulation, said second dispersing agent being selected from alkali or alkaline earth metal salts of lignosulfonate; and (iv) a wetting agent in an amount of about 0.5% to about 15% by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.5-15:0.5-15:0.5-15; with a required quantity of water to form a slurry;
(b) wet grinding the slurry obtained in step (a) to a predetermined particle size;
(c) granulating the ground slurry of step (b); and
(d) sieving the granules obtaining to a predetermined particle size.

11. The process as claimed in claim 10, wherein the blend particles are wet grinded to a particle size between 1.0 microns to about 40.0 microns.
12. The process as claimed in claim 10 or claim 11, wherein the granulated material is sieved to obtain particles having a particle size of between 0.05mm to about 1.5 mm.
13. The process as claimed in claims 10-13 additionally comprising packing the formulation obtained into suitable bags.
14. A process for the preparation of a water dispersible granular formulation, said process comprising:
(a) blending (i) sulfur in an amount of about 80% by weight of the formulation; (ii) a first dispersing agent in an amount of about 5% by weight of the formulation, said first dispersing agent being selected from phenyl naphthalene sulfonates, sulfonates of condensed naphthalene, alkali or alkaline earth metal salts of .sulfonated naphthalene and ammonium salts of sulfonated naphthalene and alkali or alkaline earth metal salts of alkyl naphthalene sulfonates; (iii) a

second dispersing agent in an amount of about 0.5% to about 15% by total weight of the formulation, said second dispersing agent being sodium lignosulfonate; and (iv) a wetting agent in an amount of about 0.5% to about 15% by total weight of the formulation, said wetting agent being selected from aryl sulfonic acid formaldehyde condensate, aralkyl sulfonic acid formaldehyde condensate and naphthalene formaldehyde condensate; wherein said first dispersing agent, said second dispersing agent and said wetting agent are present in a ratio of about 0.5 -15:0.5-15: 0.5-15 with a required quantity of water to form a slurry;
(b) wet grinding the slurry obtained in step (a) to a particle size between 1.0 microns to about 40.0 microns;
(c) granulating the ground slurry of step (b);
(d) sieving the granules obtaining to a particle size between 0.05 mm to about 1.5 mm; and
(e) packing the granules into suitable bags.

15. A water dispersible granular formulation substantially as described herein with reference to the accompanying example.
16. A process for the preparation of a water dispersible granular formulation substantially as described herein with reference to the accompanying example.