DESC:FORM 2

THE PATENTS ACT 1970
(SECTION 39 OF 1970)

&

THE PATENT RULES, 2003

COMPLETE SPECIFICATION
(Section 10 and Rule 13)

A SYNERGISTIC FUNGICIDAL SUSPENSION CONCENTRATE COMPRISING BOSCALID

We, COROMANDEL INTERNATIONAL LIMITED,
an Indian company incorporated under the Companies Act, 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 THE INVENTION
The present invention relates to a synergistic fungicidal composition of Boscalid. The composition finds use in preventing and/or treating fungal infestations in plants and plant parts. Particularly the present invention relates to a synergistic fungicidal suspension concentrate comprising Boscalid and other agrochemical auxiliaries.

The present invention specifically relates to suspension concentrate (SC) comprising crystalline Boscalid, with one or more agrochemical auxiliaries.

The present invention specifically relates to suspension concentrate (SC) comprising boscalid crystalline anhydrate modification I with one or more wetting agents, dispersing agents, antifreezing agents, biocide, viscosity modifier, buffering agent, defoamer and a solvent.

The present invention also specifically relates to suspension concentrate (SC) comprising boscalid crystalline anhydrate modification II, with one or more wetting agents, dispersing agents, antifreezing agents, biocide, viscosity modifier, buffering agent, defoamer and a solvent.

BACKGROUND OF THE INVENTION
In many horticultural and agricultural applications, plant growth regulators (growth inhibitors or growth stimulants) are applied for a variety of reasons. For example, it can be useful to increase the speed of growth, increase root formation, seedling setting and the like. It may also be useful to reduce growth to have short stems in grain culturing, reduce seed formation in citrus fruits and the like.

In many horticultural and agricultural applications, fungicides are regularly applied, to combat diseases caused by fungi. Many of the growth regulators, insecticides, fungicides, herbicides, and the like are applied on the crop by spraying in a diluted solution in water.

Generally, the farmer appreciates to use concentrated products, like liquid formulations that can easily be admixed with water to result in homogeneous mixtures without additional process steps. Furthermore, often, a farmer wants to apply several active compounds in one spray run. Hence, active compounds are generally supplied as concentrated liquids.

Boscalid is a systemic fungicide chemically known as (2-chloro-N- (4'chloro [1,1'biphenyl] -2-yl) -3-pyridinecarboxamide was first described in US5330995. It is commercially available in a range of formulations for the treatment of fungal infestations.

US7087239B2 describes Boscalid anhydrate and hydrate forms. The known anhydrate form of Boscalid is having a melting point ranges from 144-145oC and referred as modification I.

US7501384B2 describes Boscalid crystalline anhydrate modification II having a melting point ranges from 147-148?.

US7087239B2 describes crystalline hydrates of Boscalid, especially monohydrate crystalline form of Boscalid.

The present invention discloses that the suspension concentrate (SC) of crystalline Boscalid shows a synergistic activity, and this stable liquid composition can be prepared from crystalline Boscalid by adding additional agrochemical auxiliaries.

Surprisingly, it was found that the suspension concentrate (SC) of crystalline Boscalid shows a synergistic activity and efficacy when compared to other type of Boscalid formulations.

OBJECT OF THE INVENTION
One object of the present invention provides synergistic fungicidal suspension concentrate (SC) comprising crystalline Boscalid.

Another object of the present invention provides suspension concentrate (SC) comprising crystalline Boscalid with one or more wetting agents, dispersing agents, antifreezing agents, biocide, viscosity modifier, buffering agent or salt, defoamer and a solvent.

In yet another object of the present invention provides process for the preparation of Boscalid suspension concentrate (SC) comprising the steps of preparing aqueous slurry, wet milling, and gelling of wet milled slurry.

SUMMARY OF THE INVENTION
One aspect of the present invention provides synergistic fungicidal suspension concentrate (SC) comprising crystalline Boscalid.

Another aspect of the present invention provides suspension concentrate (SC) comprising crystalline Boscalid with one or more wetting agents, dispersing agents, antifreezing agents, biocide, viscosity modifier, buffering agent or a salt, defoamer and a solvent.

Another aspect of the present invention provides suspension concentrate (SC) comprising boscalid crystalline anhydrate modification I, with one or more wetting agents, dispersing agents, antifreezing agents, biocide, viscosity modifier, buffering agent or salt, defoamer and a solvent.

Another aspect of the present invention provides suspension concentrate (SC) comprising boscalid crystalline anhydrate modification II, with one or more wetting agents, dispersing agents, antifreezing agents, biocide, viscosity modifier, buffering agent or salt, defoamer and a solvent.

Yet another aspect of the present invention provides suspension concentrate (SC) comprising:
a) crystalline Boscalid in the range of 40 to 50% (w/w),
b) wetting agent in the range of 1% to 5% (w/w),
c) dispersing agent in the range of 1% to 5% (w/w),
d) antifreezing agent in the range of 1% to 40% (w/w),
e) biocide in the range of 0.1% to 0.5% (w/w),
f) buffering agent or salt in the range of 1% to 2% (w/w),
g) viscosity modifier in the range of 1% to 5% (w/w),
h) defoamer in the range of 0.1% to 1% (w/w), and
i) solvent in the range of 10% to 50% (w/w).

In yet another aspect of the present invention provides suspension concentrate (SC) comprising:
a) Boscalid crystalline anhydrate modification II in an amount of 50% (w/w),
b) polymethyl methacrylate-polyethylene glycol graft copolymer in an amount of 1.5% (w/w),
c) phosphoric acid esters of ethoxylated tristyryl phenol in an amount of 2% (w/w),
d) glycerol in an amount of 30% (w/w),
e) 1,2-benzisothiazol-3(2H)-one in an amount of 0.1% (w/w),
f) citric acid in an amount of 1% (w/w),
g) xanthan gum in an amount of 2% (w/w),
h) polydimethylsiloxane antifoam emulsion in an amount of 0.5% (w/w), and
i) water in an amount of 12.9% (w/w).

In yet another aspect of the present invention provides process for the preparation of Boscalid suspension concentrate (SC) comprising the steps of preparing aqueous slurry, wet milling, and gelling of wet milled slurry.

In yet another aspect of the present invention provides process for the preparation of Boscalid suspension concentrate (SC) comprising the steps of:
a) preparing an aqueous slurry by mixing antifreezing agent, wetting agent, dispersing agent, biocide, defoamer, solvent and buffering agent or salt in a pre-mixer.
b) adding crystalline Boscalid with stirring to from homogenized aqueous slurry,
c) wet milling the obtained slurry by passing through dyno-mill at a temperature less than 30oC, and
d) gelling the obtained wet milled slurry by adding viscosity modifying agent, and
e) stirring the mixture for 2 hours to from homogenized suspension concentrates.

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.

One embodiment of the present invention provides a synergistic fungicidal suspension concentrate (SC) comprising crystalline Boscalid.

Another embodiment of the present invention provides suspension concentrate (SC) comprising crystalline Boscalid, with one or more wetting agents, dispersing agents, antifreezing agents, biocide, viscosity modifier, buffering agent or salt, defoamer and a solvent.

Yet another embodiment of the present invention provides suspension concentrate (SC) comprising:
a) crystalline Boscalid in the range of 40 to 50% (w/w),
b) wetting agent in the range of 1% to 5% (w/w),
c) dispersing agent in the range of 1% to 5% (w/w),
d) antifreezing agent in the range of 1% to 40% (w/w),
e) biocide in the range of 0.1% to 0.5% (w/w),
f) buffering agent or salt in the range of 1% to 2% (w/w),
g) viscosity modifier in the range of 1% to 5% (w/w),
h) defoamer in the range of 0.1% to 1% (w/w), and
i) solvent in the range of 10% to 50% (w/w).

In yet another embodiment of the present invention provides suspension concentrate (SC) comprising:
a) Boscalid crystalline anhydrate modification II in an amount of 50% (w/w),
b) polymethyl methacrylate-polyethylene glycol graft copolymer in an amount of 1.5% (w/w),
c) phosphoric acid esters of ethoxylated tristyryl phenol in an amount of 2% (w/w),
d) glycerol in an amount of 30% (w/w),
e) 1,2-Benzisothiazol-3(2H)-one in an amount of 0.1% (w/w),
f) Citric acid in an amount of 1% (w/w),
g) Xanthan gum in an amount of 2% (w/w),
h) Polydimethylsiloxane antifoam emulsion in an amount of 0.5% (w/w), and
i) water in an amount of 12.9% (w/w).

According to the present invention the crystalline Boscalid may be selected from crystalline anhydrate modification I, crystalline anhydrate modification II and crystalline monohydrate, preferably crystalline anhydrate modification II.

The wetting agent is a compound that facilitates rapid wetting of the powder when added to the water. The wetting agent employed in the formulation composition is selected from the group consisting of non-ionic surfactants, anionic surfactant and a mixture of anionic and non-ionic surfactant and polymeric surfactant.

The wetting agent as used herein is selected from and not limited to a blend of anionic and nonionic surfactants (Atlox 5406B), polyoxyethylene alkyl ether (Atlox-4894), polymethyl methacrylate-polyethylene glycol graft copolymer (ATLOX-4913), fatty alcohol ethoxylate (TERSPERSE 4894), di alkyl naphthalene sulphonate sodium salt (SUPRAGIL WP), ethoxylated TSP-phosphate ester (AGRILAN 1015), polymeric emulsifier (ATLAS G-5002L), polycondensation product of naphthalene sulfonic acid, which is alkyl Naphthalene sulphonate sodium salt, Polyalkyl Naphthalene sulphonate, alkyl Naphthalene sulphonate (GEROPON DA 1349); Aqarius BP14332 Yellow IH, salts of alkylphenol condensates, salts of sulphonated lignins, salts of poly acid resin copolymers, salts of polyphenol formaldehyde resins, phosphoric acid esters of ethoxylated tristyryl phenol (SOPROPHOR 3D44), amine salt of polyaryl phenyl ether phosphate (SOPROPHOR FL), Triethanol ammonium salt of tristyryl phenyl ether phosphate (UNITOP FL), alkoxylated alkylphenols and alcohols as well as block copolymers of ethylene oxide and propylene oxide. Preferred wetting agents are polyoxyethylene alkyl ether (Atlox-4894), ethoxylated TSP-phosphate ester (AGRILAN 1015), Polyalkyl Naphthalene sulphonate, alkyl Naphthalene sulphonate (GEROPON DA 1349), phosphoric acid esters of ethoxylated tristyryl phenol (SOPROPHOR 3D44), and amine salt of poly aryl phenyl ether phosphate (SOPROPHOR FL), Triethanol ammonium salt of tristyryl phenyl ether phosphate (UNITOP FL).

The wetting agent used in the proposed composition in a range of about 1 to 10% (w/w), more preferably 1 to 5% (w/w) of the total weight of the composition.

The dispersing agent is a compound which ensures that the particles remain suspended in water. The dispersing agent can be ionic or non-ionic or a mixture of such surface-active agents or graft co-polymer dispersant.

The dispersing agents as used herein is selected from sodium lignosulphonates; sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenol ethoxylate phosphate esters; aliphatic alcohol ethoxylates; alkyl ethoxylates (GERONOL SCR); Polyoxyethylene-Polyoxypropylene Block Polymer (UNITOP 203), EO-PO Polymeric dispersant (TERSPERSE 2288); polyoxy alkylene glycol butyl ether (ETHYLANE NS 500 LQ), Polyalkyl Naphthalene sulphonate, alkyl Naphthalene sulphonate (GEROPON DA 1349), phosphoric acid esters of ethoxylated tristyryl phenol (SOPROPHOR 3D44), dispersant (Atlox METASPERSE 500L) and graft copolymers, polycarboxylates, alkyl naphthalene sulfonates (such as MORWET IP, MORWET EFW, MORWET 3028), sodium salt of naphthalene sulfonate condensate (MORWET D-425), phenol sulphonic acid condensates, alkyl sulfonates, alkenyl sulfonates, mixture of alkyl sulfonates and alkenyl sulfonates (LISSAPOL D), alkyl sulfosuccinates (GEROPON), L-Wet, methyl oleyltaurates, Polyethylene glycol 2,4,6-tris(1-phenylethyl)phenyl ether sulfate ammonium salt (SOPROPHOR 4D384) and poly vinyl alcohols. Preferred dispersing agents are polymethyl methacrylate-polyethylene glycol graft copolymer (Atlox-4913), Polyoxyethylene-Polyoxypropylene Block Polymer (UNITOP 203), Polyethylene glycol 2,4,6-tris(1-phenylethyl)phenyl ether sulfate ammonium salt (SOPROPHOR 4D384), polyoxy alkylene glycol butyl ether (ETHYLANE NS 500 LQ), Polyalkyl Naphthalene sulphonate, alkyl Naphthalene sulphonate (GEROPON DA 1349), and phosphoric acid esters of ethoxylated tristyryl phenol (SOPROPHOR 3D44).

The dispersing agent is present in the proposed composition in a range of about 1 to 10% (w/w) more preferably 1 to 5% (w/w) of the total weight of the composition.

The antifreezing agent as used herein is selected from ethylene glycol, propylene glycol, glycerol, or urea. Preferred antifreezing agents are ethylene glycol and glycerol.

The antifreezing agent used in the proposed composition in a range of about 1 to 50% (w/w), more preferably 1% to 40% (w/w) of the total weight of the composition.

The biocide as used herein is selected from Proxel GXl and Nipacide® BIT 20 which is a formaldehyde-free, in-can biocide based on benzisothiazolinone (BIT). Preferred biocide is Nipacide BIT 20.

The biocide in the proposed composition in a range of about 0.1 to 1%(w/w), more preferably 0.1 to 0.5 %(w/w) of the total weight of the composition.

The defoamer as used herein is selected from absorbed polydimethyl siloxane (Sag-1572), stearates; silicones and ethoxylates. Preferred defoamer is polydimethyl siloxane (Sag-1572).

The defoamer used in the proposed composition in a range of about 0.1 to 5% (w/w), more preferably 0.1 to 1% (w/w) of the total weight of the composition.

The viscosity modifying agent as used herein include all substances which can normally be used for this purpose in agrochemical compositions. For example, xanthan gum, Rhodopol gel (2%), PVOH, cellulose and its derivatives, clay hydrated silicates, magnesium aluminum silicates or a mixture thereof. Preferred viscosity modifying agent is xanthan gum.

The viscosity modifying agent used in the proposed composition in a range of about 1 to 10% (w/w), more preferably 1 to 5% (w/w) of the total weight of the composition.

The buffering agent or salt as used herein is citric acid and the solvent used is distilled water.

The buffering agent used in the proposed composition in a range of about 1 to 10% (w/w), more preferably 1 to 2% (w/w) of the total weight of the composition.

The solvent used in the proposed composition in a range of about 1 to 60% (w/w), more preferably 10 to 50% (w/w) of the total weight of the composition.

Yet another embodiment of the present invention provides a process for the preparation of Boscalid suspension concentrate (SC) comprising the steps of:
a) preparing an aqueous slurry of antifreezing agent, wetting agent, dispersing agent, biocide, defoamer, solvent and buffering agent or salt,
b) adding crystalline Boscalid to from homogenized aqueous slurry,
c) wet milling the obtained slurry in step (b) at less than 30oC to get wet milled slurry,
d) gelling the wet milled slurry by adding viscosity modifying agent, and
e) stirring the mixture for 2 hours to get Boscalid suspension concentrates.

According to the present invention, prepared an aqueous slurry of antifreezing agent, wetting agent, dispersing agent, biocide, defoamer, solvent and buffering agent in a pre-mixer at 20-30oC. crystalline Boscalid is added under stirring at same temperature to get homogeneous suspension. Wet milling the homogeneous suspension at less than 30oC, followed by gelling with viscosity modifying agent and stirring to get Boscalid suspension concentrate. According to the present invention, the antifreezing agent is selected from ethylene glycol and glycerol.

The further embodiment of the present invention is illustrated by the following examples, which are provided merely to be exemplary of the inventions and is not intended to limit the scope of the invention. Certain modifications and equivalents will be apparent to those skilled in the art and are intended to be included within the scope of the present invention.

EXAMPLES: Boscalid 50% suspension concentrates (SC) formulation:

EXAMPLES:
Boscalid 50% suspension concentrate (SC) formulation:
Example-1:
A suspension concentrate formulation of boscalid comprising 50% (w/w) of boscalid crystalline anhydrate modification I (Purity: 98%) as an active ingredient, 1.5% (w/w) of polymethyl methacrylate-polyethylene glycol graft copolymer (GEROPON DA 1349) as wetting or dispersing agent, 2.0% (w/w) of phosphoric acid esters of ethoxylated tristyryl phenol (SOPROPHOR 3D44) as wetting or dispersing agent, 30% (w/w) of glycerol as antifreezing agent, 0.1% (w/w) of 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) as a biocide, 1% (w/w) of citric acid as a salt, 2 % (w/w) xanthan gum (AG-RHO POL 23/W ( 2%) as viscosity modifier, 0.5% (w/w) of polydimethylsiloxane antifoam emulsion (Sag-1572) as a defoamer, and 11.8% (w/w) of distilled water as a solvent.

S. No. Ingredients Quantity (in %w/w)
1. Boscalid crystalline anhydrate modification I (Purity: 98%) 51.02
2. Polymethyl methacrylate-polyethylene glycol graft copolymer
(GEROPON DA 1349) 1.5
3. Phosphoric acid esters of ethoxylated tristyryl phenol
(SOPROPHOR 3D44) 2.0
4. Glycerol 30
5. 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) 0.1
6. Citric acid 1.0
7. Xanthan gum (AG-RHO POL 23/W ( 2%) 2.0
8. Polydimethylsiloxane antifoam emulsion (Sag-1572) 0.5
9. Distilled water 11.8
Total 100

Manufacturing process:

Step 1: Preparation of Aqueous Slurry
30 parts by weight of glycerol taken in vessel no. 1 (Pre-mixer). To this 1.5 parts by weigh of GEROPON DA 1349, 2 parts by weigh SOPROPHOR 3D44 were added. After 15 min add 0.1 parts by weight of Nipacide BIT-20 followed by 0.5 parts of SAG 1572 and 1.0 part of citric acid. Then after 15 mins distilled water was added under stirring. The mixture was stirred for 15 mins and then boscalid technical was added. The mixture was stirred for homogenization (The mixture should be thoroughly homogenized).

Step 2: Wet Milling of Slurry
The wet slurry from vessel No.1 was passed through Dyno-Mill at a temperature below 30°C and material was collected in vessel no.2 (post-mixer). Continuous stirring was maintained in both the vessels to avoid the sedimentation. The Particle Size distribution (PSD) of the sample was checked. The PSD of the material should be d90 < 15 µ. If the d90 is higher than > 15 µ then grind the mixture till the PSD value complies the specification.

Step 3: Gelling of Wet Milled Slurry
Required quantity of xanthan gum was added to the wet slurry in vessel no.2 and stirred for 3 hrs for homogenization. The sample was checked for complete analysis and packed in designated bottles.

Example-2:
A suspension concentrate comprising of 50% (w/w) Boscalid crystalline anhydrate modification II (Purity: 98%) as an active ingredient, 1.5% (w/w) of polymethyl methacrylate-polyethylene glycol graft copolymer (GEROPON DA 1349) as a wetting or dispersing agent, 2.0% (w/w) of phosphoric acid esters of ethoxylated tristyryl phenol (SOPROPHOR 3D44) as wetting or dispersing agent, 30% (w/w) of glycerol as antifreezing agent, 0.1% (w/w) of 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) as a biocide, 1% (w/w) of citric acid as a salt, 2 % (w/w) xanthan gum (AG-RHO POL 23/W ( 2%) as viscosity modifier, 0.5% (w/w) of polydimethylsiloxane antifoam emulsion (Sag-1572) as a defoamer, and 11.8% (w/w) of distilled water as a solvent.
S. No. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification II 50.0
2. Polymethyl methacrylate-polyethylene glycol graft copolymer
(GEROPON DA 1349) 1.5
3. Phosphoric acid esters of ethoxylated tristyryl phenol
(SOPROPHOR 3D44) 2.0
4. Glycerol 30.0
5. 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) 0.1
6. Citric acid 1.0
7. Xanthan gum (AG-RHO POL 23/W ( 2%) 2.0
8. Polydimethylsiloxane antifoam emulsion (Sag-1572) 0.5
9. Distilled water 12.9
Total 100

Manufacturing process:
Step 1: Preparation of Aqueous Slurry
30 parts by weight of glycerol taken in vessel no. 1 (Pre-mixer). To this 1.5 parts by weigh of GEROPON DA 1349, 2 parts by weigh SOPROPHOR 3D44 were added. After 15 min add 0.1 parts by weight of Nipacide BIT-20 followed by 0.5 parts of SAG 1572 and 1.0 part of citric acid. Then after 15 mins distilled water was added under stirring. The mixture was stirred for 15 mins and then Boscalid technical was added. The mixture was stirred for homogenization (The mixture should be thoroughly homogenized).

Step 2: Wet Milling of Slurry
The wet slurry from vessel No.1 was passed through Dyno-Mill at a temperature below 30°C and material was collected in vessel no.2 (post-mixer). Continuous stirring was maintained in both the vessels to avoid the sedimentation. The Particle Size distribution (PSD) of the sample was checked. The PSD of the material should be d90 < 15 µ. If the d90 is higher than > 15 µ then grind the mixture till the PSD value complies the specification.

Step 3: Gelling of Wet Milled Slurry
Required quantity of xanthan gum was added to the wet slurry in vessel no.2 and stirred for 3 hrs for homogenization. The sample was checked for complete analysis and packed in designated bottles.

Example-3:
A suspension concentrate formulation comprising 50% (w/w) of Boscalid crystalline anhydrate modification II (Purity: 98%) as an active ingredient, 2.0% (w/w) ethoxylated TSP-phosphate ester (AGRILAN 1015) as wetting or dispersing agent, 2.0% (w/w) polyoxy alkylene glycol butyl ether (ETHYLANE NS 500 LQ) as dispersing agent, 20.0 (w/w) of ethylene glycol as antifreezing agent, 1% (w/w) of 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) as a biocide, 2.0% (w/w) xanthan gum (AG-RHO POL 23/W ( 2%) as viscosity modifier, 0.5% (w/w) of Polydimethylsiloxane antifoam emulsion (Sag-1572) as a defoamer, and 22.38 (w/w) gm of distilled water as a solvent.
S. No. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification II 50.0
2. Ethoxylated TSP-phosphate ester (AGRILAN 1015) 2.0
3. Polyoxy alkylene glycol butyl ether (ETHYLANE NS 500 LQ) 2.0
4. Ethylene glycol 20.0
5. 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) 0.1
6. Xanthan gum (AG-RHO POL 23/W ( 2%) 2.0
7. Polydimethylsiloxane antifoam emulsion (Sag-1572) 0.5
8. Distilled water 23.4
Total 100

Manufacturing process:
Step 1: Preparation of Aqueous Slurry
20 parts by weight of ethylene glycol taken in vessel no. 1 (Pre-mixer). To this 2.0 parts by weigh of AGRILAN 1015, 2 parts by weigh ETHYLANE NS 500 LQ were added. After 15 min add 0.1 parts by weight of Nipacide BIT-20 followed by 0.5 parts of SAG 1572. Then after 15 mins distilled water was added under stirring. The mixture was stirred for 15 mins and then Boscalid technical was added. The mixture was stirred for homogenization (The mixture should be thoroughly homogenized).

Step 2: Wet Milling of Slurry
The wet slurry from vessel No.1 was passed through Dyno-Mill at a temperature below 30°C and material was collected in vessel no.2 (post-mixer). Continuous stirring was maintained in both the vessels to avoid the sedimentation. The Particle Size distribution (PSD) of the sample was checked. The PSD of the material should be d90 < 15 µ. If the d90 is higher than > 15 µ then grind the mixture till the PSD value complies the specification.

Step 3: Gelling of Wet Milled Slurry
Required quantity of xanthan gum was added to the wet slurry in vessel no.2 and stirred for 3 hrs for homogenization. The sample was checked for complete analysis and packed in designated bottles.

Example-4:
A suspension concentrate formulation of Boscalid comprising 50% (w/w) of Boscalid crystalline anhydrate modification II (Purity: 98%) as an active ingredient, 2.0% (w/w) amine salt of poly aryl phenyl ether phosphate (SOPROPHOR FL) as wetting agent, 2.0% (w/w) phosphoric acid esters of ethoxylated tristyryl phenol (SOPROPHOR 3D44) as dispersing agent, 25% (w/w) of ethylene glycol as antifreezing agent, 0.1% (w/w) of 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) as a biocide, 1.0% (w/w) Xanthan gum (AG-RHO POL 23/W ( 2%) as viscosity modifier, 5% (w/w) of polydimethylsiloxane antifoam emulsion (Sag-1572) as a defoamer, and 18.3% (w/w) of distilled water as a solvent.
S. No. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification II 50.0
2. Amine salt of poly aryl phenyl ether phosphate (SOPROPHOR FL) 2.0
3. Phosphoric acid esters of ethoxylated tristyryl phenol (SOPROPHOR 3D44) 2.0
4. Ethylene glycol 25.0
5. 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) 0.1
6. Xanthan gum (AG-RHO POL 23/W ( 2%) 1.0
7. Polydimethylsiloxane antifoam emulsion (Sag-1572) 0.5
8. Distilled water 19.4
Total 100

Manufacturing process:
Step 1: Preparation of Aqueous Slurry
25 parts by weight of ethylene glycol taken in vessel no. 1 (Pre-mixer). To these 2 parts by weigh of SOPROPHOR FL, 2 parts by weigh SOPROPHOR 3D44 were added. After 15 min add 0.1 parts by weight of Nipacide BIT-20 followed by 0.5 parts of SAG 1572. Then after 15 mins distilled water was added under stirring. The mixture was stirred for 15 mins and then Boscalid technical was added. The mixture was stirred for homogenization (The mixture should be thoroughly homogenized).

Step 2: Wet Milling of Slurry
The wet slurry from vessel No.1 was passed through Dyno-Mill at a temperature below 30°C and material was collected in vessel no.2 (post-mixer). Continuous stirring was maintained in both the vessels to avoid the sedimentation. The Particle Size distribution (PSD) of the sample was checked. The PSD of the material should be d90 < 15 µ. If the d90 is higher than > 15 µ then grind the mixture till the PSD value complies the specification.

Step 3: Gelling of Wet Milled Slurry
Required quantity of xanthan gum was added to the wet slurry in vessel no.2 and stirred for 3 hrs for homogenization. The sample was checked for complete analysis and packed in designated bottles.

Example-5:
A suspension concentrate formulation comprising 50% (w/w) of Boscalid crystalline anhydrate modification I (Purity: 98%) as an active ingredient, 1.5% (w/w) of Triethanol ammonium salt of tristyryl phenyl ether phosphate (UNITOP FL) as wetting agent, 1.5% (w/w) polyoxyethylene-polyoxypropylene block polymer (UNITOP 203) as dispersing agent, 30% (w/w) of ethylene glycol as antifreezing agent, 0.1% (w/w) of 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) as a biocide, 1.0% (w/w) Xanthan gum (AG-RHO POL 23/W ( 2%) as viscosity modifier, 0.5% (w/w) of polydimethylsiloxane antifoam emulsion (Sag-1572) as a defoamer, and 14.38 (w/w) of distilled water as a solvent.
S. No. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification II 50.0
2. Polyoxyethylene-polyoxypropylene block polymer (UNITOP 203) 1.5
3. Triethanol ammonium salt of tristyryl phenyl ether phosphate (UNITOP FL) 1.5
4. Ethylene glycol 30.0
5. 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) 0.1
6. Xanthan gum (AG-RHO POL 23/W ( 2%) 1.0
7. Polydimethylsiloxane antifoam emulsion (Sag-1572) 0.5
8. Distilled water 15.4
Total 100

Manufacturing process:
Step 1: Preparation of Aqueous Slurry
30 parts by weight of ethylene glycol taken in vessel no. 1 (Pre-mixer). To this 1.5 parts by weigh of UNITOP 203, 1.5 parts by weigh UNITOP FL were added. After 15 min add 0.1 parts by weight of Nipacide BIT-20 followed by 0.5 parts of SAG 1572. Then after 15 mins distilled water was added under stirring. The mixture was stirred for 15 mins and then Boscalid technical was added. The mixture was stirred for homogenization (The mixture should be thoroughly homogenized).

Step 2: Wet Milling of Slurry
The wet slurry from vessel No.1 was passed through Dyno-Mill at a temperature below 30°C and material was collected in vessel no.2 (post-mixer). Continuous stirring was maintained in both the vessels to avoid the sedimentation. The Particle Size distribution (PSD) of the sample was checked. The PSD of the material should be d90 < 15 µ. If the d90 is higher than > 15 µ then grind the mixture till the PSD value complies the specification.

Step 3: Gelling of Wet Milled Slurry
Required quantity of xanthan gum was added to the wet slurry in vessel no.2 and stirred for 3 hrs for homogenization. The sample was checked for complete analysis and packed in designated bottles.

Example-6:
A suspension concentrate formulation comprising 50% (w/w) of Boscalid crystalline anhydrate modification II (Purity: 98%) as an active ingredient, 1.5% (w/w) polyoxyethylene alkyl ether (Atlox-4894) as wetting agent, 1.5% (w/w) polymethyl methacrylate-polyethylene glycol graft copolymer (Atlox-4913) as dispersing agent, 5.0% (w/w) of ethylene glycol as antifreezing agent, 0.1% (w/w) of 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) as a biocide, 2.0% (w/w) xanthan gum (AG-RHO POL 23/W ( 2%) as viscosity modifier, 0.5% (w/w) of polydimethylsiloxane antifoam emulsion (Sag-1572) as a defoamer, and 38.3% (w/w) of distilled water as a solvent.
S. No. Ingredients Quantity (in %w/w)
1. Boscalid crystalline anhydrate modification II 50.0
2. Polyoxyethylene alkyl ether (Atlox-4894) 1.5
3. Polymethyl methacrylate-polyethylene glycol graft copolymer (Atlox-4913) 1.5
4. Ethylene glycol 5.0
5. 1,2-Benzisothiazol-3(2H)-one (Nipacide BIT 20) 0.1
6. Xanthan gum (AG-RHO POL 23/W ( 2%) 2.0
7. Polydimethylsiloxane antifoam emulsion (Sag-1572) 0.5
8. Distilled water 39.4
Total 100

Manufacturing process:

Step 1: Preparation of Aqueous Slurry
5 parts by weight of glycerol taken in vessel no. 1 (Pre-mixer). To this 1.5 parts by weigh of Atlox-4894, 1.5 parts by weigh Atlox-4913 were added. After 15 min add 0.1 parts by weight of Nipacide BIT-20 followed by 0.5 parts of SAG 1572. Then after 15 mins distilled water was added under stirring. The mixture was stirred for 15 mins and then Boscalid technical was added. The mixture was stirred for homogenization (The mixture should be thoroughly homogenized).

Step 2: Wet Milling of Slurry
The wet slurry from vessel No.1 was passed through Dyno-Mill at a temperature below 30°C and material was collected in vessel no.2 (post-mixer). Continuous stirring was maintained in both the vessels to avoid the sedimentation. The Particle Size distribution (PSD) of the sample was checked. The PSD of the material should be d90 < 15 µ. If the d90 is higher than > 15 µ then grind the mixture till the PSD value complies the specification.

Step 3: Gelling of Wet Milled Slurry
Required quantity of xanthan gum was added to the wet slurry in vessel no.2 and stirred for 3 hrs for homogenization. The sample was checked for complete analysis and packed in designated bottles.

SYNERGY STUDIES:

Efficacy study for Boscalid 50% in suspension concentrate (SC) form:
Trial 1: Bio-efficacy against Tomato Early blight:
Trials were conducted in randomized block design with net plot size of 5m x 6m. Tomato crops were raised with all standard agronomic practices. Spraying was done with manual operated backpack sprayer with 500 litre of water spray volume per hectare at 45 days after sowing. The observations were recorded by % disease control from ten plant. The observations were recorded before spraying and 05 DAA and 10 (days after application). The percent disease control was worked out by below formula:

Percent Disease Index (PDI) = Sum of all disease ratings X 100
Total no of assessments X Maximum disease grade

The field trials were conducted to evaluate the efficacy of different formulation of Boscalid 50% SC versus Boscalid 50% WP and Boscalid 50% WG formulations against tomato early blight.

Table 1: Early blight disease control in Tomato:
Compositions Dose (gram active per hectare) Percent disease control – Alternaria solani.
05 DAA 10 DAA
Boscalid 50% SC 150 90 84
Boscalid 50% WG 150 85 80
Boscalid 50% WP 150 82 78
SC – Suspension Concentrate, WP - Wettable Powder, WG – Wettable granule and DAA - Days after application.

The trial result shows there is a difference between the efficacy of three different formulations. Boscalid 50% SC provided excellent and longer duration control as compared to Boscalid 50 % WG and Boscalid 50% WP formulations against Early blight disease in tomato.

Trial 2: Bio-efficacy against Chilli Powdery mildew:
The field trials were conducted to evaluate the efficacy of different formulation of Boscalid 50% SC versus the existing Boscalid WP and WG formulations against Chili powdery mildew.

Table 2: Powdery mildew disease control in Chilli:
Compositions Dose (gram active per hectare) Percent disease control – Leveillula taurica
05 DAA 10 DAA
Boscalid 50% SC 150 85 81
Boscalid 50% WG 150 82 78
Boscalid 50% WP 150 78 75
SC – Suspension Concentrate, WP - Wettable Powder, WG – Wettable granular and DAA - Days after application.

The trial result shows there is a difference between the efficacy of three different formulations. Boscalid 50% SC provided excellent and longer duration control as compared to Boscalid 50 % WG and Boscalid 50% WP formulations against Powdery mildew disease in chilli.

Trial 3: Bio-efficacy against Onion purple blotch:
The field trials were conducted to evaluate the efficacy of different formulation of Boscalid 15% SC versus the Boscalid WP and WG formulations against onion purple blotch.

Table 3: Purple blotch disease control in Onion:
Compositions Dose (gram active per hectare) Percent disease control – Alternaria porri
05 DAA 10 DAA
Boscalid 50% SC 150 90 84
Boscalid 50% WG 150 88 81
Boscalid 50% WP 150 85 80
SC – Suspension Concentrate, WP - Wettable Powder, WG – Wettable granular and DAA - Days after application.

The trial result shows there is a difference between the efficacy of three different formulations. Boscalid 50% SC provided excellent and longer duration control as compared to Boscalid 50 % WG and Boscalid 50% WP formulations against purple blotch disease in Onion. ,CLAIMS:WE CLAIM:

1. A suspension concentrate composition of Boscalid comprising of:
a) crystalline Boscalid in the range of 40 to 50% (w/w),
b) wetting agent in the range of 1% to 5% (w/w),
c) dispersing agent in the range of 1% to 5% (w/w),
d) antifreezing agent in the range of 1% to 40% (w/w),
e) biocide in the range of 0.1% to 0.5% (w/w),
f) buffering agent or salt in the range of 1% to 2% (w/w),
g) viscosity modifier in the range of 1% to 5% (w/w),
h) defoamer in the range of 0.1% to 1% (w/w), and
i) solvent in the range of 10% to 50% (w/w).

2. The composition as claimed in claim 1, wherein the crystalline Boscalid is crystalline anhydrate modification I or crystalline anhydrate modification II.

3. The composition as claimed in claim 1, wherein the wetting agent is selected from the group comprising polymethyl methacrylate-polyethylene glycol graft copolymer, phosphoric acid esters of ethoxylated tristyryl phenol, ethoxylated TSP-phosphate ester, amine salt of poly aryl phenyl ether phosphate, and nonionic proprietary surfactant blend or combination.

4. The composition as claimed in claim 3, wherein the dispersing agent is selected from the group comprising poly oxy alkylene glycol butyl ether, polyethylene glycol 2,4,6-tris(1-phenylethyl)phenyl ether sulfate ammonium salt, polyoxyethylene-polyoxypropylene Block Polymer, and Methyl methacrylate graft copolymer.

5. The composition as claimed in claim 3, wherein the antifreezing agent is selected from the group comprising glycerol, ethylene glycol, and mono ethylene glycol.

6. The composition as claimed in claim 3, wherein the biocide is 1,2-benzisothiazol-3(2H)-one.

7. The composition as claimed in claim 3, wherein the buffering agent or salt is citric acid.

8. The composition as claimed in claim 3, wherein the viscosity modifier is xanthan gum.

9. The composition as claimed in claim 3, wherein the defoamer is polydimethylsiloxane antifoam emulsion.

10. The process for the preparation of Boscalid suspension concentrate (SC) composition as claimed in claim 1, comprising the steps of:
a) preparing an aqueous slurry of antifreezing agent, wetting agent, dispersing agent, biocide, defoamer, solvent and buffering agent,
b) adding Boscalid crystalline anhydrate modification II to from homogenized aqueous slurry,
c) wet milling the obtained slurry in step (b) at less than 30oC to get wet milled slurry,
d) gelling the wet milled slurry by adding viscosity modifying agent, and
e) stirring the mixture for 2 hours to get Boscalid suspension concentrates.

Dated this Seventh (7th) day of February, 2023

__________________________________
Dr. S. Padmaja
Agent for the Applicant
IN/PA/883