Abstract: ABSTRACT A SYNERGISTIC FUNGICIDAL OIL DISPERSION COMPRISING BOSCALID The present invention relates to a synergistic fungicidal composition. 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 oil dispersion comprising Boscalid and other agrochemical auxiliaries. The present invention more specifically relates to oil dispersion (OD) comprising crystalline Boscalid with one or more dispersing agent, emulsifier, rheology modifier and a base oil.
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 OIL DISPERSION 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. 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 oil dispersion comprising Boscalid and other agrochemical auxiliaries.
The present invention specifically relates to an oil dispersion composition comprising crystalline Boscalid with one or more agrochemical auxiliaries.
The present invention specifically relates to oil dispersion (OD) comprising Boscalid crystalline anhydrate modification I, with one or more dispersing agent, emulsifier, rheology modifier and a base oil.
The present invention also specifically relates to oil dispersion (OD) comprising Boscalid crystalline anhydrate modification II, with one or more dispersing agent, emulsifier, rheology modifier and a base oil.
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 144-145 oC and referred as modification I.
US7501384B2 describes Boscalid crystalline modification II having a melting point ranges from 147-148 ?.
US7087239B2 describes crystalline hydrates of Boscalid, especially monohydrate crystalline form of Boscalid.
The present inventors have developed oil dispersion of Boscalid stable formulation for the use of preventing and/or treating fungal infestations in plants and plant parts. The present invention particularly related to oil dispersion of Boscalid, prepared from crystalline anhydrate modification II shows a synergistic activity, and this liquid composition can be prepared from Boscalid crystalline anhydrate modification II by adding additional agrochemical axillaries without conversion to the hydrate form.
OBJECT OF THE INVENTION
One object of the present invention provides synergistic fungicidal oil dispersion (OD) composition comprising crystalline Boscalid.
Another object of the present invention provides oil dispersion (OD) comprising crystalline Boscalid with one or more dispersing agents, emulsifier, rheology modifier and a base oil.
In yet another object of the present invention provides process for the preparation of Boscalid oil dispersion (OD) composition comprising the steps of heating, stirring, milling, homogenizing, and packaging.
SUMMARY OF THE INVENTION
One aspect of the present invention provides a synergistic fungicidal oil dispersion (OD) composition comprising crystalline Boscalid.
Another aspect of the present invention provides an oil dispersion (OD) composition comprising crystalline Boscalid, with one or more dispersing agent, emulsifier, rheology modifier and a base oil.
Another aspect of the present invention provides an oil dispersion (OD) composition comprising Boscalid crystalline anhydrate modification I, with one or more dispersing agent, emulsifier, rheology modifier and a base oil.
Another aspect of the present invention provides an oil dispersion (OD) composition comprising Boscalid crystalline anhydrate modification II, with one or more dispersing agent, emulsifier, rheology modifier and a base oil.
Yet another aspect of the present invention provides oil dispersion (OD) composition comprising:
(a) crystalline Boscalid in the range of 10 to 15% (w/w),
(b) rheology modifier in the range of 0.1% to 5% (w/w),
(c) dispersing agent in the range of 5% to 10% (w/w),
(d) emulsifier in the range of 1% to 10% (w/w), and
(e) base oil in the range of 70% to 75% (w/w).
In yet another aspect of the present invention provides oil dispersion (OD) composition comprising:
(a) Boscalid crystalline anhydrate modification II in an amount of 15% (w/w),
(b) organic derivative of a hectorite clay and fumed silica surface treated with a hexadecyl silane in an amount of 0.9% (w/w),
(c) benzenesulfonic acid, C10-13-alkyl derivs calcium salt 2-ethylhexanol in an amount of 5% (w/w),
(d) castor oil ethoxylate with 36 EO and ethoxylate of alkyl polyethylene glycol ether in an amount of 7% (w/w), and
(e) palm methyl ester in an amount of 72.1% (w/w).
In yet another aspect of the present invention provides process for the preparation of Boscalid oil dispersion (OD) composition comprising the steps of heating, stirring, milling, homogenizing, and packaging.
In yet another aspect of the present invention provides process for the preparation of Boscalid oil dispersion (OD) composition comprising the steps of:
a) heating the base oil at 40-45°C,
b) adding a first rheology modifier, dispersing agent, emulsifiers to get clear solution,
c) adding crystalline Boscalid in portions wise over a period of ~1 hour under continuous stirring to get homogeneous solution,
d) adding second rheology modifier under continuous stirring for 30 min,
e) milling the obtained homogeneous mixture for a period of 2 hours to get the desired particle size,
f) cooling the oil dispersion obtained in step (e) to 20-30oC, and
g) isolating Boscalid oil dispersion.
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 oil dispersion (OD) comprising crystalline Boscalid.
Another embodiment of the present invention provides an oil dispersion (OD) comprising crystalline Boscalid, with one or more dispersing agent, emulsifier, rheology modifier and a base oil.
Yet another embodiment of the present invention provides oil dispersion (OD) composition comprising:
(a) crystalline Boscalid in the range of 10 to 15% (w/w),
(b) rheology modifier in the range of 0.1% to 5% (w/w),
(c) dispersing agent in the range of 5% to 10% (w/w),
(d) emulsifier in the range of 1% to 10% (w/w), and
(e) base oil in the range of 70% to 75% (w/w).
Yet another embodiment of the present invention provides oil dispersion (OD) composition comprising:
(a) Boscalid crystalline anhydrate modification II in an amount of 15% (w/w),
(b) organic derivative of a hectorite clay and fumed silica surface treated with a hexadecyl silane in an amount of 0.9% (w/w),
(c) benzenesulfonic acid, C10-13-alkyl derivs calcium salt 2-ethylhexanol in an amount of 5% (w/w),
(d) castor oil ethoxylate with 36 EO and ethoxylate of alkyl polyethylene glycol ether in an amount of 7% (w/w), and
(e) palm methyl ester in an amount of 72.1% (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 concentration of Boscalid used in the fungicidal oil dispersion (OD) is from 10% to 15% (w/w). Preferably used concentration of Boscalid is 15% (w/w) of the total weight of the composition.
Rheology modifiers as used herein includes but are not limited to organic derivative of a hectorite clay (like Benton 38, Benton 27, Benton 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, hydroxyethyl cellulose, 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.
Preferred rheology modifiers are organic derivative of a hectorite clay such as Benton 38 and Benton 1000, the fumed silicas such as Aerosil 200 and Aerosil R-816 and combination thereof.
The concentration of rheology modifiers used in the Boscalid oil dispersion (OD) is from 0.1% to 5% (w/w). Preferably concentration of rheology modifier is 0.9 % (w/w) of the total weight of the composition.
Dispersing agent as used herein includes but are not limited to ethylene oxide-propylene oxide block polymers, alkylphenol polyglycol ethers, Poly aryl alkylphenol polyethylene glycol phosphoric acid ester-Triethanol ammonium salt (DISPERSOGEN LFS), 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), calcium dodecyl benzene sulphonated (RHODOCAL 60 BER), polymeric esters (ATLOX 4916) and acrylic copolymer surfactant (ATLOX 4913). Preferred dispersing agents are calcium alkyl benzene sulphonate in 2-ethylhexanol (CALSOGEN 4814), Poly aryl alkylphenol polyethylene glycol phosphoric acid ester-Triethanol ammonium salt (DISPERSOGEN LFS), polymeric esters (ATLOX 4916) and acrylic copolymer surfactant (ATLOX 4913).
The concentration of dispersing agent used in the Boscalid oil dispersion (OD) is from 5% to 10% (w/w). Preferably concentration of dispersing agent is 5% (w/w) of the total weight of the composition.
Emulsifier as used herein includes but are not limited to nonionic, anionic, cationic and amphoteric emulsifiers, or a blend of two or more emulsifiers, aliphatic amine alkoxylates, polyoxy ethylene glycerol fatty acid esters, castor oil alkoxylates, fatty acid alkoxylates, fatty acid amide alkoxylates, fatty acid poly diethanolamides, lanolin ethoxylates, fatty acid polyglycol esters, isoforms tridecyl alcohol, fatty acid amides, alkyl poly glycosides, non-ionic surfactant blend (Atlox 309F), polyoxyethylene (40) sorbitol hexaoleate (Atlox G-1086), polyacrylate graft copolymer (DISPERSOGEN PSL 100), 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.
Preferred emulsifiers are castor oil ethoxylate with 36 mole EO (EMULSOGEN 360), polyacrylate graft copolymer (DISPERSOGEN PSL 100), Ethoxylate of alkyl polyethylene glycol ether (Lutensol TO 5), non-ionic surfactant blend (Atlox 309F), and polyoxyethylene (40) sorbitol hexaoleate (Atlox G-1086) and combination thereof.
The concentration of emulsifiers used in the fungicidal oil dispersion is from 1% to 10% (w/w). Preferably concentration of emulsifiers is 7% (w/w).
Base oil as used herein includes but are not limited to methyl soyate oil, rapeseed oil, olive oil, castor oil, rape oil, corn oil, cottonseed oil, Helianthus sunflower oil, vegetable oil, mineral oil, paraffin oil, palm methyl ester oil. Preferred base oil is palm methyl ester oil, helianthus sunflower oil, paraffin oil and vegetable oil.
The concentration of base oil used in the fungicidal oil dispersion is from 70% to 75% (w/w). Preferably concentration of base oil is 72.1% (w/w) of the total weight of the composition.
The present invention is to provides Boscalid oil dispersion (OD) composition with good sticking property, penetration and rain fasting properties, saves operational cost by milling the material, requires low dose compared to water dispersible granules, industrially and economically feasible process.
Yet another embodiment of the present invention is to provide process for the preparation of Boscalid oil dispersion (OD) comprising the steps of:
a) heating the base oil at 40-45°C,
b) adding a first rheology modifier, dispersing agent, emulsifiers to get clear solution,
c) adding crystalline Boscalid in portions wise over a period of ~1 hour under continuous stirring to get homogeneous suspension,
d) adding second rheology modifier under continuous stirring for 30 min,
e) milling the obtained homogeneous mixture for a period of 2 hours to get the desired particle size,
f) cooling the oil dispersion obtained in step (e) to 20-30oC, and
g) isolating Boscalid oil dispersion.
According to the present invention, base oil is heated to 40-45°C in the high sheer disperser. To this oil first rheology modifier is added, followed by dispersing agent, emulsifiers at same temperature to get clear solution. Crystalline Boscalid is added portion wise over a period of ~1 hour to get the homogeneous solution. Second rheology modifier is added under stirring, followed by milling the obtained homogeneous mixture to get the particle size of less than 15 microns, cooled the suspension to 20-30oC to obtain Boscalid oil dispersion.
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 15% oil dispersion (OD) formulation:
Example-1:
An oil dispersion (OD) formulation of Boscalid comprising 15% (w/w) of Boscalid crystalline anhydrate modification I (Purity: 98%)as an active ingredient, 0.4% (w/w) organic derivative of a hectorite clay (Benton 38) and 0.5% (w/w) the fumed silicas such as Aerosil R816 as rheology modifiers, 5% (w/w) calcium alkyl benzene sulphonate in 2-ethylhexanol (CALSOGEN 4814) as dispersing agent, 5% (w/w) castor oil ethoxylate with 36 mole EO (EMULSOGEN 360) and 2% (w/w) ethoxylate of alkyl polyethylene glycol ether (Lutensol TO 5) as emulsifiers, and 72.1% (w/w) of palm methyl ester oil as base oil.
S. N. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification I (Purity: 98%) 15.0
2. Organic derivative of a hectorite clay (Benton 38) 0.4
3. calcium alkyl benzene sulphonates in 2-ethylhexanol.
(CALSOGEN 4814) 5.0
4. Castor oil ethoxylate with 36 mole EO (EMULSOGEN 360) 5.0
5. Ethoxylate of alkyl polyethylene glycol ether (Lutensol TO 5) 2.0
6. Fumed silicas such as Aerosil R816 0.5
7. Palm methyl ester oil 72.1
Total 100
Manufacturing process:
Specified quantity of palm methyl ester oil in the high sheer disperser, stirred and heated to 40-45°C. To this specified quantity of organic derivative of a hectorite clay (Bentone 38) was added and stirred to form homogenized mixture. Add specified quantity of CALSOGEN 4814, EMULSOGEN-360, Lutensol TO-5 were added after every 15-20 min of interval and under continuous stirring for 20 min. Boscalid crystalline anhydrate modification I technical was added to the obtained homogenized mixture at a temperature <50°C in small portions over a period of ~1 hour under continuous stirring. Specified quantity of fumed silica (Aerosil R-816) was added and stirred for 30 min. Obtained mixture was wet milled to attain the desired particle size distribution (D90 should be ~15 micron) and transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Slowly cooled the obtained oil dispersion to room temperature and packaged in drum.
Example-2:
An oil dispersion (OD) formulation of Boscalid comprising 15% (w/w) of Boscalid crystalline anhydrate modification II (Purity: 98%) as an active ingredient, 0.4% (w/w) organic derivative of a hectorite clay (Benton 38) and 0.5% (w/w) the fumed silicas such as Aerosil R816 as rheology modifiers, 5% (w/w) calcium alkyl benzene sulphonate in 2-ethylhexanol (CALSOGEN 4814) as dispersing agent, 5% (w/w) castor oil ethoxylate with 36 mole EO (EMULSOGEN 360) and 2% (w/w) ethoxylate of alkyl polyethylene glycol ether (Lutensol TO 5) as emulsifiers, and 72.1% (w/w) of palm methyl ester oil as base oil.
S. N. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification II (Purity: 98%) 15.0
2. Organic derivative of a hectorite clay (Benton 38) 0.4
3. calcium alkyl benzene sulphonates in 2-ethylhexanol.
(CALSOGEN 4814) 5.0
4. Castor oil ethoxylate with 36 mole EO (EMULSOGEN 360) 5.0
5. Ethoxylate of alkyl polyethylene glycol ether (Lutensol TO 5) 2.0
6. Fumed silicas such as Aerosil R816 0.5
7. Palm methyl ester oil 72.1
Total 100
Manufacturing process:
Specified quantity of palm methyl ester oil in the high sheer disperser, stirred and heated to 40-45°C. To this specified quantity of organic derivative of a hectorite clay (Bentone 38) was added and stirred to form homogenized mixture. Add specified quantity of CALSOGEN 4814, EMULSOGEN-360, Lutensol TO-5 were added after every 15-20 min of interval and under continuous stirring for 20 min. Boscalid crystalline anhydrate modification II technical was added to the obtained homogenized mixture at a temperature <50°C in small portions over a period of ~1 hour under continuous stirring. Specified quantity of fumed silica (Aerosil R-816) was added and stirred for 30 min. Obtained mixture was wet milled to attain the desired particle size distribution (D90 should be ~15 micron) and transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Slowly cooled the obtained oil dispersion to room temperature and packaged in drum.
Example-3:
An oil dispersion (OD) formulation of Boscalid comprising 15% (w/w) of Boscalid crystalline anhydrate modification II (Purity: 98%) as an active ingredient, 0.1% (w/w) organic derivative of a hectorite clay (Benton 38) and 1% (w/w) the fumed silicas such as Aerosil 200 as rheology modifiers, 5% (w/w) calcium alkyl benzene sulphonate in 2-ethylhexanol (CALSOGEN 4814) as dispersing agent, 5% (w/w) castor oil ethoxylate with 36 mole EO (EMULSOGEN 360) and 73.9% (w/w) of helianthus sunflower oil as base oil.
S. No. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification II (Purity: 98%) 15.0
2. Organic derivative of a hectorite clay (Benton 38) 0.1
3. Calcium alkyl benzene sulphonates in 2-ethylhexanol (CALSOGEN 4814) 5.0
4. Castor oil ethoxylate with 36 mole EO (EMULSOGEN 360) 5.0
5. Fumed silicas such as Aerosil 200 1.0
6. Helianthus sunflower oil 73.9
Total 100
Manufacturing process:
Specified quantity of helianthus sunflower oil in the high sheer disperser, stirred and heated to 40-45°C. To this specified quantity of organic derivative of a hectorite clay (Bentone 38) was added and stirred to form homogenized mixture. Add specified quantity of CALSOGEN 4814, and EMULSOGEN-360 were added after every 15-20 min of interval and under continuous stirring for 20 min. Boscalid crystalline anhydrate modification II technical was added to the obtained homogenized mixture at a temperature <50°C in small portions over a period of ~1 hour under continuous stirring. Specified quantity of fumed silica (Aerosil 200) was added and stirred for 30 min. Obtained mixture was wet milled to attain the desired particle size distribution (D90 should be ~15 micron) and transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Slowly cooled the obtained oil dispersion to room temperature and packaged in drum.
Example-4:
An oil dispersion (OD) formulation of Boscalid comprising 15% (w/w) of Boscalid crystalline anhydrate modification II (Purity: 98%) as an active ingredient, 0.1% (w/w) organic derivative of a hectorite clay (Benton 1000) and 1% (w/w) the fumed silicas such as Aerosil 200 as rheology modifiers, 6% (w/w) poly aryl alkylphenol polyethylene glycol phosphoric acid ester-Triethanol ammonium salt (DISPERSOGEN LFS) as dispersing agent, 6% (w/w) polyacrylate graft copolymer (DISPERSOGEN PSL 100) as emulsifiers, and 71.9% (w/w) of paraffin oil (Kyros oil) as base oil.
S. No. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification II (Purity: 98%) 15.0
2. Organic derivative of a hectorite clay (Benton 1000) 0.1
3. Poly aryl alkylphenol polyethylene glycol phosphoric acid ester-Triethanol ammonium salt (DISPERSOGEN LFS) 6.0
4. polyacrylate graft copolymer (DISPERSOGEN PSL 100) 6.0
5. Fumed silicas such as Aerosil 200 1.0
6. Paraffin oil (Kyros oil) 71.9
Total 100
Manufacturing process:
Specified quantity of paraffin oil in the high sheer disperser, stirred and heated to 40-45°C. To this specified quantity of organic derivative of a hectorite clay (Bentone 1000) was added and stirred to form homogenized mixture. Add specified quantity of (DISPERSOGEN LFS), and (DISPERSOGEN PSL 100) were added after every 15-20 min of interval and under continuous stirring for 20 min. Boscalid crystalline anhydrate modification II technical was added to the obtained homogenized mixture at a temperature <50°C in small portions over a period of ~1 hour under continuous stirring. Specified quantity of fumed silica (Aerosil 200) was added and stirred for 30 min. Obtained mixture was wet milled to attain the desired particle size distribution (D90 should be ~15 micron) and transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Slowly cooled the obtained oil dispersion to room temperature and packaged in drum.
Example-5:
An oil dispersion (OD) formulation of Boscalid comprising 15% (w/w) of Boscalid crystalline anhydrate modification II (Purity: 98%) as an active ingredient, 0.1% (w/w) organic derivative of a hectorite clay (Benton 1000) and 1% (w/w) the fumed silicas such as Aerosil 200 as rheology modifiers, 7% (w/w) polymeric esters (Atlox 4916) as dispersing agent, 4% (w/w) non-ionic surfactant blend (Atlox 309F) as emulsifier, and 72.9% (w/w) of paraffin oil (Kyros oil) as base oil.
S. No. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification II (Purity 98% ) 15.0
2. Organic derivative of a hectorite clay (Benton 1000) 0.1
3. Polymeric esters (Atlox 4916) 7.0
4. Non-ionic surfactant blend (Atlox 309F) 4.0
5. Fumed silicas such as Aerosil 200 1.0
6. Paraffin oil (Kyros oil) 72.9
Total 100
Manufacturing process:
Specified quantity of paraffin oil in the high sheer disperser, stirred and heated to 40-45°C. To this specified quantity of organic derivative of a hectorite clay (Bentone 38) was added and stirred to form homogenized mixture. Add specified quantity of Atlox 4916, and Atlox 309F were added after every 15-20 min of interval and under continuous stirring for 20 min. Boscalid crystalline anhydrate modification II technical was added to the obtained homogenized mixture at a temperature <50°C in small portions over a period of ~1 hour under continuous stirring. Specified quantity of fumed silica (Aerosil 200) was added and stirred for 30 min. Obtained mixture was wet milled to attain the desired particle size distribution (D90 should be ~15 micron) and transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Slowly cooled the obtained oil dispersion to room temperature and packaged in drum.
Example-6:
An oil dispersion (OD) formulation of Boscalid comprising 15% (w/w) of Boscalid crystalline anhydrate modification II (Purity: 98%) as an active ingredient, 0.1% (w/w) organic derivative of a hectorite clay (Benton 1000) and 1% (w/w) the fumed silicas such as Aerosil 200 as rheology modifiers, 7% (w/w) acrylic copolymer surfactant (Atlox 4913) as dispersing agent, 5% (w/w) polyoxyethylene (40) sorbitol hexaoleate (Atlox G-1086) as emulsifier, and 71.9% (w/w) of vegetable oil (MSO) as base oil.
S. No. Ingredients Quantity
(in %w/w)
1. Boscalid crystalline anhydrate modification II (Purity: 98%) 15.0
2. Organic derivative of a hectorite clay (Benton 1000) 0.1
3. Acrylic copolymer surfactant (Atlox 4913) 7.0
4. Polyoxyethylene (40) sorbitol hexaoleate (Atlox G-1086) 5.0
5. Fumed silicas such as Aerosil 200 1.0
6. vegetable oil (MSO) 71.9
Total 100
Manufacturing process:
Specified quantity of vegetable oil in the high sheer disperser, stirred and heated to 40-45°C. To this specified quantity of organic derivative of a hectorite clay (Bentone 1000) was added and stirred to form homogenized mixture. Add specified quantity of Atlox 4913, and Atlox G-1086 were added after every 15-20 min of interval and under continuous stirring for 20 min. Boscalid crystalline anhydrate modification II technical was added to the obtained homogenized mixture at a temperature <50°C in small portions over a period of ~1 hour under continuous stirring. Specified quantity of fumed silica (Aerosil 200) was added and stirred for 30 min. Obtained mixture was wet milled to attain the desired particle size distribution (D90 should be ~15 micron) and transferred into a separate vessel and stirred continuously at room temperature over a period of 2 hrs. Slowly cooled the obtained oil dispersion to room temperature and packaged in drum.
Efficacy study for Boscalid 15% in an oil dispersion (OD) 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 15% OD versus Boscalid 15% WP and Boscalid 15% 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 15% OD 150 90 84
Boscalid 15% WG 150 85 80
Boscalid 15% WP 150 82 78
OD – Oil dispersion, 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 15% OD provided excellent and longer duration control as compared to Boscalid 15 % WG and Boscalid 15% 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 15% OD 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 15% OD 150 85 81
Boscalid 15% WG 150 82 78
Boscalid 15% WP 150 78 75
OD – Oil dispersion, 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 15% OD provided excellent and longer duration control as compared to Boscalid 15 % WG and Boscalid 15% 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% OD 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 15% OD 150 90 84
Boscalid 15% WG 150 88 81
Boscalid 15% WP 150 85 80
OD – Oil dispersion, 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 15% OD provided excellent and longer duration control as compared to Boscalid 15 % WG and Boscalid 15% WP formulations against purple blotch disease in Onion. ,CLAIMS:WE CLAIM:
1. An oil dispersion (OD) composition of Boscalid comprising of:
(a) crystalline Boscalid in the range of 10 to 15% (w/w),
(b) rheology modifier in the range of 0.1% to 5% (w/w),
(c) dispersing agent in the range of 5% to 10% (w/w),
(d) emulsifier in the range of 1% to 10% (w/w), and
(e) base oil in the range of 70% to 75% (w/w).
2. The composition as claimed in claim 1, wherein the crystalline Boscalid is selected from crystalline anhydrate modification I or crystalline anhydrate modification II.
3. The composition as claimed in claim 1, wherein the rheology modifier is selected from organic derivative of a hectorite clay, fumed silica surface treated with a hexadecyl silane, hydrophilic fumed silica, and combination thereof.
4. The composition as claimed in claim 1, wherein the dispersing agent is selected from calcium alkyl benzene sulphonate in 2-ethylhexanol, poly aryl alkylphenol polyethylene glycol phosphoric acid ester-Triethanol ammonium salt, polymeric ester, and polymeric surfactant.
5. The composition as claimed in claim 1, wherein the emulsifier is selected from castor oil ethoxylate with 36 EO, ethoxylate of alkyl polyethylene glycol ether, polyacrylate graft copolymer, non-ionic surfactant blend, and polyoxyethylene (40) sorbitol hexaoleate.
6. The composition as claimed in claim 1, wherein the base oil is selected from palm methyl ester oil, helianthus sunflower oil, paraffin oil, and vegetable oil.
7. The process for the preparation of an oil dispersion (OD) of Boscalid as claimed in claim 1, comprising the steps of:
a) heating the base oil at 40-45°C,
b) adding a first rheology modifier, dispersing agent, emulsifiers to get clear solution,
c) adding crystalline Boscalid in portions wise over a period of ~1 hour under continuous stirring to get homogeneous suspension,
d) adding second rheology modifier under continuous stirring for 30 min,
e) milling the obtained homogeneous mixture for a period of 2 hours to get the desired particle size,
f) cooling the oil dispersion obtained in step (e) to 20-30oC, and
g) isolating Boscalid oil dispersion.
Dated this Tenth (10th) day of February, 2023
__________________________________
Dr. S. Padmaja
Agent for the Applicant
IN/PA/883
| # | Name | Date |
|---|---|---|
| 1 | 202241010397-PROVISIONAL SPECIFICATION [26-02-2022(online)].pdf | 2022-02-26 |
| 2 | 202241010397-POWER OF AUTHORITY [26-02-2022(online)].pdf | 2022-02-26 |
| 3 | 202241010397-FORM 1 [26-02-2022(online)].pdf | 2022-02-26 |
| 4 | 202241010397-Proof of Right [19-03-2022(online)].pdf | 2022-03-19 |
| 5 | 202241010397-FORM 3 [10-02-2023(online)].pdf | 2023-02-10 |
| 6 | 202241010397-ENDORSEMENT BY INVENTORS [10-02-2023(online)].pdf | 2023-02-10 |
| 7 | 202241010397-COMPLETE SPECIFICATION [10-02-2023(online)].pdf | 2023-02-10 |
| 8 | 202241010397-FORM 18 [22-10-2024(online)].pdf | 2024-10-22 |