IP Library Granted Patent US 6,875,381
Granted Patent B2
US 6,875,381 · App. 10/126,965 · Granted Apr 5, 2005

Process for preparation of chemically stable, dry-flow, low compact, dust free, soluble granules of phosphoroamidothioates

Assignee: United Phosphorus, Ltd.
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Quick Facts
Patent No.
US 6,875,381
App. No.
10/126,965
Granted
Apr 5, 2005
Kind
B2
Abstract

Dry flow, low compact, dust free, soluble granules of phosphoroamidothioates, preferably acephate, are produced by the process of 1) pre-mixing technical grade phosphoroamidothioate with specified adjuvants and other inert ingredients; 2) grinding to produce a ground product having a preferred particle size of 5 microns to 10 microns; 3) post-mixing; 4) granulating; 5) drying; 6) sizing to required length, preferably 1.5 to 3.0 mm; 7) and sieving to remove the fines to get the desired dust free soluble granule.

Claims (97)

1. A process for preparing soluble granules comprising

a) premixing 40 to 98 wt. % an insecticidally active compound of the following formula:

wherein R and R 1 individually are an alkyl, alkenyl or alkynyl group containing up to 6 carbon atoms, R 2 is hydrogen, an alkyl group containing 1 to 18 carbon atoms, a cycloalkyl group containing 3 to 8 carbon atoms, an alkenyl group containing 2 to 18 carbon atoms or an alkynyl group containing 3 to 18 carbon atoms, R 3 is hydrogen or an alkyl group containing 1 to 6 carbon atoms, and Y is oxygen or sulfur;

0.1-5.0 wt. % a dispersing agent; 0.1-3.0 wt. % a wetting agent; 0.1-3.0 wt. % a binding agent; 0.01-0.08 wt. % an antifoaming agent; 0.01-10.0 wt. % a disintegrating agent; 0.01-1.0 wt. % a stabilizer; and fillers to make 100 wt. %, to form a premix comprising essentially 95-99% solids and 1-5% moisture and/or solids;

b) grinding said premix to produce a ground product having a predetermined particle size;

c) post-mixing said ground product to produce a mixture;

d) granulating said mixture to produce granules;

e) drying said granules to produce dry granules;

f) sizing said dry granules to produce sized granules having a predetermined length and a predetermined diameter; and

g) sieving said sized granules to separate fines which are less than said predetermined length and said predetermined diameter.

2. The process of claim 1 , wherein said ground product has a predetermined particle size of 5-10 microns.

3. The process of claim 1 , wherein said dry granules have a predetermined length of 1.5-3.0 mm.

4. The process of claim 1 , wherein said dry granules have a predetermined diameter of 0.5 to 1.0 mm.

5. The process claimed in claim 1 , wherein said fillers are solids in powder form.

6. The process of claim 1 , wherein said binding agent is a blend of sucrose and starch derivatives.

7. The process of claim 1 , wherein said wetting agent is selected from the group comprising calcium salt of alkyl aryl sulphonate and sodium salt of alkyl aryl sulphonate.

8. The process of claim 1 , wherein said dispersing agent is a derivative of sulfonated fatty alcohol.

9. The process of claim 1 , wherein said disintegrating agent is a swelling type clay selected from the group comprising bentonite and zeolite.

10. The process of claim 1 , wherein said antifoaming agent is silicon oil derivative.

11. The process of claim 1 , wherein said stabilizer is a salt of a higher fatty acid.

12. The process of claim 1 , wherein said fillers are selected from the group comprising precipitated silica and kaoline.

13. The process of claim 1 , wherein said granulation is accomplished by passing said mixture through an orifice having and inlet and an outlet.

14. The process of claim 13 , wherein said inlet has a temperature of 30-35° C.

15. The process of claim 13 , wherein said outlet has a temperature of 40-45° C.

16. The process of claim 1 , wherein said drying is accomplished by passing said granules though an air chamber.

17. The process of claim 1 , wherein said grinding is accomplished by a microniser.

18. The process of claim 1 , wherein said sizing is accomplished by an oscillating cutter.

19. The process of claim 1 , wherein said insecticidally active compound is acephate.

20. The process of claim 1 , further comprising;

h) recycling said fines into step d).

21. The process of claim 20 , wherein said insecticidally active compound is acephate.

22. The process of claim 21 , wherein said ground product has a predetermined particle size of 5-10 microns.

23. The process of claim 22 , wherein said dry granules have a predetermined length of 1.5-3.0 mm and a predetermined diameter of 0.5 to 1.0 mm.

24. The process of claim 23 , wherein said binding agent is a blend of sucrose and starch derivatives.

25. The process of claim 24 , wherein said wetting agent is selected from the group comprising calcium salt of alkyl aryl sulphonate and sodium salt of alkyl aryl sulphonate.

26. The process of claim 25 , wherein said dispersing agent is a derivative of sulfonated fatty alcohol.

27. The process of claim 26 , wherein said disintegrating agent is a swelling type clay selected from the group comprising bentonite and zeolite.

28. The process of claim 27 , wherein said antifoaming agent is silicon oil derivative.

29. The process of claim 28 , wherein said stabilizer is a salt of a higher fatty acid.

30. The process of claim 29 , wherein said fillers are selected from the group comprising precipitated silica and kaoline.

31. The process of claim 20 , wherein said granulation is accomplished by passing said mixture through an orifice having and inlet and an outlet.

32. The process of claim 31 , wherein said inlet has a temperature of 30-35° C. and said outlet has a temperature of 40-45° C.

33. The process of claim 32 , wherein said drying is accomplished by passing said granules though an air chamber.

34. The process of claim 33 , wherein said grinding is accomplished by a microniser.

35. The process of claim 34 , wherein said sizing is accomplished by an oscillating cutter.

36. A process for preparing soluble granules comprising

a) preparing a dry premix by premixing 40 to 98 wt. % an insecticidally active compound of the following formula:

wherein R and R 1 individually are an alkyl, alkenyl or alkynyl group containing up to 6 carbon atoms, R 2 is hydrogen, an alkyl group containing 1 to 18 carbon atoms, a cycloalkyl group containing 3 to 8 carbon atoms, an alkenyl group containing 2 to 18 carbon atoms or an alkynyl group containing 3 to 18 carbon atoms, R 3 is hydrogen or an alkyl group containing 1 to 6 carbon atoms, and Y is oxygen or sulfur;

0.1-3.0 wt. % a wetting agent and a filler to make 100 wt. %;

b) grinding said dry premix to produce a ground product having a predetermined particle size;

c) post-mixing said ground product to produce a mixture;

d) granulating said mixture to produce granules;

e) drying said granules to produce dry granules;

f) sizing said dry granules to produce granules having a predetermined length and a predetermined diameter; and

g) sieving said sized granules to separate fines which are less than said predetermined length and said predetermined diameter.

37. The process of claim 36 , wherein said wetting agent is selected from the group comprising calcium salt of alkyl aryl sulphonate and sodium salt of alkyl aryl sulphonate.

38. The process of claim 36 , wherein said filler is selected from the group comprising precipitated silica and kaoline.

39. The process of claim 38 , wherein said wetting agent is selected from the group comprising calcium salt of alkyl aryl sulphonate and sodium salt of alkyl aryl sulphonate.

40. The process of claim 36 , wherein said step of preparing said dry premix further comprises premixing 0.1-5.0 wt. % a dispersing agent.

41. The process of claim 40 , wherein said dispersing agent is a derivative of sulfonated fatty alcohol.

42. The process of claim 36 , wherein said step of preparing said dry premix further comprises premixing 0.1-3.0 wt. % a binding agent.

43. The process of claim 42 , wherein said binding agent is a blend of sucrose and starch derivatives.

44. The process of claim 36 , wherein said step of preparing said dry premix further comprises premixing 0.01-0.08 wt. % an antifoaming agent.

45. The process of claim 44 , wherein said antifoaming agent is a silicon oil derivative.

46. The process of claim 36 , wherein said step of preparing said dry premix further comprises premixing 0.01-10 wt. % a disintegrating agent.

47. The process of claim 46 , wherein said disintegrating agent is a swelling type clay selected from the group comprising bentonite and zeolite.

48. The process of claim 36 , wherein said step of preparing said dry premix further comprises premixing 0.01-1.0 wt. % a stabilizer.

49. The process of claim 48 , wherein said stabilizer is a salt of a higher fatty acid.

50. The process of claim 36 , wherein said insecticidally active compound is acephate.

51. The process of claim 36 , further comprising;

h) recycling said fines into step d).

52. The process of claim 51 , wherein said insecticidally active compound is acephate.

53. The process of claim 36 , wherein said dry premix is substantially free from water or solvent.

54. The process of claim 36 , wherein said step of preparing said dry premix further comprises premixing 0.1-5.0 wt. % a dispersing agent, 0.1-3.0 wt. % a binding agent, 0.01-0.08 wt. % an antifoaming agent, 0.01-10 wt. % a disintegrating agent, 0.01-1.0 wt. % a stabilizer.

55. The process of claim 54 , wherein said insecticidally active compound is acephate.

56. The process of claim 55 , wherein said dispersing agent is a derivative of sulfonated fatty alcohol, said binding agent is a blend of socrose and starch derivatives, said antifoaming agent is a silicon oil derivative, said disintegrating agent is selected from the group comprising bentonite and zeolite, and said stabilizer is a salt of a higher fatty acid.

57. The process of claim 56 , wherein said dry premix is substantially free of water or solvent.

58. The process of claim 54 , wherein said dry premix is substantially free of water or solvent.

59. A process for preparing soluble granules consisting essentially,

a) preparing a dry premix by premixing 40 to 98 wt. % an insecticidally active compound of the following formula:

wherein R and R 1 individually are an alkyl, alkenyl or alkynyl group containing up to 6 carbon atoms, R 2 is hydrogen, an alkyl group containing 1 to 18 carbon atoms, a cycloalkyl group containing 3 to 8 carbon atoms, an alkenyl group containing 2 to 18 carbon atoms or an alkynyl group containing 3 to 18 carbon atoms, R 3 is hydrogen or an alkyl group containing 1 to 6 carbon atoms, and Y is oxygen or sulfur;

0.1-5.0 wt. % a dispersing agent; 0.1-3.0 wt. % a wetting agent; 0.1-3.0 wt. % a binding agent; 0.01-0.08 wt. % an antifoaming agent; 0.01-10.0 wt. % a disintegrating agent; 0.01-1.0 wt. % a stabilizer; and a filler to make 100 wt. %;

b) grinding said dry premix to produce a ground product having a predetermined particle size;

c) post-mixing said ground product to produce a mixture;

d) granulating said mixture to produce granules;

e) drying said granules to produce dry granules;

f) sizing said dry granules to produce granules having a predetermined length and a predetermined diameter; and

g) sieving said sized granules to separate fines which are less than said predetermined length and said predetermined diameter.

60. The process of claim 59 , wherein said binding agent is a blend of sucrose and starch derivatives.

61. The process of claim 59 , wherein said wetting agent is selected from the group comprising calcium salt of alkyl aryl sulphonate and sodium salt of alkyl aryl sulphonate.

62. The process of claim 59 , wherein said dispersing agent is a derivative of sulfonated fatty alcohol.

63. The process of claim 59 , wherein said disintegrating agent is a swelling type clay selected from the group comprising bentonite and zeolite.

64. The process of claim 59 , wherein said antifoaming agent is silicon oil derivative.

65. The process of claim 59 , wherein said stabilizer is a salt of a higher fatty acid.

66. The process of claim 59 , wherein said filler is selected from the group comprising precipitated silica and kaoline.

67. The process of claim 59 , wherein said insecticidally active compound is acephate.

68. The process of claim 59 , wherein said dry premix is substantially free of water or solvent.

Assignments (6)
CHANGE OF NAME Recorded May 24, 2019
From: UNITED PHOSPHORUS LIMITED
To: UPL, LTD
Reel/Frame 049280/0847 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 24, 2019
From: UPL, LTD.
To: UPL NA INC.
Reel/Frame 049281/0001 →
CHANGE OF NAME Recorded May 24, 2019
From: UNITED PHOSPHORUS INC.
To: UPL NA INC.
Reel/Frame 049287/0702 →
CHANGE OF NAME Recorded Nov 12, 2014
From: UNITED PHOSPHORUS LIMITED
To: UPL LIMITED
Reel/Frame 034155/0563 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 3, 2004
From: UNITED PHOSPHORUS, LTD.
To: UNITED PHOSPHORUS, LTD.; UNITED PHOSPHORUS, INC.
Reel/Frame 015721/0011 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 19, 2002
From: JADHAV, PRAKASH MAHADEO; SHROFF, RAJJU DEVIDAS
To: UNITED PHOSPHORUS, LTD.
Reel/Frame 013361/0490 →
Continuity (2)
Provisional Application 6034027200 · Dec 18, 2001
Related Publication 20030127761A1 · Jul 10, 2003