초록

Methods for continuously producing HIPR silicone in water emulsions are disclosed. The methods use low shear devices, and thus the temperature of the emulsions is kept low, while enhanced particle size and viscosity are obtained.

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What is claimed is: 1. A continuous method for preparing a high internal phase ratio silicone in water emulsion which comprises: a) providing an amount of a continuous phase in a system; b) adding an amount of a dispersed phase to the system; c) providing low shear means to mix the continuous pha

What is claimed is: 1. A continuous method for preparing a high internal phase ratio silicone in water emulsion which comprises: a) providing an amount of a continuous phase in a system; b) adding an amount of a dispersed phase to the system; c) providing low shear means to mix the continuous phase and dispersed phase thus forming an intermediate emulsion; d) incrementally adding additional amounts of the dispersed phase to the intermediate emulsion while shearing, wherein the ratio of intermediate emulsion to the dispersed phase to be added is at least about 1.5 to 1; e) maintaining the amounts of continuous phase and dispersed phase in the system by continuously adding additional amounts of each to the system; and, f) removing a high internal phase ratio silicone in water emulsion from the system as it is formed wherein the high internal phase silicone in water emulsion has a viscosity of from about 50,000 cp to about 6,000,000 cp. 2. The method of claim 1 wherein the system comprises: a) at least one pump for continuously introducing components of said continuous phase into a flow line; b) at least one pump for continuously introducing said dispersed phase into the flow line; c) means defining a recirculation flow line adapted to receive the phases from the flow line; d) a recirculating pump positioned in the recirculation flow line; e) shearing means adapted to emulsify the phases within the recirculation flow line; f) an outlet adapted to permit a portion of the high internal phase ratio silicone in water emulsion to exit the recirculation flow line while the intermediate emulsion remaining within the recirculation flow line continues to pass therethrough; and, g) an inlet permitting the intermediate emulsion remaining in the flow line to continue to circulate in the recirculation flow line. 3. The method of claim 2 wherein the shearing means includes at least one static mixer. 4. The method of claim 2 wherein the system includes a means for monitoring the temperature of the intermediate emulsion. 5. The method of claim 2 wherein the system includes a means for monitoring the pressure of the intermediate emulsion. 6. The method of claim 2 wherein the portion of the high internal phase ratio silicone in water emulsion exiting the recirculation flow line through the outlet passes through a line which includes a shearing device for additional shearing of the high internal phase ratio silicone in water emulsion. 7. The method of claim 2 wherein the system includes an accumulator upstream of the recirculation pump. 8. The method of claim 2 wherein the portion of the high internal phase ratio silicone in water emulsion exiting the recirculation flow line through the outlet passes through a line which includes a pressure pump. 9. The method of claim 8 wherein the system includes an accumulator upstream of the pressure pump. 10. The method of claim 1 wherein the continuous phase comprises water and at least one emulsifier. 11. The method of claim 1 wherein the dispersed phase comprises a silicone compound selected from the group consisting of polydimethylsiloxanes, organomodified polydimethylsiloxanes and silica-filled polydimethylsiloxanes. 12. The method of claim 11 wherein the organomodified polydimethylsiloxane is (CH3)3SiO((CH3) 2SiO)500((CH3)(C3H6NHC2 H4NH2)SiO)3Si(CH3)3. 13. The method of claim 2 wherein water is added to the high internal phase silicone in water emulsion exiting the system to form a diluted final product. 14. The method of claim 13 wherein the diluted final product has mean particle sizes ranging from about 0.1 microns to about 30 microns. 15. The method of claim 13 wherein the diluted final product emulsion has a viscosity ranging from about 1 cp to about 10,000 cp. 16. The method of claim 2 wherein the high internal phase ratio silicone in water emulsion has a temperature ranging from about 10째 C. to about 80째 C. 17. The method of claim 2 further comprising cooling the dispersed phase prior to entering the flow line. 18. The method of claim 2 further comprising heating the dispersed phase prior to entering the flow line. 19. The method of claim 2 further comprising cooling the continuous phase prior to entering the flow line. 20. The method of claim 2 further comprising heating the continuous phase prior to entering the flow line. 21. The method of claim 1 wherein the system comprises: a) a closed pressure vessel; b) at least one pump for continuously introducing said continuous phase into said vessel; c) at least one pump for continuously introducing said dispersed phase into said vessel; d) agitators within said vessel capable of producing an intermediate emulsion; and, e) an outlet adapted to permit a portion of the high internal phase silicone in water emulsion to exit the closed vessel via an exit line while the intermediate emulsion remains within the vessel and is recirculated. 22. The method of claim 21 wherein the agitators of the system further comprise a wall-wiping anchor. 23. The method of claim 21 wherein the system further comprises a second agitator. 24. The method of claim 21 wherein the continuous phase comprises water and at least one emulsifier. 25. The method of claim 21 wherein the dispersed phase comprises a silicone compound selected from the group consisting of polydimethylsiloxanes, organomodified polydimethylsiloxanes and silica-filled polydimethylsiloxanes. 26. The method of claim 25 wherein the organomodified polydimethylsiloxane is (CH3)3SiO((CH3) 2SiO)500((CH3)(C3H6NHC2 H4NH2)SiO)3Si(CH3)3. 27. The method of claim 21 wherein water is added to the high internal phase silicone in water emulsion exiting the system to form the diluted final product. 28. The method of claim 21 wherein the system includes a shearing device in the exit line for additional shearing of the high internal phase silicone in water emulsion. 29. The method of claim 28 wherein the system includes a pressure pump on the exit line to feed the shearing device. 30. The method of claim 29 wherein the system includes an accumulator upstream of the pressure pump. 31. The method of claim 27 wherein the diluted final product has mean particle sizes ranging from about 0.1 microns to about 30 microns. 32. The method of claim 27 wherein the diluted final product emulsion has a viscosity ranging from about 1 cp to about 10,000 cp. 33. The method of claim 21 wherein the high internal phase silicone in water emulsion has a temperature ranging from about 10째 C. to about 80째 C. 34. The method of claim 21 further comprising a means for cooling the dispersed phase prior to entering the vessel. 35. The method of claim 21 further comprising a means for heating the dispersed phase prior to entering the vessel. 36. The method of claim 21 further comprising a means for cooling the continuous phase prior to entering the vessel. 37. The method of claim 21 further comprising a means for heating the continuous phase prior to entering the vessel. 38. The method of claim 21 further comprising a jacket around the vessel capable of regulating the intermediate emulsion's temperature. 39. The method of claim 21 wherein the system includes a means for monitoring the temperature of the intermediate emulsion. 40. The method of claim 21 wherein the system includes a means for monitoring the pressure of the intermediate emulsion. 41. The method of claim 1 wherein the system comprises: a) a series of mixing means; b) supply means for providing a stream of continuous phase and a separate stream of dispersed phase into a first mixing means to produce an intermediate emulsion; c) transporting means for forwarding the intermediate emulsion in a transporting flow line to a later mixing means; d) additional supply means for providing a stream of additional dispersed phase to the intermediate emulsion prior to its entry into the later mixing means; and, e) repeating steps (c)-(d) as necessary to form the high internal phase silicone in water emulsion. 42. The method of claim 41 wherein the amount of dispersed phase added to the mixing means is incrementally increased with a higher amount of dispersed phase added to a later mixing means in the series of mixing means. 43. The method of claim 41 wherein the series of mixing means includes a mixer selected from the group consisting of in-line static mixers, in-line rotary mixers, in-line impeller mixers, rotor-stators and combinations thereof. 44. The method of claim 43 wherein the series of mixing means comprises about 3 to about 10 mixers. 45. The method of claim 41 wherein at least one pressure pump is placed within the transporting flow line. 46. The method of claim 41 wherein the continuous phase comprises water and at least one emulsifier. 47. The method of claim 41 wherein the dispersed phase comprises a silicone compound selected from the group consisting of polydimethylsiloxanes, organomodified polydimethylsiloxanes and silica-filled polydimethylsiloxanes. 48. The method of claim 47 wherein the organomodified polydimethylsiloxane is (CH3)3SiO((CH3) 2SiO)500((CH3)(C3H6NHC2 H4NH2)SiO)3Si(CH3)3. 49. The method of claim 41 wherein water is added to the high internal phase silicone in water emulsion exiting the system to form the diluted final product. 50. The method of claim 49 wherein the diluted final product has mean particle sizes ranging from about 0.1 microns to about 30 microns. 51. The method of claim 49 wherein the diluted final product emulsion has a viscosity ranging from about 1 cp to about 10,000 cp. 52. The method of claim 41 wherein the high internal phase silicone in water emulsion has a temperature ranging from about 10째 C. to about 80째 C. 53. The method of claim 41 further comprising a means for cooling the dispersed phase prior to entering the flow line. 54. The method of claim 41 further comprising a means for heating the dispersed phase prior to entering the flow line. 55. The method of claim 41 further comprising a means for cooling the continuous phase prior to entering the flow line. 56. The method of claim 41 further comprising a means for heating the continuous phase prior to entering the flow line. 57. The method of claim 41 wherein the system includes a means for monitoring the temperature of the intermediate emulsion. 58. The method of claim 41 wherein the system includes a means for monitoring the pressure of the intermediate emulsion. 59. A continuous method for preparing a high internal phase ratio silicone in water emulsion which comprises: a) providing an amount of a continuous phase in a system; b) adding an amount of a dispersed phase to the system; c) providing low shear means to mix the continuous phase and dispersed phase thus forming an intermediate emulsion; d) incrementally adding additional amounts of the dispersed phase to the intermediate emulsion while shearing,; e) maintaining the amounts of continuous phase and dispersed phase in the system by continuously adding additional amounts of each to the system; and, f) removing a high internal phase ratio silicone in water emulsion from the system as it is formed; and wherein the system comprises: (i) at least one pump for continuously introducing components of said continuous phase into a flow line; (ii) at least one pump for continuously introducing said dispersed phase into the flow line; (iii) means defining a recirculation flow line adapted to receive the phases from the flow line; (iv) a recirculating pump positioned in the recirculation flow line; (v) shearing means adapted to emulsify the phases within the recirculation flow line; (vi) an outlet adapted to permit a portion of the high internal phase ratio silicone in water emulsion to exit the recirculation flow line while the intermediate emulsion remaining within the recirculation flow line continues to pass therethrough; and, (vii) an inlet permitting the intermediate emulsion remaining in the flow line to continue to circulate in the recirculation flow line; and further wherein the portion of the high internal phase ratio silicone in water emulsion exiting the recirculation flow line through the outlet passes through a line which includes a shearing device for additional shearing of the high internal phase ratio silicone in water emulsion and a pressure pump. 60. A continuous method for preparing a high internal phase ratio silicone in water emulsion which comprises: a) providing an amount of a continuous phase in a system; b) adding an amount of a dispersed phase to the system; c) providing low shear means to mix the continuous phase and dispersed phase thus forming an intermediate emulsion; d) incrementally adding additional amounts of the dispersed phase to the intermediate emulsion while shearing,; e) maintaining the amounts of continuous phase and dispersed phase in the system by continuously adding additional amounts of each to the system; and, f) removing a high internal phase ratio silicone in water emulsion from the system as it is formed; wherein the dispersed phase comprises (CH3)3 SiO((CH3)2SiO)500((CH3)(C3 H6NHC2H4NH2)SiO)3Si(CH 3)3.