Emulsion polymerisation method
View Patent ↗The invention relates to a method for the production of silicone in water emulsions by emulsion polymerization. The emulsion contains particles of an organopolysiloxane polymer having an average particle diameter of less than 1 μm. The method comprises: —combining a silanol end-blocked organosiloxane starting polymer, water, and a surfactant; said starting polymer having a viscosity of at least 2 Pa·s preferably at least 2.5 Pa·s preferably at least 3.5 Pa·s preferably at least 4 Pa·s and up to 150 Pa·s; —emulsifying the starting polymer by agitating or shearing the ingredients; —polymerizing the starting polymer to form a longer chain silanol end-blocked organopolysiloxane polymer; wherein at least a portion of said polymerizing step is performed at a temperature of less than or equal to 16° C. preferably less than or equal to 15° C.
1. A method of preparing an emulsion containing particles of an organopolysiloxane polymer having an average particle diameter of less than 1 μm, the method comprising:
(i) combining a silanol end-blocked organosiloxane starting polymer, water, and a surfactant, wherein said starting polymer has a viscosity of at least 2 Pa·s and up to 150 Pa·s;
(ii) emulsifying the starting polymer by agitating or shearing the starting polymer, water and surfactant;
(iii) polymerizing the starting polymer to form a longer chain silanol end-blocked organopolysiloxane polymer;
wherein at least a portion of said polymerizing step is performed at a temperature of less than or equal to 16° C., and wherein the emulsion contains less than 0.1 wt % of octamethylcyclotetrasiloxane and less than 0.1 wt % decamethylcyclopentasiloxane.
2. The method as claimed in claim 1 , wherein the viscosity of the starting polymer is up to 100 Pa·s.
3. The method as claimed in claim 1 , wherein the surfactant is an anionic surfactant.
4. The method as claimed in claim 1 , wherein the polymerizing step is started at a temperature of at least 18° C. and then lowered to said temperature of less than or equal to 16° C.
5. The method as claimed in claim 1 , wherein the portion of the polymerizing step performed at the temperature of less than or equal to 16° C. is also performed at a temperature more than 2° C.
6. The method as claimed in claim 1 , wherein the portion of the polymerizing step performed at less than or equal to 16° C. is at least 30% of the total polymerization time.
7. The method as claimed in claim 1 , wherein the polymerizing step takes place for 1 to 24 hours.
8. The method as claimed in claim 1 , wherein the average particle diameter is less than 0.8 μm.
9. The method as claimed in claim 1 , wherein the method is a continuous process and the starting polymer, surfactant and water are continuously fed to a high shear mixer in such proportions so as to form a viscous oil in water emulsion which is continuously withdrawn from the mixer.
10. The method as claimed in claim 1 , wherein the starting polymer, surfactant and water are fed into a high shear mixer through a single supply line and the pressure in the supply line at the inlet to the high shear mixer is monitored to be within 20% of a target pressure predetermined to give a desired emulsion particle size.
11. The method as claimed in claim 10 wherein the target pressure is within the range of 0.05 to 40 bar.
12. The method as claimed in claim 1 , wherein the surfactant is anionic and comprises a base.
13. The method as claimed in claim 12 , wherein the polymerizing step includes combining a condensation catalyst with the starting polymer and wherein the amount of condensation catalyst is calculated as R+ being between 0.1 and 5, wherein R+ is defined as the ratio between the molar amount of catalytically active anionic surfactant plus the molar amount of condensation catalyst, minus the molar amount of base, all divided by the molar amount of catalytically active anionic surfactant.
14. The method as claimed in claim 1 , wherein the starting polymer has a formula
wherein R 1 to R 6 represent an alkyl group containing 1-6 carbon atoms or an aryl group, and n is in the range of 300-2000.
15. The method as claimed in claim 14 , wherein n is in the range of 500-2000.
16. The method as claimed in claim 1 , wherein the viscosity of the polymerized particles after the polymerizing step is from 600 Pa·s to 5000 Pa·s.
17. A composition comprising the emulsion prepared according claim 1 .
18. The composition as claimed in claim 17 , the composition being suitable within a hair shampoo, hair conditioner, hair treatment, for skin care products, leather treatment, for paper or textile treatment or home care applications.
19. The method as claimed in claim 1 , wherein the surfactant is an anionic surfactant with one or more non-ionic surfactants.
20. A composition comprising an emulsion containing particles of a silanol end-blocked organopolysiloxane polymer having an average particle diameter of less than 1 μm, the composition containing less than 0.1 wt % of octamethylcyclotetrasiloxane and less than 0.1 wt % decamethylcyclopentasiloxane, and wherein the emulsion has an internal phase viscosity from 600 Pa·s to 5000 Pa·s.
21. The composition as claimed in claim 20 , the composition being suitable within a hair shampoo, hair conditioner, hair treatment, for skin care products, leather treatment, for paper or textile treatment or home care applications.