IP Library Granted Patent US 8,461,274
Granted Patent B2
US 8,461,274 · App. 13/060,017 · Granted Jun 11, 2013

Polysiloxane redistribution process

View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 8,461,274
App. No.
13/060,017
Granted
Jun 11, 2013
Kind
B2
Abstract

The invention pertains to the redistribution of cyclic and linear polysiloxanes by a method comprising contacting and heating a surfactant, wherein the surfactant is the salt of a protonated amine or a quaternary amine compound, an aqueous hydrochloric acid solution and a silicone, wherein the silicone is a silicon hydrolysate, D5, or DO. When the method of the invention is conducted with silicone hydrolysate, it eliminates the need to separate the silicone hydrolysate into its linear and cyclic constituents prior to redistribution.

Claims (44)

1. A process to redistribute cyclic and linear polysiloxanes, comprising:

contacting and heating a surfactant, wherein the surfactant is a salt of a protonated amine or a quaternary ammonium compound,

an aqueous hydrochloric acid solution, and

a silicone comprising a silicone hydrolysate,

wherein the silicone hydrolysate comprises from 20 to 80 weight %, based upon the weight of the silicone, linear polysiloxane, and

wherein the silicone hydrolyzate comprises a cyclic polysiloxane, and

wherein the linear polysiloxane is chlorine endblocked linear polydimethylsiloxane, and

wherein the silicone hydrolysate comprises:

from 31 to 47 weight percent D 4 ;

from 8 to 30 weight % D 5 ;

from 1 to 12 weight % D 6 ; and

from 38 to 45 weight % chlorine endblocked linear polydimethylsiloxane.

2. The process of claim 1 wherein the surfactant is a salt of a protonated amine and is formed from an amine according to formula (I):

NRR′R″  (I)

wherein R is an alkyl group, and R′ and R″ may independently be a hydrogen atom or an alkyl group having 1 to 4 carbon atoms.

3. The process of claim 2 wherein R is an alkyl group having 5 to 14 carbon atoms and each

R′ and R″ is independently a hydrogen atom or an alkyl group having 1 to 4 carbon atoms.

4. The process of claim 3 wherein the surfactant is formed from N-octylamine.

5. The process of claim 1 wherein the heating is at a temperature from 60° C. to 180° C.

6. The process of claim 1 wherein the aqueous hydrochloric acid solution is a saturated solution.

7. The process of claim 6 wherein the aqueous hydrochloric acid solution and the silicone are contacted in a ratio from 1:2 to 2:1.

8. The process of claim 1 wherein the surfactant concentration is from 0.1 wt. % to 10 weight % based upon the weight of the aqueous hydrochloric acid solution, the surfactant, and the silicone.

9. The process of claim 1 wherein the process is conducted at a pressure from 0 to 1000 kiloPascals.

10. The process of claim 1 wherein the contacting and heating step is conducted for 1 minute to 60 minutes.

11. The process of claim 1 wherein the silicone is redistributed and wherein after the process is conducted the distribution of cyclic polysiloxane is different than the distribution in the silicone contacted.

12. A process to redistribute cyclic and linear polysiloxanes, comprising:

contacting and heating a surfactant, wherein the surfactant is a salt of a protonated amine or a quaternary ammonium compound,

an aqueous hydrochloric acid solution, and

a silicone comprising silicone hydrolysate, wherein the silicone hydrolysate comprises from 20 to 80 weight %, based upon the weight of the silicone, linear polysiloxane, and

recovering hydrogen chloride as a gas.

13. The process of claim 12 , wherein the surfactant is N-octylamine hydrochloride,

the aqueous hydrochloric acid solution is a saturated aqueous hydrochloric acid solution, and the contacting is at a temperature from 60° C. to 180° C., at a pressure from 0 to 1000 kiloPascals, and for a time from 1 to 60 minutes.

14. A process to redistribute cyclic and linear polysiloxanes, comprising:

(1) contacting and heating

a surfactant, wherein the surfactant is a salt of a protonated amine or a quaternary ammonium compound,

an aqueous hydrochloric acid solution, and

a silicone comprising from 0 to <20 weight % linear polysiloxane based upon the weight of the silicone; and wherein the silicone comprises an excess of D 5 , or an excess of D 6 ; and

(2) recovering hydrogen chloride as a gas.

15. The process of claim 14 wherein the silicone comprises an excess of D 5 .

16. The process of claim 14 wherein the silicone comprises an excess of D 6 .

17. The process of claim 14 , wherein

the surfactant is N-octylamine hydrochloride,

the aqueous hydrochloric acid solution is a saturated aqueous hydrochloric acid solution, and

the contacting is at a temperature from 60° C. to 180° C., at a pressure from 0 to 1000 kiloPascals, and for a time from 1 to 60 minutes.

Assignments (1)
CHANGE OF NAME Recorded Feb 27, 2018
From: DOW CORNING CORPORATION
To: DOW SILICONES CORPORATION
Reel/Frame 045460/0278 →