Method of manufacturing silicone emulsions

• US 5,302,658 A
• Filed: 07/14/1992
• Issued: 04/12/1994
• Est. Priority Date: 07/14/1992
• Status: Expired due to Fees

• Current Assignee: Dow, Inc.
• Original Assignee: Dow, Inc.
• Inventors: Varaprath, Padmakumari J., Gee, Ronald P.
• Primary Examiner(s): Marquis, Melvyn I.
• Assistant Examiner(s): Dean, Karen A.
• Application Number:
  US07/913,555
• Time in Patent Office: 637 Days
• Field of Search: 524/837, 524/732, 252/312, 252/314, 106/287.13, 106/287.14, 514/941
• US Class Current: 524/732
• CPC Class Codes: C08J 2383/04 Polysiloxanes
• CPC Class Codes: C08J 3/03 in aqueous media

Abstract

A method is described for making an emulsion in which a mixture is formed containing a polysiloxane and a primary nonionic surfactant having an HLB value of 10 to 19. There is added to the mixture a first portion of surfactant free water gradually in a series of separate incremental steps. This is followed by the addition to the mixture of a secondary nonionic surfactant having an HLB value of 1.8-15. The mixture is stirred until the particle size of the polysiloxane in the mixture is in the range of 1-100 microns. A second portion of water is added to the mixture in an amount sufficient to provide a total content of water in the product of 25-65 percent by weight.

Claims

1. A method of making an emulsion comprising the steps of (A) forming a mixture by combining 35 to 75 percent by weight of a polysiloxane and 0.25 to 2.0 percent by weight of a primary nonionic surfactant having an HLB value of 10 to 19, and stirring the mixture until uniform:

(B) adding and dispersing 3-6 percent by weight of a first portion of surfactant free water in the mixture, the first portion of surfactant free water being added and dispersed in the mixture gradually over a period of time in a series of from about five to about ten separate incremental steps;

(C) adding to the mixture 0.25 to 2.0 percent by weight of a secondary nonionic surfactant having an HLB value of 1.8-15;

(D) stirring the mixture until the particle size of the polysiloxane in the mixture is in the range of 1-100 microns; and

(E) adding a second portion of water to the mixture in an amount to provide a total content of water in the product of 25-65 percent by weight based on the total weight of the mixture, the second portion of water being added to the mixture gradually over a period of time in a series of from about five to about ten separate incremental steps.

2. A method according to claim 1 in which the first portion of water includes a thickening agent.

3. A method according to claim 2 in which the second portion of water includes a thickening agent.

4. A method according to claim 3 in which the thickening agent is present in an amount of less than about three percent by weight based on the total weight of the mixture.

5. A method according to claim 1 in which the polysiloxane content in the mixture is 35-70 percent by weight.

6. A method according to claim 1 in which the polysiloxane is selected from the group consisting of high viscosity polysiloxanes, bi-modal polysiloxane fluids, functional polysiloxanes, and mixtures thereof.

7. A method according to claim 6 wherein the polysiloxane is a high viscosity polysiloxane having the formula:

##STR6## wherein each R is independently selected from the group consisting of the hydrogen atom, an alkyl group having at least one carbon atom, and an aryl group having 6 to 10 carbon atoms; and

each R¹ is independently selected from R, hydroxy groups, and alkoxy groups; and

w has the value such that the viscosity is at least 1,000 centistokes at 25°

C.

8. A method according to claim 7 wherein the polysiloxane has a viscosity of at least 10,000 centistokes at 25°

C.

9. A method according to claim 6 wherein the polysiloxane is a bi-modal polysiloxane fluid including at least one low viscosity polysiloxane and at least one high viscosity, nonvolatile polysiloxane.

10. A method according to claim 6 wherein the polysiloxane is a functional polysiloxanes having the formula ##STR7## wherein each R² is independently selected from the group consisting of R¹, aminoalkyl functional groups containing at least one carbon atom, carboxyalkyl functional groups containing at least one carbon atom, haloalkyl functional groups containing at least one carbon atom, acrylate functional groups, acryloxy functional groups, acrylamide functional groups, vinyl functional groups, and functional groups having the formula Q--R³ -- where Q is a functional group containing at least one atom which is not a carbon or hydrogen atom and R³ is selected from an alkylene group having at least one carbon atom and an arylene group having 6 to 10 carbon atoms;

z has a value of at least 10; and

R¹ is hydrogen, an alkyl group having at least one carbon atom, or an aryl group having 6-10 carbon atoms.

11. An emulsion prepared in accordance with the method described in claim 1.

12. A method of making an emulsion comprising the steps of (A) forming a mixture by combining 35 to 75 percent by weight of a polysiloxane and 0.25 to 2.0 percent by weight of a primary nonionic surfactant having an HLB value of 10 to 19, and stirring the mixture until uniform:

(B) adding and dispersing 3-6 percent by weight of a first portion of surfactant free water in the mixture, the first portion of surfactant free water being added and dispersed in the mixture gradually over a period of time in a series of a plurality of separate incremental steps;

(C) adding to the mixture 0.25 to 2.0 percent by weight of a secondary nonionic surfactant having an HLB value of 1.8-15;

(D) stirring the mixture until the particle size of the polysiloxane in the mixture is in the range of 1-100 microns; and

(E) adding a second portion of water to the mixture in an amount to provide a total content of water in the product of 25-65 percent by weight based on the total weight of the mixture, the second portion of water being added to the mixture gradually over a period of time in a series of a plurality of separate incremental steps.

13. An emulsion prepared in accordance with the method described in claim 12.