Preparation of polyorganosiloxanes by interfacial polymerization

• US 5,637,668 A
• Filed: 04/01/1996
• Issued: 06/10/1997
• Est. Priority Date: 04/01/1996
• Status: Expired due to Fees

• Current Assignee: Dow Corning Corporation (Dow, Inc.), University of South Australia (University of Adelaide)
• Original Assignee: Dow Corning Corporation (Dow, Inc.), University of South Australia (University of Adelaide)
• Inventors: Matisons, Jani G., Provatas, Arthur, Graiver, Daniel, Lomas, Arnold W.
• Primary Examiner(s): DEAN JR, RALPH H
• Application Number:
  US08/625,983
• Time in Patent Office: 435 Days
• Field of Search: 528/14, 528/33, 528/34
• US Class Current: 528/33
• CPC Class Codes: C08G 77/06 Preparatory processes C08G77/045 takes precedence
• CPC Class Codes: C08G 77/44 containing only polysiloxane sequences

Abstract

A process for manufacturing high molecular weight polysiloxane copolymers by interfacial polymerization. The polysiloxanes may contain phenylmethyl siloxane blocks and dimethyl siloxane blocks, alternately polymerized together to form an (A_m B_n)_x type copolymer. The interfacial polymerization process is fast, proceeds smoothly at room temperature, and is not reversible, i.e., no cyclic siloxane species are generated. The polysiloxanes can be formed as thermoplastic elastomers suitable for use as sealants, fillers, and films.

Claims

1. A method of making a block copolymer comprising (A) reacting (i) a first nonaqueous organic solvent solution of an alpha, omega-dihalopolydiorganosiloxane at or near an interface formed by the first nonaqueous organic solvent solution and (ii) a second immiscible nonaqueous organic solvent solution of a silanolate or organosilanolate of formula R"_x Si(OM)_4-x or MO(R"₂ SiO)_n M where R" is an alkyl radical of 1-6 carbon atoms, an aryl radical, an alkenyl radical, or an alkylamino radical;

x is 0-2;

n is at least one; and

M is an alkali metal;

the second solvent being immiscible in the first solvent, and organic groups on the alpha, omega-dihalopolydiorganosiloxane being different from organo groups on the silanolate or organosilanolate; and

(B) recovering the block copolymer at or near the interface.

2. A method according to claim 1 in which the first organic solvent is acetonitrile and the second organic solvent is cyclohexane.

3. A method according to claim 1 in which the alpha, omega-dihaloorganosiloxane is selected from the group consisting of 1,3-dichloro-1,3-dimethyl-1,3-diphenyldisiloxane,

1,5-dichlorohexamethyltrisiloxane,

1,7-dichlorooctamethyltetrasiloxane,

1,3-dichlorotetraisopropyldisiloxane,

1,3-dichlorotetramethyldisiloxane, and

1,3-dichlorotetraphenyldisiloxane.

4. A method according to claim 1 in which the silanolate or organosilanolate has the formula MO(R"₂ SiO)_n M where R" is an alkyl radical of 1-6 carbon atoms, an aryl radical, an alkenyl radical, or an alkylamino radical;

n is 1-20; and

M is an alkali metal.

5. A method according to claim 4 in which the silanolate or organosilanolate is potassium phenylmethylsilanolate of the formula KO[(C₆ H₅)(CH₃)SiO]_n K where n is 4-8.

6. A method according to claim 2 in which the alpha, omega-dihaloorganosiloxane is selected from the group consisting of 1,3-dichloro-1,3-dimethyl-1,3-diphenyldisiloxane,

1,5-dichlorohexamethyltrisiloxane,

1,7-dichlorooctamethyltetrasiloxane,

1,3-dichlorotetraisopropyldisiloxane,

1,3-dichlorotetramethyldisiloxane, and

1,3-dichlorotetraphenyldisiloxane.

7. A method according to claim 2 in which the silanolate or organosilanolate has the formula MO(R"₂ SiO)_n M where R" is an alkyl radical of 1-6 carbon atoms, an aryl radical, an alkenyl radical, or an alkylamino radical;

n is 1-20; and

M is an alkali metal.

8. A method according to claim 7 in which the silanolate or organosilanolate is potassium phenylmethylsilanolate of the formula KO[(C₆ H₅)(CH₃)SiO]_n K where n is 4-8.