Process for preparation of organopolysiloxanes

• US 5,130,399 A
• Filed: 05/20/1991
• Issued: 07/14/1992
• Est. Priority Date: 05/22/1990
• Status: Expired due to Fees

• Current Assignee: Shin-Etsu Chemical Company Limited
• Original Assignee: Shin-Etsu Chemical Company Limited
• Inventors: Ikeno, Masayuki, Hara, Hiroyasu
• Primary Examiner(s): Bleutge, John C.
• Assistant Examiner(s): MOORE, MARGARET G
• Application Number:
  US07/702,299
• Time in Patent Office: 421 Days
• Field of Search: 528/14, 528/33
• US Class Current: 528/14
• CPC Class Codes: C08G 77/06 Preparatory processes C08G77/045 takes precedence

Abstract

The present process for producing an organopolysiloxane is characterized in that the polymerization of an organosiloxane by using an alkali catalyst is carried out in the presence of a reversible dehydrating agent such as magnesium sulfate and calcium carbonate or an irreversible dehydrating agent such as calcium oxide. According to this manufacturing process, there is a quite distinct mutual relation between the preset composition of the organopolysiloxane to be manufactured and the viscosity of the actually manufactured organopolysiloxane.

Claims

1. A process for producing an organopolysiloxane, comprising polymerizing an organosiloxane using an alkali catalyst in the presence of a dehydrating agent.

2. A process as claimed in claim 1, wherein said dehydrating agent is at least one reversible dehydrating agent selected from the group consisting of magnesium sulfate, calcium sulfate, sodium sulfate, calcium carbonate, and alumina.

3. A process as claimed in claim 2, wherein said dehydrating agent is present in an amount of 0.15 to 1.5% by weight based on the organosiloxane.

4. A process as claimed in claim 1, wherein said dehydrating agent is at least one irreversible dehydrating agent selected from the group consisting of calcium oxide and barium oxide.

5. A process as claimed in claim 3, wherein said dehydrating agent is present in an amount of 0.15 to 1.5% by weight based on the organosiloxane.

6. A process as claimed in claim 1, wherein said alkali catalyst is at least one selected from the group consisting of alkali metal compounds, alkylphosphonium hydroxides, alkylammonium hydroxides, and 1,8-diazabicyclo(5.4.0)undecene-7.

7. A process as claimed in claim 6, wherein said alkali catalyst is an alkylphosphonium hydroxide or an alkylammonium hydroxide and the polymerization is carried out at a temperature of 100°

to 130°

C.

8. A process as claimed in claim 7, wherein said alkali catalyst is used in an amount of 0.001 to 0.1% by weight based on the raw material organosiloxane.

9. A process as claimed in claim 6, wherein said alkali catalyst is at least one alkali metal compound selected from the group consisting of NaOH, KOH, sodium silanolates, and potassium silanolates and the polymerization is carried out at a temperature of 130°

to 160°

C.

10. A process as claimed in claim 9, wherein the dehydrating agent is an irreversible dehydrating agent.

11. A process as claimed in claim 9, wherein said alkali catalyst is used in an amount such that the molar ratio of the silicon atoms in the organosiloxane to the alkali metal atom ranges from 2,000 to 5,000.

12. A process as claimed in claim 1, wherein said organosiloxane is at least one member selected from the group consisting of cyclic diorganosiloxane oligomers represented by the following formula:

##STR4## wherein R represents a substituted or unsubstituted monovalent hydrocarbon group having 1 to 10 carbon atoms and p is an integer of 3 to 10,

linear diorganosiloxane oligomers represented by the following formula;

##STR5## wherein R has the same meaning as defined above and q is an integer of 2 to 10,

and linear diorganosiloxane oligomers represented by the following formula;

##STR6## wherein R has the same meaning as defined above and r is an integer of 0 to 10.