Method for continuous production of polycarbonate-polyorganosiloxane copolymer

Patent metadata

Field	Value
Publication number	US-9359473-B2
Application number	US-201314434486-A
Country	US
Kind code	B2
Filing date	Oct 10, 2013
Priority date	Oct 12, 2012
Publication date	Jun 7, 2016
Grant date	Jun 7, 2016

Abstract

Provided is a method for economically and stably producing a high-quality polycarbonate-polyorganosiloxane copolymer excellent in, for example, transparency and impact resistance in a continuous manner. Specifically, provided is a method of continuously producing a polycarbonate-polyorganosiloxane copolymer, the method including a step (A) of continuously or intermittently taking a polymerization reaction liquid, which is obtained by polymerizing a dihydric phenol-based compound, a carbonate precursor, and a polyorganosiloxane in the presence of an alkaline compound aqueous solution and a water-insoluble organic solvent, out of a reactor, the step (A) including the following step (a-1) and the following step (a-2), the method using a dissolution tank for dissolving the dihydric phenol-based compound in the alkaline compound aqueous solution to prepare an alkaline compound aqueous solution of the dihydric phenol-based compound to be used in each of both the step (a-1) and the step (a-2), the step (a-2) including, before mixing a polycarbonate oligomer and the dihydric phenol-based compound, mixing the alkaline compound aqueous solution and the alkaline compound aqueous solution of the dihydric phenol-based compound prepared in the dissolution tank: step (a-1): a step of mixing the alkaline compound aqueous solution of the dihydric phenol-based compound prepared in the dissolution tank and the polycarbonate precursor, followed by a reaction of the mixture in the presence of the water-insoluble organic solvent to produce the polycarbonate oligomer; and step (a-2): a step of continuously or intermittently taking the polymerization reaction liquid, which is obtained by mixing the alkaline compound aqueous solution of the dihydric phenol-based compound prepared in the dissolution tank, the polycarbonate oligomer obtained in the step (a-1), and the polyorganosiloxane, and polymerizing the mixture in the presence of the water-insoluble organic solvent, out of the reactor.

First claim

The invention claimed is:

1. A method of continuously producing a polycarbonate-polyorganosiloxane copolymer by polymerizing a dihydric phenol-based compound, a carbonate precursor, and a polyorganosiloxane in a presence of a water-insoluble organic solvent and an alkaline compound aqueous solution comprising said dihydric phenol-based compound, wherein said method comprises:
(i) dissolving, in a dissolution tank, said dihydric phenol-based compound in the alkaline compound aqueous solution,

and said method further comprises step (a-1) and step (a-2)
wherein step (a-1) comprises
mixing the solution prepared in (i) and said carbonate precursor to provide a mixed solution,
preparing a polycarbonate oligomer by reacting the mixed solution in the presence of the water-insoluble organic solvent,

wherein step (a-2) comprises
preparing a preliminary polymerization product by reacting said polycarbonate oligomer with a polyorganosiloxane,
mixing the alkaline compound aqueous solution and the solution prepared in (i) to provide a diluted alkaline compound aqueous solution comprising the dihydric phenol-based compound, and
forming a polycarbonate-polyorganosiloxane copolymer by polymerizing the preliminary polymerized product and the diluted alkaline compound aqueous solution comprising the dihydric phenol-based compound in the presence of a water-insoluble organic solvent, and continuously or intermittently removing a polymerization reaction liquid from the reactor.

2. The method according to claim 1 , wherein in the dissolution tank, an alkaline compound aqueous solution of the dihydric phenol-based compound having a concentration of the dihydric phenol-based compound of 8 to 20% by mass and a concentration of an alkaline compound of 3 to 10% by mass is prepared.

3. The method according to claim 1 , wherein in the diluted alkaline compound aqueous solution, a concentration of the dihydric phenol-based compound is 5 to 12% by mass and a concentration of an alkaline compound is 5 to 20% by mass.

4. The method according to claim 1 , wherein in said forming a polycarbonate-polyorganosiloxane copolymer, a water content, is 35% by volume or less.

5. The method according to claim 1 , wherein in said forming a polycarbonate-polyorganosiloxane copolymer the polymerizing is performed in a mixer provided with a turbine blade.

6. The method according to claim 1 , wherein the dihydric phenol-based compound is a compound of formula (1) and the polyorganosiloxane is a compound of formula (2):

wherein R′ and R 2 each independently represent a halogen atom, an alkyl group having 1 to 6 carbon atoms, or an alkoxy group having 1 to 6 carbon atoms, X represents a single bond, an alkylene group having 1 to 8 carbon atoms, an alkylidene group having 2 to 8 carbon atoms, a cycloalkylene group having 5 to 15 carbon atoms, a cycloalkylidene group having 5 to 15 carbon atoms, 13 S—, —SO—, —SO 2 —, —O—, or —CO—, and a and b each independently represent an integer of 0 to 4;

wherein R 3 to R 6 each independently represent a hydrogen atom, a halogen atom, an alkyl group having 1 to 6 carbon atoms, an alkoxy group having 1 to 6 carbon atoms, or an aryl group having 6 to 12 carbon atoms, Y represents a single bond, or an organic residue including an aliphatic or aromatic moiety, n represents an average number of repetitions, Z represents a halogen atom, —R 7 OH, —R 7 —Z′—R 8 —OH, —R 7 COOH, —R 7 NH 2 , —COOH, or —SH, the R 7 represents a substituted or unsubstituted alkylene group, a substituted or unsubstituted cycloalkylene group, or a substituted or unsubstituted arylene group, the R 8 represents an arylene group having 6 to 12 ring-forming carbon atoms, the Z′ represents an alkylene group having 1 to 8 carbon atoms, an alkylidene group having 2 to 8 carbon atoms, a cycloalkylene group having 5 to 10 carbon atoms, or a cycloalkylidene group having 5 to 10 carbon atoms, and m represents 0 or 1.

7. The method according to claim 6 , wherein n in formula (2) represents 25 to 120.

8. The method according to claim 6 , wherein n in formula (2) represents 70 to 120.

9. The method according to claim 1 , wherein the alkaline compound in said alkaline compound aqueous solution is an alkaline inorganic compound.

10. The method according to claim 9 , wherein the alkaline inorganic compound is an alkali metal hydroxide.

11. The method according to claim 9 , wherein the alkaline inorganic compound is an alkaline earth metal hydroFxide.

Assignees

• Idemitsu Kosan Co

Inventors

• Nagao Yukiko
• Ishikawa Yasuhiro
• Motegi Hiroaki

Classifications

• C08G77/448

  containing polycarbonate sequences · CPC title

• C08G64/24

  and phenols · CPC title

• C08G64/186 Primary

  containing polysiloxane sequences · CPC title

• C08G77/04

  Polysiloxanes · CPC title

• C08G64/205

  characterised by the apparatus used · CPC title