Continuous production of polycarbonates

• US 3,945,969 A
• Filed: 02/01/1974
• Issued: 03/23/1976
• Est. Priority Date: 02/02/1973
• Status: Expired due to Term

• Current Assignee: BASF AG (BASF SE)
• Original Assignee: BASF AG (BASF SE)
• Inventors: Horn, Peter, Kuerten, Heribert
• Primary Examiner(s): Briggs, Sr., Wilbert J.
• Application Number:
  US05/438,753
• Time in Patent Office: 781 Days
• Field of Search: 260/47 XA, 260/77.5 D, 260/49
• US Class Current: 526/64
• CPC Class Codes: C08G 64/205 characterised by the apparatus used

Abstract

High molecular weight linear polycarbonates are prepared by continuous condensation of organic dihydroxy compounds and phosgene in two reaction zones, a mixture of an aqueous-alkaline solution of the organic dihydroxy compound and an aqueous catalyst solution being introduced at the rate of from 1 to 50 meters per second and the phosgene at the rate of from 30 to 300 meters per second into the first reaction zone and condensed, an organic solvent being incorporated into the resultant reaction mixture containing oligomer and polycarbonate and the condensation of the aqueous-organic reaction mixture carried to completion in the second reaction zone by the two-phase interfacial method.

Claims

1. A process for the continuous production of a high molecular weight polycarbonate by reaction of an organic dihydroxy compound selected from the group consisting of hydroquinone, resorcinol, pyrocatechol, 1,2-dihydroxynaphthalene, 1,4-dihydroxynaphthalene, 1,5-dihydroxynaphthalene, 4,4'"'"'-dihydroxydiphenyl, 2,2'"'"'-dihydroxydiphenyl, 4,4'"'"'-dihydroxydiphenyl sulfide, 4,4'"'"'-dihydroxydiphenyl sulfoxide, 2,2'"'"'-dihydroxydiphenylsulfone, 4,4'"'"'-dihydroxydiphenyl-sulfone, 4,4'"'"'-dihydroxydiphenyl ether, 4,4'"'"'-dihydroxybenzophenone, 1,1-(4,4'"'"'-dihydroxydiphenyl)-1-phenylethane, 1,1-(4,4'"'"'-dihydroxydiphenyl)-cyclohexane, 4,4'"'"'-dihydroxydiphenylmethane and 2,2-(4,4'"'"'-dihydroxydiphenyl)-propane with phosgene in the presence of an amine or a salt of the same wherein the reaction is carried out in a plurality of reaction zones, a mixture of an aqueous-alkaline solution (a) of the organic compound and an aqueous solution of the amine or amine salt being introduced at the rate of from 1 to 50 meters per second and the phosgene (b) at the rate of from 30 to 300 meters per second in a first mixing and reaction zone, and condensed in said first mixing and reaction zone in a mainly aqueous alkaline solution to polycarbonate oligomers or polycarbonate, an organic solvent being introduced into said first mixing and reaction zone and incorporated into the mainly aqueous solution containing polycarbonate oligomers and polycarbonate at a point located in half removed from the inlet orifice for the aqueous-alkaline solution (a) and phosgene (b) or adjacent to the point of transition into the second reaction zone in such a way that back-mixing of the organic solvent containing polycarbonate oligomers or polycarbonate with the aqueous solution does not take place or only takes place to a trivial extent, and the condensation of the aqueous organic reaction mixture being carried to completion in a second reaction zone by the two-phase interfacial method.

2. A process for the continuous production of a high molecular weight polycarbonate as claimed in claim 1 wherein the first mixing and reaction zone has an internal diameter which is from three to thirty times the means internal diameter of the stream of reactants supplied and the length of the mixing and reaction zone is from once to 20 times its diameter.

3. A process for the continuous production of high molecular weight polycarbonates as claimed in claim 1 wherein the second reaction zone has a dissipation density of from 10 to 3 ×

10⁴ KW/m³ and the ratio of the length to the diameter in the second reaction zone is from 5;

1 to 40;

1.

4. A process as claimed in claim 1 wherein the organic dihydroxy compound used is 4,4'"'"'-dihydroxydiphenylmethane or 2,2-(4,4'"'"'-dihydroxydiphenyl)-propane.

5. A process as claimed in claim 1 wherein the amount of solvent is such that the volumetric ratio of liquid aqueous reaction solution to organic solvent is from 1:

0.3 to 1;

2 and the reaction mixture thereafter has a solids content of from 3 to 20% by weight based on the total weight of the reaction mixture.

6. A process as claimed in claim 5 wherein the said ratio is from 1:

0.4 to 1;

1.

7. A process as claimed in claim 5 wherein the said ratio is about 1:

0.5.

8. A process as claimed in claim 5 wherein the solids content is from 15 to 25% by weight.

9. A process as claimed in claim 1 carried out at a temperature of from 25°

to 90°

C.

10. A process as claimed in claim 1 carried out at a temperature of from 35°

to 50°

C.

11. A process as claimed in claim 1 carried out at a pH of the reaction solution of from 8 to 13.5.

12. A process as claimed in claim 1 carried out at a pH of the reaction solution of from 8.5 to 10.5.

13. A process as claimed in claim 1 wherein the reaction solution is introduced at a speed of from 3 to 30 meters per second.

14. A process as claimed in claim 1 wherein the phosgene is introduced at a speed of from 5 to 200 meters per second.

15. A process as claimed in claim 1 wherein the first mixing and reaction zone has a mean internal diameter which is from 10 to 25 times the mean internal diameter of the stream of reactants supplied.

16. A process as claimed in claim 1 wherein the length of the mixing and reaction zone is from one and one half to five times its diameter.

17. A process as claimed in claim 1 wherein the first mixing and reaction zone is not circular and/or does not have constant cross-section throughout and its length is from once to 20 times its hydraulic diameter, as herein defined.

18. A process as claimed in claim 17 wherein the length of the first mixing and reaction zone is from one and one half to five times its hydraulic diameter.