Division of a polyarylene ether solution

Patent metadata

Field	Value
Publication number	US-9828472-B2
Application number	US-201414904491-A
Country	US
Kind code	B2
Filing date	Jul 16, 2014
Priority date	Jul 18, 2013
Publication date	Nov 28, 2017
Grant date	Nov 28, 2017

Abstract

Process for producing polyarylene ether beads from a polyarylene ether solution, comprising the steps of
i) dividing the polyarylene ether solution into droplets, ii) transferring the droplets into a precipitation bath to form polyarylene ether beads in the precipitation bath which (A) comprises at least one aprotic solvent (component (1)) and at least one protic solvent (component (2)), (B) has a temperature of 0° C. to T c , where the critical temperature T c in [° C.] can be determined by the numerical equation T c =(77−c)/0.58 in which c is the concentration of component (1) in the precipitation bath in [% by weight] and (C) has component (1) in concentrations of 5% by weight to c c , where the critical concentration c c in [% by weight] can be determined by the numerical equation c c =77−0.58*T in which T is the temperature in the precipitation bath in [° C.], where

the percentages by weight are each based on the sum of the percentages by weight of component (1) and of component (2) in the precipitation bath.

First claim

The invention claimed is:

1. A process for producing polyarylene ether beads from a polyarylene ether solution, the process comprising:
i) dividing the polyarylene ether solution into droplets; and
ii) transferring the droplets into a precipitation bath to form polyarylene ether beads in the precipitation bath,
wherein the precipitation bath
(A) comprises at least one aprotic solvent (component (1)) and at least one protic solvent (component (2));
(B) has a temperature of 0° C. to T c , where the critical temperature T c in [° C.] can be determined by the numerical equation T c =(77−c)/0.58 in which c is the concentration of component (1) in the precipitation bath in [% by weight] and
(C) has component (1) in a concentration of 12 to 70% by weight, where the percentage by weight is based on the sum of the percentages by weight of component (1) and of component (2) in the precipitation bath,
wherein the precipitation bath comprises water or alcohol as component (2),
wherein the polyarylene ether solution has a concentration of 5 to 50% by weight of polyarylene ether in the aprotic solvent, where the percentage by weight are based on the sum of the percentages by weight of the polyarylene ether and the aprotic solvent,
wherein the polyarylene ether solution in the dividing has a temperature of 15 to 250° C.,
wherein the aprotic solvent is at least one selected from the group consisting of N-methyl-2-pyrrolidone and N-ethyl-2-pyrrolidone, and
wherein, in the polyarylene ether beads precipitated from the precipitation bath in (ii), the content of particles having a particle size of less than or equal to 1000 μm is less than 1.3% by weight.

2. The process according to claim 1 ,
wherein the precipitation bath is agitated.

3. The process according to claim 1 ,
wherein the polyarylene ether solution in the dividing has a temperature of 20 to 120° C.

4. The process according to claim 1 ,
wherein the polyarylene ether solution after leaving a division apparatus covers a full distance from an exit point to a precipitation bath surface of 0.10 m to 1.20 m.

5. The process according to claim 1 ,
wherein a division apparatus comprises a capillary or die plate.

6. The process according to claim 5 ,
wherein the capillary or die plate has a diameter of 0.1 to 5.0 mm.

7. The process according to claim 1 ,
wherein the polyarylene ether solution and the precipitation bath comprise the same aprotic solvent.

8. The process according to claim 1 ,
wherein the precipitation bath comprises 12 to 50% by weight, of component (1), where the percentages by weight are each based on the sum of the percentages by weight of component (1) and component (2) in the precipitation bath.

9. The process according to claim 1 , further comprising stirring the precipitation bath when transferring the droplets into the precipitation bath.

10. The process according to claim 1 , wherein the polyarylene ether beads are individual beads which are not agglomerated.

11. The process of claim 1 , wherein, in the polyarylene ether beads precipitated from the precipitation bath in (ii), the content of particles having a particle size of less than or equal to 1000 μm is 0.93% by weight or less.

12. The process according to claim 1 , wherein the polyarylene ether beads are individual beads which are not agglomerated.

13. A process for producing polyarylene ether beads of claim 1 from a polyarylene ether solution, the process comprising:
i) dividing the polyarylene ether solution into droplets; and
ii) transferring the droplets into a precipitation bath to form polyarylene ether beads in the precipitation bath,
wherein the precipitation bath
(A) comprises at least one aprotic solvent (component (1)) and at least one protic solvent (component (2));
(B) has a temperature of 0° C. to T c , where the critical temperature T c in [° C.] can be determined by the numerical equation T c =(77−c)/0.58 in which c is the concentration of component (1) in the precipitation bath in [% by weight] and
(C) has component (1) in a concentration of 12 to 70% by weight, where the percentage by weight is based on the sum of the percentages by weight of component (1) and of component (2) in the precipitation bath,
wherein the precipitation bath comprises water or alcohol as component (2),
wherein the polyarylene ether solution has a concentration of 5 to 50% by weight of polyarylene ether in the aprotic solvent, where the percentage by weight are based on the sum of the percentages by weight of the polyarylene ether and the aprotic solvent,
wherein the polyarylene ether solution in the dividing has a temperature of 15 to 250° C.,
wherein the aprotic solvent is at least one selected from the group consisting of N-methyl-2-pyrrolidone and N-ethyl-2-pyrrolidone, and
wherein the polyarylene ether comprises at least one repeat structural unit selected from the group consisting of:

14. The process of claim 13 , wherein the polyarylene ether comprises at least one repeat structural unit selected from the group consisting of:

15. The process of claim 1 , wherein the aprotic solvent is N-methyl-2-pyrrolidone.

Assignees

• Basf Se

Inventors

• Erbes Joerg
• Lange Gerhard
• Kortekamp Tobias
• Schneider Cecile

Classifications

• C08G65/46

  Post-polymerisation treatment, e.g. recovery, purification, drying · CPC title

• C08J3/12

  Powdering or granulating · CPC title

• C08J3/14 Primary

  by precipitation from solutions {(C08J3/122 takes precedence)} · CPC title

• C08J2381/06

  Polysulfones; Polyethersulfones · CPC title

• C08G75/23

  Polyethersulfones · CPC title