Division of a polyarylene ether solution

Patent metadata

Field	Value
Publication number	US-9809686-B2
Application number	US-201414904614-A
Country	US
Kind code	B2
Filing date	Jul 16, 2014
Priority date	Jul 18, 2013
Publication date	Nov 7, 2017
Grant date	Nov 7, 2017

Abstract

The invention relates to a process for producing polyarylene ether beads from a polyarylene ether solution, comprising the steps of
i) dividing the polyarylene ether solution in a division apparatus which is made to vibrate with a frequency of 10 to 1400 Hz to obtain 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, the process comprising:
i) dividing a polyarylene ether solution in a division apparatus vibrating at a frequency of 10 to 1400 Hz to obtain droplets; and
ii) transferring the droplets into a precipitation bath to form polyarylene ether beads,
wherein:
the precipitation bath satisfies the following conditions
(A) the precipitation bath comprises at least one aprotic solvent (component (1)) and at least one protic solvent (component (2)),
(B) the precipitation bath has a temperature of 0° C. to T c , where the critical temperature T c in [° C.] is determined by the numerical equation T c =(77−c)/0.58 in which c is the concentration of the component (1) in the precipitation bath in [% by weight], and
(C) the precipitation bath has the component (1) in concentrations of 5% by weight to c c , where the critical concentration c c in [% by weight] is determined by the numerical equation c c =77−0.58*T in which T is the temperature in the precipitation bath in [° C.];
percentages by weight are each based on a sum of the percentages by weight of the component (1) and of the component (2) in the precipitation bath;
the precipitation bath comprises water, alcohol, or both, as the component (2);
the polyarylene ether solution has a concentration of 5 to 50% by weight of polyarylene ether in the at least one aprotic solvent, where percentages by weight are based on a sum of the percentages by weight of the polyarylene ether and the at least one aprotic solvent;
the polyarylene ether solution on division has a temperature of 15 to 250° C.;
the aprotic solvent is selected from the group consisting of N-methylpyrrolidone, M-ethylpyrrolidone, dimethyl sulfoxide, dimethylformamide, sulfolane, diphenyl sulfone, 1,2-dichlorobenzene, hexamethylphosphoramide and mixtures thereof; and
wherein, in the polyarylene ether beads precipitated from the precipitation bath in (ii), a content of particles having a particle size of less than or equal to 1000 μm is 2.1% by weight or less.

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 on division has a temperature of 20 to 120° C.

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

5. The process according to claim 1 , wherein the division apparatus comprises capillaries, die plates, or both.

6. The process according to claim 5 , wherein the division apparatus comprises a perforated plate comprising at least one capillary, hole, or both having 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 the 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 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 1.3% by weight or less.

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

Assignees

• Basf Se

Inventors

• Erbes Joerg
• Muessig Stefan
• Kortekamp Tobias
• Krueger Marco
• Steffen Markus
• Ulzhoefer Angela
• Schneider Cecile
• Wiedemann Alexandra
• Gramlich Simon

Classifications

• C08J3/14 Primary

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

• C08J3/12

  Powdering or granulating · CPC title

• B29K2081/06

  PSU, i.e. polysulfones; PES, i.e. polyethersulfones or derivatives thereof · CPC title

• C08G75/23

  Polyethersulfones · CPC title

• B29C48/04

  Particle-shaped (making granules B29B9/00) · CPC title