US 9,809,686 B2
Division of a polyarylene ether solution
Joerg Erbes, Karlsruhe (DE); Stefan Muessig, Ludwigshafen (DE); Tobias Kortekamp, Mannheim (DE); Marco Krueger, Mannheim (DE); Markus Steffen, Maikammer (DE); Angela Ulzhoefer, Ludwigshafen (DE); Cecile Schneider, Frankenthal (DE); Alexandra Wiedemann, Weisenheim am Berg (DE); and Simon Gramlich, Hirschberg (DE)
Assigned to BASF SE, Ludwigshafen (DE)
Appl. No. 14/904,614
Filed by BASF SE, Ludwigshafen (DE)
PCT Filed Jul. 16, 2014, PCT No. PCT/EP2014/065240
§ 371(c)(1), (2) Date Jan. 12, 2016,
PCT Pub. No. WO2015/007774, PCT Pub. Date Jan. 22, 2015.
Claims priority of application No. 13176993 (EP), filed on Jul. 18, 2013.
Prior Publication US 2016/0159990 A1, Jun. 9, 2016
This patent is subject to a terminal disclaimer.
Int. Cl. C08G 75/00 (2006.01); C08J 3/14 (2006.01); C08J 3/12 (2006.01); C08G 65/46 (2006.01); C08G 75/23 (2006.01); B29C 47/00 (2006.01); B29K 81/00 (2006.01)
CPC C08J 3/14 (2013.01) [B29C 47/0011 (2013.01); C08G 65/46 (2013.01); C08G 75/23 (2013.01); C08J 3/12 (2013.01); B29K 2081/06 (2013.01); C08J 2381/06 (2013.01); C08J 2381/08 (2013.01)] 11 Claims
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,
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 Tc, where the critical temperature Tc in [° C.] is determined by the numerical equation Tc=(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 cc, where the critical concentration cc in [% by weight] is determined by the numerical equation cc=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.