Method for precipitation of polyphenylene ether
View Patent ↗Method for precipitating polyphenylene ether which decreases fine particles therein and reduces periodic fluctuations in particle size. Method provides homogeneous polyphenylene ether particles. Polyphenylene ether particles are precipitated using mixed solution comprising good solvent for polyphenylene ether and poor solvent for polyphenylene ether. Method employs precipitation tank equipped with draft tube, stirring blade, baffle(s), solution supply port, poor solvent supply port, and exhaust port. Polyphenylene ether particles and poor solvent are added to mixed solution comprising good solvent and circularly flowed by rotation of stirring blade, polyphenylene ether solution for solution supply port, and poor solvent for poor solvent supply port, thereby precipitating polyphenylene ether particles having desired properties.
1. A method for precipitating polyphenylene ether by mixing a polyphenylene ether solution comprising polyphenylene ether and a good solvent therefor with a poor solvent for polyphenylene ether to precipitate polyphenylene ether particles, the method comprising:
using a precipitation tank equipped with (a) a draft tube, (b) an at least one-stage stirring blade disposed in the draft tube and selected from an inclined paddle blade, a screw blade and a ribbon blade, (c) one or more baffles disposed on the outside of the draft tube, (d) a solution supply port, (e) a poor solvent supply port and (f) an exhaust port;
adding, to a mixed solution comprising the good solvent, the poor solvent and polyphenylene ether particles and circularly flowing by rotation of the stirring blade (b), the polyphenylene ether solution from the solution supply port (d) and concurrently a poor solvent from the poor solvent supply port (e), thereby precipitating polyphenylene ether particles; and
discharging and recovering the precipitated polyphenylene ether particles together with the mixed solution from the exhaust port (f).
2. The method for precipitating polyphenylene ether according to claim 1 , wherein the mixed solution is overflowed from the exhaust port (f) to discharge the polyphenylene ether particles from the precipitation tank.
3. The method for precipitating polyphenylene ether according to claim 1 , wherein the ratio of the precipitation tank diameter/liquid height of the mixed solution in the precipitation tank is from 0.1 to 2, the ratio of the height of the draft tube/said liquid height is from 0.05 to 0.6, and the ratio of a vertical interval between a liquid level and the most upper portion of the draft tube/said liquid height is from 0.01 to 0.3.
4. The method for precipitating polyphenylene ether according to claim 1 , wherein the good solvent for polyphenylene ether comprises at least one solvent selected from benzene, toluene and xylene, and the poor solvent for polyphenylene ether comprises at least one solvent selected from methanol, ethanol, isopropanol, n-butanol, acetone, methyl ethyl ketone and water.
5. The method for precipitating polyphenylene ether according to claim 1 , wherein the weight ratio of the poor solvent/the good solvent in the mixed solution is from 0.3 to 2.0.
6. The method for precipitating polyphenylene ether according to claim 1 , wherein the poor solvent contains water in an amount of 0.3 to 50 parts by weight.
7. The method for precipitating polyphenylene ether according to claim 1 , wherein the mixed solution has a temperature of from 30 to 60° C.
8. The method for precipitating polyphenylene ether according to claim 1 , giving an average residence time during which the polyphenylene ether particles stay in the precipitation tank of from 2.0 to 30 minutes.