Patent ID: 9567440
Date: 2017-02-14
CPC Classifications: C08G

Claim:
1. A fiber-grade polyphenylene sulfide resin synthesis method, characterized in that the method uses sodium bisulfide and p-dichlorobenzene as raw materials, N-methyl pyrrolidone as a solvent and C5-C6 fatty acid salt as a polymerization additive for synthesis through polymerization, characterized further in that the C5-C6 fatty acid salt is C5-C6 fatty acid sodium salt, and characterized further in the following reaction steps: (1) adding NMP, 40%-50% NaOH solution and C5-C6 fatty acid into the reactor for heating to the temperature of 90-120° C. simultaneously with mixing and nitrogen protection at the velocity of 1.0˜2.0° C./min; proceeding with heat preservation for 1-3 hours before prior to further heating to temperature of 180˜200° C. at the velocity of 1.0˜2.0° C./min for dehydration; reducing temperature to 110˜130° C. after dehydration; (2) adding NaHS solution and NMP into the reactor following Step (1) for heating to temperature of 180˜200° C. at the velocity of 0.7˜1.5° C./min simultaneously with mixing and nitrogen protection prior to dehydration; further reducing temperature to 140˜160° C. when water content in the system is below 1.0 mol/mol sulfur; (3) adding PDCB and NMP into the reactor following Step (2) for heating to the temperature of 220˜240° C. within 1.0-1.5 hours prior to heat preservation for 1-3 hours; further proceeding with heating to temperature of 260˜280° C. at the velocity of 1.0˜1.5° C./min prior to heat preservation for 1-3 hours; once completed, reducing temperature to 130˜150° C. within 0.5-1 hour to obtain PPS reaction slurry; (4) proceeding with centrifugation of PPS reaction slurry as obtained through Step (3), then leaching with 130˜150° C. NMP of the same mass as the filter cake; further proceeding with leaching with hydrochloric acid solution of the same mass as the filter cake prior to mixing and collection of all filtrate; (5) repeatedly washing the filter cake as obtained in Step (4) with 70˜100° C. deionized water; further drying the filter cake to obtain polyphenylene sulfide resin.