高相对分子质量间苯撑硫醚-对苯撑硫醚的合成  

Synthesis of High Molecular Weight Poly(metaphenylene sulfide-paraphenylene sulfide)

作　　者：熊章星 蒋文伟[1] 吴小园 杨琴 罗芩 XIONG Zhang-xing;JIANG Wen-wei;WU Xiao-yuan＇;YANG Qin;LUO Qin(School of Chemical Engineering,Sichuan University,Chengdu 610065,Sichuan,China;Chengdu Huien Fine Chemical Co.,Chengdu 610065,Sichuan,China)

机构地区：[1]四川大学化学工程学院,四川成都610065 [2]成都惠恩精细化工有限责任公司,四川成都610065

出　　处：《合成纤维》2018年第6期23-27,共5页Synthetic Fiber in China

摘　　要：以硫氢化钠、氢氧化钠、对二氯苯、间二氯苯为主要原料,有机锂盐和无水乙酸钠为催化剂和助剂,N-甲基吡咯烷酮（NMP）为极性有机溶剂,在2 L高压反应釜内于220~250℃反应6 h合成间苯撑硫醚-对苯撑硫醚树脂（m-p-PPS）。为提高树脂的相对分子质量,在反应后期加入活性单体4,4＇-二氯二苯甲酮（DCBP）共聚得到间苯摩尔分数为10%~40%的系列m-p-PPS共聚物。对合成的共聚物进行特性黏度测试、红外光谱分析、X-射线衍射分析、热分析及溶解性能测试等分析表征工作,结果表明：共聚物为部分结晶性线型高分子,随着间苯含量的增加,共聚物相对分子质量降低,结晶能力减弱,热稳定性降低,而溶解性能增强;添加少量DCBP对树脂结构影响不大,但能有效提高树脂的相对分子质量。Poly（metaphenylene sultlde-parapnenylene suulue）resin （m-p-PPS） was prepared from sodium hydrosulphide, sodium hydroxide, p-dichlorobenzene and m-dichlorobenzene. It was successfully synthe- sized in a 2 L autoclave at 220-250℃ for 6 hours, with the organic lithium salt and the anhydrous sodium acetate as the catalyst and auxiliary, the N-methylpyrrolidone （NMP） as the polar organic solvent. In order to improve the molecular weight of resin, as the active monomer, 4,4＂-dichlorobenzophenone （DCBP） was added in the later period. A series of m-p-PPS copolymers containing meta-phenylene units were synthe- sized. Copolymers were characterized by intrinsic viscosity test, FTIR spectrum, X-ray diffraction spec- trum, thermal analysis and solubility properties test, and the results of experiments indicate that the copoly- mers are linear and partial crystalline. The molecular weight, crystalline ability and thermal stability de- crease with the increase of meta-phenylene content, but the solubility properties enhance instead. The small amounts of the active monomer has a little influence on the structure of the m-p-PPS, but it can in- crease the molecular weight of the resin effectively.

关 键 词：间二氯苯 合成 间苯撑硫醚-对苯撑硫醚 4 4'-二氯二苯甲酮 表征 

分 类 号：TQ314.2[化学工程—高聚物工业]