摘要
以工业硫化钠为硫源,对二氯苯在催化剂和助剂的作用下缩聚合成聚苯硫醚(PPS)。分别考察CH3COONa、PhCOO-Na、Li3PO3、CaL等为催化剂,N,N-二甲基苯胺、2,5-二氯硝基苯、1,2,4-三氯苯、对硝基苯酚等为助剂,三戊胺、环丁砜、N-甲基咪唑(NMI)、N-甲基吡咯烷酮(NMP)、吗啡啉等为溶剂,在170-210℃反应3h,220-240℃反应4h,得到产品PPS。用红外光谱、元素分析、TGA、DSC对所制备PPS进行表征;用特性粘度法测定PPS的相对分子质量(Mr)。结果表明:以NMI为溶剂,添加15%的NMP可代替溶剂NMP合成PPS;以自制的络合物CaL为催化剂、N,N-二甲基苯胺作为助剂,PPS收率在92%以上,tm(熔点)可达289℃,Mr为48 199。
Poly （Phenylene Sulfide） （PPS） was synthesized from Sodium Sulfide and p--dichlorobenzene in the presence of catalysts and additives. Some catalysts （CH3COONa, PhCOONa, Li3PO3, CaL） and some additives （N, N-- dimethylaniline, 2,5-- dichloronitrobenzene, 1,2,4-- trichlorobenzene, p-- nitro-phenol） were investigated, and the solvents （triamylamine, tetramethylene sulfone, N-- methylimidazole （NMI）, N--methylpyrrolidone （NMP）, morpholine） were tested, respectively. The reaction was carried out from 170-210℃ for 3h to 220-240℃ for 4h. The resulting PPS was characterized by FT--IR, Element analysis, TGA and DSC. The molecular weight was determined by intrinsic viscosity method. The results show that： NMI containing 15% NMP can replace NMP as the solvent, and 92% PPS can be obtained at the melting point of 289℃ and the average viscosity molecular weight of 48199 （Mr）, using syn- thesized complex CaL as a catalyst and N,N--dimethylaniline as an additive.
出处
《常州大学学报（自然科学版）》
CAS
2012年第2期17-21,共5页
Journal of Changzhou University：Natural Science Edition
关键词
聚苯硫醚
催化剂
溶剂
助剂
合成
poly（p-- phenylene sulfide）
catalysts
solvents
additives
synthesis
