[1]储海霞,单玉华,丁永红,等.硫化钠法合成PPS的溶剂和催化体系的考察[J].常州大学学报(自然科学版),2012,(02):17-21.
　CHU Hai-xia,SHAN Yu-hua,DING Yong-hong,et al.Investigation of the Solvents and Catalysts in Poly(Phenylene Sulfide)Synthesis[J].Journal of Changzhou University(Natural Science Edition),2012,(02):17-21.
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硫化钠法合成PPS的溶剂和催化体系的考察()
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常州大学学报(自然科学版)[ISSN:2095-0411/CN:32-1822/N]

卷:
期数:
2012年02期
页码:
17-21
栏目:
出版日期:
2012-03-30

文章信息/Info

Title:
Investigation of the Solvents and Catalysts in Poly(Phenylene Sulfide)Synthesis
作者:
储海霞1; 单玉华1; 丁永红2; 鲁墨弘1; 李明时1
1.常州大学 江苏省精细石油化工重点实验室,江苏 常州 213164; 2.常州大学 材料科学与工程学院,江苏 常州 213164
Author(s):
CHU Hai-xia1; SHAN Yu-hua1; DING Yong-hong2; LU Mo-hong1; LI Ming-shi1
1.Key Laboratory of Jiangsu Fine Petrochemical Engineering,Changzhou University,Changzhou 213164,China; 2.School of Materials Science and Engineering,ChangzhouUniversity,Changzhou 213164,China
关键词:
聚苯硫醚;  催化剂;  溶剂;  助剂;  合成
Keywords:
poly(p-phenylene sulfide);  catalysts;  solvents;  additives;  synthesis
分类号:
TQ 322
文献标志码:
A
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、PhCOONa、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3 h,220-240 ℃反应4 h,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。
Abstract:
Poly(Phenylene Sulfide)(PPS)was synthesized from SodiumSulfide 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-nitrophenol)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 3 h to 220-240 ℃ for 4 h. 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 meltingpoint of 289 ℃ and the average viscosity molecular weight of 48199(Mr),using synthesized complex CaL as a catalyst and N,N-dimethylaniline as an additive.

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备注/Memo

备注/Memo:
作者简介:储海霞(1984-),女,江苏东台人,硕士生; 通讯联系人:单玉华。
更新日期/Last Update: 2012-03-30