Abstract:The reactions of polyvinyl benzene with chlorosulfonic acid were performed under different ratio and reaction time and the results of chloro-sulfonation were detected by infrared spectrometer (380FT-IR). The characteristic peak at 1 601.5 cm-1 belongs to benzene ring and was selected as the internal standard peak. Two characteristic peaks at 1 377.4 and 3 476.8 cm-1 were selected as reference peaks, and belong to sulfonyl chloride and sulfonic group respectively. According to the Lambert-Beer law, the absorbance at 1 377.4 and 3 476.8 cm-1 was detected and compared with absorbance at 1 601.5 cm-1 respectively. The value of A1 377.4∶A3 476.8 was used to express uniformity of polystyrol sulfonyl chloride resins. The results show that: (a) After 0.5 h, A1 377.4∶A1 601.5 rises quickly with the prolonging of reaction time; and A3 476.8∶A1 601.5 rises too,but descends after 1 h. And the value of A1 377.4∶A3 476.8 rises with the prolonging of reaction time after 1 h. (b) When the ratio of HSO3Cl and PS is less than 1∶1, A3 476.8∶A1 601.5 rises with the ratio increasing, but when the ratio of HSO3Cl and PS is more than 1∶1, A3 476.8∶A1 601.5 descends while A1 377.4∶A1 601.5 appears and increases following the increase in the ratio. As the ratio was 4∶1, A1 377.4∶A1 601.5 and A3 476.8∶A1 601.5 show stabilization. In one step reaction condition, as the ratio of HSO3Cl and PS is 4∶1, the reaction can enhance uniformity of PS-SO2Cl at 60 ℃ for 5 h (the loading of sulfonyl chloride is 4.0 mmol·g-1). It was also confirmed that the function group uniformity of polystyrol sulfonyl chloride resins could be determined by infrared spectroscopy conveniently and quickly. Meanwhile, this method could be adopted to determine the function group uniformity practicably and widely.
林弦,魏荣卿,刘晓宁*,周蕊. 红外光谱法研究聚苯乙烯磺酰氯树脂功能基团的均一性[J]. 光谱学与光谱分析, 2009, 29(07): 1801-1804.
LIN Xian, WEI Rong-qing, LIU Xiao-ning*, ZHOU Rui. Study on the Function Group Uniformity of Polystyrol Sulfonyl Chloride Resins by Infrared Spectra. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2009, 29(07): 1801-1804.
[1] Alexander M V, Khandekar A C, Samant S D. Journal of Molecular Catalysis A: Chemical, 2004, (223): 75. [2] Paul Laidlaw, Donald Bethell, Stephen M Brown, et al. Journal of Molecular Catalysis A: Chemical, 2002, 178: 205. [3] HUANG Wen-qiang, HE Bing-lin(黄文强,何炳林). Ion Exchange and Adsorption(离子交换与吸附), 1991, 7(4): 287. [4] HUANG Wen-qiang, REN Qi-sheng, HE Bing-lin(黄文强,任启生,何炳林). Ion Exchange and Adsorption(离子交换与吸附), 1990, 6(3): 223. [5] Bogoczek R. Elzbieta Kociolek-Balawejder. Reactive Polymers, 1987, 12: 57. [6] CHEN Zhong-xiu, JIANG Lin-feng, DING Tong-fu, et al(陈钟秀,蒋林峰,丁同富,等). Journal of Chemical Engineering of Chinese Universities(高校化学工程学报), 2004, 18(2): 254. [7] Koichi Kamahori, Shoichi Tada, Koichi Ito, et al. Tetrahedron: Asymmetry, 1995, 6(10): 2547. [8] HUANG Wen-qiang, LI Chen-xi, MEN Ai-ju, et al(黄文强,李晨曦,门爱菊,等). Chemical Journal of Chinese Universities(高等学校化学学报), 1993. 14(3): 432. [9] Aifuluosi L C, LI Shou-chun, FU Zhi-ri, et al(莱·索·埃弗罗丝,李寿春,付志日,等). Journal of Dalian University of Technology(大连理工大学学报), 1959, (2): 38. [10] QU Qi-shu, TANG Xiao-qing, WANG Cheng-yin, et al. Analytica Chimica Acta, 2006, 572: 212. [11] Bacquet M, Salunkhe M, Caze C. Reactive Polymers, 1991, 16(1): 61. [12] LIU Ying, WEI Rong-qing, LIU Xiao-ning, et al(刘迎, 魏荣卿,刘晓宁,等). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2009,29(3):661. [13] XUE QI(薛奇). Spectral Methods of Research on Polymer Structure(高分子结构研究中的光谱方法). Beijing: Higher Education Press(北京:高等教育出版社), 1995. 80. [14] LI Gu, XI Shi-ping, LIU Zhen-xing, et al((李谷,席世平,刘振兴,等). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 1999, 19(3): 289. [15] WU Qiang, YANG Shu-zhen, LUO Jun-tao, et al(吴强,杨淑珍,罗君涛,等). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2000, 20(5): 606.