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工程科学与技术:2017,49(3):197-201
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聚烯丙基胺的合成、表征及其与硫化氢反应
(1.西南石油大学 石油天然气装备教育部重点实验室, 四川 成都 610500;2.四川大学 高分子科学与工程学院, 四川 成都 610065)
Synthesis,Characterization and Reaction with H2S of Poly(allylamine)
(1.Key Lab. for Petroleum-gas Equipment of EMC, Southwest Petroleum Univ., Chengdu 610500, China;2.College of Polymer Sci. and Eng., Sichuan Univ., Chengdu 610065, China)
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投稿时间:2016-10-19    修订日期:2017-03-29
中文摘要: 随着聚烯丙基胺在染整,水处理,气体吸附等领域的广泛应用,聚烯丙基胺的需求越来越大。然而,用烯丙基胺单体直接聚合会存在严重的衰减链转移现象,而无法得到高分子量的产物,用加氢方法制备,实验过程繁琐。本文采用先对烯丙基胺单体进行盐酸化,消除衰减链转移现象,再利用(NH42S2O8和NaHSO3作为引发剂,对烯丙基胺盐酸盐进行自由基聚合,使用离子交换树脂对聚烯丙基胺盐酸盐进行离子交换处理,获得聚烯丙基胺。对聚烯丙基胺进行红外光谱和核磁结构表征,结果表明红外光谱在997 cm-1处对应的C=C键和945 cm-1处对应的=C-H键消失,说明单体被成功聚合。氢核磁谱图表明C上有3种氢,这与聚合物的结构相对应,也说明聚合物被成功合成。利用紫外光谱,X射线光电子能谱(XPS)和能量散射X射线能谱(EDX)探究聚合物与硫化氢的反应。紫外光谱显示,聚合物与硫化氢反应后,最大吸收峰的波长出现红移,并且强度增加。EDX测试表明与硫化氢气体反应后的聚合物表面存在着硫元素,并且表面硫原子百分率达到4.62%。XPS谱图表明,聚合物与硫化氢气体反应后,存在两种硫元素,经过分析说明聚烯丙基胺与硫化氢气体反应既存在着化学反应过程,同时还有物理吸附的过程。本文采用简单的自由基聚合制备聚烯丙基胺,并将其与硫化氢气体反应,实验表明聚烯丙基胺可以用作硫化氢气体的吸收剂。
Abstract:With the widely used of polyallylamine in many areas,such as dyeing and finishing,water treatment,gas adsorption,the demand of polyallylamine is growing.However,there is a serious chain transfer reaction by directly polymerizing the monomer of allyl amine to get polyallylamine,so it is unable to get high molecular weight products.And also,the experiment is cumbersome by using hydrogenation methods to prepare polyallylamine.Therefore,it is necessary to develop new methods to prepare polyallylamine.Using allylamine hydrochloride as monomer,(NH4)2S2O8 and NaHSO3 as initiating systems,Poly(allylamine) was prepared through the free radical polymerization at 50 ℃.The structure of poly(allylamine) was characterized by 1H-NMR and Fourier transform infrared (FTIR) spectrophotometer.The results of FTIR showed that the peaks at 997 cm-1 (due to C=C bonds) and 945 cm-1 (due to =C-H bonds) disappear after polymerization.The 1H-NMR showed that there are three different hydrogen atoms on the prepared polyallylamine.The results of FTIR and 1H-NMR indicated that the polyallylamine was successfully synthesized.The polymer reaction with hydrogen sulfide was studied and UV absorption spectrum indicated the wavelength of maximal absorption peak has redshift after reaction as well as the absorption intensity was increased.Energy Dispersive X-ray Detector (EDX) showed that there has sulfur at the surface of polymer after exposed to H2S with 1min.Besides,the result of EDX showed that there is 4.62 percent of sulfur atom on the surface of polymer after reacted with H2S.X-ray photoelectron spectroscopy (XPS) confirmed that there has chemical reaction and physical adsorption when the polymer exposed to H2S atmosphere.
文章编号:201601160     中图分类号:    文献标志码:
基金项目:国家自然科学基金资助项目(41474142);石油天然气装备教育部重点实验室开放基金资助项目(OGE201402-04)
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唐东林,出毅能,王瞧,李瑞海.聚烯丙基胺的合成、表征及其与硫化氢反应[J].工程科学与技术,2017,49(3):197-201.
TANG Donglin,CHU Yineng,WANG Qiao,LI Ruihai.Synthesis,Characterization and Reaction with H2S of Poly(allylamine)[J].Advanced Engineering Sciences,2017,49(3):197-201.