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[1]郭雅妮,何俭,刘承美,等.4,4′二羟基二苯硫醚环氧树脂的合成与表征[J].武汉工程大学学报,2014,(10):26-30.[doi:103969/jissn16742869201409006]
　GUO Ya ni,HE Jian,LIU Cheng mei,et al.Synthesis and characterization of 4, 4′thiodiphenol epoxy[J].Journal of Wuhan Institute of Technology,2014,(10):26-30.[doi:103969/jissn16742869201409006]
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4,4′二羟基二苯硫醚环氧树脂的合成与表征(/HTML)
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《武汉工程大学学报》[ISSN:1674-2869/CN:42-1779/TQ]

卷:
期数:
2014年10期
页码:
26-30
栏目:
材料科学与工程
出版日期:
2014-10-30

文章信息/Info

Title:
Synthesis and characterization of 4, 4′thiodiphenol epoxy
文章编号:
16742869(2014)010002605
作者:
郭雅妮1; 何俭1; 刘承美2; 骆沛尧1
1.武汉工程大学材料科学与工程学院，湖北 武汉 430074；2.华中科技大学化学与化工学院，湖北 武汉 430074
Author(s):
GUO Yani1; HE Jian1; LIU Chengmei2; LUO Peiyao1
1． School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430074, China2．School of Chemistry & Chemical Engineering, Huazhong University of Science and Technology, Wuhan 430074, China
关键词:
4; 4′二羟基二苯硫醚; 环氧树脂; 合成
Keywords:
4; 4′thiodiphenyl; epoxy resin; synthesis
分类号:
TQ323.5
DOI:
103969/jissn16742869201409006
文献标志码:
A
摘要:
以4,4′二羟基二苯硫醚、环氧氯丙烷为原料，四正丁基溴化铵为催化剂，合成了4,4′二羟基二苯硫醚环氧树脂，通过核磁共振氢谱、碳谱、傅立叶变换红外光谱表征了产物的结构.利用正交实验法研究了反应温度、醚化时间、闭环时间、原料配比对合成反应的影响, 优化后的反应条件为：4,4′二羟基二苯硫醚与环氧氯丙烷、四正丁基溴化铵的摩尔比为1∶10∶0.02，反应温度90 ℃，醚化时间4 h，闭环时间2 h，氢氧化钠与4,4′二羟基二苯硫醚的摩尔比为1.2∶1.优化反应得到产物的环氧值为4.599 mmol/g，产率为87.79%.通过对产物的结构表征，验证了两步法合成工艺路线的可行性.
Abstract:
4,4′thiodiphenol epoxy was synthesized by using 4,4′thiodiphenyl and epichlorohydrin as raw materials and using tetrabutylammonium bromide as a catalyst. The chemical structure of the product was confirmed by 1H nuclear magnetic resonance spectra, 13C nuclear magnetic resonance and fourier transform infrared. The effects of reaction temperature, etherification reaction time, ring closure reaction time and molar ratio of raw materials on the yield of the product were studied by an orthogonal experiment method. The optimum reaction conditions were confirmed as follows：the molar ratio of epichlorohydrin, tetrabutylammonium bromide and 4,4′thiodiphenyl is 10∶0.02∶1,and the molar ratio of sodium hydroxide and 4,4′thiodiphenyl is 1.2∶1, reaction temperature is 90 ℃, the etherification reaction time and the ring closure reaction time are 4 hours and 2 hours, respectively. Under these conditions, the epoxide value of the product is 4.599 mmol/g and the yield is 87.79%. The results of structure characterization show that the twostep preparation process is feasible.

参考文献/References:

［1］SHERMAN C L, ZEIGLER R C, VERGHESE N E, et al. Structureproperty relationships of controlled epoxy networks with quantified levels of excess epoxy etherification ［J］. Polymer，2008， 49:11641172.［2］CHIU Y，TSAI H，CHOU I，et al. Preparation，intermolecular motion，and thermal properties of thiodiphenyl epoxy ［J］. Journal of Applied Polymer Science，2010，118:21162125.［3］杨柏，吕长利，沈家骢. 高性能聚合物光学材料［M］. 北京: 化学工业出版社，2005：325.YANG Bai，L Changli，Sheng Jiacong. High performance polymer optical materials［M］. Beijing：Chemical Industry Press，2005：325. (in Chinese)［4］LUO C，ZUO J，ZHAO J. Synthesis and property of epoxy prepolymer and curing agent with high refractive index［J］. High Performance Polymers，2013，25:986991.［5］郭雅妮，何俭，骆沛尧. 高折射率环氧树脂的研究进展［J］. 武汉工程大学学报，2014，36(7):5358.GUO Yani，HE Jian，LUO Peiyao. The research of high index epoxy resin ［J］. Journal of Wuhan Institute of Technology，2014，36(7):5358.(in Chinese)［6］李志红. 双酚F环氧树脂的改性研究 ［D］. 长沙:国防科学技术大学，2004.LI Zhihong. Research on the modification of bisphenol F epoxy resin ［D］.Changsha： National University of Defense Technology，2004.（in Chinese）

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备注/Memo

备注/Memo:
收稿日期：20140901基金项目：湖北省自然科学基金项目（2012FFC10501）；地方高校国家级大学生创新创业训练计划项目（201310490006）；武汉工程大学科学研究基金项目（11115032）作者简介：郭雅妮（1975），女，山东平度人，副教授，博士．研究方向：功能高分子材料．
更新日期/Last Update: 2014-11-21