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[1]彭永利,罗灿,陈柏光.1,3二溴2,2二(溴甲基)丙烷的合成及结构表征[J].武汉工程大学学报,2013,(07):37-42.[doi:103969/jissn16742869201307008]
 PENG Yong li,LUO Can,CHEN Bai guang.Synthesis and structure characterization of 1,3dibromo2,2Bis(bromomethyl) propane[J].Journal of Wuhan Institute of Technology,2013,(07):37-42.[doi:103969/jissn16742869201307008]
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《武汉工程大学学报》[ISSN:1674-2869/CN:42-1779/TQ]

卷:
期数:
2013年07期
页码:
37-42
栏目:
资源与土木工程
出版日期:
2013-07-31

文章信息/Info

Title:
Synthesis and structure characterization of 1,3dibromo2,2Bis(bromomethyl) propane
文章编号:
16742869(2013)07003706
作者:
彭永利罗灿陈柏光
武汉工程大学材料科学与工程学院,湖北 武汉 430074
Author(s):
PENG YongliLUO CanCHEN Baiguang
Shool of Materials Science and Engineering,Wuhan Institute of Technology,Wuhan 430074,China
关键词:
13二溴22二(溴甲基)丙烷季戊四醇苯磺酰氯
Keywords:
13dibromo22two(bromomethyl) propane pentaerythritol benzenesulfonyl chloride
分类号:
O622.2
DOI:
103969/jissn16742869201307008
文献标志码:
A
摘要:
为了解决1,3二溴2,2二(溴甲基)丙烷因其生产工艺条件复杂,产率低而难以实现工业化生产的问题,以季戊四醇和苯磺酰氯、溴化钠为原料,通过两步法合成1,3二溴2,2二(溴甲基)丙烷.利用四因素三水平正交实验研究了反应时间、反应温度、催化剂用量及反应物投料比4个因素对1,3二溴2,2二(溴甲基)丙烷产率的影响,并得到了优化工艺参数:反应时间20 h,反应温度150 ℃,催化剂质量分数5%,投料比1∶6.2时,1,3二溴2,2二(溴甲基)丙烷的产率最高可达90.85%.红外图谱显示:羟基特征峰完全消失,生成了碳溴单键;核磁氢鐠图显示3.59处亚甲基上的质子单峰,无其它杂质峰.该法合成的1,3二溴2,2二(溴甲基)丙烷产率明显提高,且产物纯净,无副产物生成,无须提纯可直接使用,对实现1,3二溴2,2二(溴甲基)丙烷的工业化生产有着重要意义.
Abstract:
To solve the problems of complicated production process conditions, low production rate of 1,3dibromo2,2Bis(bromomethyl)propane, pentaerythritol and benzenesulfonyl chloride,sodium bromide were applied as raw materials to prepare pentaerythrityl bromide through twostep method. The optimum preparation technology of pentaerythritol bromide was studied by orthogonal experiment of four factors and three levels , the optimum process parameters are reaction time of 12 h, reaction temperature of 150 ℃, catalyst of 5%, feed ratio of 1∶6.2, the yield of pentaerythritol bromide reaches to 90.85%. Infrared spectrum shows that the hydroxyl characteristic peak disappeares entirely, brominecarbon bond is generated. Hydrogen nuclear magnetic praseodymium figure shows that the methel protons unimodal appears on 3.59. As a result, the production rate increases significantly by this way, and the product is pure without byproducts and can be used directly. It has important significance for the commercial process of 1,3dibromo2,2Bis(bromomethyl) propane.

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备注/Memo

备注/Memo:
收稿日期:20130415作者简介:彭永利(1968),男,黑龙江清宝人,教授,博士研究生导师.研究方向:热固性树脂及其复合材料.
更新日期/Last Update: 2013-07-31