1,3-二溴-2,2-二(溴甲基)丙烷的合成及结构表征

Synthesis and structure characterization of 1,3-dibromo-2,2-Bis(bromomethyl) propane

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20h,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.

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.