D101型大孔吸附树脂的溴甲基化及反应条件优化  

Bromine methylation of D101 macroporous adsorption resin and optimization of reaction condition

作　　者：岳方 孙涛[1] 刘春晖 马晓莉 杨晋[1,3] Yue Fang;Sun Tao;Liu Chunhui;Ma Xiaoli;Yang Jin(Department of Chemistry and Chemical Engineering,North Minzu University,Yinchuan 750021;Key Laboratory of Basic Chemical Technology of State Ethnic Affairs Committee,North Minzu University,Yinchuan 750021;Ningxia Natural Medicine Engineering Technology Center,Yinchuan 750021)

机构地区：[1]北方民族大学化学与化学工程学院,银川750021 [2]北方民族大学化工技术基础国家民委重点实验室,银川750021 [3]宁夏天然药物工程技术研究中心,银川750021

出　　处：《化工新型材料》2020年第12期162-166,共5页New Chemical Materials

基　　金：北方民族大学重点科研项目(科技创新类2019KJ16,2017KJ16);国家自然科学基金(21565001);宁夏回族自治区重点研发计划(2019BFH02004)。

摘　　要：根据Blanc反应原理,以氢溴酸为溴甲基化试剂,对D101型大孔吸附树脂进行溴甲基化反应研究。在氢溴酸过量的条件下,通过单因素实验确定了反应温度、反应时间和浓硫酸用量对溴甲基化反应的影响,在此基础上,以溴含量为响应值设计响应面实验。通过响应面实验得到最佳反应条件为:反应时间9h,反应温度93℃,浓硫酸用量39.5mL。在该条件下可制备溴含量为4.522mmol/g的大孔吸附树脂,为树脂的进一步改性、功能化奠定了基础。The bromine methylation reaction of D101 macroporous adsorption resin(MAR)was performed via the blanc reaction principle,and hydrobromic acid was used as bromomethylation reagent.The influences of reaction temperature,reaction time and the amount of concentrated sulfuric acid were determined by single factor experiments under the condition of hydrobromic acid excess.Accordingly,with bromine content as the response value,response surface test was designed.The results showed that the optimal reaction conditions were:reaction time 9 h,reaction temperature 93℃,concentrated sulfuric acid dosage 39.5 mL.Under this condition,the content of bromine modified on resin was 4.522 mmol/g.This method can provide the foundation for MAR’s modification and functionalization.

关 键 词：Blanc反应原理 溴甲基化反应 大孔吸附树脂 溴含量 响应面法 

分 类 号：TQ32[化学工程—合成树脂塑料工业]