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 9h,reaction temperature 93℃,concentrated sulfuric acid dosage 39.5mL.Under this condition,the content of bromine modified on resin was 4.522mmol/g.This method can provide the foundation for MARs modification and functionalization.
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