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机构地区:[1]台州职业技术学院生化制药研发中心,台州318000 [2]浙江尖峰海州制药有限公司,台州318000
出 处:《离子交换与吸附》2013年第6期543-550,共8页Ion Exchange and Adsorption
基 金:浙江省教育厅科研项目(No.Y201018296);台州市科技计划项目(102XCP10)
摘 要:以大孔强酸型阳离子交换树脂(ResS03H)与35%硝酸作为硝化剂,通过单因素试验考察了2,6-二叔丁基苯酚(DTBP)硝化反应的影响因素,并用正交试验优化了工艺条件,得到最优的工艺条件为:催化剂用量为15g树脂/60mmol硝酸,硝酸浓度为35%,硝酸用量为DTBP摩尔量的1.20倍,在0-5℃下滴加约1h,然后升温至10℃反应1h,DTBP已基本反应完全,产品2,6-二叔丁基对硝基苯酚(DTBNP)的产率达到90%以上,且树脂重复使用性能良好。The influencing factors of nitration of 2,6-di-tert-butylphenol (DTBP) were investigated by single factor experiment using strong acid ion-exchange resins (ResSO3H) and 35% nitric acid as nitrating agents. The nitration conditions were optimized by orthogonal experiments and the optimum conditions were obtained as follows: the ratio of resin to nitric acid was 12g/60mmol, the concentration of nitric acid was 35%, the amount of nitric acid was 1.20 times of the mole number of DTBP. The nitric acid was added by dropping into the mixture of DTBP and ResSOaH for about one hour at 0-5℃, then the system was heated at 10℃ and reacted for another one hour until DTBP was completely reacted. The yield of the product 2,6-di-tert-butyl-4-nitrophenol (DTBNP) was above 90%. Besides, the resins had good reusability.
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