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作 者:徐志华 张永富 茹雨晴 Xu Zhihua;Zhang Yongfu;Ru Yuqing(Shandong Daguan Biochemical Technology Co.,Ltd.,Linyi 276616,China;Qingdao Common Development Consulting Co.,Ltd.,Qingdao 266199,China;College of Chemical Engineering,Qingdao University of Science and Technology,Qingdao 266042,China)
机构地区:[1]山东达冠生化科技股份有限公司,山东临沂276616 [2]青岛和合共生顾问有限公司,山东青岛266199 [3]青岛科技大学化工学院,山东青岛266042
出 处:《山东化工》2021年第23期36-38,共3页Shandong Chemical Industry
摘 要:采用无毒无害的绿色化工原料碳酸二甲酯(DMC)代替有毒有害的硫酸二甲酯、碘甲烷、氯甲烷等作为对甲基苯酚甲基化反应的甲基化试剂,合成对甲基苯甲醚,通过催化剂筛选研究实验确定该反应的催化剂,然后研究对甲基苯酚与DMC配比对反应的影响,确定最佳配比,最后研究催化剂用量、反应温度及反应时间对反应转化率的影响,结果表明:该工艺催化剂的最佳选择为NaY分子筛催化剂,最佳物料配比为:m(对甲基苯酚)∶m(DMC)∶m(NaY分子筛)=1∶2.5∶0.06,最佳反应温度为145℃,最佳反应时间为5 h,此条件下对甲基苯酚转化率高达99.5%,对甲基苯甲醚的选择性大于99%,反应无废水和废固产生,实现高效清洁合成目标。Use non-toxic and harmless green chemical raw material dimethyl carbonate(DMC)instead of toxic and harmful dimethyl sulfate,methyl iodide,methyl chloride,etc.as methylation reagents for the methylation reaction of p-methylphenol to synthesize p-methyl Anisole,the catalyst for the reaction is determined through the catalyst screening experiment,and then the influence of the ratio of p-methylphenol and DMC on the reaction is studied,and the best ratio is determined.Finally,the catalyst dosage,reaction temperature and reaction time are studied on the conversion rate of the reaction.The results show that the best choice of catalyst for this process is NaY molecular sieve catalyst,and the best material ratio is:m(p-methylphenol):m(DMC):m(NaY molecular sieve)=1∶2.5∶0.06.The optimal reaction temperature is 145℃,and the optimal reaction time is 5 hours.Under these conditions,the conversion rate of p-methylphenol is as high as 99.5%,the selectivity of p-methyl anisole is greater than 99%,and there is no waste water and waste solids during the reaction.Achieve the goal of efficient clean synthesis.
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