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3-甲基-6-叔丁基苯酚的合成

Synthesis of 3-Methyl-6-t-butylphenol

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【作者】 吕九琢冯雷徐亚贤柴金荣沈静

【Author】 L Jiu-zhuo~1,FENG Lei~2,XU Ya-xian~1,CHAI Jin-rong~1,SHEN Jing~1 (1.Department of Chemical Engineering,Beijing Institute of Petrochemical Technology,Beijng 102617,China;2.Department of Chemical Engeering,Beijing University of Chemical Technology,Beijing 100029,China)

【机构】 北京石油化工学院化学工程系北京化工大学化学工程学院北京石油化工学院化学工程系 北京 102617北京 100029北京 102617北京 102617

【摘要】 对3 甲基 6 叔丁基苯酚的合成工艺进行了研究。合成工艺分为两步,第1步:以浓硫酸为催化剂,n(间甲酚)∶n(异丁烯)=1 00∶0 95,催化剂的用量为间甲酚总质量的2 0%,反应温度为80℃,常压,反应时间为3h。反应结束后用w(NaOH)=20%水溶液处理,将有机相在0 001MPa下蒸馏,收集120~123℃的馏分即为3 甲基 6 叔丁基苯酚,收率为78%(以间甲酚计)。第2步:将分出3 甲基 6 叔丁基苯酚后剩余的釜底液进行烷基转移反应,按m(间甲酚)∶m(釜底液)=1∶2,不通入异丁烯,其他条件和后处理方法同第1步反应,得到3 甲基 6 叔丁基苯酚。釜底液的一次回收利用率达到70%,3 甲基 6 叔丁基苯酚的总收率达到93 4%。

【Abstract】 An improvement on the synthetic method of 3-methyl-6-t-butylphenol was studied. The process was divided into two steps.Firstly,3-methyl-6-t-butylphenol was prepared by the reaction of m-cresol and isobutylene in mole ratio 1∶0.95 with sulfuric acid as catalyst(2.0% the weight of m-cresol) at 80 ℃ under atmospheric pressure for 3 h.The reaction mixture was treated with 20% NaOH solution and the organic phase was distilled under 0.001 MPa.3-Methyl-6-t-butylphenol was collected at 120-123 ℃ in 78% yield(referred to cresol).In the second step,3-methyl-6-t-butylphenol was obtained by alkyl transfer reaction of the by-products(distillation residue in the first step) with cresol in mass ratio 2∶1.By this method,recovery of the by-products amounted to 70%,and the total yield of 3-methyl-6-t-butylphenol reached 93.4%.

  • 【分类号】O625.312
  • 【被引频次】17
  • 【下载频次】340
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