3-甲基-6-叔丁基苯酚的合成 |
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引用本文: | 吕九琢,冯雷,徐亚贤,柴金荣,沈静.3-甲基-6-叔丁基苯酚的合成[J].精细化工,2003,20(11):685-688. |
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作者姓名: | 吕九琢 冯雷 徐亚贤 柴金荣 沈静 |
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作者单位: | 1. 北京石油化工学院,化学工程系,北京,102617 2. 北京化工大学,化学工程学院,北京,100029 |
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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%。
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关 键 词: | 3-甲基-6-叔丁基苯酚 烷基化反应 烷基转移反应 抗氧剂 |
文章编号: | 1003-5214(2003)11-0685-04 |
Synthesis of 3-Methyl-6-t-butylphenol |
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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%. |
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Keywords: | 3-methyl-6-t-butylphenol alkylation alkyl transfer antioxidants |
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