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1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯的常压合成新工艺
引用本文:尹振晏,李艳云,祝九娣.1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯的常压合成新工艺[J].精细石油化工,2009,26(3).
作者姓名:尹振晏  李艳云  祝九娣
作者单位:1. 北京石油化工学院化工系,北京,102617
2. 北京科宇菲化工有限责任公司,北京,102400
摘    要:以2,6-二叔丁基苯酚、多聚甲醛和均三甲苯为原料,经两步常压反应合成了1,3,5-三甲基-2,4,6-三(3, 5-二叔丁基-4-羟基苄基)苯(即抗氧剂330)。通过正交设计,分别对两步合成反应的影响因素进行了考察,最优条件为:第一步,以甲醇为溶剂,n(2,6-二叔丁基苯酚):n(多聚甲醛)=1:1.6,反应时间为8 h,以二甲胺水(w=33%)溶液为催化剂,收率可达83.8%;第二步,以二氯甲烷为溶剂,n(均三甲苯):n(3,4-二叔丁基-4-羟基苄基甲基醚)=1:3.9,以H_2SO_4(w=80%)为催化剂,反应时间为1 h,收率可达90.4%。对产物进行了IR、元素分析、熔点及透光率测定,确定产物为目标产物。该工艺所得产物纯度高、成本低、三废少。

关 键 词:抗氧剂  2  6-二叔丁基苯酚  3  5-二叔丁基-4-羟基苄基甲基醚  1  3  5-三甲基-2  4  6-三(3  5-二叔丁基-4-羟基苄基)苯  合成

SYNTHESIS OF 1,3,5-TRIMETHYL-2,4,6-TRIS(3,5-DI-tert-BUTYL-4-HYDROXYBENZYL) BENZENE
Yin Zhenyan,Li Yanyun,Zhu Jiudi.SYNTHESIS OF 1,3,5-TRIMETHYL-2,4,6-TRIS(3,5-DI-tert-BUTYL-4-HYDROXYBENZYL) BENZENE[J].Speciality Petrochemicals,2009,26(3).
Authors:Yin Zhenyan  Li Yanyun  Zhu Jiudi
Affiliation:Yin Zhenyan~1,Li Yanyun~1 and Zhu Jiudi~2 (1.Department of Chemical Engineering,Beijing Institute of Petro-Chemical Technology,Beijing 102617,China,2.Beijing KYF Chemicals Co.,LTD,Beijing 102400,China)
Abstract:1,3,5-Trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl) benzene was synthesized using 2,6-di-tert-butyl phenol,paraformadehyde and misitylene as raw materials in two steps.Factors influencing the reactions were studied.The optimum conditions were determined though orthogonally arranged experiments as follows:(1) molar ratio of 2,6-di-tert-butyl phenol):paraformaldehyde= 1:1.6,reaction time 8 h,dimethylamino solution(w=33%) as catalyst,methanol as solvent.The overall yield of 3,5-di-tert-4-hydroxyl ben...
Keywords:antioxidant  2  6-di-tert-butyl phenol  3  5-di-tert-4-hydroxyl benzyl methyl ether  1  5-trimethyl-2  4  6-tris(3  5-di-tert-butyl-4-hydroxybenzyl) benzene  synthesis  
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