抗氧剂626的合成工艺研究  

Synthesis Technology of Antioxidant 626

作　　者：张敏宏[1] 张新军[1] 张毅[1] 史建公[1] 

机构地区：[1]中国石化催化剂有限公司北京燕山分公司,北京102400

出　　处：《河北北方学院学报（自然科学版）》2014年第1期6-12,共7页Journal of Hebei North University:Natural Science Edition

基　　金：中国石化股份有限公司支持项目(208058)

摘　　要：以三氯化磷、季戊四醇及2，4-二叔丁基苯酚为原料，采用二步法合成抗氧剂626。首先由三氯化磷与季戊四醇反应生成二氯代季戊四醇亚磷酸酯（Ⅰ），然后再与2，4-二叔丁基苯酚反应生成抗氧剂626（Ⅱ）。研究了原料配比、反应温度、反应时间、溶剂及催化剂等因素对原料转化率和产物收率的影响，利用正交设计对二步反应的工艺条件进行了优化，得到了合成抗氧剂626的优化工艺条件：原料物质的量之比为季戊四醇∶三氯化磷∶2，4-二叔丁基苯酚＝1.0∶2.25∶2.52；第1步反应温度为（60±3）℃，反应时间8 h；第2步反应温度（62±3）℃，反应时间10 h；催化剂用量为原料总投料质量的3％；溶剂为二甲苯，体系压力为0.08～0.09 MPa，结晶溶剂为异丙醇，洗涤溶剂为甲醇；以2，4-二叔丁基苯酚计目标产品，收率约为75％。Using phosphorus trichloride,pentaerythritol and 2,4-di-tertiary-butyl phenol as raw ma-terials,antioxidant 626 was synthesized in two steps.In the first step,pentaerythritol reacted with phos-phorus trichloride to form dichloro pentaerythritol phosphite (Ⅰ),then I continually reacted with 2,4-di-tertiary-butyl phenol to produce antioxidant 626 (Ⅱ).The influences of raw material ratio,reaction temperature,reaction time,solvent and catalyst on the conversion of raw material and product yield in two reactions were thoroughly investigated,process conditions of two reactions were optimized according to the orthogonal design.The optimization of process conditions of synthetic antioxidant 626 were ob-tained as follows:the ratio of the amount of raw material for pentaerythritol/phosphorus trichloride/2,4-di tertiary butyl phenol was equal to 2.52/1.0/2.25;the first reaction temperature was (60±3)℃,the reaction time 8 h,the second reaction temperature was (62±3)℃,reaction time 10 h;catalyst accoun-ted for 3% of the total feeding quality,Solvent was xylene,reaction system pressure was 0.08~0.09 MPa,crystallization solvent is isopropyl alcohol and cleaning solvent was methanol,and under the above optimization conditions,the antioxidant 626 yield was about 75%.

关 键 词：抗氧剂 626 季戊四醇 三氯化磷 2 4-二叔丁基苯酚 双亚磷酸酯 合成 

分 类 号：TQ225.24[化学工程—有机化工]