抗氧剂1076的合成工艺优化  

Synthesis process optimization of antioxidant 1076

作　　者：徐进云[1,2] 王迪迪 杨俊玲 XU Jin-yun;WANG Di-di;YANG Jun-ling(School of Environmental and Chemical Engineering,Tianjin Polytechnic University,Tianjin 300387,China;Tianjin Textile Fiber Interface Technology Engineering Center,Tianjin 300270,China)

机构地区：[1]天津工业大学化学与化工学院,天津300387 [2]天津市纺织纤维界面处理技术工程中心,天津300270

出　　处：《天津工业大学学报》2019年第2期50-56,共7页Journal of Tiangong University

基　　金：中石化资助项目(217010-3)

摘　　要：为探究抗氧剂1076的最佳合成工艺,在有机金属催化剂催化条件下,采用3-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯(简称3,5-甲酯)与十八碳醇进行酯交换反应,制备3-(3,5-二叔丁基-4-羟基苯基)丙酸十八碳醇酯(抗氧剂1076),分析溶剂和催化剂种类、反应时间、物料配比、反应温度等因素对反应收率的影响;采用高效液相色谱仪、傅里叶变换红外光谱仪、核磁共振仪等设备对产品结构进行表征,并使用热失重法测试其热稳定性,采用差式扫描量热法测试其氧化安定性。结果表明:产品收率随着反应温度的提高和反应时间的延长先增大后减小,随着物料摩尔比的增加而增大;最佳工艺条件为采用甲基环乙烷作为溶剂,异辛酸锌作为催化剂,3,5-甲酯与十八碳醇的摩尔比为1.03∶1,反应时间为3.5 h,反应温度为130℃,催化剂质量分数为反应物的2.5%时,产品收率提高到97%;合成产品分子结构与理论分子结构一致,且产品纯度较高(97.75%),有很高的热稳定性和抗氧化活性,热分解温度达317℃,起始氧化温度达361.4℃。In order to explore the best synthetic process of antioxidant 1076,3-(3,5-ditert butyl-4-hydroxyphenyl)octadecanol propionate(antioxidant 1076)is prepared through transesterification reaction of(3,5-ditert butyl-4-hydroxyphenyl)methyl propionate(abbreviated as 3,5-methyl ester)with octadecanol catalyzed by organome-tallic catalyst.The effects of solvents and catalysts,reaction time,material ratio and reaction temperature on the reaction yield are analyzed.The product is characterized by Fourier transform infrared spectrometer,NMR and HPLC,and its thermal stability is tested by the thermogravimetry differential,and the oxidation stability is measured by the differential scanning calorimetry.The results show that the product yield first increases and then decreases with the increase of reaction temperature and reaction time,and increases with the increase of material molar ratio;the optimum technological conditions is using methyl cyclohexane as solvent and zinc isooctanoate as catalyst,the mole ratio of 3,5-methyl ester to octadecanol is 1.03∶1,the reaction time is 3.5 h,the reaction temperature is 130℃,the mass fraction of catalyst is 2.5%of the reactants,and the yield is increased to 97%.The molecular structure of synthetic product is consistent with the theoretical molecular structure.The product has high purity(97.75%),high thermal stability and oxidation stability,the decomposition temperature is 317℃and the initial oxidation temperature is 361.4℃.

关 键 词：抗氧剂1076 有机金属催化剂 十八碳醇 酯交换 氧化安定性 工艺优化 

分 类 号：TQ314.249[化学工程—高聚物工业]