一种无灰抗氧剂的合成新工艺

采用氢氧化钾为催化剂合成了抗氧剂中间产物3-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯.一种新的钛酸酯类催化剂用于中间产物与2-乙基己醇进行酯交换反应,合成的产品色度浅、有效成分含量高,抗氧性能好.产物经色谱分离获得了纯品,用元素分析、IR和1HNMR对产物及中间产物的结构进行了表征.元素分析结果表明,产物的C、H和O的质量分数与理论计算结果基本相同.对比产物与工业样品的红外光谱图,可确定产物与工业样品具有相同的结构.核磁共振分析表明,产品的分子式与预测分子吻合.最后用HPLC外标法对最终产物中有效成分的含量进行了测定,粗产物中目标物的质量分数达到91.3%,而工业品为77%.

A new technology for the preparation of a kind of ashless antioxydant

Methyl 3-(3,5-ditertbutyl--4-hydroxyphenyl) propionate is prepared by using KOH as the catalyst instead of traditional (CH3)3COK,which is the intermediate product in the preparation of the objective product 3-(3,5-Di-tert-butyl-4-hydroxyphenyl) propionate-2'-Ethylhexyl(EDTHP).The objective product is obtained by the transesterification of the intermediate product and 2-ethylyexanol.It has light color,high content of effective component and good anti-oxidation property.The objective product is characterized by element analysis,IR and 1HNMR,and the results show that,the mass fractions of C,H and O in the objective production are as great as the theoretically calculated mass fractions;the structure of the objective product is the same as that of industrial sample according to their infrared spectrogram;its molecular formula is the same as the predicted molecular formula according to its 1HNMR analysis result.The content of effective component in rough product is determined by HPLC external standard method,it reaches to 91.3%,while the content of effective component in industrial sample is 77.0%.