摘要
以饱和醇与四氯化钛为原料,通过酯化反应合成单烷氧基型钛酸酯偶联剂。本文分析了反应中原料配比、反应时间、反应方式、溶剂与底物饱和醇的种类对酯化合成效率及钛酸酯品质的影响。结果表明,酯化反应合成钛酸酯偶联剂反应受饱和醇的位阻影响,随位阻增加,单烷氧基钛酸酯偶联剂收率略下降,通常来说,可在饱和醇的回流温度下,采用四氯化钛滴入醇与60~90℃沸程的石油醚的混合溶液中,四氯化钛与醇的摩尔比为1:4.4,溶剂为混合原料质量份100%,采用溶剂微回流与微负压工艺替代中和剂的使用,保温4h,可得到符合国标要求的单烷氧基钛酸酯产品,收率90%以上,无需引入中和剂,可大大提高合成效率。
Monoalkoxy titanate coupling agent was synthesized from saturated alcohol and titanium tetrachloride by esterification reaction.The effects of the ratio of raw materials,reaction time,reaction mode,solvent and substrate saturated alcohol on the synthesis efficiency of esterification and the quality of titanate were analyzed.The results show that the esterification reaction to synthesis of titanate coupling agent is affected by the steric hindrance of saturated alcohol,and the yield of monanoxy titanate coupling agent decreases slightly with the increase of steric hindrance.Usually,titanium tetrachloride can be dropped into the mixed solution of alcohol and petroleum ether boiling at 60~90℃ under the reflux temperature of saturated alcohol.The molar ratio of titanium tetrachloride to alcohol is 1:4.4.The solvent is 100% of the mass of the mixed raw materials.The use of neutralizer is replaced by solvent micro-reflux and micro-negative pressure process.
作者
周煜华
杨静
刘广生
裴忠强
Zhou Yu-hua;Yang Jing;Liu Guang-sheng;Pei Zhong-qiang(Jiangxi ChenGuang New Material Inc.,Jiujiang Jiangxi 332500,China)
出处
《江西化工》
2023年第2期70-72,共3页
Jiangxi Chemical Industry
