二异丙基二硫代磷酸富马酸二丁酯的合成

用异丙醇、五硫化二磷合成二异丙基二硫代磷酸(Ⅰ)。以对甲苯磺酸为催化剂,Ⅰ与富马酸二丁酯进行反应,合成了润滑油无灰添加剂二异丙基二硫代磷酸富马酸二丁酯(Ⅱ),对合成的工艺条件进行探讨。结果表明:合成Ⅰ的较佳条件为:五硫化二磷与异丙醇的摩尔比在(1.05～1.1)∶1,反应温度控制在60～70℃之间,物料反应彻底,产物的质量好。合成Ⅱ的较佳条件为:Ⅰ与富马酸二丁酯的摩尔比1∶(1.05～1.10),对甲苯磺酸的用量在投料总量的0.8%～1.0%,反应温度130～140℃,酸值低,色泽好。总收率可达98%。

Synthesis of diisopropyl phosphorodithioic acid dibutyl fumarate

Synthesis of diisopropyl phosphorodithioic acid from isopropanol and phosphorus pentasulfide on toluene-p-sulfonic acid catalyst, then react with dibutyl fumarate, lube oil ashless additive of diisopropyl phosphorodithioic acid dibutyl fumarate was obtained, and then discussed the synthesis technology, the result showed that the optimum condition are as follows: the mole ratio of phosphorus pentasulfide to isopropanol is (1.05～1.1)∶1, temperature is 60～70℃, the quality of product is good. The optimum condition of synthesis(Ⅱ) are: the mole ratio of I to dibutyl fumarate is 1∶(1.05～110),the amount of toluene-p-sulfonic acid is 0.8%～1.0% of reactants, reaction temperature is 130～140℃,the yield may up to 98%, acid value and tint is good.