摘要
以正丁醇和异辛醇与五硫化二磷酸化反应制得二烷基二硫代磷酸,然后二烷基二硫代磷酸与氧化锌成盐合成二烷基二硫代磷酸锌(ZDDP)。制酸阶段与成盐阶段都采用4因素3水平进行正交实验,通过因素时收率影响的分析,得出制备ZDDP最佳工艺条件为:制酸阶段,醇与五硫化二磷的摩尔比为4.2∶1,加料温度为60℃,反应温度为95℃,反应时间为1.5 h;成盐阶段,氧化锌过量20%,加料温度为70℃,反应温度为85℃,反应时间为3 h。该工艺可使产品pH值大于6,收率大于98%。
In this paper we proposed a way of synthesizing zinc dialkyl-dithio-phosphale with phosphorus pentasulfide,zinc oxide, n-butanol and 2-ethyl-hexanol as the raw materials. First of all, added phosphorus pentasulfide into the n-butanol and 2-ethyl-hexanol,so it changed into dialkyl-dithio-phosphate. Then used dialkyl-dithio-phosphate and zinc oxide as the reactants to produce zinc dialkyl-dithio-phosphate. The optimum preparation technology was conducted by orthogonal design L9(34) with different ratios on yield of product. The initial conditions of synthesizing technology were determined :in acid making, n-butanol and 2- ethyl-hexanol: phosphorus pentasulfide = 4.2 : 1, the charging temperature was 60 ℃, reaction temperature was 95 ℃, reaction time was 1.5 h;in the salification, zinc oxide excess was 20 %, charging temperature was 70 ℃ ,reaction temperature was 85℃ ,reaction time was 3 h. The pH of the product exceeded 5.5. The yield of the product exceeded 98 %.
出处
《化工科技》
CAS
2006年第2期13-15,共3页
Science & Technology in Chemical Industry
基金
国家重点新产品计划项目(2001ED650023)
作者简介
张颖(1972-).女,辽宁抚顺人,抚顺职业技术学院讲师,硕士,从事有机合成,功能材料研究。