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高温抗氧剂ZDDP合成方法的研究
Research on the synthetic method for high temperature oxidation inhibitor of zinc dialkyl-dithio-phosphate(ZDDP)
【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%。
【Abstract】 In this paper we proposed a way of synthesizing zinc dialkyl-dithio-phosphate 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 % .
【Key words】 High temperature oxidation inhibitor; Zinc dialkyl-dithio-phosphate; Dialkyl-dithio-phosphate;
- 【文献出处】 化工科技 ,Science & Technology in Chemical Industry , 编辑部邮箱 ,2006年02期
- 【分类号】TE624.82
- 【被引频次】2
- 【下载频次】350