十八碳酰柠檬酸三丁酯的合成及在汽车快干漆中的应用  

Synthesis of ETBC and Application in Car Quick-drying Paint

作　　者：冯德进 张志刚 

机构地区：[1]兰州吉利汽车工业有限公司,兰州730087

出　　处：《现代涂料与涂装》2012年第12期4-7,共4页Modern Paint & Finishing

摘　　要：本文以柠檬酸、正丁醇、硬脂酸和三氯化磷等为原料合成了一种新型高效无毒增塑剂十八碳酰柠檬酸三丁酯(ETBC)。通过正交试验确定最佳合成工艺条件:1)柠檬酸和正丁醇在物质的量比4.6∶1.0,反应温度120℃,催化剂用量2.0%下合成柠檬酸三丁酯;2)硬脂酸和三氯化磷在物质的量比5∶2,反应温度64℃,反应时间6 h下合成十八碳酰氯;3)柠檬酸三丁酯和十八碳酰氯在物质的量比1.00∶1.05,反应温度56℃,催化剂用量1%下合成目标产物ETBC。得到的ETBC常温下为蜡白色固体,密度为0.984 g/cm3,熔点为43～45℃,闪点为223℃,酸值AV=10.13 mgKOH/g。通过对其在快干汽车漆中的应用和增塑性能的检测,得出ETBC在除附着力外的其他性能均优于DOP;ETBC在除附着力、柔韧性外的其他性能与DBP相当。在毒性方面,ETBC远远优于DOP和DBP。ETBC可以替代DOP在涂料行业的地位。In this paper, an efficient non-toxic plasticizer ETBC was synthesized by citric acid, n-butyl alcohol, stearie acid and phosphorus tri-chloride as raw materials. The best synthesis process was determined by orthogonal experiments： tri-butyl citrate was synthesized with citric acid and n-butyl alcohol as raw materials and their molar ratio of alcohol to acid： 4.6 ： 1.0, reaction temperature： 120℃, amount of catalyst： 2.0%, then stearyl chloride was synthesized with stearic acid and phosphorus triehloride, molar ratio of stearic acid and phosphorus trichloride： 5 ： 2, reaction temperature： 64 ℃, reaction time： 6 h. At last, the target compound tri-butyl stearyl citrate was synthesized with tri-butyl citrate and stearyl chloride, molar ratio of tri-butyl citrate to stearyl chloride： 1.00 ： 1.05, reaction temperature： 56 ℃, amount of catalyst： 1.0%. The tri-butyl stearyl citrate thus obtained was a wax-like white solid at ambient temperature and its density was 0.984 g/cm3, melting point of 43-45 ℃, flash point of 223 ℃, acid value of 10.13 mgKOH/g. By testing its application and plasticize performance in ear quick-drying paint, the properties of ETBC are better than DOP except adhesion： the properties of ETBC correspond to DBP except adhesion and flexibility. In toxicity, ETBC is far superior to DOP and DBP. ETBC can replace the status of DOP in the paint industry.

关 键 词：柠檬酸三丁酯 十八碳酰氯 十八碳酰柠檬酸三丁酯 无毒增塑剂 

分 类 号：TQ630[化学工程—精细化工]