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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, citric acid, n-butanol, stearic acid and phosphorus trichloride as raw materials to synthesize a new type of non-toxic plasticizer octadecanoyl tributyl citrate (ETBC). The optimum synthesis conditions were determined by orthogonal test: 1) Synthesis of tributyl citrate with citric acid and n-butanol at molar ratio 4.6:1.0, reaction temperature 120 ℃ and catalyst 2.0%; 2) Phosphorus trichloride in the material ratio of 5: 2, the reaction temperature is 64 ℃, the reaction time 6 h synthesis of octadecanoyl chloride; 3) tributyl citrate and octadecanoyl chloride in the material ratio of 1.00: 1.05, The reaction temperature of 56 ℃, the amount of catalyst 1% synthesis of the target product ETBC. The resulting ETBC was a waxy white solid at room temperature with a density of 0.984 g / cm3, a melting point of 43-45 ° C, a flash point of 223 ° C and an acid value AV = 10.13 mgKOH / g. Through the application in fast-drying automobile paint and the testing of plasticizing property, it is concluded that the performance of ETBC is better than that of DOP except adhesion; ETBC has the same performance as DBP except adhesion and flexibility. In terms of toxicity, ETBC is far superior to DOP and DBP. ETBC can replace DOP in the paint industry status.