摘要
以柠檬酸、正丁醇、硬脂酸、三氯化磷为原料,通过正交试验方法合成了一种新型的高效无毒增塑剂十八碳酰柠檬酸三丁酯(OTBC)。首先确定了当正丁醇和柠檬酸物质的量比为4.6:1,反应温度为120℃,催化剂的质量分数为2.0%时合成了柠檬酸三丁酯;然后在硬脂酸和三氯化磷物质的量比为5:2,反应温度为64℃,反应时间为6h的条件下合成了十八碳酰氯;最后以合成的柠檬酸三丁酯和十八碳酰氯物质的量比为1:1.05,反应温度为56℃,催化剂的质量分数为2%合成了十八碳酰柠檬酸三丁酯。合成的十八碳酰柠檬酸三丁酯常温下为蜡白色固体,密度为0.984g/cm3,相对分子量为626,熔程为43~45℃,闪点为223℃,酸值Ay=10.13mgKOH/g。并运用红外光谱和热重分析对产品进行了鉴定,通过对OTBC和邻苯二甲酸二辛酯(DOP)增塑聚氯乙烯(PVC)进行对比研究。结果表明,当m(OTBC):m(PVC)=30:100时,OTBC增塑PVC材料的拉伸强度、断裂伸长率及抗低温性能优于DOP增塑PVC材料。
A novel and efficient environmental friendly plasticizer octodecyl acyl tributyl citrate (OTBC) was prepared using citrate, n-butanol, octadeeanoic acid and phosphorus triehloride by orthogonal experiments. At first, tributyl citrate was prepared under the condition of the molar ratio for citrate and n-butanol was 4.6:1, temperature of reaction was 120 ℃ and catalyst mass fraction was 2.0%. Then octodecyl acyl chloride was synthesized sustained for 6 hours with molar ratio of octadecanoic acid and phosphorus trichloride was 5:2, temperature of reaction was 64 ℃. Finally OTBC was prepared under the condition of molar ratio of tributyl citrate and octodecyl aeyl chloride was 1 : 1.05, temperature of reaction was 56℃ and catalyst mass fraction was 2. 0%. OTBC was waxes white solid under room temperature, density was 0. 984 g/cm3, molecular weight was 626, melting range from 43 ℃ to 45 ℃, flash point was 223℃, acid value was 10. 13 mgKOH/g. The product was identified by FTIR and TG analysis. Comparative study was carried on polyvinyl chloride (PVC) plasticized with OTBC and DOP. The result proved that the performance of tensile strength, elongation at break and resistance to cold of OTBC plastized PVC was better than DOP's when m(OTBC):m (PVC) was 30:100.
出处
《塑料工业》
CAS
CSCD
北大核心
2011年第2期78-82,共5页
China Plastics Industry
基金
教育部国家大学生创新性实验项目基金