甲基磺酸镧催化合成无毒增塑剂柠檬酸三丁酯

合成了甲基磺酸镧,研究了以甲基磺酸镧为催化剂合成无毒增塑剂柠檬酸三丁酯,考察了催化剂用量、醇酸物质的量比、反应温度等因素对反应结果的影响,对合成的产品进行了红外光谱分析。实验结果表明,甲基磺酸镧催化合成柠檬酸三丁酯的最佳条件为:n(正丁醇)∶n(柠檬酸)=4.50∶1,催化剂用量为0.25%(以酸的物质的量计),反应温度120~130°C,在最佳反应条件下,柠檬酸三丁酯收率在98.5%以上。反应结束后,催化剂通过简单的相分离即可重复使用。甲基磺酸镧重复使用5次后,其催化活性无明显下降,产品收率仍可达到90%以上。

Synthesis of Nontoxic Plasticizer Tri-n-butyl Citrate Using Lanthanum Methanesulfonate as Catalyst

Lanthanum methanesulfonate was synthesized and used as a catalyst in the esterification of citric acid with butanol.The effects of amount of catalyst,alcohol/acid molar ratio and reaction temperature were investigated.The products were analyzed by means of FT IR spectroscopy.The optimum conditions for the synthesis of TBC over lanthanum methanesulfonate are: molar ratio of butanol to citric acid,4.50∶1;amount of catalyst,0.25%(molar percentage of citric acid) and reaction temperature,120~130°C.The yield can be over 98.5% under optimum conditions.The catalyst can be reused by simple phase-separation after reaction.It was used repeatedly for 5 times without obvious loss of activity and with the yield still over 90.0%.