水杨酸(2,2,6,6-四甲基-4-羟基哌啶)酯的合成研究

Study on Synthesis of Light Stabilizer 2,2,6,6-tetramethyl-4-piperidyl Salicylate

以颗粒状活性炭负载四丁基钛酸酯作催化剂,水杨酸甲酯、2,2,6,6-四甲基-4-羟基哌啶为原料合成受阻胺光稳定剂HALS,水杨酸(2,2,6,6-四甲基-4-羟基哌啶)酯,分别研究了反应温度、反应时间、原料配比和催化剂用量等条件对合成反应的影响。得到了合成水杨酸(2,2,6,6-四甲基-4-羟基哌啶)酯最适宜的条件是:反应温度为100～120℃,反应时间7h,n(水杨酸甲酯)∶n(2,2,6,6-四甲基-4-羟基哌啶)为0.1∶0.115;催化剂的用量为1.0g、溶剂的用量为30g(水杨酸甲酯为0.1mol的情况下)。水杨酸(2,2,6,6-四甲基-4-羟基哌啶)酯的收率超过95.04%,产品熔点为207～208℃。该催化剂具有价廉易得、催化活性好、不腐蚀设备、无环境污染等优点。

The hindered amine light stablizer （HALS） 2,2,6,6-tetramethyl-4-piperidyl salicylate was synthesized by using tetra-ten-butyl titanate supported on granular activated carbon as the catalyst for the reaction of methyl salicylate and 2,2,6,6-tetramethy1-4-piperidinol. The effects of reaction temperature, reaction time,materials ratio, the quantity of catalyst on the synthesis were studied, and the optimal technological conditions were given as follows：reaction temperature is 100-120℃ ,reaction time is 7 h, n （methyl salicylate）：n （2,2,6,6-tetramethyl--4-piperidinol） is 0.1：0.115, the quantity of catalysts is 1.0 g, the quantity of solvent is 30 g （when methyl salicylate is 0.1mol）.The yield of 2,2,6,6-tetramethyl-4-piperidyl salicylate is over 95.04%. Melting point of the product is 207-208℃. Experimental results show that the catalyst has many advantages, such as easy preparation,low cost and high activity, non-corrosive and pollution-free to the environment.