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摘要
将自制的具有keggin结构的磷钨酸掺杂在溶胶-凝胶法制备的SiO2上作催化剂，以水杨酸和正丁醇为反应原料，对H3[α-PW12O40]-SiO2的催化性能进行研究。结果表明，当酸与醇的摩尔比为1：6、催化剂质量为酸质量的12%、反应时间为2.5 h、催化剂的负载量为10%时，酯化收率高达94%。催化剂循环使用3次，酯化收率变化不大。同时，在优化反应条件后，可较高收率地合成其他多种水杨酸酯。
Abstract
Self-made phosphotungstic acid with a Keggin structure is doped into SiO2 that is prepared by sol-gel method.The catalytic properties of as-prepared H3[α-PW12O40]-SiO2 are evaluated through using salicylic acid and n-butanol as raw materials to make salicylate.It is shown that the yield of esterification reaction can reach 94% when the molar ratio of salicylic acid to n-butanol is 1:6,the dosage of catalyst is 12% that of acid mass,the reaction lasts for 2.5 h and the load of catalyst is 10%.The esterification yield remains stable after the catalyst is reused for 3 times without any treatment.Furthermore,many other salicylate esters can also be synthesized at a high yield under optimized reaction conditions.
关键词
溶胶-凝胶法
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酯化反应
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负载
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水杨酸酯
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二氧化硅
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磷钨酸
Key words
sol-gel method
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esterification reaction
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load
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salicylate
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silica
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phosphotungstic acid
Author summay
蒋卫华(1975-),男,硕士,实验师,研究方向为精细有机合成,jwh2005dz@163.com
SiO2掺杂磷钨酸催化合成水杨酸酯的研究[J].
, 2020, 40(4): 89-93,98 DOI:10.16606/j.cnki.issn0253-4320.2020.04.020
