溶胶-凝胶法制备PW_(12)/SiO_2催化合成尼泊金丁酯  

Preparation of PW_(12)/SiO_2 catalyst by sol-gel method and its application in Butyl Nipagin synthesis

作　　者：王少鹏 王会娜 李靖靖 王宇飞 WANG Shao-peng;WANG Hui-na;LI Jing-jing;WANG Yu-fei(College of Chemical Engineering and Food,Zhengzhou Institute of Technolgy,Zhengzhou 450044;The 36th middle school of Zhengzhou,Zhengzhou 450042)

机构地区：[1]郑州工程技术学院化工食品学院,郑州450044 [2]郑州市第36中学,郑州450042

出　　处：《中国食品添加剂》2018年第7期132-137,共6页China Food Additives

基　　金：河南省科技厅开放合作基金(172106000067);郑州工程技术学院科技创新基金(CXTD2017K2)

摘　　要：利用溶胶-凝胶法,将磷钨酸(Keggin型)负载于SiO_2上,制备出负载型催化剂PW_(12)/SiO_2,并采用XRD、N_2吸附-脱附、FT-IR、TG-DTA等技术对催化剂进行了表征。将其用于催化合成尼泊金丁酯,并对工艺条件进行了优化,实验表明:催化剂具有较大的孔径、孔容及比表面积,且负载后PW_(12)的Keggin型结构不变。当醇酸摩尔比为3∶1,PW_(12)负载量为30%,催化剂用量为4%,反应温度为130℃,反应时间为3h,酯收率可达85.6%。催化剂重复使用5次,催化性能稳定。PW（12）/SiO2 were prepared using sol-gel method by immobolizing PW（12）（Keggin type）on SiO2. The characterizations of the catalyst were tested through XRD,N2 adsorption-desorption,FT-IR,TG-DTA methods. The catalyst were used in the synthesis of Butyl Nipagin,and the process conditions were optimized. The results showed that the catalyst had large aperture,pore volume and specific surface area,and Keggin type of PW（12） were maintained. The optimum conditions were ：mole ratio of alcohol and acid 3 ∶ 1,the loading of PW（12） 30%,the amount of catalyst 4%,reaction temperature 130℃,reaction time 3 h. Ester yield could reach 85.6% under the above conditions. The catalysts were able to reuse 5 times with stable performance.

关 键 词：溶胶-凝胶法 磷钨酸 SIO2 负载型催化剂 尼泊金丁酯 

分 类 号：TS202.3[轻工技术与工程—食品科学]