超强酸SO_4^(2-)/TiO_2催化合成反丁烯二酸果糖甲酯研究  

Study on Synthesis of Fructose Methyl Fumarate Catalyzed by SO_4^(2-)/TiO_2

作　　者：周如金[1] 黄敏[1] 张庆[1] 钟广杰[1] 林展[1] 余育玲[1] 

机构地区：[1]广东石油化工学院化工与环境工程学院,茂名525000

出　　处：《中国粮油学报》2012年第1期97-102,共6页Journal of the Chinese Cereals and Oils Association

基　　金：广东省自然科学基金(5300953);广东省教育厅自然科学研究项目(04J013);广东石油化工学院(原茂名学院)科学研究资助(200401003)

摘　　要：筛选并制备了固体超强酸SO24-/TiO2催化合成反丁烯二酸果糖甲酯。反应分为3步:马来酸酐先和果糖反应生成顺丁烯二酸单果糖酯、顺丁烯二酸单果糖酯异构化和反丁烯二酸单果糖酯与甲醇酯化反应生成反丁烯二酸果糖甲酯。单因素法确定的"一锅法"合成具有较高抗菌活性的反丁烯二酸果糖甲酯的工艺为:60℃下将顺酐熔化后加入占反应物总质量8%的SO42-/TiO2和与顺酐物质的量比为1∶4的果糖,将温度升至80℃保温反应3 h。然后向反应体系中加入占反应物总质量5%的由盐酸与亚硫酰氯质量比为1∶1构成的异构化剂以及为顺酐物质的量1.3倍的甲醇,70℃下保温反应2 h。反应液经过滤、中和即可得淡黄色的反丁烯二酸果糖甲酯。By selecting and preparing solid superacid SO^-/TiO2 as a catalyst, the fructose methyl fumarate （ FMF）, a new type of preservatives and mold preventives, was synthesized. The process of synthesizing FMF includ- ed three reactions ： mono - Fructose maleate （MFM） first obtained by esterification of maleic anhydride and fructose ; the formation of FMF by isomerization of MFM and then reaction with methanol. An optimizing ＂one pot＂ technology for synthesizing the FMF with higher antimicrobial activity by single factors method was as follows： The maleic anhydride, 4 times of fructose, was melted firstly at 60℃ in a reactor with magnetic stir. The reaction temperature was increased to 80℃ and maintained for 3h after fructose and 8% SO4^2-/TiOa（mass percent） of the total amount of reactant were added. Then, the 5% （mass percent to total reactant） isomerization catalyst, HC1/SOC12 of mass ratio 1 ： 1, and methanol, 1.3 mole times of maleic anhydride, were together put in the reactor. At the meantime, the temperature was decreased to 70℃ and maintained for another 2 h. The reaction mixture was isolated by suction filtration, and filter liquor was added to an aqueous slkali of pH 8. The FMF was separated out in the upper of aqueous slkali.

关 键 词：反丁烯二酸果糖甲酯 固体超强酸 防腐剂 合成 

分 类 号：TQ917[化学工程]