三聚磷酸二氢铝/载硫硅藻土催化合成柠檬酸三丁酯  

Synthesis of Tributyl Citrate Catalyzed by Aluminum Dihydrogen Tripolyphosphate / Loaded Sulfur Diatomite

作　　者：黄润均[1] 谢威[2] 王璟[3] 陈东莲[1] 黄增尉[3] 韦冬萍[3] 马少妹[3] 袁爱群[3] 

机构地区：[1]桂林理工大学南宁分校,广西南宁530001 [2]广西工业职业技术学院,广西南宁530006 [3]广西民族大学化学与生态工程学院化学与生物转化过程新技术重点实验室,广西南宁530006

出　　处：《塑料工业》2015年第1期105-108,120,共5页China Plastics Industry

基　　金：2014广西科技开发项目(桂科转14125002-6);2014南宁市科技开发项目(20145201);2013广西教育厅项目(2013YB105;200103YB041);2014广西工业职业技术学院项目

摘　　要：在P∶Al =3∶1（物质的量比）,100℃下,磷酸和氢氧化铝反应生成双氢磷酸铝,硅藻土在硫气氛下进行载硫处理后得到载硫硅藻土,以载硫硅藻土作为载体,与双氢磷酸铝混合,300℃下煅烧,获得三聚磷酸二氢铝/载硫硅藻土催化剂,采用单因素实验、正交设计实验考察其催化合成柠檬酸三丁酯反应中各实验因素对酯化率的影响并获得较佳反应条件.结果表明,当三聚磷酸二氢铝∶载硫硅藻土=3∶5（质量比）时制备的催化剂效果最好.3个主要因素的影响顺序为：醇酸物质的量比＞反应时间＞催化剂用量,较佳的反应条件是：反应时间5h,催化剂用量13％,醇酸物质的量比5,反应温度130～150℃,其酯化率达97.0％,该催化剂可重复使用5次.Both phosphoric acid and aluminum hydroxide were mixed with the P/Al moral ratio of 3： 1, 100 ℃ to obtain aluminum dihydrogen phosphate. Diatomite was used as carrier sulfur to mix with aluminum dihydrogen phosphate and was undergone calcination at 300 ℃ after the diatomite contained sulfur. The ATP/ loaded sulfur diatomite catalyst was obtained and both single factor experiment and orthogonal test were used to investigate the effect of preparation technology on the synthesis of tributyl citrate reaction. The results showed that the best yield was obtained when the mass ratio of aluminum dihydrogen tripolyphosphate to loaded sulfur diatomite was 3：5 （mass ratio）. The three main influencing factors were in the order as follows：mole ratio of citric acid to butanol 〉 reaction time 〉 quantity of catalyst. The optimal technical condition was： butanol to citric acid of 5, reaction time of 5 h, the quantity of catalyst of 13% , reaction temperature of 130 - 150 ℃, esterification rate was 97.0%. This catalyst can be re-used five times.

关 键 词：三聚磷酸二氢铝 柠檬酸三丁酯 硅藻土 催化 

分 类 号：TQ414[化学工程]