MCM-41催化剂的制备、表征及其催化合成乙酰水杨酸.pdf

石油化工
?176
PETROCHEMICAL TECHNOLOGY
2014年第43卷第2期
HP2W1OMCM-41催化剂的制备、表征
及其催化合成乙酰水杨酸
曹小华,王原平,雷艳虹',徐常龙,占昌朝
(1.九江学院化学与环境工程学院,江西九江332005;2.九江职业大学,江西九江332000
摘要]采用浸渍法将 Dawson结构的磷钨酸H,P2W1O。2(简写为P2W1)负载在MCM-41分子筛上,制备出新型P2W:MCM-41
催化剂;采用FTIR,XRD,SEM,EDS等方法対催化剂进行了表征。表征结果显示,P2 W,/MCM-4]催化剂既保持了MCM
41分子筛的孔道结构,又保持了P2W3的 Dawson?结构。同时研究了P2W1MCM-4]催化剂对乙酰水杨酸合成反应的活性、通过
正交实验确定了优化工艺条件:n(水杨酸):n(乙酸府)=1.0:1.5、P2W:MCM-41催化剂用量2.7%(基于反应物的质量)
反应温度80℃、反应时间10min。在此优化条件下,乙酰水杨酸收率为8819%。P2W1wMCM-41催化剂重复使用5次,乙酰水
杨酸收率仍可达76.7%。
关键词] Dawsons结构;MCM-41分子筛;磷钨酸MCM-41催化剂:;乙酰水杨酸
文章编号]1000-8144(2014)02-0176-05
[中图分类号]TQ426.91
[文献标志码]A
Preparation and Characterization of I P W O/ MCM-41 Catalyst for
Acetylsalicylic Acid Synthesis
Cao Xiaohua, Wang Yanping, Lei Yanhong, Xu Changlong, Zhan Changchao
(1. School of Chemical and Environmental Engineering, Jiujiang University, Jiujiang Jiangxi 332005, China
2. Jiujiang Vocational University, Jiujiang liangxi 332000, China
Abstract P W /MCM-41 catalyst was prepared by an immersion method to load phosphotungstic
acid (Hs, W1SO62, Abbrev. P, W18)with Dawson structure on MCM-41 molecular sieves and
characterized by means of FTIR, XRD, SEM and EDS. The original structures of both P2 Ws and
MCM-41 molecular sieves were maintained after the loading. The catalytic performance of the P, W/
MCM-41 catalyst in the synthesis of acetylsalicylic acid from salicylic acid and acetic anhydride was
investigated by orthogonal Experiments. The results showed that under the optimal conditions of
mole ratio of salicylic acid to acetic anhydride 1.0: 1.5, mass fraction of P2 Wi8/MCM-41 to the total
reactants 2.7%, reaction temperature 80 C and reaction time 10 min, the yield of acetylsalicylic acid
reached 88. 1%0, which still was 76.7% after the catalyst was regenerated and reused for 5 times
Keywords Dawson structure; MCM-41 molecular sieve; phosphotungstic acid/mcm-41
catalyst acetylsalicylic acid
乙酰水杨酸又名阿司匹林,是一-种典型的解绿色、高效合成乙酰水杨酸的工艺已引起广泛关
热、痛和抗炎药,是世界上最受欢迎的药物之
一,而且其应用范闱还在不断拓展2。目前,ゴ:[收稿日期]2013-08-23:[修改稿日期』12013-10-28
业上主要通过浓硫酸催化乙酸酐与水杨酸进行酰作者箇介」曹小华(1978-)?男,江西省都昌县人,博士,副
化反应合成乙酰水杨酸,虽然工艺成熟,但存在
教授,电话0792-831106,电邮 caojlmmy(@l26,com
L基金项目』国家自然科学基金项目(21161009);江西省白然科
产品收率不高、副反应多、设备腐蚀严重以及ア产学基金项日(20132BAB200,20A100:江面省教
生大量废液污染环境等不足3。因此,近年来育厅科技项目(G323):九江学院科技项日(203KUO0)