摘要
以双氧水改性活性炭负载三聚磷酸二氢铝为催化剂合成阿司匹林,采用单因素实验考察反应温度(A)、酐酸比(C)、反应时间(D)、催化剂用量(B)对阿司匹林收率的影响,采用响应面实验获得较佳的工艺条件。结果表明,该催化反应中对阿司匹林收率影响的顺序依次为合成温度、酐酸比、反应时间、催化剂用量。该催化剂较佳的催化反应条件顺序依次为催化剂用量、反应时间、酐酸比、反应温度。反应温度78.6℃,催化剂加入量占总反应物的6.5 wt%,酐酸比3.72∶1,反应时间47 min,收率86.9%。催化剂重复使用5次后,催化效率仍可达83.2%。响应面实验回归拟合模型为:Y=86.04+0.22×A-1.31×B-0.77×C+1.05×D+0.95×A×B+0.27×A×C-0.73×A×D+0.95×B×C-1.48×B×D-0.30×C×D-3.44×A^2-3.00×B^2-5.40×C^2-4.84×D^2。
Salicylic acid and acetic anhydride was used as reagents to synthesize aspirin under catalysis of aluminum dihydrogen tripolyphosphate/loaded modified activated carbon catalyst. Then single-factor experiments were used to explore the effect of mole ratio of salicylic acid with acetic anhydride, reaction time, temperature and quantity of catalyst on the yield of aspirin. Response surface design was used to obtain the optimization technical conditions of the synthesis of aspirin. The results show that the four main factors influencing the yield of aspirin are in the following order：temperature 〉 mole ratio of salicylic acid with acetic an- hydride 〉 reaction time 〉 quantity of catalyst. The optimal technical conditions are：temperature 78.6 ~C ,acetic anhydride to sali- cylic acid 3.72：1 ,reaction time 47 min,the quantity of catalyst 6.5%. The yield of aspirin is 86.9% ,which is close to the pre- dict value. After the catalyst reuse five times,the yield is 83.2%. Its regression model fitting is ： Y = 86. 04 ＋ 0. 22 ×A - 1.31 ×B-0.77xC＋1.05×D＋0.95×A×B＋0.27×A×C-0.73×A×D＋0.95 ×B×C-1.48×B×D-0.30×C×D-3.44× A-3.00×B2-5.40×C×-4.84×D2.
出处
《化学试剂》
CAS
北大核心
2016年第10期949-953,共5页
Chemical Reagents
基金
广西高校科研基金资助项目(KY2015YB445)
广西工业院科研基金资助项目(KY2014056005)
关键词
三聚磷酸二氢铝
阿司匹林
活性炭
催化
aluminum dihydrogen tripolyphosphate
aspirin
activated carbon
catalyze
