| SO~(2-)_4 改性交联蒙脱土固体酸催化合成水杨酸正丁酯 |
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| 引用本文： | 秦国平,郭锡坤,谌宁.SO~(2-)_4 改性交联蒙脱土固体酸催化合成水杨酸正丁酯[J].精细化工,2003,20(6):352-354. |
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| 作者姓名： | 秦国平 郭锡坤 谌宁 |
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| 作者单位： | 汕头大学,化学系,广东,汕头,515063 |
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| 基金项目： | 广东省教育厅自然科学研究资助项目(200064);汕头大学研究与发展基金资助项目;汕头大学工业催化"211工程"建设资助项目 |
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| 摘 要： | 制备了SO2-4改性硅锆双组分交联蒙脱土固体酸催化剂(SO2-4/SiZrM),用于水杨酸(C7H6O3)和正丁醇(C4H10O)的酯化反应,与传统酯化反应催化剂浓硫酸、磷钨酸、硫酸铁铵以及其他单组分交联剂交联的蒙脱土做酯化反应的催化剂相比,SO2-4/SiZrM有更好的催化活性。考察了带水剂的选择、酸醇量比〔n(C7H6O3)∶n(C4H10O)〕、催化剂用量〔w(SO2-4/SiZrM)〕、反应时间(t)、反应温度(θ)对催化合成水杨酸正丁酯(C11H14O3)的影响,并对合成的产物进行了折光率、红外光谱分析。酯化反应的最佳条件为:C4H10O为带水剂、n(C7H6O3)∶n(C4H10O)=1∶1 65、催化剂占酸投料质量的百分比为w(SO2-4/SiZrM)=6 5%、t=6h、θ=120～135℃,水杨酸的转化率可达88 22%,产物中w(C11H14O3)>99 9%。
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| 关 键 词： | 硅锆交联剂 固体酸 水杨酸正丁酯 蒙脱土 |
| 文章编号： | 1003-5214(2003)06-0352-04 |
| 修稿时间： | 2002年9月23日 |
Synthesis of n-Butyl Salicylate Catalyzed by SO2-4 Modified Cross-linked Montmorillonite Solid Acid |
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| Abstract: | The mixed SiZr pillared montmorillonite,modified by SO2-4,was used as solid acid catalyst (SO2-4/SiZrM) in the esterification reaction of salicylic acid (C7H6O3) and n butyl alcohol (C4H10O).The results showed that SO2-4/SiZrM exhibited higher activity in the synthesis of n butyl salicylate (C11H14O3) than the traditional catalysts,such as concentrated sulfuric acid,phosphotungstic acid,ferric ammonium sulfate and other sorts of pillared montmorillonite.In the presence of SO2-4/SiZrM,the optimized reaction conditions for preparing C11H14O3 were as follows.Excess of n butyl alcohol acted as water entrainer,n(C7H6O3)∶n(C4H10O)=1∶165,w(SO2-4/SiZrM) was 65% the weight of salicylic acid,reaction time was 6 h,and reaction temperature was 120-135 ℃.Conversion of salicylic acid amounted to 8822% and w(C11H14O3) was over 999% tested by GC analysis. |
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| Keywords: | SiZr pillared agent solid acid n-butyl salicylate montmorillonite |
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