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对甲苯磺酸改性SBA-15的合成及催化合成乙酸正丁酯

Synthesis and catalytic activity of TsOH-modified SBA-15 mesoporous molecular sieve

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【作者】 田志茗邓启刚孙慧赵德丰

【Author】 TIAN Zhi-ming1,2,DENG Qi-gang2,SUN Hui2,ZHAO De-feng1(1.State Key Laboratory of Fine Chemicals,Dalian University of Technology,Dalian 116012,China;2.College of Chemistry and Chemical Engineering of Qiqihar University,Qiqihar 161006,China)

【机构】 大连理工大学国家重点实验室齐齐哈尔大学化学与化工学院大连理工大学国家重点实验室 辽宁大连116012黑龙江齐齐哈尔161006辽宁大连116012

【摘要】 采用浸渍法将含有磺酸基的对甲苯磺酸负载在SBA-15表面上,合成含有一定酸性的固体酸催化剂TsOH-SBA-15。催化剂的制备条件为:对甲苯磺酸的浸渍浓度为0.5 mol/L,焙烧温度为300℃,焙烧时间为4 h。用XRD,IR,DTA/TGA,氮吸附-脱附等方法对改性后的样品进行表征。结果表明,改性后的SBA-15分子筛的结构未发生变化,仍具有有序孔道结构。TsOH-SBA-15催化剂对冰乙酸和正丁醇的酯化反应具有较高的活性,正交实验结果为:反应时间80 m in,n(冰乙酸)∶n(正丁醇)=1∶1.2,催化剂用量为冰乙酸质量的5%,此时酯化率可达到95%。

【Abstract】 The SBA-15 mesoporous silica materials containing alkyl sulfonic acid group was prepared by impregnating TsOH to the surface of SBA-15.The catalyst prepared by impregnating SBA-15 in solution of 0.5 mol/L TsOH and being calcined at 300 ℃ for 4 h acetate.The samples were characterized by XRD,IR,DTA/TGA,N2 adsorption-desorption techniques.The TsOH-SBA-15 keeps the highly ordered mesoporous structure and does not change the mesoporous channel structure of SBA-15 molecular sieve.TsOH-SBA-15 was an excellent catalyst to synthesis of n-butyl acetate.The optimum conditions of the esterification by orthogonal experiments were studied:The mole ratio of acetic acid to n-butanol 1 ∶1.2,the amount of catalyst 5%,reaction time 80 min.The yield of n-butyl acetate could reach 95%.

  • 【文献出处】 应用化工 ,Applied Chemical Industry , 编辑部邮箱 ,2007年08期
  • 【分类号】TQ225.24
  • 【被引频次】8
  • 【下载频次】343
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