蔡城辉,范明明,张萍波.双酸位分子筛的制备及催化合成单癸酸甘油酯[J].中国油脂,2022,47(12):.[CAI Chenghui, FAN Mingming, ZHANG Pingbo.Preparation of molecular sieves with double-acid active sites and catalytic synthesis of glycerol monodecanoate[J].China Oils and Fats,2022,47(12):.]
双酸位分子筛的制备及催化合成单癸酸甘油酯
Preparation of molecular sieves with double-acid active sites and catalytic synthesis of glycerol monodecanoate
  
DOI:
中文关键词:  介孔分子筛;双酸位;Ti-SBA-15-SO3H  酯化反应;单癸酸甘油酯
英文关键词:mesoporous molecular sieve  double-acid active sites  Ti-SBA-15-SO3H  esterification  glycerol monodecanoate
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作者单位
蔡城辉,范明明,张萍波 江南大学 化学与材料工程学院江苏 无锡 214122 
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中文摘要:
      为了制备适用于催化合成单癸酸甘油酯(GMC)的催化活性高、重复利用性强以及热稳定性好的固体酸催化剂,以钛酸四丁酯为钛源、正硅酸乙酯为硅源,采用软模板法在酸性条件下合成Ti-SBA-15,再通过有机接枝的方法引入磺酸基团,制备了同时含有Bronsted酸位点和Lewis酸位点的介孔分子筛催化剂Ti-SBA-15-SO3H。采用XRD、FT-IR、Py-IR、BET、EDS等表征手段对该催化剂的表面结构、化学键、酸性位点及酸量、孔道结构、元素分布进行评价,对总酸量进行了测定。以甘油与癸酸酯化合成GMC反应作为探针反应,考察了介孔分子筛催化剂的催化活性。结果表明,Ti的掺入为介孔分子筛提供了Lewis酸位点,引入的磺酸基团增加了介孔分子筛的Bronsted酸位点,同时所制得的Ti-SBA-15-SO3H保留了SBA-15原有表面和孔道结构。该催化剂在反应时间5 h、反应温度150℃、甘油与癸酸物质的量比4∶1、催化剂用量4%(以总反应物质量计)的条件下,癸酸转化率接近98%,GMC收率达78%以上。该催化剂在循环使用4次之后,GMC收率仍高于70%。制备得到的双酸位分子筛催化剂催化活性高、重复利用性强、热稳定性好,适用于催化合成GMC。
英文摘要:
      In order to prepare solid acid catalyst with high catalytic activity, strong reusability and good thermal stability for the catalytic synthesis of glycerol monodecanoate(GMC),with tetrabutyl titanate as titanium source and tetraethyl orthosilicate as silicon source, Ti-SBA-15 was synthesized under acidic conditions by soft template method, and sulfonic acid group was introduced by organic grafting. Finally, a mesoporous molecular sieve catalyst Ti-SBA-15-SO3H containing both Bronsted and Lewis acid sites was successfully prepared. The surface structure, chemical bonds, acidic sites and acidity, pore structure and element distribution of the catalyst were characterized by XRD, FT-IR, Py-IR, BET and EDS. The total acidity was determined. The catalytic activity of mesoporous molecular sieve catalysts was investigated by using the esterification of glycerol with capric acid to prepare GMC as a probe reaction.The results showed that Ti doping provided Lewis acid sites for mesoporous molecular sieves, and the introduction of sulfonic acid groups increased the Bronsted acid sites of mesoporous molecular sieves.At the same time, the prepared Ti-SBA-15-SO3H retained the original surface and pore structure of SBA-15. With Ti-SBA-15-SO3H as the catalyst, under the conditions of reaction time 5 h, reaction temperature 150℃, molar ratio of glycerol to capric acid 4∶1 and catalyst dosage 4% (based on total reactants mass), the conversion rate of capric acid was close to 98%, and the yield of GMC was over 78%. After the catalyst was recycled 4 times, the GMC yield was still higher than 70%.The prepared molecular sieve catalyst with double-acid active sites has high catalytic activity, strong reusability and good thermal stability, and is suitable for the catalytic synthesis of GMC.
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