Preparation of molecular sieves with double-acid active sites and catalytic synthesis of glycerol monodecanoate
  
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KeyWord:mesoporous molecular sieve  double-acid active sites  Ti-SBA-15-SO3H  esterification  glycerol monodecanoate
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Author NameAffiliation
CAI Chenghui, FAN Mingming, ZHANG Pingbo School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122,Jiangsu, China 
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Abstract:
      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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