固体酸SO_4~(2-)/SiO_2-TiO_2催化合成乙酰水杨酸研究
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摘要
以水杨酸和乙酸酐为原料,用SO~(2-)_4/SiO_(2-)TiO_2固体酸为催化合成乙酰水杨酸,考察了TiO_2与SiO_2质量比、硫酸浸渍量、浸渍时间、煅烧温度等因素对乙酰水杨酸产率影响,通过红外光谱、扫描电镜和激光粒度仪对催化剂或合成产物进行了表征。得到最佳反应条件:SiO_2:TiO_2质量比为0.4:1、硫酸浸渍量与TiO_2质量比为0.49:1、浸渍时间为26 h、煅烧温度为400℃,该条件下制备的固体酸催化合成乙酰水杨酸产率为65%。该催化剂具有易与反应体系分离,对设备腐蚀性小,可再生等优点。
Used salicylic acid and acetic anhydride as raw materials,synthesis of Acetylsalicylic acid with SO_4~(2-)/SiO_(2-)TiO_2 solid acid as catalyst,The mass ratio of TiO_2 to SiO_2,sulfuric acid impregnation,dipping time,effect of calcination temperature and other factors on the catalytic performance of SO_4~(2-)/SiO_(2-)TiO_2 were investigated.By means of infrared spectrometer,field emission scanning electron microscope and laser particle sizer were used to analyze and characterize it.The best reaction conditions were obtained:the SiO_2:TiO_2 mass ratio was 0.4:1,Sulfuric acid impregnation amount was 0.49:1,The soaking time was 26 h and the roasting temperature was 400℃,and the yield of acetylsalicylic acid was 65%under this condition.The catalyst is easy to be separated from the reaction system,and has the advantages of small corrosion,renewable.
Used salicylic acid and acetic anhydride as raw materials,synthesis of Acetylsalicylic acid with SO_4~(2-)/SiO_(2-)TiO_2 solid acid as catalyst,The mass ratio of TiO_2 to SiO_2,sulfuric acid impregnation,dipping time,effect of calcination temperature and other factors on the catalytic performance of SO_4~(2-)/SiO_(2-)TiO_2 were investigated.By means of infrared spectrometer,field emission scanning electron microscope and laser particle sizer were used to analyze and characterize it.The best reaction conditions were obtained:the SiO_2:TiO_2 mass ratio was 0.4:1,Sulfuric acid impregnation amount was 0.49:1,The soaking time was 26 h and the roasting temperature was 400℃,and the yield of acetylsalicylic acid was 65%under this condition.The catalyst is easy to be separated from the reaction system,and has the advantages of small corrosion,renewable.
引文
[1]Zheng Z,Huang H H,Ma X,et al.Production of diacylglycerols by esterification of oleic acid with glycerol catalyzed by diatomite loaded SO2-4/TiO2[J].Journal of Industrial and Engineering Chemistry,2017,30(6):1-10.
[2]张宁.S2O82-/TiO2-Al2O3催化水解花生壳制备乙酰丙酸的研究[J].化学研究与应用,2013,25(4):536-540.
[3]Song Z X,Zhang Q L,Ning P,et al.Introduction manner of sulfate acid for improving the performance of SO42-/CeO2 on selective catalytic reduction of NO by NH3[J].Journal of Rare Earths,2016,34(7):667-674.
[4]Venugopalarao N,Ravi V,Pudukulathan Z.SO/SnO2-catalyzed C3-Alkylation of 4-Hydroxycoumarin with secondary benzyl alcohols and O-Alkylation with O-Acetyl compounds[J].International Journal of Organic Chemistry,2012,2:287-294.
[5]Huang Z X,Lin Y X,Li L,et al.Preparation and shaping of solid acid SO/TiO2 and its application for esterification of propylene glycol monomethyl ether and acetic acid[J].Chinese Journal of Chemical Engineering,2017,25(9):1207-1216.
[6]Imteaz A,Nazmul A,Dinesh K,et al.Liquid-phase dehydration of sorbitol to isosorbide using sulfated titania as a solid acid catalyst[J].Chemical Engineering Science,2013,93:91-95.
[7]Li H J,Song H L,Chen L W,et al.Designed SO/Fe2O3-SiO2 solid acids for polyoxymethylene dimethyl ethers synthesis:The acid sites control and reaction pathways[J].Applied Catalysis B:Environmental,2015,165:466-476.
[8]黄宏升,金华峰.新型固体酸 SO/B2O3/ZrO2的制备及其催化酯化反应性能研究[J].化学研究与应用,2016,28(3):343-349.
[9]曹小华,王原平,雷艳虹,等.H6P2W18O62/MCM-41催化剂的制备、表征及其催化合成乙酰水杨酸[J].石油化工,2014,43(2):176-180.
[10]占昌朝,曹小华,严平,等.碳基固体酸催化合成乙酰水杨酸[J].化工进展,31(5):1121-1125.
[11]陈桂,周育辉,唐梦婷,等.超声辅助SiO2-Al2O3催化合成乙酰水杨酸工艺研究[J].怀化学院学报,2016.35(5):37-40.
[12]王广建,韩亚飞,王芳,等.超声波辅助合成钛硅分子筛及其脱硫性能的研究[J].高校化学工程学报,2016,30(1):189-194.
[13]钟少锋.预氧化聚丙烯腈纤维膜负载SO/TiO2固体酸催化剂的制备及其催化性能研究[J].化学研究与应用,2015,27(5):595-599.
[2]张宁.S2O82-/TiO2-Al2O3催化水解花生壳制备乙酰丙酸的研究[J].化学研究与应用,2013,25(4):536-540.
[3]Song Z X,Zhang Q L,Ning P,et al.Introduction manner of sulfate acid for improving the performance of SO42-/CeO2 on selective catalytic reduction of NO by NH3[J].Journal of Rare Earths,2016,34(7):667-674.
[4]Venugopalarao N,Ravi V,Pudukulathan Z.SO/SnO2-catalyzed C3-Alkylation of 4-Hydroxycoumarin with secondary benzyl alcohols and O-Alkylation with O-Acetyl compounds[J].International Journal of Organic Chemistry,2012,2:287-294.
[5]Huang Z X,Lin Y X,Li L,et al.Preparation and shaping of solid acid SO/TiO2 and its application for esterification of propylene glycol monomethyl ether and acetic acid[J].Chinese Journal of Chemical Engineering,2017,25(9):1207-1216.
[6]Imteaz A,Nazmul A,Dinesh K,et al.Liquid-phase dehydration of sorbitol to isosorbide using sulfated titania as a solid acid catalyst[J].Chemical Engineering Science,2013,93:91-95.
[7]Li H J,Song H L,Chen L W,et al.Designed SO/Fe2O3-SiO2 solid acids for polyoxymethylene dimethyl ethers synthesis:The acid sites control and reaction pathways[J].Applied Catalysis B:Environmental,2015,165:466-476.
[8]黄宏升,金华峰.新型固体酸 SO/B2O3/ZrO2的制备及其催化酯化反应性能研究[J].化学研究与应用,2016,28(3):343-349.
[9]曹小华,王原平,雷艳虹,等.H6P2W18O62/MCM-41催化剂的制备、表征及其催化合成乙酰水杨酸[J].石油化工,2014,43(2):176-180.
[10]占昌朝,曹小华,严平,等.碳基固体酸催化合成乙酰水杨酸[J].化工进展,31(5):1121-1125.
[11]陈桂,周育辉,唐梦婷,等.超声辅助SiO2-Al2O3催化合成乙酰水杨酸工艺研究[J].怀化学院学报,2016.35(5):37-40.
[12]王广建,韩亚飞,王芳,等.超声波辅助合成钛硅分子筛及其脱硫性能的研究[J].高校化学工程学报,2016,30(1):189-194.
[13]钟少锋.预氧化聚丙烯腈纤维膜负载SO/TiO2固体酸催化剂的制备及其催化性能研究[J].化学研究与应用,2015,27(5):595-599.