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机构地区:[1]四川大学化工学院,四川成都610065 [2]成都惠恩精细化工有限责任公司,四川成都610065
出 处:《应用化工》2014年第2期277-280,283,共5页Applied Chemical Industry
摘 要:以竹材为原料,硫酸为磺化剂,通过炭化-磺化法制得竹炭基固体磺酸催化剂,并用于癸二酸和正丁醇的酯化反应,考察了制备条件对催化剂活性的影响。采用傅里叶红外光谱(FTIR)、X射线衍射(XRD)、扫描电子显微镜仪(SEM)及热失重分析(TGA)等手段对催化剂进行表征。结果表明,在炭化温度325℃下炭化1 h,磺化温度125℃下磺化1 h制得的催化剂,其含酸量可达到1.4 mmol/g,在催化癸二酸和正丁醇的酯化反应中,转化率高达99%,此时催化剂的催化活性最高,且催化剂可循环多次利用。此竹炭基固体磺酸催化剂具有无定形炭结构,热稳定性可达230℃。The novel carbon-based solid acids were synthesized through the carbonation and then sulfona- tion of the bamboo charcoal in sulfuric acid. The esterification of sebacic acid and n-butyl alcohol was taken as the model reaction to investigate the impact of preparation parameters on the catalyst activity. FTIR,XRD,SEM and TGA were used to characterize the catalyst. The results showed that the carbon-based solid acid catalyst was prepared under the optimal conditions of carbonization at 325 ℃ for 1 h and then sulfonation at 125 ℃ for 1 h exhibiting higher catalytic activity, it' s sulfuric acid group can be reached 1.4 mmol/g. The conversion rate of sebacic acid reached 99% after reaction and the catalyst can be recycled for several times. Through characterization of the catalyst the carbon-based solid acid catalyst exhibit amorphous carbon structure and the onset thermal decomposition temperature of carbon-based solid acid catalyst is above 230 ℃.
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