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摘要
采用溶胶-凝胶法和浸渍法制备了La3+/CNMS-SO3H固体酸催化剂,催化剂的优化工艺为:La3+浓度为0.021 mol/L、硫酸浸渍浓度为2 mol/L、煅烧温度为500℃;通过BET、NH3-TPD、Py-FTIR等对催化剂的性质与结构进行表征。探究了单因素对α-蒎烯转化率及正龙脑收率的影响,结果表明,烯酸摩尔比为1:0.5、La3+/CNMS-SO3H质量为松节油质量的8%、温度为100℃、时间为8 h时,正龙脑的收率最高为40.83%,α-蒎烯转化率为100%;催化剂在重复使用6次之后,转化率仍在99%之上,龙脑的收率下降3%。
Abstract
La3+/CNMS-SO3H,a solid acid catalyst,is prepared by sol-gel method and impregnation method.Its properties and structure are characterized by BET,NH3-TPD,Py-FTIR,etc.The optimized preparation process for the catalyst is as follows:La3+ concentration is 0.021 mol·L-1,sulfuric acid impregnation concentration is 2 mol·L-1,and calcination temperature is at 500℃.Impacts of single factor on the conversion of α-pinene and the yield of borneol over the catalyst is explored.Results show that the highest yield of borneol can reach 40.83% and the conversion rate of α-pinene can achieve 100% when the molar ratio of α-pinene to oxalic acid is 1:0.5,the mass of La3+/CNMS-SO3H is 8% that of turpentine,temperature remains at 100℃,and reaction lasts for 8 h.After the catalyst has been used for 6 times,the conversion of α-pinene is still above 99%,and the yield of borneol drops by 3%.
关键词
La3+/CNMS-SO3H
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稳定性
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催化
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正龙脑
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酯化
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固体酸
Key words
La3+/CNMS-SO3H
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stability
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catalysis
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borneol
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esterification
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solid acid
Author summay
郭炜(1994-),男,硕士研究生,主要从事植物化工研究,531566942@qq.com
La3+/CNMS-SO3H固体酸的制备及其催化合成正龙脑的研究[J].
现代化工, 2021, 41(2): 107-113,119 DOI:10.16606/j.cnki.issn0253-4320.2021.02.021