固体碱催化剂MgO@SBA-15催化大豆油制备生物柴油的研究
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摘要
以SBA-15分子筛为载体,采用浸渍法通过负载MgO制备了MgO@SBA-15固体碱催化剂,并对其进行了X射线衍射和N2吸附-脱附等分析表征,考察了焙烧温度、MgO负载量、醇油物质的量比和催化剂用量等因素对催化剂性能的影响。结果表明:MgO负载量为15%(质量分数)的MgO@SBA-15催化剂能够很好地保持SBA-15原有的介孔特征,且MgO在SiO2骨架上高度分散;在焙烧温度500℃、MgO负载量为15%时催化剂活性最佳;在醇油物质的量比为9∶1、催化剂用量为大豆油质量的3%、反应时间为3h的条件下,生物柴油的产率达到91.83%。
The solid base catalyst with SBA-15 molecular sieve as the carrier was prepared through loading MgO by the immersion method,and the catalyst was characterized by XRD and N2 adsorption-desorption isotherm.The results indicated that catalyst with 15%of MgO@SBA-15 could well maintain original mesoporous structure and MgO was highly dispersed on the silica skeleton.The effects of the different calcination temperature,catalyst dosage,ratio of alcohol to oil and mass ratio of catalyst to oil were investigated.The results indicated that the calcination temperature was 500℃,15% of MgO loading,the molar ratio of alcohol to oil 9∶1,and mass ratio of catalyst to oil 3%,the reaction time 3 h,the synthetically catalytic characteristics of MgO@SBA-15 was the best,and the biodiesel yield can reach up to 91.83%.
The solid base catalyst with SBA-15 molecular sieve as the carrier was prepared through loading MgO by the immersion method,and the catalyst was characterized by XRD and N2 adsorption-desorption isotherm.The results indicated that catalyst with 15%of MgO@SBA-15 could well maintain original mesoporous structure and MgO was highly dispersed on the silica skeleton.The effects of the different calcination temperature,catalyst dosage,ratio of alcohol to oil and mass ratio of catalyst to oil were investigated.The results indicated that the calcination temperature was 500℃,15% of MgO loading,the molar ratio of alcohol to oil 9∶1,and mass ratio of catalyst to oil 3%,the reaction time 3 h,the synthetically catalytic characteristics of MgO@SBA-15 was the best,and the biodiesel yield can reach up to 91.83%.
引文
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[2]Sun L B,Kou J H,Chun Y,et al.New attempt at directly generating superbasicity on mesoporous silica SBA-15[J].Inorganic Chemistry,2008,47(10):4199-4208.
[3]王健,李会鹏,赵华,等.K2O/Na2O-SBA-15催化大豆油合成生物柴油工艺条件优化[J].石化技术与应用,2014,32(2):127-130.
[4]蔡钒,张彬彬,林静,等.酯交换制生物柴油的CaO固体碱催化剂[J].物理化学学报,2008,24(10):1817-1823.
[5]丁平亮,田志茗,邓启刚.Ca-Mg-Al类水滑石催化大豆油甲醇酯交换制备生物柴油[J].工业催化,2011,19(11):84-87.
[6]Radwan Nagi R E.Influence of La2O3and ZrO2as promoters on surface and catalytic properties of CuO/MgO system prepared by sol-gel method[J].Applied Catalysis A:General,2006,299(1):103-121.
[7]魏一伦,曹毅,朱建华,等.MgO/SBA-15固体碱介孔材料的研制[J].无机化学学报,2003,19(3):233-239.
[8]白海鑫,刘小花,王喜云,等.SBA-15负载MgO催化大豆油与甲醇酯交换反应制备生物柴油的研究[J].河南农业大学学报,2010,44(6):656-659.
[9]Sun H,Han J X,Ding Y Q,et al.One-pot syntyesized mesoporous Ca/SBA-15solid base for transesterification of sunflower oil with methanol[J].Applied Catalysis A:General,2010,390(2):26-34.
[10]候谦奋,张前前,郭荣华,等.Ca/SBA-15固体碱催化剂的合成、表征及其催化餐饮废油制备生物柴油的研究[J].化学与生物工程,2015,32(8):28-34.
[11]Zhao D Y,Feng J L,Huo Q S,et al.Triblock copolymer synthesesof mesoporous silica with periodic 50to 300angstrom pores[J].Science,1998,279(5350):548-552.
[12]刘伟伟,苏有勇,张无敌,等.生物柴油中甘油含量测定方法的研究[J].可再生能源,2005,121(3):14-16.
[13]李雪真.K2O/CaO-SBA-15催化大豆油制备生物柴油研究[J].当代化工,2015,44(5):929-931.
[14]陈杰博,苏金为,祁建民,等.介孔固体碱KNO3/ZrO2的制备及催化红麻籽油制备生物柴油[J].化工进展,2010,29(z1):162-165.
[15]陈杰博,苏金为,祁建民,等.纳米固体碱CaO-ZrO2催化红麻籽油制备生物柴油[J].应用化学,2011,28(3):267-271.
[16]Ma H B,Li S F,Wang B Y,et al.Transesterification of rapeseed oil for synthesizing biodiesel by K/KOH/γ-Al2O3asheterogeneous base catalyst[J].Journal of the American Oil Chemsts'Society,2007,85(1):263-270.
[17]刘守庆,李雪梅,赵雷修,等.固体碱CaO催化橡胶籽油制备生物柴油的研究[J].中国油脂,2012,37(7):59-62.