利用固体催化剂制备丙酮缩甘油的工艺研究
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摘要
以固体酸作为催化剂,以甘油和丙酮为原料合成丙酮缩甘油,考察了反应温度、反应时间、反应物配比、催化剂用量对反应的影响。实验结果表明,甲苯为带水剂,催化剂用量为甘油质量的6%,原料n(甘油)∶n(丙酮)为1∶3,反应时间为6 h,反应的温度为80℃,丙酮缩甘油的产率可达80%。本文采用固体酸作为催化剂,产品易分离且无需除酸,后处理简单。
Solid acid was used as a catalyst for the synthesis of acetone glycerin to synthesize solketal. The effect of reaction temperature,reaction time,reactant ratio and the amount of catalyst on the reaction was investigated. The experimental results showed that amount of catalyst was 6% of the glycerin quality,raw materials n( glycerol) ∶n( acetone) was 1∶3,toluene was used as the water-carrying agent,the reaction time was 6 h,the reaction temperature was 80 ℃,solketal yield was up to 80%. Using solid acid as a catalyst,the product was easy to separate and without removing acid.
Solid acid was used as a catalyst for the synthesis of acetone glycerin to synthesize solketal. The effect of reaction temperature,reaction time,reactant ratio and the amount of catalyst on the reaction was investigated. The experimental results showed that amount of catalyst was 6% of the glycerin quality,raw materials n( glycerol) ∶n( acetone) was 1∶3,toluene was used as the water-carrying agent,the reaction time was 6 h,the reaction temperature was 80 ℃,solketal yield was up to 80%. Using solid acid as a catalyst,the product was easy to separate and without removing acid.
引文
[1]Rabindran Jenny B,Pandurangan A.AI-MCM-41 as an efficient heterogeneous catalyst in the actualization of cyclohexanone with methanol,ethylene glycol and pentaerythr1-tol[J].Journal of Molecular Catalysis A(Chemical),2006(256):184-192.
[2]龚菁,王云翔,钱蕙.微波辐射稀土固体超强酸催化合成苯甲醛乙二醇缩酮[J].精细化工,2004,21(12):920-922.
[3]Kim J,Cho G.Thermal storage/release,durability and temperature sensing properties of thermostatic fabrics treated with octadecanecontaining microcapsules[J].Textile Re-search Journa,2002,72(12):1093-1098.
[4]吕宝兰,杨水金,孙艳德.磷钨酸在催化合成酯类和缩醛(酮)中应用研究进展[J].化工科技,2005,13(3):49-54.
[5]梁学正,刘彩华,高珊,等.HMCM-22沸石分子筛催化合成缩醛(酮)[J].化工进展,2005,24(12):1383-1385.
[6]任立国.二氧化钛负载磷钨酸固体酸催化合成苯甲醛甘油缩醛[J].抚顺石油学院学报,2008(4):2-5.
[7]李晓燕,肖国民,魏瑞平,等.Al Cl3改性阳离子交换树脂催化合成异丙叉甘油[J].过程工程学报,2008,8(2):263-266.
[8]高艳芬.苯甲酸甘油单酯的制备[J].医学研究与教育,2010,7(4):2-4.
[9]黄文芳.叶立德化学[M].湖北华中师范大学出版社,1993:3-281.
[10]Mori K,Takigawa T,Matsuo T.Synthesis of Brefeldin[J].Tetrahedron,1979,35:933-940.
[2]龚菁,王云翔,钱蕙.微波辐射稀土固体超强酸催化合成苯甲醛乙二醇缩酮[J].精细化工,2004,21(12):920-922.
[3]Kim J,Cho G.Thermal storage/release,durability and temperature sensing properties of thermostatic fabrics treated with octadecanecontaining microcapsules[J].Textile Re-search Journa,2002,72(12):1093-1098.
[4]吕宝兰,杨水金,孙艳德.磷钨酸在催化合成酯类和缩醛(酮)中应用研究进展[J].化工科技,2005,13(3):49-54.
[5]梁学正,刘彩华,高珊,等.HMCM-22沸石分子筛催化合成缩醛(酮)[J].化工进展,2005,24(12):1383-1385.
[6]任立国.二氧化钛负载磷钨酸固体酸催化合成苯甲醛甘油缩醛[J].抚顺石油学院学报,2008(4):2-5.
[7]李晓燕,肖国民,魏瑞平,等.Al Cl3改性阳离子交换树脂催化合成异丙叉甘油[J].过程工程学报,2008,8(2):263-266.
[8]高艳芬.苯甲酸甘油单酯的制备[J].医学研究与教育,2010,7(4):2-4.
[9]黄文芳.叶立德化学[M].湖北华中师范大学出版社,1993:3-281.
[10]Mori K,Takigawa T,Matsuo T.Synthesis of Brefeldin[J].Tetrahedron,1979,35:933-940.