Ga_2O_3-凹凸棒固体酸催化剂对苯甲醛乙二醇缩醛的催化合成  

Synthesis of Benzaldehyde Glycol Acetal with Ga_2O_3-Attapulgite Solid Acid Catalyst

作　　者：李恩博[1] 段伟萍 

机构地区：[1]河北北方学院理学院,河北张家口075000 [2]张家口市第二十一中学,河北张家口075000

出　　处：《河北北方学院学报（自然科学版）》2017年第1期25-28,共4页Journal of Hebei North University:Natural Science Edition

基　　金：河北省科技厅项目(15211033);河北省教育厅项目(Z2014023)

摘　　要：目的将凹凸棒黏土负载Ga_2O_3制备的Ga_2O_3-凹凸棒固体酸催化剂,用于苯甲醛乙二醇缩醛的合成。方法以凹凸棒黏土、Ga(NO3)3作为原料,采用沉淀法制备Ga_2O_3-凹凸棒固体酸催化剂。以苯甲醛、乙二醇作为反应物,催化合成苯甲醛乙二醇缩醛,通过红外光谱和折光率的测定对合成产物的结构进行表征,通过正交实验方法对醛醇物质的量比、催化剂使用量、反应温度、反应时间等合成反应条件进行考察和优化,通过正交分析和对比实验对催化剂的催化活性进行探讨,同时进行催化剂重复使用性实验研究。结果合成产物结构由红外光谱和折光率检测确定。当苯甲醛使用量为0.2mol时,苯甲醛乙二醇缩醛合成的最佳反应条件为n(苯甲醛)∶n(乙二醇)=1∶1.6,当催化剂使用量为0.7g,反应温度为105℃,反应时间为90min时,所得产品收率不低于86.0%,所制催化剂的催化效果与催化剂使用量有关。催化剂经6次重复使用,所得产品收率仍达77.3%,高于浓硫酸催化法和空白对照实验所得产品收率,同时所得产品成色更好。结论使用所制得的催化剂合成了苯甲醛乙二醇缩醛,该催化剂具有较强的催化活性和良好的重复使用性。Objective Ga_2O_3-attapulgite solid acid catalyst was prepared by attapulgite loading Ga_2O_3,and it was used for synthesis of benzaldehyde glycol acetal.Methods The Ga_2O_3-attapulgite solid acid catalyst was prepared by precipitation method with attapulgite and Ga(NO3)3as raw material,and benzaldehyde glycol acetal(synthetic production)was synthesized from benzaldehyde and ethylene glycol as reaction substance.Synthetic products were characterized by IR,refractive index.The synthesis conditions of production,such as molar ratio of alcohol to aldehyde,mass of catalyst,reaction temperature and reaction time,were studied by orthogonal experiment method.The catalyst activity was discussed by orthogonal analysis and contrast experiment.The reusability of catalyst was also investigated.Results The structure of product was determined by IR and refractive index.The suitable conditions for preparation of products were:n(benzaldehyde)∶n(ethylene glycol)was 1∶1.6(benzaldehyde was 0.2mol),the mass of catalyst was 0.7g,the reaction proceeded at 105 ℃ for 90 min,the yield of production was no less than 86.0%,and the effect of catalyst was controlled by the mass of catalyst.It could reach to77.3% after catalyst was uesd for 6times being higher than those in catalysis by H2SO4 and contrast experiment.Conclusion The catalyst showed better activity and reusability when used for synthesis of benzaldehyde glycol acetal.

关 键 词：凹凸棒黏土 GA2O3 苯甲醛乙二醇缩醛 催化 正交实验方法 

分 类 号：O643[理学—物理化学]