无机化学学报

纳米复合固体超强酸SO₄^2-/ZnFe₂O₄的制备与催化合成癸二酸二乙酯的研究

Preparation of Nano Solid Superacid SO₄^2-/ZnFe₂O₄ and Catalyzed Synthesis of Diethyl Sebacate

作者	单位
金华峰	安康师范专科学校化学系,安康 725000
李文戈	清华大学材料科学与工程系,北京 100084

摘要: 以硫酸盐为原料,添加NaOH和NaHCO₃以制备出碱式碳酸盐前驱体,合成出新型的纳米固体超强酸催化剂SO₄^2-/ZnFe₂O₄,经XRD、BET、IR等检测,粒径为35nm,比表面积很大(137m^2-1),粒度均匀。首次以该固体酸为催化剂,癸二酸和无水乙醇为原料合成癸二酸二乙酯,考察了影响反应的因素。结果表明,醇酸摩尔比为4.0∶1,催化剂用量为1.0g(癸二酸0.1mol),带水剂苯15mL,反应时间2.5h是最佳反应条件,酯化率可达91%,并推断出该催化剂的酸强度-16.02< H_o< -14.52.

关键词: 纳米复合固体超强酸 SO₄^2-/ZnFe₂O₄ 癸二酸二乙酯催化合成

基金项目:

Abstract: Ferrite nanocrystalline materials are prepared by roasting basic carbonate precursor synthesized with very fine crystalline grain by using sulfate, NaOH and NaHCO₃.The new nanosolid superacid SO₄^2-/ZnFe₂O₄ is prepared by using nanometer chemical technology. The structure of catalyst has been studied by XRD, BET and IR methods. The results show that SO₄^2-/ZnFe₂O₄ is superfine solid(35nm) belong to nanocrystal and has high specific surface area (137.0mg²·g^-1).The synthesis of diethyl sebacate from absolute ethanol and sebacic acid with solid superacid SO₄^2-/ZnFe₂O₄ as catalyst has been studied. The influence factors of the reaction had been investigated.The results showed that the optimum conditions are as follows.The weight of the catalyst was 1.0g (if the weight of sebacic acid was 0.1mol );molar ratio of absolute ethanol to sebacic acid was 4.0∶1; the reaction time was 2.5h; the taking water reagent(benzene)was 15mL. The yield of diethyl sebacate was about 91%. The catalytic activity and strength of acid (-16.02< H_o<-14.52) were measured.

Keywords: nanosolid superacid SO₄^2-/ZnFe₂O₄ diethyl sebacate catalysis synthesis

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金华峰,李文戈.纳米复合固体超强酸SO₄^2-/ZnFe₂O₄的制备与催化合成癸二酸二乙酯的研究[J].无机化学学报,2002,18(3):265-268.

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