引用本文:
金华峰, 李宝璋. 纳米复合固体超强酸S2O82-/CoFe2O4催化合成癸二酸二乙酯[J]. 应用化学,
2003, 20(1): 10-14.
Citation: JIN Hua-Feng, LI Bao-Zhang. Preparation of Nanosized Solid Superacid S2O82-/CoFe2O4 and Catalytic Synthesis of Diethyl Sebacate[J]. Chinese Journal of Applied Chemistry, 2003, 20(1): 10-14.
Citation: JIN Hua-Feng, LI Bao-Zhang. Preparation of Nanosized Solid Superacid S2O82-/CoFe2O4 and Catalytic Synthesis of Diethyl Sebacate[J]. Chinese Journal of Applied Chemistry, 2003, 20(1): 10-14.
纳米复合固体超强酸S2O82-/CoFe2O4催化合成癸二酸二乙酯
摘要:
将硫酸钴、硫酸亚铁在NaOH溶液中与NaHCO3反应制得碱式碳酸盐前驱体,后者用(NH4)2S2O8浸渍、干燥,再经500℃焙烧得到固体超强酸催化剂S2O82-/CoFe2O4。产物经XRD、TEM、BET、TG-DTA及化学法等检测,含硫量4.52%,粒径为42 nm,比表面积为146 m2/g,粒度均匀。催化剂的酸强度处于-16.02和-14.52之间。以该固体酸为催化剂,由癸二酸和无水乙醇合成了癸二酸二乙酯。最佳反应条件为:n(醇):n(酸)=4.0:1.0,癸二酸0.1 mol,催化剂1.0 g,反应时间25h。在此反应条件下,酯化率可达93.6%。
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关键词:
- 纳米复合固体超强酸
- / S2O82-/CoFe2O4
- / 癸二酸二乙酯
- / 催化酯化反应
English
Preparation of Nanosized Solid Superacid S2O82-/CoFe2O4 and Catalytic Synthesis of Diethyl Sebacate
Abstract:
Reacting the mixture of fine cobalt sulfate and ferrous sulfate with PEG-600 in NaOH solution(at pH=9.0) gave a precusor, CoFeO(OH)2O, which after immersion in (NH4O)2S2O8 solution, reacting, drying and calcinating at 500℃ afforded the title solid superacid S2O82-/CoFe2O4. The compound was characterized by XRD, TEM, BET, TG-DTA techniques and chemical analysis. The results show that S2O82-/CoFe2O4 was sized in 42 nm with specific surface area of 146 m2/g. The solid superacid S2O82-/CoFe2O4 was used as catalyst in synthesis of diethyl sebacate from absolute ethanol and sebacic acid. At the conditions of 1.0 g catalyst with the acid strength of -16.02< H0< -14.52, 0.1 mol sebacic acid, molar ratio of absolute ehtanol to sebacic acid 4.0:1.0, and reaction time of 2.5 h, diethyl sebacate in yield of 93.6% was obtained.
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Key words:
- nanosized solid superacid
- / S2O82-/CoFe2O4
- / diethyl sebacate
- / catalytic esterification
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