纳米复合固体超强酸S_2O_8^(2-)/CoFe_2O_4催化合成癸二酸二乙酯  

Preparation of Nanosized Solid Superacid S_2O_8^(2-)/CoFe_2O_4 and Catalytic Synthesis of Diethyl Sebacate

作　　者：金华峰[1] 李宝璋[2] 

机构地区：[1]安康师范专科学校化学系,安康725000 [2]西北大学化工系

出　　处：《应用化学》2003年第1期10-14,共5页Chinese Journal of Applied Chemistry

基　　金：陕西省教育厅自然科学专项应用基础研究项目 (0 1JK2 0 3);中国石油天然气集团公司科学研究与开发项目 (990 816 0 3);安康师专科研基金项目 (2 0 0 2AZXZR0 0 3)

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 ) 2 S2 O8浸渍、干燥 ,再经 5 0 0℃焙烧得到固体超强酸催化剂S2 O2 -8/CoFe2 O4 。产物经XRD、TEM、BET、TG DTA及化学法等检测 ,含硫量 4 5 2 % ,粒径为 4 2nm ,比表面积为 1 4 6m2 /g ,粒度均匀。催化剂的酸强度处于 -1 6 0 2和-1 4 5 2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 1mol,催化剂 1 0 g ,反应时间 2 5h。在此反应条件下 ,酯化率可达 93 6%。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)_2, which after immersion in (NH_4)_2S_2O_8 solution, reacting, drying and calcinating at 500 ℃ afforded the title solid superacid S_2O 2- _8/CoFe_2O_4. The compound was characterized by XRD, TEM, BET, TG-DTA techniques and chemical analysis. The results show that S_2O 2- _8/CoFe_2O_4 was sized in 42 nm with specific surface area of 146 m 2/g. The solid superacid S_2O 2- _8/CoFe_2O_4 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<H_0<-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.

关 键 词：催化合成 纳米复合固体超强酸 S2O8^2-/CoFe2O4 癸二酸二乙酯 催化酯化反应 催化剂 

分 类 号：O623.624[理学—有机化学] O643.32[理学—化学]