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化学工业与工程 2010, Vol. 27 Issue (1) :7-10    DOI:
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硼酸三丁酯的合成
张吉初;张海渤;刘霞;张丽芳;
北京石油化工学院化工系;
Synthesis of Tributyl Borate
ZHANG Ji-chu,ZHANG Hai-bo,LIU Xia,ZHANG Li-fang(Chemical Engineering Department, Beijing Institute of Petrochemical Technology, Beijing 102617, China)
(Chemical Engineering Department, Beijing Institute of Petrochemical Technology, Beijing 102617, China

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摘要 以正丁醇和硼酸为原料采用微波辐射法合成硼酸三丁酯,考察了催化剂、带水剂、反应时间和反应温度对反应的影响。通过试验得到适宜工艺条件(试验室)为:硼酸用量为0.10mol、n(正丁醇)/n(硼酸)为5.2(正丁醇兼作带水剂)、m(NaHSO4催化剂)/m(原料总量)为2.2%和微波辐射时间为13.0min。该条件下产品平均收率为87.4%,反应速率(以酯的收率计)约是常规加热法的18~20倍。通过元素和红外光谱分析对产品进行了物性及结构表征。
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张吉初
张海渤
刘霞
张丽芳
关键词硼酸三丁酯   微波辐射   酯化反应   合成     
Abstract: Tributyl borate was synthesized by esterification of boric acid with n-butanol under microwave irradiation. The effects of catalyst, water-carrying reagent, reaction time and reaction temperature have been investigated. The optimum condition of reaction has been found: boric acid 6.2 g(0.10 mol), n-butanol 47.4 mL(0.52 mol, also as water-carrying reagent), one hydrated sodium bisulfate as catalyst 1.0 g (2.2% of the total mass of raw materials), microwave irradiation time 13.0 min, the average yield of product is 87.4%. The reaction under microwave irradiation was about 18—20 times faster than that under conventional heating. The physical property and structure of product have been characterized by IR and elementary analysis.
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Received 2010-01-15; published 2010-01-15
引用本文:   
张吉初;张海渤;刘霞;张丽芳;.硼酸三丁酯的合成[J].  化学工业与工程, 2010,27(1): 7-10
ZHANG Ji-chu,ZHANG Hai-bo,LIU Xia,ZHANG Li-fang.Synthesis of Tributyl Borate[J].  Chemcial Industry and Engineering, 2010,27(1): 7-10
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