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化学工业与工程 2014, Vol. 31 Issue (2) :18-23    DOI: 10.13353/j.issn.1004.9533.2014.02.004
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己二酸二酰肼合成工艺研究
杨俊阁1, 宋宝东1, 张华堂2
(1天津大学化工学院,天津 300072; 2山东潍坊科麦化工有限公司,山东 潍坊 262700)
Synthesis of Adipic Acid Dihydrazide by Two Steps
YANG  Jun-Ge1, SONG  Bao-Dong1, ZHANG  Hua-Tang2
(1School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China; 
2Shandong Weifang Kemai Chemical Coporation, Weifang 262700, China)

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摘要 对两步法合成己二酸二酰肼(ADH)的工艺条件进行了研究。首先采用己二酸和甲醇酯化反应合成了己二酸二甲酯,然后将己二酸二甲酯与水合肼酰肼化,得到了高纯度己二酸二酰肼,并确定了适宜的工艺条件:对于酯化反应,催化剂为KHSO4,用量为己二酸质量数的5.5%,n(醇)/n(酸)为4.0,反应时间1.0 h,在该条件下,产品己二酸二甲酯质量分数高达99.8%,收率为77%;对于酰肼化反应,n(肼)/n(酯)、n(醇)/n(酯)比均为4.0,反应时间为1.5 h,此条件下,ADH收率达99%,质量分数高达99.5%。
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杨俊阁1
宋宝东1
张华堂2
关键词己二酸二酰肼(ADH)   己二酸二甲酯   己二酸   水合肼   甲醇     
Abstract: The synthesis of adipic acid dihydrazide by two steps was investigated in this paper. Adipic acid was first esterified with methanol under the catalysis of KHSO4 to give dimethyl adipate, which was further reacted with hydrazine hydrate to produce adipic acid dihydrazide (ADH) with a high purity. The optimal conditions for the esterification reaction were determined as catalyst amount was 5.5% of the weight amount of adipic acid, molar ratio of methanol to adipic acid was 4.0, reaction time was 1.0 h. Under these conditions, the purity of dimethyl adipate was as high as 998% and the yield was 77%. For the hydrazide reaction, the optimal conditions were: molar ratio of both hydrazine hydrate and methanol to dimethyl adipate was 4.0, reaction time was 1.5 h. Under these conditions, the yield of adipic acid dihydrazide reached 99% and the purity was 99.5%.
Keywordsadipic acid dihydrazide   dimethyl adipate   adipic acid   hydrazine hydrate   methanol     
Received 2013-01-11;
Corresponding Authors: 宋宝东,电话:(022)27403584,E-mail:bdsong@tju.edu.cn。     Email: bdsong@tju.edu.cn
About author: 杨俊阁(1986-),女,硕士研究生,主要从事己二酸二酰肼合成及应用研究。
引用本文:   
杨俊阁, 宋宝东, 张华堂.己二酸二酰肼合成工艺研究[J].  化学工业与工程, 2014,31(2): 18-23
YANG Jun-Ge, SONG Bao-Dong, ZHANG Hua-Tang.Synthesis of Adipic Acid Dihydrazide by Two Steps[J].  Chemcial Industry and Engineering, 2014,31(2): 18-23
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