Daminozide production method capable of reducing residual amount of UDMH (unsymmetric dimethyl hydrazine)
A production method and residue technology, applied in hydrazide preparation, organic chemistry, etc., can solve the problems of high UDMH content, and achieve the effects of high purity, good effect, and simple process control method
Inactive Publication Date: 2013-04-17
XIAN HANGJIE CHEM TECH
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Problems solved by technology
[0005] In order to solve the relatively high content of residual UDMH in the bijiu synthesized by the existing bijiu synthesis method, the present invention provides a kind of bijiu production method that reduces the residual amount of UDMH
Method used
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Embodiment
[0025] 1) Dissolution of succinic anhydride: Weigh 100 parts of succinic anhydride and add it into the reaction vessel, then add 400 parts of acetonitrile and stir it to fully dissolve it to make an acid anhydride solution;
[0026] 2] Weigh 60 parts of unsymmetrical dimethylhydrazine, and heat the above solution under stirring.
[0027] 3) When the temperature of the solution is 10°C, under stirring, add the acetonitrile solution of succinic anhydride dropwise with unsymmetrical dimethylhydrazine: adopt a dropping rate of 2L / min, keep the reaction temperature at 30°C-40°C until partial When dimethylhydrazine is added dropwise completely, after continuing to stir and react for 1 hour, collect the reaction solution;
[0028] 4) The collected reaction solution in step 3] is put into a centrifuge for centrifugation to obtain a bisulphate containing a small amount of acetonitrile;
[0029] 5] Vacuum-dry at 90°C for 2-3 hours to obtain Biju containing a small amount of acetonitril...
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The invention relates to a daminozide production method capable of reducing the residual amount of UDMH (unsymmetric dimethyl hydrazine), comprising the following steps of: 1) preparing the raw materials unsymmetric dimethyl hydrazine, succinic anhydride and acetonitrile in a mass part ratio of (56 to 61): 100: (300 to 500); 2) dissolving succinic anhydride by acetonitrile until the mass concentration of succinic anhydride is 25-33%; 3) dripping unsymmetric dimethyl hydrazine in the acetonitrile solution dissolved with succinic anhydride with stirring; 4) placing the collected reaction solution in a centrifugal machine, and performing centrifugal separation; and 5) performing vacuum-drying on daminozide containing trace acetonitrile for 2 to 3 hours at 80-90 DEG C, thereby obtaining daminozide. According to the daminozide production method, the problem of high content of residual UDMH in the existing daminozide is solved; a production process is improved, and finally, the residual amount (not greater than 30 ppm) of UDMH in the daminozide product is reduced to a technical index of export product requirements from 60-90 ppm before the improvement.
Description
technical field [0001] The invention belongs to the field of chemical and pharmaceutical intermediates, and in particular relates to a relatively long-term production method for reducing the residual amount of UDMH. Background technique [0002] Unsymmetrical dimethylhydrazine (UDMH) is an excellent hydrazine fuel with good specific thrust and storage performance, and is widely used in military and aerospace fields. However, it is toxic, corrosive, irritating, volatile, hygroscopic and adsorbable, and has both long-term and short-term adverse effects on the human body. The scrapped unsymmetrical dimethylhydrazine or its sewage must be treated. [0003] The process of synthesizing unsymmetrical dimethylhydrazine is relatively simple, the product has high purity and good effect, and the synthesis and application of this product have great development prospects at home and abroad. In addition to being used as a high-efficiency plant regulator, in recent years, Bijiu has been u...
Claims
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IPC IPC(8): C07C243/28C07C241/04
Inventor 闫小宁白海龙李军平姚忠东吉卉许东兴苏雪春王卫国陈帅郭友杨玲闫昳姝韦雄雄
Owner XIAN HANGJIE CHEM TECH