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Method for synthesizing bis-isobutyronitrile hydrazine

A technology of diisobutyronitrile and synthesis method, which is applied in chemical instruments and methods, preparation of carboxylic acid nitrile, preparation of organic compounds, etc. Quality and other problems, to achieve the effect of improving the reaction yield, reducing the amount of addition, and expanding the production capacity

Active Publication Date: 2009-06-03
SHANGHAI NO 4 REAGENT & H V CHEM
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  • Abstract
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Problems solved by technology

But, the method of applying mechanically mother liquor water has brought problems to production, one, after applying mechanically mother liquor water for many times, due to the increase of impurity content, the intermediate product diisobutyronitrile product color of generation can turn yellow sometimes, cannot guarantee The quality of final product azobisisobutyronitrile; Two, the intermediate product diisobutyronitrile preparation method described in CN1785963 is similar to the classic diisobutyronitrile preparation method, all needs to add a large amount of water as diluent. Dispersion, the amount of water added is 7 to 10 times (molar ratio) of the amount of acetone cyanohydrin. Due to the addition of a large amount of water, the volume of the reaction device will inevitably expand

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  • Method for synthesizing bis-isobutyronitrile hydrazine

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Embodiment 1

[0012] The preparation of embodiment 1 diisobutyronitrile hydrazine

[0013] In a 500ml flask, add 129 grams (1.50 moles) of 98.9% acetone cyanohydrin, 0.2 grams (0.00061 moles) of 98% tetrabutylammonium bromide and 50 grams (2.78 moles) of water. Concentration is 47.5 grams (0.76 mol) of industrial hydrazine hydrate of 80%. After the dropwise addition was completed, the temperature was raised to 60° C. and kept for 3 hours. Then the reactant was cooled to 5° C. to precipitate a solid, which was filtered and dried under reduced pressure (vacuum degree: 0.098 MPa) at room temperature for 8 hours to obtain 124.0 g of white crystalline diisobutyronitrile product. According to gas chromatography analysis, the purity of diisobutyronitrile hydrazine is 98.7%, and the reaction yield is 98.23% (calculated in acetone cyanohydrin).

[0014] The spectral analysis of product diisobutyronitrile hydrazine is as follows:

[0015] Infrared absorption spectrum characteristic frequency (cm ...

Embodiment 2

[0017] The preparation of embodiment 2 diisobutyronitrile hydrazine

[0018] In a 500ml flask, add 129 grams (1.50 moles) of 98.9% acetone cyanohydrin, 1 gram (0.00894 moles) of 98% tetramethylammonium chloride and 45 grams (2.5 moles) of water. Concentration is 48 grams (0.767 mol) of industrial hydrazine hydrate of 80%. After the dropwise addition was completed, the temperature was raised to 70° C. and kept for 4 hours. Then the reactant was cooled to 5° C. to precipitate a solid, filtered, and dried under reduced pressure (0.098 MPa) at room temperature for 10 hours to obtain 124.5 grams of a white crystalline diisobutyronitrile product, which was analyzed by gas chromatography. The purity of nitrile hydrazine is 98.5%, and the reaction yield is 98.42% (calculated in acetone cyanohydrin).

Embodiment 3

[0019] The preparation of embodiment 3 diisobutyronitrile hydrazine

[0020] In a 500ml flask, add 129 grams (1.50 moles) of 98.9% acetone cyanohydrin, 0.5 grams (0.00296 moles) of 98% tetraethylammonium chloride and 70 grams (3.89 moles) of water. 99 grams (0.791 moles) of industrial hydrazine hydrate with a concentration of 40%. After the dropwise addition was completed, the temperature was raised to 65° C. and kept for 5 hours. Then the reactant was cooled to 5° C., a solid was precipitated, filtered, and dried under reduced pressure (0.098 MPa) at room temperature for 9 hours to obtain 123.8 grams of a white crystalline diisobutyronitrile product, which was analyzed by gas chromatography. The purity of nitrile hydrazine is 99.1%, and the reaction yield is 98.47% (calculated in acetone cyanohydrin).

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Abstract

The invention relates to a method for synthesizing bis-isobutyronitrile hydrazine. Acetone cyanohydrins and hydrazine hydrate are used as raw materials to carry out condensation reaction by the action of phase transfer catalyst quaternary ammonium compound. The phase transfer catalyst not only promotes the reaction speed and enhances the synthesis yield to 98.23 percent to 98.60 percent, but also reduces the addition of water in the reaction, thus improving the productivity greatly and reducing the production cost as the phase transfer catalyst also takes effects of dispersing. A product has stable quality, and the purity of the product is more than 98 percent. Therefore, the method for synthesizing the bis-isobutyronitrile hydrazine is a method fit for industrialized production.

Description

technical field [0001] The present invention relates to the synthetic method of organic compound diisobutyronitrile hydrazine. Background technique [0002] Diisobutyronitrile hydrazine belongs to an organic chemical product, mainly used in the production of initiator azobisisobutyronitrile. [0003] About the synthetic method of diisobutyronitrile hydrazine, it is mainly discussed in the preparation technology of azobisisobutyronitrile. In the Chinese patent CN1785963 "Preparation method of azobisisobutyronitrile" published in June 2006, it involves the synthesis of diisobutyronitrile hydrazine as an intermediate product. The method is to add diisobutyronitrile mother liquid water (need to adjust the pH value to 4-5) produced in the previous reaction to acetone cyanohydrin, replace the clear water that should be added during the reaction, and then carry out condensation reaction with hydrazine hydrate. The purpose is to use saturated diisobutyronitrile hydrazine in the mo...

Claims

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Application Information

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IPC IPC(8): C07C255/66C07C253/30
Inventor 陆稼麟杜骏周琴
Owner SHANGHAI NO 4 REAGENT & H V CHEM
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