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Azelanitrile preparation method

A technology for azelaic nitrile and glutaraldehyde, which is applied in the field of preparing azelaic nitrile by one-pot method, can solve the problems of intractable treatment of three wastes, high cost of raw materials, corrosiveness, etc., and achieves low cost, reduced production cost and good yield Effect

Active Publication Date: 2019-08-06
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a kind of preparation method of azelanitrile, in order to solve the problem in the prior art that raw material cost is high, corrosivity, toxicity are big, and three wastes are difficult to handle

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0045] Using methanol as solvent to prepare azelaonitrile

[0046] The reaction formula is as follows:

[0047]

[0048] (1) Condensation, decarboxylation and hydrogenation reactions: In an autoclave, add 50g (0.5mol) glutaraldehyde, 250g methanol, stir to dissolve, at room temperature, add 2.5g (29.4mmol) piperidine, 1.77g (29.5mmol) ) Acetic acid, the mixture is stirred for 60 minutes, and then 85 g (1 mol) of cyanoacetic acid is added in batches. During the addition, the temperature of the system is maintained not to exceed 40°C. After the addition is complete, continue to stir at room temperature for 2 to 3 hrs. Subsequently, in the autoclave, continue to add 5g palladium-carbon catalyst (5% water), seal the reactor, evacuate, replace with nitrogen, and then pass in hydrogen, the pressure is maintained at 4.0MPa, the reaction temperature is maintained at 45°C, the reaction continues During 12hrs, every 2hrs, use the purge valve to release the carbon dioxide generated by the r...

Embodiment 2

[0051] Using ethanol as solvent to prepare azelaonitrile

[0052] Azelaonitrile was prepared in the same manner as in Example 1, except that 250 g of ethanol was used instead of 250 g of methanol in step (1). The resulting azelaonitrile yield was 70.1% and purity was 98.1%.

Embodiment 3

[0054] Preparation of Azela Nitrile with N,N-Dimethylformamide as Solvent

[0055] Except that 250 g of N,N-dimethylformamide was used instead of 250 g of methanol in step (1), the reaction was performed in the same manner as in step (1) of Example 1.

[0056] Then the obtained reaction liquid is subjected to vacuum distillation, the temperature is controlled not to be higher than 100° C. The solvent N,N-dimethylformamide is distilled out, and then the temperature is raised for vacuum distillation to collect azelaonitrile products.

[0057] The obtained azela nitrile yield was 77.8%, and the purity was 98.9%.

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Abstract

The invention relates to an azelanitrile preparation method, which comprises: (1) dissolving glutaraldehyde in a solvent, adding a condensation catalyst and an optional cocatalyst, adding cyanoaceticacid in batches to maintain the temperature of the reaction solution of not more than 40 DEG C, and carrying out a condensation reaction, wherein a molar ratio of the glutaraldehyde to the cyanoaceticacid is 1:2; and (2) further adding a palladium carbon catalyst (Pd / C) to the condensation reaction liquid obtained in the step (1), introducing hydrogen gas, maintaining the pressure, heating, and carrying out a decarboxylation and hydrogenation reaction to obtain azelanitrile, wherein the hydrogen pressure is 3.0-4.0 MPa. According to the present invention, the method can perform the reaction by using the one-step method so as to eliminate the separation and purification process of the intermediate product, such that the reaction process is simple, and the cost is low.

Description

Technical field [0001] The present invention relates to a method for preparing azela nitrile. Specifically, the present invention relates to a method for preparing azela nitrile by a one-pot method, which can realize condensation, decarboxylation and hydrogenation reactions in one step. Background technique [0002] Azelalonitrile is an important chemical raw material that can be used to produce high-temperature nylon P9AT, and can also be used in industries such as pharmaceuticals. [0003] In the prior art, there are three main methods for the production of azelaonitrile: 1. Using azelaic acid (azaleic acid) as a raw material, ammoniated to obtain azelaamide, and then dehydrating to prepare azelaonitrile; 2. Using 1,9 -Dihalogenated nonane as raw material, obtained by substitution reaction with inorganic cyanide; 3. Nonanediol ammonolysis dehydration to prepare azelaonitrile. For example, US patent US4139547, Chinese patent CN102701991, etc. adopt a method of preparing azelayl c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/04
CPCC07C253/30C07C255/04C07C255/23C07C255/09
Inventor 张捷赵会娟潘小君王耀红张敏生
Owner BEIJING RISUN TECH CO LTD
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