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A kind of preparation method of azelanitrile

A technology of azelanitrile and glutaraldehyde, which is applied in the field of preparing azelanitrile by one-pot method, can solve the problems of difficult treatment of three wastes, high cost of raw materials, corrosion, etc., achieve low cost, reduce production cost, and good yield Effect

Active Publication Date: 2022-04-19
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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  • A kind of preparation method of azelanitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Using Methanol as Solvent to Prepare Azelanitrile

[0046] The reaction formula is as follows:

[0047]

[0048] (1) Condensation, decarboxylation and hydrogenation reactions: In the 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 was stirred for 60 min, and then 85 g (1 mol) of cyanoacetic acid was added in batches. During the addition, the temperature of the system was kept not exceeding 40°C. After the addition was complete, the stirring was continued at room temperature for 2-3 hrs. Subsequently, in the autoclave, continue to add 5g of palladium-carbon catalyst (5% containing water), close the reactor, evacuate, use nitrogen replacement, then feed hydrogen, the pressure is maintained at 4.0MPa, the reaction temperature is maintained at 45 ° C, and the reaction continues During 12hrs, every 2hrs, use the release valve to release the carbo...

Embodiment 2

[0051] Using ethanol as solvent to prepare azelanitrile

[0052] Azelanitrile 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 yield of the obtained azelanitrile was 70.1%, and the purity was 98.1%.

Embodiment 3

[0054] Preparation of Azelanitrile Using 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 carried out in the same manner as in step (1) of Example 1.

[0056] Then, the obtained reaction liquid is subjected to vacuum distillation, and the solvent N,N-dimethylformamide is distilled out by controlling the temperature not to be higher than 100° C., and then the temperature is raised for vacuum distillation, and azelanitrile product is collected.

[0057] The yield of the obtained azelanitrile was 77.8%, and the purity was 98.9%.

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Abstract

The present invention relates to a kind of preparation method of azelanitrile, this method comprises the following steps: (1) dissolving glutaraldehyde in solvent, adding condensation catalyst, optional co-catalyst, then adding cyanoacetic acid in batches to keep reaction solution The temperature is not more than 40 DEG C, carry out condensation reaction, wherein, the mol ratio of described glutaraldehyde and cyanoacetic acid is 1:2; (2) in the condensation reaction liquid that step (1) obtains, further add palladium carbon catalyst (Pd / C), feeding hydrogen, keeping the pressure, heating, performing decarboxylation and hydrogenation reactions to obtain azelanitrile, wherein the hydrogen pressure is 3.0-4.0 MPa. The method for preparing azelanitrile of the present invention can be reacted in one step, omitting the separation and purification process of intermediate products, so the reaction process is simple and the cost is low.

Description

technical field [0001] The invention relates to a method for preparing azelanitrile. Specifically, the invention relates to a method for preparing azelanitrile by using a one-pot method. The method can realize condensation, decarboxylation and hydrogenation reactions in one step. Background technique [0002] Azelanitrile is an important chemical raw material, which can be used to produce high-temperature nylon P9AT, and can also be used in pharmaceutical and other industries. [0003] In the prior art, the production of azelaic acid mainly contains three methods: 1, take azelaic acid (azelaic acid) as raw material, after ammoniation obtains azelaic acid amide, dehydration prepares azelaic acid again; 2, use 1,9 -Dihalogenated nonane is used as raw material, which is obtained by substitution reaction with inorganic cyanide; 3. Azelanitrile is prepared by ammonolysis and dehydration of nonanediol. For example, U.S. Patent US4139547, Chinese Patent CN102701991, etc. adopt the...

Claims

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Application Information

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Patent Type & Authority Patents(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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