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Two-step preparation method of 6-aminocapronitrile

A technology of aminocapronitrile and aminocapronamide is applied in the field of preparing hexamethylenediamine key intermediate 6-aminocapronitrile by two-step method, and can solve the problems of affecting the operation stability of the device, increasing the polymer, and coking of the catalyst.

Active Publication Date: 2021-08-27
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The main purpose of the present invention is to provide a kind of method that two-step method prepares 6-aminocapronitrile, to solve the problem in the prior art that one-step method prepares 6-aminocapronitrile catalyst easy coking deactivation influences the running stability of device, also solves In the original two-step patent application, first hydrolysis and then ammoniation, resulting in increased energy consumption, increased polymers, and the problem of catalyst coking in catalytic ammoniation dehydration

Method used

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  • Two-step preparation method of 6-aminocapronitrile
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  • Two-step preparation method of 6-aminocapronitrile

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Weigh 22.63g (0.2mol) of caprolactam into a 500ml autoclave, then add 34g of toluene, start stirring and heat up to 60±2°C to dissolve. After the ammonia gas passes through the preheater, the temperature reaches 150°C, and it is passed into the pressure kettle. The temperature of the material in the reactor continues to rise to 200-250°C, and the hot ammonia gas is continuously fed in, with a back pressure of 2.5MPa. After stirring for about 20 hours, the temperature is reduced and the pressure is released. Obtain 59g of toluene solution of the crude product of 6-aminocaproamide, and the reaction process consumes 20g of ammonia gas in total. After testing, the mass percentage of 6-aminocaproamide is 72.18%, the conversion rate of caprolactam is 73.1%, and the selectivity of 6-aminocaproamide is 95.3%. The detection results of the polymerization by-products are shown in Table 1 below.

[0060] Transfer the toluene solution of the crude 6-aminocaproamide to a pressure-re...

Embodiment 2

[0062] Weigh 22.63g (0.2mol) of caprolactam into a 500ml autoclave, then add 68g of acetonitrile, start stirring and heat up to 30±2°C to dissolve. After the ammonia gas passes through the preheater, the temperature reaches 250°C, and it is passed into the pressure kettle. The temperature of the material in the reactor continues to rise to 300-350°C, and the hot ammonia gas is continuously fed in, with a back pressure of 3.0MPa. After stirring for about 20 hours, the temperature is released and the pressure is released. Obtain 89g of acetonitrile solution of the crude product of 6-aminocaproamide, and consume 31g of ammonia gas in the reaction process. After testing, the mass percentage of 6-aminocaproamide is 83.94%, the conversion rate of caprolactam is 82.7%, and the selectivity of 6-aminocaproamide is 97.1%. The detection results of the polymerization by-products are shown in Table 1 below.

[0063] Transfer the acetonitrile solution of crude 6-aminocaproamide to a pressu...

Embodiment 3

[0065] Weigh 22.63g (0.2mol) of caprolactam into a 500ml autoclave, then add 25g of chlorobenzene, start stirring and heat up to 70±2°C to dissolve. After the ammonia gas passes through the preheater, the temperature reaches 200°C, and it is passed into the pressure vessel. The temperature of the material in the reaction vessel continues to rise to 300-350°C, and the hot ammonia gas is continuously introduced, with a back pressure of 3.0MPa. After stirring for about 13 hours, the temperature is reduced and the pressure is released. Obtain 46g of crude chlorobenzene solution of 6-aminocaproamide, and consume 23g of ammonia gas in the reaction process. After testing, the mass percentage of 6-aminocaproamide is 75.51%, the conversion rate of caprolactam is 76.5%, and the selectivity of 6-aminocaproamide is 95.7%. The detection results of the polymerization by-products are shown in Table 1 below.

[0066] Transfer the acetonitrile solution of the crude product of 6-aminocaproamid...

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Abstract

The invention relates to a two-step preparation method of 6-aminocapronitrile. The two-step preparation method comprises the following steps: carrying out ammonolysis reaction on caprolactam in an inert solvent or in a molten state and hot ammonia gas to obtain 6-aminohexanamide, and dehydrating the 6-aminohexanamide in the presence of a dehydrating agent to obtain 6-aminocapronitrile. According to the invention, ring-opening ammonolysis is carried out under an anhydrous condition, so that polymerization of ammonolysis products is effectively controlled, and generation of by-products is reduced; and under the condition of no catalyst, the dehydrating agent is directly used for dehydration reaction, so that the problems of catalyst coking, short catalyst service life and the like in a catalytic dehydration process are effectively avoided.

Description

technical field [0001] The invention relates to the technical field of synthesis of hexamethylenediamine, in particular to a two-step method for preparing the key intermediate of hexamethylenediamine, 6-aminocapronitrile. Background technique [0002] 1,6-hexamethylenediamine is an intermediate of important high-performance materials such as nylon 66, nylon 610, etc. It is also used in the production of polyurethane, such as 1,6-hexamethylene diisocyanate (HDI), and can also be used as urea-formaldehyde resin, ring Curing agent for epoxy resin. [0003] According to different raw materials, there are four main production methods of hexamethylenediamine, which are butadiene method, acrylonitrile method, adipic acid method and caprolactam method. [0004] The butadiene method usually uses transition metal complexes such as Rh, Ni, and Ru as catalysts, and introduces two molecules of hydrocyanic acid into butadiene, and the addition reaction produces adiponitrile, which is the...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C255/24C07C231/08C07C237/06
CPCC07C253/20C07C231/08C07C237/06C07C255/24Y02P20/52
Inventor 谢增勇杨学林王耀红王树平刘东磊陈西波党伟荣
Owner BEIJING RISUN TECH CO LTD
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