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Method for preparing 6-aminocapronitrile by gas phase method

A technology of aminocapronitrile and gas phase method, applied in the field of preparing 6-aminocapronitrile by gas phase method, can solve the problems of unsatisfactory reaction effect, low reaction conversion rate and the like, and is suitable for large-scale popularization and application and has high reaction conversion rate. , the effect of simple preparation process

Inactive Publication Date: 2018-01-19
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are fewer patents on the preparation of 6-aminocapronitrile by caprolactam as raw material. Although patents such as US2234566 and FR1573490 have mentioned the technology of using caprolactam to prepare 6-aminocapronitrile, the reaction effect is not ideal; some documents refer to the use of calcium phosphate , Magnesium phosphate and other phosphates, but the reaction conversion rate is low, generally less than 50%

Method used

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  • Method for preparing 6-aminocapronitrile by gas phase method
  • Method for preparing 6-aminocapronitrile by gas phase method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Fully mix 6 g / h of caprolactam vapor with 18 L / h of hot ammonia gas (the mass ratio of ammonia gas to CPL is 2.3), and the temperature of ammonia gas is 270°C. The mixed steam of caprolactam and ammonia is contacted with 1g catalyst, the contact time is 0.1s, the reaction temperature is 300°C, the reaction pressure is 0.1mpa, and the catalyst is silicon dioxide. The reaction conversion rate is 57.3%, and the selectivity is 97.8%. The effluent of the ammoniation reaction is deaminated, dehydrated, and 99.6% of 6-aminocapronitrile can be obtained after rectification under reduced pressure.

[0030] In this embodiment, the bottom temperature of the vacuum distillation tower is 150° C., and the vacuum degree is 2 torr. When the tower top temperature is 20° C., ammonia and water are evaporated; when the tower top temperature is 130° C., 6-aminocapronitrile is evaporated.

Embodiment 2

[0032] Fully mix 6 g / h of caprolactam vapor with 48 L / h of hot ammonia gas (the mass ratio of ammonia gas to CPL is 6), and the temperature of ammonia gas is 320°C. The mixed steam of caprolactam and ammonia is contacted with 5g catalyst, the contact time is 0.5s, the reaction temperature is 340°C, the reaction pressure is 0.5mpa, and the catalyst is activated alumina. The reaction conversion rate is 78%, and the selectivity is 98.3%. The effluent of the ammoniation reaction is deaminated and dehydrated, and 99.8% of 6-aminocapronitrile can be obtained after rectification under reduced pressure.

[0033] In this embodiment, the temperature at the bottom of the vacuum distillation tower is 152°C, and the vacuum degree is 2.4torr. When the temperature at the top of the tower is 25°C, ammonia and water are evaporated; when the temperature at the top of the tower is 131°C, 6-aminocapronitrile is evaporated. .

Embodiment 3

[0035] Fully mix 6 g / h of caprolactam vapor with 90 L / h of hot ammonia gas (the mass ratio of ammonia gas to CPL is 11.4), and the temperature of ammonia gas is 350°C. The mixed steam of caprolactam and ammonia is contacted with 10g of catalyst, the contact time is 1s, the reaction temperature is 350°C, the reaction pressure is 0.3mpa, and the catalyst is cerium oxide. The conversion rate of the reaction is 85%, and the selectivity is 98.5%. The effluent of the ammoniation reaction is deaminated and dehydrated, and 99.8% of 6-aminocapronitrile can be obtained after rectification under reduced pressure.

[0036] In this embodiment, the temperature at the bottom of the vacuum distillation tower is 155°C, and the vacuum degree is 2.8 torr. When the temperature at the top of the tower is 28°C, ammonia and water are evaporated; when the temperature at the top of the tower is 135°C, 6-aminocapronitrile is evaporated. .

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Abstract

The invention provides a method for preparing 6-aminocapronitrile by a gas phase method. The method uses caprolactam as a raw material, and comprises the following steps of S1, mixing caprolactam vapor with an hot ammonia gas according to a certain mass ratio; S2, subjecting a mixture of the caprolactam vapor and the hot ammonia gas, which is obtained in the step S1, to ammoniation and dehydrationreaction in a condition that a catalyst exists, so as to obtain ammoniated efflux; S3, separating and purifying the ammoniated efflux obtained in the step S2, so as to obtain the pure 6-aminocapronitrile. The method for preparing the 6-aminocapronitrile by the gas phase method, which is provided by the invention, is relatively high in reaction conversion ratio which can be up to 96 percent or above, and is simple in preparation process.

Description

technical field [0001] The invention belongs to the technical field of preparation of aminonitrile, and in particular relates to a method for preparing 6-aminocapronitrile by a gas phase method. Background technique [0002] 6-Aminocapronitrile is an important chemical intermediate that can be used to produce 1,6-hexamethylenediamine by complete hydrogenation, which can be used to produce the polymer nylon 66. At present, the preparation of 6-aminocapronitrile is mainly obtained by partial hydrogenation of 1,6 adiponitrile, such as patents CN1238334C and CN101309897B, or by hydroformylation of pentenenitrile, such as patent CN1100752C. There are fewer patents on the preparation of 6-aminocapronitrile by caprolactam as raw material. Although patents such as US2234566 and FR1573490 have mentioned the technology of using caprolactam to prepare 6-aminocapronitrile, the reaction effect is not ideal; some documents refer to the use of calcium phosphate , Magnesium phosphate and o...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C255/24
Inventor 史文涛杨克俭王聪武金丹杨琦武孙承宇崔艳杰
Owner CHINA TIANCHEN ENG
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