Method for preparing 1,4-cyclohexanediamine at high pressure

A technology of cyclohexanediamine and cyclohexanediol, applied in the field of preparation of cyclohexanediamine, can solve the problems of hidden dangers in production safety, expensive metal catalysts and the like, and achieve the effects of improving safety and reducing costs

Inactive Publication Date: 2014-07-02
江苏恒祥化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] This route is currently a relatively mature route for industrialization, but the use of hydrogen in the production process of this route has potential safety hazards in production, and the metal catalysts used are expensive, so it is necessary to develop a low-cost, high-safety process route

Method used

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  • Method for preparing 1,4-cyclohexanediamine at high pressure

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Experimental program
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Effect test

Embodiment 1

[0019] Add 53g of 1,4-cyclohexanediol and 30g of liquid ammonia into a 1L autoclave, control the temperature of 10-15MPa, and react at a temperature of 220°C-250°C for 12-14h, and take samples for analysis by GC. 1,4-cyclohexanediol Amines 95.1%, 1,4-cyclohexanediol 0.2%, polymer 3.8%.

Embodiment 2

[0021] Put 116g of 1,4-cyclohexanediol and 60g of liquid ammonia into a 1L autoclave, control the temperature of 10-15MPa, and react for 12-14h at a temperature of 220°C-250°C, and take samples for analysis by GC. 1,4-cyclohexanediol Amine 95.7%, 1,4-cyclohexanediol 0.15%, polymer 3.54%;

[0022] The sample was taken out, the water was distilled off, and rectified under reduced pressure to obtain 106.3 g of white solid 1,4-cyclohexanediamine, with a yield of 93.1% and a GC purity of 99.84%.

Embodiment 3

[0024] Add 232g of 1,4-cyclohexanediol and 120g of liquid ammonia into a 1L autoclave, control the reaction pressure at 10-15MPa, and the temperature at 220°C-250°C, react for 12-14h, take samples and analyze GC, 1,4 - Cyclohexanediamine 96.1%, 1,4-cyclohexanediol 0.13%, polymer 3.04%;

[0025] The sample was taken out, the water was distilled off, and rectified under reduced pressure to obtain 213.4 g of white solid 1,4-cyclohexanediamine, with a yield of 93.5% and a GC purity of 99.88%.

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Abstract

The invention discloses a method for preparing 1,4-cyclohexanediamine at high pressure. The method comprises the following steps: adding 1,4-cyclohexanediol and liquid ammonia or 25% ammonium hydroxide to a high-pressure reaction kettle; and reacting at 10-15MPa for 12 hours, wherein the reaction temperature is 220-250 DEG C, so as to obtain a target product 1,4-cyclohexanediamine. The preparation method disclosed by the invention is short in technological process, low in production cost, and high in production security, the product conversion rate is more than 95%, and the product yield is about 93%.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanediamine, in particular to a method for preparing 1,4-cyclohexanediamine under high pressure. Background technique [0002] 1,4-cyclohexanediamine, as an organic amine with symmetrical structure and no aromatic ring, is widely used in textiles, papermaking, artificial leather, plastic processing, and liquid crystal material production, and can also be used as raw materials for dyes and pharmaceutical intermediates, especially It is a new raw material for the manufacture of urethane, polyamide resin, etc. Due to the superiority of its structure, it will definitely replace 1,4-butanediamine and p-phenylenediamine in many applications in the future. [0003] At present, the catalytic hydrogenation of p-phenylenediamine is widely used to prepare 1,4-cyclohexanediamine, and its production process route is as follows: [0004] [0005] This route is currently a relatively mature route for industr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/16C07C211/36
Inventor 邱志刚雍成松
Owner 江苏恒祥化学股份有限公司
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