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Method for preparing 1,4-diaminocyclohexane

A technology of cyclohexanediamine and cyclohexanediol, which is applied in the field of preparation of cyclohexanediamine, can solve the problems of expensive metal catalysts and potential safety hazards in production, and achieve the effects of improving safety and reducing costs

Inactive Publication Date: 2015-10-28
陈爱华
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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-diaminocyclohexane
  • Method for preparing 1,4-diaminocyclohexane
  • Method for preparing 1,4-diaminocyclohexane

Examples

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 Amine 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 at a temperature of 220°C-250°C for 12-14h, and sample and analyze GC, 1,4-cyclohexanediol Amine 95.7%, 1,4-cyclohexanediol 0.15%, polymer 3.54%;

[0022] The sample was taken out, and after water was distilled off, 106.3 g of white solid 1,4-cyclohexanediamine was obtained by rectification under reduced pressure, 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 for analysis by 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-diaminocyclohexane. The method comprises the following steps that 1,4-cyclohexanediol and liquid ammonia or 25% ammonium water are added into a high-pressure reactor to be reacted for 12 h at 10-15 MPa, the reaction temperature is 220 DEG C-250 DEG C, and the target product 1,4-diaminocyclohexane is obtained. The preparation method is short in technology process, low in production cost and high in production security, the product conversion rate is above 95 percent, and the finished product yield is about 93 percent.

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 陈爱华
Owner 陈爱华
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