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Preparation method for high-purity dicyclohexyl amine

A dicyclohexylamine, high-purity technology, applied in the field of resource utilization and preparation of high-purity dicyclohexylamine, can solve problems such as harsh operating conditions, high-pressure equipment, and environmental pollution, and achieve high catalyst activity and long service life , The effect of simple process

Active Publication Date: 2013-10-30
JIANGSU NUOMENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The common disadvantage of the catalytic systems in the above documents is that the operating conditions are too harsh and require high pressure equipment
In addition, some catalysts contain chromium, which will cause environmental pollution and endanger human health, which is not in line with the development direction of green chemical industry. Some catalysts require expensive metals
The above shortcomings make these processes difficult to apply and promote in industry, and it is necessary to develop a new preparation method and process to solve the above-mentioned problems and deficiencies

Method used

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  • Preparation method for high-purity dicyclohexyl amine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The hydrofining reactor is a tubular fixed-bed reactor with an inner diameter of 20mm. The catalyst is a nickel-based high-activity catalyst with a fixed volume of 15 mL. The catalyst is installed in the isothermal zone of the reactor, and the particle size is 20 mesh to 40 mesh. The mass ratio of each metal element of the catalyst is: Ni:Al:Mo=85:5: 5. The crude dicyclohexylamine and hydrogen are fed from the upper part of the reactor to carry out the hydrofining reaction, the products are collected and analyzed continuously from the lower end of the reactor, and the hydrogen after gas-liquid separation is recovered and reused.

[0019] The crude dicyclohexylamine injection composition (percentage by weight) is 10.15% of cyclohexylamine, 5.11% of aniline, 79.91% of dicyclohexylamine, 0.31% of dicyclohexylimine, 0.1% of cyclohexylaniline, and 1.88% of cyclohexylaniline .

[0020] Reaction conditions: 180°C, 3.5MPa, liquid volume space velocity 0.2h -1 , Hydrogen oil ...

Embodiment 2

[0024] Reaction raw materials, operation method, catalyst and consumption are as embodiment 1

[0025] Reaction conditions: 150°C, 3.5MPa, liquid volume space velocity 0.5h -1 , Hydrogen oil ratio 400.

[0026] Product distribution after hydrofining: 5.82% cyclohexylamine, 0.02% aniline, 92.61% dicyclohexylamine, 0% dicyclohexyl imine, 0.01% cyclohexylaniline, 0.02% cyclohexene aniline.

Embodiment 3

[0028] Reaction raw materials, operation method, catalyst and consumption are as embodiment 1

[0029] Reaction conditions: 140°C, 1.0MPa, liquid volume space velocity 0.4h -1 , Hydrogen oil ratio 500.

[0030] Product distribution after hydrofining: 5.93%, aniline 0.02%, dicyclohexylamine 92.4%, dicyclohexylimide 0%, cyclohexylaniline 0.01%, cyclohexene aniline 0.04%.

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Abstract

The invention discloses a resource utilization preparation method for high-purity dicyclohexyl amine. The method has the characteristics of low temperature, low pressure, large variable scale of raw material component content and long service life of a catalyst, and can be widely applied and popularized in industrial production. The preparation method for high-purity dicyclohexyl amine disclosed by the invention comprises the following steps of: preparing crude dicyclohexyl amine by performing catalytic hydrogenation on aniline with the conventional method; and refining the crude dicyclohexyl amine into high-purity dicyclohexyl amine, wherein a method for refining the crude dicyclohexyl amine into high-purity dicyclohexyl amine comprises the following steps of: introducing crude dicyclohexyl amine and hydrogen into a fixed bed tubular reactor in the presence of a granular nickel-based high-activity catalyst under the condition that the reaction pressure is 0.1-3 MPa, the reaction temperature is 140-210 DEG C, the liquid air speed is 0.2-2.5 h<-1>, and the hydrogen-oil volume ratio is 100-1,000.

Description

technical field [0001] The invention relates to a recycling method, in particular to a resource utilization preparation method of high-purity dicyclohexylamine. Background technique [0002] Dicyclohexylamine is mainly used in synthetic rubber accelerators, metal corrosion inhibitors, surfactants, oilfield chemicals, pharmaceuticals and pesticides. With the advancement of science and technology, its new applications are constantly being developed, and most of the fine chemicals synthesized from it are promising new products. In the process of preparing cyclohexylamine and by-product dicyclohexylamine by catalytic hydrogenation of aniline, the production ratio of dicyclohexylamine is doubled by adjusting the reaction conditions, but no matter how the reaction conditions are adjusted, the obtained crude dicyclohexylamine Hexylamine will still contain unreacted aniline, cyclohexylamine, dicyclohexylamine, cyclohexylaniline, cyclohexene aniline. Their presence not only affects...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/35C07C209/84C07C209/72C07C209/70B01J23/883B01J35/02B01J35/00
Inventor 梅华於德伟
Owner JIANGSU NUOMENG CHEM
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