Preparation method of hydrogenation catalyst and method for synthesizing DMAPA (dimethyl amionopropylamine) by applying catalyst

A technology of hydrogenation catalyst and auxiliary agent, applied in the preparation of organic compounds, metal/metal oxide/metal hydroxide catalyst, preparation of amino compounds, etc., can solve the problems of wasting raw materials, increasing production and operation costs, and reducing The effect of output, saving cost of raw material consumption, and reducing consumption

Inactive Publication Date: 2015-04-08
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the defects that a large amount of heavy slag produced by DMAPA synthesis units in the prior art needs to be processed every year, which not only wastes raw materials, but also increases production and operation costs, and provides a method for preparing a hydrogenation catalyst and using the catalyst to synthesize DMAPA The method for the preparation method of the hydrogenation catalyst of the present invention is simple, can be directly prepared in existing equipment, is convenient to large-scale industrial preparation, and the hydrogenation catalyst of preparation can effectively improve propionitrile in the method for synthesizing DMAPA The selectivity of preparing DMAPA reduces the consumption of synthetic raw materials, especially acrylonitrile, and also greatly reduces the content of secondary amines in the product, avoiding excessive heavy residue in the product, and reducing the investment and production and operation costs of the DMAPA synthesis unit

Method used

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  • Preparation method of hydrogenation catalyst and method for synthesizing DMAPA (dimethyl amionopropylamine) by applying catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In parts by mass, weigh the following raw materials, Ni: 50 parts; Al: 46 parts; Co: 1.5 parts; La: 0.2 parts; Cr: 1.0 parts; Fe: 0.8 parts; The raw materials are uniformly mixed and melted at a temperature of 3000°C, cooled under the protection of nitrogen to form a solid alloy, and then crushed and sieved to obtain alloy powder with 80-150 mesh particles; in 30% sodium hydroxide solution Activate to remove most of the Al in the alloy powder, and then wash with deionized water until the pH value is 9-10, and the obtained product is a hydrogenation catalyst.

[0032] Add acrylonitrile to the synthesis kettle, and add dimethylamine dropwise to the synthesis kettle under the conditions of stirring at 50°C and circulating cooling water, wherein the molar ratio of acrylonitrile to the dimethylamine added dropwise is 1 : 1, a small amount of dimethylamine is removed through vacuum distillation to obtain N,N-dimethylpropionitrile;

[0033] Take 1000 g of N,N-dimethylpropioni...

Embodiment 2

[0035] In parts by mass, weigh the following raw materials, Ni: 48 parts; Al: 48 parts; Co: 1.5 parts; La: 0.2 parts; Cr: 1.0 parts; Fe: 0.8 parts; The raw materials are uniformly mixed and melted at a temperature of 2500°C, cooled under the protection of nitrogen to form a solid alloy, and then crushed and sieved to obtain alloy powder with 120-250 mesh particles; in 30% sodium hydroxide solution Activate to remove most of the Al in the alloy powder, and then wash with deionized water until the pH value is 9-10, and the obtained product is a hydrogenation catalyst.

[0036] Add acrylonitrile to the synthesis kettle, and add dimethylamine dropwise to the synthesis kettle under the conditions of stirring at 50°C and circulating cooling water, wherein the molar ratio of acrylonitrile to the dimethylamine added dropwise is 1 : 1, a small amount of dimethylamine is removed through vacuum distillation to obtain N,N-dimethylpropionitrile;

[0037] Take 500 g of prepared N,N-dimethy...

Embodiment 3

[0039] In parts by mass, weigh the following raw materials, Ni: 49 parts; Al: 45 parts; Co: 2 parts; La: 0.5 parts; Cr: 1.5 parts; Fe: 1 part; The raw materials are uniformly mixed and melted at a temperature of 2800°C, cooled under the protection of nitrogen to form a solid alloy, and then crushed and sieved to obtain alloy powder with 120-250 mesh particles; in 30% sodium hydroxide solution Activate to remove most of the Al in the alloy powder, and then wash with deionized water until the pH value is 9-10, and the obtained product is a hydrogenation catalyst.

[0040] Add acrylonitrile to the synthesis kettle, and add dimethylamine dropwise to the synthesis kettle under the conditions of stirring at 50°C and circulating cooling water, wherein the molar ratio of acrylonitrile to the dimethylamine added dropwise is 1 : 1, a small amount of dimethylamine is removed through vacuum distillation to obtain N,N-dimethylpropionitrile;

[0041] Take 1000 g of N,N-dimethylpropionitril...

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Abstract

The invention discloses a preparation method of a hydrogenation catalyst and a method for synthesizing DMAPA (dimethyl amionopropylamine) by applying the catalyst, wherein the hydrogenation catalyst is prepared by taking Ni, Al and auxiliaries as raw materials; the method for synthesizing DMAPA by applying the catalyst comprises the following steps: a, adding acrylonitrile into a synthetic kettle to react with dimethylamine to prepare N,N-dimethyl propionitrile; and b, adding N,N-dimethyl propionitrile into a high-pressure kettle, adding the hydrogenation catalyst and liquid ammonia, raising the temperature to 100-150 DEG C, introducing hydrogen, and maintaining the reaction temperature while stirring till the pressure in the high-pressure kettle does not decline, so as to obtain the product which is DMAPA. The preparation method of the hydrogenation catalyst disclosed by the invention is simple in process. The invention further provides the method for synthesizing DMAPA, wherein the consumption of raw materials acrylonitrile and dimethylamine can be greatly reduced and the treatment expense of a lot of hazardous wastes is lowered.

Description

technical field [0001] The invention relates to a method for preparing a catalyst and a method for using the catalyst, in particular to a method for preparing a hydrogenation catalyst and a method for synthesizing DMAPA with the catalyst. Background technique [0002] DMAPA is an important intermediate, which is mainly used in surfactants and polyurethane catalysts. It is also a raw material for the preparation of accelerators, and has strong anti-corrosion properties. [0003] Patent CN102617356A summarizes the synthesis method of DMAPA, but it is different from the domestic production synthesis method. The main reason is that the domestic production of DMAPA is mainly for the purpose, and the synthesis method provided by this patent is for the purpose of effectively utilizing the corresponding nitrile raw materials. [0004] Patent 200610102303.X adopts the chemical synthesis method to synthesize the highly selective Ni, Co, additives and rare earth metal synthesis cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/887C07C211/11C07C209/48
Inventor 欧阳亮金秀华熊宝存李中生周雍玉徐三善
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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