Copper-zinc catalyst for preparing N-methylaniline and N,N-dimethylaniline as well as preparation method and application of copper-zinc catalyst

A technology of dimethylaniline and methylaniline, which is applied in the field of copper-zinc catalyst and its preparation, can solve the problems of simplification, strong pollution, complex reaction process, etc., and achieve cost reduction, simple reaction process, and few types of raw materials Effect

Pending Publication Date: 2022-01-28
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional industrial production of N-methylaniline and N,N-dimethylaniline has the disadvantages of strong pollution, complex reaction process, and certain danger, and single production

Method used

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  • Copper-zinc catalyst for preparing N-methylaniline and N,N-dimethylaniline as well as preparation method and application of copper-zinc catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: A catalyst for preparing N-methylaniline and N,N-dimethylaniline and a method for preparing N-methylaniline and N,N-dimethylaniline

[0024] (1) The preparation method of copper-zinc catalyst:

[0025] S1. First weigh 53g of sodium carbonate and dissolve it in 530g of water and stir at 70°C and 300r / min;

[0026] S2. Weigh again 74.4g zinc nitrate hexahydrate and 60.4g copper nitrate trihydrate and dissolve them in 200g water, drop them into the sodium carbonate solution through a constant pressure dropping funnel, the pH is 7.5 after the addition is complete, continue to react for 1h, and naturally Aged for 2 hours under cooling, then washed twice and then suction filtered;

[0027] S3. The precipitate after suction filtration was dried at 90° C. for 8 hours, and then calcined at 400° C. for 4 hours. Characterized by BET, the specific surface area of ​​the catalyst is 17.1m 2 / g, pore size 16.6nm.

[0028] (2) Utilize above-mentioned copper-zinc catalyst...

Embodiment 2

[0033] Example 2: A catalyst for preparing N-methylaniline and N,N-dimethylaniline and a method for preparing N-methylaniline and N,N-dimethylaniline

[0034] (1) The preparation method of copper-zinc catalyst:

[0035] S1. First weigh 53g of sodium carbonate and dissolve it in 530g of water and stir at 70°C and 300r / min;

[0036] S2. Take again 99.2g zinc nitrate hexahydrate and 40.3g copper nitrate trihydrate and dissolve them in 200g water, drop them into the sodium carbonate solution through a constant pressure dropping funnel, after the addition is complete, the pH is 7.5, continue to react for 1h, naturally Aged for 2 hours under cooling, then washed twice and then suction filtered;

[0037] S3. The precipitate after suction filtration was dried at 90° C. for 8 hours, and then calcined at 400° C. for 4 hours. Characterized by BET, the specific surface area of ​​the catalyst is 21.8m 2 / g, pore size 19.7nm.

[0038] (2) Utilize above-mentioned copper-zinc catalyst to ...

Embodiment 3

[0043] Example 3: A catalyst for preparing N-methylaniline and N,N-dimethylaniline and a method for preparing N-methylaniline and N,N-dimethylaniline

[0044] (1) The preparation method of copper-zinc catalyst:

[0045] S1. First weigh 127.2g of sodium carbonate and dissolve it in 1272g of water and stir at 70°C and 300r / min;

[0046] S2. Weigh again 119g of zinc nitrate hexahydrate and 193.2g of copper nitrate trihydrate and dissolve them in 500g of water, drop them into the sodium carbonate solution through a constant pressure dropping funnel, after the addition is complete, the pH is 7.5, continue to react for 1h, and cool naturally Aged for 2 hours, then washed twice and filtered with suction;

[0047] S3. The precipitate after suction filtration was dried at 90° C. for 8 hours, and then calcined at 400° C. for 4 hours. Characterized by BET, the specific surface area of ​​the catalyst is 17.2m 2 / g, pore size 17.2nm.

[0048] (2) Utilize above-mentioned copper-zinc cat...

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Abstract

The invention belongs to the technical field of catalyst N-methylation, and particularly relates to a copper-zinc catalyst for preparing N-methylaniline and N,N-dimethylaniline as well as a preparation method and application of the copper-zinc catalyst. The molar ratio of copper to zinc in the copper-zinc catalyst is (3:1)-(1:4), the specific surface area of the catalyst is controlled to be 15-30 m<2>/g, and the pore diameter is 15-25nm. The preparation method comprises the following steps: carrying out compression molding on a copper-zinc catalyst and graphite together, loading the molded material into a fixed bed reactor, carrying out catalytic reduction, and adjusting specific process conditions by taking aniline and methanol as raw materials in the fixed bed reactor to obtain N-methylaniline and/or N,N-dimethylaniline. According to the method, the problems of low yield, simplification and the like of the traditional preparation of the N-methylaniline and the N,N-dimethylaniline are solved, and meanwhile, the catalyst disclosed by the invention is few in raw material variety and simple in reaction process, so that the cost of preparing the N-methylaniline and the N,N-dimethylaniline is also greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of catalyst N-methylation, and in particular relates to a copper-zinc catalyst used for preparing N-methylaniline and N,N-dimethylaniline, a preparation method and application thereof. Background technique [0002] N-methylation of aniline is an important reaction in industry. N,N-dimethylaniline is an important chemical intermediate, which is widely used in the production and manufacturing industries of dyes, medicines, pesticides, explosives, plastics, etc. curing accelerator. DMA has a relatively large consumption in the field of dyes and spices. For dyes, there are common azo dyes, basic bright yellow, basic violet, etc. For spices, there is vanillin, which is used in the synthesis of dexon in pesticides. consumption is also high. At the same time, as the main intermediate in the production of N,N-dimethylaniline, N-methylaniline is also an important chemical intermediate and is used in a wide range of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/80B01J35/10C07C209/18C07C211/48
CPCB01J35/1014B01J35/1061B01J23/80C07C209/18C07C211/48
Inventor 何明阳王震孙中华钱俊峰吴中陈群
Owner CHANGZHOU UNIV
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