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Catalyst for preparing m-xylylenediamine through hydrogenation of isophthalonitrile as well as preparation method and application of catalyst

A technology of isophthalonitrile and m-xylylenediamine, which is applied in the field of catalysts for preparing m-xylylenediamine by hydrogenation of isophthalonitrile and its preparation field, can solve the problems of lack of catalyst stability, unfavorable continuous operation, Exploring and other issues to achieve the effect of avoiding efficiency reduction, high specific surface area, and large pore structure

Pending Publication Date: 2022-07-29
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it did not investigate the stability of the catalyst, and the catalytic reaction still adopts the trickle bed reaction mode, which is not conducive to continuous operation

Method used

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  • Catalyst for preparing m-xylylenediamine through hydrogenation of isophthalonitrile as well as preparation method and application of catalyst
  • Catalyst for preparing m-xylylenediamine through hydrogenation of isophthalonitrile as well as preparation method and application of catalyst
  • Catalyst for preparing m-xylylenediamine through hydrogenation of isophthalonitrile as well as preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1) dissolving nickel nitrate with deionized water, wherein, the concentration of nickel ions in the solution is 0.5M, and the solution volume is 75mL;

[0059] 2) Weighing citric acid and adding it to the solution of step 1), stirring into a homogeneous solution, wherein the pH value of the solution is 5;

[0060] 3) Weigh 10 grams of aluminum sol and add it to the solution in step 2), stir at room temperature for 2 hours, then heat up to 90°C and stir for 1 hour;

[0061] 4) dissolving cobalt nitrate with deionized water, wherein the concentration of cobalt ions in the solution is 0.1M, and the solution volume is 100mL;

[0062] 5) measure a certain amount of hydrazine hydrate and add it to the solution of step 4), stir into a homogeneous solution, wherein the mol ratio of hydrazine hydrate and cobalt ion is 4:1;

[0063] 6) adding the solution of step 5) to the solution of step 3), stirring and mixing for 4 hours;

[0064] 7) The solution obtained in step 6) was the...

Embodiment 2

[0068] 1) dissolving nickel nitrate with deionized water, wherein, the concentration of nickel ions in the solution is 0.5M, and the solution volume is 75mL;

[0069] 2) Weighing citric acid and adding it to the solution of step 1), stirring into a homogeneous solution, wherein the pH value of the solution is 5;

[0070] 3) Weigh 10 grams of aluminum sol and add it to the solution in step 2), stir at room temperature for 2 hours, then heat up to 90°C and stir for 1 hour;

[0071] 4) dissolving cobalt nitrate with deionized water, wherein the concentration of cobalt ions in the solution is 0.2M, and the solution volume is 75mL;

[0072] 5) measure a certain amount of hydrazine hydrate and add it to the solution of step 4), stir into a homogeneous solution, wherein the mol ratio of hydrazine hydrate and cobalt ion is 4:1;

[0073] 6) adding the solution of step 5) to the solution of step 3), stirring and mixing for 4 hours;

[0074] 7) The solution obtained in step 6) was then...

Embodiment 3

[0078] 1) dissolving nickel nitrate with deionized water, wherein, the concentration of nickel ions in the solution is 0.4M, and the solution volume is 100mL;

[0079] 2) Weighing citric acid and adding it to the solution of step 1), stirring into a homogeneous solution, wherein the pH value of the solution is 5;

[0080] 3) Weigh 10 grams of aluminum sol and add it to the solution in step 2), stir at room temperature for 2 hours, then heat up to 90°C and stir for 1 hour;

[0081] 4) dissolving cobalt nitrate with deionized water, wherein the concentration of cobalt ions in the solution is 0.3M, and the solution volume is 50mL;

[0082] 5) measure a certain amount of hydrazine hydrate and add it to the solution of step 4), stir into a homogeneous solution, wherein the mol ratio of hydrazine hydrate and cobalt ion is 4:1;

[0083] 6) adding the solution of step 5) to the solution of step 3), stirring and mixing for 4 hours;

[0084] 7) The solution obtained in step 6) was the...

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Abstract

The invention discloses a catalyst for preparing m-xylylenediamine through hydrogenation of isophthalonitrile, the catalyst takes Ni and Co as active components and silica sol or alumina sol as a carrier, the content of Ni is 0.1%-50% of the mass of the catalyst, and the content of Co is 0.1%-25% of the mass of the catalyst. The invention also discloses a preparation method and application of the compound. The catalyst provided by the invention is a high-performance hydrogenation catalyst which is prepared by a two-step method of peptizing complexation and coordination adsorption and has uniformly distributed double metal alloy layers. The bimetallic alloy catalyst prepared by a novel two-step method shows excellent catalytic performance in the reaction process of preparing m-xylylenediamine through hydrogenation of isophthalonitrile, the conversion rate is 100%, the highest selectivity can reach 99.6%, and the stability is tested after 1000 hours.

Description

technical field [0001] The invention relates to the technical field of nitrile hydrogenation catalysts, in particular to a catalyst for preparing m-xylylenediamine by hydrogenation of isophthalonitrile, and a preparation method and application thereof. Background technique [0002] Meta-xylylenediamine is abbreviated as MXDA. It is a colorless liquid with an almond odor. It has various characteristics of aromatic amines, low toxicity, low volatility, good heat resistance, water resistance and chemical resistance. It is an epoxy resin curing agent with many excellent properties due to the advantages of suitability and good quality of cured materials. As an important fine chemical intermediate, m-xylylenediamine can be used as a raw material for the production of polyurethane, nylon and other products. There are also important applications. [0003] There are many synthetic methods of m-xylylenediamine, and there are two technical synthesis paths most commonly used in indust...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J37/18C07C211/27C07C209/48
CPCB01J23/755B01J37/18C07C209/48C07C211/27Y02P20/584
Inventor 陈兴坤王雪鹏
Owner ZHEJIANG NORMAL UNIVERSITY
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