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Preparation method of m-xylylenediamine

A technique for m-xylylenediamine and the preparation of m-xylylenediamine, which is applied in the field of preparation of m-xylylenediamine, can solve the problems of reducing catalyst acidity, affecting economy and the like, and achieves the effect of promoting dispersion

Active Publication Date: 2018-01-05
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101062898 discloses a kind of solvent with mixed xylene and liquid ammonia, using Ni / MgO-SiO 2 Catalyst and two-stage hydrogenation process, a method for completely converting isophthalonitrile into m-xylylenediamine, the total yield of m-xylylenediamine is 99.5%, and the amount of MgO added is 1%-2% of the total mass of the catalyst , the introduction of MgO reduces the acidity of the catalyst, inhibits the formation of condensation polymers, prolongs the life of the catalyst, and improves the hydrogenation yield, but the two-stage hydrogenation process affects the economics of this process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 29.7g Ni(NO 3 ) 2 ·6H 2 O, 19.1g Mg(NO 3 ) 2 ·6H 2 O and 7.4g Al(NO 3 ) 3 9H 2 Dissolve O in water to make a 100ml solution; take another 24.1g Na 2 CO 3 Dissolve in water to make 100ml solution. Add the above two solutions dropwise to 200ml of distilled water at the same time under stirring to form a green precipitate. After washing the precipitate with distilled water, add 200ml of n-butanol, evaporate to dryness in a water bath, dry in a 393K oven, and then press into tablets. Crush and sieve 20-40 mesh, reduce the catalyst precursor particles in flowing hydrogen at 723K for 2 hours, hydrogen GSVH=1000h -1 , then at room temperature with 0.5% O 2 / N 2 The mixed gas is passivated to obtain catalyst A.

Embodiment 2

[0023] Weigh 29.7g Ni(NO 3 ) 2 ·6H 2 O, 22.3g Mg(NO 3 ) 2 ·6H 2 O and 3.7g Al(NO 3 ) 3 9H 2 Dissolve O in water to make a 100ml solution; take another 23.8g Na 2 CO 3 Dissolve in water to make 100ml solution. Add the above two solutions dropwise to 200ml of distilled water at the same time under stirring to form a green precipitate. After washing the precipitate with distilled water, add 200ml of n-butanol, evaporate to dryness in a water bath, dry in a 393K oven, and then press into tablets. Crush and sieve 20-40 mesh, reduce the catalyst precursor particles in flowing hydrogen at 723K for 2 hours, hydrogen GSVH=1000h -1 , then at room temperature with 0.5% O 2 / N 2 The mixed gas is passivated to obtain catalyst B.

Embodiment 3

[0025] Weigh 29.7g Ni(NO 3 ) 2 ·6H 2 O, 23.9g Mg(NO 3 ) 2 ·6H 2 O and 1.8gAl(NO 3 ) 3 9H 2 Dissolve O in water to make a 100ml solution; take another 23.6g Na 2 CO 3 Dissolve in water to make 100ml solution. Add the above two solutions dropwise to 200ml of distilled water at the same time under stirring to form a green precipitate. After washing the precipitate with distilled water, add 200ml of n-butanol, evaporate to dryness in a water bath, dry in a 393K oven, and then press into tablets. Crush and sieve 20-40 mesh, reduce the catalyst precursor particles in flowing hydrogen at 723K for 2 hours, hydrogen GSVH=1000h -1 , then at room temperature with 0.5% O 2 / N 2 The mixed gas is passivated to obtain catalyst C.

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Abstract

A preparation method of m-xylylenediamine is characterized in that a fixed bed reactor is used, a solution obtained through dissolving isophthalonitrile in a mixed solvent is pumped into a bed packedwith a Ni / MgAlO catalyst, and the isophthalonitrile reacts with hydrogen at a temperature of 60-140 DEG C under a pressure of 1.0-8.0 MPa at a mass space velocity of the isophthalonitrile being 0.1-5h<-1> according to a molar ratio of the hydrogen to the isophthalonitrile being (5-50):1 to generate the m-xylylenediamine. The highest yield of the m-xylylenediamine under preferred reaction conditions reaches 100%, and the preparation method can be used for industrial continuous production.

Description

technical field [0001] The invention relates to a preparation method of m-xylylenediamine, which belongs to the technical field of catalytic hydrogenation. technical background [0002] m-xylylenediamine (MXDA) is an epoxy resin curing agent with excellent performance. It has the advantages of low temperature curing, heat resistance, water resistance, good chemical corrosion resistance, low viscosity and easy operation. It can also be used in polyurethane , polyamide, rubber additives, pesticides, fiber finishing agents, rust removers, chelating agents, lubricants, paper processing aids and electronic chemicals, etc. It is a fine chemical with a wide range of applications and high added value. [0003] M-xylylenediamine is generally produced by catalytic hydrogenation of isophthalonitrile. The domestic industrial production of m-xylylenediamine is still based on the batch reaction of the reactor, the production scale is small, the catalyst particles are fine, easy to pulver...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/48C07C211/51B01J23/755
Inventor 沈俭一陈慧袁蒋雨王小干傅玉川
Owner NANJING UNIV