Method for preparing m-xylylenediamine

A technology of m-xylylenediamine and isophthalonitrile, which is applied in the field of preparing m-xylylenediamine, can solve the problems of poor m-xylylenediamine selectivity, high reaction pressure and high energy consumption, and achieve improved selectivity and reduced Effects of Reaction Pressure and Energy Consumption

Inactive Publication Date: 2012-09-26
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

But utilize above-mentioned technical reaction pressure and energy consumption height, and the selectivity difference of product m-xylylenediamine

Method used

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  • Method for preparing m-xylylenediamine

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Embodiment 1

[0017] The catalyst used is 10%Ni-5%Cu-5%Re / diatomaceous earth. The carrier is diatomaceous earth, which is sieved into 20-40 mesh. The catalyst active components Ni, Cu and Re were supported on the carrier diatomite by conventional impregnation method. 3.0 grams of catalyst were activated by hydrogen before the reaction, and the activation conditions were: GHSV=1000h -1 , 0.2MPaG, 375°C, reduction time 5 hours. A trickle bed reactor is used. At a reaction temperature of 80°C and a reaction pressure of 10.0MPaG, H 2 / isophthalonitrile=100 (molar ratio), isophthalonitrile / m-xylylenediamine / NH 3 =10:10:80 (weight ratio), isophthalonitrile liquid space velocity is 0.8h -1 , the reaction time is 50h, sampling analysis. SE-30 capillary column, FID detector. Normalized by area. The results of the reactions are summarized in Table 1.

Embodiment 2

[0019] Adopting reaction temperature is 60 ℃, other conditions are identical with embodiment 1.

Embodiment 3

[0021] Adopting reaction temperature is 100 ℃, other conditions are identical with embodiment 1.

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Abstract

The invention discloses a method for preparing m-xylylenediamine. The method is characterized in that a reaction system comprises isophthalonitrile, ammonia, hydrogen and a catalyst; a reaction temperature is in a range of 60 to 100 DEG C; reaction pressure is in a range of 1.0 to 20.0MPa; a mole ratio of H2 to isophthalonitrile is in a range of 10-200; a weight ratio of isophthalonitrile to m-xylylenediamine to NH3 is (3-20): (3-20): (60-94); an airspeed of an isophthalonitrile liquid is in a range of 0.3 to 1.8h<-1>; the catalyst adopts diatomite, Al2O3, active carbon or SiO2 as a carrier and is loaded with one or more of transition metals of Ni and Co as active ingredients and preferably, is loaded with Ni; one or more auxiliary agents are selected from Re, Cu, Cr, Ru, Fe and their oxides; and in a fixed bed reactor, under the ammonia reaction of the catalyst, the high activity and high selectivity transformation of an isophthalonitrile/m-xylylenediamine solution into m-xylylenediamine is realized.

Description

technical field [0001] The invention relates to a method for preparing m-xylylenediamine by hydrogenation of isophthalonitrile as a raw material, in particular by a method for using isophthalonitrile / m-xylylenediamine solution as a raw material A method for converting ammonia to m-xylylenediamine by hydrogenation. technical background [0002] M-xylylenediamine is a colorless liquid with an almond smell. It is an epoxy resin curing agent with excellent performance and a wide range of uses. It is also an important fine chemical intermediate and can be used to synthesize polyurethane and xylene nylon resins. 1,3 -Bis(aminomethyl)cyclohexane, serialized epoxy resins, rubber additives, lubricants, paper processing agents, pesticides, fiber finishing agents, rust inhibitors, chelating agents and electronic chemicals, etc. [0003] M-xylylenediamine is prepared by liquid-phase hydrogenation of isophthalonitrile, and isophthalonitrile is prepared by ammoxidation of m-xylene with a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/51C07C209/48
Inventor 丁云杰严丽王涛吕元马立新
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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