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Isophthalonitrile dehydration hydrogenation method

A technology of isophthalonitrile and phthalonitrile, applied in chemical instruments and methods, preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of shortening the use of catalysts and hydrolysis Side reactions and other problems, to achieve the effect of simplifying operation, reducing the rate of polycondensate formation and reducing the cost of hydrogenation

Inactive Publication Date: 2012-05-23
上海博润石化科技发展有限公司
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Problems solved by technology

[0007] In the above technical scheme, although high-purity m-xylylenediamine products can be produced, due to the acidity of the catalyst, when the raw material contains a small amount of water, isophthalonitrile will also undergo hydrolysis in addition to the hydrogenation reaction. Side reaction, the resulting polycondensate precursors 3-cyanobenzamide and 3-cyanobenzoic acid will undergo a series of condensation reactions with hydrogenation intermediates and products, and the resulting polymer will cover the surface of the catalyst , so that the use of the catalyst is significantly shortened, requiring frequent regeneration

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Embodiment 1～8

[0029] The dehydration reactor is a φ25mm×1000mm stainless steel tube reactor, and the reaction tube is filled with spherical molecular sieves with a diameter of 3-5mm and a pore size of 0.3nm. The dehydration conditions are: the temperature is room temperature, and the space velocity is 2 to 5 hours -1 .

[0030] The hydrogenation reactor is two φ25mm×1000mm stainless steel tubular reactors in series. The reaction tubes are filled with 50ml (first stage) and 25ml (second stage) of nickel-containing catalysts with a diameter of 1 / 8″ respectively, and the bottom of the reactor is filled with inert ceramic balls. .Catalyst Ni / MgO-SiO 2 The content of Ni in the medium is 22%, the content of NiO is 46%, the content of MgO is 1-2%, and the rest is carrier.

[0031] The mixed xylene-isophthalonitrile-liquid ammonia solution is preheated and then pumped into the dehydration reactor from the top at a set rate. After dehydration, the material is then pumped into the first-stage hydro...

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Abstract

The invention discloses a method of isophthalonitrile dehydration and hydrogenation, which comprises the following steps: stripping moisture in the fixed bed with molecular dewatering screen under room temperature ; setting the air speed of dehydration at 2-5h<-1>; proceeding hydrogenation under the function of activator; proceeding hydrogenation in two series tubular reactor. This invention decreases the generating speed of polycondensation and dewatering speed of middle product of hydrogenation, which can prolong durability of activator.

Description

technical field [0001] The invention relates to a method for dehydration and hydrogenation of isophthalonitrile, in particular to removing the moisture contained in the hydrogenation raw material with a dehydration molecular sieve before entering the catalyst bed, and then dehydrating the raw material in Ni / MgO-SiO 2 Hydrogenation is carried out under the action of a catalyst. Due to the removal of moisture in the raw material, the formation rate of polycondensate and the hydrolysis rate of raw material or hydrogenation intermediate product are reduced, thereby prolonging the service life of the catalyst. Background technique [0002] M-xylylenediamine is mainly used in epoxy resin curing agent and nylon modified polymer monomer. Usually m-xylylenediamine is produced by hydrogenation of isophthalonitrile. The hydrogenation reaction can adopt tank-type intermittent hydrogenation or fixed-bed continuous hydrogenation process, and the catalysts are all fine-grained catalysts ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/48C07C211/51B01J23/755B01J21/10B01J32/00B01J35/08
Inventor 倪俊
Owner 上海博润石化科技发展有限公司
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