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Preparation method of meta-xylylene diamine

A technology for m-xylylenediamine and isophthalonitrile, which is applied in the field of preparing m-xylylenediamine, can solve problems such as difficulty in meeting heat transfer requirements, catalyst damage, limited heat exchange area, etc., and achieves convenient cleaning and equipment installation, The effect of smooth response and strict response control

Active Publication Date: 2011-01-26
CAC NANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The coil heat exchanger installed in the autoclave can only provide a limited heat transfer area, which is difficult to meet the heat transfer requirements of the reaction
In addition, the use of coil heat exchangers is likely to cause damage to the catalyst

Method used

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  • Preparation method of meta-xylylene diamine

Examples

Experimental program
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Embodiment Construction

[0024] In the 1m with hydrogen gas inlet distributor and external circulation corrugated casing heat exchanger 3 Drop into 63kg isophthalonitrile (IPN) successively in autoclave, 200L toluene, 150L ethanol, 1Kg potassium hydroxide, 1Kg water and 8Kg Raney's nickel catalyst, close still, use H 2 Fill to 0.3Mpa and replace the air three times, then pass H 2 To the reaction pressure of 2-3pa, turn on stirring and heat to 90-100°C, turn on the high-pressure pump to circulate the reaction liquid once every 10 minutes, and pour 80°C deionized water into the corrugated casing with a flow rate of 20M 3 / h; continuously pass hydrogen until no more hydrogen is absorbed, stop the high-pressure pump at this time, cool the reaction solution to 30°C and stop stirring, and use N 2 Replaced 3 times, settled the reaction solution for 30 minutes to separate the catalyst, pressed out the supernatant (MXDA reaction solution), and used the catalyst in the lower layer. The analytical yield of m-x...

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Abstract

The invention discloses a preparation method of meta-xylylene diamine. In an autoclave, Raney Nickel is used as a catalyst, the mixture of arene and alcohol is used as a solvent, and a hydrogenation reaction of m-phthalonitrile is performed for 20 to 90 minutes at the temperature of 40 to 120 DEG C and under a pressure of 2 to 10 MPa to generate the meta-xylylene diamine, wherein the hydrogenation reaction is performed by using a hydrogen intake distributor in the autoclave; the heat exchanger of the autoclave employs an external circulating heat exchanger and the reaction liquid in need of exchanging heat is pumped into the external circulating heat exchanger by a high pressure pump to exchange heat. The reaction of the preparation method of meta-xylylene diamine is stable and performed quickly under a low pressure with high yield.

Description

Technical field: [0001] The invention relates to a method for preparing m-xylylenediamine. Background technique: [0002] m-xylylenediamine is an important intermediate of organic raw materials, mainly used in the manufacture of epoxy resin curing agent, rubber additives, photosensitive plastics, polyurethane resin and coatings, and can also be used in pesticides, fiber finishing agents, antirust agents , lubricants, etc. [0003] Foreign countries began to produce MXDA in the early 1970s, and Japan's Mitsubishi Gas and Showa Denko put into production 4000 tons / year and 2000 tons / year production devices respectively in the early 1980s. At present, Japan's Mitsubishi gas industrial production method adopts the trickle bed continuous method, with an annual output of 50,000-100,000 tons. BASF in Germany adopts the fixed-bed catalytic method, but there are very few domestic manufacturers. [0004] The reaction undergoes an intermediate process of hydrogenation of isophthaloni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/27C07C209/48
Inventor 李海娟黄志文王海波田晓宏
Owner CAC NANTONG CHEM
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