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A kind of preparation method of m-xylylenediamine

A technology for m-xylylenediamine and isophthalonitrile, which is applied in the field of preparation of high-purity m-xylylenediamine, can solve the problems of large loss of isophthalonitrile, complicated operation, many three wastes, etc. The effect of reducing the dosage of liquid ammonia, simplifying the operation process and improving the quality

Active Publication Date: 2021-07-23
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In view of the problems existing in the extraction step and hydrogenation step in the process of preparing m-xylylenediamine from m-xylene in the above patent, such as many steps, complicated operation, large loss of isophthalonitrile, high energy consumption and three wastes etc., it is urgent to develop new preparation technology to improve these deficiencies

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1) Ammoxidation reaction:

[0059] Ammoxidation uses catalysts with alumina as a carrier, the carrier content accounts for 55% of the catalyst weight, and other components are composed of V, Cr, Mo and P in a ratio of 1:1:0.1:0.1. Fill 5kg of this catalyst in the fluidized bed reactor, the reaction raw material is preheated to 400 DEG C before entering the reactor, the reaction hot spot temperature is 450 DEG C, the source of oxygen is air, m-xylene: ammonia: the mol ratio of air is 3: 20:77. The reaction pressure is 0.02-0.05MPa. The gas residence time is controlled at 0.5s. The gas containing isophthalonitrile was obtained. Based on the m-xylene added to the reaction system, the molar yield of IPN was 85.1%, and the yield of methylbenzonitrile was 2.5%.

[0060] 2) Solvent extraction:

[0061] The gas containing isophthalonitrile is added to the extraction tower from the bottom of the extraction tower. The inner diameter of the extraction tower is 100mm, the heig...

Embodiment 2

[0069] 1) Ammoxidation reaction:

[0070] Ammoxidation uses catalysts with alumina as the carrier, the carrier content accounts for 55% of the catalyst weight, and other components are composed of V, Cr, Mo and Fe in a ratio of 1:1:0.1:0.1. Load 5kg of the catalyst into the fluidized bed reactor. The reaction raw material is preheated to a reaction hot spot temperature of 480°C before entering the reactor. The oxygen source is air, and the volume ratio of m-xylene:ammonia:air is 1:6:28. The reaction pressure is 0.02-0.05MPa. The gas residence time is controlled at 1s. The gas containing isophthalonitrile was obtained. Based on the m-xylene added to the reaction system, the molar yield of IPN was 85.3%, and the yield of methylbenzonitrile was 2.5%.

[0071] 2) Solvent extraction:

[0072] The gas containing isophthalonitrile is added to the extraction tower from the bottom of the extraction tower. The inner diameter of the extraction tower is 100mm, the height is 850mm, and...

Embodiment 3

[0080] 1) Ammoxidation reaction:

[0081] Ammoxidation adopts catalyst with alumina as the carrier, the carrier content accounts for 55% of the catalyst weight, and other components are composed of V, Cr, Fe and P in the ratio of 1:1:0.1:0.1. Load 5kg of the catalyst into the fluidized bed reactor. The reaction raw material is preheated to a reaction hot spot temperature of 350°C before entering the reactor. The source of oxygen is air. The molar ratio of m-xylene:ammonia:air is 1:4:20. The reaction pressure is 0.02-0.05MPa. The gas residence time is controlled at 1s. The gas containing isophthalonitrile was obtained. Based on the m-xylene added to the reaction system, the molar yield of IPN was 84.9%, and the yield of methylbenzonitrile was 2.5%.

[0082] 2) Solvent extraction:

[0083]The gas containing isophthalonitrile is added to the extraction tower from the bottom of the extraction tower. The inner diameter of the extraction tower is 100mm, the height is 850mm, and ...

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PUM

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Abstract

The invention provides a preparation method of m-xylylenediamine. In this process, m-xylene is converted to isophthalonitrile by ammoxidation. The resulting isophthalonitrile is extracted with N-alkylpyrazoles. The extracted isophthalonitrile solution is decarboxylated by the resin and then enters the hydrogenation reactor for hydrogenation reaction to obtain the m-xylylenediamine reaction liquid. Finally, high-purity (>99.9%) m-xylylenediamine was obtained through rectification and separation. The method has the characteristics of simple reaction process, low energy consumption, simple operation, high yield of m-xylylenediamine, high purity of m-xylylenediamine, and the like.

Description

technical field [0001] The invention belongs to the field of synthesis of organic amines, and relates to a preparation method of high-purity m-xylylenediamine. Background technique [0002] m-xylylenediamine (MXDA for short) is a colorless transparent liquid, soluble in water and organic solvents, and is mainly used as a curing agent for epoxy resin and a polymer monomer for nylon modification. The epoxy resin curing agent prepared with MXDA has excellent curing performance, good heat resistance, water resistance and chemical corrosion resistance, and can obtain a transparent cured resin with an extremely smooth surface; a new type of nylon prepared with MXDA as a modified monomer Resin - m-xylene nylon resin has good resistance to oxygen permeability and carbon dioxide loss. MXDA can also be used to synthesize the monomer m-xylene dicyanate (MXDI for short) of polyurethane. Compared with the currently commonly used diphenylmethane diisocyanate (MDI for short), the product ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/48C07C211/27C07C253/34C07C255/51
CPCC07C209/48C07C253/02C07C253/34C07C211/27C07C255/51
Inventor 丁可王明永王磊胡江林靳少华王坤刘运海曾伟杨恒东赵欣陈永杨洋宋延方
Owner WANHUA CHEM GRP CO LTD
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