Catalyst system and method for preparing m-xylylenediamine

A technology of m-xylylenediamine and isophthalonitrile, which is applied in the field of catalytic hydrogenation, can solve the problems of high cost, lack of economic advantages, and difficulty in meeting the needs of long-term operation, and achieves the effect of high-efficiency operation.

Active Publication Date: 2020-04-21
WANHUA CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of two-stage fixed-bed reactors requires more costs in design and construction, and does not have economic advantages. In addition, the development

Method used

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  • Catalyst system and method for preparing m-xylylenediamine
  • Catalyst system and method for preparing m-xylylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0075] Example 1

[0076] Fill 10mL of commercially available 30%Co-3%Cr supported catalyst and 40mL of commercially available 35%Ni-5%Fe supported catalyst (both mass fractions) into the middle section of a 100mL fixed bed reaction tube, based on Co catalyst Located on top of Ni-based catalyst. Reducing with hydrogen to activate the catalyst, the reaction temperature is set to 60℃, the reaction pressure is set to 13MPa, the molar ratio of hydrogen to isophthalonitrile is 5:1, and the mass ratio of raw materials is isophthalonitrile:ethanol:liquid ammonia 2:15:10 after mixing at volumetric space velocity 2.5h -1 Pump into the reaction tube to react. The results of the reaction are shown in Table 2.

Example Embodiment

[0077] Example 2

[0078] Load 15mL of commercially available 30%Co-3%Cr supported catalyst and 35mL of commercially available 35%Ni-5%Fe supported catalyst (both mass fractions) into the middle section of a 100mL fixed bed reaction tube, based on Co catalyst Located on top of Ni-based catalyst. Reducing with hydrogen to activate the catalyst, the reaction temperature is set to 80℃, the reaction pressure is set to 12MPa, the molar ratio of hydrogen to isophthalonitrile is 8:1, and the raw materials are based on the mass ratio of isophthalonitrile: tetrahydrofuran: liquid ammonia 1:1:10 after mixing at a volumetric space velocity of 1.5h -1 Pump into the reaction tube to react. The results of the reaction are shown in Table 2.

Example Embodiment

[0079] Example 3

[0080] Fill 20mL of commercially available 30%Co-3%Cr supported catalyst and 30mL of commercially available 35%Ni-5%Fe supported catalyst (both mass fractions) into the middle section of a 100mL fixed bed reaction tube, based on Co. Located on top of Ni-based catalyst. Reducing with hydrogen to activate the catalyst, the reaction temperature is set to 50℃, the reaction pressure is set to 6MPa, the molar ratio of hydrogen to isophthalonitrile is 6:1, and the raw material is based on the mass ratio of isophthalonitrile: tetrahydrofuran: liquid ammonia 2:15:20 after mixing at volumetric space velocity for 1h -1 Pump into the reaction tube to react. The results of the reaction are shown in Table 2.

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Abstract

The invention discloses a catalyst system for preparing m-xylylenediamine through hydrogenation of isophthalonitrile in the presence of liquid ammonia and a solvent and a method for preparing m-xylylenediamine by adopting the catalyst system. The catalyst system comprises a Co-based catalyst, a Ni-based catalyst, the solvent and an auxiliary agent for the catalyst system, wherein the Co-based catalyst and the Ni-based catalyst are sequentially arranged along the material flow direction. Compared with a single catalyst and catalysts with different grading sequences, the catalyst with the grading sequence of the invention has the following advantages: the operation time can be prolonged, and the operation stability can be improved.

Description

technical field [0001] The application belongs to the field of catalytic hydrogenation, and in particular relates to a catalyst system and method for preparing m-xylylenediamine by hydrogenating isophthalonitrile as a raw material. Background technique [0002] m-Xylylenediamine, MXDA for short, is a colorless liquid at room temperature, soluble in water and organic solvents. Its special structure not only makes it an epoxy resin curing agent with excellent performance, but also an important chemical intermediate with wide application. At present, the production of m-xylylenediamine is mainly obtained by hydrogenation of isophthalonitrile. In the existing hydrogenation process for producing m-xylylenediamine, the commonly used reactors include tank reactors and fixed-bed reactors. Tank reactors are generally used for batch reactions, while fixed-bed reactors are used for continuous reactions. Since the fixed-bed continuous process is obviously superior to the tank-type bat...

Claims

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Application Information

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IPC IPC(8): B01J23/86C07C209/48C07C211/27
CPCB01J23/866B01J23/868C07C209/48C07C211/27Y02P20/584
Inventor 蒋玉鑫王明永王磊胡江林曾伟丁可刘运海靳少华赵欣陈永宋延方杨洋黎源
Owner WANHUA CHEM GRP
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