Energy-saving method for preparing amine compound by continuous hydrogenation of nitrile compound

An amine compound and compound technology, which is applied in the field of energy-saving nitrile compound continuous hydrogenation to prepare amine compound, can solve the problems of reduced catalyst life, reduced production cost, reduced selectivity and catalyst life, etc.

Pending Publication Date: 2021-03-23
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the verification experiment also found that replacing 5% of the solvent with the outlet material of the reactor will cause the selectivity of the target amine to drop to about 95%. If the ratio of outlet material replacement is continued to increase to 10%, the conversion rate will drop to 94.5% while the selectivity decreases. % or so, at the same time the catalyst life is significantly re

Method used

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  • Energy-saving method for preparing amine compound by continuous hydrogenation of nitrile compound
  • Energy-saving method for preparing amine compound by continuous hydrogenation of nitrile compound
  • Energy-saving method for preparing amine compound by continuous hydrogenation of nitrile compound

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0078] Example 1

[0079] Benzophenonitrile (MXPN) continuous hydroformamine (MXDA), the preparation method of adoption, such as image 3 As shown, the mark 1-15 marked in the figure is the material flow stock number.

[0080] The single drip bed reactor size is D = 0.1 M, TL = 2m. The catalyst (CAT-1) is filled in the upper segment of the reactor, and the upper and lower ends are 0.3m height to prevent the catalyst loss, and then secure the catalyst to the porcelain ball in the straight section. Even in the reactor bed, 2 multi-point multi-thermocouple temperature probes are uniformly inserted to instantly measure the temperature change of the bed. The ring tube gas collector is provided in the lower level of the reactor, and the tube diameter of the annular tube is calculated from 5 kPa, and the annular tube ring diameter is 0.06m; open a hole in the lower portion of the annular tube, according to The collected gas was reduced by a hole in a hole computation of 8, and the open h...

Example Embodiment

[0124] Example 2

[0125] The preparation method refers to Example 1, and the difference is only the catalyst Cat-1 is replaced with CAT-3. The feedstock is still MXPN, the solvent is a liquid ammonia, a feed ratio, a feed temperature, amino nitrile ratio, reaction temperature and pressure With the first example, the reactor volume is 100 mL, length 1m, 20 mm inner diameter, and 50 ml of catalyst loading. The raw material feed was 375 ml / h, and the results of 840h were shown in Table 8. It can be found that when the magnesium oxide is not added in the catalyst, the catalyst activity is relatively stable, but as the reaction time continues, the surface of the catalyst is gradually reorganized, and the catalyst activity gradually reduces the increase of amino nitrile, and excessive hydrogenates 1.3 ring The dimethylamine content has gradually increased, indicating that the specificity of the catalyst has gradually decreased.

[0126] Example 1 The reaction situation in Example 2 w...

Example Embodiment

[0129] Example 3

[0130] The preparation method refer to Example 1, and the difference is only to replace the catalyst Cat-1 to CAT-5. The reaction conditions of the feed composition and proportion, the temperature, the ammoniamonitrile ratio, the reaction temperature and pressure, etc., the reactor volume is 100 ml, length 1m, and 20 mm inner diameter, and 50 ml of catalyst loading. The raw material feed is 375 ml / h, and the results of 72h are shown in Table 9. It can be found that MXPN conversion has no significant change as compared with Example 1, but the product selectivity is significantly reduced, and the benzymamine in the by-product (including 1.3-cyclohexamethylamine, methylbenzylamine, benzamine, etc. ) Significantly increased, secondary and three-degree amide recombination of three-zero-like amides.

[0131] Table 9

[0132]

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Abstract

The invention relates to an energy-saving method for preparing an amine compound by continuous hydrogenation of a nitrile compound. The method comprises the following steps: 1) mixing a nitrile compound with an ammonia-containing organic solvent, feeding the mixture into a reactor filled with a catalyst, introducing hydrogen at the same time, and carrying out a hydrogenation reaction in a catalystfilling layer; 2) separating the material after the hydrogenation reaction in the step 1) into a gas phase and a liquid phase, and then separately leading the gas phase and the liquid phase out of the reactor; (3) separating the gas phase led out of the reactor in the step (2) to recover the ammonia-containing organic solvent, then replacing part of a fresh ammonia-containing organic solvent in the step (1) with the recovered ammonia-containing organic solvent, mixing the ammonia-containing organic solvent with the nitrile compound, and then circulating the mixture back to the reactor; and 4)removing the solvent from the liquid phase led out of the reactor in the step 2) to obtain the amine compound. According to the method, the solvent separation load is reduced by 40% or more on the basis of maintaining high conversion rate of raw materials and high selectivity of products, and the production energy consumption and equipment investment are greatly reduced.

Description

technical field [0001] The present invention relates to a method for preparing amine compounds by continuous hydrogenation of energy-saving nitrile compounds, in particular to the preparation of nitriles (especially isophorone nitrile or phthalonitrile) by high-pressure continuous hydrogenation in the presence of liquid ammonia Amines (isophoronediamine or xylylenediamine) method. Background technique [0002] In industry, the hydrogenation of nitriles to produce amines mainly includes continuous fixed-bed and continuous (or batch) tank-type production processes, comprehensive catalyst life, reaction conversion rate and selectivity, equipment investment and operational complexity and other factors. Major manufacturers are currently Both adopt high-pressure fixed-bed production process. However, there are still many problems to be solved in the fixed bed production process due to harsh reaction conditions, large proportion of solvent, expensive catalyst and short life. [0...

Claims

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Application Information

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IPC IPC(8): C07C211/27C07C209/48C07C209/86C07C211/36B01J23/847B01J23/887B01J23/755B01J23/83B01J35/10
CPCC07C209/48C07C209/86B01J23/8472B01J23/002B01J23/8871B01J23/755B01J23/83B01J35/023B01J35/1019B01J35/1061C07C2601/14C07C211/27C07C211/36Y02P20/584
Inventor 朱洪亮蒋玉鑫王静胡展乔小飞
Owner WANHUA CHEM GRP CO LTD
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