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Reductive amination catalyst and preparation method

A catalyst and amination technology, which is applied in the direction of physical/chemical process catalysts, molecular sieve catalysts, amino compound preparation, etc. It can solve the problems of difficult continuous production of catalysts, low industrial application value, and short life, so as to improve nucleation and crystal grains Formation, improvement of activity, effect of enhancing activity

Active Publication Date: 2018-05-04
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the catalysts reported above have the problems of being difficult to be used in continuous production or having low activity and short life, and have low industrial application value.

Method used

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  • Reductive amination catalyst and preparation method
  • Reductive amination catalyst and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Catalyst preparation:

[0031] At room temperature, add 74.0g nickel nitrate hexahydrate, 36.1g ferric nitrate nonahydrate, 2.6g rhodium chloride trihydrate into a mixed solvent of 60mL methanol and 240mL water, add 10mL ethanolamine, stir evenly, then add 30g titanium oxide and 49gY molecular sieve; the resulting mixture was left standing at room temperature for 24h, the solvent was removed under reduced pressure at 30°C, and dried at 120°C; shaped and calcined at 600°C for 4h to obtain the catalyst precursor; The volume space velocity is 1000h -1 hydrogen reduction for 3h to obtain the catalyst.

[0032] Catalytic Performance Evaluation:

[0033] Cool naturally to a temperature of 160°C, at a pressure of 8 MPa, the molar ratio of hydrogen to 1,2-propylenediamine is 2.5:1, and the molar ratio of raw material liquid ammonia to 1,2-propylene glycol is 15:1,1,2-propylene glycol Feed liquid space velocity is 1.56g / g cat The performance of the catalyst was evaluated und...

Embodiment 2

[0035] Catalyst preparation:

[0036] At room temperature, add 98.6g of nickel nitrate hexahydrate, 4.1g of ruthenium trichloride trihydrate and 13.6g of zinc nitrate hexahydrate into a mixed solvent of 70mL of ethanol and 210mL of water, add 10mL of ethanolamine, stir evenly, and then add 40g of fumed white Carbon black and 35g mordenite; the resulting mixture was left standing at room temperature for 12h, the solvent was removed under reduced pressure at 50°C, and dried at 120°C; shaped and calcined at 500°C for 4h to obtain the catalyst precursor; the catalyst precursor was heated at 450°C under normal pressure Under the condition, with the volumetric space velocity as 800h -1 The hydrogen reduction 4h, obtains described catalyst.

[0037] The catalytic performance evaluation conditions are the same as in Example 1, and the results are shown in Table 1.

Embodiment 3

[0039] Catalyst preparation:

[0040] At room temperature, add 123.3g of nickel nitrate hexahydrate and 5.1g of rhodium trichloride trihydrate into a mixed solvent of 60mL of n-propanol and 240mL of water, add 8mL of ethanolamine, stir well, then add 30g of fumed silica and 43g of β molecular sieve The resulting mixture was allowed to stand at room temperature for 16 hours, and the solvent was removed under reduced pressure at 50°C, and dried at 120°C; shaped and calcined at 450°C for 5 hours to obtain the catalyst precursor; Speed ​​is 600h -1 The hydrogen reduction 4h, obtains described catalyst.

[0041] The catalytic performance evaluation conditions are the same as in Example 1, and the results are shown in Table 1.

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Abstract

The invention relates to a reductive amination catalyst and a preparation method. The reductive amination catalyst consists of aM*bA*cX1*(100-a-b-c)X2, in the formula, M represents an active componentmetal and / or an oxide thereof; A represents an auxiliary active component; X1 and X2 represent two carriers; a, b and c respectively represent mass percentages of M, A and X1; a is greater than or equal to 0.1 and less than or equal to 50; b is greater than or equal to 0.1 and less than or equal to 50; c is greater than or equal to 0.1 and less than or equal to 90. The preparation method of the catalyst comprises the following steps: mixing an alcohol with water so as to obtain a mixed solvent; adding ethanol amine; dissolving soluble salts of the active component M and the auxiliary active component A in the mixed solution; leaving to stand, depressurizing to remove the solvent, drying, molding, and roasting so as to obtain a catalyst precursor; performing reduction in the presence of hydrogen, thereby obtaining the catalyst. The catalyst provided by the invention has activity and stability prior to those of the prior art, and has remarkable industrial application values.

Description

technical field [0001] The invention relates to a reductive amination catalyst and a preparation method, in particular to a reductive amination catalyst and a preparation method for preparing propylenediamine from propylene glycol. Background technique [0002] Propylenediamine includes 1,2-propylenediamine and 1,3-propylenediamine. Propylenediamine is a very important organic chemical raw material and intermediate, widely used in pharmaceuticals, pesticides, dyes, oils, epoxy resins, spandex, coatings and other industries. 1,3-propylenediamine with a linear structure shows better performance than ethylenediamine in many fields. With the development of downstream industries, the market demand for propylenediamine continues to increase, and its application range is also wider. However, domestic production capacity is limited and mainly depends on imports. [0003] At present, there are mainly two methods for preparing propylenediamine. One is to use dichloropropane as a ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/14B01J29/24B01J29/26B01J29/46B01J29/48B01J29/76C07C209/16
CPCB01J29/146B01J29/24B01J29/26B01J29/46B01J29/48B01J29/7615B01J2229/18C07C211/11C07C209/16
Inventor 余秦伟吕剑杨建明梅苏宁赵锋伟惠丰李亚妮袁俊张前
Owner XIAN MODERN CHEM RES INST
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