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Catalyst for reductive methylation of amines and its preparation and application

An amine methylation and catalyst technology, which is applied in the field of preparation of catalytic amine methylation catalysts, can solve the problems of high cost and lack of material sources, and achieves the effects of convenient operation, improved methylation efficiency and high catalytic efficiency.

Active Publication Date: 2020-09-01
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Noble metal catalysts can achieve good selectivity and catalytic activity, but the source of materials is scarce and the cost is high. There is an urgent need for a non-precious metal-based catalyst with high catalytic activity in the industry.

Method used

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  • Catalyst for reductive methylation of amines and its preparation and application
  • Catalyst for reductive methylation of amines and its preparation and application
  • Catalyst for reductive methylation of amines and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] A method for preparing a high-density grain boundary catalyst for the methylation reaction of amines, and its application in the methylation reaction of amines, comprising the following steps:

[0077] 1. Synthesis of HGB-In2O3 (indium oxide nanocatalyst with high density grain boundary)

[0078] 1) Dissolve 3 mmol of indium acetate, 1.62 mmol of 4,4'-bipyridine and 3 mmol of 2,2'-biphenyldicarboxylic acid in 45 mL of deionized water, and then stir at room temperature for 30 minutes.

[0079] 2) The solution was transferred to a 50 mL Teflon-lined autoclave, which was then sealed and heated at 150° C. for 20 hours.

[0080] 3) After cooling the mixture to room temperature, the precipitate was collected by centrifugation, washed three times with deionized water, ethanol and acetone, respectively, and then dried at 60° C. for 12 hours.

[0081] 4) Calcining the obtained In-MOF in a muffle furnace at 350°C for 3 hours to obtain HGB-In2O3 (indium oxide nanocatalyst with hi...

Embodiment 2

[0122] The catalyst prepared in Example 1 was tested for cycle stability. The method of embodiment 1 is repeated, and the cycle is carried out five times, and each test test result is shown in Figure 11 , the test data are shown in Table 1.

[0123] Table 1

[0124]

[0125] From figure 1 It can be seen from the data in Table 1 that the catalyst of the present invention has good catalytic activity, not only that, but also good cycle stability.

Embodiment 3

[0127] Compared with Example 1, the only difference is that the temperature of the calcination process is 300°C. According to the formula, the calculated grain boundary density is 98000. Using the same test method as in Example 1, it was found that the final 9h conversion rate was 45.7%.

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Abstract

The invention discloses the field of catalytic materials and specifically provides a catalyst for reduced aminomethylation. The catalyst is In2O3 nanocrystal with grain boundary density being not lower than 75,000 m / mg. The invention also provides a preparation method of the catalyst. The catalyst is prepared by calcining a metal-organic framework material of indium in an oxygen-bearing atmosphere and at 300-400 DEG C. It is innovatively found that grain boundary density of the product is regulated by controlling calcination temperature of the metal-organic framework material of indium. And it is found that the grain boundary density has linear relation with catalytic activity. A catalyst with high grain boundary density has more excellent catalytic performance. The preparation method of the catalyst is simple and is convenient to operate. The catalyst has high catalytic efficiency, is low-cost, and can be recycled.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials and catalysis, and in particular relates to a preparation method and application of a catalytic amine methylation catalyst with high performance and low cost. Background technique [0002] Methyl-substituted amines widely exist in natural products, and have important applications in large chemical industry, fine chemical industry, pharmaceuticals and dyes. [0003] Some amine methylation methods have been reported in the prior art, for example, formaldehyde is used as a source of C, and carboxylic acid is used as a reducing agent to perform one-step methylation of amines. In addition, the technology of methylating amines with methylating reagents such as methyl iodide, dimethyl sulfate, methyl p-toluenesulfonate, and diazomethane has also been reported in the prior art. The existing methylation methods have defects such as high drug toxicity and unsatisfactory catalytic performance, w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/08B82Y30/00B82Y40/00C07C209/28C07C211/48C07C211/52C07D209/08
CPCB01J23/08B82Y30/00B82Y40/00C07C209/28C07D209/08C07C211/48C07C211/52
Inventor 王梁炳王利容解杨岑子
Owner CENT SOUTH UNIV
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