Nitrogen-doped carbon material supporting cobalt catalyst and method therewith of catalytic hydrogenation reductive amination to produce amine compounds

A nitrogen-doped carbon and cobalt catalyst technology, which is applied in the direction of catalyst activation/preparation, reductive alkylation preparation, organic compound preparation, etc., can solve the problems of high reaction pressure, equipment corrosion, poor product quality, etc., and achieve the goal of reaction Mild conditions, reduced reaction pressure, and reduced production costs

Inactive Publication Date: 2017-04-05
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the ammonolysis of halogenated hydrocarbons is no longer used at home and abroad due to serious equipment corrosion and three wastes, low yield, and poor product quality. Instead, it is mainly produced by clean processes such as the hydrogenation ammonia method, and the reaction pressure of this method is relatively high. Lead to high benzylamine production cost, and benzylamine yield is not high

Method used

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  • Nitrogen-doped carbon material supporting cobalt catalyst and method therewith of catalytic hydrogenation reductive amination to produce amine compounds
  • Nitrogen-doped carbon material supporting cobalt catalyst and method therewith of catalytic hydrogenation reductive amination to produce amine compounds
  • Nitrogen-doped carbon material supporting cobalt catalyst and method therewith of catalytic hydrogenation reductive amination to produce amine compounds

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Experimental program
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Effect test

Embodiment 1

[0029] A nitrogen-doped carbon material supported cobalt catalyst, prepared by the following method:

[0030] 1) Dissolve 5.5g 2-methylimidazole in 20mL water to obtain 2-methylimidazole solution, dissolve 0.45g cobalt nitrate hexahydrate in 3mL water to obtain cobalt nitrate solution, add cobalt nitrate solution to 2-methylimidazole In the imidazole solution, a mixed solution was obtained, and the mixed solution was stirred and reacted at room temperature (25° C.) for 6 hours. After the reaction was completed, the obtained mixed system was centrifuged and filtered, and the filter cake was washed with water and methanol in sequence, and the obtained solid was vacuum Dry to obtain MOF material ZIF-67;

[0031] Carry out X-ray diffraction analysis to the nitrogen-doped carbon material supported cobalt catalyst prepared in Example 1, the X-ray diffraction pattern of gained is as follows figure 1 As shown, it shows that we have successfully prepared ZIF-67.

[0032] 2) Under the...

Embodiment 2

[0035] The operation and steps are the same as in Example 1, only the calcination temperature is changed, and the calcination temperature is changed to 800°C, and the obtained nitrogen-doped carbon material supports the cobalt catalyst Co / N-C, which is marked as catalyst B.

Embodiment 3

[0037] The operation and steps were the same as in Example 1, only the calcination temperature was changed, and the calcination temperature was changed to 900° C., and the obtained nitrogen-doped carbon material supported cobalt catalyst Co / N-C, which was marked as catalyst C.

[0038] Carry out X-ray diffraction analysis to the nitrogen-doped carbon material supported cobalt catalyst prepared in embodiment 1-3, the X-ray diffraction pattern of gained is as follows image 3 shown, from image 3 It can be seen that the three peaks at 44.2°, 51.6°, and 76.0° correspond to the three crystal planes of Co(111), Co(200), and Co(200) respectively (JCPDS No.15-0806), further indicating that the cobalt nanoparticles exist. Compared image 3 , it can be found that there are more characteristic peaks of metallic cobalt, and the characteristic peaks of ZIF-67 disappear.

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Abstract

The invention discloses a nitrogen-doped carbon material supporting cobalt catalyst and a method therewith of catalytic hydrogenation reductive amination to produce primary amine compounds. The catalyst is prepared through the steps of: 1) preparing a MOF material ZIF-67; and 2) under protection of nitrogen gas, calcining the MOF material ZIF-67 at 200-1000 DEG C for 1-10 h to produce the nitrogen-doped carbon material supporting cobalt catalyst Co / N-C. The method of catalytic hydrogenation reductive amination to produce the primary amine compounds with the catalyst includes the steps of: in an organic solvent, adding a carbonyl compound, ammonia water and the nitrogen-doped carbon material supporting cobalt catalyst, feeding hydrogen gas, and performing a reaction at 50-150 DEG C under 0.1-5 MPa for 0.5-20.0 h to produce the amine compounds. The preparation method of the catalyst is simple in operations. The catalyst can be used for producing the primary amine compounds in a manner of catalytic hydrogenation reductive amination. In the method, the primary amine compounds are produced with the carbonyl compound as a raw material through catalytic hydrogenation by means of the catalyst, so that the method has mild reaction conditions and is high in yield.

Description

technical field [0001] The invention relates to the technical field of preparing amines by catalytic hydrogenation, and more specifically relates to a nitrogen-doped carbon material-supported cobalt catalyst and a method for preparing amine compounds by catalytic hydrogenation-reductive amination thereof. Background technique [0002] Primary amine compounds are oily liquids with a slight ammonia smell. They are weakly alkaline and miscible with most organic solvents. They are highly irritating and toxic to the skin and mucous membranes. [0003] Primary amine compounds are important organic chemical raw materials and fine chemical intermediates, used in medicine, pesticides, surfactants, dyes, explosives, CO 2 Absorbents and other aspects have a wide range of applications. The production methods of primary amine compounds mainly include reductive amination of carbonyl compounds, ammonolysis of halides, hydrogenation ammonia method, hydrogenation method of nitriles, aminoly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/08C07B43/04C07C209/26C07C211/27C07C211/29C07C211/30C07C211/03C07C211/17C07C211/21C07C211/38C07C211/49C07C213/02C07C217/58C07D307/52C07D307/58
CPCB01J27/24B01J37/086C07B43/04C07C209/26C07C213/02C07D307/52C07D307/58C07C211/27C07C211/29C07C211/30C07C211/03C07C211/17C07C211/21C07C211/38C07C211/49C07C217/58
Inventor 张泽会周鹏刘冰姜亮
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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