Selective ammoniation hydrogenation catalyst, preparation method thereof and synthesis method of hexamethyleneimine

A technology of hydrogenation catalyst and synthesis method, which is applied in the direction of catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., and can solve the problem of rising product cost and high cost of cycloheximide , high price of caprolactam, etc., to achieve the effect of mild reaction conditions and good economic benefits

Pending Publication Date: 2022-05-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, caprolactam is expensive, resulting in higher cost of final product cycloheximide
On t

Method used

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  • Selective ammoniation hydrogenation catalyst, preparation method thereof and synthesis method of hexamethyleneimine
  • Selective ammoniation hydrogenation catalyst, preparation method thereof and synthesis method of hexamethyleneimine
  • Selective ammoniation hydrogenation catalyst, preparation method thereof and synthesis method of hexamethyleneimine

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Experimental program
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Embodiment approach

[0026] In the first embodiment of the selective ammoniation hydrogenation catalyst provided by the present invention, based on the total weight of the catalyst, in terms of metal, the catalyst contains 88wt%-99.9wt% of Ni, 0.01-10wt% of the first A modifying metal component and 0-2 wt% of a second modifying metal component.

[0027] Preferably, the selective hydrogenation hydrogenation catalyst contains 0.02-5wt% Sn.

[0028] Preferably, 0.02-2 wt% of a second modifying metal component is also contained.

[0029] Preferably, the second modifying metal component is Pd.

[0030] The preparation method of the first embodiment of the selective ammoniation hydrogenation catalyst comprises:

[0031] a) adding NiAl alloy to NaOH and / or KOH aqueous solution to dissolve Al in the alloy to obtain Ni solid powder;

[0032] b) separating the Ni solid powder in step a) and dispersing it into a low-carbon alcohol, adding a soluble Sn salt and an optional second modified metal component p...

Embodiment 1

[0068] Catalyst A preparation method is as follows:

[0069] a) adding 10g of NiAl alloy to 20wt% NaOH aqueous solution to dissolve Al in the alloy to obtain 5g of Ni solid powder;

[0070] b) washing the solid powder prepared in step a) with ethanol or water;

[0071] c) Disperse the solid powder in b) into 20ml of ethanol, add SnCl containing 0.2g of tin 2 ;

[0072] d) Add 0.4gNaBH 4 reducing c) the mixture;

[0073] e) washing the solid obtained in d) with ethanol, which is catalyst A.

[0074] The composition of the catalyst A is as follows: the content of Ni is 96wt%, and the content of Sn is 4wt%.

Embodiment 2

[0076] Catalyst B preparation method is as follows:

[0077] a) adding 10g of NiAl alloy to 20wt% NaOH aqueous solution to dissolve Al in the alloy to obtain 5g of Ni solid powder;

[0078] b) washing the solid powder prepared in step a) with ethanol or water;

[0079] c) Disperse the solid powder in b) into 20ml of ethanol, add SnCl containing 0.5g of tin 4 , and palladium acetylacetonate containing Pd 0.01g;

[0080] d) reducing the solid obtained in c) at 70 degrees under 1MPa hydrogen pressure;

[0081] e) washing the solid obtained in d) with ethanol, which is catalyst B.

[0082] The composition of the catalyst B is as follows: the content of Ni is 90.8wt%, the content of Sn is 9wt%, and the content of Pd is 0.2wt%.

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Abstract

The invention relates to a selective ammoniation hydrogenation catalyst, a preparation method thereof and a synthesis method of cycloheximine, the selective ammoniation hydrogenation catalyst comprises an active metal Ni, 0.01-10 wt% of a first modified component Sn, an optional heat-resistant inorganic oxide carrier and an optional second modified metal component, and the second modified metal component is selected from one or more of Pt, Ag, Pd, Co and Cu. According to the synthesis method of the cycloheximine, provided by the invention, adipic dialdehyde and adipic dialdehyde acetal are used as reaction raw materials, so that the reaction raw materials are cheaper and easier to obtain, the reaction conditions are milder, and better economic benefits are achieved.

Description

technical field [0001] The invention relates to the field of chemical synthesis, more specifically, to a selective ammoniation hydrogenation catalyst and a method for synthesizing cycloheximide. Background technique [0002] Cyclohexyl imine is an important organic compound. Such compounds can be combined with aluminum alkyls to form organometallic compounds. In addition, the special ring structure of cycloheximide and its derivatives also make it an important pharmaceutical intermediate. In addition, cycloheximide is also used to prepare special ionic liquids. For example, CN102146058A discloses an ionic liquid using imine nitrogen-containing heterocyclic rings as cations and a preparation method of the ionic liquid. The sulfonic acid ionic liquid prepared by using cyclohexyl imine has good catalytic activity for acid-catalyzed esterification reaction and the like. CN102516203A discloses an ionic liquid solid acid synthesized from cycloheximide and heteropolyacid radica...

Claims

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Application Information

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IPC IPC(8): B01J23/835B01J23/89B01J37/18B01J37/02C07D295/023C07D295/027
CPCB01J23/835B01J23/8966B01J37/18B01J37/0201C07D295/023C07D295/027Y02P20/584
Inventor 刘凌涛王海京宗保宁毛俊义朱振兴罗一斌张同旺朱丙田韩颖
Owner CHINA PETROLEUM & CHEM CORP
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