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Cycloheximine synthesis method, adipic dialdehyde selective ammoniation hydrogenation catalyst and preparation method of adipic dialdehyde selective ammoniation hydrogenation catalyst

A technology of cyclohexyl imine 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 high cost of cyclohexyl imine and the price of caprolactam Expensive and other issues, to achieve the effect of good catalytic effect and easy preparation

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

Method used

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  • Cycloheximine synthesis method, adipic dialdehyde selective ammoniation hydrogenation catalyst and preparation method of adipic dialdehyde selective ammoniation hydrogenation catalyst
  • Cycloheximine synthesis method, adipic dialdehyde selective ammoniation hydrogenation catalyst and preparation method of adipic dialdehyde selective ammoniation hydrogenation catalyst
  • Cycloheximine synthesis method, adipic dialdehyde selective ammoniation hydrogenation catalyst and preparation method of adipic dialdehyde selective ammoniation hydrogenation catalyst

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preparation example Construction

[0039] A preparation method for adipaldehyde selective ammoniation hydrogenation catalyst, comprising the following steps:

[0040] a) using an impregnation method to impregnate the precursor salt of Ru and the modified metal component on the carrier;

[0041] b) drying the impregnated mixture in step a) at 100-130 degrees;

[0042] c) using hydrogen to reduce the solid obtained in step b) at 300-500 degrees;

[0043] The precursor salt of Ru and the modified metal component is a nitrate or chloride salt of Ru and the modified metal component; the carrier is selected from alumina, zirconia, magnesium oxide, titanium dioxide, niobium oxide and oxide One or a mixture of vanadium.

[0044] In the preparation method of the catalyst provided by the present invention, wherein the weight ratio of the Ru precursor salt, the modified metal precursor salt and the carrier is such that in the prepared catalyst, based on the total weight of the catalyst, in terms of metal, The content o...

Embodiment 1

[0051] Catalyst A preparation method is as follows:

[0052] a) RuCl containing 0.1g of Ru 3 and AgNO containing Ag0.02g 3Dissolve in 20ml aqueous solution, impregnate equal volume into 5g carrier Al 2 o 3 superior;

[0053] b) drying the impregnated mixture in step a) at 110°C;

[0054] c) The solid obtained in the hydrogen reduction step b) at 420 degrees is the catalyst A.

[0055] The composition of the catalyst is: the content of Ru is 2wt%, the content of Ag is 0.4wt%, and the rest is Al 2 o 3 .

Embodiment 2

[0057] Catalyst B preparation method is as follows:

[0058] a) RuCl containing 0.1g of Ru 3 and Cu(NO 3 ) 2 Dissolve in 20ml aqueous solution, impregnate equal volume into 10g carrier Al 2 o 3 superior;

[0059] b) drying the impregnated mixture in step a) at 120 degrees;

[0060] c) The solid obtained in the hydrogen reduction step b) at 400 degrees is the catalyst B.

[0061] The composition of the catalyst is: the content of Ru is 10wt%, the content of Cu is 2wt%, and the rest is Al 2 o 3 .

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Abstract

The invention relates to a synthesis method of cycloheximine, an adipic dialdehyde selective ammoniation hydrogenation catalyst and a preparation method thereof, in the presence of a Ru-containing supported catalyst, adipic dialdehyde, adipic dialdehyde monoacetal or adipic dialdehyde diacetal, hydrogen and ammonia react to generate the cycloheximine, the reaction temperature is 100-300 DEG C, and the pressure is 0.5-10 MPa. The selective ammoniation hydrogenation catalyst is composed of an active metal Ru, a metal oxide carrier and a modified metal component, and the modified metal component is selected from one or more of Pt, Ag, Pd, Co, Cu and Sn. According to the method provided by the invention, adipic dialdehyde and adipic dialdehyde acetal are adopted as reaction raw materials which are cheaper and easier to obtain, and the reaction conditions are milder, so that the method has better economic benefits.

Description

technical field [0001] The invention relates to the field of synthesis of cyclohexyl imine, and discloses a method for catalytically synthesizing cyclohexyl imine from adipaldehyde, its acetal and ammonia. 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 heteropoly...

Claims

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Application Information

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IPC IPC(8): C07D223/04B01J23/46B01J23/89B01J23/50B01J37/02B01J37/18
CPCC07D223/04B01J23/462B01J23/8913B01J23/8926B01J23/8966B01J23/894B01J23/898B01J23/50B01J37/0201B01J37/18Y02P20/584
Inventor 刘凌涛王海京宗保宁毛俊义朱振兴罗一斌袁清
Owner CHINA PETROLEUM & CHEM CORP
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