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Preparation method for manganese dioxide composite catalyst and synthetic method for 2-pyridylaldehyde

A composite catalyst, manganese dioxide technology, used in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem that the catalyst cannot be recycled, pollutes the environment, is easy to pass Oxidation and other problems, to achieve the effect of cost saving, low reaction cost and no environmental pollution

Active Publication Date: 2015-03-11
ANHUI XINGYU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the problems in the prior art that the catalyst cannot be recycled, pollutes the environment, and is easily overoxidized, the present invention provides a method for preparing a manganese dioxide composite catalyst and a method for synthesizing 2-pyridylaldehyde, which can be fixed on attapulgite. MnO 2 As a catalyst, 2-pyridinecarbaldehyde is obtained by oxidation of 2-pyridinemethanol, and the reaction yield is high. After the reaction, the catalyst can be recycled by magnetic precipitation method, which does not pollute the environment and save costs, and is suitable for industrial applications

Method used

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  • Preparation method for manganese dioxide composite catalyst and synthetic method for 2-pyridylaldehyde

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Embodiment 1

[0038] Such as figure 1 and figure 2 as shown,

[0039] A kind of preparation method of manganese dioxide composite catalyst, its steps are:

[0040] (1) Mix the attapulgite mineral powder and deionized water at a mass ratio of 1:4, stir for 40 minutes, then let it stand for 2 hours, discard the supernatant liquid and the lower layer of sand, and obtain the suspension of attapulgite. The attapulgite obtained after liquid centrifugation is placed in an oven and dried at 80°C for subsequent use;

[0041] (2) Mix the attapulgite obtained in the above steps with 2.5mol / L sulfuric acid solution at a mass ratio of 1:3, stir at 80°C for 1 hour, then cool to room temperature, rinse with deionized water until neutral, and drying and grinding in an oven at 80°C, passing through a 200-mesh sieve to obtain acid-modified attapulgite;

[0042] (3) Add the acid-modified attapulgite obtained in the above steps into 0.15mol / L potassium permanganate solution, the mass ratio of potassium pe...

Embodiment 2

[0054] A kind of preparation method of manganese dioxide composite catalyst, its steps are:

[0055] (1) Mix the attapulgite mineral powder and deionized water at a mass ratio of 1:4, stir for 40 minutes, then let it stand for 2 hours, discard the supernatant liquid and the lower layer of sand, and obtain the suspension of attapulgite. The attapulgite obtained after liquid centrifugation is placed in an oven and dried at 80°C for subsequent use;

[0056] (2) Mix the attapulgite obtained in the above steps with 2.5mol / L sulfuric acid solution at a mass ratio of 1:3, stir at 80°C for 1 hour, then cool to room temperature, rinse with deionized water until neutral, and drying and grinding in an oven at 80°C, passing through a 200-mesh sieve to obtain acid-modified attapulgite;

[0057] (3) Add the acid-modified attapulgite obtained in the above steps into 0.25mol / L potassium permanganate solution, the mass ratio of potassium permanganate solution to attapulgite is 2.5:1, at 40°C ...

Embodiment 3

[0069] A kind of preparation method of manganese dioxide composite catalyst, its steps are:

[0070] (1) Mix the attapulgite mineral powder and deionized water at a mass ratio of 1:4, stir for 40 minutes, then let it stand for 2 hours, discard the supernatant liquid and the lower layer of sand, and obtain the suspension of attapulgite. The attapulgite obtained after liquid centrifugation is placed in an oven and dried at 80°C for subsequent use;

[0071] (2) Mix the attapulgite obtained in the above steps with 2.5mol / L sulfuric acid solution at a mass ratio of 1:3, stir at 80°C for 1 hour, then cool to room temperature, rinse with deionized water until neutral, and drying and grinding in an oven at 80°C, passing through a 200-mesh sieve to obtain acid-modified attapulgite;

[0072] (3) Add the acid-modified attapulgite obtained in the above steps into 0.30mol / L potassium permanganate solution, the mass ratio of potassium permanganate solution to attapulgite is 2:1, at 40°C S...

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Abstract

The invention discloses a preparation method for manganese dioxide composite catalyst and a synthetic method for 2-pyridylaldehyde, and belongs to the field of organic synthesis. The preparation method comprises the following steps: firstly, loading potassium permanganate to acid-modified attapulgite to obtain MnO4<->-attapulgite; secondly, loading Fe3O4 to the MnO4<->-attapulgite by a coprecipitation method, and roasting to obtain the MnO2 composite catalyst with high catalytic activity. According to the preparation method, the catalytic advantages of MnO2 are successfully combined with the quick separation advantages of the attapulgite-Fe3O4 magnetic material, so that MnO2 in the catalyst can be recycled; when the MnO2 composite catalyst is used for preparing 2-pyridylaldehyde, the reaction yield is high, the conditions are mild, and the catalyst can be separated from reaction liquid through a magnetic sedimentation method and recycled after the reaction is finished. The preparation method has the advantages of little environmental pollution, low reaction cost and the like, and is suitable for industrialized application.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of a pharmaceutical intermediate, more specifically, a preparation method of a manganese dioxide composite catalyst and a synthesis method of 2-pyridinecarbaldehyde. Background technique [0002] 2-Pyridinecarbaldehyde is an intermediate of the laxative bisacodyl (bisacody1), and is also widely used as a raw material for fine organic synthesis. There are many kinds of 2-pyridinecarbaldehyde synthesis routes reported in the literature, but they are mainly based on two different starting materials. Obtain 2-pyridine formaldehyde (Huang Shengtang, Huang Wenlong, Zhang Huibin. The improvement of 2-pyridine formaldehyde synthetic technique [J]. Chemical Reagent, 2005,27 (1): 58); - Oxidation, rearrangement, hydrolysis and then oxidation to prepare 2-pyridinecarbaldehyde (Shan Shiming, Yu Shuqin, Liao Hong, etc. Synthesis of 2-pyridinecarbaldehyde [J]....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/889C07D213/48
CPCY02P20/584
Inventor 张宽宇金文艺丁亮李静张升
Owner ANHUI XINGYU CHEM
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