Catalyst for preparing 2,2'-bipyridine by pyridine coupling and preparation method and application thereof

A catalyst, bipyridine technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as catalyst failure and reaction yield decline, and achieve good stability, high activity, high Effects of activity and stability

Pending Publication Date: 2020-02-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method still uses pyridine and Raney nickel catalysts, and the reaction temperature is controlled between 200-240°C (in the experiment, it is best to carry o

Method used

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  • Catalyst for preparing 2,2'-bipyridine by pyridine coupling and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The spherical alumina carrier containing 3.0% silica is treated with one or more solutions of about 3% oxalic acid, nitric acid, sulfuric acid and hydrochloric acid at 80°C, then washed 1-2 times with water, and dried at 120°C. Calcined at 650°C for 3 hours to obtain a catalyst carrier;

[0021] According to the content of the active component nickel, nickel nitrate and polyvinylpyrrolidone were dissolved in water to form a solution. After vacuuming the modified alumina carrier, the impregnation solution was sucked into the carrier by conventional impregnation method, and then aged at 80 °C 2 hours, drying at 80°C for 6 hours, drying at 120°C for 12 hours, and calcination at 450°C for 3 hours; the calcined catalyst was reduced by passing hydrogen at 550°C for 5 hours.

[0022] Catalyst A prepared in this example contains 21% nickel, and 5% polyvinylpyrrolidone is added to the impregnation solution.

Embodiment 2

[0024] Catalyst B is prepared in the same manner as in Example 1, except that the nickel content of the catalyst is 25%, and 2% cetyltrimethylammonium bromide (CTAB) and 3% polyvinylpyrrolidone (PVP) are added in the impregnation solution. ).

Embodiment 3

[0026] Catalyst C was prepared in the same manner as in Example 1, except that the nickel content of the catalyst was 30%, and 5% polyvinylpyrrolidone (PVP) was added to the impregnation solution.

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PUM

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Abstract

The invention provides a catalyst for preparing 2,2'-bipyridine by pyridine coupling and a preparation method and application thereof. The catalyst takes nickel as a main active component, and macroporous alumina modified by one or more of silica, oxalic acid, nitric acid, sulfuric acid and hydrochloric acid as a carrier, and adopts a conventional impregnation method to prepare the nickel/aluminacatalyst. During impregnation, L-arginine, cetyltrimethylammonium bromide (CTAB), polyvinylpyrrolidone (PVP) and the like are added to promote metal dispersion. The catalyst can be used to realize continuous reaction for preparing the 2,2'-bipyridine by pyridine coupling in a fixed bed reactor.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a catalyst for preparing 2,2'-bipyridine through pyridine coupling, a preparation method and an application thereof. Background technique [0002] 2,2'-Bipyridine is an important fine chemical and drug synthesis intermediate, at the same time, it is also a unique chelating agent, used to detect metal ion indicators, photosensitizers and ligands for metal organic catalysts, etc. . Especially in recent years, with the prohibition of the highly toxic herbicide paraquat, the synthesis and production of the less toxic herbicide diquat will be put on an important agenda. The main raw material for the synthesis of diquat is 2,2'-bipyridine. Therefore, this product has important social significance and industrial application prospects for the development of pyridine downstream products, especially the development and production of low-toxicity pesticides. [0003]...

Claims

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Application Information

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IPC IPC(8): B01J23/755C07D213/127C07D213/22
CPCB01J23/755B01J35/0066B01J37/0018B01J37/0207C07D213/127C07D213/22
Inventor 王玉忠刘盛林徐龙伢朱向学李秀杰谢素娟陈福存张爽
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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