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Raney nickel catalytic preparation method of 2,2'-bipyridine

A catalytic preparation, Raney nickel technology, applied in the direction of organic chemistry, etc., can solve the problems of staying, unable to achieve large-scale production, low reaction yield, etc., to avoid waste, good economic and social benefits, and simple operation. Effect

Inactive Publication Date: 2016-04-06
安徽千和新材料科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2004, Chen Jiang of Zhejiang University of Technology reported (Chen Jiang. Synthesis of the herbicide diquat and its intermediates [D]. Hangzhou: Zhejiang University of Technology, 2004: 19-45) Raney nickel production 2,2 The production technique of '-bipyridine, it is to be raw material with pyridine, carries out heterogeneous reaction under the catalysis of Raney nickel, but this technique only stops at the theoretical research stage, and the yield of reaction is not high (7~11%), cannot Realize continuous large-scale production

Method used

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  • Raney nickel catalytic preparation method of 2,2'-bipyridine
  • Raney nickel catalytic preparation method of 2,2'-bipyridine

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: first add 1000Kg pyridine into the evaporator, and then add 150Kg activated Raney nickel catalyst into the reactor. Slowly heat the pyridine in the evaporator to 115°C, the pyridine vapor rises to the cooling tower to become liquid droplets and flows back into the reactor, the liquid level in the reactor rises gradually, turn on the stirrer and heating mantle of the reactor, adjust The temperature of the heating mantle is 110-113°C. After the reaction was carried out for 15 hours, add 20Kg of Raney nickel catalyst to the reactor and continue the reaction for 10 hours; then add 15Kg of Raney nickel catalyst to the reactor and continue the reaction for 8 hours to stop. The reaction liquid was distilled under reduced pressure, 800Kg of petroleum ether was added to the distillation residue and the temperature in the kettle was lowered to 45°C, then the petroleum ether mixture was filtered, and the filtrate was distilled to dryness to obtain 627.5Kg of 2,2'-bip...

Embodiment 2

[0020] Example 2: First add 1300Kg of pyridine to the evaporator, and then add 220Kg of activated Raney nickel catalyst into the reactor. Slowly heat the pyridine in the evaporator to 115°C, the pyridine vapor rises to the cooling tower to become liquid droplets and flows back into the reactor, the liquid level in the reactor rises gradually, turn on the stirrer and heating mantle of the reactor, adjust The temperature of the heating mantle is 112-114°C. After the reaction was carried out for 15 hours, 22Kg of Raney nickel catalyst was added to the reactor, and the reaction was continued for 10 hours. Add 20Kg of Raney nickel catalyst to the reactor again, continue to react for 8.5h and stop. The reaction liquid was distilled under reduced pressure, 1000Kg petroleum ether was added to the distillation residue and the temperature in the kettle was lowered to 40°C, then the petroleum ether mixture was filtered, and the filtrate was distilled to dryness to obtain 710.5Kg 2,2'-bi...

Embodiment 3

[0021] Example 3: 1700Kg of pyridine was first added to the evaporator, and 300Kg of activated Raney nickel catalyst was added into the reactor. Slowly heat the pyridine in the evaporator to 115°C, the pyridine vapor rises to the cooling tower to become liquid droplets and flows back into the reactor, the liquid level in the reactor rises gradually, turn on the stirrer and heating mantle of the reactor, adjust The temperature of the heating mantle is 113-114°C. After the reaction was carried out for 15 hours, 32Kg of Raney nickel catalyst was added to the reactor, and the reaction was continued for 10 hours. Add 30Kg of Raney nickel catalyst to the reactor again, continue to react for 8h and stop. The reaction liquid was distilled under reduced pressure, 1500Kg of petroleum ether was added to the distillation residue and the temperature in the kettle was lowered to 43°C, then the petroleum ether mixture was filtered, and the filtrate was distilled to dryness to obtain 1170.4K...

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Abstract

The invention discloses a Raney nickel catalytic preparation method of 2,2'-bipyridine and belongs to the technical field of organic synthesis. The method comprises the following steps: pretreating raw materials to make purity of pyridine reach 99.8 wt% and above, carrying out dehydrogenation activation on a Raney nickel catalyst, and carrying out catalytic dehydrogenation coupled reaction, extraction separation and distillation purification so as to obtain 2,2'-bipyridine. Purity content is below 3 wt%. By reasonably combining soxhlet extraction principle and fluidized-bed process, timely separation of the product and the catalyst can be effectively guaranteed, service life of the catalyst is prolonged, side reaction can be reduced, and product purity is ensured. The method is clean and environmentally friendly. All solvents, including pyridine which hasn't participated in the reaction, can be recycled. The method is pollution-free to the environment. Waste of raw materials is avoided. The method has remarkably economic and social benefits.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a Raney nickel-catalyzed preparation method of 2,2'-bipyridine. Background technique [0002] 2,2'-Bipyridine is one of the isomers of bipyridine. Its appearance is white or light pink crystalline powder, with a melting point of 69.7°C and a boiling point of 272-273°C. It is a bidentate chelating ligand that can form complexes with many metal ions, so it can be used as a redox indicator. It also has many applications in the preparation of pharmaceutical and pesticide intermediates. For example, it is also an intermediate product of "Diquat" herbicide. In addition, the complexes with ruthenium and platinum have strong luminescent properties, and can be used as important organic materials in optoelectronics, and have great potential application value. [0003] The market prospect of 2,2'-bipyridine is broad. At present, the domestic production process mainly...

Claims

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Application Information

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IPC IPC(8): C07D213/22C07D213/127
CPCC07D213/127C07D213/22
Inventor 张千峰王猛陈向莹刘凤兰
Owner 安徽千和新材料科技发展有限公司
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