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Preparation method of 2, 2'-bipyridine

A bipyridine and pyridine technology, which is applied in the field of bipyridine preparation, can solve the problems of easy spontaneous combustion of Raney nickel, environmental hazards, and difficult operation control, and achieve the effects of low equipment requirements, environmental friendliness, and safe operation

Active Publication Date: 2017-06-06
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

But there are following problems: the raw material is expensive (the synthesis of 2-chloropyridine is more difficult); in addition, due to the high corrosiveness of halogen-containing reactants, special reaction equipment must be used, and environmental hazards are brought
As for the previous preparation method using Raney nickel as a catalyst, because Raney nickel is very easy to spontaneously combust, it is difficult to control the operation during the preparation process, and there are potential safety hazards

Method used

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  • Preparation method of 2, 2'-bipyridine
  • Preparation method of 2, 2'-bipyridine
  • Preparation method of 2, 2'-bipyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Weigh 100g 5wt% Ni / γ-Al 2 o 3 The catalyst was placed in a quartz tube, reduced by passing hydrogen for 6 hours at 450°C, and purging by passing nitrogen for 3 hours at the same temperature, and then continuing to pass nitrogen and cooling down to room temperature. Add the reduced catalyst into a 500mL glass three-necked flask, connect a 200mL separatory funnel with one side opening, close the middle opening, and connect the other side opening with a water pump for vacuuming. After evacuating for 2 hours, the pipeline connecting the three-necked flask and the water pump was cut off. Measure 200mL of pyridine into a 200mL separatory funnel, and add pyridine into the three-necked flask. After the addition was complete, the middle opening of the three-necked flask was connected to a condensing reflux tube. Heat the three-necked flask to 110°C, and cool the three-necked flask to 60°C after 12 hours of reflux reaction. Pour the reacted mixture into a vertical fusing glas...

Embodiment 2

[0050] Weigh 100g 10wt% Ni / γ-Al 2 o 3The catalyst was placed in a quartz tube, and reduced by passing hydrogen for 6 hours at 480°C, and purging by passing nitrogen for 3 hours at the same temperature, and then continuing to pass nitrogen and cooling down to room temperature. Add the reduced catalyst into a 500mL glass three-necked flask, connect a 200mL separatory funnel with one side opening, close the middle opening, and connect the other side opening with a water pump for vacuuming. After evacuating for 2 hours, the pipeline connecting the three-necked flask and the water pump was cut off. Measure 200mL of pyridine into a 200mL separatory funnel, and add pyridine into the three-necked flask. After the addition was complete, the middle opening of the three-necked flask was connected to a condensing reflux tube. Heat the three-necked flask to 115°C, and cool the three-necked flask to 60°C after reflux reaction for 24 hours. Pour the reacted mixture into a vertical fusing...

Embodiment 3

[0052] Weigh 100g 20wt% Ni / γ-Al 2 o 3 The catalyst was placed in a quartz tube and reduced by flowing hydrogen at 480°C for 8 hours, and then purging with nitrogen for 3 hours at the same temperature, then continuing to pass nitrogen and cooling down to room temperature. Add the reduced catalyst into a 500mL glass three-necked flask, connect a 200mL separatory funnel with one side opening, close the middle opening, and connect the other side opening with a water pump for vacuuming. After evacuating for 2 hours, the pipeline connecting the three-necked flask and the water pump was cut off. Measure 200mL of pyridine into a 200mL separatory funnel, and add pyridine into the three-necked flask. After the addition was complete, the middle opening of the three-necked flask was connected to a condensing reflux tube. Heat the three-necked flask to 120°C, and cool the three-necked flask to 60°C after 48 hours of reflux reaction. Pour the reacted mixture into a vertical fusing glass...

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Abstract

The invention relates to a preparation method of bipyridine, in particular to a preparation method of 2, 2'-bipyridine. The method includes: taking pyridine as the raw material, adopting supported nickel as the catalyst, carrying out dehydrogenation coupling reaction on pyridine under certain conditions, then conducting filtration, distillation, washing, chromatography, recrystallization and other separation steps to purify the product, thus obtaining a 2, 2'-bipyridine product. Compared with the traditional direct coupling method and halogen method, the method provided by the invention is safe and convenient for operation, and is environment-friendly.

Description

technical field [0001] The invention relates to a preparation method of bipyridine, in particular to a preparation method of 2,2'-bipyridine. Background technique [0002] There are six isomers of bipyridine, namely 2,2'-, 3,3'-, 4,4'-, 2,3'-, 2,4'- and 3,4'-bipyridine. Among them, the more common and widely used ones are 2,2'- and 4,4'-bipyridine. Its main uses include the following two aspects: 1. It is used in organic synthesis and pharmaceutical intermediates; 2. It is used as an analytical reagent for the determination of ferrous, silver, cadmium, and molybdenum ions. At present, its main use is as an intermediate for the production of herbicides, such as 2,2'-bipyridine and 4,4'-bipyridine as "diquat" ( ) and “paraquat” ( ) intermediates. [0003] Herbicides have always been the most active part of the world pesticide market. Paraquat is currently the second-largest herbicide in the world's market share, but due to the fact that it has no effective antidote when...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/22C07D213/127
Inventor 王从新田志坚李科达李鹏马怀军曲炜徐仁顺潘振栋王冬娥
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI