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Synthesis method of 2,2'-dipyridine by using supported bimetal nano catalyst

A bimetallic nanometer and synthesis method technology, which is applied in the synthesis field of 2,2'-bipyridine, can solve the problems of complex synthesis route of metal complex catalyst, inconsistent nature pollution, limited production and application value, etc., and achieves high catalytic performance. Activity and product selectivity, easy recovery and reuse, high production efficiency

Active Publication Date: 2016-08-17
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this method, the synthesis route of the metal complex catalyst is complex and expensive; the Ru complex catalyst used is a homogeneous catalyst, the recovery is complicated, and the industrial reuse is difficult, so the production and application value is limited
[0008] In summary, although bipyridine has many synthetic routes, chloropyridine is still produced by Uullman coupling reaction in industry, and the essential pollution of this method does not conform to the concept of modern green chemical industry

Method used

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  • Synthesis method of 2,2'-dipyridine by using supported bimetal nano catalyst
  • Synthesis method of 2,2'-dipyridine by using supported bimetal nano catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1: In-situ loading method Pd@γ-Al 2 o 3 Preparation and catalytic reaction of metal nanocatalysts

[0032] (1) Preparation of catalyst

[0033] Weigh 2.00g PdCl 2 Put it into a container, add 20mL of deionized water, stir until completely dissolved; weigh 4g of γ-Al 2 o 3 Add it to the above solution, stir for 4 hours to form a paste, dry at 75°C for 12 hours, take out the above solid and grind it evenly, and put the ground particles in a nitrogen-hydrogen mixed atmosphere (the volume ratio of nitrogen and hydrogen is 1:1) 450 ℃ activation treatment for 4h, that is, to obtain 5.03g supported metal nanocatalyst Pd@γ-Al 2 o 3 .

[0034] (2) Catalytic synthesis of 2,2'-bipyridine

[0035] Catalyst 4g and 40g pyridine prepared by step (1) are added in autoclave, with N 2 Replace the O in it 2 Finally, seal the autoclave; start the autoclave to stir, and heat to the autoclave temperature of 400 ° C; stop heating after 8 hours of reaction, until the autoclav...

Embodiment 2

[0036] Example 2: Cu@γAl in situ loading method 2 o 3 Preparation and catalytic reaction of metal nanocatalysts

[0037] (1) Preparation of catalyst

[0038] Weigh 5.34g CuCl 2 2H 2 Put O into a container, add 20mL of deionized water, stir until completely dissolved; weigh 5g of γ-Al 2 o 3 Add it to the above solution, stir for 4 hours to form a paste, dry at 75°C for 12 hours, take out the above solid and grind it evenly, and put the ground particles in a nitrogen-hydrogen mixed atmosphere (the volume ratio of nitrogen and hydrogen is 1:1) 450 ℃ activation treatment for 5h, that is, 6.89g supported metal nanocatalyst Cu@γ-Al was obtained 2 o 3 .

[0039] (2) Catalytic synthesis of 2,2'-bipyridine

[0040] Catalyst 4g and 30g pyridine prepared by step (1) are added in autoclave, with N 2 Replace the O in it 2 Finally, seal the autoclave; start the autoclave to stir, and heat to the autoclave temperature of 400 ° C; stop heating after 10 hours of reaction, until the ...

Embodiment 3

[0041] Example 3: In-situ loading method Pd-Ni@γ-Al 2 o 3 (Pd and Ni molar ratio is 2:1) preparation and catalytic reaction of bimetallic nanocatalysts

[0042] (1) Preparation of catalyst

[0043] Weigh 2.34g PdCl 2 and 1.92g Ni(NO 3 ) 2 ·6H 2 O was put into a container, added 30mL of deionized water, and stirred until completely dissolved; weighed 4g of γ-Al 2 o 3 , added to the above solution and stirred for 4 hours to form a paste, dried at 75°C for 12 hours, the above solid was taken out and ground evenly, and the ground particles were placed in a nitrogen-hydrogen mixed atmosphere (the volume ratio of nitrogen and hydrogen was 1:1) 500 After activating at ℃ for 5.5h, 5.59g of supported bimetallic nanocatalyst Pd-Ni@γ-Al was obtained 2 o 3 .

[0044] (2) Catalytic synthesis of 2,2'-bipyridine

[0045] Catalyst 5.0g and 50g pyridine prepared by step (1) are added in the autoclave, with N 2 Replace the O in it 2 Finally, seal the autoclave; start the autoclave ...

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Abstract

The invention discloses a synthesis method of 2,2'-dipyridine by using a supported bimetal nano catalyst. The method is characterized in that the supported bimetal nano catalyst M1-M2@Al2O3 is utilized to catalyze the direct coupling reaction of pyridine so as to synthesize the 2,2'-dipyridine. The supported bimetal nano catalyst M1-M2@Al2O3 uses Al2O3 as a supporter and any two different metals M1 and M2 as active components, wherein M1 and M2 are respectively and independently selected from noble metals Pd, Pt, Ru, Au, Ag and Rh, or non-noble metals Ni, Cu, Fe, Zn and Co. By using the supported bimetal nano catalyst in direct coupling production of 2,2'-dipyridine from pyridine, the method has high production efficiency, conforms to the atom economy principle in chemical industry production, does not generate any pollutant which is harmful to the environment, and thus, is a green chemical-industry intermediate production technique.

Description

1. Technical field [0001] The invention relates to a synthesis method of 2,2'-bipyridine, in particular to a method for directly coupling pyridine to synthesize 2,2'-bipyridine with a supported bimetallic nanometer catalyst. 2. Background technology [0002] As one of the isomers of bipyridine, 2,2'-bipyridine can be used as a ligand, photosensitizer, indicator for detecting metal ions, etc.; 2,2'-bipyridine is also an important intermediate in organic chemical production, For example, as a key intermediate in the production of herbicide diquat. The widely used cheap herbicide paraquat is highly toxic and has no specific antidote after human and animal poisoning, so its application is limited. Diquat herbicide is the best alternative to paraquat, and its main raw material, 2,2'-bipyridyl, determines its production cost. Therefore, the research and development of 2,2'bipyridine green production technology with high yield, low cost, good safety and low pollution will have im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/127C07D213/22B01J23/44B01J23/72B01J23/755B01J23/89
CPCC07D213/22B01J21/04B01J23/38B01J23/70B01J23/44B01J23/72B01J23/755B01J23/892B01J23/8926C07D213/127B01J37/18B01J23/002B01J23/40B01J23/60B01J23/66B01J23/80B01J23/89B01J37/0036B01J37/0201B01J37/0215B01J2523/00Y02P20/584B01J35/393B01J35/23B01J2523/31B01J2523/824B01J2523/847B01J2523/17B01J2523/821B01J2523/828
Inventor 冯乙巳王光宇姜伟伟
Owner HEFEI UNIV OF TECH
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