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Alkaline heterogeneous catalyst for nitrogen formylation reaction and preparation and application thereof

A heterogeneous catalyst and chemical reaction technology, which is applied in the preparation of organic compounds, physical/chemical process catalysts, carboxylic acid amide preparation, etc., can solve the problems of harsh reaction conditions, difficult separation of catalysts and reaction materials, and low reactivity. Achieve the effects of simple preparation method, excellent catalytic reaction performance and high stability

Active Publication Date: 2021-06-04
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

[0004] The homogeneous catalytic system has higher catalytic activity and selectivity of the target product under milder reaction conditions, but it is difficult to separate the catalyst from the reaction material
Compared with homogeneous catalysis, the biggest advantage of heterogeneous catalysis is that the catalyst and the reaction materials are easy to separate. The main problems are harsh reaction conditions and relatively low reactivity.

Method used

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  • Alkaline heterogeneous catalyst for nitrogen formylation reaction and preparation and application thereof
  • Alkaline heterogeneous catalyst for nitrogen formylation reaction and preparation and application thereof
  • Alkaline heterogeneous catalyst for nitrogen formylation reaction and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Under 298K and argon protective atmosphere, 3.0 g of three (4-vinylphenyl) phosphine and 0.95 km of noide sodium sulfonate were dissolved in 50.0 ml of tetrahydrofuran solvent, and 0.075 grams of free radical initiator poll were added to the solution. Nitrogen isobutile, stirred for 3 hours. The stirred solution was moved to a hydroelectric autoclave, and the solvent heat method was polymerized at 373K and an inert gas protection atmosphere for 24 h. After the above polymerization was cooled to room temperature, the solvent was vacuum under 333k temperature conditions, i.e., a porous organic copolymer containing triphenylphosphine and sodium sulfonate.

[0028] At 298K and inert gas protection atmosphere, 0.0156 grams of umbrella chloride (II) dimer dissolved in 40 ml of tetrahydrofuran solvent was added to 1.0 g of triphenylphosphine and sodium sulfonate were added. The porous organic copolymer is stirred for 24 hours. Subsequently, the solvent is vacuum to remove the solv...

Embodiment 2

[0030] In Example 2, in addition to weighing 0.078 grams of umbrella chloride (II) dimer replacing 0.0156 grams of umbrella chloride (II) dimer, the remaining catalyst preparation process and implementation Example 1 is the same.

Embodiment 3

[0032] In Example 3, in addition to weighing 0.03 g of palladium palladium alternative 0.0156 grams of an umbrella chloride (II) dimer, the remaining catalyst preparation process was the same as in Example 1.

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Abstract

The invention relates to an alkaline heterogeneous catalyst and a preparation method and application thereof, in particular to an alkaline heterogeneous catalyst applied to a nitrogen formylation reaction, which comprises a metal component and an organic ligand copolymer, and the organic ligand copolymer is a copolymer which is generated through solvothermal copolymerization of a phosphine ligand containing vinyl functionalization and an organic alkali monomer containing vinyl functionalization and has a large specific surface area and a hierarchical pore structure. On one hand, organic alkali is introduced into the copolymer carrier, so that the solid heterogeneous catalyst has alkalinity, the forward movement of nitrogen formylation reaction is promoted, and the reaction activity is improved; and on the other hand, the metal components and P atoms of the copolymer carrier are highly dispersed and stably exist on the carrier due to coordination. Therefore, the alkaline heterogeneous catalyst provided by the invention has excellent nitrogen formylation reaction performance and stability; and the catalyst is easy to separate from reactants and products, and has a wide industrial application prospect.

Description

Technical field [0001] The present invention relates to an alkaline polyhase catalyst and a preparation method and application thereof for a nitrogenation reaction, and is a multi-phase catalytic technology. Background technique [0002] The formation reaction of the amine is one of the most organic synthesis and medical chemistry. The formamide is an organic synthesis important intermediate and is widely used in synthesizing various drugs. The formamide can be used as an organic synthetic raw material, a paper treatment agent, a softener of the fiber industry, can also be used as an analytical reagent for measuring the amino acid content of the rice; and the formamide is also an advantal organic solvent, which can be used for separating chlorosilane, purifying oil. Further, in addition, the formation of the formamide has a lively reactivity, and a variety of reactions can occur, except for three hydrogen participation in reaction, dehydration, de-removal CO, introduction of amin...

Claims

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Application Information

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IPC IPC(8): B01J31/24B01J35/10C07B43/06C07C231/10C07C233/03C07D295/185
CPCB01J31/1691B01J31/2409C07B43/06C07C231/10C07D295/185B01J2531/821B01J2531/824B01J2531/847B01J2540/32B01J35/60B01J35/617C07C233/03
Inventor 丁云杰王国庆严丽姜淼程显波
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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