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Preparation method and application of silver-modified phosphorus-tungsten oxygen cluster catalyst

A catalyst, phosphotungsten technology, applied in the directions of organic chemistry methods, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem that the catalytic activity needs to be improved, and achieve the effect of easy separation and good catalytic activity.

Active Publication Date: 2018-06-08
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of this invention is to solve the problem that the catalytic activity of simple polymetallic oxygen cluster catalysts needs to be improved in the Mannich reaction process

Method used

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  • Preparation method and application of silver-modified phosphorus-tungsten oxygen cluster catalyst
  • Preparation method and application of silver-modified phosphorus-tungsten oxygen cluster catalyst
  • Preparation method and application of silver-modified phosphorus-tungsten oxygen cluster catalyst

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Experimental program
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Effect test

Embodiment 1

[0028] Embodiment 1: compound [Ag 3 (C 14 h 11 N 5 ) 2 (DMSO) 4 ][PW 12 o 40 ] · Preparation of 2DMSO

[0029] Add the organic ligand 4,6-bis(pyridin-2-yl)pyrimidin-2-amine (0.2mmol) and 10mL dimethyl sulfoxide in sequence in a clean beaker, stir at room temperature for 30 min, add silver nitrate (0.1 mmol), magnetically stirred for 30 min, then added H 3 PW 12 o 40 (0.1mmol) reacted for 3h, after the reaction was completed, cooled to room temperature, filtered, and the filtrate was slowly evaporated at room temperature, and a block single crystal was obtained in about a week. The yield is about 26%.

Embodiment 2

[0030] Embodiment 2: compound [Ag 3 (C 14 h 11 N 5 ) 2 (DMSO) 4 ][PW 12 o 40 ] · Preparation of 2DMSO

[0031] Add organic ligand 4,6-bis(pyridin-2-yl)pyrimidin-2-amine (0.2mmol), 15mL dimethyl sulfoxide in a clean beaker, stir at room temperature for 30 min, add silver nitrate (0.2 mmol), magnetically stirred for 15 min, then added H 3 PW 12 o 40 (0.1mmol) reacted for 3h, after the reaction was completed, filtered, and the filtrate was slowly evaporated at room temperature, and a block single crystal was obtained in about a week. The yield is about 35%.

Embodiment 3

[0032] Embodiment 3: compound [Ag 3 (C 14 h 11N 5 ) 2 (DMSO) 4 ][PW 12 o 40 ] · Preparation of 2DMSO

[0033] Add the organic ligand 4,6-bis(pyridin-2-yl)pyrimidin-2-amine (0.2mmol) and 10mL dimethyl sulfoxide in sequence in a clean beaker, stir at room temperature for 30 min, add silver nitrate (0.2mmol), electromagnetically stirred for 20 minutes, then added H 3 PW 12 o 40 (0.1mmol) reacted for 4h, after the reaction was completed, filtered, and the filtrate was slowly evaporated at room temperature, and a block single crystal was obtained in about a week. The yield is about 45%.

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Abstract

The invention discloses a preparation method of a silver-modified phosphorus-tungsten oxygen cluster catalyst. According to the method, silver nitrate, an organic ligand 4,6-di(pyridine-2-yl)pyrimidine-2-amine, phosphotungstic acid and dimethyl sulfoxide are put into a beaker to react, and after the reaction is finished, filtration is carried out, and the filtrate is slowly volatilized to obtain crystals of the silver-modified phosphorus-tungsten oxygen cluster catalyst. The method provided by the invention has the characteristics of high reaction speed, simple reaction process, high purity ofan obtained product, simple post treatment and the like. Moreover, in catalysis of a one-pot reaction of phenylacetylene, formaldehyde and hexahydropyridine, the conversion rate is as high as 99%, and the selectivity is as high as 100%.

Description

technical field [0001] The invention belongs to the technical field of catalyst material preparation, and relates to a preparation method and application of a silver-modified phosphotungsten-oxygen cluster catalyst. Background technique [0002] Inorganic-organic hybrid materials have recently become a hot research field for scientists, especially the hybrid materials obtained by combining metal-oxygen clusters with organic ligands. They not only have various structures, but also have potential applications in many fields. Prospects, such as catalysis, hydrogen storage, molecular adsorption, magnetism, and photochemistry. Polyoxometalates (POMs for short) have become a well-known inorganic building block due to their excellent catalytic performance and their chemical stability, including oxidation stability, thermal stability and hydrolytic stability. As an important branch of POMs, phosphotungstate has become a very important option for constructing hybrid materials based ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/34B01J27/188C07F1/10C07D211/14
CPCB01J27/188B01J31/34B01J2231/346B01J2531/0241B01J2531/17C07B2200/13C07D211/14C07F1/005
Inventor 张海潮付明月崔传生黄现强
Owner LIAOCHENG UNIV
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