Tetramethylammonium dizinc-vanadium oxygen-cluster catalyst as well as preparation method and application thereof

A technology of tetramethylammonium and tetramethylammonium hydroxide is applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. There are problems such as halogen, and the effect of simple preparation method is achieved

Inactive Publication Date: 2017-05-24
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of this invention is to catalyze the problems such as the presence of halogens

Method used

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  • Tetramethylammonium dizinc-vanadium oxygen-cluster catalyst as well as preparation method and application thereof
  • Tetramethylammonium dizinc-vanadium oxygen-cluster catalyst as well as preparation method and application thereof
  • Tetramethylammonium dizinc-vanadium oxygen-cluster catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

specific example 1

[0034] Specific example 1: compound [Zn(H 2 O) 6 ] 2 [(CH 3 ) 4 N] 2 V 10 o 28 2H 2 Preparation of O

[0035] In a clean beaker, add vanadium pentoxide (10mmol), tetramethylammonium hydroxide (10mmol), Zn(OAc) 2 (4mmol) and 15mL water, stirred vigorously for 12h, then raised the temperature to 40°C, reacted for 60min, cooled to room temperature after the reaction, filtered, stood still, the filtrate volatilized slowly, and a red substance was obtained after 4-5 days. The yield is about 63%.

specific example 2

[0036] Specific example 2: compound [Zn(H 2 O) 6 ] 2 [(CH 3 ) 4 N] 2 V 10 o 28 2H 2 Preparation of O

[0037] In a clean beaker, add vanadium pentoxide (15mmol), tetramethylammonium hydroxide (20mmol), Zn(OAc) 2 (6mmol) and 20mL water, stirred vigorously for 16h, then raised the temperature to 70°C, reacted for 100min, cooled to room temperature after the reaction, filtered, stood still, the filtrate slowly evaporated, and a red substance was obtained after 4-5 days. The yield is about 67%.

specific example 3

[0038] Specific example 3: compound [Zn(H 2 O) 6 ]2 [(CH 3 ) 4 N] 2 V 10 o 28 2H 2 Preparation of O

[0039] In a clean beaker, add vanadium pentoxide (12mmol), tetramethylammonium hydroxide (16mmol), Zn(OAc) 2 (5mmol) and 10mL of water, stirred vigorously for 12h, then heated up to 40°C, reacted for 60minmin, cooled to room temperature after the reaction, filtered, stood still, the filtrate slowly evaporated, and a red substance was obtained after 4-5 days. The yield is about 58%.

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Abstract

The invention discloses a preparation method of a tetramethylammonium dizinc-dcavanadium oxygen-cluster single-component catalyst. Such a method comprises the following steps of putting zinc acetate, vanadium pentoxide, tetramethylammonium hydroxide and water into a beaker to carry out a reaction, after the reaction is finished, carrying out filtration, and slowly volatilizing filtrate, so as to obtain a crystal of the tetramethylammonium dizinc-dcavanadium oxygen-cluster single-component catalyst. The method provided by the invention has the advantages that a reaction speed is quick, a reaction process is simple, an obtained product is high in purity, and the post treatment is simple. In a cycloaddition reaction of carbon dioxide, the conversation ratio is up to 94.7 percent, and the selectivity is up to 95.6 percent.

Description

technical field [0001] The invention belongs to the technical field of catalyst material preparation, and relates to the preparation technology of tetramethylammonium dizinc-decavanadium oxygen cluster catalyst. [0002] technical background [0003] Polymetallic oxygen clusters are a class of polymetallic oxygen cluster compounds containing transition elements such as molybdenum, tungsten, vanadium, niobium and tantalum. The rich metal composition and electron-rich effect of polymetallic oxygen clusters determine their strong acidity and strong oxidative properties, so polymetallic oxygen cluster compounds exhibit excellent catalytic properties in many organic synthesis reactions. At present, the catalytic chemistry of polymetallic oxygen clusters has become one of the most promising research directions in the field of polymetallic oxygen cluster science, and has attracted extensive attention from chemists. [0004] Meanwhile, it is well known that carbon dioxide is a typic...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J31/16B01J31/36C07D317/36
CPCB01J31/0239B01J31/16B01J31/36B01J2531/26C07D317/36
Inventor 赫庆鹏任永和闫新宇孟德武黄现强
Owner LIAOCHENG UNIV
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