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Palladium catalyst for synthesizing oxalate using liquid phase coupling method and use thereof

A catalyst and oxalate technology, which is applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, carbon monoxide or formate reaction preparation, etc. It can solve the problem of difficult product separation and catalyst synthesis of catalysts The problems of low yield and short catalyst life are achieved, and the effects of high selectivity, long catalyst life and high reaction yield are achieved.

Inactive Publication Date: 2008-11-19
HUAZHONG UNIV OF SCI & TECH +1
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to study a kind of high activity and high selectivity N-N A palladium complex catalyst with bidentate ligands, the catalyst is used in the synthesis of nitrite and CO liquid-phase catalytic coupling reaction, the reaction formula is as follows:

Method used

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  • Palladium catalyst for synthesizing oxalate using liquid phase coupling method and use thereof
  • Palladium catalyst for synthesizing oxalate using liquid phase coupling method and use thereof
  • Palladium catalyst for synthesizing oxalate using liquid phase coupling method and use thereof

Examples

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Effect test

example 1

[0024] Pd(phen)Cl 2 (Phen is 1,10-phenanthroline) preparation

[0025] 1gPdCl 2 Mix with 1.5mL of 36% concentrated hydrochloric acid and 40mL of water, heat until dissolved, add 0.84g of KCl crystals in boiling state, continue to stir the reaction solution for 2h, cool, concentrate, and precipitate crystals to obtain K 2 PdCl 4 About 1.0g. Contains 5.6mmolK in 20mL 2 PdCl 4 To the aqueous solution, 20 ml of ethanol solution containing 5.6 mmol of phen was added to adjust the pH value to 4.47, and the reaction was stirred at 40° C. for 1 h to obtain a yellow precipitate. The precipitate was washed with deionized water until pH = 7, and dried in vacuo to obtain 1.2 g of the product. Take prepared Pd(phen)Cl 2 0.117g, PPh 3 Add 0.264g, 5.4g ethyl nitrite, and 35mL ethanol into the autoclave, first pass 1.0MPa of CO to replace the air for 3 times, then pass CO to 3.0MPa, control the temperature at 60°C, and react for 6h. After the reaction is completed, the reaction Liqui...

example 2

[0027] Take prepared Pd(phen)Cl 2 0.117g, PPh 3 Add 0.264g, 6.4g of propyl nitrite, and 35mL of n-propanol into the autoclave, first pass 1.0MPa of CO to replace the air for 3 times, then pass CO to 4.5MPa, control the temperature at 60°C, and react for 6h. After the reaction, The reaction solution was filtered, and the catalyst was dried to recover. The filtrate was analyzed by GC, and the yield of dipropyl oxalate was 65.3%, and the selectivity of dipropyl oxalate was 95.2%.

example 3

[0029] Take prepared Pd(phen)Cl 2 0.117g, PPh 3 Add 0.264g, 7.4g of butyl nitrite, and 35mL of n-butanol into the autoclave, first pass 1.0MPa of CO to replace the air for 3 times, then pass CO to 3.0MPa, control the temperature at 60°C, and react for 6h. After the reaction, The reaction solution was filtered, and the catalyst was dried to recover. The filtrate was analyzed by GC, and the yield of dibutyl oxalate was 47.2%, and the selectivity of dibutyl oxalate was 93.6%.

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Abstract

The invention relates to a catalyst of palladium complex containing N-N bidentate ligand used for synthesizing oxalate through the liquid phase coupling method as well as the preparation and the application methods thereof. Aiming at the disadvantages of the prior catalyst for synthesizing oxalate that the synthetic ratio is low, the catalyst is not easy to separate from the product and the service life is short, a catalyst of palladium complex containing N-N bidentate ligand with high activity and high selectivity is invented, and the catalyst is applied to the liquid phase coupling reaction synthesis of nitric acid ester and CO. The catalyst has the advantages that the preparation is easy, the selectivity is high, the catalyst is easy to separate from the product, and the service life of the catalyst is long.

Description

technical field [0001] The invention relates to a palladium complex catalyst containing N-N bidentate ligands suitable for synthesizing oxalate by liquid phase coupling method and its preparation and application method. technical background [0002] Oxalate is an important chemical raw material, which can be used to manufacture oxalic acid, oxamide, ethylene glycol, and intermediates of certain drugs and dyes. Catalyzed synthesis of oxalate from carbon monoxide and nitrite opens up a new and important route for Cl chemistry to produce oxalate. Especially for my country's lack of petroleum resources and rich coal resources, this route of coal chemical synthesis of oxalate is of strategic significance. [0003] Synthesis of oxalate from carbon monoxide and nitrite is divided into liquid-phase method and gas-phase method. The gas-phase method synthesizes dimethyl oxalate or diethyl oxalate from methyl nitrite or ethyl nitrite in the gas phase. It has been studied for nearly 3...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/24B01J31/28C07C69/36C07C67/37
Inventor 李光兴陈腊山梅付名袁卫萍陈丽娟吕仪军张永康安铁夫熊辉王明国李涛张少英
Owner HUAZHONG UNIV OF SCI & TECH
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