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A Class of Formic Acid Dehydrogenation Catalyst and Its Application

A technology of catalyst and catalyst concentration, applied in the direction of physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, hydrogen, etc. Low efficiency and other problems, to achieve the effect of high catalytic efficiency, simple structure and easy synthesis

Active Publication Date: 2021-07-09
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

In 2015, Himeda, Fujita, Mucherman and others reported that TON of 2,050,000 can be obtained (ACS Catal.2015,5, 5496-5504), but the reaction is carried out at 60°C, and it takes 580 hours to complete the reaction. The reaction efficiency is low and it is not suitable for large quantities. Practical applications requiring hydrogen rapidly
Later, they reported another type of catalyst, a complex formed by pyridine and imidazoline ligands and iridium (Catal.Sci.Technol., 2016, 6, 988-992), which shortened the reaction time of formic acid dehydrogenation to 363h , but the catalytic activity is still low
In 2016, Kawanami's research group reported that the dehydrogenation of formic acid can reach TON of 5,000,000 (ChemSusChem 2016,9,2749-2753), but it requires a reaction time of 2600h and the catalytic activity is lower
The raw materials for synthesizing this type of catalyst are cheap, the synthesis steps are simple, and are suitable for mass production; this type of catalyst can be generated in situ, and the complex can also be prepared before the reaction. The reaction operation is simple, no protection and dehydrogenation treatment are required, and the stability is good. , the application in the formic acid dehydrogenation reaction has not been reported at home and abroad

Method used

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  • A Class of Formic Acid Dehydrogenation Catalyst and Its Application
  • A Class of Formic Acid Dehydrogenation Catalyst and Its Application
  • A Class of Formic Acid Dehydrogenation Catalyst and Its Application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Use glyoxaldoxime L1 as ligand, FA (1.0M, 10.0mL), 60°C.

[0026] Weigh [Cp*IrCl 2 ] 2 (4.0mg, 5.0μmol) and L1 (1.42mg, 12μmol) were placed in a reagent bottle, and 1.0mL of purified water was added to prepare an aqueous solution of the in-situ catalyst. Add magnetons, water (9.42mL) and formic acid (10mmol, 0.38mL) to a Schlenk reaction tube or bottle, seal with a rubber stopper, connect the branch to the rubber tube; put the reaction bottle into a water bath at 60°C and stir to stabilize After 10 minutes, pipette 0.2mL (1.0μmol) of the prepared catalyst solution into the reaction bottle quickly with a pipette gun, seal the reaction bottle, and immediately put the rubber hose connected to the branch pipe into the water basin, fill it with water and stand it upside down In a 500mL graduated cylinder, the timer starts, and the gas is collected by the drainage method. Calculate the amount of gas collected per unit time, calculate TON and TOF, V(CO 2 )=Volume / 2 of the ...

Embodiment 2

[0028] Same as Example 1, except that the ligand (Z)-N'-hydroxypicolinimidamide L2 was used instead of L1 for the reaction, and the results are shown in Example 2 in Table 1.

Embodiment 3

[0030] The same as in Example 1, except that the ligand 1,2-dimethyldimethylacetate oxime L3 was used instead of L1 for the reaction, and the results are shown in Example 3 in Table 1.

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Abstract

The invention is a kind of formic acid dehydrogenation catalyst; the catalyst includes a metal and a ligand, the metal is iridium, rhodium, ruthenium, cobalt, etc., and the ligand is an amino-substituted oxime ether compound; this type of catalyst is used for the dehydrogenation of formic acid for the first time Reaction, the highest TON can reach 505×10 at 70°C 4 , is the highest value reported so far, and the highest TON can reach 400×10 at 90°C 4 , is the highest value reported at this temperature.

Description

technical field [0001] The present invention relates to a kind of catalyst that is used for the dehydrogenation of formic acid, specifically by a kind of bidentate or polydentate ligand of oxime ether imine structure that contains amino substitution and various metals of iridium, rhodium, ruthenium and cobalt Catalysts for precursor formation. Background technique [0002] Formic acid, as a liquid hydrogen storage material, has attracted widespread attention. An ideal formic acid decomposition hydrogen production catalytic system should meet the following conditions: (1) the catalyst is stable, the raw materials are easy to obtain, and the preparation is simple; (2) the reaction is solvent-free or uses water as a solvent; (3) without any additives; (4) can Decompose pure formic acid or relatively concentrated formic acid; (5) High catalytic efficiency; (6) The reaction can be carried out in large quantities, and the operation is simple, without additional operations such as...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C01B3/22
CPCB01J31/1805B01J31/1815B01J31/2295B01J2531/0241B01J2531/827C01B3/22C01B2203/1047C01B2203/1211C01B2203/1223C01B2203/1229
Inventor 李灿卢胜梅王志君李军王集杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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