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Method for catalyzing hydrogen production of formic acid by iridium-immobilized metal organic framework material

A metal-organic framework, solid-supported technology, used in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., to avoid deactivation

Active Publication Date: 2019-10-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the hydrogen production from formic acid aqueous system catalyzed by iridium-supported metal-organic frameworks.

Method used

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  • Method for catalyzing hydrogen production of formic acid by iridium-immobilized metal organic framework material
  • Method for catalyzing hydrogen production of formic acid by iridium-immobilized metal organic framework material
  • Method for catalyzing hydrogen production of formic acid by iridium-immobilized metal organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0038] 0.68g NH 2 Add BDC and 100mL DMF to a flask placed in an oil bath, stir magnetically until the solid is completely dissolved; after the temperature rises to 110°C, use a constant pressure funnel to dissolve the 3 ·6H 2 O solution (1.80g AlCl 3 ·6H 2 (0 and 50mL DMF mixed with ultrasound) were slowly added dropwise to the flask within 90min; after continuing to stir at a constant temperature for 3h, turn off the stirring and let stand for 20h; after the reaction was completed, slowly drop to room temperature and suction filter under reduced pressure, and wash the yellow solid three times with DMF. Then the obtained crude product was extracted overnight with ethanol Soxhlet, dried and activated under vacuum at 100°C to obtain pure NH 2 -MIL-101(Al).

[0039] 0.07g DMAP, 50mLDMA, 0.96g NH 2 -MIL-101(Al) was mixed evenly and added to the autoclave, and reacted at 80°C for 30 minutes in a nitrogen atmosphere; after cooling down, 0.75g PCCH was added under magnetic stirr...

Embodiment 2

[0041] Embodiment 2 gained NH 2 - PXRD patterns, nitrogen adsorption-desorption isotherms, and SEM images of MIL-101(Al) and MOF-101-2 Figure 1-3 as shown ( image 3 where a is NH 2 - MIL-101 (Al); b is MOF-101-2). After the iridium is immobilized, the MOF still maintains the original crystal structure, but the specific surface area is greatly reduced due to the presence of iridium components in the pores. -NH on organic linker 2 The steric effect of the complexation of the ligand and the metal ion is increased, resulting in a decrease in the crystallinity of the MOF, and there is no regular octahedral structure.

[0042] Table 1 The influence of different iridium solid loads on the production of hydrogen from formic acid

[0043] Example 1 2 3 Iridium theoretical immobilized capacity / (wt.%) 10 15 20 Mass of iridium hydrate / g 0.07 0.11 0.15 Reaction time / min 240 180 195 Gas volume / mL 353 418 356

Embodiment 4-6

[0045] Referring to Example 2, MOF-101-2 with a theoretical loading of iridium of 15 wt.% was synthesized. According to Table 2, pour 20-80mg MOF-101-2 into the flask, and place the flask in an oil bath that has been preheated to 50°C. After 20 minutes, inject 5 mL of 2M formic acid aqueous solution into the flask, start magnetic stirring, and start timing. When the gas production is less than 2 mL after 5 minutes, stop the reaction, and pour water into the flask to exhaust the gas remaining in the device. See Table 2 for the gas production of formic acid decomposition under different catalyst dosages. For Examples 4-7, the content of CO in the reaction product gas is no more than 10ppm, H 2 and CO 2 The concentration ratio is 1:1.

[0046] Table 2 The influence of catalyst dosage on formic acid hydrogen production

[0047] Example 4 2 5 6 Catalyst dosage / mg 20 40 60 80 Reaction time / min 288 180 142 129 Gas volume / mL 386 418 430 43...

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Abstract

The invention discloses a method for catalyzing hydrogen production of formic acid by an iridium-immobilized metal organic framework material. According to the method, modifiable NH2-MIL-101 (Al) withstable chemical properties and high specific surface area is taken as a base, an amino group is modified, an amide-type iridium-based complex is introduced into the NH2-MIL-101 (Al), and accordingly,the iridium-immobilized metal organic framework material is obtained. The iridium-immobilized metal organic framework material has excellent performance in catalyzing hydrogen production of a formicacid aqueous solution system. 60mg of catalysts and 5mL of 2M formic acid aqueous solutions are added to a flask for a reaction at 50 DEG C, the conversion rate of the formic acid is 88%, the selectivity of hydrogen is close to 100% (CO (10ppm), and the TOF can reach 332h<-1>. The catalysts are recycled for three times, and the catalytic activity of the catalysts is not obviously lowered.

Description

technical field [0001] The invention belongs to the field of hydrogen production from formic acid, and in particular relates to a method for producing hydrogen from formic acid catalyzed by an iridium-supported metal-organic framework material. Background technique [0002] h 2 Not only is it a highly efficient and clean energy with great potential, but also H 2 It also plays an important role in biomass conversion technology. For example, the original bio-oil obtained from biomass pyrolysis and liquefaction can be used as fuel after catalytic hydrofining, lignin hydrogenolysis to prepare aromatic monomers, and biomass derivative furfural to hydrogenate tetrahydrofurfuryl alcohol, etc. In the field of hydrogen energy technology, developing technologies that can store and release high-purity hydrogen safely and efficiently is an important goal. In addition to good stability, high energy density and various preparation channels (biomass conversion, CO 2 In addition to cata...

Claims

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Application Information

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IPC IPC(8): C01B3/22B01J31/22
CPCC01B3/22B01J31/2243B01J31/1691B01J2531/31C01B2203/0277C01B2203/1047C01B2203/1082
Inventor 常杰马彩珺李伟瑞付严
Owner SOUTH CHINA UNIV OF TECH
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