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Preparation method of thermal conduction enhanced metal organic framework gas storage material

A metal-organic framework and enhanced thermal conductivity technology, which can be applied to 4/14 groups of organic compounds without C-metal bonds, 6/16 groups of organic compounds without C-metal bonds, organic chemistry, etc. It can solve the problem of reducing the effective adsorption of gases. Quantity and other issues, to achieve the effect of mild reaction conditions, simple process and suitable for large-scale production

Active Publication Date: 2015-05-20
UNIV OF SCI & TECH BEIJING
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Problems solved by technology

Based on the above characteristics of metal-organic framework materials, a new type of metal-organic framework material is developed as a gas adsorbent to solve the problem of reducing the effective adsorption capacity of gas due to the thermal effect of the adsorption and desorption process in the field of gas adsorption, which has broad application prospects.

Method used

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  • Preparation method of thermal conduction enhanced metal organic framework gas storage material
  • Preparation method of thermal conduction enhanced metal organic framework gas storage material
  • Preparation method of thermal conduction enhanced metal organic framework gas storage material

Examples

Experimental program
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Effect test

Embodiment example 1

[0029] (1) ZrCl 4 (0.4g, 1.7mmol) was dissolved in 75mL of DMF, ultrasonically dispersed until dissolved; 2.85mL (850mmol) of acetic acid was added during ultrasonication; at the same time, aminoterephthalic acid (0.311g, 1.7mmol) was dissolved in 25mL of DMF At the same time, pour it into a 250mL round-bottomed flask, add 0.125mL (0.007mmol) of deionized water at the end, plug the bottle tightly, ultrasonically disperse at 60°C for a period of time, and then put it into an oil bath at 120°C Stand in the middle for 24h. After the reaction was finished, it was centrifuged, and the lower layer of precipitate was soaked in DMF for two hours, and then centrifuged. Then washed several times with ethanol and dried in vacuum at 150°C for 5h to obtain UiO-66-NH 2 .

[0030] (2) Take UiO-66-NH 2 (0.2g, 0.113mmol) was dissolved in 5mL of chloroform, and 1,3-propanesultone (0.144g, 1.18mmol) was added and stirred overnight. Subsequently, HAuCl was added to the reaction solution unde...

Embodiment example 2

[0034] (1) CrCl 3 (0.27g) and 2-nitroterephthalic acid (0.21g) were fully dissolved in 5mL of deionized water, stirred at room temperature for 30min, moved to a 25mL reaction kettle, and reacted at 180°C for 96h. The product was centrifuged, washed with a mixed solvent of ethanol and water, and dried in a vacuum oven at 60°C for 24 hours to obtain MIL-101-NO 2 (Cr).

[0035] (2) Take MIL-101-NO 2 (Cr) (0.1g) and SnCl 2 2H 2 O (3.26g) was dissolved in 20mL of ethanol, stirred at 70°C for 6h, and then redispersed in 20mL of concentrated hydrochloric acid after centrifugation. After the reaction, the precipitate was obtained by centrifugation, and then dispersed in 25 mL of ethanol. In order to ensure the controllable reduction of gold nanoparticles in the MOFs pores, multiple adsorption and reduction methods were used to reduce the number of gold nanoparticles on the surface of MOFs materials. Add HAuCl in ice bath 4 Aqueous solution of precursor (0.3mL, 0.025M), stirring ...

Embodiment example 3

[0038] (1) Mix 2-aminoterephthalic acid (1.636g, 5.5mmol) with Zn(NO 3 ) 2 4H 2 O (0.37g, 2mmol) and 50mL DMF were mixed and stirred at room temperature for 30min, divided into 5 scintillation vials, kept in an oven at 55°C for 96h, and then CTAB (0.728g, 2mmol) was added to each scintillation vial55 ℃ heating and stirring until CTAB is completely dissolved, and then transferred to an oven at 105 ℃ for 90 minutes. Take out the scintillation vial, add TEA (0.278mL, 2mmol) respectively, stir for 10min, centrifuge, use solvent DMF, CHCl 3 Washed three times respectively, oven-dried at 40°C, and then vacuum-dried to obtain IRMOF-3.

[0039] (2) Disperse IRMOF-3 (0.27g, 0.27mmol) in 20mL CHCl 3 Glyoxal (220mg, 40wt% aqueous solution) was added dropwise at room temperature, and the reaction was stirred for 24h to modify the aldehyde group in the channel of IRMOF-3. Then add AgNO to the reaction vessel 3 Precursor aqueous solution (2.5mL, 0.025M), stirred and adsorbed for 4h, t...

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Abstract

The invention relates to a preparation method of a thermal conduction enhanced metal organic framework gas storage material and belongs to the field of nanocomposites. The preparation method comprises the following steps: firstly selectively preparing a metal organic framework material with a large surface area and a high micropore proportion; performing synthesis post-modification on the metal organic framework material by a 'one-pot' method, regulating the polarity and contained functional groups of pores, immobilizing metal nanoparticles inside the pores to enhance the thermal conduction property of the metal organic framework material; adsorbing industrial gas by utilizing the ultra-large specific surface area and the nano duct structure of the metal organic framework material, wherein the thermal conduction enhanced adsorption material can be used for quickly transmitting the heat generated in the adsorption and desorption process of the industrial gas. The metal organic framework industrial gas adsorber prepared by the invention can be used for efficiently adsorbing and desorbing the industrial gas and effectively improving the thermal conduction property of the adsorber, and avoiding the influence of the heat effect on the adsorption quantity in the adsorption and desorption process. The preparation method provided by the invention has the advantages of use of readily available and inexpensive raw materials, simple process, and mild reaction conditions and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the industrial field of nanocomposite materials and industrial gas storage, and in particular relates to a preparation method of a heat conduction-enhanced metal-organic framework material used for industrial gas adsorption and storage. Background technique [0002] With the rapid development of our country's economy and the rise of our country as a global manufacturing power, the important position and role of the industrial gas industry, one of the basic industrial elements of the national economy, in the national economy has become increasingly prominent. Due to the low density of industrial gases, they need to be compressed before they can be stored and transported. Common storage methods mainly include compressed gases (gases that are completely gaseous when pressurized at -50°C; this category includes critical temperatures less than or equal to All gases at -50°C), liquefied gases (gases that are partly liquefied in press...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D53/02C07F7/00C07F11/00C07F3/06
CPCB01J20/223B01J20/226B01J20/28002B01J2220/46B01J2220/4806B01J2220/4812C07F3/06C07F7/003C07F11/005
Inventor 栾奕禹杰齐悦彭雄杨明
Owner UNIV OF SCI & TECH BEIJING
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