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Preparation method for MOF-5 metal-organic frameworks

A metal-organic framework, MOF-5 technology, applied in chemical instruments and methods, other chemical processes, hydrogen separation, etc., can solve the problems of poor interpenetrating MOF-5 crystal quality and high cost, and achieve good thermal stability. Strong hydrogen storage capacity and the effect of improving hydrogen storage capacity

Inactive Publication Date: 2014-11-19
INST OF MECHANICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The currently reported methods for preparing interpenetrating MOF-5 are mostly solvothermal methods. The quality of interpenetrating MOF-5 crystals prepared by this method is poor and the cost is high

Method used

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  • Preparation method for MOF-5 metal-organic frameworks
  • Preparation method for MOF-5 metal-organic frameworks
  • Preparation method for MOF-5 metal-organic frameworks

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] The MOF-5 metal-organic framework of interpenetrating structure is prepared by a method comprising the following steps:

[0068] 1. Use 10g of 4A molecular sieves to remove water from 500ml of N,N-dimethylformamide (DMF) solvent for 24 hours, set aside. Molecular sieves need to be activated at 400°C for 36 hours before use.

[0069] 2. Get 1.66g zinc nitrate hexahydrate (Zn(NO 3 ) 2 ·6H 2 O) and 0.35g terephthalic acid (H 2 BDC) was dissolved in 50 ml of dehydrated DMF solvent, and 550 μL of triethylamine (TEA) was added to immediately produce a white precipitate.

[0070] 3. The white precipitate produced in (2) was filtered off, and the remaining clear solution was heated at 105° C. for 24 hours to produce MOF-5 crystals.

[0071] 4. After the MOF-5 crystals collected in (3) were washed three times with 30ml of dewatered DMF solvent, the MOF-5 crystals were sealed and soaked in 30ml of chloroform at room temperature for 7 days, and the chloroform was changed ever...

Embodiment 2

[0075] The MOF-5 metal-organic framework with interpenetrating structure doped with carbon nanotubes is prepared by a method comprising the following steps:

[0076] 1. Use 15g of 4A molecular sieves to remove water from 800ml of N,N-dimethylformamide (DMF) solvent for 36 hours, set aside. Molecular sieves need to be activated at 450°C for 24 hours before use.

[0077] 2. Get 3.33g zinc nitrate hexahydrate (Zn(NO 3 ) 2 ·6H 2 O) and 0.71g terephthalic acid (H 2 BDC) was dissolved in 120 ml of dehydrated DMF solvent, and 1100 μL of triethylamine (TEA) was added to immediately produce a white precipitate.

[0078] 3. Filter off the produced white precipitate, add 30 mg of carboxy-functionalized multi-walled carbon nanotubes (MWCNTs) to the remaining clear liquid, and disperse the MWCNTs uniformly by ultrasonication. The solution was heated at 95 °C for 36 h to generate MOF-5 / MWCNTs composites.

[0079] 4. After the MOF-5 / MWCNTs complex collected in 4. was repeatedly washed ...

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Abstract

The invention discloses a preparation method for MOF-5 metal-organic frameworks of interpenetrating structures. The preparation method comprises the following steps: (1) dissolving Zn(NO3)2.6H2O and H2BDC into a DMF solvent; adding TEA (triethylamine) to produce white precipitate and then filtering, wherein a filtrate is a precursor solution; and (2) heating for 24 to 48 hours at 90 to 110 DEG C to obtain MOF-5 crystals. The preparation method integrates the advantages of a TEA direct mixing method and a solvothermal method. Firstly, a reaction solution with the relatively high concentration is required for preparing the interpenetrating structures, while the reaction solution with the relatively high concentration can damage the MOF-5 seed crystals, and the damage can be avoided by adding the TEA; secondly, the white precipitate produced after the TEA is added is removed, and a remained clarified liquor is reserved for performing reaction, so that the high crystallinity of the MOF-5 crystals is guaranteed; in addition, the TEA is also introduced into intergranular mesoporous, so that the hydrogen storage capacity of interpenetrated MOF-5 is improved. The preparation method disclosed by the invention can also be used for preparing the carbon-material-doped interpenetrated MOF-5. The MOF-5 metal-organic frameworks of the interpenetrating structures, which are prepared by the preparation method, have the high hydrogen storage capacity and the high thermal stability.

Description

technical field [0001] The invention relates to a method for preparing a hydrogen storage material, in particular to a method for preparing a metal organic framework MOF-5 metal. Background technique [0002] As a clean energy, hydrogen has the advantages of high energy, low density, and wide sources. However, its flammable and explosive properties limit the application of hydrogen. Therefore, ensuring the safety of hydrogen during storage and transportation is the basic condition for its wide application. At present, hydrogen is usually liquefied by pressurization or cooling, and then stored and transported in liquid form, but the energy consumption and cost are too high. Therefore, the use of porous materials as hydrogen storage media to achieve low-cost, high-efficiency hydrogen storage and safe transportation has become a research goal. [0003] Compared with traditional porous materials, metal-organic frameworks (MOFs) materials have the characteristics of high speci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01D53/02C01B3/56
Inventor 姜恒冯亚菲陈猛王育人
Owner INST OF MECHANICS - CHINESE ACAD OF SCI
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