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Method for preparing metal organic framework-graphene oxide composite material

A metal-organic framework and composite material technology, applied in the field of composite material preparation, can solve problems such as low atomic density, and achieve the effects of increasing atomic density, improving pore volume, and improving adsorption capacity

Active Publication Date: 2014-12-24
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, although the specific surface area of ​​MOFs is large, their atomic density is small

Method used

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  • Method for preparing metal organic framework-graphene oxide composite material
  • Method for preparing metal organic framework-graphene oxide composite material
  • Method for preparing metal organic framework-graphene oxide composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 2 g of graphite powder with a particle size of 60 μm to 4 g of NaNO 3 and 200mL concentrated sulfuric acid mixture, fully stirred in an ice bath, while slowly adding 20g KMnO 4 . Then the ice bath was removed, and after stirring for 48 hours, 1120 mL of deionized water at 60°C and 80 mL of H 2 o 2 , filtered, washed with water to remove excess acid, centrifuged, and spray-dried to obtain GO as a solid powder. According to GrO and Cr(NO 3 ) 3 9H 2The mass ratio of O was 1:100 to configure the reaction solution, and 0.02 g GO was dispersed in 25 mL deionized water for 180 min sonication to obtain the GrO aqueous solution. Add 2g Cr(NO 3 ) 3 9H 2 O, 1.66g H 2 BDC and 0.2mL HF were reacted at 230°C for 62 hours to obtain the GrOMIL-53 composite. Finally, the obtained material was rinsed with DMF for 3 times, then soaked for 24 hours, replaced with DMF every 12 hours, dried, and then kept at 250°C for 12 hours, then activated under vacuum at 130°C for 12 hours...

Embodiment 2

[0029] Add 4 g of graphite powder with a particle size of 30 μm to 4 g of NaNO 3 and 200mL concentrated sulfuric acid mixture, fully stirred in an ice bath, while slowly adding 24g KMNO 4 . Then remove the ice bath, continue to stir for 12 hours, add 1120 mL of 70 ° C deionized water, and finally add 80 mL of H 2 o 2 , filtered, washed with water to remove excess acid, centrifuged, and spray-dried to obtain solid powder GO. According to GrO and Cr(NO 3 ) 3 9H 2 The mass ratio of O was 5:100 to configure the reaction solution, and 0.2 g GO was dispersed in 25 mL deionized water for 120 min sonication to obtain the GrO aqueous solution. Add 4g Cr(NO 3 ) 3 9H 2 O, 1.66g H 2 BDC and 0.2mL HF were reacted at 220°C for 67 hours to obtain the GrOMIL-53 composite. Finally, the obtained material was rinsed with DMF for 5 times, then soaked for 48 hours, DMF was replaced every 18 hours, dried, then kept at 280°C for 18 hours, and vacuum activated at 150°C for 12 hours, the ob...

Embodiment 3

[0031] Add 8 g of graphite powder with a particle size of 20 μm to 4 g of NaNO 3 and 200mL concentrated sulfuric acid mixture, fully stirred in an ice bath, while slowly adding 16gKMNO 4 . Then the ice bath was removed, and after stirring for 24 hours, 1120 mL of 80°C deionized water and 80 mL of H 2 o 2 , filtered, washed with water to remove excess acid, centrifuged, and spray-dried to obtain solid powder GO. According to GrO and Cr(NO 3 ) 3 9H 2 The mass ratio of O was 10:100 to configure the reaction solution, and 0.05 g GO was dispersed in 25 mL deionized water for 60 min of power ultrasonic treatment to obtain the GrO aqueous solution. Add 0.5g Cr(NO 3 ) 3 9H 2 O, 1.66g H 2 BDC and 0.2mL HF were reacted at 210°C for 72 hours to obtain the GrOMIL-53 composite. Finally, the obtained material is rinsed twice with DMF, then soaked for 72 hours, replaced with DMF every 24 hours, dried, and then kept at 300°C for 12 hours, and then vacuum activated at 180°C for 8 ho...

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Abstract

The invention discloses a method for preparing a metal organic framework-graphene oxide composite material. The method comprises the following steps: adding graphite powder into a mixed solution of concentrated sulfuric acid, sodium nitrate and potassium permanganate for oxidizing, adding water for hydrolyzing, and finally, adding H2O2, thereby obtaining graphene oxide; filtering, washing with water, centrifuging, and performing spray drying, thereby obtaining solid powder GO; and dispersing the solid powder GO in water, performing ultrasonic treatment, adding Cr(NO3)3.9H2O, terephthalic acid and hydrofluoric acid, reacting at the temperature of 210-230 DEG C for 67-77 hours, washing and soaking by using N,N-dimethyl formamide, drying, and activating, thereby obtaining the purified GrO@MIL-53 adsorbing material, namely the metal organic framework-graphene oxide composite material. Compared with common MIL-53, the adsorbent prepared by the method has the advantages that the specific surface area and pore volume are increased, and the adsorbent has relatively high CO2 adsorption capacity.

Description

technical field [0001] The invention relates to a method for preparing a composite material, in particular to a method for preparing a metal organic framework-graphene oxide composite material. Background technique [0002] With the development of social industrialization, a series of environmental problems have gradually emerged. Among them, global warming is the most urgent problem facing human society. Excessive burning of fossil fuels, such as oil and coal, produces a large amount of greenhouse gases, which is the root cause of global warming. CO 2 is the main greenhouse gas. Since societies have industrialized, atmospheric CO 2 Concentrations have increased by about 30%, and it is projected that by the end of the century, CO 2 Concentrations will double or triple the current levels. How to effectively treat CO 2 Capture and storage has become a research hotspot. [0003] Carbon dioxide capture technology is the CO produced by industry and related energy industri...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30
Inventor 李忠黄文玉肖静夏启斌王勋刘江
Owner SOUTH CHINA UNIV OF TECH
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