Preparation method of metal organic framework-graphite oxide composite

A metal-organic framework and composite material technology, which is applied in the field of preparation of metal-organic framework-graphene oxide composite materials, can solve problems such as low atomic density, and achieve the effects of improving adsorption capacity, large specific surface area, and improving the performance of adsorbing water vapor.

Active Publication Date: 2015-07-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main reason is that although this type of material has a large specific surface area, its atomic density is small

Method used

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  • Preparation method of metal organic framework-graphite oxide composite
  • Preparation method of metal organic framework-graphite oxide composite
  • Preparation method of metal organic framework-graphite oxide composite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 4 g of graphite powder with a particle size of 60 μm to 4 g of NaNO 3 and 200mL of concentrated sulfuric acid (concentration: 95%), fully stirred in an ice bath, and at the same time with 1g min -1 Add 24gKMNO at a rate of 4 . Then remove the ice bath, continue stirring for 12 hours, add 1120mL water and 80mL H 2 o 2 , filtered to remove excess acid, centrifuged, and vacuum dried to obtain solid powder GO. Put GO in N 2 Heat treatment at 1050° C. for 1 min in the atmosphere to obtain solid powder GrO. According to GrO and Cr(NO 3 ) 3 9H 2 The mass ratio of O was 1:5 to configure the reaction solution, disperse 0.8g GrO in 48mL water and perform ultrasonic treatment with a power of 1000W and a frequency of 27kHz for 30min, and then add 4g Cr(NO 3 ) 3 9H 2 O, 1.64g H 2 BDC and 0.5mL HF were reacted at 210°C for 9 hours to obtain the GrOMIL-101 composite. Finally, the obtained material was soaked in ethanol at 100°C for 8 hours, then filtered, dried, and t...

Embodiment 2

[0029] Add 4 g of graphite powder with a particle size of 30 μm to 4 g of NaNO 3 and 200mL of concentrated sulfuric acid (concentration: 96%), fully stirred in an ice bath, and at the same time with 3g min -1 Add 24gKMNO at a rate of 4 . Then remove the ice bath, continue stirring for 12 hours, add 1120mL water and 80mL H 2 o 2 , filtered to remove excess acid, centrifuged, and vacuum dried to obtain solid powder GO. GO was heat-treated at 350 °C for 90 min in an Ar atmosphere to obtain solid powder GrO. According to GrO and Cr(NO 3 ) 3 9H 2The mass ratio of O was 1:10 to configure the reaction solution, 0.4g GrO was dispersed in 48mL water and subjected to ultrasonic treatment with a power of 1000W and a frequency of 27kHz for 30min, and then 4g Cr(NO 3 ) 3 9H 2 O and 1.64g H 2 BDC and react at 230 °C for 7 hours to obtain the GrOMIL-101 composite. Finally, the obtained material was soaked in ethanol at 100°C for 10 hours, then filtered, dried, and then washed wit...

Embodiment 3

[0031] Add 4 g of graphite powder with a particle size of 20 μm to 4 g of NaNO 3 and 200mL of concentrated sulfuric acid (concentration: 98%), fully stirred in an ice bath, and at the same time with 2g min -1 Add 24gKMNO at a rate of 4 . Then remove the ice bath, continue to stir for 24 hours, add 1120mL water and 80mL H 2 o 2 , filtered to remove excess acid, centrifuged, and vacuum dried to obtain solid powder GO. Put GO in N 2 Heat treatment at 350° C. for 60 min in the atmosphere to obtain solid powder GrO. According to GrO and Cr(NO 3 ) 3 9H 2 The mass ratio of O was 1:200 to configure the reaction solution, disperse 0.02g GrO in 48mL water and perform ultrasonic treatment with a power of 1000W and a frequency of 27kHz for 30min, then add 4g Cr(NO 3 ) 3 9H 2 O and 1.64gH 2 BDC and react at 220°C for 8 hours to obtain the GrOMIL-101 composite. Finally, the obtained material was soaked in ethanol at 100°C for 12 hours, then filtered, dried, and then washed with...

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Abstract

The invention discloses a preparation method of a metal organic framework-graphite oxide composite, which comprises the following steps of: (1) preparing solid powdered graphite oxide, (2) performing high temperature reduction on solid powdered graphite oxide in an inert gas atmosphere to form graphite oxide powder, (3) dispersing the graphite oxide powder obtained in Step (2) for ultrasonic treatment, then adding Cr(NO3)3.9H2O and H2BDC mixed liquid for reaction at 210-230 DEG C to form a coarse metal organic framework-graphite oxide composite, and (4) performing soak cleaning on the coarse metal organic framework-graphite oxide composite obtained in Step (3) with an alcohol solution and an ammonium fluoride solution sequentially, and finally obtaining the purified metal organic framework-graphite oxide composite. An adsorbent prepared by the method has a large specific surface, developed micropores and very high water vapor adsorption capacity.

Description

technical field [0001] The invention relates to a water vapor adsorption material, in particular to a preparation method of a metal organic framework-graphene oxide composite material. Background technique [0002] Air humidity has an important impact on industrial production process, product quality control, food safety and human comfort. In the industrial production process, if the air humidity is too high, it will affect the synthesis process and yield of some reaction products; in product quality control, if the influence of air humidity is ignored, the product quality will be seriously affected; in the catering service industry If the humidity of the food storage environment is not effectively controlled, it will lead to mold and deterioration of the food; in the work or home environment, if a comfortable and dry environment is not created, the work efficiency of workers will be reduced and human health will be affected. Therefore, the development of efficient air dehu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/02B01J20/30
Inventor 李忠周欣夏启斌肖静颜健孙雪娇
Owner SOUTH CHINA UNIV OF TECH
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