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Mesoporous and microporous hierarchical structure carbon and preparation method thereof

A hierarchical structure, mesoporous and microporous technology, applied in the field of porous carbon materials, can solve the problems of a single type of carbon material pores and difficult to meet application requirements, achieve a wide range of application value, eliminate non-catalytic deposition, and mild conditions.

Active Publication Date: 2021-12-17
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In summary, the above methods all require high-temperature preparation conditions of at least 700 °C, and the obtained carbon materials have a single type of pore, which is difficult to meet a wide range of application requirements.

Method used

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  • Mesoporous and microporous hierarchical structure carbon and preparation method thereof
  • Mesoporous and microporous hierarchical structure carbon and preparation method thereof
  • Mesoporous and microporous hierarchical structure carbon and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Step 1: obtaining a NaY molecular sieve with a mesoporous and microporous hierarchical structure. Disperse 5 g of NaY molecular sieve (CVB100, Si / Al=2.6) in 0.3M NH 4 HF 2 The solution was magnetically stirred at 95° C. for 6 h, centrifuged and washed with deionized water until neutral, and the obtained solid product was dried overnight in a drying oven at 60° C.

[0021] Step 2: Ion exchange. The 3.3g molecular sieve that step 1 obtains and the 0.5M CaCl of 100ml 2 The solutions were mixed well, and then the mixed solution was magnetically stirred at 80° C. for 3 h, filtered with suction, and the obtained solid was washed with a large amount of deionized water, and the above operation was repeated twice. Dry the solid product obtained for the second time in a drying oven at 60° C. overnight to obtain ion-exchanged molecular sieves.

[0022] Step 3: Chemical Vapor Deposition. Transfer the molecular sieve obtained in step 2 to a tube furnace, and use N 2 The air in...

Embodiment 2

[0025] Step 1: obtaining a NaY molecular sieve with a mesoporous and microporous hierarchical structure. First, NaY type molecular sieve (CVB100, Si / Al=2.6) and 1.0M NH 4 The Cl solution was uniformly mixed according to the liquid-solid ratio of 20:1, magnetically stirred at 90 °C for 3 h, repeated three times, and the sample was thoroughly washed with deionized water, and the sample was dried in an oven at 60 °C overnight. 5g of dried molecular sieves and 5g (NH 4 ) 2 SO 4 The solid was dispersed in 50 g of deionized water at room temperature, and then 5 g of NH 4 F solid with 17.5g of 1.0MH 2 C 2 0 4 solution, and the resulting suspension was stirred at room temperature for 6 hours, filtered with suction, washed, and dried at 60°C for 12 hours.

[0026] Step 2: Ion exchange. The 3.3g molecular sieve that step 1 obtains and the 0.5M CaCl of 100ml 2The solutions were mixed well, and then the mixed solution was magnetically stirred at 80° C. for 3 h, filtered with suct...

Embodiment 3

[0030] Step 1: obtaining a NaY molecular sieve with a mesoporous and microporous hierarchical structure. Evenly disperse 6.7g NaY type molecular sieve (CVB100, Si / Al=2.6) in 100ml of 0.11M H 4 In the EDTA solution, reflux at 100°C and magnetically stir for 6h, centrifuge and wash with deionized water until neutral; then, uniformly mix the obtained solid product with 200ml of 0.2M NaOH solution, stir magnetically at 65°C for 30min, centrifuge Separate and wash with deionized water until neutral; finally, the product obtained in the previous step is evenly dispersed in 100ml of 0.11M Na 2 h 2 In EDTA solution, reflux at 100°C and magnetically stir for 6h, centrifuge, wash, and dry at 60°C for 12h.

[0031] Step 2: Ion exchange. The 3.3g molecular sieve that step 1 obtains and the 0.5M CaCl of 100ml 2 The solutions were mixed well, and then the mixed solution was magnetically stirred at 80° C. for 3 h, filtered with suction, and the obtained solid was washed with a large amou...

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Abstract

The invention relates to mesoporous and microporous hierarchical structure carbon and a preparation method thereof. The mesoporous and microporous hierarchical structure carbon has two pore channel types of mesopores and micropores at the same time, and is prepared by taking a molecular sieve with a mesoporous and microporous hierarchical structure as a template and utilizing a chemical vapor deposition technology. Compared with a traditional porous carbon material synthesis method, the method only needs relatively mild conditions of medium and low temperature (350-550 DEG C) and medium and low pressure (200-600 torr), so that non-catalytic deposition of carbon is greatly reduced, and the quality of the carbon material is improved. Besides, the mesoporous and microporous hierarchical structure carbon combines the advantages of the mesopores and the micropores, a mesoporous channel is introduced while the large specific surface area and the advantages of a microporous structure are reserved, the defects that single microporous carbon is short in diffusion distance and large in mass transfer resistance are overcome, diffusion and transmission of materials in the channel are facilitated, and wide application prospects and development potentials are realized in the fields of energy storage, catalysis and the like.

Description

technical field [0001] The invention belongs to the field of porous carbon materials, and in particular relates to a method for preparing mesoporous and microporous hierarchical carbon. It is characterized in that: using molecular sieves with mesoporous and microporous hierarchical structures as templates, introducing active sites into molecular sieves through cation exchange, and using chemical vapor deposition technology to catalyze the decomposition of carbon source gases and the decomposition of carbon under medium-low temperature and medium-low pressure conditions deposition, and finally etching away the molecular sieve template to obtain the mesoporous and microporous hierarchical carbon. The key of this technology is to control the temperature and pressure of carbon deposition at medium and low temperature of 350-550°C and medium and low pressure of 200-600Torr, respectively, in order to prevent non-selective deposition of carbon on the outer surface of molecular sieves...

Claims

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Application Information

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IPC IPC(8): C01B32/05
CPCC01B32/05
Inventor 杨广武程元壮田忠诚
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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