Preparation method of boron/nitrogen-doped microporous carbon material

A technology of element doping and microporous carbon, which is applied in the preparation/purification of carbon, chemical instruments and methods, and other chemical processes. It can solve the problem of small surface area, uneven pore size distribution, and wide pore size distribution of porous carbon materials. problems, to achieve the effects of doping and concentrated micropore size distribution, simple preparation process, and easy operation

Inactive Publication Date: 2014-01-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

However, due to the characteristics of the pore properties of the current template materials, such as large pore size, uneven pore size distr...

Method used

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  • Preparation method of boron/nitrogen-doped microporous carbon material
  • Preparation method of boron/nitrogen-doped microporous carbon material
  • Preparation method of boron/nitrogen-doped microporous carbon material

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Embodiment 1

[0030] 1. Weigh 2.933g of zinc nitrate hexahydrate and 6.489g of dimethylimidazole and dissolve them in 200ml of methanol solution respectively. Stir vigorously for 3h~6h and stand still overnight. The product was filtered, washed with fresh methanol solution, and vacuumed overnight at 30 °C to prepare a ZIF-8 sample. Apply vacuum at 300°C for 4 hours to obtain the activated ZIF-8 sample.

[0031] 2. Add 3ml, 2mol / L ammonia borane solution to one gram of activated ZIF-8 sample in an argon atmosphere glove box, ultrasonically impregnate for 5h, and vacuum dry overnight at room temperature. A composite material of ammonia borane and metal-organic framework compound ZIF-8 was prepared.

[0032] 3. Put the above composite material into a high-temperature furnace, use an argon atmosphere (gas flow rate is 100-400mL / min), raise the temperature to 800-1200°C at a heating rate of 1-10°C / min, and heat it up at 800-1200 °C was kept for 2-10 hours, and cooled to room temperature...

Embodiment 2

[0035] The 0.4g boron-nitrogen-doped microporous carbon material prepared in Example 1 was placed in a 9mm sample tube of the Absorb-1 physical adsorption instrument of Quanta Corporation, USA, and heated overnight at 200°C in a sealed vacuum. The low-pressure hydrogen adsorption experiment was carried out under two temperature conditions of 77K and 87K.

[0036] Depend on Figure 4 It can be seen that under the hydrogen pressure conditions of 77K and 820mmHg, each gram of boron-nitrogen-doped microporous carbon material can adsorb 204cm 3 Hydrogen, the corresponding mass fraction is 1.83wt%.

Embodiment 3

[0038] The microporous carbon material doped with 0.3 g of boron and nitrogen elements prepared in Example 1 was placed in a 9 mm sample tube of the Absorb-1 physical adsorption instrument of Quanta Corporation, USA, and heated in a sealed vacuum at 200 ° C overnight. Under the constant temperature condition of 273K, the low-pressure carbon dioxide adsorption experiment was carried out.

[0039] Depend on Figure 5 It can be seen that under the pressure conditions of 273K and 780mmHg, each gram of boron and nitrogen doped microporous carbon materials can adsorb 100cm 3 of carbon dioxide.

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Abstract

The invention relates to a preparation method and gas adsorption properties of a boron/nitrogen-doped microporous carbon material, particularly a boron/nitrogen-doped microporous carbon material prepared by using metal organic framework ZIF-8 (zeolitic imidazolate framework-8) and boron nitrogen compounds as precursors by a high-temperature sintering method and gas adsorption properties of the boron/nitrogen-doped microporous carbon material for hydrogen, carbon dioxide, nitrogen and the like. The preparation method comprises the following steps: 1) preparing the porous metal organic framework ZIF-8; 2) limiting the boron nitrogen compounds (such as ammonia borane) to the inside of the pores of the metal organic framework ZIF-8 by a solution impregnating method; and 3) carrying out high-temperature sintering on the composite material in an argon atmosphere to obtain the boron/nitrogen-doped microporous carbon material. The preparation technique is simple; and the prepared carbon material implements simultaneous doping of boron and nitrogen and centralized distribution of micropore sizes, and has favorable adsorption property for hydrogen and selective adsorption property for carbon dioxide.

Description

technical field [0001] The invention relates to a method for preparing a microporous carbon material doped with boron and nitrogen elements and its gas adsorption performance. Specifically, the metal-organic framework compound ZIF-8 and the boron-nitrogen compound ammonia borane are used as precursors through a high-temperature sintering method The prepared microporous carbon materials doped with boron and nitrogen elements and their adsorption properties of hydrogen, carbon dioxide, nitrogen and other gases. Background technique [0002] Nanoporous carbon materials have been widely used in gas adsorption and separation, catalyst supports and electrode materials due to their high specific surface area, large pore volume and excellent chemical stability. The methods used to synthesize nanoporous carbon materials mainly include the following: 1) physical and chemical activation; 2) chemical vapor deposition; 3) polymer carbonization; 4) template method, etc. Among them, the t...

Claims

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Application Information

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IPC IPC(8): C01B31/02B01J20/20C01B32/05
Inventor 孙立贤司晓亮徐芬张箭王自强
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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