ZIF-based nitrogen-doped porous carbon material and preparation method thereof

A nitrogen-doped porous carbon and calcium carbonate technology, applied in the field of material chemistry, can solve the problems of polluting pore expanders, template agents that are difficult to remove, and easy to collapse in morphology.

Active Publication Date: 2022-04-05
GUANGXI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a ZIF-based nitrogen-doped porous carbon material and its preparation method to solve the problems of difficult removal of traditional templates, easy collapse of appearance, and introduction of polluting pore-enlarging agents

Method used

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  • ZIF-based nitrogen-doped porous carbon material and preparation method thereof
  • ZIF-based nitrogen-doped porous carbon material and preparation method thereof
  • ZIF-based nitrogen-doped porous carbon material and preparation method thereof

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Embodiment 1

[0045] A preparation method of ZIF-based nitrogen-doped porous carbon material, comprising the following steps:

[0046] (1) Configure 0.4mol·L respectively -1 Calcium Chloride (CaCl 2 ) aqueous solution 490mL, 0.4mol L -1 of sodium carbonate (Na 2 CO 3 ) aqueous solution 490mL, 2g L -1 Polyvinylpyrrolidone (PVP) aqueous solution 20mL. Under the temperature condition of 35°C, the three solutions were sealed and stirred evenly; the polyvinylpyrrolidone (PVP) solution was evenly divided into two parts (10mL), and respectively added to CaCl 2 solution and Na 2 CO 3 In the solution, keep stirring in a water bath at 35°C for 30 minutes to make it fully stirred evenly; add CaCl 2 The solution was quickly poured into vigorously stirred Na 2 CO 3 In solution at 600r·min -1 Under the condition of a certain stirring speed, the slurry after the reaction was suction-filtered, washed with absolute ethanol and deionized water, the above operation was repeated three times, and vac...

Embodiment 2

[0055] A preparation method of ZIF-based nitrogen-doped porous carbon material, comprising the following steps:

[0056] Except following change, all the other are the same as embodiment 1. Add 0.1 g zinc nitrate hexahydrate crystals to CaCO 3 @PDA solution, stirred at room temperature for 1 h. Add 0.3 mL of triethylamine to the dimethylimidazole solution, and stir at room temperature for 30 min. The well-mixed dimethylimidazole solution was added dropwise to the CaCO 3 @PDA solution, at room temperature at 550r·min -1 The conditions were stirred for 1h. After the reaction, the slurry was suction filtered, washed with ethanol, and dried under vacuum at 80°C for 5 hours to obtain CaCO 3 @PDA @ZIF-8 composite. Weigh a certain mass of CaCO 3 The @PDA@ZIF-8 sample is placed in a tube furnace and subjected to high-temperature carbonization under the protection of nitrogen. The carbonization conditions are: 5°C min -1 The rate at which CaCO 3 The @PDA@ZIF-8 sample was raise...

Embodiment 3

[0058] A preparation method of ZIF-based nitrogen-doped porous carbon material, comprising the following steps:

[0059] Except following change, all the other are the same as embodiment 2. Weigh a certain mass of CaCO 3 The @PDA sample is placed in a tube furnace and subjected to high-temperature carbonization under the protection of nitrogen. The carbonization conditions are: 5°C min -1 The rate at which CaCO 3 The @PDA@ZIF-8 sample was raised from room temperature to 900 °C, kept at a constant temperature for 2 hours, and then naturally cooled to room temperature. The intermediate product CaO@S-NGPC-ZIF-8 was obtained, which was washed to neutrality with deionized water (the washing procedure was the same as

[0060] Example 1), the ZIF-based nitrogen-doped porous carbon material S-NGPC-ZIF-8 was finally obtained.

[0061] Case Analysis

[0062] Such as figure 1 As shown, the nitrogen-doped porous carbon material S-NGPC-ZIF-8 prepared in Example 1 of the present inven...

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Abstract

The invention discloses a ZIF-based nitrogen-doped porous carbon material and a preparation method thereof. The solid spherical calcium carbonate is used as a template and a pore-enlarging agent, a polydopamine film is loaded, and then zeolite imidazole framework crystal ZIF-8 is induced to grow on the surface thereof. , to obtain the nitrogen-containing precursor CaCO 3 @PDA@ZIF‑8, after high-temperature carbonization and water washing, a hollow spherical ZIF-based nitrogen-doped porous carbon material S‑NGPC‑ZIF‑8 was prepared. In the high temperature carbonization process of the present invention, the composite material CaCO 3 Calcium carbonate in @PDA@ZIF‑8 not only plays a supporting role in morphology, but the CO released by its pyrolysis 2 It also has the effect of high-efficiency pore expansion, and the evaporation of ZIF‑8 crystal zinc ions during the pyrolysis process also plays a role in secondary pore expansion. This method not only solves the problems of difficult removal and easy collapse of the shape of traditional templates, The introduction of contaminating pore expanders is also avoided.

Description

technical field [0001] The invention belongs to the technical field of material chemistry, and in particular relates to a ZIF-based nitrogen-doped porous carbon material and a preparation method thereof. Background technique [0002] In recent years, hollow spherical carbon materials have received extensive attention from scholars, mainly for the following two reasons: (1) The porous structure of the hollow spherical shape is conducive to the diffusion of gas, thereby increasing the adsorption rate; (2) The hollow volume inside the spherical shape can adapt to The shrinkage of the volume during the carbonization process has a certain anti-sintering ability. Nitrogen-doped porous carbon material refers to the carbon material obtained by doping nitrogen into the surface or inside of the porous carbon material. Nitrogen doping often improves the surface properties of the carbon material or changes the internal structure of the carbon material, thereby improving the a certain a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05B01J20/20B01J20/28B01J20/30
CPCB01J20/20C01B32/05B01J20/28B01J20/30
Inventor 童张法关浩宇贺鑫廖丹葵崔学民李立硕
Owner GUANGXI UNIV
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