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Method for preparing mesoporous boron nitride with uniform pores by adopting molten mass bubble template process

A template method and boron nitride technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve problems such as complex process, template residue, and difficulty in obtaining regular mesoporous boron nitride materials, and achieve a simple technical route , Reagents are cheap and easy to obtain, and the technical difficulty is small

Active Publication Date: 2018-07-13
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the raw material used in the chemical foaming method is expensive ammonia borane, and the specific surface area of ​​the generated porous boron nitride is less than 150m 2 / g; while the traditional template used in the template method needs to pre-process the template, and then remove the template, the process is complicated, and there will be template residue
The preparation routes of these porous boron nitrides are affected by organic boron and nitrogen sources and hard templates, and it is difficult to use bulk commercial boron and nitrogen sources to obtain regular mesoporous boron nitride materials (such as 10 grams or more) on a larger scale There are difficulties, which restrict the research and application exploration of mesoporous boron nitride in the fields of hydrogen energy storage, carbon dioxide adsorption, and environmental damage reduction such as oil spills and wastewater.

Method used

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  • Method for preparing mesoporous boron nitride with uniform pores by adopting molten mass bubble template process
  • Method for preparing mesoporous boron nitride with uniform pores by adopting molten mass bubble template process
  • Method for preparing mesoporous boron nitride with uniform pores by adopting molten mass bubble template process

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Take 100 grams of boric acid, 400 grams of urea and 1 gram of ferric nitrate and mix them evenly, raise the temperature in an electric furnace to 300 degrees Celsius at a rate of 10 degrees Celsius / min and keep it for 20 minutes to obtain a precursor, and then cure it at 700 degrees Celsius for 1 minute. Put the precursor into the graphite boat nitrogen-hydrogen mixture (5wt% H 2 / N 2 ) under the protection of the atmosphere, the temperature was raised to 1000°C at a heating rate of 10°C / min, and the crude product was obtained by keeping the temperature for 2 hours. Then the crude product was placed in 500 ml of 0.5 mol / L hydrochloric acid and stirred at 60°C for 2 hours. The product was filtered, washed with deionized water and ethanol, and dried for 12 hours. 40 g of product were obtained.

[0033] figure 1 Show that the obtained product is pure boron nitride, figure 2 It is a transmission electron microscope photo of the obtained product. It can be seen that t...

Embodiment 2

[0035] Take 100 grams of boric acid, 270 grams of urea, 30 grams of ammonium carbonate and 2 grams of cobalt nitrate and mix them evenly, heat them up to 220 degrees Celsius at a heating rate of 10 degrees Celsius / min and keep them warm for 2 hours in an electric furnace to obtain a precursor, which will be cured at 700 degrees Celsius for 10 minute. Put the precursor into the graphite boat nitrogen-hydrogen mixture (2 wt. %H 2 / N 2 ) under the protection of the atmosphere, the temperature was raised to 1000°C at a heating rate of 10°C / min, and the crude product was obtained by keeping the temperature for 2 hours. Then the crude product was placed in 500 ml of 3 mol / L hydrochloric acid and stirred at 40°C for 4 hours. The product was filtered, washed with deionized water and ethanol, and dried. The specific surface area of ​​the sample was measured to be 220 m 2 / g, the most probable pore diameter is 25nm, and the pore size mainly ranges from 8 to 50 nm.

Embodiment 3

[0037] Take 10 grams of boric acid, 90 grams of boron oxide powder, 800 grams of urea, and 5 grams of ferric nitrate and mix them evenly. Heat the temperature in an electric furnace to 500 degrees Celsius for 6 minutes at a heating rate of 10 degrees Celsius / min, and then cure at 700 degrees Celsius for 20 minutes. Put the precursor into the graphite boat nitrogen-hydrogen mixture (20wt.% NH 3 / N 2 ) under the protection of an atmosphere, the temperature was raised to 900°C at a heating rate of 10°C / min, and the crude product was obtained by keeping the temperature for 3 hours. Then the crude product was placed in 500 ml of 1 mol / L hydrochloric acid and stirred at 50°C for 4 hours. The product was filtered, washed with deionized water and ethanol, and dried for 12 hours. The specific surface area of ​​the obtained product was 150 m 2 / g, TEM picture see Figure 5 . The most probable pore diameter is 23 nm, and the pore size mainly ranges from 8 to 50 nm.

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Abstract

The invention discloses a method for preparing mesoporous boron nitride with uniform pores by adopting a molten mass bubble template process. The method comprises the following steps: mixing a nitrogen source, a boron source and an additive; keeping a temperature of 220 to 500 DEG C for 0.1 to 2 hours; subsequently, keeping the temperature of 700 DEG C for 1 to 20 minutes; forming pores to obtaina precursor; performing pyrolysis at 900 to 1300 DEG C in nitrogen, hydrogen-nitrogen mixed gas or nitrogen-ammonia mixed gas to obtain a rough product; washing the rough product in hydrochloric acidand filtering; cleaning the product with deionized water and ethanol to obtain porous boron nitride powder. The method disclosed by the invention has the advantages that a product specific surface area is 150 to 600m<2> / g, the most probable size of apertures is 18 to 25nm, a technological route is simple, and the method is suitable for mass preparation.

Description

technical field [0001] The invention belongs to the preparation technology of porous boron nitride, and in particular relates to a method for preparing mesoporous boron nitride with uniform pore size distribution and high specific surface area as a nano-bubble template in a molten body. Background technique [0002] Porous boron nitride with excellent chemical stability, thermal stability and excellent oxidation resistance. At the same time, it also has the characteristics of low density, high porosity, and large specific surface area. It has great application value in sewage treatment, gas adsorption (purification), hydrogen storage, catalyst carrier, and non-metallic catalysis. It is a research topic at home and abroad in recent years. one of the focus of attention. However, at present, bulk commercialized hexagonal boron nitride is mainly micron-sized products, and the specific surface area is mostly less than 20㎡ / g, and porous boron nitride with large specific surface a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064
CPCC01B21/064C01P2004/04C01P2002/72C01P2006/12C01P2006/17C01P2006/16
Inventor 王连成吕宝亮杨夕丁瑞敏
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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