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Millimeter-scale nitrogen-doped porous carbon sphere as well as preparation and application thereof

A nitrogen-doped porous carbon, millimeter-scale technology, applied in the preparation/purification of carbon, other chemical processes, chemical instruments and methods, etc., can solve the problems affecting the recycling and regeneration of carbon materials, the limitation of use scenarios, and the lack of regulation of performance. Achieve the effect of improving yield and mechanical strength, broad market prospects, and low requirements for equipment conditions

Pending Publication Date: 2022-03-08
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the high-efficiency assembly of lignin and chitosan to prepare functional biomass materials is regarded as a promising method for the utilization of biomass resources, for example, chitosan / lignin blend degradable film (patent CN 101220176B) , lignin-chitosan porous scaffold material (patent CN 111760074 A), sodium alginate-lignin composite beads (patent CN 110947368A), magnetic chitosan lignosulfonate graphene oxide adsorbent (patent CN 105251466 A), lignin xanthate bentonite composite ball (patent CN 106582550 A), chitosan / lignin composite organic material (Int.J.Biol.Macromol.2019,132,1304-1317; Chem.Eng.J .2014,254,491-502.), chitosan / lignin composite sponge (Environ.Sci.Nano 2020,7(3):793-802.), but lignin / chitosan composite microbeads and their There are few research reports on the preparation of derivatized porous carbon (spheres) and its adsorption of environmental pollutants, and the carbon materials derived from lignin / chitosan composites are generally carbon powders, which have certain limitations in their application scenarios
[0004] To sum up, the current technical methods still have: 1) Biomass-based porous carbon (spheres) has disadvantages such as long preparation cycle, high energy consumption, low and uneven distribution of heteroatoms, and lack of performance control, which cannot meet practical applications. 2) The preparation process of related carbon materials is easy to pulverize, and the particle size of the prepared carbon materials is small, making it more difficult to separate after adsorption in the solution, which in turn affects the cycle of carbon materials regeneration

Method used

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  • Millimeter-scale nitrogen-doped porous carbon sphere as well as preparation and application thereof
  • Millimeter-scale nitrogen-doped porous carbon sphere as well as preparation and application thereof
  • Millimeter-scale nitrogen-doped porous carbon sphere as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085](1) Weigh 2.0g sodium lignosulfonate and 2.0g chitosan in a beaker, add 30mL distilled water to disperse, then add 15mL of 2mol / L hydrochloric acid solution, stir it in a water bath at room temperature for 1h It is fully dissolved to obtain suspension A, and then under the condition of 20r / min magnetic stirring, at a rate of 2 drops / s, the height of the droplet is 2cm from the liquid surface, and 100mL of hydrogen with a mass concentration of 8% is added dropwise Carry out gel self-assembly in the potassium oxide solution, after the dropwise addition, stand and solidify for 10 hours, filter and separate to obtain wet gel microbeads;

[0086] (2) Mix the wet gel beads with a certain amount of water, and then filter, which can be repeated several times until the pH of the filtrate is 7, and the solid is then subjected to vacuum freeze-drying for 20 hours to obtain the precursor xerogel beads, which are dried and stored for later use .

[0087] (3) Weigh 2.0 g of xerogel b...

Embodiment 2

[0090] (1) Weigh 2.0g sodium lignosulfonate and 2.0g chitosan in a beaker, add 30mL distilled water to disperse, then add 20mL of 3mol / L hydrochloric acid solution, stir it in a water bath at room temperature for 1h It is fully dissolved to obtain a suspension A, and then under the condition of 20r / min magnetic stirring, at a rate of 2 drops / s, the height of the droplet is 1cm from the liquid surface, and 100mL of hydrogen with a mass concentration of 9% is added dropwise Carry out gel self-assembly in the potassium oxide solution, after the dropwise addition, stand and solidify for 10 hours, filter and separate to obtain wet gel microbeads;

[0091] (2) Mix the wet gel beads with water, and then filter, which can be repeated several times until the pH of the filtrate is 8, and the solid is then subjected to vacuum freeze-drying for 20 hours to obtain the precursor xerogel beads, which are dried and stored for later use.

[0092] (3) Weigh 2.0 g of xerogel balls and place them...

Embodiment 3

[0094] (1) Weigh 1.0g sodium lignosulfonate and 3.0g chitosan in a beaker, add 50mL distilled water to disperse, then add 20mL of 3mol / L hydrochloric acid solution, stir it in a water bath at room temperature for 1h It is fully dissolved to obtain a suspension A, and then under the condition of 20r / min magnetic stirring, at a rate of 2 drops / s, the height of the droplet is 3cm from the liquid surface, and 100mL of hydrogen with a mass concentration of 9% is added dropwise Carry out gel self-assembly in the potassium oxide solution, after the dropwise addition, stand and solidify for 10 hours, filter and separate to obtain wet gel microbeads;

[0095] (2) The wet gel beads were mixed with water, and then filtered until the pH of the filtrate was 7, and the solid was vacuum freeze-dried for 20 hours to obtain the precursor xerogel beads, which were dried and stored for later use.

[0096] (3) Weigh 2.0 g of xerogel balls and place them in a horizontal tubular reactor under the c...

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Abstract

The invention belongs to the field of preparation of carbon adsorbents, and particularly provides a preparation method of millimeter-scale nitrogen-doped porous carbon spheres, a mixed solution A dissolved with lignin, chitosan and acid is obtained, then the mixed solution A is dropwise added into an alkali solution under the stirring condition for self-assembly, solid-liquid separation is performed after standing and curing, and lignin-chitosan gel microspheres are obtained; treating the gel microspheres by using a water-containing solvent, and then carrying out solid-liquid separation to obtain a solid and a solution with the pH value of 7-9; carrying out vacuum freeze drying treatment on the solid to obtain precursor spheres; the water-containing solvent is water or a mixed solvent of water and an organic solvent, and the organic solvent is a solvent capable of being mixed and dissolved with water; and performing pyrolysis carbonization on the precursor spheres at the temperature of 500-800 DEG C in a protective atmosphere, and then washing and drying a carbonized product to obtain the nitrogen-doped porous carbon spheres. The method can be used for preparing the millimeter-scale carbon spheres with excellent adsorption performance.

Description

technical field [0001] The invention belongs to the technical field of preparation of porous carbon materials, and in particular relates to the preparation of a millimeter-scale nitrogen-doped porous carbon sphere adsorption material. Background technique [0002] In recent years, highly toxic phenolic compounds, such as phenol, p-nitrophenol, o-nitrophenol, o-aminophenol, etc., produced in chemical, pharmaceutical, cosmetic, and dye industries, can be harmful to organisms even at low concentrations. May cause harmful effects which need to be removed before discharge to the aquatic environment. At the same time, in order to meet the needs of the country's "carbon neutrality" and "carbon peaking", CO 2 Efficient capture, storage and transformation of ions are also of great significance. Green and clean nuclear energy, as a new energy source that is currently attracting attention, is also one of the main sources of electric energy. However, the radioactive iodine nuclides di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/02B01D53/04B01J20/30C01B32/05C02F1/28C02F101/20C02F101/30
CPCB01J20/02B01D53/04C02F1/281C01B32/05B01J20/3078B01D2257/504B01D2257/708B01D2257/202B01D2258/0283C02F2101/20C02F2101/30Y02C20/40
Inventor 邵礼书刘子辉徐润峰陈介南罗卫华詹鹏张林彭婉婷田斌斌甘柏瑶
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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