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Nitrogen-doped spherical porous carbon, its preparation method and its application

A technology of porous carbon and nitrogen doping, applied in the field of coal chemical industry, can solve the problem of low yield of carbon materials, and achieve the effect of wide sources, high nitrogen content, and high pelleting rate

Active Publication Date: 2021-12-07
CHNA ENERGY INVESTMENT CORP LTD +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Nitrogen-doped porous carbons have been prepared directly from conventional imidazolium cationic ionic liquids. It has been reported that the main defect is that the yield of carbon materials is low (generally less than 30%, lower than pitch)

Method used

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  • Nitrogen-doped spherical porous carbon, its preparation method and its application

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preparation example Construction

[0022] As described in the background art, in a conventional ionic liquid imidazolium cation Preparation of Nitrogen-doped carbon present low yield and low specific surface area of ​​the porous carbon problems method. In order to solve the above problems, the present application provides a method for producing a nitrogen-doped spherical porous carbon, the production method comprising: a coal liquefaction process and bitumen sulfonated sequentially hydration treatment to obtain a soluble sulfonated asphalt; the soluble sulfo asphalt, water and a cationic ion-imidazol-liquid mixing to obtain a mixture, an imidazolium cation is the imidazolium cation ionic liquid bromine or chloride salt; the mixture was spray-dried to obtain spherical granules pitch; and in a nitrogen or inert gas under the protection of the spherical particles pitch carbonization and activation sequence to give spherical porous carbon doped with nitrogen.

[0023] The above preparation method, using relatively inex...

Embodiment 1

[0040] The 1500g particle diameter is less than 0.2 mm, and the ash is 0.001%, the softening point is 110 ° C, the coolification value of 50%, after 98% concentrated sulfonation, then dissolved by ion water, centrifugation is not soluble. The solid solids were obtained, and the soluble sulfonated asphalt was evaporated.

[0041] The soluble sulfonated asphalt was dissolved in a certain amount of deionized water, prepared a concentration of 20% sulfonated asphalt aqueous solution A. In the sulfonated asphalt aqueous solution A, 952 g of 1-acetonitrile-3-butylimazole cationic chloride ([CMBIM] CL) was added in accordance with mass ratio 1: 1 (ionic liquid: soluble sulfonated asphalt), and after stirring, dissolved, Get a mixed solution B.

[0042] By pump pressing, the mixed solution B is pressed into the spray drying tower in the feed temperature of 80 ° C, the feed pressure is 20 MPa, and the 528g spherical degree is collected from the bottom of the tower, and the particle size is...

Embodiment 2

[0045] The 1800g particle diameter is less than 0.2 mm, and the ash is 0.009%, the softening point is 131 ° C, the coal liquidification bitumen having a cocuplex value is 52.6%, and after 98% concentrated sulfonation, it is dissolved by ion water, and the centrifugation is dissolved. The solid solids were obtained, and the soluble sulfonated asphalt was evaporated.

[0046] The soluble sulfonated asphalt was dissolved in a certain amount of deionized water, prepared a sulfonated asphalt aqueous solution A having a concentration of 17%. In the sulfonated asphalt aqueous solution A, 345 g of 1-vinyl-3-acetonitrile primary immeolam cationic bromide salt ([CMVIM] BR) was added in accordance with mass ratio 1: 3 (ionic liquid: soluble sulfonated asphalt), and after stirring, dissolve, Get a mixed solution B.

[0047] By pumping pressure delivery, the mixed solution B is pressed into the spray drying tower in the feed temperature, the mixed solution B is pressed into the spray drying to...

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Abstract

The invention provides a nitrogen-doped spherical porous carbon, its preparation method and application. The preparation method comprises: sequentially performing sulfonation treatment and hydration treatment on coal liquefaction asphalt to obtain soluble sulfonated asphalt; mixing soluble sulfonated asphalt, water and imidazolium cationic ionic liquid to obtain a mixed solution, imidazolium cationic ionic liquid It is bromide or chloride salt of imidazolium cation; the mixed solution is spray-dried to obtain spherical asphalt particles; and under the protection of nitrogen or inert gas, the spherical asphalt particles are sequentially carbonized and activated to obtain nitrogen-doped spherical porous carbon. Nitrogen-doped spherical porous carbon prepared from imidazolium cation bromide or chloride salt has a high nitrogen content, and the preparation process by spray drying technology has simple steps, strong continuous operability, high production efficiency, and ball formation rate High, high sphericity and adjustable microsphere particle size, so the above-mentioned spheroidization process can improve the yield and specific surface area of ​​porous carbon.

Description

Technical field [0001] The present invention relates to coal chemical industry, particularly, to a nitrogen-doped spherical porous carbon, their preparation and their use. Background technique [0002] The residue is the non-target coal liquefaction products of coal liquefaction process, about 30% of the administered amount of coal is a high ash, high sulfur and high calorific value material, mainly non-liquefied oil distillate (n-hexane solubles) , asphaltene (n-hexane-soluble matter insoluble in tetrahydrofuran), and the inorganic composition is not coal conversion. Unconverted 30%, accounting for the total amount of the residue insoluble in tetrahydrofuran of organic residue refers to coal, the coal is mainly composed of inorganic minerals and the applied catalyst composition, about 20% of the total residue. Non-liquefied oil distillate and about 50% asphaltenes in the residue, mainly composed of condensed polycyclic aromatic hydrocarbons having a high aromatic carbon content ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/336C01B32/348C01B32/33H01G11/34H01G11/24B01J32/00A61M1/36
CPCC01B32/336C01B32/348C01B32/33H01G11/34H01G11/24B01J27/24A61M1/3679A61M1/3621A61M2202/0413A61M2202/0021Y02E60/13
Inventor 程时富常鸿雁向柠辛凡文章序文李克健舒歌平
Owner CHNA ENERGY INVESTMENT CORP LTD
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