Method for preparing nitrogen-containing ordered mesoporous carbon (OMC) materials based on biomass bases

A biomass and mesoporous carbon technology, applied in the preparation/purification of carbon, can solve the problems of high preparation cost and environmental pollution

Active Publication Date: 2013-12-25
ZHONGYING CHANGJIANG INTERNATIONAL NEW ENERGY INVESTMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the carbon source polymer resin used in this method is phenolic resin, urea-formaldehyde resin, etc., and a non-aqueous solvent is used, which not only causes higher preparation costs of materials, but also causes environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] at 50 o After adding NaOH aqueous solution to the system of 2.0 g cardanol and 0.2 g phenol under C and stirring for 10 min, adjust the pH of the system to 14, then add 2.45 g furfural to it and continue stirring for 10 min, and slowly raise the temperature to 75 o After C reacted for 3 h, the pH value of the solution was adjusted to 7.0 with dilute hydrochloric acid solution, at 45 o C was distilled under reduced pressure for 2 h to remove water in the system. Then dissolve in ethanol and stir evenly overnight for 12 hours, and centrifuge to remove the precipitated sodium chloride impurities to obtain an ethanol solution of phenolic condensation oligomers for use.

[0025] 3.2g linear polyethyleneimine (molecular weight 10000) and 3g nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) dissolved in 20mL 85 o In C water, after stirring for 3 hours, the structure-directing agent solution was obtained, then the ethanol solution of the above-mentioned phenolic condensation oligomer w...

Embodiment 2

[0027] at 30 o C in 2.0 g urushiol and 0.1 g phenol, add NaOH aqueous solution and stir for 10 min, adjust the pH of the system to 13, add 1.25 g furfural and continue stirring for 15 min, slowly heat up to 60 o After C reacted for 5 h, the pH of the solution was adjusted to 7.0 with dilute nitric acid solution, at 45 o C vacuum distillation 1.5 h to remove the water in the system. Dissolve in ethanol and stir evenly overnight for 12 h, and centrifuge to remove the precipitated solid impurities to obtain an ethanol solution of phenolic condensation oligomers for use.

[0028] Dissolve linear polyethyleneimine and cobalt nitrate in 30mL 75 o Stir in C water to obtain a structure-directing agent solution, the molar ratio of the cobalt nitrate and the imine group in the linear polyethyleneimine is 0.3:1, then add the ethanol solution of the above-mentioned phenolic condensation oligomer to it and mix at 75 o C is stirred evenly and then the resulting solution is transferred to...

Embodiment 3

[0030] at 25 o Add NaOH aqueous solution to 2.8g guaiacol and 0.4g phenol under C and stir for 20 minutes, adjust the pH of the system to 11, add 2.0g furfural and continue stirring for 30 minutes, 65 o After C reacted for 4 h, the pH value of the solution was adjusted to 7.0 with dilute sulfuric acid solution, and at 35 o C was distilled under reduced pressure for 2 h to remove water in the system. Dissolve in ethanol and stir evenly overnight, and centrifuge to remove the precipitated solid to obtain an ethanol solution of phenolic condensation oligomers for use.

[0031] Dissolve polyethylene glycol-linear polyethyleneimine-polyethylene glycol, aluminum nitrate in 30mL 80 o In C water, stir to obtain a structure-directing agent solution, the molar ratio of aluminum nitrate to polyethylene glycol-linear polyethyleneimine-polyethylene glycol imine group is 0.6:1, and then add phenolic condensation oligomerization The ethanol solution of the compound is mixed, and the mass ...

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Abstract

The invention relates to a method for preparing nitrogen-containing ordered mesoporous carbon (OMC) materials based on biomass bases. The method comprises the following steps of preparing a structure-directly agent solution; adding a phenolic aldehyde condensation oligomer prepared through phenolic aldehyde condensation reaction between biomass phenols instead of part of phenols and furfural to the structure-directly agent solution, heating the mixture to 75-100 DEG C, stirring the materials uniformly, then reacting at 100-200 DEG C for 6-72 hours, filtering and drying the reactant, then roasting the reactant at 350-500 DEG C for 1-3 hours in an inert atmosphere, then carrying out acid pickling and drying and then carrying out high temperature carbonization at 600-900 DEG C for 1-5 hours under the protection of the inert atmosphere, thus obtaining the nitrogen-containing OMC materials. The method has the advantages that cheap regenerable biomass phenols are adopted instead of part of phenols, thus solving the problem of current energy regeneration; the structure-directly agent solution formed by adopting combined action of a specific metal ion compound and a polymer containing imidogen can be used for regulating the specific surface area according to the actual requirements.

Description

technical field [0001] The invention relates to the field of preparation of ordered mesoporous carbon materials, in particular to a method for preparing nitrogen-containing ordered mesoporous carbon materials based on biomass. Background technique [0002] Due to their large specific surface, controllable structure and morphology, excellent thermal and chemical stability, mesoporous carbon materials are widely used in the fields of electrode materials, energy storage, gas separation, catalysts and chromatographic column packing. Since the structurally ordered mesoporous carbon was first reported in 1999, the synthesis of new mesoscopically ordered carbon materials has attracted more and more attention. A series of ordered mesoporous carbons with different structures and morphologies have been synthesized by using various mesoporous silica templates with different structures and carbon sources. [0003] However, this synthetic route has many steps and is too cumbersome, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 方章建张岩丰郑兴才程宇婷陶磊明
Owner ZHONGYING CHANGJIANG INTERNATIONAL NEW ENERGY INVESTMENT CO LTD
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