Preparation method of porous carbon microsphere

A technology of porous carbon and microspheres, which is applied in the field of preparation of porous carbon microspheres, can solve the problems of cumbersome and unsatisfactory preparation methods, and achieve the effects of cheap preparation of raw materials, uniform particle size and no special equipment requirements.

Inactive Publication Date: 2014-02-12
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the membrane emulsification method and the template method can prepare carbon microspheres with uniform particle size, but the former requires a special membrane material with uniform pore size and corresponding devices, and the latter needs to prepare porous silica microspheres with uniform particle size in advance. The method is cumbersome
Present various preparation methods all have such and such shortcomings, are not ideal

Method used

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  • Preparation method of porous carbon microsphere
  • Preparation method of porous carbon microsphere
  • Preparation method of porous carbon microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Porous carbon microspheres with an average particle size of 8.1 μm

[0033] Include the following six steps in order:

[0034] ① Mix 2.20g catechol, 2.03g formaldehyde aqueous solution (37wt%), and 19.2g silica sol (36nm, 16.2wt%) evenly, and adjust the pH to 1.60 with hydrochloric acid.

[0035] ② Under the protection of nitrogen, the reaction was rapidly stirred at 60°C. The reaction was monitored with an optical microscope until the microspheres no longer grew larger, then the reaction was stopped and cooled to room temperature.

[0036] ③ Centrifuge the suspension obtained in step ②, wash the precipitate three times with distilled water, dry it in vacuum at 110°C for 8 hours, and cool to room temperature.

[0037] ④ The above dried composite microspheres were sintered at high temperature under the protection of nitrogen. The sintering steps are as follows: raise the temperature from room temperature to 350°C within 30 minutes, keep at 350°C for 2 h...

Embodiment 2

[0040] Example 2: Porous carbon microspheres with an average particle size of 4.5 μm

[0041] Include the following six steps in order:

[0042] ① Mix 2.75 g catechol, 2.03 g formaldehyde aqueous solution (37wt%), and 23.0 g silica sol (36nm, 16.2wt%) evenly, and adjust the pH to 1.80 with hydrochloric acid.

[0043]② Under the protection of nitrogen, the reaction was rapidly stirred at 60°C. The reaction was monitored with an optical microscope until the microspheres no longer grew larger, then the reaction was stopped and cooled to room temperature.

[0044] ③ Centrifuge the suspension obtained in step ②, wash the precipitate three times with distilled water, dry it in vacuum at 110°C for 8 hours, and cool to room temperature.

[0045] ④ The above dried composite microspheres were sintered at high temperature under the protection of nitrogen. The sintering steps are as follows: raise the temperature from room temperature to 350°C within 30 minutes, keep at 350°C for 2...

Embodiment 3

[0048] Example 3: Porous carbon microspheres with an average particle size of 7.8 μm

[0049] ① Mix 1.50g catechol, 1.37g formaldehyde aqueous solution (37wt%), and 19.2g silica sol (100nm, 13.5wt%) evenly, and adjust the pH to 1.60 with sulfuric acid.

[0050] ② Under the protection of nitrogen, the reaction was rapidly stirred at 60°C. The reaction was monitored with an optical microscope until the microspheres no longer grew larger, then the reaction was stopped and cooled to room temperature.

[0051] ③ Centrifuge the suspension obtained in step ②, wash the precipitate three times with distilled water, dry it in vacuum at 110°C for 8 hours, and cool to room temperature.

[0052] ④ The above dried composite microspheres were sintered at high temperature under the protection of nitrogen. The sintering steps are as follows: raise the temperature from room temperature to 350°C within 30 minutes, keep at 350°C for 2 hours, continue to raise the temperature, rise to 600°C ...

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Abstract

The invention discloses a preparation method of a porous carbon microsphere. The preparation method comprises the following steps: subjecting o-dihydroxybenzene and formaldehyde to carry out polymerization reactions in a silica sol solution under the catalytic action of acid so as to obtain compound microspheres of o-dihydroxybenzene-formaldehyde resin-oxidized nano particles, and then subjecting the compound microspheres to the processes of carbonization and silicon oxide removing so as to obtain porous carbon microspheres with a even particle size. The size of the porous carbon microsphere is in a micron scale range; the porous carbon microsphere has a good spherical shape and a rough surface, is rich in medium holes with a size of 10 to 40 nanometers, integrally has two hole structures, namely the medium hole and the micro hole, and has a large specific surface area. The porous carbon microsphere has a high purity, and the carbon content can reach 95% or more.

Description

technical field [0001] The invention belongs to a method for preparing porous carbon microspheres, in particular to a method for preparing catechol and formaldehyde resin polymer-silica gel nanoparticle composite microspheres by using modified polymerization-induced colloid aggregation and converting them into porous carbon microspheres. Background technique [0002] Porous carbon materials have a series of excellent characteristics such as low density, high strength, high temperature resistance, chemical corrosion resistance, radiation resistance, high electrical conductivity, small expansion coefficient, and good biocompatibility of general carbon materials, and at the same time have porous and large specific surface area. Its structural properties are widely used in the fields of adsorption materials, catalyst supports, battery electrode materials, supercapacitors and composite materials. Compared with bulk materials and uneven powder materials, spherical porous carbon ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 刘霞魏征蒋生祥王立成
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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