A kind of preparation method of high ortho thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane

A technology of activated carbon fiber membrane and high ortho position, which is applied in fiber processing, fiber chemical characteristics, textiles and papermaking, etc., can solve the problems of cumbersome preparation of phenolic-based hollow activated carbon fibers, low molecular weight of thermosetting phenolic resin, and difficulty in large-area application. Achieve the effect of high molecular weight, high para-activity and high spinnability

Active Publication Date: 2020-04-24
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims at the problems of long curing time, multiple curing processes, high cost and environmental pollution of thermoplastic phenolic resins, of low molecular weight and poor spinnability of thermosetting phenolic resins, and tedious preparation of phenolic-based hollow activated carbon fibers, high cost, heavy environmental pollution, It is difficult to apply in a large area. Using phenols and aldehydes to react under the action of a catalyst, a high-ortho-position phenolic resin is obtained, and reacted with aldehydes to obtain a high-ortho-position thermosetting phenolic resin. A coaxial electrospinning method is used to prepare a Preparation method of continuous, flexible and high-ortho thermosetting phenolic-based hollow nano-activated carbon fibers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of preparation method of high ortho-position thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane, the steps are as follows:

[0026] (1) Heat phenol and formaldehyde to 98°C under the action of the first catalyst zinc acetate, add acid catalyst oxalic acid after reacting for 1 hour, and react for another 0.5 hour; dehydration under reduced pressure, the vacuum degree is at 8000Pa, and the temperature at this stage drops to 30°C for 0.2h, then gradually warming up to 100°C for 0.3h, constant temperature for 0.5h to obtain a high ortho thermal phenolic resin; wherein the molar ratio of phenol:formaldehyde is 1:0.8, the mass of phenol:zinc acetate:oxalic acid The ratio is 100:0.5:0.5;

[0027](2) The obtained high ortho phenolic resin was dissolved in methanol, then added formaldehyde and reacted at 45°C for 3 hours under the action of the second catalyst triethanolamine, cooled down to room temperature, added hydrochloric acid to make ...

Embodiment 2

[0031] A kind of preparation method of high ortho-position thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane, the steps are as follows:

[0032] (1) Heat p-cresol and acetaldehyde to 98°C under the action of the first catalyst zinc acetate, react for 2 hours, add acid catalyst sulfuric acid, and react for another 1 hour; dehydration under reduced pressure, the vacuum degree is at 6000Pa, the temperature at this stage is first Drop to 40°C for 0.5h, then gradually raise the temperature to 110°C for 0.5h, keep the temperature for 1h to obtain high ortho phenolic resin; wherein the molar ratio of p-cresol: acetaldehyde is 1:1.2, p-cresol: acetic acid Zinc: sulfuric acid is 100:0.5:0.5;

[0033] (2) The obtained high ortho phenolic resin was dissolved in ethanol, then added acetaldehyde and reacted at 50°C for 4 hours under the action of the second catalyst barium acetate, cooled to room temperature, added sulfuric acid to make the pH = 5.5, and fil...

Embodiment 3

[0037] A kind of preparation method of high ortho-position thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane, the steps are as follows:

[0038] (1) Heat phenol, p-cresol and paraformaldehyde to 105°C under the action of the first catalyst zinc oxide, add acid catalyst sulfuric acid after reacting for 3 hours, and react for another 1.5 hours; vacuum dehydration, vacuum degree is 4000Pa, At this stage, the temperature first drops to 50°C for 1 hour, then gradually increases the temperature to 120°C for 1 hour, and keeps the temperature for 2 hours to obtain a high ortho-position phenolic resin; among them, phenol: p-cresol: paraformaldehyde (according to the aldehyde functional group contained) The mol ratio is 0.5:0.5:01.4, p-cresol: zinc oxide: the mass ratio of sulfuric acid is 50:0.8:0.4;

[0039] (2) The obtained high-ortho phenolic resin was dissolved in methanol, then paraformaldehyde was added to react at 55°C for 5 hours under the action...

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Abstract

The invention discloses a manufacturing method for a high-ortho thermosetting phenolic-aldehyde based hollow nano-gradient activated carbon fiber film. The method comprises the following steps: makingphenols and aldehyde compounds react under the action of a catalyst, to manufacture a high-ortho phenolic resin; dissolving the high-ortho phenolic resin in alcohols, and reacting with an aldehyde compound under the action of a catalyst, to manufacture a high-ortho thermosetting phenolic resin; using the high-ortho thermosetting phenolic resin as a carbon precursor solution, using coaxial electrospinning, heating and curing to obtain high-ortho thermosetting phenolic fiber films whose skin-core structures are partially miscible; then performing carbonization and activation under protection ofinert gas, to obtain the high-ortho thermosetting phenolic-aldehyde based hollow nano-gradient activated carbon fiber film. Compared with the prior art, the method is advantaged by simple process, friendly environment, and controllable structure.

Description

technical field [0001] The invention belongs to the field of preparation of special carbon materials, and specifically relates to a method for preparing a phenolic-based hollow nano-activated carbon fiber membrane by using a high-ortho-position thermosetting phenolic resin as a carbon precursor through coaxial electrospinning, curing, carbonization, and activation. Background technique [0002] Phenolic-based hollow activated carbon fiber has physical and chemical properties such as high specific surface area, low density, high strength and chemical stability, and has become one of the extremely important development directions in the field of materials. However, ordinary phenolic resins have unavoidable defects as carbon precursors. Thermoplastic phenolic resins have the problems of long curing time, multiple curing processes, high cost and environmental pollution, while thermosetting phenolic resins have low molecular weight and poor spinnability. Compared with solid activ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D04H1/728D01D5/00D01F9/24
CPCD01D5/0015D01F9/24D04H1/728
Inventor 焦明立张彩云何建新刁泉宋梦曹健拱荣华任东雪
Owner ZHONGYUAN ENGINEERING COLLEGE
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