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Preparation method of epoxy modified high-ortho-position thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane

A technology of activated carbon fiber membrane and epoxy modification, which is used in heating/cooling fabrics, non-woven fabrics, textiles and papermaking, etc. high performance, high para-activity, and simple preparation process

Active Publication Date: 2018-12-07
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention aims at the problems of long curing time, many procedures, high cost and environmental pollution of thermoplastic phenolic resins, low molecular weight of thermosetting phenolic resins and poor spinnability, tedious preparation of phenolic-based hollow activated carbon fibers, high cost, heavy environmental pollution, and difficulty in large-scale production. In order to solve the problem of area application, and further improve the mechanical properties of phenolic-based hollow activated carbon fibers, use phenols, aldehydes, and epoxy haloalkanes to react under the action of catalysts to obtain epoxy-modified high-ortho-position phenolic resins, and react with aldehydes to obtain rings Oxygen-modified high-ortho thermosetting phenolic resin, a continuous and flexible epoxy-modified high-ortho thermosetting phenolic-based hollow nano-activated carbon fiber prepared by coaxial electrospinning

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method of epoxy-modified high-ortho-position thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane, the steps are as follows:

[0023] (1) Heat phenol, formaldehyde and epichlorohydrin to 92°C under the action of catalyst zinc acetate, add the second catalyst oxalic acid after reacting for 1 hour, and react for another hour; dehydration under reduced pressure, the vacuum degree is at 8000Pa, the temperature at this stage is first Drop to 30 DEG C, gradually heat up to 100 DEG C, constant temperature 0.2h, obtain epoxy modified high ortho thermal phenolic resin; Wherein phenol: the molar ratio of formaldehyde is 1:0.8, phenols: the mass ratio of epichlorohydrin is 100:5, phenol: zinc acetate: the mass ratio of oxalic acid is 100:0.5:0.5;

[0024] (2) The obtained epoxy-modified high-ortho phenolic resin was dissolved in methanol, then added formaldehyde and reacted at 45°C for 2.5h under the action of catalyst triethanolamine, co...

Embodiment 2

[0028] A preparation method of epoxy-modified high-ortho-position thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane, the steps are as follows:

[0029] (1) Heat m-cresol, acetaldehyde, and epibromopropane under the action of catalyst zinc acetate to 98°C, add the second catalyst sulfuric acid after reacting for 2 hours, and react for another hour; dehydration under reduced pressure, the vacuum degree is 6000Pa, this The stage temperature first drops to 40°C, then gradually rises to 110°C, and keeps the temperature for 1 hour to obtain epoxy-modified high-ortho-position phenolic resin; wherein the molar ratio of m-cresol: acetaldehyde is 1:1.2, phenols: epoxybromopropane The mass ratio is 100:10, m-cresol: zinc acetate: sulfuric acid is 100:0.5:0.5;

[0030] (2) The obtained epoxy-modified high-ortho phenolic resin was dissolved in ethanol, then added acetaldehyde and reacted at 50°C for 4 hours under the action of catalyst barium acetate, cooled...

Embodiment 3

[0034] A preparation method of epoxy-modified high-ortho-position thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane, the steps are as follows:

[0035] (1) Heat phenol, m-cresol, paraformaldehyde and epichlorobutane under the action of zinc oxide catalyst to 105°C, add the second catalyst sulfuric acid after reacting for 3 hours, and react for 1.5 hours; dehydration under reduced pressure, vacuum The temperature is at 4000Pa. At this stage, the temperature first drops to 50°C, then gradually rises to 120°C, and keeps the temperature for 2 hours to obtain epoxy-modified high-ortho-position phenolic resin; wherein phenol:m-cresol:paraformaldehyde (according to the aldehyde functional group contained Total) molar ratio is 0.5:0.5:01.4, phenols: the mass ratio of epoxy chlorobutane is 100:20, m-cresol: zinc oxide: the mass ratio of sulfuric acid is 50:0.8:0.4;

[0036] (2) The obtained epoxy-modified high-ortho phenolic resin was dissolved in methan...

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Abstract

The invention discloses a preparation method of an epoxy modified high-ortho-position thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane. The preparation method comprises the following steps that phenol compounds, aldehyde compounds and epoxy haloalkane react under the function of a catalyst to prepare epoxy modified high-ortho-position phenolic resin; the epoxy modified high-ortho-position phenolic resin is dissolved in alcohol compounds and reacts with aldehyde compounds under the function of a catalyst to prepare epoxy modified high-ortho-position thermosetting phenolic resin; the epoxy modified high-ortho-position thermosetting phenolic resin serves as a carbon precursor solution, coaxial static electricity spinning is adopted, heating curing is conductedto obtain an epoxy modified high-ortho-position thermosetting phenolic fiber membrane the peel and core of which are partially dissolved; then carbonization and activation are conducted under the protection of inert gas to obtain the epoxy modified high-ortho-position thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane. Compared with the prior art, the method has theadvantages that the process is simple, the method is environmentally friendly, the structure is controllable, the spinnability of a stock solution is good, the curing rate is high, and the mechanicalproperty is high.

Description

technical field [0001] The invention belongs to the field of preparation of special carbon materials, and specifically relates to the use of epoxy-modified high-ortho-position thermosetting phenolic resin as a carbon precursor to obtain epoxy-modified high-ortho-position phenolic groups through coaxial electrospinning, curing, carbonization, and activation. Preparation method of hollow nano activated carbon fiber membrane. Background technique [0002] Due to its hollow structure, high ortho-position thermosetting phenolic-based activated carbon fibers have higher specific surface area, better adsorption performance, electrochemical properties, mechanical properties and thermal insulation properties than ordinary phenolic-based activated carbon fibers, and solve the problem of thermoplastic phenolic resins. The problems of long curing time, many processes, high cost and environmental pollution, as well as the problems of low molecular weight and poor spinnability of thermose...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D04H1/728D04H1/4382D04H1/4391D06C7/04C08G8/10C08G8/28C08G8/04C08G8/12C08G8/24
CPCC08G8/04C08G8/10C08G8/12C08G8/24C08G8/28D04H1/4382D04H1/4391D04H1/728D06C7/04
Inventor 曹健张彩云杨凯刁泉刘淑萍任东雪米立伟余木火
Owner ZHONGYUAN ENGINEERING COLLEGE
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