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

An activated carbon fiber membrane, boron modification technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problems affecting the adsorption performance of activated carbon materials, long curing cycle of thermoplastic phenolic, low molecular weight of thermosetting phenolic, etc. Improve initial decomposition temperature, high molecular weight, high para-activity

Active Publication Date: 2020-01-10
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Phenolic resin has many advantages as a carbon precursor, but its heat resistance is relatively poor. In addition, thermoplastic phenolic resin has long curing cycle, many processes, high cost and pollutes the environment. Thermosetting phenolic resin has low molecular weight and poor spinnability.
[0003] At present, the methods for preparing phenolic-based hollow activated carbon fibers include semi-solidification-dissolution method and special-shaped spinneret spinning method, but the prepared fibers are relatively thick, the preparation is cumbersome, the cost is high, the environment is heavy, and it is difficult to apply coaxial electrospinning in large areas. The silk method can solve the above problems very well.
Although the coaxial electrospinning method has been widely used in the preparation and production of various polymer-based micro-nano hollow fibers, it has not been applied to the spinning of high-ortho thermosetting phenolic resins.
At the same time, regardless of the traditional spinning method or electrospinning, the pore size distribution of the obtained hollow activated carbon fiber is uniform, and the size of the pores on the inner and outer walls of the fiber remains unchanged, which affects the adsorption performance of the activated carbon material.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A method for preparing a high-ortho boron-modified thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane, the steps are as follows:

[0023] (1) Boil phenol, formaldehyde and boric acid under the action of zinc acetate for 2 hours, add concentrated sulfuric acid dropwise to continue the reaction for 0.5 hours, dehydrate under reduced pressure, cool down to 40°C, slowly raise the temperature to 105°C, and react at constant temperature for 0.1h to obtain high Ortho boron modified thermoplastic phenolic resin; wherein the molar ratio of phenol to formaldehyde is 1:0.7, the mass ratio of phenol to zinc acetate is 100:1, the mass ratio of phenol to concentrated sulfuric acid is 100:0.2, the total of phenol+formaldehyde The mass ratio of mass to boric acid is 100:1;

[0024] (2) The obtained high-ortho-boron modified phenolic resin was dissolved in methanol, then added formaldehyde and reacted at 45°C for 3 hours under the action of triethanolamine...

Embodiment 2

[0028] A method for preparing a high-ortho boron-modified thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane, the steps are as follows:

[0029] (1) Boil phenol, acetaldehyde, and boric acid under the action of chromium acetate for 2.5 hours, add dropwise hydrochloric acid to continue the reaction for 1 hour, dehydrate under reduced pressure, lower the temperature to 40°C, slowly raise the temperature to 115°C, and react at constant temperature for 0.5h to obtain high Ortho boron modified thermoplastic phenolic resin, wherein the molar ratio of phenol to acetaldehyde is 1:0.8, the mass ratio of phenol to chromium acetate is 100:1, the mass ratio of phenol to hydrochloric acid is 100:0.5, the total of phenol+formaldehyde The mass ratio of mass and boric acid is 100:3;

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

Embodiment 3

[0034] A method for preparing a high-ortho boron-modified thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane, the steps are as follows:

[0035] (1) Boil phenol, furfural, and boric acid under the action of cobalt acetate for 3 hours, add dropwise phosphoric acid to continue the reaction for 1.5 hours, dehydrate under reduced pressure, cool down to 40°C, slowly raise the temperature to 125°C, and react at constant temperature for 1 hour to obtain high ortho Boron modified thermoplastic phenolic resin, wherein the molar ratio of phenol and furfural is 1:0.8, the mass ratio of phenol and cobalt acetate is 100:1.5, the mass ratio of phenol and phosphoric acid is 100:0.7, the total mass of phenol+furfural and boric acid The mass ratio is 100:4;

[0036] (2) The obtained high-ortho boron modified phenolic resin was dissolved in methanol, then furfural was added to react at 55°C for 5h under the action of catalyst barium carbonate, cooled to room tempe...

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Abstract

The invention discloses a preparation method of a highly-ortho boron-modified thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane. The preparation method of the highly-ortho boron-modified thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane comprises performing reversed decompressed dehydration on phenol and aldehyde compounds and boric acid with catalysts to obtain highly-ortho boron-modified phenolic resin; then dissolving the highly-ortho boron-modified phenolic resin into alcohol and aldehyde compounds with catalysts for reactionto obtain highly-ortho boron-modified thermosetting phenolic resin; taking the highly-ortho boron-modified thermosetting phenolic resin as a carbon precursor solution for coaxial electrostatic spinning, and then performing heating curing to obtain a highly-ortho boron-modified highly-ortho thermosetting phenolic fiber membrane with the skin-core structure partly inter-soluble; under protection ofN2, performing carbonization and activation to obtain the highly-ortho boron-modified thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane. Compared with the prior art, the preparation method of the highly-ortho boron-modified thermosetting phenolic-based hollow nano-gradient activated carbon fiber membrane is simple and easy to implement, environmentally friendly, controllable in hollowness and high in yield of carbon fiber as well as mechanical performance.

Description

technical field [0001] The invention belongs to the field of preparation of special carbon materials, and in particular relates to a preparation method of high-ortho-boron-modified thermosetting phenolic-based hollow nanometer gradient activated carbon fiber membrane. Background technique [0002] Phenolic resin has many advantages as a carbon precursor, but its heat resistance is relatively poor. In addition, thermoplastic phenolic resin has long curing cycle, many processes, high cost and pollutes the environment. Thermosetting phenolic resin has low molecular weight and poor spinnability. Problems have been unavoidable. In order to improve the heat resistance of phenolic fiber, chemical methods are usually used to modify the resin. The molecular structure of boron-modified phenolic resin contains B-O bonds with relatively high bond energy, which greatly improves the heat resistance and the initial decomposition temperature of the resin. Improvement, the thermal residual r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/318C01B32/336C01B32/348C08G8/28
CPCC01B32/318C01B32/336C01B32/348C08G8/28
Inventor 焦明立张彩云杨凯何建新拱荣华崔世忠朱根兴李洁
Owner ZHONGYUAN ENGINEERING COLLEGE
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