A method for preparing boron-modified high-ortho phenolic fiber by wet spinning

A technology of wet spinning and phenolic fiber, which is applied in rayon manufacturing, fiber chemical characteristics, textiles and paper making, etc. It can solve the problems of difficulty in large-scale production and pollution of electrospinning, and achieve environmental protection in the production process and reduce energy consumption , the effect of improving stability

Active Publication Date: 2021-03-16
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the serious pollution in the solidification process of melt spinning and the difficulty of large-scale production of electrospinning in the prior art, the present invention proposes a heat-resistant and flame-retardant boron-modified high-ortho The preparation method of phenolic fiber

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A method for preparing boron-modified high-ortho phenolic fibers by wet spinning, specifically comprising the following steps:

[0028] (1) Phenol, formaldehyde and boric acid (molar ratio of phenol to formaldehyde is 1:0.75, boric acid:phenol=1wt%) are heated to boiling under the action of zinc acetate (the mass of phenol is calculated as 100, and zinc acetate is 1). The reaction was carried out for 2 hours, and concentrated sulfuric acid (the mass ratio of phenol to concentrated sulfuric acid was 100:0.2) was added dropwise, and the reaction was continued for 0.5 hours. The dehydration was performed under reduced pressure, and the temperature was lowered to 40 °C within 1 hour, and then heated to 105 °C within 5 hours. , the vacuum degree is 8500Pa, and the reaction is 0.1h until the solution is viscous to obtain boron-modified high-ortho thermoplastic phenolic resin;

[0029] (2) The obtained boron-modified high-ortho thermoplastic phenolic resin is dissolved in etha...

Embodiment 2

[0034] A method for preparing boron-modified high-ortho phenolic fibers by wet spinning, specifically comprising the following steps:

[0035] (1) Heating phenol, acetaldehyde and boric acid (the molar ratio of phenol to acetaldehyde is 1:1, boric acid:phenol=12wt%) under the action of cadmium acetate (100 for phenol and 3 for cadmium acetate) The reaction was boiled for 6 hours, hydrochloric acid was added dropwise (the mass ratio of phenol to hydrochloric acid was 100:2), the reaction was continued for 4 hours, decompressed and dehydrated, and the temperature was lowered to 60 °C within 2 hours, and then heated to 170 °C within 5 hours. The temperature is 8500Pa, and the reaction is carried out for 4h until the solution is viscous to obtain a boron-modified high-ortho thermoplastic phenolic resin;

[0036](2) The obtained boron-modified high-ortho thermoplastic phenolic resin is dissolved in ethanol (the mass ratio of boron-modified high-ortho thermoplastic phenolic resin to...

Embodiment 3

[0041] A method for preparing boron-modified high-ortho phenolic fibers by wet spinning, specifically comprising the following steps:

[0042] (1) Phenol, furfural, and boric acid (the molar ratio of phenol to furfural is 1:0.8, boric acid:phenol=3wt%) are heated to boiling under the action of cobalt acetate (the mass of phenol is 100, and the cobalt acetate is 2). After 3 hours of reaction, phosphoric acid was added dropwise (the mass ratio of phenol to phosphoric acid was 100:1), the reaction was continued for 2 hours, dehydration under reduced pressure was performed, and the temperature was lowered to 50 °C within 1.5 hours, and then heated to 130 °C within 5 hours, and the vacuum The degree is 8500Pa, and the reaction is until the solution is viscous to obtain a boron-modified high-ortho thermoplastic phenolic resin;

[0043] (2) The obtained boron-modified high-ortho thermoplastic phenolic resin is dissolved in ethanol (the mass ratio of boron-modified high-ortho thermopl...

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Abstract

The invention discloses a method for preparing a boron modified high ortho-phenolic fiber by utilizing wet spinning. The method comprises the following steps: generating a boron modified high ortho thermoplastic phenolic resin from the reaction of phenolic compound, aldehyde compound and boric acid under the action of catalyst; dissolving the acquired boron modified high ortho thermoplastic phenolic resin in absolute ethyl alcohol and then reacting with aldehydes, thereby acquiring a boron modified high ortho thermosetting phenolic resin; mixing with absolute ethyl alcohol, polyvinyl butyral,and the like, and uniformly stirring and performing wet spinning and thermosetting, thereby acquiring the boron modified high ortho-phenolic fiber. According to the method disclosed by the invention,the boron modified thermosetting phenolic resin is taken as the raw material for preparing the phenolic fiber through wet spinning, and the boron modified high ortho-phenolic fiber with excellent mechanical property and high limit oxygen index can be acquired without solution curing, so that the preparation step is reduced, the pollution is reduced and the cost is lowered.

Description

technical field [0001] The invention belongs to the field of preparation of flame-retardant and temperature-resistant special fibers, in particular to a method for preparing boron-modified high-ortho phenolic fibers by wet spinning. Background technique [0002] Phenolic fiber has low thermal conductivity and high limiting oxygen index, and has less smoke during combustion, non-toxic, no melting and dripping phenomenon, and has instantaneous high temperature resistance, because it is at the flame temperature or even higher temperature. Carbonization and decomposition will occur, and carbon dioxide and water will be released to take away heat. It is a good flame-retardant and heat-insulating material. [0003] Although phenolic fibers are suitably prepared by melt-spinning processes, this method has been approved and commercialized. However, due to the low molecular weight of the precursor phenolic resin, the primary fibers are extremely brittle, and the subsequent procedure...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/94D01F1/10C08G8/28
CPCC08G8/28D01F1/10D01F6/94
Inventor 焦明立任东雪刁泉杨凯刘红燕张彩云米立伟余木火
Owner ZHONGYUAN ENGINEERING COLLEGE
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