A method for preparing high ortho thermosetting phenolic fiber by wet spinning

A wet spinning and phenolic fiber technology, applied in the field of flame retardant, can solve the problems of pollution electrospinning, difficult mass production, etc., and achieve the effects of reducing energy consumption, simple processing and high molecular weight

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

[0004] 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 method for preparing heat-resistant and flame-retardant high-ortho-position phenolic fibers through wet spinning technology. method, that is, phenols and aldehyde compounds react under the action of a catalyst, and the generated high-ortho thermoplastic phenolic resin continues to react with aldehyde compounds to generate a high-ortho thermosetting phenolic resin; the obtained high-ortho thermosetting Phenolic resin, anhydrous ethanol, polyvinyl butyral prepared spinning stock solution, wet spinning, and then curing treatment, to obtain flame-retardant, heat-resistant phenolic fiber prepared by wet spinning

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A method for preparing high-ortho position thermosetting phenolic fibers by wet spinning, specifically comprising the following steps:

[0025] (1) Heat phenol and formaldehyde (the molar ratio of phenol to formaldehyde is 1:0.8) under the action of zinc acetate (100 parts by mass of phenol, 1 part by mass of zinc acetate), heat to boiling for 2 hours, add concentrated Sulfuric acid (the mass ratio of phenol to concentrated sulfuric acid is 100:0.2), continue to react for 0.5h, carry out dehydration under reduced pressure, and lower the temperature to 40°C, then raise the temperature to 105°C at 1°C / min, vacuum degree is 8500Pa, react for 0.1h, Obtain high ortho-position thermoplastic phenolic resin until the solution is viscous;

[0026] (2) The obtained high-ortho-position thermoplastic phenolic resin is dissolved in ethanol (the mass ratio of high-ortho-position thermoplastic phenolic resin to absolute ethanol is 3:4), and in triethanolamine (the mass ratio of trieth...

Embodiment 2

[0030] A method for preparing high-ortho position thermosetting phenolic fibers by wet spinning, specifically comprising the following steps:

[0031] (1) Heat phenol and acetaldehyde (the molar ratio of phenol to acetaldehyde is 1:1) under the action of cadmium acetate (phenol is calculated as 100, cadmium acetate is 3), and heated to boiling for 6 hours, and hydrochloric acid (phenol The mass ratio with hydrochloric acid is 100:2), continue to react for 4h, carry out dehydration under reduced pressure, and lower the temperature to 85°C, then raise the temperature to 170°C at 1°C / min, keep the temperature at 8500Pa for 4h to react until the solution is viscous, and get High ortho thermoplastic phenolic resin;

[0032] (2) The obtained high-ortho-position thermoplastic phenolic resin is dissolved in ethanol (the mass ratio of high-ortho-position thermoplastic phenolic resin to absolute ethanol is 3:9), and in ammonium hydroxide (ammonium hydroxide and high-ortho-position therm...

Embodiment 3

[0036] A method for preparing high-ortho position thermosetting phenolic fibers by wet spinning, specifically comprising the following steps:

[0037] (1) Heat phenol and furfural (the molar ratio of phenol to furfural is 1:0.9) under the action of cobalt acetate (phenol is calculated as 100, cobalt acetate is 2), and heated to boiling for 3 hours, then dropwise add phosphoric acid (phenol and phosphoric acid The mass ratio of 100:1), continue to react for 2h, carry out dehydration under reduced pressure, and lower the temperature to 70°C, then raise the temperature to 130°C at 0.5°C / min, vacuum degree is 8500Pa, keep constant temperature for 3h to react until the solution becomes viscous High ortho thermoplastic phenolic resin;

[0038] (2) The obtained high-ortho-position thermoplastic phenolic resin is dissolved in ethanol (the mass ratio of high-ortho-position thermoplastic phenolic resin to absolute ethanol is 3:7), and in ammonium hydroxide (ammonium hydroxide and high-o...

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Abstract

The invention discloses a method for preparing high-ortho thermosetting phenol-formaldehyde fibers by wet spinning. Phenol compounds and aldehyde compounds undergo a reaction under the action of a catalyst, and high-ortho thermoplastic phenol-formaldehyde resin is formed; the obtained thermoplastic phenol-formaldehyde resin is dissolved in absolute ethyl alcohol, undergoes a reaction with aldehydes under the action of a basic catalyst and is neutralized with an acid to obtain the high-ortho thermosetting phenol-formaldehyde resin; the high-ortho thermosetting phenol-formaldehyde resin is mixedand stirred evenly with absolute ethyl alcohol, polyvinyl butyral and the like, the mixture is subjected to wet spinning, and primary fibers are thermocured to obtain the phenol-formaldehyde fibers prepared by the wet spinning. The method can obtain the phenol-formaldehyde fibers with good mechanical properties and high limit oxygen index without solution curing, reduces the manufacturing steps,reduces pollution and saves energy.

Description

technical field [0001] The invention belongs to the field of preparation of flame-retardant and temperature-resistant special fibers, and in particular relates to a method for preparing high-ortho-position thermosetting 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, is non-toxic, has no melting dripping phenomenon, and has instant high temperature resistance, because it can withstand flame temperature or even higher temperature. It will be carbonized, decomposed, and carbon dioxide and water will be released to take away heat. It is a good flame-retardant and heat-insulating material. [0003] Although the preparation of phenolic fibers is suitable for the melt-spinning process, this method has been recognized and industrialized. However, due to the low molecular weight of the precursor phenolic resin, the nascent fiber is extremely brittle, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/94D01F1/07D01F1/10D01D5/06D01D10/02C08G8/10C08G8/04C08G8/06C08G8/12
CPCC08G8/04C08G8/06C08G8/10C08G8/12D01D5/06D01D10/02D01F1/07D01F1/10D01F6/94
Inventor 焦明立任东雪宋梦刁泉杨凯桑向东张彩云曹健姚冬刚
Owner ZHONGYUAN ENGINEERING COLLEGE
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