Method for preparing epoxy-modified high-ortho thermosetting phenol-formaldehyde fibers by wet spinning

A technology of epoxy modification and wet spinning, which is applied in the direction of wet spinning, rayon manufacturing, fiber chemical characteristics, etc. It can solve the problems of pollution in the production process, mechanical properties of polluted phenolic fibers, and poor performance, so as to improve the reaction Efficiency, high para-activity, simple processing effect

Active Publication Date: 2019-01-15
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of serious pollution and poor mechanical properties of phenolic fibers in the prior art during solidification by melt spinning, the present invention proposes a heat-resistant and flame-retardant epoxy-modified high-ortho The preparation method of thermosetting phenolic fiber is simple, the production process has less pollution, and the performance of the prepared epoxy-modified high-ortho thermosetting phenolic fiber is better

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In this embodiment, wet spinning is used to prepare epoxy-modified high-ortho thermosetting phenolic fiber, and the steps are as follows:

[0028] (1) Phenol, formaldehyde, epichlorohydrin (the molar ratio of phenol to formaldehyde is 1:0.7, the mass ratio of phenol to epichlorohydrin is 100:7) in zinc acetate (phenol is based on 100 mass parts, acetic acid Zinc is 1 part by mass), heated to boiling and reacted for 2 hours, added dropwise concentrated sulfuric acid (the mass ratio of phenol to concentrated sulfuric acid was 100:0.2), continued to react for 0.5 hours, carried out dehydration under reduced pressure, and lowered the temperature within 1 hour to 40°C, then heated to 105°C within 5 hours, with a vacuum of 8500Pa, and reacted for 0.1h until the solution became viscous to obtain epoxy-modified high-ortho thermoplastic phenolic resin;

[0029] (2) The obtained epoxy-modified high-ortho-position thermoplastic phenolic resin was dissolved in ethanol (the mass rat...

Embodiment 2

[0033] In this embodiment, wet spinning is used to prepare epoxy-modified high-ortho thermosetting phenolic fiber, and the steps are as follows:

[0034] (1) Mix phenol, acetaldehyde and epichlorohydrin (the molar ratio of phenol to acetaldehyde is 1:1, and the mass ratio of phenol to epichlorohydrin is 100:40) in cadmium acetate (phenol is calculated as 100, acetic acid Under the action of cadmium 3), heat to boiling and react for 6 hours, add dropwise hydrochloric acid (the mass ratio of phenol to hydrochloric acid is 100:2), continue to react for 4 hours, carry out dehydration under reduced pressure, and reduce the temperature to 65°C within 1 hour, and then Raise the temperature to 170°C within 5 hours, the vacuum degree is 8500Pa, and react for 4 hours until the solution is viscous to obtain epoxy-modified high-ortho thermoplastic phenolic resin;

[0035](2) The obtained epoxy-modified high-ortho-position thermoplastic phenolic resin was dissolved in ethanol (the mass rat...

Embodiment 3

[0039] In this embodiment, wet spinning is used to prepare epoxy-modified high-ortho thermosetting phenolic fiber, and the steps are as follows:

[0040] (1) Mix phenol, furfural, and epichlorohydrin (the molar ratio of phenol to furfural is 1:0.8, and the mass ratio of phenol to epichlorohydrin is 100:10) in cadmium acetate (phenol is calculated as 100, cadmium acetate is 2) Under the action of the reaction, heat to boiling for 3 hours, add dropwise phosphoric acid (the mass ratio of phenol to phosphoric acid is 100:1), continue the reaction for 2 hours, carry out dehydration under reduced pressure, and reduce the temperature to 45°C within 1 hour, and then in 5 Heat up to 130°C within hours, vacuum at 8500Pa, react for 3 hours until the solution is viscous to obtain epichlorohydrin high ortho thermoplastic phenolic resin;

[0041] (2) The obtained epoxy-modified high-ortho-position thermoplastic phenolic resin was dissolved in ethanol (the mass ratio of epoxy-modified high-o...

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Abstract

The invention discloses a method for preparing epoxy-modified high-ortho thermosetting phenol-formaldehyde fibers by wet spinning. Phenol compounds, aldehyde compounds and epoxy haloalkane undergo a reaction under the action of a catalyst, and epoxy-modified high-ortho thermoplastic phenol-formaldehyde resin is formed; the obtained epoxy-modified high-ortho thermoplastic phenol-formaldehyde resinis 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 epoxy-modified high-ortho thermosetting phenol-formaldehyde resin; the epoxy-modified high-ortho thermosetting phenol-formaldehyde resin is mixed and stirred evenly with absolute ethyl alcohol, polyvinyl butyral and the like, the mixture issubjected to wet spinning, and primary fibers are thermocured to obtain the epoxy-modified high-ortho phenol-formaldehyde fibers prepared by the wet spinning. According to the method, the flexibilityof phenol-formaldehyde molecules is increased by modification with epoxy haloalkane, the toughness of the phenol-formaldehyde fibers is improved, the phenol-formaldehyde fibers with good mechanical properties and high limit oxygen index can be obtained without solution curing, the manufacturing steps are reduced, the pollution is reduced and the energy is saved.

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 epoxy-modified high-ortho-position thermosetting phenolic fibers by wet spinning. Background technique [0002] As a good flame-retardant and heat-insulating material, phenolic fiber has low thermal conductivity and high limiting oxygen index, burns with less smoke, is non-toxic, and has no melt dripping phenomenon. [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 the subsequent process is difficult to operate; and how to make the fiber into an insoluble and infusible polycondensate with a three-dimensional crosslinked structure is the difficulty of this process. In order to imp...

Claims

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Application Information

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IPC IPC(8): D01F6/94D01F1/07D01F1/10D01D5/06C08G8/28
CPCC08G8/28D01D5/06D01F1/07D01F1/10D01F6/94
Inventor 焦明立任东雪杨凯朱根兴李洁张彩云姚冬刚桑向东
Owner ZHONGYUAN ENGINEERING COLLEGE
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