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Preparation method of epoxy chloropropane toughened high-ortho phenolic fiber

A technology of epichlorohydrin and phenolic fibers, applied in the chemical characteristics of fibers, melt spinning, textiles and papermaking, etc., can solve the problems of low tensile strength and poor toughness of phenolic fibers, and achieve fast cross-linking rate and regular structure. , the effect of simple and easy response

Inactive Publication Date: 2013-12-25
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention overcomes the shortcomings of low tensile strength and poor toughness of general phenolic fibers, and provides a preparation method of epichlorohydrin toughened high-ortho phenolic fibers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: a preparation method of epichlorohydrin toughened high ortho phenolic fiber, comprising the following steps: (1) heating epichlorohydrin, phenol, formaldehyde, zinc acetate to boiling, and reacting; (2 ) add concentrated sulfuric acid to continue the boiling reaction, wash with high temperature water, cool down, and then continue to heat up in decompression dehydration, remove the water and impurities in the solution and the reaction, and obtain epichlorohydrin toughened high-ortho-position phenolic resin; (3) Obtain The epichlorohydrin toughened phenolic resin is melt-spun and drawn to obtain high-ortho-position phenolic fiber precursors. The high-ortho-position phenolic fiber precursors are cured and cross-linked in a coagulation bath containing formaldehyde and HCl to obtain epoxy chlorine Propane toughened high ortho phenolic fibers.

Embodiment 2

[0016] Embodiment 2: A preparation method of epichlorohydrin toughened high-ortho phenolic fiber, wherein the mass ratio of phenol: formaldehyde (according to 100% formaldehyde content) is 1: 0.24 ~ 0.30, the mass ratio of phenol: zinc acetate The ratio is 1:0.005~0.04, and the mass ratio of phenol: epichlorohydrin is 1:0.05~0.4. , The mass ratio of phenol:concentrated sulfuric acid is 1:0.001~0.01.

[0017] Others are the same as embodiment 1.

Embodiment 3

[0018] Embodiment 3: A kind of preparation method of epoxy chlorohydrin toughened high ortho-position phenolic fiber, comprises the following steps: (1) phenol, formaldehyde, zinc acetate are heated to boiling, react, add epoxy chlorine after reaction finishes Propane; (2) add concentrated sulfuric acid to continue the boiling reaction, wash with high temperature water, cool down, and then continue to heat up in decompression dehydration, remove the water and impurities in the solution and the reaction, and obtain epichlorohydrin toughened high ortho phenolic resin; (3) The obtained epichlorohydrin toughened phenolic resin is melt-spun and drawn to obtain high-ortho-position phenolic fiber precursors, and the high-ortho-position phenolic fiber precursors are cured and crosslinked in a coagulation bath containing formaldehyde and HCl. Obtain epichlorohydrin toughened high ortho phenolic fiber.

[0019] Among them, the mass ratio of phenol: formaldehyde (based on 100% formaldehy...

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Abstract

A preparation method of an epoxy chloropropane toughened high-ortho phenolic fiber comprises the following steps of heating phenol, methanal, zinc acetate and epoxy chloropropane to boiling for reaction, adding concentrated sulfuric acid for boiling and reaction continuously, washing with high-temperature water, cooling, continuously heating up during pressure reduction and dehydration, obtaining epoxy chloropropane toughened high-ortho phenolic resin, performing melt spinning on the epoxy chloropropane toughened phenolic resin, drawing to form a high-ortho phenolic fiber filament, heating, curing and crosslinking the high-ortho phenolic fiber filament in a coagulating bath containing methanal and HC1, and obtaining the epoxy chloropropane toughened high-ortho phenolic fiber. Compared with the prior art, the method has the advantages of simple and practicable reaction, good spinnability of a stock solution, high curing rate and high mechanical properties.

Description

technical field [0001] The invention belongs to the field of preparation of polymer flame-retardant functional fibers, and specifically relates to a preparation method of high-ortho-position phenolic fibers toughened by epichlorohydrin. Background technique [0002] Phenolic fiber is a three-dimensional cross-linked flame-retardant organic fiber, which was first successfully developed in 1968 by Dr. J. Economy of the American Carborundum Company [US Pat. 3650102]. It was originally planned to be used as a cheap carbon fiber in aerospace, but the test found that the mechanical strength of phenolic carbon fiber was insufficient to meet the needs of aerospace; and its own characteristics such as flame retardancy and ablation resistance promoted the further development of phenolic fiber. The advent of the fiber broke the inherent concept that three-dimensional cross-linked resins cannot be formed into fibers. [0003] Due to the presence of methylene groups connecting two benze...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/78D01F11/08D01D5/08
Inventor 焦明立杨凯刘红燕陈燕张旺玺
Owner ZHONGYUAN ENGINEERING COLLEGE
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