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Preparation method of boric acid modified high ortho phenolic fiber

A phenolic fiber, high ortho-position technology is applied in the field of preparation of high-performance flame-retardant fibers, which can solve the problems of low tensile strength and poor heat resistance of phenolic fibers, and achieve improved spinning performance, short curing time, and difficulty in spinning. small effect

Active Publication Date: 2015-11-04
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 is to overcome the shortcomings of low tensile strength and poor heat resistance of general phenolic fibers, and provide a preparation method of boric acid modified high-ortho phenolic fibers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: A preparation method of boric acid modified high ortho phenolic fiber, solution A prepared by mixing phenol and formaldehyde at a molar ratio of 1:1.3; under the action of sodium carbonate, react for 2 hours at 75°C to obtain high content of o-hydroxymethylphenol, wherein the mass ratio of phenol:sodium carbonate is 1:0.05; then boric acid is added to it, heated and refluxed for a period of time to obtain boric acid modified high ortho phenolic mother liquor.

[0023] Mix phenol and formaldehyde according to the molar ratio of 1:0.8 to make solution B. The molar ratio of phenol in solution B: phenol in solution A is 9:1, and boil for 4 hours under the action of zinc acetate. Solution B The mass ratio of phenol:zinc acetate in solution A is 1:0.025. After the reaction, it is mixed with boric acid modified high ortho phenolic mother liquor, and concentrated sulfuric acid is added to neutralize the total phenol in solution A and solution B: The mass ratio of conc...

Embodiment 2

[0025] Example 2: A method for preparing boric acid-modified high-ortho-position phenolic fibers. Mix phenol and formaldehyde in a molar ratio of 1:1.3 to obtain solution A. In zinc acetate (the mass ratio of phenol:zinc acetate is 1:0.045 ) at 75°C for 2 hours to obtain a high content of o-hydroxymethylphenol; then add boric acid to it, the molar ratio of boric acid to phenol in solution A is 0.01~0.4:1, heat to 70~100°C, Reflux reaction for 2 to 5 hours to prepare boric acid modified high ortho phenolic mother liquor.

[0026] Mix phenol and formaldehyde with solution B according to the molar ratio of 1:0.8. The molar ratio of phenol in solution B: phenol in solution A is 9:1. In zinc acetate (the mass ratio of phenol in solution B: zinc acetate is 1 : 0.025) under the action of boiling reaction for 4h, mixed with high ortho phenolic mother liquor, adding concentrated sulfuric acid (the mass ratio of total phenol in solution A and solution B: concentrated sulfuric acid is 1:...

Embodiment 3

[0028] Embodiment 3: A kind of preparation method of boric acid modified high ortho phenolic fiber, the solution A prepared by mixing phenol and formaldehyde according to the molar ratio of 1:1.3, in zinc acetate (phenol: the mass ratio of zinc acetate is 1: 0.045) at 75°C, react for 2 hours to obtain a high content of o-hydroxymethylphenol, then add boric acid to it, heat and reflux for a period of time to prepare boric acid modified high ortho phenolic mother liquor.

[0029] Solution B prepared by mixing phenol and formaldehyde at a molar ratio of 1:0.75, the molar ratio of phenol in solution B: phenol in solution A = 4.5:1, in zinc acetate (the mass ratio of phenol: zinc acetate is 1:0.025 ) under the action of boiling reaction for 5 hours, mixed with high ortho phenolic mother liquor, adding concentrated sulfuric acid (the mass ratio of total phenol in solution A and solution B: concentrated sulfuric acid is 1:0.0025) to continue boiling reaction, reflux for 1 hour to obta...

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Abstract

A preparation method of a boric acid modified high-ortho phenolic fiber comprises the following steps: (1) matching phenyl hydroxide and formaldehyde to obtain a solution A, and reacting under the action of sodium carbonate or zinc acetate to obtain a salicylidene phenol solution; (2) adding boric acid in the salicylidene phenol solution to obtain a boric acid modified high-ortho phenolic mother liquor; (3) matching phenyl hydroxide and formaldehyde to obtain a solution B, performing an additive reaction under the action of zinc acetate, mixing the reactant with the high-ortho phenolic mother liquor obtained in the step (2), and adding strong sulfuric to obtain a boric acid modified high-ortho phenolic solution; (4) performing high-temperature water cleaning so as to obtain boric acid modified high-ortho thermoplastic phenolic resin suitable for spinning after temperature reduction; (5) performing melt spinning on the obtained boric acid modified high-ortho thermoplastic phenolic resin to obtain the boric acid modified high-ortho phenolic fiber. Compared with the prior art, the reaction is simple and feasible, the curing rate and the fiber heat resistance are high, the mechanical property is excellent, and the spinning stock solution is prepared by mixing with the mother liquor, so that the spinning performance is improved.

Description

technical field [0001] The invention belongs to the field of preparation of high-performance flame-retardant fibers, and in particular relates to a preparation method of boric acid-modified high-ortho-position phenolic fibers. Background technique [0002] Ordinary phenolic can be used for a long time below 200°C, but obvious oxidation will occur if the temperature exceeds this temperature. And as the temperature rises, the phenolic formaldehyde will undergo pyrolysis and carbonization successively. In order to improve the heat resistance of phenolic fibers, chemical methods are usually used to modify the resin, such as etherification, esterification, and heavy metal chelation of phenolic hydroxyl groups of phenolic fibers [Wang Hongbin, Dang Jiangmin, Ren Rui, etc., Synthetic Fiber Industry , 2012, 35(2), 12-15, US Pat 4851279]. Through these methods, the heat resistance of ordinary phenolic formaldehyde is improved, and the application range of phenolic formaldehyde fibe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/78D01F11/08
Inventor 杨凯焦明立刘红艳王双华
Owner ZHONGYUAN ENGINEERING COLLEGE
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