Preparing method for ablation-resistant high-ortho phenolic fibers

A high-ortho-position, boron-phenolic technology, which is applied in the fields of fiber chemical characteristics, melt spinning, chemical post-treatment of synthetic polymer artificial filaments, etc., can solve the problems of long-term application in special fields, lack of ablation resistance, and fiber mechanical properties Poor problems, achieve high O/P) value, fast curing rate, improved mechanical properties and flame retardancy

Inactive Publication Date: 2016-02-17
ZHONGYUAN ENGINEERING COLLEGE
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the poor spinning performance of the phenolic fiber in the prior art, it often needs to be blended with PVA or PA for spinning, and the obtained fiber has poor mechanical properties, insufficient heat resistance, and lack of ablation resistance, so it is difficult to apply for a long time in special fields

Method used

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  • Preparing method for ablation-resistant high-ortho phenolic fibers

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Mix phenol (100g) and formaldehyde (68.9g) according to the molar ratio of 1:0.8, then add 1g of titanium citrate catalyst, boil for 2.9h; add diluted concentrated sulfuric acid (concentrated sulfuric acid is 0.1ml), continue the reaction for 50min; reduce pressure Dehydration for 0.5h, the temperature of the resin reaches 90°C; add 1g of boric acid for modification reaction, and boil at constant temperature for 2 hours; dehydration under reduced pressure, when the resin temperature rises to 100°C, the material is discharged to obtain a molecular weight of 26000Da, O / P (o High ortho boric acid phenolic resin with a para-position ratio) value of 4.5 and a viscosity of 24.5cP at 140°C;

[0027] The resin was melt-spun at 120°C, and the nascent fibers were put into the prepared solidification solution (aqueous solution with a mass fraction of formaldehyde of 8% and a mass fraction of hydrochloric acid of 12%), and the temperature was gradually raised from room temperature (...

Embodiment 2

[0031] Mix phenol (100g) and formaldehyde (73.3g) according to the molar ratio of 1:0.85, then add 2g of titanium citrate catalyst, boil for 2h; add dilute concentrated sulfuric acid (concentrated sulfuric acid is 0.3ml), continue the reaction for 30min; dehydration under reduced pressure 3h, the temperature of the resin reaches 97°C; add 10g of boric acid for modification reaction, boil at constant temperature for 2 hours; dehydrate under reduced pressure, when the resin temperature rises to 130°C, the material is discharged to obtain a molecular weight of 5000Da, O / P (ortho-para High ortho boric acid phenolic resin with a ratio of 7.8 and a viscosity of 9.5cP at 140°C;

[0032] The resin was melt-spun at 160°C, and the nascent fiber was put into the prepared solidification solution (formaldehyde mass fraction 6%, hydrochloric acid mass fraction 12% aqueous solution), and the temperature was gradually raised from room temperature (6°C every 2 minutes) to 95°C, constant temper...

Embodiment 3

[0036] The high-ortho-boron phenolic fiber and phenolic resin obtained in embodiment 2 are compounded according to a mass ratio of 4:6 to obtain a high-ortho-boron phenolic fiber / phenolic resin composite material, and the thermal conductivity of the composite material is 0.39W / m*K, The linear ablation rate is -0.010mm / s, the mass ablation rate of oxyacetylene flame is 0.0213g / s, and the density is 1.31g / cm 3 , 1000 ℃ under nitrogen atmosphere, the carbon residue is 75%, and the limiting oxygen index is 40. The results show that the composite material has good interfacial bonding, excellent ablation resistance, better heat insulation, heat resistance and flame retardancy than phenolic resin, and the synergistic effect is obvious.

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Abstract

The invention discloses a preparing method for ablation-resistant high-ortho phenolic fibers. A phenolic compound and formaldehyde are mixed according to a certain proportion, then a certain amount of citric acid as a catalyst is added, and a boiling reaction is carried out for 0.5-4 h; diluted concentrated sulfuric acid is added, and the reaction continues for 30-50 min; decompression and dehydration are carried out for 0.5-2.9 h, boric acid accounting for 1-8% by mass is added for a modification reaction after the temperature reaches 90-97 DEG C, and boiling is carried out for 2 h at the constant temperature; decompression and dehydration are carried out, and dehydration is stopped when the temperature of resin reaches 110 DEG C; the resin is subjected to melt spinning at 120-160 DEG C; nascent fibers are put into a prepared curing solution, the temperature is increased to 95 DEG C gradually from the room temperature, and the nascent fibers are naturally cooled to the room temperature after constant temperature is achieved; the temperature is gradually increased for thermosetting under the nitrogen condition. The fiber strength of the high-ortho phenolic fibers ranges from 3 cN/dtex to 36 cN/dtex, the modulus ranges from 40 cN/dtex to 400 cN/dtex, and the cross-linking degree ranges from 32% to 38%.

Description

technical field [0001] The invention belongs to the field of preparation of special ablation-resistant fibers, in particular to a preparation method of ablation-resistant high-ortho boron phenolic fibers. Background technique [0002] Ordinary phenolic can be used for a long time below 150°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 the phenolic hydroxyl groups of phenolic fibers [Wang Hongbin, Dang Jiangmin, Ren Rui, etc., Synthetic Fiber Industry , 2012, 35(2), 12-15, USPat4851279]. Through these methods, the heat resistance of ordinary phenolic formaldehyde is improved, and the application range of phenolic formaldehyde fiber is expanded. At t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/78D01F11/08C08G8/28D01D5/08
Inventor 杨凯焦明立刁泉曹健宋慧娟陈燕米立伟朱方龙
Owner ZHONGYUAN ENGINEERING COLLEGE
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