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A kind of method for preparing phenolic modified melamine fiber by single-pot method

A melamine fiber modification technology, which is applied in the wet spinning method, conjugated synthetic polymer artificial filament, etc., can solve the problems of high residual carbon rate of phenolic fiber, hindering the development of melamine fiber, and high functionality of melamine. Fast spinning speed, easy curing and cross-linking, and more linear structures

Active Publication Date: 2022-07-15
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, melamine has disadvantages such as high functionality and high cross-linking degree. It is not easy to synthesize or the resin has a short storage time after synthesis, thus hindering the development of melamine fiber. How to improve the high performance of melamine fiber has become the focus of research.
[0003] Phenolic fiber has the characteristics of high carbon residue rate, high limiting oxygen index, good flame retardancy, etc., and it does not prolong combustion in high-temperature flames, and self-extinguishes after leaving the flame. Elements, in the high temperature flame, the amount of smoke is very small, no toxic gas is produced, and the original shape can be well maintained after carbonization [Ma Liuqiang, Zhou Xiumin, Li Xiaolin. Research progress on phenolic resin modification[J]. Plastics, 2004, 33(5): 39-42.], has excellent flame retardancy, smokeless and non-toxic properties, but the preparation process is polluted, the preparation steps are many, and the efficiency is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The method for preparing phenolic modified melamine fibers by the single-pot method of the present embodiment is as follows:

[0023] Dissolve PVA in water to obtain a 1wt% PVA aqueous solution, add melamine, formaldehyde, and phenol, adjust the pH to 7.4 with sodium hydroxide, and react at 45 °C for 0.5 h. The molar ratio of melamine to phenol and formaldehyde is 1:0.5:1 , the mass ratio of PVA and melamine is 1:0.7, adjust the pH to 4.0 with hydrochloric acid, react at 35°C for 0.7h, and finally adjust the pH to 7.4 with sodium hydroxide, and react at 40°C for 0.4h to obtain the modified melamine resin solution.

[0024] The obtained spinning solution was wet-spun, using a saturated sodium sulfate aqueous solution with a weight content of 0.1% boric acid as a coagulation bath, and the winding speed was 10 m / min at a temperature of 10 °C to obtain spun fibers, and then dried at 20 °C. The temperature was increased to 150 °C / min, the temperature was kept constant for 0...

Embodiment 2

[0027] The method for preparing phenolic modified melamine fibers by the single-pot method of the present embodiment is as follows:

[0028] Dissolve PVA in water to obtain a 30wt% PVA aqueous solution, add melamine, glutaraldehyde, and cardanol, adjust the pH to 11 with calcium hydroxide, and react at 95°C for 6 hours. Melamine, cardanol, and glutaraldehyde (according to the content of The molar ratio of PVA and melamine is 1:3:5, the mass ratio of PVA and melamine is 1:7, the pH is adjusted to 6.9 with oxalic acid, the reaction is carried out at 90 ° C for 5h, and finally the pH is adjusted with calcium hydroxide Reaction at 10.5, 90 °C for 8 h to obtain a modified melamine resin solution.

[0029] The obtained spinning solution was wet-spun, using a saturated sodium sulfate aqueous solution with a weight content of 5% boric acid as a coagulation bath, and a winding speed of 500 m / min at a temperature of 60 °C to obtain spun fibers, and then dried at 40 °C. The temperature ...

Embodiment 3

[0032] The method for preparing phenolic modified melamine fibers by the single-pot method of the present embodiment is as follows:

[0033] Dissolve PVA in water to obtain a 5wt% PVA aqueous solution, add melamine, acetaldehyde, and chlorophenol, adjust the pH to 8 with potassium hydroxide, and react at 50 °C for 1 h. The molar ratio of PVA and melamine is 1:1:2, the mass ratio of PVA and melamine is 1:1, the pH is adjusted to 5 with sulfuric acid, the reaction is carried out at 50 ° C for 1 h, and finally the pH is adjusted to 8 with potassium hydroxide , 50 ℃ of reaction 1h, to obtain the modified melamine resin solution.

[0034] The obtained spinning solution was spun by wet method, using a saturated sodium sulfate aqueous solution with a weight content of 2% boric acid as a coagulation bath, and a winding speed of 100 m / min at a temperature of 20 °C to obtain spun fibers, and then dried at 25 °C. The temperature was increased to 160 °C / min, the temperature was kept cons...

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Abstract

The invention discloses a method for preparing phenolic modified melamine fibers by a single-pot method. Melamine, phenolic compounds and aldehyde compounds are added to a polymer aqueous solution, and after the alkali-acid-base reaction is completed, wet spinning is used. The spinning machine is used for spinning, and the nascent fiber wound by the coagulation bath is heated and solidified in an oven, and the temperature is lowered to obtain the modified melamine fiber. The invention prepares the modified melamine fiber by single-pot reaction and wet spinning, the fiber has a three-dimensional cross-linked structure, and the fiber has good flame retardant performance, less toxic gas during combustion, no thick smoke, good toughness, and has a wide range of properties. application prospects.

Description

technical field [0001] The invention belongs to the field of preparation of special fibers, in particular to a single-pot method for preparing a phenolic compound-modified melamine resin, and a preparation method for obtaining functional modified melamine fibers by wet spinning and thermal curing. Background technique [0002] Melamine fiber is a new type of flame retardant fiber, which is produced by condensation polymerization of melamine and formaldehyde. Melamine fiber has good flame retardancy, good water absorption, good dyeability, high temperature resistance, limiting oxygen index (LOI) of 32, no melting or dripping during combustion, which can avoid secondary fires [Ni Ke, Ren Zhonghai, Du Wenqin. Flame retardant properties and development and application of melamine fibers [J]. Chemical Fiber and Textile Technology, 2015, 44(3): 28-32.], melamine is cheap and has been widely used in some high temperature fields. However, melamine has disadvantages such as high fun...

Claims

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Application Information

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IPC IPC(8): D01F8/16D01F8/10C08G14/10D01D5/06
CPCD01F8/16D01F8/10C08G14/10D01D5/06
Inventor 杨凯焦明立张啸梅贾万顺李洁庹武刘让同
Owner ZHONGYUAN ENGINEERING COLLEGE
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