Antioxidation polyphenylene sulfide/modified nano silicon dioxide composite fiber and preparation method thereof

A nano-silica, polyphenylene sulfide technology, applied in the direction of fiber chemical characteristics, single-component synthetic polymer rayon, rayon manufacturing, etc., can solve the problems of anti-oxidation effect to be discussed, shorten the preparation process, etc., to achieve Effects of improved anti-oxidation performance, good dispersibility, and increased strength retention

Active Publication Date: 2019-09-06
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN105544001A discloses a method for directly preparing polyphenylene sulfide modified short fibers by modifying polyphenylene sulfide powder, which is to introduce polyphenylene sulfide and nano-silicon dioxide into a screw extruder to melt and extrude until homogenized Homogenized and mixed in the kettle, then sent to the filter by the melt pump, cooled by metering pump, spinning box, spinneret, ring blowing, oiling, drafting, heat setting machine setting, curling, relaxation setting machine relaxation Shaping, cutting and packaging to obtain polyphenylene sulfide modified staple fibers, mainly to provide a set of modified polyphenylene sulfide fibers that shorten the preparation process, simplify equipment configuration, improve preparation efficiency, reduce costs, save energy and ensure consistent quality. The phenylene sulfide fiber method, although this process method produces PPD short fibers with better mechanical properties, but its anti-oxidation effect remains to be discussed

Method used

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  • Antioxidation polyphenylene sulfide/modified nano silicon dioxide composite fiber and preparation method thereof
  • Antioxidation polyphenylene sulfide/modified nano silicon dioxide composite fiber and preparation method thereof
  • Antioxidation polyphenylene sulfide/modified nano silicon dioxide composite fiber and preparation method thereof

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Experimental program
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Embodiment 1

[0030] Embodiment 1: the preparation process of modified nano silicon dioxide is as follows figure 1 shown. Weigh 2g of nano-silica and pour it into a 250ml three-neck flask, then add 150ml of ethanol aqueous solution (ethanol: water = 3:1); the frequency of ultrasonic vibration is 40 kHz ultrasonic vibration for 60 min, put it into a heating mantle to heat and stir; Slowly add 0.3 g of KH792 dropwise into the three-necked flask, adjust the pH to 3 with hydrochloric acid; add 2 g of 3,5 di-tert-butyl-4-hydroxyphenylpropionic acid (AO) into the three-necked flask. Set the temperature to 70°C, condense to reflux, and stir for 12 h. After the reaction, put the product in a centrifuge and centrifuge at a speed of 6500 r / min for 5 min; wash and centrifuge repeatedly with ethanol solution until the pH of the solution is neutral, put it in a vacuum drying oven, and dry it at 110 °C After 10 h, the modified nano-silica was obtained.

[0031] Put the polyphenylene sulfide resin into...

Embodiment 2

[0042] Embodiment 2: the preparation process of modified nano silicon dioxide is as follows figure 1 shown. Weigh 2g of nano-silica and pour it into a 250ml three-neck flask, then add 100ml of ethanol aqueous solution (ethanol: water = 1:1); the frequency of ultrasonic vibration is 45 kHz ultrasonic vibration for 30 min, put it into a heating mantle to heat and stir; Slowly add 0.2 g KH792 dropwise to the three-necked flask, adjust the pH to 3 with hydrochloric acid; add 1.0 g of 3,5-di-tert-butyl-4-hydroxyphenylpropionic acid (AO) to the three-necked flask. Set the temperature at 50°C, condense to reflux, and stir for 15 h. After the reaction, put the product in a centrifuge and centrifuge at a speed of 6500 r / min for 5 min; wash and centrifuge repeatedly with ethanol solution until the pH of the solution is neutral, put it in a vacuum drying oven, and dry it at 80°C After 12 h, the modified nano-silica was obtained.

[0043] Put the polyphenylene sulfide resin into a vacu...

Embodiment 3

[0049] Embodiment 3: the preparation process of modified nano silicon dioxide is as follows figure 1 shown. Weigh 2g of nano-silica and pour it into a 250ml three-neck flask, then add 200ml of ethanol aqueous solution (ethanol: water = 2:1); the frequency of ultrasonic vibration is 50 kHz ultrasonic vibration for 40 min, put it into a heating mantle to heat and stir; Slowly add 1 g of KH792 dropwise to the three-necked flask, adjust the pH to 3 with hydrochloric acid; add 4 g of 3,5-di-tert-butyl-4-hydroxyphenylpropionic acid (AO) to the three-necked flask. Set the temperature to 80°C, condense to reflux, and stir for 10 h. After the reaction, put the product in a centrifuge and centrifuge at a speed of 6500 r / min for 5 min; wash and centrifuge repeatedly with ethanol solution until the pH of the solution is neutral, put it in a vacuum drying oven, and dry it at 100 °C 8 h to obtain modified nano-silica.

[0050] Put the polyphenylene sulfide resin into a vacuum drum dryer,...

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Abstract

The invention belongs to the technical field of chemical fiber and provides antioxidation polyphenylene sulfide / modified nano silicon dioxide composite fiber and a preparation method thereof. The composite fiber is prepared from polyphenylene sulfide and modified nano silicon dioxide proportionally, and modified nano silicon dioxide is formed by using a silane coupling agent to load an antioxidantonto the surface of modified nano silicon dioxide through chemical grafting reaction. Fiber number of the composite fiber prepared by the method is 1.0-5.0dtex, breaking strength is 2.0-3.0cN / dtex, elongation rate at break is 45-48%, and oxidative induction temperature is 470-480 DEG C; breaking strength retention rate of the composite fiber after being treated at temperature of 220 DEG C for 360h is 85-90%; compared with pure PPS fiber, oxidative induction temperature of the composite fiber is increased by about 20 DEG C, strength retention rate is increased by 20-25% after the composite fiber is treated at temperature of 220 DEG C for 360h, and antioxidation performance of the composite fiber is improved obviously.

Description

technical field [0001] The invention belongs to the technical field of chemical fibers, and in particular relates to an anti-oxidation polyphenylene sulfide / modified nano silicon dioxide composite fiber and a preparation method thereof. Background technique [0002] Polyphenylene sulfide, full name polyphenylene sulfide, English full name Polyphenylene Sulfide, referred to as PPS, is a semi-crystalline high polymer, its molecular structure formula: [0003] [0004] There are a large number of benzene rings on the molecular chain of polyphenylene sulfide, which makes the macromolecular chain have good rigidity and heat resistance, and the thioether bond can endow the macromolecular chain with certain flexibility, and the benzene ring and the thioether bond alternate The connection makes the macromolecular structure symmetrical and regular, and has high crystallinity, which makes the PPS fiber excellent in performance, has a very wide range of applications, and is highly v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/94D01F1/10
CPCD01F6/94D01F1/10
Inventor 连丹丹韩汶欣卢建军任靖屹张蕊萍王慧娟
Owner TAIYUAN UNIV OF TECH
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