Preparation method of polyphenylene sulfide sulfone ketone fibers

A technology of polyphenylene sulfide and sulfone ketone, which is applied in the field of preparation of polyphenylene sulfide sulfone ketone fibers, can solve the problems of high-quality product industrialization difficulty, low average molecular weight of polymerization products, high polymerization cost, etc., and achieve inhibition of oxidative fracture , Improve flexibility, improve the effect of comprehensive performance

Pending Publication Date: 2021-10-08
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the modification process is relatively complicated, the polymerization is difficult to control, the average molecular weight of the polymerization product is low, and the polymerization cost is relatively high, so the industrialization of high-quality products is difficult.

Method used

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  • Preparation method of polyphenylene sulfide sulfone ketone fibers
  • Preparation method of polyphenylene sulfide sulfone ketone fibers
  • Preparation method of polyphenylene sulfide sulfone ketone fibers

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preparation example Construction

[0031] The invention provides a kind of preparation method (abbreviation method) of polyphenylene sulfide sulfone ketone fiber, it is characterized in that, this method comprises the following steps:

[0032] (1) Ketogenic PPS: Using metal oxide as a catalyst, the fiber-grade PPS resin, metal oxide and carboxylic acid are reacted by screw extrusion and blended and melted in a screw extruder by one-step in-situ spinning to prepare ketone-containing PPS. PPS tow; or use the screw extrusion reaction of fiber grade PPS resin, metal oxide and carboxylic acid to blend, melt and granulate in the screw extruder to prepare ketone-containing PPS granules, and then use ketone-containing PPS granules as raw materials for granulation Melt spinning to prepare ketone-containing PPS tow; the carboxylic acid is a dicarboxylic acid or a polycarboxylic acid;

[0033] Preferably, in step (1), the dicarboxylic acid is terephthalic acid, naphthalene dicarboxylic acid, cyclohexanedicarboxylic acid, ...

Embodiment 1

[0052] (1) 5g terephthalic acid, 1g TiO 2 Blending and melting granulation with 494gPPS resin in a twin-screw extruder at high temperature, the feeding port temperature of the screw extruder is 265°C, the die head temperature is 310°C, and the temperature in the middle zone of the spinning screw is controlled at 300-325°C to prepare ketone-containing PPS resin chips;

[0053] Then melt-spin ketone-containing PPS resin slices to obtain ketone-containing PPS tow; the temperature of the feed port is 305°C, the temperature of the second zone is 320-330°C, the third zone is 325-335°C, and the fourth zone is 325-335°C. The temperature is 315°C; the hot stretching temperature is 95°C, and the stretching ratio is 3.5 times;

[0054] (2) Immerse the ketone-containing PPS tow (tensile strength 5.5CN / dt, elongation at break 28%) into 10wt% H 2 o 2 , 10wt% acetic acid, 0.1wt% HCl in water, the mass ratio of ketone-containing PPS tow and oxidant solution is 1:5, soaked at 60°C for 30min...

Embodiment 2

[0064] (1) 3g malonic acid, 0.5g SnO 2 Blending and melting granulation with 496.5g PPS resin in a twin-screw extruder at high temperature, the feed port temperature of the screw extruder is 260°C, the die head temperature is 315°C, and the temperature in the middle zone of the spinning screw is 295-320°C to prepare ketone-containing PPS Resin chips;

[0065] Then melt-spin ketone-containing PPS resin slices to obtain ketone-containing PPS tow; the temperature of the feed port is 305°C, the second zone is 325°C, the third zone is 325°C, the fourth zone is 330°C, and the die head temperature is 315°C; The stretching temperature is 100°C, and the stretching ratio is 4 times;

[0066] (2) Immerse ketone-containing PPS tow (tensile strength 5.3CN / dt, elongation at break 32%) in the benzene of 15wt% benzoyl peroxide, 5wt% butyric acid, 0.1wt% benzenesulfonic acid, containing The mass ratio of the ketone PPS tow to the oxidizing agent solution is 1:11, soaked at 60°C for 10 minute...

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Abstract

The invention discloses a preparation method of polyphenylene sulfide sulfone ketone fibers. The method comprises the following steps of firstly, by taking a metal oxide as a catalyst, carrying out a screw extrusion reaction on PPS resin, the metal oxide and dicarboxylic acid or polycarboxylic acid to prepare ketone-containing PPS tows; placing the ketone-containing PPS tows in an oxidation system, and carrying out an oxidation reaction under the action of an oxidation catalyst to obtain polyphenylene sulfide sulfone ketone nascent fibers; and removing impurities from the polyphenylene sulfide sulphone ketone nascent fibers, and performing drying to obtain the polyphenylene sulfide sulphone ketone fibers. According to the invention, a Friedel-Crafts acylation cross-linking reaction among PPS molecular chains is realized in a molten state, cross-linking or chain extension among PPS molecules is realized, and ketone groups are introduced into the PPS molecules; and PPS fibers with the cross-linked or chain-extended ketone groups are oxidized, controllable oxidation of S atoms is realized, the introduction of sulfonyl and sulfoxide groups is realized, and PPS modified fibers containing ketone and sulfone or ketone and sulfoxide and having the advantages of high temperature resistance, solvent resistance, creep resistance, molt drip resistance, oxidation resistance, high toughness and high strength are obtained.

Description

technical field [0001] The invention relates to the technical field of PPS modification, in particular to a preparation method of polyphenylene sulfide sulfone ketone fiber. Background technique [0002] Polyphenylene sulfide (PPS) is a thermoplastic resin with a phenylthio group in the main chain of the molecule. Because of its excellent high temperature resistance, corrosion resistance, radiation resistance, and flame retardancy, it is widely used in high temperature and harsh environments. However, because PPS fiber is easy to creep and shrink, there is a droplet phenomenon, and it is not resistant to oxidation and low in temperature resistance, and its use in environments above 180 ° C is limited. Although active research and development at home and abroad have initially formed a certain production capacity of PPS fiber or modified fiber (ZL201510631820.5 and ZL201510350644.8), but PPS derivative fiber products still have poor toughness, low strength, UV resistance, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/94D01F1/10D01F11/08
CPCD01F6/94D01F1/106D01F11/08
Inventor 李振环
Owner TIANJIN POLYTECHNIC UNIV
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