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Preparation method of polycarbosilane non-melting fiber

A technology of polycarbosilane fiber and polycarbosilane, which is applied in the field of polycarbosilane, can solve the problem of high oxygen content in silicon carbide fiber, achieve the effects of less environmental pollution, avoid high oxygen content in insoluble air, and have good application prospects

Active Publication Date: 2020-03-20
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of polycarbosilane non-melting fibers, which solves the technical problem of excessive oxygen content in silicon carbide fibers in the prior art

Method used

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  • Preparation method of polycarbosilane non-melting fiber

Examples

Experimental program
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Embodiment 1

[0026] 100g of polycarbosilane with a softening point of 187°C and an oxygen content of 0.62wt% was dissolved in toluene with 10g of 1,3,5-trivinyl-1,3,5-trimethylcyclotrisilazane, React at 200°C for 3 hours, and distill off the solvent to obtain polycarbosilane for spinning; put polycarbosilane for spinning into the spinning barrel, melt spinning at 328°C, and introduce the concentration through the atomization spraying device after the fibers are bundled. Obtain polycarbosilane fiber for the ethanol solution of 20wt% azobisisobutyronitrile and Irgacure 1800, wherein the introduction amount of azobisisobutyronitrile and Irgacure 1800 is 1.0wt% (relative to polycarbosilane fiber); Carbosilane fibers are placed in ultraviolet light with a wavelength of 200-280nm, and the intensity of ultraviolet light is 2mW / cm 2 10cm under the ultraviolet light generator, under the condition of ultraviolet light, according to the temperature rise rate of 60 ℃ / hour to 60 ℃, after holding for ...

Embodiment 2

[0028] 100g of polycarbosilane with a softening point of 165°C and an oxygen content of 0.3wt% and 15g of tetramethyldivinyldisilazane dissolved in xylene were mixed, reacted at 250°C for 5 hours, and the solvent was distilled off to obtain spinning Use polycarbosilane; put polycarbosilane for spinning into the spinning barrel, melt spinning at 400°C, and introduce dicumyl peroxide with a concentration of 50wt% and ultraviolet light through an atomizing spraying device after the fibers are bundled. The acetone solution of agent 907 obtains polycarbosilane fiber, wherein the introduction amount of initiator is 0.1wt% (relative to polycarbosilane fiber); Polycarbosilane fiber is placed in ultraviolet light wavelength and is 200-280nm, and ultraviolet light power is 10mW / cm 2Under the ultraviolet light generator at 5cm, under the condition of ultraviolet light, the temperature was raised to 100°C at a rate of 1°C / hour, and the polycarbosilane pre-cured fiber was obtained after h...

Embodiment 3

[0030] 100g of polycarbosilane with a softening point of 214°C and an oxygen content of 0.4wt% and 30g of tetramethyldivinyldisilazane dissolved in phenyl-n-hexane were mixed, reacted at 150°C for 1 hour, and the solvent was distilled off to obtain spinning Polycarbosilane for silk; put polycarbosilane for spinning into the spinning cylinder, melt spinning at 325°C, and after the fibers are bundled, introduce a benzoyl peroxide ether solution with a concentration of 1wt% through an atomizing spraying device to obtain Polycarbosilane fiber, wherein the introduction amount of initiator is 2.3wt% (relative to polycarbosilane fiber); Polycarbosilane fiber is placed in ultraviolet light wavelength and is 320-400nm, and ultraviolet light power is 0.1mW / cm 2 50cm under the ultraviolet light generator, under the condition of ultraviolet light, the temperature was raised to 100°C at a rate of 20°C / hour, and the polycarbosilane pre-cured fiber was obtained after 3 hours of heat preservat...

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Abstract

The invention provides a preparation method of polycarbosilane non-melting fiber. The preparation method comprises the following steps: (1) performing blending reaction on polycarbosilane and vinyl silazane, thus obtaining polycarbosilane for spinning; (2) performing melt spinning on the polycarbosilane for spinning, and introducing an initiator, thus obtaining polycarbosilane fiber; (3) crosslinking the polycarbosilane fiber under the action of ultraviolet light and heat, thus obtaining polycarbosilane precurable fiber; and (4) performing thermal treatment on the polycarbosilane precurable fiber in an inert atmosphere, thus obtaining the polycarbosilane non-melting fiber. The preparation method can realize low-oxygen unmelting (less than or equal to 2 weight percent) of the polycarbosilane fiber; used equipment is simple, and the preparation method is relatively low in cost, low in environmental pollution and suitable for industrial continuous production and has an extremely good application prospect in preparation of high-performance SiC fiber.

Description

technical field [0001] The invention relates to the technical field of polycarbosilane, in particular to a preparation method of polycarbosilane non-melting fibers. Background technique [0002] Continuous SiC fiber has high strength, high modulus, excellent resistance to high temperature oxidation, creep resistance, and good compatibility with ceramic matrix. It is an ideal reinforcement for preparing high-performance ceramic matrix composites. The precursor conversion method is the most successful method for preparing fine-diameter continuous SiC fibers, which includes the synthesis of precursor polycarbosilane, melt spinning of polycarbosilane, non-melting of polycarbosilane fibers and high temperature of non-melting polycarbosilane fibers burnt. Among them, the non-melting of polycarbosilane fibers makes polycarbosilane fibers change from thermoplastic polymers to thermosetting polymers, so that the shape of the fibers can be maintained during the subsequent thermal dec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/10D01F11/00C08G77/60C04B35/80
CPCC04B35/80C08G77/60D01F9/10D01F11/00
Inventor 王小宙王浩王军简科邵长伟
Owner NAT UNIV OF DEFENSE TECH