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Oxygen-free non-melting Polycarbosilane fiber preparation method and device

A polycarbosilane fiber and melting device technology, which is applied in the chemical characteristics of fibers, chemical post-processing of synthetic polymer rayon filaments, textiles and papermaking, etc. The effect of lowering temperature and improving uniformity

Active Publication Date: 2014-10-08
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since conventional devices are based on circulating air ovens, when polycarbosilane fibers are loaded for chemical vapor infusion, the atmosphere concentration and temperature at different positions of polycarbosilane fibers are very different, which often causes polycarbosilane fibers The uniformity of the non-melting degree is poor

Method used

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  • Oxygen-free non-melting Polycarbosilane fiber preparation method and device
  • Oxygen-free non-melting Polycarbosilane fiber preparation method and device
  • Oxygen-free non-melting Polycarbosilane fiber preparation method and device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Impregnate 100g of polycarbosilane fibers with 10g of dibenzoyl peroxide solution (solvent is acetone) with a mass fraction of 10% in a continuous method, the impregnation speed is 0.5m / min, the impregnation time is 24s, and wound into polycarbonate Silane fiber precursor tube; (2) Then, place the impregnated polycarbosilane fiber precursor tube in a blast oven at 60°C and dry until the moisture content is 0.5wt%; (3) Dry the polycarbosilane fiber precursor tube The carbosilane fiber precursor tube is placed on the round roller heated by the shaft center, the anaerobic non-melting device is evacuated to 10Pa, and then the nitrogen gas (purity is 99.999%) is replaced to normal pressure, and repeated three times, 100g of divinylsilane After the gasification chamber is gasified, it circulates in the device through the circulating fan; (4) raise the temperature of the tube furnace to 100°C at a rate of 5°C / h, keep the temperature constant for 6h, and then raise the tempe...

Embodiment 2

[0052] (1) Impregnate 100g of polycarbosilane fibers with 5g of di-tert-butyl peroxide solution (solvent is ethanol) with a mass fraction of 5% by continuous method, the impregnation speed is 0.6m / min, the impregnation time is 20s, and wound into polycarbonate Silane fiber precursor tube; (2) Then, place the impregnated polycarbosilane fiber precursor tube in a blast oven at 50°C and dry until the water content is 0.5wt%; (3) Dry the polycarbosilane fiber precursor tube The carbosilane fiber precursor tube is placed on the round roller heated by the shaft center, the anaerobic non-melting device is evacuated to 8Pa, and then the argon gas (purity is 99.999%) is replaced to normal pressure, and repeated three times, 50g of tetravinylsilane is placed in After gasification in the gasification chamber, the circulating fan circulates in the device; (4) Heat the tube furnace to 130°C at a rate of 10°C / h, keep the temperature constant for 12 hours, and then raise the temperature to 40...

Embodiment 3

[0054] (1) Impregnate 300g of polycarbosilane fibers with 15% mass fraction of azobisisobutyronitrile solution (the solvent is a mixed solution, in which ethanol accounts for 95wt% and water accounts for 5wt%) 20g by continuous method, and the impregnation speed is 1.0m / min, the impregnation time is 12s, and it is wound into a polycarbosilane fiber precursor tube; (2) Then, place the impregnated polycarbosilane fiber precursor tube in a blast oven at 40°C and dry until the water content is 0.5wt%; (3) Place the dried polycarbosilane fiber precursor cylinder on a round roller heated at the center of the axis, vacuumize the anaerobic non-melting device to 5Pa, and then replace argon (purity is 99.999%) to Normal pressure, repeated four times, after gasification of 180g divinylmethylphenylsilane in the gasification chamber, circulate in the device through the circulation fan; (4) raise the temperature of the tube furnace to 155 ℃, and keep the temperature constant for 16 hours, ...

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Abstract

The invention provides an oxygen-free non-melting polycarbosilane fiber preparation method and device. The method comprises the following steps: immersing polycarbosilane fibers into a solution of a peroxide or azo-compound free radical initiator; drying and putting the polycarbosilane fibers into a heating device; vacuumizing and replacing nitrogen or argon; gasifying silane containing vinyl or silazane containing vinyl and circulating in the device; carrying out two-section temperature rising heating under an axis-heating temperature field; and cooling to a room temperature to obtain oxygen-free non-melting polycarbosilane fibers. The invention further provides the oxygen-free non-melting polycarbosilane fiber preparation device which comprises a gasification chamber (1), a circulating fan (2), a reverse spoiler (3), an axis heating circular roller (4) and a tube furnace (5). The oxygen-free non-melting polycarbosilane fiber preparation method and device have the advantages that a chemical gas phase non-melting method is adopted to prevent introduction of oxygen; the non-smelting process of the polycarbosilane fibers is completed under a low temperature; an airflow field of an active atmosphere is uniform; the axis heating is used for uniformly heating the fibers at different positions.

Description

technical field [0001] The invention relates to a crosslinking method and device for polycarbosilane fibers, in particular to an oxygen-free non-melting method and device for polycarbosilane fibers. Background technique [0002] Polycarbosilane fiber is an organic polymer fiber prepared by spinning polycarbosilane, and it is also a fibril of silicon carbide ceramic fiber. In order to prevent the fibrils from melting and losing their fiber shape during the mineralization process, it is necessary to form a three-dimensional network structure before the fibrils are melted. This process is called non-melting. After polycarbosilane fiber is not melted, it is no longer melted, and it can maintain the shape of the fiber during the process of high-temperature inorganicization. The non-melting method of polycarbosilane plays an extremely important role in the composition, structure and properties of SiC fibers. [0003] At present, polycarbosilane fiber non-melting methods include ...

Claims

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Application Information

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IPC IPC(8): D01F11/08D01F9/10C04B35/565
Inventor 邵长伟王军王浩宋永才简科王小宙
Owner NAT UNIV OF DEFENSE TECH
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