Catalytic crosslinking method for polycarbosilane fiber

A technology of polycarbosilane fiber and cross-linking method, which is applied in the chemical characteristics of fibers, chemical post-treatment of synthetic polymer rayon filaments, textiles and papermaking, etc. Simple process, suitable for mass production

Active Publication Date: 2012-07-18
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The oxygen content of the prepared SiC fiber is 6wt%~9wt%, and

Method used

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  • Catalytic crosslinking method for polycarbosilane fiber
  • Catalytic crosslinking method for polycarbosilane fiber
  • Catalytic crosslinking method for polycarbosilane fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Preparation of catalyst solution: Dissolve 0.1 g of chloroplatinic acid in 100 mL of deionized water to prepare a catalyst solution; (2) Spin PCS fibrils (FT IR such as figure 1 As shown) the beam slowly passes through the catalyst chloroplatinic acid aqueous solution tank and dries in the air; (3) Place the PCS fibrils containing the catalyst in a chemical vapor phase crosslinking system, vacuumize and fill it with high-purity nitrogen to normal pressure, Repeat 3 times; (4) Introduce 1,3-butadiene gas; (5) Program temperature rise to 180°C, reaction time 6h; (6) Heat up to 450°C, keep warm for 6h, then cool to room temperature to obtain PCS Cross-linked fibers (FT IR as figure 2 shown).

[0033] 2100cm in the FT IR spectrum -1 Si-H absorption peak with 1250cm -1 Si-CH 3 The absorbance ratio of the absorption peak (A Si-H / A Si-CH3 ) to study the Si-H bond content of PCS and crosslinked fibers. From figure 1 The FT IR can calculate the SiH content of PCS f...

Embodiment 2

[0035] (1) Dissolve 0.2g of potassium tetrachloroplatinite in 100mL of deionized water to prepare a catalyst solution; (2) Slowly pass the spun PCS fibril bundles through the tank of potassium tetrachloroplatinite aqueous solution, and dry in the air ; (3) Put the PCS fibrils containing the catalyst potassium tetrachloroplatinite in the chemical vapor phase crosslinking system, fill it with high-purity nitrogen to normal pressure after vacuuming, and repeat three times; (4) Pass 1,4- Pentadiene gas; (5) program temperature rise to 180°C, reaction time 6h; (6) program temperature rise to 450°C, keep warm for 6h, after cooling, PCS cross-linked fiber can be obtained.

[0036] The FT IR spectrogram of gained PCS cross-linked fiber and figure 2 Basically the same, only the intensity of the absorption peak is slightly different. According to the FT IR spectrum, the calculated Si-H bond content of the crosslinked fiber is 0.135, the Si-H bond reaction degree is 85.9%, and the gel ...

Embodiment 3

[0038] (1) Dissolve 0.3g of triphenylphosphine rhodium chloride in 100mL of ethanol to prepare ethanol solution of catalyst triphenylphosphine rhodium chloride; (2) Spray catalyst triphenylphosphine rhodium chloride ethanol solution on (3) place the PCS fibrils containing the catalyst triphenylphosphine rhodium chloride in a chemical vapor phase cross-linking system, and fill it with high-purity nitrogen to normal pressure after vacuuming, Repeat 3 times; (4) Introduce acetylene gas; (5) Program temperature rise to 200°C, reaction time 8h; (6) Program temperature rise to 460°C, keep warm for 8h; PCS crosslinked fiber can be obtained after cooling.

[0039] FT IR spectra of PCS crosslinked fibers and figure 2 Basically the same, only the intensity of the absorption peak is slightly different. According to the FT IR spectrum, the calculated Si-H bond content of the crosslinked fiber is 0.167, the Si-H bond reaction degree is 82.6%, and the gel content is 98.4%. The ceramic yi...

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Abstract

The invention discloses a catalytic crosslinking method for polycarbosilane fiber. The catalytic crosslinking method comprises the following steps of: catalytic solution preparation: taking 0.1-0.3g of catalyst noble metal compound to dissolve in 100mL of deionized water or ethanol; causing polycarbosilane fibril to pass through a catalyst aqueous solution slot, or spraying catalyst ethanol solution onto the polycarbosilane fibril through a spraying method, and drying; arranging the polycarbosilane fibril (which is obtained in step two) containing the catalyst noble metal compound into a chemical gaseous phase crosslinking system, vacuumizing, exchanging gas in a kettle by nitrogen to normal pressure, and repeating for 2-4 times; introducing alkadiene or alkyne; conducting programmable heating to 50-250DEG C, and reacting for 0.5-12h; and heating to 350-500DEG C, keeping warm for 0.5-2h, and cooling to the room temperature to obtain the polycarbosilane fiber. The catalytic crosslinking method has simple and convenient technology and low cost and is suitable for large-scale production.

Description

technical field [0001] The invention relates to a crosslinking method of a polycarbosilane precursor, in particular to a catalytic crosslinking method of polycarbosilane fibers. Background technique [0002] As a new type of ceramic fiber, silicon carbide (SiC) fiber has the characteristics of low density, high specific strength, high specific modulus, small linear expansion coefficient, high temperature resistance, corrosion resistance, high strength, etc. Good composite compatibility, it is an ideal reinforcing fiber for high performance composite materials. At the same time, SiC fiber integrates structure, stealth and heat protection, and has broad application prospects in some high-tech fields such as aerospace, aviation, weapons, ships and nuclear industries. [0003] The organic precursor conversion method uses organic polymers (mostly organometallic polymers) as raw materials, utilizes their soluble and fusible characteristics to achieve molding, and undergoes high-t...

Claims

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Application Information

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IPC IPC(8): D01F11/08D01F9/10C04B35/565
Inventor 谢征芳王军宋永才卲长伟
Owner NAT UNIV OF DEFENSE TECH
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