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Method and equipment of preparing high performance zirconium oxide continuous fiber

A continuous fiber, zirconia technology, applied in the direction of zirconia, inorganic raw material rayon, etc., can solve the problems that continuous fibers cannot be prepared by melting method, the zirconium dispersion in the mixing method is not uniform enough, and can not be used continuously, etc. Molecular weight distribution range, reduction of property non-uniformity, effect of improving fiber properties

Inactive Publication Date: 2003-12-03
绍兴市圣诺超高温晶体纤维材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the melting point of zirconia is too high, its continuous fiber cannot be prepared by melting method, only various precursor methods as mentioned above can be used, and the existing technologies all have their own shortcomings.
From the perspective of the precursor system, the zirconium content in the impregnation method is too low, and it is difficult to prepare high-strength zirconia fibers; from the performance of the spinning solution, the dispersion of zirconium in the mixing method is not uniform enough, the spinning is easy to block and the preparation of nano-sized zirconia The microparticle process is very complicated. The properties of the sol spinning solution in the sol-gel method are not stable, and it is easy to spontaneously turn into a gel, which affects spinning or even cannot be used continuously; in terms of heat treatment, there are also certain deficiencies.
Therefore, the existing technology is difficult to ensure that the prepared zirconia fibers are as continuous as carbon fibers and quartz fibers and can have high strength.

Method used

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  • Method and equipment of preparing high performance zirconium oxide continuous fiber
  • Method and equipment of preparing high performance zirconium oxide continuous fiber
  • Method and equipment of preparing high performance zirconium oxide continuous fiber

Examples

Experimental program
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Effect test

Embodiment 1

[0053] (1) 97.0 grams of high-purity zirconium oxychloride (ZrOCl 2 ·8H 2 O) be dissolved in 1000 milliliters of methanol, under ice bath at 0~4 ℃, according to the ratio of zirconium oxychloride: acetylacetone: triethylamine=1: 1.5: 2 in molar ratio, successively add 46.0 milliliters of acetylacetone dropwise and 84.0 ml of triethylamine, stirring continuously during the dropwise addition, after the dropwise addition, remove the ice bath, continue to stir at room temperature for 2 hours, evaporate the solvent methanol with a rotary evaporator, until dry, add 500 ml of tetrahydrofuran, stir vigorously After 1 hour, filter with suction to remove the white precipitate, then use a rotary evaporator to evaporate the solvent tetrahydrofuran from the filtrate until a dried light yellow hardened substance is obtained, add 700 ml of n-hexane, stir vigorously for 24 hours, filter with suction, and dry the precipitated filter cake to obtain 61.2 grams of zirconium polyacetylacetonate w...

Embodiment 2

[0058] As described in Example 1, the difference is that 97.0 grams of high-purity zirconium oxychloride is replaced by 97.0 grams of commercially pure zirconium oxychloride in step (1), and the tensile strength of the continuous zirconia fiber obtained is the result of comparative example 1 slightly worse.

Embodiment 3

[0060] As described in Example 1, the difference is that the ratio of zirconium oxychloride in step (1): the molar ratio of acetylacetone=1:1.5 is changed to 1:1, that is, 46.0 milliliters of acetylacetone is changed to 30.7 milliliters of acetylacetone , The tensile strength of the obtained zirconia continuous fiber is slightly higher than that of Example 1.

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Abstract

A process for preparing high-performance continuous fibre of zirconium oxide includes such steps as synthesizing acetylacetone-zirconium polymer as precursor from acetylacetone and zirconium oxychloride as main materials, dissolving in methanol to obtain the spinning solution, drying spinning to obtain continuous fibre of precursor, heat treating in a multifunctional sintering furnace by special atmosphere and high-temp. airflow spraying for stretching. Its advantages are high tensile strength (over 2.6 GPa) and long length up to several kilometers.

Description

(1) Technical field [0001] The invention relates to a method for preparing high-performance high-temperature oxide fibers, in particular to a method for preparing continuous zirconia fibers with high strength, high toughness, high temperature resistance and good heat insulation, belonging to the field of structural and functional fiber materials . (2) Background technology [0002] With the development of economy and science and technology, fiber materials such as quartz fiber, carbon fiber, glass fiber and oxide ceramic fiber are playing an increasingly important role in optical communication, aerospace, military and other high-tech and cutting-edge technology fields. important role. [0003] Zirconia continuous fiber is a structural and functional material with great application potential. Compared with other fibers, it has many unique and irreplaceable superior properties. The thermal conductivity of zirconia is the smallest among all metal oxides, which determines that...

Claims

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Application Information

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IPC IPC(8): C01G25/02C04B35/48D01F9/08
Inventor 许东刘和义侯宪钦王彦玲汪晨吕孟凯袁多荣陈代荣刘久荣潘梅
Owner 绍兴市圣诺超高温晶体纤维材料有限公司
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