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Method for preparing continuous zirconia crystal fiber through zirconium acetate oxide-methanol system

A technology of zirconium oxyacetate and crystal fiber, which is applied in the fields of fiber chemical characteristics, climate sustainability, and final product manufacturing, etc., can solve the problems that continuous fibers cannot be melted, precursor fibers are not easily drawn, and the preparation process is complicated. The effect of improving draftability, reducing time and atmosphere consumption, and cheap raw materials

Active Publication Date: 2014-08-20
山东德艾普节能材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Since the melting point of zirconia itself is too high (2715°C) and the melt viscosity is small, its continuous fiber cannot be prepared by melting, and only various precursor methods can be used. The specific method has been described in detail in the patent CN1206397C , but there are still some deficiencies in existing methods
From the perspective of the precursor system, although the method of the organic polyzirconium precursor can prepare a stable precursor sol, the preparation process is complicated, the control conditions are harsh, the viscosity is not easy to control, and the organic solvent volatilizes too fast during the spinning process. The body fiber is brittle and difficult to draw; the study found that in the process of transforming the precursor fiber into the zirconia crystal fiber, the rapid and effective resolution of the ligand and the nucleation temperature, size and uniformity of the zirconia crystal grains have a great influence on the continuity of the fiber. , strength, etc. have an important influence on

Method used

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  • Method for preparing continuous zirconia crystal fiber through zirconium acetate oxide-methanol system
  • Method for preparing continuous zirconia crystal fiber through zirconium acetate oxide-methanol system
  • Method for preparing continuous zirconia crystal fiber through zirconium acetate oxide-methanol system

Examples

Experimental program
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Effect test

Embodiment 1

[0036] (1) Use zirconium oxychloride octahydrate as zirconium source to prepare zirconium oxychloride precursor sol: weigh 100g of zirconium oxychloride and dissolve it in 100ml of anhydrous methanol, and stir until completely dissolved at room temperature around 25°C to form zirconium oxychloride methanol solution; according to the mol ratio of zirconium oxychloride and potassium acetate is 1:2.0, take by weighing 60.9g potassium acetate and be dissolved in 150ml anhydrous methanol to form the methanol solution of potassium acetate; Potassium acetate methanol solution is slowly added dropwise to oxygen Zirconium chloride solution, while vigorously stirring, produced a large amount of white potassium chloride precipitate. The above mixed solution was left to stand at 20°C for 24 hours to allow the precipitate to fully sink to the bottom, and then a solution of zirconium acetate was obtained by vacuum filtration, and the potassium chloride precipitate was separated.

[0037] Ac...

Embodiment 2

[0042] (1) Use basic zirconium carbonate as zirconium source to prepare zirconyl acetate precursor sol: according to the molar ratio of basic zirconium carbonate: glacial acetic acid: anhydrous methanol as 1:2:2, weigh 250g basic zirconium carbonate (molecular formula ZrOCO 3 ·nH 2 O, where ZrO 2 The content of glacial acetic acid and anhydrous methanol is 40wt%), weigh corresponding glacial acetic acid and anhydrous methanol and mix uniformly at the same time, slowly add the mixed solution of glacial acetic acid and anhydrous methanol to basic zirconium carbonate and carry out solid-liquid reaction, until solid dissolves completely, reacts The liquid turns into a transparent solution, and the methanol solution of the polyzirconium precursor is obtained. According to the composition ratio requirements of tetragonal phase and cubic phase coexistence and only cubic phase, the molar ratio is ZrO 2 : Y 2 o 3 = 94.3: 5.7 was mixed with 29 g of yttrium nitrate hexahydrate, conc...

Embodiment 3

[0046] Embodiment 3: As described in Example 1, the difference is that the mol ratio of zirconium oxychloride and potassium acetate is 1:1.8 in the step (1), and 54.8g potassium acetate is dissolved in 150ml methyl alcohol to form potassium acetate methanol solution.

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Abstract

The invention relates to a method for preparing a continuous zirconia crystal fiber through a zirconium acetate oxide-methanol system. The method comprises the following steps: with zirconium oxychloride, acetate or basic zirconium carbonate, glacial acetic acid and methanol as raw materials respectively, performing one-step synthesis to obtain a zirconium acetate oxide precursor sol spinning solution, performing dry spinning combined with a drawing technology to obtain a continuous zirconia precursor fiber, performing pressure resolution in organic steam, water vapor or a mixed atmosphere, and performing medium-high-temperature atmosphere heat treatment to obtain the high-performance continuous zirconia crystal fiber. The fiber is dense, transparent and excellent in high-temperature performance.

Description

technical field [0001] The invention relates to a method for preparing continuous zirconia crystal fibers with high performance and ultra-high temperature resistance, in particular to a method for preparing continuous zirconia crystal fibers with a zirconyl acetate-methanol system, which belongs to the field of structural and functional fiber materials. Background technique [0002] Continuous zirconia crystal fiber is a structural and functional material with great application potential, and it is playing an increasingly important role in aerospace, military and other high-tech and cutting-edge technology fields. [0003] Zirconia crystal fibers are divided into short fibers and continuous fibers. Due to the technical difficulty in the preparation of zirconia fibers, fibers with a length greater than 1 meter are converted into continuous fibers in the world. In the research led by Professor Xu Dong of the State Key Laboratory of Crystal Materials of Shandong University Befo...

Claims

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Application Information

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IPC IPC(8): D01F9/10D01F13/00
CPCY02P70/62
Inventor 许东朱陆益刘雪松王新强张光辉
Owner 山东德艾普节能材料有限公司
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