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Preparation of complete stable cubic phase zircite crystal fibre

A technology of phase zirconia and crystal fiber, which is applied in the field of refractory materials and heat preservation, can solve the problems of being short, can only be used in environments below 1600 °C, has little practical significance, and is easy to pulverize, etc., and achieves moderate strength and high temperature The effect of stable performance and simple process

Inactive Publication Date: 2009-08-05
SHANDONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the fiber cotton prepared by this patent is a tetragonal phase or a mixture of tetragonal phase and cubic phase. It is easy to pulverize at high temperature and has a short service life. It can only be used in an environment below 1600 ° C. At the same time, the solvent used in this patent is methanol. The physical damage of the operating workers is great, and the practical application is of little significance

Method used

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  • Preparation of complete stable cubic phase zircite crystal fibre
  • Preparation of complete stable cubic phase zircite crystal fibre
  • Preparation of complete stable cubic phase zircite crystal fibre

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The preparation method of the fully stable cubic phase zirconia crystal fiber of the present invention adopts the following steps:

[0036] (1) Weigh zirconium oxychloride (ZrOCl 2 ·8H 2(2) 100g, be dissolved in 800ml ethanol, be zirconium oxychloride according to molar ratio: acetylacetone: the ratio of triethylamine=1:1.8:2.5, measure 60ml acetylacetone and 110ml triethylamine, be dissolved in 800 milliliters jointly In ethanol, under stirring conditions at 5°C, atomize the ethanol dilution of acetylacetone and triethylamine into the ethanol dilution of zirconium oxychloride, and continue stirring for 3 hours after the addition to obtain a golden yellow transparent reaction solution. Remove the solvent ethanol by rotary evaporation at 40°C until it is nearly dry, and obtain a light yellow sticky substance. Add 500ml of acetone according to the ratio of zirconium oxychloride: acetone = 100g:500ml, stir to dissolve the soluble matter, and press filter to remove the ins...

Embodiment 2

[0042] As described in Example 1, the difference is that 100 grams of zirconium oxychloride (ZrOCl) was weighed in step (1). 2 ·8H 2 O) be dissolved in 800ml ethanol instead be dissolved in 900ml ethanol, and change the ratio of zirconium oxychloride: the mol ratio of acetylacetone=1:1.8 to 1:2.0, be about to change 60 milliliters of acetylacetone into 67 milliliters of acetylacetone , be dissolved in 900 milliliters of ethanol together with 110ml triethylamine, simultaneously with reactant zirconium oxychloride in step (2): the ratio of ethanol=100g: 20ml, 70g of gained product are dissolved in 20ml ethanol, change according to Reactant zirconium oxychloride: the ratio of ethanol=100g:30ml, 70g of the product obtained is dissolved in 30ml ethanol.

Embodiment 3

[0044] As described in Example 1, the difference is that 100 grams of zirconium oxychloride (ZrOCl) was weighed in step (1). 2 ·8H 2 O) be dissolved in 800ml ethanol instead be dissolved in 1000ml ethanol, and zirconium oxychloride: the mol ratio of acetylacetone=1:1.8 is changed into 1:1.9, is about to change 60 milliliters of acetylacetones into 63 milliliters of acetylacetones , and 110ml triethylamine are dissolved in 1000 milliliters of ethanol, simultaneously with reactant zirconium oxychloride: ethanol=100g: 20ml ratio in the step (2), the obtained product zirconium polyacetylacetonate 70g is dissolved in 20ml ethanol In the present invention, according to the ratio of the reactant zirconium oxychloride: ethanol=100g: 40ml, 70g of the obtained product was dissolved in 40ml of ethanol.

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Abstract

The invention relates to a method of preparing full-stable and cubic-phase zirconia crystal fibers, which mainly comprises the following steps: using zirconium oxychloride, acetylacetone and triethylamine as main raw material and using ethanol as diluent solvent to directly react at a temperature of 0 DEG C to 50 DEG C under a stirring condition so as to generate an organic polymer solution comprising zirconium; evaporating the ethanol and using acetone as solvent to dissolve soluble substances and filter and remove an undissolved substance of triethylamine hydrochloride; recycling the acetone, dissolving the obtained products and yttrium salt to the ethanol to prepare a spinning solution which is centrifugally flung at a high speed to obtain organic polymer fibers comprising zirconium; and carrying out heat treatment in a special atmosphere and ultra-high temperature treatment of the organic polymer fibers comprising zirconium. The invention has simple preparation technology and can recycle the solvent, and the prepared crystal fibers have single ingredients, high purity and stable high-temperature performance and can be used in a range from 1700 DEG C to 2150 DEG C for a long time.

Description

technical field [0001] The invention relates to a preparation method of zirconia crystal fiber, in particular to a preparation method of fully stable cubic phase zirconia crystal fiber, which belongs to the technical field of thermal insulation and refractory materials. Background technique [0002] Zirconia has excellent physical and chemical properties such as high melting point (2715°C), low high-temperature vapor pressure, corrosion resistance, and oxidation resistance. It is widely used as thermal insulation and refractory materials in high-temperature fields above 1700°C. At present, the form of hollow spherical bricks is generally used. use. Compared with crystal fibers, hollow ball bricks have larger thermal conductivity, higher heat capacity, and poor thermal insulation effect. However, the maximum service temperature of traditional mullite crystal fiber and alumina crystal fiber is only 1400°C and 1600°C, which cannot be used in a high temperature environment abov...

Claims

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Application Information

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IPC IPC(8): D01F9/12C01G25/02
Inventor 侯宪钦李现祥
Owner SHANDONG UNIV
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