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Method for preparing zirconium oxide refractory fibre

A technology of refractory fiber and zirconia, applied in the field of refractory fiber materials, can solve the problems of high preparation cost, low fiber strength, complicated process steps, etc., and achieve the effect of low cost, good spinning performance and high purity

Active Publication Date: 2011-07-06
山东红阳高温节能材料股份有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0049] The present invention aims at the shortcomings of the existing zirconia fiber preparation techniques, such as low fiber strength obtained by the dipping method, unstable spinning solution by the mixing method, expensive raw materials for the sol-gel method, and organic pollution by the organic polyzirconium method. Larger, and the common problems of complex process steps, high preparation costs, and difficulty in industrialization of each method, a very simple inorganic colloid spinning method is provided to prepare high-quality zirconia refractory fibers, that is, the use of oxychlorination Zirconium and hydrogen peroxide aqueous solution are used as the main raw materials, and yttrium trichloride or yttrium nitrate is used as the phase stabilizer raw material. Under appropriate temperature, stirring and air extraction conditions, the above raw materials are mixed and reacted according to a certain stoichiometric ratio, and then the pressure is reduced. Concentrate to obtain high-viscosity inorganic zirconium spinnable adhesive liquid, obtain inorganic zirconium gel fiber through centrifugation, heat-treat and sinter the gel fiber, and finally obtain the preparation method of zirconia refractory fiber

Method used

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Examples

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Effect test

Embodiment 1

[0068] (1) Preparation of inorganic zirconium spinnable glue: according to the composition ratio requirements of tetragonal zirconia (molar ratio ZrO 2 : Y 2 o 3 =97:3), weigh 100g zirconium oxychloride (ZrOCl 2 ·8H 2 O, molecular weight 322.25, purity > 99.5%) and 5.82g yttrium trichloride (YCl 3 ·6H 2 (2, molecular weight 303.36, purity > 99.9%); In addition, according to the molar ratio of zirconium oxychloride: the ratio of hydrogen peroxide=1: 4.5, measure 143mL mass percentage concentration and be 30% hydrogen peroxide aqueous solution (H 2 o 2 / H 2 O, analytically pure); under stirring and pumping conditions, hydrogen peroxide aqueous solution was mixed with zirconium oxychloride and yttrium trichloride, reacted and accompanied by chlorine gas release, after the reaction was completed, the resulting solution was heated to 70 Under reduced pressure distillation at ℃ to remove excess water, until an inorganic zirconium spinnable adhesive solution with a viscosity o...

Embodiment 2

[0072] As described in Example 1, the difference is that step (1) is changed to "preparation of inorganic zirconium spinnable glue: according to the composition ratio requirements of cubic phase zirconia (molar ratio ZrO 2 : Y 2 o 3 =92:8), weigh 100g zirconium oxychloride (ZrOCl 2 ·8H 2 O, molecular weight 322.25, purity > 99.5%) and 16.37g yttrium trichloride (YCl 3 ·6H 2 (2, molecular weight 303.36, purity > 99.9%); In addition, according to the molar ratio of zirconium oxychloride: the ratio of hydrogen peroxide=1: 5.5, measure 174mL mass percent concentration and be 30% hydrogen peroxide aqueous solution (H 2 o 2 / H 2 O, analytically pure); under stirring and pumping conditions, hydrogen peroxide aqueous solution was mixed with zirconium oxychloride and yttrium trichloride, reacted and accompanied by the release of chlorine gas, after the reaction was completed, the resulting solution was warmed up to 80 °C to carry out vacuum distillation to remove excess water un...

Embodiment 3

[0074] As described in Example 1, the difference is that step (1) is changed to "preparation of inorganic zirconium spinnable glue: according to the composition ratio requirements of the coexistence of tetragonal phase and cubic phase zirconia (molar ratio ZrO 2 : Y 2 o 3 =95:5), weigh 100g zirconium oxychloride (ZrOCl 2 ·8H 2 O, molecular weight 322.25, purity > 99.5%) and 9.91g yttrium trichloride (YCl 3 ·6H 2 (2, molecular weight 303.36, purity > 99.9%); According to the ratio of zirconium oxychloride: hydrogen peroxide=1: 5 in addition, measure 158mL mass percent concentration and be 30% hydrogen peroxide aqueous solution (H 2 o 2 / H 2 O, analytically pure); under stirring and pumping conditions, hydrogen peroxide aqueous solution was mixed with zirconium oxychloride and yttrium trichloride, reacted and accompanied by chlorine gas release, after the reaction was completed, the resulting solution was heated to 75 °C to carry out vacuum distillation to remove excess w...

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Abstract

The present invention provides a method for preparing a zirconium oxide refractory fiber. The method adopts zirconium oxychloride, aqueous hydrogen peroxide solution, yttrium chloride or yttrium nitrate as raw material, the inorganic zirconium spinnable glue solution is made by reaction and compression, the gelatinous fiber can be obtained by centrifugal fiber forming, and after heat treating sintering the zirconium oxide refractory fiber which has the following advantages can be obtained: crystal phase composition with square phase and / or cubic phase zirconium oxide, purity up to 99.5% above, diameter around 5 mu m, length approximate continuous, soft and flexible property and without slag including sphere. The using temperature of the fiber is above 1600 DEG C, the material can be used as extreme temperature refractory, heat insulation material, protecting material, ablative material, satellite battery separator material and the like, used for the fields of aerospace, war industry and national defense, atomic energy and the like; the fiber can also be used as the flame-proof heat-insulating material of the extraordinary high-temperature electric furnace with temperature 1600 DEGC to 2200 DEG C, the oil or gas burning furnace and other extraordinary high-temperature heating mechanism, and is used for the fields of ceramic sintering, crystal growth, metal smelting, petroleum cracking, scientific researching and the like. The invention totally adopts the inorganic raw material, has the advantages of low cost, no pollution, simple technique and excellent effect.

Description

(1) Technical field [0001] The invention relates to a preparation method of an ultra-high temperature zirconia refractory fiber, belonging to the field of refractory fiber materials. (2) Background technology [0002] The traditional refractory fiber refers to aluminum silicate fiber, which was successfully prepared in 1941 by Babcock Wilcox Company of the United States. Because refractory fiber has the advantages of light weight, good heat insulation, small heat capacity, high temperature resistance, thermal shock resistance, etc., it is also easy to process and form various products such as blankets, felts, boards, cloth, paper, special-shaped parts, etc., and the construction is convenient. And it has been widely used in many fields such as steel, electric power, petroleum, building materials, chemical industry, electronics, aerospace and scientific research, and the output of refractory fiber in the world is increasing year by year. [0003] However, with the rapid deve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/66C04B35/48
Inventor 刘和义孙启宝张敏
Owner 山东红阳高温节能材料股份有限公司
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