Zirconium oxide fabrics prepared from organic polyzirconium fore spinning solution by silk process

A technology of zirconia fiber and precursor fiber, which is applied in the field of refractory fiber materials, can solve the problems of poor stability of sol spinning solution, no braidability, narrow application range, etc., and achieve good market application prospects, good spinning performance, The effect of simple and easy route

Inactive Publication Date: 2005-02-23
绍兴市圣诺超高温晶体纤维材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method can produce zirconia fiber felt with high monofilament strength and low cost, it also has inherent disadvantages: such as poor stability of sol spinning solution, easy to gel and fail; spun gel The fibers are bonded to each other due to moisture, and after calcination, only a fiber mat with a network structure can be obtained, which does not have weaving properties and has a narrow application range.

Method used

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  • Zirconium oxide fabrics prepared from organic polyzirconium fore spinning solution by silk process
  • Zirconium oxide fabrics prepared from organic polyzirconium fore spinning solution by silk process
  • Zirconium oxide fabrics prepared from organic polyzirconium fore spinning solution by silk process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Weigh 97 grams of zirconium oxychloride (ZrOCl 2 ·8H 2 (2), be dissolved in 400ml methanol, be zirconium oxychloride according to molar ratio: acetylacetone: the ratio of triethylamine=1: 1: 2, measure 31ml acetylacetone and 84ml triethylamine, be dissolved in 400 milliliters of methanol jointly , under stirring conditions at 4°C, drop the methanol dilution of acetylacetone and triethylamine into the methanol dilution of zirconium oxychloride, and continue stirring for 2 hours after dropping to obtain a golden yellow transparent reaction solution. Distill the methanol solvent under reduced pressure at 40°C until it is almost dry to obtain a light yellow sticky substance. Add 300ml tetrahydrofuran according to the ratio of zirconium oxychloride: tetrahydrofuran = 97g: 300ml, stir to dissolve the soluble matter, and remove the insoluble matter by suction filtration. The white precipitate of triethylamine hydrochloride was obtained, and the golden yellow transparent f...

Embodiment 2

[0041] As described in Example 1, the difference is that 97 grams of zirconium oxychloride (ZrOCl) was weighed in step (1). 2 ·8H 2 O) being dissolved in 400ml methanol is changed into being dissolved in 500ml methanol, and the ratio of the mol ratio=1:1 of zirconium oxychloride: acetylacetone is changed to 1: 1.2, is about to change 31 milliliters of acetylacetone into 37 milliliters of acetylacetone , be dissolved in 500 milliliters of methanol together with 84ml triethylamine, simultaneously in step (2) according to reactant zirconium oxychloride: the ratio of methanol=97g: 200ml, the resulting product zirconium polyacetylacetonate 66g is dissolved in 200ml methanol In the process, according to the ratio of reactant zirconium oxychloride: methanol=97g: 300ml, the resulting product zirconium polyacetylacetonate 67g was dissolved in 300ml methanol, and the spinnability of the obtained spinning solution was slightly better than that of example 1. , the average length of zirco...

Embodiment 3

[0043] As described in Example 1, the difference is that 97 grams of zirconium oxychloride (ZrOCl) was weighed in step (1). 2 ·8H 2 O) being dissolved in 400ml methanol is changed into being dissolved in 600ml methanol, and the ratio of zirconium oxychloride: the mol ratio of acetylacetone=1: 1 is changed to 1: 1.4, is about to change 31 milliliters of acetylacetone into 43 milliliters of acetylacetone , be dissolved in 600 milliliters of methanol together with 84ml triethylamine, simultaneously in step (2) according to reactant zirconium oxychloride: the ratio of methanol=97g: 200ml, the resulting product zirconium polyacetylacetonate 66g is dissolved in 200ml methanol In the process, according to the ratio of reactant zirconium oxychloride: methanol=97g: 400ml, the resulting product zirconium polyacetylacetonate 68g is dissolved in 400ml methanol, and the spinnability of the resulting spinning solution is slightly better than that of Example 2. , the average length of the z...

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Abstract

The manufacture method of a kind of zirconia fibre cotton relates to the field of resistance of fire fibre material. We compose van-style acetamide acetone zirconium polymer according to chloridze zirconia, acetamide acetone and three-ethylamine. We use methanol as the dilute impregnant, we mix round them to let hloridize zirconia, acetamide acetone and three-ethylamine react at 40-20 deg.C, and we can receive poly-acetamide acetone zirconium van-substance. Four-hydrogen furan filtrate and remove the outgrowth hydrochloric three-ethylamine. The offspring dissolve in the filature liquid made of methanol. After centrifugal swing, we can receive van-substance fibre. After we do special hear treatment, the zirconia fibre cotton we receive has the characteristic of good filature ability, high content of zirconium, equality andclarity and jarles capability. It can be used as industrial stove, roomage fusion stove, atomic energy reactor and the high temperature heat insulation material used in aviation and military. The material of the invention cost low, the method is easy, the impregnant can be recycled, the preparation of fibre cost low.

Description

(1) Technical field [0001] The invention relates to a method for preparing oxide refractory fiber cotton, in particular to a method for preparing polycrystalline zirconia fiber cotton with high temperature resistance, good heat insulation and high strength, and belongs to the field of refractory fiber materials. (2) Background technology [0002] Ceramic fiber is a kind of fibrous lightweight refractory material. It has the advantages of light weight, high temperature resistance, good thermal stability, low thermal conductivity, small specific heat capacity and mechanical vibration resistance. It has been widely used in metallurgy, machinery, petroleum, chemical industry, electronics, etc. , Shipbuilding, transportation, light industry and other industrial sectors and cutting-edge technology fields such as aerospace and atomic energy have been widely used. The world's major industrial countries are competing to develop the ceramic fiber industry. Common refractory fibers are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08
Inventor 许东刘和义侯宪钦赵相金王彦玲杜伟张光辉王新强吕孟凯袁多荣
Owner 绍兴市圣诺超高温晶体纤维材料有限公司
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