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Method for preparing organic poly-zirconium precursor or silk-thrawn liquor thereof for zirconia fiber production by one-step solvent method

A technology of zirconia fiber and zirconium precursor, which is applied in the field of preparation of organic polyzirconium precursor or its spinning liquid, can solve the problems of high product cost and complicated process, and achieve simplified production process, simplified process flow and high yield Improved effect

Inactive Publication Date: 2012-11-07
SHANDONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wherein CN03112408.9, CN200410024262.7 and CN200910013781.7 adopt multiple solvents to prepare polyacetylacetonate zirconium precursor in multiple steps. Although industrialized production has been realized, the process is relatively complicated, resulting in high product cost. Therefore, further research is needed Improve

Method used

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  • Method for preparing organic poly-zirconium precursor or silk-thrawn liquor thereof for zirconia fiber production by one-step solvent method
  • Method for preparing organic poly-zirconium precursor or silk-thrawn liquor thereof for zirconia fiber production by one-step solvent method
  • Method for preparing organic poly-zirconium precursor or silk-thrawn liquor thereof for zirconia fiber production by one-step solvent method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Weigh 100g of zirconium oxychloride octahydrate, 31.1g of acetylacetone and 18.6g of ethylenediamine respectively, and add them into 880g of methanol under stirring conditions at 0~50°C for a full reaction for 3 hours to obtain zirconium polyacetylacetonate and ethylenediamine hydrochloride, the crude product of ethylenediamine hydrochloride was removed by suction filtration to obtain a methanol solution of zirconium polyacetylacetonate, and the resulting solution was concentrated under reduced pressure at 20-50°C to recover methanol to obtain a light yellow precursor polyacetylacetonate Zirconium 74.3g (such as figure 1 ); the crude product of ethylenediamine hydrochloride removed by suction filtration was recrystallized with pure water to obtain 39.8 g of high-purity ethylenediamine hydrochloride crystals with a purity of 99.0%.

Embodiment 2

[0047] As described in Example 1, the difference is that the methanol solvent is replaced by 880 g of ethanol solvent. After concentration under reduced pressure, 74.6 g of the light yellow precursor polyacetylacetonate zirconium was obtained; the crude product of ethylenediamine hydrochloride removed by suction filtration was recrystallized with pure water to obtain 40.1 g of high-purity ethylenediamine hydrochloride crystals with a purity of 99.0% .

Embodiment 3

[0049] As described in Example 1, the difference is that methanol was replaced by isopropanol to obtain a light yellow precursor zirconium polyacetylacetonate.

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Abstract

The invention relates to a method for preparing organic poly-zirconium precursor or silk-thrawn liquor thereof for zirconia fiber production by one-step solvent method. The method includes proportioning zirconium oxychloride octahydrate, ligand acetyl acetone, ethyl acetoacetate or alcohol ether, precipitation separation agent C1-C5 which is straight-chain diamine or branched-chaine diamine, triethanolamine, ornithine or ammonia gas, phase stabilizer which is yttrium, calcium, magnesium or cerium chloride and the like according a certain ratio, adding solvent C1-C4 alcohol or mixture solvent thereof to sufficiently react with stirring at the temperature of 0-50 DEG C, filtering to remove hydrochloride, subjecting the obtained solution to pressure reduction and concentration at the temperature of 20-50 DEG C to obtain organic poly-zirconium precursor or silk-thrawn liquor; and obtaining high-quality zirconia crystal fibers by centrifugal silk throwing and fiber thermal treatment. Compared with the conventional zirconia fiber preparation technology, the method for preparing organic poly-zirconium precursor has the advantages of simple process, low cost, high yield, environment-friendliness, and product obtained is high in quality and the like.

Description

technical field [0001] The invention relates to a method for preparing an organic polyzirconium precursor or its spinning solution for producing zirconia crystal fibers by using an organic polyzirconium method, in particular to a method for preparing the organic polyzirconium precursor or its spinning solution by a one-step solvent method. Background technique [0002] With the advancement of cutting-edge technology and the rapid development of modern industry, the requirements for the temperature resistance and heat insulation performance of refractory and heat-insulating fibers are getting higher and higher. It is used for a long time and has the disadvantage of high energy consumption. Zirconia is currently the only oxide with high temperature resistance, the lowest thermal conductivity, the lowest high temperature vapor pressure and excellent acid and alkali corrosion resistance. Compared with other inorganic fibers, zirconia fibers have many unique and irreplaceable su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/00C04B35/48
Inventor 许东王新强朱陆益刘久荣张光辉林学军刘雪松
Owner SHANDONG UNIV
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