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
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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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