Preparation method for high-purity nanometer-type poly-hydroxy zirconium chloride sol

A polyhydroxyzirconium chloride, nano-type technology, applied in the direction of zirconium halide, nanotechnology, etc., can solve the problems of harsh hydrolysis conditions, cumbersome process, high raw material cost, etc., and achieve the effect of ensuring nano characteristics, high purity and good stability

Inactive Publication Date: 2012-05-23
LUYANG ENERGY SAVING MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the zirconia precursor sol prepared by hydrolysis of zirconium alkoxide has stable colloid and uniform particle size distribution, the hydrolysis conditions are harsh and the cost of raw materials is high [see: Process for preparing zirconia sols and / or zirconia forms, US5238625]; the coprecipitation method is cumbersome , the water-soluble salt of zirconium needs to be precipitated by ammonia method, filtered, washed, and then dissolved by acid or alcohol [see: Preparation and Characterization of Ultrafine Zirconia, Industrial Catalysis, 16 (2008) 23-25]; The law requires high temperature and high pressure, and the disadvantage is that only nano-powders can be prepared, while fibers and films cannot be prepared.

Method used

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  • Preparation method for high-purity nanometer-type poly-hydroxy zirconium chloride sol
  • Preparation method for high-purity nanometer-type poly-hydroxy zirconium chloride sol
  • Preparation method for high-purity nanometer-type poly-hydroxy zirconium chloride sol

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Experimental program
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Effect test

Embodiment 1

[0027] Put 617g of zirconium carbonate powder in water to form a suspension, filter to remove impurities and set aside. Weigh 117g of industrial hydrochloric acid with a concentration of 31wt%, dilute it to 10wt%, add it to the reflux device, and heat up to 50°C; add the zirconium carbonate powder treated above into the hydrochloric acid solution, stir and heat to 80°C until completely dissolved ; Add 25g yttrium chloride, further reflux hydrolysis, until the solution is completely clear and transparent. The solution was distilled under reduced pressure at 80° C. and dehydrated to a concentration of 25 wt % to obtain the final colloid. The particle size distribution of the obtained colloid is shown in figure 1 , and the infrared spectrum after drying is shown in figure 2 , the XRD pattern after calcination at 1000°C is shown in image 3 .

Embodiment 2

[0029] Put 174g of zirconium carbonate powder in water to form a suspension, filter to remove impurities and set aside. Weigh 50g of industrial hydrochloric acid with a concentration of 31wt%, dilute it to 10wt%, add it to the reflux device, and heat up to 50°C; add the zirconium carbonate powder treated above into the hydrochloric acid solution, stir and heat to 70°C until completely dissolved ; Add 10.18g yttrium chloride, further reflux hydrolysis, until the solution is completely clear and transparent. The solution was distilled under reduced pressure at 60° C. and dehydrated to a concentration of 30 wt % to obtain the final colloid.

Embodiment 3

[0031] Put 323 zirconium carbonate powder in water to form a suspension, filter to remove impurities and set aside. Weigh 78.5g of industrial hydrochloric acid with a concentration of 31wt%, dilute it to 8wt%, add it to the reflux device, and heat up to 50°C; add the zirconium carbonate powder treated above into the hydrochloric acid solution, stir and heat to 90°C until completely Dissolve; add 7.9g of yttrium acetate, further reflux and hydrolyze until the solution is completely clear and transparent. The solution was distilled under reduced pressure at 70° C. and dehydrated to a concentration of 40 wt % to obtain the final colloid.

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Abstract

The invention relates to a preparation method for high-purity nanometer-type poly-hydroxy zirconium chloride sol, which is characterized by comprising the following steps: (1) adding water into hydrochloric acid to prepare hydrochloric acid solution of which the concentration is 3-6mol/l, adding water into zirconium carbonate powder while stirring to prepare even suspension, and adding the filtered zirconium carbonate powder into the hydrochloric acid solution to be evenly stirred; (2) back flowing and hydrolyzing the mixture obtained in the step (1) at the temperature of 70-90DEG C until the zirconium carbonate is completely dissolved; (3) adding phase stabilizing agent of which the molar percentage by weight is 3-8% into the solution obtained in the step (2) by taking the mole number of zirconium oxide as a base number, and evenly stirring; and (4) carrying out reduced pressure distillation and dehydration on the mixed liquor obtained in the step (3) at the temperature of 60-80DEG C, and obtaining the poly-hydroxy zirconium chloride sol of which the concentration is 20-40% after filtering. The obtained sol has the advantages of high purity and good stability and is clear and transparent. On a modular level, the sol can be easily doped, and certain organic matters or inorganic matters are added according to the use requirement, so zirconium oxide products of different performances can be conveniently prepared.

Description

technical field [0001] The invention relates to a preparation method of high-purity nano-type polyhydroxy zirconium chloride sol, which belongs to the field of inorganic polymer sol synthesis. Background technique [0002] Zirconia ceramics is an important structural and functional material with excellent physical and chemical properties. Its development, research and application have attracted great attention from all over the world. Based on the size effect of nanomaterials, zirconia materials are nanosized and prepared into nanoscale ZrO with uniform structure 2 Materials (powder, film, fiber, block, etc.), can further expand the performance and application of zirconia materials. [0003] The preparation of uniform, stable, compositional and structurally adjustable zirconia precursors (paste or polyzirconium compounds) by chemical methods is an important prerequisite for the preparation of zirconia nanomaterials and the key to ensuring their nano-performance. The curren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/04B82Y40/00
Inventor 李呈顺鹿成洪鹿俊华岳耀辉徐营
Owner LUYANG ENERGY SAVING MATERIALS CO LTD
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