Preparation method of zirconium oxide colloidal sol

A technology of zirconium oxide and zirconium oxychloride, applied in the direction of zirconium oxide, etc., can solve the problems of poor colloid time stability and wide particle size distribution, and achieve the effects of strong versatility, low reaction temperature and high purity

Inactive Publication Date: 2007-04-18
上海西源新能源技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the colloid prepared in this way has poor time stability, wide particle size ...

Method used

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  • Preparation method of zirconium oxide colloidal sol

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Experimental program
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Effect test

Embodiment 1

[0026] Weigh 10g ZrOCl 2 ·H 2 O, molar ratio: Zr 4+ :H 2 o 2 The ratio of =1:2.8 takes by weighing 8.44g concentration and is 35% hydrogen peroxide. Calculated according to the preparation concentration of 0.5mol / L sol, the final volume of the solution is 62ml, remove the 7.6ml of water introduced by hydrogen peroxide, and then measure 50ml of deionized water (leaving a small amount of room for the final supplement), according to the ratio of A:B=4:1 Divide into two parts, take A to dissolve ZrOCl 2 ·H 20, and add 2.5ml of acetone, acetylacetone, PEG200 mixed solution whose volume ratio is: 2:1:1. Take B and mix it with hydrogen peroxide, and add 2ml of ethanol. Under continuous vigorous stirring, add dropwise at a speed of 0.5ml / min. After the dropwise addition, continue to stir for 3 hours and make up the solution volume to 62ml, so that the final solution concentration is 0.5mol / l, then stand still and age for 5-10 hours. Prepared ZrO 2 The particle size distribut...

Embodiment 2

[0028] Weigh 10g ZrOCl 2 ·H 2 O, molar ratio: Zr 4+ :H 2 o 2 The ratio of =1:4.3 takes by weighing 12.96g concentration and is 35% hydrogen peroxide. Calculated according to the preparation concentration of 0.5mol / L sol, the final solution volume is 62ml, remove the water volume introduced by hydrogen peroxide 11.6ml, then measure 50ml deionized water, divide it into two parts according to the ratio of A:B=4:1, take A to dissolve ZrOCl 2 ·H 2 0, and add 4.5ml of acetone, acetylacetone, PEG200 mixed solution whose volume ratio is: 2:1:1. Mix B with hydrogen peroxide and add 2ml of ethylene glycol. Under continuous vigorous stirring, add dropwise at a rate of 0.3ml / min. After the dropwise addition, continue to stir for 3 hours and make up the solution volume to 62ml, so that the final solution concentration is 0.5mol / l, then stand still and age for 5-10 hours. Prepared ZrO 2 The particle size distribution of the sol is shown in area B in Figure 1.

Embodiment 3

[0030] Weigh 10gZrOC1 2 ·H 2 O, molar ratio: Zr 4+ :H 2 o 2 =The ratio of 1:6.5 takes by weighing 19.59g concentration and is the hydrogen peroxide of 35%. According to the calculation of the preparation concentration of 0.5mol / L sol, the final solution volume is 62ml, remove the water volume introduced by hydrogen peroxide 17.9ml, then measure 42ml of deionized water, divide it into two parts according to the ratio of A:B=3:1, take A to dissolve ZrOCl 2 ·H 2 0, and the volume ratio of the mixed solution of acetone, acetylacetone, and PEG200 added in 5.5 ml is: 2:1:1. Mix B with hydrogen peroxide and add 2ml of ethylene glycol. Under continuous vigorous stirring, add dropwise at a rate of 0.1ml / min. After the dropwise addition, continue to stir for 3 hours and make up the solution volume to 62ml, so that the final solution concentration is 0.5mol / l, then stand still and age for 5-10 hours. Prepared ZrO 2 The particle size distribution of the sol is shown in area C in...

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Abstract

The present invention discloses a method for preparing zirconium oxide sol. Said method includes the following steps: using zirconium oxychloride as precursor body, using hydrogen peroxide as hydrolysis accelerating agent, utilizing strong oxidative property of hydrogen peroxide to make chlorine ions be reduced into chlorine gas and make said chlorine gas be overflowed so as to obtain the colloid whose particle size distribution is narrow. Said invention makes the zirconium oxychloride be dissolved in a proper quantity of mixed solution formed from alcohol, water and surfactant, uniformly mixes and stirs them, and selects proper surfactant, and utilizes a simple technological process to prepare high-purity and stable zirconium oxide sole whose particle size can be controlled and particle size distribution is narrow.

Description

technical field [0001] The invention relates to the technical field of sol-gel method, in particular to a preparation method of zirconia sol, which can be used as a precursor of high-purity nano-zirconia powder and composite zirconia functional ceramics. Background technique [0002] Zirconia is widely used in many fields due to its unique properties. ZrO 2 It is the only metal oxide that is acidic, basic, oxidizing, and reducing at the same time. As a carrier or catalyst, it shows unique catalytic activity and selectivity in the field of catalytic technology. Zirconia has excellent properties such as high temperature resistance, corrosion resistance, high mechanical strength, and low friction coefficient, and has become one of the key research ceramics in the field of functional materials. Structural ceramic components prepared from it, such as cutting tools, molds, bearings, high-temperature refractory materials, etc., have excellent mechanical and physical properties. ...

Claims

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Application Information

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IPC IPC(8): C01G25/02C04B35/48C04B35/624
Inventor 段雷许高杰杨晔李勇崔平
Owner 上海西源新能源技术有限公司
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