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Modified zirconium oxide particle powder, modified zirconium oxide particle dispersed sol and making method thereof

A manufacturing method and technology of zirconia, applied in the direction of zirconia, etc., can solve the problems of reduced surface potential, reduced dispersibility, particle agglomeration, etc., and achieve the effects of excellent dispersion stability, reduced transportation costs, and excellent fluidity

Active Publication Date: 2014-07-16
JGC CATALYSTS & CHEM LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although titanium dioxide particles have a high refractive index, their dispersion stability is poor, and titanium dioxide itself has photocatalytic activity, so there are problems in light resistance and weather resistance.
[0008] At present, in order to improve the dispersibility and stability of various metal oxide sols, the surface is treated with an organosilicon compound (organosilane coupling agent). The active region can be dispersed stably, but there is a problem that when washing and purifying to remove the alkali component, the surface potential decreases and the dispersibility decreases significantly.
[0009] In particular, in the presence of a base that is a catalyst for hydrolysis of an organosilicon compound, the treatment of the organosilicon compound on the surface of the surface-treated zirconia fine particles becomes non-uniform, possibly due to the presence of alkali ions, and the resulting surface-treated The dispersibility and stability of the zirconia particles are not satisfied
[0010] On the other hand, when no alkali coexists, that is, when a hydrolysis catalyst is not used, the hydrolysis rate of trifunctional or less organosilicon compounds is slow, unreacted organosilicon compounds remain, and surface treatment may be insufficient.
[0011] In addition, when an acid is used as a hydrolysis catalyst, there is a tendency to form a chain-shaped hydrolysis product on the surface of the particles, and the resulting particles may aggregate or cause poor dispersibility.

Method used

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  • Modified zirconium oxide particle powder, modified zirconium oxide particle dispersed sol and making method thereof
  • Modified zirconium oxide particle powder, modified zirconium oxide particle dispersed sol and making method thereof
  • Modified zirconium oxide particle powder, modified zirconium oxide particle dispersed sol and making method thereof

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preparation example Construction

[0108] Preparation method of zirconia particles

[0109] In the present invention, after (a) degumming or dissolving the zirconium hydroxide gel in the presence of potassium hydroxide and hydrogen peroxide, (b) performing hydrothermal treatment, and (c) washing, such oxidized Zirconium particles.

[0110]First, the zirconium hydroxide gel is debonded or dissolved in the presence of potassium hydroxide and hydrogen peroxide. The zirconium hydroxide gel is not particularly limited as long as it can be debonded or dissolved in the presence of potassium hydroxide and hydrogen peroxide. For example, a zirconium hydroxide gel obtained by hydrolyzing or neutralizing a zirconium compound (including zirconium oxide hydrate, zirconium hydroxide, etc.).

[0111] The zirconium compound can be exemplified by zirconium chloride (ZrCl 2 ), zirconium oxychloride (ZrOCl 2 ), zirconium nitrate, zirconium oxynitrate, zirconium sulfate, zirconium carbonate, zirconium acetate, etc., and zirc...

Embodiment 1

[0181] Preparation of modified zirconia particles (1) powder

[0182] 317.9 kg of zirconium hydroxide gel having a solid concentration of 9.5% by weight was suspended in 535.3 kg of water to prepare a zirconium hydroxide gel dispersion having a solid concentration of 3.5% by weight.

[0183] Next, 354.9 kg of a KOH aqueous solution with a concentration of 17 wt %, 302.0 kg of an aqueous hydrogen peroxide solution with a concentration of 35 wt %, and 88.5 kg of an aqueous solution of tartaric acid with a concentration of 10 wt % were added to the zirconium hydroxide gel dispersion with a solid content concentration of 3.5 wt %. kg, and stirred at 30° C. for 2 hours to debond the zirconium hydroxide gel. process (a)

[0184] At this time, (M OH ) / (M Zr ) is 20, (M PO ) / (M Zr ) is 10. Next, 88.5 kg of an aqueous solution of tartaric acid having a concentration of 10% by weight was added to the solution obtained by debonding the zirconium hydroxide gel, and hydrothermal ...

Embodiment 2

[0231] Preparation of modified zirconia particles (2) powder

[0232] In Example 1, a modified zirconia fine particle (2) powder was produced in the same manner except that the powder was dried at 40°C for 24 hours. Process (f)

[0233] The obtained modified zirconia fine particle (2) powder was measured for moisture content, crystallinity, average particle diameter, angle of repose, and refractive index. Table 1 shows the results. also, 29 The chemical shift values ​​and half widths of the main peaks of the SiMAS NMR spectrum are shown in the table.

[0234] Preparation of Modified Zirconia Particles (2) Organic Solvent Dispersion

[0235] In Example 1, a methanol dispersion of the modified zirconia fine particles (2) and the modified zirconia fine particles (2) having a solid content concentration of 30% by weight were obtained in the same manner except that the powder of the modified zirconia fine particles (2) was used. MIBK dispersion.

[0236] The average partic...

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Abstract

The invention provides modified zirconium oxide particle powder with excellent dispersibility and fluidity, a modified zirconium oxide particle dispersed sol and a making method thereof. Being the powder of modified zirconium oxide particles subjected to organosilicon compound surface treatment, the powder is characterized in that, an average secondary particle size (DM2) is in the range of 5-500nm, an average primary particle size (DM1) is in the range of 5-500nm, and the ratio (DM2) / (DM1) of the average secondary particle size (DM2) to the average primary particle size (DM1) is in the range of 1-10. The organosilicon compound is shown as the formula (1). The content of the organosilicon compound in the particle is, in terms of Rn-SiO(4-n) / 2( with n being an integer of 1-3), 1-50wt%, and the half width of the main peak of the <29>Si MAS NMR spectrum is in the range of 3-15ppm. Rn-SiX4-n (1) (In the formula, R is bstituted or substituted alkyl of C1-10, and can be the same to each other or different, X can be alkoxy, hydroxy, halogen and hydrogen of C1-4, and n is an integer of 1-3).

Description

technical field [0001] The present invention relates to a modified zirconia fine particle powder excellent in dispersibility and fluidity, a dispersion using the modified zirconia fine particle powder, and a method for producing the same. Background technique [0002] At present, silica, alumina, titania, zirconia, zinc oxide, antimony pentoxide, cerium oxide, tin oxide, silica·alumina, silica·zirconia and other colloidal particles are known as optical materials. It is used in a coating etc. to adjust the refractive index. For example, silica is used as a low refractive index material, alumina is used as a medium refractive index material, and titania, zirconia, etc. are used as a high refractive index material. [0003] Although titanium dioxide particles have a high refractive index, their dispersion stability is poor, and titanium dioxide itself has photocatalytic activity, so there are problems in light resistance, weather resistance, and the like. Therefore, by compou...

Claims

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Application Information

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IPC IPC(8): C01G25/02
Inventor 山口纯松田政幸村口良
Owner JGC CATALYSTS & CHEM LTD
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