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Process for production of alkaline zirconia sol

A manufacturing method and technology of zirconia, applied in zirconia, sol preparation, chemical instruments and methods, etc., can solve the problems of gelation, unstable reaction system, etc.

Inactive Publication Date: 2010-12-29
NISSAN CHEM IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] As mentioned above, various production methods of zirconia sol have been proposed so far, but many methods are production methods of hydrolyzing zirconium salt in an acidic region and heating, so the reaction system becomes unstable due to the generated fine particles. Unstable and prone to gelation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] 1306.1 g of tetramethylammonium bicarbonate aqueous solution (manufactured by Tama Chemical Industry Co., Ltd., containing 44.5% by mass in terms of tetramethylammonium hydroxide) and 592.2 g of pure water were added to a 3-liter glass container to form a diluted aqueous solution. While stirring the aqueous solution, zirconyl carbonate powder (ZrOCO 3 , produced by Daiichi Raw Element Chemical Industry Co., Ltd., according to ZrO 2 The total content is 42.1% by mass. ), added 801.7g by total amount. After completion of the addition, the mixed liquid was aged at 105° C. for 6 hours while heating to 105° C. while stirring, and adding pure water as appropriate to adjust the concentration. At the end of the slaking, the mixture is slurry, according to ZrO 2 The total content is 12.5% ​​by mass, and the pH is 10.7. This slurry was transferred to a stainless steel autoclave container, and a hydrothermal synthesis reaction was performed at 140° C. for 3 hours with stirring...

Embodiment 2

[0074] 1171.0 g of the raw material basic zirconia sol (A) prepared in the same manner as in Example 1 and 79.0 g of pure water were placed in a 3 L glass container. While stirring the solution, slowly add ZrO 2 20.0% by mass of zirconium basic ammonium carbonate solution (manufactured by Nippon Light Metal) was added in total, and 500.0 g was added in total, and stirred for 30 minutes after the addition to form a raw material mixture. The mixed solution contains 32.4% by mass of ZrO 2 , and the conversion of basic zirconia sol to ZrO 2 After the conversion of the solid content and basic ammonium zirconium carbonate into ZrO 2 The mass ratio of the final solid content (solid content ratio) was 5:1, and pH was 9.6 (step I). The raw material mixture was heated to 75°C with stirring, and then heated at 75°C for 1 hour. The liquid obtained after this heating also had no gel, and was completely sol-formed. Next, slowly add ZrO 2 20.0% by mass of zirconium basic ammonium carbo...

Embodiment 3

[0076] 585.5 g of the basic zirconia sol (A) and 664.5 g of pure water prepared in the same manner as in Example 1 were placed in a 3 L glass container. While stirring the solution, slowly add ZrO 2 625.0 g of basic ammonium zirconium carbonate solution (manufactured by Nippon Light Metal) containing 20.0% by mass was added in total, and stirred for 30 minutes after the addition to form a raw material mixed liquid. The mixed solution contains 20.0% by mass of ZrO 2 , and the conversion of basic zirconia sol to ZrO 2 After the conversion of the solid content and basic ammonium zirconium carbonate into ZrO 2 The mass ratio of the final solid content (solid content ratio) was 2:1, and the pH was 9.6 (step I). The raw material mixture was heated to 75°C with stirring, and then heated at 75°C for 1 hour. The liquid obtained after this heating also had no gel, and was completely sol-formed. Next, slowly add ZrO 2 It contained 20.0% by mass of zirconium basic ammonium carbonate...

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Abstract

A process for producing an alkaline zirconia sol comprising a step (I) in which an alkaline zirconia sol (A) is mixed with a basic zirconium carbonate (B1), the alkaline zirconia sol (A) being produced by a process comprising a step (i) in which a zirconium salt (B2) is heated in an aqueous medium containing a quaternary ammonium carbonate at a temperature of 60 to 110 DEG C and a step (ii) in which the resulting product is treated hydrothermally at a temperature of 110 to 250 DEG C; more specifically, a process for producing an alkaline zirconia sol comprising a step (I) in which an alkalinezirconia sol (ZrO2) (A) is mixed with a basic zirconium carbonate (B1) at such a ratio that the solid content of the alkaline zirconium in terms of ZrO2 (As) and the solid content of the basic zirconium carbonate in terms of ZrO2 (Bs) have the following relationship: Bs / As=0.05 to 4.0 by weight and a step (II) in which a mixed solution given in the step (I) is aged at a temperature of 20 to 100 DEG C. The process can produce an alkaline zirconia sol which is stable and has a wide range of particle size distribution.

Description

technical field [0001] The present invention relates to a production method of zirconia sol, and provides a production method of basic and stable zirconia sol. Background technique [0002] In the past, as a method of obtaining zirconia sol, a method of heating and hydrolyzing an aqueous solution of a zirconium salt, a method of adding an aqueous solution of hydrogen peroxide to an aqueous solution of a zirconium salt and heating, and a method of heating zirconium hydroxide in an alkaline region are known. methods, etc., for example, the following methods are proposed. [0003] It has been proposed to hydrolyze the reaction products of ammonium zirconium carbonate and chelating agents (for example, hydroxyphenols, aminoalcohols, hydroxyacids, polycarboxylic acids, aldols, amino acids, β-diketones) method (see Patent Document 1). [0004] In addition, it is also proposed to keep the aqueous suspension containing zirconium hydroxide at a temperature of 80° C. or higher under...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02C01G25/00B01J13/00
CPCB01J13/0008C01G25/00C01G25/02B01J13/003B01J13/00
Inventor 大森丰加藤博和山口健二
Owner NISSAN CHEM IND LTD
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