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Process for hydrothermally preparing zirconium oxychloride with low alkali consumption

A technology of zirconium oxychloride and process method, applied in chemical instruments and methods, inorganic chemistry, zirconium compounds, etc., can solve the problems of high purity, large NaOH consumption, environmental pollution, etc., to promote reaction efficiency, promote reaction speed, The effect of reducing consumption

Active Publication Date: 2013-04-03
安徽通湾科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to solve the problems of large NaOH consumption, high energy consumption, excessive alkali cannot be recycled, and serious pollution to the environment in the process of producing zirconium oxychloride by zircon sand alkali fusion method, and to provide a low-consumption alkaline water A process for thermally preparing zirconium oxychloride, the zirconium oxychloride product obtained by this method has low impurity content and high purity

Method used

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  • Process for hydrothermally preparing zirconium oxychloride with low alkali consumption

Examples

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Effect test

Embodiment 1

[0042] Sodium hydroxide is formulated into an aqueous solution of 50% by weight, and 3000g of ZrSiO 4 Add 1146g of D50: 1μm ultrafine zircon sand with a molar ratio of 1:6 to NaOH, stir and make slurry, and put it into a 5L high-pressure reactor. The reaction temperature is 300°C, the reaction pressure is adjusted to 7MPa, and the reaction time is 3h. Solid-liquid separation removes excess alkali, then the product of solid-liquid separation is fully dissolved with hydrochloric acid aqueous solution of concentration 20%Wt, and reaction molar ratio is excessive 15%, obtains reactant H 2 SiO 3 , ZrOCl 2 and NaCl aqueous solution, solid-liquid separation to remove impurities such as silicic acid, and the remaining liquid is steamed under negative pressure at 120°C to hydrolyze ZrO(OH) 2 Precipitate, control pH5-6, separate solid-liquid and wash the precipitate, remove sodium ions, and get ZrO(OH) 2 The filter cake is fully dissolved with hydrochloric acid aqueous solution with ...

Embodiment 2

[0044] Sodium hydroxide is formulated into an aqueous solution of 40% by weight, and 3000g is taken according to ZrSiO 4 Add 917g of D50: 1μm ultrafine zircon sand at a molar ratio of 1:6 to NaOH, stir and make slurry, and put it into a 5L high-pressure reactor. The reaction temperature is 250°C, and the reaction pressure is adjusted to 5MPa. Solid-liquid separation removes excess alkali, then the product of solid-liquid separation is fully dissolved with a hydrochloric acid aqueous solution with a concentration of 15%Wt, and the reaction molar ratio is excessive by 10%, to obtain reactant H 2 SiO 3 , ZrOCl 2 and NaCl aqueous solution, solid-liquid separation to remove impurities such as silicic acid, and the remaining liquid is steamed under negative pressure at 100°C to hydrolyze ZrO(OH) 2 Precipitate, control pH5-6, separate solid-liquid and wash the precipitate, remove sodium ions, and get ZrO(OH) 2 The filter cake is fully dissolved with hydrochloric acid aqueous solut...

Embodiment 3

[0046] Sodium hydroxide is formulated into an aqueous solution of 30% by weight, and 3000g of ZrSiO 4 Add 1375g of D50: 5μm superfine zircon sand with a molar ratio of 1:3 to NaOH, stir and make slurry, and put it into a 5L autoclave, the reaction temperature is 200°C, the reaction pressure is adjusted to 3MPa, and the reaction time is 12h. Liquid separation removes excessive alkali, then the product of solid-liquid separation is fully dissolved with the hydrochloric acid aqueous solution of concentration 20%Wt, and reaction molar ratio is excessive 20%, obtains reactant H 2 SiO 3 , ZrOCl 2 and NaCl aqueous solution, solid-liquid separation to remove impurities such as silicic acid, and the remaining liquid is steamed with negative pressure at 110°C to hydrolyze ZrO(OH) 2 Precipitate, control pH5-6, separate solid-liquid and wash the precipitate, remove sodium ions, and get ZrO(OH) 2 The filter cake is fully dissolved with hydrochloric acid aqueous solution with a concentra...

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Abstract

The invention relates to a process for hydrothermally preparing zirconium oxychloride with low alkali consumption, and belongs to the technical field of compound preparation. The process comprises the following steps: stirring crushed superfine zircon sand (ZrSiO4) powder with a NaOH solution to prepare slurry, and then placing the slurry into an autoclave to perform hydrothermal reaction, and thus generating amorphous or crystalline acmite sodium zirconium silicate (Na2ZrSiO5) precursors under a condition with the temperature of 200-300 DEG C, the pressure of 3-7MPa and the reaction time of 3-12 hours; and then removing sodium by use of hydrochloric acid, removing silicon, purifying, concentrating and crystallizing to obtain zirconium oxychloride crystals. The process can be used for not only solving the problems such as high NaOH consumption, high energy consumption, recycling incapability of excessive alkali and serious pollution to the environment in the process of preparing the zirconium oxychloride from zircon sand by an alkali fusion method, but also realizing low impurity content and high purity of a zirconium oxychloride product obtained by the method.

Description

technical field [0001] The invention relates to a process for preparing zirconium oxychloride by hydrothermal method with low alkali consumption, and belongs to the technical field of compound preparation. Background technique [0002] Zirconium oxychloride is widely used, it can be used as raw material of mordant dye and additive of mordant, color fixer, deodorant, flame retardant, etc. It is also an important raw material for industrial-grade and high-purity zirconia and nano-ultrafine zirconia. Nano zirconia has excellent physical and chemical properties such as high melting point, high strength, wear resistance, and corrosion resistance, and is mainly used in the manufacture of structural ceramics and functional materials; zirconium carbonate, zirconium sulfate, and zirconium nitrate can be prepared using zirconium oxychloride as raw material , Zirconium hydroxide and other zirconium chemicals are widely used in ceramics, chemical industry, light industry, electronics a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00
Inventor 周涛赵蜀春
Owner 安徽通湾科技有限公司
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