Method for preparing high purity hydrous zirconium oxide and zircon salt with zirconium oxychloride mother solution

A hydrated zirconia and zirconium oxychloride technology, applied in zirconia, chemical instruments and methods, zirconium compounds, etc., can solve the problems of underutilization of hydrochloric acid, waste of resources, inability to remove and so on

Inactive Publication Date: 2008-10-29
LOMON BILLIONS GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of these two methods is that a large amount of impurities such as sodium, titanium, silicon, and iron in the mother liquor are brought into the system, and it is almost impossible to remove them. They can...

Method used

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  • Method for preparing high purity hydrous zirconium oxide and zircon salt with zirconium oxychloride mother solution
  • Method for preparing high purity hydrous zirconium oxide and zircon salt with zirconium oxychloride mother solution
  • Method for preparing high purity hydrous zirconium oxide and zircon salt with zirconium oxychloride mother solution

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Contains ZrO 2 37.58g / l, HC1 179.58g / l and TiO 2 15.04g / l, Fe 2 o 3 20.20g / l, Na 2 2000ml of mother liquor of O18.62g / l impurity is placed in a distillation bottle, heated and concentrated to about 1 / 3 of the original volume. Make up water to 2000ml, continuously add 30% sodium sulfite aqueous solution in this solution, heat slowly simultaneously, constantly detect solution with pH test paper, when being 1.2 to pH, stop adding sodium sulfite, continue heating to boiling. In this way, the zirconium ions in the solution are precipitated in the form of hydrous zirconia. Filter the hydrated zirconia precipitate, wash it with water, and use 5% potassium ferricyanide solution to test the washing solution until no blue color appears, indicating that the ferrous ions contained in the precipitate meet the requirements. Dissolve the hydrated zirconia precipitate with 500 milliliters of 25% hydrochloric acid to obtain an aqueous solution of zirconium oxychloride, concentrate...

Embodiment 2

[0033] Contains ZrO 2 37.58g / l, HCl 179.58g / l and lots of TiO 2 15.04g / l, Fe 2 o 3 20.20g / l, Na 2 O 18.62g / l and other impurities mother liquor 2000ml, placed in a distillation bottle, heated and concentrated to about 1 / 3 of the original volume. Make up water to 2000ml, continuously add 30% ammonium sulfite aqueous solution in this solution, heat slowly simultaneously, constantly detect solution with pH test paper, when pH is 0.9, stop adding ammonium sulfite, continue heating to boiling. In this way, the zirconium ions in the solution are precipitated in the form of hydrous zirconia. Filter the hydrated zirconia precipitate, wash it with water, and use 5% potassium ferricyanide solution to test the washing solution until no blue color appears, indicating that the ferrous ions contained in the precipitate meet the requirements. Dissolve the hydrated zirconia precipitate with 500 milliliters of 25% hydrochloric acid to obtain an aqueous solution of zirconium oxychloride, c...

Embodiment 3

[0035] Contains ZrO 2 37.58g / l, HCl 179.58g / l and lots of TiO 2 15.04g / l, Fe 2 o 3 20.20g / l, Na 2 2000ml of the mother liquor of impurities such as O18.62g / l is placed in a distillation bottle, heated and concentrated to about 1 / 3 of the original volume. Make up water to 2000ml, continuously add 30% potassium sulfite aqueous solution in this solution, slowly heat simultaneously, constantly detect solution with pH test paper, when being 1.2 to pH, stop adding potassium sulfite, continue heating to boiling. In this way, the zirconium ions in the solution are precipitated in the form of hydrous zirconia. Filter the hydrated zirconia precipitate, wash it with water, and use 5% potassium ferricyanide solution to test the washing solution until no blue color appears, indicating that the ferrous ions contained in the precipitate meet the requirements. Dissolve the hydrated zirconia precipitate with 500 milliliters of 25% hydrochloric acid to obtain an aqueous solution of zirconi...

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Abstract

The invention discloses a method of a mother liquid for preparing hydrous zirconium oxide with high purity and a zirconium salt in the production process of zirconium oxychloride. The invention comprises the processes of concentration, hydrolysis, acid corrosion, secondary concentration, crystallization and acid pickling. The invention employs the mother liquid that produces the zirconium oxychloride as the raw material to produce the hydrous zirconium oxide with the high purity, prepare the high value zirconium salt and recycle hydrochloride in the solution. In the process of removing impurities from the solution, a lot of impurities are removed, which leads the product to have the high purity, stable performance and good quality; the hydrochloride can be used repeatedly, which reduces the production cost; the production process of the invention is simple and convenient and is suitable for large scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing high-purity hydrated zirconia from mother liquor in the production process of zirconium oxychloride and a method for preparing zirconium salt. Background technique [0002] A large amount of acidic zirconium-containing mother liquor is produced in the production process of zirconium oxychloride. If it is returned to the production system, impurities such as sodium, titanium, silicon, and iron in the mother liquor cannot be removed. As the production cycle progresses, it can only be enriched more and more, giving Normal production brings many unfavorable factors. If the mother liquor is discharged, it will cause environmental pollution, waste of resources, and increase of production costs. Therefore, how to rationally recycle this part of mother liquor has become the focus of many enterprises and scientific research departments. [00...

Claims

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Application Information

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IPC IPC(8): C01G25/02C01G25/00
Inventor 杨民乐杨朋芝申朝春郭焦星
Owner LOMON BILLIONS GRP CO LTD
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