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Method for preparing high-purity zirconium sulfate tetrahydrate by purifying desilicated zirconia

A zirconium sulfate tetrahydrate and zirconium desiliconization technology, which is applied in the direction of zirconium sulfate and air quality improvement, can solve the problems of cumbersome procedures, environmental pollution, low efficiency, etc., and achieve the goals of avoiding air pollution, low impurity content, and improving production efficiency Effect

Inactive Publication Date: 2018-05-08
SHANDONG LEIBAO ZIRCONIUM SCI&TECH
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  • Description
  • Claims
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Problems solved by technology

[0003] The traditional process requires two crystallization treatments. The production of the traditional process is to evaporate and concentrate crystallization under the hydrochloric acid system. After crystallization, water-soluble secondary crystallization is required to obtain qualified zirconium sulfate tetrahydrate. Not only the process is cumbersome, but also the environment is polluted and the efficiency is low.

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  • Method for preparing high-purity zirconium sulfate tetrahydrate by purifying desilicated zirconia

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Ingredients: mix desiliconized zirconium, sodium carbonate and sulfuric acid in a mass ratio of 1:0.1:3;

[0034] (2) Acidification reaction: the above mixture is roasted at 700° C. to make it react to generate sulfate, and the conversion rate is 95%;

[0035] (3) Catalysis: Add sodium carbonate and use its characteristic carbonate to accelerate the boiling reaction;

[0036] (4) Leaching: adding sulfate into water for leaching, the solid-to-liquid ratio is 1:6, the temperature is controlled at 65°C, the acidity is controlled at 7mol / L, and the leaching time is controlled at 2h;

[0037] (5) Press filtration: after the leaching is finished, carry out solid-liquid separation with a plate and frame machine, and press filter to remove the clear liquid;

[0038] (6) Evaporation and concentration: the clear liquid is evaporated and concentrated, and the Baume degree of the concentrated feed liquid is controlled at 30 ° Bé to obtain a concentrated solution;

[0039] (7)...

Embodiment 2

[0045] (1) Ingredients: mix desiliconized zirconium, sodium carbonate and sulfuric acid in a mass ratio of 1:0.2:2.5;

[0046] (2) Acidification reaction: the above mixture is roasted at 800°C to react to generate sulfate, and the conversion rate is 96.5%;

[0047] (3) Catalysis: Add sodium carbonate and use its characteristic carbonate to accelerate the boiling reaction;

[0048] (4) Leaching: add sulfate into water for leaching, the solid-to-liquid ratio is 1:4, the temperature is controlled at 55°C, the acidity is controlled at 5mol / L, and the leaching time is controlled at 3h;

[0049] (5) Press filtration: after the leaching is finished, carry out solid-liquid separation with a plate and frame machine, and press filter to remove the clear liquid;

[0050] (6) Evaporation and concentration: the clear liquid is evaporated and concentrated, and the Baume degree of the concentrated feed liquid is controlled at 37 ° Bé to obtain a concentrated solution;

[0051] (7) Crystall...

Embodiment 3

[0057] (1) Ingredients: mix desiliconized zirconium, sodium carbonate and sulfuric acid according to 1:0.3:3 in parts by mass;

[0058] (2) Acidification reaction: the above mixture is roasted at 830° C. to make it react to generate sulfate, and the conversion rate is 92.8%;

[0059] (3) Catalysis: Add sodium carbonate and use its characteristic carbonate to accelerate the boiling reaction;

[0060] (4) Leaching: add sulfate into water for leaching, the solid-to-liquid ratio is 1:2, the temperature is controlled at 70°C, the acidity is controlled at 8mol / L, and the leaching time is controlled at 2h;

[0061](5) Press filtration: after the leaching is finished, carry out solid-liquid separation with a plate and frame machine, and press filter to remove the clear liquid;

[0062] (6) Evaporation and concentration: the clear liquid is evaporated and concentrated, and the Baume degree of the concentrated feed liquid is controlled at 34 ° Bé to obtain a concentrated solution;

[...

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Abstract

The invention relates to a method for preparing high-purity zirconium sulfate tetrahydrate by purifying desilicated zirconia, and belongs to the technical field of refractory material preparation. Themethod for preparing high-purity zirconium sulfate tetrahydrate by purifying desilicated zirconia includes the steps that desilicated zirconia is subjected to an acidification reaction to convert thezirconia component in desilicated zirconia into sulfate, and sulfate is subjected to filtration, purification and crystallization to obtain high-purity zirconium sulfate tetrahydrate, wherein the acidification reaction is a roasting reaction of desilicated zirconia and sulfuric acid under the catalysis of sodium carbonate. The preparing method is scientific, reasonable, simple, and easy to implement, saves energy, avoids air pollution and improves production efficiency; after desilicated zirconia is purified, the obtained product is white, the mass content of ZrO2 in zirconium sulfate tetrahydrate is higher than 33%, and the purity is high.

Description

technical field [0001] The invention relates to a method for purifying and preparing high-purity zirconium sulfate tetrahydrate from desiliconized zirconium, belonging to the technical field of refractory material preparation. Background technique [0002] Desiliconized zirconium is a solid solution of zirconium made by high-temperature melting and desiliconization. At present, there is no way to dissolve and test it at low temperature. Now it can only be used as a low-grade refractory material through simple processing. In order to improve its use value, we invented a A new technological method solves this difficult problem, makes it purified, and realizes its true value. The purified zirconium sulfate tetrahydrate is mainly used as a catalyst for tanning high-grade leather and preparing intermediate products of other zirconium compounds. It can also be used as a cod liver oil decolorizer, precipitated and separated amino acids (such as glutamic acid), etc., and is used as ...

Claims

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Application Information

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IPC IPC(8): C01G25/06
CPCC01G25/06C01P2006/80Y02A50/20
Inventor 王光强刘学燕周有福王育峰韩雍雍
Owner SHANDONG LEIBAO ZIRCONIUM SCI&TECH
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