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Method for preparing potassium fluozirconate through fluosilicic acid

A technology of potassium fluorozirconate and fluorosilicic acid, which is applied in chemical instruments and methods, zirconium compounds, inorganic chemistry, etc., can solve the problems of potassium fluorozirconate production cost, lack of market competitiveness, etc., and alleviate environmental protection. Pressure and its impact on the surrounding environment, providing production benefits, less useful effects

Inactive Publication Date: 2013-01-16
HUNAN NONFERROUS FLUORIDE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the traditional production process of potassium fluozirconate mostly uses potassium hydrofluoric acid chloride method, which makes the production cost of potassium fluozirconate greatly affected by raw materials and lacks market competitiveness

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] This embodiment uses fluosilicic acid, zirconium oxychloride and potassium chloride as the main raw materials, specifically comprising the following steps:

[0025] (1) First add 1000mL of fluosilicic acid solution into the leaching tank, then heat it to 70°C, start stirring, add 180g of zirconium oxychloride into the fluosilicic acid solution, react and leaching for 5 hours under heat preservation conditions, the reaction equation for:

[0026] h 2 SiF 6 +ZrOCl 2 ·8H 2 O→H 2 ZrF 6 +SiO2 2 +2HCl+7H 2 O;

[0027] (2) Filter the fluozirconic acid solution obtained by leaching, wash the filter residue with sand filter water for 3 times, and then dry it to obtain a white carbon black product;

[0028] (3) Use the acid-base titration method to detect the amount of unreacted fluorosilicic acid in the filtrate of step (2) and the first washing water mixture, then add 30g of sodium chloride to remove the unreacted fluorosilicic acid, React for 10 minutes, the reactio...

Embodiment 2

[0036] This embodiment uses fluosilicic acid, zirconium oxychloride and potassium chloride as the main raw materials, specifically comprising the following steps:

[0037] (1) First add 1000ml of fluosilicic acid solution into the leaching tank, then heat to 80°C, start stirring, add 560g of zirconium oxychloride into the fluosilicic acid solution, react and leaching for 4 hours under heat preservation conditions, the reaction equation for:

[0038] h 2 SiF 6 +ZrOCl 2 ·8H 2 O→H 2 ZrF 6 +SiO2 2 +2HCl+7H 2 O;

[0039] (2) Filtrate the fluozirconic acid solution obtained by leaching, wash the filter residue with sand filter water for 3 times, and then dry it to obtain a white carbon black product;

[0040] (3) Use the acid-base titration method to detect the amount of unreacted fluorosilicic acid in the filtrate of step (2) and the first washing water mixture, then add 80g of sodium chloride to remove the unreacted fluorosilicic acid, React for 20 minutes, the reaction...

Embodiment 3

[0048] This embodiment uses fluosilicic acid, zirconium oxychloride and potassium chloride as the main raw materials, specifically comprising the following steps:

[0049] (1) First add 1000ml of fluosilicic acid solution into the leaching tank, then heat to 90°C, start stirring, add 1300g of zirconium oxychloride into the fluosilicic acid solution, and react and leach for 3 hours under heat preservation conditions, the reaction equation for:

[0050] h 2 SiF 6 +ZrOCl 2 ·8H 2 O→H 2 ZrF 6 +SiO22 +2HCl+7H 2 O;

[0051] (2) Filtrate the fluozirconic acid solution obtained by leaching, wash the filter residue with sand filter water for 3 times, and then dry it to obtain a white carbon black product;

[0052] (3) Use the acid-base titration method to detect the amount of unreacted fluorosilicic acid in the filtrate of step (2) and the first washing water mixture, then add 150g of sodium chloride to remove the unreacted fluorosilicic acid, React for 30 minutes, the reactio...

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Abstract

The invention provides a method for preparing potassium fluozirconate through fluosilicic acid. The method comprises the steps as follows: (1) adding a fluosilicic acid solution to a leaching groove, then heating to reach 40 to 100 DEG C, starting to agitate, and adding the zirconium oxychloride with the theoretical amount to the fluosilicic acid solution; reacting and leaching for 1 to 5 hours under constant temperature condition; (2) filtering the fluosilicic acid obtained by leaching; washing the filter residue, then parching the filter residue to obtain a white carbon black product; (3) adding sodium chloride with theoretical amount to the mixture of the filtrate and the first washing water to obtain the sodium fluosilicate size; (4) filtering the obtained size, washing, and drying to obtain sodium fluosilicate; (5) adding the filtrate in step (4) into the potassium chloride solution with the theoretical amount to react for 30 to 60 minutes, and filtering to obtain paste; and (6) washing the obtained paste through water, and then parching to obtain the finished product. According to the method provided by the invention, the raw materials are easy to obtain, and low in cost, thus the producing cost can be greatly reduced; and meanwhile, the valuable white carbon black and sodium fluosilicate can be produced.

Description

technical field [0001] The invention relates to a method for preparing potassium fluozirconate with fluosilicic acid, in particular to a method for preparing potassium fluozirconate with fluosilicic acid, zirconium oxychloride and potassium chloride as main raw materials. Background technique [0002] Potassium fluozirconate is widely used, mainly used in the production of metal zirconium and other zirconium compounds, and also in the production of aluminum-magnesium alloys, atomic energy industry, ceramics and glass. The scale of related industries using potassium fluozirconate is stable, and with the development of the atomic energy industry, the demand for potassium fluozirconate will increase. Therefore, the market for potassium fluozirconate is very broad. [0003] At present, the traditional production process of potassium fluozirconate mostly uses potassium hydrofluoric acid chloride method, which makes the production cost of potassium fluozirconate greatly affected b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00
Inventor 舒友黄忠孝刘峙军李飞跃刘龙平李志光李文英
Owner HUNAN NONFERROUS FLUORIDE CHEM
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