Method for refining stannous fluoride

A technology of stannous fluoride and a refining method, applied in the direction of tin halide and the like, can solve the problems of low purity of stannous fluoride, many impurities, low purity of stannous fluoride, etc., and achieves good heat exchange and simple post-processing. , the response is easy to control the effect

Inactive Publication Date: 2020-02-21
GUANGDONG GUANGHUA SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the stannous fluoride obtained by the disclosed preparation method of stannous fluoride generally has the problems of low purity and many impurities. Existing research generally focuses on the di

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Add 700g barium hydroxide to 700g mass concentration of 40% hydrofluoric acid aqueous solution, react 30min, obtain barium fluoride slurry;

[0037] (2) Add 480g of stannous sulfate to the above-mentioned barium fluoride slurry, react for 60min, filter, remove the barium sulfate solid, collect the filtrate and dry to obtain the crude product of stannous fluoride, which is detected by ICP inductively coupled plasma emission spectrometry , the purity of the crude stannous fluoride is 76.8%.

[0038] (3) Add 350 g of the above-mentioned stannous fluoride crude product into a crystallization tank, add 700 g of methanol and 3.5 g of ascorbic acid, cool in an ice-water bath at 15° C. for 2 hours, obtain needle-shaped crystals, filter, and separate solid and liquid to obtain stannous fluoride tin solid;

[0039] (4) Transfer the solid obtained in step (3) into a drying device, and dry under the conditions of 80° C. and a pressure of 20 kPa to obtain stannous fluoride powd...

Embodiment 2

[0042] (1) Take the stannous fluoride crude product obtained in Example 1, add 350 g of the above-mentioned stannous fluoride crude product into a crystallization tank, add 2500 g of ethanol and 6 g of hydrazine hydrate, cool in an ice-water bath at 5 ° C for 3 h, and obtain needle-shaped crystals, filtered, and solid-liquid separation to obtain stannous fluoride solid;

[0043] (2) Transfer the solid obtained in step (1) into a drying device, and dry it under the conditions of a temperature of 40° C. and a pressure of 5 kPa to obtain stannous fluoride powder.

[0044] Detected by ICP inductively coupled plasma emission spectrometry, the purity of the refined stannous fluoride is 99.75%, and the content of impurities such as iron, lead and antimony is ≤0.005%. After calculation, the yield of refined stannous fluoride is 97.2%.

Embodiment 3

[0046] (1) Take the stannous fluoride crude product obtained in Example 1, add 320 g of the above-mentioned stannous fluoride crude product into a crystallization tank, add 2500 g of chloroform and 5 g of catechol, cool in an ice-water bath at 0 ° C for 3 h, and obtain needles crystal, filtered, and solid-liquid separation to obtain stannous fluoride solid;

[0047] (2) Transfer the solid obtained in the step (1) into a drying device, and dry under the conditions of a temperature of 60° C. and a pressure of 25 kPa to obtain stannous fluoride powder.

[0048] Detected by ICP inductively coupled plasma emission spectrometry, the purity of the refined stannous fluoride is 99.70%, and the content of impurities such as iron, lead and antimony is ≤0.005%. After calculation, the yield of refined stannous fluoride is 98.6%.

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Abstract

The invention relates to a refining method of stannous fluoride. The refining method comprises the following steps: mixing a stannous fluoride crude product, an antioxidant and an organic solvent to obtain a mixture; crystallizing the mixture, then filtering, collecting a solid, and drying to obtain a stannous fluoride refined product; wherein the mass of the antioxidant accounts for 1%-5% of themass of the stannous fluoride crude product. The method is simple in process, low in implementation cost, stable in product, high in purity, controllable in quality and easy to industrialize.

Description

technical field [0001] The invention relates to the field of synthesis of fine chemicals, in particular to a refining method of stannous fluoride. Background technique [0002] Stannous fluoride is an important water-soluble fluoride salt. Since the 1950s, it has been widely used as a product for the prevention and treatment of oral diseases, such as in toothpaste, mouthwash and pharmaceutical additives. When used in mouthwash, due to its dual anti-caries effects of tin ions and negative ions, it can be used as an excellent tooth decay agent, effectively preventing periodontitis and dental plaque, etc. It has a good curative effect on bacterial and fungal infections. [0003] At present, the stannous fluoride obtained by the disclosed preparation method of stannous fluoride generally has the problems of low purity and many impurities. Existing research generally focuses on the direction of developing new synthetic routes to increase the concentration of the product . And ...

Claims

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Application Information

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IPC IPC(8): C01G19/04
CPCC01G19/04
Inventor 李立平黄司平许彬肖炜彬
Owner GUANGDONG GUANGHUA SCI TECH
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