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The preparation method of stannous fluoride

A technology of stannous fluoride and barium fluoride, which is applied in the field of preparation of fine chemicals, can solve the problems of high production cost, inflammability and explosion, and complicated process flow, and achieves favorable storage and stability, mild reaction conditions, Environmentally friendly effect

Active Publication Date: 2022-05-03
GUANGDONG GUANGHUA SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (5) CN105800675A patent, using tin dioxide and calcium fluoride reaction to prepare stannous fluoride, the material containing tin dioxide, calcium fluoride and sodium carboxymethyl cellulose are ground and mixed, and placed in CO and CO 2 In a mixed atmosphere, roast at a temperature of 500°C to 1000°C to recover stannous fluoride from the roasting flue gas. Although this scheme has the advantage of high product purity, it consumes a lot of energy and the carbon monoxide used is poisonous. And it is flammable and explosive. In addition, the roasting temperature of this scheme exceeds 300 ° C. During the roasting process, stannous fluoride is easy to polymerize and form polymers, which affects product performance.
[0009] In summary, the existing methods for preparing stannous fluoride still have the disadvantages of complex process flow, low yield and purity, and high production cost.

Method used

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  • The preparation method of stannous fluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) add 200g mass concentration 10% hydrofluoric acid aqueous solution in reactor, open and stir, add 60g stannous sulfate solid in above-mentioned hydrofluoric acid aqueous solution, dissolve completely, obtain the hydrofluoric acid solution of stannous sulfate. Starting from the addition of stannous sulfate, nitrogen gas is passed into the hydrofluoric acid aqueous solution, and the flow rate is controlled so that no liquid splashes out.

[0035] (2) Take by weighing 36g barium fluoride and join in the stannous sulfate hydrofluoric acid solution in the step (1) with the speed of 15g / min, after adding, continue to react for 10 minutes. During the reaction process, nitrogen gas was continuously passed into the solution, and the flow rate was controlled so that no liquid splashed out.

[0036] (3) Carry out solid-liquid separation to the solution after step (2) reaction, the obtained filtrate is evaporated and concentrated to crystallization at 80°C, then vacuum-dried at...

Embodiment 2

[0040] (1) add the hydrofluoric acid aqueous solution of 500g mass concentration 10% in reactor, open and stir, add 125g stannous sulfate solid in above-mentioned hydrofluoric acid aqueous solution, dissolve and obtain the hydrofluoric acid solution of stannous sulfate completely. Starting from the addition of stannous sulfate, nitrogen gas is passed into the hydrofluoric acid aqueous solution, and the flow rate is controlled so that no liquid splashes out.

[0041] (2) Take by weighing 102g barium fluoride and join in the hydrofluoric acid solution of tin protosulfate in the step (1) with the speed of 25g / min, after feeding finishes, continue reaction 30 minutes. During the reaction process, nitrogen gas was continuously passed into the solution, and the flow rate was controlled so that no liquid splashed out.

[0042] (3) The solution after the reaction in step (2) is subjected to solid-liquid separation, and the obtained filtrate is evaporated and concentrated to crystalliz...

Embodiment 3

[0045] (1) add the hydrofluoric acid aqueous solution of 2000g mass concentration 5% in reactor, open and stir, add 400g stannous sulfate solid in above-mentioned hydrofluoric acid aqueous solution, dissolve and obtain the hydrofluoric acid solution of stannous sulfate completely. Starting from the addition of stannous sulfate, nitrogen gas is passed into the hydrofluoric acid aqueous solution, and the flow rate is controlled so that no liquid splashes out.

[0046] (2) Take by weighing 360g barium fluoride and join in the hydrofluoric acid solution of tin protosulfate in the step (1) with the speed of 30g / min, after feeding finishes, continue reaction 30 minutes. During the reaction process, nitrogen gas was continuously passed into the solution, and the flow rate was controlled so that no liquid splashed out.

[0047](3) The solution after the reaction in step (2) is subjected to solid-liquid separation, and the obtained filtrate is evaporated and concentrated to crystalliza...

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Abstract

The present invention relates to a preparation method of stannous fluoride. The preparation method comprises the following steps: mixing an aqueous hydrofluoric acid solution and stannous sulfate to obtain a hydrofluoric acid solution of stannous sulfate; adding barium fluoride to the hydrofluoric acid solution of stannous sulfate, and reacting to obtain a fluoride solution The stannous hydrofluoric acid solution is filtered, and the filtrate is concentrated and dried to obtain stannous fluoride. The above method adopts a brand-new reaction route, and the prepared stannous fluoride product has high yield and purity, low production cost and simple technological process.

Description

technical field [0001] The present invention relates to the preparation of fine chemicals, in particular to the preparation 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, there are not many disclosed methods for preparing stannous fluoride, mainly the following: [0004] (1) US3172724A patent, prepared by the reaction of elemental tin and hydrofluoric acid at a temperature of 63-80°C, the principle is 2Sn+4HF+O 2 = 2SnF 2 +2H 2 O. Due to the prese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/04C01F11/46
CPCC01G19/04C01F11/462C01P2006/80
Inventor 王辉李煜乾唐燕华张建锋
Owner GUANGDONG GUANGHUA SCI TECH
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