Method for preparing stannous fluoride by sing hydrofluoric acid

A technology of stannous fluoride and hydrofluoric acid, applied in tin halide and other directions, can solve the problems of low product purity, low economic significance and high cost, and achieve the effects of easy availability of raw materials, high economic significance and low cost

Inactive Publication Date: 2014-12-24
HUNAN NONFERROUS FLUORIDE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) In US3172724A (disclosure date: March 09, 1965), stannous fluoride was prepared by reacting at 63-80°C with elemental tin flakes and hydrofluoric acid with a mass concentration of 20-30%. Though this method can obtain stannous fluoride product, the purity of product is not high, and productive rate is low;
[0005] (2) In the 1982 Czech patent document No. 231928, stannous fluoride was obtained by direct ion exchange with stannous chloride and sodium fluoride. This method is simple to operate, but the residual sodium fluoride in the product is difficult to remove, and the residual Sodium fluoride reduces the use effect and efficiency of stannous fluoride;
[0006] (3) In CN1141884A (published on February 05, 1997), tin protofluoride was prepared by substitution reaction with elemental tin powder and copper fluoride. This method is easy to operate and the obtained product has high purity, but requires the The mesh number is high, and the prices of high mesh tin powder and copper fluoride are quite expensive, which makes the cost of this method too high and has little economic significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Present embodiment takes hydrofluoric acid, stannous oxide as raw material, specifically comprises the following steps:

[0021] (1) First add 80ml of hydrofluoric acid with a mass concentration of 40.0% (silicon content is 0.03wt%) into the reactor, start stirring, then add 10g of tin pellets, and then add 100g of stannous oxide at a speed of 18g / min Add in hydrofluoric acid, after the addition, continue to react for 15 minutes, after the reaction, take out the tin packet;

[0022] Reaction equation: SnO+2HF→SnF 2 +H 2 O;

[0023] Added stannous oxide is an industrial grade product, and the particle size is 100 mesh;

[0024] From the beginning of adding stannous oxide to the end of the reaction, nitrogen gas is passed into the hydrofluoric acid, and the flow rate is controlled at no liquid splashing;

[0025] (2) Heating to 75°C and maintaining the temperature, stirring to concentrate, vacuum drying, the vacuum degree is 90Pa, the drying temperature is 105°C, and ...

Embodiment 2

[0028] Present embodiment takes hydrofluoric acid, stannous oxide as raw material, specifically comprises the following steps:

[0029] (1) First add 180ml of hydrofluoric acid with a mass concentration of 31.4% (silicon content is 0.03wt%) into the reactor, start stirring, then add 20g of tin pellets, and then add 200g of stannous oxide at a speed of 20g / min Add it into the hydrofluoric acid, after the addition, continue to react for 20 minutes, after the reaction, take out the tin packet;

[0030] Reaction equation: SnO+2HF→SnF 2 +H 2 O;

[0031] The added stannous oxide is an industrial grade product with a particle size of 200 mesh;

[0032] From the beginning of adding stannous oxide to the end of the reaction, nitrogen gas is passed into the hydrofluoric acid, and the flow rate is controlled at no liquid splashing;

[0033] (2) Heating to 85°C and maintaining the temperature, stirring and concentrating, and vacuum drying with a vacuum degree of 95 Pa, a drying temper...

Embodiment 3

[0036] Present embodiment takes hydrofluoric acid, stannous oxide as raw material, specifically comprises the following steps:

[0037] (1) First add 285ml of hydrofluoric acid with a mass concentration of 47.9% (silicon content is 0.03wt%) into the reactor, start stirring, then add 50g of tin pellets, and then add 500g of stannous oxide at a speed of 22g / min Add in hydrofluoric acid, after the addition, continue to react for 30 minutes, after the reaction, take out the tin packet;

[0038] Reaction equation: SnO+2HF→SnF 2 +H 2 O;

[0039] The added stannous oxide is an industrial grade product, and the particle size is 325 mesh;

[0040] From the beginning of adding stannous oxide to the end of the reaction, nitrogen gas is passed into the hydrofluoric acid, and the flow rate is controlled at no liquid splashing;

[0041] (2) Heating to 95°C, and maintaining the temperature, stirring, concentrating, and vacuum drying, the vacuum degree is 100 Pa, the drying temperature is...

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Abstract

A method for preparing stannous fluoride by sing hydrofluoric acid. The method uses hydrofluoric acid and stannous oxide as raw materials, and includes the following steps: (1) first adding hydrofluoric acid into a reactor, staring to stir, then adding a tin granular package in the equivalent of 8-12 wt% of the theoretical amount of stannous oxide, then adding the theoretical amount of stannous oxide into hydrofluoric acid at a speed of 15-25g / min, after material addition, continuing the reaction for 15-30 min, and after the reaction, removing the tin granular package; and from the addition of stannous oxide to the end of the reaction, introducing nitrogen into hydrofluoric acid, wherein the flow is controlled that no liquid spills; and (2) heating to 75-95 DEG C, maintaining the temperature, stirring for concentrating, and conducting vacuum drying to obtain a finished product. The stannous fluoride prepared by the method provided by the invention has low cost, high product yield and high purity.

Description

technical field [0001] The invention relates to a method for preparing stannous fluoride with hydrofluoric acid, in particular to a method for preparing stannous fluoride with hydrofluoric acid and stannous oxide as raw materials. Background technique [0002] Stannous fluoride is mainly used in toothpaste, mouthwash, brazing flux and pharmaceutical additives, and is most widely used in toothpaste and mouthwash. The surface hardness and wear resistance of teeth treated with an appropriate amount of stannous fluoride are increased, which can effectively prevent gingivitis and dental plaque. [0003] At present, the method for preparing stannous fluoride reported mainly contains three kinds: [0004] (1) In US3172724A (disclosure date: March 09, 1965), stannous fluoride was prepared by reacting at 63-80°C with elemental tin flakes and hydrofluoric acid with a mass concentration of 20-30%. Though this method can obtain stannous fluoride product, the purity of product is not h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/04
Inventor 朱亮李飞跃黄忠孝刘峙军李文英
Owner HUNAN NONFERROUS FLUORIDE CHEM
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