CN102557079A - Preparation method of sodium fluoride - Google Patents
Preparation method of sodium fluoride Download PDFInfo
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- CN102557079A CN102557079A CN2012100467452A CN201210046745A CN102557079A CN 102557079 A CN102557079 A CN 102557079A CN 2012100467452 A CN2012100467452 A CN 2012100467452A CN 201210046745 A CN201210046745 A CN 201210046745A CN 102557079 A CN102557079 A CN 102557079A
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- sodium sulfate
- sodium
- sodium fluoride
- fluoride
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Abstract
The invention discloses a preparation method of sodium fluoride. The preparation method comprises the following steps: adding sodium sulfate solution at the mass percentage concentration of 12 to 28 percent into ammonium fluoride solution at the temperature of between 30 and 65 DEG C to generate sodium sulfate precipitate, wherein the ammonium fluoride at the mass percentage concentration of 8 to 50 percent serves as a raw material and the adding speed of the sodium sulfate is 40 to 200 ml/min; reacting for 60 to 130 minutes by controlling the stirring speed to 130 to 400 r/min; performing solid liquid separation to obtain sodium sulfate filter cakes; washing the filter cakes by using deionized water; and drying to obtain the sodium sulfate products. Compared with the prior art, the method has the advantages of using the sodium sulfate as the raw material instead of the conventional sodium chloride, preventing chloride ions from entering a production system, reducing corrosion-resistant requirement of the equipment and saving production cost. The method is simple and practical in process route and provides technological theory support for production of the sodium fluoride in the fluorine chemical industry enterprises.
Description
Technical field
The invention belongs to the fluorine chemical field, relate in particular to a kind of preparation method of Sodium Fluoride.
Background technology
Sodium Fluoride is widely used one type of fluorine chemical product in the fluorine chemical industry, and Sodium Fluoride is colourless shinny crystal or white powder, proportion 2.25,1695 ℃ of 993 ℃ of boiling points of fusing point.Water-soluble and hydrofluoric acid, little alcohol that is melted into.The aqueous solution is weakly alkaline, is dissolved in hydrofluoric acid and forms sodium bifluoride, can etching glass.
Sodium Fluoride is mainly used in the application industry and makes Phosphating Accelerant, makes phosphatization liquid stable, phosphatization refinement, improvement phosphatize phosphate coat performance.The Al3+ that sealing has the very big negative catalysis of hazardness in aluminium and the alloy phosphating thereof makes phosphatization carry out wood preservative, agricultural insecticide, Brewing industry sterilant, medical sanitas, solder flux, alkaline zincate galvanizing additive and enamel, paper-making industry etc. smoothly.
Fluorochemical is added in the toothpaste can plays anticaries action, because fluorochemical and enamel effect can form fluorapatite at enamel surface, improve adamantine hardness and capacity antacid, and can reduce the formation of bacterial plaque, reduce the sickness rate of carious tooth.The consumption of Sodium Fluoride in toothpaste is generally 0.22～0.33%.
It is the raw material production Sodium Fluoride that prior art mainly adopts Neutral ammonium fluoride and sodium-chlor; With sodium-chlor is raw materials for production; In production system, introduce cl ions; High to the requirement of production unit rot-resistant, in production technique, introduced cl ions and will be difficult to from Production Flow Chart, go out, line causes disadvantageous effect to forming a complete production network.
Summary of the invention
The objective of the invention is to overcome above-mentioned is the shortcoming of raw material production Sodium Fluoride with sodium-chlor, and a kind of highly effective, simple to operate, the preparation method that other production lines in the production system do not caused the Sodium Fluoride of disadvantageous effect are provided.
The present invention provides a kind of preparation method of Sodium Fluoride, and this method may further comprise the steps:
(1) be raw material with mass percentage concentration 8%～50% Neutral ammonium fluoride; The metabisulfite solution (add-on of sodium sulfate be theoretical amount 110%～150%) that between 30 ℃ to～65 ℃, in ammonium fluoride solution, adds mass percentage concentration 12%～28%; The adding speed of sodium sulfate is 40ml/min～200ml/min, generates the Sodium Fluoride deposition; Stirring velocity is controlled between 130r/min～400r/min, reaction 60min～130min, ageing 40min～90min; Solid-liquid separation obtains the Sodium Fluoride filter cake; Repeatedly wash the Sodium Fluoride filter cake with deionized water, and dry under 110 ℃～140 ℃, obtain the Sodium Fluoride product.
Compared with prior art; It is raw material that the present invention has replaced conventional sodium-chlor with sodium sulfate; Avoid cl ions to get into production system, reduced the requirement for anticorrosion of equipment, practiced thrift production cost; Operational path simple possible of the present invention provides the technical know-how support to fluorine chemical enterprise production Sodium Fluoride simultaneously.
Below, further specify beneficial effect of the present invention through embodiment.
Embodiment
Embodiment 1
The ammonium fluoride solution that in polytetrafluoroethylene beaker, adds 200g mass percentage concentration 8%; Turn on agitator; Control stirring velocity 130r/min; In ammonium fluoride solution, add the metabisulfite solution (add-on of sodium sulfate be theoretical amount 110%) of 281.44g mass percentage concentration 12%, the adding speed of sodium sulfate is 40ml/min; Control reaction temperature is 30 ℃, reaction 60min, and ageing 40min, solid-liquid separation, with deionized water wash Sodium Fluoride filter cake, oven dry Sodium Fluoride filter cake obtains the Sodium Fluoride product under 110 ℃.
Embodiment 2
The ammonium fluoride solution that in polytetrafluoroethylene beaker, adds 200g mass percentage concentration 19%; Turn on agitator; Control stirring velocity 220r/min; In ammonium fluoride solution, add the metabisulfite solution (add-on of sodium sulfate be theoretical amount 120%) of 583.35g mass percentage concentration 15%, the adding speed of sodium sulfate is 70ml/min; Control reaction temperature is 41 ℃, reaction 85min, and ageing 55min, solid-liquid separation, with deionized water wash Sodium Fluoride filter cake, oven dry Sodium Fluoride filter cake obtains the Sodium Fluoride product under 120 ℃.
Embodiment 3
The ammonium fluoride solution that in polytetrafluoroethylene beaker, adds 200g mass percentage concentration 31%; Turn on agitator; Control stirring velocity 270r/min; In ammonium fluoride solution, add the metabisulfite solution (add-on of sodium sulfate be theoretical amount 130%) of 736.50g mass percentage concentration 21%, the adding speed of sodium sulfate is 120ml/min; Control reaction temperature is 45 ℃, reaction 90min, and ageing 70min, solid-liquid separation, with deionized water wash Sodium Fluoride filter cake, oven dry Sodium Fluoride filter cake obtains the Sodium Fluoride product under 130 ℃.
Embodiment 4
The ammonium fluoride solution that in polytetrafluoroethylene beaker, adds 200g mass percentage concentration 42%; Turn on agitator; Control stirring velocity 330r/min; In ammonium fluoride solution, add the metabisulfite solution (add-on of sodium sulfate be theoretical amount 140%) of 940.27g mass percentage concentration 24%, the adding speed of sodium sulfate is 150ml/min; Control reaction temperature is 58 ℃, reaction 125min, and ageing 80min, solid-liquid separation, with deionized water wash Sodium Fluoride filter cake, oven dry Sodium Fluoride filter cake obtains the Sodium Fluoride product under 140 ℃.
Embodiment 5
The ammonium fluoride solution that in polytetrafluoroethylene beaker, adds 200g mass percentage concentration 48%; Turn on agitator; Control stirring velocity 400r/min; In ammonium fluoride solution, add the metabisulfite solution (add-on of sodium sulfate be theoretical amount 150%) of 986.87g mass percentage concentration 28%, the adding speed of sodium sulfate is 200ml/min; Control reaction temperature is 65 ℃, reaction 130min, and ageing 90min, solid-liquid separation, with deionized water wash Sodium Fluoride filter cake, oven dry Sodium Fluoride filter cake obtains the Sodium Fluoride product under 150 ℃.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any pro forma restriction; Anyly do not break away from technical scheme content of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, all still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (1)
1. the preparation method of a Sodium Fluoride is characterized in that this method may further comprise the steps:
(1) be raw material with mass percentage concentration 8%～50% Neutral ammonium fluoride; The metabisulfite solution that between 30 ℃ to～65 ℃, in ammonium fluoride solution, adds mass percentage concentration 12%～28%; The add-on of sodium sulfate is 110%～150% of a theoretical amount; The adding speed of sodium sulfate is 40ml/min～200ml/min, generates the Sodium Fluoride deposition; Stirring velocity is controlled between 130r/min～400r/min, reaction 60min～130min, ageing 40min～90min; Solid-liquid separation obtains the Sodium Fluoride filter cake; Repeatedly wash the Sodium Fluoride filter cake with deionized water, and dry under 110 ℃～140 ℃, obtain the Sodium Fluoride product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100467452A CN102557079A (en) | 2012-02-28 | 2012-02-28 | Preparation method of sodium fluoride |
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| CN2012100467452A CN102557079A (en) | 2012-02-28 | 2012-02-28 | Preparation method of sodium fluoride |
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| CN102557079A true CN102557079A (en) | 2012-07-11 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104150458A (en) * | 2014-07-29 | 2014-11-19 | 瓮福（集团）有限责任公司 | Method for separating and recycling chloride ions from chlorine-containing phosphate ores |
| CN106698479A (en) * | 2017-01-24 | 2017-05-24 | 陈可 | Non-aqueous complete-dissolution refining method of sodium fluoride containing organic impurities |
| KR20210105727A (en) * | 2020-02-19 | 2021-08-27 | 최윤진 | Method of recovering high quality sodium fluoride by treating waste water including fluorine compound with ammonium ion |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1511560A (en) * | 1922-06-30 | 1924-10-14 | Grasselli Chemical Co | Process of making a double salt of sodium fluorid and sodium sulphate |
| CN101376507A (en) * | 2007-08-30 | 2009-03-04 | 多氟多化工股份有限公司 | Method for producing sodium fluoride |
-
2012
- 2012-02-28 CN CN2012100467452A patent/CN102557079A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1511560A (en) * | 1922-06-30 | 1924-10-14 | Grasselli Chemical Co | Process of making a double salt of sodium fluorid and sodium sulphate |
| CN101376507A (en) * | 2007-08-30 | 2009-03-04 | 多氟多化工股份有限公司 | Method for producing sodium fluoride |
Non-Patent Citations (1)
| Title |
|---|
| 席明权: "铵盐复分解法制备氟化钠", 《绵阳农专学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104150458A (en) * | 2014-07-29 | 2014-11-19 | 瓮福（集团）有限责任公司 | Method for separating and recycling chloride ions from chlorine-containing phosphate ores |
| CN104150458B (en) * | 2014-07-29 | 2016-09-14 | 瓮福（集团）有限责任公司 | A kind of method separating and recovering chloride ion from chloride rock phosphate in powder |
| CN106698479A (en) * | 2017-01-24 | 2017-05-24 | 陈可 | Non-aqueous complete-dissolution refining method of sodium fluoride containing organic impurities |
| CN106698479B (en) * | 2017-01-24 | 2017-12-12 | 陈一可 | The non-aqueous complete molten process for purification of sodium fluoride containing organic impurities |
| KR20210105727A (en) * | 2020-02-19 | 2021-08-27 | 최윤진 | Method of recovering high quality sodium fluoride by treating waste water including fluorine compound with ammonium ion |
| KR102356642B1 (en) * | 2020-02-19 | 2022-01-27 | 최윤진 | Method of recovering high quality sodium fluoride by treating waste water including fluorine compound with ammonium ion |
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Application publication date: 20120711 |