CN101462734A - Method for preparing potassium borofluoride from fluorine-containing potassium chloride - Google Patents
Method for preparing potassium borofluoride from fluorine-containing potassium chloride Download PDFInfo
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- CN101462734A CN101462734A CNA2008100307870A CN200810030787A CN101462734A CN 101462734 A CN101462734 A CN 101462734A CN A2008100307870 A CNA2008100307870 A CN A2008100307870A CN 200810030787 A CN200810030787 A CN 200810030787A CN 101462734 A CN101462734 A CN 101462734A
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- potassium fluoborate
- repone
- hydrofluoric acid
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Abstract
The invention provides a method for preparing potassium fluoborate from fluorine-containing potassium chloride, which belongs to a method for producing potassium fluoborate. The method mainly solves the technical problems that the prior art is high in cost for producing potassium fluoborate, and is difficult to reuse resources, and the like. A technical proposal of the method has the key points that water is first added into a synthesis groove; fluorine-containing potassium chloride, borax or boric acid and hydrofluoric acid are added for synthesis reaction while the water is stirred; the raw materials are added according to the measurement mixture ratio of pure substances as follows: 0.1 to 1 m<3> of water, 100 kilograms of fluorine-containing potassium chloride, 65 to 95 kilograms of borax or boric acid and 0.2 to 0.6 m<3> of hydrofluoric acid in the synthesis groove; reaction temperature is controlled to be between 0 and 100 DEG C; and after reaction performs for 5 to 300 minutes, a potassium fluoborate product is obtained through filtration, washing, separation and drying. The method can solve the problem of utilizing fluorine-containing potassium chloride resources, enables fluorine and potassium which are contained by the fluorine-containing potassium chloride to be fully utilized, can reduce production cost, is convenient for industrial production, and has both good economic benefit and good social benefit.
Description
Technical field
The present invention relates to a kind of method of producing potassium fluoborate, especially a kind of method of utilizing fluorine-containing Repone K to prepare potassium fluoborate.
Background technology
Potassium fluoborate is mainly used in the production Al-Ti-B alloy, or is used as the fusing assistant of hot weld, brazing, or is used for the casting production of magnalium, makes the raw material of boron trifluoride and other villiaumite and is used for electrochemical process and reagent.At present, the traditional processing technology of potassium fluoborate is: generate fluoroboric acid earlier with hydrofluoric acid and borax or acid reaction, again with salt of wormwood or potassium hydroxide or Repone K neutralization reaction and potassium fluoborate.Fluorine-containing Repone K is the mixture of a kind of Repone K and Potassium monofluoride, is the byproduct of organic fluorocompound production process, conventional separation method separation difficulty, and the utilization of resources is restricted.
Summary of the invention
The purpose of this invention is to provide the fluorine-containing Repone K that utilizes that a kind of waste material utilizes again, production cost is lower and prepare the method for potassium fluoborate.
The technical solution adopted for the present invention to solve the technical problems is: add entry earlier in synthetic groove, add fluorine-containing Repone K, borax, hydrofluoric acid more while stirring and carry out building-up reactions, temperature of reaction is between 0~100 ℃, 5~300 minutes reaction times, after reaction finishes, make the potassium fluoborate product through filtration, washing, separation, drying.Each raw material adds by following pure substance metering proportion, and the amount of water in the synthetic groove is 0.1~1m
3, fluorine-containing Repone K 100kg, borax 65~95kg, hydrofluoric acid 0.2~0.6m
3, temperature of reaction is 20~90 ℃, the reaction times: 45~300 minutes.Its optimum ratio is: water 1.7m
3, fluorine-containing Repone K 515kg, borax 440kg, hydrofluoric acid 2.00m
3, room temperature reaction 45~220 minutes.
The present invention also can adopt following method production: add entry earlier in synthetic groove, add fluorine-containing Repone K, boric acid, hydrofluoric acid more while stirring and carry out building-up reactions, 0~100 ℃ of temperature of reaction, 5~300 minutes reaction times, after reaction finishes, through filtration, washing, separate, dry, pack the potassium fluoborate product.Each raw material adds by following pure substance metering proportion, and the amount of water in the synthetic groove is 0.1~1m
3, fluorine-containing Repone K 100kg, boric acid 65~95kg, hydrofluoric acid 0.2~0.6m
3, temperature of reaction is 20~90 ℃, the reaction times: 45~300 minutes.Its optimum ratio is: water 1.1m
3, fluorine-containing Repone K 328kg, boric acid 243kg, hydrofluoric acid 1.35m
3, room temperature reaction 45~220 minutes.
The present invention can adopt the raw material of following content: the F content of fluorine-containing Repone K is 1~20%, the B of borax or boric acid
2O
3Content is 10~40%, and the HF content of hydrofluoric acid is 15~50%.
The invention has the beneficial effects as follows: utilize fluorine-containing Repone K to produce the resource reutilization problem that potassium fluoborate not only can solve fluorine-containing Repone K, and because fluorine-containing Repone K is byproduct, price is lower than salt of wormwood, potassium hydroxide, Repone K, utilize it to produce potassium fluoborate, its institute is fluorine-containing, potassium can be fully used, can reduce the potassium fluoborate production cost, for a more economical shortcut is found in potassium fluoborate production, simultaneously easy suitability for industrialized production.It had both had good economic benefit, had good social benefit again.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
That the invention will be further described is as follows below in conjunction with embodiment:
Earlier add entry in synthetic groove, add fluorine-containing Repone K, borax or boric acid while stirring again, hydrofluoric acid carries out building-up reactions, preferred plan is to add raw material in this order.Each raw material adds by following pure substance metering proportion, and the amount of water in the synthetic groove is 0.1~1m
3, fluorine-containing Repone K 100kg, borax or boric acid 65~95kg, hydrofluoric acid 0.2~0.6m
3Temperature of reaction between 0~100 ℃, 5~300 minutes reaction times; Preferable reaction temperature is 20~90 ℃, and the preferred reaction time is 60~180 minutes.After reaction finishes, through filtration, washing, separate, dry, pack the potassium fluoborate product.
Embodiment 1: the present invention can adopt impure raw material, but each raw material adds water 1.1m by following pure substance metering proportion adding at synthetic groove
3, open and stir, add the fluorine-containing Repone K of 328kg, 243kg boric acid, 1.35m
3The down reaction 150 minutes of hydrofluoric acid, room temperature condition, optimal reaction temperature is 30-50 ℃, more after filtration, washing, separation, dry potassium fluoborate product.Consult Fig. 1.
Embodiment 2: the present invention can adopt impure raw material, but each raw material adds water 1.7m by following pure substance metering proportion adding at synthetic groove
3, open stirring, add the fluorine-containing Repone K of 515kg, 440kg borax, 2.00m
3Hydrofluoric acid, room temperature reaction 200 minutes, optimal reaction temperature are 25~45 ℃, more after filtration, washing, separation, dry potassium fluoborate product.Consult Fig. 1.
Embodiment 3: the present invention can adopt impure raw material, as adopts the raw material of following content: the F content of fluorine-containing Repone K is 1~20%, the B of borax or boric acid
2O
3Content is 10~40%, and the HF content of hydrofluoric acid is 15~50%.Each raw material is still pressed the pure substance metering proportion and is added.All the other consult Fig. 1 with above-mentioned embodiment.
Adopt the inventive method can produce high-grade product.Potassium fluoborate company standard as shown in table 1 and product various performance parameters of the present invention contrast.
Table 1:
Claims (7)
1, a kind of method of utilizing fluorine-containing Repone K to prepare potassium fluoborate, it is characterized in that: in synthetic groove, add entry earlier, add fluorine-containing Repone K, borax, hydrofluoric acid more while stirring and carry out building-up reactions, temperature of reaction is between 0~100 ℃, 5~300 minutes reaction times, after reaction finishes, make the potassium fluoborate product through filtration, washing, separation, drying.
2, the method for utilizing fluorine-containing Repone K to prepare potassium fluoborate according to claim 1 is characterized in that: each raw material adds by following pure substance metering proportion, and the amount of water in the synthetic groove is 0.1~1m
3, fluorine-containing Repone K 100kg, borax 65~95kg, hydrofluoric acid 0.2~0.6m
3, temperature of reaction is 20~90 ℃, the reaction times: 45~300 minutes.
3, the method for utilizing fluorine-containing Repone K to prepare potassium fluoborate according to claim 1 is characterized in that: water 1.7m
3, fluorine-containing Repone K 515kg, borax 440kg, hydrofluoric acid 2.00m
3, room temperature reaction 45~220 minutes.
4, a kind of method of utilizing fluorine-containing Repone K to prepare potassium fluoborate, it is characterized in that: in synthetic groove, add entry earlier, add fluorine-containing Repone K, boric acid, hydrofluoric acid more while stirring and carry out building-up reactions, 0~100 ℃ of temperature of reaction, 5~300 minutes reaction times, after reaction finishes, through filtration, washing, separate, dry, pack the potassium fluoborate product.
5, the method for utilizing fluorine-containing Repone K to prepare potassium fluoborate according to claim 4 is characterized in that: each raw material adds by following pure substance metering proportion, and the amount of water in the synthetic groove is 0.1~1m
3, fluorine-containing Repone K 100kg, boric acid 65~95kg, hydrofluoric acid 0.2~0.6m
3, temperature of reaction is 20~90 ℃, the reaction times: 45~300 minutes.
6, the method for utilizing fluorine-containing Repone K to prepare potassium fluoborate according to claim 2 is characterized in that: water 1.1m
3, fluorine-containing Repone K 328kg, boric acid 243kg, hydrofluoric acid 1.35m
3, room temperature reaction 45~220 minutes.
7, according to claim 1,2,3,4, the 5 or 6 described methods of utilizing fluorine-containing Repone K to prepare potassium fluoborate, it is characterized in that: in each proportioning raw material, the fluorine content of fluorine-containing Repone K is 1~20%, the B of borax or boric acid
2O
3Content is 10~40%, and the HF content of hydrofluoric acid is 15~50%.
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CNA2008100307870A CN101462734A (en) | 2008-03-12 | 2008-03-12 | Method for preparing potassium borofluoride from fluorine-containing potassium chloride |
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CNA2008100307870A CN101462734A (en) | 2008-03-12 | 2008-03-12 | Method for preparing potassium borofluoride from fluorine-containing potassium chloride |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103332700A (en) * | 2013-07-23 | 2013-10-02 | 森田化工(张家港)有限公司 | Method for preparing potassium borofluoride through fluorine-containing wastewater |
CN110436475A (en) * | 2019-09-11 | 2019-11-12 | 北京镭硼科技有限责任公司 | A kind of preparation method of high-purity fluorine boric-10 acid potassium |
-
2008
- 2008-03-12 CN CNA2008100307870A patent/CN101462734A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103332700A (en) * | 2013-07-23 | 2013-10-02 | 森田化工(张家港)有限公司 | Method for preparing potassium borofluoride through fluorine-containing wastewater |
CN103332700B (en) * | 2013-07-23 | 2015-02-04 | 森田化工(张家港)有限公司 | Method for preparing potassium borofluoride through fluorine-containing wastewater |
CN110436475A (en) * | 2019-09-11 | 2019-11-12 | 北京镭硼科技有限责任公司 | A kind of preparation method of high-purity fluorine boric-10 acid potassium |
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