CN103332700A - Method for preparing potassium borofluoride through fluorine-containing wastewater - Google Patents
Method for preparing potassium borofluoride through fluorine-containing wastewater Download PDFInfo
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- CN103332700A CN103332700A CN2013103100647A CN201310310064A CN103332700A CN 103332700 A CN103332700 A CN 103332700A CN 2013103100647 A CN2013103100647 A CN 2013103100647A CN 201310310064 A CN201310310064 A CN 201310310064A CN 103332700 A CN103332700 A CN 103332700A
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Abstract
The invention relates to a method for preparing potassium borofluoride through fluorine-containing wastewater. The method is characterized by comprising the following steps: (1) utilizing water to regulate the hydrogen fluoride content of the fluorine-containing wastewater until the mass content of hydrogen fluoride is 12%-17%; (2) completely mixing the wastewater after treatment in the step (1) with potassium chloride saturated solution according to a mass ratio of (3-5):1 so as to fluorate; (3) mixing borax with the wastewater after treatment in the step (1) according to a mass ratio of 1: (3-5), and stirring so as to completely dissolve the borax; mixing solution in the step 2 with solution in the step 3 according to a mass ratio of (0.8-1.2):1, stirring to react, and continuously separating potassium fluoborate out in a reaction process so as to prepare potassium fluoborate suspension; and (5) solid-liquid separating, washing and drying the potassium fluoborate suspension in the step (4) so as to obtain a potassium fluoborate product. The potassium fluoborate product prepared by the method can satisfy the requirements of potassium fluoborate use factories.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of method that is prepared potassium fluoborate by fluoride waste.
Background technology
Potassium fluoborate, molecular formula KBF
4
, molecular weight 125.90, relative density (d20) 2.498,350 ℃ of fusing points, white powder or do not have the coloured particles xln is slightly soluble in water, ethanol, ether, be insoluble to alkaline solution, can be decomposed into boron trifluoride by strong acid, molten altogether with alkali-metal carbonate, generate fluorochemical and borate.
Potassium fluoborate also is used for mould material, electrochemical engineering and the chemical experiment of manufacturing, aluminium and the magnesium casting usefulness of boron trifluoride as analytical reagent and solubility promoter.
The production of potassium fluoborate, traditional method are to adopt boric acid, hydrogen fluoride, potassium hydroxide as raw material, and the first step boric acid and hydrogen fluoride reaction earlier generate fluoroboric acid, second the step again with the potassium hydroxide neutralization reaction, generate potassium fluoborate, through filtration, washing, drying, obtain the potassium fluoborate product.The method of traditional mode of production potassium fluoborate exists cost height, problems such as complex process.
On the other hand, fluoride waste is as one of main waste water that produces in the Chemical Manufacture, and is big for the pollution of environment.In addition, contain the compound price of fluorine element often than higher.Therefore, enterprise handles the fluorochemical that reclaims simultaneously in the waste water with fluoride waste usually through wastewater processing technology, to reach the purpose that reduces environmental pollution and resource continuous utilization, but in the prior art, no matter any method of wastewater treatment all needs the extra input sewage treatment equipment of enterprise and manpower etc., and then increase cost greatly.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, a kind of method that is prepared potassium fluoborate by fluoride waste is provided, the fluoride waste that produces when adopting enterprise to produce, Potassium monofluoride, borax are as the raw material production potassium fluoborate, after filtration, washing, drying, obtain the potassium fluoborate product.The present invention rationally utilizes fluoride waste to prepare potassium fluoborate, for reducing environmental pollution, reducing production costs, promote sustained development of enterprises, very important meaning is arranged.
For solving above technical problem, the present invention takes following technical scheme:
A kind ofly prepare the method for potassium fluoborate by fluoride waste, may further comprise the steps:
(1) water is regulated the hydrogen fluoride content in the described fluoride waste, is 12% ~ 17% until described hydrofluoric mass content, and wherein, described fluoride waste is for producing the fluoride waste that lithium hexafluoro phosphate produces;
(2) waste water that will handle through step (1) is that 3 ~ 5:1 fully mixes with saturated potassium chloride solution by mass ratio, makes and carries out fluoridation, and the described fluoridation time is 20min ~ 40min;
(3) be that 1:3 ~ 5 mix with the waste water of handling through step (1) by mass ratio with borax, stir, make described borax dissolve fully;
(4) be that 0.8 ~ 1.2:1 mixes with the solution of step (2) and the solution of step (3) by mass ratio, stirring reaction, the reaction times is controlled at 1.5h ~ 3h, and temperature of reaction is controlled at 80 ℃ ~ 100 ℃, constantly there is potassium fluoborate to separate out in the reaction process, makes the potassium fluoborate suspension liquid;
(5) with potassium fluoborate suspension liquid in the step (4) through solid-liquid separation, washing, drying, make the potassium fluoborate product.
According to the present invention, the hydrofluoric mass content that basic composition is of fluoride waste described in the step (1) is 18% ~ 25%, and the mass content of hydrogenchloride is 18% ~ 25%.
Preferably, washing is that water carries out centrifuge washing in whizzer described in the step (5), and the pH=6.5 of water outlet to be washed ~ 7.5 o'clock stop washing.
Preferably, drying described in the step (5) is dry in drying machine, and be 10h ~ 24h time of drying, and drying temperature is 100 ℃ ~ 120 ℃.
Particularly, described drying machine is rotary drier.
Preferably, the potassium fluoborate transferred product that step (5) makes is pulverized to pulverizer, made Powdered potassium fluoborate product.
Preferably, the purity of described potassium fluoborate product is more than or equal to 99%.
Because the enforcement of technique scheme, the present invention compared with prior art has following advantage:
The present invention is to be the feedstock production potassium fluoborate with fluoride waste, Repone K, borax, and various raw material sources are abundant, and raw material is easy to get and is cheap, technological process is simple, operation control is simple and convenient, production efficiency height, reactivity, product yield height, good product quality, and reduced the pollution of environment effectively, and reducing production cost, the potassium fluoborate product purity that finally makes can reach more than 99%, other metals and nonmetal index are all controlled in the reasonable scope, meet the needs of customers.Therefore, the present invention has good economic worth and social value.
Embodiment
The present invention will be further described in detail below in conjunction with specific embodiment:
Embodiment 1
Present embodiment is raw material with the fluoride waste of producing the lithium hexafluoro phosphate generation in the Chemical Manufacture, and the essential property of fluoride waste is as follows: hydrofluoric mass content is roughly 20%, and the mass content of hydrogenchloride is roughly 20%.
The concrete steps of method that fluoride waste prepares potassium fluoborate are as follows:
(1) water is regulated hydrofluoric content in the fluoride waste, is roughly 15% until hydrofluoric mass content, in the actually operating, uses carbon steel liner PE material basin as the waste water regulating tank usually;
(2) preparing saturated potassium chloride solution earlier, is that 1:4 fully mix with the waste water of handling through step (1) by mass ratio with saturated potassium chloride solution then, makes and carries out fluoridation, and the fluoridation time is 30min;
(3) be that 1:3 mix with the waste water of handling through step (1) by mass ratio with the solid borax, stir, make borax dissolve fully;
(4) be that 1:1 mixes with the solution of step (2) and the solution of step (3) by mass ratio, stirring reaction, the reaction times is controlled at 2h, and temperature of reaction is controlled at 80 ℃ ~ 100 ℃, constantly has potassium fluoborate to separate out in the reaction process, makes the potassium fluoborate suspension liquid;
(5) use whizzer through solid-liquid separation potassium fluoborate suspension liquid in the step (4), the solid water in whizzer that separates the back gained carries out centrifuge washing, pH=6.5 ~ 7.5 of the water outlet after washing, to wash solid transfer dry 12h to the rotary drier of back gained then, drying temperature is 110 ℃, makes block potassium fluoborate product;
(6) the block potassium fluoborate transferred product that makes in the step (5) is pulverized to disintegrating machine, made Powdered potassium fluoborate product, product purity reaches 99%.
The result shows, handle the above-mentioned fluoride waste of 1t, can produce 200kg potassium fluoborate product, required cost is roughly 2000 yuan, compares the cost (cost is roughly 5000 yuan) of handling the above-mentioned fluoride waste of 1t and uses produced in conventional processes 200kg potassium fluoborate product (cost is roughly 3000 yuan) nearly to hang down 33.3%.
Embodiment 2
Present embodiment is raw material with the fluoride waste of producing the lithium hexafluoro phosphate generation in the Chemical Manufacture, and the essential property of fluoride waste is as follows: hydrofluoric mass content is roughly 18%, and the mass content of hydrogenchloride is roughly 18%.
The concrete steps of method that fluoride waste prepares potassium fluoborate are as follows:
(1) water is regulated hydrofluoric content in the fluoride waste, is roughly 12% until hydrofluoric mass content, in the actually operating, uses carbon steel liner PE material basin as the waste water regulating tank usually;
(2) preparing saturated potassium chloride solution earlier, is that 1:5 fully mix with the waste water of handling through step (1) by mass ratio with saturated potassium chloride solution then, makes and carries out fluoridation, and the time of fluoridizing is 40min;
(3) be that 1:4 mix with the waste water of handling through step (1) by mass ratio with the solid borax, stir, make borax dissolve fully;
(4) be that 1.2:1 mixes with the solution of step (2) and the solution of step (3) by mass ratio, stirring reaction, the reaction times is controlled at 3h, and temperature of reaction is controlled at 80 ℃ ~ 100 ℃, constantly has potassium fluoborate to separate out in the reaction process, makes the potassium fluoborate suspension liquid;
(5) use whizzer through solid-liquid separation potassium fluoborate suspension liquid in the step (4), the solid water in whizzer that separates the back gained carries out centrifuge washing, pH=6.5 ~ 7.5 of the water outlet after washing, to wash solid transfer dry 20h to the rotary drier of back gained then, drying temperature is 120 ℃, makes block potassium fluoborate product;
(6) the block potassium fluoborate transferred product that makes in the step (5) is pulverized to disintegrating machine, made Powdered potassium fluoborate product, product purity reaches 99%.
The result shows, handle the above-mentioned fluoride waste of 1t, can produce 150kg potassium fluoborate product, required cost is roughly 1500 yuan, compares the cost (cost is roughly 4000 yuan) of handling the above-mentioned fluoride waste of 1t and uses produced in conventional processes 150kg potassium fluoborate product (cost is roughly 2250 yuan) nearly to hang down 33.3%.
To sum up, preparation method of the present invention compared with prior art has following advantage:
1, the traditional technology of comparing, reaction raw materials is easy to get, and is with low cost, reacts simple to operation, and the fluoride waste that chemical workshop is produced is rationally handled in safety, environmental protection simultaneously, and remarkable in economical benefits has also been protected environment greatly.
2, the main raw of the used fluoride waste adjusting of the present invention equipment used is carbon steel liner PE material, and the stainless steel of comparing, steel lining tetrafluoro, Hastelloy have very big cost advantage.
More than the present invention has been done detailed description; its purpose is to allow the personage that is familiar with this art can understand content of the present invention and is implemented; can not limit protection scope of the present invention with this; and the invention is not restricted to the embodiments described; the equivalence that all spirit according to the present invention are done changes or modifies, and all should be encompassed within protection scope of the present invention.
Claims (7)
1. one kind prepares the method for potassium fluoborate by fluoride waste, it is characterized in that, may further comprise the steps:
(1) water is regulated the hydrogen fluoride content in the described fluoride waste, is 12% ~ 17% until described hydrofluoric mass content, and wherein, described fluoride waste is for producing the fluoride waste that lithium hexafluoro phosphate produces;
(2) waste water that will handle through step (1) is that 3 ~ 5:1 fully mixes with saturated potassium chloride solution by mass ratio, makes and carries out fluoridation, and the described fluoridation time is 20min ~ 40min;
(3) be that 1:3 ~ 5 mix with the waste water of handling through step (1) by mass ratio with borax, stir, make described borax dissolve fully;
(4) be that 0.8 ~ 1.2:1 mixes with the solution of step (2) and the solution of step (3) by mass ratio, stirring reaction, the reaction times is controlled at 1.5h ~ 3h, and temperature of reaction is controlled at 80 ℃ ~ 100 ℃, constantly there is potassium fluoborate to separate out in the reaction process, makes the potassium fluoborate suspension liquid;
(5) with potassium fluoborate suspension liquid in the step (4) through solid-liquid separation, washing, drying, make the potassium fluoborate product.
2. preparation method according to claim 1 is characterized in that, the hydrofluoric mass content that basic composition is of fluoride waste described in the step (1) is 18% ~ 25%, and the mass content of hydrogenchloride is 18% ~ 25%.
3. preparation method according to claim 1 is characterized in that, washing is that water carries out centrifuge washing in whizzer described in the step (5), and the pH=6.5 of water outlet to be washed ~ 7.5 o'clock stop washing.
4. preparation method according to claim 1 is characterized in that, drying described in the step (5) is dry in drying machine, and be 10h ~ 24h time of drying, and drying temperature is 100 ℃ ~ 120 ℃.
5. preparation method according to claim 4 is characterized in that, described drying machine is rotary drier.
6. preparation method according to claim 1 is characterized in that, the potassium fluoborate transferred product that step (5) makes is pulverized to pulverizer, makes Powdered potassium fluoborate product.
7. according to claim 1 or 6 described preparation methods, it is characterized in that the purity of described potassium fluoborate product is more than or equal to 99%.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104891517A (en) * | 2015-06-09 | 2015-09-09 | 天津金牛电源材料有限责任公司 | Method for producing potassium borofluoride by utilizing lithium hexafluorophosphate recovery acid mixture |
| CN105731482A (en) * | 2016-01-15 | 2016-07-06 | 江苏新泰材料科技股份有限公司 | Method for preparing potassium fluoborate from fluorine-containing wastewater |
| CN105819462A (en) * | 2016-03-16 | 2016-08-03 | 宜春金洋新材料股份有限公司 | Method of preparing fluoroboric acid from fluorine containing wastewater |
| CN107098356A (en) * | 2016-02-23 | 2017-08-29 | 达州励志环保科技有限公司 | A kind of preparation method of potassium fluoborate |
| CN107902665A (en) * | 2017-11-01 | 2018-04-13 | 江西省东沿药业有限公司 | A kind of fluorine method for treating waste liquid |
| CN108529631A (en) * | 2018-04-28 | 2018-09-14 | 惠晶显示科技（苏州）有限公司 | A kind of liquid crystal cell thinning industry waste slag treatment method |
| CN109354034A (en) * | 2018-11-22 | 2019-02-19 | 山东罗欣药业集团股份有限公司 | A kind of fluorine-containing waste liquid borofluoride exchange crystallization recovery technology of cephalo |
| CN109368652A (en) * | 2018-11-26 | 2019-02-22 | 江苏新泰材料科技有限公司 | A kind of method that tail gas absorption waste liquid prepares potassium fluoborate |
| CN110510625A (en) * | 2019-09-20 | 2019-11-29 | 四川师范大学 | The method and potassium fluoborate of the fluorine-containing aqueous slkali separation fluorine of bastnaesite and application |
| CN114262040A (en) * | 2021-11-30 | 2022-04-01 | 锦洋高新材料股份有限公司 | Method for preparing potassium fluoborate by using fluorine-containing wastewater |
| CN114436292A (en) * | 2022-02-21 | 2022-05-06 | 中船(邯郸)派瑞特种气体股份有限公司 | Treatment method of organic sylvite wastewater |
| CN117228681A (en) * | 2023-09-26 | 2023-12-15 | 衡阳市东氟新材料股份有限公司 | Preparation method of potassium fluoborate |
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| CN101462734A (en) * | 2008-03-12 | 2009-06-24 | 湖南有色氟化学有限责任公司 | Method for preparing potassium borofluoride from fluorine-containing potassium chloride |
| CN102275947A (en) * | 2011-05-30 | 2011-12-14 | 天津金牛电源材料有限责任公司 | Method for preparing potassium fluoborate by using mixed acid containing hydrogen fluoride |
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| CN101462734A (en) * | 2008-03-12 | 2009-06-24 | 湖南有色氟化学有限责任公司 | Method for preparing potassium borofluoride from fluorine-containing potassium chloride |
| CN102275947A (en) * | 2011-05-30 | 2011-12-14 | 天津金牛电源材料有限责任公司 | Method for preparing potassium fluoborate by using mixed acid containing hydrogen fluoride |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104891517A (en) * | 2015-06-09 | 2015-09-09 | 天津金牛电源材料有限责任公司 | Method for producing potassium borofluoride by utilizing lithium hexafluorophosphate recovery acid mixture |
| CN105731482A (en) * | 2016-01-15 | 2016-07-06 | 江苏新泰材料科技股份有限公司 | Method for preparing potassium fluoborate from fluorine-containing wastewater |
| CN107098356A (en) * | 2016-02-23 | 2017-08-29 | 达州励志环保科技有限公司 | A kind of preparation method of potassium fluoborate |
| CN105819462A (en) * | 2016-03-16 | 2016-08-03 | 宜春金洋新材料股份有限公司 | Method of preparing fluoroboric acid from fluorine containing wastewater |
| CN107902665A (en) * | 2017-11-01 | 2018-04-13 | 江西省东沿药业有限公司 | A kind of fluorine method for treating waste liquid |
| CN108529631A (en) * | 2018-04-28 | 2018-09-14 | 惠晶显示科技（苏州）有限公司 | A kind of liquid crystal cell thinning industry waste slag treatment method |
| CN109354034A (en) * | 2018-11-22 | 2019-02-19 | 山东罗欣药业集团股份有限公司 | A kind of fluorine-containing waste liquid borofluoride exchange crystallization recovery technology of cephalo |
| CN109368652A (en) * | 2018-11-26 | 2019-02-22 | 江苏新泰材料科技有限公司 | A kind of method that tail gas absorption waste liquid prepares potassium fluoborate |
| CN110510625A (en) * | 2019-09-20 | 2019-11-29 | 四川师范大学 | The method and potassium fluoborate of the fluorine-containing aqueous slkali separation fluorine of bastnaesite and application |
| CN110510625B (en) * | 2019-09-20 | 2022-11-01 | 四川师范大学 | Method for separating fluorine from bastnaesite fluorine-containing alkali solution, potassium fluoborate and application |
| CN114262040A (en) * | 2021-11-30 | 2022-04-01 | 锦洋高新材料股份有限公司 | Method for preparing potassium fluoborate by using fluorine-containing wastewater |
| CN114436292A (en) * | 2022-02-21 | 2022-05-06 | 中船(邯郸)派瑞特种气体股份有限公司 | Treatment method of organic sylvite wastewater |
| CN117228681A (en) * | 2023-09-26 | 2023-12-15 | 衡阳市东氟新材料股份有限公司 | Preparation method of potassium fluoborate |
| CN117228681B (en) * | 2023-09-26 | 2024-02-23 | 衡阳市东氟新材料股份有限公司 | Preparation method of potassium fluoborate |
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Address after: 215600 Suzhou, Jiangsu Yangtze River International Chemical Industrial Park on the eastern side of the Yangtze River Road on the south side of the Yellow Sea Patentee after: Morita new energy materials (Zhangjiagang) Co., Ltd. Address before: 215600 Suzhou, Jiangsu Yangtze River International Chemical Industrial Park on the eastern side of the Yangtze River Road on the south side of the Yellow Sea Patentee before: Sentian Chemical Industry (Zhangjiagang) Co., Ltd. |