CN103332700B - Method for preparing potassium borofluoride through fluorine-containing wastewater - Google Patents
Method for preparing potassium borofluoride through fluorine-containing wastewater Download PDFInfo
- Publication number
- CN103332700B CN103332700B CN201310310064.7A CN201310310064A CN103332700B CN 103332700 B CN103332700 B CN 103332700B CN 201310310064 A CN201310310064 A CN 201310310064A CN 103332700 B CN103332700 B CN 103332700B
- Authority
- CN
- China
- Prior art keywords
- potassium fluoborate
- potassium
- washing
- drying
- product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Removal Of Specific Substances (AREA)
- Processing Of Solid Wastes (AREA)
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 being prepared potassium fluoborate by fluoride waste.
Background technology
potassium fluoborate, molecular formula KBF
4
, molecular weight 125.90, relative density (d20) 2.498, fusing point 350 DEG C, white powder or colourless granules xln, be slightly soluble in water, ethanol, ether, be insoluble to alkaline solution, boron trifluoride can be decomposed into by strong acid, molten altogether with alkali-metal carbonate, generate fluorochemical and borate.
potassium fluoborate is used as analytical reagent and solubility promoter, also for the manufacture of boron trifluoride, aluminium and the mould material of magnesium casting, electrochemical engineering and chemical experiment.
the production of potassium fluoborate, traditional method adopts boric acid, hydrogen fluoride, potassium hydroxide as raw material, and the first step boric acid and hydrogen fluoride first react generation fluoroboric acid, second step again with potassium hydroxide neutralization reaction, generate potassium fluoborate, through filtration, washing, drying, obtain potassium fluoborate product.It is high to there is cost in the method for traditional mode of production potassium fluoborate, the problems such as complex process.
on the other hand, fluoride waste is as one of main waste water produced in Chemical Manufacture, and the pollution for environment is large.In addition, the compound price containing fluorine element is often higher.Therefore, fluoride waste is reclaimed the fluorochemical in waste water by enterprise usually simultaneously through wastewater processing technology process, to reach the object reducing environmental pollution and resource continuous utilization, but in prior art, the input sewage treatment equipment no matter any method of wastewater treatment all needs enterprise extra and manpower etc., and then greatly increase cost.
Summary of the invention
technical problem to be solved by this invention overcomes the deficiencies in the prior art, a kind of method being prepared potassium fluoborate by fluoride waste is provided, the fluoride waste produced when adopting enterprise to produce, Potassium monofluoride, borax are as raw material production potassium fluoborate, after filtration, washing, dry, obtain potassium fluoborate product.Appropriate application fluoride waste of the present invention prepares potassium fluoborate, for the Sustainable development reducing environmental pollution, reduce production cost, promote enterprise, is all of great significance.
for solving above technical problem, the present invention takes following technical scheme:
prepared a method for potassium fluoborate by fluoride waste, comprise the following steps:
(1) hydrogen fluoride content in fluoride waste described in water use regulation, until described hydrofluoric mass content is 12% ~ 17%, wherein, described fluoride waste is the fluoride waste producing lithium hexafluoro phosphate generation;
(2) be that 3 ~ 5:1 fully mixes in mass ratio by the waste water processed through step (1) and saturated potassium chloride solution, make to carry out fluoridation, the described fluoridation time is 20min ~ 40min;
(3) borax is mixed for 1:3 ~ 5 in mass ratio with the waste water processed through step (1), stir, described borax is dissolved completely;
(4) by the solution of the solution of step (2) and step (3) be 0.8 ~ 1.2:1 mixing in mass ratio, stirring reaction, the reaction times controls at 1.5h ~ 3h, and temperature of reaction controls at 80 DEG C ~ 100 DEG C, potassium fluoborate is constantly had to separate out in reaction process, obtained potassium fluoborate suspension liquid;
(5) by potassium fluoborate suspension liquid in step (4) through solid-liquid separation, washing, drying, obtained potassium fluoborate product.
according to the present invention, the hydrofluoric mass content that basic composition is of fluoride waste described in step (1) is 18% ~ 25%, and the mass content of hydrogenchloride is 18% ~ 25%.
preferably, described in step (5), washing carries out centrifuge washing with water in centrifuges, when pH=6.5 ~ 7.5 of the water outlet of washing, stops washing.
preferably, drying described in step (5) is dry in drying machine, and time of drying is 10h ~ 24h, and drying temperature is 100 DEG C ~ 120 DEG C.
particularly, described drying machine is rotary drier.
preferably, the potassium fluoborate transferred product that step (5) is obtained is pulverized to pulverizer, obtained Powdered potassium fluoborate product.
preferably, the purity of described potassium fluoborate product is more than or equal to 99%.
due to the enforcement of technique scheme, the present invention compared with prior art tool has the following advantages:
the present invention prepares potassium fluoborate, various abundant raw material source with fluoride waste, Repone K, borax for raw material, and raw material is easy to get and cheap, technological process is simple, operation controls simple and convenient, and production efficiency is high, and reactivity, product yield are high, good product quality, and significantly reduce the pollution of environment, reduce production cost, final obtained potassium fluoborate product purity can reach more than 99%, other metals and nonmetal index all control in the reasonable scope, meet the needs of customers.Therefore, the present invention has good economic worth and social value.
Embodiment
below in conjunction with specific embodiment, the present invention will be further described in detail:
embodiment 1
the present embodiment is to produce the fluoride waste of lithium hexafluoro phosphate generation for raw material in Chemical Manufacture, 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 that fluoride waste prepares the method for potassium fluoborate are as follows:
(1) hydrofluoric content in water use regulation fluoride waste, until hydrofluoric mass content is roughly 15%, in actually operating, uses carbon steel liner PE material basin as wastewater regulation tank usually;
(2) first prepare saturated potassium chloride solution, then fully mixed for 1:4 in mass ratio with the waste water processed through step (1) by saturated potassium chloride solution, make to carry out fluoridation, the fluoridation time is 30min;
(3) by solid borax with the waste water processed through step (1) in mass ratio for 1:3 mixes, stir, borax is dissolved completely;
(4) by the solution of the solution of step (2) and step (3) be 1:1 mixing in mass ratio, stirring reaction, the reaction times controls at 2h, and temperature of reaction controls at 80 DEG C ~ 100 DEG C, constantly has potassium fluoborate to separate out in reaction process, obtains potassium fluoborate suspension liquid;
(5) use whizzer through solid-liquid separation potassium fluoborate suspension liquid in step (4), after being separated, the solid of gained carries out centrifuge washing with water in centrifuges, until pH=6.5 ~ 7.5 of water outlet after washing, then by solid transfer dry 12h to rotary drier of gained after washing, drying temperature is 110 DEG C, obtained block potassium fluoborate product;
(6) pulverize in block potassium fluoborate transferred product to disintegrating machine obtained in step (5), obtained Powdered potassium fluoborate product, product purity reaches 99%.
result shows, the above-mentioned fluoride waste of process 1t, 200kg potassium fluoborate product can be produced, required cost is roughly 2000 yuan, compares the cost (cost is roughly 5000 yuan) of the above-mentioned fluoride waste of process 1t and use produced in conventional processes 200kg potassium fluoborate product (cost is roughly 3000 yuan) is low by 33.3% nearly.
embodiment 2
the present embodiment is to produce the fluoride waste of lithium hexafluoro phosphate generation for raw material in Chemical Manufacture, 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 that fluoride waste prepares the method for potassium fluoborate are as follows:
(1) hydrofluoric content in water use regulation fluoride waste, until hydrofluoric mass content is roughly 12%, in actually operating, uses carbon steel liner PE material basin as wastewater regulation tank usually;
(2) first prepare saturated potassium chloride solution, then fully mixed for 1:5 in mass ratio with the waste water processed through step (1) by saturated potassium chloride solution, make to carry out fluoridation, the time of fluoridizing is 40min;
(3) by solid borax with the waste water processed through step (1) in mass ratio for 1:4 mixes, stir, borax is dissolved completely;
(4) by the solution of the solution of step (2) and step (3) be 1.2:1 mixing in mass ratio, stirring reaction, the reaction times controls at 3h, and temperature of reaction controls at 80 DEG C ~ 100 DEG C, constantly has potassium fluoborate to separate out in reaction process, obtains potassium fluoborate suspension liquid;
(5) use whizzer through solid-liquid separation potassium fluoborate suspension liquid in step (4), after being separated, the solid of gained carries out centrifuge washing with water in centrifuges, until pH=6.5 ~ 7.5 of water outlet after washing, then by solid transfer dry 20h to rotary drier of gained after washing, drying temperature is 120 DEG C, obtained block potassium fluoborate product;
(6) pulverize in block potassium fluoborate transferred product to disintegrating machine obtained in step (5), obtained Powdered potassium fluoborate product, product purity reaches 99%.
result shows, the above-mentioned fluoride waste of process 1t, 150kg potassium fluoborate product can be produced, required cost is roughly 1500 yuan, compares the cost (cost is roughly 4000 yuan) of the above-mentioned fluoride waste of process 1t and use produced in conventional processes 150kg potassium fluoborate product (cost is roughly 2250 yuan) is low by 33.3% nearly.
to sum up, preparation method of the present invention compared with prior art, has following advantage:
1, compare traditional technology, reaction raw materials is easy to get, with low cost, reacts simple to operation, safety, environmental protection, simultaneously the reasonable fluoride waste produced of process chemical workshop, and remarkable in economical benefits, also protects environment greatly.
2, the present invention's fluoride waste used regulates the main raw of equipment used to be carbon steel liner PE material, and stainless steel of comparing, steel lining tetrafluoro, Hastelloy have very large cost advantage.
above to invention has been detailed description; its object is to allow the personage being familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; and the invention is not restricted to the embodiments described; the equivalence change that all spirit according to the present invention are done or modification, all should be encompassed within protection scope of the present invention.
Claims (6)
1. prepared a method for potassium fluoborate by fluoride waste, it is characterized in that, comprise the following steps:
(1) hydrogen fluoride content in fluoride waste described in water use regulation, until described hydrofluoric mass content is 12% ~ 17%, wherein, described fluoride waste is the fluoride waste producing lithium hexafluoro phosphate generation;
(2) be that 3 ~ 5:1 fully mixes in mass ratio by the waste water processed through step (1) and saturated potassium chloride solution, make to carry out fluoridation, the described fluoridation time is 20min ~ 40min;
(3) borax is mixed for 1:3 ~ 5 in mass ratio with the waste water processed through step (1), stir, described borax is dissolved completely;
(4) by the solution of the solution of step (2) and step (3) be 0.8 ~ 1.2:1 mixing in mass ratio, stirring reaction, the reaction times controls at 1.5h ~ 3h, and temperature of reaction controls at 80 DEG C ~ 100 DEG C, potassium fluoborate is constantly had to separate out in reaction process, obtained potassium fluoborate suspension liquid;
(5) by potassium fluoborate suspension liquid in step (4) through solid-liquid separation, washing, drying, obtained potassium fluoborate product, the purity of described potassium fluoborate product is more than or equal to 99%.
2. preparation method according to claim 1, is characterized in that, in fluoride waste described in step (1), hydrofluoric mass content is 18% ~ 25%, and the mass content of hydrogenchloride is 18% ~ 25%.
3. preparation method according to claim 1, is characterized in that, described in step (5), washing carries out centrifuge washing with water in centrifuges, when pH=6.5 ~ 7.5 of the water outlet of washing, stops washing.
4. preparation method according to claim 1, is characterized in that, drying described in step (5) is dry in drying machine, and time of drying is 10h ~ 24h, and drying temperature is 100 DEG C ~ 120 DEG C.
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) is obtained is pulverized to pulverizer, obtained Powdered potassium fluoborate product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310310064.7A CN103332700B (en) | 2013-07-23 | 2013-07-23 | Method for preparing potassium borofluoride through fluorine-containing wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310310064.7A CN103332700B (en) | 2013-07-23 | 2013-07-23 | Method for preparing potassium borofluoride through fluorine-containing wastewater |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103332700A CN103332700A (en) | 2013-10-02 |
| CN103332700B true CN103332700B (en) | 2015-02-04 |
Family
ID=49240929
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310310064.7A Active CN103332700B (en) | 2013-07-23 | 2013-07-23 | Method for preparing potassium borofluoride through fluorine-containing wastewater |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103332700B (en) |
Families Citing this family (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 |
| 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 |
| CN105819462B (en) * | 2016-03-16 | 2017-04-12 | 宜春金洋新材料股份有限公司 | Method of preparing fluoroboric acid from fluorine containing wastewater |
| CN107902665B (en) * | 2017-11-01 | 2020-04-14 | 江西省东沿药业有限公司 | Fluorine waste liquid treatment method |
| 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 |
| 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 |
| CN114436292B (en) * | 2022-02-21 | 2023-04-28 | 中船(邯郸)派瑞特种气体股份有限公司 | Treatment method of organic potassium salt wastewater |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2013
- 2013-07-23 CN CN201310310064.7A patent/CN103332700B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103332700A (en) | 2013-10-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103332700B (en) | Method for preparing potassium borofluoride through fluorine-containing wastewater | |
| CN102001686B (en) | Process for producing potassium fluoride and white carbon black by decomposing potassium feldspar with fluorine-containing acid at low temperature | |
| CN104925837A (en) | Method of preparing lithium salt by recovering lithium deposition mother liquor of battery grade lithium carbonate | |
| CN102383179B (en) | A kind of method that industrial waste acid and phosphogypsum fully utilize | |
| CN108923092A (en) | A kind of waste and old lithium ionic cell electrolyte processing method | |
| CN102351160A (en) | Method for preparing battery grade lithium dihydrogen phosphate with high-purity lithium carbonate lithium depositing mother solution | |
| CN102515203B (en) | Processing method of wastes produced when battery grade lithium fluoride is manufactured by adopting carbonization method | |
| CN104495889B (en) | The method of a kind of industrial microwave process potassium bearing rock | |
| CN104030332A (en) | Method for reclaiming cryolite from fluorine containing pesticide industrial waste residues | |
| CN102060461B (en) | Cement composite grinding aid and preparation method thereof | |
| CN102211782B (en) | Treatment method for producing sodium silicofluoride as byproduct in inorganic fluoride production process | |
| CN102001688B (en) | Process for producing potassium sulfate by decomposing potassium feldspar at low temperature with fluorine-containing acid | |
| CN103073031B (en) | Method for preparing lithium fluoride from phosphate fertilizer by-product sodium fluoride | |
| CN104445281B (en) | Trichlorosilane elution circuit waste residue method of comprehensive utilization | |
| CN102001691B (en) | Process for producing potassium nitrate by decomposing potassium feldspar at low temperature through fluorine-contained acid | |
| CN103923379A (en) | Method for preparing fire retardation polymer composite material by using boron mud | |
| CN102249256A (en) | Process for preparing boron trifluoride gas | |
| CN103303974A (en) | Method for recycling waste silicon slag discharged in production of zirconyl chloride | |
| CN106881062A (en) | A kind of preparation method of the magnesium hydroxide-flyash built agent for processing fluoride waste | |
| CN203976418U (en) | A kind ofly take Repone K, Sweet natural gas and realize the production system of comprehensive utilization of resources as raw material | |
| CN102874855A (en) | Lithium-containing sodium cryolite and preparation method thereof | |
| CN103936041B (en) | A kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid | |
| CN107337228A (en) | A kind of Aluminiferous waste slag integrated treatment recovery method | |
| CN104446598B (en) | A kind of fire-retardant fireproof insulation material based on boron mud and preparation method thereof | |
| CN104017998B (en) | A kind of manganese slag for comprehensive Application way |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
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. |