CN101423224A - Potassium borofluoride preparation method based on fluosilicic acid and boron rock - Google Patents
Potassium borofluoride preparation method based on fluosilicic acid and boron rock Download PDFInfo
- Publication number
- CN101423224A CN101423224A CNA2008101437509A CN200810143750A CN101423224A CN 101423224 A CN101423224 A CN 101423224A CN A2008101437509 A CNA2008101437509 A CN A2008101437509A CN 200810143750 A CN200810143750 A CN 200810143750A CN 101423224 A CN101423224 A CN 101423224A
- Authority
- CN
- China
- Prior art keywords
- potassium
- preparation
- silicofluoric acid
- boron rock
- boron
- 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.)
- Pending
Links
Landscapes
- Removal Of Specific Substances (AREA)
Abstract
The invention relates to a preparation method of potassium fluoroborate based on fluosilicic acid and boron ore. The leaching of the boron ore is carried out by using the fluosilicic acid, a potassium fluoroborate product is synthesized by filtering, removing impurities and refining; the steps are as follows: I the fluosilicic acid and the boron ore are selected to produce leaching solution; II the leaching solution is filtered, the residues are removed and filtrate is remained; III an N-type impurity removal agent is added in the filtrate to remove the impurities, the impurities are removed by filtration and refining solution is remained; IV potassium chloride is added in the refining solution to carry out synthesis reaction; V the solution is filtered to obtain a potassium fluoroborate ointment; and VI the potassium fluoroborate ointment is dried to obtain the product. The prepration method adopts the technical proposal of: leaching the boron ore from the fluosilicic acid, filtering, removing the impurities, refining and finally synthesizing the potassium fluoroborate product by using the refining solution and the potassium chloride solution, thereby overcoming the shortcomings that the traditional production process of the potassium fluoroborate uses the non-renewable strategic reserve-fluorspar, borax and boric acid are in short supply, the price is higher, the production cost of the traditional production process is high, and the like. The preparation method is applicable for preparing prepare inorganic fluoride and especially applicable for preparing the potassium fluoroborate by using the fluosilicic acid and the boron ore.
Description
Technical field
The present invention relates to the preparation of inorganic fluoride, relate in particular to potassium borofluoride preparation method based on silicofluoric acid and boron rock.
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.The preparation of traditional processing technology hydrofluoric acid will be used non-renewable strategic reserves thing-fluorite, and the borax boric acid also source of goods is in short supply, and is on the high side, traditional processing technology production cost height.Silicofluoric acid is mainly the by product of phosphate fertilizer and hydrogen fluoride production process, and is cheap and easy to get, and China Liaoning and area, Qinghai-Tibet boron resource are also very abundant.
Summary of the invention
At above-mentioned situation, the purpose of this invention is to provide a kind of potassium borofluoride preparation method based on silicofluoric acid and boron rock, this method is simple, the convenience, with low cost of drawing materials of technology both, can alleviate borax boric acid situation in short supply again, has also saved fluorite resource simultaneously.
For achieving the above object, based on the potassium borofluoride preparation method of silicofluoric acid and boron rock, it leaches boron rock with silicofluoric acid earlier, more after filtration, removal of impurities, refining, the step with refined liquid and the synthetic potassium fluoborate product of Klorvess Liquid is at last:
I, choose silicofluoric acid, boron rock and make leach liquor, standby;
II, above-mentioned leach liquor is filtered, reserved filtrate removes slag;
Add N type cleaner in III, the above-mentioned filtrate and carry out removal of impurities, filter decon and stay refined liquid;
Add Repone K in IV, the above-mentioned refined liquid and carry out building-up reactions;
V, filtering solution obtain potassium fluoroborate ointment;
VI, potassium fluoroborate ointment drying obtain product.
For achieving the above object, its further step is:
Boron rock is trioxygen-containingization two boron (B
2O
3) 15%-50%.
B in the boron rock
2O
3With the silicofluoric acid mol ratio be 1: 0.6-1.5.
Silicofluoric acid concentration is 8%-30%.
Extraction temperature is 55 ℃-95 ℃ among the step I.
Temperature of reaction is 40 ℃-95 ℃ among the step IV.
N type cleaner is a kind of in Sodium Fluoride or yellow soda ash or sodium-chlor or the sodium sulfate or their combination.
The present invention adopts from silicofluoric acid and leaches boron rock, again after filtration, removal of impurities, refining, at last with the technical scheme of the synthetic potassium fluoborate product of refined liquid and Klorvess Liquid, it has overcome in the potassium fluoborate traditional processing technology must the non-renewable strategic reserves thing-fluorite of use, and borax, the boric acid source of goods are in short supply, on the high side, defectives such as traditional processing technology production cost height.
The beneficial effect that the present invention is produced compared to existing technology:
I, utilize silicofluoric acid and boron rock to prepare potassium fluoborate, easily realize suitability for industrialized production;
II, can reduce the potassium fluoborate production cost;
III, can save fluorite resource, alleviate the situation in short supply of borax, boric acid, both have good economic benefit, have good social benefit again.
The present invention is fit to the preparation of inorganic fluoride, is particularly suitable for the preparation with the potassium fluoborate of silicofluoric acid and boron rock.
The present invention is described in further detail below in conjunction with embodiment.
Embodiment
Embodiment 1: add silicofluoric acid 6.2m at leaching vat
3, concentration is 10%, boron rock (B
2O
315%) presses B
2O
3With the silicofluoric acid mol ratio is to add at 1: 0.8; 95 ℃ were leached 180 minutes, filtered, and filtrate adds N type cleaner 300kg removal of impurities 60 minutes, filter refined liquid, refined liquid and 2.5m
3Synthetic 80 minutes of Klorvess Liquid (200g/l), 70 ℃ of temperature of reaction refilter, wash, separate, dry potassium fluoborate product 385kg.
Embodiment 2: add silicofluoric acid 6.2m at leaching vat
3, concentration is 20%, boron rock (B
2O
310%) presses B
2O
3With the silicofluoric acid mol ratio is to add at 1: 1.2; 85 ℃ were leached 140 minutes, filtered, and filtrate adds N type cleaner 620kg removal of impurities 120 minutes, filter refined liquid, refined liquid and 4.8m
3Synthetic 90 minutes of Klorvess Liquid (220g/l), 40 ℃ of temperature of reaction refilter, wash, separate, dry potassium fluoborate product 950kg.
Embodiment 3: add silicofluoric acid 6.2m at leaching vat
3, concentration is 15%, boron rock (B
2O
340%) presses B
2O
3With the silicofluoric acid mol ratio is to add at 1: 0.6; 60 ℃ were leached 300 minutes, filtered, and filtrate adds N type cleaner 500kg removal of impurities 180 minutes, filter refined liquid, refined liquid and 3.0m
3Synthetic 150 minutes of Klorvess Liquid (250g/l), 85 ℃ of temperature of reaction refilter, wash, separate, dry potassium fluoborate product 770kg.
Embodiment 4: add silicofluoric acid 6.2m at leaching vat
3, concentration is 8%, boron rock (B
2O
330%) presses B
2O
3With the silicofluoric acid mol ratio is to add at 1: 1.2; 70 ℃ were leached 300 minutes, filtered, and filtrate adds N type cleaner 280kg removal of impurities 160 minutes, filter refined liquid, refined liquid and 2.2m
3Synthetic 150 minutes of Klorvess Liquid (200g/l), 80 ℃ of temperature of reaction refilter, wash, separate, dry potassium fluoborate product 480kg.
Embodiment 5: add silicofluoric acid 6.2m at leaching vat
3, concentration is 30%, boron rock (B
2O
320%) presses B
2O
3With the silicofluoric acid mol ratio is to add at 1: 1.5; 55 ℃ were leached 300 minutes, filtered, and filtrate adds N type cleaner 760kg removal of impurities 170 minutes, filter refined liquid, refined liquid and 7.5m
3Synthetic 150 minutes of Klorvess Liquid (200g/l), 95 ℃ of temperature of reaction refilter, wash, separate, dry potassium fluoborate product 1482kg.
N type cleaner is in the foregoing description: a kind of in Sodium Fluoride or yellow soda ash or sodium-chlor or the sodium sulfate or their combination.
Adopt preparation method of the present invention to 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:
Below only be preferred embodiment of the present invention, according to above-mentioned design of the present invention, those skilled in the art also can make various modifications and conversion to this.For example, leach liquor in silicofluoric acid and the boron rock, filtered liquid are added modification and the conversion that N type cleaner carries out removal of impurities reaction etc.Yet similar this conversion and modification all belong to essence of the present invention.
Claims (7)
1, based on the potassium borofluoride preparation method of silicofluoric acid and boron rock, it is characterized in that it earlier leaches boron rock with silicofluoric acid, more after filtration, and removal of impurities, refining, the step of synthesizing the potassium fluoborate product with refined liquid and Klorvess Liquid is at last:
I, choose silicofluoric acid, boron rock and make leach liquor, standby;
II, above-mentioned leach liquor is filtered, reserved filtrate removes slag;
Add N type cleaner in III, the above-mentioned filtrate and carry out removal of impurities, filter decon and stay refined liquid;
Add Repone K in IV, the above-mentioned refined liquid and carry out building-up reactions;
V, filtering solution obtain potassium fluoroborate ointment;
VI, potassium fluoroborate ointment drying obtain product.
2, the potassium borofluoride preparation method based on silicofluoric acid and boron rock according to claim 1 is characterized in that boron rock is trioxygen-containingization two boron (B
2O
3) 15%-50%.
3, the potassium borofluoride preparation method based on silicofluoric acid and boron rock according to claim 1 is characterized in that B in the boron rock
2O
3With the silicofluoric acid mol ratio be 1:0.6-1.5.
4, the potassium borofluoride preparation method based on silicofluoric acid and boron rock according to claim 1 is characterized in that silicofluoric acid concentration is 8%-30%.
5, the potassium borofluoride preparation method based on silicofluoric acid and boron rock according to claim 1 is characterized in that extraction temperature is 55 ℃-95 ℃ among the step I.
6, the potassium borofluoride preparation method based on silicofluoric acid and boron rock according to claim 1 is characterized in that temperature of reaction is 40 ℃-95 ℃ among the step IV.
7, the potassium borofluoride preparation method based on silicofluoric acid and boron rock according to claim 1 is characterized in that N type cleaner is a kind of in Sodium Fluoride or yellow soda ash or sodium-chlor or the sodium sulfate or their combination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101437509A CN101423224A (en) | 2008-11-28 | 2008-11-28 | Potassium borofluoride preparation method based on fluosilicic acid and boron rock |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101437509A CN101423224A (en) | 2008-11-28 | 2008-11-28 | Potassium borofluoride preparation method based on fluosilicic acid and boron rock |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101423224A true CN101423224A (en) | 2009-05-06 |
Family
ID=40614137
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101437509A Pending CN101423224A (en) | 2008-11-28 | 2008-11-28 | Potassium borofluoride preparation method based on fluosilicic acid and boron rock |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101423224A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914809A (en) * | 2010-08-11 | 2010-12-15 | 中国科学院新疆理化技术研究所 | Nonlinear optical crystal of potassium borate chloride compound and preparation method as well as application thereof |
| CN102874868A (en) * | 2012-11-02 | 2013-01-16 | 湖南有色湘乡氟化学有限公司 | Method for preparing potassium fluozirconate through fluosilicic acid |
| 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 |
| 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 |
| 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 |
-
2008
- 2008-11-28 CN CNA2008101437509A patent/CN101423224A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914809A (en) * | 2010-08-11 | 2010-12-15 | 中国科学院新疆理化技术研究所 | Nonlinear optical crystal of potassium borate chloride compound and preparation method as well as application thereof |
| CN101914809B (en) * | 2010-08-11 | 2014-03-12 | 中国科学院新疆理化技术研究所 | Nonlinear optical crystal of potassium borate chloride compound and preparation method as well as application thereof |
| CN102874868A (en) * | 2012-11-02 | 2013-01-16 | 湖南有色湘乡氟化学有限公司 | Method for preparing potassium fluozirconate through fluosilicic acid |
| 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 |
| 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 |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102718234B (en) | Method for extracting lithium carbonate from lepidolite | |
| CN106517256A (en) | Method for producing lithium hydroxide monohydrate from lithium carbonate | |
| CN103103358B (en) | Method for recovering metal by use of APT (ammonium paratungstate) waste slag | |
| CN103103349B (en) | Method for decomposing bayan obo rare earth ore concentrate by acid and alkali combination at low temperature | |
| CN101423224A (en) | Potassium borofluoride preparation method based on fluosilicic acid and boron rock | |
| CN102603000A (en) | Process for preparing high-purity vanadium pentoxide by adopting ammonium metavanadate as raw material | |
| CN101648702A (en) | Method for preparing tellurium dioxide by using crude tellurium as raw material | |
| CN102251106A (en) | Method for decomposing rare earth concentrate in Baotou by alkaline process | |
| CN103318959A (en) | Production method for sodium pyroantimonate by using high-temperature high-pressure pure-oxygen oxidation | |
| CN104591268B (en) | Utilize the method that excellent grade stannous chloride prepared by low stannum waste residue | |
| CN103319307B (en) | A kind of method preparing soda soap | |
| CN102586629A (en) | Recycling preparation method for producing titanium sponge and co-producing potassium cryolite with potassium fluotitanate as intermediate raw material | |
| CN103073031A (en) | Method for preparing lithium fluoride from phosphate fertilizer by-product sodium fluoride | |
| CN102586628A (en) | Cyclic co-production method of sponge titanium and sodium fluoroaluminate with sodium fluorotitanate as intermediate material | |
| CN106892443B (en) | Utilize the process of ion-exchange high purity lithium carbonate | |
| CN102633267A (en) | Preparation method of nano SiO2 | |
| CN101629250A (en) | Method for reclaiming soluble manganese from electrolytic metal manganese filter-press residues | |
| CN103757246A (en) | Method for producing high-purity gold | |
| CN104099479B (en) | A kind of using acid and alkali combination method produces the processing method of zinc compound | |
| CN102815680B (en) | Method for producing lithium phosphate by using lithium-containing waste liquid | |
| CN101602516A (en) | The preparation method of aluminum fluoride | |
| CN101475168B (en) | Method for washing active carbon | |
| CN110723747B (en) | Method for recovering and preparing high-quality zinc oxide from zinc waste | |
| EP2631216A1 (en) | Method for cyclically preparing boron and coproducing potassium cryolite using potassium fluoborate as intermediate material | |
| CN105883836A (en) | Co-production method of sodium metasilicate and sodium fluoride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20090506 |