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
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- 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
- 239000002253 acid Substances 0.000 title claims abstract description 41
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000011435 rock Substances 0.000 title claims description 29
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims description 28
- 229910052700 potassium Inorganic materials 0.000 title claims description 28
- 239000011591 potassium Substances 0.000 title claims description 28
- 239000012535 impurity Substances 0.000 claims abstract description 16
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 15
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- -1 potassium fluoroborate Chemical compound 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000007670 refining Methods 0.000 claims abstract description 8
- 239000002674 ointment Substances 0.000 claims abstract description 6
- 230000002194 synthesizing effect Effects 0.000 claims abstract 2
- 239000007788 liquid Substances 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 14
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000011775 sodium fluoride Substances 0.000 claims description 3
- 235000013024 sodium fluoride Nutrition 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000002386 leaching Methods 0.000 abstract description 9
- 229910021538 borax Inorganic materials 0.000 abstract description 6
- 239000004328 sodium tetraborate Substances 0.000 abstract description 6
- 235000010339 sodium tetraborate Nutrition 0.000 abstract description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 abstract description 5
- 239000004327 boric acid Substances 0.000 abstract description 5
- 239000010436 fluorite Substances 0.000 abstract description 5
- 229910001506 inorganic fluoride Inorganic materials 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 235000011164 potassium chloride Nutrition 0.000 abstract 2
- 239000001103 potassium chloride Substances 0.000 abstract 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 description 1
- 229910000521 B alloy Inorganic materials 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 229910001051 Magnalium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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 |
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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 | Compound potassium chloroborate nonlinear optical crystal, preparation method and use |
| 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 | Method for separating fluorine from fluorine-containing alkali solution of bastnaesite, potassium fluoroborate 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 | Compound potassium chloroborate nonlinear optical crystal, preparation method and use |
| 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 | Method for separating fluorine from fluorine-containing alkali solution of bastnaesite, potassium fluoroborate 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 |
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Open date: 20090506 |