CN103058224A - Method for recycling fluorine-producing ammonium fluoride in wet-process phosphoric acid tail gas - Google Patents
Method for recycling fluorine-producing ammonium fluoride in wet-process phosphoric acid tail gas Download PDFInfo
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- CN103058224A CN103058224A CN2013100097356A CN201310009735A CN103058224A CN 103058224 A CN103058224 A CN 103058224A CN 2013100097356 A CN2013100097356 A CN 2013100097356A CN 201310009735 A CN201310009735 A CN 201310009735A CN 103058224 A CN103058224 A CN 103058224A
- Authority
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- China
- Prior art keywords
- ammonium fluoride
- liquid
- phosphoric acid
- tail gas
- fluorine
- 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.)
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- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 title claims abstract description 85
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 64
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 34
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 24
- 239000011737 fluorine Substances 0.000 title claims abstract description 24
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title abstract description 23
- 238000004064 recycling Methods 0.000 title abstract 3
- 238000002425 crystallisation Methods 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000006229 carbon black Substances 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000010521 absorption reaction Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000012452 mother liquor Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000005915 ammonolysis reaction Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 27
- 235000019241 carbon black Nutrition 0.000 description 13
- 238000005406 washing Methods 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 3
- 229940070337 ammonium silicofluoride Drugs 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- 239000002367 phosphate rock Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 229940053652 fluorinse Drugs 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for recycling fluorine-producing ammonium fluoride in wet-process phosphoric acid tail gas. The method comprises the following steps of: (1) fluosilicic acid liquid production through absorbing: using an ammonium fluoride absorption liquid to circularly wash and absorb fluorine-containing gas; (2) ammonium fluoride production through ammonolysis reaction: filling ammonia into the produced fluosilicic acid liquid until the pH value is between 8.5 and 10.5, precipitating white carbon black out, filtering to obtain solid white carbon black and the ammonium fluoride liquid, and returning the required amount of the ammonium fluoride liquid to wet-process phosphoric acid tail gas; (3) concentrating: mixing the residual ammonium fluoride liquid and mother liquid after the ammonium fluoride crystallization, and concentrating until the mass concentration of the ammonium fluoride is between 55-85%; and (4) crystallization and separation: delivering the ammonium fluoride liquid with the mass concentration of 55-85% to a cooling crystallizer to cool and crystallize, thus obtaining a solid-liquid ammonium fluoride mixture, filtering the solid-liquid ammonium fluoride mixture to obtain ammonium fluoride crystals, and returning the mother liquid to be concentrated. After the method is adopted, the recycling rate of the fluorine-containing gas is greatly increased, and a good effect is obtained.
Description
Technical field
The present invention relates to Neutral ammonium fluoride, reclaim specifically the method that fluorine is produced ammonium fluoride in the phosphoric acid by wet process tail gas.
Background technology
Producing a large amount of fluoro-gas of generation in the process phosphoric acid with Rock Phosphate (72Min BPL), present modal method is that water absorbs the generation silicofluoric acid, silicofluoric acid is produced other products again, reclaims fluorine resource associated with phosphate rock.
Reclaiming at present fluorine resource associated with phosphate rock produces the ammonium fluoride method and has: the application of application number 200710066136.2, and carry out substep aminating reaction, filtration, washing, drying take silicofluoric acid and ammoniacal liquor as raw material and make white carbon black and high density ammonium fluoride mother liquor.Application number is 201010183204.5 application, at-5 ~ 30 ℃, adds simultaneously silicofluoric acid and ammoniacal liquor in the reactor, control pH value successive reaction, obtain white carbon black filter cake and ammonium fluoride solution, the white carbon black filter cake is through washing dried white carbon black product, and filtrate is ammonium fluoride solution.
Above-mentioned technology is take phosphoric acid by wet process by-product fluosilicic acid and ammoniacal liquor as raw material, and the Wet-process Phosphoric Acid Production process water absorbs fluoro-gas, and to produce the yield of silicofluoric acid own not high, also has in a large number fluorine-containing (20 ~ 50%) not reclaim, and resource does not take full advantage of.It is low to produce simultaneously filtrate ammonium fluoride concentration, and energy consumption is high in concentration process.
201210110205.6 number application be under 95 ~ 108 ℃ of conditions, to dissolve fluorine-containing white residue with 18 ~ 25% ammonium fluoride solution, make white carbon black 30 ~ 50 ℃ of aminating reactions, filtration, washing, dryings, the ammonium fluoride mother liquor makes the ammonium fluoride crystal through concentrated, crystallization, separation.This technology is dissolved fluorine-containing white residue at comparatively high temps, the lesser temps aminating reaction, and product process is long, and energy consumption is high, and it is low to produce simultaneously filtrate ammonium fluoride concentration, and energy consumption is high in concentration process.
Summary of the invention
The object of the invention is to overcome above-mentioned shortcoming and a kind of energy consumption that can improve ammonium fluoride concentration, reduce concentration process is provided, can reclaims the method that fluoro-gas is produced ammonium fluoride in the phosphoric acid by wet process tail gas.
Technical scheme of the present invention is: a kind of method that reclaims fluorine production ammonium fluoride in the phosphoric acid by wet process tail gas, and it comprises following steps:
(1) absorbs and to produce the silicofluoric acid ammonia solution: be that 15%～50% absorption liquid carries out the fluoro-gas in the circulation cleaning absorption phosphoric acid by wet process tail gas with the Neutral ammonium fluoride massfraction;
In the recovery method of fluorine, temperature is controlled at 20～60 ℃ during gas absorption process in the above-mentioned phosphoric acid by wet process tail gas.
Above-mentioned total reaction equation is as follows:
2mNH
4F +2nHF+（m+n）SiF
4 = m(NH
4)
2SiF
6+nH
2SiF
6
According to phosphoric acid by wet process tail gas fluorine content in flow and the tail gas per hour, the ammonium fluoride consumption is theoretical consumption 0.8-2 times, obtain transparent silicate fluoride solution by continuous blow-down (it is constant to keep the circulation cleaning liquid measure) or intermittently washing after the flow proportional interpolation washing (discharging after once adding relatively large Fluorinse circulation cleaning certain hour, at interpolation Fluorinse circulation cleaning).
(2) aminating reaction is produced ammonium fluoride: make silicate fluoride solution and pass into ammonia to pH value 8.5-10.5, the Precipitation white carbon black, filtration obtains the white carbon black solid and mass concentration is 15-50% ammonium fluoride solution, and this ammonium fluoride solution is by returning with phosphoric acid by wet process tail gas aequum.
(3) concentrated: remaining ammonium fluoride solution mixes with mother liquor after the ammonium fluoride crystallization, enter in the concentrating unit ,-0.015 ~-concentrate under the 0.06MPa pressure, until the mass concentration 55-85% of ammonium fluoride;
(4) crystallization and separation: be that 55-85% ammonium fluoride solution is delivered to the cooling crystallizer crystallisation by cooling with mass concentration, separate out the ammonium fluoride crystal, obtain the ammonium fluoride solidliquid mixture, its filtering separation is got the ammonium fluoride crystal, mother liquor returns concentrated, and so circulation realizes the ammonium fluoride crystallisation process.
The invention has the beneficial effects as follows: after adopting the inventive method, greatly improved the recovery utilization rate of fluoro-gas in the phosphoric acid by wet process tail gas, made in the phosphoric acid tail gas fluorine content from 10.5g/m
3More than be reduced to 0.05g/m
3, reach the emission standard of fluorine content in the Wet-process Phosphoric Acid Production tail gas; Improve simultaneously phosphoric acid by wet process associated fluorine resource utilization ratio, make and adopt traditional fluorine recovery method Wet Phosphoric Acid Plant associated fluorine resource fluorine rate of recovery to bring up to more than 70% from about 40%.
Embodiment
Below by embodiment, further specify beneficial effect of the present invention.
Certain factory adopts method of the present invention, and implementation is as follows:
Embodiment 1
A kind of method that reclaims fluorine production ammonium fluoride in the phosphoric acid by wet process tail gas comprises following steps:
(1) with massfraction is first 20% Neutral ammonium fluoride absorbent solution; To squeeze into phosphoric acid by wet process tail cleaning device with pump again and carry out through the four-stage counter-current circulation cleaning, absorb the fluoro-gas in the wet-process phosphoric acid reaction flue gas, absorption temperature will be controlled at 50 ~ 55 ℃.Making ammonium fluosilicate solution and continuous blow-down ammonium silicofluoride storage tank stores.
(2) pass into ammonia to pH value 9.5 Precipitation white carbon blacks, filtration obtains the white carbon black solid and mass concentration is 20% ammonium fluoride solution, and this ammonium fluoride solution is by returning with phosphoric acid by wet process tail gas aequum.
(3) concentrated: remaining ammonium fluoride solution mixes with mother liquor after the ammonium fluoride crystallization, enters in the concentrating unit, concentrates under-0.03MPa pressure, until the mass concentration 65% of ammonium fluoride.
(4) crystallization and separation: be that 65% ammonium fluoride solution is delivered to cooling crystallizer with mass concentration, crystallisation by cooling 3 hours is separated out the ammonium fluoride crystal, obtain the ammonium fluoride solidliquid mixture, its filtering separation is got the ammonium fluoride crystal, and mother liquor returns concentrated, and so circulation realizes the ammonium fluoride crystallisation process.
Embodiment 2
A kind of method that reclaims fluorine production ammonium fluoride in the phosphoric acid by wet process tail gas comprises following steps:
(1) with massfraction is first 30% Neutral ammonium fluoride absorbent solution; To squeeze into phosphoric acid by wet process tail cleaning device with pump again and carry out through the four-stage counter-current circulation cleaning, absorb the fluoro-gas in the wet-process phosphoric acid reaction flue gas, absorption temperature will be controlled at 40 ~ 45 ℃.Making ammonium fluosilicate solution and continuous blow-down ammonium silicofluoride storage tank stores.
(2) pass into ammonia to pH value 9.0 Precipitation white carbon blacks, filtration obtains the white carbon black solid and mass concentration is 30% ammonium fluoride solution, and this ammonium fluoride solution is by returning with phosphoric acid by wet process tail gas aequum.
(3) concentrated: remaining ammonium fluoride solution mixes with mother liquor after the ammonium fluoride crystallization, enters in the concentrating unit, concentrates under-0.05MPa pressure, until the mass concentration 70% of ammonium fluoride.
(4) crystallization and separation: be that 70% ammonium fluoride solution is delivered to cooling crystallizer with mass concentration, crystallisation by cooling 5 hours is separated out the ammonium fluoride crystal, obtain the ammonium fluoride solidliquid mixture, its filtering separation is got the ammonium fluoride crystal, and mother liquor returns concentrated, and so circulation realizes the ammonium fluoride crystallisation process.
Embodiment 3
A kind of method that reclaims fluorine production ammonium fluoride in the phosphoric acid by wet process tail gas comprises following steps:
(1) with massfraction is first 40% Neutral ammonium fluoride absorbent solution; To squeeze into phosphoric acid by wet process tail cleaning device with pump again and carry out through the four-stage counter-current circulation cleaning, absorb the fluoro-gas in the wet-process phosphoric acid reaction flue gas, absorption temperature will be controlled at 45 ~ 50 ℃.Making ammonium fluosilicate solution and continuous blow-down ammonium silicofluoride storage tank stores.
(2) pass into ammonia to pH value 10.0 Precipitation white carbon blacks, filtration obtains the white carbon black solid and mass concentration is 40% ammonium fluoride solution, and this ammonium fluoride solution is by returning with phosphoric acid by wet process tail gas aequum.
(3) concentrated: remaining ammonium fluoride solution mixes with mother liquor after the ammonium fluoride crystallization, enters in the concentrating unit, concentrates under-0.04MPa pressure, until the mass concentration 75% of ammonium fluoride.
(4) crystallization and separation: be that 75% ammonium fluoride solution is delivered to cooling crystallizer with mass concentration, crystallisation by cooling 4 hours is separated out the ammonium fluoride crystal, obtain the ammonium fluoride solidliquid mixture, its filtering separation is got the ammonium fluoride crystal, and mother liquor returns concentrated, and so circulation realizes the ammonium fluoride crystallisation process.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment does according to technical spirit of the present invention.
Claims (3)
1. one kind is reclaimed the method that fluorine is produced ammonium fluoride in the phosphoric acid by wet process tail gas, it is characterized in that it comprises following steps:
(1) absorbs and to produce the silicofluoric acid ammonia solution: be that 15%～50% absorption liquid carries out the fluoro-gas in the circulation cleaning absorption phosphoric acid by wet process tail gas with the Neutral ammonium fluoride massfraction; Temperature is controlled at 20～60 ℃ during described gas absorption process;
(2) aminating reaction is produced ammonium fluoride: make silicate fluoride solution and pass into ammonia to pH value 8.5-10.5, the Precipitation white carbon black, filtration obtains the white carbon black solid and mass concentration is 15-50% ammonium fluoride solution, and this ammonium fluoride solution is by returning with phosphoric acid by wet process tail gas aequum;
(3) concentrated: remaining ammonium fluoride solution mixes with mother liquor after the ammonium fluoride crystallization, enter in the concentrating unit ,-0.015 ~-concentrate under the 0.06MPa pressure, until the mass concentration 55-85% of ammonium fluoride;
(4) crystallization and separation: be that 55-85% ammonium fluoride solution is delivered to the cooling crystallizer crystallisation by cooling with mass concentration, separate out the ammonium fluoride crystal, obtain the ammonium fluoride solidliquid mixture, its filtering separation is got the ammonium fluoride crystal, mother liquor returns concentrated, and so circulation realizes the ammonium fluoride crystallisation process.
2. method according to claim 1 is characterized in that in the described step (1), temperature is controlled at 40～55 ℃ during gas absorption process.
3. method according to claim 1 is characterized in that in the described step (1), and the ammonium fluoride consumption is theoretical consumption 0.8-2 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100097356A CN103058224A (en) | 2013-01-11 | 2013-01-11 | Method for recycling fluorine-producing ammonium fluoride in wet-process phosphoric acid tail gas |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100097356A CN103058224A (en) | 2013-01-11 | 2013-01-11 | Method for recycling fluorine-producing ammonium fluoride in wet-process phosphoric acid tail gas |
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|---|---|
| CN103058224A true CN103058224A (en) | 2013-04-24 |
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| CN2013100097356A Pending CN103058224A (en) | 2013-01-11 | 2013-01-11 | Method for recycling fluorine-producing ammonium fluoride in wet-process phosphoric acid tail gas |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107522519A (en) * | 2017-07-27 | 2017-12-29 | 宜昌鄂中化工有限公司 | A kind of recycling technique of wet process phosphoric acid by-product fluosilicic acid |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0616601A1 (en) * | 1990-12-31 | 1994-09-28 | Phosphate Engineering & Constr | Production of phosphoric acid and hydrogen fluoride. |
| CN1721044A (en) * | 2005-05-24 | 2006-01-18 | 夏克立 | Fluorine-containing waste gas utilization method in phosphorus fertilizer production |
| CN101139094A (en) * | 2007-08-24 | 2008-03-12 | 云南云天化国际化工股份有限公司 | Method for preparing big-compensating forcing white carbon black and high concentration ammonium fluoride through aminating of fluosilicic acid |
| CN101671036A (en) * | 2009-08-03 | 2010-03-17 | 瓮福（集团）有限责任公司 | Method for preparing ammonium fluoride with high purity |
| CN102491369A (en) * | 2011-12-02 | 2012-06-13 | 瓮福（集团）有限责任公司 | Method for producing ammonium fluoride by recovering fluorine resources |
-
2013
- 2013-01-11 CN CN2013100097356A patent/CN103058224A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0616601A1 (en) * | 1990-12-31 | 1994-09-28 | Phosphate Engineering & Constr | Production of phosphoric acid and hydrogen fluoride. |
| CN1721044A (en) * | 2005-05-24 | 2006-01-18 | 夏克立 | Fluorine-containing waste gas utilization method in phosphorus fertilizer production |
| CN101139094A (en) * | 2007-08-24 | 2008-03-12 | 云南云天化国际化工股份有限公司 | Method for preparing big-compensating forcing white carbon black and high concentration ammonium fluoride through aminating of fluosilicic acid |
| CN101671036A (en) * | 2009-08-03 | 2010-03-17 | 瓮福（集团）有限责任公司 | Method for preparing ammonium fluoride with high purity |
| CN102491369A (en) * | 2011-12-02 | 2012-06-13 | 瓮福（集团）有限责任公司 | Method for producing ammonium fluoride by recovering fluorine resources |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107522519A (en) * | 2017-07-27 | 2017-12-29 | 宜昌鄂中化工有限公司 | A kind of recycling technique of wet process phosphoric acid by-product fluosilicic acid |
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Application publication date: 20130424 |