CN115784238B - Method for recycling soluble fluorine in phosphogypsum - Google Patents
Method for recycling soluble fluorine in phosphogypsum Download PDFInfo
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- CN115784238B CN115784238B CN202211275262.XA CN202211275262A CN115784238B CN 115784238 B CN115784238 B CN 115784238B CN 202211275262 A CN202211275262 A CN 202211275262A CN 115784238 B CN115784238 B CN 115784238B
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- phosphogypsum
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- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 64
- 239000011737 fluorine Substances 0.000 title claims abstract description 64
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000004064 recycling Methods 0.000 title abstract description 7
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 title 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 62
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000000706 filtrate Substances 0.000 claims abstract description 30
- 239000002253 acid Substances 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000010440 gypsum Substances 0.000 claims abstract description 14
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 14
- 239000003381 stabilizer Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 8
- 230000005587 bubbling Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims description 8
- 229960003540 oxyquinoline Drugs 0.000 claims description 8
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims description 5
- 239000001433 sodium tartrate Substances 0.000 claims description 5
- 229960002167 sodium tartrate Drugs 0.000 claims description 5
- 235000011004 sodium tartrates Nutrition 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 239000010456 wollastonite Substances 0.000 claims description 2
- 229910052882 wollastonite Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 230000001131 transforming effect Effects 0.000 claims 1
- 238000005406 washing Methods 0.000 abstract description 25
- 238000001704 evaporation Methods 0.000 abstract description 14
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000007599 discharging Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 239000002910 solid waste Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000002440 industrial waste Substances 0.000 description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 239000005909 Kieselgur Substances 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical group [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- -1 fluorine ions Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a method for recycling soluble fluorine in phosphogypsum, which comprises the steps of heating a phosphogypsum decomposer, adding solid phosphogypsum and a phosphogypsum decomposition accelerator, stirring at constant temperature, reacting while filtering while the mixture is hot, transferring filtrate to a container, adding a metal ion stabilizer, adding a fluorine conversion agent, continuously bubbling air into the filtrate, discharging gas phase escaping from a flask into the atmosphere after washing the bottle with clear water, evaporating and crystallizing liquid in the flask after reaction, washing the escaping gas phase with the same bottle, filtering after crystallization is completed to obtain filtrate and gypsum crystals with low impurity content, returning the filtrate as circulating liquid, and obtaining liquid in the bottle is fluosilicic acid solution. The method is simple to operate, mild in reaction condition, and beneficial to recycling of solid waste, and purification and impurity removal are realized in the process of fluorine recovery in phosphogypsum.
Description
Technical Field
The invention belongs to the field of wet-process phosphoric acid solid waste purification, and particularly relates to a method for recovering soluble fluorine in phosphogypsum.
Background
Phosphogypsum is industrial waste residue discharged in the process of producing phosphoric acid by decomposing phosphate ore with sulfuric acid, and about 5 t phosphogypsum is produced every l t phosphoric acid is produced. It is particularly important to find an effective recycling method.
Soluble fluorine in phosphogypsum mainly exists in the forms of NaF and KF, and insoluble fluorine mainly exists in the forms of NasAlF6, caSiF6 and CaF. Fluorine has great influence on the application performance of the phosphogypsum product such as the strength of a hardened body, the setting time and the like, so that research on removal and recycling of fluorine in phosphogypsum has important practical significance on comprehensive utilization of phosphogypsum. At present, the prior art for removing fluorine in phosphogypsum mainly comprises the processes of washing and purifying, lime neutralization, acid leaching, calcination and the like. The water washing method can effectively remove the soluble phosphorus and the soluble fluorine in phosphogypsum, but needs to solve the secondary pollution caused by the washing liquid in the water washing process. The calcination method can effectively remove the eutectic phosphorus, but has higher energy consumption and cost. In the research aspect of removing phosphorus and fluorine by a lime neutralization method, wang Ying and the like are used for removing phosphorus and fluorine from certain phosphogypsum under the conditions that the mixing amount of quicklime is 8 percent and the aging time is 24 hours, the removal rate of soluble phosphorus in phosphogypsum is close to 100 percent, but the removal rate of soluble fluorine is lower than 70.45 percent, and the consumption of lime is higher; in the research aspect of removing phosphorus and fluorine by an acid leaching method, zhao Gongtao and the like leach phosphogypsum by 30% sulfuric acid, and the phosphorus and fluorine removal rates are 97.47% and 68.97%, respectively.
The prior art has a certain effect on removing fluorine, but the removed fluorine element is often present in wastewater or solid mixture and is still difficult to recycle, so that the invention not only realizes the purification of phosphogypsum in the phosphogypsum treatment process, but also can separate fluorine in phosphogypsum at the same time, thereby achieving the aim of recycling.
Disclosure of Invention
In order to achieve the above purpose, the technical scheme of the invention is as follows: a process for recovering soluble fluorine from phosphogypsum includes such steps as heating the phosphogypsum decomposer to 70-90 deg.C, adding a certain amount of solid phosphogypsum and a proper amount of phosphogypsum decomposition promoter, stirring at constant temp for reaction for 1-3 hr, filtering while it is hot, holding temp at 80-90 deg.C, adding metal ion stabilizer to filtrate for 30-60 min, adding fluorine converting agent, blowing air into filtrate, washing the gas phase in flask, exhausting to atmosphere, reaction for 2-3 hr, washing with water, and collecting fluorosilicic acid solution.
In the further technical scheme, evaporating and crystallizing the reacted liquid, washing and collecting the escaped gas phase with the same washing bottle, filtering after crystallization to obtain filtrate and gypsum crystals with low impurity content, and returning the filtrate as phosphogypsum decomposer for use, wherein the liquid obtained in the washing bottle is fluosilicic acid solution.
In the scheme, the phosphogypsum decomposer is industrial waste sulfuric acid or a mixture of byproduct sulfuric acid, any one of phosphoric acid and hydrochloric acid, and the mass concentration of the phosphogypsum decomposer is 10-40%.
In the above scheme, the decomposition accelerator is one or two of sodium citrate, sodium tartrate, phthalic acid and oxalic acid. The addition amount of the decomposition accelerator is 0.2% -1% of the mass of the solid phosphogypsum.
In the scheme, the metal ion stabilizer is one or two of 8-hydroxyquinoline, triethanolamine, ethylenediamine tetramethylene sodium phosphate and the like. The metal ion stabilizer accounts for 0.5-1% of the mass of the filtrate.
In the scheme, the fluorine conversion agent is a mixture of any one of industrial waste residues, wollastonite and diatomite. The fluorine conversion agent accounts for 0.4 to 0.7 percent of the mass of the filtrate.
In the scheme, the metal ion curing agent and the fluorine conversion agent are added in the sequence of adding the metal ion curing agent at intervals of 30-60 minutes before adding the fluorine conversion agent.
In the scheme, the fluosilicic acid solution is colorless and transparent strong acid liquid and is a main raw material for preparing fluosilicate and hydrofluoric acid.
According to the technical scheme, the phosphogypsum is dissolved in an acidic environment, most of soluble fluorine and a small part of insoluble fluorine in the phosphogypsum are dissolved, the phosphogypsum exists in a fluorine ion form in the solution, and the introduced decomposition accelerator can dissolve the phosphogypsum to the greatest extent, so that fluorine elements wrapped in the phosphogypsum are released. The metal ion stabilizer can carry out a complex reaction with metal ions in the solution to prevent the metal ions from carrying out a precipitation reaction with dissolved free fluorine, the fluorine conversion agent is high-purity high-activity silicon dioxide, the free fluorine ions are converted into silicon tetrafluoride in the solution, and under certain temperature and inflation conditions, the silicon tetrafluoride escapes from the solution system in a gas form, and the fluosilicic acid solution is obtained through water absorption.
Detailed Description
The invention is further described below in connection with specific embodiments.
Example 1
Preparing a dilute solution with the mass fraction of 30% from industrial waste sulfuric acid, heating 1000 parts of the solution to 90 ℃, adding 500 parts of phosphogypsum (fluorine content is 0.8%) serving as a raw material and 0.5 part of sodium tartrate, stirring at constant temperature for reacting for 3 hours, filtering while the reaction is hot, transferring filtrate to a closed container, keeping the constant temperature at 85 ℃, adding 1.5 parts of 8-hydroxyquinoline into the filtrate, reacting for 30 minutes, adding 1.5 parts of industrial waste residues, continuously bubbling air into a reaction system, discharging gas phase escaped from a flask into the atmosphere after washing a bottle filled with deionized water, evaporating and crystallizing liquid in the flask after reacting for 3 hours, washing the escaped gas phase with the same bottle washing, stopping evaporating until crystals appear in the flask, filtering evaporating slurry to obtain filtrate and gypsum crystals, and obtaining the liquid in the bottle washing as a fluosilicic acid solution with low concentration. The analysis and determination show that the fluorine content of gypsum crystal is 0.3%, and the obtained solution only contains fluorine and silicon elements, and the fluosilicic acid content is 2%.
Example 2
Preparing a dilute solution with the mass fraction of 30% from industrial waste sulfuric acid, heating 1000 parts of the solution to 90 ℃, adding 500 parts of phosphogypsum (fluorine content is 0.8%) serving as a raw material and 1.0 part of sodium tartrate, stirring at constant temperature for reacting for 3 hours, filtering while the reaction is hot, transferring filtrate to a closed container, keeping the constant temperature at 85 ℃, adding 2.5 parts of 8-hydroxyquinoline into the filtrate, reacting for 30 minutes, adding 2.5 parts of diatomite, continuously bubbling air into a reaction system, discharging gas phase escaped from a flask into the atmosphere after washing a bottle filled with deionized water, evaporating and crystallizing liquid in the flask after reacting for 3 hours, washing the escaped gas phase with the same bottle, stopping evaporating until crystals appear in the flask, filtering evaporating slurry to obtain filtrate and gypsum crystals, and obtaining the liquid in the bottle washing as a fluosilicic acid solution with low concentration. The analysis and determination show that the fluorine content of gypsum crystal is 0.1%, and the obtained solution only contains fluorine and silicon elements, and the fluosilicic acid content is 2.5%.
Example 2-1
The method and procedure are the same as in example 2, with only changing the conditions: to the filtrate, 2.5 parts of 8-hydroxyquinoline was added, and after 60 minutes of reaction, 2.5 parts of diatomaceous earth was further added. The analysis and determination show that the fluorine content of gypsum crystal is 0.08%, and the obtained solution only contains fluorine and silicon elements, and the fluosilicic acid content is 2.7%.
Example 2-2
The method and procedure are the same as in example 2, with only changing the conditions: to the filtrate, 2.5 parts of 8-hydroxyquinoline was added, and after 90 minutes of reaction, 2.5 parts of diatomaceous earth was added. The analysis and determination show that the fluorine content of gypsum crystal is 0.12%, and the obtained solution only contains fluorine and silicon elements, and the fluosilicic acid content is 2.1%.
Examples 2 to 3
The method and procedure are the same as in example 2, with only changing the conditions: to the filtrate, 2.5 parts of 8-hydroxyquinoline was added, and after 10 minutes of reaction, 2.5 parts of diatomaceous earth was added. The analysis and determination show that the fluorine content of gypsum crystal is 0.15%, and the obtained solution only contains fluorine and silicon elements, and the fluosilicic acid content is 1.8%.
Example 3
Preparing a dilute solution with the mass fraction of 30% from industrial waste sulfuric acid, heating 1000 parts of the solution to 90 ℃, adding 500 parts of phosphogypsum (fluorine content is 0.8%) serving as a raw material and 1.0 part of sodium tartrate, stirring at constant temperature for reacting for 3 hours, filtering while the reaction is hot, transferring filtrate to a closed container, keeping the constant temperature at 85 ℃, adding 2.5 parts of diatomite, reacting for 30 minutes, adding 2.5 parts of 8-hydroxyquinoline, continuously bubbling air into a reaction system, discharging gas phase escaping from the flask into the atmosphere after washing a bottle filled with deionized water, evaporating and crystallizing the liquid in the flask after reacting for 3 hours, washing the escaping gas phase with the same washing bottle until the crystals appear in the flask, stopping evaporating, filtering the evaporating slurry to obtain filtrate and gypsum crystals, and obtaining the liquid in the washing bottle which is a fluosilicic acid solution with low concentration. The analysis and determination show that the fluorine content of gypsum crystal is 0.7%, and the obtained solution only contains fluorine and silicon elements, and the fluosilicic acid content is 0.2%.
Example 4
Preparing a dilute solution with the mass fraction of 30% from industrial waste sulfuric acid, heating 1000 parts of the solution to 90 ℃, adding 500 parts of phosphogypsum (fluorine content is 0.8%) serving as a raw material and 1.0 part of oxalic acid, stirring at constant temperature for reaction for 3 hours, filtering while the reaction is hot, transferring filtrate to a closed container, keeping the constant temperature at 85 ℃, adding 2.5 parts of ethylenediamine tetramethylene sodium phosphate, reacting for 30 minutes, adding 2.5 parts of diatomite, enabling a reaction system not to bulge air, discharging gas phase escaping from a flask to the atmosphere after washing a bottle filled with deionized water, performing evaporation crystallization on liquid in the flask after reaction for 3 hours, washing the escaping gas phase with the same bottle, stopping evaporation until crystals appear in the flask, filtering evaporation slurry to obtain filtrate and gypsum crystals, and obtaining the liquid in the bottle washing is a fluosilicic acid solution with low concentration. The analysis and determination show that the fluorine content of gypsum crystal is 0.6%, and the obtained solution only contains fluorine and silicon elements, and the fluosilicic acid content is 0.8%.
Claims (10)
1. A method for recovering soluble fluorine from phosphogypsum, comprising the steps of:
(1) Adding solid phosphogypsum and a decomposition accelerator into phosphogypsum decomposer, stirring and reacting, and filtering, wherein the phosphogypsum decomposer is one or a mixture of sulfuric acid, phosphoric acid and hydrochloric acid, and the decomposition accelerator is one or a mixture of sodium citrate, sodium tartrate, phthalic acid and oxalic acid;
(2) Adding a metal ion stabilizer into the filtrate obtained in the step (1), stirring, adding a fluorine conversion agent, and continuously bubbling air into the filtrate to react, wherein gas phase escaping in the reaction process is collected by water to obtain a fluosilicic acid solution; the metal ion stabilizer is one or two of 8-hydroxyquinoline, triethanolamine and ethylenediamine tetramethylene sodium phosphate; the fluorine conversion agent is wollastonite or diatomite.
2. The method for recovering soluble fluorine from phosphogypsum as claimed in claim 1, wherein the mass concentration of phosphogypsum decomposer in the step (1) is 10-40%.
3. The method for recovering soluble fluorine from phosphogypsum as claimed in claim 2, wherein the addition amount of the decomposition accelerator in the step (1) is 0.2% -1% by mass of the solid phosphogypsum.
4. The method for recovering soluble fluorine from phosphogypsum according to claim 3, wherein the stirring reaction condition in the step (1) is 70 ℃ to 90 ℃ and the reaction time is 1 to 3 hours.
5. The method for recovering soluble fluorine from phosphogypsum according to claim 4, wherein the metal ion stabilizer is added after the temperature of the filtrate in step (2) is raised to 80-90 ℃.
6. The method for recovering soluble fluorine from phosphogypsum according to claim 5, wherein the metal ion stabilizer in step (2) is 0.5% -1% of the mass of the filtrate.
7. The method for recovering soluble fluorine from phosphogypsum of claim 6, wherein the fluorine transforming agent in step (2) is 0.4% -0.7% of the mass of the filtrate.
8. The method for recovering soluble fluorine from phosphogypsum according to claim 7, wherein the addition sequence of the metal ion stabilizer and the fluorine conversion agent is that the metal ion stabilizer is added first, and then the fluorine conversion agent is added after 30-60 minutes of interval.
9. The method for recovering soluble fluorine from phosphogypsum according to claim 7, wherein the liquid obtained after the completion of the reaction in step (2) is evaporated and crystallized, the escaped gas phase is collected with water to obtain fluosilicic acid solution, the filtrate and gypsum crystals are obtained by filtration after the completion of crystallization, and the filtrate is returned to step (1) to be used as a circulating liquid.
10. The fluorosilicic acid solution prepared by the method according to any one of claims 1 to 9, wherein the fluorosilicic acid solution contains 1 to 3 mass percent of fluorosilicic acid.
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