CN108862224A - A kind of method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate - Google Patents
A kind of method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate Download PDFInfo
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- CN108862224A CN108862224A CN201810678622.8A CN201810678622A CN108862224A CN 108862224 A CN108862224 A CN 108862224A CN 201810678622 A CN201810678622 A CN 201810678622A CN 108862224 A CN108862224 A CN 108862224A
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- phosphoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
Abstract
The present invention relates to a kind of methods that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate, include the following steps：A, phosphoric acid by wet process ammonification slurry slag and water are configured to slurry；B, it is slowly added to sulfuric acid into slurry to be reacted, is filtered after reaction, obtain phosphorous leachate；C, by after leachate cooling, crystallization, filtering, de-magging leachate is obtained；D, anhydrous sodium sulfate solid is added into de-magging leachate to be reacted, stands, filters after reaction, is purified liquid；E, green vitriol solid is added into scavenging solution, it is aoxidized after stirring and dissolving with hydrogenperoxide steam generator, surfactant is added, the pH of solution is adjusted to there are a large amount of white precipitates with aqueous slkali, and cooling after the reaction was continued a period of time grinds after standing sedimentation, being filtered, washed, drying and obtain light yellow phosphoric acid iron powder.Operation of the present invention is simple, processing cost is cheap, provides a kind of utilization ways of phosphoric acid by wet process ammonification slurry slag for industrial grade monoammonium phosphate manufacturing enterprise.
Description
Technical field
The invention belongs to the fields of open pit mining in chemical industry, and in particular to Wet-process Phosphoric Acid Production PHOSPHORIC ACID TECH.GRADE
The recoverying and utilizing method of phosphorus in a kind of phosphoric acid by wet process ammonification slurry slag generated during monoammonium.
Background technique
Phosphoric acid by wet process ammonification slurry slag is during preparing industrial grade monoammonium phosphate from wet-process phosphoric acid in logical ammonia and phosphoric acid by wet process
The filter cake generated after filtering.Main component includes NH4H2PO4、(NH4)2HPO4(Fe, Al) NH4(HPO4)2·0.5H2O、
(Fe,Al)Mg(NH4)2(HPO4)2·F3Etc. water-insoluble complex compound.Essential element includes P, Mg, F, Al, and specific data are such as
Shown in table 1.General butt P2O5For content 30%~40%, most of enterprise directly will be used as agricultural fertilizer after the drying of slurry slag,
But its fertilizer efficiency is poor, and overall economic efficiency is lower.
Table 1 phosphoric acid by wet process ammonification slurry slag (butt) component list
| Component | P2O5 | Fe2O3 | Al2O3 | MgO | F | CaO |
| Mass fraction | 37.27% | 1.75% | 4.79% | 9.32% | 7.92% | 1.02% |
A large amount of phosphoric acid by wet process ammonification slurry slag will be generated during " slurry process " produces industrial grade monoammonium phosphate,
The industrial grade monoammonium phosphate of every 1 ton of production will generate 1~3 ton of phosphoric acid by wet process ammonification slurry slag not waited.Most of enterprise will
Slurry slag is added in monoammonium phosphate process units for producing powdery monoammonium phosphate.But because of Mg in slurry slag2+, Fe3+, Al3+Etc. miscellaneous
Matter content is higher, and reaction generates the solubility in citric acids such as magnesium dihydrogen phosphate and iron, aluminium or insoluble compound, is easy deposition fouling, makes defeated
Send line clogging.The powdery monoammonium phosphate device cycle of operation is caused to shorten.Therefore how to digest and efficiently use phosphoric acid by wet process ammonia
Material screenings becomes the problem that major phosphorous chemical industry manufacturing enterprise is faced.
Contain a large amount of solubility in citric acid available phosphorus in phosphoric acid by wet process ammonification slurry slag, therefore seems to the utilization of wherein phosphor resource
It is very necessary.
Summary of the invention
The purpose of the present invention is to provide a kind of method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate, this method is benefit
Have with the by-product phosphoric acid by wet process ammonification slurry slag production generated in industrial grade monoammonium phosphate production process compared with high added value
Phosphatic process.
The technical proposal adopted by the invention to solve the above technical problems is that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate
Method, which is characterized in that include the following steps：
Phosphoric acid by wet process ammonification slurry slag and water are configured to slurry by a；
B is slowly added to sulfuric acid into slurry and is reacted, and filters after reaction, obtains phosphorous leachate；
Leachate is cooled down, is crystallized, after filtering by c, obtains de-magging leachate；
Sodium salt solid is added into de-magging leachate and is reacted by d, stands, filters after reaction, is purified liquid；
Ferrous salt solid is added into scavenging solution by e, is aoxidized after stirring and dissolving with hydrogenperoxide steam generator, and surface-active is added
Agent adjusts the pH of solution to there are a large amount of white precipitates with aqueous slkali, cooling, standing sedimentation, mistake after the reaction was continued a period of time
Grinding obtains light yellow phosphoric acid iron powder after filter, washing, drying.
According to the above scheme, the phosphoric acid by wet process ammonification slurry slag is to utilize preparing industrial grade monoammonium phosphate from wet-process phosphoric acid mistake
Lead to the filter cake generated after the filtering of ammonia neutralising phosphoric acid in journey.
According to the above scheme, water described in step a is distilled water；The slurry solid content is 30~40wt.%.
According to the above scheme, the mass concentration of sulfuric acid is 98% in step b, and the additional amount of sulfuric acid is phosphoric acid by wet process ammonification slurry
The 60~100% of slag butt quality, reaction temperature are 60~100 DEG C, and the reaction time is 30~80min.
According to the above scheme, decrease temperature crystalline temperature described in step c is 8~12 DEG C.
According to the above scheme, sodium salt described in step d is anhydrous sodium sulfate, natrium carbonicum calcinatum, one in anhydrous sodium chloride
Kind.
According to the above scheme, the molar ratio of sodium salt described in step d and fluorine in de-magging leachate is 0.6：1~1.2：1, instead
It is 20~100min between seasonable, reaction temperature is 30~80 DEG C.
According to the above scheme, ferrous salt described in step e is green vitriol.
According to the above scheme, the molar ratio of phosphorus is 1 in ferrous salt described in step e and scavenging solution：1~1：4, reaction temperature
It is 60~90 DEG C, the reaction time is 1~3h.
According to the above scheme, surfactant described in step e is Macrogol 6000, neopelex, ten
One of six alkyl trimethyl ammonium bromides, dosage are the 1%~5% of ferrous salt quality；The aqueous slkali is sodium hydroxide
Solution；The range for adjusting pH value of solution is 0.5~2.
The reaction that present invention process process occurs is as follows：
(NH4)2HPO4+H2SO4=H3PO4+(NH4)2SO4
2NH4H2PO4+H2SO4=2H3PO4+(NH4)2SO4
MgHPO4+H2SO4=H3PO4+MgSO4
FeMg(NH4)2(HPO4)2·F3+2H2SO4=FePO4 ↓+MgSO4+3HF↑+H3PO4+(NH4)2SO4
AlMg(NH4)2(HPO4)2·F3+2H2SO4=AlPO4 ↓+MgSO4+3HF↑+H3PO4+(NH4)2SO4
CaHPO4+H2SO4=CaSO4↓+H3PO4
2FeNH4(HPO4)2·0.5H2O+H2SO4=2FePO4 ↓+2H3PO4+(NH4)2SO4+H2O
2AlNH4(HPO4)2·0.5H2O+H2SO4=2AlPO4 ↓+2H3PO4+(NH4)2SO4+H2O
2Na++SiF6 2-=Na2SiF6
2PO4 3-+2Fe2++H2O2+2H+=2FePO4↓+2H2O
The beneficial effects of the invention are as follows：
(1) present invention can efficiently use the valuable components phosphorus source contained in phosphoric acid by wet process ammonification slurry slag, be used to prepare
With high added value ferric phosphate salt product, the secondary use of resource is realized；
(2) rate of recovery of phosphorus in phosphoric acid by wet process ammonification slurry slag can be made up to 60% or more using method of the invention, institute
The iron phosphorus molar ratio of phosphoric acid iron product obtained is close to 1；
(3) the simple, short processing time of the invention with process flow, the spies such as equipment requirement is simple, and operation is easy, is safe
Point.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Below by embodiment, invention is further described in detail, but the scope of the present invention is not limited in described
Hold.
Embodiment 1
A. phosphoric acid by wet process ammonification slurry slag 50g (P is taken2O5Content is 30.64%), water to be added to be made into the slag of solid content 30wt.%
Slurry, by slurry butt quality 60% into slurry be added 98% the concentrated sulfuric acid, be stirred to react 1h at 90 DEG C.Filtering, obtains
Phosphorous leachate, P in the leachate2O5Content is 10.37%, and the leaching rate of phosphorus is 89.76%；
B. leachate step A obtained obtains de-magging leachate after cooling at a temperature of 12 DEG C, crystallization, filtering, analyses
Crystal main component out is six water magnesium sulfate ammoniums, and the removal efficiency of magnesium is up to 58.12%；
C. into the de-magging leachate that step B obtains, according to fluorine content therein in molar ratio 1：1 is added anhydrous sodium sulfate
Solid is reacted, and 60 DEG C of reaction temperature, defluorinate scavenging solution is obtained by filtration in reaction time 60min after reaction.Filter cake is fluorine
Sodium metasilicate, the removal efficiency of fluorine is up to 54.03%；
D. into the defluorinate scavenging solution that step C obtains, according to phosphorus content therein in molar ratio 1：1 is added seven hydrated sulfuric acids
Ferrous iron is stoichiometrically added 1.2 times of theoretical value of hydrogenperoxide steam generator oxidation, the polyethylene glycol of molysite quality 1% is added
6000, sodium hydroxide solution is slowly added dropwise and adjusts pH to 0.5, then proceedes to be stirred to react, 80 DEG C of reaction temperature, reacts 60min
Afterwards cooling, standing sedimentation, be filtered, washed, dry after grinding obtain light yellow phosphoric acid iron powder.
Iron phosphorus molar ratio is 0.9539 in phosphoric acid iron product, and the utilization rate of phosphorus is 63.45% in scavenging solution.
Embodiment 2
A. phosphoric acid by wet process ammonification slurry slag 50g (P is taken2O5Content is 30.64%), water to be added to be made into the slag of solid content 30wt.%
Slurry, by slurry butt quality 70% into slurry be added 98% the concentrated sulfuric acid, be stirred to react 1h at 90 DEG C.Filtering, is contained
Phosphorus leachate, P in the leachate2O5Content is 10.58%, and the leaching rate of phosphorus is 90.46%；
B. leachate step A obtained obtains de-magging leachate after cooling at a temperature of 11 DEG C, crystallization, filtering, analyses
Crystal main component out is six water magnesium sulfate ammoniums, and the removal efficiency of magnesium is up to 58.94%；
C. into the de-magging leachate that step B obtains, according to fluorine content therein in molar ratio 1.2：1 is added anhydrous slufuric acid
Sodium solid is reacted, reaction temperature 60, defluorinate scavenging solution is obtained by filtration in reaction time 60min after reaction.Filter cake is
Prodan, the removal efficiency of fluorine is up to 59.07%；
D. into the defluorinate scavenging solution that step C obtains, according to phosphorus content therein in molar ratio 1：1 is added seven hydrated sulfuric acids
Ferrous iron is stoichiometrically added 1.2 times of theoretical value of hydrogenperoxide steam generator oxidation, the polyethylene glycol of molysite quality 2% is added
6000, sodium hydroxide solution is slowly added dropwise and adjusts pH to 1.0, then proceedes to be stirred to react, 80 DEG C of reaction temperature, reacts 60min
Afterwards cooling, standing sedimentation, be filtered, washed, dry after grinding obtain light yellow phosphoric acid iron powder.
Iron phosphorus molar ratio is 0.9649 in phosphoric acid iron product, and the utilization rate of phosphorus is 64.32% in scavenging solution.
Embodiment 3
A. phosphoric acid by wet process ammonification slurry slag 50g (P is taken2O5Content is 30.64%), water to be added to be made into the slag of solid content 30wt.%
Slurry, by slurry butt quality 80% into slurry be added 98% the concentrated sulfuric acid, be stirred to react 1h at 90 DEG C.Filtering, obtains
Phosphorous leachate, P in the leachate2O5Content is 10.20%, and the leaching rate of phosphorus is 92.78%；
B. leachate step A obtained obtains de-magging leachate after cooling at a temperature of 10 DEG C, crystallization, filtering, analyses
Crystal main component out is six water magnesium sulfate ammoniums, and the removal efficiency of magnesium is up to 59.65%；
C. into the de-magging leachate that step B obtains, according to fluorine content therein in molar ratio 1.4：1 is added anhydrous slufuric acid
Sodium solid is reacted, reaction temperature 60, defluorinate scavenging solution is obtained by filtration in reaction time 60min after reaction.Filter cake is
Prodan, the removal efficiency of fluorine is up to 60.13%；
D. into the defluorinate scavenging solution that step C obtains, according to phosphorus content therein in molar ratio 1：1 is added seven hydrated sulfuric acids
Ferrous iron is stoichiometrically added 1.2 times of theoretical value of hydrogenperoxide steam generator oxidation, the dodecyl of molysite quality 3% is added
Benzene sulfonic acid sodium salt is slowly added dropwise sodium hydroxide solution and adjusts pH to 1.5, then proceedes to be stirred to react, 80 DEG C of reaction temperature reactions
Cooling after 60min, standing sedimentation, be filtered, washed, dry after grinding obtain light yellow phosphoric acid iron powder.
Iron phosphorus molar ratio is 0.9753 in phosphoric acid iron product, and the utilization rate of phosphorus is 65.74% in scavenging solution
Embodiment 4
A. phosphoric acid by wet process ammonification slurry slag 50g (P is taken2O5Content is 30.64%), water to be added to be made into the slag of solid content 30wt.%
Slurry, by slurry butt quality 90% into slurry be added 98% the concentrated sulfuric acid, be stirred to react 1h at 90 DEG C.Filtering, obtains
Phosphorous leachate, P in the leachate2O5Content is 10.44%, and the leaching rate of phosphorus is 93.90%；
B. leachate step A obtained obtains de-magging leachate after cooling at a temperature of 9 DEG C, crystallization, filtering, is precipitated
Crystal main component be six water magnesium sulfate ammoniums, the removal efficiency of magnesium is up to 60.72%；
C. into the de-magging leachate that step B obtains, according to fluorine content therein in molar ratio 1.2：1 is added anhydrous slufuric acid
Sodium solid is reacted, reaction temperature 60, defluorinate scavenging solution is obtained by filtration in reaction time 80min after reaction.Filter cake is
Prodan, the removal efficiency of fluorine is up to 61.23%；
D. into the defluorinate scavenging solution that step C obtains, according to phosphorus content therein in molar ratio 1：1 is added seven hydrated sulfuric acids
Ferrous iron is stoichiometrically added 1.2 times of theoretical value of hydrogenperoxide steam generator oxidation, the cetyl of molysite quality 3% is added
Trimethylammonium bromide is slowly added dropwise sodium hydroxide solution and adjusts pH to 2.0, then proceedes to be stirred to react, 80 DEG C of reaction temperature, instead
Grinding obtains light yellow phosphoric acid iron powder after answering cooling after 60min, standing sedimentation, being filtered, washed, dry.
Iron phosphorus molar ratio is 1.087 in phosphoric acid iron product, and the utilization rate of phosphorus is 67.12% in scavenging solution.
Embodiment 5
A. phosphoric acid by wet process ammonification slurry slag 50g (P is taken2O5Content is 30.64%), water to be added to be made into the slag of solid content 30wt.%
Slurry, by slurry butt quality 100% into slurry be added 98% the concentrated sulfuric acid, be stirred to react 1h at 90 DEG C.Filtering, obtains
Phosphorous leachate, P in the leachate2O5Content is 10.62%, and the leaching rate of phosphorus is 94.12%.
B. leachate step A obtained obtains de-magging leachate after cooling at a temperature of 8 DEG C, crystallization, filtering, is precipitated
Crystal main component be six water magnesium sulfate ammoniums, the removal efficiency of magnesium is up to 61.83%.
C. into the de-magging leachate that step B obtains, according to fluorine content therein in molar ratio 1.2：1 is added anhydrous slufuric acid
Sodium solid is reacted, and 60 DEG C of reaction temperature, defluorinate scavenging solution is obtained by filtration in reaction time 100min after reaction.Filter cake
For prodan, the removal efficiency of fluorine is up to 62.46%.
D. into the defluorinate scavenging solution that step C obtains, according to phosphorus content therein in molar ratio 1：1 is added seven hydrated sulfuric acids
Ferrous iron is stoichiometrically added 1.2 times of theoretical value of hydrogenperoxide steam generator oxidation, the polyethylene glycol of molysite quality 3% is added
6000, sodium hydroxide solution is slowly added dropwise and adjusts pH to 2.0, then proceedes to be stirred to react, 90 DEG C of reaction temperature, reacts 60min
Afterwards cooling, standing sedimentation, be filtered, washed, dry after grinding obtain light yellow phosphoric acid iron powder.
Iron phosphorus molar ratio is 1.083 in phosphoric acid iron product, and the utilization rate of phosphorus is 67.38% in scavenging solution.
Embodiment 6
A. phosphoric acid by wet process ammonification slurry slag 50g (P is taken2O5Content is 30.64%), water to be added to be made into the slag of solid content 30wt.%
Slurry, by slurry butt quality 100% into slurry be added 98% the concentrated sulfuric acid, be stirred to react 1h at 90 DEG C.Filtering, obtains
Phosphorous leachate, P in the leachate2O5Content is 10.62%, and the leaching rate of phosphorus is 94.12%.
B. leachate step A obtained obtains de-magging leachate after cooling at a temperature of 8 DEG C, crystallization, filtering, is precipitated
Crystal main component be six water magnesium sulfate ammoniums, the removal efficiency of magnesium is up to 61.83%.
C. into the de-magging leachate that step B obtains, according to fluorine content therein in molar ratio 1.2：1 is added Carbon Dioxide
Sodium solid is reacted, and 60 DEG C of reaction temperature, defluorinate scavenging solution is obtained by filtration in reaction time 100min after reaction.Filter cake
For prodan, the removal efficiency of fluorine is up to 61.56%.
D. into the defluorinate scavenging solution that step C obtains, according to phosphorus content therein in molar ratio 1：1 is added seven hydrated sulfuric acids
Ferrous iron is stoichiometrically added 1.2 times of theoretical value of hydrogenperoxide steam generator oxidation, the polyethylene glycol of molysite quality 3% is added
6000, sodium hydroxide solution is slowly added dropwise and adjusts pH to 2.0, then proceedes to be stirred to react, 90 DEG C of reaction temperature, reacts 60min
Afterwards cooling, standing sedimentation, be filtered, washed, dry after grinding obtain light yellow phosphoric acid iron powder.
Iron phosphorus molar ratio is 1.072 in phosphoric acid iron product, and the utilization rate of phosphorus is 67.65% in scavenging solution.
Embodiment 7
A. phosphoric acid by wet process ammonification slurry slag 50g (P is taken2O5Content is 30.64%), water to be added to be made into the slag of solid content 30wt.%
Slurry, by slurry butt quality 100% into slurry be added 98% the concentrated sulfuric acid, be stirred to react 1h at 90 DEG C.Filtering, obtains
Phosphorous leachate, P in the leachate2O5Content is 10.62%, and the leaching rate of phosphorus is 94.12%.
B. leachate step A obtained obtains de-magging leachate after cooling at a temperature of 8 DEG C, crystallization, filtering, is precipitated
Crystal main component be six water magnesium sulfate ammoniums, the removal efficiency of magnesium is up to 61.83%.
C. into the de-magging leachate that step B obtains, according to fluorine content therein in molar ratio 1.2：1 is added anhydrous chlorination
Sodium solid is reacted, and 60 DEG C of reaction temperature, defluorinate scavenging solution is obtained by filtration in reaction time 100min after reaction.Filter cake
For prodan, the removal efficiency of fluorine is up to 60.75%.
D. into the defluorinate scavenging solution that step C obtains, according to phosphorus content therein in molar ratio 1：1 is added seven hydrated sulfuric acids
Ferrous iron is stoichiometrically added 1.2 times of theoretical value of hydrogenperoxide steam generator oxidation, the polyethylene glycol of molysite quality 3% is added
6000, sodium hydroxide solution is slowly added dropwise and adjusts pH to 2.0, then proceedes to be stirred to react, 90 DEG C of reaction temperature, reacts 60min
Afterwards cooling, standing sedimentation, be filtered, washed, dry after grinding obtain light yellow phosphoric acid iron powder.
Iron phosphorus molar ratio is 1.078 in phosphoric acid iron product, and the utilization rate of phosphorus is 68.04% in scavenging solution.
Claims (10)
1. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate, which is characterized in that include the following steps：
Phosphoric acid by wet process ammonification slurry slag and water are configured to slurry by a；
B is slowly added to sulfuric acid into slurry and is reacted, and filters after reaction, obtains phosphorous leachate；
Leachate is cooled down, is crystallized, after filtering by c, obtains de-magging leachate；
Sodium salt solid is added into de-magging leachate and is reacted by d, stands, filters after reaction, is purified liquid；
Ferrous salt solid is added into scavenging solution by e, is aoxidized after stirring and dissolving with hydrogenperoxide steam generator, and surfactant is added, and uses
Aqueous slkali adjusts the pH of solution to there are a large amount of white precipitates, and cooling after the reaction was continued a period of time standing sedimentation, is filtered, washed
Grinding obtains light yellow phosphoric acid iron powder after washing, drying.
2. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate according to claim 1, it is characterised in that：In step a
The phosphoric acid by wet process ammonification slurry slag is to utilize ammonia neutralising phosphoric acid mistake logical during preparing industrial grade monoammonium phosphate from wet-process phosphoric acid
The filter cake generated after filter.
3. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate according to claim 1, it is characterised in that：In step a
The water is distilled water；The slurry solid content is 30~40wt.%.
4. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate according to claim 1, it is characterised in that：In step b
The mass concentration of sulfuric acid is 98%, and the additional amount of sulfuric acid is the 60~100% of phosphoric acid by wet process ammonification slurry slag butt quality, reaction
Temperature is 60~100 DEG C, and the reaction time is 30~80min.
5. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate according to claim 1, it is characterised in that：In step c
The decrease temperature crystalline temperature is 8~12 DEG C.
6. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate according to claim 1, it is characterised in that：In step d
The sodium salt is one of anhydrous sodium sulfate, natrium carbonicum calcinatum, anhydrous sodium chloride.
7. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate according to claim 1, it is characterised in that：In step d
The molar ratio of fluorine is 0.6 in the sodium salt and de-magging leachate：1~1.2：1, the reaction time is 20~100min, reaction temperature
Degree is 30~80 DEG C.
8. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate according to claim 1, it is characterised in that：In step e
The ferrous salt is green vitriol.
9. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate according to claim 1, it is characterised in that：In step e
The molar ratio of phosphorus is 1 in the ferrous salt and scavenging solution：1~1：4, reaction temperature be 60~90 DEG C, the reaction time be 1~
3h。
10. the method that phosphoric acid by wet process ammonification slurry slag prepares ferric phosphate according to claim 1, it is characterised in that：In step e
The surfactant be one of Macrogol 6000, neopelex, cetyl trimethylammonium bromide,
Dosage is the 1%~5% of ferrous salt quality；The aqueous slkali is sodium hydroxide solution；Adjust pH value of solution range be 0.5~
2。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113307243A (en) * | 2021-07-08 | 2021-08-27 | 河南佰利新能源材料有限公司 | Method for preparing iron phosphate by recycling mother liquor |
| CN113460989A (en) * | 2021-07-01 | 2021-10-01 | 四川宏达股份有限公司 | Battery-grade iron phosphate and preparation method thereof |
| CN116282717A (en) * | 2023-03-24 | 2023-06-23 | 湖北朗润环保科技有限公司 | Comprehensive treatment method for production wastewater |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995006004A1 (en) * | 1993-08-26 | 1995-03-02 | Kemira Oy | Treatment method for waste water sludge comprising at least one metal |
| CN101462704A (en) * | 2008-12-29 | 2009-06-24 | 刘世琦 | Production method of ultrafine cell level ferric orthophosphate |
| CN102515129A (en) * | 2011-12-20 | 2012-06-27 | 江苏中电长迅能源材料有限公司 | Preparation method for submicron battery-grade ferric phosphate |
| JP2013161654A (en) * | 2012-02-06 | 2013-08-19 | Sumitomo Metal Mining Co Ltd | Positive electrode active material for lithium secondary battery and method for manufacturing the same, precursor of positive electrode active material and method for manufacturing the same, and lithium secondary battery including positive electrode active material |
| CN106684485A (en) * | 2016-12-19 | 2017-05-17 | 天齐锂业股份有限公司 | Method for recovering waste/used lithium iron phosphate positive-pole material by acid leaching method |
| CN107827113A (en) * | 2017-11-29 | 2018-03-23 | 湖北祥云(集团)化工股份有限公司 | In a kind of industrial monoammonium phosphate and slurry in fluorine recovery method |
-
2018
- 2018-06-27 CN CN201810678622.8A patent/CN108862224B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995006004A1 (en) * | 1993-08-26 | 1995-03-02 | Kemira Oy | Treatment method for waste water sludge comprising at least one metal |
| CN101462704A (en) * | 2008-12-29 | 2009-06-24 | 刘世琦 | Production method of ultrafine cell level ferric orthophosphate |
| CN102515129A (en) * | 2011-12-20 | 2012-06-27 | 江苏中电长迅能源材料有限公司 | Preparation method for submicron battery-grade ferric phosphate |
| JP2013161654A (en) * | 2012-02-06 | 2013-08-19 | Sumitomo Metal Mining Co Ltd | Positive electrode active material for lithium secondary battery and method for manufacturing the same, precursor of positive electrode active material and method for manufacturing the same, and lithium secondary battery including positive electrode active material |
| CN106684485A (en) * | 2016-12-19 | 2017-05-17 | 天齐锂业股份有限公司 | Method for recovering waste/used lithium iron phosphate positive-pole material by acid leaching method |
| CN107827113A (en) * | 2017-11-29 | 2018-03-23 | 湖北祥云(集团)化工股份有限公司 | In a kind of industrial monoammonium phosphate and slurry in fluorine recovery method |
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| CN113460989A (en) * | 2021-07-01 | 2021-10-01 | 四川宏达股份有限公司 | Battery-grade iron phosphate and preparation method thereof |
| CN113307243A (en) * | 2021-07-08 | 2021-08-27 | 河南佰利新能源材料有限公司 | Method for preparing iron phosphate by recycling mother liquor |
| CN116282717A (en) * | 2023-03-24 | 2023-06-23 | 湖北朗润环保科技有限公司 | Comprehensive treatment method for production wastewater |
| CN116282717B (en) * | 2023-03-24 | 2024-03-12 | 湖北朗润环保科技有限公司 | Comprehensive treatment method for production wastewater |
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Denomination of invention: A Method for Preparing Iron Phosphate from Wet Process Phosphoric Acid Ammoniation Slurry Effective date of registration: 20230731 Granted publication date: 20211112 Pledgee: Bank of China Limited Huanggang branch Pledgor: HUBEI XIANGYUN (Group) CHEMICAL Co.,Ltd. Registration number: Y2023420000318 |