CN110255520A - A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater - Google Patents
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater Download PDFInfo
- Publication number
- CN110255520A CN110255520A CN201910412494.7A CN201910412494A CN110255520A CN 110255520 A CN110255520 A CN 110255520A CN 201910412494 A CN201910412494 A CN 201910412494A CN 110255520 A CN110255520 A CN 110255520A
- Authority
- CN
- China
- Prior art keywords
- industrial wastewater
- phosphate
- added
- phosphoric acid
- grade iron
- 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
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 title claims abstract description 94
- 239000010842 industrial wastewater Substances 0.000 title claims abstract description 78
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910000398 iron phosphate Inorganic materials 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 31
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 26
- 238000000605 extraction Methods 0.000 title claims abstract description 22
- 239000005955 Ferric phosphate Substances 0.000 claims abstract description 56
- 229940032958 ferric phosphate Drugs 0.000 claims abstract description 56
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims abstract description 56
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 37
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 33
- 239000011574 phosphorus Substances 0.000 claims abstract description 33
- 229910052742 iron Inorganic materials 0.000 claims abstract description 23
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims description 35
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 25
- 239000012065 filter cake Substances 0.000 claims description 22
- BMTOKWDUYJKSCN-UHFFFAOYSA-K iron(3+);phosphate;dihydrate Chemical compound O.O.[Fe+3].[O-]P([O-])([O-])=O BMTOKWDUYJKSCN-UHFFFAOYSA-K 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 13
- 239000007800 oxidant agent Substances 0.000 claims description 13
- 230000001590 oxidative effect Effects 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- 238000006479 redox reaction Methods 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910001448 ferrous ion Inorganic materials 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000002910 solid waste Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000012141 concentrate Substances 0.000 abstract description 2
- 230000001143 conditioned effect Effects 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 239000011790 ferrous sulphate Substances 0.000 description 19
- 235000003891 ferrous sulphate Nutrition 0.000 description 19
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 19
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 19
- 239000002351 wastewater Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 239000008139 complexing agent Substances 0.000 description 9
- -1 iron ion Chemical class 0.000 description 9
- 238000004321 preservation Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000001506 calcium phosphate Substances 0.000 description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 235000019837 monoammonium phosphate Nutrition 0.000 description 1
- 239000006012 monoammonium phosphate Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses the methods that phosphoric acid in a kind of extraction industrial wastewater prepares battery-grade iron phosphate, comprising the following steps: determines phosphorus source；Synthesize ferric phosphate presoma；Synthesize ferric phosphate and calcining.The invention has the advantages that 1, this method is to fix the industrial wastewater of phosphorus content as phosphorus source, by, in specific conditioned response, obtaining ferric phosphate presoma, the presoma is subsequent to concentrate synthesis ferric phosphate with source of iron, precipitating reagent etc., preparation process is simple and convenient, reduces cost of human and material resources；2, it fundamentally solves current ferric phosphate washes to generate a large amount of solid wastes, cause the problems such as environmental pollution and processing solid waste valuableness expense, realizes the recycling of phosphor resource in washes；3, the battery-grade iron phosphate sample impurity content being prepared is lower than 50ppm, can be used as battery-grade iron phosphate lithium raw materials for production, has high economic benefit.
Description
Technical field
The present invention relates to novel energy resource material technology fields, and in particular to phosphoric acid prepares LITHIUM BATTERY in a kind of extraction industrial wastewater
The method of ferric phosphate.
Background technique
Relevant enterprise, which produces, contains a large amount of phosphate radical and micro other impurities ion in waste water.The work of mainstream at present
Industry treatment of Phosphorus Containing Waste Water process flow is: ferrous sulfate being added into industrial wastewater, the rear lime that is added adjusts pH value to 6~8, makes
Useless iron, phosphate radical in washes etc. are respectively formed hydroxide or calcium phosphate precipitation, and the rear flocculant that is added is condensed into blocks
Accelerate precipitating.It is blocking using automatic plate frame press filter plate filters pressing.Dephosphorization is carried out using calcium hydroxide, the calcium phosphate generated except iron
Equal byproducts added value is low, can only handle at a low price as solid waste at present.Prior art CN201811455629 .X discloses one kind
The circulation utilization method of phosphorous industrial wastewater, in industrial wastewater phosphor resource and nitrogen resource all recycled.The party
Method need by phosphorous industrial wastewater treatment system ammonium sulfate and monoammonium phosphate mixed solution be diluted with water, obtain phosphorus source, though
So improve the utilization rate of phosphorus, but complex process, previous work amount is larger, and variable is more, and homogeneity of product is bad, and needs
A set of individual equipment is designed to synthesize, while needing to put into a large amount of man power and material, does not meet chasing after for Business Economic Benefit
It asks.
Angle is pursued from the existing developing direction of enterprise and economic benefit, solves the problems, such as phosphoric acid in industrial wastewater, is improved
The byproduct added value that Industrial Wastewater Treatment obtains, the preparation method for providing a kind of battery-grade iron phosphate are of great significance.
Summary of the invention
In order to solve the above technical problems, the present invention provides phosphoric acid in a kind of extraction industrial wastewater to prepare battery-grade iron phosphate
Method, simple process, processing cost is lower, while improving the added value of ferric phosphate Phosphorus From Wastewater resource, realizes resource
Reuse reduces ferric phosphate production cost, has high economic benefit.
The technical solution adopted by the present invention is that:
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: into phosphorous industrial wastewater add flocculant clean, after to after removal of impurities industrial wastewater carry out
Filters pressing obtains the industrial wastewater that phosphorous mass fraction is 4000-8000ppm；
B, it synthesizes ferric phosphate presoma: a certain amount of source of iron being added in step a in finally obtained industrial wastewater, the iron
The ratio of the phosphorus content in iron content and industrial wastewater in source be 1:1-1.8:1, be added liquid alkaline, obtain turbid solution, then plus
Enter alkali and adjust reaction pH to 2-11, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Oxidant is then added in value, and redox reaction occurs, and high-purity phosphate dihydrate iron is prepared in high temperature；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 600-
700℃。
Further, the flocculant in step a is PAC or PAM.
Further, the source of iron in step b is the solution containing ferrous ion.
Further, the liquid alkaline in step b is sodium hydroxide solution or ammonia spirit.
Further, the reaction time of fast reaction is 10-100min in step b.
Further, the high temperature in step c be 60-95 DEG C, preferably 70-80 DEG C,
Reaction time is 2-4h.
Further, the acid of the adjusting pH value in step c is phosphoric acid, and the purpose pH value finally adjusted is 2-3.
Further, the oxidant in step c is hydrogen peroxide or ozone.
The beneficial effects of the present invention are: 1, this method is to fix the industrial wastewater of phosphorus content as phosphorus source, by with source of iron
With liquid alkaline in specific conditioned response, ferric phosphate presoma is obtained, the presoma is subsequent to concentrate synthesis ferric phosphate, preparation process
It is simple and convenient, reduce cost of human and material resources；2, fundamentally solve current ferric phosphate washes generate a large amount of solid wastes,
The problems such as causing environmental pollution and processing solid waste valuableness expense, realizes the recycling of phosphor resource in washes；3, it is prepared
Battery-grade iron phosphate sample impurity content be lower than 50ppm, can be used as battery-grade iron phosphate lithium raw materials for production, warp with higher
Ji benefit.
Specific embodiment
In order to deepen the understanding of the present invention, the present invention will be described in further detail with reference to the examples below, the embodiment
For explaining only the invention, it does not restrict the protection scope of the present invention.
Embodiment 1
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: adding flocculant or complexing agent into phosphorous industrial wastewater and clean, after to the work after removal of impurities
Industry waste water carries out filters pressing and obtains the industrial wastewater that phosphorous mass fraction is 7000-8000ppm；
B, it synthesizes ferric phosphate presoma: ferrous sulfate is added in step a in finally obtained industrial wastewater, wherein be added
The ratio of the amount of phosphorus in the amount and industrial wastewater of iron ion in ferrous sulfate is 1:1-1.8:1, and liquid alkaline is added, obtains muddiness
Liquid is then added alkali and adjusts reaction pH to 8.5, and fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Value is then added oxidant, redox reaction occurs, high-purity phosphate dihydrate iron is prepared in heat preservation 4h at 75 DEG C to 2.0；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 650
℃。
Embodiment 2
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: adding flocculant or complexing agent into phosphorous industrial wastewater and clean, after to the work after removal of impurities
Industry waste water carries out filters pressing and obtains the industrial wastewater that phosphorous mass fraction is 5000-6000ppm；
B, it synthesizes ferric phosphate presoma: ferrous sulfate is added in step a in finally obtained industrial wastewater, wherein be added
The ratio of the amount of phosphorus in the amount and industrial wastewater of iron ion in ferrous sulfate is 1.5:1, and liquid alkaline is added, obtains turbid solution,
Alkali is then added and adjusts reaction pH to 7.5, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Value is then added oxidant, redox reaction occurs, high-purity phosphate dihydrate iron is prepared in heat preservation 4h at 75 DEG C to 2.0；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 650
℃。
Embodiment 3
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: adding flocculant or complexing agent into phosphorous industrial wastewater and clean, after to the work after removal of impurities
Industry waste water carries out filters pressing and obtains the industrial wastewater that phosphorous mass fraction is 5000-6000ppm；
B, it synthesizes ferric phosphate presoma: ferrous sulfate is added in step a in finally obtained industrial wastewater, wherein be added
The ratio of the amount of phosphorus in the amount and industrial wastewater of iron ion in ferrous sulfate is 1.5:1, and liquid alkaline is added, obtains turbid solution,
Alkali is then added and adjusts reaction pH to 7.0, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Value is then added oxidant, redox reaction occurs, high-purity phosphate dihydrate iron is prepared in heat preservation 4h at 75 DEG C to 2.0；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 650
℃。
Embodiment 4
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: adding flocculant or complexing agent into phosphorous industrial wastewater and clean, after to the work after removal of impurities
Industry waste water carries out filters pressing and obtains the industrial wastewater that phosphorous mass fraction is 5000-6000ppm；
B, it synthesizes ferric phosphate presoma: ferrous sulfate is added in step a in finally obtained industrial wastewater, wherein be added
The ratio of the amount of phosphorus in the amount and industrial wastewater of iron ion in ferrous sulfate is 1.5:1, and liquid alkaline is added, obtains turbid solution,
Alkali is then added and adjusts reaction pH to 6.5, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Value is then added oxidant, redox reaction occurs, high-purity phosphate dihydrate iron is prepared in heat preservation 4h at 75 DEG C to 2.0；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 650
℃。
Embodiment 5
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: adding flocculant or complexing agent into phosphorous industrial wastewater and clean, after to the work after removal of impurities
Industry waste water carries out filters pressing and obtains the industrial wastewater that phosphorous mass fraction is 5000-6000ppm；
B, it synthesizes ferric phosphate presoma: ferrous sulfate is added in step a in finally obtained industrial wastewater, wherein be added
The ratio of the amount of phosphorus in the amount and industrial wastewater of iron ion in ferrous sulfate is 1.5:1, and liquid alkaline is added, obtains turbid solution,
Alkali is then added and adjusts reaction pH to 5.5, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Value is then added oxidant, redox reaction occurs, high-purity phosphate dihydrate iron is prepared in heat preservation 4h at 75 DEG C to 2.0；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 650
℃。
Embodiment 6
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: adding flocculant or complexing agent into phosphorous industrial wastewater and clean, after to the work after removal of impurities
Industry waste water carries out filters pressing and obtains the industrial wastewater that phosphorous mass fraction is 5000-6000ppm；
B, it synthesizes ferric phosphate presoma: ferrous sulfate is added in step a in finally obtained industrial wastewater, wherein be added
The ratio of the amount of phosphorus in the amount and industrial wastewater of iron ion in ferrous sulfate is 1.45:1, and liquid alkaline is added, obtains turbid solution,
Alkali is then added and adjusts reaction pH to 7, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Value is then added oxidant, redox reaction occurs, high-purity phosphate dihydrate iron is prepared in heat preservation 4h at 75 DEG C to 2.0；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 650
℃。
Embodiment 7
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: adding flocculant or complexing agent into phosphorous industrial wastewater and clean, after to the work after removal of impurities
Industry waste water carries out filters pressing and obtains the industrial wastewater that phosphorous mass fraction is 5000-6000ppm；
B, it synthesizes ferric phosphate presoma: ferrous sulfate is added in step a in finally obtained industrial wastewater, wherein be added
The ratio of the amount of phosphorus in the amount and industrial wastewater of iron ion in ferrous sulfate is 1.35:1, and liquid alkaline is added, obtains turbid solution,
Alkali is then added and adjusts reaction pH to 7, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Value is then added oxidant, redox reaction occurs, high-purity phosphate dihydrate iron is prepared in heat preservation 4h at 75 DEG C to 2.0；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 650
℃。
Embodiment 8
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: adding flocculant or complexing agent into phosphorous industrial wastewater and clean, after to the work after removal of impurities
Industry waste water carries out filters pressing and obtains the industrial wastewater that phosphorous mass fraction is 5000-6000ppm；
B, it synthesizes ferric phosphate presoma: ferrous sulfate is added in step a in finally obtained industrial wastewater, wherein be added
The ratio of the amount of phosphorus in the amount and industrial wastewater of iron ion in ferrous sulfate is 1.25:1, and liquid alkaline is added, obtains turbid solution,
Alkali is then added and adjusts reaction pH to 7, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Value is then added oxidant, redox reaction occurs, high-purity phosphate dihydrate iron is prepared in heat preservation 4h at 75 DEG C to 2.0；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 650
℃。
Embodiment 9
A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater, specific steps are as follows:
A, determine phosphorus source: adding flocculant or complexing agent into phosphorous industrial wastewater and clean, after to the work after removal of impurities
Industry waste water carries out filters pressing and obtains the industrial wastewater that phosphorous mass fraction is 5000-6000ppm；
B, it synthesizes ferric phosphate presoma: ferrous sulfate is added in step a in finally obtained industrial wastewater, wherein be added
The ratio of the amount of phosphorus in the amount and industrial wastewater of iron ion in ferrous sulfate is 1.15:1, and liquid alkaline is added, obtains turbid solution,
Alkali is then added and adjusts reaction pH to 7, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Value is then added oxidant, redox reaction occurs, high-purity phosphate dihydrate iron is prepared in heat preservation 4h at 75 DEG C to 2.0；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 650
℃。
After the phosphorous industrial wastewater of above-described embodiment 1- embodiment 9 mentions phosphorus synthesis ferric phosphate presoma, Phosphorus From Wastewater residual
Amount is respectively 41ppm, 0.9ppm, 0.8ppm, 10ppm, 95ppm, 0 ppm, 92 ppm, 314 ppm and 638 ppm；
The yield of the battery-grade iron phosphate synthesized in above-described embodiment 1- embodiment 9 is calculated, calculation formula are as follows: produce
The molal quantity of molal quantity/addition iron of iron, calculated result are as shown in the table in rate=actual product:
| Serial number | Yield % |
| Embodiment 1 | 100.2 |
| Embodiment 2 | 98.2 |
| Embodiment 3 | 95.5 |
| Embodiment 4 | 91.2 |
| Embodiment 5 | 89.2 |
| Embodiment 6 | 97.2 |
| Embodiment 7 | 98.5 |
| Embodiment 8 | 98.3 |
| Embodiment 9 | 99.5 |
The battery-grade iron phosphate being prepared in Example 2 carries out the detection of impurity content, inspection by atomic absorption spectrography (AAS)
Survey instrument are as follows: WFX-30B, testing result are as shown in the table:
Claims (8)
1. a kind of extract the method that phosphoric acid prepares battery-grade iron phosphate in industrial wastewater, which is characterized in that concrete operation step is such as
Under:
A, determine phosphorus source: into phosphorous industrial wastewater add flocculant clean, after to after removal of impurities industrial wastewater carry out
Filters pressing obtains the industrial wastewater that phosphorous mass fraction is 4000-8000ppm；
B, it synthesizes ferric phosphate presoma: a certain amount of source of iron being added in step a in finally obtained industrial wastewater, the iron
The ratio of the phosphorus content in iron content and industrial wastewater in source be 1:1-1.8:1, be added liquid alkaline, obtain turbid solution, then plus
Enter alkali and adjust reaction pH to 2-11, fast reaction obtains ferric phosphate presoma at room temperature, and filter cake is obtained by filtration；
C, it synthesizes ferric phosphate: the ferric phosphate presoma filter cake being prepared in step b being added in reaction kettle, acid for adjusting pH is added
Oxidant is then added in value, and redox reaction occurs, and high-purity phosphate dihydrate iron is prepared in high temperature；
D, it calcines: the phosphate dihydrate iron being prepared in step c being calcined to obtain battery-grade iron phosphate, the temperature of calcining is 600-
700℃。
2. the method that phosphoric acid prepares battery-grade iron phosphate in a kind of extraction industrial wastewater according to claim 1, feature
It is, the flocculant in step a is PAC or PAM.
3. the method that phosphoric acid prepares battery-grade iron phosphate in a kind of extraction industrial wastewater according to claim 1, feature
It is, the source of iron in step b is the solution containing ferrous ion.
4. the method that phosphoric acid prepares battery-grade iron phosphate in a kind of extraction industrial wastewater according to claim 1, feature
It is, the liquid alkaline in step b is sodium hydroxide solution or ammonia spirit.
5. the method that phosphoric acid prepares battery-grade iron phosphate in a kind of extraction industrial wastewater according to claim 1, feature
It is, the reaction time of fast reaction is 10-100min in step b.
6. the method that phosphoric acid prepares battery-grade iron phosphate in a kind of extraction industrial wastewater according to claim 1, feature
Be, the high temperature in step c be 60-95 DEG C, preferably 70-80 DEG C,
Reaction time is 2-4h.
7. the method that phosphoric acid prepares battery-grade iron phosphate in a kind of extraction industrial wastewater according to claim 1, feature
It is, the acid of the adjusting pH value in step c is phosphoric acid, and the purpose pH value finally adjusted is 2-3.
8. the method that phosphoric acid prepares battery-grade iron phosphate in a kind of extraction industrial wastewater according to claim 1, feature
It is, the oxidant in step c is hydrogen peroxide or ozone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910412494.7A CN110255520A (en) | 2019-05-17 | 2019-05-17 | A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910412494.7A CN110255520A (en) | 2019-05-17 | 2019-05-17 | A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110255520A true CN110255520A (en) | 2019-09-20 |
Family
ID=67913294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910412494.7A Pending CN110255520A (en) | 2019-05-17 | 2019-05-17 | A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110255520A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110436428A (en) * | 2019-07-08 | 2019-11-12 | 湖南雅城新材料有限公司 | A kind of preparation method of sheet-form iron phosphate, sheet-form iron phosphate obtained and its application |
| CN115124013A (en) * | 2022-08-05 | 2022-09-30 | 衢州华友钴新材料有限公司 | Preparation method of battery-grade ferric orthophosphate |
| CN115448276A (en) * | 2022-08-16 | 2022-12-09 | 四川龙蟒磷化工有限公司 | Battery anode material precursor and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000037692A (en) * | 1998-07-23 | 2000-02-08 | Tokyu Car Corp | Method and apparatus for dephosphorizing and desalting industrial waste water |
| JP2008195558A (en) * | 2007-02-09 | 2008-08-28 | Sharp Corp | Method for recovering resource |
| CN106829906A (en) * | 2017-03-13 | 2017-06-13 | 成都育芽科技有限公司 | A kind of preparation method of new energy battery-grade iron phosphate |
| CN108609595A (en) * | 2018-05-10 | 2018-10-02 | 湖南雅城新材料有限公司 | Ferric phosphate and its preparation method and application |
| CN108946694A (en) * | 2018-08-14 | 2018-12-07 | 南通百川新材料有限公司 | A kind of hydrothermal synthesis method of battery-grade iron phosphate |
| CN109368612A (en) * | 2018-11-30 | 2019-02-22 | 乳源东阳光磁性材料有限公司 | Method for preparing battery-grade iron phosphate by using iron phosphate production wastewater and iron phosphate prepared by method |
-
2019
- 2019-05-17 CN CN201910412494.7A patent/CN110255520A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000037692A (en) * | 1998-07-23 | 2000-02-08 | Tokyu Car Corp | Method and apparatus for dephosphorizing and desalting industrial waste water |
| JP2008195558A (en) * | 2007-02-09 | 2008-08-28 | Sharp Corp | Method for recovering resource |
| CN106829906A (en) * | 2017-03-13 | 2017-06-13 | 成都育芽科技有限公司 | A kind of preparation method of new energy battery-grade iron phosphate |
| CN108609595A (en) * | 2018-05-10 | 2018-10-02 | 湖南雅城新材料有限公司 | Ferric phosphate and its preparation method and application |
| CN108946694A (en) * | 2018-08-14 | 2018-12-07 | 南通百川新材料有限公司 | A kind of hydrothermal synthesis method of battery-grade iron phosphate |
| CN109368612A (en) * | 2018-11-30 | 2019-02-22 | 乳源东阳光磁性材料有限公司 | Method for preparing battery-grade iron phosphate by using iron phosphate production wastewater and iron phosphate prepared by method |
Non-Patent Citations (3)
| Title |
|---|
| 彭爱国等: "电池级超微细磷酸铁的制备", 《武汉工程大学学报》 * |
| 李雅: "分步沉淀去除磷酸铁生产废水中的磷酸根和硫酸根", 《化工环保》 * |
| 赵欢: "高磷酸性废水回收处理试验研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110436428A (en) * | 2019-07-08 | 2019-11-12 | 湖南雅城新材料有限公司 | A kind of preparation method of sheet-form iron phosphate, sheet-form iron phosphate obtained and its application |
| CN115124013A (en) * | 2022-08-05 | 2022-09-30 | 衢州华友钴新材料有限公司 | Preparation method of battery-grade ferric orthophosphate |
| CN115124013B (en) * | 2022-08-05 | 2023-08-29 | 衢州华友钴新材料有限公司 | Preparation method of battery-grade ferric orthophosphate |
| CN115448276A (en) * | 2022-08-16 | 2022-12-09 | 四川龙蟒磷化工有限公司 | Battery anode material precursor and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102101662B (en) | Preparation method and product of ferric phosphate | |
| CN110255520A (en) | A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater | |
| CN110482512A (en) | A kind of preparation method of battery-grade iron phosphate | |
| CN111847416A (en) | Method for preparing hydrated iron phosphate from ferrous sulfate serving as titanium dioxide byproduct | |
| CN105417771A (en) | Efficient-nitrogen-and-phosphorus-removing and resource recycling technology and device for iron phosphate production wastewater | |
| CN110589788A (en) | Method for recycling wastewater in battery-grade iron phosphate synthesis process | |
| CN111498940B (en) | Separation treatment method of phosphorus-containing and fluorine-containing phosphogypsum washing waste liquid | |
| CN105600763B (en) | A kind of method that fluoride salt method of purification produces industrial monoammonium phosphate | |
| WO2024055467A1 (en) | Method for preparing iron phosphate by using phosphorite and ferrous sulfate | |
| CN110342483A (en) | A method of battery-grade iron phosphate is prepared using lithium phosphate waste material | |
| CN114906829B (en) | Method for preparing battery-grade ferric phosphate by adopting agricultural-grade wet-process phosphoric acid | |
| KR102243162B1 (en) | A solid fertilizer manufacturing method by ammonia including hydrofluoric acid waste water | |
| CN106278390A (en) | A kind of phosphoric acid by wet process acid sludge comprehensive reutilization method | |
| CN113336356A (en) | Phosphogypsum leachate recycling treatment and utilization method | |
| CN111333050B (en) | Combined production of magnesium ammonium phosphate and MgCO from phosphorus tailings and phosphogypsum 3 And by-product NH 4 Cl process | |
| CN106745631B (en) | Method for removing fluorine and arsenic in tungsten smelting wastewater | |
| CN107416863B (en) | Method for preparing industrial-grade ammonium salt from wastewater generated in iron phosphate production | |
| CN107686192A (en) | A kind of phosphorous and Ammonia-nitrogen wastewater treatment technology | |
| CN102502715B (en) | Method for reclaiming reagent-grade anhydrous sodium sulfate from basic nickel carbonate production waste liquor | |
| CN106830416A (en) | A kind of method that guanite precipitation method process desulfurization wastewater | |
| CN115340074B (en) | Method and system for preparing phosphoric acid by utilizing titanium white waste acid | |
| CN105347321A (en) | Method for producing ammonium phosphate by using low-grade low-concentration raffinate acid | |
| CN115490365A (en) | Method for comprehensively treating alkaline uranium-containing fluorine-containing wastewater through uranium conversion | |
| CN108328592A (en) | A kind of technique for using phosphoric acid by wet process to produce magnesium monohydrogen phosphate for raw material | |
| CN104591110A (en) | Method for preparing low-sulfur-content calcium dihydrogen phosphate by concentrating wet-process phosphoric acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190920 |