CN106904587A - A kind of preparation method of LiFePO 4 - Google Patents
A kind of preparation method of LiFePO 4 Download PDFInfo
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- CN106904587A CN106904587A CN201710145016.5A CN201710145016A CN106904587A CN 106904587 A CN106904587 A CN 106904587A CN 201710145016 A CN201710145016 A CN 201710145016A CN 106904587 A CN106904587 A CN 106904587A
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- tail gas
- lifepo
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- 229910010707 LiFePO 4 Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000007789 gas Substances 0.000 claims abstract description 97
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 84
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 42
- 238000005245 sintering Methods 0.000 claims abstract description 42
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000005202 decontamination Methods 0.000 claims abstract description 26
- 230000003588 decontaminative effect Effects 0.000 claims abstract description 26
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 24
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 24
- 239000002250 absorbent Substances 0.000 claims abstract description 21
- 230000002745 absorbent Effects 0.000 claims abstract description 21
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 21
- 239000003337 fertilizer Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 40
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 38
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 28
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 26
- 229910052744 lithium Inorganic materials 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 24
- 239000003463 adsorbent Substances 0.000 claims description 23
- 239000002994 raw material Substances 0.000 claims description 21
- 238000005507 spraying Methods 0.000 claims description 20
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 19
- 229910052742 iron Inorganic materials 0.000 claims description 19
- 229910052698 phosphorus Inorganic materials 0.000 claims description 19
- 239000011574 phosphorus Substances 0.000 claims description 19
- 238000003746 solid phase reaction Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 15
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 239000007921 spray Substances 0.000 claims description 12
- 239000010457 zeolite Substances 0.000 claims description 12
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 11
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 11
- 239000002562 thickening agent Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910021536 Zeolite Inorganic materials 0.000 claims description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 10
- 230000001404 mediated effect Effects 0.000 claims description 10
- 238000001179 sorption measurement Methods 0.000 claims description 10
- 239000008187 granular material Substances 0.000 claims description 8
- 238000004898 kneading Methods 0.000 claims description 8
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 7
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 239000001119 stannous chloride Substances 0.000 claims description 7
- 235000011150 stannous chloride Nutrition 0.000 claims description 7
- 239000010455 vermiculite Substances 0.000 claims description 7
- 229910052902 vermiculite Inorganic materials 0.000 claims description 7
- 235000019354 vermiculite Nutrition 0.000 claims description 7
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 6
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 6
- 229960000892 attapulgite Drugs 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 229910052625 palygorskite Inorganic materials 0.000 claims description 6
- 238000005373 pervaporation Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 5
- 229940062993 ferrous oxalate Drugs 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims description 5
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 4
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 238000000746 purification Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 230000000505 pernicious effect Effects 0.000 abstract description 2
- 238000003836 solid-state method Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 230000009102 absorption Effects 0.000 description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 239000008103 glucose Substances 0.000 description 6
- 229910000904 FeC2O4 Inorganic materials 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical class ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229910052493 LiFePO4 Inorganic materials 0.000 description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 3
- IGEZMQWPBDNNPS-UHFFFAOYSA-N B.CO Chemical compound B.CO IGEZMQWPBDNNPS-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 229940116007 ferrous phosphate Drugs 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 229910000155 iron(II) phosphate Inorganic materials 0.000 description 2
- SDEKDNPYZOERBP-UHFFFAOYSA-H iron(ii) phosphate Chemical compound [Fe+2].[Fe+2].[Fe+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SDEKDNPYZOERBP-UHFFFAOYSA-H 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000012913 prioritisation Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- 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
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
- C01C1/242—Preparation from ammonia and sulfuric acid or sulfur trioxide
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/25—Coated, impregnated or composite adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/502—Carbon monoxide
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Treating Waste Gases (AREA)
Abstract
A kind of preparation method of LiFePO 4, described method carries out high-efficient purification treatment to the tail gas produced in LiFePO 4 high temperature solid-state method production process, achieves good technique effect and considerable economy, environmental benefit.The present invention is processed the ammonia in tail gas using ammonia decontamination tower; the chemical fertilizer containing ammonium sulfate is finally given for selling; the ammonia composition in roasting process is effectively utilized, the cost of large-scale production is reduced, environment has not only been protected but also has been achieved objective economic benefit.The present invention is exchanged heat using nitrogen with high-temperature tail gas, has preheated nitrogen in advance before sintering, effectively make use of tail gas heat quantity, improves reaction rate and product purity, saves energy consumption, reduce further energy consumption.The present invention removes carbon monoxide in tail gas using absorbent for carbon monooxide, further reduces pernicious gas in tail gas, and environmental benefit is obvious.
Description
Technical field
It is application for a patent for invention the invention belongs to field of lithium ion battery《A kind of lithium ion battery material LiFePO 4
Preparation method》（Application number：2015102532337）Division.Specifically related to a kind of preparation method of LiFePO 4, the method
Tail gas to being produced in LiFePO 4 production process carries out high-efficient purification treatment, turn waste into wealth with considerable economic benefit and
Environmental benefit.
Background technology
Lithium ion battery has been widely used for mobile communication, notebook computer, shooting as high-energy-density electrochmical power source
The fields such as machine, camera, portable instrument, be also various countries study energetically electric automobile, space power system it is first-selected supporting
Power supply, the first-selection as fungible energy source.
LiFePO 4 is lithium ion battery electrode material recently newly developed, is mainly used in power lithium-ion battery, is made
For positive active material is used, custom is also referred to as LiFePO4, its chemical formula in this area：LiFePO4。
The advantage as electrode material of LiFePO 4 is：1. high-energy-density, its theoretical specific capacity is 170mAh/
G, product actual specific capacity is more than 150 mAh/g.2. security, is current safest anode material for lithium-ion batteries；And
And without any harmful heavy metal element.3. long lifespan, under the conditions of 100%DOD, can with discharge and recharge 2000 times with
On, this is that reason LiFePO4 lattice stability is good, and the insertion of lithium ion and the influence deviate to lattice are little, so have good
Good invertibity.4. memory-less effect.5. excellent electrical property, the lithium battery of lithium iron phosphate cathode material, it is possible to use big times
Rate charges, and can most be full of battery in 30 minutes soon now.
The synthetic method of LiFePO 4 has solid sintering technology, hydro-thermal method, sol-gel process, reversed phase lithium inserting process, electrolysis to burn
Connection etc..Solid sintering technology prepares LiFePO 4 has that price is low, pollute that small, equipment service efficiency is high, sample electrochemistry
The advantages of good, tap density of energy is big, heavy-current discharge performance is preferable.It is industrial to prepare LiFePO 4 using solid sintering technology
One of main method of use.But harmful gases can be produced in solid-phase sintering process, main component has ammonia, titanium dioxide
The pernicious gases such as carbon, carbon monoxide.
The tail not produced in suitable purification above-mentioned solid phase sintering process LiFePO 4 production process in the prior art
The processing method of gas, if the directly outer above-mentioned tail gas of discharge, significant damage is brought to environment.Therefore solid phase method prepares ferrous phosphate
The tail gas clean-up produced during lithium is technical problem urgently to be resolved hurrily in lithium ion battery preparation field.
The content of the invention
It is an object of the invention to the shortcoming for overcoming prior art to exist, there is provided a kind of preparation method of LiFePO 4,
Tail gas to being produced in LiFePO 4 production process carries out high-efficient purification treatment, using ammonia decontamination tower to the ammonia in tail gas
Processed, and finally given the chemical fertilizer containing ammonium sulfate, carbon monoxide is removed using absorbent for carbon monooxide.
The method of the present invention has the advantages that purification efficiency is high, turns waste into wealth, and realizes preferably economic benefit and Environmental Effect
Benefit.
Technical scheme is as follows.
A kind of LiFePO 4 preparation method, it is characterised in that comprise the following steps：
The raw material high-temperature solid phase reaction method that step (1), selection prepare LiFePO 4 prepares LiFePO 4 product.
Step (2), by step (1) solid phase reaction produce high-temperature tail gas be passed through tubular heat exchanger, after heat exchange, tail gas
Temperature is reduced to 50 DEG C.
Step (3), the tail gas after step (2) treatment is passed through ammonia decontamination tower and is processed.Tail gas is by positioned at ammonia
The gas feed of purifying column tower body middle and lower part enters in tower, with the acid solution spraying layer of tower body inner upper spray and lower sulfuric acid is sour
Liquid contact absorbs ammonia and forms ammonium sulfate, and tail gas after the demister demisting positioned at acid solution spraying layer top by flowing through tower body top
Leave ammonia decontamination tower in the gas outlet in portion.Using circulating pump will be located at tower body inner lower collecting tank in collect liquid and
Fresh sulfuric acid acid solution in fresh acid storage is delivered to acid solution spraying layer and is circulated spray.
Step (4), terminate circulated sprinkling after, the liquid pumping collected the collecting tank of ammonia decontamination tower using draw-off pump is extremely
Thickener, in thickener, ammonium sulfate obtains the fertilizer of liquid containing ammonium sulfate after pervaporation, precipitation, filtering, drying.
Step (5), the tail gas of gas outlet that step (3) is flowed out at the top of tower body is delivered to comprising an oxidation using booster pump
The carbon monoxide adsorption device of carbon adsorbent, operating pressure is 1.5Mpa.The composition of the absorbent for carbon monooxide is：By weight
Component, is 38 parts of stannous chloride, 10 parts of montmorillonite, 18 parts of Cu-ZSM-5 types zeolite, 8 parts of aluminium hydroxide, 8 parts of vermiculite and concave convex rod
28 parts of stone.
Step (6), by step (5) treatment after tail gas by emptier empty.
Raw material described in above-mentioned step (1) is source of iron, phosphorus source, lithium source, and specific source of iron, phosphorus source, lithium source are respectively grass
Sour ferrous iron, ammonium dihydrogen phosphate, lithium carbonate；Described high-temperature solid phase reaction method is：According to source of iron：Phosphorus source：Lithium source=1:1:1 rubs
You grind ratio batch mixing；Calcined under logical nitrogen environment at 600 DEG C~700 DEG C during material is gone into pre-burning stove after mill-drying,
Sintering time is 1~5 hour, once sintered that ball milling is carried out to material afterwards, then carries out double sintering, and the temperature of double sintering is
650 DEG C~750 DEG C, sintering time is 1~5 hour, and double sintering atmosphere is nitrogen；Classification packaging, obtains ferrous phosphate afterwards
Lithium product.
In prioritization scheme, for once sintered and double sintering nitrogen as low-temperature heat exchange fluid in the step
(2) tubular heat exchanger is exchanged heat with high-temperature tail gas.
The preparation method of above-mentioned absorbent for carbon monooxide is：Cu-ZSM-5 types zeolite is toasted 20 points in 100 DEG C of baking ovens
Clock, it is standby.Batch mixing is obtained after each raw material is mixed, batch mixing is added into kneader, add 10 parts of water and 5 parts of ethanol to enter to kneader
Row is mediated, and 10 minutes kneading times, obtains kneading material.Material will be mediated and is processed into spheric granules, spheric granules is put into baking oven,
Taken out within 180 minutes in 300 DEG C of bakings, after after natural cooling, be made absorbent for carbon monooxide.
In prioritization scheme, tail gas is by after carbon monoxide adsorption device absorption, CO contents are less than 20ppm in tail gas.
It is once sintered react including：
FeC2O4·H2O+2NH4H2PO4+Li2CO3=2LiFePO4+2NH3↑+3CO2↑+2CO↑+7H2O↑。
In this area, when high temperature solid-state preparation method prepares LiFePO 4, it is also possible to add carbon coating agent, typically grape
Sugar, glucose sugar addition can be：Glucose is with the molar ratio of lithium source： 0.2-0.5:1.
In the present invention, for further save energy, accomplish Waste Heat Reuse, the present invention dexterously devises high using nitrogen
Warm tail gas continues to exchange heat, and has preheated nitrogen in advance before sintering, improves reaction rate and product purity, and reduce tail gas
Heat, is easy to subsequent treatment.Therefore currently preferred heat-exchange method is：Make for once sintered and double sintering nitrogen
It is low-temperature heat exchange fluid in the step（2）Tubular heat exchanger exchanged heat with high-temperature tail gas.
Due to the high risk of CO in the present invention, in order to further reduce the concentration of CO, the present invention can be selected preferably
CO adsorbents.Described preferred adsorbent be with stannous chloride, montmorillonite, Cu-ZSM-5 types zeolite, aluminium hydroxide, vermiculite,
And attapulgite is raw material preparation；Described preparation method includes：It is stannous chloride 38-42 parts, illiteracy that component by weight is weighed
De- 10-15 parts of soil, 18-23 parts, aluminium hydroxide 8-10 parts, vermiculite 8-10 parts and attapulgite 28-35 parts of Cu-ZSM-5 type zeolites,
Cu-ZSM-5 types zeolite is toasted -150 minutes 20 minutes in 100 DEG C of baking ovens, it is standby；Batch mixing is obtained after each raw material is mixed, will be mixed
Material adds kneader, adds 10-15 parts of water and 5-10 parts of ethanol to be mediated to kneader, kneading time 10-15 minutes, obtains
Mediate material；Material will be mediated and be processed into spheric granules, spheric granules is put into baking oven, in 300 DEG C of -320 DEG C of baking 180-200
Minute take out, after after natural cooling, being made CO adsorbents.
When adsorbing for 50 DEG C, CO CO absorptions under 30mmHg are 3.57mmol/ to the CO adsorbents for preparing of the invention
G, is 4.13mmol/g during 25 DEG C of absorption.When being desorbed at 100 DEG C, more than 90% CO can be desorbed out, 150 DEG C of desorptions
When, more than 95% CO can be desorbed out.When in 50 DEG C of absorption N2When, N2In 230mmHg, adsorbance is only 0.64mmol/
g.Therefore CO adsorbents of the invention have good absorption selection activity.The raw material of above-mentioned preferred CO adsorbents of the invention
Stannous chloride and Cu-ZSM-5 type zeolites have been used simultaneously, the less technology of adsorbent adsorbance of the prior art has been overcome
Problem, the selectivity that the adsorbance and absorption that improve adsorbent is used in combination of the two.Meanwhile, the illiteracy that the present invention is used takes off
The gas adsorbability materials such as soil, vermiculite and attapulgite have special pore passage structure.According to proportioning of the invention and side
Method prepare after, between their pore structure mutually left and right, can sorbing carbon monoxide, turn avoid the absorption to nitrogen so that
CO after absorption is easily desorbed, and improves treatment effect.Therefore CO adsorbents of the invention have good technique effect.
The present invention achieves excellent technique effect.
Technical scheme overcomes the technical problem of prior art presence, and effective treatment has been carried out to tail gas, takes
Obtained good technique effect and considerable economy, environmental benefit.
LiFePO 4 prepared by present invention production has that chemical property is good, tap density big, heavy-current discharge performance
Preferably the advantages of.
The present invention carries out high-efficient purification treatment to the tail gas produced in LiFePO 4 production process, uses ammonia decontamination tower
Ammonia in tail gas is processed.Described ammonia decontamination tower is equipment commonly used in the trade, and tower body, acid solution are included its structure more
Groove, the acid solution spraying layer positioned at tower body inner upper, the demister positioned at acid solution spraying layer top and inside tower body
The collecting tank of bottom.The present invention finally gives the chemical fertilizer containing ammonium sulfate for selling, and is effectively utilized the ammonia in roasting process
Composition, reduces the cost of large-scale production, the cost of increased ammonia absorber obtained due to the sale of ammonium sulfate fertilizer
Rational balance, had not only protected environment but also had achieved objective economic benefit.
The present invention continues to exchange heat due to cleverly devising using nitrogen high-temperature tail gas, has preheated nitrogen in advance before sintering
Gas, effectively make use of tail gas heat quantity, improve reaction rate and product purity, save energy consumption, reduce further into
This.
The present invention removes carbon monoxide in tail gas using absorbent for carbon monooxide, further reduces harmful gas in tail gas
Body, environmental benefit is obvious.The preferred absorbent for carbon monooxide that especially present invention is developed so that CO contents are less than in tail gas
10ppm and the adsorbent are easy to regeneration, and desorption is simple, and service life is longer, can stablize adsorption-desorption run 1000 times with
On.
Specific embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1：
A kind of preparation method of LiFePO 4, comprises the following steps：
Step（1）, selection prepares the raw material high-temperature solid phase reaction method of LiFePO 4 and prepares LiFePO 4 product；Step
（1）Described in raw material be source of iron, phosphorus source, lithium source, specific source of iron, phosphorus source, lithium source be respectively ferrous oxalate, ammonium dihydrogen phosphate,
Lithium carbonate；Described high-temperature solid phase reaction method is：According to source of iron：Phosphorus source：Lithium source=1:1:1 molar ratio batch mixing grinding；Grinding
Material is gone to after drying calcined under leading to nitrogen environment at 600 DEG C in pre-burning stove, sintering time is 1 hour, it is once sintered it
Ball milling is carried out to material afterwards, then carries out double sintering, the temperature of double sintering is 650 DEG C, and sintering time is 1 hour, secondary burning
Knot atmosphere is nitrogen；Classification packaging, obtains LiFePO 4 product afterwards；It is once sintered react including：
FeC2O4·H2O+2NH4H2PO4+Li2CO3=2LiFePO4+2NH3↑+3CO2↑+2CO↑+7H2O↑；
Step（2）, by step（1）The tail gas that middle solid phase reaction is produced is passed through tubular heat exchanger, after heat exchange, exhaust temperature reduction
To 50 DEG C；
Step（3）, by step（2）Tail gas after treatment is passed through ammonia decontamination tower and is processed；Tail gas is by positioned at ammonia decontamination
The gas feed of tower tower body middle and lower part enters in tower, with the acid solution spraying layer of tower body inner upper spray and under sulfuric acid acid solution connect
Touch and absorb ammonia formation ammonium sulfate, tail gas is flowed through at the top of tower body by after the demister demisting positioned at acid solution spraying layer top
Leave ammonia decontamination tower in gas outlet；The liquid and fresh collected in the collecting tank of tower body inner lower will be located at using circulating pump
Fresh sulfuric acid acid solution in acid storage is delivered to acid solution spraying layer and is circulated spray；
Step（4）, terminate circulated sprinkling after, the liquid pumping collected the collecting tank of ammonia decontamination tower using draw-off pump is to concentrating
Groove, in thickener, ammonium sulfate obtains liquid containing ammonium sulfate fertilizer after pervaporation, precipitation, filtering, drying；Liquid containing ammonium sulfate fertilizer
The weight nitroxide content of material is 16%, and sulphur weight content is 18.0%；
Step（5）, by step（3）The tail gas of the gas outlet at the top of outflow tower body is delivered to using booster pump to be inhaled comprising carbon monoxide
Attached dose of carbon monoxide adsorption device, operating pressure is 1.5Mpa；Wherein described absorbent for carbon monooxide is in art
Conventional adsorbent；CO contents are 20ppm in tail gas after absorption；
Step（6）, by step（5）Tail gas after treatment is emptied by emptier.
It is pointed out that the step（1）Technical purpose be that selection prepares the raw material of LiFePO 4 and carries out solid phase
Reaction prepares LiFePO 4 product, and preparation technology parameter therein is prior art, namely raw material is solid in the prior art
Source of iron, phosphorus source, lithium source, method are that the preparation technology of secondary clacining may be incorporated for the present invention, and the present embodiment is only one specific
Implementation method, however it is not limited to above-mentioned technological parameter.
Absorbent for carbon monooxide described in embodiment 1 is commercially available prod, MCO-1 type absorbent for carbon monooxide（Shandong hundred million
Coal mechanized equipment Manufacturing Co., Ltd sells product）.
Embodiment 2：
A kind of preparation method of LiFePO 4, comprises the following steps：
Step（1）, selection prepares the raw material high-temperature solid phase reaction method of LiFePO 4 and prepares LiFePO 4 product.Step
（1）Described in raw material be source of iron, phosphorus source, lithium source, specific source of iron, phosphorus source, lithium source be respectively ferrous oxalate, ammonium dihydrogen phosphate,
Lithium carbonate.Described high-temperature solid phase reaction method is：According to source of iron：Phosphorus source：Lithium source=1:1:1 molar ratio batch mixing grinding.Grinding
Material is gone to after drying calcined under leading to nitrogen environment at 700 DEG C in pre-burning stove, sintering time is 5 hours, it is once sintered it
Ball milling is carried out to material afterwards, then carries out double sintering, the temperature of double sintering is 750 DEG C, and sintering time is 5 hours, secondary burning
Knot atmosphere is nitrogen.Classification packaging, obtains LiFePO 4 product afterwards.It is once sintered react including：
FeC2O4·H2O+2NH4H2PO4+Li2CO3=2LiFePO4+2NH3↑+3CO2↑+2CO↑+7H2O↑。
Step（2）, by step（1）The high-temperature tail gas that middle solid phase reaction is produced are passed through tubular heat exchanger, after heat exchange, tail gas
Temperature is reduced to 50 DEG C.The low-temperature heat exchange fluid of heat exchange is for once sintered and double sintering nitrogen.
Step（3）, by step（2）Tail gas after treatment is passed through ammonia decontamination tower and is processed.Applied in the present embodiment
Acid solution is sulfuric acid acid solution.Tail gas is entered in tower by the gas feed of ammonia decontamination tower tower body middle and lower part, with tower body inner upper
Acid solution spraying layer spray and lower sulfuric acid acid solution contact absorbs ammonia and forms ammonium sulfate, tail gas passes through on acid solution spraying layer
Leave ammonia decontamination tower in the gas outlet flowed through at the top of tower body after the demister demisting in portion.Will be inside tower body using circulating pump
Fresh sulfuric acid acid solution in the liquid collected in the collecting tank of bottom and fresh acid storage is delivered to acid solution spraying layer and is followed
Ring spray is drenched.
Step（4）, terminate circulated sprinkling after, the liquid pumping collected the collecting tank of ammonia decontamination tower using draw-off pump is extremely
Thickener, in thickener, ammonium sulfate obtains liquid containing ammonium sulfate fertilizer after pervaporation, precipitation, filtering, drying.Sulfur acid
The weight nitroxide content of ammonium fertilizer is 16%, and sulphur weight content is 18.0%.
Step（5）, by step（3）The tail gas of the gas outlet at the top of outflow tower body is delivered to comprising an oxidation using booster pump
The carbon monoxide adsorption device of carbon adsorbent, operating pressure is 1.5Mpa.Wherein described absorbent for carbon monooxide is an oxidation
Carbon adsorbent A.CO contents are 10ppm in tail gas after absorption.
Step（6）, by step（5）Tail gas after treatment is emptied by emptier.
In embodiment 2, the preparation method of described absorbent for carbon monooxide A is：It is stannous chloride that component is weighed by weight
28 parts of 38 parts, 10 parts of montmorillonite, 18 parts of Cu-ZSM-5 types zeolite, 8 parts of aluminium hydroxide, 8 parts of vermiculite and attapulgite, by Cu-
ZSM-5 types zeolite is toasted 20 minutes in 100 DEG C of baking ovens, standby.Batch mixing is obtained after each raw material is mixed, batch mixing is added into kneader,
Add 10 parts of water and 5 parts of ethanol to be mediated to kneader, 10 minutes kneading times, obtain kneading material.Material will be mediated to add
Work globulate particle, baking oven is put into by spheric granules, is taken out within 180 minutes in 300 DEG C of bakings, after after natural cooling, being made an oxygen
Change carbon adsorbent A.
Embodiment 3：
A kind of preparation method of LiFePO 4, comprises the following steps：
Step（1）, selection prepares the raw material high-temperature solid phase reaction method of LiFePO 4 and prepares LiFePO 4 product.Step
（1）In, source of iron, phosphorus source, lithium source and carbon source are weighed, specific source of iron, phosphorus source, lithium source and carbon source are respectively ferrous oxalate, di(2-ethylhexyl)phosphate
Hydrogen ammonium, lithium carbonate and glucose.Addition is iron：Phosphorus：Lithium=1:1:1（Molar ratio）, glucose is with the molar ratio of lithium source
0.2：1.Described high-temperature solid phase reaction method is：Raw material is ground according to molar ratio batch mixing.Material is gone to after mill-drying
Calcined under leading to nitrogen environment at 600 DEG C in pre-burning stove, sintering time is 1 hour, once sintered to carry out ball milling to material afterwards,
Double sintering is carried out again, and the temperature of double sintering is 650 DEG C, and sintering time is 1 hour, and double sintering atmosphere is nitrogen.Afterwards
Classification packaging, obtains LiFePO 4 product.It is once sintered react including：
FeC2O4·H2O+2NH4H2PO4+Li2CO3=2LiFePO4+2NH3↑+3CO2↑+2CO↑+7H2O↑。
Step（2）, by step（1）The high-temperature tail gas that middle solid phase reaction is produced are passed through tubular heat exchanger, after heat exchange, tail gas
Temperature is reduced to 50 DEG C.The low-temperature heat exchange fluid of heat exchange is for once sintered and double sintering nitrogen.
Step（3）, by step（2）Tail gas after treatment is passed through ammonia decontamination tower and is processed.Tail gas is by positioned at ammonia
The gas feed of purifying column tower body middle and lower part enters in tower, with the acid solution spraying layer of tower body inner upper spray and lower sulfuric acid is sour
Liquid contact absorbs ammonia and forms ammonium sulfate, and tail gas after the demister demisting positioned at acid solution spraying layer top by flowing through tower body top
Leave ammonia decontamination tower in the gas outlet in portion.Using circulating pump will be located at tower body inner lower collecting tank in collect liquid and
Fresh sulfuric acid acid solution in fresh acid storage is delivered to acid solution spraying layer and is circulated spray.
Step（4）, terminate circulated sprinkling after, the liquid pumping collected the collecting tank of ammonia decontamination tower using draw-off pump is extremely
Thickener, in thickener, ammonium sulfate obtains liquid containing ammonium sulfate fertilizer after pervaporation, precipitation, filtering, drying.Sulfur acid
The weight nitroxide content of ammonium fertilizer is 16%, and sulphur weight content is 18.0%.
Step（5）, by step（3）The tail gas of the gas outlet at the top of outflow tower body is delivered to comprising an oxidation using booster pump
The carbon monoxide adsorption device of carbon adsorbent, operating pressure is 1.5Mpa.Wherein described absorbent for carbon monooxide is an oxidation
Carbon adsorbent B.CO contents are 8ppm in tail gas after absorption.
Step（6）, by step（5）Tail gas after treatment is emptied by emptier.
In embodiment 3, described absorbent for carbon monooxide B preparation methods are：It is stannous chloride 42 that component by weight is weighed
35 parts of part, 15 parts of montmorillonite, 23 parts of Cu-ZSM-5 types zeolite, 10 parts of aluminium hydroxide, 10 parts of vermiculite and attapulgite, by Cu-
ZSM-5 types zeolite is toasted 150 minutes in 100 DEG C of baking ovens, standby.Batch mixing is obtained after each raw material is mixed, batch mixing is added into kneader,
Add 15 parts of water and 10 parts of ethanol to be mediated to kneader, 15 minutes kneading times, obtain kneading material.Material will be mediated to add
Work globulate particle, baking oven is put into by spheric granules, is taken out within 200 minutes in 320 DEG C of bakings, after after natural cooling, being made an oxygen
Change carbon adsorbent B.
Embodiment 4：
A kind of preparation method of LiFePO 4, comprises the following steps：
Step（1）, selection prepares the raw material high-temperature solid phase reaction method of LiFePO 4 and prepares LiFePO 4 product.Step
（1）In, source of iron, phosphorus source, lithium source and carbon source are weighed, specific source of iron, phosphorus source, lithium source and carbon source are respectively ferrous oxalate, di(2-ethylhexyl)phosphate
Hydrogen ammonium, lithium carbonate and glucose.Addition is iron：Phosphorus：Lithium=1:1:1（Molar ratio）, glucose is with the molar ratio of lithium source
0.5：1.Described high-temperature solid phase reaction method is：Raw material is ground according to molar ratio batch mixing.Material is gone to after mill-drying
Calcined under leading to nitrogen environment at 700 DEG C in pre-burning stove, sintering time is 5 hours, once sintered to carry out ball milling to material afterwards,
Double sintering is carried out again, and the temperature of double sintering is 750 DEG C, and sintering time is 5 hours, and double sintering atmosphere is nitrogen.Afterwards
Classification packaging, obtains LiFePO 4 product.It is once sintered react including：
FeC2O4·H2O+2NH4H2PO4+Li2CO3=2LiFePO4+2NH3↑+3CO2↑+2CO↑+7H2O↑。
Step（2）, by step（1）The tail gas that middle solid phase reaction is produced is passed through tubular heat exchanger, after heat exchange, exhaust temperature
It is reduced to 50 DEG C.
Step（3）, by step（2）Tail gas after treatment is passed through ammonia decontamination tower and is processed.Tail gas is by positioned at ammonia
The gas feed of purifying column tower body middle and lower part enters in tower, with the acid solution spraying layer of tower body inner upper spray and lower sulfuric acid is sour
Liquid contact absorbs ammonia and forms ammonium sulfate, and tail gas after the demister demisting positioned at acid solution spraying layer top by flowing through tower body top
Leave ammonia decontamination tower in the gas outlet in portion.Using circulating pump will be located at tower body inner lower collecting tank in collect liquid and
Fresh sulfuric acid acid solution in fresh acid storage is delivered to acid solution spraying layer and is circulated spray.
Step（4）, the liquid pumping collected the collecting tank of ammonia decontamination tower using draw-off pump to thickener, in thickener
In, ammonium sulfate obtains liquid containing ammonium sulfate fertilizer after pervaporation, precipitation, filtering, drying.The weight nitroxide of liquid containing ammonium sulfate fertilizer contains
It is 16% to measure, and sulphur weight content is 18.0%.
Step（5）, by step（3）The tail gas of the gas outlet at the top of outflow tower body is delivered to comprising an oxidation using booster pump
The carbon monoxide adsorption device of carbon adsorbent, operating pressure is 1.5Mpa.Wherein described absorbent for carbon monooxide is an oxidation
Carbon adsorbent B.CO contents are 9ppm in tail gas after absorption.
Step（6）, by step（5）Tail gas after treatment is emptied by emptier.
Described absorbent for carbon monooxide B preparation methods are same as Example 3.
It is pointed out that added to the absorbent for carbon monooxide in carbon monoxide adsorption device in above-described embodiment 1-4
Quality be identical, by comparing, absorbent for carbon monooxide present in prior art can reduce the concentration of CO
To 20ppm.But, currently preferred CO adsorbents are capable of the concentration of low CO to below 10ppm.This explanation is in same amount
Under the conditions of, currently preferred CO adsorbents have adsorption capacity higher.
Core of the invention is the use of step of preparation process and involved absorbent for carbon monooxide.And in embodiment
Each involved hardware, such as pre-burning stove, calcining furnace, ball mill device, heat exchanger, ammonia decontamination tower, draw-off pump, thickener, increasing
Press pump, carbon monoxide adsorption device, tail gas emptier are equipment of the prior art, can be bought from market, not specifically
It is defined in its concrete structure, therefore does not tire out one by one herein and state.And milling time in preparation technology, drying means, Ball-milling Time,
Sulfuric acid concentration, liquid evaporation, precipitation, filtering, stoving process etc. for technique effect of the invention without influence, from prior art
In known parameters both may be used.
Claims (5)
1. a kind of LiFePO 4 preparation method, it is characterised in that comprise the following steps：
The raw material high-temperature solid phase reaction method that step (1), selection prepare LiFePO 4 prepares LiFePO 4 product；
Step (2), by step (1) solid phase reaction produce high-temperature tail gas be passed through tubular heat exchanger, after heat exchange, exhaust temperature
It is reduced to 50 DEG C；
Step (3), the tail gas after step (2) treatment is passed through ammonia decontamination tower and is processed；Tail gas is by positioned at ammonia decontamination
The gas feed of tower tower body middle and lower part enters in tower, with the acid solution spraying layer of tower body inner upper spray and under sulfuric acid acid solution connect
Touch and absorb ammonia formation ammonium sulfate, tail gas is flowed through at the top of tower body by after the demister demisting positioned at acid solution spraying layer top
Leave ammonia decontamination tower in gas outlet；The liquid and fresh collected in the collecting tank of tower body inner lower will be located at using circulating pump
Fresh sulfuric acid acid solution in acid storage is delivered to acid solution spraying layer and is circulated spray；
After step (4), termination circulated sprinkling, the liquid pumping for being collected the collecting tank of ammonia decontamination tower using draw-off pump is extremely concentrated
Groove, in thickener, ammonium sulfate obtains the fertilizer of liquid containing ammonium sulfate after pervaporation, precipitation, filtering, drying；
Step (5), by step (3) flow out tower body at the top of gas outlet tail gas using booster pump be delivered to comprising carbon monoxide inhale
Attached dose of carbon monoxide adsorption device, operating pressure is 1.5Mpa；The composition of the absorbent for carbon monooxide is：Group by weight
Point, it is 38 parts of stannous chloride, 10 parts of montmorillonite, 18 parts of Cu-ZSM-5 types zeolite, 8 parts of aluminium hydroxide, 8 parts of vermiculite and attapulgite
28 parts；
Step (6), by step (5) treatment after tail gas by emptier empty.
2. a kind of LiFePO 4 preparation method according to claim 1, it is characterised in that institute in described step (1)
The raw material stated is source of iron, phosphorus source, lithium source, and specific source of iron, phosphorus source, lithium source are respectively ferrous oxalate, ammonium dihydrogen phosphate, lithium carbonate；
Described high-temperature solid phase reaction method is：According to source of iron：Phosphorus source：Lithium source=1:1:1 molar ratio batch mixing grinding；Mill-drying
Calcined under logical nitrogen environment at 600 DEG C~700 DEG C during material is gone into pre-burning stove afterwards, sintering time is 1~5 hour, once
Ball milling is carried out after sintering to material, then carries out double sintering, the temperature of double sintering is 650 DEG C~750 DEG C, and sintering time is
1~5 hour, double sintering atmosphere was nitrogen；Classification packaging, obtains LiFePO 4 product afterwards.
3. a kind of LiFePO 4 preparation method according to claim 2, it is characterised in that for once sintered and two
Tubular heat exchanger of the nitrogen of secondary sintering as low-temperature heat exchange fluid in the step (2) is exchanged heat with high-temperature tail gas.
4. a kind of LiFePO 4 preparation method according to claim 1, it is characterised in that described carbon monoxide is inhaled
Attached dose of preparation method is：Cu-ZSM-5 types zeolite is toasted 20 minutes in 100 DEG C of baking ovens, it is standby；After each raw material is mixed
Batch mixing, kneader is added by batch mixing, adds 10 parts of water and 5 parts of ethanol to be mediated to kneader, 10 minutes kneading times, is obtained
Mediate material；Material will be mediated and is processed into spheric granules, spheric granules is put into baking oven, taken out within 180 minutes in 300 DEG C of bakings,
After after natural cooling, absorbent for carbon monooxide is made.
5. a kind of LiFePO 4 preparation method according to claim 1, it is characterised in that tail gas is by carbon monoxide
After adsorbent equipment absorption, CO contents are less than 20ppm in tail gas.
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| CN102225753A (en) * | 2011-05-13 | 2011-10-26 | 浙江大学 | Preparation method for lithium ion battery cathode materials |
| CN103418337A (en) * | 2012-05-24 | 2013-12-04 | 程会 | Carbon monoxide adsorbent |
| CN104492242A (en) * | 2014-12-17 | 2015-04-08 | 合肥恒力电子装备公司 | Kiln exhaust gas purifying device and kiln exhaust gas purifying method |
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| CN101927152A (en) * | 2010-03-12 | 2010-12-29 | 大连海鑫化工有限公司 | High-strength gas purifying and separating adsorbent as well as preparation and application thereof |
| CN102225753A (en) * | 2011-05-13 | 2011-10-26 | 浙江大学 | Preparation method for lithium ion battery cathode materials |
| CN103418337A (en) * | 2012-05-24 | 2013-12-04 | 程会 | Carbon monoxide adsorbent |
| CN104492242A (en) * | 2014-12-17 | 2015-04-08 | 合肥恒力电子装备公司 | Kiln exhaust gas purifying device and kiln exhaust gas purifying method |
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