CN114702020B - Production line for preparing nano lithium iron phosphate from titanium dioxide auxiliary waste ferrous sulfate - Google Patents
Production line for preparing nano lithium iron phosphate from titanium dioxide auxiliary waste ferrous sulfate Download PDFInfo
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- CN114702020B CN114702020B CN202210499486.2A CN202210499486A CN114702020B CN 114702020 B CN114702020 B CN 114702020B CN 202210499486 A CN202210499486 A CN 202210499486A CN 114702020 B CN114702020 B CN 114702020B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 57
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 title claims abstract description 55
- 239000011790 ferrous sulphate Substances 0.000 title claims abstract description 49
- 235000003891 ferrous sulphate Nutrition 0.000 title claims abstract description 49
- 229910000359 iron(II) sulfate Inorganic materials 0.000 title claims abstract description 49
- 239000002699 waste material Substances 0.000 title claims abstract description 43
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 22
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 76
- 238000002360 preparation method Methods 0.000 claims abstract description 76
- 230000003647 oxidation Effects 0.000 claims abstract description 67
- 230000032683 aging Effects 0.000 claims abstract description 63
- 238000001035 drying Methods 0.000 claims abstract description 38
- 238000005406 washing Methods 0.000 claims abstract description 31
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 29
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 26
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 18
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000000746 purification Methods 0.000 claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 196
- 239000000654 additive Substances 0.000 claims description 107
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 105
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 96
- 230000000996 additive effect Effects 0.000 claims description 95
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 58
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 47
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 44
- 239000002002 slurry Substances 0.000 claims description 44
- 239000005955 Ferric phosphate Substances 0.000 claims description 37
- 229940032958 ferric phosphate Drugs 0.000 claims description 37
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims description 37
- 239000007788 liquid Substances 0.000 claims description 35
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 33
- 235000010215 titanium dioxide Nutrition 0.000 claims description 33
- 239000012065 filter cake Substances 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 23
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 238000011045 prefiltration Methods 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000000706 filtrate Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 239000001488 sodium phosphate Substances 0.000 claims description 14
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 14
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 14
- 238000010009 beating Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 238000004090 dissolution Methods 0.000 claims description 10
- 238000005485 electric heating Methods 0.000 claims description 10
- 238000004806 packaging method and process Methods 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 10
- 238000001238 wet grinding Methods 0.000 claims description 10
- 238000003860 storage Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000011010 flushing procedure Methods 0.000 claims description 8
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 7
- 239000008103 glucose Substances 0.000 claims description 7
- 238000004537 pulping Methods 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- 239000006260 foam Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 235000011837 pasties Nutrition 0.000 claims description 4
- 238000009837 dry grinding Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000010902 jet-milling Methods 0.000 claims description 2
- 230000001276 controlling effect Effects 0.000 claims 2
- 230000001105 regulatory effect Effects 0.000 claims 2
- 229940116007 ferrous phosphate Drugs 0.000 abstract description 5
- 229910000155 iron(II) phosphate Inorganic materials 0.000 abstract description 5
- 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 abstract description 5
- 238000004140 cleaning Methods 0.000 abstract description 3
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 136
- 238000010586 diagram Methods 0.000 description 11
- 239000010865 sewage Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 206010063385 Intellectualisation Diseases 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001038 titanium pigment Substances 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
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Compounds Of Iron (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a production line for preparing nano lithium iron phosphate from titanium dioxide auxiliary waste ferrous sulfate. The invention comprises a purification system, an oxidation system, a batching system, a synthesis system, an aging system, a washing and filtering system, a drying system and a lithium doping system. The invention realizes accurate raw material preparation, uniform solution stirring, oxidation prevention of protective gas, self-cleaning function, on-line or remote monitoring of flow, pressure, pH, temperature and the like, and achieves the aim of low-cost, continuous and large-scale production of nano ferrous phosphate.
Description
Technical Field
The invention belongs to the technical field of new materials, relates to a production line for producing nano lithium iron phosphate by using byproduct waste ferrous sulfate in the industrial production of titanium dioxide, and in particular relates to a production line for preparing nano lithium iron phosphate by using titanium dioxide auxiliary waste ferrous sulfate.
Background
The byproduct ferrous phosphate generated in titanium dioxide industrialization is industrial waste, and is accumulated in stock form at present, so that not only is the iron resource utilization rate low and the land resource waste caused, but also environmental problems such as dust, water source and soil pollution are caused, a large amount of auxiliary waste ferrous sulfate is piled up, so that the ecological environmental problem is caused, and the auxiliary waste ferrous sulfate is piled up to cause the iron resource waste.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a production line for preparing nano lithium iron phosphate from titanium dioxide auxiliary waste ferrous sulfate, which is used for realizing accurate raw material preparation, uniform solution stirring, oxidation prevention of protective gas, self-cleaning function, online or remote monitoring of flow, pressure, pH, temperature and the like, and achieving the purposes of low-cost, continuous and large-scale nano ferrous phosphate production.
In order to achieve the aim, the production line for preparing the nano lithium iron phosphate by using the titanium dioxide auxiliary waste ferrous sulfate comprises a purification system, an oxidation system, a batching system, a synthesis system, an aging system, a washing and filtering system, a drying system and a lithium doping system; wherein,,
a purification system comprising a dissolution tank and a prefilter;
a dissolving tank stirrer is arranged in the dissolving tank, and a dissolving tank steam inlet, a dissolving tank deoxidized water inlet and a dissolving tank titanium dioxide auxiliary waste ferrous sulfate inlet are arranged at the top end of the dissolving tank; the bottom end of the dissolving tank is connected with the inlet of the prefilter through a dissolving tank bottom pump;
the oxidation system comprises an oxidation kettle and an iron sulfate buffer tank;
the oxidation kettle is provided with an oxidation kettle stirrer, and the top end of the oxidation kettle is provided with an oxidation kettle steam inlet, an oxidation kettle deoxidized water inlet, an oxidation kettle ferrous sulfate solution inlet, a concentrated sulfuric acid inlet and a hydrogen peroxide inlet; the oxidation kettle is respectively connected with an output port of the prefilter, a steam conveying pipe, a deoxidized water conveying pipe, a concentrated sulfuric acid conveying pipe and a hydrogen peroxide conveying pipe, and ferrous sulfate filtrate obtained by purifying the prefilter automatically flows into an oxidation system; the oxidation kettle is communicated with the ferric sulfate buffer tank through an oxidation kettle tank bottom pump, and ferric sulfate solution obtained by oxidation is conveyed to the ferric sulfate buffer tank through the oxidation kettle tank bottom pump; the ferric sulfate buffer tank is provided with a ferric sulfate buffer tank stirrer, the bottom of the ferric sulfate buffer tank is connected with a ferric sulfate solution delivery pump, and the ferric sulfate solution is delivered to the synthesis system through the ferric sulfate solution delivery pump;
The phosphoric acid batching system comprises a phosphoric acid solution preparation tank and a phosphoric acid solution buffer tank, wherein the phosphoric acid solution preparation tank is provided with a phosphoric acid solution preparation tank stirrer;
the top end of the phosphoric acid solution preparation tank is provided with a steam inlet of the phosphoric acid solution preparation tank, an oxygen-removing water inlet of an oxidation kettle of the phosphoric acid solution preparation tank, a phosphoric acid inlet and a sodium hydroxide solution inlet; the phosphoric acid solution preparation tank is connected with the steam conveying pipe, the deoxidized water conveying pipe, the sodium hydroxide solution conveying pipe and the phosphoric acid conveying pipe; the tank body is provided with a phosphoric acid solution preparation tank liquid level meter, a phosphoric acid solution preparation tank pH meter and a phosphoric acid solution preparation tank thermometer, the bottom of the phosphoric acid solution preparation tank is connected with a phosphoric acid solution buffer tank through a phosphoric acid solution pouring pump, and the prepared sodium phosphate solution is conveyed into the phosphoric acid solution buffer tank; the phosphoric acid solution buffer tank is provided with a phosphoric acid solution buffer tank stirrer, the phosphoric acid solution buffer tank is provided with a phosphoric acid solution buffer tank liquid level meter, a phosphoric acid solution buffer tank pH meter and a phosphoric acid solution buffer tank thermometer, the bottom of the phosphoric acid solution buffer tank is connected with a phosphoric acid solution delivery pump, and the phosphoric acid solution is delivered to the synthesis system through the phosphoric acid solution delivery pump;
the additive batching system comprises an additive batching tank and an additive buffer tank;
The top end of the additive preparation tank is provided with a steam inlet of the additive preparation tank, an deoxidized water inlet of the additive preparation tank and an additive inlet of the additive preparation tank, and the additive preparation tank is connected with a steam conveying pipe, a deoxidized water conveying pipe and an additive conveying pipe; the additive preparation tank is provided with an additive preparation tank liquid level gauge and an additive preparation tank stirrer, and the bottom of the additive preparation tank is connected with the upper part of the additive buffer tank through an additive solution pouring pump;
the additive buffer tank is provided with an additive buffer tank liquid level gauge and an additive buffer tank stirrer, the bottom of the additive buffer tank is connected with an additive solution delivery pump, and the additive solution is delivered to the synthesis system through the additive solution delivery pump;
a synthesis system comprising a first reactor, a second reactor;
the first reactor is provided with a first reactor stirrer and a first reactor pH meter, and the top end of the first reactor is provided with a first reactor steam inlet and a first reactor deaerated water inlet; the first reactor is connected with a steam conveying pipe and a deoxidized water conveying pipe;
the second reactor is provided with a second reactor stirrer and a second reactor pH meter, and the top end of the second reactor is provided with a second reactor steam inlet and a second reactor deaerated water inlet; the second reactor is connected with a steam conveying pipe and a deoxidized water conveying pipe;
The first reactor and the second reactor are connected with ferric sulfate solution output by the oxidation system, sodium phosphate solution output by the phosphoric acid batching system and additive solution output by the additive batching system, the ferric sulfate solution, the sodium phosphate solution output by the phosphoric acid batching system and the additive solution output by the additive batching system are respectively shunted and then respectively enter the two reactors in a three-strand parallel flow mode to carry out synthesis reaction, a shunt pipeline is provided with a flowmeter, and the synthesized nano ferric phosphate foam flows out of the upper parts of the two reactors and flows into the aging system automatically after being merged;
the aging system comprises at least 3 aging tanks, wherein an aging tank stirrer is arranged in the aging tanks, the aging tanks are connected with a steam conveying pipe, a nitrogen conveying pipe, a condensation water conveying pipe and a nano ferric phosphate slurry conveying pipe of the synthesis system, the aging tanks are provided with an aging tank liquid level meter and an aging tank thermometer, the bottoms of the aging tanks are connected in parallel through an output pipe and are connected with an aging tank bottom pump, and the nano ferric phosphate slurry is conveyed into the washing and filtering system through the aging tank bottom pump;
the filter washing system comprises a first-stage filter press and a second-stage filter press, wherein nano ferric phosphate slurry output by the aging system enters the first-stage filter press to be primarily filtered, a belt conveyor is arranged at the lower part of the first-stage filter press, a beating tank is arranged below the output end of the belt conveyor, and the output end is opposite to the inlet of the beating tank; the bottom of the pulping tank is connected with the upper part of another pulping tank through a slurry conveying pump, the bottom of the pulping tank is connected with the input end of a secondary filter press through a secondary filter pressing feeding pump, a belt conveyor is arranged below the secondary filter press, and a nano ferric phosphate filter cake output by the secondary filter press is automatically dropped into the belt conveyor to be sent to a drying system;
The drying system comprises a vacuum dryer, the bottom of the vacuum dryer is communicated with the top of a storage bin, a nano iron phosphate filter cake output by the washing and filtering system enters the vacuum dryer to be dried for the first time to form powder, the powder enters the storage bin through discharging, the storage bin conveys the powder to a rotary furnace through a hopper type lifter A, a spiral conveyor and a hopper type lifter B are sequentially arranged at the output end of the rotary furnace, the powder enters a first demagnetizer through lifting of the hopper type lifter B, and a packaging bin is arranged at the output port of the first demagnetizer;
the lithium doping system comprises a coarse grinding machine and a mixing bin, wherein lithium carbonate particles in the packaging bin enter the mixing bin after entering the coarse grinding machine through a first feeding machine for dry grinding; the iron phosphate powder output by the drying system enters a mixing bin through a second feeding machine, and the glucose powder enters the mixing bin through a third feeding machine respectively; the output port of the mixing bin is connected with the inlet of the wet mill, the wet mill is connected with the deoxidized water conveying pipe, and the output port of the wet mill is connected with the inlet of the spray dryer; the outlet of the spray dryer is connected with a second demagnetizer, the outlet of the second demagnetizer is connected with an electric heating roller kiln, the electric heating roller kiln pulverizes lithium iron phosphate particles through an airflow pulverizer, the outlet at the bottom end of the airflow pulverizer is connected with the inlet of the sieving machine, and the outlet of the sieving machine is provided with a third demagnetizer.
Preferably, the prefilter is a common plate and frame filter press with purge air.
Preferably, each liquid conveying pipe is provided with a control valve.
Further, a DC control system is also provided, which comprises a control module, an operation panel table, an industrial personal computer and a display; the PH meter, the thermometer and the pressure transmitter in all the systems are responsible for collecting signals on site, and send the signals to a control module for on-line on-site display or remote industrial personal computer display or display screen centralized display; the flowmeter is responsible for collecting signals, sending a control module to a line for on-site display or remote transmission industrial personal computer display or display screen for centralized display, and simultaneously providing control signals for controlling the opening and closing of the valve on the batching conveying pipe; the liquid level meter is responsible for collecting signals, sending a line of on-site display or remote transmission industrial personal computer display or centralized display of a display screen to the control module, and simultaneously providing control signals for controlling the opening and closing of a control valve on the feeding conveying pipe; the pump motor, the stirring motor and the conveying motor are powered on and off through the control module; the display is responsible for intensively displaying various returned field collected data and the processed record curves; the industrial personal computer is responsible for assigning values to the process parameters and returning instantaneous values for displaying the field process parameters; the operating panel table is responsible for inching control, manual automatic control mode conversion, power supply indication and electric appliance state display functions.
The preparation method for preparing the nano lithium iron phosphate by using the titanium white auxiliary waste ferrous sulfate as a raw material by adopting the production line specifically comprises the following steps:
s1, taking titanium dioxide auxiliary waste ferrous sulfate as a raw material, introducing steam, adding deoxidized water, stirring, and automatically flowing the ferrous sulfate solution purified by a prefilter into an oxidation kettle;
s2, adding concentrated sulfuric acid and hydrogen peroxide into an oxidation kettle to oxidize to obtain ferric sulfate solution, entering an iron sulfate buffer tank, adding deoxidized water into the buffer tank, and respectively entering a first reactor and a second reactor in a three-strand parallel flow mode after the ferric sulfate solution, the prepared sodium phosphate solution and the additive solution in the buffer tank are all split;
s3, the synthesized nano ferric phosphate foam is respectively discharged from the upper end sides of the two reactors and flows into an aging tank automatically after being converged, steam, nitrogen and condensed water are introduced into the aging tank for stirring and aging, the nano ferric phosphate slurry obtained by aging is conveyed into a first-stage filter press and a second-stage filter press through an aging tank bottom pump to be sequentially washed and filtered, a filter cake is obtained, and the filter cake is dried and demagnetized to obtain nano ferric phosphate powder;
s4, the nano iron phosphate powder, glucose powder and lithium carbonate powder enter a mixed material, and then oxygen-removing water is added for wet grinding, drying, demagnetizing, calcining, jet milling, screening and demagnetizing to obtain a finished product of lithium iron phosphate.
Preferably, in S3, the condensed water comes from a vacuum dryer in the drying system.
Preferably, in S3, the nano iron phosphate slurry output by the aging system enters the first-stage filter press 52 to perform primary filtration, the filtrate flows away through a pipeline, deoxygenated water is introduced into the filter press to perform pressure flushing on the filter cake in the machine, the deoxygenated water is reversely introduced into the filter press after the filtrate flows away, the filter cake in the machine is squeezed and squeezed, finally, the discharged filter cake is self-dropped and adjusted into a belt conveyor to be sent into a pulping tank, the nano iron phosphate slurry is conveyed into a slurry buffer tank through a slurry conveying pump, the nano iron phosphate slurry is conveyed into the second-stage filter press through a second-stage filter press feeding pump, the deoxygenated water is introduced into the filter press to perform pressure flushing on the filter cake in the machine after the filtrate flows away, the deoxygenated water is reversely introduced into the filter press to squeeze and squeeze the filter cake in the machine, and finally, the discharged filter cake is self-dropped and adjusted into the belt conveyor to be sent to the drying system.
Preferably, in S4, the three materials are mixed uniformly, then the mixture enters a wet mill, deoxygenated water is added into the wet mill for secondary wet milling, and the pasty mixture after wet milling enters a spray dryer for drying, so that a granular mixture is formed after drying.
Preferably, in S4, the granular mixture is formed after drying, and is discharged and falls into an electric heating roller kiln through a magnetic remover for removing iron, and the granular mixture is calcined to form lithium iron phosphate particles.
The invention relates to a production line for preparing nano lithium iron phosphate from titanium white auxiliary waste ferrous sulfate, which is applied to the preparation of nano lithium iron phosphate from titanium white auxiliary waste ferrous sulfate.
The production line for preparing nano lithium iron phosphate from titanium dioxide auxiliary waste ferrous sulfate has the beneficial effects that:
1. the nanometer lithium iron phosphate production line adopts a chemical wet method, the secondary waste ferrous sulfate generated in the titanium pigment production process is purified and oxidized, then reacts with phosphoric acid and other additives in a self-proprietary multiphase interface reactor (patent number: PCT/CN 2020/088001) to generate a nanometer ferric phosphate precursor, and finally lithium is doped into the precursor to form a nanometer lithium iron phosphate product. The production line is matched with a patent reactor for design, a whole set of industrial production line for producing nano lithium iron phosphate by using titanium white auxiliary waste ferrous sulfate is formed, the preparation of nano lithium iron phosphate is successfully realized, and verified that the nano precursor is beneficial to doping lithium and can improve the multiplying power performance of the anode material. At present, the production line has a production scale of 1500 tons per year, and the subsequent amplification design of 50 ten thousand tons per year production scale is maintained; the high-value utilization of the secondary waste ferrous phosphate resources is realized through the nanocrystallization reaction process, so that the secondary waste ferrous sulfate is subjected to resource conversion, and a positive electrode material is stably provided for the lithium battery manufacturing industry;
2. According to the invention, an iron powder charging port is added to a dissolving tank in the purification system, so that titanium in the titanium white auxiliary waste can be simultaneously extracted when the titanium white auxiliary waste is dissolved; the PH meter is arranged in the dissolution tank, so that the acidity and alkalinity of the solution in the tank can be accurately detected, deoxidized water is used for dissolution, external impurity ions are prevented from entering the dissolution tank along with the solvent, and the titanium white auxiliary waste is directly filtered after being dissolved by the prefilter, so that the purification target is completed at one time;
3. the oxidation system of the invention accurately measures the flow of the concentrated sulfuric acid and the hydrogen peroxide when entering the ferrous sulfate oxidation kettle, thereby saving the waste problem after the acid is excessive; the accurate measurement of the dosage of the concentrated sulfuric acid and the hydrogen peroxide is combined with a PH meter arranged on a ferrous sulfate oxidation kettle, so that the problems of extreme acid-base change and difficult regulation of the solution in the ferrous sulfate tank are solved; the bottom pump of the oxidation kettle adopts a centrifugal pump with good corrosion resistance and wear resistance, and simultaneously uses deoxidized water to cool the sealing device, so that the long-time conveying working condition of the strong acid ferric sulfate solution can be well adapted while no impurity ions are introduced; the pipeline for the deoxidized water to enter the ferrous sulfate oxidation kettle is provided with a flowmeter, and the ferrous sulfate oxidation kettle simultaneously plays a role in batching ferric sulfate solution, so that the ferric sulfate solution is ensured to be conveyed to the synthesis process in an accurate concentration;
4. When the sodium hydroxide solution, phosphoric acid and deoxidized water enter the phosphoric acid solution preparation tank, the phosphoric acid dosing system accurately measures the sodium hydroxide solution, the phosphoric acid and the deoxidized water, so that the concentration preparation accuracy of the disodium hydrogen phosphate solution is ensured; the phosphoric acid solution buffer tank is provided with a stirring function, so that micro-deposition caused by crystallization and precipitation of salt solution at the bottom of the tank can be treated, and the disodium hydrogen phosphate solution is ensured to be conveyed to a synthesis process in a liquid phase and an accurate concentration; the phosphoric acid solution pouring pump adopts a centrifugal pump with good corrosion resistance and wear resistance, and simultaneously uses deoxygenated water to cool the sealing device, so that the long-time conveying working condition of the non-neutral ferric sulfate solution caused by concentration gradient formed by uneven stirring of the phosphoric acid solution preparation tank can be well adapted while no impurity ions are introduced;
5. according to the invention, when the additive and deoxidized water enter the additive preparation tank, the additive dosing system accurately measures the additive and deoxidized water, so that the concentration preparation accuracy of the additive solution is ensured; the additive buffer tank is provided with a stirring function, so that micro-deposition caused by crystallization and precipitation of the additive solution at the bottom of the tank can be treated, and the additive solution is ensured to be conveyed to a synthesis process in a liquid phase and an accurate concentration; the additive solution pouring pump adopts a centrifugal pump with good corrosion resistance and wear resistance, and simultaneously uses deoxygenated water to cool the sealing device, so that the long-time conveying working condition of the non-neutral additive solution caused by uneven stirring of the additive preparation tank can be well adapted while no impurity ions are introduced;
6. The bubble liquid film reactor of the synthesis system constructs a nano reaction environment to directly generate nano ferric phosphate; the bubble liquid film reactor has the characteristics of uniform stirring, normal-pressure synthesis and continuous feeding, and is used for industrial mass production; the modular characteristic that the ferric sulfate solution, the disodium hydrogen phosphate solution and the coating agent solution are input simultaneously in equal volume to the bubble liquid film reactor reduces the design, selection and construction complexity of feeding assistance;
7. the aging tank of the aging system has a stirring function, so that accumulation of sediments at the bottom of the tank is prevented; the aging tank is communicated with a back-blowing pipeline, so that bubbles in the tank are conveniently broken, and the aging tank is convenient for conveying the nano ferric phosphate slurry outwards; the ageing tank is heated by steam and has temperature detection, thereby being beneficial to controlling the ageing temperature and improving the synthesis effect of the nano ferric phosphate; the condensed water sent by the drying procedure is used as the water for the tank washing for trial, so that the water consumption of a production line is saved;
8. the filter washing system selects the best membrane filter press in the industry, so that the water content of a filter cake is reduced to the greatest extent possible; the filter press with the self-cleaning function is adopted, so that the number of times of washing and filtering is reduced, the number of filter presses and rinsing tanks is reduced in response, and a part of investment cost is saved; the filter press with cloth washing function is adopted, so that the labor intensity is reduced, and the labor cost is saved; the slurry buffer tank is added, so that the filter press is prevented from stopping operation due to untimely unloading and the cutting off of the preamble, the continuous working of the ageing and filtering procedures is ensured, and the production cost is saved; fifthly, the filter press is used for washing, squeezing and cloth washing by deoxidizing water, so that foreign impurity ions are prevented from polluting filter cakes along with the washing water;
9. According to the invention, the drying system adopts a mode of primary drying of a vacuum dryer and secondary drying of a rotary kiln, so that the overall drying effect of the nano ferric phosphate is improved; after the vacuum drier is used for drying, the nano ferric phosphate is changed into fine particle powder, which is beneficial to the heat transfer effect of the rotary kiln during drying; the demagnetizer timely demagnetizes, so that the purity of the ferric phosphate is improved; the application of the bucket elevator saves the installation space; the design of the storage bin ensures the continuous operation of the vacuum dryer and the rotary kiln, and avoids the cost loss caused by the preamble shutdown; the design of the bucket elevator and the packaging bin saves the investment cost of purchasing and packaging;
10. the feeding machine in the lithium-doped system solves the problem of accurate proportioning of three materials, namely ferric phosphate, lithium carbonate and glucose; the coarse grinding machine is used to make industrial lithium carbonate particles smaller, which is favorable for fully and uniformly mixing three materials; the use of the wet mill ensures that the three materials are further fully mixed, thereby improving the chemical reaction effect of the lithium doped; the use of the spray dryer enables the mixed materials to enter the electric heating roller kiln in a particle form, so that a calcination heat transfer effect is provided; using an air flow pulverizer to enable lithium iron phosphate to reach a powder state required by a battery anode material; the sieving machine sieves out blocky lithium iron phosphate, the demagnetizer removes iron and the vacuum dryer dries, so that the quality of lithium iron phosphate powder is improved together;
11. The DCS control system greatly improves the automation, informatization and intellectualization levels of the production line, reduces the labor intensity and the labor number, and timely arranges and detects faults and production safety hidden trouble; the DC control system helps the chemical production line to realize high control precision requirements, improves chemical reaction effects, and reduces material waste; the central display can intensively display the whole production process, and helps enterprises to achieve the intelligent factory building objective.
Drawings
FIG. 1 is a process diagram corresponding to a production line system;
FIG. 2 is a schematic diagram of a purification system;
FIG. 3 is a schematic diagram of an oxidation system;
FIG. 4 is a schematic diagram of a phosphoric acid dosing system;
FIG. 5 is a schematic diagram of an additive dosing system;
FIG. 6 is a schematic diagram of a synthesis system;
FIG. 7 is a schematic diagram of an aging system;
FIG. 8 is a schematic diagram of a wash filtration system;
FIG. 9 is a schematic diagram of a drying system;
FIG. 10 is a schematic diagram of a lithium doped system;
FIG. 11 is a schematic diagram of a DCS system.
In the figure: a 1-dissolving tank thermometer, a 1-1-oxidation kettle thermometer, a 1-3-phosphoric acid solution preparing tank thermometer, a 1-4-phosphoric acid solution buffer tank thermometer, a 1-9-aging tank thermometer,
2-dissolving tank pH meter, 2-1-oxidation kettle tank pH meter, 2-3 phosphoric acid solution preparation tank pH meter, 2-4-phosphoric acid solution buffer tank pH meter, 2-7-first reactor pH meter, 2-8-second reactor pH meter, 3-dissolving tank, 301-dissolving tank steam inlet, 302-dissolving tank deoxidized water inlet, 303-dissolving tank titanium white auxiliary waste ferrous sulfate inlet, 4-dissolving tank bottom pump,
5-prefilter,
6-1-oxidation kettle liquid level meter, 6-3-phosphoric acid solution preparation tank liquid level meter, 6-4-phosphoric acid solution buffer tank liquid level meter, 6-5-additive preparation tank liquid level meter, 6-6-additive buffer tank liquid level meter, 6-9-aging tank liquid level meter, 6-10-beating tank liquid level meter, 6-11-slurry buffer tank liquid level meter, and,
7-dissolving tank stirrer, 7-1-oxidation tank stirrer, 7-2-ferric sulfate buffer tank stirrer, 7-3-phosphoric acid solution preparation tank stirrer, 7-4-phosphoric acid solution buffer tank stirrer, 7-5-additive preparation tank stirrer, 7-6-additive buffer tank stirrer, 7-7 first reactor stirrer, 7-8-second reactor stirrer, 7-9-aging tank stirrer, 7-10-beating tank stirrer, 7-11-slurry buffer tank stirrer,
12-oxidation reactor, 1201-oxidation reactor steam inlet, 1202-oxidation reactor deoxidized water inlet, 1203-oxidation reactor ferrous sulfate solution inlet, 1204-concentrated sulfuric acid inlet, 1205-hydrogen peroxide inlet, 13-oxidation reactor tank bottom pump, 14-ferric sulfate buffer tank, 15-ferric sulfate solution delivery pump,
23-phosphoric acid solution preparation tank, 2301-phosphoric acid solution preparation tank steam inlet, 2302-phosphoric acid solution preparation tank oxidation kettle deoxidized water inlet, 2303-phosphoric acid inlet, 2304-sodium hydroxide solution inlet, 24-phosphoric acid solution pouring pump, 26-phosphoric acid solution conveying pump
33-additive preparation tank, 3301-additive preparation tank steam inlet, 3302-additive preparation tank deoxygenated water inlet, 3303-additive preparation tank additive inlet, 34-additive solution pouring pump, 35-additive buffer tank, 36-additive solution delivery pump,
41-first reactor, 4101-first reactor steam inlet, 4102-first reactor deoxygenated water inlet, 44-second reactor, 4401-second reactor steam inlet, 4402-second reactor deoxygenated water inlet, 47-aging tank, 49-aging tank bottom pump,
52-first-stage filter press, 53-belt conveyor, 54-beating tank, 56-slurry conveying pump, 58-second-stage filter press feeding pump, 59-slurry buffer tank,
61-secondary filter press, 64-vacuum drier, 65-storage bin, 66-hopper type lifter A, 67-rotary furnace, 68-screw conveyor, 66-1-hopper type lifter B,
70-packaging bin, 71-first demagnetizer, 71-1-second demagnetizer, 72-first feeder, 72-1 second feeder, 72-2-third feeder, 73-coarse mill, 74-mixing bin, 77-wet mill, 78-spray dryer,
80-electric heating roller kiln, 82-sieving machine, 83-jet mill and 84-phosphoric acid solution buffer tank.
Detailed Description
Example 1
The invention relates to a production line for preparing nano lithium iron phosphate from titanium dioxide auxiliary waste ferrous sulfate, which is shown in figures 1-11, and comprises a purification system, an oxidation system, a batching system, a synthesis system, an aging system, a washing and filtering system, a drying system and a lithium doping system; wherein,,
a purification system comprising a dissolution tank 3 and a prefilter 5;
the upper end of the dissolution tank 3 is provided with a stirrer 7, steam is introduced, deoxygenated water is introduced, after the titanium white auxiliary waste ferrous sulfate enters the tank for stirring, ferrous sulfate solution and tank washing sewage are discharged from the tank, an iron powder charging port is added in the dissolution tank, and titanium in the titanium white auxiliary waste can be simultaneously extracted when the titanium white auxiliary waste is dissolved; the tank body is provided with a dissolving tank pH meter 2 and a dissolving tank thermometer 1; the prefilter 5 is a common plate-and-frame filter press and is provided with a purified air purge; the ferrous phosphate solution obtained under the dissolution tank 3 is pressed into a prefilter 5 through a dissolution tank bottom pump 4, and the purified ferrous sulfate filtrate automatically flows into an oxidation system.
The oxidation system comprises an oxidation kettle 12 and an iron sulfate buffer tank 14, wherein the upper end of the oxidation kettle 12 is provided with an oxidation kettle stirrer 7-1, steam is introduced, oxygen is removed by water, ferrous sulfate solution automatically flows, concentrated sulfuric acid is conveyed by a concentrated sulfuric acid pump 8, hydrogen peroxide is conveyed by a hydrogen peroxide pump 9 and enters the kettle from the upper end of the oxidation kettle 12 respectively, the kettle body is provided with an oxidation kettle liquid level meter 6-1, an oxidation kettle pH meter 2-1 and an oxidation kettle thermometer 1-1, a centrifugal pump with good corrosion resistance and wear resistance is adopted as an oxidation kettle bottom pump, iron sulfate solution and tank washing sewage are discharged from the kettle, and ferric sulfate solution obtained by oxidation is conveyed by an oxidation kettle bottom pump 13 and enters the iron sulfate buffer tank 14 from the upper end; the ferric sulfate buffer tank stirrer 7-2 is used for feeding deoxidized water, and the lower end liquid is conveyed into a synthesis system through the ferric sulfate solution conveying pump 15;
The concentrated sulfuric acid tank is connected with a distribution tank car through a pipeline, a valve and an instrument to periodically send concentrated sulfuric acid into the tank, and the concentrated sulfuric acid discharged from the concentrated sulfuric acid tank is conveyed into an oxidation kettle through a sulfuric acid pump 8; the hydrogen peroxide discharged from the lower end of the hydrogen peroxide diluting tank is conveyed into the oxidation kettle by a hydrogen peroxide pump 9, and the upper end of the hydrogen peroxide diluting tank is connected with a delivery tank car through a pipeline, a valve and a meter to periodically convey hydrogen peroxide into the tank.
The batching system comprises a phosphoric acid batching system and an additive batching system;
a phosphoric acid dosing system comprising a phosphoric acid solution preparation tank 23 and a phosphoric acid solution buffer tank 84;
the upper end of the phosphoric acid solution preparation tank 23 is provided with a phosphoric acid solution preparation tank stirrer 7-3, steam is introduced, oxygen-removed water is introduced, sodium hydroxide solution enters the tank from the upper end through a pipeline, a valve and a meter, constant-volume barreled phosphoric acid enters the tank from the upper end through a portable pump, the tank body is provided with a phosphoric acid solution preparation tank liquid level meter 6-3, a phosphoric acid solution preparation tank pH meter 2-3 and a phosphoric acid solution preparation tank thermometer 1-3, sodium sulfate solution and tank washing sewage are discharged from the tank, and the prepared sodium phosphate solution enters the tank from the upper end of a phosphoric acid solution buffer tank 84 through a phosphoric acid solution pouring pump 24; the upper end of the phosphoric acid solution buffer tank 84 is provided with a phosphoric acid solution buffer tank stirrer 7-4, a phosphoric acid solution buffer tank liquid level meter 6-4, a phosphoric acid solution buffer tank pH meter 2-4 and a phosphoric acid solution buffer tank thermometer 1-4, and sodium sulfate solution which is discharged from the lower end enters the synthesis system through a phosphoric acid solution conveying pump.
An additive dosing system comprising an additive dosing tank 33 and an additive buffer tank 35;
the upper end of the additive preparation tank 33 is provided with an additive preparation tank stirrer 7-5, steam is introduced, oxygen-removed water is introduced, constant-volume barreled additive is conveyed into the preparation tank 33 through a portable pump 32, the tank body of the preparation tank 33 is provided with an additive preparation tank liquid level meter 6-5, additive solution and tank washing sewage are discharged from the lower end of the tank, and the prepared additive solution is conveyed from an additive buffer tank 35 into the tank through an additive solution tank pouring pump 34; the upper end of the additive buffer tank 35 is provided with an additive buffer tank stirrer 7-6, an additive buffer tank liquid level meter 6-6, additive solution and tank washing sewage are discharged from the lower part of the tank, and the additive solution discharged from the lower end of the tank enters the synthesis system through an additive solution conveying pump 36.
The synthesis system comprises a first reactor 41 and a second reactor 44, wherein the two reactors belong to similar patent equipment with different volumes, the first reactor 41 is provided with a first reactor stirrer 7-7 and a first reactor pH meter 2-7, and the top end of the first reactor 41 is provided with a first reactor steam inlet 4101 and a first reactor deoxygenated water inlet 4102; the first reactor 41 is connected with a steam conveying pipe and a deoxidized water conveying pipe;
the second reactor 44 is provided with a second reactor stirrer 7-8 and a second reactor pH meter 2-8, and the top end of the second reactor 44 is provided with a second reactor steam inlet 4401 and a second reactor deaerated water inlet 4402; the second reactor 44 is connected with a steam conveying pipe and a deoxidized water conveying pipe;
The first reactor 41 and the second reactor 44 are connected with ferric sulfate solution output by the oxidation system, sodium phosphate solution output by the phosphoric acid batching system and additive solution output by the additive batching system, and the ferric sulfate solution, the sodium phosphate solution output by the phosphoric acid batching system and the additive solution output by the additive batching system are respectively delivered into the two reactors in a three-strand parallel flow mode to carry out synthesis reaction after being split, and a flow meter is arranged on a split pipe, so that the synthesized nano ferric phosphate foam flows out of the upper parts of the two reactors respectively, flows into an aging system automatically after being combined.
The ageing system comprises at least 3 ageing tanks 47, wherein an ageing tank stirrer 7-9, steam, nitrogen and condensed water from a vacuum dryer 64 are arranged in the ageing tanks 47, nano ferric phosphate slurry from the synthesis system respectively enters the 3 ageing tanks 47, the ageing tanks 47 are provided with an ageing tank liquid level meter 6-9 and an ageing tank thermometer 1-9, and nano ferric phosphate slurry and tank washing sewage are discharged from the lower ends of the tanks; and conveying the aged nano ferric phosphate slurry into a washing and filtering system through an aging tank bottom pump.
The washing and filtering system comprises a first-stage filter press 52 and a second-stage filter press 61, wherein the filter press has the functions of feeding, washing, squeezing, cloth washing and back blowing; the aged nano ferric phosphate slurry enters the first-stage filter press 52 for primary filtration, deoxygenated water is introduced into the first-stage filter press 52 for pressure flushing of filter cakes in the machine after the filtrate flows away through a pipeline, deoxygenated water is reversely introduced into the filter press after the filtrate flows away, then the filter cakes in the machine are squeezed and squeezed, and finally, the discharged filter cakes are automatically dropped and transferred into the belt conveyor 53 to be sent into the pulping tank 54; the upper end of the beating tank 54 is provided with a beating tank stirrer 7-10, oxygen-removing water is fed in, the tank body is provided with a beating tank liquid level meter 6-10, nano ferric phosphate slurry and tank washing sewage are discharged from the lower end of the tank, and the nano ferric phosphate slurry is conveyed into a slurry buffer tank 59 through a slurry conveying pump 56; the upper end of the slurry buffer tank 59 is provided with a slurry buffer tank stirrer 7-11, the tank body is provided with a slurry buffer tank liquid level meter 6-11, and nano ferric phosphate slurry and tank washing sewage are discharged from the lower end of the tank; the nano ferric phosphate slurry is conveyed into a secondary filter press 61 through a secondary filter pressing feed pump 58, after filtrate flows away through a pipeline, deoxygenated water is introduced into the secondary filter press 61 to carry out pressure flushing on an in-machine filter cake, after the filtrate flows away, deoxygenated water is reversely introduced into the filter press to squeeze and squeeze the in-machine filter cake, and finally, the discharged filter cake is automatically dropped into a belt conveyor 53 to be sent to a drying system.
The drying system comprises a vacuum dryer 64, the nano iron phosphate filter cake obtained by washing enters the vacuum dryer 64, the nano iron phosphate powder formed by primary drying enters a storage bin 65 through discharging, and a hopper lifter A66 lifts the nano iron phosphate powder from the bin 65 and feeds the nano iron phosphate powder into a rotary furnace 67; the nano iron phosphate powder formed by secondary drying of the rotary furnace is discharged and enters a screw conveyor 68, then is lifted by a hopper type lifter B66-1, is deironized by a first demagnetizer 71 and falls into a packaging bin 70; after the nano iron phosphate powder enters the packaging bag, the forklift is transported to a lithium-doped system.
The lithium doping system comprises a coarse mill 73 and a mixing bin 74, wherein lithium carbonate particles enter the coarse mill 73 through a first feeding machine 72 for primary dry grinding and then enter the mixing bin 74; the ferric phosphate powder outputted by the drying system enters a mixing bin 74 through a second feeding machine 72-1, and the glucose powder enters the mixing bin 74 through a third feeding machine 72-2 respectively; the three materials are mixed uniformly and then enter a wet mill 77 to be added with deoxidized water for secondary wet milling; the pasty mixture after wet grinding enters a spray dryer 78 to be dried to form a granular mixture, and the granular mixture falls into an electric heating roller kiln 80 after being deironized by a second demagnetizer 71-1 during discharging; the electric roller kiln 80 calcines the granular mixture to form lithium iron phosphate granules; the lithium iron phosphate particles enter a jet mill 83 for milling to form lithium iron phosphate powder; and (3) the lithium iron phosphate powder enters a sieving machine 82 for sieving, and the discharged material is subjected to iron removal by a third demagnetizer 71-2 and then is subjected to discharging packaging of the finished lithium iron phosphate product.
The DC control system comprises a control module, an operation panel table, an industrial personal computer and a display;
the pH meter, the thermometer and the pressure transmitter in all the process systems are responsible for collecting signals on site, and send the signals to a control module for on-site display on line or remote industrial personal computer display or display screen centralized display; the flowmeter is responsible for collecting signals, sending a control module to a line of field display or remote transmission industrial personal computer display or display screen for centralized display, and simultaneously providing control signals for opening and closing the batching valve; the liquid level meter is responsible for collecting signals, sending a line of on-site display or remote transmission industrial personal computer display or centralized display of a display screen to the control module, and simultaneously providing control signals for controlling the opening and closing of the feeding valve; the pump motor, the stirring motor and the conveying motor are powered on and off through the control module; the display is responsible for intensively displaying various returned field collected data and the processed record curves; the industrial personal computer is responsible for assigning values to the process parameters and returning instantaneous values for displaying the field process parameters; the operating panel table is responsible for the functions of inching control, manual automatic control mode conversion, power supply indication, electric appliance state display and the like.
Other systems or devices: the production line requirements of steam, deoxygenated water, back blowing and the like are all met by matching commercial complete equipment or by conveying the existing pipelines of enterprises; the wastewater treatment requirements are provided by an in-house or industrial park wastewater treatment system.
The preparation method for preparing nano lithium iron phosphate by using titanium dioxide auxiliary waste ferrous sulfate as raw material by adopting the production line specifically comprises the following steps of
S1, taking titanium dioxide auxiliary waste ferrous sulfate as a raw material, introducing steam, adding deoxidized water, stirring, and automatically flowing the ferrous sulfate solution purified by the prefilter 5 into an oxidation kettle;
s2, adding concentrated sulfuric acid and hydrogen peroxide into an oxidation kettle to oxidize to obtain ferric sulfate solution, feeding the ferric sulfate solution into a ferric sulfate buffer tank 14, adding deoxidized water into the buffer tank, and respectively feeding the ferric sulfate solution, the prepared sodium phosphate solution and the additive solution in the buffer tank into a first reactor 41 and a second reactor 44 in a three-strand parallel flow mode after the ferric sulfate solution, the prepared sodium phosphate solution and the additive solution are all split;
s3, the synthesized nano iron phosphate foam is respectively discharged from the upper end sides of the two reactors and flows into an ageing tank 47 automatically after converging, steam, nitrogen and condensed water are introduced into the ageing tank 47 for stirring and ageing, the condensed water is delivered from a vacuum dryer 64 in a drying system, the aged nano iron phosphate slurry enters a first-stage filter press 52 for primary filtration through a bottom pump of the ageing tank, deoxygenated water is introduced into the first-stage filter press 52 after filtrate flows out through a pipeline for pressure flushing of filter cakes in the machine, deoxygenated water is reversely introduced into the filter press after filtrate flows out for squeezing water of filter press, finally, the discharged filter cakes are automatically dropped into a belt conveyor 53 for delivering into a pulping tank 54, the nano iron phosphate slurry is delivered into a slurry buffer tank 60 through a slurry delivery pump 56, the nano iron phosphate slurry is delivered into a second-stage filter press 61 through a second-stage filter press feed pump 58, the deoxygenated water is introduced into the second-stage filter press 61 for pressure flushing of filter press after filtrate flows out, the deoxygenated water is reversely introduced into the filter press for squeezing water of filter cake in the machine after filtrate flows out, and finally, the discharged filter cakes are automatically dropped into a belt conveyor 53 for delivering into a drying system for removing magnetic phosphate powder, thereby obtaining nano iron phosphate;
S4, the nano iron phosphate powder, glucose powder and lithium carbonate powder enter a mixed material, the three materials are mixed uniformly, then enter a wet mill 77, deoxidized water is added for secondary wet milling, the pasty mixture after wet milling enters a spray dryer 78 for drying, a granular mixture is formed after drying, the granular mixture is discharged and falls into an electric heating roller kiln 80 through a first demagnetizer 71 after being dried, the granular mixture is calcined to form lithium iron phosphate particles, and the lithium iron phosphate finished product is obtained through air current crushing, screening and demagnetizing.
Claims (7)
1. A production line for preparing nano lithium iron phosphate from titanium dioxide auxiliary waste ferrous sulfate is characterized in that:
comprises a purification system, an oxidation system, a batching system, a synthesis system, an aging system, a washing and filtering system, a drying system and a lithium doping system; wherein,,
a purification system comprising a dissolution tank (3) and a prefilter (5);
a dissolving tank stirrer (7) is arranged in the dissolving tank (3), and a dissolving tank steam inlet (301), a dissolving tank deoxidized water inlet (302) and a dissolving tank titanium white auxiliary waste ferrous sulfate inlet (303) are arranged at the top end of the dissolving tank (3); the bottom end of the dissolving tank (3) is connected with the inlet of the prefilter (5) through a dissolving tank bottom pump (4);
An oxidation system comprising an oxidation kettle (12) and an iron sulfate buffer tank (14);
the oxidation kettle (12) is provided with an oxidation kettle stirrer (7-1), and the top end of the oxidation kettle (12) is provided with an oxidation kettle steam inlet (1201), an oxidation kettle deoxidized water inlet (1202), an oxidation kettle ferrous sulfate solution inlet (1203), a concentrated sulfuric acid inlet (1204) and a hydrogen peroxide inlet (1205); the oxidation kettle (12) is respectively connected with an output port of the prefilter (5), a steam conveying pipe, a deoxidized water conveying pipe, a concentrated sulfuric acid conveying pipe and a hydrogen peroxide conveying pipe, and ferrous sulfate filtrate purified by the prefilter (5) automatically flows into an oxidation system; the oxidation kettle (12) is communicated with the ferric sulfate buffer tank (14) through an oxidation kettle tank bottom pump (13), and ferric sulfate solution obtained by oxidation is conveyed to the ferric sulfate buffer tank (14) through the oxidation kettle tank bottom pump (13); the ferric sulfate buffer tank (14) is provided with a ferric sulfate buffer tank stirrer (7-2), the bottom of the ferric sulfate buffer tank (14) is connected with a ferric sulfate solution delivery pump (15), and the ferric sulfate solution is delivered to the synthesis system through the ferric sulfate solution delivery pump (15);
the batching system comprises a phosphoric acid batching system and an additive batching system;
the phosphoric acid batching system comprises a phosphoric acid solution preparation tank (23) and a phosphoric acid solution buffer tank (84), wherein the phosphoric acid solution preparation tank (23) is provided with a phosphoric acid solution preparation tank stirrer (7-3);
A steam inlet (2301) of the phosphoric acid solution preparation tank, a deoxidized water inlet (2302) of the oxidation kettle of the phosphoric acid solution preparation tank, a phosphoric acid inlet (2303) and a sodium hydroxide solution inlet (2304) are arranged at the top end of the phosphoric acid solution preparation tank (23); the phosphoric acid solution preparation tank (23) is connected with a steam conveying pipe, a deoxidized water conveying pipe, a sodium hydroxide solution conveying pipe and a phosphoric acid conveying pipe; the tank body is provided with a phosphoric acid solution preparation tank liquid level meter (6-3), a phosphoric acid solution preparation tank pH meter (2-3) and a phosphoric acid solution preparation tank thermometer (1-3), the bottom of the phosphoric acid solution preparation tank (23) is connected with a phosphoric acid solution buffer tank (84) through a phosphoric acid solution pouring pump (24), and the prepared sodium phosphate solution is conveyed into the phosphoric acid solution buffer tank (84); the phosphoric acid solution buffer tank (84) is provided with a phosphoric acid solution buffer tank stirrer (7-4), the phosphoric acid solution buffer tank (84) is provided with a phosphoric acid solution buffer tank liquid level meter (6-4), a phosphoric acid solution buffer tank pH meter (2-4) and a phosphoric acid solution buffer tank thermometer (1-4), the bottom of the phosphoric acid solution buffer tank (84) is connected with a phosphoric acid solution delivery pump (26), and the phosphoric acid solution is delivered to the synthesis system through the phosphoric acid solution delivery pump (26);
An additive dosing system comprising an additive dosing tank (33) and an additive buffer tank (35);
the top end of the additive preparation tank (33) is provided with an additive preparation tank steam inlet (3301), an additive preparation tank deoxidized water inlet (3302) and an additive preparation tank additive inlet (3303), and the additive preparation tank (33)
The device is connected with a steam conveying pipe, a deoxidized water conveying pipe and an additive conveying pipe; the additive preparation tank (33) is provided with an additive preparation tank liquid level meter (6-5) and an additive preparation tank stirrer (7-5), and the bottom of the additive preparation tank (33) is connected with the upper part of the additive buffer tank (35) through an additive solution pouring pump (34);
the additive buffer tank (35) is provided with an additive buffer tank liquid level meter (6-6) and an additive buffer tank stirrer (7-6), the bottom of the additive buffer tank (35) is connected with an additive solution delivery pump (36), and the additive solution is delivered to the synthesis system through the additive solution delivery pump (36);
a synthesis system comprising a first reactor (41), a second reactor (44);
the first reactor (41) is provided with a first reactor stirrer (7-7) and a first reactor pH meter (2-7), and the top end of the first reactor (41) is provided with a first reactor steam inlet (4101) and a first reactor deoxygenated water inlet (4102); the first reactor (41) is connected with a steam conveying pipe and a deoxidized water conveying pipe;
The second reactor (44) is provided with a second reactor stirrer (7-8) and a second reactor pH meter (2-8), and the top end of the second reactor (44) is provided with a second reactor steam inlet (4401) and a second reactor deaerated water inlet (4402); the second reactor (44) is connected with the steam conveying pipe and the deoxidized water conveying pipe;
the first reactor (41) and the second reactor (44) are connected with ferric sulfate solution output by the oxidation system, sodium phosphate solution output by the phosphoric acid batching system and additive solution output by the additive batching system, the ferric sulfate solution, the sodium phosphate solution output by the phosphoric acid batching system and the additive solution output by the additive batching system are respectively delivered into the two reactors in three parallel flow mode for synthesis reaction after being split, a flow meter is arranged on a split pipe, and the synthesized nano ferric phosphate foam flows out of the upper parts of the two reactors and flows into the aging system automatically after being combined;
the aging system comprises at least 3 aging tanks (47), wherein an aging tank stirrer (7-9) is arranged in the aging tanks (47), the aging tanks (47) are connected with a steam conveying pipe, a nitrogen conveying pipe, a condensed water conveying pipe and a nano ferric phosphate slurry conveying pipe of the synthesis system, the aging tanks (47) are provided with an aging tank liquid level meter and an aging tank thermometer, the bottoms of the aging tanks (47) are connected in parallel through an output pipe and are connected with an aging tank bottom pump (49), and nano ferric phosphate slurry is conveyed into the washing and filtering system through the aging tank bottom pump (49);
The washing and filtering system comprises a first-stage filter press (52) and a second-stage filter press (61), wherein nano ferric phosphate slurry output by the aging system enters the first-stage filter press (52) for primary filtration, a belt conveyor (53) is arranged at the lower part of the first-stage filter press (52), a beating tank (54) is arranged below the output end of the belt conveyor (53), and the output end is opposite to the inlet of the beating tank (54); the bottom of the beating tank (54) is connected with the upper part of another beating tank through a slurry conveying pump (56), the bottom of the beating tank is connected with the input end of a secondary filter press (61) through a secondary filter pressing feeding pump (58), a belt conveyor is arranged below the secondary filter press (61), and a nano iron phosphate filter cake output by the secondary filter press (61) is automatically dropped into the belt conveyor to be sent to a drying system;
the drying system comprises a vacuum dryer (64), the bottom of the vacuum dryer (64) is communicated with the top of a storage bin (65), a nano iron phosphate filter cake output by the washing and filtering system enters the vacuum dryer (64) to be dried for the first time to form powder, the powder enters the storage bin (65) through discharging, the storage bin (65) conveys the powder to a rotary furnace (67) through a hopper lifter A (66), a spiral conveyor (68) and a hopper lifter B (66-1) are sequentially arranged at the output end of the rotary furnace (67), the powder is lifted into a first demagnetizer (71) through the hopper lifter B (66-1), and a packaging bin (70) is arranged at an output port of the first demagnetizer (71);
The lithium doping system comprises a coarse grinding machine (73) and a mixing bin (74), wherein lithium carbonate particles in a packaging bin (70) enter the coarse grinding machine (73) through a first feeding machine (72) and enter the mixing bin (74) after dry grinding; the ferric phosphate powder output by the drying system enters a mixing bin (74) through a second feeding machine (72-1), and the glucose powder enters the mixing bin (74) through a third feeding machine (72-2) respectively; the output port of the mixing bin (74) is connected with the inlet of a wet mill (77), the wet mill (77) is connected with a deoxidized water conveying pipe, and the output port of the wet mill (77) is connected with the inlet of a spray dryer (78); the outlet of the spray dryer (78) is connected with a second demagnetizer (71-1), the outlet of the second demagnetizer (71-1) is connected with an electric heating roller kiln (80), the electric heating roller kiln (80) pulverizes lithium iron phosphate particles through an airflow pulverizer (83), the outlet at the bottom end of the airflow pulverizer (83) is connected with the inlet of a sieving machine (82), and the outlet of the sieving machine (82) is provided with a third demagnetizer (71-2);
the prefilter (5) is a common plate-and-frame filter press with purified air blowing;
control valves are arranged on the liquid conveying pipes;
the system is also provided with a DC control system, which comprises a control module, an operation panel table, an industrial personal computer and a display; the pH meters, the thermometers and the pressure transmitters in all the systems are responsible for collecting signals on site, and sending the signals to a control module for on-line on-site display or remote industrial personal computer display or display screen centralized display; the flowmeter is responsible for collecting signals, sending a control module to a line for on-site display or remote transmission industrial personal computer display or display screen for centralized display, and simultaneously providing control signals for controlling the opening and closing of the valve on the batching conveying pipe; the liquid level meter is responsible for collecting signals, sending a line of on-site display or remote transmission industrial personal computer display or centralized display of a display screen to the control module, and simultaneously providing control signals for controlling the opening and closing of a control valve on the feeding conveying pipe; the pump motor, the stirring motor and the conveying motor are powered on and off through the control module; the display is responsible for intensively displaying various returned field collected data and the processed record curves; the industrial personal computer is responsible for assigning values to the process parameters and returning instantaneous values for displaying the field process parameters; the operating panel table is responsible for inching control, manual automatic control mode conversion, power supply indication and electric appliance state display functions.
2. A method for preparing nano lithium iron phosphate by using titanium dioxide auxiliary waste ferrous sulfate as a raw material by adopting the production line according to claim 1, which is characterized in that: the method specifically comprises the following steps:
s1, taking titanium dioxide auxiliary waste ferrous sulfate as a raw material, introducing steam, feeding deoxidized water, stirring, and enabling a ferrous sulfate solution purified by a prefilter (5) to automatically flow into an oxidation kettle;
s2, adding concentrated sulfuric acid and hydrogen peroxide into an oxidation kettle to oxidize to obtain ferric sulfate solution, feeding the ferric sulfate solution into a ferric sulfate buffer tank (14), adding deoxidized water into the buffer tank, and respectively feeding the ferric sulfate solution, the prepared sodium phosphate solution and the additive solution in the buffer tank into a first reactor (41) and a second reactor (44) in a three-strand parallel flow mode after the ferric sulfate solution, the prepared sodium phosphate solution and the additive solution are all split;
s3, the synthesized nano ferric phosphate foam is respectively discharged from the upper end sides of the two reactors and flows into an aging tank (47) automatically after being converged, steam, nitrogen and condensed water are introduced into the aging tank for stirring and aging, the aged nano ferric phosphate slurry is conveyed into a first-stage filter press (52) and a second-stage filter press (61) for washing and filtering sequentially through an aging tank bottom pump, a filter cake is obtained, and the filter cake is dried and demagnetized to obtain nano ferric phosphate powder;
s4, the nano iron phosphate powder, glucose powder and lithium carbonate powder enter a mixed material, and then oxygen-removing water is added for wet grinding, drying, demagnetizing, calcining, jet milling, screening and demagnetizing to obtain a finished product of lithium iron phosphate.
3. The method for preparing nano lithium iron phosphate by using titanium dioxide auxiliary waste ferrous sulfate as a raw material according to claim 2, which is characterized in that: the condensate comes from a vacuum dryer (64) in the drying system.
4. The method for preparing nano lithium iron phosphate by using titanium white auxiliary waste ferrous sulfate as a raw material according to claim 3, which is characterized in that: in S3, nano ferric phosphate slurry output by the aging system enters the first-stage filter press (52) for primary filtration, deoxygenated water is introduced into the first-stage filter press (52) after filtrate flows away through a pipeline to carry out pressure flushing on an in-machine filter cake, deoxygenated water is reversely introduced into the filter press after filtrate flows away to squeeze and squeeze water on the in-machine filter cake, finally, a discharged filter cake is self-dropped and regulated into a belt conveyor (53) to be sent into a pulping tank (54), nano ferric phosphate slurry is conveyed into a slurry buffer tank (60) through a slurry conveying pump (56), nano ferric phosphate slurry is conveyed into a second-stage filter press (61) through a second-stage filter press feeding pump (58), deoxygenated water is introduced into the second-stage filter press (61) after filtrate flows away through a pipeline to carry out pressure flushing on the in-machine filter cake, deoxygenated water is reversely introduced into the filter press to squeeze and finally, the discharged filter cake is self-dropped and regulated into the belt conveyor (53) to be sent into a drying system.
5. The method for preparing nano lithium iron phosphate by using titanium dioxide secondary waste ferrous sulfate as a raw material, which is characterized by comprising the following steps of: and S4, uniformly mixing the three materials, then, adding deoxidized water into a wet mill (77) for secondary wet milling, and drying the pasty mixture after wet milling in a spray dryer (78) to form a granular mixture.
6. The method for preparing nano lithium iron phosphate by using titanium dioxide secondary waste ferrous sulfate as a raw material according to claim 5, which is characterized in that: and S4, removing iron by a first demagnetizer (71) and falling into an electric heating roller kiln (80) when the granular mixture formed after drying is discharged, and calcining the granular mixture to form lithium iron phosphate particles.
7. The production line for preparing nano lithium iron phosphate from titanium dioxide auxiliary waste ferrous sulfate, which is characterized by comprising the following steps of: the method is applied to the preparation of nano lithium iron phosphate by using titanium dioxide secondary waste ferrous sulfate.
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