CN204407414U - LiFePO4 solvent heat Preparation equipment - Google Patents
LiFePO4 solvent heat Preparation equipment Download PDFInfo
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- CN204407414U CN204407414U CN201520055775.9U CN201520055775U CN204407414U CN 204407414 U CN204407414 U CN 204407414U CN 201520055775 U CN201520055775 U CN 201520055775U CN 204407414 U CN204407414 U CN 204407414U
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- 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
Abstract
A kind of LiFePO4 solvent heat Preparation equipment, comprise product and prepare unit and liquid waste processing cycling element, described product is prepared unit and is comprised the feed arrangement connected successively, reaction unit, filter and countercurrent washing device, described liquid waste processing cycling element comprises interconnective flash distillation plant and equipment for separating liquid from solid, described filter is separated the filtrate obtained and enters described countercurrent washing device, filtrate enters flash distillation plant and dewaters, mixture after described flash distillation plant dewaters enters equipment for separating liquid from solid and carries out Separation of Solid and Liquid, obtain organic solvent and accessory substance respectively, a described organic solvent part returns described feed arrangement and again prepares burden, enter countercurrent washing device together with the isolated water of a part of and described flash distillation plant and countercurrent washing is carried out to filtrate, the cleaning solution that countercurrent washing obtains enters liquid waste processing cycling element and carries out liquid waste processing together with filtrate.
Description
Technical field
The utility model relates to anode active material of lithium ion battery preparation field, is specifically related to a kind of solvent heat Preparation equipment of LiFePO4.
Background technology
LiFePO4 (LiFePO4, LFP), as a kind of important anode active material of lithium ion battery, has a wide range of applications in the market of energy storage and electrokinetic cell.The preparation of current LFP mainly contains two large class process routes, be respectively with ferrous oxalate technique (A123 Systems company of the U.S. etc.), iron oxide red technique (Valence Technology company of the U.S. etc.), ferric phosphate technique (Canadian Phostech Lithium company, A123 Systems company of the U.S. etc.) for the solid-phase process preparation of representative and with solvent heat process route (Clariant Chemicals company of Switzerland, Hanwa Chemical company of Korea S etc.) for representing Liquid preparation methods technique.
Solid-phase process preparation becomes a kind of preparation technology be most widely used in prior art because production cost is low, but use LFP particle size distribution heterogeneity, product poor controllability that solid-phase process preparation is prepared, thus limit the performance of the chemical property of LFP own, cause properties of product to reduce.Liquid preparation methods technique especially solvent heat preparation technology compared to solid-phase process preparation, have and easily realize that low temperature synthesis serialization, product crystallization purity are high, even particle size distribution, easily realize the advantage such as in-situ carburization, electrochemical performance, but solvent heat preparation technology is usually using the mixed solvent of water and organic solvent as the reaction medium of solvent heat, a large amount of waste liquid can be produced in preparation process, how rationally processing a large amount of waste liquid, the lithium resource in recycling waste liquid and organic solvent are the keys of Liquid preparation methods technique.Prior art is when carrying out lithium resource and organic solvent reclaims, because lithium salts is dissolved in the mixed solvent of water and organic solvent composition, the general method of distillation that adopts comes lithium salts in Recycling of waste liquid and organic solvent, but carry out distilling the distillation equipment needing to use complexity, and the energy consumption of distillation is very high, causes the production cost of LEP significantly to increase; If do not reclaimed the lithium resource in waste liquid and organic solvent, then can cause a large amount of wastes of lithium resource and organic solvent, the production cost of LEP can be caused equally significantly to increase.
Utility model content
In view of this, necessaryly provide a kind of and can prepare high-quality LiFePO 4 material and the low LiFePO4 solvent heat Preparation equipment of production cost.
A kind of LiFePO4 solvent heat Preparation equipment, comprise product and prepare unit and liquid waste processing cycling element, described product is prepared unit and is comprised the feed arrangement connected successively, reaction unit, filter and countercurrent washing device, described liquid waste processing cycling element comprises interconnective flash distillation plant and equipment for separating liquid from solid, the waste liquid that described liquid waste processing cycling element is used for preparing described product unit generation processes and utilizes, described waste liquid comprises organic solvent, water and accessory substance, described organic solvent and water dissolve each other, described accessory substance is water-soluble and be insoluble to described organic solvent,
Described filter is used for filtering the product in described reaction unit, filters the filtrate obtained and enters described countercurrent washing device, filters the filtrate obtained and enters described flash distillation plant; Described flash distillation plant is used for carrying out flash distillation to described filtrate and dewaters, and flash separation water out enters described countercurrent washing device, and the mixture that flash separation goes out enters described equipment for separating liquid from solid; Described equipment for separating liquid from solid is used for carrying out Separation of Solid and Liquid to described mixture, and the organic solvent part that Separation of Solid and Liquid obtains reenters described feed arrangement, and another part enters described countercurrent washing device; Enter in described countercurrent washing device together with the organic solvent that described flash separation water out and described Separation of Solid and Liquid obtain and countercurrent washing is carried out to described filtrate, obtain the LiFePO4 of purifying after countercurrent washing, the cleaning solution produced after countercurrent washing enters described liquid waste processing cycling element as described waste liquid together with described filtered fluid to carry out processing and utilizing.
The LiFePO4 solvent heat Preparation equipment that the utility model provides, by flash distillation plant and equipment for separating liquid from solid, integrated treatment is carried out to waste liquid, these two kinds device structure is simple, energy consumption is low, fast and efficiently the water in waste liquid, organic solvent and separation of by-products can be opened, reduce the production cost of LFP; Water, organic solvent and accessory substance is obtained respectively through the process of described liquid waste processing cycling element, wherein this organic solvent part can return described feed arrangement and again prepares burden, a part can be washed the filtrate in described countercurrent washing device together with water, cleaning solution after washing can reenter described liquid waste processing cycling element to carry out processing and recycling, this LiFePO4 solvent heat Preparation equipment can carry out integrated treatment and utilization to waste liquid, thus greatly reduce the use of fresh organic solvent, significantly reduce the production cost of LFP further.
Accompanying drawing explanation
The LiFePO4 solvent heat preparation technology schematic flow sheet that Fig. 1 provides for the utility model.
The LiFePO4 solvent heat Preparation equipment structural representation that Fig. 2 provides for the utility model.
Main element symbol description
| LiFePO4 solvent heat Preparation equipment | 10 |
| Product prepares unit | 100 |
| Feed arrangement | 110 |
| Organic solvent head tank | 111 |
| First mixing tank | 112 |
| Second mixing tank | 113 |
| 3rd mixing tank | 114 |
| Reaction unit | 120 |
| Solvent thermal reaction still | 121 |
| Gauge | 122 |
| Feed pump | 123 |
| Discharging pump | 124 |
| Filter | 130 |
| Filtration feed mouth | 131 |
| Filter discharging opening | 132 |
| Filter liquid outlet | 133 |
| Countercurrent washing device | 140 |
| Countercurrent washing charging aperture | 141 |
| Countercurrent washing discharging opening | 142 |
| Countercurrent washing inlet | 143 |
| Countercurrent washing liquid outlet | 144 |
| First sink | 145 |
| Second sink | 146 |
| 3rd sink | 147 |
| Liquid waste processing cycling element | 200 |
| Flash distillation plant | 210 |
| Flash distillation inlet | 211 |
| Flash distillation liquid outlet | 212 |
| Flash distillation discharging opening | 213 |
| Preheater | 214 |
| Gas-liquid separator | 215 |
| Equipment for separating liquid from solid | 220 |
| Separation of Solid and Liquid charging aperture | 221 |
| Separation of Solid and Liquid discharging mouth | 222 |
| Separation of Solid and Liquid fluid mouth | 223 |
| Delivery pump | 300 |
Following embodiment will further illustrate the utility model in conjunction with above-mentioned accompanying drawing.
Embodiment
The LiFePO4 solvent heat preparation technology provided the utility model below in conjunction with the accompanying drawings and the specific embodiments and Preparation equipment are described in further detail.
Refer to Fig. 1, the utility model provides a kind of LiFePO4 solvent heat preparation technology, comprising:
S1, provides organic solvent, ferrous sulfate, lithium hydroxide and phosphoric acid solution, and described phosphoric acid solution comprises water and phosphoric acid;
S2, mixes described organic solvent, ferrous sulfate, lithium hydroxide and phosphoric acid solution, obtains precursor solution;
S3, makes described precursor solution carry out solvent thermal reaction, obtains the first suspension-turbid liquid after completion of the reaction;
S4, filter described first suspension-turbid liquid, obtain LiFePO4 wet stock and filtered fluid respectively, described filtered fluid comprises described organic solvent, water and lithium sulfate;
S5, carries out flash distillation by described filtered fluid, obtains water and the second suspension-turbid liquid respectively, and described second suspension-turbid liquid comprises described organic solvent and lithium sulfate, and described lithium sulfate is suspended in described organic solvent with the form of precipitation;
S6, carries out Separation of Solid and Liquid to described second suspension-turbid liquid, obtains described lithium sulfate and described organic solvent respectively, and this organic solvent part returns step S1 and recycles, and another part enters step S7 and uses;
S7, by the described organic solvent mixing of part obtained in the described water obtained in step S5 and step S6, countercurrent washing is carried out to described LiFePO4 wet stock, obtain the LiFePO4 wet stock after purifying and cleaning solution respectively, the constituent of described cleaning solution is identical with the constituent of described filtered fluid, is returned in step S5 by this cleaning solution and recycles together with described filtered fluid;
S8, the LiFePO4 wet stock after dry described purifying, obtains described LiFePO4 crystal.
In step sl, described organic solvent can dissolve each other with water, and can dissolve described ferrous sulfate and lithium hydroxide, but this organic solvent can not dissolve lithium sulfate.Described organic solvent can one or more for being selected from ethanol, ethylene glycol, glycerol, diethylene glycol (DEG), triethylene glycol, tetraethylene glycol, butantriol, n-butanol and isobutanol, are preferably one or more in ethanol, ethylene glycol and glycerol.Organic solvent described in the utility model embodiment is ethylene glycol.Described ferrous sulfate is specifically as follows ferrous sulfate heptahydrate (FeSO
47H
2o).Described lithium hydroxide is specifically as follows Lithium hydroxide monohydrate (LiOHH
2o).In described phosphoric acid solution, the mass ratio of phosphoric acid can be 40% to 86%.In the utility model embodiment, in described phosphoric acid solution, the mass ratio of phosphoric acid is 85%.
In step s 2, in described precursor solution, described organic solvent and described water are mixed to form mixed solvent, and this mixed solvent is the reaction medium of described solvent thermal reaction.Preferably, the mol ratio of described lithium hydroxide and ferrous sulfate is more than or equal to 3:1, and the mol ratio within the scope of this can ensure that the ferrous ion in described ferrous sulfate is all transformed in described LiFePO4 crystal in described solvent thermal reaction.
The mode that described organic solvent, ferrous sulfate, lithium hydroxide and phosphoric acid solution carry out mixing is not limit, as long as described precursor solution can be obtained.In the utility model embodiment, first described organic solvent and described ferrous sulfate are carried out being mixed to get the first mixed solution, described organic solvent and described lithium hydroxide are mixed to get the second mixed solution, more described first mixed solution, the second mixed solution and phosphoric acid solution are carried out being mixed to get described precursor solution.
In step s3, synthesized described LiFePO4 crystal after described solvent thermal reaction, described LiFePO4 crystal is dispersed in described mixed solvent.The accessory substance lithium sulfate that described first suspension-turbid liquid comprises described LiFePO4 crystal, described mixed solvent and is dissolved in described mixed solvent.The temperature of described solvent thermal reaction can be 120 DEG C ~ 300 DEG C, and pressure limit can be 0.2MPa ~ 2.0MPa, and the reaction time can be 0.5 hour ~ 10 hours.
In step s 4 which, the method for described filtration can be the filter method that filtration under diminished pressure, pressure filtration, vacuum filtration etc. are conventional.In the utility model embodiment, continuous precision film filter is adopted to filter described first suspension-turbid liquid.The temperature of described filtration is preferably 80 DEG C ~ 180 DEG C, and described in this temperature range, the first suspension-turbid liquid has lower viscosity, thus be conducive to described first suspension-turbid liquid realize filter fast and efficiently.More preferably, the temperature of described filtration is preferably 100 ~ 140 DEG C.
In step s 5, directly water is separated from described 3rd mixed solution by the method for flash distillation, described lithium sulfate can be made to separate out in described organic solvent with the form of precipitation, thus form described second suspension-turbid liquid.Be appreciated that, also a small amount of unreacted phosphate radical may be contained in described filtered fluid, this a small amount of unreacted phosphate radical can change lithium phosphate precipitation in flash process separates out in the lump in described organic solvent, therefore may there is a small amount of lithium phosphate precipitation in described second suspension-turbid liquid.
Described flash distillation refers to that the saturated water of relatively high pressure enters after in the container of relatively low pressure and becomes the process of water vapour because the unexpected reduction of pressure makes described saturated water seethe with excitement.In the utility model embodiment, the concrete steps of described flash distillation comprise:
S51, is preheated to 100 DEG C to 160 DEG C at ambient pressure by described filtered fluid in a preheater;
S52, pass in a gas-liquid separator by the described filtered fluid being preheated to 100 DEG C to 160 DEG C, the pressure in this gas-liquid separator is 3kPa to 60kPa.
Between 100 DEG C to 160 DEG C, the water in described filtered fluid reaches capacity state, and when to enter pressure be the gas-liquid separator of 3kPa to 60kPa to this filtered fluid, the water in described filtered fluid seethes with excitement rapidly vaporization, thus spins off from described filtered fluid rapidly.
In step s 6, described accessory substance lithium sulfate and described organic solvent quick separating can namely be made by simple Separation of Solid and Liquid.Isolated described lithium sulfate can be passed through the highly basic process such as NaOH, again obtained described lithium hydroxide raw material.Isolated described organic solvent major part returns in step S1 and recycles, and adopts the mode of countercurrent washing to wash after another part mixes with the water flashed off in step S6 to described LiFePO4 wet stock.Be appreciated that described a small amount of lithium phosphate precipitation also can be followed described lithium sulfate and is separated in the lump.In the utility model embodiment, the method for described Separation of Solid and Liquid is centrifugation.
In the step s 7, the object of described countercurrent washing takes away, the impurity such as sulfate radical, lithium ion adsorbed in described LiFePO4 wet stock to realize the purifying to described LiFePO4 wet stock.Described countercurrent washing can be multi-stage countercurrent washing, and described multi-stage countercurrent washing can carry out purifying to described LiFePO4 wet stock quickly and efficiently.In the utility model embodiment, described countercurrent washing is three stage countercurrent washings.Cleaning solution after described countercurrent washing is identical with the constituent of described filtered fluid, and this cleaning solution can enter to reenter in step S6 and carry out processing and recycling together with described filtered fluid.
In step s 8, carrying out dry mode to the LiFePO4 wet stock of described purifying can be the conventional drying method such as natural air drying, spraying dry, heat drying, vacuumize, microwave drying.
The LiFePO4 solvent heat preparation technology that the utility model provides provides two recycle circuits and carrys out integrated treatment and utilize waste liquid, article one, be organic solvent recycle circuit, organic solvent becomes waste liquid after described solvent thermal reaction, and the organic solvent that liquid waste processing obtains is further used as raw material and again participates in reaction; Article one, be cleaning solution recycle circuit, the water that liquid waste processing obtains and organic solvent can carry out countercurrent washing to described LiFePO4 wet stock, and the cleaning solution that countercurrent washing is reacted complete can again carry out liquid waste processing and obtain water and organic solvent.
The LiFePO4 solvent heat preparation technology that the utility model provides, by the method for flash distillation and centrifugation, integrated treatment is carried out to waste liquid, fast and efficiently the water in waste liquid, organic solvent and lithium sulfate separation of by-products can be opened, these two kinds of methods realization simple to operate, easy and energy consumption is lower, thus reduce the production cost of LFP; By two recycle circuits, waste liquid is fully utilized, significantly reduce the consumption of fresh organic solvent, and significantly reduce the production cost of LFP further.The LiFePO4 solvent heat preparation technology that the utility model provides, the consumption of organic solvent in existing preparation technology can be made to be reduced to 1 cubic metre of/ton of LFP by 32 cubic metres of/ton of LFP, and the production cost of LFP can be made within existing about 100,000 yuan/ton lower to 3.5 ten thousand yuan/ton.
The LiFePO4 solvent heat preparation technology that the utility model provides, there is low temperature synthesis serialization, easily realize the advantages such as in-situ carburization, the LFP product crystallization purity prepared is high, even particle size distribution, electrochemical performance, and whole production process does not produce the secondary pollutions such as waste liquid, waste residue and waste gas, real energy-saving and environment friendly, there is very strong exemplary effect, meet national energy-saving environmental requirement.
Refer to Fig. 2, the utility model provides a kind of LiFePO4 solvent heat Preparation equipment 10 further, comprises product and prepares unit 100 and liquid waste processing cycling element 200.Described product is prepared unit 100 and is comprised the feed arrangement 110, reaction unit 120, filter 130 and the countercurrent washing device 140 that connect successively.Described liquid waste processing cycling element 200 comprises interconnective flash distillation plant 210 and equipment for separating liquid from solid 220.
Described feed arrangement 110 is for providing reaction raw materials for described reaction unit 120.Described reaction raw materials is described organic solvent, ferrous sulfate, lithium hydroxide and phosphoric acid solution.In the utility model embodiment, described feed arrangement 110 comprises organic solvent materials tank 111, first mixing tank 112, second mixing tank 113 and the 3rd mixing tank 114.Described organic solvent head tank 111 is connected with described first mixing tank 112 and the second mixing tank 113 respectively.Described first mixing tank 112 and the second mixing tank 113 are connected with described 3rd mixing tank 114 simultaneously.Described organic solvent head tank 111 is for providing described organic solvent for described first mixing tank 112 and the second mixing tank 113.Described first mixing tank 112 is for being undertaken being mixed to form described first mixed solution by described organic solvent and described ferrous sulfate.Described second mixing tank 113 is for being undertaken being mixed to form described second mixed solution by described organic solvent and described lithium hydroxide.Described 3rd mixing tank 114 for described first mixed solution, the second mixed solution and phosphoric acid solution are mixed to form described precursor solution, described precursor solution and described reaction raw materials.Be appreciated that those skilled in the art also can adopt other feed arrangements to provide described reaction raw materials for described reaction unit 120.
Described reaction unit 120 carries out solvent thermal reaction for making described reaction raw materials, thus synthesizes described LiFePO4 crystal.Described reaction unit 120 comprises a solvent thermal reaction still 121, and this solvent thermal reaction still 121 is places that described solvent thermal reaction carries out.In the utility model embodiment, this solvent thermal reaction still 121 is a high temperature and high pressure kettle.Particularly, described solvent thermal reaction still 121 can be a sealing autoclave, by to sealing autoclave pressurization or utilize the self-generated pressure of reactor steam inside to make reactor internal pressure increase, thus the reaction raw materials of reactor inside is reacted under high-temperature and high-pressure conditions.Described reaction unit 120 can comprise a gauge 122 further, and this gauge 122 is for controlling the input of reaction raw materials described in described solvent thermal reaction still 121.
Described filter 130 is for filtering described first suspension-turbid liquid.Described filter 130 comprises a filtration feed mouth 131, and filters discharging opening 132 and a filtration liquid outlet 133.Described filtration feed mouth 131 is connected with described reaction unit 120, and described first suspension-turbid liquid is entered in described filter 130 by described filtration feed mouth 131.Described filtration discharging opening 132 is connected with described countercurrent washing device 140, filters the described LiFePO4 wet stock obtained and enters described countercurrent washing device 140 by described filtration discharging opening 132.Described filtration liquid outlet 133 is connected with described flash distillation plant 210, filters the described filtered fluid obtained and enters described flash distillation plant 210 by described filtration liquid outlet 133.This filter 130 can be the typical filter equipment such as tubular filter, continous way pressing filter, film filter, vacuum filter.In the utility model embodiment, described filter 130 is continuous precision film filter.
Described countercurrent washing device 140 is for carrying out washing purifying to described LiFePO4 wet stock.Described countercurrent washing device 140 comprises countercurrent washing charging aperture 141, countercurrent washing discharging opening 142, countercurrent washing inlet 143 and a countercurrent washing liquid outlet 144.Described countercurrent washing charging aperture 141 is connected with described filtration discharging opening 132, the LiFePO4 wet stock obtained after described filtration enters described countercurrent washing device 140 from described countercurrent washing charging aperture 141, and the LiFePO4 wet stock after described purifying is from the discharging of described countercurrent washing discharging opening 142 and enter next step operation.Described countercurrent washing inlet 143 is connected with described flash distillation plant 210 and equipment for separating liquid from solid 220 respectively, and the described organic solvent that the water flashed off and centrifugation obtain enters described countercurrent washing device from described countercurrent washing inlet 143 simultaneously.Described countercurrent washing liquid outlet 144 is connected with described flash distillation plant 210, and the described filtered fluid obtained after countercurrent washing enters described flash distillation plant 210 by described countercurrent washing liquid outlet 144.
In the utility model embodiment, described countercurrent washing device 140 is one or three stage countercurrent wash mills, and this countercurrent washing device 140 comprises the first sink 145, second sink 146 and the 3rd sink 147 that connect successively; Described countercurrent washing charging aperture 141 and countercurrent washing liquid outlet 144 are arranged on described first sink 145, and described countercurrent washing discharging opening 142 and countercurrent washing inlet 143 are arranged on described 3rd sink 147; When carrying out countercurrent washing, described LiFePO4 wet stock moves from described first sink 145 to described 3rd sink 147, and described water and organic solvent move from described 3rd sink 147 to described first sink 145.
Described flash distillation plant 210 for carrying out flash distillation to described filtered fluid directly to remove the water in described filtered fluid, and obtains described second suspension-turbid liquid.Described flash distillation plant 210 comprises flash distillation inlet 211, flash distillation liquid outlet 212 and a flash distillation discharging opening 213.Described flash distillation inlet 211 is connected with described filtration liquid outlet 133 and countercurrent washing liquid outlet 144 respectively, and the described filtered fluid that filtration obtains and the described filtered fluid that countercurrent washing obtains enter described flash distillation plant 210 from described flash distillation inlet 211.Described flash distillation liquid outlet 212 is connected with described countercurrent washing inlet 143, and the water flashed off enters described countercurrent washing device 140 by described flash distillation liquid outlet 212.Described flash distillation discharging opening 213 is connected with described equipment for separating liquid from solid 220, and described second suspension-turbid liquid that flash distillation obtains enters described equipment for separating liquid from solid 220 by described flash distillation discharging opening 213.
In the utility model embodiment, described flash distillation plant 210 comprises interconnective preheater 214 and gas-liquid separator 215.Described preheater 214, for heating described filtered fluid, to reach capacity state to make the water in described filtered fluid.Described gas-liquid separator 215 can provide vacuum environment, to seethe with excitement rapidly in a low pressure environment vaporization to make the water in the described filtered fluid after described preheater preheats.Described flash distillation inlet 211 is arranged on described preheater 214, and described flash distillation liquid outlet 212 and flash distillation discharging opening 213 are arranged on described gas-liquid separator 215.
Described equipment for separating liquid from solid 220 is for carrying out Separation of Solid and Liquid to the lithium sulfate in described second suspension-turbid liquid and organic solvent.Described equipment for separating liquid from solid 220 comprises Separation of Solid and Liquid charging aperture 221, Separation of Solid and Liquid discharging mouth 222 and a Separation of Solid and Liquid fluid mouth 223.Described Separation of Solid and Liquid charging aperture 221 is connected with described flash distillation discharging opening 213, and described second suspension-turbid liquid enters described equipment for separating liquid from solid 220 by described Separation of Solid and Liquid charging aperture 221.Described lithium sulfate is from the discharging of described Separation of Solid and Liquid discharging mouth 222.Described Separation of Solid and Liquid fluid mouth 223 is connected with described feed arrangement 110 with described countercurrent washing inlet 143 respectively, a described organic solvent part for solid-liquid separation enters described feed arrangement 110 and again prepares burden, and another part enters in described countercurrent washing device 140 and carries out washing purifying to described LiFePO4 wet stock together with the water removed in described flash distillation plant 210.In the utility model embodiment, described equipment for separating liquid from solid 220 is centrifugal separator.
Described LiFePO4 solvent heat Preparation equipment can comprise multiple delivery pump 300 further, and this delivery pump 300 is for being delivered to another device by the material of liquid state from a device.
The LiFePO4 solvent heat Preparation equipment that the utility model provides, by flash distillation plant and equipment for separating liquid from solid, integrated treatment is carried out to waste liquid, these two kinds device structure is simple, energy consumption is low, fast and efficiently the water in waste liquid, organic solvent and lithium sulfate separation of by-products can be opened, reduce the production cost of LFP.The liquid outlet of described flash distillation plant is connected with described countercurrent washing device inlet respectively with the liquid outlet of described equipment for separating liquid from solid, the water that can make to utilize liquid waste processing to obtain and organic solvent carry out countercurrent washing to described LiFePO4 wet stock, the liquid outlet of described countercurrent washing device is connected with the inlet of flash distillation plant further, the complete cleaning solution of countercurrent washing can enter liquid waste processing range site further and carry out liquid waste processing, thus forms the recycle circuit of a cleaning solution; The liquid outlet of described equipment for separating liquid from solid is also connected with described feed arrangement, the organic solvent that liquid waste processing can be made to obtain again is prepared burden and is reacted, thus form an organic solvent recycle circuit, the foundation of these two recycle circuits greatly reduces the use of fresh organic solvent, significantly reduces the production cost of LFP further.
Claims (10)
1. a LiFePO4 solvent heat Preparation equipment, it is characterized in that, comprise product and prepare unit and liquid waste processing cycling element, described product is prepared unit and is comprised the feed arrangement connected successively, reaction unit, filter and countercurrent washing device, described liquid waste processing cycling element comprises interconnective flash distillation plant and equipment for separating liquid from solid, the waste liquid that described liquid waste processing cycling element is used for preparing described product unit generation processes and utilizes, described waste liquid comprises organic solvent, water and accessory substance, described organic solvent and water dissolve each other, described accessory substance is water-soluble and be insoluble to described organic solvent,
Described filter is used for filtering the product in described reaction unit, filters the filtrate obtained and enters described countercurrent washing device, filters the filtrate obtained and enters described flash distillation plant; Described flash distillation plant is used for carrying out flash distillation to described filtrate and dewaters, and flash separation water out enters described countercurrent washing device, and the mixture that flash separation goes out enters described equipment for separating liquid from solid; Described equipment for separating liquid from solid is used for carrying out Separation of Solid and Liquid to described mixture, and the organic solvent part that Separation of Solid and Liquid obtains reenters described feed arrangement, and another part enters described countercurrent washing device; Enter in described countercurrent washing device together with the organic solvent that described flash separation water out and described Separation of Solid and Liquid obtain and countercurrent washing is carried out to described filtrate, obtain the LiFePO4 of purifying after countercurrent washing, the cleaning solution produced after countercurrent washing enters described liquid waste processing cycling element as described waste liquid together with described filtered fluid to carry out processing and utilizing.
2. LiFePO4 solvent heat Preparation equipment as claimed in claim 1, it is characterized in that, described filter comprises a filtration discharging opening and and filters liquid outlet, described countercurrent washing device comprises a countercurrent washing charging aperture, a countercurrent washing discharging opening, a countercurrent washing inlet and a countercurrent washing liquid outlet, described flash distillation plant comprises a flash distillation inlet, a flash distillation liquid outlet and a flash distillation discharging opening, and described equipment for separating liquid from solid comprises a Separation of Solid and Liquid charging aperture, a Separation of Solid and Liquid discharging mouth and a Separation of Solid and Liquid fluid mouth; Described filtration liquid outlet is connected with described flash distillation inlet, and described flash distillation discharging opening is connected with described Separation of Solid and Liquid charging aperture, and described Separation of Solid and Liquid fluid mouth is connected with described feed arrangement; Described filtration discharging opening is connected with described countercurrent washing charging aperture, and described flash distillation liquid outlet is connected with described countercurrent washing inlet with described Separation of Solid and Liquid fluid mouth simultaneously, and described countercurrent washing liquid outlet is connected with described flash distillation inlet.
3. LiFePO4 solvent heat Preparation equipment as claimed in claim 1, it is characterized in that, described feed arrangement comprises organic solvent materials tank, the first mixing tank, the second mixing tank and the 3rd mixing tank, described organic solvent head tank is connected with described first mixing tank and the second mixing tank respectively, and described first mixing tank and the second mixing tank are connected with described 3rd mixing tank simultaneously.
4. LiFePO4 solvent heat Preparation equipment as claimed in claim 1, it is characterized in that, described reaction unit comprises a solvent thermal reaction still and a gauge, and this gauge is for controlling the input of reaction raw materials in described solvent thermal reaction still.
5. LiFePO4 solvent heat Preparation equipment as claimed in claim 1, it is characterized in that, described filter is continuous precision film filter.
6. LiFePO4 solvent heat Preparation equipment as claimed in claim 1, it is characterized in that, described countercurrent washing device is one or three stage countercurrent wash mills, this countercurrent washing device comprises the first sink, the second sink and the 3rd sink that connect successively, described filtrate moves from described first sink to the direction of described 3rd sink, and the organic solvent that described flash separation water out and described Separation of Solid and Liquid obtain is from described 3rd sink to described first sink flowing.
7. LiFePO4 solvent heat Preparation equipment as claimed in claim 6, it is characterized in that, described countercurrent washing device comprises a countercurrent washing charging aperture, a countercurrent washing discharging opening, a countercurrent washing inlet and a countercurrent washing liquid outlet, described countercurrent washing charging aperture and countercurrent washing liquid outlet are arranged on described first sink, and described countercurrent washing discharging opening and countercurrent washing inlet are arranged on described 3rd sink.
8. LiFePO4 solvent heat Preparation equipment as claimed in claim 1, it is characterized in that, described flash distillation plant comprises interconnective preheater and gas-liquid separator, described preheater is used for heating described filtrate, thus make the water in described filtrate reach hypersaturated state, described gas-liquid separator is used for providing vacuum environment, thus water is separated from described filtrate.
9. LiFePO4 solvent heat Preparation equipment as claimed in claim 8, it is characterized in that, described flash distillation plant comprises a flash distillation inlet, a flash distillation liquid outlet and a flash distillation discharging opening, described flash distillation inlet is arranged on described preheater, and described flash distillation liquid outlet and flash distillation discharging opening are arranged on described gas-liquid separator.
10. LiFePO4 solvent heat Preparation equipment as claimed in claim 1, it is characterized in that, described equipment for separating liquid from solid is centrifugal separator.
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| CN201520055775.9U CN204407414U (en) | 2015-01-27 | 2015-01-27 | LiFePO4 solvent heat Preparation equipment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201520055775.9U CN204407414U (en) | 2015-01-27 | 2015-01-27 | LiFePO4 solvent heat Preparation equipment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104577122A (en) * | 2015-01-27 | 2015-04-29 | 江苏华东锂电技术研究院有限公司 | Lithium iron phosphate solvothermal preparation device |
| WO2016119593A1 (en) * | 2015-01-27 | 2016-08-04 | 江苏华东锂电技术研究院有限公司 | Lithium iron phosphate solvothermal preparation process |
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2015
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104577122A (en) * | 2015-01-27 | 2015-04-29 | 江苏华东锂电技术研究院有限公司 | Lithium iron phosphate solvothermal preparation device |
| WO2016119594A1 (en) * | 2015-01-27 | 2016-08-04 | 江苏华东锂电技术研究院有限公司 | Lithium iron phosphate solvothermal preparation equipment |
| WO2016119593A1 (en) * | 2015-01-27 | 2016-08-04 | 江苏华东锂电技术研究院有限公司 | Lithium iron phosphate solvothermal preparation process |
| US20170320737A1 (en) * | 2015-01-27 | 2017-11-09 | Jiangsu Huadong Institute Of Li-Ion Battery Co., Ltd. | Solvothermal method for making lithium iron phosphate |
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Effective date of registration: 20170508 Address after: Yangshe shoal Lake Park in Suzhou Branch Chong Hua Chang Lu 215699 cities in Jiangsu city of Zhangjiagang Province Co-patentee after: Tsinghua University Patentee after: Jiangsu annals of New Energy Materials Technology Co., Ltd. Address before: Suzhou City, Jiangsu province 215699 Zhangjiagang Yang Hua Chang Lu Co-patentee before: Tsinghua University Patentee before: Jiangsu Huadong Institute of Li-ion Battery Co., Ltd. |