CN116598589B - Preparation method of sodium ion battery electrolyte - Google Patents
Preparation method of sodium ion battery electrolyte Download PDFInfo
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- CN116598589B CN116598589B CN202310613014.XA CN202310613014A CN116598589B CN 116598589 B CN116598589 B CN 116598589B CN 202310613014 A CN202310613014 A CN 202310613014A CN 116598589 B CN116598589 B CN 116598589B
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 53
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 145
- 239000002994 raw material Substances 0.000 claims abstract description 72
- 238000003756 stirring Methods 0.000 claims abstract description 71
- 239000002904 solvent Substances 0.000 claims abstract description 50
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 34
- 230000018044 dehydration Effects 0.000 claims abstract description 33
- 239000000654 additive Substances 0.000 claims abstract description 23
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 239000003063 flame retardant Substances 0.000 claims abstract description 18
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- 239000003223 protective agent Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 45
- 239000007788 liquid Substances 0.000 claims description 31
- 238000001816 cooling Methods 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 17
- 238000010992 reflux Methods 0.000 claims description 16
- 239000007921 spray Substances 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 13
- 239000002808 molecular sieve Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 10
- 239000011815 overcharge protection agent Substances 0.000 claims description 8
- 239000000110 cooling liquid Substances 0.000 claims description 7
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 6
- 230000000149 penetrating effect Effects 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000002826 coolant Substances 0.000 claims description 4
- HHNHBFLGXIUXCM-GFCCVEGCSA-N cyclohexylbenzene Chemical group [CH]1CCCC[C@@H]1C1=CC=CC=C1 HHNHBFLGXIUXCM-GFCCVEGCSA-N 0.000 claims description 4
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 4
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 claims description 4
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 4
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 claims description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 3
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 3
- QXZNUMVOKMLCEX-UHFFFAOYSA-N [Na].FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F Chemical compound [Na].FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F QXZNUMVOKMLCEX-UHFFFAOYSA-N 0.000 claims description 3
- 235000010290 biphenyl Nutrition 0.000 claims description 3
- 239000004305 biphenyl Substances 0.000 claims description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 claims description 3
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 claims description 2
- -1 sodium hexafluorophosphate Chemical compound 0.000 claims description 2
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 claims description 2
- 229910001488 sodium perchlorate Inorganic materials 0.000 claims description 2
- XXYVTWLMBUGXOK-UHFFFAOYSA-N [Na].FS(=N)F Chemical compound [Na].FS(=N)F XXYVTWLMBUGXOK-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 239000007789 gas Substances 0.000 abstract description 6
- 238000005406 washing Methods 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 239000002912 waste gas Substances 0.000 abstract 1
- 238000007789 sealing Methods 0.000 description 12
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- VCCATSJUUVERFU-UHFFFAOYSA-N sodium bis(fluorosulfonyl)azanide Chemical compound FS(=O)(=O)N([Na])S(F)(=O)=O VCCATSJUUVERFU-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- BFDWBSRJQZPEEB-UHFFFAOYSA-L sodium fluorophosphate Chemical compound [Na+].[Na+].[O-]P([O-])(F)=O BFDWBSRJQZPEEB-UHFFFAOYSA-L 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/70—Pre-treatment of the materials to be mixed
- B01F23/707—Extracting materials to be mixed from a stream of fluid or from a solid containing them, e.g. by adsorption, absorption or distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
- B01F33/821—Combinations of dissimilar mixers with consecutive receptacles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
-
- 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
The invention discloses a preparation method of sodium ion battery electrolyte, which comprises the following raw materials in parts by weight: 5-10 parts of sodium salt, 75-100 parts of solvent, 0.5-50 parts of flame retardant additive and 0.1-0.2 part of overcharge protective agent, wherein the sodium ion battery electrolyte is prepared by a mixing system, and the specific steps comprise solvent dehydration, sodium salt dissolution, additive premixing, final stirring, detection discharging and the like. According to the invention, various raw materials of the sodium ion battery electrolyte are mixed by the mixing kettle, the sodium salt, the flame retardant additive and the overcharge protective agent can be uniformly dissolved in the solvent, so that the stability of the electrolyte is improved, and the tail gas volatilized in the mixing preparation process is subjected to water washing and activated carbon adsorption treatment, so that the waste gas pollution is reduced.
Description
Technical Field
The invention belongs to the technical field of power batteries, and particularly relates to a preparation method of a sodium ion battery electrolyte.
Background
The modern society consumes more and more fossil fuel and has serious environmental pollution. New clean energy sources such as solar energy, tidal energy, wind energy, geothermal energy and the like are attracting more and more attention, but the energy sources need to be stored in batteries for better use. The lead-acid battery has the advantages of mature technology, low cost, low energy density, large environmental hazard, poor deep charge and discharge performance, short service life and the like, the lithium ion battery has high energy density, the organic electrolyte is inflammable and explosive, the safety problem exists, the lithium ion battery has higher cost, and the sodium ion battery is a candidate with very good application prospect in the field due to the factors of rich raw material sources, environmental friendliness, low price and the like.
Although the sodium ion battery has the potential advantage of low cost, the cycle life, the multiplying power performance and the like of the sodium ion battery still cannot meet the requirements of the current large-scale energy storage technology, and meanwhile, as electrolyte used by the sodium ion battery is a flammable carbonate and/or ether solvent system, under the conditions of overcharging, short circuit or heating and the like, the sodium ion battery can generate fire, combustion or explosion, so that safety accidents are caused. Therefore, additives such as flame retardant additives, overcharge protection agents, stabilizers and the like are generally added into the electrolyte of the sodium ion battery to improve the performance of the electrolyte, and the additives are required to be mixed with a solvent in the preparation process of the electrolyte, but the additives are difficult to be uniformly mixed with the electrolyte solvent due to high viscosity of many electrolyte solvents and solid powder and liquid in the additives, so that the performance stability of the electrolyte is poor in the subsequent use process.
Disclosure of Invention
In order to solve the defects in the background art, the invention aims to provide a preparation method of the sodium ion battery electrolyte, which comprises the steps of mixing various raw materials of the sodium ion battery electrolyte through a mixing kettle, uniformly dissolving sodium salt, a flame retardant additive and an overcharge protective agent in a solvent, connecting a spray tower and an adsorption tower for tail gas treatment to the mixing kettle, and washing and adsorbing active carbon by using the solvent such as carbonic acid with extremely low concentration in nitrogen naturally volatilized in the mixing preparation process.
The aim of the invention can be achieved by the following technical scheme:
the invention provides a preparation method of sodium ion battery electrolyte, which comprises the following raw materials in parts by weight: 5-10 parts of sodium salt, 75-100 parts of solvent, 0.5-50 parts of flame retardant additive and 0.1-0.2 part of overcharge protective agent;
the sodium ion battery electrolyte is prepared through a mixing system, and specifically comprises the following steps:
s1, feeding a raw material solvent to be dehydrated into a dehydration tower through a feed pump, dehydrating the raw material through a molecular sieve column in the dehydration tower, temporarily storing the dehydrated liquid raw material in a transit tank, conveying the liquid raw material in the transit tank to the dehydration tower through a reflux pump for dehydration, and circularly dehydrating until the water content of the raw material sample test is lower than 15mg/L, wherein the material conveying flow rate of the feed pump and the reflux pump is 2-4 m/h;
s2, a cooling pump is started, cooling water is circulated through a cooling jacket and a heat exchanger of the mixing kettle, the temperature of the mixing kettle is reduced to 4-6 ℃ through the cooling water, raw material solvent which does not need to be dehydrated is added into the mixing kettle from a storage tank by utilizing nitrogen pressure, the material transferring pressure is 0.2-0.3 MPa, meanwhile, solid raw materials are added into the mixing kettle through a powder feeding pipe, the feeding rate is 2-3 kg/min, stirring is started after the liquid level in the mixing kettle is higher than the bottom end of a return pipe, and the temperature of the mixing kettle is maintained to be 5+/-3 ℃ in the stirring process;
s3, stirring and mixing for 15-30 min, then conveying the dehydrated raw material solvent to a mixing kettle through a feeding pump, wherein the material conveying flow rate of the feeding pump is 2-4 m/h, simultaneously adding the flame retardant additive and the overcharge protective agent into the mixing kettle from a storage tank by utilizing nitrogen pressure, and rapidly mixing the flame retardant additive and the overcharge protective agent with the solvent through a premixing mechanism, wherein the feeding rate is 0.1-0.5 kg/min;
s4, continuously controlling the rotation of the stirring shaft to mix all the raw materials in the mixing kettle, opening a control valve at the air outlet of the mixing kettle in the mixing process, and treating partial solvent carried by naturally volatilized nitrogen through the spray tower and the adsorption tower;
s5, sampling and detecting, discharging electrolyte from a discharge hole at the bottom of the mixing kettle after the electrolyte is qualified, and pressing the electrolyte into a stainless steel packaging barrel through nitrogen after two-stage filtration of the first filter and the second filter.
Further preferably, the sodium salt is one of sodium hexafluorophosphate, sodium bis (trifluoromethylsulfonyl) imide, sodium perchlorate, sodium bis (fluorosulfonyl) imide.
Further preferably, the solvent is at least two or more of ethylene carbonate, propylene carbonate, diethyl carbonate, 1, 3-dioxolane, dimethyl carbonate, methylethyl carbonate, and dimethoxyethane.
Further preferably, the flame retardant additive is one of trimethyl phosphate, triethyl phosphate, triphenyl phosphate, methyl dimethyl phosphate, trimethyl phosphite, triethyl phosphite or triphenyl phosphite, and the overcharge protecting agent is cyclohexylbenzene or biphenyl.
Further preferably, in the stirring process of the steps S2-S4, the sliding seat is driven by the second motor to move upwards or downwards every 3-5 min, so that the driving disc is meshed with the first gear or the third gear respectively, the second driving shaft is driven to rotate in different directions, the stirring blades are further adjusted to rotate to different angles, and when the stirring blades rotate along with the stirring shaft, liquid in the mixing kettle can be driven to flow upwards or downwards.
Still preferably, the mixing system comprises a dehydration tower, the inside molecular sieve column that is equipped with of the dehydration tower, the discharge gate of dehydration tower links to each other with the feed inlet of transfer jar, the feed inlet of dehydration tower links to each other with the discharge end of feed pump and backwash pump respectively, the feed inlet of backwash pump links to each other with the backwash port of transfer jar, the discharge gate of transfer jar links to each other with the feed inlet of charge pump, the discharge end of charge pump links to each other with the first feed inlet of mixing kettle lateral wall, the second feed inlet at mixing kettle top links to each other with the discharge gate of storage tank, the coolant liquid inlet of mixing kettle links to each other with the discharge end of cooling pump, the feed inlet of cooling pump links to each other with the output of heat exchanger, the coolant liquid outlet of mixing kettle links to each other with the input of heat exchanger, the gas vent at mixing kettle top links to each other with the air inlet of spray tower, the gas outlet of spray tower links to each other with the air inlet of adsorption tower, the mixing kettle bottom is equipped with the discharge gate, the discharge gate of mixing kettle links to each other with the feed inlet of first filter, the discharge gate of first filter links to each other with the feed inlet of second filter.
Still preferably, the mixing kettle comprises a tank body, the lower side of the outer wall of the tank body is provided with a cooling jacket, a cooling water pipeline surrounding the tank body is arranged in the cooling jacket, a cooling liquid inlet and a cooling liquid outlet are formed in the surface of the cooling jacket, a sealing cover is arranged at the top of the mixing kettle and is fixed with the tank body through bolts, a driving box and a powder feeding pipe are fixedly installed at the top of the sealing cover, a driving mechanism is arranged in the driving box, a stirring shaft and a first driving shaft are arranged on the surface of the sealing cover in a penetrating manner and are in sealing and rotating connection with the sealing cover, the stirring shaft is a hollow shaft, a second driving shaft is arranged in the stirring shaft in a penetrating manner, stirring blades are symmetrically arranged on the outer wall of the lower end of the stirring shaft and are in rotating connection with the stirring shaft, the lower end of the second driving shaft is meshed with a rotating shaft of the stirring blades through bevel gears, the stirring shaft, the upper ends of the first driving shaft and the second driving shaft are connected with the driving mechanism, the lower end of the first driving shaft penetrates through the premixing mechanism, and the premixing mechanism is fixedly installed on the inner wall of the tank body.
Still preferably, the premixing mechanism comprises a vertically arranged backflow pipe, the lower end of the backflow pipe is open, a first driving shaft penetrates through the backflow pipe, a turbine is fixedly arranged on the surface of the first driving shaft inside the backflow pipe, a premixing pipe is sleeved on the outer wall of the upper end of the backflow pipe, the top of the premixing pipe is open, a backflow hole is formed in the side wall of the backflow pipe, corresponding to the bottom of the premixing pipe, a first feeding pipe penetrates through the middle of the side wall of the backflow pipe, the first feeding pipe is tangent to the inner wall of the backflow pipe, the outer wall of the premixing pipe is fixed with the inner wall of the tank body through a mounting frame, a drainage pipe is sleeved on the outer wall of the upper end of the premixing pipe, the pipe orifice of the upper end of the drainage pipe is higher than the premixing pipe, and a drainage port extending outwards in a radial direction is formed in one side, away from the inner wall of the tank body, of the drainage pipe;
the first drive shaft is the hollow shaft, and first drive shaft top fixed mounting rotary joint, rotary joint link to each other with the second inlet pipe, and the feed liquor hole has been seted up to first drive shaft lower extreme surface.
Further preferably, the driving mechanism comprises a vertically arranged mounting plate, a first gear shaft and a second gear shaft are arranged on the mounting plate in a penetrating mode, the first gear shaft and the second gear shaft are connected with the mounting plate in a rotating mode, the first gear and the second gear are fixedly installed at two ends of the first gear shaft respectively, a third gear and a fourth gear are fixedly installed at two ends of the second gear shaft respectively, the second gear and the fourth gear are meshed with an output shaft of the first motor, the lower side of the third gear is meshed with the stirring shaft, and the lower side of the fourth gear is meshed with the first driving shaft.
Still preferably, a driving disc is arranged between the first gear and the third gear, the driving disc is rotationally connected with a sliding seat, the sliding seat is fixedly connected with a sliding block, the sliding block is in threaded fit with a screw rod, the screw rod is vertically arranged inside a sliding rail in a penetrating mode, a screw rod driving box is rotationally connected with the top end of the screw rod and fixedly connected with an output shaft of a second motor, a driving hole is formed in the middle of the driving disc, the upper end of the second driving shaft penetrates through the driving hole, a bar key is fixedly mounted on the inner wall of the driving hole, a key groove is vertically formed in the surface of the second driving shaft, the bar key is matched with the key groove, and meshing teeth of one quarter of circumference are fixedly mounted on the upper surface and the lower surface of the driving disc.
The invention has the beneficial effects that:
according to the preparation method of the sodium ion battery electrolyte, a novel mixing system is adopted, the mixing system can be used for feeding different electrolyte solvents respectively, the solvents to be dehydrated are dehydrated through a molecular sieve column until the water content is less than 15mg/L, then the solvents are mixed with other materials, all the materials are mixed in a mixing kettle, and as salt raw materials are dissolved and are the heat emitted, the mixing kettle has a cooling function, the solvents can be kept at a certain temperature, the solvents are prevented from volatilizing due to temperature rise, and meanwhile, the mixing kettle is connected with a spray tower and an adsorption tower for tail gas treatment, and can be used for carrying out water washing and activated carbon adsorption treatment on the solvents with very low concentration carbonic acid and the like in nitrogen which are naturally volatilized in the mixing preparation process.
The premixing mechanism of the mixing kettle can not only pre-mix the raw materials newly added through the first feeding pipe and the second feeding pipe with the raw materials in the mixing kettle, but also continuously lift the raw materials at the lower layer in the mixing kettle to the upper layer, thereby improving the stirring effect. In addition, the driving mechanism of the mixing kettle drives the sliding seat to move up and down through the second motor, so that the driving disc is meshed with the first gear or the third gear, and as the surface of the driving disc is provided with meshing teeth with a quarter of circumference, the rotation angle of the driving disc is limited in a certain range, so that the second driving shaft can only rotate clockwise or anticlockwise by a certain angle, the rotating shaft of the stirring blade is meshed with the second driving shaft through the bevel gear, and therefore the stirring blade is switched between a left inclined angle and a right inclined angle.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of the overall structure of the mixing system of the present invention;
FIG. 2 is a schematic diagram of the overall structure of the mixing tank of the present invention;
FIG. 3 is a schematic cross-sectional structural view of the mixing tank of the present invention;
FIG. 4 is a schematic cross-sectional structural view of a mixing tank premixing mechanism of the present invention;
FIG. 5 is a schematic cross-sectional view of a mixing tank drive case of the present invention;
fig. 6 is an enlarged schematic view of the structure of the present invention at position a of fig. 5.
In the figure: 1-dehydration tower, 2-transfer tank, 3-storage tank, 4-mixing tank, 5-heat exchanger, 6-spray tower, 7-adsorption tower, 8-first filter, 9-second filter, 10-feed pump, 11-reflux pump, 12-feed pump, 13-cooling pump, 14-tank, 15-cooling jacket, 16-sealing cover, 17-driving box, 18-driving mechanism, 19-stirring shaft, 20-first driving shaft, 21-second driving shaft, 22-stirring blade, 23-premixing mechanism, 24-reflux pipe, 25-turbine, 26-premixing pipe, 27-reflux hole, 28-first feeding pipe, 29-mounting frame, 30-drainage port, 31-rotary joint, 32-second feeding pipe, 33-mounting plate, 34-first gear shaft, 35-second gear shaft, 36-first gear, 37-second gear, 38-third gear, 39-fourth gear, 40-powder feeding pipe, 41-first motor, 42-driving disk, 43-sliding seat, 44-sliding block, 45-screw rod, 46-sliding rail, 47-second motor, 48-driving hole, 49-bar key, 50-key groove, 51-meshing tooth, 52-drainage pipe, 53-liquid inlet.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the sodium ion battery electrolyte comprises the following raw materials in parts by weight: 5 parts of sodium fluorophosphate, 25 parts of ethylene carbonate, 25 parts of diethyl carbonate, 30 parts of dimethyl carbonate, 10 parts of trimethyl phosphate, 10 parts of triphenyl phosphate, 5 parts of trimethyl phosphite and 0.1 part of cyclohexylbenzene;
the sodium ion battery electrolyte is prepared through a mixing system and specifically comprises the following steps of:
s1, feeding a raw material solvent to be dehydrated into a dehydration tower 1 through a feed pump 10, dehydrating the raw material through a molecular sieve column in the dehydration tower 1, temporarily storing the dehydrated liquid raw material in a transfer tank 2, conveying the liquid raw material in the transfer tank 2 to the dehydration tower 1 again through a reflux pump 11 for dehydration, and circularly dehydrating until the water content of the raw material sample test is lower than 15mg/L, wherein the material conveying flow rate of the feed pump 10 and the reflux pump 11 is 2 m/h;
s2, a cooling pump 13 is opened, cooling water is circulated through a cooling jacket 15 and a heat exchanger 5 of the mixing kettle 4, the temperature of the mixing kettle 4 is reduced to 4 ℃ through the cooling water, raw material solvent which does not need to be dehydrated is added into the mixing kettle 4 from a storage tank 3 by utilizing nitrogen pressure, the material transferring pressure is 0.2MPa, meanwhile, solid raw materials are added into the mixing kettle 4 through a powder feed pipe 40, the feeding rate is 2kg/min, stirring is started after the liquid level in the mixing kettle 4 is higher than the bottom end of a return pipe 24, and the temperature of the mixing kettle 4 is maintained at 2 ℃ in the stirring process;
s3, stirring and mixing for 15min, then conveying the dehydrated raw material solvent to a mixing kettle 4 through a feeding pump 12, conveying the material with the flow rate of 2 m/h through the feeding pump 12, simultaneously adding the flame retardant additive and the overcharge protection agent into the mixing kettle 4 from a storage tank 3 by utilizing nitrogen pressure, and rapidly mixing the flame retardant additive and the overcharge protection agent with the solvent through a premixing mechanism 23, wherein the feeding rate is 0.1 kg/min;
s4, continuously controlling the stirring shaft 19 to rotate so as to mix the raw materials in the mixing kettle 4, opening a control valve at the air outlet of the mixing kettle 4 in the mixing process, and treating partial solvent carried by naturally volatilized nitrogen through the spray tower 6 and the adsorption tower 7;
s5, sampling and detecting, discharging electrolyte from a discharge hole at the bottom of the mixing kettle 4 after the electrolyte is detected to be qualified, and pressing the electrolyte into a stainless steel ladle barrel through nitrogen after the electrolyte is subjected to two-stage filtration of the first filter 8 and the second filter 9.
Example two
The preparation method of the sodium ion battery electrolyte comprises the following raw materials in parts by weight: 10 parts of sodium bis (trifluoromethylsulfonyl) imide, 40 parts of propylene carbonate, 40 parts of 1, 3-dioxolane, 15 parts of triethyl phosphate, 15 parts of dimethyl methylphosphonate, 15 parts of triethyl phosphite and 0.15 part of biphenyl;
the sodium ion battery electrolyte is prepared through a mixing system and specifically comprises the following steps of:
s1, feeding a raw material solvent to be dehydrated into a dehydration tower 1 through a feed pump 10, dehydrating the raw material through a molecular sieve column in the dehydration tower 1, temporarily storing the dehydrated liquid raw material in a transfer tank 2, conveying the liquid raw material in the transfer tank 2 to the dehydration tower 1 again through a reflux pump 11 for dehydration, and circularly dehydrating until the water content of the raw material sample test is lower than 15mg/L, wherein the material conveying flow rate of the feed pump 10 and the reflux pump 11 is 3 m/h;
s2, a cooling pump 13 is started, cooling water is circulated through a cooling jacket 15 and a heat exchanger 5 of the mixing kettle 4, the temperature of the mixing kettle 4 is reduced to 5 ℃ through the cooling water, raw material solvent which does not need to be dehydrated is added into the mixing kettle 4 from a storage tank 3 by utilizing nitrogen pressure, the material transferring pressure is 0.25MPa, meanwhile, solid raw materials are added into the mixing kettle 4 through a powder feed pipe 40, the feeding rate is 2.5kg/min, stirring is started after the liquid level in the mixing kettle 4 is higher than the bottom end of a return pipe 24, and the temperature of the mixing kettle 4 is maintained to 5 ℃ in the stirring process;
s3, stirring and mixing for 20min, then conveying the dehydrated raw material solvent to a mixing kettle 4 through a feeding pump 12, feeding the material with the feeding pump 12 at a material conveying flow rate of 3 m/h, simultaneously adding the flame retardant additive and the overcharge protection agent into the mixing kettle 4 from a storage tank 3 by utilizing nitrogen pressure, and rapidly mixing the flame retardant additive and the overcharge protection agent with the solvent through a premixing mechanism 23, wherein the feeding rate is 0.25 kg/min;
s4, continuously controlling the stirring shaft 19 to rotate so as to mix the raw materials in the mixing kettle 4, opening a control valve at the air outlet of the mixing kettle 4 in the mixing process, and treating partial solvent carried by naturally volatilized nitrogen through the spray tower 6 and the adsorption tower 7;
s5, sampling and detecting, discharging electrolyte from a discharge hole at the bottom of the mixing kettle 4 after the electrolyte is detected to be qualified, and pressing the electrolyte into a stainless steel ladle barrel through nitrogen after the electrolyte is subjected to two-stage filtration of the first filter 8 and the second filter 9.
Example III
The preparation method of the sodium ion battery electrolyte comprises the following raw materials in parts by weight: 8 parts of sodium bis (fluorosulfonyl) imide, 50 parts of methyl ethyl carbonate, 50 parts of dimethoxyethane, 0.5 part of triphenyl phosphate, 0.5 part of trimethyl phosphite, 1 part of triphenyl phosphite and 0.2 part of cyclohexylbenzene;
the sodium ion battery electrolyte is prepared through a mixing system and specifically comprises the following steps of:
s1, feeding a raw material solvent to be dehydrated into a dehydration tower 1 through a feed pump 10, dehydrating the raw material through a molecular sieve column in the dehydration tower 1, temporarily storing the dehydrated liquid raw material in a transfer tank 2, conveying the liquid raw material in the transfer tank 2 to the dehydration tower 1 again through a reflux pump 11 for dehydration, and circularly dehydrating until the water content of the raw material sample test is lower than 15mg/L, wherein the material conveying flow rate of the feed pump 10 and the reflux pump 11 is 4 m/h;
s2, a cooling pump 13 is opened, cooling water is circulated through a cooling jacket 15 and a heat exchanger 5 of the mixing kettle 4, the temperature of the mixing kettle 4 is reduced to 6 ℃ through the cooling water, raw material solvent which does not need to be dehydrated is added into the mixing kettle 4 from a storage tank 3 by utilizing nitrogen pressure, the material transferring pressure is 0.3MPa, meanwhile, solid raw materials are added into the mixing kettle 4 through a powder feed pipe 40, the feeding rate is 3kg/min, stirring is started after the liquid level in the mixing kettle 4 is higher than the bottom end of a return pipe 24, and the temperature of the mixing kettle 4 is maintained at 8 ℃ in the stirring process;
s3, stirring and mixing for 30min, then conveying the dehydrated raw material solvent to a mixing kettle 4 through a feeding pump 12, conveying the material with the material conveying flow of the feeding pump 12 for 4 m/h, simultaneously adding the flame retardant additive and the overcharge protection agent into the mixing kettle 4 from a storage tank 3 by utilizing nitrogen pressure, and rapidly mixing the flame retardant additive and the overcharge protection agent with the solvent through a premixing mechanism 23, wherein the feeding rate is 0.5 kg/min;
s4, continuously controlling the stirring shaft 19 to rotate so as to mix the raw materials in the mixing kettle 4, opening a control valve at the air outlet of the mixing kettle 4 in the mixing process, and treating partial solvent carried by naturally volatilized nitrogen through the spray tower 6 and the adsorption tower 7;
s5, sampling and detecting, discharging electrolyte from a discharge hole at the bottom of the mixing kettle 4 after the electrolyte is detected to be qualified, and pressing the electrolyte into a stainless steel ladle barrel through nitrogen after the electrolyte is subjected to two-stage filtration of the first filter 8 and the second filter 9.
In embodiments 1-3, the sliding seat 43 is driven to move up or down every 4min by the second motor 47 during stirring, so that the driving disc 42 is meshed with the first gear 36 or the third gear 38 respectively, thereby driving the second driving shaft 21 to rotate in different directions, further adjusting the stirring vane 22 to rotate to different angles, and when the stirring vane 22 rotates along with the stirring shaft 19, the liquid in the mixing kettle 4 can be driven to flow up or down.
The mixing system comprises a dehydration tower 1, wherein a molecular sieve column is arranged in the dehydration tower 1, a discharge port of the dehydration tower 1 is connected with a discharge port of a transfer tank 2, the discharge port of the dehydration tower 1 is respectively connected with discharge ports of a feed pump 10 and a return pump 11, the feed port of the return pump 11 is connected with a return port of the transfer tank 2, the discharge port of the transfer tank 2 is connected with a feed port of a feed pump 12, the discharge port of the feed pump 12 is connected with a first feed port of a side wall of a mixing kettle 4, a second feed port of the top of the mixing kettle 4 is connected with a discharge port of a storage tank 3, a cooling liquid inlet of the mixing kettle 4 is connected with a discharge port of a cooling pump 13, the feed port of the cooling pump 13 is connected with an output port of a heat exchanger 5, a cooling liquid outlet of the mixing kettle 4 is connected with an input port of the heat exchanger 5, an exhaust port of the top of the mixing kettle 4 is connected with an air inlet of a spray tower 6, the discharge port of the spray tower 6 is connected with an air inlet of an adsorption tower 7, the bottom of the mixing kettle 4 is provided with a discharge port, the discharge port of the mixing kettle 4 is connected with a feed port of a first filter 8, and a discharge port of the first filter 8 is connected with a second filter 9.
The mixing system can feed different electrolyte solvents respectively, the solvent to be dehydrated is dehydrated through a molecular sieve column until the moisture content is less than 15mg/L, then the dehydrated solvent is mixed with other materials, all materials are mixed in the mixing kettle 4, and as the heat emitted when the salt raw materials are dissolved, the mixing kettle 4 has a cooling function, so that the solvent can be kept at a certain temperature, the solvent volatilization caused by the temperature rise is prevented, meanwhile, the mixing kettle 4 is connected with the spray tower 6 and the adsorption tower 7 for tail gas treatment, and the water washing and the activated carbon adsorption treatment can be carried out on the solvent such as carbonic acid with extremely low concentration in nitrogen gas naturally volatilized in the mixing preparation process.
The mixing kettle 4 comprises a tank 144, a cooling jacket 15 is arranged on the lower side of the outer wall of the tank 144, a cooling water pipeline surrounding the tank 14 is arranged in the cooling jacket 15, a cooling liquid inlet and a cooling liquid outlet are formed in the surface of the cooling jacket 15, a sealing cover 16 is arranged at the top of the mixing kettle 4, the sealing cover 16 is fixed with the tank 144 through bolts, a driving box 17 and a powder feeding pipe 40 are fixedly arranged at the top of the sealing cover 16, a driving mechanism 18 is arranged in the driving box 17, a stirring shaft 19 and a first driving shaft 20 penetrate through the surface of the sealing cover 16, the stirring shaft 19 and the first driving shaft 20 are in sealing and rotating connection with the sealing cover 16, the stirring shaft 19 is a hollow shaft, a second driving shaft 21 penetrates through the inside of the stirring shaft 19, stirring blades 22 are symmetrically arranged on the outer wall of the lower end of the stirring shaft 19 and are in rotating connection with the stirring shaft 19, the lower end of the second driving shaft 21 is meshed with the rotating shaft of the stirring blades 22 through a bevel gear, the stirring shaft 19, the upper ends of the first driving shaft 20 and the second driving shaft 21 are connected with the driving mechanism 18, the lower end of the first driving shaft 20 penetrates through a premixing mechanism 23, and the premixing mechanism 23 is fixedly arranged on the inner wall of the tank 144.
The premixing mechanism 23 comprises a vertically arranged backflow pipe 24, the lower end of the backflow pipe 24 is open, a first driving shaft 20 penetrates through the backflow pipe 24, a turbine 25 is fixedly arranged on the surface of the first driving shaft 20 in the backflow pipe 24, a premixing pipe 26 is sleeved on the outer wall of the upper end of the backflow pipe 24, the top of the premixing pipe 26 is open, a backflow hole 27 is formed in the side wall of the backflow pipe 24, which corresponds to the bottom of the premixing pipe 26, a first feeding pipe 28 penetrates through the middle of the side wall of the backflow pipe 24, the first feeding pipe 28 is tangential to the inner wall of the backflow pipe 24, the outer wall of the premixing pipe 26 is fixed with the inner wall of the tank 14 through a mounting frame 29, a drainage pipe 52 is sleeved on the outer wall of the upper end of the premixing pipe 26, the pipe orifice of the upper end of the drainage pipe 52 is higher than the premixing pipe 26, and a drainage port 30 extending radially outwards is formed in one side of the drainage pipe 52, which is far away from the inner wall of the tank 14;
the first driving shaft 20 is a hollow shaft, the top end of the first driving shaft 20 is fixedly provided with a rotary joint 31, the rotary joint 31 is connected with the second feeding pipe 32, and the lower end surface of the first driving shaft 20 is provided with a liquid inlet 53.
The premixing mechanism 23 is respectively connected with the first feeding pipe 28 and the second feeding pipe 32, meanwhile, the premixing mechanism 23 continuously lifts the liquid raw material at the lower layer of the mixing kettle 4 into the premixing pipe 26 through the backflow pipe 24, the raw material entering the mixing kettle 4 from the second feeding pipe 32 enters the backflow pipe 24 through the liquid inlet 53 on the surface of the first driving shaft 20 and then is mixed with the liquid raw material at the backflow pipe 26, the raw material entering the mixing kettle 4 from the first feeding pipe 28 is tangential to the inner wall of the premixing pipe 26, the liquid inside the premixing pipe can be driven to flow in a ring shape, the raw material entering from the first feeding pipe 28 and the second feeding pipe 32 and the raw material at the backflow pipe 4 can be uniformly premixed, the premixed raw material overflows into the drainage pipe 52 and finally flows down through the drainage port 30, and falls on the upper layer of the raw material in the mixing kettle 4, so that the raw material newly added through the first feeding pipe 28 and the second feeding pipe 32 can be premixed with the raw material in the mixing kettle 4 through the premixing mechanism 24, the raw material at the lower layer of the mixing kettle 4 can be continuously lifted, and the stirring effect of the raw material at the upper layer can be improved.
The driving mechanism 18 comprises a vertically arranged mounting plate 33, a first gear shaft 34 and a second gear shaft 35 are arranged on the mounting plate 33 in a penetrating mode, the first gear shaft 34 and the second gear shaft 35 are connected with the mounting plate 33 in a rotating mode, a first gear 36 and a second gear 37 are fixedly installed at two ends of the first gear shaft 34 respectively, a third gear 38 and a fourth gear 39 are fixedly installed at two ends of the second gear shaft 35 respectively, the second gear 37 and the fourth gear 39 are meshed with an output shaft of the first motor 41, the lower side of the third gear 38 is meshed with the stirring shaft 19, and the lower side of the fourth gear 39 is meshed with the first driving shaft 20.
A driving disc 42 is arranged between the first gear 36 and the third gear 38, the driving disc 42 is rotationally connected with a sliding seat 43, the sliding seat 43 is fixedly connected with a sliding block 44, the sliding block 44 is in threaded fit with a screw rod 45, the screw rod 45 vertically penetrates through a sliding rail 46, a screw rod 45 driving box 17 is rotationally connected, the top end of the screw rod 45 is fixedly connected with an output shaft of a second motor 47, a driving hole 48 is formed in the middle of the driving disc 42, the upper end of a second driving shaft 21 penetrates through the driving hole 48, a bar key 49 is fixedly arranged on the inner wall of the driving hole 48, a key groove 50 is vertically formed in the surface of the second driving shaft 21, the bar key 49 is matched with the key groove 50, and a quarter-circumference meshing tooth 51 is fixedly arranged on the upper surface and the lower surface of the driving disc 42.
The driving mechanism 18 drives the stirring shaft 19 to drive the stirring blade 22 to rotate through the first motor 41, and drives the first driving shaft 20 to drive the turbine 25 to rotate, so that the raw materials at the lower layer of the mixing kettle 4 are lifted and returned through the return pipe 24. Meanwhile, the driving mechanism 18 drives the sliding seat 43 to move up and down through the second motor 47, so that the driving disc 42 is selectively meshed with the first gear 36 or the third gear 38, and as the surface of the driving disc 42 is provided with a quarter circumference meshing tooth 51, the rotation angle of the driving disc 42 is limited to a certain range, so that the second driving shaft 21 can only rotate clockwise or anticlockwise by a certain angle, and the rotating shaft of the stirring blade 22 is meshed with the second driving shaft 21 through a bevel gear, so that the stirring blade 22 is also switched between a left inclined angle and a right inclined angle, and when the stirring blade 22 rotates along with the stirring shaft 19, the two inclined angles just drive liquid in the mixing kettle 4 to flow upwards or downwards, thereby improving the stirring and mixing effects.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.
Claims (6)
1. The preparation method of the sodium ion battery electrolyte is characterized by comprising the following raw materials in parts by weight: 5-10 parts of sodium salt, 75-100 parts of solvent, 0.5-50 parts of flame retardant additive and 0.1-0.2 part of overcharge protective agent;
the sodium ion battery electrolyte is prepared through a mixing system and specifically comprises the following steps of:
s1, feeding a raw material solvent to be dehydrated into a dehydration tower (1) through a feed pump (10), dehydrating the raw material through a molecular sieve column in the dehydration tower (1), temporarily storing the dehydrated liquid raw material in a transfer tank (2), conveying the liquid raw material in the transfer tank (2) to the dehydration tower (1) for dehydration through a reflux pump (11), and circularly dehydrating until the water content of the raw material sample test is lower than 15mg/L, wherein the material conveying flow rate of the feed pump (10) and the reflux pump (11) is 2-4 m/h;
s2, a cooling pump (13) is opened, cooling water is circulated through a cooling jacket (15) and a heat exchanger (5) of the mixing kettle (4), the temperature of the mixing kettle (4) is reduced to 4-6 ℃ through the cooling water, raw material solvent which does not need to be dehydrated is added into the mixing kettle (4) from a storage tank (3) by utilizing nitrogen pressure, the material conversion pressure is 0.2-0.3 MPa, meanwhile, solid raw materials are added into the mixing kettle (4) through a powder feed pipe (40), the feeding rate is 2-3 kg/min, stirring is started after the liquid level in the mixing kettle (4) is higher than the bottom end of a return pipe (24), and the temperature of the mixing kettle (4) is maintained to be 5+/-3 ℃ in the stirring process;
s3, stirring and mixing for 15-30 min, then conveying the dehydrated raw material solvent to a mixing kettle (4) through a feeding pump (12), conveying the material with the feeding pump (12) at the material conveying flow rate of 2-4 m/h, simultaneously adding the flame retardant additive and the overcharge protective agent into the mixing kettle (4) from a storage tank (3) by utilizing nitrogen pressure, and rapidly mixing the flame retardant additive and the overcharge protective agent with the solvent through a premixing mechanism (23) at the feeding rate of 0.1-0.5 kg/min;
s4, continuously controlling the stirring shaft (19) to rotate so as to mix the raw materials in the mixing kettle (4), opening a control valve at the air outlet of the mixing kettle (4) in the mixing process, and treating partial solvent carried by naturally volatilized nitrogen through the spray tower (6) and the adsorption tower (7);
s5, sampling and detecting, discharging electrolyte from a discharge port at the bottom of the mixing kettle (4) after the electrolyte is qualified, and pressing the electrolyte into a stainless steel ladle barrel through nitrogen after the electrolyte is subjected to two-stage filtration of a first filter (8) and a second filter (9);
mixing kettle (4) including jar body (14), jar body (14) outer wall downside is equipped with cooling jacket (15), cooling jacket (15) inside is equipped with the cooling water piping who encircles jar body (14), cooling jacket (15) surface is equipped with coolant liquid inlet and coolant liquid outlet, mixing kettle (4) top is equipped with sealed lid (16), sealed lid (16) are fixed with jar body (14) through the bolt, sealed lid (16) top fixed mounting drive case (17) and powder inlet pipe (40), the inside actuating mechanism (18) that is equipped with of drive case (17), sealed lid (16) surface run through be equipped with (19) and first drive shaft (20), (19) and first drive shaft (20) all are connected with sealed lid (16) seal rotation, (19) are (19), the inside run through of (19) are equipped with second drive shaft (21), sealed lid (19) lower extreme outer wall symmetry is equipped with stirring leaf (22), stirring leaf (22) rotate (19) and stirring leaf (19) are connected with (21), stirring leaf (19) are connected through the pivot of second drive shaft (21), bevel gear (22) and stirring leaf (22) end meshing The upper ends of the first driving shaft (20) and the second driving shaft (21) are connected with the driving mechanism (18), the lower end of the first driving shaft (20) penetrates through the premixing mechanism (23), and the premixing mechanism (23) is fixedly arranged on the inner wall of the tank body (14);
the premixing mechanism (23) comprises a vertically arranged backflow pipe (24), the lower end of the backflow pipe (24) is open, the first driving shaft (20) penetrates through the backflow pipe (24), a turbine (25) is fixedly installed on the surface of the first driving shaft (20) inside the backflow pipe (24), a premixing pipe (26) is sleeved on the outer wall of the upper end of the backflow pipe (24), the top of the premixing pipe (26) is open, a backflow hole (27) is formed in the side wall of the backflow pipe (24) corresponding to the bottom of the premixing pipe (26), a first feeding pipe (28) penetrates through the middle of the side wall of the backflow pipe (24), the first feeding pipe (28) is tangent to the inner wall of the backflow pipe (24), the outer wall of the premixing pipe (26) is fixed with the inner wall of the tank body (14) through a mounting frame (29), a drainage pipe (52) is sleeved on the outer wall of the upper end of the premixing pipe (26), the pipe mouth of the upper end of the drainage pipe (52) is higher than the premixing pipe (26), and a drainage port (30) extending radially outwards is formed in one side, far away from the inner wall of the tank body (14);
the first driving shaft (20) is a hollow shaft, a rotary joint (31) is fixedly arranged at the top end of the first driving shaft (20), the rotary joint (31) is connected with a second feeding pipe (32), and a liquid inlet hole (53) is formed in the surface of the lower end of the first driving shaft (20);
the driving mechanism (18) comprises a vertically arranged mounting plate (33), a first gear shaft (34) and a second gear shaft (35) are arranged on the mounting plate (33) in a penetrating mode, the first gear shaft (34) and the second gear shaft (35) are both in rotary connection with the mounting plate (33), a first gear (36) and a second gear (37) are respectively and fixedly arranged at two ends of the first gear shaft (34), a third gear (38) and a fourth gear (39) are respectively and fixedly arranged at two ends of the second gear shaft (35), the second gear (37) and the fourth gear (39) are meshed with an output shaft of a first motor (41), the lower side of the third gear (38) is meshed with the stirring shaft (19), and the lower side of the fourth gear (39) is meshed with the first driving shaft (20);
be equipped with driving disk (42) between first gear (36) and third gear (38), driving disk (42) rotate with sliding seat (43) and be connected, sliding seat (43) and slider (44) fixed connection, slider (44) and lead screw (45) screw thread fit, lead screw (45) vertically run through and set up inside slide rail (46), lead screw (45) driving box (17) rotate and connect, driving hole (48) have been seted up in the middle of driving disk (42) with the output shaft fixed connection of second motor (47), driving hole (48) are run through to second drive shaft (21) upper end, bar key (49) are fixed mounting to driving hole (48) inner wall, bar key (50) have been seted up on second drive shaft (21) surface vertically, bar key (49) and key groove (50) cooperation, the meshing tooth (51) of the equal fixed mounting quarter circumference in upper and lower surface of driving disk (42).
2. The method for preparing a sodium ion battery electrolyte according to claim 1, wherein the sodium salt is one of sodium hexafluorophosphate, sodium bis (trifluoromethylsulfonyl) imide, sodium perchlorate and sodium difluorosulfimide.
3. The method for preparing a sodium ion battery electrolyte according to claim 1, wherein the solvent is at least two or more of ethylene carbonate, propylene carbonate, diethyl carbonate, 1, 3-dioxolane, dimethyl carbonate, methyl ethyl carbonate, and dimethoxyethane.
4. The method for preparing the electrolyte of the sodium ion battery according to claim 1, wherein the flame retardant additive is one of trimethyl phosphate, triethyl phosphate, triphenyl phosphate, dimethyl methylphosphonate, trimethyl phosphite, triethyl phosphite or triphenyl phosphite, and the overcharge protection agent is cyclohexylbenzene or biphenyl.
5. The method for preparing the sodium ion battery electrolyte according to claim 1, wherein in the stirring process of the steps S2 to S4, the second motor (47) drives the sliding seat (43) to move upwards or downwards every 3 to 5 minutes, so that the driving disc (42) is meshed with the first gear (36) or the third gear (38) respectively, thereby driving the second driving shaft (21) to rotate in different directions, further adjusting the stirring blade (22) to rotate to different angles, and when the stirring blade (22) rotates along with the stirring shaft (19), driving the liquid in the mixing kettle (4) to flow upwards or downwards.
6. The preparation method of the sodium ion battery electrolyte according to claim 1, wherein the mixing system comprises a dehydration tower (1), a molecular sieve column is arranged inside the dehydration tower (1), a discharge port of the dehydration tower (1) is connected with a discharge port of a transfer tank (2), a discharge port of the dehydration tower (1) is respectively connected with a discharge port of a feed pump (10) and a discharge port of a reflux pump (11), a discharge port of the reflux pump (11) is connected with a reflux port of the transfer tank (2), a discharge port of the transfer tank (2) is connected with a feed port of a feed pump (12), a discharge port of the feed pump (12) is connected with a first feed port of a side wall of a mixing kettle (4), a second feed port at the top of the mixing kettle (4) is connected with a discharge port of a storage tank (3), a cooling liquid inlet of the mixing kettle (4) is connected with a discharge port of a cooling pump (13), a feed port of the cooling pump (13) is connected with an output port of a heat exchanger (5), a discharge port of the mixing kettle (4) is connected with a discharge port of the mixing kettle (6) is connected with a discharge port of the spray tank (6), a discharge port of the mixing kettle (4) is connected with a discharge port of the spray tank (6), the discharge port of the mixing kettle (4) is connected with the feed inlet of the first filter (8), and the discharge port of the first filter (8) is connected with the feed inlet of the second filter (9).
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| CN115189031A (en) * | 2022-07-15 | 2022-10-14 | 洛阳大生新能源开发有限公司 | Lithium battery organic electrolyte production equipment |
| CN115282829A (en) * | 2022-08-17 | 2022-11-04 | 中交公路养护工程技术有限公司 | Biomass asphalt regenerant production and preparation device |
| CN217829870U (en) * | 2022-07-06 | 2022-11-18 | 广东铂索新材料科技有限公司 | Chemical stirring kettle capable of stirring more uniformly |
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2023
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| WO2018069331A1 (en) * | 2016-10-10 | 2018-04-19 | Ingeniatrics Tecnologías, S.L. | Apparatus and method of mixing at least two liquids |
| CN113937344A (en) * | 2021-10-14 | 2022-01-14 | 南京星梵电子科技有限公司 | Durable high-temperature wave electrolyte and preparation device and method thereof |
| CN217114502U (en) * | 2021-12-14 | 2022-08-02 | 成都宏焘新材料有限公司 | Lithium battery electrolyte processing production line |
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| CN114984829A (en) * | 2022-05-26 | 2022-09-02 | 四川有你一面食品有限公司 | Full-automatic brine preparation device and brine mixing method thereof |
| CN217829870U (en) * | 2022-07-06 | 2022-11-18 | 广东铂索新材料科技有限公司 | Chemical stirring kettle capable of stirring more uniformly |
| CN115189031A (en) * | 2022-07-15 | 2022-10-14 | 洛阳大生新能源开发有限公司 | Lithium battery organic electrolyte production equipment |
| CN114989899A (en) * | 2022-07-18 | 2022-09-02 | 安徽亿人安股份有限公司 | Medical alkaline multienzyme cleaning agent and application thereof |
| CN115282829A (en) * | 2022-08-17 | 2022-11-04 | 中交公路养护工程技术有限公司 | Biomass asphalt regenerant production and preparation device |
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| CN116598589A (en) | 2023-08-15 |
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