CN113937344A - Durable high-temperature wave electrolyte and preparation device and method thereof - Google Patents
Durable high-temperature wave electrolyte and preparation device and method thereof Download PDFInfo
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Abstract
The invention relates to a durable high-temperature wave electrolyte, a preparation device and a preparation method thereof, wherein the durable high-temperature wave electrolyte comprises the following components in parts by weight: 4.1-8.2% of graphene dispersion liquid, 3.6-10.5% of salt additive, 8.1-11.4% of high-temperature resistant additive, 0.5-2.1% of functional additive, 0.1-2.8% of activating agent, 1.5-3.1% of stabilizing agent, 1.2-2.8% of inorganic acid, 0-1.3% of potassium permanganate and the balance of non-aqueous solvent. On one hand, the production efficiency of the electrolyte and the stability and reliability of the quality of the electrolyte product are effectively improved, and meanwhile, the high-temperature resistance of the electrolyte is effectively improved and the production cost is reduced; on the other hand, the defect that oxidative deterioration occurs between the raw materials and oxygen in the production of the electrolyte is effectively overcome, and the efficiency and the quality of mixing among the components in the mixing operation of the electrolyte are improved, so that the molecular acting force among the components of the electrolyte is improved, and the comprehensive performance and the quality of the electrolyte product are improved.
Description
Technical Field
The invention relates to a durable high-temperature wave electrolyte and a preparation device and method thereof, belonging to the technical field of energy materials and chemical engineering.
Background
The electrolyte is one of the main materials of various power battery equipment such as lithium batteries, lead-acid batteries and the like at present, plays an important role in the charge and discharge performance of the batteries, the energy storage performance of the batteries, the high temperature resistance performance and the anti-explosion performance of the battery equipment during operation, but in the actual production and configuration of the electrolyte, on one hand, the raw material components for configuring the electrolyte are often various and the contents of heavy metal ions and toxic and harmful organic matters are often high, so that the raw material cost for producing and preparing the electrolyte product is high, the production difficulty is high, meanwhile, a large amount of cost consumed by produced tail gas, waste liquid and the like is subjected to harmless treatment in the electrolyte production, and the production cost of the electrolyte is further increased; on the other hand, the high temperature resistance of the traditional electrolyte and the molecular acting force among the components of the electrolyte are relatively weak, so that the quality of the electrolyte product is caused, and the high temperature resistance, the large current impact resistance and the overload resistance are relatively poor in use; in addition, the traditional electrolyte formula liquid can only meet the matched use requirement of a specific type of battery product, and has poor universality, so that great negative effects are caused on the flexibility and the universality of the electrolyte.
Therefore, in order to solve the problem, it is urgently needed to develop a durable high-temperature wave electrolyte and a preparation method thereof so as to meet the requirement of practical use.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the durable high-temperature wave electrolyte, and the preparation device and the preparation method thereof, so that the high-temperature resistance of the electrolyte is effectively improved, the production cost is reduced, the production process is simplified, the production cost is effectively reduced, the defect that the raw materials and oxygen are oxidized and deteriorated in the production of the electrolyte is effectively overcome, and the comprehensive performance and the quality of the electrolyte product are improved.
The durable high-temperature wave electrolyte comprises the following components in parts by weight: 4.1-8.2% of graphene dispersion liquid, 3.6-10.5% of salt additive, 8.1-11.4% of high-temperature resistant additive, 0.5-2.1% of functional additive, 0.1-2.8% of activating agent, 1.5-3.1% of stabilizing agent, 1.2-2.8% of inorganic acid, 0-1.3% of potassium permanganate and the balance of non-aqueous solvent.
Further, the graphene dispersion liquid is oily, wherein the particle size is 1-10 mu m, the thickness is 0.8-1.0nm, the number of layers is less than or equal to 3, and the purity is not less than 99%.
Further, the salt additive is any one of a lithium salt and a sodium salt, wherein the lithium salt comprises any one of lithium hexafluorophosphate, lithium bis (oxalato) borate and lithium bis (fluorooxalato) borate; the sodium salt is at least one of sodium hexafluorophosphate, sodium chloride, sodium fluoride, sodium sulfate, sodium carbonate, sodium phosphate, sodium nitrate, sodium difluorooxalate, sodium pyrophosphate, sodium dodecylbenzene sulfonate, sodium dodecyl sulfate, trisodium citrate, sodium metaborate, sodium borate, sodium molybdate, sodium tungstate, sodium bromide, sodium nitrite, sodium iodate, sodium iodide, sodium silicate, sodium lignosulfonate, sodium oxalate, sodium aluminate, sodium methanesulfonate, sodium acetate, sodium dichromate, sodium hexafluoroarsenate, sodium tetrafluoroborate, sodium perchlorate and sodium trifluoromethanesulfonimide.
Further, the high-temperature resistant additive is tetra-n-propyl zirconate; the functional additive is biphenyl, vinylene carbonate, fluoroethylene carbonate, sultone, ethylene sulfite, fluorosulfonate and acid anhydride; activators include, but are not limited to, sodium dodecylbenzene sulfonate; the stabilizer is one or more of phosphate and active pyrophosphate which are mixed in any proportion; the inorganic acid is any one of hydrochloric acid, sulfuric acid and phosphoric acid.
Further, the non-aqueous solvent is any one of ethylene carbonate, dimethyl carbonate, ethyl butyrate, methyl butyrate, dioxolane, tetrafuran and ethyl acetate.
The invention also provides a preparation device of the durable high-temperature wave electrolyte, which comprises a bearing frame, a lifting driving mechanism, a reaction kettle, a sealing cover, a vacuum pump, a booster pump, an ultrasonic oscillation mechanism, an electromagnetic heating mechanism, an irradiation heating mechanism, a bracket, a bearing column, an air pressure sensor, an oxygen concentration sensor and a driving circuit, wherein the bearing frame is of a columnar frame structure with the axis vertical to the horizontal plane, the reaction kettle is embedded in the bearing frame, is coaxially distributed with the bearing frame and is in sliding connection with the bearing frame through at least two lifting driving mechanisms, the upper end surface of the reaction kettle is connected with the sealing cover to form a closed cavity structure, an exhaust port, an air inlet and a charging port are arranged on the upper end surface of the side wall of the reaction kettle, the exhaust port and the air inlet are symmetrically distributed on two sides of the axis of the reaction kettle, the feeding port is positioned between the exhaust port and the air inlet, the exhaust port, the air inlet and the feeding port are all provided with a control valve, the exhaust port and the air inlet are respectively communicated with the vacuum pump and the booster pump through the control valve, the bracket is embedded in the reaction kettle and coaxially distributed with the reaction kettle, the bracket is of a star-shaped frame structure, the diameter of the bracket is 20% -60% of the inner diameter of the reaction kettle, the upper end face of the bracket is connected with the bearing column and coaxially distributed with the bearing column, the bearing column is connected with the sealing cover through a lifting driving mechanism and coaxially distributed with the reaction kettle, the distance between the bracket and the upper end face of the reaction kettle is 5% -95% of the depth of the reaction kettle, the number of the ultrasonic oscillation mechanisms is at least three, the ultrasonic oscillation mechanisms are uniformly distributed around the axis of the reaction kettle and connected with the lower end face of the bracket, the electromagnetic heating mechanisms are at least two, uniformly distributed around the axis of the reaction kettle and embedded in the bottom of the reaction kettle, and electromagnetic heating mechanism total area is 5% -10% of reation kettle bottom area, irradiation heating mechanism is three at least, inlays in sealed lid lower extreme face and irradiation heating mechanism axis and reation kettle axis intersect and be 10-60 contained angles, baroceptor, oxygen concentration sensor are all one to inlay terminal surface under the sealed lid, vacuum pump, booster pump, drive circuit and bear frame surface connection, and drive circuit in addition respectively with vacuum pump, booster pump, ultrasonic oscillation mechanism, electromagnetic heating mechanism, irradiation heating mechanism, baroceptor, oxygen concentration sensor and control valve electrical connection.
Further, the bracket include base, guide bar, the base is the arbitrary platelike frame structure of circular and regular polygon, the base side surface is connected with three at least guide bars, just guide bar and bearing post vertical distribution, the guide bar is hollow column structure, and all establishes 1-4 ultrasonic oscillation mechanism in every guide bar, and each ultrasonic oscillation mechanism each other parallel and along the guide bar axis direction equipartition.
The invention also aims to provide a preparation method for preparing the durable high-temperature wave electrolyte by using the preparation equipment, which comprises the following steps:
s1, presetting electrolyte, namely firstly adding a non-aqueous solvent into a reaction kettle, replacing air in the reaction kettle with inert gas, increasing the air pressure in the reaction kettle to 1.5-2.3 times of the standard atmospheric pressure, then sealing the reaction kettle, raising the temperature of the reaction kettle to 60-90 ℃ at a constant speed, and preserving heat and pressure for 10-20 minutes;
s2, preparing electrolyte, after the step S1 is completed, determining the type of a salt additive, premixing the selected salt additive with graphene dispersion liquid, the salt additive, a high-temperature-resistant additive, a functional additive, an activator, a stabilizer, inorganic acid and potassium permanganate, adding the premix into a non-aqueous solvent in a reaction kettle at a constant speed within 3-10 minutes after premixing, ultrasonically homogenizing the mixed solution for 30-60 minutes, simultaneously reducing the temperature of the mixture in the reaction kettle to 50-60 ℃ at a constant speed within the first 5-10 minutes of ultrasonic homogenization, carrying out heat preservation and pressure maintaining homogenization for 20-30 minutes, reducing the temperature to 35-40 ℃ at a constant speed within the last 10-15 minutes, and standing for 10-30 minutes after ultrasonic homogenization is stopped to obtain the finished electrolyte.
Further, in the step S2, when the salt additive is selected, the concentration of the sodium salt raw material is 1-2.5 times of the lithium salt.
According to the invention, through optimizing the raw materials in the electrolyte, the production efficiency of the electrolyte and the stability and reliability of the quality of the electrolyte product are effectively improved, the high-temperature resistance of the electrolyte is effectively improved, the production cost is reduced, and meanwhile, the requirements of the matched use of a lead-acid battery, a lithium battery and a sodium battery can be flexibly met according to the use requirements; on the other hand, the electrolyte production equipment is integrated in the unified bearing rack, the efficiency of electrolyte production operation is effectively improved, the production process is simplified, the production cost is effectively reduced, in production, in addition, the defect of oxidative deterioration between the raw materials and oxygen in the electrolyte production is effectively overcome through a low-oxygen high-pressure environment formed by inert gas in the reaction kettle, in addition, the efficiency and the quality of mixing among the components in the electrolyte mixing operation are improved through the high-pressure environment, the reaction efficiency among the raw material components is improved, the molecular acting force among the electrolyte components is improved, and the comprehensive performance and the quality of an electrolyte product are improved.
Drawings
The invention is described in detail below with reference to the drawings and the detailed description;
FIG. 1 is a schematic flow diagram of the process of the present invention;
FIG. 2 is a schematic view of a manufacturing apparatus;
reference numbers in the figures: 1. a bearing frame; 2. a lifting drive mechanism; 3. a reaction kettle; 31. an exhaust port; 32. an air inlet; 33. a feed inlet; 4. a sealing cover; 5. a vacuum pump; 6. a booster pump; 7. an ultrasonic oscillation mechanism; 8. an electromagnetic heating mechanism; 9. an irradiation heating mechanism; 10. a bracket; 101. a base; 102. a guide bar; 11. a load bearing column; 12. an air pressure sensor; 13. an oxygen concentration sensor; 14. a drive circuit.
Detailed Description
In order to facilitate the implementation of the technical means, creation features, achievement of the purpose and the efficacy of the invention, the invention is further described below with reference to specific embodiments.
Example 1
As shown in figure 1, the durable high-temperature wave electrolyte comprises the following components in parts by weight: 4.1% of graphene dispersion liquid, 3.6% of salt additive, 8.1% of high-temperature-resistant additive, 0.5% of functional additive, 0.1% of activating agent, 1.5% of stabilizing agent, 1.2% of inorganic acid and the balance of non-aqueous solvent.
In this embodiment, the graphene dispersion is oily, wherein the particle size is 1 μm, the thickness is 0.8nm, the number of layers is not more than 3, and the purity is not less than 99%.
Wherein the salt additive is lithium hexafluorophosphate.
Meanwhile, the high-temperature resistant additive is tetra-n-propyl zirconate; the functional additive is biphenyl; activators include, but are not limited to, sodium dodecylbenzene sulfonate; the stabilizer is phosphate; the inorganic acid is hydrochloric acid.
In this embodiment, the nonaqueous solvent is ethylene carbonate.
A preparation method of durable high-temperature wave electrolyte comprises the following steps:
s1, presetting electrolyte, namely firstly adding a non-aqueous solvent into a reaction kettle 3, replacing air in the reaction kettle 3 with inert gas, increasing the air pressure in the reaction kettle 3 to 1.5 times of the standard atmospheric pressure, then sealing the reaction kettle 3, raising the temperature of the reaction kettle 3 to 60 ℃ at a constant speed, and preserving the temperature and the pressure for 10 minutes;
s2, preparing electrolyte, after the step S1 is completed, determining the type of a salt additive, premixing the selected salt additive with the graphene dispersion liquid, the salt additive, the high-temperature-resistant additive, the functional additive, the activator, the stabilizer, the inorganic acid and the potassium permanganate, adding the premix into the non-aqueous solvent in the reaction kettle 3 at a constant speed within 3 minutes after premixing, ultrasonically homogenizing the mixed solution for 30 minutes, simultaneously reducing the temperature of the mixture in the reaction kettle 3 to 50 ℃ at a constant speed within the first 5 minutes of ultrasonic homogenization, preserving heat, maintaining pressure, homogenizing for 20 minutes, reducing the temperature to 35 ℃ at a constant speed within the last 10 minutes, stopping ultrasonic homogenization, preserving pressure, and standing for 10 minutes to obtain the finished electrolyte.
Example 2
As shown in figure 1, the durable high-temperature wave electrolyte comprises the following components in parts by weight: 8.2% of graphene dispersion liquid, 10.5% of salt additive, 11.4% of high-temperature-resistant additive, 2.1% of functional additive, 2.8% of activating agent, 3.1% of stabilizing agent, 2.8% of inorganic acid, 3% of potassium permanganate and the balance of non-aqueous solvent.
In this embodiment, the graphene dispersion is oily, wherein the particle size is 10 μm, the thickness is 1.0nm, the number of layers is less than or equal to 3, and the purity is not less than 99%.
Meanwhile, the salt additive is any one of lithium salt and sodium salt, wherein the lithium salt comprises any one of lithium hexafluorophosphate, lithium bis (oxalato) borate and lithium bis (oxalato) borate; the sodium salt is sodium difluorooxalate sodium borate.
In the embodiment, the high-temperature resistant additive is tetra-n-propyl zirconate; the functional additive is vinylene carbonate; activators include, but are not limited to, sodium dodecylbenzene sulfonate; the stabilizer is active pyrophosphate; the inorganic acid is sulfuric acid.
In this embodiment, the non-aqueous solvent is ethyl butyrate.
A preparation method of durable high-temperature wave electrolyte comprises the following steps:
s1, presetting electrolyte, namely firstly adding a non-aqueous solvent into a reaction kettle 3, replacing air in the reaction kettle 3 with inert gas, increasing the air pressure in the reaction kettle 3 to 2.3 times of the standard atmospheric pressure, then sealing the reaction kettle 3, raising the temperature of the reaction kettle 3 to 90 ℃ at a constant speed, and preserving the temperature and the pressure for 20 minutes;
s2, preparing electrolyte, after the step S1 is completed, determining the type of a salt additive, premixing the selected salt additive with the graphene dispersion liquid, the salt additive, the high-temperature-resistant additive, the functional additive, the activator, the stabilizer, the inorganic acid and the potassium permanganate, adding the premix into the non-aqueous solvent in the reaction kettle 3 at a constant speed within 10 minutes after premixing, ultrasonically homogenizing the mixed solution for 60 minutes, simultaneously reducing the temperature of the mixture in the reaction kettle 3 to 60 ℃ at a constant speed within the first 10 minutes of ultrasonic homogenization, preserving heat, maintaining pressure and homogenizing for 30 minutes, reducing the temperature to 40 ℃ at a constant speed within the last 15 minutes, stopping ultrasonic homogenization, preserving pressure and standing for 30 minutes to obtain the finished electrolyte.
Example 3
As shown in figure 1, the durable high-temperature wave electrolyte comprises the following components in parts by weight: 6.2% of graphene dispersion liquid, 7.5% of salt additive, 9.3% of high-temperature-resistant additive, 1.1% of functional additive, 0.8% of activating agent, 2.1% of stabilizing agent, 1.8% of inorganic acid, 0.3% of potassium permanganate and the balance of non-aqueous solvent.
In this embodiment, the graphene dispersion is oily, wherein the particle size is 5 μm, the thickness is 0.9nm, the number of layers is not more than 3, and the purity is not less than 99%.
In this embodiment, the salt additive is lithium bis (fluorooxalato) borate; sodium salt sodium trifluoromethanesulfonylimide.
Meanwhile, the high-temperature resistant additive is tetra-n-propyl zirconate; the functional additive is sultone; activators include, but are not limited to, sodium dodecylbenzene sulfonate; the stabilizer is phosphate, active pyrophosphate 1: 1, mixing in proportion; the inorganic acid is phosphoric acid.
In addition, the non-aqueous solvent is tetra-strong furan.
A preparation method of durable high-temperature wave electrolyte comprises the following steps:
s1, presetting electrolyte, namely firstly adding a non-aqueous solvent into a reaction kettle 3, replacing air in the reaction kettle 3 with inert gas, increasing the air pressure in the reaction kettle 3 to 1.8 times of the standard atmospheric pressure, then sealing the reaction kettle 3, raising the temperature of the reaction kettle 3 to 70 ℃ at a constant speed, and preserving the temperature and the pressure for 15 minutes;
s2, preparing electrolyte, after the step S1 is completed, determining the type of a salt additive, premixing the selected salt additive with the graphene dispersion liquid, the salt additive, the high-temperature-resistant additive, the functional additive, the activator, the stabilizer, the inorganic acid and the potassium permanganate, adding the premix into the non-aqueous solvent in the reaction kettle 3 at a constant speed within 7 minutes after premixing, ultrasonically homogenizing the mixed solution for 45 minutes, simultaneously reducing the temperature of the mixture in the reaction kettle 3 to 55 ℃ at a constant speed within the first 6 minutes of ultrasonic homogenization, carrying out heat preservation, pressure maintaining and homogenization for 25 minutes, reducing the temperature to 38 ℃ at a constant speed within the last 12 minutes, stopping ultrasonic homogenization, carrying out pressure maintaining and homogenization for 20 minutes, and obtaining the finished electrolyte.
Example 4
As shown in figure 1, the durable high-temperature wave electrolyte comprises the following components in parts by weight: 7.2% of graphene dispersion liquid, 4.5% of salt additive, 10.1% of high-temperature-resistant additive, 1.5% of functional additive, 1.5% of activating agent, 2.1% of stabilizing agent, 2.1% of inorganic acid, 1.1% of potassium permanganate and the balance of non-aqueous solvent.
The graphene dispersion liquid is oily, the particle size is 9 micrometers, the thickness is 0.9nm, the number of layers is less than or equal to 3, and the purity is not less than 99%.
Meanwhile, the salt additive is trisodium citrate.
In the embodiment, the high-temperature resistant additive is tetra-n-propyl zirconate; the functional additive is anhydride; activators include, but are not limited to, sodium dodecylbenzene sulfonate; the stabilizer is phosphate and active pyrophosphate which are mixed in any proportion; the inorganic acid is hydrochloric acid.
In addition, the non-aqueous solvent is methyl butyrate.
A preparation method of durable high-temperature wave electrolyte comprises the following steps:
s1, presetting electrolyte, namely firstly adding a non-aqueous solvent into a reaction kettle 3, replacing air in the reaction kettle 3 with inert gas, increasing the air pressure in the reaction kettle 3 to 1.7 times of the standard atmospheric pressure, then sealing the reaction kettle 3, raising the temperature of the reaction kettle 3 to 85 ℃ at a constant speed, and preserving the temperature and the pressure for 16 minutes;
s2, preparing electrolyte, after the step S1 is completed, determining the type of a salt additive, premixing the selected salt additive with the graphene dispersion liquid, the salt additive, the high-temperature-resistant additive, the functional additive, the activator, the stabilizer, the inorganic acid and the potassium permanganate, adding the premix into the non-aqueous solvent in the reaction kettle 3 at a constant speed within 9 minutes after premixing, ultrasonically homogenizing the mixed solution for 40 minutes, simultaneously reducing the temperature of the mixture in the reaction kettle 3 to 50 ℃ at a constant speed within the first 7 minutes of ultrasonic homogenization, preserving heat, maintaining pressure, homogenizing for 30 minutes, reducing the temperature to 40 ℃ at a constant speed within the last 10 minutes, maintaining pressure and standing for 10 minutes after the ultrasonic homogenization is stopped, and obtaining the finished electrolyte.
Example 5
As shown in figure 1, the durable high-temperature wave electrolyte comprises the following components in parts by weight: 4.1-8.2% of graphene dispersion liquid, 3.6-10.5% of salt additive, 8.1-11.4% of high-temperature resistant additive, 0.5-2.1% of functional additive, 0.1-2.8% of activating agent, 1.5-3.1% of stabilizing agent, 1.2-2.8% of inorganic acid, 0-1.3% of potassium permanganate and the balance of non-aqueous solvent.
The graphene dispersion liquid is oily, the particle size is 1-10 mu m, the thickness is 0.8-1.0nm, the number of layers is less than or equal to 3, and the purity is not less than 99%.
The salt additive is any one of a lithium salt and a sodium salt, wherein the lithium salt includes any one of lithium hexafluorophosphate, lithium bis (oxalato) borate and lithium bis (oxalato) borate; the sodium salt is at least one of sodium hexafluorophosphate, sodium chloride, sodium fluoride, sodium sulfate, sodium carbonate, sodium phosphate, sodium nitrate, sodium difluorooxalate, sodium pyrophosphate, sodium dodecylbenzene sulfonate, sodium dodecyl sulfate, trisodium citrate, sodium metaborate, sodium borate, sodium molybdate, sodium tungstate, sodium bromide, sodium nitrite, sodium iodate, sodium iodide, sodium silicate, sodium lignosulfonate, sodium oxalate, sodium aluminate, sodium methanesulfonate, sodium acetate, sodium dichromate, sodium hexafluoroarsenate, sodium tetrafluoroborate, sodium perchlorate and sodium trifluoromethanesulfonimide.
In addition, the high-temperature resistant additive is tetra-n-propyl zirconate; the functional additive is biphenyl, vinylene carbonate, fluoroethylene carbonate, sultone, ethylene sulfite, fluorosulfonate and acid anhydride; activators include, but are not limited to, sodium dodecylbenzene sulfonate; the stabilizer is one or more of phosphate and active pyrophosphate which are mixed in any proportion; the inorganic acid is any one of hydrochloric acid, sulfuric acid and phosphoric acid.
In this embodiment, the nonaqueous solvent is any one of ethylene carbonate, dimethyl carbonate, ethyl butyrate, methyl butyrate, dioxolane, tetrafuran, and ethyl acetate.
A preparation method of durable high-temperature wave electrolyte comprises the following steps:
s1, presetting electrolyte, namely firstly adding a non-aqueous solvent into a reaction kettle 3, replacing air in the reaction kettle 3 with inert gas, increasing the air pressure in the reaction kettle 3 to 2.2 times of the standard atmospheric pressure, then sealing the reaction kettle 3, raising the temperature of the reaction kettle 3 to 80 ℃ at a constant speed, and preserving the temperature and the pressure for 15 minutes;
s2, preparing electrolyte, after the step S1 is completed, determining the type of a salt additive, premixing the selected salt additive with the graphene dispersion liquid, the salt additive, the high-temperature-resistant additive, the functional additive, the activator, the stabilizer, the inorganic acid and the potassium permanganate, adding the premix into the non-aqueous solvent in the reaction kettle 3 at a constant speed within 5 minutes after premixing, ultrasonically homogenizing the mixed solution for 40 minutes, simultaneously reducing the temperature of the mixture in the reaction kettle 3 to 55 ℃ at a constant speed within the first 5 minutes of ultrasonic homogenization, preserving heat, maintaining pressure and homogenizing for 22 minutes, reducing the temperature to 37 ℃ at a constant speed within the last 14 minutes, maintaining pressure and homogenizing for 18 minutes after ultrasonic homogenization is stopped, and obtaining the finished electrolyte.
In this embodiment, in the step S2, when the salt additive is selected, the concentration of the sodium salt raw material is 1-2.5 times of the lithium salt.
In the specific implementation of the invention, as shown in fig. 2, a device for preparing durable high-temperature wave electrolyte comprises a bearing rack 1, a lifting driving mechanism 2, a reaction kettle 3, a sealing cover 4, a vacuum pump 5, a booster pump 6, an ultrasonic oscillation mechanism 7, an electromagnetic heating mechanism 8, an irradiation heating mechanism 9, a bracket 10, a bearing column 11, an air pressure sensor 12, an oxygen concentration sensor 13 and a driving circuit 14, wherein the bearing rack 1 is a columnar frame structure with an axis vertical to a horizontal plane, the reaction kettle 3 is embedded in the bearing rack 1, is coaxially distributed with the bearing rack 1 and is slidably connected with the bearing rack 1 through at least two lifting driving mechanisms 2, the upper end face of the reaction kettle 3 is connected with the sealing cover 4 to form a closed cavity structure, an exhaust port 31, an air inlet 32 and a charging port 33 are arranged on the upper end face of the side wall of the reaction kettle 3, wherein the exhaust port 31 and the air inlet 32 are symmetrically distributed on two sides of the axis of the reaction kettle 3, the feed inlet 33 is positioned between the exhaust port 31 and the air inlet 32, the exhaust port 31, the air inlet 32 and the feed inlet 33 are all provided with a control valve 15, the exhaust port 31 and the air inlet 32 are respectively communicated with the vacuum pump 5 and the booster pump 6 through the control valve 15, the bracket 10 is embedded in the reaction kettle 3 and coaxially distributed with the reaction kettle 3, the bracket 10 is of a star-shaped frame structure, the diameter of the bracket 10 is 20% -60% of the inner diameter of the reaction kettle 3, the upper end face of the bracket 10 is connected with the bearing column 11 and coaxially distributed with the bearing column 11, the bearing column 11 is additionally connected with the sealing cover 4 through the lifting driving mechanism 2 and coaxially distributed with the reaction kettle 3, the distance between the bracket 10 and the upper end face of the reaction kettle 3 is 5% -95% of the depth of the reaction kettle 3, and the ultrasonic oscillation mechanisms 7 are at least three, are uniformly distributed around the axis of the reaction kettle 3 and are connected with the lower end surface of the bracket 10, at least two electromagnetic heating mechanisms 8 are uniformly distributed around the axis of the reaction kettle 3 and are embedded at the bottom of the reaction kettle 3, the total area of the electromagnetic heating mechanisms 8 is 5-10% of the bottom area of the reaction kettle 3, at least three irradiation heating mechanisms 9 are embedded in the lower end face of the sealing cover 4, the axial line of the irradiation heating mechanism 9 is intersected with the axial line of the reaction kettle 3 and forms an included angle of 10-60 degrees, the pressure sensor 12 and the oxygen concentration sensor 13 are both one, and is embedded on the lower end surface of the sealing cover 4, the vacuum pump 5, the booster pump 6 and the drive circuit 14 are connected with the outer surface of the bearing frame 1, and the driving circuit 14 is respectively and electrically connected with the vacuum pump 5, the booster pump 6, the ultrasonic oscillation mechanism 7, the electromagnetic heating mechanism 8, the irradiation heating mechanism 9, the air pressure sensor 12, the oxygen concentration sensor 13 and the control valve 15.
In this embodiment, the bracket 10 includes a base 101 and guide rods 102, the base 101 is a circular or regular polygonal plate-shaped frame structure, the side surface of the base 101 is connected to at least three guide rods 102, the guide rods 102 are perpendicular to the support post 11, the guide rods 102 are hollow cylindrical structures, 1 to 4 ultrasonic oscillation mechanisms 7 are arranged in each guide rod 102, and the ultrasonic oscillation mechanisms 7 are mutually parallel and uniformly distributed along the axial direction of the guide rods 102.
In the production and preparation of the electrolyte, the use amount of the graphene dispersion liquid can be adjusted, and the types of the salt additive and the inorganic acid can be selected, so that the requirement of matching use of a lead-acid battery, a lithium battery and a sodium battery can be met flexibly, and the flexibility and the universality of use of the electrolyte are effectively improved.
According to the invention, through optimizing the raw materials in the electrolyte, on one hand, the production efficiency of the electrolyte, the stability and the reliability of the quality of the electrolyte product are effectively improved, and simultaneously, the high temperature resistance of the electrolyte is effectively improved and the production cost is reduced; on the other hand, the electrolyte production equipment is integrated in the unified bearing rack, the efficiency of electrolyte production operation is effectively improved, the production process is simplified, the production cost is effectively reduced, in production, in addition, the defect of oxidative deterioration between the raw materials and oxygen in the electrolyte production is effectively overcome through a low-oxygen high-pressure environment formed by inert gas in the reaction kettle, in addition, the efficiency and the quality of mixing among the components in the electrolyte mixing operation are improved through the high-pressure environment, the reaction efficiency among the raw material components is improved, the molecular acting force among the electrolyte components is improved, and the comprehensive performance and the quality of an electrolyte product are improved.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A durable high-temperature wave electrolyte is characterized in that: the durable high-temperature wave electrolyte comprises the following components in parts by weight: 4.1-8.2% of graphene dispersion liquid, 3.6-10.5% of salt additive, 8.1-11.4% of high-temperature resistant additive, 0.5-2.1% of functional additive, 0.1-2.8% of activating agent, 1.5-3.1% of stabilizing agent, 1.2-2.8% of inorganic acid, 0-1.3% of potassium permanganate and the balance of non-aqueous solvent.
2. The durable high temperature wave electrolyte of claim 1, wherein: the graphene dispersion liquid is oily, wherein the particle size is 1-10 mu m, the thickness is 0.8-1.0nm, the number of layers is less than or equal to 3, and the purity is not less than 99%.
3. The durable high temperature wave electrolyte of claim 1, wherein: the salt additive is any one of lithium salt and sodium salt, wherein the lithium salt comprises any one of lithium hexafluorophosphate, lithium bis (oxalato) borate and lithium bis (oxalato) borate; the sodium salt is at least one of sodium hexafluorophosphate, sodium chloride, sodium fluoride, sodium sulfate, sodium carbonate, sodium phosphate, sodium nitrate, sodium difluorooxalate, sodium pyrophosphate, sodium dodecylbenzene sulfonate, sodium dodecyl sulfate, trisodium citrate, sodium metaborate, sodium borate, sodium molybdate, sodium tungstate, sodium bromide, sodium nitrite, sodium iodate, sodium iodide, sodium silicate, sodium lignosulfonate, sodium oxalate, sodium aluminate, sodium methanesulfonate, sodium acetate, sodium dichromate, sodium hexafluoroarsenate, sodium tetrafluoroborate, sodium perchlorate and sodium trifluoromethanesulfonimide.
4. The durable high temperature wave electrolyte of claim 1, wherein: the high-temperature resistant additive is tetra-n-propyl zirconate; the functional additive is biphenyl, vinylene carbonate, fluoroethylene carbonate, sultone, ethylene sulfite, fluorosulfonate and acid anhydride; activators include, but are not limited to, sodium dodecylbenzene sulfonate; the stabilizer is one or more of phosphate and active pyrophosphate which are mixed in any proportion; the inorganic acid is any one of hydrochloric acid, sulfuric acid and phosphoric acid.
5. The durable high temperature wave electrolyte of claim 1, wherein: the non-aqueous solvent is any one of ethylene carbonate, dimethyl carbonate, ethyl butyrate, methyl butyrate, dioxolane, tetrafuran and ethyl acetate.
6. A manufacturing apparatus for manufacturing the durable high temperature wave electrolyte of any one of claims 1 to 5, characterized in that: the preparation equipment of the durable high-temperature wave electrolyte comprises a bearing frame (1), a lifting driving mechanism (2), a reaction kettle (3), a sealing cover (4), a vacuum pump (5), a booster pump (6), an ultrasonic oscillation mechanism (7), an electromagnetic heating mechanism (8), an irradiation heating mechanism (9), a bracket (10), a bearing column (11), an air pressure sensor (12), an oxygen concentration sensor (13) and a driving circuit (14), wherein the bearing frame (1) is a columnar frame structure with an axis and a horizontal plane vertically distributed, the reaction kettle (3) is embedded in the bearing frame (1), is coaxially distributed with the bearing frame (1) and is in sliding connection with the bearing frame (1) through at least two lifting driving mechanisms (2), the upper end face of the reaction kettle (3) is connected with the sealing cover (4) to form a closed cavity structure, and an exhaust port (31) is formed in the upper end face of the side wall of the reaction kettle (3), An air inlet (32) and a charge door (33), wherein gas vent (31) and air inlet (32) symmetric distribution are in reation kettle (3) axis both sides, charge door (33) are located position between gas vent (31) and air inlet (32), a control valve (15) are all established to gas vent (31), air inlet (32) and charge door (33), and gas vent (31), air inlet (32) communicate with vacuum pump (5), booster pump (6) through control valve (15) respectively, inlay in reation kettle (3) bracket (10) with reation kettle (3) coaxial distribution.
7. The apparatus for preparing a durable high temperature wave electrolyte as claimed in claim 6, wherein: the bracket (10) is of a star-shaped frame structure, the diameter of the bracket (10) is 20% -60% of the inner diameter of the reaction kettle (3), the upper end face of the bracket (10) is connected with the bearing column (11) and coaxially distributed with the bearing column (11), the bearing column (11) is connected with the sealing cover (4) through the lifting driving mechanism (2) and coaxially distributed with the reaction kettle (3), the distance between the bracket (10) and the upper end face of the reaction kettle (3) is 5% -95% of the depth of the reaction kettle (3), at least three ultrasonic oscillation mechanisms (7) are uniformly distributed around the axis of the reaction kettle (3) and connected with the lower end face of the bracket (10), at least two electromagnetic heating mechanisms (8) are uniformly distributed around the axis of the reaction kettle (3) and embedded at the bottom of the reaction kettle (3), and the total bottom area of the electromagnetic heating mechanisms (8) is 5% -10% of the volume of the reaction kettle (3), the irradiation heating mechanism (9) is at least three, is embedded in the lower end face of the sealing cover (4), the axis of the irradiation heating mechanism (9) is intersected with the axis of the reaction kettle (3) and forms an included angle of 10-60 degrees, the pressure sensor (12) and the oxygen concentration sensor (13) are all one, and are embedded in the lower end face of the sealing cover (4), the vacuum pump (5), the booster pump (6) and the driving circuit (14) are connected with the outer surface of the bearing rack (1), and the driving circuit (14) is respectively connected with the vacuum pump (5), the booster pump (6), the ultrasonic oscillation mechanism (7), the electromagnetic heating mechanism (8), the irradiation heating mechanism (9), the pressure sensor (12), the oxygen concentration sensor (13) and the control valve (15).
8. The apparatus for preparing a durable high temperature wave electrolyte as claimed in claim 6, wherein: bracket (10) including base (101), guide bar (102), base (101) are the arbitrary platelike frame structure of circular and regular polygon, base (101) side surface is connected with at least three guide bar (102), just guide bar (102) and bearing post (11) vertical distribution, guide bar (102) are hollow column structure, and all establish 1-4 ultrasonic oscillation mechanism (7) in every guide bar (102), and each ultrasonic oscillation mechanism (7) each other parallel and along guide bar (102) axis direction equipartition.
9. A manufacturing method using the manufacturing apparatus of a durable high temperature wave electrolyte according to claim 6, characterized in that: the preparation method of the durable high-temperature wave electrolyte comprises the following steps:
s1, presetting electrolyte, namely firstly adding a non-aqueous solvent into a reaction kettle (3), replacing air in the reaction kettle (3) with inert gas, increasing the air pressure in the reaction kettle (3) to 1.5-2.3 times of the standard atmospheric pressure, then sealing the reaction kettle (3), uniformly heating the reaction kettle (3) to 60-90 ℃, and preserving heat and pressure for 10-20 minutes;
s2, preparing electrolyte, after the step S1 is completed, determining the type of a salt additive, premixing the selected salt additive with graphene dispersion liquid, the salt additive, a high-temperature-resistant additive, a functional additive, an activator, a stabilizer, an inorganic acid and potassium permanganate, adding the premix into a non-aqueous solvent in a reaction kettle (3) at a constant speed within 3-10 minutes after premixing, ultrasonically homogenizing the mixed liquid for 30-60 minutes, simultaneously reducing the temperature of a mixture in the reaction kettle (3) to 50-60 ℃ within the first 5-10 minutes of ultrasonic homogenization, keeping the temperature and pressure for homogenization for 20-30 minutes, reducing the temperature to 35-40 ℃ at a constant speed within the last 10-15 minutes, and keeping the pressure and standing for 10-30 minutes after ultrasonic homogenization is stopped to obtain the finished electrolyte.
10. The method according to claim 9, wherein the method further comprises: in the step S2, when the salt additive is selected, the concentration of the sodium salt raw material is 1-2.5 times of the lithium salt.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114486460A (en) * | 2022-01-28 | 2022-05-13 | 东方电气(广州)重型机器有限公司 | Electrolyte of austenitic stainless steel and application thereof |
| CN116598589A (en) * | 2023-05-29 | 2023-08-15 | 江苏丰山全诺新能源科技有限公司 | Preparation method of wide-temperature flame-retardant sodium ion battery electrolyte |
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2021
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114486460A (en) * | 2022-01-28 | 2022-05-13 | 东方电气(广州)重型机器有限公司 | Electrolyte of austenitic stainless steel and application thereof |
| CN116598589A (en) * | 2023-05-29 | 2023-08-15 | 江苏丰山全诺新能源科技有限公司 | Preparation method of wide-temperature flame-retardant sodium ion battery electrolyte |
| CN116598589B (en) * | 2023-05-29 | 2024-02-13 | 江苏丰山全诺新能源科技有限公司 | Preparation method of sodium ion battery electrolyte |
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