CN220176900U - Solvent recovery device for liquid phase cladding material - Google Patents
Solvent recovery device for liquid phase cladding material Download PDFInfo
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- CN220176900U CN220176900U CN202320946042.9U CN202320946042U CN220176900U CN 220176900 U CN220176900 U CN 220176900U CN 202320946042 U CN202320946042 U CN 202320946042U CN 220176900 U CN220176900 U CN 220176900U
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- 239000002904 solvent Substances 0.000 title claims abstract description 96
- 238000011084 recovery Methods 0.000 title claims abstract description 63
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- 239000000463 material Substances 0.000 title claims abstract description 53
- 238000005253 cladding Methods 0.000 title claims description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000011261 inert gas Substances 0.000 claims abstract description 38
- 239000011248 coating agent Substances 0.000 claims abstract description 36
- 238000000576 coating method Methods 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims description 55
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 10
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- 238000000034 method Methods 0.000 description 21
- 239000010439 graphite Substances 0.000 description 17
- 229910002804 graphite Inorganic materials 0.000 description 17
- 230000000694 effects Effects 0.000 description 11
- 239000003960 organic solvent Substances 0.000 description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 8
- 239000010405 anode material Substances 0.000 description 8
- 239000007773 negative electrode material Substances 0.000 description 8
- 239000010406 cathode material Substances 0.000 description 6
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- 238000002360 preparation method Methods 0.000 description 3
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
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Abstract
The utility model provides a solvent recovery device of a liquid-phase coating material, which comprises a reaction device, a filter, at least one condenser and a collecting device, wherein the filter, the at least one condenser and the collecting device are sequentially connected from an air outlet of the reaction device; the reaction device is provided with an inert gas inlet. The solvent recovery device is provided with the inert gas inlet to introduce inert gas into the solvent recovery device, so that the gaseous solvent can be conveniently and rapidly drained to the condenser in a high-efficiency manner, and side reactions caused by introducing air are avoided; meanwhile, the filter arranged between the condenser and the reaction kettle can effectively prevent the blockage of a condensation pipeline and avoid the danger caused by the overhigh pressure; through collocation with horizontal condenser and vertical condenser mutually, can make the condensation route tortuous and lengthen, effectively promote the rate of recovery, and set up vertical condenser in the rear, be favorable to increasing the velocity of flow of comdenstion water, can guarantee the cleanness of pipeline, prevent the production of incrustation scale.
Description
Technical Field
The utility model belongs to the technical field of battery manufacturing, relates to a device for recovering solvents of a battery coating material during manufacturing, and particularly relates to a solvent recovery device for a liquid-phase coating material.
Background
The graphite negative electrode material has the advantages of low cost, abundant reserves, high specific capacity, low lithium intercalation and deintercalation platform, long cycle life and the like, and plays a dominant role in a negative electrode material system of a lithium ion battery. However, in the practical application process, the compatibility of graphite and an organic solvent electrolyte is poor, excessive SEI (solid electrolyte interface) films are formed on the surfaces of the graphite and the organic solvent electrolyte, active lithium in the electrolyte is consumed, partial capacity is irreversible, meanwhile, the impedance of an electrode/electrolyte interface is increased, the lithium ion conduction rate is reduced, and the problems of peeling of graphite flakes, reduced cycle performance and the like are easily caused in the charge and discharge process.
Aiming at the defects of the graphite cathode material, the asphalt is generally dissolved in an organic solvent by a liquid phase method, and the graphite material is coated and modified to further improve the electrochemical performance of the graphite cathode material.
CN106486653a discloses a preparation method of a liquid phase coated modified graphite negative electrode material, which comprises the steps of mixing graphite fine powder with a liquid coating agent dissolved in a solvent in a high-speed mixer at a high temperature, heating and high speed, adding the mixture into a continuous coating machine for coating to obtain a precursor, carrying out high-temperature heat treatment under the protection of inert gas in a tubular furnace, preserving heat, and cooling to room temperature to obtain the liquid phase coated modified graphite negative electrode material; the liquid coating agent is one of petroleum residual oil, liquid epoxy resin, phenolic resin dissolved in alcohol and liquid asphalt, and the solvent comprises ethanol, acetone and other organic solvents.
CN213913529U discloses a graphite negative electrode material liquid phase cladding device, which comprises a cladding box and a fixed barrel for cladding, wherein stirring components or scraping plates are arranged in the cladding box and the fixed barrel to stir the solution sufficiently for the second time, so that the compatibility of the solution is effectively improved, and the cleaning is more convenient; the right side of cladding case is provided with the water tank, still is provided with drum and the flow channel that is used for vapor to make full use of vapor's heat, waste heat can heat fixed bucket, then cools off in the water tank, can realize vapor's recycle.
The negative electrode material prepared by the liquid phase method has the advantages of good chemical uniformity, small product particle size, low production cost, simple working procedure and the like, and can effectively improve the first effect and ensure the cycle performance. However, the organic solvent used in the liquid phase method is not effectively treated, and besides ethanol and acetone, tetrahydrofuran (THF) and the like are usually used in the liquid phase method, so that the solvent is easy to volatilize, a large amount of the solvent can escape in the kneading and coating process, and the solvent is usually directly discharged into the air by heating in the subsequent process, so that the toxic solvent is easy to cause environmental pollution and human body hazard.
The amount of the organic solvent used in the liquid phase method is small, and when the amount is generally 10 to 20%, the solvent is rarely recycled due to easy volatilization, but when the product is to be subjected to pilot-scale or large-scale mass production, the total amount of the solvent is large, and the method has recycling value. However, the prior art lacks an effective scheme for recycling the organic solvent in the preparation of the anode material by liquid phase coating.
Disclosure of Invention
Aiming at the defects of the prior art, the utility model aims to provide a solvent recovery device of a liquid phase coating material, which comprises a reaction device, a filter, at least one condenser and a collecting device, wherein the filter, the at least one condenser and the collecting device are sequentially connected from an air outlet of the reaction device. The filter arranged between the condenser and the reaction kettle of the solvent recovery device can effectively prevent the blockage of a condensation pipeline and avoid dangers caused by overhigh pressure; at least one condenser is arranged, so that a condensing path can be bent and prolonged, and the recovery rate is effectively improved.
To achieve the purpose, the utility model adopts the following technical scheme:
in a first aspect, the utility model provides a solvent recovery device for a liquid-phase coating material, which comprises a reaction device, wherein the reaction device is provided with a feeding cylinder and an air outlet; and the air outlet is connected with a filter, at least one condenser and a collecting device which are sequentially arranged along the output direction of the air.
The filter arranged between the reaction kettle and the condenser can effectively prevent the blockage of the condensing pipeline, for example, after the solvent is volatilized in the reaction device, the graphite anode material coated by liquid phase is easy to cause the lifting of graphite powder to enter the condensing pipeline in the condenser, the pipeline is gradually blocked, the cooling efficiency is reduced, the internal pressure is easy to be excessively high to cause danger due to continuous congestion, and graphite powder impurities are easy to be contained in the solvent obtained by condensation and recovery so as not to meet the use requirement, so that the filter is necessary when the solvent is recovered from the liquid phase coating material.
As a preferable technical scheme of the utility model, a stirring device is arranged in the reaction device, the stirring device comprises a motor arranged outside the reaction device and a stirring shaft in transmission connection with the motor, and the stirring shaft stretches into the reaction device.
Preferably, the stirring shaft is provided with double helical stirring sheets and/or sigma-type stirring sheets.
When the liquid phase method is used for coating the anode material, the coating effect can be influenced by stirring, and the double-helical-ribbon stirring piece and/or the sigma-type stirring piece can effectively promote the stirring to be more uniform, so that the coating effect of the anode material is improved, the solvent can be more promoted to be fully volatilized, and the subsequent recovery is facilitated.
Illustratively, the double-ribbon structure comprises a main ribbon and a secondary ribbon, wherein the main ribbon is wound on a shaft section of the stirring shaft positioned in the reaction device, the secondary ribbon is positioned on the inner side of the main ribbon and wound on the stirring shaft, the spiral directions of the two ribbons are opposite, the main ribbon is used for lifting materials upwards, the secondary ribbon pushes the lifted materials downwards, so that material circulation is promoted, and at least one shoveling plate can be further arranged between the main ribbon and the secondary ribbon, so that the materials are pushed to the periphery in the falling process, and the materials are prevented from being accumulated at the bottom.
The sigma-type stirring blade comprises two low-speed twist stirring paddles, the stirring process has the advantages of low clearance and no dead angle, the low-speed stirring paddles have strong kneading action and do not interfere with each other to move, further the materials are driven to move up and down/left and right circularly, a high-speed stirring shaft can be further arranged, two sawtooth dispersing discs which rotate and revolve are arranged on the high-speed stirring shaft, the materials are guaranteed to be mixed more fully, and the uniform stirring effect is improved.
As a preferable technical scheme of the utility model, a heating device is arranged inside the reaction device.
Preferably, the reaction device comprises an inner liner and an outer insulation layer.
In the liquid phase method, only one solvent is usually used, and only the solvent is required to be collected in the subsequent condensation process, so that the sufficient evaporation and condensation effects of the solvent are ensured, and the temperature in the process of volatilizing the solvent by heating is strictly controlled. Illustratively, the reactor of the present utility model may be a stainless steel high temperature reactor with an internal liner plus external insulation structure.
As a preferable technical scheme of the utility model, the reaction device is provided with an inert gas inlet.
Preferably, the inert gas inlet is provided with a flow meter for controlling the flow rate of the inert gas.
According to the solvent recovery device, the inert gas inlet is arranged on the reaction device so as to introduce inert gas into the reaction device, so that the solvent is fully volatilized, the volatilized gaseous solvent is quickly and efficiently led into the condenser for liquefaction, and meanwhile, the high-temperature material can be prevented from reacting by contacting with air.
When the inert gas inlet is arranged and inert gas is introduced into the interior, the inert gas further drives dust to raise, so that a filter is required to be arranged, the problem of overlarge internal pressure caused by continuous introduction of the inert gas due to blockage is prevented, and potential safety hazards are avoided.
As a preferred technical solution of the present utility model, the condenser comprises at least one horizontal condenser and at least one vertical condenser connected to the last horizontal condenser along the output direction of the gas.
The utility model adopts a mode of combining the horizontal condenser and the vertical condenser, can prolong the condensing path and make the condensing pipeline zigzag, thereby effectively liquefying and recovering the gaseous solvent, improving the recovery efficiency, and the vertical condenser is arranged at the rear, thereby being beneficial to increasing the flow rate of the condensed water flowing vertically, being not easy to generate scale and ensuring the cleanness of the pipeline.
As a preferable technical scheme of the utility model, when the number of the horizontal condensers is more than or equal to two, the horizontal condensers are mutually connected in parallel; when the number of the vertical condensers is more than or equal to two, the vertical condensers are mutually connected in parallel.
As the preferable technical scheme of the utility model, the water inlet of the horizontal condenser is connected with the water chiller, the water outlet of the horizontal condenser is connected with the water inlet of the vertical condenser, and the water outlet of the vertical condenser is connected with the water chiller to enable condensate water to flow back and circulate.
In the utility model, the condensed water pipelines of the horizontal condenser and the vertical condenser are communicated and are commonly connected in the same water chiller.
As a preferable technical scheme of the utility model, the solvent recovery device of the liquid-phase coating material further comprises an automatic control module, wherein the automatic control module is electrically connected with the reaction device and the water chiller, and is used for controlling the stirring rate, the heating temperature and the flow of inert gas of the reaction device and controlling the temperature of condensed water generated by the water chiller.
As a preferred technical scheme of the utility model, the collecting device is provided with a vacuumizing interface.
According to the utility model, the vacuum-pumping interface is arranged on the collecting device and is connected with external vacuum equipment, so that a negative pressure environment is provided inside the solvent recovery device, the circulation of gas solvent is accelerated, and the condensation recovery is assisted.
According to the preferred technical scheme, a discharge hole of the collecting device is connected with a material extracting device for extracting the condensed and recovered solvent.
Illustratively, the recovery method of the present utility model using the solvent recovery device for liquid phase clad material comprises the steps of: transferring the liquid-phase coating material into a reaction device, heating and stirring to promote the solvent to volatilize, introducing inert gas, leading the gaseous solvent into a horizontal condenser for primary condensation after passing through a filter under the drainage effect of the inert gas, then into a vertical condenser for secondary condensation, recovering the liquid-phase coating material in a collecting device after condensing, and carrying out secondary utilization after being extracted by a material extracting device.
In addition, in the use process of the solvent recovery device of the liquid phase coating material provided by the utility model, parameters such as heating temperature, stirring rate, inert gas flow, condensate water temperature and the like influence recovery efficiency, and the best solvent recovery efficiency can be achieved by setting proper parameters.
Specifically, since the boiling point of the solvent used for coating the anode material by the liquid phase method is usually 100 ℃ or lower, the heating temperature in the reaction apparatus is preferably set to 120 to 150 ℃, for example, 120 ℃, 123 ℃, 126 ℃, 129 ℃, 132 ℃, 135 ℃, 138 ℃, 141 ℃, 144 ℃, 147 ℃, 120 ℃, or the like, but the present utility model is not limited to the above-mentioned values, and other non-mentioned values within the above-mentioned value ranges are similarly applicable.
It should be noted that, too high temperature can cause the organic solvent to volatilize rapidly in a short time, so that part of the gas solvent can not be condensed and discharged in time, and the yield is reduced; too low a temperature can result in too long condensation time, prolonged production time, and increased cost.
Preferably, the stirring rate in the reaction apparatus is set to 20 to 30Hz, for example, 20Hz, 21Hz, 22Hz, 23Hz, 24Hz, 25Hz, 26Hz, 27Hz, 28Hz, 29Hz or 30Hz, etc., but is not limited to the recited values, and other non-recited values within the above-mentioned range are equally applicable.
It is noted that too fast stirring speed can increase dust in the high-temperature kettle, which causes the filter to be blocked, slows down the service life of the filter and prevents solvent gas from entering the condenser; too slow stirring speed can lead to too slow solvent volatilization, reduce evaporation efficiency, and lead to difficult material agglomeration and discharging.
Preferably, the flow rate of the inert gas in the reaction apparatus is set to 100 to 200L/h, for example, 100L/h, 110L/h, 120L/h, 130L/h, 140L/h, 150L/h, 160L/h, 170L/h, 180L/h, 190L/h or 200L/h, etc., but not limited to the recited values, and other non-recited values within the above-mentioned range are equally applicable.
It should be noted that, when the amount of inert gas introduced is not too small, it is difficult to drain the gaseous solvent from the reaction apparatus to the condenser; the excessive flow of the inert gas can lead to incomplete condensation of the solvent gas and direct discharge of the solvent gas along with the inert gas, thereby reducing the recovery rate and polluting the environment. The inert gas includes at least one of nitrogen or argon.
Preferably, the temperature of the condensed water produced by the water chiller is 5 to 18 ℃, for example, 5 ℃, 6 ℃, 7 ℃, 8 ℃, 9 ℃, 10 ℃, 11 ℃, 12 ℃, 13 ℃, 14 ℃, 15 ℃, 16 ℃, 17 ℃, 18 ℃, or the like, but the condensed water is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value ranges are equally applicable.
The temperature of the condensed water can be judged and regulated according to the outflow temperature T1 of the water outlet of the last vertical condenser, and the temperature T1 is less than or equal to 20 ℃.
Compared with the prior art, the utility model has the beneficial effects that:
(1) According to the solvent recovery device, the inert gas inlet is arranged to introduce inert gas into the solvent recovery device, so that the solvent is fully volatilized, the volatilized gaseous solvent is quickly and efficiently led into the condenser to be liquefied, and meanwhile, the high-temperature material can be prevented from reacting by contacting with air; the filter arranged between the reaction kettle and the condenser can effectively prevent the blockage of a condensation pipeline, avoid dangers caused by overhigh pressure, and reduce solid phase impurities in the condensed and recovered solvent; the combination mode of the horizontal condenser and the vertical condenser can prolong the condensing path and make the condensing pipeline zigzag, so that the gaseous solvent is effectively liquefied and recovered, the recovery efficiency is improved, and the vertical condenser is arranged at the rear, thereby being beneficial to increasing the flow rate of the condensed water flowing vertically, being not easy to generate scale and ensuring the cleanness of a pipeline;
(2) The reaction device provided by the utility model has the advantages that the heat preservation effect can be effectively enhanced by using the structure of the inner lining and the outer heat preservation, so that the organic solvent can still be completely volatilized continuously through good heat preservation after the reaction device stops heating;
(3) According to the utility model, the double helical stirring sheets and/or the sigma-type stirring sheets are arranged, so that the stirring promotion is more uniform, the coating effect of the cathode material is improved on one hand, the sufficient volatilization of the solvent is promoted on the other hand, and the subsequent recovery is facilitated;
(4) According to the utility model, the vacuum-pumping interface is arranged on the collecting device and is connected with external vacuum equipment, so that a negative pressure environment is provided inside the solvent recovery device, the circulation of gas solvent is accelerated, and the condensation recovery is assisted.
Drawings
FIG. 1 is a schematic view of a solvent recovery apparatus for a liquid-phase clad material in example 1;
FIG. 2 is an internal schematic view of the reaction apparatus in example 6;
FIG. 3 is an internal schematic view of the reaction apparatus in example 7;
the device comprises a 1-reaction device, an 11-blanking port, a 12-air outlet, a 13-inert gas inlet, a 14-stirring shaft, a 15-external heat insulation layer, a 16-feeding cylinder, a 2-filter, a 3-horizontal condenser, a water inlet of a 31-horizontal condenser, a water outlet of a 32-horizontal condenser, a 4-vertical condenser, a water inlet of a 41-vertical condenser, a water outlet of a 42-vertical condenser, a 5-collecting device, a 51-vacuumizing interface and a 6-material sucking pump.
Detailed Description
In order to make the technical solution, objects and advantages of the present utility model more apparent, the present utility model will be described in further detail by means of specific examples of embodiments with reference to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the utility model, are not intended to limit the utility model.
In the description of the present utility model, it should be noted that the directions or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present utility model and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present utility model, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. For the electrical and communication fields, either a wired connection or a wireless connection is possible. The specific meaning of the above terms in the present utility model will be understood in specific cases by those of ordinary skill in the art.
Example 1
The embodiment provides a solvent recovery device of a liquid-phase coating material, the schematic diagram of which is shown in fig. 1, wherein the solvent recovery device of the liquid-phase coating material comprises a reaction device 1, and the reaction device 1 is provided with a feeding barrel 16, a discharging opening 11 and an air outlet 12; the air outlet 12 is connected with a filter 2, a horizontal condenser 3, a vertical condenser 4 and a collecting device 5 which are sequentially arranged along the output direction of air;
the reaction device 1 is provided with an inert gas inlet 13 and is connected with an external inert gas source; the inert gas inlet 13 is provided with a flowmeter for controlling the flow rate of inert gas;
a stirring device and a heating device are arranged in the reaction device 1; the stirring device comprises a motor arranged outside the reaction device 1 and a stirring shaft 14 in transmission connection with the motor, and the stirring shaft 14 stretches into the reaction device 1;
the reaction device 1 comprises an inner lining and an outer heat-insulating layer 15;
the water inlet 31 of the horizontal condenser 3 is connected with a water chiller, the water outlet 32 of the horizontal condenser 3 is connected with the water inlet 41 of the vertical condenser 4, and the water outlet 42 of the vertical condenser 4 is connected with the water chiller to enable condensate water to flow back and circulate;
a discharge hole of the collecting device 5 is connected with a material pump 6 for extracting the condensed and recovered solvent;
the solvent recovery device of the liquid-phase coating material further comprises an automatic control module, wherein the automatic control module is electrically connected with a stirring device, a heating device and a flowmeter arranged at an inert gas inlet 13 in the reaction device 1 and is electrically connected with the cold water machine, and is used for controlling the stirring rate, the heating temperature and the flow of inert gas of the reaction device 1 and controlling the temperature of condensed water generated by the cold water machine;
in the embodiment, the reaction device 1 is a 100L stainless steel (sus 304) high-temperature reaction kettle, the power of a motor is 5.5Kw/4P, and a 5.5KW frequency converter and a gear reducer are arranged; the specification of the horizontal condenser 3 is 12m 2 The main body is sus304, and the shell is Q235-B; the specification of the vertical condenser 4 is 6m 2 The main material is sus30And 4, the shell is Q235-B.
Example 2
The present embodiment provides a solvent recovery device for a liquid phase coating material, and compared with embodiment 1, the solvent recovery device for a liquid phase coating material in this embodiment is different in that: two parallel horizontal condensers 3 and two parallel vertical condensers 4 are arranged; and the collecting device 5 is provided with a vacuum-pumping port 51 and connected to an external vacuum apparatus, the other conditions are exactly the same as those of embodiment 1 except for the above.
Example 3
The present embodiment provides a solvent recovery device for a liquid phase coating material, and compared with embodiment 1, the solvent recovery device for a liquid phase coating material in this embodiment is different in that: two horizontal condensers 3 and two vertical condensers 4 which are sequentially connected in series are arranged; and the collecting device 5 is provided with a vacuum-pumping port 51 and connected to an external vacuum apparatus, the other conditions are exactly the same as those of embodiment 1 except for the above.
Example 4
The present embodiment provides a solvent recovery device for a liquid phase coating material, which is similar to embodiment 1 except that the inert gas inlet 13 is not provided in the reaction device 1 in comparison with embodiment 1.
Example 5
The present embodiment provides a solvent recovery device for a liquid phase clad material, which is not provided with a vertical condenser 4 as compared with embodiment 1, and the other conditions are exactly the same as embodiment 1 except for the above.
Example 6
Compared with the embodiment 1, as shown in fig. 2, the solvent recovery device for the liquid-phase coating material is provided in the stirring shaft 14 of the embodiment, the structure of the double spiral bands comprises a main spiral band and a secondary spiral band, wherein the main spiral band is wound on a shaft section of the stirring shaft 14 positioned in the reaction device 1, the secondary spiral band is positioned on the inner side of the main spiral band and wound on the stirring shaft 14, the spiral directions of the two spiral bands are opposite, and four shoveling plates are arranged between the main spiral band and the secondary spiral band, and other conditions are identical to those of the embodiment 1 except the above.
Example 7
In the present embodiment, as compared with embodiment 1, as shown in fig. 3, a sigma-type stirring blade is provided on the stirring shaft 14 of the present embodiment, a high-speed stirring shaft is further provided inside the reaction apparatus 1, and two sawtooth dispersion plates rotating and revolving are provided on the high-speed stirring shaft, and the other conditions are exactly the same as those of embodiment 1 except for the above.
Comparative example 1
The present comparative example provides a solvent recovery apparatus for a liquid-phase clad material, which is identical to that of example 1 except that the filter 2 is not provided in the solvent recovery apparatus for a liquid-phase clad material in comparison with example 1.
The conventional preparation method of the liquid-phase coated negative electrode material uses tetrahydrofuran as a solvent, fully dissolves medium-temperature asphalt in the tetrahydrofuran, uniformly mixes and kneads an asphalt solution and graphitized powder, starts heating to completely evaporate the solvent, and carbonizes at 1150 ℃ to obtain the liquid-phase coated graphite negative electrode material. Wherein the median particle diameter D50 is 13.68 mu m, and the tap density is 1.03g/cm 3 The energy density is 355.90wh/kg, and the first coulomb efficiency can reach 95.15 percent.
Transferring the liquid-phase coated graphite anode material which is not volatilized by the solvent into reaction devices of solvent recovery devices provided by examples and comparative examples respectively, setting a heating temperature of 130 ℃, setting a stirring rate of 25Hz, heating and stirring for 4 hours, stopping heating, continuously introducing nitrogen with a flow rate of 150L/h in the process, setting the temperature of condensed water generated by a cold water machine to be 12 ℃, and always keeping the temperature of the condensed water before the condensed water flows back to the cold water machine to be less than or equal to 20 ℃; stopping collecting after heating is turned off for 2 hours;
extracting the condensed and recovered solvent in the collecting device by a material extracting device, and calculating the recovery rate; the liquid phase coated graphite cathode material in the reaction device is collected through a feed opening and tested for particle size and tap density, and the particle size and the tap density are tested by using British Markov MASTAERSTER and Dandong Baite BT-302 instruments respectively. Meanwhile, the obtained liquid phase coated graphite cathode material is used for manufacturing a button cell, and the manufacturing method comprises the following steps: mixing binder and conductive agent in certain proportion, adding graphite cathode material, stirring again to obtain slurry, coating, preheating, drying, rolling, punching, assembling, activating to obtain button cell, and testing energy density and initial effect, wherein the results are recorded in table 1.
TABLE 1
Note that: in Table 1, the solvent recovery rate "/" indicates that the solvent recovery rate could not be calculated.
As can be seen from table 1:
the graphite anode material prepared by the solvent recovery device has basically no difference in particle size and tap density results as compared with the graphite anode material prepared by the conventional method, and the energy density and the first effect are slightly improved; in the embodiment 2, two parallel horizontal condensers and two parallel vertical condensers are combined, and the collecting tank is in a negative pressure state, so that condensed solvent is more beneficial to entering the collecting tank, and compared with the embodiment 1, the condensing capacity can be enhanced, and the solvent recovery efficiency can be improved; in example 3, two horizontal condensers and two vertical condensers are connected in series in order, and recovery efficiency can be improved as compared with example 1, but the series connection method may interfere with other parts in actual installation of equipment, and has high requirements for construction. The absence of the filtration device in comparative example 1 resulted in the graphite micropowder entering the cooling line to the collection tank, which made it difficult to calculate the actual yield of solvent and also blocked the line in severe cases. In example 4, no inert gas was introduced, which resulted in accumulation of the gaseous solvent in the autoclave, and when the internal pressure of the cooling autoclave reached a certain pressure, a small portion of the gaseous solvent was fed to the condensing apparatus for recovery, so that the condensing effect was extremely poor if no inert gas was introduced. In example 5, the vertical condenser is omitted, but the cooling flow rate and the heat transfer coefficient of the vertical condenser are high, so that the condensation effect is greatly reduced, and in examples 6 and 7, double helical stirring sheets and/or sigma type stirring sheets are arranged on the stirring shaft, so that the solvent recovery efficiency is improved.
The foregoing is merely illustrative of the present utility model, and the present utility model is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that fall within the technical scope of the present utility model disclosed herein are within the scope of the present utility model.
Claims (11)
1. The solvent recovery device for the liquid-phase coating material is characterized by comprising a reaction device (1), wherein the reaction device (1) is provided with a feed cylinder (16), a feed opening (11) and an air outlet (12); along the output direction of gas, gas outlet (12) are connected with filter (2), at least one condenser and collection device (5) that set gradually.
2. The solvent recovery device for liquid phase coating materials according to claim 1, wherein a stirring device is arranged inside the reaction device (1), the stirring device comprises a motor arranged outside the reaction device (1), and a stirring shaft (14) in transmission connection with the motor, and the stirring shaft (14) stretches into the reaction device (1).
3. The solvent recovery device for liquid phase coating materials according to claim 2, wherein the stirring shaft (14) is provided with a double helical ribbon stirring blade and/or a sigma type stirring blade.
4. The solvent recovery device for liquid phase cladding material according to claim 1, wherein a heating device is provided inside the reaction device (1); the reaction device (1) comprises an inner lining and an outer heat-insulating layer (15).
5. The solvent recovery device for liquid phase cladding material according to claim 1, wherein the reaction device (1) is provided with an inert gas inlet (13); the inert gas inlet (13) is provided with a flowmeter for controlling the flow rate of the inert gas.
6. A solvent recovery device for a liquid phase cladding material according to any one of claims 1-5, wherein said condenser comprises at least one horizontal condenser (3), and further comprises at least one vertical condenser (4) connected to the last horizontal condenser (3) in the output direction of the gas.
7. The solvent recovery device for liquid phase coating material according to claim 6, wherein when the number of the horizontal condensers (3) is two or more, the horizontal condensers (3) are arranged in parallel with each other; when the number of the vertical condensers (4) is more than or equal to two, the vertical condensers (4) are mutually connected in parallel.
8. The solvent recovery device for liquid phase coating materials according to claim 6, wherein the water inlet (31) of the horizontal condenser (3) is connected to a water chiller, the water outlet (32) of the horizontal condenser (3) is connected to the water inlet (41) of the vertical condenser (4), and the water outlet (42) of the vertical condenser (4) is connected to the water chiller to circulate condensed water in a reflux manner.
9. The solvent recovery device for liquid phase coating materials according to claim 8, further comprising an automatic control module, wherein the automatic control module is electrically connected with the reaction device (1) and the water chiller, and is used for controlling the stirring rate, the heating temperature and the flow rate of inert gas of the reaction device and simultaneously controlling the temperature of condensed water generated by the water chiller.
10. Solvent recovery device for liquid phase cladding material according to claim 1, wherein the collecting device (5) is provided with a vacuum-pumping interface (51).
11. The solvent recovery device for liquid phase cladding materials according to claim 1, wherein a discharge port of the collecting device (5) is connected with a pumping device (6) for pumping the condensed and recovered solvent.
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