CN117096550B - Method for recovering oil-containing waste film from wet lithium battery diaphragm by dropping liquid - Google Patents
Method for recovering oil-containing waste film from wet lithium battery diaphragm by dropping liquid Download PDFInfo
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- CN117096550B CN117096550B CN202311354827.8A CN202311354827A CN117096550B CN 117096550 B CN117096550 B CN 117096550B CN 202311354827 A CN202311354827 A CN 202311354827A CN 117096550 B CN117096550 B CN 117096550B
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- 239000007788 liquid Substances 0.000 title claims abstract description 113
- 239000002699 waste material Substances 0.000 title claims abstract description 85
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000000605 extraction Methods 0.000 claims abstract description 146
- 238000004821 distillation Methods 0.000 claims abstract description 77
- 238000011084 recovery Methods 0.000 claims abstract description 43
- 238000001035 drying Methods 0.000 claims abstract description 42
- 238000001914 filtration Methods 0.000 claims abstract description 37
- 239000012528 membrane Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims description 59
- 238000004140 cleaning Methods 0.000 claims description 58
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 54
- 238000003860 storage Methods 0.000 claims description 54
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- 238000007599 discharging Methods 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 18
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 12
- 239000003208 petroleum Substances 0.000 claims description 12
- 238000004064 recycling Methods 0.000 claims description 11
- 238000007084 catalytic combustion reaction Methods 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 6
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethyl cyclohexane Natural products CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 claims description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 abstract description 18
- 239000011174 green composite Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 22
- 239000003795 chemical substances by application Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a drip recovery method of an oil-containing waste film in a wet lithium battery diaphragm, which belongs to the field of lithium battery diaphragm recovery and comprises the following steps: throwing an oily waste film produced by a wet method into a diaphragm crusher for crushing; placing the crushed diaphragm in a hydraulic press to separate white oil; feeding the hydraulic diaphragm into a centrifugal machine, and centrifugally separating white oil; drying the membrane after centrifugal separation of white oil to obtain an oil-containing waste membrane to be separated later; fifthly, adding the waste oil-containing film to be separated into an extraction kettle, and adding an extractant into a distillation kettle; heating the distillation kettle until the extractant boils to generate extractant vapor, condensing the vapor into the extraction kettle, and dripping liquid from the extraction kettle to the distillation kettle for 3-10 times; and before the last dropping, filtering and drying the oil film and the extract, and separating the extract and the white oil by distillation and rectification of the extract. The invention replaces the green composite extractant of methylene dichloride on one hand, and improves the white oil extraction efficiency and the quality of waste films on the other hand.
Description
Technical Field
The invention relates to recovery of a lithium battery diaphragm, in particular to a method for recovering dropping liquid of an oil-containing waste film in a wet lithium battery diaphragm.
Background
The Lithium Ion Battery (LIB) has the advantages of high safety performance, small self-discharge degree, long cycle life and the like, and is widely applied to the fields of electric automobiles, 3C digital products, portable electronic equipment, energy storage materials and the like. The lithium battery diaphragm is used as one of important elements of the inner layer of the lithium battery, and the performance of the lithium battery diaphragm determines the interface structure, the internal resistance and the like of the battery, and directly influences the characteristics of the battery, such as capacity, circulation, safety performance and the like. Therefore, the separator having excellent performance plays an important role in improving the overall performance of the battery. The lithium battery diaphragm production method is mainly divided into a wet method and a dry method, and compared with the dry method process, the diaphragm prepared by the wet method process has more excellent thickness uniformity and physical and chemical properties, the aperture size and the porosity are easier to control, and the lithium battery diaphragm occupies most of high-end diaphragm markets.
In the wet diaphragm production, firstly, polyolefin resin and low molecular weight white oil are mixed, melted and extruded, and the thickness and uniformity of the diaphragm are optimized through a biaxial stretching process; and then, using dichloromethane as an extracting agent to extract white oil in the holes of the diaphragm to form the lithium battery diaphragm containing micropores. In the whole process, extrusion and stretching of the diaphragm can generate a certain amount of waste oil-containing waste films. The traditional incineration method is adopted to treat the oily waste film, so that high-toxicity waste gas such as dioxin and the like is easy to generate, the environment is polluted, and the polyolefin film and the white oil cannot be reused. Therefore, based on a wet process, the white oil and the waste film are separated by adopting an extraction method, and the white oil and the extractant are separated by rectification, so that the separation and recycling of the white oil and the waste film are realized, and the method is a treatment mode with great potential. However, by adopting the traditional extraction process and extraction equipment (such as CN111584795A and CN 207371140U), the extractant has large usage amount, high volatility and low white oil extraction efficiency (50% -75%), the quality of the deoiled film is affected, and the problem of environmental pollution is more likely to occur. In addition, the traditional extraction process mostly uses methylene dichloride as an extracting agent, wherein the methylene dichloride belongs to an ozone-consuming chemical substance, and can cause ozone decomposition after escaping to the atmosphere to form an ozone cavity.
Therefore, the development of the novel green extractant and the efficient extraction separation recovery process and equipment is not only the resource utilization of the wet lithium battery oil-containing waste film, but also the strict requirements of the nation on environmental protection.
The above background is for the convenience of understanding the present invention and is not a known art which has been disclosed to the general public before the application of the present invention.
Disclosure of Invention
Aiming at the defects, the invention provides a drip recovery method of an oil-containing waste film in a wet lithium battery diaphragm, which is characterized in that a green composite extractant capable of replacing dichloromethane is developed on one hand, and a high-efficiency extraction separation process and equipment are developed on the other hand, so that the white oil extraction efficiency and the quality of the waste film are improved, and the recycling and recycling of the oil-containing waste film of the lithium battery are realized.
The technical proposal is as follows: the method for recovering the oil-containing waste film in the wet lithium battery diaphragm is characterized by comprising the following steps of:
throwing an oily waste film produced by a wet method into a diaphragm crusher for crushing;
placing the crushed diaphragm in a hydraulic press to separate white oil;
feeding the hydraulic diaphragm into a centrifugal machine, and centrifugally separating white oil;
drying the membrane after centrifugal separation of white oil to obtain an oil-containing waste membrane to be separated later;
fifthly, adding the waste oil-containing film to be separated into an extraction kettle, and adding an extractant into a distillation kettle;
heating the distillation kettle until the extractant boils to generate extractant vapor, condensing the vapor into the extraction kettle, and dripping liquid from the extraction kettle to the distillation kettle for 3-10 times;
and before the last dropping, filtering and drying the oil film and the extract, and separating the extract and the white oil by distillation and rectification of the extract.
Further, the device adopted in the step (II) is a device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm comprises an extraction kettle, a distillation kettle, a rectifying tower, an extractant storage tank and a white oil storage tank, the upper part of the rectifying tower is connected with the extractant storage tank, the lower part of the rectifying tower is connected with the white oil storage tank, an oil film feeding port is arranged on the upper part of the extraction kettle, the bottom of the extraction kettle is connected with an oil film discharging pipe with an oil film discharging valve, the upper part of the extraction kettle is connected with a gas inlet pipe and a gas outlet pipe, the upper part of the extraction kettle is also connected with a reflux cleaning integrated pipe, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm further comprises a first condenser and a reflux pipe, the other end of the gas outlet pipe is connected with the first condenser, the first condenser is also connected with the reflux pipe, the reflux valve is arranged on the reflux pipe, the extractant storage tank is connected with a cleaning pipe, a cleaning valve is arranged on the cleaning pipe, a return pipe and the other end of a reflux cleaning integrated pipe are communicated through a three-way valve, an extractant conveying pump is arranged on the reflux cleaning integrated pipe, the other end of a gas inlet pipe is connected with a distillation still, the bottom of the extraction still is also connected with a liquid outlet pipe, the other end of the liquid outlet pipe is connected with the distillation still, the liquid outlet pipe is provided with an inverted U-shaped section, an upward convex bent pipe is connected between two vertical sections of the inverted U-shaped section, a lower valve is arranged on the bent pipe, an upper valve is arranged on the inverted U-shaped section, the upper valve is arranged above the lower valve, a mixed liquid drain pipe is connected at the bottom of the distillation still, a mixed liquid drain valve is arranged on the mixed liquid drain pipe, the other end of the mixed liquid drain pipe is connected with the middle part of the distillation still, the other end of the extractant preassembling conveying pipe is connected with the extractant storage tank, the extractant preassembling conveying pipe is provided with an extractant preassembling conveying pump.
Further, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm is also provided with a catalytic combustion device.
Further, the liquid outlet pipe is connected with an extractant recovery pipe, an extractant recovery valve is arranged on the extractant recovery pipe, and the other end of the extractant recovery pipe is connected with an extractant storage tank.
Further, a second condenser is connected between the top of the rectifying tower and the extractant storage tank.
Further, an extractant replenishing pipe is connected to the extractant storage tank, and an extractant replenishing valve is arranged on the extractant replenishing pipe; the reflux cleaning integrated pipe extends into the extraction kettle, and a spray header is arranged at the end of the reflux cleaning integrated pipe in the extraction kettle.
Further, the device of oily waste film deoiling in the wet process lithium cell diaphragm is exclusively used in still being provided with and filters integrative jar of stoving, and the oil film discharging pipe other end is connected with the integrative jar of filtration stoving, is provided with the filter in the integrative jar of filtration stoving, and dry film export has been seted up to the filter top, filters the integrative jar of stoving and still is connected with stoving steam pipe, installs the stoving steam valve on the stoving steam pipe, and the stoving steam pipe other end is connected with extraction kettle upper portion, and the integrative jar bottom of filtration stoving is connected with the filtrate recovery pipe, installs the filtrate recovery valve on the filtrate recovery pipe, and the filtrate recovery pipe other end is connected with distillation kettle upper portion.
Further, an ultrasonic device and a diaphragm baffle are arranged in the extraction kettle, the diaphragm baffle is arranged at a position close to the liquid outlet pipe, and the diaphragm baffle is of a net-shaped structure.
Further, the device adopted in the extraction tank is a device special for removing oil from the oil-containing waste film in the diaphragm of the wet lithium battery, the device special for removing oil from the oil-containing waste film in the diaphragm of the wet lithium battery comprises an extraction kettle, a distillation still, a rectifying tower, an extractant storage tank and a white oil storage tank, the upper part of the rectifying tower is connected with the extractant storage tank, the lower part of the rectifying tower is connected with the white oil storage tank, the upper part of the extraction kettle is provided with an oil film feed port, the bottom of the extraction kettle is connected with an oil film discharge pipe with an oil film discharge valve, the upper part of the extraction kettle is connected with a gas inlet pipe and a gas outlet pipe, the upper part of the extraction kettle is also connected with an integrated pipe for reflux cleaning, the device special for removing oil from the oil-containing waste film in the diaphragm of the wet lithium battery also comprises a first condenser and a reflux pipe, the other end of the gas outlet pipe is connected with the first condenser, the first condenser is also connected with the reflux pipe, a reflux valve is arranged on the reflux pipe, the extractant storage tank is connected with an inlet liquid cleaning valve, the other end of the reflux pipe is arranged on the reflux pipe, the inlet liquid cleaning valve is connected with the reflux pipe, the other end of the reflux pipe is connected with a three-way valve, the other end of the reflux cleaning pipe is connected with the reflux pipe through an integrated pipe, the upper end of the reflux pipe is connected with the reflux pipe, the reflux pipe is connected with the upper end of the reflux pipe, the reflux pipe is connected with the reflux pipe, the upper end of the reflux pipe is connected with the reflux pipe, the reflux pipe is connected with the upper pipe, and the upper end of the reflux pipe is connected with the reflux pipe, and the reflux pipe is connected with the upper end of the reflux pipe, and the reflux pipe is connected with the upper and the upper-type, and the pump is connected with the pump and the pump, the extractant preassembling conveying pipe is provided with an extractant preassembling conveying pump.
Further, the extractant is ethyl acetate and petroleum ether, wherein the ethyl acetate: the volume ratio of petroleum ether is 1-9:1.
further, the extractant is ethyl acetate and cyclohexane, wherein ethyl acetate: the volume ratio of cyclohexane is 1-9:1.
further, the extractant is ethyl acetate, petroleum ether and cyclohexane, wherein ethyl acetate: petroleum ether: the volume ratio of cyclohexane is 1-8:1-2:1.
compared with the prior art, the invention has the beneficial effects that:
aiming at the problems of large usage amount of extracting agent dichloromethane, high volatility, strong toxicity, damage to an ozone layer, low extraction rate of white oil, poor quality of a recovered diaphragm and the like in the traditional extraction method for recovering the oily waste film of the wet lithium battery, the invention develops a green composite extracting agent capable of replacing the dichloromethane on one hand, and develops an efficient extraction separation process and equipment on the other hand so as to improve the extraction efficiency of the white oil and the quality of the waste film and realize the recycling and reutilization of the oily waste film of the lithium battery.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a device dedicated to degreasing an oil-containing waste film in a wet lithium battery diaphragm;
FIG. 2 is a schematic diagram of the overall structure of another device of the invention dedicated to degreasing the oil-containing waste film in the wet lithium battery separator;
FIG. 3 is a schematic diagram showing the overall structure of an apparatus for removing oil from an oily waste film in a wet lithium battery separator of comparative examples 1 to 11;
in fig. 1: 1. the catalytic combustion device 2, the first condenser, 3, the oil film feed inlet, 4, the extraction kettle, 5, the drying steam valve, 6, the ultrasonic device, 7, the oil film discharge pipe, 8, the filtration and drying integrated tank, 9, the dry film outlet, 10, the filter plate, 11, the spray header, 12, the diaphragm baffle, 13, the extractant recovery valve, 14, the filtrate recovery valve, 15, the upper valve, 16, the extractant recovery pipe, 17, the gas inlet pipe, 18, the mixed liquor drain pipe, 19, the distillation kettle, 20, the mixed liquor drain valve, 21, the rectification tower, 22, the second condenser, 23, the white oil storage tank, 24, the extractant replenishing valve, 25, the extractant storage tank, 26, the extractant delivery pump, 27, the gas outlet pipe, 28, the reflux cleaning integrated pipe, 29, the oil film discharge valve, 30, the liquid outlet pipe, 31, the inverted U-shaped section, 32, the elbow pipe, 33, the lower valve, 34, the reflux pipe, 35, the reflux valve, 36, the cleaning pipe, 37, the cleaning valve, 38, the preassembly pipe, the extractant delivery pipe, 39, the extractant delivery pump, and the extractant delivery pump;
in fig. 2:1. the catalytic combustion device 2, the first condenser, 3, the oil film feed inlet, 4, the extraction kettle, 5, the drying steam valve, 6, the ultrasonic device, 7, the oil film discharge pipe, 8, the filtration and drying integrated tank, 9, the dry film outlet, 10, the filter plate, 11, the spray header, 12, the diaphragm baffle, 13, the extractant recovery valve, 14, the filtrate recovery valve, 15, the upper valve, 16, the extractant recovery pipe, 17, the gas inlet pipe, 18, the mixed liquor drain pipe, 19, the distillation kettle, 20, the mixed liquor drain valve, 21, the rectification tower, 22, the second condenser, 23, the white oil storage tank, 24, the extractant replenishing valve, 25, the extractant storage tank, 26, the extractant delivery pump, 27, the gas outlet pipe, 40, the integral pipe for reflux cleaning of feed liquor, 29, the oil film discharge valve, 30, the liquid outlet pipe, 31, the inverted U-shaped section, 32, the bent pipe, 33, the lower valve, 34, the return pipe, 35, the reflux valve, 41, the feed liquor cleaning pipe, 42, the feed liquor cleaning valve, 38, the extractant delivery pipe, 39 and the extractant delivery pump.
In fig. 3; 43. and (3) an extraction kettle.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1
Referring to fig. 1, fig. 1 is a schematic diagram of the overall structure of a device dedicated for removing oil from an oil-containing waste film in a wet lithium battery separator.
The device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm comprises an extraction kettle 4, a distillation kettle 19, a rectifying tower 21, an extractant storage tank 25 and a white oil storage tank 23, wherein the upper part of the rectifying tower 21 is connected with the extractant storage tank 25, the lower part of the rectifying tower 21 is connected with the white oil storage tank 23, an oil film feeding port 3 is arranged at the upper part of the extraction kettle 4, an oil film discharging pipe 7 with an oil film discharging valve 29 is connected at the bottom of the extraction kettle, a gas inlet pipe 17 and a gas outlet pipe 27 are connected at the upper part of the extraction kettle 4, a reflux cleaning integrated pipe 28 is also connected at the upper part of the extraction kettle 4, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm further comprises a first condenser 2 and a reflux pipe 34, the other end of the gas outlet pipe 27 is connected with the first condenser 2, the first condenser 2 is also connected with the reflux pipe 34, a reflux valve 35 is arranged on the reflux pipe 34, the extractant storage tank 25 is connected with a cleaning pipe 36, the cleaning pipe 36 is provided with a cleaning valve 37, the other ends of the cleaning pipe 36, the return pipe 34 and the reflux cleaning integrated pipe 28 are communicated through a three-way valve, the reflux cleaning integrated pipe 28 is provided with an extractant delivery pump 26, the other end of the gas inlet pipe 17 is connected with the distillation still 19, the bottom of the extraction still 4 is also connected with a liquid outlet pipe 30, the other end of the liquid outlet pipe 30 is connected with the distillation still 19, the liquid outlet pipe 30 is provided with an inverted U-shaped section 31, an upward convex bent pipe 32 is connected between two vertical sections of the inverted U-shaped section 31, the bent pipe 32 is provided with a lower valve 33, the inverted U-shaped section 31 is provided with an upper valve 15, the upper valve 15 is arranged above the lower valve 33, the bottom of the distillation still 19 is connected with a mixed liquor liquid discharge pipe 18, the mixed liquor discharge valve 20 is arranged on the mixed liquor discharge pipe 18, the other end of the mixed liquor discharge pipe 18 is connected with the middle part of the distillation still 21, the distillation still 19 is also connected with an extractant preassembling delivery pipe 38, the other end of the extractant preassembly conveying pipe 38 is connected with the extractant storage tank 25, and an extractant preassembly conveying pump 39 is arranged on the extractant preassembly conveying pipe 38.
Further, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm is also provided with a catalytic combustion device 1, and the catalytic combustion device 1 is used for treating the uncondensed extractant so as not to pollute the environment.
Further, the liquid outlet pipe 30 is connected with an extractant recovery pipe 16, an extractant recovery valve 13 is installed on the extractant recovery pipe 16, and the other end of the extractant recovery pipe 16 is connected with an extractant storage tank 25.
Further, a second condenser 22 is connected between the top of the rectifying tower 21 and the extractant storage tank 25, and the second condenser 22 condenses and recovers the extractant separated from the rectifying tower 21.
Further, an extractant replenishing pipe is connected to the extractant reservoir tank 25, and an extractant replenishing valve 24 is installed in the extractant replenishing pipe to replenish the amount of lost extractant by opening the extractant replenishing valve 24.
Further, the device of the oily waste film deoiling in the wet lithium battery diaphragm is exclusively used in still being provided with and filters integrative jar 8 of stoving, and the oil film discharging pipe 7 other end is connected with integrative jar 8 of filtration stoving, is provided with filter 10 in the integrative jar 8 of filtration stoving, and dry film export 9 has been seted up to filter 10 top, and integrative jar 8 of filtration stoving still is connected with the stoving steam pipe, installs stoving steam valve 5 on the stoving steam pipe, and the stoving steam pipe other end is connected with extraction cauldron 4 upper portion, and integrative jar 8 bottom of filtration stoving is connected with the filtrate recovery pipe, installs filtrate recovery valve 14 on the filtrate recovery pipe, and the filtrate recovery pipe other end is connected with distillation cauldron 19 upper portion. The filtering and drying integrated tank 8 filters oil film and extract liquid and dries oil film surface extractant.
Further, a reflux cleaning integrated pipe 28 extends into the extraction kettle 4, and a spray header 11 is arranged at the end of the reflux cleaning integrated pipe, which is positioned in the extraction kettle 4.
Further, an ultrasonic device 6 is arranged in the extraction kettle 4, and the ultrasonic device 6 is used for promoting the extraction effect.
Further, a diaphragm baffle 12 is arranged in the extraction kettle 4, the diaphragm baffle 12 is arranged near the liquid outlet pipe 30, the diaphragm baffle 12 is of a net structure, and the extraction liquid is filtered, so that an oil film is prevented from blocking the liquid outlet pipe 30.
During operation, the pretreated oily waste film is added into the extraction kettle 4 through the oil film feed port 3 (the ultrasonic device 6 can be opened for auxiliary extraction), a valve on the extraction agent preassembly conveying pipe 38 is opened, the extraction agent is pumped into the distillation kettle 19 (the amount of the pumped extraction agent is about twice the amount of the extraction agent needed by the position of the bent pipe 32 when the liquid level of the extraction kettle 4 reaches the position of the bent pipe 32), the lower valve 33 is opened (the upper valve 15 is closed), the distillation kettle 19 distills the volatile extraction agent under constant power, the extraction agent steam enters the extraction kettle 4 from the distillation kettle 19 and then is condensed back into the extraction kettle 4 through the first condenser 2 to extract the oily waste film, the uncondensed extraction agent is subjected to tail gas treatment through the catalytic combustion device 1 until the liquid level in the extraction kettle 4 reaches the position of the bent pipe 32, the mixed liquid of the extraction liquid and the extracted white oil is dripped into the distillation kettle 19 from the bent pipe 32, and the temperature of the mixed liquid of the extraction liquid and the extracted white oil is equal to the normal temperature or low temperature of the distillation kettle 19, so that the evaporation of the distillation kettle 19 is reduced, the evaporation gas amount of the distillation kettle 19 is reduced, the liquid level of the extraction kettle 4 is lower than the position of the bent pipe 32, the liquid level of the liquid is not required by the distillation kettle 19, and the liquid level of the liquid is not reduced by the weight of the distillation kettle 4, and the liquid is up to be up to about 9%, and the liquid drop of the liquid content of the liquid is up to about 9%, and the liquid drop of the liquid is up to about 9% by weight of the distillation kettle 4, and is more than 9.
And before the last dripping, opening the upper valve 15, closing the lower valve 33, when the liquid level of the extractant in the extraction kettle 4 reaches the position of the previous bent pipe 32, opening the oil film discharging valve 29 on the oil film discharging pipe 7, discharging the extractant and the oil film into the filtering and drying integrated tank 8, opening the cleaning valve 37, and cleaning the residual diaphragm in the extraction kettle 4. In the filtering and drying integrated tank 8, the extraction liquid flows into the lower end through the filter plate 10, the filtered extraction liquid is pumped into the distillation kettle 19, the filtered diaphragm is used for drying and drying the residual extractant on the surface of the diaphragm in the filtering and drying integrated tank 8, and the volatile extractant vapor in the filtering and drying integrated tank 8 is condensed back to the extraction kettle 4 through the first condenser. The oil film discharge valve 29 is closed, and the extractant recovery valve 13 is opened to recover the extractant into the extractant reservoir tank 25. The dried membrane is recovered from the dry film outlet 9. When no condensate in the extraction kettle 4 drops, the mixed liquid drain valve 20 is opened to introduce the residual nonvolatile liquid into the rectifying tower 21, the white oil and the extractant are further separated, the rectified extractant is condensed and recovered by the second condenser 22, and the white oil is discharged into the white oil storage tank 23 from the lower end of the rectifying tower 21.
When the second oil film is extracted, the extractant replenishing valve 24 is opened to replenish lost extractant for the second oil film extraction.
Example 2
Referring to fig. 2, fig. 2 is a schematic diagram of the overall structure of a device dedicated for removing oil from an oil-containing waste film in a wet-process lithium battery separator according to another working mode of the present invention.
The device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm comprises an extraction kettle 4, a distillation kettle 19, a rectifying tower 21, an extractant storage tank 25 and a white oil storage tank 23, wherein the upper part of the rectifying tower 21 is connected with the extractant storage tank 25, the lower part of the rectifying tower 21 is connected with the white oil storage tank 23, an oil film feeding port 3 is arranged at the upper part of the extraction kettle 4, an oil film discharging pipe 7 with an oil film discharging valve 29 is connected at the bottom of the extraction kettle, a gas inlet pipe 17 and a gas outlet pipe 27 are connected at the upper part of the extraction kettle 4, an integral pipe 40 for liquid inlet backflow cleaning is also connected at the upper part of the extraction kettle 4, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm further comprises a first condenser 2 and a backflow pipe 34, the other end of the gas outlet pipe 27 is connected with the first condenser 2, the first condenser 2 is further connected with the backflow pipe 34, a backflow valve 35 is arranged on the backflow pipe 34, the extractant storage tank 25 is connected with a liquid inlet cleaning pipe 41, the liquid inlet cleaning pipe 41 is provided with a liquid inlet cleaning valve 42, the liquid inlet cleaning pipe 41, a return pipe 34 and the other end of the liquid inlet return cleaning integrated pipe 40 are communicated through a three-way valve, the liquid inlet return cleaning integrated pipe 40 is provided with an extractant delivery pump 26, the other end of the gas inlet pipe 17 is connected with the distillation still 19, the bottom of the extraction still 4 is also connected with a liquid outlet pipe 30, the other end of the liquid outlet pipe 30 is connected with the distillation still 19, the liquid outlet pipe 30 is provided with an inverted U-shaped section 31, an upward convex elbow pipe 32 is connected between two vertical sections of the inverted U-shaped section 31, the elbow pipe 32 is provided with a lower valve 33, the inverted U-shaped section 31 is provided with an upper valve 15, the upper valve 15 is arranged above the lower valve 33, the bottom of the distillation still 19 is connected with a mixed liquid discharge pipe 18, the mixed liquid discharge valve 20 is arranged on the mixed liquid discharge pipe 18, the other end of the mixed liquid discharge pipe 18 is connected with the middle part of the distillation still 21, the distillation still 19 is also connected with an extractant preassembling delivery pipe 38, the other end of the extractant preassembly conveying pipe 38 is connected with the extractant storage tank 25, and an extractant preassembly conveying pump 39 is arranged on the extractant preassembly conveying pipe 38.
Further, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm is also provided with a catalytic combustion device 1, and the catalytic combustion device 1 is used for treating the uncondensed extractant so as not to pollute the environment.
Further, the liquid outlet pipe 30 is connected with an extractant recovery pipe 16, an extractant recovery valve 13 is installed on the extractant recovery pipe 16, and the other end of the extractant recovery pipe 16 is connected with an extractant storage tank 25.
Further, a second condenser 22 is connected between the top of the rectifying tower 21 and the extractant storage tank 25, and the second condenser 22 condenses and recovers the extractant separated from the rectifying tower 21.
Further, an extractant replenishing pipe is connected to the extractant reservoir tank 25, and an extractant replenishing valve 24 is installed in the extractant replenishing pipe to replenish the amount of lost extractant by opening the extractant replenishing valve 24.
Further, the device of the oily waste film deoiling in the wet lithium battery diaphragm is exclusively used in still being provided with and filters integrative jar 8 of stoving, and the oil film discharging pipe 7 other end is connected with integrative jar 8 of filtration stoving, is provided with filter 10 in the integrative jar 8 of filtration stoving, and dry film export 9 has been seted up to filter 10 top, and integrative jar 8 of filtration stoving still is connected with the stoving steam pipe, installs stoving steam valve 5 on the stoving steam pipe, and the stoving steam pipe other end is connected with extraction cauldron 4 upper portion, and integrative jar 8 bottom of filtration stoving is connected with the filtrate recovery pipe, installs filtrate recovery valve 14 on the filtrate recovery pipe, and the filtrate recovery pipe other end is connected with distillation cauldron 19 upper portion. The filtering and drying integrated tank 8 filters oil film and extract liquid and dries oil film surface extractant.
Further, an integral liquid inlet reflux cleaning pipe 40 extends into the extraction kettle 4, and a spray header 11 is arranged at the end of the integral liquid inlet reflux cleaning pipe, which is positioned in the extraction kettle 4.
Further, an ultrasonic device 6 is arranged in the extraction kettle 4, and the ultrasonic device 6 is used for promoting the extraction effect.
Further, a diaphragm baffle 12 is arranged in the extraction kettle 4, the diaphragm baffle 12 is arranged near the liquid outlet pipe 30, the diaphragm baffle 12 is of a net structure, and the extraction liquid is filtered, so that an oil film is prevented from blocking the liquid outlet pipe 30.
During operation, the pretreated oily waste film is added into an extraction kettle 4 through an oil film feed port 3 (an ultrasonic device 6 can be opened for auxiliary extraction), a valve on an extractant preassembling conveying pipe 38 is opened, extractant is pumped into a distillation kettle 19 (the amount of the pumped extractant is about 1 time of the amount of the required extractant at the position of a liquid level of the extraction kettle 4 reaching the position of the bent pipe 32), a lower valve 33 is opened (an upper valve 15 is closed), a liquid inlet cleaning valve 42 is opened, extractant is pumped into the extraction kettle 4 (the amount of the pumped extractant is about 1 time of the amount of the required extractant at the position of the liquid level of the extraction kettle 4 reaching the position of the bent pipe 32), the liquid inlet cleaning valve 42 is closed, the distillation kettle 19 distills the volatile extractant under constant power, and extractant steam enters the extraction kettle 4 from the distillation kettle 19 and is condensed back into the extraction kettle 4 through a first condenser 2 to extract the oily waste film, the uncondensed extractant is treated by tail gas through the catalytic combustion device 1 until the liquid level in the extraction kettle 4 reaches the position of the bent pipe 32, the mixed liquor of the extractant and the extracted white oil is dripped into the distillation kettle 19 from the bent pipe 32, the temperature of the mixed liquor of the extractant and the extracted white oil is normal temperature or low temperature because the power of the distillation kettle 19 is unchanged, which is equivalent to cooling the distillation kettle 19, so that the evaporation amount of the distillation kettle 19 becomes small, the liquid level of the extraction kettle 4 is lower than the position of the bent pipe 32, no more liquid is dripped into the distillation kettle 19, the evaporation amount of the distillation kettle 19 is increased until the liquid level of the extraction kettle 4 reaches the position of the bent pipe 32, the next liquid dripping is carried out for 3-10 times, the extraction is completed, and the oil removal rate can reach 90% -99.9% (oil-containing waste film with 70 wt%) oil content.
And before the last dripping, opening the upper valve 15, closing the lower valve 33, when the liquid level of the extractant in the extraction kettle 4 reaches the position of the previous bent pipe 32, opening the oil film discharging valve 29 on the oil film discharging pipe 7, discharging the extractant and the oil film into the filtering and drying integrated tank 8, opening the liquid inlet cleaning valve 42, and cleaning the residual diaphragm in the extraction kettle 4. In the filtering and drying integrated tank 8, the extraction liquid flows into the lower end through the filter plate 10, the filtered extraction liquid is pumped into the distillation kettle 19, the filtered diaphragm is used for drying and drying the residual extractant on the surface of the diaphragm in the filtering and drying integrated tank 8, and the volatile extractant vapor in the filtering and drying integrated tank 8 is condensed back to the extraction kettle 4 through the first condenser. The oil film discharge valve 29 is closed, and the extractant recovery valve 13 is opened to recover the extractant into the extractant reservoir tank 25. The dried membrane is recovered from the dry film outlet 9. When no condensate in the extraction kettle 4 drops, the mixed liquid drain valve 20 is opened to introduce the residual nonvolatile liquid into the rectifying tower 21, the white oil and the extractant are further separated, the rectified extractant is condensed and recovered by the second condenser 22, and the white oil is discharged into the white oil storage tank 23 from the lower end of the rectifying tower 21.
When the second oil film is extracted, the extractant replenishing valve 24 is opened to replenish lost extractant for the second oil film extraction.
Example 2 compared with example 1, half of the extractant is directly added into the extraction kettle 4, so that the energy required by evaporation of the extractant is saved, and the energy consumption is saved.
Example 3
The method comprises the steps of putting an oil-containing waste film (oil content of 70 wt%) produced by a wet method into a diaphragm grinder for grinding, wherein the size of the oil-containing waste film in any direction is 10-15mm.
And placing the crushed diaphragm in a hydraulic press, maintaining the pressure at 10MPa for 5 minutes, and separating the white oil for 1 time, wherein the white oil removal rate is about 15%.
And thirdly, feeding the hydraulic diaphragm into a centrifugal machine, and centrifugally separating the white oil, wherein the white oil removal rate is about 8%.
And (3) drying the membrane after centrifugal separation of the white oil for 30min at 120 ℃, removing surface moisture and reducing viscosity of the white oil to obtain the waste membrane containing oil to be separated later.
The embodiments 4 to 13 of the present invention use the device special for removing oil from the oil-containing waste film in the wet-process lithium battery diaphragm of the embodiment 1 to recycle the oil-containing waste film in the wet-process lithium battery diaphragm.
Examples 4 to 13
Examples 4 to 13 the oily waste films were extracted by the following methods, and examples 4 to 13 were identical except that the extractant was different.
Taking 5kg of the waste oil-containing membrane to be separated in the subsequent process of example 3, adding into an extraction kettle 4, and adding 25L of extractant into a distillation kettle 19.
The distillation still heating temperature is set to the extractant boiling temperature, heating power is maintained unchanged, the extractant is volatilized by condensing and entering the extraction still, and 3-10 times of bent pipe 32 dripping liquid to the distillation still 19 occurs.
The lower valve 33 is closed, the upper valve 15 is opened, when the liquid level of the extraction kettle rises to the height of the bent pipe (namely before the last dripping occurs), an oil film and an extracting agent are discharged into the integrated filtering and drying tank 8 (drying is carried out at 120 ℃ for 30 min), the cleaning valve 37 is opened to clean the residual diaphragm, and the diaphragm in the filtering and drying device is dried.
The mixture liquid in the integrated filtering and drying tank 8 is pumped into the distillation still 19, the oil film discharging valve 29 is closed, the distillation still 19 is continuously heated to separate the mixture of the extractant and the white oil, the extractant recovery valve 13 is opened, and the extractant enters the extractant storage tank 25 from the extractant recovery valve 13 through evaporation and condensation.
And fifthly, discharging the azeotrope left in the distillation kettle 19 into a rectifying tower 21 for further rectifying and separating, recycling the volatilized extractant to an extractant storage tank 25 through a condensing device, and enabling the white oil to enter a white oil storage tank 23.
The results are shown in Table 1 below.
TABLE 1 comparison of oil removal effects for different times of extractions with different extractants
* Extraction 3 times means that the bent tube 32 drops 3 times into the still 19, and so on.
The diaphragms of examples 4-13 from the dry film outlet were observed, and the diaphragms recovered by extraction were free from significant deformation, smooth and clean in surface and oil-free, and excellent in quality.
The following device for removing oil from the oil-containing waste film in the wet lithium battery separator according to comparative examples 1 to 11 is a device for recovering and treating the oil-containing waste film in the wet lithium battery separator according to comparative examples 1 to 11, as shown in fig. 3, and is a conventional extraction rectifying device, and an ultrasonic device and a stirring kettle are arranged in an extraction kettle 43.
Comparative examples 1 to 11
Comparative examples 1 to 11 oily waste films were extracted by the following method, and comparative examples 1 to 11 were identical except that the extractant was different.
Taking 5kg of the oil-containing waste film to be separated in the follow-up process of example 3, adding the waste film into an extraction kettle 43, adding 15L of an extractant into the extraction kettle 43, and stirring and extracting for 10min at normal temperature.
And (5) filtering the extract and an oil film, drying at 120 ℃ for 30min, and removing the residual extractant on the surface of the oil film.
The dried oil film is placed into the extraction kettle 43 again, the process of the oil film is repeated twice, and three-level extraction is completed.
The results are shown in Table 2 below.
And (5) carrying out subsequent processes on the extracted mixed solution and the oil film.
TABLE 2 comparison of oil removal effects for different times of extractions with different extractants
The final membranes (3 times of total filtration and drying) of comparative examples 1-11 from the dry film outlet were observed, and the membranes recovered by extraction had significant deformation and a matte surface.
As can be seen from tables 1-2, under the same extraction agent, the extraction process of the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm has improved oil removal rate compared with the existing extraction process, and under the same extraction process, the mixed extraction agent achieves a synergistic extraction effect.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The method for recovering the oil-containing waste film in the wet lithium battery diaphragm is characterized by comprising the following steps of:
throwing an oily waste film produced by a wet method into a diaphragm crusher for crushing;
placing the crushed diaphragm in a hydraulic press to separate white oil;
feeding the hydraulic diaphragm into a centrifugal machine, and centrifugally separating white oil;
drying the membrane after centrifugal separation of white oil to obtain an oil-containing waste membrane to be separated later;
fifthly, adding the waste oil-containing film to be separated into an extraction kettle, and adding an extractant into a distillation kettle;
heating the distillation kettle until the extractant boils to generate extractant vapor, condensing the vapor into the extraction kettle, and dripping liquid from the extraction kettle to the distillation kettle for 3-10 times;
before the last dropping, filtering and drying the oil film and the extract, and separating the extract and the white oil by distillation and rectification;
the device adopted in the step (a) is a device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm comprises an extraction kettle, a distillation kettle, a rectifying tower, an extractant storage tank and a white oil storage tank, wherein the upper part of the rectifying tower is connected with the extractant storage tank, the lower part of the rectifying tower is connected with the white oil storage tank, an oil film feeding port is formed in the upper part of the extraction kettle, an oil film discharging pipe with an oil film discharging valve is connected at the bottom of the oil film feeding port, a gas inlet pipe and a gas outlet pipe are connected at the upper part of the extraction kettle, a reflux cleaning integrated pipe is also connected at the upper part of the extraction kettle, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm further comprises a first condenser and a reflux pipe, the other end of the gas outlet pipe is connected with the first condenser, the first condenser is also connected with the reflux pipe, and the reflux valve is arranged on the reflux pipe, the extractant storage tank is connected with a cleaning pipe, a cleaning valve is arranged on the cleaning pipe, a return pipe and the other end of a reflux cleaning integrated pipe are communicated through a three-way valve, an extractant conveying pump is arranged on the reflux cleaning integrated pipe, the other end of a gas inlet pipe is connected with a distillation still, the bottom of the extraction still is also connected with a liquid outlet pipe, the other end of the liquid outlet pipe is connected with the distillation still, the liquid outlet pipe is provided with an inverted U-shaped section, an upward convex bent pipe is connected between two vertical sections of the inverted U-shaped section, a lower valve is arranged on the bent pipe, an upper valve is arranged on the inverted U-shaped section, the upper valve is arranged above the lower valve, a mixed liquid drain pipe is connected at the bottom of the distillation still, a mixed liquid drain valve is arranged on the mixed liquid drain pipe, the other end of the mixed liquid drain pipe is connected with the middle part of the distillation still, the other end of the extractant preassembling conveying pipe is connected with the extractant storage tank, the extractant preassembling conveying pipe is provided with an extractant preassembling conveying pump;
the extractant is ethyl acetate and petroleum ether, wherein the ethyl acetate: the volume ratio of petroleum ether is 1-9:1, a step of; or (b)
The extractant is ethyl acetate and cyclohexane, wherein the ethyl acetate: the volume ratio of cyclohexane is 1-9:1, a step of; or (b)
The extractant is ethyl acetate, petroleum ether and cyclohexane, wherein the ethyl acetate: petroleum ether: the volume ratio of cyclohexane is 1-8:1-2:1.
2. the method for recycling the oil-containing waste film in the wet-process lithium battery diaphragm according to claim 1, wherein the device special for removing the oil from the oil-containing waste film in the wet-process lithium battery diaphragm is further provided with a catalytic combustion device.
3. The method for recovering the oil-containing waste film from the wet lithium battery diaphragm according to claim 2, wherein the liquid outlet pipe is connected with an extractant recovery pipe, an extractant recovery valve is installed on the extractant recovery pipe, and the other end of the extractant recovery pipe is connected with an extractant storage tank.
4. The method for recovering oil-containing waste film from wet lithium battery separator according to claim 3, wherein a second condenser is connected between the top of the rectifying tower and the extractant storage tank.
5. The method for recovering the oil-containing waste film from the wet lithium battery diaphragm according to claim 4, wherein the extractant storage tank is connected with an extractant replenishing pipe, and the extractant replenishing pipe is provided with an extractant replenishing valve; the reflux cleaning integrated pipe extends into the extraction kettle, and a spray header is arranged at the end of the reflux cleaning integrated pipe in the extraction kettle.
6. The method for recycling the oil-containing waste film in the wet lithium battery diaphragm according to claim 4, wherein the device special for removing the oil from the oil-containing waste film in the wet lithium battery diaphragm is further provided with a filtering and drying integrated tank, the other end of the oil film discharging pipe is connected with the filtering and drying integrated tank, a filter plate is arranged in the filtering and drying integrated tank, a dry film outlet is formed above the filter plate, the filtering and drying integrated tank is further connected with a drying steam pipe, a drying steam valve is arranged on the drying steam pipe, the other end of the drying steam pipe is connected with the upper part of the extraction kettle, the bottom of the filtering and drying integrated tank is connected with a filtrate recycling pipe, a filtrate recycling valve is arranged on the filtrate recycling pipe, and the other end of the filtrate recycling pipe is connected with the upper part of the distillation kettle.
7. The method for recovering the oil-containing waste film from the wet lithium battery diaphragm according to claim 4, wherein the ultrasonic device and the diaphragm baffle are installed in the extraction kettle, the diaphragm baffle is installed at the position close to the liquid outlet pipe, and the diaphragm baffle is of a net-shaped structure.
8. The method for recovering the oil-containing waste film in the wet lithium battery diaphragm is characterized by comprising the following steps of:
throwing an oily waste film produced by a wet method into a diaphragm crusher for crushing;
placing the crushed diaphragm in a hydraulic press to separate white oil;
feeding the hydraulic diaphragm into a centrifugal machine, and centrifugally separating white oil;
drying the membrane after centrifugal separation of white oil to obtain an oil-containing waste membrane to be separated later;
fifthly, adding the waste oil-containing film to be separated into an extraction kettle, and adding an extractant into a distillation kettle;
heating the distillation kettle until the extractant boils to generate extractant vapor, condensing the vapor into the extraction kettle, and dripping liquid from the extraction kettle to the distillation kettle for 3-10 times;
before the last dropping, filtering and drying the oil film and the extract, and separating the extract and the white oil by distillation and rectification;
the device adopted in the step (a) is a device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm comprises an extraction kettle, a distillation kettle, a rectifying tower, an extractant storage tank and a white oil storage tank, wherein the upper part of the rectifying tower is connected with the extractant storage tank, the lower part of the rectifying tower is connected with the white oil storage tank, an oil film feeding port is formed in the upper part of the extraction kettle, an oil film discharging pipe with an oil film discharging valve is connected at the bottom of the oil film feeding port, a gas inlet pipe and a gas outlet pipe are connected at the upper part of the extraction kettle, an integral pipe for backflow and cleaning of liquid inlet is also connected at the upper part of the extraction kettle, the device special for removing oil from the oil-containing waste film in the wet lithium battery diaphragm further comprises a first condenser and a backflow pipe, the other end of the gas outlet pipe is connected with the first condenser, the first condenser is also connected with the backflow pipe, a backflow valve is arranged on the backflow pipe, the extractant storage tank is connected with a liquid inlet cleaning pipe, the liquid inlet cleaning pipe is provided with a liquid inlet cleaning valve, the other ends of the liquid inlet cleaning pipe, the return pipe and the liquid inlet return cleaning integrated pipe are communicated through a three-way valve, the liquid inlet return cleaning integrated pipe is provided with an extractant conveying pump, the other end of the gas inlet pipe is connected with a distillation still, the bottom of the extraction still is also connected with a liquid outlet pipe, the other end of the liquid outlet pipe is connected with the distillation still, the liquid outlet pipe is provided with an inverted U-shaped section, an upward convex bent pipe is connected between two vertical sections of the inverted U-shaped section, a lower valve is arranged on the bent pipe, an upper valve is arranged on the inverted U-shaped section, the upper valve is arranged above the lower valve, the bottom of the distillation still is connected with a mixed liquid discharge pipe, the mixed liquid discharge pipe is provided with a mixed liquid discharge valve, the other end of the mixed liquid discharge pipe is connected with the middle part of the distillation still, the other end of the extractant preassembling conveying pipe is connected with an extractant storage tank, the extractant preassembling conveying pipe is provided with an extractant preassembling conveying pump;
the extractant is ethyl acetate and petroleum ether, wherein the ethyl acetate: the volume ratio of petroleum ether is 1-9:1, a step of; or (b)
The extractant is ethyl acetate and cyclohexane, wherein the ethyl acetate: the volume ratio of cyclohexane is 1-9:1, a step of; or (b)
The extractant is ethyl acetate, petroleum ether and cyclohexane, wherein the ethyl acetate: petroleum ether: the volume ratio of cyclohexane is 1-8:1-2:1.
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