CN213924578U - Dichloromethane recovery device in production process of wet lithium battery diaphragm - Google Patents

Dichloromethane recovery device in production process of wet lithium battery diaphragm Download PDF

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CN213924578U
CN213924578U CN202022450019.XU CN202022450019U CN213924578U CN 213924578 U CN213924578 U CN 213924578U CN 202022450019 U CN202022450019 U CN 202022450019U CN 213924578 U CN213924578 U CN 213924578U
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tower
dichloromethane
atmospheric
reboiler
refining
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魏明
白耀宗
张富成
刘杲珺
周阳
陈淳
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Sinoma Lithium Film Co Ltd
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Sinoma Lithium Film Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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Abstract

The utility model discloses a dichloromethane recovery unit in wet process lithium battery diaphragm production process, it includes pressurization refining tower, ordinary pressure refining tower, top of the tower condenser, dichloromethane layering jar, dichloromethane condensate pump, dichloromethane backwash pump and waste water treatment device. By utilizing double-effect rectification and condensate layering separation technology, a new energy-saving process for separating and recovering the extraction mixed liquid dichloromethane is established. The tower top steam enters a tower top condenser for condensation and then enters a dichloromethane layering tank for layering separation; wastewater overflows into wastewater treatment equipment, and high-purity dichloromethane is discharged through a liquid level control system to realize the recycling of the dichloromethane. The utility model discloses it is high to the mixed liquid dichloromethane recovery efficiency of extraction, the system energy consumption is low, and it is high to retrieve dichloromethane finished product purity, has reduced diaphragm manufacturing cost, and product competitiveness obtains promoting.

Description

Dichloromethane recovery device in production process of wet lithium battery diaphragm
Technical Field
The utility model relates to a wet process lithium battery diaphragm production technical field specifically is energy-conserving new technology of waste liquid recovery in the wet process lithium battery diaphragm production process, makes the mixed liquid rectification piece-rate system energy consumption of extraction reduce by 30% more, and energy-conserving effect is showing, retrieves dichloromethane purity and is greater than 99.9%, effectively reduces lithium battery diaphragm manufacturing cost, has promoted product competitiveness.
Background
The lithium ion battery diaphragm has the functions of insulating the positive electrode and the negative electrode to prevent short circuit, enabling lithium ions to freely pass through, and preventing the positive electrode and the negative electrode from contacting through a hole closing function under the condition of overcharge or temperature rise to achieve the insulating function; the capacity, the cycle performance, the charge-discharge current density and other key performances of the lithium battery can be influenced. The production process flow of the wet lithium ion battery diaphragm roughly comprises the following steps: feeding and proportioning, extruding and plasticizing, casting sheet cooling, biaxial stretching, extracting and drying, traction trimming, rolling and inspection, slitting and packaging. In the production process of the diaphragm, white oil serving as a pore-forming agent is uniformly distributed in a molecular chain, dichloromethane serving as an extraction liquid in an extraction process extracts the pore-forming agent white oil, separation of the white oil in the diaphragm is realized, and the diaphragm forms a compact and uniform microporous structure. The extraction process produces extraction mixture liquid with main components of dichloromethane, white oil and small amount of water. In the existing wet-process lithium battery diaphragm production process, the recovery rate of the extraction mixed liquid is low, the energy consumption of a rectification system is high, the purity of the recovered solvent is low, the diaphragm production cost is directly high, and the product competitiveness is reduced.
SUMMERY OF THE UTILITY MODEL
In order to solve the problem, the utility model provides a new energy-saving process for recovering methylene dichloride of a wet lithium battery diaphragm, the principle and the flow of which are shown in the attached drawing of the specification. The separation of the dichloromethane is completed by two towers, namely a pressurized refining tower and an atmospheric refining tower, and the tower top steam of the pressurized refining tower is used as a heat source of a first reboiler of the atmospheric refining tower to recover the condensation latent heat of the tower top steam, thereby achieving the purposes of energy conservation and consumption reduction. Meanwhile, the condensed liquid-phase dichloromethane enters a dichloromethane layering tank to separate and discharge wastewater, so that the high-purity output of dichloromethane finished products can be effectively realized.
The utility model discloses at first, dichloromethane recovery unit in wet process lithium battery diaphragm production process, it includes pressurization refining tower, ordinary pressure refining tower, top of the tower condenser, dichloromethane layering jar, dichloromethane condensate pump, dichloromethane pans, dichloromethane delivery pump, dichloromethane backwash pump, waste water treatment equipment, wherein:
extracting mixed liquor from an extraction tank of a lithium battery diaphragm production device is respectively sent into a pressurizing refining tower and a normal-pressure refining tower, tower top steam of the pressurizing refining tower and tower top steam of the normal-pressure refining tower are mixed and then jointly enter a tower top condenser, a liquid-phase dichloromethane solvent enters a dichloromethane layering tank after condensation and cooling, and the liquid-phase dichloromethane solvent is layered and separated into a wastewater layer and a dichloromethane layer in the dichloromethane layering tank;
through the liquid level control of the dichloromethane layering tank, the layered wastewater is discharged into the wastewater treatment equipment, and the layered liquid-phase dichloromethane is pumped into the dichloromethane intermediate tank by the dichloromethane condensate pump;
a part of liquid-phase dichloromethane in the dichloromethane intermediate tank is pumped out by the dichloromethane output pump, so that dichloromethane is recycled; the other part is pumped out by the dichloromethane reflux pump and respectively enters the pressurizing refining tower and the normal pressure refining tower to realize reflux.
Preferably, the top of the tower top condenser is filled with uncondensed gas, the top of the methylene dichloride layering tank is filled with uncondensed gas and the top of the methylene dichloride intermediate tank is filled with uncondensed gas, the uncondensed gas is discharged through a pipeline, and the three uncondensed gas outer discharge pipelines are connected into the same waste gas pipeline and connected into the gas recovery system.
Preferably, the pipelines returned to the pressure refining tower and the atmospheric refining tower are provided with flow meters and regulating valve devices, so that the return flow rates fed into the pressure refining tower and the atmospheric refining tower can be respectively regulated.
Preferably, the pressurized refining tower is connected with a pressurized tower reboiler for heating; the pressurized tower reboiler uses low pressure steam as a heat source, and the heat required by the pressurized tower reboiler is realized by adjusting the amount of the low pressure heating steam introduced into the pressurized tower reboiler.
Preferably, the atmospheric refining tower is connected with a first reboiler of the atmospheric tower and a second reboiler of the atmospheric tower, the first reboiler of the atmospheric tower is connected with the top of the pressurized refining tower, and the tower top steam of the pressurized refining tower enters the first reboiler of the atmospheric tower to be used as a heat source; the second reboiler of the atmospheric tower uses low-pressure steam as a heat source, and the heat required at the bottom of the atmospheric refining tower is realized by adjusting the amount of low-pressure heating steam introduced into the second reboiler of the atmospheric tower.
Preferably, the tower bottoms of the pressurized refining tower and the atmospheric refining tower are sent to a second reboiler of the atmospheric tower for further evaporation, and the tower bottoms of the second reboiler of the atmospheric tower are pumped out by the crude white oil sending pump and enter the white oil rectification system.
Preferably, the extraction mixed liquor is sent into the pressurization refining tower through a pressurization tower charging pump, the extraction mixed liquor is sent into the normal pressure refining tower through a normal pressure tower charging pump, the pressurization tower charging pump and the normal pressure tower charging pump are frequency conversion horizontal gear pumps, and the conveying capacity is adjusted through a PLC control system.
The utility model also discloses a dichloromethane recovery method in wet process lithium cell diaphragm production process, it includes following step:
-feeding the extraction mixture from the extraction tank of the lithium battery diaphragm production plant into a pressurized refining tower and a normal pressure refining tower, respectively;
-the top steam of the pressurized refining tower is mixed with the top steam of the atmospheric refining tower and then is cooled and condensed;
-the liquid phase dichloromethane solvent is separated into a wastewater layer and a dichloromethane layer by layering after condensation and cooling;
discharging the layered wastewater into the wastewater treatment equipment, and pumping the layered liquid-phase dichloromethane into a dichloromethane intermediate tank;
pumping out a part of liquid-phase dichloromethane in the dichloromethane intermediate tank by a dichloromethane output pump to realize dichloromethane recycling; the other part is pumped out by a methylene dichloride reflux pump and respectively enters the pressurizing refining tower and the normal pressure refining tower to realize reflux.
Specifically, the method comprises the following steps:
the technological parameters of the pressurized refining tower are as follows: the operation pressure is 260-300 kpa, the temperature of the top steam is 68-73 ℃, the temperature of the bottom steam is 90-110 ℃, the rectification reflux ratio is 0.2-0.4, and the number of theoretical plates is more than 12.
The technological parameters of the normal pressure refining tower are as follows: the operation pressure is 90-115 kpa, the temperature of the top steam is 35-40 ℃, the temperature of the bottom of the tower is 42-48 ℃, the rectification reflux ratio is 0.1-0.3, and the number of theoretical plates is more than 10.
Specifically, the method comprises the following steps:
the pressurized refining tower is connected with a pressurized tower reboiler for heating; the heat required by the reboiler of the pressurizing tower is realized by adjusting the amount of low-pressure heating steam introduced into the reboiler of the pressurizing tower; the heating temperature of a reboiler of the pressurizing tower is 135-142 ℃;
the normal pressure refining tower is connected with a first reboiler of the normal pressure tower and a second reboiler of the normal pressure tower, the first reboiler of the normal pressure tower is connected with the top of the pressurizing refining tower, and tower top steam of the pressurizing refining tower enters the first reboiler of the normal pressure tower to be used as a heat source; the heat required by the tower bottom of the normal pressure refining tower is realized by adjusting the amount of low-pressure heating steam introduced into a second reboiler of the normal pressure tower; the heating temperature of the second reboiler of the atmospheric tower is 135-142 ℃.
The beneficial effects of the utility model
The utility model provides a dichloromethane recovery unit and method in wet process lithium cell diaphragm production process utilizes economic benefits and social benefits rectification and condensate layering separation technique, has established the new technology of extraction mixed liquid dichloromethane separation recovery energy-conservation.
The tower top steam enters a tower top condenser for condensation and then enters a dichloromethane layering tank for layering separation; wastewater overflows into wastewater treatment equipment, and high-purity dichloromethane is discharged through a liquid level control system to realize the recycling of the dichloromethane.
The separation of the dichloromethane is completed by 2 towers of a pressurized refining tower and an atmospheric refining tower, and the top steam of the pressurized refining tower is used as a heat source of a first reboiler of the atmospheric refining tower to recover the condensation latent heat of the top steam of the pressurized refining tower, thereby achieving the purposes of energy conservation and consumption reduction.
The utility model discloses make rectifying system energy consumption reduce by 30% more, energy-conserving effect is showing, retrieves the dichloromethane purity and is greater than 99.9%, has reduced unfamiliar manufacturing cost, and product competitiveness obtains promoting.
Drawings
Fig. 1 is the utility model relates to a wet process lithium cell diaphragm dichloromethane retrieves economizer schematic diagram.
Wherein: 1-pressurizing refining tower, 2-atmospheric refining tower, 3-pressurizing tower charging pump, 4-atmospheric tower charging pump, 5-pressurizing tower reboiler, 6-atmospheric tower first reboiler, 7-atmospheric tower second reboiler, 8-tower top condenser, 9-dichloromethane layering tank, 10-dichloromethane condensate pump, 11-dichloromethane intermediate tank, 12-dichloromethane output pump, 13-dichloromethane reflux pump, 14-crude white oil delivery pump, 15 white oil rectification system, 16-gas recovery and 17-wastewater treatment equipment.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Aiming at 1.2 million square meter lithium film production equipment produced by xx lithium battery diaphragm company every year, the extraction mixed liquid material discharged by extraction process equipment comprises the following components: 94-96 wt% of dichloromethane, 4-6 wt% of white oil and a small amount of water, wherein the annual production time is 8000 hours, the temperature of the extraction mixed liquor is 20-23 ℃, the design treatment capacity of the extraction liquid rectification recovery equipment is 40t/h, and the product purity is as follows: 99.9 wt% methylene chloride. The process of the utility model is shown in the attached figure 1 of the specification: the system comprises a pressurized refining tower 1, an atmospheric refining tower 2, a pressurized tower charging pump 3, an atmospheric tower charging pump 4, a pressurized tower reboiler 5, an atmospheric tower first reboiler 6, an atmospheric tower second reboiler 7, a tower top condenser 8, a dichloromethane layering tank 9, a dichloromethane condensate pump 10, a dichloromethane intermediate tank 11, a dichloromethane output pump 12, a dichloromethane reflux pump 13, a crude white oil delivery pump 14, a white oil rectification system 15, a gas recovery system 16 and a wastewater treatment device 17. The extraction mixed liquid from the extraction tank of the lithium battery diaphragm production device is pumped into the pressurizing and refining tower 1 by the pressurizing tower charging pump 3, the kettle of the pressurizing and refining tower 1 is heated by the pressurizing tower reboiler 5, the pressurizing tower reboiler 5 uses low-pressure steam as a heat source, the heat required by the pressurizing tower reboiler 5 is realized by adjusting the amount of the low-pressure heating steam introduced into the pressurizing tower reboiler 5, and the high-temperature overhead steam of the pressurizing and refining tower 1 enters the first reboiler 6 of the normal pressure tower to be used as the heat source to recover the condensation latent heat of the high-temperature overhead steam. The other path of extraction mixed liquid from an extraction tank of a lithium battery diaphragm production device is pumped into the normal pressure refining tower 2 by the normal pressure tower charging pump 4, the normal pressure refining tower 2 is provided with 2 reboilers which are a normal pressure tower first reboiler 6 and a normal pressure tower second reboiler 7 respectively, the normal pressure tower first reboiler 6 uses the high temperature overhead vapor of the pressurized refining tower 1 as a heat source to recover the vaporization latent heat of the overhead vapor, the normal pressure tower first reboiler can be used as a condenser of the pressurized refining tower, the normal pressure tower second reboiler 7 uses low pressure vapor as a heat source, the heat required at the bottom of the normal pressure refining tower 2 is realized by adjusting the low pressure heating vapor amount led into the normal pressure tower second reboiler 7, and the normal pressure refining tower realizes double-effect distillation by using the overhead vapor separated by the pressurized refining tower as a heat source, and the tower bottom liquid of the pressurized refining tower 1 and the tower bottom liquid of the atmospheric refining tower 2 are sent to the atmospheric tower second reboiler 7 for further evaporation, the evaporated gas-phase dichloromethane returns to the atmospheric rectifying tower, and the tower bottom liquid evaporated by the atmospheric tower second reboiler 7 is pumped into a white oil rectifying system 15 by the crude white oil delivery pump 14 for further separation. Gas-phase dichloromethane is extracted from tower plates at the tops of the pressurized refining tower 1 and the normal-pressure refining tower 2, high-temperature tower top steam of the pressurized refining tower 1 enters the first reboiler 6 of the normal-pressure tower to realize heat exchange, then is mixed with the tower top steam of the normal-pressure refining tower 2 and then jointly enters the tower top condenser 8, liquid-phase dichloromethane solvent enters the dichloromethane layering tank 9 after condensation and cooling, and the liquid-phase dichloromethane solvent in the dichloromethane layering tank 9 is layered into a wastewater layer and a dichloromethane layer. Through the liquid level control system of the dichloromethane layering tank 9, the layered wastewater enters the wastewater treatment equipment 17, and the layered liquid dichloromethane is pumped into the dichloromethane intermediate tank 11 by the dichloromethane condensate pump 10 to be stored. And one part of the dichloromethane intermediate tank 11 liquid-phase dichloromethane is pumped out by the dichloromethane output pump 12 to realize the recycling of dichloromethane, and the other part of the dichloromethane intermediate tank 11 liquid-phase dichloromethane is pumped out by the dichloromethane reflux pump 13 to respectively enter the pressurizing and refining tower 1 and the normal-pressure refining tower 2 to realize reflux re-rectification. The pipelines which flow back to the pressure refining tower 1 and the normal pressure refining tower 2 are provided with a flow meter and a regulating valve device which can respectively regulate the flow back which is pumped into the pressure refining tower 1 and the normal pressure refining tower 2. The top of the tower condenser 8 is not condensed gas, the dichloromethane layering tank 9 is not condensed gas and the dichloromethane intermediate tank 11 is not condensed gas are extracted through pipelines, and the three non-condensed gas external discharge pipelines are connected into the same waste gas pipeline and are connected into the gas recovery system for treatment 16.
The technological parameters of the pressurized refining tower 1 are as follows: the technological parameters of the pressurized refining tower 1 are as follows: the operating pressure is 260-300 kpa, the temperature of the steam at the top of the tower is 68-73 ℃, the temperature at the bottom of the tower is 90-110 ℃, the heating temperature of a reboiler of a pressurizing tower is 135-142 ℃, the rectification reflux ratio is 0.2-0.4, and the number of theoretical plates is more than 12.
The technological parameters of the atmospheric refining tower 2 are as follows: the operating pressure is 90-115 kpa, the temperature of the top steam is 35-40 ℃, the temperature of the bottom of the tower is 42-48 ℃, the heating temperature of a second reboiler 7 of the atmospheric tower is 135-142 ℃, the rectification reflux ratio is 0.1-0.3, and the number of theoretical plates is more than 10.
Compared with the traditional process, the novel energy-saving process for recovering the dichloromethane by utilizing the double-effect rectification and the layered separation of the condensate reduces the consumption of saturated steam of a dichloromethane recovery system from 7.1 ton/h to 4.6 ton/h, saves energy by 2.5 ton/h, achieves the energy-saving rate of 35 percent and saves the saturated steam by 1.98 ten thousand ton/year; in addition, the consumption of the circulating cooling water of the system is reduced to 360 tons/hour from 480 tons/hour, the consumption of the circulating cooling water is reduced by 120 tons/hour, the energy saving rate reaches 25 percent, and the cooling water is saved by 95 ten thousand tons/year.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications, additions and substitutions for the specific embodiments described herein may be made by those skilled in the art without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.

Claims (7)

1. The utility model provides a dichloromethane recovery unit in wet process lithium cell diaphragm production process, it includes pressurization refining tower (1), ordinary pressure refining tower (2), overhead condenser (8), dichloromethane layering jar (9), dichloromethane condensate pump (10), dichloromethane pans (11), dichloromethane delivery pump (12), dichloromethane reflux pump (13), waste water treatment equipment (17) its characterized in that, wherein:
extracting mixed liquor from an extraction tank of a lithium battery diaphragm production device is respectively sent into a pressurizing refining tower (1) and a normal-pressure refining tower (2), tower top steam of the pressurizing refining tower (1) and tower top steam of the normal-pressure refining tower (2) are mixed and then jointly sent into a tower top condenser (8), a liquid-phase dichloromethane solvent enters a dichloromethane layering tank (9) after condensation and cooling, and the liquid-phase dichloromethane solvent is layered and separated into a wastewater layer and a dichloromethane layer in the dichloromethane layering tank (9);
the liquid level of the dichloromethane layering tank (9) is controlled, the layered wastewater is discharged into the wastewater treatment equipment (17), and the layered liquid-phase dichloromethane is pumped into the dichloromethane intermediate tank (11) by the dichloromethane condensate pump (10);
a part of liquid-phase dichloromethane in the dichloromethane intermediate tank (11) is pumped out by the dichloromethane output pump (12), so that dichloromethane is recycled; the other part of the mixture is pumped out by the dichloromethane reflux pump (13) and respectively enters the pressurizing refining tower (1) and the normal pressure refining tower (2) to realize reflux.
2. The device according to claim 1, characterized in that the uncondensed gas at the top of the overhead condenser (8), the uncondensed gas at the top of the methylene dichloride layering tank (9) and the uncondensed gas at the top of the methylene dichloride intermediate tank (11) are discharged through pipelines, and the three uncondensed gas outer discharge pipelines are connected to the same waste gas pipeline and connected to a gas recovery system (16).
3. The apparatus according to claim 1, wherein the pipes leading back to the pressure refining tower (1) and the atmospheric refining tower (2) are provided with flow meters and regulating valve devices for regulating the amount of reflux to the pressure refining tower (1) and the atmospheric refining tower (2), respectively.
4. The apparatus according to claim 1, wherein the pressurized refining column (1) is connected to a pressurized column reboiler (5) for heating; the pressurizing tower reboiler (5) uses low-pressure steam as a heat source, and the heat required by the pressurizing tower reboiler (5) is realized by adjusting the amount of the low-pressure heating steam introduced into the pressurizing tower reboiler (5).
5. The device according to claim 1, characterized in that the atmospheric tower (2) is connected with a first reboiler (6) of the atmospheric tower and a second reboiler (7) of the atmospheric tower, the first reboiler (6) of the atmospheric tower is connected with the top of the pressurized refining tower (1), and the overhead vapor of the pressurized refining tower (1) enters the first reboiler (6) of the atmospheric tower as a heat source; the second reboiler (7) of the atmospheric tower uses low-pressure steam as a heat source, and the heat required at the bottom of the atmospheric refining tower (2) is realized by adjusting the amount of the low-pressure heating steam introduced into the second reboiler (7) of the atmospheric tower.
6. The device according to claim 5, characterized in that the bottoms of the pressurized refining tower (1) and the atmospheric refining tower (2) are sent to the second reboiler (7) of the atmospheric tower for further evaporation, and the bottoms of the second reboiler (7) of the atmospheric tower are pumped out by the crude white oil sending pump (14) to enter the white oil rectification system (15).
7. The device according to claim 1, characterized in that the extraction mixture is fed into the pressurized refining tower (1) through a pressurized tower feed pump (3), the extraction mixture is fed into the atmospheric refining tower (2) through an atmospheric tower feed pump (4), the pressurized tower feed pump (3) and the atmospheric tower feed pump (4) are variable frequency horizontal gear pumps, and the conveying capacity is adjusted through a PLC control system.
CN202022450019.XU 2020-10-29 2020-10-29 Dichloromethane recovery device in production process of wet lithium battery diaphragm Active CN213924578U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112174773A (en) * 2020-10-29 2021-01-05 中材锂膜有限公司 Dichloromethane recovery device and method in wet lithium battery diaphragm production process

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112174773A (en) * 2020-10-29 2021-01-05 中材锂膜有限公司 Dichloromethane recovery device and method in wet lithium battery diaphragm production process

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