[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

WO2021082448A1 - Apparatus for ultrasonic wave-assisted drying of lithium battery electrolyte, and drying method - Google Patents

Apparatus for ultrasonic wave-assisted drying of lithium battery electrolyte, and drying method Download PDF

Info

Publication number
WO2021082448A1
WO2021082448A1 PCT/CN2020/094587 CN2020094587W WO2021082448A1 WO 2021082448 A1 WO2021082448 A1 WO 2021082448A1 CN 2020094587 W CN2020094587 W CN 2020094587W WO 2021082448 A1 WO2021082448 A1 WO 2021082448A1
Authority
WO
WIPO (PCT)
Prior art keywords
drying
lithium battery
ultrasonic
battery electrolyte
temperature
Prior art date
Application number
PCT/CN2020/094587
Other languages
French (fr)
Chinese (zh)
Inventor
梁海波
黎小琼
陈志强
谢文健
陈新滋
Original Assignee
广州理文科技有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 广州理文科技有限公司 filed Critical 广州理文科技有限公司
Priority to PCT/CN2020/094587 priority Critical patent/WO2021082448A1/en
Priority to CN202080005190.XA priority patent/CN112739971A/en
Publication of WO2021082448A1 publication Critical patent/WO2021082448A1/en

Links

Images

Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00—Drying solid materials or objects by processes not involving the application of heat
    • F26B5/02—Drying solid materials or objects by processes not involving the application of heat by using ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/14—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects using gases or vapours other than air or steam, e.g. inert gases
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B23/00—Heating arrangements
    • F26B23/10—Heating arrangements using tubes or passages containing heated fluids, e.g. acting as radiative elements; Closed-loop systems
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00—Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B9/00—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards
    • F26B9/06—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards in stationary drums or chambers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention belongs to the field of lithium battery electrolyte drying, in particular to a device and a drying method for assisting the drying of lithium battery electrolyte by ultrasonic waves.
  • Lithium-ion secondary batteries have the advantages of high voltage, large specific energy, long cycle life, stable discharge performance, and good safety. Therefore, they have developed rapidly in recent years and have broad application prospects.
  • Lithium-ion secondary batteries are mainly composed of cathode materials, carbon anode materials and electrolyte.
  • the electrolyte mainly includes organic solvents and electrolytes.
  • the electrolyte must have the advantages of high conductivity, good chemical and electrochemical stability, wide usable temperature range, and good safety. The improvement of electrochemical performance of electrolyte in lithium battery will greatly improve the performance of lithium ion battery.
  • the current domestic lithium battery electrolytes generally have the problem of high moisture content.
  • moisture has a crucial impact on the performance of lithium-ion batteries.
  • High moisture will cause the decomposition of lithium salts in the electrolyte and affect the positive and negative electrodes.
  • the material and aluminum foil have a certain corrosive effect, which causes the battery capacity to decrease and attenuate, the discharge time becomes shorter, the internal resistance increases, and the battery swells, which causes the battery's performance to drop rapidly.
  • the traditional method of heating and vacuum drying is mainly used in the industry to dehydrate the lithium battery electrolyte.
  • This kind of baking and vacuuming method has high drying energy consumption, low efficiency and high drying temperature. The high temperature causes the decomposition of the lithium battery electrolyte, which affects the quality of the lithium battery electrolyte.
  • Ultrasonic waves are sound waves with a frequency ⁇ 20kHz. Ultrasonic waves have the characteristics of strong propagation direction and large vibration acceleration of medium particles. Ultrasound has a variety of physical and chemical effects. The interaction between ultrasound and media can be divided into three types: thermal mechanism, mechanical mechanism, and cavitation mechanism. Ultrasound is directly and effectively coupled to the process of vacuum heating and drying of the lithium battery electrolyte, and the powerful shock wave, micro jet and thermal effect generated by the cavitation of the ultrasonic wave can be used to realize the heat and mass transfer process of the lithium battery electrolyte during the vacuum drying process. Strengthen, and achieve the purpose of shortening the drying time, lowering the drying temperature, and improving the drying efficiency, which can achieve energy-saving effects and reduce the burden on enterprises.
  • the technical problem to be solved by the present invention is to propose an ultrasonic assisted drying device and drying method for lithium battery electrolyte that can shorten the drying time, lower the drying temperature, and improve the drying efficiency .
  • An ultrasonic-assisted device for drying lithium battery electrolyte and a drying method including a temperature-controlled heating water bath, an ultrasonic system, and a vacuum pump. There are heating rods and thermocouples in the temperature-controlled heating water bath. An ultrasonic vibrator is arranged at the bottom of the temperature-controlled heating water bath, and the ultrasonic vibrator is connected with the ultrasonic generator. The vacuum pump is connected to the drying flask through a pipeline, and the connection port adopts a flange interface design. An on-off valve and a vent valve are sequentially arranged in the pipeline, and a vacuum gauge is set between the on-off valve and the flange interface. The vacuum pump is located between the on-off valve and the vent valve.
  • the temperature-controlled heating water bath is provided with a heating rod and a thermocouple.
  • the bottom of the temperature-controlled heating water bath is provided with an ultrasonic vibrator, and the ultrasonic vibrator is connected with the ultrasonic generator.
  • the vacuum pump is connected to the drying flask through a pipeline, and the connection port adopts a flange interface design.
  • a further solution an on-off valve and a vent valve are arranged in the pipeline in sequence, and a vacuum gauge is arranged between the on-off valve and the flange interface.
  • the vacuum pump is located between the on-off valve and the vent valve.
  • Another object of the present invention is to provide an ultrasonic-assisted device and drying method for drying lithium battery electrolyte, including the following steps:
  • the drying flask is connected to the vacuum pump pipeline through the flange interface. Turn on the vacuum pump, on-off valve and vent valve to perform vacuum processing and adjust the vacuum degree;
  • the temperature control range of the water bath in step 1 is 25-90°C.
  • the vacuum degree of step 2 ranges from 4 to 250 torr.
  • the working parameters of the ultrasonic generator in step 3 are working time of 5 to 240 min, working power of 1 to 20 kW, and ultrasonic frequency of 20 to 80 kHz.
  • the room temperature range to be reached in the step 4 for cooling is 25-35°C.
  • the inert gas in step 5 is one or more combinations of nitrogen, argon, neon, helium, and carbon dioxide.
  • the steps 3 to 4 can be a single batch cycle process. According to the water content of the lithium battery electrolyte and the water removal efficiency, the number of this cycle process can be 2-100 times.
  • the present invention addresses the problems of large energy consumption, low efficiency, and high drying temperature in the existing traditional heating and vacuum drying method, and proposes an ultrasonic assisted drying device and drying method for lithium battery electrolyte.
  • the powerful shock waves and micro jets generated by ultrasonic waves through cavitation can make the water disperse more evenly in the lithium battery electrolyte, and it can also cause internal friction on the internal particles of the lithium battery electrolyte, thereby forming inside the lithium battery electrolyte that is conducive to the diffusion of water molecules.
  • the tiny channel combined with the heating and vacuuming process, promotes the transportation of water molecules to the outside of the system.
  • this method can shorten the drying time and improve the drying efficiency
  • this method can reduce the drying temperature and prevent the lithium battery electrolyte from decomposing due to excessive temperature.
  • FIG. 1 is a schematic diagram of the structure of an ultrasonic-assisted drying device of lithium battery electrolyte according to the present invention
  • a device and a drying method for assisting the drying of lithium battery electrolyte by ultrasound include a temperature-controlled heating water bath (1), an ultrasonic system, and a vacuum pump (8).
  • a heating rod (3) and a thermocouple (2) are arranged in the temperature-controlled heating water bath (1).
  • An ultrasonic vibrator (4) is arranged at the bottom of the temperature-controlled heating water bath (1), and the ultrasonic vibrator (4) is connected with the ultrasonic generator (5).
  • the vacuum pump (8) is connected with the drying flask through a pipeline, and the connection port is designed with a flange interface (6).
  • An on-off valve (9) and a vent valve (10) are sequentially arranged in the pipeline, and a vacuum gauge (7) is arranged between the on-off valve (9) and the flange interface (6).
  • the vacuum pump (8) is located between the on-off valve (9) and the vent valve (10).
  • An ultrasonic-assisted device for drying lithium battery electrolyte and a drying method specifically include the following steps: 1Start a temperature-controlled heating water bath to heat the electric heating rod, and adjust the thermocouple parameters to control the temperature of the water bath to 80°C. 2After the water bath is basically constant temperature to the setting, transfer 10Kg of the lithium battery electrolyte (water content ⁇ 5000ppm) to be dried into the drying bottle.
  • the drying flask is connected to the vacuum pump pipeline through the flange interface. Turn on the vacuum pump, on-off valve and vent valve to perform vacuum processing, and adjust the vacuum to 7torr. 3Turn on the ultrasonic generator, and work continuously for 120min at a power of 10kW and a frequency of 35kHz.
  • the water content of the lithium battery electrolyte is 28.3ppm, which takes 120 minutes; under the same conditions, the water content of the lithium battery electrolyte reaches 28.3ppm, and the traditional heating and vacuum drying method takes 200 minutes.
  • Ultrasonic assistance Heating vacuum drying technology can significantly shorten the drying time.
  • the operation of this embodiment is basically the same as that of embodiment 1, except that the temperature of the water bath in step 1 is set to 60° C., and other conditions remain unchanged.
  • the water content of the lithium battery electrolyte is 41.6ppm, while the traditional heating and vacuum drying method is at a temperature of 80°C, a vacuum of 7torr, and an operating time of 120min.
  • the water content of the lithium battery electrolyte is 52.8ppm.
  • ultrasonic-assisted heating vacuum drying technology can achieve a lower water content (41.6ppm) at a lower drying temperature (60°C) than traditional heating vacuum drying technology. Ultrasonic-assisted heating vacuum drying Technology can significantly reduce the drying temperature.
  • the operation of this embodiment is basically the same as that of embodiment 1, except that the ultrasonic power of this embodiment is 15kW, the frequency is 25kHz, and the continuous working time is 240min.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Combustion & Propulsion (AREA)
  • Health & Medical Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Molecular Biology (AREA)
  • Electrochemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Sustainable Development (AREA)
  • Secondary Cells (AREA)

Abstract

Disclosed in the present invention are an apparatus for ultrasonic wave-assisted drying of a lithium battery electrolyte, and a drying method, the apparatus comprising a temperature-controlled heating water bath, an ultrasonic wave system, and a vacuum pump. A heating rod and a thermocouple are provided in the temperature-controlled heating water bath. An ultrasonic wave oscillator is provided at the bottom of the temperature-controlled heating water bath, the ultrasonic wave oscillator being connected to an ultrasonic wave generator. The vacuum pump is connected to a drying bottle by means of a pipeline, the connection being designed using a flange interface. A switch valve and a vent valve are sequentially provided in the pipeline, a vacuum gauge is provided between the switch valve and the flange interface, and the vacuum pump is positioned in between the switch valve and the vent valve. In the present invention, by means of providing an apparatus for ultrasonic wave-enhanced vacuum drying of a lithium battery electrolyte, ultrasonic wave-enhanced vacuum drying technology is used to accelerate transmission of moisture from a lithium battery electrolyte to outside the system during a drying process. The method features a simple structure and convenient operation, and can markedly reduce the drying time of a lithium battery electrolyte and reduce the drying temperature for same.

Description

一种超声波协助干燥锂电池电解质的装置及干燥方法Device for assisting in drying lithium battery electrolyte by ultrasonic and drying method 技术领域Technical field
本发明属于锂电池电解质干燥领域，具体是一种超声波协助干燥锂电池电解质的装置及干燥方法。The invention belongs to the field of lithium battery electrolyte drying, in particular to a device and a drying method for assisting the drying of lithium battery electrolyte by ultrasonic waves.
背景技术Background technique
锂离子二次电池具有电压高、比能量大、循环寿命长、放电性能稳定、安全性好、等优点，因此，近年来得到了迅速的发展，并且具有广阔的应用前景。锂离子二次电池主要是由正极材料、碳负极材料和电解液组成。电解液主要包括有机溶剂和电解质，作为锂离子二次电池的关键技术之一，其中电解质必须具备导电率高、化学及电化学稳定性好，可使用的温度范围宽、安全性好等优点，电解质在锂电池中电化学性能的提高，将大大改善锂离子电池的性能。Lithium-ion secondary batteries have the advantages of high voltage, large specific energy, long cycle life, stable discharge performance, and good safety. Therefore, they have developed rapidly in recent years and have broad application prospects. Lithium-ion secondary batteries are mainly composed of cathode materials, carbon anode materials and electrolyte. The electrolyte mainly includes organic solvents and electrolytes. As one of the key technologies of lithium-ion secondary batteries, the electrolyte must have the advantages of high conductivity, good chemical and electrochemical stability, wide usable temperature range, and good safety. The improvement of electrochemical performance of electrolyte in lithium battery will greatly improve the performance of lithium ion battery.
然而，目前国内的锂电池电解质普遍存在水分含量偏高的问题，其中水分对锂离子电池的性能有着至关重要的影响，水分的偏高会导致电解液中锂盐的分解并对正负极材料、铝箔都有一定的腐蚀作用，使电池容量下降衰减，放电时刻变短，内阻增大，电池胀大等现象，从而导致电池的性能急速下降。目前，行业内主要采用加热真空干燥的传统方法对锂电池电解质进行脱水，这种烘烤抽真空方法干燥能耗较大，效率较低，且干燥温度高。温度高又导致锂电池电解质的分解，从而影响锂电池电解质的品质。However, the current domestic lithium battery electrolytes generally have the problem of high moisture content. Among them, moisture has a crucial impact on the performance of lithium-ion batteries. High moisture will cause the decomposition of lithium salts in the electrolyte and affect the positive and negative electrodes. The material and aluminum foil have a certain corrosive effect, which causes the battery capacity to decrease and attenuate, the discharge time becomes shorter, the internal resistance increases, and the battery swells, which causes the battery's performance to drop rapidly. At present, the traditional method of heating and vacuum drying is mainly used in the industry to dehydrate the lithium battery electrolyte. This kind of baking and vacuuming method has high drying energy consumption, low efficiency and high drying temperature. The high temperature causes the decomposition of the lithium battery electrolyte, which affects the quality of the lithium battery electrolyte.
超声波是频率≥20kHz的声波，超声波具有传播方向性强，介质质点振动加速度大等特点。超声波有多种物理和化学效应，超声波与媒质的相互作用可分为热机制、机械机制和空化机制三种。将超声波直接有效耦合于真空加热干燥锂电池电解质过程中，利用超声波的空化作用产生的强大冲击波和微射流及热学效应等特点，可实现真空干燥过程中对锂电池电解质传热传质过程的强化，并达到缩短干燥时间，降低干燥温度，提高干燥效率的目的，可实现节能效果，减少企业负担。Ultrasonic waves are sound waves with a frequency ≥ 20kHz. Ultrasonic waves have the characteristics of strong propagation direction and large vibration acceleration of medium particles. Ultrasound has a variety of physical and chemical effects. The interaction between ultrasound and media can be divided into three types: thermal mechanism, mechanical mechanism, and cavitation mechanism. Ultrasound is directly and effectively coupled to the process of vacuum heating and drying of the lithium battery electrolyte, and the powerful shock wave, micro jet and thermal effect generated by the cavitation of the ultrasonic wave can be used to realize the heat and mass transfer process of the lithium battery electrolyte during the vacuum drying process. Strengthen, and achieve the purpose of shortening the drying time, lowering the drying temperature, and improving the drying efficiency, which can achieve energy-saving effects and reduce the burden on enterprises.
发明内容Summary of the invention
1.针对现有的传统加热真空干燥法的缺陷，本发明所要解决的技术问题是，提出能缩短干燥时间，降低干燥温度，提高干燥效率的一种超声波协助干燥锂电池电解质的装置及干燥方法。1. Aiming at the defects of the existing traditional heating and vacuum drying method, the technical problem to be solved by the present invention is to propose an ultrasonic assisted drying device and drying method for lithium battery electrolyte that can shorten the drying time, lower the drying temperature, and improve the drying efficiency .
2.本发明的目的可以通过以下技术方案实现：2. The purpose of the present invention can be achieved through the following technical solutions:
3.一种超声波协助干燥锂电池电解质的装置及干燥方法，包括温控加热水浴槽、超声波系统、真空泵。温控加热水浴槽内设有加热棒与热电偶。温控加热水浴槽底部设有超声波振子，超声波振子与超声波发生器连接。真空泵通过管道与干燥瓶相连，连接口采用法兰接口设计。管道内依次设置开关阀、放空阀，开关阀与法兰接口之间设置真空表。真空泵位于开关阀与放空阀之间。3. An ultrasonic-assisted device for drying lithium battery electrolyte and a drying method, including a temperature-controlled heating water bath, an ultrasonic system, and a vacuum pump. There are heating rods and thermocouples in the temperature-controlled heating water bath. An ultrasonic vibrator is arranged at the bottom of the temperature-controlled heating water bath, and the ultrasonic vibrator is connected with the ultrasonic generator. The vacuum pump is connected to the drying flask through a pipeline, and the connection port adopts a flange interface design. An on-off valve and a vent valve are sequentially arranged in the pipeline, and a vacuum gauge is set between the on-off valve and the flange interface. The vacuum pump is located between the on-off valve and the vent valve.
4.进一步方案，所述的温控加热水浴槽内设有加热棒与热电偶。4. A further solution, the temperature-controlled heating water bath is provided with a heating rod and a thermocouple.
5.进一步方案，所述的温控加热水浴槽底部设有超声波振子，超声波振子与超声波发生器连接。5. A further solution, the bottom of the temperature-controlled heating water bath is provided with an ultrasonic vibrator, and the ultrasonic vibrator is connected with the ultrasonic generator.
6.进一步方案，所述的真空泵通过管道与干燥瓶相连，连接口采用法兰接口设计。6. A further solution, the vacuum pump is connected to the drying flask through a pipeline, and the connection port adopts a flange interface design.
7.进一步方案，所述的管道内依次设置开关阀、放空阀，开关阀与法兰接口之间设置真空表。7. A further solution: an on-off valve and a vent valve are arranged in the pipeline in sequence, and a vacuum gauge is arranged between the on-off valve and the flange interface.
8.进一步方案，所述的真空泵位于开关阀与放空阀之间。8. A further solution, the vacuum pump is located between the on-off valve and the vent valve.
9.本发明的另外一个目的在于提出一种超声波协助干燥锂电池电解质的装置及干燥方法，包括以下步骤：9. Another object of the present invention is to provide an ultrasonic-assisted device and drying method for drying lithium battery electrolyte, including the following steps:
①.启动温控加热水浴槽进行电热棒加热，调节热电偶参数控制水浴温度。①. Start the temperature-controlled heating water bath to heat the electric heating rod, and adjust the thermocouple parameters to control the temperature of the water bath.
②.待水浴基本恒温至设定后，将待干燥的锂电池电解质移至干燥瓶中。干燥瓶通过法兰接口与真空泵管道连接好。打开真空泵、开关阀与放空阀，进行抽真空处理，调节真空度；②. After the basic constant temperature of the water bath reaches the setting, move the lithium battery electrolyte to be dried into the drying bottle. The drying flask is connected to the vacuum pump pipeline through the flange interface. Turn on the vacuum pump, on-off valve and vent valve to perform vacuum processing and adjust the vacuum degree;
③.打开超声波发生器，设定超声波发生器的工作参数；③. Turn on the ultrasonic generator and set the working parameters of the ultrasonic generator;
④.关闭超声波发生器，关闭温控加热水浴槽，让水浴温度下降至室温。④. Turn off the ultrasonic generator, turn off the temperature-controlled heating water bath, and let the temperature of the water bath drop to room temperature.
⑤.关闭真空泵，慢慢打开放空阀，充入干燥惰性气体，把真空度调节至常压。⑤. Turn off the vacuum pump, slowly open the vent valve, fill with dry inert gas, and adjust the vacuum to normal pressure.
⑥.打开法兰接口，把干燥瓶移出温控加热水浴槽，更换下一批待干燥的锂电池电解质即可以继续工作。⑥. Open the flange interface, remove the drying bottle out of the temperature-controlled heating water bath, and replace the next batch of lithium battery electrolyte to be dried to continue working.
10.进一步方案，所述的步骤①的水浴温度控制范围为25～90℃。10. A further solution, the temperature control range of the water bath in step ① is 25-90°C.
11.进一步方案，所述的步骤②的真空度范围在4～250torr。11. In a further solution, the vacuum degree of step ② ranges from 4 to 250 torr.
12.进一步方案，所述的步骤③的超声波发生器的工作参数为工作时间在5～240min，工作功率为1～20kW，超声波的频率为20～80kHz。12. A further solution, the working parameters of the ultrasonic generator in step ③ are working time of 5 to 240 min, working power of 1 to 20 kW, and ultrasonic frequency of 20 to 80 kHz.
13.进一步方案，所述的步骤④的降温所要达到的室温区间为25～35℃。13. A further scheme, the room temperature range to be reached in the step ④ for cooling is 25-35°C.
14.进一步方案，所述的步骤⑤的惰性气体为氮气、氩气、氖气、氦气、二氧化碳的一种或者多种组合。14. Further solution, the inert gas in step ⑤ is one or more combinations of nitrogen, argon, neon, helium, and carbon dioxide.
15.进一步方案，所述的步骤③～④可以为单个批次的循环过程，根据锂电池电解质的含水量与除水效率判定，此循环过程的次数可以为2-100次。15. Further solution, the steps ③ to ④ can be a single batch cycle process. According to the water content of the lithium battery electrolyte and the water removal efficiency, the number of this cycle process can be 2-100 times.
16.本发明针对现有的传统加热真空干燥法存在的能耗较大，效率较低，且干燥温度高的问题，提出一种超声波协助干燥锂电池电解质的装置及干燥方法。超声波通过空化作用产生的强大冲击波和微射流能够使水分在锂电池电解质中分散更均匀，还能是锂电池电解质内部质点产生内摩擦，从而在锂电池电解质内部形成有利于水分子往外扩散的微小通道，配合加热与抽真空过程，促使水分子往体系外部输送。16. The present invention addresses the problems of large energy consumption, low efficiency, and high drying temperature in the existing traditional heating and vacuum drying method, and proposes an ultrasonic assisted drying device and drying method for lithium battery electrolyte. The powerful shock waves and micro jets generated by ultrasonic waves through cavitation can make the water disperse more evenly in the lithium battery electrolyte, and it can also cause internal friction on the internal particles of the lithium battery electrolyte, thereby forming inside the lithium battery electrolyte that is conducive to the diffusion of water molecules. The tiny channel, combined with the heating and vacuuming process, promotes the transportation of water molecules to the outside of the system.
17.本发明的有益效果：17. The beneficial effects of the present invention:
(1)与传统加热真空干燥法相比，该方法可以缩短干燥时间，提高干燥效率；(1) Compared with the traditional heating and vacuum drying method, this method can shorten the drying time and improve the drying efficiency;
(2)与传统加热真空干燥法相比，该方法可以降低干燥温度，防止温度过高导致锂电池电解质的分解。(2) Compared with the traditional heating and vacuum drying method, this method can reduce the drying temperature and prevent the lithium battery electrolyte from decomposing due to excessive temperature.
附图说明Description of the drawings
图1为本发明超声波协助干燥锂电池电解质的装置结构示意图；FIG. 1 is a schematic diagram of the structure of an ultrasonic-assisted drying device of lithium battery electrolyte according to the present invention;
图中，1－温控加热水浴槽，2－热电偶，3－加热棒，4－超声波振子，5－超声波发生器，6－法兰接口，7－真空泵，8－真空泵，9－开关阀，10－放空阀。In the picture, 1-temperature controlled heating water bath, 2-thermocouple, 3-heating rod, 4-ultrasonic vibrator, 5-ultrasonic generator, 6-flange interface, 7-vacuum pump, 8-vacuum pump, 9-switch valve , 10-Vent valve.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明作进一步详细描述。The present invention will be further described in detail below in conjunction with the drawings and specific embodiments.
如图1所示，一种超声波协助干燥锂电池电解质的装置及干燥方法，包括温 控加热水浴槽(1)、超声波系统、真空泵(8)。温控加热水浴槽(1)内设有加热棒(3)与热电偶(2)。温控加热水浴槽(1)底部设有超声波振子(4)，超声波振子(4)与超声波发生器(5)连接。真空泵(8)通过管道与干燥瓶相连，连接口采用法兰接口(6)设计。管道内依次设置开关阀(9)、放空阀(10)，开关阀(9)与法兰接口(6)之间设置真空表(7)。真空泵(8)位于开关阀(9)与放空阀(10)之间。As shown in Fig. 1, a device and a drying method for assisting the drying of lithium battery electrolyte by ultrasound include a temperature-controlled heating water bath (1), an ultrasonic system, and a vacuum pump (8). A heating rod (3) and a thermocouple (2) are arranged in the temperature-controlled heating water bath (1). An ultrasonic vibrator (4) is arranged at the bottom of the temperature-controlled heating water bath (1), and the ultrasonic vibrator (4) is connected with the ultrasonic generator (5). The vacuum pump (8) is connected with the drying flask through a pipeline, and the connection port is designed with a flange interface (6). An on-off valve (9) and a vent valve (10) are sequentially arranged in the pipeline, and a vacuum gauge (7) is arranged between the on-off valve (9) and the flange interface (6). The vacuum pump (8) is located between the on-off valve (9) and the vent valve (10).
实施例1Example 1
一种超声波协助干燥锂电池电解质的装置及干燥方法，具体包括以下步骤：①启动温控加热水浴槽进行电热棒加热，调节热电偶参数控制水浴温度为80℃。②待水浴基本恒温至设定后，将待干燥的锂电池电解质(含水量≥5000ppm)10Kg移至干燥瓶中。干燥瓶通过法兰接口与真空泵管道连接好。打开真空泵、开关阀与放空阀，进行抽真空处理，调节真空度达到7torr。③打开超声波发生器，以10kW的功率以及35kHz的频率连续工作120min。④关闭超声波发生器，关闭温控加热水浴槽，让水浴温度下降30℃。⑤关闭真空泵，慢慢打开放空阀，充入干燥氮气，真空度调节回常压760torr。⑥打开法兰接口，把干燥瓶移出温控加热水浴槽。取出锂电池电解质检测含水量为28.3ppm。An ultrasonic-assisted device for drying lithium battery electrolyte and a drying method specifically include the following steps: ①Start a temperature-controlled heating water bath to heat the electric heating rod, and adjust the thermocouple parameters to control the temperature of the water bath to 80°C. ②After the water bath is basically constant temperature to the setting, transfer 10Kg of the lithium battery electrolyte (water content ≥5000ppm) to be dried into the drying bottle. The drying flask is connected to the vacuum pump pipeline through the flange interface. Turn on the vacuum pump, on-off valve and vent valve to perform vacuum processing, and adjust the vacuum to 7torr. ③Turn on the ultrasonic generator, and work continuously for 120min at a power of 10kW and a frequency of 35kHz. ④Turn off the ultrasonic generator, turn off the temperature-controlled heating water bath, and let the temperature of the water bath drop by 30°C. ⑤Turn off the vacuum pump, slowly open the vent valve, fill with dry nitrogen, and adjust the vacuum back to normal pressure of 760torr. ⑥Open the flange interface and remove the drying flask out of the temperature-controlled heating water bath. The electrolyte of the lithium battery was taken out and the water content was 28.3ppm.
超声波协助加热真空干燥锂电池电解质后，锂电池电解质检测含水量为28.3ppm，耗时120min；在相同条件下，锂电池电解质含水量达到28.3ppm，传统加热真空干燥法耗时需要200min，超声波协助加热真空干燥技术可明显缩短干燥时间。After ultrasonic-assisted heating and vacuum drying of the lithium battery electrolyte, the water content of the lithium battery electrolyte is 28.3ppm, which takes 120 minutes; under the same conditions, the water content of the lithium battery electrolyte reaches 28.3ppm, and the traditional heating and vacuum drying method takes 200 minutes. Ultrasonic assistance Heating vacuum drying technology can significantly shorten the drying time.
实施例2Example 2
本实施例与实施例1操作基本相同，不同之处在于步骤①的水浴温度设置为60℃，其他条件不变。检测锂电池电解质含水量为41.6ppm，而传统加热真空干燥法在温度80℃，真空度7torr，操作时间为120min条件下，检测锂电池电解质含水量为52.8ppm。The operation of this embodiment is basically the same as that of embodiment 1, except that the temperature of the water bath in step ① is set to 60° C., and other conditions remain unchanged. The water content of the lithium battery electrolyte is 41.6ppm, while the traditional heating and vacuum drying method is at a temperature of 80°C, a vacuum of 7torr, and an operating time of 120min. The water content of the lithium battery electrolyte is 52.8ppm.
在相同的干燥时间下，超声波协助加热真空干燥技术较于传统加热真空干燥技术，可以在更低的干燥温度(60℃)下，达到更低的水含量(41.6ppm)，超声波协助加热真空干燥技术可以明显降低干燥温度。Under the same drying time, ultrasonic-assisted heating vacuum drying technology can achieve a lower water content (41.6ppm) at a lower drying temperature (60℃) than traditional heating vacuum drying technology. Ultrasonic-assisted heating vacuum drying Technology can significantly reduce the drying temperature.
实施例3Example 3
本实施例与实施例1操作基本相同，不同之处在于本实施例的超声波功率为15kW，频率为25kHz，连续工作时间为240min。The operation of this embodiment is basically the same as that of embodiment 1, except that the ultrasonic power of this embodiment is 15kW, the frequency is 25kHz, and the continuous working time is 240min.
实施例4Example 4
本实施例与实施例3操作基本相同，不同之处在于本实施例的水浴温度为60℃。The operation of this embodiment is basically the same as that of embodiment 3, except that the temperature of the water bath in this embodiment is 60°C.
实施例5Example 5
本实施例与实施例3操作基本相同，不同之处在于本实施例的真空度为5torr。The operation of this embodiment is basically the same as that of Embodiment 3, except that the vacuum degree of this embodiment is 5 torr.

Claims (13)

  1. 一种超声波协助干燥锂电池电解质的装置，其特征在于，包括温控加热水浴槽(1)、超声波系统、真空泵(8)；温控加热水浴槽(1)内设有加热棒(3)与热电偶(2)；温控加热水浴槽(1)底部设有超声波振子(4)，超声波振子(4)与超声波发生器(5)连接；真空泵(8)通过管道与干燥瓶相连，连接口采用法兰接口(6)设计；管道内依次设置开关阀(9)、放空阀(10)，开关阀(9)与法兰接口(6)之间设置真空表(7)；真空泵(8)位于开关阀(9)与放空阀(10)之间。An ultrasonic-assisted device for drying lithium battery electrolyte, which is characterized by comprising a temperature-controlled heating water bath (1), an ultrasonic system, and a vacuum pump (8); the temperature-controlled heating water bath (1) is provided with heating rods (3) and Thermocouple (2); the bottom of the temperature-controlled heating water bath (1) is equipped with an ultrasonic vibrator (4), the ultrasonic vibrator (4) is connected with the ultrasonic generator (5); the vacuum pump (8) is connected to the drying bottle through a pipe, and the connection port The flange interface (6) design is adopted; the on-off valve (9), the vent valve (10) are arranged in the pipeline in turn, the vacuum gauge (7) is set between the on-off valve (9) and the flange interface (6); the vacuum pump (8) Located between the on-off valve (9) and the vent valve (10).
  2. 根据权利要求1所述的一种超声波协助干燥锂电池电解质的装置，其特征在于，所述的温控加热水浴槽(1)内设有加热棒(3)与热电偶(2)。The device for assisting the drying of lithium battery electrolyte with ultrasonic waves according to claim 1, characterized in that, a heating rod (3) and a thermocouple (2) are provided in the temperature-controlled heating water bath (1).
  3. 根据权利要求1所述的一种超声波协助干燥锂电池电解质的装置，其特征在于，所述的温控加热水浴槽(1)底部设有超声波振子(4)，超声波振子(4)与超声波发生器(5)连接。The device for assisting the drying of lithium battery electrolyte with ultrasonic according to claim 1, wherein the bottom of the temperature-controlled heating water bath (1) is provided with an ultrasonic vibrator (4), the ultrasonic vibrator (4) and the ultrasonic generator器(5) is connected.
  4. 根据权利要求1所述的一种超声波协助干燥锂电池电解质的装置，其特征在于，所述的真空泵(8)通过管道与干燥瓶相连，连接口采用法兰接口(6)设计。An ultrasonic assisted drying device for lithium battery electrolyte according to claim 1, characterized in that the vacuum pump (8) is connected to the drying flask through a pipe, and the connection port is designed with a flange interface (6).
  5. 根据权利要求1所述的一种超声波协助干燥锂电池电解质的装置，其特征在于，所述的管道内依次设置开关阀(9)、放空阀(10)，开关阀(9)与法兰接口(6)之间设置真空表(7)。The device for assisting the drying of lithium battery electrolyte with ultrasonic waves according to claim 1, characterized in that an on-off valve (9), a vent valve (10) are arranged in the pipeline in sequence, the on-off valve (9) and the flange interface A vacuum gauge (7) is set between (6).
  6. 根据权利要求1所述的一种超声波协助干燥锂电池电解质的装置，其特征在于，所述的真空泵(8)位于开关阀(9)与放空阀(10)之间。The device for assisting the drying of lithium battery electrolyte with ultrasonic waves according to claim 1, characterized in that the vacuum pump (8) is located between the on-off valve (9) and the vent valve (10).
  7. 一种超声波协助干燥锂电池电解质的干燥方法，使用根据权利要求1-6所述的装置，其特征在于，包括以下操作步骤：An ultrasonic-assisted drying method for lithium battery electrolyte, using the device according to claims 1-6, characterized in that it comprises the following operation steps:
    ①.启动温控加热水浴槽(1)进行电热棒加热，调节热电偶(2)参数控制水浴温度；①. Start the temperature-controlled heating water bath (1) for heating by the electric heating rod, and adjust the parameters of the thermocouple (2) to control the temperature of the water bath;
    ②.待水浴基本恒温至设定后，将待干燥的锂电池电解质移至干燥瓶中；干燥瓶通过法兰接口(6)与真空泵(8)管道连接好；打开真空泵(8)、开关阀(9)与放空阀(10)，进行抽真空处理，调节真空度；②. After the basic constant temperature of the water bath reaches the setting, move the lithium battery electrolyte to be dried into the drying flask; the drying flask is connected to the vacuum pump (8) pipeline through the flange interface (6); open the vacuum pump (8) and the switch valve (9) Perform vacuum treatment with the vent valve (10) to adjust the vacuum degree;
    ③.打开超声波发生器(5)，设定超声波发生器(5)的工作参数；③. Turn on the ultrasonic generator (5) and set the working parameters of the ultrasonic generator (5);
    ④.关闭超声波发生器(5)，关闭温控加热水浴槽(1)，让水浴温度下降至室温；④. Turn off the ultrasonic generator (5), turn off the temperature-controlled heating water bath (1), and let the temperature of the water bath drop to room temperature;
    ⑤.关闭真空泵(8)，慢慢打开放空阀(10)，充入干燥惰性气体，把真空度调节至常压；⑤. Turn off the vacuum pump (8), slowly open the vent valve (10), fill with dry inert gas, and adjust the vacuum to normal pressure;
    ⑥.打开法兰接口(6)，把干燥瓶移出温控加热水浴槽(1)，更换下一批待干燥的锂电池电解质即可以继续工作。⑥. Open the flange interface (6), remove the drying flask out of the temperature-controlled heating water bath (1), and replace the next batch of lithium battery electrolyte to be dried to continue working.
  8. 根据权利要求7所述的一种超声波协助干燥锂电池电解质的干燥方法，其特征在于，所述的步骤①的水浴温度控制范围为25～90℃。An ultrasonic-assisted drying method for lithium battery electrolyte according to claim 7, characterized in that the temperature control range of the water bath in the step (1) is 25-90°C.
  9. 根据权利要求7所述的一种超声波协助干燥锂电池电解质的干燥方法，其特征在于，所述的步骤②的真空度范围在4～250torr。An ultrasonic-assisted drying method for drying lithium battery electrolyte according to claim 7, wherein the vacuum degree of step ② is in the range of 4 to 250 Torr.
  10. 根据权利要求7所述的一种超声波协助干燥锂电池电解质的干燥方法，其特征在于，所述的步骤③的超声波发生器(5)的工作参数为工作时间在5～240min，工作功率为1～20kW，超声波的频率为20～80kHz。An ultrasonic-assisted drying method for lithium battery electrolyte according to claim 7, characterized in that the working parameters of the ultrasonic generator (5) in step ③ are working time of 5 to 240 minutes, and working power of 1. ～20kW, the frequency of ultrasound is 20～80kHz.
  11. 根据权利要求7所述的一种超声波协助干燥锂电池电解质的干燥方法，其特征在于，所述的步骤④的降温所要达到的室温区间为25～35℃。An ultrasonic-assisted drying method for lithium battery electrolyte according to claim 7, characterized in that the room temperature range to be reached for cooling in step ④ is 25-35°C.
  12. 根据权利要求7所述的一种超声波协助干燥锂电池电解质的干燥方法，其特征在于，所述的步骤⑤的惰性气体为氮气、氩气、氖气、氦气、二氧化碳的一种或者多种组合。An ultrasonic-assisted drying method for lithium battery electrolyte according to claim 7, wherein the inert gas in step ⑤ is one or more of nitrogen, argon, neon, helium, and carbon dioxide combination.
  13. 根据权利要求7所述的一种超声波协助干燥锂电池电解质的干燥方法，其特征在于，所述的步骤③～④可以为单个批次的循环过程，根据锂电池电解质的含水量与除水效率判定，此循环过程的次数可以为2-100次。An ultrasonic-assisted drying method for lithium battery electrolyte according to claim 7, characterized in that the steps ③ to ④ can be a single batch cycle process, according to the water content of the lithium battery electrolyte and the water removal efficiency It is judged that the number of this cycle process can be 2-100 times.
PCT/CN2020/094587 2020-06-05 2020-06-05 Apparatus for ultrasonic wave-assisted drying of lithium battery electrolyte, and drying method WO2021082448A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/CN2020/094587 WO2021082448A1 (en) 2020-06-05 2020-06-05 Apparatus for ultrasonic wave-assisted drying of lithium battery electrolyte, and drying method
CN202080005190.XA CN112739971A (en) 2020-06-05 2020-06-05 Device and method for drying lithium battery electrolyte assisted by ultrasonic waves

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2020/094587 WO2021082448A1 (en) 2020-06-05 2020-06-05 Apparatus for ultrasonic wave-assisted drying of lithium battery electrolyte, and drying method

Publications (1)

Publication Number Publication Date
WO2021082448A1 true WO2021082448A1 (en) 2021-05-06

Family

ID=75609550

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2020/094587 WO2021082448A1 (en) 2020-06-05 2020-06-05 Apparatus for ultrasonic wave-assisted drying of lithium battery electrolyte, and drying method

Country Status (2)

Country Link
CN (1) CN112739971A (en)
WO (1) WO2021082448A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114050321A (en) * 2021-11-22 2022-02-15 上海兰钧新能源科技有限公司 Baking process and baking device for lithium ion battery
CN114659341A (en) * 2022-03-02 2022-06-24 上海兰钧新能源科技有限公司 Control method for baking lithium ion battery

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102921178A (en) * 2012-11-19 2013-02-13 青岛大学 Anti-oxidization evaporation and drying device and method
CN203139653U (en) * 2013-03-22 2013-08-21 湖北工业大学 Ultrasonic evaporimeter
CN205683600U (en) * 2016-06-01 2016-11-16 甘肃农业大学 The vacuum concentrating apparatus of ultrasonic combined thermal drivers auxiliary

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016138684A (en) * 2015-01-27 2016-08-04 株式会社Ｓｃｒｅｅｎホールディングス Drying device and drying method
CN107388735A (en) * 2017-07-18 2017-11-24 南京国轩电池有限公司 A kind of intensified by ultrasonic wave heated-air drying power lithium-ion battery device and drying means
CN108645125A (en) * 2018-04-28 2018-10-12 南京农业大学 A kind of method and its drying device of contact ultrasonic auxiliary heated-air drying fruits and vegetables
CN108709411A (en) * 2018-06-22 2018-10-26 新乡市盛达电源科技有限公司 A kind of battery case production device for cleaning and air-drying
CN109786627A (en) * 2019-01-28 2019-05-21 中国科学院兰州化学物理研究所 A kind of preparation method of super close electrolyte lithium battery diaphragm
CN110230917A (en) * 2019-06-17 2019-09-13 新疆骏强科技发展有限公司 Device for drying anhydrous lithium iodide and preparation method of anhydrous lithium iodide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102921178A (en) * 2012-11-19 2013-02-13 青岛大学 Anti-oxidization evaporation and drying device and method
CN203139653U (en) * 2013-03-22 2013-08-21 湖北工业大学 Ultrasonic evaporimeter
CN205683600U (en) * 2016-06-01 2016-11-16 甘肃农业大学 The vacuum concentrating apparatus of ultrasonic combined thermal drivers auxiliary

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114050321A (en) * 2021-11-22 2022-02-15 上海兰钧新能源科技有限公司 Baking process and baking device for lithium ion battery
CN114659341A (en) * 2022-03-02 2022-06-24 上海兰钧新能源科技有限公司 Control method for baking lithium ion battery

Also Published As

Publication number Publication date
CN112739971A (en) 2021-04-30

Similar Documents

Publication Publication Date Title
WO2021082448A1 (en) Apparatus for ultrasonic wave-assisted drying of lithium battery electrolyte, and drying method
CN106941167B (en) Porous composite negative electrode material of lithium ion battery and preparation method thereof
CN112331947B (en) Lithium battery discharging method in lithium battery recycling and disassembling process
WO2011079409A1 (en) Method of recycling and reusing spent lithium iron phosphate power battery
CN108550825B (en) Method for preparing silicon-carbon cathode material of lithium ion battery
CN108346793B (en) Preparation method and application of nano-silicon with porous structure
WO2022268055A1 (en) Method for preparing nio@comoo4/nf capacitor electrode
JP2015135195A (en) Pole plate drying device for secondary battery and pole plate drying method
WO2023050466A1 (en) Method for preparing hard carbon negative electrode of lithium/sodium ion battery by using biomass charcoal
CN107171036B (en) A kind of recovery and treatment method of nickel-cobalt-manganese ternary system battery capacitor
CN105890291A (en) Drying method for high-capacity lithium ion battery cell
CN113488701A (en) Baking method for aluminum-shell lithium ion battery
CN110668433A (en) Method for preparing graphite/graphene composite material by supercritical carbon dioxide fluid and application
TWI635648B (en) Method of optimizing flow battery with carbon electrode
WO2021232664A1 (en) Online evaluation method for molten carbonate fuel cell separator roasting
CN208835158U (en) A kind of lithium ion battery separator manufacturing process orientation stretching device
CN118089338A (en) Drying method for square-shell sodium-ion battery cell
WO2022193550A1 (en) Molten carbonate fuel cell preheating device and method
CN211926536U (en) Push plate furnace heat preservation and heat dissipation device for lithium ion battery production
CN115441080A (en) Direct recovery and regeneration method of oxide solid electrolyte
CN211719716U (en) Lithium battery pack capable of avoiding damage of components caused by overheating
CN210631985U (en) Special dispersion devices of electric motor car lithium cell cathode material
CN217462681U (en) Material pumping equipment for negative electrode material
JP3189763U (en) Battery plate drying device
CN221928188U (en) Battery manufacturing apparatus

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 20882451

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 20882451

Country of ref document: EP

Kind code of ref document: A1