Oxygen content monitoring device and system for synthesizing ternary precursor

Abstract

The utility model provides an oxygen content monitoring device and a system for synthesizing a ternary precursor. The oxygen content monitoring device comprises a shell, a first flow cell, a second flow cell, a fluorescent oxygen electrode and a polarographic oxygen electrode, the first flow cell and the second flow cell are arranged on the shell at an interval, the fluorescent oxygen electrode is arranged in the first flow cell, the polarographic oxygen electrode is arranged in the second flow cell, and the first flow cell is inclined and inverted. According to the oxygen content monitoring device provided by the utility model, the fluorescent oxygen electrode and the polarographic oxygen electrode are arranged, and the flow cell corresponding to the fluorescent oxygen electrode is inclined and inverted, so that different requirements of customers can be met, and the accuracy of a detection result is improved. The system for synthesizing the ternary precursor provided by the utility model is beneficial to improving the control precision of the oxygen content in the production process, thereby being beneficial to improving the production yield.

Description

TECHNICAL FIELD

[0001] The utility model belongs to lithium battery material field, concretely relates to an oxygen content monitoring device and system for synthesizing ternary precursor. BACKGROUND

[0002] With the gradual exhaustion of non-renewable energy such as oil and natural gas and the increasing emphasis on environmental protection, especially with the rapid development of new energy vehicles, energy storage, power tools and 3C electronic products and other industries, the demand for lithium batteries is rapidly increasing, and thus the demand for raw materials for lithium battery production, including ternary cathode materials, is also rapidly increasing.

[0003] Ternary precursor is an important upstream material for producing ternary cathode material. In the production process of ternary precursor, in order to avoid the oxidation of metal ions, it needs to be carried out under the protection of inert gas. However, in order to meet product demand, sometimes a mixture of trace oxygen and inert gas needs to be introduced to change the reaction environment. The amount of oxygen in the reaction stage of preparing ternary precursor must be strictly controlled in real time. However, the existing oxygen content detector is usually a single detection mode, which is difficult to meet the multiple detection needs of users and is prone to detection errors.

[0004] It should be noted that the above introduction to the technical background is only to facilitate a clear and complete description of the technical solutions of the present application, and to facilitate the understanding of those skilled in the art. The above technical solutions cannot be considered as known to those skilled in the art just because they are described in the background section of the present application. CONTENT OF THE UTILITY MODEL

[0005] In view of the above-mentioned shortcomings of the prior art, the purpose of the present utility model is to provide an oxygen content monitoring device and a system for synthesizing ternary precursor, to solve the problems of the existing oxygen content detector, which is usually a single detection mode, difficult to meet the multiple detection needs of users, and prone to detection errors.

[0006] To achieve the above-mentioned purposes and other related purposes, the present utility model provides an oxygen content monitoring device, which comprises a shell, a first flow cell, a second flow cell, a fluorescent oxygen electrode and a polarographic oxygen electrode. The first flow cell and the second flow cell are arranged on the shell with a spacing. The fluorescent oxygen electrode is placed in the first flow cell, and the polarographic oxygen electrode is placed in the second flow cell. The first flow cell is inclined and inverted.

[0007] Optionally, the first flow cell and the second flow cell are connected to each other by a pipeline.

[0008] Optionally, the oxygen content monitoring device is further provided with a sampling pump and a filter, and the sampling pump is connected to the first flow cell and the second flow cell through the filter.

[0009] Optionally, the oxygen content monitoring device further comprises a peristaltic pump in communication with the filter for discharging liquid in the filter.

[0010] Optionally, the oxygen content monitoring device further comprises a display electrically connected with the fluorescent oxygen electrode and the polarographic oxygen electrode, and a cover body openably connected with the shell, and a transparent observation window corresponding to the display is arranged on the cover body.

[0011] Optionally, the oxygen content monitoring device further comprises a support arranged at the bottom of the shell.

[0012] Optionally, the oxygen content monitoring device is further provided with a detection gas device for detecting whether the oxygen content monitoring device is stable and / or there is abnormal air tightness, the detection gas device being in communication with the first flow cell and the second flow cell.

[0013] The utility model also provides a system for synthesizing ternary precursor, the system comprises a reaction kettle and the oxygen content monitoring device as described in any one of the above schemes, and the oxygen content monitoring device is in communication with the reaction kettle.

[0014] Optionally, the reaction kettle is multiple, and the multiple reaction kettles are connected to the same oxygen content monitoring device through a multi-channel valve.

[0015] Optionally, a two-way valve and a mass flow meter are arranged on the feed gas pipeline of each reaction kettle.

[0016] As described above, the oxygen content monitoring device and the system for synthesizing ternary precursor provided by the utility model have the following beneficial effects: the oxygen content monitoring device provided by the utility model is provided with two electrodes, i.e., a fluorescent oxygen electrode and a polarographic oxygen electrode, and the flow cell corresponding to the fluorescent oxygen electrode is inclined and inverted, so that different needs of customers can be met, and the accuracy of detection results is improved. The system for synthesizing ternary precursor provided by the utility model is helpful to improve the control precision of oxygen content in the production process, thereby helping to improve the production yield. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 An exemplary front view of the oxygen content monitoring device provided by the utility model is shown.

[0018] Figure 2 A connection relationship schematic view of the local structure of the oxygen content monitoring device provided by the utility model is shown.

[0019] Figure 3 A connection relationship schematic view of each structure of the system for synthesizing ternary precursor provided by the utility model is shown.

[0020] Figure 4The image shown is an exemplary left view of the system for synthesizing ternary precursors provided by this invention.

[0021] Figure 5 The image shown is an exemplary right view of the system for synthesizing ternary precursors provided by this invention. Detailed Implementation

[0022] The following specific examples illustrate the implementation of this utility model. Those skilled in the art can easily understand other advantages and effects of this utility model from the content disclosed in this specification. This utility model can also be implemented or applied through other different specific embodiments, and various details in this specification can be modified or changed based on different viewpoints and applications without departing from the spirit of this utility model. For ease of explanation, when detailing the embodiments of this utility model, the cross-sectional views showing the device structure may be partially enlarged without adhering to the general scale, and the schematic diagrams are merely examples and should not limit the scope of protection of this utility model. Furthermore, in actual manufacturing, the three-dimensional spatial dimensions of length, width, and depth should be included.

[0023] For ease of description, spatial relation terms such as “below,” “under,” “lower than,” “below,” “above,” and “upper” may be used herein to describe the relationship between one element or feature shown in the accompanying drawings and other elements or features. It will be understood that these spatial relation terms are intended to include directions other than those depicted in the drawings for devices in use or operation. Furthermore, when a layer is referred to as being “between” two layers, it may be the only layer between the two layers, or there may be one or more layers in between.

[0024] It should be noted that the illustrations provided in this embodiment are only schematic representations of the basic concept of this utility model. Therefore, the drawings only show components related to this utility model and are not drawn according to the actual number, shape, and size of the components in the actual implementation. In the actual implementation, the form, quantity, and proportion of each component can be arbitrarily changed, and the layout of the components may also be more complex. To keep the illustrations as concise as possible, not all structures are indicated in the drawings.

[0025] like Figures 1 to 2 As shown, this embodiment provides an oxygen content monitoring device that can be used to detect the oxygen content in a test sample, such as a liquid or gas. It includes a housing 11, a first flow cell 12, a second flow cell 13, a fluorescent oxygen electrode 14, and a polarographic oxygen electrode 15.

[0026] The shell 11 can also be referred to as a back plate, which can be made of metal material such as 316L stainless steel, and can withstand harsh environmental conditions in industrial processes. The shell 11 can be generally square-shaped to accommodate the layout of the related components. The shell 11 has a first flow cell 12 and a second flow cell 13, and a groove for fixing the fluorescent oxygen electrode 14 and the polarographic oxygen electrode 15. The first flow cell 12 and the second flow cell 13 can be detachably arranged on the shell 11. For example, the first flow cell 12 and the second flow cell 13 can be made of corrosion-resistant transparent material and embedded in the corresponding groove of the shell 11. Both flow cells are provided with a sample inlet channel and a sample outlet channel, or the sample inlet channel and the sample outlet channel can be the same, which is determined according to specific needs, and is not strictly limited. The size of the two flow cells, including the size of the flow cell and the inlet channel of the test sample, such as the inlet channel of the test gas, can be determined according to the gas flow, and is also not limited.

[0027] In this embodiment, the fluorescent oxygen electrode 14 is placed in the first flow cell 12, and the polarographic oxygen electrode 15 is placed in the second flow cell 13. During detection, the electrode film head of each electrode needs to be completely immersed in the corresponding flow cell to ensure that the test sample fully surrounds the corresponding electrode film head and ensures the accuracy of the measurement results. The fluorescent oxygen electrode 14 irradiates the fluorescent material with LED light, the fluorescent material absorbs light energy and releases fluorescence, and the dissolved oxygen can absorb the transition electrons in the fluorescent material to cause fluorescence quenching, reduce the fluorescence intensity and fluorescence time, and detect the concentration of dissolved oxygen by checking the change of fluorescence intensity or the length of fluorescence time. The polarographic oxygen electrode 15 uses an electrochemical method, which converts dissolved oxygen on the surface of the metal electrode into oxygen negative ions by receiving electrons, and finally converts into hydroxyl groups. The concentration of dissolved oxygen is detected by measuring the current change of this process. These two methods of measuring oxygen concentration have advantages and disadvantages, and in this embodiment, both electrodes are provided, and users can choose one electrode according to needs, or use both electrodes for measurement and data comparison, which can meet the different needs of users and improve the detection accuracy. In addition, in this embodiment, the first flow cell 12 is inclined and inverted, for example, the first flow cell 12 is placed with the outlet inclined downward at an angle of 45°, which can make the liquid in the test sample gas discharged from the outlet due to the action of gravity, and can effectively avoid the problem of inaccurate measurement results caused by liquid accumulation when collecting gas with high humidity for a long time.

[0028] The first flow cell 12 and the second flow cell 13 can each be in communication with a sample source to be tested. In a preferred embodiment provided by the present application, however, the first flow cell 12 and the second flow cell 13 are in communication with each other through a pipeline 16. In other words, the two are in series, and thus share a sampling channel, which can simplify the structure of the device and facilitate the miniaturization of the whole. For example, in the present embodiment, the first flow cell 12 is directly in communication with the sampling pipeline, and the second flow cell 13 is in series at the rear end of the first flow cell 12. In further examples, a control valve (not shown) can be provided on the pipeline connecting the two, so as to close the other testing channel when only one testing channel is enabled.

[0029] In a preferred example, the oxygen content monitoring device is further provided with a sampling pump 17 and a filter 18, the sampling pump 17 being in communication with the first flow cell 12 and the second flow cell 13 via the filter 18. Thus, the sample to be tested sampled by the sampling pump 17 first passes through the filter 18 before entering the first flow cell 12 and the second flow cell 13. The provision of the sampling pump 17 can enable periodic sampling by setting a sampling period. The provision of the filter 18 can filter water vapor and particulate impurities in the sample to be tested, which can further improve the accuracy of the detection results.

[0030] In further examples, the oxygen content monitoring device further includes a waste liquid pump 19, for example, a peristaltic pump, which is in communication with the filter 18 and can discharge liquid in the filter 18 at regular intervals. A waste liquid valve 20 can be provided on the liquid discharge pipeline of the waste liquid pump 19.

[0031] The oxygen content monitoring device can be connected to an external device, for example, a remote monitoring terminal, to transmit the detection results to the remote terminal. In a preferred example provided by the present application, the oxygen content monitoring device is provided with a display 21 electrically connected to the fluorescent oxygen electrode 14 and the polarographic oxygen electrode 15. The display 21 can be located at the upper part of the device, i.e., above the electrodes, or the positional relationship of the structures can be adjusted otherwise. The display 21 can display the detection results of the electrodes in real time on site, which greatly improves the portability of the oxygen content monitoring device. To protect the electrodes and other structures from corrosion by the external environment, the oxygen content monitoring device is provided with a cover 22 that is hingedly connected to the shell 11. The cover 22 can also be made of metal materials such as stainless steel. Further, the cover 22 can be provided with a transparent observation window 221 corresponding to the display 21, which can be made of high-strength glass. For example, as shown in FIG. 1, the cover 22 is provided with an upper observation window corresponding to the display 21 and a lower observation window corresponding to each flow cell. In some examples, the oxygen content monitoring device can further include an alarm (not shown), which can be electrically connected to the electrodes to issue an alarm when the detection results exceed a safety threshold. Figure 1 ​

[0032] In some examples, the oxygen content monitoring device further comprises a support 23 arranged at the bottom of the shell 11, the support 23 can be fixedly connected or detachably connected with the shell 11, and the support 23 can adopt a similar height-adjustable structure such as a scissor lift. The support 23 is arranged to lift the shell 11, which can further protect the structure in the shell 11, and the height of the device can be flexibly adjusted according to the detection requirements.

[0033] In some examples, the oxygen content monitoring device is further provided with a detection gas device (which can be referred to as Figure 3 The detection gas device is in communication with the first flow cell 12 and the second flow cell 13. The detection gas device, for example, comprises a high-purity nitrogen or helium detection gas source 24, the detection gas source 24 is in communication with each flow cell through a detection gas pipeline, and a control valve (not labeled) can be arranged on the detection gas pipeline to control the on-off of the detection gas. The detection principle is generally that, for example, the nitrogen gas used by the detection gas has a concentration of 99.999% high-purity nitrogen, by judging whether the measurement value of the electrode during the nitrogen purging process is lower than a certain set value (such as 0.01%), and is stable within a period of time, it can be determined that the electrode performance is good and the system gas tightness is good.

[0034] The oxygen content monitoring device provided by the present application can meet the different detection requirements of customers by arranging two kinds of electrodes of the fluorescent oxygen electrode and the polarographic oxygen electrode, and tilting and inverting the flow cell corresponding to the fluorescent oxygen electrode, and can improve the accuracy of the detection results. The oxygen content monitoring device provided by the present application can be used for detecting the oxygen content in liquid and gas, and is especially suitable for application occasions with very high precision requirements for oxygen content concentration.

[0035] As Figures 3 to 5 The utility model further provides a system for synthesizing ternary precursor, the system includes reaction kettle 25 and the oxygen content monitoring device as described in any preceding scheme, the oxygen content monitoring device communicates with reaction kettle 25. Thus the introduction of the oxygen content monitoring device can be cited in full, for the purpose of brevity not to repeat.

[0036] The reaction kettles 25 can be single or multiple. For example, in the preferred example, the reaction kettles 25 are two or more, and the multiple reaction kettles 25 are connected to the same oxygen content monitoring device through a multi-channel valve 26, which can periodically sample and monitor the gas in each reaction kettle 25. Such a setting can reduce the number of monitoring devices and simplify the system structure. At the same time, the same set of monitoring devices is used for sampling and monitoring of different reaction kettles 25, ensuring the same of the monitoring standard, which helps to improve the production yield of the system. For example, in the present embodiment, the system includes four reaction kettles 25 (i.e., four working channels), and the four reaction kettles 25 are connected to the same multi-channel valve 26 through a pipeline provided with a sampling valve 31, and finally connected to the same oxygen content monitoring device. As an example, the detection gas source 24 for detecting whether the oxygen content monitoring device is stable and / or there is an air tightness abnormality is also connected to the oxygen content monitoring device through the multi-channel valve 26.

[0037] In order to improve the control accuracy of the reaction gas, a two-way valve 27 and a mass flow meter 28 are arranged on the feed gas pipeline of each reaction kettle 25. For example, in the present embodiment, the reaction gas source includes an oxygen source 29 and a nitrogen source 30, and the two gas channels are provided with two-way valves 27 and mass flow meters 28.

[0038] The exemplary working process of the system for synthesizing ternary precursors provided by the present embodiment is as follows (taking a system with four working channels as an example):

[0039] (1) After exhausting each flow cell, the sampling pump extracts nitrogen into the flow cell of each electrode, and the system judges the stability and whether there is an air tightness abnormality according to the electrode measurement value. After judging normal, the next step is performed.

[0040] (2) Open the sampling valve of channel 1, and the sampling pump extracts the filtered sample into the electrode flow cell. After a period of time, the electrode measurement value is stable, the current oxygen content data is recorded, the sampling pump and the sampling valve are closed, and the nitrogen and air flow rates required to be introduced into the reaction kettle are calculated. The set parameters are issued to the two mass flow meters of channel 1.

[0041] (3) Open the sampling valve of channel 2, and the sampling pump extracts the filtered sample into the electrode flow cell. After a period of time, the electrode measurement value is stable, the current oxygen content data is recorded, the sampling pump and the sampling valve are closed, and the nitrogen and air flow rates required to be introduced into the reaction kettle are calculated. The set parameters are issued to the two mass flow meters of channel 2.

[0042] (4) Open the sampling valve of channel 3, and the sampling pump extracts the filtered sample into the electrode flow cell. After a period of time, the electrode measurement value is stable, the current oxygen content data is recorded, the sampling pump and the sampling valve are closed, and the nitrogen and air flow rates required to be introduced into the reaction kettle are calculated. The set parameters are issued to the two mass flow meters of channel 3.

[0043] (5) Open the sampling valve of channel 4, and the sampling pump extracts the filtered sample into the electrode flow cell; after a period of time, the current oxygen content data is recorded when the electrode measurement value is stable, the sampling pump and the sampling valve are closed, and the nitrogen gas and air flow rates required to be introduced into the No. 4 reactor are calculated, and the set parameters are issued to the two mass flow meters of channel 4.

[0044] (6) Open the peristaltic pump to empty the accumulated liquid in the filter.

[0045] (7) Repeat steps (1) to (6).

[0046] The system provided by the embodiment is used for synthesizing ternary precursors, and can improve the control precision of oxygen content and help improve the production yield.

[0047] In summary, the oxygen content monitoring device and the system for synthesizing ternary precursors are provided. The oxygen content monitoring device provided by the utility model has two electrodes of fluorescent oxygen electrode and polarographic oxygen electrode, and the flow cell corresponding to the fluorescent oxygen electrode is inclined and inverted, which can meet different needs of customers and improve the accuracy of detection results. The system for synthesizing ternary precursors provided by the utility model helps improve the control precision of oxygen content in the production process, thereby helping improve the production yield.

[0048] Therefore, the utility model effectively overcomes various shortcomings in the prior art and has high industrial utilization value.

[0049] The above embodiments only exemplarily illustrate the principles and effects of the utility model, and are not used to limit the utility model. Any person skilled in the art can modify or change the above embodiments without departing from the spirit and scope of the utility model. Therefore, all equivalent modifications or changes completed by those skilled in the art without departing from the spirit and technical thought disclosed by the utility model should be covered by the claims of the utility model.

Claims

1. An oxygen content monitoring device, characterized by, The oxygen content monitoring device comprises a shell, a first flow cell, a second flow cell, a fluorescent oxygen electrode and a polarographic oxygen electrode, the first flow cell and the second flow cell are arranged on the shell in a spaced manner, the fluorescent oxygen electrode is arranged in the first flow cell, the polarographic oxygen electrode is arranged in the second flow cell, and the first flow cell is inclined and inverted.

2. The oxygen content monitoring apparatus according to claim 1, characterized by The first flow cell and the second flow cell are connected to each other through a pipeline.

3. The oxygen content monitoring apparatus of claim 1, wherein The oxygen content monitoring device is further provided with a sampling pump and a filter, the sampling pump is communicated with the first flow cell and the second flow cell through the filter.

4. The oxygen content monitoring apparatus according to claim 3, characterized by The oxygen content monitoring device further comprises a peristaltic pump which is communicated with the filter and is used for discharging the liquid in the filter.

5. The oxygen content monitoring apparatus of claim 1, wherein The oxygen content monitoring device further comprises a display which is electrically connected with the fluorescent oxygen electrode and the polarographic oxygen electrode, and a cover which is openably and closably connected with the shell, and the cover is provided with a transparent observation window corresponding to the display.

6. The oxygen content monitoring apparatus of claim 1, wherein The oxygen content monitoring device further comprises a support which is arranged at the bottom of the shell.

7. The oxygen content monitoring apparatus of claim 1, wherein The oxygen content monitoring device is further provided with a detection gas device which is used for detecting whether the oxygen content monitoring device is stable and / or there is abnormal air tightness, and the detection gas device is communicated with the first flow cell and the second flow cell.

8. A system for synthesizing a ternary precursor, characterized by, The system comprises a reaction kettle and the oxygen content monitoring device according to any one of claims 1 to 7, and the oxygen content monitoring device is communicated with the reaction kettle.

9. The system of claim 8, wherein, The reaction kettle is multiple, and the multiple reaction kettles are connected to the same oxygen content monitoring device through a multi-channel valve.

10. The system of claim 9, wherein, Two-way valves and mass flow meters are arranged on the feed gas pipelines of the reaction kettles.

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