Gas production testing device

Abstract

The utility model provides a gas production testing device. The gas production testing device comprises a tank body, a stirring mechanism, a constant temperature mechanism, a gas measuring mechanism and a vacuumizing mechanism, according to the gas production testing device, by arranging the stirring mechanism, the constant temperature mechanism, the vacuumizing mechanism, the gas measuring mechanism and other structures, real-time monitoring of the gas production rate can be achieved under the condition that the actual production working conditions (including the stirring process, the constant temperature process and the like) are restored as much as possible, data can be automatically recorded and exported, and the working efficiency is improved. And then calculating by combining an ideal gas state equation to obtain an accurate gas production volume so as to complete quantitative analysis of the gas. In addition, the gas production testing device is further provided with a gas component analyzer, components of the produced gas can be detected, and qualitative analysis of the gas is completed.

Description

Technical Field

[0001] The present application relates to the technical field of gas analysis, and in particular to a gas production testing device. Background Art

[0002] Silicon-based negative electrode materials, such as pre-lithium silicon oxide, gas-phase silicon carbon, etc., may produce gas in aqueous slurry, which may cause quality problems of the electrode such as electrode pinholes, pits, uneven surface density, poor bonding, etc., which greatly affect the application of silicon-based negative electrode materials. Therefore, the gas production evaluation of silicon-based negative electrode material products has become an important indicator for evaluating such products.

[0003] At present, the assessment of gas production in battery factories and material factories is relatively rough, generally including visual inspection, drainage method and syringe method. Visual inspection method: After the negative electrode material is made into a water-based slurry, it is placed in a beaker and observed by naked eye to see if bubbles are generated. Drainage method: The homogenized silicon negative electrode slurry is encapsulated in an aluminum-plastic film, and the volume change is measured by the drainage method to obtain the gas production. Syringe method: The homogenized silicon negative electrode slurry is drawn into a syringe and the syringe is blocked. The generated gas pushes the syringe, and the gas production is obtained by reading the gas production volume.

[0004] However, the visual method is more subjective and lacks quantitative indicators, and it is impossible to measure the actual gas production. The drainage method requires multiple drainage volume measurements, the test interval is long, and the slurry is prone to sinking to the bottom. It cannot truly simulate the homogenization state in actual production, and requires a lot of manual operation and readings. The process is complicated and the test error is large. Although the syringe method is easy to read, the test accuracy is low due to the poor air tightness of the syringe, and there is also the problem of slurry sinking to the bottom. Utility Model Content

[0005] In view of this, the present application proposes a gas production testing device to solve the problem that the gas production evaluation method in the prior art cannot accurately detect the gas production volume.

[0006] One embodiment of the present application proposes a gas production testing device, including a tank body, a stirring mechanism, a constant temperature mechanism, a gas measuring mechanism and a vacuum mechanism. The tank body includes a side wall and a bottom wall, and the side wall and the bottom wall together form a cavity. Part of the stirring mechanism is located in the cavity, and the other part is located outside the cavity. The constant temperature mechanism includes a liquid inlet, a liquid outlet and a flow channel, and the liquid inlet and the liquid outlet are both provided on the tank body. The flow channel is provided inside the side wall and / or the bottom wall, and the flow channel is connected to the liquid inlet and the liquid outlet. The gas measuring mechanism is provided on the tank body and connected to the cavity, and the gas measuring mechanism is used to measure the pressure in the cavity. The vacuum mechanism is provided on the tank body and connected to the cavity.

[0007] In one embodiment, the gas measuring mechanism includes a first pipeline and a pressure gauge connected to the first pipeline, and the first pipeline is arranged on the tank body and communicated with the cavity.

[0008] In one embodiment, the gas measurement mechanism further includes a data collector connected to the pressure gauge.

[0009] In one embodiment, the vacuum pumping mechanism includes a second pipe and a vacuum pump connected to the second pipe, and the second pipe is arranged on the tank body and communicated with the cavity.

[0010] In one embodiment, the gas production testing device further includes a gas composition analyzer, and the gas composition analyzer is connected to the cavity.

[0011] In one embodiment, the second pipeline includes a main pipeline, a first branch conduit, and a second branch conduit that are connected. One end of the main pipeline is arranged on the tank body and is connected to the cavity, and the other end of the main pipeline is connected to the first branch conduit and the second branch conduit. One end of the first branch conduit away from the main pipeline is connected to the vacuum pump, and one end of the second branch conduit away from the main pipeline is connected to the gas composition analyzer.

[0012] In one embodiment, a first valve is disposed on the first branch conduit, and a second valve is disposed on the second branch conduit.

[0013] In one embodiment, the tank body further comprises a sealing cover, and the sealing cover is arranged at one end of the side wall away from the bottom wall to seal the cavity.

[0014] In one embodiment, the tank body further comprises a sealing ring, and the sealing ring is arranged between the sealing cover and the side wall.

[0015] In one embodiment, the stirring mechanism includes a driving member, a stirring shaft connected to the driving member, and a dispersion disk connected to the stirring shaft. The dispersion disk is located in the cavity, the driving member is located outside the cavity, and one end of the stirring shaft away from the dispersion disk passes through the cavity.

[0016] By setting up structures such as a stirring mechanism, a constant temperature mechanism, a vacuum mechanism, and a gas measuring mechanism, the present application can realize real-time monitoring of gas production under the conditions of actual production (including stirring, constant temperature, etc.), and can automatically record and export data, and then calculate in combination with the ideal gas state equation to obtain an accurate gas production volume and complete a quantitative analysis of the gas. In addition, the gas production test device of the present application is also provided with a gas composition analyzer, which can detect the composition of the generated gas and complete a qualitative analysis of the gas. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic structural diagram of a gas production testing device according to one embodiment of the present application.

[0018] Main component symbols

[0019] Gas production test device 100

[0020] Tank 10

[0021] Stirring mechanism 20

[0022] Constant temperature mechanism 30

[0023] Gas measuring mechanism 40

[0024] Vacuuming mechanism 50

[0025] Side wall 11

[0026] Bottom wall 12

[0027] Sealing cover 13

[0028] Sealing ring 14

[0029] Cavity 101

[0030] Driving member 21

[0031] Stirring shaft 22

[0032] Dispersion disc 23

[0033] Liquid inlet 31

[0034] Liquid outlet 32

[0035] Runner 33

[0036] First pipeline 41

[0037] Pressure gauge 42

[0038] Data Collector 43

[0039] Second pipeline 51

[0040] Main pipeline 511

[0041] First branch conduit 512

[0042] Second branch catheter 513

[0043] First valve 52

[0044] Second valve 53

[0045] The following specific implementation manner will further illustrate the embodiments of the present application in conjunction with the above-mentioned drawings. DETAILED DESCRIPTION

[0046] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the technical field of the present application. The terms used herein are only for the purpose of describing specific implementation methods and are not intended to limit the present application embodiments.

[0047] It should be noted that all directional indications in the embodiments of the present application (such as up, down, left, right, front, back, etc.) are only used to explain the relative position relationship, movement status, etc. between the components under a certain specific posture (as shown in the accompanying drawings). If the specific posture changes, the directional indication will also change accordingly.

[0048] It should be noted that when a component is referred to as being "fixed to" or "mounted on" another component, it can be directly on the other component or there can be a central component. When a component is considered to be "set on" another component, it can be directly set on the other component or there can be a central component at the same time.

[0049] Some embodiments of the present application are described in detail below in conjunction with the accompanying drawings. In the absence of conflict, the following embodiments and features in the embodiments can be combined with each other.

[0050] See also Figure 1 , the present application provides a gas production test device 100, which can perform quantitative and qualitative analysis on the gas production of silicon-based negative electrode aqueous homogenous slurry, and can not only accurately measure the gas production volume of the slurry, but also analyze the composition of the gas. The silicon-based negative electrode aqueous homogenous slurry may be, but is not limited to, a composite slurry of silicon oxide and graphite, the silicon oxide content may be 10%wt~30%wt, and the graphite content may be 70%wt~90%wt. Of course, the gas production test device 100 can also perform quantitative and qualitative analysis on the gas produced by other slurries. Figure 1 As shown, the gas production testing device 100 includes a tank body 10 , a stirring mechanism 20 , a constant temperature mechanism 30 , a gas measuring mechanism 40 and a vacuuming mechanism 50 .

[0051] like Figure 1As shown, the tank body 10 may be cylindrical, including a side wall 11 and a bottom wall 12. The side wall 11 and the bottom wall 12 enclose a cavity 101, and the cavity 101 can be used to contain slurry (which may be but is not limited to silicon-based negative electrode aqueous homogenized slurry). Graduation lines may be set on the side wall 11 to facilitate reading the volume of the slurry in the cavity 101. The material of the tank body 10 should be a material that does not react with the silicon-based negative electrode aqueous homogenized slurry. For example, the material of the tank body 10 may be plastic, silica gel, glass, quartz, etc. The volume of the tank body 10 may be 5L, and the volume of the aqueous slurry contained may be 2.5L to 3.5L. In other embodiments, the volume of the aqueous slurry may be adaptively adjusted according to the volume of the tank body 10.

[0052] like Figure 1 As shown, in some embodiments, the tank body 10 further includes a sealing cover 13. The sealing cover 13 may be disposed at one end of the side wall 11 away from the bottom wall 12, and its shape is adapted to the opening of the cavity 101 to seal the cavity 101. Further, the tank body 10 may further include a sealing ring 14, which may be disposed between the sealing cover 13 and the side wall 11 to further improve the airtightness of the cavity 101. The material of the sealing cover 13 may be, but not limited to, plastic, silica gel, glass, quartz, etc. The material of the sealing ring 14 may be, but not limited to, rubber, graphite, polytetrafluoroethylene, etc.

[0053] like Figure 1 As shown, part of the stirring mechanism 20 is located in the cavity 101, and the other part is located outside the cavity 101. The stirring mechanism 20 is used to stir the slurry sample (which may be but is not limited to silicon-based negative electrode aqueous homogenous slurry) in the cavity 101 to prevent the slurry from sinking to the bottom and keep the slurry in a homogenous state.

[0054] In some embodiments, the stirring mechanism 20 may include a driving member 21, a stirring shaft 22 connected to the driving member, and a dispersion disk 23 connected to the stirring shaft 22. That is, the stirring shaft 22 is located between the driving member 21 and the dispersion disk 23, one end of the stirring shaft 22 is connected to the driving member 21, and the other end is connected to the dispersion disk 23. The dispersion disk 23 is located in the cavity 101, and the driving member 21 is located outside the cavity 101. Part of the stirring shaft 22 is located in the cavity 101, and part is located outside the cavity 102, wherein one end of the stirring shaft 22 away from the dispersion disk 23 passes through the cavity 101. The driving member 21 may be, but is not limited to, a motor, and its rotation speed may be 2000r / min to 10000r / min. The dispersion disk 23 may be roughly disc-shaped, and its diameter may be more than 40mm, for example, 40mm, 50mm, 60mm, etc., which are not listed here one by one. The driving member 21 drives the stirring shaft 22 to rotate, and the stirring shaft 22 drives the dispersion disk 23 to rotate. The dispersion disk 23 stirs the slurry to prevent it from sinking to the bottom, thereby maintaining the slurry in a homogenous state.

[0055] like Figure 1As shown, the constant temperature mechanism 30 includes a liquid inlet 31, a liquid outlet 32 ​​and a flow channel 33. The liquid inlet 31 and the liquid outlet 32 ​​are both arranged on the tank body 10. In this embodiment, the liquid inlet 31 is arranged on one end of the side wall 11 close to the bottom wall 12, and the liquid outlet 32 ​​is arranged on one end of the side wall 11 close to the sealing cover 13. The liquid inlet 31 can be used to connect the liquid inlet pipeline (not shown in the figure), and the liquid outlet 32 ​​can be used to connect the liquid outlet pipeline (not shown in the figure). The flow channel 33 can be arranged inside the side wall 11, or inside the side wall 11 and the bottom wall 12, or inside the bottom wall 12. One end of the flow channel 33 is connected to the liquid inlet 31, and the other end is connected to the liquid outlet 32. By introducing a cooling medium (which can be but is not limited to water) into the constant temperature mechanism 30, the temperature (15°C to 25°C) inside the tank body 10 can be kept relatively stable. For example, the liquid inlet 31 may be connected to a water inlet pipe of a water chiller, and the liquid outlet 32 ​​may be connected to a water outlet pipe of the water chiller. Water flows into the flow channel 33 through the liquid inlet 31 and then flows out to the liquid outlet 32 ​​.

[0056] like Figure 1 As shown, the gas measuring mechanism 40 is provided on the tank body 10 and communicated with the cavity 101, and the gas measuring mechanism 40 is used to measure the pressure in the cavity 101. In some embodiments, the gas measuring mechanism 40 includes a first pipe 41 and a pressure gauge 42 connected to the first pipe 41, and the first pipe 41 is provided on the tank body 10 and communicated with the cavity 101. The first pipe 41 penetrates the sealing cover 13 and the sealing ring 14 along the thickness direction of the sealing cover 13, so as to be able to communicate with the cavity 101. The pressure gauge 42 is located outside the cavity 101, and the pressure gauge 42 is connected to one end of the first pipe 41 away from the cavity 101. The pressure gauge 42 can provide real-time feedback on the change of the amount of gas inside the tank body 10.

[0057] Furthermore, if Figure 1 As shown, the gas measurement mechanism 40 may further include a data collector 43 connected to the pressure gauge 42, and the data collector 43 is located outside the cavity 101. The data collector 43 may be a voltage recorder data collector, whose response voltage is linearly related to the air pressure curve, and the air pressure can be calculated by the voltage, which is convenient for reading and data storage and recording.

[0058] like Figure 1 As shown, the vacuum mechanism 50 is disposed on the tank 10 and communicated with the cavity 101. The vacuum mechanism 50 is used to vacuum the cavity 101, and the vacuum degree in the cavity 101 (the value obtained by subtracting the atmospheric pressure from the air pressure in the cavity) can be -0.04 kpa to -0.10 kpa.

[0059] In some embodiments, Figure 1As shown, the vacuum mechanism 50 includes a second pipe 51 and a vacuum pump (not shown) connected to the second pipe 51. The second pipe 51 is arranged on the tank body 10 and communicates with the cavity 101. The second pipe 51 penetrates the sealing cover 13 and the sealing ring 14 along the thickness direction of the sealing cover 13.

[0060] In some embodiments, Figure 1 As shown, the gas production test device 100 also includes a gas composition analyzer (not shown), which is connected to the cavity 101. The gas composition analyzer can be a laser Raman spectrometer gas analyzer, which can quickly respond to and analyze multiple gas components such as H2, N2, O2, CO, CO2, CH4, C2H2, C3H8, H2S, etc., with a measurement accuracy of ≤±1% FS. In some embodiments, the gas composition analyzer can be connected to the cavity 101 through an independent third pipeline (not shown), and the third pipeline can penetrate the sealing cover 13 and the sealing ring 14 along the thickness direction of the sealing cover 13.

[0061] In some embodiments, Figure 1 As shown, the gas composition analyzer can also be connected to the cavity 101 through the second pipe 51. In this embodiment, the second pipe 51 can be roughly "Y"-shaped, and can include a main pipe 511, a first branch pipe 512, and a second branch pipe 516 that are connected. One end of the main pipe 511 passes through the sealing cover 13 and the sealing ring 14 along the thickness direction of the sealing cover 13, so as to be connected to the cavity 101, and the other end of the main pipe 511 is connected to the first branch pipe 512 and the second branch pipe 513. The end of the first branch pipe 512 away from the main pipe 511 is connected to the vacuum pump, and the end of the second branch pipe 513 away from the main pipe 511 is connected to the gas composition analyzer.

[0062] Furthermore, if Figure 1 As shown, a first valve 52 is provided on the first branch conduit 512, and a second valve 53 is provided on the second branch conduit 513. The first valve 52 can control whether the first branch conduit 512 is in communication with the main conduit 511, thereby controlling whether the first branch conduit 512 is in communication with the cavity 101. The second valve 53 can control whether the second branch conduit 513 is in communication with the main conduit 511, thereby controlling whether the second branch conduit 513 is in communication with the cavity 101.

[0063] The following will introduce the steps of the gas generation test device 100 for performing a gas generation test on a silicon-based negative electrode aqueous slurry.

[0064] A composite slurry (volume can be 2.5L) of silicon dioxide (10%wt) and graphite (90%wt) is prepared in a tank body 10 (volume can be 5L). The volume of the slurry is read as V0 through the scale inside the tank body 10, and the volume of the tank body 10 can be recorded as V.

[0065] The sealing cover 13 is covered, the first valve 52 is opened, and the second valve 53 is closed. The vacuum pump is turned on to evacuate the cavity 101, and when the vacuum degree in the cavity 101 reaches -0.04 kPa, the first valve 52 is closed, and the vacuum pump is turned off.

[0066] The liquid inlet 31 is connected to the water inlet pipe of the chiller, and the liquid outlet 32 ​​is connected to the water outlet pipe of the chiller, and the constant temperature is set to 15°C.

[0067] Turn on the driving member (electrode) of the stirring mechanism 40 to make the dispersion disk 23 (whose diameter can be 40 mm) stir (the speed can be 2000 r / min). Turn on the pressure gauge 42 and the data acquisition device 43 to record the pressure gauge value. The data acquisition step can be 1 time / min. The stirring can be continued for 24 hours and then the data can be exported.

[0068] After completing the above operations, the amount of gas generated during the stirring process, n (mol), is calculated by the ideal gas state equation "Formula 1, P1V1 = nRT". In Formula 1, P1 is the difference between the real-time reading and the initial reading of the pressure gauge, in Pa; V1 = V-V0, in L; R is the molar gas constant, i.e. 8.314 J / (mol·K); T is the constant temperature set in the tank 10, in K.

[0069] Then, the volume V2 of the generated gas under atmospheric pressure is calculated by the ideal gas state equation "Formula 2, P2V2 = nRT". In Formula 2, V2 is the volume of the generated gas under atmospheric pressure, in L; P2 is the atmospheric pressure, i.e. 10 5 Pa; n is the amount of gas calculated by Formula 1, in mol; R is the molar gas constant, i.e. 8.314 J / (mol·K); T is the constant temperature set in the tank body 10, in K.

[0070] The gas production test device 100 of the present application is provided with a stirring mechanism 20, a constant temperature mechanism 30, a vacuum mechanism 50 and a gas measuring mechanism 40 and other structures, and can realize real-time monitoring of gas production under the working conditions (including stirring, constant temperature and other processes) that are restored as much as possible to the actual production conditions, and can automatically record and export data, and then calculate in combination with the ideal gas state equation to obtain an accurate gas production volume and complete the quantitative analysis of the gas. In addition, the gas production test device 100 of the present application is also provided with a gas composition analyzer that can detect the composition of the generated gas and complete the qualitative analysis of the gas.

[0071] The above descriptions are some specific implementations of the present application, but they are not limited to these implementations in actual application. For ordinary technicians in this field, other variations and changes made according to the technical concept of the present application should all fall within the protection scope of the present application.

Claims

1. A gas production testing device, characterized in that: include: The tank body comprises a side wall and a bottom wall, wherein the side wall and the bottom wall together form a cavity; a stirring mechanism, wherein a portion of the stirring mechanism is located in the cavity and another portion of the stirring mechanism is located outside the cavity; A constant temperature mechanism, comprising a liquid inlet, a liquid outlet and a flow channel, wherein the liquid inlet and the liquid outlet are both arranged on the tank body, the flow channel is arranged inside the side wall and / or the bottom wall, and the flow channel is communicated with the liquid inlet and the liquid outlet; a gas measuring mechanism, disposed on the tank body and connected to the cavity, the gas measuring mechanism being used to measure the pressure in the cavity; and The vacuum pumping mechanism is arranged on the tank body and communicated with the cavity.

2. The gas production testing device according to claim 1, characterized in that: The gas measuring mechanism comprises a first pipeline and a pressure gauge connected to the first pipeline, wherein the first pipeline is arranged on the tank body and communicated with the cavity.

3. The gas production testing device according to claim 2, characterized in that: The gas measurement mechanism also includes a data collector connected to the pressure gauge.

4. The gas production testing device according to claim 1, characterized in that: The vacuum pumping mechanism includes a second pipeline and a vacuum pump connected to the second pipeline, wherein the second pipeline is arranged on the tank body and communicated with the cavity.

5. The gas production testing device according to claim 4, characterized in that: The gas production testing device further comprises a gas composition analyzer, and the gas composition analyzer is communicated with the cavity.

6. The gas production testing device according to claim 5, characterized in that: The second pipeline includes a main pipeline, a first branch conduit and a second branch conduit that are connected, one end of the main pipeline is arranged on the tank body and connected to the cavity, and the other end of the main pipeline is connected to the first branch conduit and the second branch conduit; One end of the first branch conduit away from the main conduit is connected to the vacuum pump, and one end of the second branch conduit away from the main conduit is connected to the gas composition analyzer.

7. The gas production testing device according to claim 6, characterized in that: The first branch conduit is provided with a first valve, and the second branch conduit is provided with a second valve.

8. The gas production testing device according to claim 1, characterized in that: The tank body further comprises a sealing cover, which is arranged at one end of the side wall away from the bottom wall to seal the cavity.

9. The gas production testing device according to claim 8, characterized in that: The tank body further comprises a sealing ring, and the sealing ring is arranged between the sealing cover and the side wall.

10. The gas production testing device according to claim 1, characterized in that: The stirring mechanism includes a driving member, a stirring shaft connected to the driving member, and a dispersion disk connected to the stirring shaft, the dispersion disk is located in the cavity, the driving member is located outside the cavity, and one end of the stirring shaft away from the dispersion disk passes through the cavity.

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