H2S gas release amount detection device for sulfide electrolyte

Abstract

The utility model discloses a H2S gas release amount detection device for sulfide electrolyte, which relates to the technical field of solid-state batteries and functional materials and comprises a constant-temperature glove box, a detection mechanism is arranged on the outer side of the constant-temperature glove box, and the detection mechanism comprises a detection unit, a detection unit and a control unit, the method comprises the following steps: firstly, moving a sealed sulfide electrolyte sample to be detected onto a first gas real-time monitoring probe in a constant-temperature glove box through an openable hatch cover at the top, opening a nitrogen steel cylinder valve, feeding back H2O gas concentration by the first gas real-time monitoring probe, enabling nitrogen to pass through a first glass bottle at a certain flow rate, unsealing the sealed sample, and detecting the sulfide electrolyte sample to be detected; the second gas real-time monitoring probe begins to collect and record the real-time release amount of the H2S gas, and black precipitates begin to appear in the second glass bottle, so that the accuracy and repeatability of detecting the release amount of the H2S gas of the sulfide electrolyte are improved, and the released H2S gas is effectively treated.

Description

Technical Field

[0001] This utility model relates to the field of solid-state battery and functional materials technology, specifically to a device for detecting the H2S gas release of sulfide electrolytes. Background Technology

[0002] Sulfide electrolytes are unstable in air, especially when they react with trace amounts of water (H2O) in the air, which damages the electrolyte structure, reduces its conductivity, and releases a flammable, rotten egg-smelling, and toxic gas called hydrogen sulfide.

[0003] According to the patent titled "A Device for Detecting H2S Release from Sulfides" (Patent Publication No.: CN208476718U, Patent Publication Date: 2019-02-05), the device includes a constant temperature and humidity chamber and a built-in sealed chamber inside the chamber. The constant temperature and humidity chamber has an operating window. A gas probe and a real-time monitoring probe are installed on the inner wall of the built-in sealed chamber. A cover is installed on the top. A platform is installed at the bottom for placing a sealed sample stage, and a fan is installed inside the platform. The sealed sample stage has an openable and closable top cover. The constant temperature and humidity chamber can accurately and quickly simulate different temperature and humidity environments. The testing device is fully sealed, and data acquisition is real-time and accurate, ensuring the safe use of sulfide electrolytes.

[0004] Based on the aforementioned existing technologies, current H2S gas release detection devices for sulfide electrolytes still have the following problems: existing detection technologies typically place the H2S gas detection probe next to the sample to monitor the H2S gas concentration near the probe in real time, which introduces certain errors and results in poor accuracy and repeatability. At the same time, existing detection technologies cannot effectively handle the released H2S gas, posing potential hazards to detection personnel and the environment. Furthermore, H2S gas released outdoors is toxic to most plants and animals, and can also pollute the air and water, damaging the ecosystem. Therefore, this utility model provides an H2S gas release detection device for sulfide electrolytes. Utility Model Content

[0005] To address the shortcomings of existing technologies, this invention provides a device for detecting H2S gas release from sulfide electrolytes. This device solves the following problems associated with existing H2S gas release detection devices for sulfide electrolytes: Existing detection technologies typically place the H2S gas detection probe next to the sample to monitor the H2S gas concentration near the probe in real time, which introduces errors and results in poor accuracy and repeatability. Furthermore, existing detection technologies cannot effectively handle released H2S gas, posing potential hazards to testing personnel and the environment. In addition, H2S gas released outdoors is toxic to most plants and animals, pollutes the air and water, and damages ecosystems.

[0006] To achieve the above objectives, this utility model provides the following technical solution: a device for detecting the H2S gas release of sulfide electrolytes, comprising a constant-temperature glove box, wherein a detection mechanism is provided on the outside of the constant-temperature glove box to improve the accuracy and repeatability of detecting the H2S gas release of sulfide electrolytes and to effectively process the released H2S gas. The detection mechanism includes:

[0007] The detection unit, located on the outside of the constant temperature glove box, includes a first real-time gas monitoring probe fixedly installed on the left side of the constant temperature glove box via a conduit. A first glass bottle is fixedly connected to the left side of the first real-time gas monitoring probe via an inverted hanging mechanism, and a connecting pipe is fixedly installed on the left side of the constant temperature glove box. A second real-time gas monitoring probe is fixedly installed on the right side of the constant temperature glove box, and a second glass bottle is fixedly connected to the second real-time gas monitoring probe via a conduit. A third glass bottle is fixedly connected to the right side of the second glass bottle via a conduit. The first real-time gas monitoring probe on the left side of the constant temperature glove box accurately detects the concentration of water vapor and nitrogen, while the second real-time gas monitoring probe on the right side of the constant temperature glove box accurately detects the concentration of H2S gas. The H2S gas released by the sulfide electrolyte is completely absorbed by the Pb(CH3COO)2 solution in the second glass bottle.

[0008] The simulation unit is located inside the temperature-controlled glove box and is used to simulate the sloshing of sulfide electrolytes during movement.

[0009] Preferably, the temperature-controlled glove box has an openable cover on top, and an operating window is provided on the top of the cover. A rubber glove is provided on the operating window to facilitate the operation of test samples in a closed system. A temperature controller is provided on the outside of the temperature-controlled glove box.

[0010] Preferably, both the second and third glass bottles contain a Pb(CH3COO)2 solution. H2S gas reacts in the second glass bottle to form a black PbS precipitate, and the absorption of H2S gas released by the sulfide electrolyte in the second glass bottle is detected through the third glass bottle.

[0011] Preferably, the conduit and connecting pipe on the left side of the first glass bottle are both connected to a high-purity nitrogen cylinder equipped with a pressure reducing valve.

[0012] Preferably, the simulation unit includes a housing fixedly installed at the bottom of the inner cavity of a constant temperature glove box. An installation plate is fixedly installed inside the housing. A fixing rod is fixedly installed on one side of the installation plate, and a motor is fixedly installed on the other side of the installation plate. A rotating disk is fixedly installed through the middle of the installation plate and the fixing rod at the output end of the motor. A linkage rod is rotatably installed on one side of the rotating disk. A rotating shaft is rotatably installed inside the fixing rod. A set of connecting rods is fixedly installed on the surface of the rotating shaft. A sliding column is fixedly installed on the inner side of the connecting rod. The linkage rod is slidably installed on the surface of the sliding column. A turntable for placing samples is fixedly installed through the housing at the top of the rotating shaft.

[0013] Preferably, a fan is provided on the front side of the housing to accelerate the airflow speed inside the box.

[0014] This invention provides a device for detecting the H2S gas release of sulfide electrolytes. Compared with the prior art, it has the following advantages:

[0015] 1. This device for detecting H2S gas release from sulfide electrolytes, equipped with a detection unit, firstly transfers a sealed sample of the sulfide electrolyte to be tested through a top-openable cover onto a first real-time gas monitoring probe in a constant-temperature glove box. Simultaneously, the fan and thermostat are activated, and the nitrogen cylinder valve is opened. The first real-time gas monitoring probe provides feedback on the H2O gas concentration, and nitrogen flows through the first glass bottle at a certain flow rate. After the humidity and temperature inside the box stabilize, the sealed sample is opened, and the second real-time gas monitoring probe begins to collect and record the real-time release of H2S gas. Black precipitate begins to appear in the second glass bottle, thereby improving the accuracy and repeatability of detecting H2S gas release from sulfide electrolytes and effectively handling the released H2S gas.

[0016] 2. This H2S gas release detection device for sulfide electrolytes is equipped with a simulation unit. The motor drives the rotating disk to rotate, and the rotating disk drives the linkage rod to rotate circumferentially. While rotating, the linkage rod slides on the surface of the sliding column. The linkage rod drives the rotating shaft to rotate back and forth through the connecting rod. The rotating shaft drives the sample to be tested on the rotating disk to shake back and forth, thereby simulating the H2S gas release during the movement of sulfide electrolytes. Attached Figure Description

[0017] Figure 1 This is a frontal perspective view of the three-dimensional structure of this utility model;

[0018] Figure 2 This is a cross-sectional perspective view of the present invention.

[0019] Figure 3 This is a three-dimensional structural diagram of the simulation unit of this utility model;

[0020] Figure 4 This is a cross-sectional three-dimensional structural diagram of the simulation unit of this utility model.

[0021] In the diagram: 1-Constant temperature glove box, 2-Detection mechanism, 21-Detection unit, 211-First gas real-time monitoring probe, 212-First glass bottle, 213-Second gas real-time monitoring probe, 214-Second glass bottle, 215-Third glass bottle, 216-Connecting pipe, 22-Simulation unit, 221-Housing, 222-Fan, 223-Mounting plate, 224-Fixing rod, 225-Motor, 226-Rotating disk, 227-Linkage rod, 228-Rotating shaft, 229-Connecting rod, 2210-Sliding column. Detailed Implementation

[0022] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0023] Please see Figures 1-4 This utility model provides a technical solution:

[0024] A device for detecting H2S gas release from sulfide electrolytes includes a constant-temperature glove box 1. A detection mechanism 2 is installed on the outside of the constant-temperature glove box 1 to improve the accuracy and repeatability of detecting H2S gas release from sulfide electrolytes and to effectively handle the released H2S gas. The detection mechanism 2 includes:

[0025] The detection unit 21 is located on the outside of the constant temperature glove box 1. It includes a first gas real-time monitoring probe 211 fixedly installed on the left side of the constant temperature glove box 1 via a conduit. A first glass bottle 212 is fixedly connected to the left side of the first gas real-time monitoring probe 211 via an inverted connection. A connecting pipe 216 is fixedly installed on the left side of the constant temperature glove box 1. A second gas real-time monitoring probe 213 is fixedly installed on the right side of the constant temperature glove box 1. A second glass bottle 214 is fixedly connected to the second gas real-time monitoring probe 213 via a conduit. A third glass bottle 215 is fixedly connected to the right side of the second glass bottle 214 via a conduit. The first gas real-time monitoring probe 211 on the left side of the constant temperature glove box 1 accurately detects the concentration of water vapor and nitrogen. The second gas real-time monitoring probe 213 on the right side of the constant temperature glove box 1 accurately detects the concentration of H2S gas. The H2S gas released by the sulfide electrolyte is completely absorbed by the Pb(CH3COO)2 solution in the second glass bottle 214.

[0026] The simulation unit 22 is located inside the constant temperature glove box 1 and is used to simulate the shaking of the sulfide electrolyte during movement.

[0027] First, the sealed sulfide electrolyte sample to be tested is transferred through the top openable cover onto the first gas real-time monitoring probe 211 in the constant temperature glove box 1. At the same time, the fan 222 and the constant temperature controller are started, and the nitrogen cylinder valve is opened. The first gas real-time monitoring probe 211 reports the H2O gas concentration, and nitrogen flows through the first glass bottle 212 at a certain flow rate. After the humidity and temperature inside the box stabilize, the sealed sample is opened, and the second gas real-time monitoring probe 213 begins to collect and record the real-time release of H2S gas. Black precipitate begins to appear in the second glass bottle 214, thereby improving the accuracy and repeatability of detecting the H2S gas release of the sulfide electrolyte and effectively handling the released H2S gas.

[0028] In this embodiment, the top of the constant temperature glove box 1 is provided with an openable cover, and the top of the cover is provided with an operating window. Rubber gloves are provided on the operating window to facilitate the operation of test samples in a closed system. A constant temperature controller is provided on the outside of the constant temperature glove box 1.

[0029] The thermostat can simulate atmospheres with different temperatures and humidity levels, accurately detect the amount of H2S released, and completely absorb the H2S gas generated during the test. It has excellent detection accuracy and environmental friendliness, providing a guarantee for the safe and efficient detection of sulfide electrolytes.

[0030] The first gas real-time monitoring probe 211 can monitor water vapor concentration and has wireless transmission capabilities, enabling it to transmit the detected data to a wirelessly connected computer in real time for data recording and analysis.

[0031] The constant temperature glove box 1 can control the temperature environment of the sulfide electrolyte exposed to moisture by a constant temperature controller set on the outside, and adjust the opening of the pressure reducing valve connected to the first gas real-time monitoring probe 211 near the left side of the constant temperature glove box 1 according to the water vapor gas concentration, thereby controlling the humidity environment of the sulfide electrolyte exposed to moisture.

[0032] In this embodiment, both the second glass bottle 214 and the third glass bottle 215 contain Pb(CH3COO)2 solution. H2S gas reacts in the second glass bottle 214 to form a black PbS precipitate. The absorption of H2S gas released by the sulfide electrolyte in the second glass bottle 214 is detected by the third glass bottle 215.

[0033] The reaction formula for H2S gas in the second glass bottle 214 is:

[0034] Pb(CH3 COO)2+H2S→PbS↓+2CH3COOH

[0035] In this embodiment, the conduit and connecting pipe 216 on the left side of the first glass bottle 212 are both connected to a high-purity nitrogen cylinder equipped with a pressure reducing valve.

[0036] All tubing is made of glass, and the high-purity nitrogen cylinders with pressure reducing valves have a nitrogen purity of 99.999%.

[0037] The liquid filling capacity of all glass bottles is 10%-99% of their volume, preferably 50%-80%, ensuring that the liquid level exceeds the long straight glass conduit but does not exceed the short straight glass conduit.

[0038] The probe on the left side of the constant temperature glove box 1 can accurately detect the concentration of water vapor and nitrogen, while the probe on the right side of the glove box can accurately detect the concentration of H2S gas.

[0039] In this embodiment, the simulation unit 22 includes a housing 221 fixedly installed at the bottom of the inner cavity of the constant temperature glove box 1. An installation plate 223 is fixedly installed inside the housing 221. A fixing rod 224 is fixedly installed on one side of the installation plate 223, and a motor 225 is fixedly installed on the other side of the installation plate 223. A rotating disk 226 is fixedly installed through the middle of the installation plate 223 and the fixing rod 224 at the output end of the motor 225. A linkage rod 227 is rotatably installed on one side of the rotating disk 226. A rotating shaft 228 is rotatably installed inside the fixing rod 224. A set of connecting rods 229 is fixedly installed on the surface of the rotating shaft 228. A sliding column 2210 is fixedly installed on the inner side of the connecting rod 229. The linkage rod 227 is slidably installed on the surface of the sliding column 2210. A turntable for placing samples is fixedly installed through the housing 221 at the top end of the rotating shaft 228.

[0040] The motor 225 drives the rotating disk 226 to rotate, and the rotating disk 226 drives the linkage rod 227 to rotate in a circle. While rotating, the linkage rod 227 slides on the surface of the sliding column 2210. The linkage rod 227 drives the rotating shaft 228 to rotate back and forth through the connecting rod 229. The rotating shaft 228 drives the sample to be tested on the rotating disk to shake back and forth, thereby simulating the H2S gas release during the movement of sulfide electrolyte.

[0041] In this embodiment, a fan 222 is provided on the front side of the housing 221 to accelerate the airflow speed inside the box.

[0042] The fan 222, located on the front side of the housing 221, is used to accelerate the airflow speed inside the chamber, which helps to improve the accuracy of the detection.

[0043] Furthermore, any content not described in detail in this specification is existing technology known to those skilled in the art.

[0044] During operation, the sealed sulfide electrolyte sample to be tested is first moved into the turntable in the constant temperature glove box 1 through the top openable cover, and at the same time the fan 222 and the constant temperature controller are started.

[0045] Next, the nitrogen cylinder valve is opened, and the opening of the pressure reducing valve connected to this side is adjusted according to the H2O gas concentration fed back by the first gas real-time monitoring probe 211, so that nitrogen gas passes through the first glass bottle 212 containing H2O liquid at a certain flow rate.

[0046] After the humidity and temperature inside the chamber stabilize, the sealed sample is opened. Simultaneously, motor 225 drives rotating disk 226 to rotate, which in turn drives linkage rod 227 to rotate circumferentially. While rotating, the disk slides on the surface of sliding column 2210. Linkage rod 227 drives rotating shaft 228 to reciprocate via connecting rod 229. Rotating shaft 228 causes the sample to be tested on the turntable to oscillate back and forth. At this time, the second real-time gas monitoring probe 213 begins to collect and record the real-time release of H2S gas. Black precipitate begins to appear in the second glass bottle 214 containing Pb(CH3COO)2 solution, while no obvious change is observed in the third glass bottle 215.

[0047] After a unit time, the nitrogen cylinder valve is closed, and all detection and control systems are shut down. The contents in 214 are filtered, washed with water, washed with alcohol, and dried. The resulting black precipitate is weighed and recorded, and the total H2S gas release per unit time is calculated.

[0048] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0049] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A device for detecting H2S gas release from sulfide electrolytes, comprising a constant temperature glove box (1), characterized in that: The constant temperature glove box (1) is equipped with a detection mechanism (2) on its outer side to improve the accuracy and repeatability of detecting the H2S gas release of sulfide electrolytes and to effectively handle the released H2S gas. The detection mechanism (2) includes: The detection unit (21) is located on the outside of the constant temperature glove box (1), including a first gas real-time monitoring probe (211) fixedly installed on the left side of the constant temperature glove box (1) via a conduit, and a first glass bottle (212) is fixedly connected to the left side of the first gas real-time monitoring probe (211) via an inverted hanging method, and a connecting pipe (216) is fixedly installed on the left side of the constant temperature glove box (1), and a second gas real-time monitoring probe (213) is fixedly installed on the right side of the constant temperature glove box (1), and the second gas real-time monitoring probe (213) is connected to the first glass bottle (212) via a conduit. A second glass bottle (214) is fixedly connected to the tube. A third glass bottle (215) is fixedly connected to the right side of the second glass bottle (214) via a conduit. The concentrations of water vapor and nitrogen are accurately detected by the first real-time gas monitoring probe (211) on the left side of the constant temperature glove box (1). The concentration of H2S gas is accurately detected by the second real-time gas monitoring probe (213) on the right side of the constant temperature glove box (1). The H2S gas released by the sulfide electrolyte is completely absorbed by the Pb(CH3COO)2 solution in the second glass bottle (214). The simulation unit (22) is located inside the constant temperature glove box (1) and is used to simulate the shaking of the sulfide electrolyte during movement.

2. The H2S gas release detection device for sulfide electrolytes according to claim 1, characterized in that: The thermostatic glove box (1) is provided with an openable cover on the top, and an operation window is provided on the top of the cover. Rubber gloves are provided on the operation window to facilitate the operation of test samples in a closed system. A thermostatic controller is provided on the outside of the thermostatic glove box (1).

3. The H2S gas release detection device for sulfide electrolytes according to claim 1, characterized in that: The second glass bottle (214) and the third glass bottle (215) are both filled with Pb(CH3COO)2 solution. H2S gas reacts in the second glass bottle (214) to form a black PbS precipitate. The absorption of H2S gas released by the sulfide electrolyte in the second glass bottle (214) is detected by the third glass bottle (215).

4. The H2S gas release detection device for sulfide electrolytes according to claim 1, characterized in that: The conduit and connecting pipe (216) on the left side of the first glass bottle (212) are both connected to a high-purity nitrogen cylinder with a pressure reducing valve.

5. The H2S gas release detection device for sulfide electrolytes according to claim 1, characterized in that: The simulation unit (22) includes a housing (221) fixedly installed at the bottom of the inner cavity of the constant temperature glove box (1). An installation plate (223) is fixedly installed inside the housing (221). A fixing rod (224) is fixedly installed on one side of the installation plate (223), and a motor (225) is fixedly installed on the other side of the installation plate (223). A rotating disk (226) is fixedly installed at the output end of the motor (225) through the space between the installation plate (223) and the fixing rod (224). A linkage rod (227) is rotatably mounted on one side of the rotating disk (226). A rotating shaft (228) is rotatably mounted inside the fixed rod (224). A set of connecting rods (229) is fixedly mounted on the surface of the rotating shaft (228). A sliding column (2210) is fixedly mounted on the inner side of the connecting rod (229). The linkage rod (227) is slidably mounted on the surface of the sliding column (2210). The top of the rotating shaft (228) is fixedly mounted with a turntable through the housing (221) for placing samples.

6. The H2S gas release detection device for sulfide electrolytes according to claim 5, characterized in that: A fan (222) is provided on the front side of the housing (221) to accelerate the airflow speed inside the box.

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