Full-automatic hydrogen storage adsorption instrument with cycle life testing function

Abstract

The invention discloses a full-automatic hydrogen storage adsorption instrument with a cycle life testing function. Wherein the upper and lower ends of the lifting device are fixed with the shell and drive the temperature control device to move up and down, the sample chamber is suspended below a top plate of the shell, and the sample chamber directly faces a sample insertion hole of the temperature control device; a sample containing part is formed in the center of the top end of the copper heat sink, and a cylindrical water containing cavity is defined by the copper heat sink and the shell on the outer side; a heating rod is arranged in the copper heat sink, and a thermocouple connected with a control system is mounted in the copper heat sink; cooling air channels are uniformly formed in the copper heat sink, and the two ends of each cooling air channel are connected with inflation equipment through an air inlet and an air outlet respectively; the control system comprises a cooling module. The integrated design of the water bath and the heating furnace is adopted, so that the trouble of replacing the water bath and the heating furnace is avoided, and accurate temperature control can be realized in different temperature intervals.

Description

Technical Field

[0001] The present invention belongs to the technical field of equipment for analyzing gas materials by measuring gas pressure, and in particular is a full-automatic hydrogen storage adsorption instrument with a cycle life test function. Background Art

[0002] In the hydrogen energy industry chain, the safe storage and transportation of hydrogen has always been a bottleneck restricting the development of the industry. Compared with the currently commonly used high-pressure gaseous hydrogen storage and transportation technology, solid-state hydrogen storage technology has the advantages of low hydrogen storage pressure, high hydrogen storage density, and high safety. It is considered to be one of the advantageous technologies for high-density and high-safety storage and transportation of hydrogen. The hydrogen storage adsorption instrument and the cycle life tester are precision instruments for standardizing the PCT curve and cycle life of hydrogen storage materials, respectively. Both generally use the internationally accepted Sieverts isochoric method to test the hydrogen absorption and desorption performance of hydrogen storage materials. The basic principle is to accurately measure the change in system hydrogen pressure before and after the hydrogen storage material sample absorbs / desorbs hydrogen in a closed system with a calibrated volume at a certain constant temperature, so as to test the hydrogen storage and desorption performance of hydrogen storage materials. Among them, the test of the PCT curve requires higher temperature accuracy. In the low temperature zone, the water bath method is generally used, and high-temperature activation is required at the same time. This requires the hydrogen storage adsorption instrument to be equipped with a high-temperature heating furnace and a low-temperature water bath, and can be switched in time. The cycle life test requires rapid temperature rise and fall to improve the test efficiency. The natural cooling of the heating furnace cannot meet the requirements. Summary of the invention

[0003] In view of the problems existing in the background technology, the present invention provides a fully automatic hydrogen storage adsorption instrument with a cycle life test function, and the technical solution includes: a gas circuit system, a circulating water supply device, a shell, a sample chamber, a temperature control device and a lifting device, wherein the upper and lower ends of the lifting device are fixed to the shell, and drive the temperature control device to move up and down, the sample chamber is suspended below the top plate of the shell, and the sample chamber is directly opposite to the sample insertion hole of the temperature control device;

[0004] The temperature control device comprises: a copper heat sink, a sample holding part, an air inlet, an air outlet, a shell, a water inlet, a water outlet, a heating rod and a thermocouple. The sample holding part is opened at the center of the top of the copper heat sink. The copper heat sink and the outer shell form a cylindrical water holding chamber. A water inlet communicating with the water holding chamber is provided below the side wall of the shell. A water outlet communicating with the water holding chamber is provided above the side wall of the shell. The water inlet and the water outlet are connected to an external circulating water supply device through a circulating water interface.

[0005] A plurality of heating rods are arranged in the copper heat sink, and a thermocouple connected to the control system is installed in the copper heat sink; a sample insertion hole matching the shape and size of the sample receiving part is opened on the top of the shell, and after the temperature control device rises, the sample chamber enters the sample receiving part;

[0006] Cooling air channels are evenly arranged in the copper heat sink, and both ends of the cooling water channel are connected to the charging device through the air inlet and the air outlet respectively; the control system includes a cooling module, and the cooling module is respectively connected to the thermocouple, the circulating water supply device, the charging device, the lifting device and the heating rod.

[0007] When the cooling module is working, it first determines the ambient temperature of the sample chamber and receives the temperature sent back by the thermocouple:

[0008] When the temperature sent back by the thermocouple is above 200℃, the system enters the inflation cooling mode, turns on the inflation device to fill cold air through the air inlet and discharges it from the air outlet until the temperature reaches the target temperature or 200℃, then stops inflating; then automatically enters the chiller cooling mode;

[0009] When the temperature transmitted back by the thermocouple is lower than 200℃, the chiller enters the cooling mode, the chiller starts working, cold water enters from the water inlet and is discharged into the chiller from the water outlet, forming a cycle, thereby completing the rapid cooling of the copper heat sink and the sample chamber.

[0010] The control system also includes: a temperature-raising and temperature-constant module, which is respectively connected to the thermocouple, the circulating water supply device, the lifting device and the heating rod.

[0011] The control process of the temperature rising and constant temperature module in the low temperature zone and the high temperature zone is as follows:

[0012] Heating and constant temperature low temperature zone control process: When the temperature is set in the low temperature zone, the heating rod and the chiller work at the same time, the lifting device controls the temperature control device to rise, so that the sample chamber is inserted into the copper heat sink, and cold water enters the furnace body from the water inlet and is discharged from the water outlet, taking away the heat of the copper heat sink. At the same time, the heating rod heats the copper heat sink. Under the joint action of the heating rod and the chiller, the temperature of the copper heat sink reaches a dynamic balance, so that the test can be carried out in the sample chamber;

[0013] Heating and constant temperature high temperature zone control process: When the temperature is set in the high temperature zone, the chiller does not work, and the water automatically flows back to the chiller below from the water inlet and the pipeline under the action of gravity; the heating rod works, and the lifting device controls the temperature control device to rise, so that the sample chamber is inserted into the copper heat sink. The heating rod heats the copper heat sink, and the test is carried out in the sample chamber after the temperature reaches the setting.

[0014] The low temperature zone is less than 90°C, and the high temperature zone is greater than or equal to 90°C.

[0015] The beneficial effects of the present invention are:

[0016] 1. It integrates the functions of hydrogen storage adsorption instrument and cycle life tester, and adopts the integrated design of water bath and heating furnace, which eliminates the trouble of replacing water bath and heating furnace. It can achieve precise temperature control in different temperature ranges to meet the PCT curve test of hydrogen storage materials;

[0017] 2. The combination of air cooling and water cooling can quickly increase and decrease the temperature, thus improving the efficiency of cycle life testing. The cooling air duct is set in the copper heat sink to achieve continuous operation of the cooling process during switching. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a front schematic diagram of an embodiment of a fully automatic hydrogen storage adsorption instrument with a cycle life test function of the present invention;

[0019] Figure 2 It is a side schematic diagram of a hydrogen storage adsorption instrument in an embodiment of the present invention;

[0020] Figure 3 This is a schematic diagram of the structure of a temperature control device in an embodiment of the present invention;

[0021] Figure 4 It is a partial connection diagram of the control system in an embodiment of the present invention;

[0022] Figure 5 Schematic diagram of the working process of the cooling module in an embodiment of the present invention;

[0023] Figure 6 Schematic diagram of gas circuit connection in an embodiment of the present invention.

[0024] Among them: 1 shell; 2 sample chamber; 3 temperature control device; 4 circulating water interface; 5 lifting device; 6 copper heat sink; 7 sample holding part; 8 air inlet; 9 air outlet; 10 shell; 11 water inlet; 12 water outlet; 13 heating rod; 14 thermocouple; 15 sample insertion hole; hydrogen valve 301; pressure gauge 302; high pressure transmitter 303; low pressure transmitter 304; pressure regulating valve 305; gas tank valve 306; low pressure sensor valve 307; sample chamber valve 308; drain valve 309; vacuum valve 310; one-way valve 311; gas tank 312. DETAILED DESCRIPTION

[0025] The present invention is further described in detail below in conjunction with the accompanying drawings.

[0026] like Figure 1 to Figure 3 The embodiment of the hydrogen storage adsorption instrument of the present invention shown in the figure comprises: a gas circuit system, a circulating water supply device, a housing 1, a sample chamber 2, a temperature control device 3 and a lifting device 5, wherein the upper and lower ends of the lifting device 5 are fixed to the housing 1, and drive the temperature control device 3 to move up and down, and the sample chamber 2 is suspended below the top plate of the housing 1 and faces the sample insertion hole 15 of the temperature control device 3;

[0027] The temperature control device 3 includes: a copper heat sink 6, a sample holding portion 7, an air inlet 8, an air outlet 9, a shell 10, a water inlet 11, a water outlet 12, a heating rod 13 and a thermocouple 14. The sample holding portion 7 is opened at the center of the top of the copper heat sink 6. The copper heat sink 6 and the outer shell 10 form a cylindrical water holding chamber. The lower side wall of the shell 10 is provided with a water inlet 11 connected to the water holding chamber. The upper side wall of the shell 10 is provided with a water outlet 12 connected to the water holding chamber. The water inlet 11 and the water outlet 12 are both connected to the circulating water interface 4 and thus connected to the external circulating water tank and the circulating water providing device to provide circulating water.

[0028] The copper heat sink 6 is evenly provided with cooling channels, and both ends of the cooling channels are connected to the charging device through the air inlet 8 and the air outlet 9 respectively;

[0029] A plurality of heating rods 13 are provided in the copper heat sink 6, and a thermocouple 14 connected to the control system is installed in the copper heat sink 6;

[0030] The top of the housing 10 is provided with a sample insertion hole 15 that matches the shape and size of the sample receiving portion 7, so that after the temperature control device 3 rises, the sample chamber 2 enters the sample receiving portion 7;

[0031] The temperature control device adopts an integrated design of water bath and heating furnace, which can achieve precise temperature control in different temperature ranges to meet the PCT curve test of hydrogen storage materials; at the same time, the combination of air cooling and water cooling can quickly increase and decrease the temperature to meet the cycle life test.

[0032] Under the control of the control system, the temperature control device can be automatically raised and lowered through the lifting system to complete the temperature rise and fall processing of the sample chamber. The temperature control device adopts an integrated design of a water bath and a heating furnace, and can achieve precise temperature control in different temperature ranges to meet the PCT curve test of hydrogen storage materials. At the same time, the combination of air cooling and water cooling can quickly raise and lower the temperature, thereby improving the efficiency of the cycle life test of hydrogen storage materials.

[0033] The control system also has the functions of PCT test of hydrogen storage materials, hydrogen absorption and desorption kinetics test and cycle life test; Figure 4 The control system shown includes a heating and constant temperature module and a cooling module, wherein the heating and constant temperature module is respectively connected to the thermocouple, the circulating water supply device (chiller), the lifting device 5 and the heating rod 13; the cooling module is respectively connected to the thermocouple, the circulating water supply device, the inflation device, the lifting device 5 and the heating rod 13.

[0034] The heating and constant temperature methods of the heating and constant temperature module are as follows:

[0035] Heating and constant temperature low temperature zone control process: When the temperature is set in the low temperature zone (less than 90°C), the heating rod and the chiller work at the same time, and the lifting device 5 controls the temperature control device 3 (furnace body) to rise, so that the sample chamber is inserted into the copper heat sink, and cold water enters the furnace body from the water inlet and is discharged from the water outlet, taking away the heat of the copper heat sink. At the same time, the heating rod heats the copper heat sink. Under the joint action of the heating rod and the chiller, the temperature of the copper heat sink reaches a dynamic balance, so that the test is carried out in the sample chamber 2;

[0036] Heating and constant temperature high temperature zone control process: When the set temperature is in the high temperature zone (greater than or equal to 90°C), the chiller does not work, and water automatically flows back to the chiller below from the water inlet and the pipeline under the action of gravity; the heating rod works, and the lifting device 5 controls the temperature control device 3 (furnace body) to rise, so that the sample chamber is inserted into the copper heat sink, and the heating rod heats the copper heat sink. After the temperature reaches the setting, the test is carried out in the sample chamber 2.

[0037] When the cooling module works Figure 5 As shown, the ambient temperature (temperature) of the sample chamber 2 is first judged, and the temperature sent back by the thermocouple is received. When the temperature sent back by the thermocouple is above 200°C, the air-filling cooling mode is entered, and the air-filling device is turned on to fill cold air through the air inlet and discharge it from the air outlet until the temperature reaches the target temperature or 200°C, and the air-filling is stopped; then the water-cooling machine cooling mode is automatically entered;

[0038] When the temperature sent back by the thermocouple is lower than 200℃, the chiller enters the cooling mode, the chiller starts working, cold water enters from the water inlet and is discharged into the chiller from the water outlet, forming a cycle, thereby completing the rapid cooling of the copper heat sink and the sample chamber. After reaching the target temperature, the cooling module stops operating and feeds back the target temperature signal to the control system and displays it, which can automatically control and directly complete the cooling; thus, hydrogen absorption and desorption kinetics test, cycle life test and hydrogen storage material PCT curve test can be carried out uninterruptedly according to demand.

[0039] like Figure 6As shown, the gas circuit for testing the sample includes: a hydrogen valve 301, a pressure gauge 302, a high-pressure pressure transmitter 303, a pressure regulating valve 305, a gas tank valve 306, a high-pressure three-way, a gas storage three-way, a low-pressure four-way, a gas storage tank 312, an exhaust valve 309, a vacuum valve 310 and a one-way valve 311, wherein the hydrogen source sequentially passes through the hydrogen valve 301, the pressure gauge 302, the pressure regulating valve 305, the high-pressure three-way, the gas storage three-way, the low-pressure four-way, the exhaust valve 309 and the one-way valve 311. 1 is connected to the emptying outlet, wherein the third passage of the high-pressure three-way is connected to the high-pressure pressure transmitter 303, the third passage of the gas storage three-way is connected to the gas storage tank 312 through the gas storage tank valve 306, the third passage of the low-pressure four-way is connected to the low-pressure pressure transmitter 304 through the low-pressure sensor valve 307, the fourth passage of the low-pressure four-way is connected to the sample chamber 2 through the sample chamber valve 308, and a bypass is set on the pipeline before the emptying valve 309 to be connected to the vacuum pumping equipment through the vacuum valve 310.

[0040] During operation, when the target set pressure is lower than 1.5MPa, the low pressure sensor valve 307 is automatically opened, and the low pressure pressure transmitter is used to collect pressure data; when the pressure is lower than 1.5MPa, the low pressure sensor valve 307 is closed, and the low pressure pressure transmitter is used.

[0041] Hydrogen absorption and desorption kinetics tests include:

[0042] Step A: Hydrogen absorption and desorption kinetics test,

[0043] Step A1 Input the corresponding sample tank hydrogen absorption initial temperature Trs (such as 100°C), hydrogen filling pressure (MPa), hydrogen filling mode (△P), ambient temperature T d (℃), heating rate v (℃ / min), holding time t k (min), ambient temperature T d It can be monitored through real-time acquisition display.

[0044] In step A2, the valves are initially closed. The gas storage tank valve 306, the hydrogen valve 301, and the pressure regulating valve 305 are opened. The pressure increase rate is controlled by the pressure control 1, and a certain pressure of hydrogen (such as 5 MPa) is charged into the system pipeline and the pressure accumulator. Then, the hydrogen valve 301 and the pressure regulating valve 305 are closed, and the pressure value is recorded through the high-pressure pressure transmitter. The maximum pressure does not exceed 20 MPa. After the pressure stabilizes for a period of time (such as 5 minutes), the pressure value P is recorded. d ;

[0045] Step A3: the control system changes the temperature of the copper heat sink 6 until the sample tank hydrogen absorption initial temperature Trs (target temperature) is reached;

[0046] Step A4: Then open the sample chamber valve 308, and the control system calls the temperature rise and constant temperature module according to the input data to continuously heat and maintain the temperature of the copper heat sink 6. The hydrogen storage material begins to absorb hydrogen, and the pressure begins to drop. The instantaneous pressure value P of the system is recorded through the high-pressure pressure transmitter. r During the whole process, real-time recording of pressure can be achieved, with a minimum data interval of 1s (this interval is adjustable).

[0047] Step A6 calculates the hydrogen absorption capacity of the hydrogen storage material through the system pressure change and draws the time-pressure-capacity curve.

[0048] After the hydrogen absorption process is completed in step A6, the system stops working. While outputting this table, the original pressure, temperature and other data can be collected and recorded in the background and exported.

[0049] Step B: Hydrogen release kinetics test,

[0050] Step B1 Input the corresponding sample tank hydrogen release initial temperature Tr (such as 300°C), hydrogen release heating rate v (such as 5°C / min), hydrogen release insulation time t k (e.g. 500min), vacuum time of pipeline before hydrogen discharge (e.g. 20min), hydrogen discharge insulation time t k (min), ambient temperature T d (℃) can be monitored through real-time acquisition display;

[0051] Step B2: The control system changes the temperature of the copper heat sink 6 until the set hydrogen release initial temperature Tr (target temperature) is reached;

[0052] Step B3 enters the automatic control hydrogen release process: open the sample chamber valve 308 and the gas tank valve 306, and record a pressure value Pr at this time.

[0053] Step B4: Close the sample chamber valve 308 and open the vacuum valve 310. At this time, the vacuum pumping time t before hydrogen release begins to be calculated. After the vacuum pumping time reaches the set value (such as 20 minutes), the vacuum valve 310 is closed.

[0054] Step B5 opens the sample chamber valve 308, and the control system calls the temperature rise and constant temperature module to continuously heat and maintain the temperature of the copper heat sink 6 according to the input data; at the same time, the high-pressure pressure transmitter continuously collects the hydrogen degassing pressure change data Pr'.

[0055] In the process of step A3 and step B2 of this embodiment, the control system quickly changes the temperature in the copper heat sink 6 according to demand, without taking the sample chamber 2 out of the sample holding portion 7, so there is no need to change the environment of the sample chamber 2, and the test efficiency is higher.

[0056] If continuous cycle life test is required, call back to step A after step B, and stop the test after the set number of cycles.

[0057] PCT curve test of hydrogen storage materials. The key to PCT curve test lies in the controllability of hydrogen charging and discharging. The rise and fall of hydrogen charging pressure is controlled by pneumatic actuators and pressure reducing valves, thereby controlling the hydrogen charging rate, ensuring hydrogen charging efficiency while avoiding the impact of strong airflow on system pipelines.

[0058] Step C: Conduct hydrogen charging PCT curve test

[0059] Step C1, input the temperature required for hydrogen absorption (such as 100° C.), the first hydrogen charging target pressure value, the second hydrogen charging target pressure value, …, the last hydrogen charging target pressure value, the single-step hydrogen absorption time, and the hydrogen absorption pressure stabilization time (such as 5 minutes);

[0060] Step C2: The valves are initially closed. After the low pressure sensor valve 307 is opened, the hydrogen valve 301 and the pressure regulating valve 305 are opened after 1 second.

[0061] Step C3, start the first step of hydrogen filling: fill the system with hydrogen of the first hydrogen filling target pressure value, select a suitable pressure transmitter to monitor the pressure value according to the set target pressure range, and record the pressure value after the pressure stabilizes for a long time (such as 5 minutes) to serve as the first pressure value of the system pressure Pd1. At this time, the pressure in the sample tank is recorded as Pr1, and the first Pr1 value is 0MPa.

[0062] Step C4, then calling the temperature control module to make the copper heat sink 6 reach the set temperature required for hydrogen absorption and maintain the temperature;

[0063] Step C5, open the sample chamber valve 308, the hydrogen storage material starts to absorb hydrogen, the pressure starts to drop, and after waiting for the single-step hydrogen absorption time, the pressure value is recorded as Pr1' through the pressure transmitter. The hydrogen absorption amount Δn1 of the hydrogen storage material in this step is calculated by combining the pressure changes of Pd1, Pr1, and Pr1' with the system and the sample tank volume.

[0064] Step C6: After the first step of hydrogen absorption test is completed, the system closes the sample chamber valve 308, and after 1 second, performs the second hydrogen charging;

[0065] Step C7, second hydrogen filling: open the hydrogen valve 301 and the pressure regulating valve 305, automatically fill with hydrogen to the second target pressure value, then close V1, and after stabilization for a period of time (such as 5 minutes), select a suitable pressure transmitter to monitor the pressure value according to the set target pressure range and record the pressure value Pd2. The pressure in the sample tank is the pressure Pr1' after the first hydrogen absorption as the pressure Pr2 of the second hydrogen absorption, and then open the sample chamber valve 308, the hydrogen storage material absorbs hydrogen again, and after a period of time (i.e., single-step hydrogen absorption time), the pressure value is recorded as Pr2' through the pressure transmitter, and the hydrogen absorption amount Δn2 of the hydrogen storage material in this step is calculated through the pressure changes of Pd2, Pr2, and Pr2', combined with the system and the sample tank volume.

[0066] Repeat steps C6 and C7 from the third hydrogen charging to the final hydrogen charging until all hydrogen charging steps are completed.

[0067] Step D: Perform a hydrogen release PCT curve test. After the hydrogen absorption process is completed, hydrogen is released according to the set hydrogen release target pressure value.

[0068] Step D1, input the temperature required for hydrogen desorption (such as 100° C.), the first hydrogen desorption target pressure value, the second hydrogen desorption target pressure value, …, the last hydrogen desorption target pressure value, the single-step hydrogen desorption time, and the hydrogen desorption pressure stabilization time (such as 5 minutes);

[0069] Step D2, first hydrogen release: first close the sample chamber valve 308, and after 1 second, open the drain valve 309 (when the pressure of the set first hydrogen release target pressure value is higher than 0.5 MPa), and slowly discharge the hydrogen in the system into the atmosphere. When the hydrogen release target pressure is reached, the drain valve 309 is closed (when the pressure of the set first hydrogen release target pressure value is lower than 0.2 atm, after 1 second, open the vacuum valve 310, use a vacuum pump to evacuate the system, and after reaching the target pressure, close the vacuum valve 310).

[0070] Step D3: After the hydrogen discharge pressure stabilizes for a certain period of time (e.g., 5 minutes), record the pressure value of the pressure transmitter as Pd x+1 At this time, the pressure in the sample tank is Pr x+1 The equilibrium pressure Pr at the end of the PCT test with the maximum hydrogen absorption in the previous step x ',

[0071] Step D4, then calling the temperature control module to make the copper heat sink 6 reach the set temperature required for hydrogen absorption and maintain the temperature;

[0072] Step D5: Open the sample chamber valve 308, the hydrogen storage material starts to release hydrogen, and the system pressure increases. After a period of time (such as 30 minutes) of hydrogen release, the pressure value is recorded as Pr by the pressure transmitter. x+1 ', through Pd x+1 , Pr x+1, Pr x+1 'Pressure change, combined with the system and sample tank volume, calculate the hydrogen release amount Δn1 of the hydrogen storage material in this step.

[0073] Step D6: After the first step of hydrogen release is completed, the sample chamber valve 308 is closed after 1 second.

[0074] Step D7, second hydrogen release: open the drain valve 309 or the vacuum valve 310 to release hydrogen (or evacuate) to reach the second hydrogen release target pressure, close the drain valve 309 or the vacuum valve 310, and after stabilization for a period of time (5 minutes), record the pressure value through the pressure transmitter as the second hydrogen release Pd x+2 , pressure in the sample tank Pr x+2 This is the pressure Pr after the first hydrogen release is completed. x+1 ', then open the sample chamber valve 308, the hydrogen storage material starts to release hydrogen, the system pressure increases, and after a period of time (such as 30 minutes) of hydrogen release, the pressure value is recorded by the pressure transmitter as Pr x+2 ', through Pd x+2 , Pr x+2 Pr x+2 'Pressure change, combined with the system and sample tank volume, calculate the hydrogen release amount Δn2 of the hydrogen storage material in this step.

[0075] Repeat steps D6 and D7 from the third to the last hydrogen release until all hydrogen release steps are completed. And so on, all hydrogen release steps are completed.

[0076] During the test, the recorded data can be checked at any time and the PC (pressure-capacity) curve can be directly drawn. After all the tests in step C and step D are completed, a complete PCT curve test table for hydrogen absorption and desorption storage materials is formed.

[0077] Example 1

[0078] Put 2g of LaNi5 into the sample chamber and activate it at 200℃. The PCT curve hydrogen absorption and desorption temperature is set to 20℃. Under the action of the lifting device, the temperature control device rises to make the sample chamber enter the copper heat sink cavity. After the temperature stabilizes for 30 minutes, the PCT curve automatic test begins. Because 20℃ is a low temperature zone, a water bath is used for heat preservation.

[0079] Example 2

[0080] Place 2g of LaNi5 in the sample chamber and perform high-temperature activation at 200℃. The hydrogen absorption temperature for the cycle life test is set to 20℃, and the hydrogen release temperature is 200℃. Under the action of the lifting device, the temperature control device rises to allow the sample chamber to enter the copper heat sink cavity. After the temperature stabilizes for 30 minutes, the hydrogen absorption curve is automatically tested. Because 20℃ is a low temperature zone, a water bath is used for heat preservation. After the hydrogen absorption is completed, the water automatically flows back into the chiller, and the heating rod is heated to 200℃ for hydrogen release. After the hydrogen release is completed, the copper heat sink is pneumatically cooled by air cooling. When the temperature is lower than 150℃, the chiller starts working, and water enters the temperature control device for rapid water cooling. When the temperature reaches 20℃, the second hydrogen absorption is performed.

Claims

1. A fully automatic hydrogen storage adsorption instrument with cycle life test function, characterized in that: include: An air circuit system, a circulating water supply device, a housing (1), a sample chamber (2), a temperature control device (3) and a lifting device (5), wherein the upper and lower ends of the lifting device (5) are fixed to the housing (1), the sample chamber (2) is suspended below the top plate of the housing (1), and the sample chamber (2) is directly opposite to the sample insertion hole (15) of the temperature control device (3); The temperature control device (3) comprises: a copper heat sink (6), a sample receiving portion (7), an air inlet (8), an air outlet (9), a shell (10), a water inlet (11), a water outlet (12), a heating rod (13) and a thermocouple (14); the sample receiving portion (7) is provided at the center of the top of the copper heat sink (6); the copper heat sink (6) and the outer shell (10) form a cylindrical water receiving chamber; a water inlet (11) communicating with the water receiving chamber is provided below the side wall of the shell (10); a water outlet (12) communicating with the water receiving chamber is provided above the side wall of the shell (10); the water inlet (11) and the water outlet (12) are connected to an external circulating water supply device via a circulating water interface (4); A plurality of heating rods (13) are arranged in the copper heat sink (6), and a thermocouple (14) connected to a control system is installed in the copper heat sink (6); a sample insertion hole (15) having a shape and size matching that of the sample receiving portion (7) is opened on the top of the shell (10), and after the temperature control device (3) rises; cooling air channels are evenly arranged in the copper heat sink (6), and both ends of the cooling water channel are respectively connected to the inflation device through an air inlet (8) and an air outlet (9).

2. The fully automatic hydrogen storage adsorption instrument with cycle life test function according to claim 1, characterized in that: The control system includes a cooling module, which is respectively connected to the thermocouple, the circulating water supply device, the inflation device, the lifting device (5) and the heating rod (13); When the cooling module is working, it first determines the ambient temperature of the sample chamber and receives the temperature sent back by the thermocouple: When the temperature sent back by the thermocouple is above 200℃, the system enters the inflation cooling mode, turns on the inflation device to fill cold air through the air inlet and discharges it from the air outlet until the temperature reaches the target temperature or 200℃, then stops inflating; then automatically enters the chiller cooling mode; When the temperature transmitted back by the thermocouple is lower than 200℃, the chiller enters the cooling mode, the chiller starts working, cold water enters from the water inlet and is discharged into the chiller from the water outlet, forming a cycle, thereby completing the rapid cooling of the copper heat sink and the sample chamber.

3. A fully automatic hydrogen storage adsorption instrument with cycle life test function according to claim 1 or 2, characterized in that: The control system further comprises a temperature-raising and temperature-constant module, which is respectively connected to the thermocouple, the circulating water supply device, the lifting device (5) and the heating rod (13).

4. The fully automatic hydrogen storage adsorption instrument with cycle life test function according to claim 3, characterized in that: The control process of the temperature rising and constant temperature module in the low temperature zone and the high temperature zone is as follows: Heating and constant temperature low temperature zone control process: When the temperature is set in the low temperature zone, the heating rod and the chiller work at the same time, the lifting device controls the temperature control device to rise, so that the sample chamber is inserted into the copper heat sink, and cold water enters the furnace body from the water inlet and is discharged from the water outlet, taking away the heat of the copper heat sink. At the same time, the heating rod heats the copper heat sink. Under the joint action of the heating rod and the chiller, the temperature of the copper heat sink reaches a dynamic balance, so that the test can be carried out in the sample chamber; Heating and constant temperature high temperature zone control process: When the temperature is set in the high temperature zone, the chiller does not work, and the water automatically flows back to the chiller below from the water inlet and the pipeline under the action of gravity; the heating rod works, and the lifting device controls the temperature control device to rise, so that the sample chamber is inserted into the copper heat sink. The heating rod heats the copper heat sink, and the test is carried out in the sample chamber after the temperature reaches the setting.

5. The fully automatic hydrogen storage adsorption instrument with cycle life test function according to claim 4, characterized in that: The low temperature zone is less than 90°C, and the high temperature zone is greater than or equal to 90°C.

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