CN116399752A - Safety monitoring device and method for solid metal hydrogen absorption and desorption dynamic process - Google Patents
Safety monitoring device and method for solid metal hydrogen absorption and desorption dynamic process Download PDFInfo
- Publication number
- CN116399752A CN116399752A CN202310192049.0A CN202310192049A CN116399752A CN 116399752 A CN116399752 A CN 116399752A CN 202310192049 A CN202310192049 A CN 202310192049A CN 116399752 A CN116399752 A CN 116399752A
- Authority
- CN
- China
- Prior art keywords
- tank
- hydrogen
- sample
- hydrogen absorption
- sample tank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000001257 hydrogen Substances 0.000 title claims abstract description 135
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 135
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 65
- 238000003795 desorption Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000007787 solid Substances 0.000 title claims abstract description 26
- 239000002184 metal Substances 0.000 title claims abstract description 25
- 230000008569 process Effects 0.000 title claims abstract description 18
- 238000012806 monitoring device Methods 0.000 title claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 63
- 230000005540 biological transmission Effects 0.000 claims abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 238000012544 monitoring process Methods 0.000 claims abstract description 22
- 230000008054 signal transmission Effects 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000012360 testing method Methods 0.000 claims description 18
- 230000006835 compression Effects 0.000 claims description 12
- 238000007906 compression Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 7
- 238000005984 hydrogenation reaction Methods 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000011232 storage material Substances 0.000 abstract description 5
- 230000008859 change Effects 0.000 description 7
- 150000002431 hydrogen Chemical class 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/16—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by heating the material
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Combustion & Propulsion (AREA)
- Engineering & Computer Science (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses a safety monitoring device and a safety monitoring method for a solid metal hydrogen absorption and desorption dynamic process, wherein the safety monitoring device comprises an oil bath heating device, a reference tank, a sample tank, a first pressure sensor, a second pressure sensor, a data monitoring and collecting system, a vacuum pump, a gas unit and a gas transmission pipeline; the reference tank and the sample tank are respectively positioned in the oil bath heating device; the first pressure sensor and the second pressure sensor are respectively arranged at the top valves of the reference tank and the sample tank and are respectively connected to the data monitoring and acquisition system through signal transmission lines; the top valves of the reference tank and the sample tank are sequentially connected in series on the gas transmission pipeline, and the vacuum pump and the gas unit are respectively arranged at the end parts of the gas transmission pipeline. The device can record the hydrogen absorption and desorption rates and the hydrogen absorption and desorption amounts at different stages, explore the main influencing factors of the hydrogen absorption and desorption, realize the safety monitoring of the solid metal hydrogen absorption and desorption dynamic process, and provide data support for the safety of the practical application of the hydrogen storage material.
Description
Technical Field
The invention relates to the field of solid hydrogen storage, in particular to a solid metal hydrogen absorption and desorption dynamic process safety monitoring device and method.
Background
Most of the existing hydrogen storage devices are fully automatic, and hydrogen storage materials in a container are heated through an external thermocouple so as to realize the adsorption or release of hydrogen, so that PCT curves and Q-t curves of the whole process are obtained. Although the method can explore the better dynamics and thermodynamic performance of different hydrogen storage materials under the conditions of temperature and pressure, the hydrogen storage device does not pay attention to the hydrogen absorption and desorption rates and the hydrogen absorption and desorption amounts of different stages, and the main influencing factors of the hydrogen absorption and desorption at each stage cannot be clarified. And the existing device mainly adopts electromagnetic heating, so that the heating is not uniform enough, and the accuracy of data cannot be ensured.
Disclosure of Invention
The invention aims to: aiming at the defects of the prior art, the technical problem to be solved by the invention is to provide the safety monitoring device for the hydrogen absorption and desorption dynamic process of the solid metal so as to monitor the hydrogen absorption and desorption dynamic process of the solid metal more accurately and in real time.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the safety monitoring device for the hydrogen absorption and desorption dynamic process of the solid metal comprises an oil bath heating device, a reference tank, a sample tank, a first pressure sensor, a second pressure sensor, a data monitoring and collecting system, a vacuum pump, a gas unit and a gas transmission pipeline;
the reference tank and the sample tank are respectively positioned in the oil bath heating device; the first pressure sensor is arranged at the top valve of the reference tank; the second pressure sensor is arranged at the top valve of the sample tank; the first pressure sensor and the second pressure sensor are connected to the data monitoring and collecting system through signal transmission lines;
the top valves of the reference tank and the sample tank are sequentially connected in series on the gas transmission pipeline, and the vacuum pump and the gas unit are respectively arranged at the end parts of the gas transmission pipeline.
Further, the gas unit comprises a nitrogen cylinder and a hydrogen cylinder; the vacuum pump, the nitrogen cylinder and the hydrogen cylinder are connected in parallel at the front side of the gas transmission pipeline.
Further, a first valve is arranged at the parallel connection part of the vacuum pump and the nitrogen cylinder; a second valve is arranged at the parallel connection interface of the hydrogen cylinders; a third valve is arranged on the front side of the gas transmission pipeline; a branch pipe is arranged on the gas transmission pipeline between the reference tank and the sample tank, and a fifth valve is arranged on the branch pipe; a fourth valve is arranged on the gas transmission pipeline between the rear side of the reference tank and the joint of the branch pipes; a sixth valve is arranged on the gas transmission pipeline between the front side of the sample tank and the joint of the branch pipes; a seventh valve is arranged on the gas transmission pipeline at the rear side of the sample tank.
Further, the oil bath heating device comprises an oil bath box, a lifting platform, a flip cover, a console, a lifting cylinder and a stirring device; the reference tank and the sample tank are respectively arranged in the oil bath tank; the lifting platform is positioned at the top of the oil bath box, four corners of the bottom of the lifting platform are respectively connected with lifting cylinders, and the lifting of the lifting platform is controlled through the telescopic movement of the lifting cylinders; the stirring device is arranged in the center of the lifting platform and is lifted together with the lifting platform; the control console is positioned outside the oil bath box and is in circuit connection with the heating device, the lifting cylinder and the stirring device in the oil bath box; the flip is hinged to the upper portion of the lifting platform, and two through holes for leading out the gas transmission pipeline are reserved in the flip corresponding to the reference tank and the sample tank.
Further, the bottom of the lifting platform is also provided with four groups of limiting rods; four groups of limiting blocks are correspondingly arranged at the top of the oil bath box, the limiting rod penetrates through the limiting block, a rubber sleeve is sleeved at the bottom end of the limiting rod, and the size of the rubber sleeve is larger than that of a penetrating hole in the limiting block.
Furthermore, the invention also provides a method for testing the hydrogen absorption and desorption characteristics of the solid metal by adopting the device, which comprises the following steps:
s1: connecting and sealing the reference tank and the sample tank with a gas transmission pipeline, and immersing the reference tank and the sample tank in an oil bath heating device;
s2: opening a vacuum pump, vacuumizing the reference tank and the sample tank through a gas transmission pipeline, and then cutting off corresponding pipelines of the vacuum pump;
s3: setting a test temperature of an oil bath heating device, and heating a reference tank and a sample tank to the test temperature;
s4: inputting hydrogen with certain pressure into a reference tank through a gas unit, then communicating the reference tank with a sample tank, enabling part of hydrogen in the reference tank to enter the sample tank, testing sample materials in the sample tank to perform hydrogen absorption reaction, recording balance time and balance pressure after the pressure in the tank is stable, and calculating hydrogen variation according to variation of the pressure in the tank before and after the reaction and a gas state equation;
s5: closing a sample tank, gradually injecting hydrogen into a reference tank in the same amount, and communicating the reference tank with the sample tank after each hydrogenation is completed to obtain balance points and balance time of different hydrogen absorption amounts, and stopping hydrogenation when the hydrogen absorption amount is not increased;
s6: purging and evacuating residual hydrogen in the reference tank, and then vacuumizing;
s7: a curve of the equilibrium hydrogen pressure versus hydrogen absorption concentration (PCT curve) of the sample under the test temperature conditions during the hydrogen absorption and desorption cycle, and a curve of the amount of hydrogen absorption and desorption of the sample over time (Q-t curve) were obtained. PCT curves are isothermal curves describing the relationship between equilibrium hydrogen pressure and hydrogen absorption concentration of an alloy or metal hydride during a hydrogen absorption and desorption cycle, and are very important characteristic curves for characterizing the thermodynamic performance of a hydrogen storage material.
Preferably, in step S3, the test temperature of the oil bath heating device is controlled to be 100-400 ℃.
Preferably, in step S4, the pressure of the hydrogen gas inputted into the reference tank is controlled to be 0.01 to 4MPa.
Preferably, in step S4, the method for calculating the hydrogen variation is as follows:
wherein ΔC—Single step Hydrogen absorption Capacity, i.e., hydrogen variation, in wt%;
w-hydride mass, g; calculation can be performed by hydrogen reduction amount according to mass conservation;
r-ideal gas constant, r= 8.314472j·mol -1 ·K -1 ；
P 1 -referring to tank pressure, MPa after hydrogen is introduced;
V 1 -reference tank volume, mL;
Z 1 -a pre-reaction reference tank volume compression factor;
T 1 -referring to the tank temperature before the reaction, c;
P 2 -pressure of sample tank before hydrogen is introduced, MPa;
V 2 -sample tank volume, mL;
Z 2 -a pre-reaction sample tank volume compression factor;
P eq -the equilibrium pressure in the sample tank and the reference tank, MPa;
Z 1 ' reference tank volume compression factor after reaction;
T 2 -equilibrium temperature in sample tank and reference tank, i.e. oil bath set temperature, deg.c;
Z 2 ' -sample tank volume compression factor after reaction.
Preferably, in step S5, the pressure of hydrogen gas injected into the reference tank is 0.01 to 0.05MPa each time.
The beneficial effects are that:
(1) The invention provides a semi-automatic solid metal hydrogen absorption and desorption dynamic process safety monitoring device which can record the hydrogen absorption and desorption rates and the hydrogen absorption and desorption amounts of different stages, explore the main influencing factors of the hydrogen absorption and desorption of each stage, realize the safety monitoring of the solid metal hydrogen absorption and desorption dynamic process and provide data support for the safety application of hydrogen storage materials.
(2) The device adopts the high-precision pressure sensor and designs gaskets with different sizes for the reference tank and the sample tank so as to change the volume of the tank body, thereby increasing the monitoring range and the precision of the material performance and simultaneously obtaining more accurate experimental results.
Drawings
The foregoing and/or other advantages of the invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings and detailed description.
Fig. 1 is a schematic diagram of the overall structure of the safety monitoring device for the hydrogen absorption and desorption kinetics process of the solid metal.
Fig. 2 is a schematic diagram of the structure of the oil bath heating device in the test apparatus.
FIG. 3 is a graph showing the kinetics of hydrogen absorption obtained by the device of the present invention at various temperatures.
FIG. 4 is a PCT curve obtained for the device of the present invention.
Wherein each reference numeral represents:
1-a vacuum pump; 2-nitrogen cylinder; 3-hydrogen cylinder; 4-a first valve; 5-a second valve; 6-a third valve; 7-a first pressure sensor; 8-a reference tank; 9-an oil bath heating device; 10-a data monitoring and collecting system; 11-fourth valve; 12-a fifth valve; 13-sixth valve; 14-a second pressure sensor; 15-sample tank; 16-seventh valve.
91-an oil bath box; 92-lifting the platform; 93-flip cover; 94-console; 95-lifting the cylinder; 96-stirring device; 97-limiting blocks; 98-through holes.
Detailed Description
The invention will be better understood from the following examples.
As shown in fig. 1, the safety monitoring device for the hydrogen absorption and desorption kinetics process of the solid metal comprises an oil bath heating device 9, a reference tank 8, a sample tank 15, a first pressure sensor 7, a second pressure sensor 14, a data monitoring and collecting system 10, a vacuum pump 1, a gas unit and a gas transmission pipeline.
Wherein the reference tank 8 and the sample tank 15 are respectively positioned in the oil bath heating device 9; the first pressure sensor 7 is arranged at the top valve of the reference tank 8; the second pressure sensor 14 is arranged at the top valve of the sample tank 15; the first pressure sensor 7 and the second pressure sensor 14 are connected to the data monitoring and acquisition system 10 through signal transmission lines.
In this embodiment, the first pressure sensor 7 and the second pressure sensor 14 are used in the Japanese cross river EJX A (EJX A-JCS4N-017EL/NF21/HAC 0-4.0 MPa).
The top valves of the reference tank 8 and the sample tank 15 are sequentially connected in series on the gas transmission pipeline, and the vacuum pump 1 and the gas unit are respectively arranged at the end parts of the gas transmission pipeline.
The gas unit comprises a nitrogen cylinder 2 and a hydrogen cylinder 3; the vacuum pump 1, the nitrogen cylinder 2 and the hydrogen cylinder 3 are connected in parallel at the front side of the gas transmission pipeline.
A first valve 4 is arranged at the parallel connection part of the vacuum pump 1 and the nitrogen cylinder 2; a second valve 5 is arranged at the parallel connection interface of the hydrogen cylinder 3; a third valve 6 is arranged on the front side of the gas transmission pipeline; a branch pipe is arranged on the gas transmission pipeline between the reference tank 8 and the sample tank 15, and a fifth valve 12 is arranged on the branch pipe; a fourth valve 11 is arranged on the gas transmission pipeline between the rear side of the reference tank 8 and the joint of the branch pipes; a sixth valve 13 is arranged on the gas transmission pipeline between the front side of the sample tank 15 and the joint of the branch pipes; a seventh valve 16 is provided in the gas transfer line at the rear side of the sample tank 15.
The left end of the reference tank 8 is connected with an outlet pipeline of the vacuum pump 1 and inlet pipelines of the nitrogen cylinder 2 and the hydrogen cylinder 3, and the functions are to introduce nitrogen, hydrogen and vacuumize into the system respectively. Hydrogen is filled into the reference tank 8 to serve as a gas source of an experiment system, and experiments of different materials are set by controlling the hydrogen filling amount. The first pressure sensor 7 on the reference tank 8 records its pressure change in real time and transmits it to the data monitoring and acquisition system 10. The right side of the reference tank 8 is connected with a fourth valve 11, a fifth valve 12 and a sixth valve 13. Wherein, the fourth valve 11 and the sixth valve 13 control the experimental gas to flow from the reference tank 8 to the sample tank 15, and the fifth valve 12 is used for releasing excessive hydrogen.
The sample tank 15 is used for placing experimental materials, the volume of the sample tank can be changed by adding gaskets to change the volume so as to adapt to different amounts of materials, the gasket adopts 304 stainless steel, and gasket external diameter and jar internal diameter phase-match. The second pressure sensor 14 on the sample tank 15 records its pressure change in real time and transmits it to the data monitoring and acquisition system 10. The right side of the sample tank 15 is connected with a system air outlet pipeline and a seventh valve 16 for exhausting residual gas in the system.
As shown in fig. 2, the oil bath heating device 9 includes an oil bath tank 91, a lifting platform 92, a flip cover 93, a console 94, a lifting cylinder 95, and a stirring device 96; the reference tank 8 and the sample tank 15 are respectively arranged in the oil bath tank 91; the lifting platform 92 is positioned at the top of the oil bath box 91, four corners of the bottom of the lifting platform are respectively connected with lifting cylinders 95, and lifting of the lifting platform 92 is controlled through telescopic movement of the lifting cylinders 95; the stirring device 96 is arranged in the center of the lifting platform 92 and is lifted together with the lifting platform 92; the control console 94 is positioned outside the oil bath tank 91 and is in circuit connection with a heating device, a lifting cylinder 95 and a stirring device 96 in the oil bath tank 91; the flip 93 is hinged to the upper part of the lifting platform 92, and two through holes 98 for leading out the gas transmission pipeline are reserved corresponding to the reference tank 8 and the sample tank 15.
Four groups of limiting rods 96 are also arranged at the bottom of the lifting platform 92; four groups of limit blocks 97 are correspondingly arranged at the top of the oil bath tank 91, the limit rods 96 penetrate through the limit blocks 97, rubber sleeves are sleeved at the bottom ends of the limit rods 96, and the sizes of the rubber sleeves are larger than through holes in the limit blocks 97.
The lifting cylinder 95 is supplied with air from the air compressor, and lifts the reference tank 8 and the sample tank 15 for loading and unloading. Six screw thread posts are arranged on the sample tank 15 to fix the tank top, so that the tightness of the hydrogen storage tank and the safety of experiments are ensured. The oil bath 91 is internally provided with a stirring device 96 which is positioned in the middle of the reference tank 8 and the sample tank 15, so that the heating is uniform and stable in the heating process. The control buttons are provided on the outside of the oil bath 91 at the control panel 94, including start and stop, heating and pause, up and down, and temperature setting (up to 400 c) and speed control.
Taking an alloy as an example, the method for safely monitoring the hydrogen absorption and desorption kinetics process of the solid metal by adopting the device comprises the following steps:
s1: connecting and sealing the reference tank 8 and the sample tank 15 with a gas transmission pipeline, and immersing the gas transmission pipeline in an oil bath heating device 9;
s2: the first valve 4 is opened to the direction that the vacuum pump 1 is connected with the main pipeline, the third valve 6, the fourth valve 11 and the sixth valve 13 are opened, and the fifth valve 12 and the seventh valve 16 are closed. Opening the vacuum pump 1, vacuumizing the reference tank 8 and the sample tank 15 through the gas transmission pipeline, and then cutting off corresponding pipelines of the vacuum pump 1;
s3: setting the test temperature of the oil bath heating device 9 to be 200 ℃, and heating the reference tank 8 and the sample tank 15 to the test temperature;
s4: inputting 0.01MPa hydrogen into a reference tank 8 through a gas unit, closing a second valve 5 and a third valve 6, then rapidly opening a sixth valve 13, communicating the reference tank 8 with a sample tank 15, enabling part of hydrogen in the reference tank 8 to enter the sample tank 15, testing sample materials in the sample tank 15 to perform hydrogen absorption reaction, recording balance time and balance pressure after the pressure in the tank is stable, and calculating hydrogen variation according to variation of the pressure in the tank before and after the reaction and a gas state equation;
s5: closing the sixth valve 13 and the sample tank 15, then gradually injecting hydrogen into the reference tank 8 in the same amount of 0.01MPa each time, opening the sixth valve 13 to communicate the reference tank 8 and the sample tank 15 after each time of hydrogenation is completed, obtaining balance points and balance time of different hydrogen absorption amounts, and stopping hydrogenation when the hydrogen absorption amount is not increased any more;
s6: closing a sixth valve 13, purging and evacuating residual hydrogen in the reference tank, and then vacuumizing;
s7: finally, a curve (PCT curve) of the relationship between the equilibrium hydrogen pressure and the hydrogen absorption concentration of the sample at 200 ℃ in the hydrogen absorption and desorption cycle process and a curve (Q-t curve) of the change of the hydrogen absorption and desorption amounts of a plurality of samples with time are obtained.
S8: changing the set temperature, increasing or decreasing with 20 ℃ as gradient, respectively setting five groups of experiments, and repeating the above operation to obtain PCT curve and hydrogen absorption amount change curve (Q-t curve) with time at different temperatures. The hydrogen absorption rate is faster at which temperature the analysis is performed.
In step S4, the method for calculating the hydrogen variation is as follows:
wherein ΔC—Single step Hydrogen absorption Capacity, i.e., hydrogen variation, in wt%;
w-hydride mass, g; calculation can be performed by hydrogen reduction amount according to mass conservation;
r-ideal gas constant, r= 8.314472j·mol -1 K -1 ；
P 1 -referring to tank pressure, MPa after hydrogen is introduced; i.e. the first pressure sensor 7 measures the pressure, including the reference tank 8, and the piping between the third valve 6, the fifth valve 12, the sixth valve 13.
V 1 -reference tank volume, mL; including the volume between the pipes between the third valve 6, the fifth valve 12, the sixth valve 13; the volume calibration of the reference tank and the surrounding pipelines is measured by the external test tube through a drainage method
Z 1 -a pre-reaction reference tank volume compression factor; a pipeline among the third valve 6, the fifth valve 12 and the sixth valve 13, which comprises a reference tank 8; can be calculated by specific temperature and specific pressure;
T 1 -referring to the tank temperature before the reaction, c; p (P) 2 -pressure of sample tank before hydrogen is introduced, MPa;
V 2 -sample tankProduct, mL; a pipeline comprising a sample tank 15, a sixth valve 13 and a seventh valve; the volume calibration of the sample tank and the surrounding pipelines is measured by a drainage method through an external test tube;
Z 2 -a pre-reaction sample tank volume compression factor; a pipeline comprising a sample tank 15, a sixth valve 13 and a seventh valve; can be calculated by specific temperature and specific pressure;
P eq -equilibrium pressure in the sample tank, MPa; z is Z 1 ' reference tank volume compression factor after reaction;
T 2 -equilibrium temperature in sample tank and reference tank, i.e. oil bath set temperature, deg.c;
Z 2 ' sample tank volume compression factor after reaction; a pipeline comprising a sample tank 15, a sixth valve 13 and a seventh valve; can be calculated by a specific temperature and a specific pressure.
As shown in fig. 3 and 4, the hydrogen absorption kinetics curves and PCT curves at different temperatures obtainable with the device of the present invention are shown. As can be seen from the figures: as the temperature increases, the hydrogen absorption rate of the alloy is faster and faster; with the rise of temperature, the height of the platform pressure area rises, (the physical nature of the platform pressure is the stability of hydride, the lower the platform pressure of the alloy is, the more favorable for hydrogen absorption and the unfavorable for hydrogen desorption, and conversely, the favorable for hydrogen desorption and the unfavorable for hydrogen absorption), the higher the temperature is, the worse the stability of the alloy is, and the favorable for hydrogen desorption is.
The device can also realize the hydrogen discharge test, for example, after the hydrogen absorption in the sample tank 15 is complete, the hydrogen in the reference tank 8 is evacuated, the first valve 4 and the third valve 6 are closed after the evacuation, the fourth valve 11 and the sixth valve 13 are opened, and at the moment, the pressure difference exists between the sample tank 15 and the reference tank 8, so that the hydrogen discharge can be realized. The hydrogen release amount can be deduced through the change value of the pressure. After the hydrogen is completely discharged, the hydrogen discharge time is recorded, the temperature of the oil bath is changed, the experiment is repeated, the hydrogen discharge time at different temperatures is recorded, and the hydrogen discharge rate at different temperatures can be compared.
The invention provides a method for safely monitoring the hydrogen absorption and desorption dynamic process of solid metal, and the method and the way for realizing the technical scheme are numerous, the above description is only a preferred embodiment of the invention, and it should be pointed out that a plurality of improvements and modifications can be made to those skilled in the art without departing from the principle of the invention, and the improvements and modifications are also considered as the protection scope of the invention. The components not explicitly described in this embodiment can be implemented by using the prior art.
Claims (10)
1. The safety monitoring device for the hydrogen absorption and desorption dynamic process of the solid metal is characterized by comprising an oil bath heating device (9), a reference tank (8), a sample tank (15), a first pressure sensor (7), a second pressure sensor (14), a data monitoring and collecting system (10), a vacuum pump (1), a gas unit and a gas transmission pipeline;
the reference tank (8) and the sample tank (15) are respectively positioned in the oil bath heating device (9); the first pressure sensor (7) is arranged at the top valve of the reference tank (8); the second pressure sensor (14) is arranged at the top valve of the sample tank (15); the first pressure sensor (7) and the second pressure sensor (14) are connected to the data monitoring and collecting system (10) through signal transmission lines;
the top valves of the reference tank (8) and the sample tank (15) are sequentially connected in series on the gas transmission pipeline, and the vacuum pump (1) and the gas unit are respectively arranged at the end parts of the gas transmission pipeline.
2. The solid metal hydrogen absorption and desorption kinetics safety monitoring device according to claim 1, wherein the gas unit comprises a nitrogen cylinder (2) and a hydrogen cylinder (3); the vacuum pump (1), the nitrogen cylinder (2) and the hydrogen cylinder (3) are connected in parallel at the front side of the gas transmission pipeline.
3. The safety monitoring device for the hydrogen absorption and desorption kinetics of the solid metal according to claim 1, wherein a first valve (4) is arranged at the parallel connection part of the vacuum pump (1) and the nitrogen cylinder (2); a second valve (5) is arranged at the parallel connection interface of the hydrogen cylinder (3); a third valve (6) is arranged on the front side of the gas transmission pipeline; a branch pipe is arranged on a gas transmission pipeline between the reference tank (8) and the sample tank (15), and a fifth valve (12) is arranged on the branch pipe; a fourth valve (11) is arranged on the gas transmission pipeline between the rear side of the reference tank (8) and the joint of the branch pipes; a sixth valve (13) is arranged on the gas transmission pipeline between the front side of the sample tank (15) and the joint of the branch pipes; a seventh valve (16) is arranged on the gas transmission pipeline at the rear side of the sample tank (15).
4. The safety monitoring device for the hydrogen absorption and desorption kinetics of the solid metal according to claim 1, wherein the oil bath heating device (9) comprises an oil bath box (91), a lifting platform (92), a flip cover (93), a console (94), a lifting cylinder (95) and a stirring device (96); the reference tank (8) and the sample tank (15) are respectively arranged in the oil bath tank (91); the lifting platform (92) is positioned at the top of the oil bath box (91), four corners of the bottom of the lifting platform are respectively connected with lifting cylinders (95), and lifting of the lifting platform (92) is controlled through telescopic movement of the lifting cylinders (95); the stirring device (96) is arranged in the center of the lifting platform (92) and is lifted together with the lifting platform (92); the control console (94) is positioned outside the oil bath box (91) and is in circuit connection with a heating device, a lifting cylinder (95) and a stirring device (96) in the oil bath box (91); the flip (93) is hinged to the upper part of the lifting platform (92), and two through holes (98) for leading out a gas transmission pipeline are reserved corresponding to the reference tank (8) and the sample tank (15).
5. The safety monitoring device for the hydrogen absorption and desorption kinetics of the solid metal according to claim 4, wherein the bottom of the lifting platform (92) is further provided with four groups of limiting rods (96); four groups of limit blocks (97) are correspondingly arranged at the top of the oil bath box (91), the limit rod (96) penetrates through the limit block (97), a rubber sleeve is sleeved at the bottom end of the limit rod (96), and the size of the rubber sleeve is larger than that of a through hole in the limit block (97).
6. A method for monitoring the hydrogen absorption and desorption kinetics of a solid metal by using the device of claim 1, comprising the steps of:
s1: connecting and sealing a reference tank (8) and a sample tank (15) with a gas transmission pipeline, and immersing the reference tank and the sample tank in an oil bath heating device (9);
s2: opening a vacuum pump (1), vacuumizing a reference tank (8) and a sample tank (15) through a gas transmission pipeline, and then cutting off a pipeline corresponding to the vacuum pump (1);
s3: setting a test temperature of an oil bath heating device (9), and heating a reference tank (8) and a sample tank (15) to the test temperature;
s4: inputting hydrogen with a certain pressure into a reference tank (8) through a gas unit, then communicating the reference tank (8) with a sample tank (15), enabling part of hydrogen in the reference tank (8) to enter the sample tank (15), testing sample materials in the sample tank (15) to perform hydrogen absorption reaction, recording balance time and balance pressure after the pressure in the tank is stable, and calculating hydrogen variation according to variation of the pressure in the tank before and after the reaction and a gas state equation;
s5: closing the sample tank (15), then gradually injecting hydrogen into the reference tank (8) in the same amount, and after each hydrogenation is completed, communicating the reference tank (8) with the sample tank (15) to obtain balance points and balance time of different hydrogen absorption amounts, and stopping hydrogenation until the hydrogen absorption amount is not increased any more;
s6: purging and evacuating residual hydrogen in the reference tank, and then vacuumizing;
s7: and obtaining a relationship curve of equilibrium hydrogen pressure and hydrogen absorption concentration of the sample under the test temperature condition in the hydrogen absorption and desorption cycle process and a curve of time variation of the hydrogen absorption and desorption quantity of the sample.
7. The method for monitoring the hydrogen absorption and desorption kinetics of solid metal according to claim 6, wherein in the step S3, the test temperature of the oil bath heating device (9) is controlled to be 100-400 ℃.
8. The method for monitoring the hydrogen absorption and desorption kinetics of solid metal according to claim 6, wherein in the step S4, the pressure of the hydrogen input into the reference tank (8) is controlled to be 0.01-4 MPa.
9. The method for monitoring the hydrogen absorption and desorption kinetics of solid metal according to claim 6, wherein in step S4, the method for calculating the hydrogen variation is as follows:
wherein ΔC—Single step Hydrogen absorption Capacity, i.e., hydrogen variation, in wt%;
w-hydride mass, g;
r-ideal gas constant, r= 8.314472j·mol -1 ·K -1 ；
P 1 -referring to tank pressure, MPa after hydrogen is introduced;
V 1 -reference tank volume, mL;
Z 1 -a pre-reaction reference tank volume compression factor;
T 1 -referring to the tank temperature before the reaction, c;
P 2 -pressure of sample tank before hydrogen is introduced, MPa;
V 2 -sample tank volume, mL;
Z 2 -a pre-reaction sample tank volume compression factor;
P eq -equilibrium pressure in the sample tank, MPa;
T 2 -equilibrium temperature in sample tank and reference tank, i.e. oil bath set temperature, deg.c;
Z 1 ' reference tank volume compression factor after reaction;
Z 2 ' -sample tank volume compression factor after reaction.
10. The method for monitoring the hydrogen absorption and desorption kinetics of solid metal according to claim 6, wherein in step S5, the pressure of hydrogen gas injected into the reference tank (8) is 0.01-0.05 MPa each time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310192049.0A CN116399752A (en) | 2023-03-02 | 2023-03-02 | Safety monitoring device and method for solid metal hydrogen absorption and desorption dynamic process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310192049.0A CN116399752A (en) | 2023-03-02 | 2023-03-02 | Safety monitoring device and method for solid metal hydrogen absorption and desorption dynamic process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116399752A true CN116399752A (en) | 2023-07-07 |
Family
ID=87011424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310192049.0A Pending CN116399752A (en) | 2023-03-02 | 2023-03-02 | Safety monitoring device and method for solid metal hydrogen absorption and desorption dynamic process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116399752A (en) |
-
2023
- 2023-03-02 CN CN202310192049.0A patent/CN116399752A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111208037B (en) | Method for measuring absolute adsorption quantity of rock sample and method for measuring isothermal adsorption curve of rock sample | |
| CN110160885A (en) | The experimental provision and method of the lower measurement hyposmosis Permeability Oe Coal And Porous Rock And Fractured Rock of multi- scenarios method effect | |
| CN105569637A (en) | Heavy oil thermal recovery microscopic displacement experiment system | |
| CN109932272B (en) | CO (carbon monoxide) 2 Displacement experiment system and displacement experiment method | |
| CN206848111U (en) | Normal temperature and pressure gas solubility determines device | |
| CN109386729A (en) | A kind of pearlife fill system and its fill method | |
| CN116399752A (en) | Safety monitoring device and method for solid metal hydrogen absorption and desorption dynamic process | |
| CN106542600B (en) | Simple and accurate laboratory deoxygenation device and method | |
| US3653414A (en) | Method of charging a thermostatic system with a condensible and a noncondensible medium | |
| CN111777027B (en) | Novel liquid filling equipment | |
| CN112484942A (en) | Method and system for measuring leakage rate of small-volume container | |
| CN110542574A (en) | device for verifying self-blocking behavior of sodium and carbon dioxide reactant and test method | |
| CN102305346B (en) | Low-temperature liquid recovery equipment based on automatic control | |
| CN107340204B (en) | Method for measuring multiple isotherms during a complete charge | |
| CN113916748B (en) | Device and method for measuring shale matrix permeability and recovery ratio by light oil | |
| CN215218624U (en) | Testing arrangement that contains gas coal frost heaving effect | |
| CN213091384U (en) | Large triaxial mechanical test device for simulating freeze-thaw cycle coarse-grained soil | |
| CN107328452A (en) | A kind of device and its operating method for determining irregular seal cavity volume | |
| CN209841472U (en) | Vacuum equipment gassing sampling device | |
| CN114396817A (en) | Liquid metal heat pipe packaging device and method | |
| CN107315025A (en) | The pressure compensation and bleeder of HTHP thermal insulation test process | |
| CN107315029A (en) | The pressure compensation and drainage method of HTHP thermal insulation test process | |
| CN116793893B (en) | Hydrogen content testing device and testing method for high-pressure hydrogen-contacting material | |
| CN216612516U (en) | Oil storage tank for hydrophilic lubricating oil | |
| CN219571619U (en) | System for be used for filling of liquid ammonia in ammonothermal method autoclave |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |