CN112326501B - A hydrogen storage material multiple performance testing system and testing method - Google Patents
A hydrogen storage material multiple performance testing system and testing method Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 284
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 284
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 278
- 238000012360 testing method Methods 0.000 title claims abstract description 85
- 239000011232 storage material Substances 0.000 title claims abstract description 66
- 239000007789 gas Substances 0.000 claims abstract description 177
- 238000003860 storage Methods 0.000 claims abstract description 116
- 238000006243 chemical reaction Methods 0.000 claims abstract description 67
- 238000012544 monitoring process Methods 0.000 claims abstract description 31
- 238000012545 processing Methods 0.000 claims abstract description 19
- 238000005259 measurement Methods 0.000 claims abstract description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 144
- 239000001569 carbon dioxide Substances 0.000 claims description 72
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 72
- 230000008859 change Effects 0.000 claims description 52
- 239000004215 Carbon black (E152) Substances 0.000 claims description 47
- 229930195733 hydrocarbon Natural products 0.000 claims description 47
- 150000002430 hydrocarbons Chemical class 0.000 claims description 47
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 46
- 238000000034 method Methods 0.000 claims description 36
- 238000010521 absorption reaction Methods 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 23
- 230000008569 process Effects 0.000 claims description 22
- 239000001307 helium Substances 0.000 claims description 19
- 229910052734 helium Inorganic materials 0.000 claims description 19
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 19
- 229910000831 Steel Inorganic materials 0.000 claims description 18
- 239000010959 steel Substances 0.000 claims description 18
- 239000000498 cooling water Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 13
- 150000002431 hydrogen Chemical class 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000013094 purity test Methods 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims 2
- 230000007423 decrease Effects 0.000 claims 1
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 238000003795 desorption Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000004590 computer program Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- 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
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Abstract
本发明涉及储氢材料性能测试技术领域，公开了一种储氢材料多种性能测试系统，包括主管路、高压气源子系统、气体储存子系统、反应子系统、温度控制子系统、热导监测子系统、排气子系统、数据采集处理子系统、第一压力传感器和第二压力传感器；本系统可完成：反应室容积的标定、测定反应室的泄漏率、不同氢气纯度下储氢材料的性能测试、储/释氢前后氢气纯度测定、不同初始氢气纯度下储氢材料的循环寿命的测试等。本发明还公开了一种氢材料多种性能测试系统的测试方法，由计算机控制，操作方便、测量参数齐全、精准度较高，从而更好地获得储氢材料在不同充氢纯度下的性能。
The present invention relates to the technical field of hydrogen storage material performance testing, and discloses a hydrogen storage material multiple performance testing system, including a main pipeline, a high-pressure gas source subsystem, a gas storage subsystem, a reaction subsystem, a temperature control subsystem, a thermal conductivity monitoring subsystem, an exhaust subsystem, a data acquisition and processing subsystem, a first pressure sensor, and a second pressure sensor; the system can complete: calibration of the reaction chamber volume, determination of the leakage rate of the reaction chamber, performance testing of hydrogen storage materials under different hydrogen purities, determination of hydrogen purity before and after hydrogen storage/release, and testing of the cycle life of hydrogen storage materials under different initial hydrogen purities, etc. The present invention also discloses a testing method for a hydrogen material multiple performance testing system, which is controlled by a computer, is easy to operate, has complete measurement parameters, and has high accuracy, so as to better obtain the performance of hydrogen storage materials under different hydrogen charging purities.
Description
Technical Field
The invention relates to the technical field of performance testing of hydrogen storage materials, in particular to a system and a method for testing various performances of a hydrogen storage material.
Background
The hydrogen is used as a clean energy source, has the characteristics of large reserve quantity, easy preparation, no pollution and the like, and has great potential as a new energy source for replacing the traditional energy source under the time background of constructing a resource-saving and environment-friendly society. The preparation, storage and transportation of hydrogen are all key problems in utilizing hydrogen energy.
The existing hydrogen storage technology can be divided into three types, namely a gaseous hydrogen storage technology, a liquid hydrogen storage technology, a solid hydrogen storage technology and a solid hydrogen storage material, wherein the gaseous hydrogen storage technology compresses hydrogen to store the hydrogen in a high-pressure container, the liquid hydrogen storage technology stores the liquefied hydrogen in a heat-insulating container after low-temperature high-pressure liquefaction, and the solid hydrogen storage technology combines the hydrogen and the solid hydrogen storage material in a physical or chemical mode. The three methods are widely applied in different fields. The continuous emergence of various hydrogen storage materials has also prompted the continued advancement of hydrogen storage material testing methods.
The patent name of 201210462073.3 is a new method for representing the hydrogen absorption and desorption PCT curve of a hydrogen storage material and a testing device thereof, and discloses a testing device capable of representing the hydrogen absorption and desorption PCT curve of the hydrogen storage material. Application number: 201811635247.5, a patent name, namely an automatic tester for the cycle life of a hydrogen storage material and a testing method, discloses an automatic tester for the cycle life of the hydrogen storage material, which is mainly used for automatic testing of the cycle life of the hydrogen storage material, can obtain the hydrogen charging and discharging performance change of the hydrogen storage material under different cycle times through automatic testing set by a computer, but ignores whether hydrogen after multiple cycles can lead to the reduction of the purity of the hydrogen so as not to meet the production and design requirements.
The hydrogen storage performance of the hydrogen storage material, the cycle life of the hydrogen storage material and the change of the purity of the hydrogen before and after the hydrogen storage technology is used are all important parameters for checking whether the hydrogen storage material can be put into use. The pressure-composition isotherm (PCT curve) is an important characteristic curve taking into consideration the performance of the hydrogen storage material, and can obtain the adsorption amount of the hydrogen storage material at a certain temperature, the decomposition pressure value of the hydride, and the like. The hydrogen storage material has disproportionation reaction in the repeated use process, so that a small part of powder is generated to be coagulated, the process is irreversible, and the hydrogen storage capacity and the service life of the hydrogen storage material are greatly reduced. Thus, the cycle life of the material is also an important parameter. The hydrogen purity is reduced, so that the hydrogen cannot meet the design requirement and the production safety, and cannot meet the use requirement of a user on high-purity hydrogen, so that the change of the hydrogen purity before and after hydrogen storage is tested, whether the reason for influencing the hydrogen purity is found out, and further improvement measures are found out.
Therefore, it is necessary to design a hydrogen storage material performance test system that can accommodate a variety of conditions and measure a plurality of parameters simultaneously.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a system for testing various performances of a hydrogen storage material, which is used for testing the performances of the hydrogen storage material under different initial hydrogen purities, detecting the hydrogen storage/release capacity, the cycle life and the hydrogen purity change before and after reaction of the hydrogen storage material. The invention also provides a method for testing various performances of the hydrogen storage material, which has simple steps and is convenient to implement.
The hydrogen storage material performance test system comprises a main pipeline, a high-pressure gas source subsystem, a gas storage subsystem, a reaction subsystem, a temperature control subsystem, a thermal conductivity monitoring subsystem, an exhaust subsystem, a data acquisition processing subsystem, a first pressure sensor and a second pressure sensor, wherein the high-pressure gas source subsystem comprises a pure argon gas cylinder, a pure helium gas cylinder, a high-pressure hydrogen cylinder, a pure carbon dioxide gas cylinder, a first filter, a first stop valve, a second stop valve, a first electric control valve and a second electric control valve, the first filter is arranged at the outlet ends of the pure argon gas cylinder, the pure helium gas cylinder, the high-pressure hydrogen cylinder and the pure carbon dioxide gas cylinder, the pure argon gas cylinder is connected with the main pipeline through the first stop valve, the pure helium gas cylinder is connected with the main pipeline through the second stop valve, the high-pressure hydrogen cylinder is connected with the pure carbon dioxide gas cylinder through the first electric control valve and the second electric control valve, and is positioned in front of a third electric control valve on the main pipeline;
The gas storage subsystem comprises a first gas storage tank, a second filter, a fifth electric control valve and a sixth electric control valve, wherein the second filter is arranged at the opening ends of the first gas storage tank and the second gas storage tank, the opening end of the first gas storage tank is connected with a main pipeline through the fifth electric control valve, the opening end of the second gas storage tank is connected with the main pipeline through the sixth electric control valve, and the connection parts of the first gas storage tank and the second gas storage tank and the main pipeline are sequentially positioned behind the third electric control valve;
The reaction subsystem comprises a reaction chamber, a third filter, a fourth electric control valve and a third stop valve, wherein an air inlet of the reaction chamber is connected with a main pipeline and is positioned between the joint of a first air storage tank and the main pipeline and the joint of a second air storage tank and the main pipeline, the third filter, the fourth electric control valve and the third stop valve are sequentially arranged between the air inlet of the reaction chamber and the main pipeline;
The main pipeline is also provided with a seventh electric control valve, the seventh electric control valve is positioned at the rear of the joint of the second air storage tank and the main pipeline, the exhaust subsystem and the thermal conductivity monitoring subsystem are connected with the main pipeline and positioned at the rear of the seventh electric control valve, and the temperature control subsystem, the thermal conductivity monitoring subsystem, the exhaust subsystem, the first electric control valve, the second electric control valve, the third electric control valve, the fourth electric control valve, the fifth electric control valve, the sixth electric control valve, the seventh electric control valve, the first pressure sensor and the second pressure sensor are all connected with the data acquisition processing subsystem.
The reaction chamber comprises a sample chamber and a jacket type heat exchanger, wherein the jacket type heat exchanger is coated on the periphery of the sample chamber, an air inlet is formed in the top end of the sample chamber, a high-temperature steam inlet is formed in the top end of one side of the jacket type heat exchanger, a cooling water inlet is formed in the bottom end of the other side of the jacket type heat exchanger, a cooling water outlet is formed in the top end of the other side of the jacket type heat exchanger, a condensed water outlet is formed in the bottom end of the other side of the jacket type heat exchanger, and the high-temperature steam inlet and the cooling water inlet are connected with a temperature control subsystem.
Further, the thermal conductivity monitoring subsystem comprises a thermal conduit connected with the main pipeline, a fourth stop valve, a first heater and a thermal conductivity cell are sequentially installed on the thermal conduit, and the first heater and the thermal conductivity cell are connected with the data acquisition and processing subsystem.
Further, the exhaust subsystem includes an evacuation portion and a vacuum portion, each connected and in parallel with the main conduit; the evacuation part comprises a first branch and a second branch which are connected with a main pipeline, a first flow limiting valve is arranged on the first branch, a fifth stop valve and a carbon dioxide steel cylinder are sequentially arranged on the second branch, the vacuum part comprises a vacuumizing pipeline connected with the main pipeline, and an eighth electric control valve, a second flow limiting valve and a vacuum pump which are sequentially arranged on the vacuumizing pipeline, and the eighth electric control valve is connected with the data acquisition and processing subsystem.
Further, the temperature control subsystem comprises a second heater and a cooler, and the second heater and the cooler are connected with the reaction chamber and the data acquisition and processing subsystem.
The data acquisition processing subsystem comprises a computer and a concentrator, wherein the first electric control valve, the second electric control valve, the third electric control valve, the fourth electric control valve, the fifth electric control valve, the sixth electric control valve, the seventh electric control valve, the thermal conductivity monitoring subsystem, the exhaust subsystem, the temperature control subsystem, the first pressure sensor and the second pressure sensor are all connected with the computer through the concentrator.
Further, a safety valve is arranged on each of the first gas storage tank and the second gas storage tank in the gas storage subsystem.
A testing method of a hydrogen storage material multiple performance testing system comprises the following steps:
And S101, vacuumizing a testing system, namely placing a sample in a sample chamber, placing the sample in a jacketed heat exchanger, connecting a third filter with a fourth electric control valve, connecting the testing system through a third stop valve, opening a seventh electric control valve, an eighth electric control valve and a second flow limiting valve, closing a first stop valve, a second stop valve, a fourth stop valve, a first electric control valve, a second electric control valve and a first flow limiting valve, and opening a vacuum pump to vacuumize for about 15-20 min.
And S201, calibrating the volume of the test system, namely closing all valves, opening a first stop valve, a third electric control valve and a fifth electric control valve, introducing pure argon into the system, recording the pressure in the system at the moment by a first pressure sensor to obtain P 1, opening the third stop valve and the fourth electric control valve to enable the argon in the circulation system to enter a sample chamber, and recording the reading of a second pressure sensor at the moment to obtain P 2.
The existing gas state equation pv= nZRT, where P is the pressure, V is the reaction chamber volume, n is the amount of argon species, R is the gas molar constant, Z is the compression factor:
From P 2Vs=(P1-P2)V1Z2/Z1, the volume of the reaction chamber V s can be determined, where V 1 is the volume of the first hydrogen storage bottle and the compression factor Z 1、Z2 is a function of pressure at constant temperature;
Repeating the step S201 for several times, obtaining a plurality of V s and obtaining an average value so as to reduce errors;
S202, closing all valves, opening a second stop valve, a third electric control valve and a fifth electric control valve, introducing pure helium into the system, recording the pressure in the system at the moment by a first pressure sensor, opening the third stop valve and the fourth electric control valve, enabling helium in the circulating system to enter a sample chamber, and recording the reading of the second pressure sensor at the moment.
Step S202 is repeated as above and V t is obtained from pv= nZRT and averaged, and the average of V s and V t is normally substantially equal.
S301, testing the leakage rate of the test system, namely opening a first electric control valve, a third electric control valve, a fourth electric control valve and a third stop valve, closing a seventh electric control valve, after 8-15 MPa of hydrogen is introduced into the system, closing the first electric control valve and the third electric control valve, operating for 10-20 hours at room temperature, monitoring the pressure changes of a sample chamber, a first air storage tank and a second air storage tank in the process, and performing linear fitting on pressure data of all measurement points to obtain the leakage rate, wherein the leakage rate of a container with good tightness is under 10 -8 mol/S under normal conditions.
S401, after S101-S301 are completed, the test system can conduct the following parameter measurement:
Determination of the purity of the initial hydrogen:
And opening a high-pressure hydrogen cylinder, a pure carbon dioxide steel cylinder, a first electric control valve, a second electric control valve and a fifth electric control valve, controlling the first electric control valve and the second electric control valve by a computer to adjust the flow of hydrogen and carbon dioxide so as to change the purity of the hydrogen in the hydrocarbon mixed gas, enabling the hydrogen and the carbon dioxide to enter the system through a first filter, enabling the hydrogen and the carbon dioxide to flow into a first gas storage tank for a period of time to be uniformly mixed, closing the third electric control valve, opening a seventh electric control valve and a fourth stop valve, enabling the hydrocarbon mixed gas to be heated to a high temperature of 300-500 ℃ through a first heater, entering a heat conduction pool, and recording the heat conductivity lambda 1 at the moment.
Determining the hydrogen storage/release properties of the hydrogen storage material:
And (3) hydrogen is absorbed, namely a fourth electric control valve, a third stop valve, a sixth electric control valve and a seventh electric control valve are closed, a high-pressure hydrogen cylinder, a first electric control valve and a fifth electric control valve are opened, hydrogen enters the system through a first filter, flows into a first gas storage tank for a period of time, pressure change is monitored through a first pressure sensor, then the third stop valve and the fourth electric control valve are opened, the temperature of a sample chamber is kept at a proper low temperature T 1 by a cooler, at the moment, the hydrogen flows into a reaction chamber, the pressure change condition along with time in the hydrogen absorption process is recorded by a second pressure sensor, the pressure is continuously increased, then a hydrogen absorption platform appears, the pressure rises again, and the pressure of the hydrogen absorption platform is recorded.
And (3) discharging hydrogen, namely closing a fifth electric control valve, opening a sixth electric control valve, keeping the temperature of the sample chamber at a proper high temperature T2 by using a second heater, enabling the hydrogen in the sample chamber to flow into a second gas storage tank, opening a fifth stop valve, a seventh electric control valve and a first flow limiting valve when the pressure displayed by the first pressure sensor is similar to the pressure displayed by the second pressure sensor, slowly discharging the hydrogen in the second gas storage tank into the air, and recording the data of the pressure change of the system along with the time by using the second pressure sensor to obtain a PCT curve.
The properties of the hydrogen storage material were determined for different initial hydrogen purities:
the hydrogen absorption process comprises the steps of closing a fourth electric control valve, a third stop valve, a sixth electric control valve and a seventh electric control valve, opening a high-pressure hydrogen cylinder, a pure carbon dioxide cylinder, a first electric control valve, a second electric control valve and a fifth electric control valve, enabling hydrogen and carbon dioxide to enter a main pipeline through a first filter and be mixed, flowing into a first gas storage tank, waiting for a period of time and uniformly mixing, monitoring pressure change through a first pressure sensor, opening the third stop valve and the fourth electric control valve, keeping the temperature of a reaction chamber at a proper low temperature T 1 by using a cooler, enabling hydrocarbon mixed gas to flow into the reaction chamber, recording the pressure change along with time in the hydrogen absorption process by using a second pressure sensor, continuously increasing the pressure, and recording the pressure of a hydrogen absorption platform;
And (3) discharging hydrogen, namely closing a fifth electric control valve, opening a sixth electric control valve, keeping the temperature of the reaction chamber at a proper high temperature T 2 by using a second heater, enabling the hydrocarbon mixed gas in the reaction chamber to flow into a second gas storage tank, opening a fifth stop valve, a seventh electric control valve and a first flow limiting valve when the pressure displayed by the first pressure sensor is similar to the pressure displayed by the second pressure sensor, slowly discharging the hydrocarbon mixed gas in the second gas storage tank into the air, and recording the pressure change of the system along with time by using the second pressure sensor to obtain a pressure-component isotherm (PCT curve) under the purity of the hydrogen.
The hydrogen and carbon dioxide flow rates are regulated by a computer so that the purity of the hydrogen in the hydrocarbon mixed gas is 95%, 90%, 75% and 50% respectively for testing.
Determining the cycle life of the hydrogen storage material at different initial hydrogen purities:
And 1, closing a third stop valve, a sixth electric control valve and a seventh electric control valve, opening a high-pressure hydrogen cylinder, a pure carbon dioxide steel cylinder, a first electric control valve, a second electric control valve, a third electric control valve and a fifth electric control valve, controlling the first electric control valve and the second electric control valve to adjust the flow of hydrogen and carbon dioxide by a computer so as to change the purity of the hydrogen in the hydrocarbon mixed gas, mixing the hydrogen and the carbon dioxide in a system through a first filter, flowing into a first gas storage tank, waiting for a period of time to uniformly mix, monitoring the pressure change through a first pressure sensor, closing the third electric control valve after the pressure reaches a certain value, recording the system pressure P 3 at the moment, opening the third stop valve and the second electric control valve, flowing the hydrocarbon mixed gas into a reaction chamber, keeping the temperature of the reaction chamber to be a low temperature T 1 by a cooler, monitoring the pressure change by a second pressure sensor, and recording the pressure P 4 after the pressure change is stabilized.
And 2, closing a fifth electric control valve, opening a sixth electric control valve, using a second heater to keep the temperature of the reaction chamber at a high temperature T 2, enabling the hydrocarbon mixed gas in the reaction chamber to flow to a second gas storage tank, reducing the pressure of the system, monitoring the pressure change through a second pressure sensor, recording the pressure P 5 at the moment, opening a seventh electric control valve, a fifth stop valve and a first flow limiting valve, enabling the purity of hydrogen to be reduced after the hydrocarbon mixed gas is mixed with carbon dioxide, exhausting the gas in the system to the air, closing the fifth stop valve and the first flow limiting valve, opening the eighth electric control valve and the second flow limiting valve, and vacuumizing the system for 15-20min.
Setting the circulation times in a computer, circulating the step 1 and the step 2 for a plurality of times, automatically stopping after the circulation times are reached, and recording data.
Determination of the purity variation of hydrogen before and after cycling:
Initial hydrogen purity testing step:
And opening a high-pressure hydrogen cylinder, a pure carbon dioxide steel cylinder, a first electric control valve, a second electric control valve and a fifth electric control valve, controlling the first electric control valve and the second electric control valve by a computer to adjust the flow of hydrogen and carbon dioxide so as to change the purity of the hydrogen in the hydrocarbon mixed gas, respectively entering the system through a first filter to mix the hydrogen and the carbon dioxide, flowing into a first air storage tank, waiting for a period of time to uniformly mix the hydrogen and the carbon dioxide, then closing the third electric control valve, opening a seventh electric control valve and a fourth stop valve, heating the hydrocarbon mixed gas to a high temperature of 300-500 ℃ through a first heater, entering a thermal conductivity tank, and recording the thermal conductivity lambda 1 at the moment.
The hydrogen purity after circulation test step:
and only opening a fourth electric control valve, a third stop valve, a seventh electric control valve and a fourth stop valve, and allowing hydrocarbon mixed gas to flow out of the sample chamber, heating to a high temperature of 300-500 ℃ by a first heater, then entering a thermal conductivity pool, and recording the thermal conductivity lambda 2 at the moment.
Compared with the prior art, the invention has the following advantages:
1. The test system can adapt to various conditions and simultaneously measure the performance of the hydrogen storage material with various parameters. The high-pressure gas source of the test system consists of four gases, and the purity of the hydrogen in the hydrocarbon mixed gas entering the system can be changed by changing the flow of the hydrogen and the carbon dioxide, so that the performance parameters of the hydrogen storage material under different initial hydrogen purities can be obtained. The test system combines the hydrogen absorption and desorption test subsystem and the thermal conductivity monitoring subsystem, and can determine various performances of the hydrogen storage material through program setting, and the test system is convenient and safe to use and has comprehensive and sufficient monitoring parameters. The pressure sensor, the electric control valve and the temperature control subsystem of the test system are connected with the data acquisition and processing subsystem, and can automatically control the charging and discharging temperature and the valve to open and close in the circulation process, so that the test system can be operated for a long time, the manual operation is reduced, and the test efficiency and the test accuracy are improved.
2. The testing process of the testing system is controlled by a computer, the operation is convenient, the measuring parameters are complete, the accuracy is high, and the performance of the hydrogen storage material under different hydrogen charging purities can be better obtained.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application. In the drawings:
FIG. 1 is a schematic diagram showing the construction of a system for testing various properties of a hydrogen storage material according to the present invention;
FIG. 2 shows a schematic structural view of a reaction chamber according to the present invention;
In the figure, 1 is a main pipeline; 101 is a third electrically controlled valve; 102 is a seventh electrically controlled valve; 2 is a high-pressure gas source subsystem, 201 is a pure argon gas cylinder, 202 is a pure helium gas cylinder, 203 is a high-pressure hydrogen cylinder, 204 is a pure carbon dioxide cylinder, 205 is a first filter, 206 is a first stop valve, 207 is a second stop valve, 208 is a first electric control valve, 209 is a second electric control valve, 3 is a gas storage subsystem, 301 is a first gas storage tank, 302 is a second gas storage tank, 303 is a second filter, 304 is a fifth electric control valve, 305 is a sixth electric control valve, 4 is a reaction subsystem, 401 is a reaction chamber, 402 is a third filter, 403 is a fourth electric control valve, 404 is a third stop valve, 405 is a sample chamber, 406 is a jacketed heat exchanger, 407 is a gas inlet, 408 is a high-temperature steam inlet, 409 is a cooling water inlet, 410 is a cooling water outlet 411 is a condensed water outlet, 5 is a temperature control subsystem, 501 is a second heater, 502 is a cooler, 6 is a thermal conductivity monitoring subsystem, 601 is a heat conduction pipeline, 602 is a fourth stop valve, 603 is a first heater, 604 is a fifth electric control valve, 305 is a sixth electric control valve, 305 is a fourth heat exchanger, 305 is a vacuum pump, 404 is a vacuum pump to be tested, 702 is a vacuum stop valve is a vacuum pump to be tested, and a vacuum pump is a vacuum stop valve is a vacuum pump to be tested, and is a vacuum stop valve, and is a vacuum pump is a vacuum stop valve, and a vacuum valve is used as a vacuum stop valve, and a vacuum pump, and is a vacuum.
Detailed Description
The invention is further described below with reference to the drawings and examples.
The system for testing various performances of the hydrogen storage materials comprises a main pipeline 1, a high-pressure gas source subsystem 2, a gas storage subsystem 3, a reaction subsystem 4, a temperature control subsystem 5, a thermal conductivity monitoring subsystem 6, an exhaust subsystem 7, a data acquisition processing subsystem, a first pressure sensor 8 and a second pressure sensor 9, wherein the high-pressure gas source subsystem 2 comprises a pure argon cylinder 201, a pure helium cylinder 202, a high-pressure hydrogen cylinder 203, a pure carbon dioxide cylinder 204, a first filter 205, a first stop valve 206, a second stop valve 207, a first electric control valve 208 and a second electric control valve 209, the outlet ends of the pure argon cylinder 201, the pure helium 202, the high-pressure hydrogen cylinder 203 and the pure carbon dioxide cylinder 204 are respectively provided with the first filter 205, the pure argon cylinder 201 is connected with the main pipeline 1 through the first stop valve 206, the pure helium cylinder 202 is connected with the pure carbon dioxide cylinder 204 through the second electric control valve 208 through the first electric control valve 209, and the pure carbon dioxide cylinder 204 is positioned on the main pipeline 1, and the constant-flow stable gas source system is provided with the constant-pressure gas source system 101. The pure argon gas bottle 201, the pure helium gas bottle 202, the high-pressure hydrogen bottle 203 and the pure carbon dioxide gas bottle 204 are 140mm in diameter and 580mm in height and can bear 10-30 MPa, wherein the purity of hydrogen gas of a gas source is not lower than 99.999%, the purity of carbon dioxide is not lower than 99.999%, the purity of helium gas is not lower than 99.999% and the purity of argon gas is not lower than 99.999%. A filter is arranged between the gas storage steel cylinder and the valve, so that the detection system is ensured to be free from impurity introduction.
The gas storage subsystem 3 comprises a first gas storage tank 301, a second gas storage tank 302, a second filter 303, a fifth electric control valve 304 and a sixth electric control valve 305, wherein the second filter 303 is arranged at the open ends of the first gas storage tank 301 and the second gas storage tank 302, the open end of the first gas storage tank 301 is connected with the main pipeline 1 through the fifth electric control valve 304, the open end of the second gas storage tank 302 is connected with the main pipeline 1 through the sixth electric control valve 305, the connection parts of the first gas storage tank 301 and the second gas storage tank 302 and the main pipeline 1 are sequentially positioned behind the third electric control valve 101, and the gas storage subsystem 3 is used for temporarily storing hydrocarbon mixed gas entering from the high-pressure gas source subsystem 2, so that the hydrogen to be tested and the carbon dioxide are uniformly mixed and the pressure is stabilized, and then the mixed gas is introduced into the reaction chamber 401 for absorption, and the accuracy of the test is ensured. The diameters of the two air storage tanks are 108mm, the height is 150mm, and the bearing capacity is 10-30 MPa. The pressure change in the first gas storage tank can be monitored through the first pressure sensor, meanwhile, the two gas storage tanks are respectively connected with the safety valve 12, and exhaust gas can be automatically opened when the pressure is too high, so that safety accidents caused by the too high pressure are prevented. The fifth electric control valve 304 and the sixth electric control valve 305 are connected with the hub 11, semi-automatic operation can be realized through computer program control, and hydrocarbon mixed gas entering the test system from the high-pressure gas source subsystem 2 firstly enters the first gas storage tank 301 to be uniformly mixed, and then enters the reaction subsystem 4 after being stabilized.
The reaction subsystem 4 comprises a reaction chamber 401, a third filter 402, a fourth electric control valve 403 and a third stop valve 404, wherein an air inlet 407 of the reaction chamber 401 is connected with the main pipeline 1 and is positioned between the connection part of the first air storage tank 301 and the main pipeline 1 and the connection part of the second air storage tank 302 and the main pipeline 1, the third filter 402, the fourth electric control valve 403 and the third stop valve 404 are sequentially arranged between the air inlet 407 of the reaction chamber 401 and the main pipeline 1, the first pressure sensor 8 is arranged on the main pipeline 1 and is positioned between the first air storage tank 301 and the reaction chamber 401, the second pressure sensor 9 is arranged between the fourth electric control valve 403 and the third stop valve 404, and the temperature control subsystem 5 is connected with the reaction chamber 401.
The main pipeline 1 is further provided with a seventh electric control valve 102, the seventh electric control valve 102 is located at the rear of the joint of the second air storage tank 302 and the main pipeline 1, the exhaust subsystem 7 and the thermal conductivity monitoring subsystem 6 are connected with the main pipeline 1 and located at the rear of the seventh electric control valve 102, and the temperature control subsystem 5, the thermal conductivity monitoring subsystem 6, the exhaust subsystem 7, the first electric control valve 208, the second electric control valve 209, the third electric control valve 101, the fourth electric control valve 403, the fifth electric control valve 304, the sixth electric control valve 305, the seventh electric control valve 102, the first pressure sensor 8 and the second pressure sensor 9 are all connected with the data acquisition processing subsystem.
As shown in FIG. 2, the reaction chamber 401 comprises a sample chamber 405 and a jacketed heat exchanger 406, wherein the jacketed heat exchanger 406 and the sample chamber 405 are S-1L type double-layer glass reaction kettles, an air inlet 407 is formed in the top end of the sample chamber 405, a high-temperature steam inlet 408 is formed in the top end of one side of the jacketed heat exchanger 406, a cooling water inlet 409 is formed in the bottom end of the jacketed heat exchanger, a cooling water outlet 410 is formed in the top end of the other side of the jacketed heat exchanger, a condensed water outlet 411 is formed in the bottom end of the jacketed heat exchanger, and the high-temperature steam inlet 408 and the cooling water inlet 409 are connected with a temperature control subsystem. As shown in fig. 2, a hydrogen storage material (sample 13 to be measured) is placed in a sample chamber 405, a mixed gas of hydrogen and carbon dioxide enters a reaction subsystem 4 from an air inlet 407, when the reaction subsystem 4 is cooled, cooling water flows from a cooling water inlet 409 to a cooling water outlet 410 from bottom to top, and when the reaction subsystem 4 is heated, high-temperature steam flows from a high-temperature steam inlet 408 to a condensed water outlet 411 from top to bottom. The reaction subsystem 4 is connected with the temperature control subsystem 5, and the temperature is controlled to control the hydrogen storage/release operation, so that the cooler 502 is opened to supply cooling water to enable the interior of the jacketed heat exchanger 406 to be at a low temperature T 1 in the hydrogen absorption process of the hydrogen storage material, and the second heater 501 is opened to supply high-temperature steam to enable the interior of the jacketed heat exchanger 406 to be at a high temperature T 2 in the hydrogen storage material hydrogen release process. The jacketed heat exchanger 406 serves to keep the heat warm.
The thermal conductivity monitoring subsystem 6 comprises a thermal conduit 601 connected with the main pipeline 1, a fourth stop valve 602, a first heater 603 and a thermal conductivity cell 604 are sequentially installed on the thermal conduit 601, and the first heater 603 and the thermal conductivity cell 504 are connected with the computer 10. The gas to be measured passing through the first heater 603 is heated to a high temperature of 300-500 ℃ and enters the thermal conductivity cell 604, and the detection principle is that the temperature of the thermosensitive element is changed according to the concentration change of the gas to be measured, so that the resistance is changed, and the Wheatstone bridge is unbalanced to generate an electric signal.
The exhaust subsystem 7 comprises an exhaust part and a vacuum part which are connected with the main pipeline 1 in parallel, wherein the exhaust part comprises a first branch 701 and a second branch 703 which are connected with the main pipeline 1, a first flow limiting valve 702 is arranged on the first branch 701, a fifth stop valve 704 and a carbon dioxide steel cylinder 705 are sequentially arranged on the second branch 703, the vacuum part comprises a vacuumizing pipeline 706 connected with the main pipeline 1, and an eighth electric control valve 707, a second flow limiting valve 708 and a vacuum pump 709 which are sequentially arranged on the vacuumizing pipeline 706, and the eighth electric control valve 707 is connected with a computer. The exhaust subsystem 7 is connected with the main pipeline 1 through a seventh electric control valve 102, and consists of an evacuation part and a vacuum part which are connected in parallel, wherein the evacuation part is provided with a carbon dioxide steel bottle 705, and the discharged carbon dioxide is mixed with the hydrogen discharged by the test system and then discharged into the air to prevent the explosion caused by the overhigh concentration of the hydrogen. The vacuum pump 709 is arranged at the vacuum part, the gas in the system is pumped out before the test, the interference of other impurities (such as water vapor) is eliminated, the mixed gas with accurate proportion is ensured to be carried out, and the eighth electric control valve 707 in the vacuumizing pipeline 706 is connected with the second flow limiting valve 708, so that the gas flow can be effectively controlled during vacuumizing, and the loss of the sample in the reaction chamber caused by suck-back can be prevented.
The temperature control subsystem 5 includes a second heater 501 and a cooler 502, both the second heater 501 (existing electric steam generator) and the cooler 502 (existing cooling water circulation device) being connected to the reaction chamber 401 and the computer 10. The hot steam or cold flow required for the test is provided to the reaction chamber 401 by the control of the computer 10.
The data acquisition and processing subsystem comprises a computer 10 and a hub 11, wherein the first to eighth electric control valves, the first pressure sensor 8, the second pressure sensor 9, the first and second heaters, the cooler 502 and the heat conduction pool 604 are all connected with the computer 10 through the hub 11. The method is used for recording parameters such as hydrogen purity, system pressure, temperature and the like in the hydrogen storage/release process. The hydrogen storage/release system comprises a thermal conductivity cell 604, a first pressure sensor and a second pressure sensor, wherein the first pressure sensor and the second pressure sensor are connected with a computer to monitor the change of the purity of hydrogen and the change of the pressure of a system in the hydrogen storage/release process, the computer is connected with a second heater 501 and a cooler 502 to change the hydrogen storage/release state of a material by changing the temperature, and meanwhile, the computer is connected with a first electric control valve, a second electric control valve and an eighth electric control valve, and the opening and the closing of the valves can be controlled according to program setting.
A testing method of a hydrogen storage material multiple performance testing system comprises the following steps:
And S101, vacuumizing a testing system, namely placing a sample 13 to be tested in a sample chamber, placing the sample chamber in a jacketed heat exchanger, connecting a third filter with a fourth electric control valve, connecting the testing system through a third stop valve, opening a seventh electric control valve, an eighth electric control valve and a second flow limiting valve, closing a first stop valve, a second stop valve, a fourth stop valve, a first electric control valve, a second electric control valve and a first flow limiting valve, and opening a vacuum pump to vacuumize for about 15-20 min.
And S201, calibrating the volume of the test system, namely closing all valves, opening a first stop valve, a third electric control valve and a fifth electric control valve, introducing pure argon into the system, recording the pressure in the system at the moment by a first pressure sensor to obtain P 1, opening the third stop valve and the fourth electric control valve to enable the argon in the circulation system to enter a sample chamber, and recording the reading of a second pressure sensor at the moment to obtain P 2. When the volume is calibrated, pure helium and pure argon are used, so that the material in the reaction chamber is prevented from being sucked into hydrogen in advance to influence the subsequent test.
The existing gas state equation pv= nZRT, where P is the pressure, V is the reaction chamber volume, n is the amount of argon species, R is the gas molar constant, Z is the compression factor:
From P 2Vs=(P1-P2)V1Z2/Z1, the volume of the reaction chamber V s can be determined, where V 1 is the volume of the first hydrogen storage bottle and the compression factor Z 1、Z2 is a function of pressure at constant temperature;
Repeating the step S201 for several times, obtaining a plurality of V s and obtaining an average value so as to reduce errors;
S202, closing all valves, opening a second stop valve, a third electric control valve and a fifth electric control valve, introducing pure helium into the system, recording the pressure in the system at the moment by a first pressure sensor, opening the third stop valve and the fourth electric control valve, enabling helium in the circulating system to enter a sample chamber, and recording the reading of the second pressure sensor at the moment.
Step S202 is repeated as above and V t is obtained from pv= nZRT and averaged, and the average of V s and V t is normally substantially equal.
S301, testing the leakage rate of the test system, namely opening a first electric control valve, a third electric control valve, a fourth electric control valve and a third stop valve, closing a seventh electric control valve, after 8-15 MPa of hydrogen is introduced into the system, closing the first electric control valve and the third electric control valve, operating for 10-20 hours at room temperature, monitoring the pressure changes of a sample chamber, a first air storage tank and a second air storage tank in the process, and performing linear fitting on pressure data of all measurement points to obtain the leakage rate, wherein the leakage rate of a container with good tightness is under 10 -8 mol/S under normal conditions.
S401, after S101-S301 are completed, the test system can conduct the following parameter measurement:
Determination of the purity of the initial hydrogen:
And opening a high-pressure hydrogen cylinder, a pure carbon dioxide steel cylinder, a first electric control valve, a second electric control valve and a fifth electric control valve, controlling the first electric control valve and the second electric control valve by a computer to adjust the flow of hydrogen and carbon dioxide so as to change the purity of the hydrogen in the hydrocarbon mixed gas, enabling the hydrogen and the carbon dioxide to enter the system through a first filter, enabling the hydrogen and the carbon dioxide to flow into a first gas storage tank for a period of time to be uniformly mixed, closing the third electric control valve, opening a seventh electric control valve and a fourth stop valve, enabling the hydrocarbon mixed gas to be heated to a high temperature of 300-500 ℃ through a first heater, entering a heat conduction pool, and recording the heat conductivity lambda 1 at the moment.
Determining the hydrogen storage/release properties of the hydrogen storage material:
And (3) hydrogen is absorbed, namely a fourth electric control valve, a third stop valve, a sixth electric control valve and a seventh electric control valve are closed, a high-pressure hydrogen cylinder, a first electric control valve and a fifth electric control valve are opened, hydrogen enters the system through a first filter, flows into a first gas storage tank for a period of time, pressure change is monitored through a first pressure sensor, then the third stop valve and the fourth electric control valve are opened, the temperature of a sample chamber is kept at a proper low temperature T 1 by a cooler, at the moment, the hydrogen flows into a reaction chamber, the pressure change condition along with time in the hydrogen absorption process is recorded by a second pressure sensor, the pressure is continuously increased, then a hydrogen absorption platform appears, the pressure rises again, and the pressure of the hydrogen absorption platform is recorded.
And (3) discharging hydrogen, namely closing a fifth electric control valve, opening a sixth electric control valve, keeping the temperature of the sample chamber at a proper high temperature T 2 by using a second heater, enabling the hydrogen in the sample chamber to flow into a second gas storage tank, opening a fifth stop valve, a seventh electric control valve and a first flow limiting valve when the pressure displayed by the first pressure sensor is similar to the pressure displayed by the second pressure sensor, slowly discharging the hydrogen in the second gas storage tank into the air, and recording the data of the pressure change of the system along with time by using the second pressure sensor to obtain a PCT curve.
Performance test of hydrogen storage materials at different initial hydrogen purities:
the hydrogen absorption process comprises the steps of closing a fourth electric control valve, a third stop valve, a sixth electric control valve and a seventh electric control valve, opening a high-pressure hydrogen cylinder, a pure carbon dioxide cylinder, a first electric control valve, a second electric control valve and a fifth electric control valve, enabling hydrogen and carbon dioxide to enter a main pipeline through a first filter and be mixed, flowing into a first gas storage tank, waiting for a period of time and uniformly mixing, monitoring pressure change through a first pressure sensor, opening the third stop valve and the fourth electric control valve, keeping the temperature of a reaction chamber at a proper low temperature T 1 by using a cooler, enabling hydrocarbon mixed gas to flow into the reaction chamber, recording the pressure change along with time in the hydrogen absorption process by using a second pressure sensor, continuously increasing the pressure, and recording the pressure of a hydrogen absorption platform;
And (3) discharging hydrogen, namely closing a fifth electric control valve, opening a sixth electric control valve, keeping the temperature of the reaction chamber at a proper high temperature T 2 by using a second heater, enabling the hydrocarbon mixed gas in the reaction chamber to flow into a second gas storage tank, opening a fifth stop valve, a seventh electric control valve and a first flow limiting valve when the pressure displayed by the first pressure sensor is similar to the pressure displayed by the second pressure sensor, slowly discharging the hydrocarbon mixed gas in the second gas storage tank into the air, and recording the pressure change of the system along with time by using the second pressure sensor to obtain a PCT curve under the purity of the hydrogen.
The hydrogen and carbon dioxide flow rates are regulated by a computer so that the purity of the hydrogen in the hydrocarbon mixed gas is 95%, 90%, 75% and 50% respectively for testing.
Test to determine the cycle life of hydrogen storage materials at different initial hydrogen purities:
And 1, closing a third stop valve, a sixth electric control valve and a seventh electric control valve, opening a high-pressure hydrogen cylinder, a pure carbon dioxide steel cylinder, a first electric control valve, a second electric control valve, a third electric control valve and a fifth electric control valve, controlling the first electric control valve and the second electric control valve to adjust the flow of hydrogen and carbon dioxide by a computer so as to change the purity of the hydrogen in the hydrocarbon mixed gas, mixing the hydrogen and the carbon dioxide in a system through a first filter, flowing into a first gas storage tank, waiting for a period of time to uniformly mix, monitoring the pressure change through a first pressure sensor, closing the third electric control valve after the pressure reaches a certain value, recording the system pressure P 3 at the moment, opening the third stop valve and the second electric control valve, flowing the hydrocarbon mixed gas into a reaction chamber, keeping the temperature of the reaction chamber to be a low temperature T 1 by a cooler, monitoring the pressure change by a second pressure sensor, and recording the pressure P 4 after the pressure change is stabilized.
And 2, closing a fifth electric control valve, opening a sixth electric control valve, using a second heater to keep the temperature of the reaction chamber at a high temperature T 2, enabling the hydrocarbon mixed gas in the reaction chamber to flow to a second gas storage tank, reducing the pressure of the system, monitoring the pressure change through a second pressure sensor, recording the pressure P 5 at the moment, opening a seventh electric control valve, a fifth stop valve and a first flow limiting valve, enabling the purity of hydrogen to be reduced after the hydrocarbon mixed gas is mixed with carbon dioxide, exhausting the gas in the system to the air, closing the fifth stop valve and the first flow limiting valve, opening the eighth electric control valve and the second flow limiting valve, and vacuumizing the system for 15-20min.
Setting the circulation times in a computer, circulating the step 1 and the step 2 for a plurality of times, automatically stopping after the circulation times are reached, and recording data.
Determination of the purity variation of hydrogen before and after cycling:
Initial hydrogen purity testing step:
And opening a high-pressure hydrogen cylinder, a pure carbon dioxide steel cylinder, a first electric control valve, a second electric control valve and a fifth electric control valve, controlling the first electric control valve and the second electric control valve by a computer to adjust the flow of hydrogen and carbon dioxide so as to change the purity of the hydrogen in the hydrocarbon mixed gas, respectively entering the system through a first filter to mix the hydrogen and the carbon dioxide, flowing into a first air storage tank, waiting for a period of time to uniformly mix the hydrogen and the carbon dioxide, then closing the third electric control valve, opening a seventh electric control valve and a fourth stop valve, heating the hydrocarbon mixed gas to a high temperature of 300-500 ℃ through a first heater, entering a thermal conductivity tank, and recording the thermal conductivity lambda 1 at the moment.
The hydrogen purity after circulation test step:
and only opening a fourth electric control valve, a third stop valve, a seventh electric control valve and a fourth stop valve, and allowing hydrocarbon mixed gas to flow out of the sample chamber, heating to a high temperature of 300-500 ℃ by a first heater, then entering a thermal conductivity pool, and recording the thermal conductivity lambda 2 at the moment.
For specific use, reference may be made to the following operations:
preparation of the system before testing:
the pure argon cylinder and the first filter are connected with the first stop valve, the pure helium cylinder and the first filter are connected with the second stop valve, the high-pressure hydrogen cylinder and the first filter are connected with the first electric control valve, the pure carbon dioxide cylinder and the first filter are connected with the second electric control valve, and the pure carbon dioxide cylinder is connected with the main pipeline through the third electric control valve to serve as a high-pressure gas source for providing stable flow rate gas for the system. The first air storage tank and the second air storage tank are connected with the main pipeline through a fifth electric control valve and a sixth electric control valve respectively and are used for temporarily storing gas to ensure the accuracy of the test. The sample chamber is arranged in a jacketed heat exchanger, the jacketed heat exchanger is connected with a main pipeline through a fourth electric control valve and a third stop valve, the jacketed heat exchanger is simultaneously connected with a second heater and a cooler, the second heater and the cooler respectively provide water vapor and cooling water, and the temperature of the reaction subsystem is controlled to control hydrogen storage/release operation. The exhaust subsystem is connected with the main pipeline through a seventh electric control valve, the evacuation pipeline is connected with the carbon dioxide steel cylinder, the exhaust subsystem is communicated with the outside (is convenient to exhaust to the air) through a first flow limiting valve, and the vacuumizing pipeline is connected with the vacuum pump through an eighth electric control valve and a second flow limiting valve. The computer is connected with the thermal conductivity cell, the cooler, the first heater, the second heater, the first pressure sensor and the second pressure sensor through the connecting hub, and records parameters such as hydrogen purity, system pressure, temperature and the like in the hydrogen storage/release process.
Curve test:
Placing a sample to be tested in a sample chamber, placing the sample into a jacketed heat exchanger, connecting a third filter and a fourth electric control valve, connecting the jacketed heat exchanger with a test system through a third stop valve, connecting the jacketed heat exchanger with a cooler, cooling to 20 ℃, closing all valves, opening a high-pressure hydrogen cylinder, a pure carbon dioxide steel cylinder, first to third electric control valves and a fifth electric control valve, controlling the flow of hydrogen and carbon dioxide to enable the purity of the hydrogen in the hydrocarbon mixed gas to reach 95%, then enabling the hydrocarbon mixed gas to flow to a first gas storage tank, closing the third electric control valve when the set pressure is reached, opening the third stop valve and the fourth electric control valve, enabling the hydrocarbon mixed gas to flow into the sample chamber, monitoring the pressure change of the reaction chamber through a second pressure sensor, making a PCT curve through a computer, recording the pressure of a hydrogen absorption and release platform, closing the cooler after the sample is saturated with hydrogen absorption, setting the heating temperature to 100 ℃, closing the fifth electric control valve, opening the sixth electric control valve, enabling the hydrocarbon mixed gas in the sample chamber to flow to the second gas storage tank, and obtaining a hydrogen volume equation through the second pressure sensor.
Cycle life test:
And 1, placing a sample to be tested in a sample chamber, placing the sample into a jacketed heat exchanger, connecting a third filter and a fourth electric control valve, and connecting a test system through a third stop valve, wherein the temperatures of a cooler and a second heater are respectively 20 ℃ and 100 ℃.
And 2, after the system is vacuumized, closing all valves, opening a high-pressure hydrogen cylinder and first to third electric control valves, controlling the flow of hydrogen and carbon dioxide to enable the purity of the hydrogen in the hydrocarbon mixed gas to reach 95%, enabling the hydrocarbon mixed gas to flow into a first gas storage tank, opening a cooler after the two gases are uniformly mixed and the pressure reading of a first pressure sensor is stable, setting the cooling temperature to be 20 ℃, opening a third stop valve and a fourth electric control valve, enabling the hydrocarbon mixed gas to flow into a sample chamber, enabling a sample to absorb the hydrogen, and monitoring the pressure change in the sample chamber through a second pressure sensor.
And 3, when the pressure in the sample chamber reaches the pressure of the hydrogen absorption and desorption platform, opening a second heater, setting the heating temperature to be 100 ℃, closing a fifth electric control valve, opening a sixth electric control valve, enabling the mixed gas of the carbon and the hydrogen in the sample chamber to flow to a second gas storage tank, after the pressure of the first pressure sensor and the pressure of the second pressure sensor are stable, opening a seventh electric control valve, a fifth stop valve and a first flow limiting valve, combining the mixed gas of the carbon and the carbon dioxide exhausted by a carbon dioxide steel cylinder, reducing the purity of the hydrogen, exhausting the hydrogen into the air, and when the pressure of the system is reduced to about 0.2MPa, closing the fifth stop valve and the first flow limiting valve, opening an eighth electric control valve and the second flow limiting valve, and opening a vacuum pump to vacuumize the system for 20min.
Setting the circulation times through a data acquisition and processing subsystem, and carrying out the steps 2-3 (sequentially circulating for 200, 500 and 1000 times, and monitoring the change of the hydrogen storage capacity in the circulation process).
The data acquisition processing subsystem is used for setting the purity of the hydrogen to be 90%, 75% and 50% respectively, and measuring the change of the hydrogen storage capacity in the circulation process under different initial hydrogen purities so as to explore the influence of different hydrogen purities on the circulation life of the hydrogen storage material.
Hydrogen purity test before and after cycling
Placing a sample to be tested in a sample chamber, placing the sample into a jacketed heat exchanger, connecting a third filter and a fourth electric control valve, connecting a test system through a third stop valve, vacuumizing the system to 20 ℃ and 100 ℃ respectively, closing all valves, opening a high-pressure hydrogen cylinder, a first electric control valve, a third electric control valve, a seventh electric control valve and a fourth stop valve, heating hydrogen to 400 ℃ through a second heater, entering a thermal conductivity pool, and recording the thermal conductivity lambda 1 at the moment. After the sample to be tested is circulated for 200, 500 and 1000 times, the third electric control valve, the fifth electric control valve and the sixth electric control valve are closed, the fourth electric control valve, the seventh electric control valve, the third stop valve and the fourth stop valve are opened, hydrogen flows out of the sample chamber, is heated to 400 ℃ by the first heater and then enters the thermal conductivity cell, and the change of the thermal conductivity lambda 2 and the comparison lambda 1 and lambda 2 at the moment is recorded.
Social and economic benefit analysis
The invention adopts the volumetric method as the basis, can carry out various performance tests on the same sample, and can continuously determine the hydrogen storage/release performance, the cycle life and the hydrogen purity change before and after hydrogen storage of the hydrogen storage material under different initial hydrogen purities. The decomposition pressure of the sample at any temperature can be obtained through a PCT curve, and the PCT curve is an important index of the performance of the hydrogen storage material and is also a theoretical basis for exploring a new hydrogen storage material. The conventional method for obtaining the hydrogen storage/release performance by knowing the surface structure morphology and the surface components before and after the hydrogen storage/release of the sample by using a scanning electron microscope is expensive and cannot obtain a plurality of parameters, while the gravimetric method obtains the hydrogen storage performance by measuring the mass change before and after the hydrogen storage/release or making a weight loss curve, but the sample is easy to be polluted in the transferring process, and the method has limited application in the aspect of alloy hydrogen storage.
The first and second pressure sensors, the first heater, the second heater and the cooler, and the first to eighth electric control valves are connected through a computer, and then parameters are set in a computer program, wherein the set parameters comprise the heating temperature of the reaction chamber, the cooling temperature, the heating temperature of the heat conduction subsystem, the circulation times and the opening and closing of the corresponding valves. The method can automatically detect the cycle life under different hydrogen purities by a computer program, thereby greatly saving the trouble of manual operation.
The above embodiments are preferred examples of the present invention, and the present invention is not limited thereto, and any other modifications or equivalent substitutions made without departing from the technical aspects of the present invention are included in the scope of the present invention.
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| CN113933208B (en) * | 2021-10-13 | 2024-11-08 | 扬州大学 | A hydrogen storage material hydrogen absorption and desorption cycle life test device and test method |
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| CN115032114A (en) * | 2022-05-17 | 2022-09-09 | 江苏氢枫能源装备有限公司 | Hydrogen storage material performance testing device and testing method thereof |
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