Activating and sampling device for solid hydrogen storage alloy material

Abstract

The utility model provides a solid hydrogen storage alloy material activating and sampling device, which belongs to the technical field of solid hydrogen storage and comprises an activating unit and a sampling unit, the activating unit comprises a high and low temperature all-in-one machine, a helium steel cylinder and a hydrogen steel cylinder, the sampling unit comprises a glove box, and the high and low temperature all-in-one machine is communicated with a circulating water tank. The solid hydrogen storage alloy material activating and sampling device solves the problems that an existing solid hydrogen storage alloy material activating and sampling device cannot repeatedly activate a solid hydrogen storage alloy material, the hydrogen absorption and hydrogen desorption capacity of the solid hydrogen storage alloy material is reduced, and the practicability is greatly reduced.

Description

Technical Field

[0001] The utility model belongs to the technical field of solid-state hydrogen storage, and in particular relates to an activation sampling device for a solid-state hydrogen storage alloy material. Background Art

[0002] Hydrogen energy is a secondary energy source with abundant sources, green and low carbon, and wide applications. It is gradually becoming one of the important carriers of global energy transformation and development. The hydrogen energy industry chain is mainly divided into hydrogen production, hydrogen storage, hydrogen transportation and hydrogen use. Among them, hydrogen storage is divided into compressed gaseous hydrogen storage, low-temperature liquid hydrogen storage, liquid hydride hydrogen storage and solid hydrogen storage. The alloy material uses titanium alloy, which can reversibly absorb and release hydrogen under certain temperature and pressure. During the hydrogen absorption process of the hydrogen storage alloy, hydrogen enters the metal lattice gap of the hydrogen storage alloy in the form of hydrogen atoms to form metal hydride. The hydrogen absorption process releases heat and the hydrogen release process absorbs heat. The hydrogen absorption and desorption process of the hydrogen storage alloy is completely reversible. The hydrogen storage alloy cannot absorb hydrogen at the beginning, and of course it will not release hydrogen. Instead, it needs to first come into contact with a hydrogen atmosphere under high temperature and high pressure, and then reduce the pressure and evacuate, and repeat this process many times. The process of activation is necessary before the practical application of hydrogen storage alloys. Multiple hydrogen absorption and desorption reactions are carried out to improve hydrogen storage efficiency and cycle stability. Sufficient hydrogen permeation and discharge are required between each hydrogen absorption and desorption reaction. The technical principle of solid-state hydrogen storage is to utilize the reversible reaction of hydrogen adsorption, storage and release by metal alloys, carbonaceous materials, organic liquid materials, metal frames, etc. Its advantages are high hydrogen storage volume density, low energy consumption and good safety. As a carrier of hydrogen storage alloys, the design of hydrogen storage equipment is closely related to the material properties of hydrogen storage alloys. Therefore, under the condition that the hydrogen storage alloys have mature and reliable hydrogen absorption and desorption performance, it is necessary to propose a solid-state hydrogen storage alloy material activation sampling device.

[0003] The existing solid hydrogen storage alloy material activation sampling device cannot repeatedly activate the solid hydrogen storage alloy material, which reduces the hydrogen absorption and desorption capacity of the solid hydrogen storage alloy material and greatly reduces its practicality. Utility Model Content

[0004] The utility model provides a solid hydrogen storage alloy material activation sampling device, which aims to solve the problem that the existing solid hydrogen storage alloy material activation sampling device cannot repeatedly activate the solid hydrogen storage alloy material, reduces the hydrogen absorption and desorption capacity of the solid hydrogen storage alloy material, and greatly reduces practicality.

[0005] An embodiment of the present utility model provides a solid hydrogen storage alloy material activation sampling device, comprising an activation unit and a sampling unit, wherein the activation unit comprises a high and low temperature integrated machine, a helium cylinder and a hydrogen cylinder, the sampling unit comprises a glove box, and the high and low temperature integrated machine is connected to a circulating water tank.

[0006] Furthermore, the high and low temperature integrated machine is connected to a water inlet pipeline and a water return pipeline.

[0007] By adopting the above technical solution, it is convenient to connect the high and low temperature integrated machine with the circulating water tank, the high and low temperature integrated machine can provide constant temperature conditions for activation, and the helium cylinder and hydrogen cylinder can provide gas source for the activation unit.

[0008] Furthermore, the circulating water tank is connected to the water inlet pipeline, and the circulating water tank is connected to the return water pipeline. An activation bottle is placed in the circulating water tank, and the lower end of the activation bottle is sealed with a wire plug. The activation bottle is filled with alloy material, and the circulating water tank is filled with circulating water. The upper end of the activation bottle is fixedly connected to a filter plate, and the upper end of the activation bottle is connected to a tube body, and the other end of the tube body is provided with a stem, and the other end of the stem is provided with a threaded joint, and the other end of the threaded joint is connected to a three-way valve, and the left end of the three-way valve is connected to a hose, and a one-way valve 2 is provided on the hose, and the other end of the hose is connected to a vacuum pump, and the other end of the vacuum pump is connected to a discharge pipe.

[0009] By adopting the above technical solution, the three-way valve facilitates the distribution and control of the hydrogen, helium pipelines and vacuum pipelines, the vacuum pump facilitates the vacuum treatment of the entire device, the material and volume of the activation bottle can be designed as needed according to the alloy material properties, activation temperature and sampling mass, and through the setting of the circulating water tank and circulating water, a water bath is used to facilitate providing the temperature conditions for hydrogen absorption and desorption.

[0010] Furthermore, the helium cylinder is connected to a helium pressure reducer, the other end of the helium pressure reducer is connected to a metal pipeline, a one-way valve three is provided on the metal pipeline, the other end of the metal pipeline is connected to a three-way joint, and the three-way joint is connected to the three-way valve.

[0011] By adopting the above technical solution, the setting of the helium cylinder makes it easy to fill the activation unit with helium for pressure testing, which is beneficial to ensure that the strength of each part in the device is qualified and there is no leakage at the joints. After passing the pressure test, the alloy material is loaded to facilitate subsequent activation treatment.

[0012] Furthermore, the hydrogen cylinder is connected to a hydrogen pressure reducer, the other end of the hydrogen pressure reducer is connected to a trachea, a one-way valve is provided on the trachea, and the other end of the trachea is connected to the three-way joint.

[0013] By adopting the above technical solution, the main steps of activation are heating, vacuuming, helium filling, vacuuming, hydrogen filling, and vacuuming, among which heating and vacuuming are beneficial to increasing the activity of the alloy material and removing moisture from the device and the alloy material. Vacuuming after helium filling is convenient for completely removing the air in the device, and vacuuming after hydrogen filling is convenient for activating the alloy material. The number of hydrogen filling and vacuuming will vary depending on the alloy material, and the interval time between hydrogen filling and vacuuming will also vary depending on the alloy material. After the activation of the alloy material is completed, the activation result is tested. The activation bottle is first vacuumed, and then the water temperature is lowered and a stable cycle is maintained through the high and low temperature integrated machine to meet the hydrogen absorption temperature requirements of the alloy material. Turn on the hydrogen source, record the pressure value, adjust the high-pressure hydrogen to the hydrogen absorption pressure range of the alloy material through the hydrogen pressure reducer, provide hydrogen, and the alloy material will start the hydrogen absorption reaction. After the pressure stabilizes, record the pressure value again. Calculate the theoretical hydrogen absorption amount based on the filling quality of the alloy material and the hydrogen absorption capacity after complete activation. Then calculate the theoretical hydrogen release amount based on the recorded pressure value and the volume parameter of the hydrogen cylinder. Compare the hydrogen absorption amount of the alloy material with the hydrogen release amount of the hydrogen cylinder. When the two are equivalent, the alloy material is successfully activated. At this time, stop providing the gas source, turn off the high and low temperature integrated machine, adjust the three-way valve to the closed position, and separate the tube body and the stem to facilitate the removal of the activated bottle containing the alloy material from the circulating water tank for the next sampling operation.

[0014] Furthermore, a filling tube is placed in the glove box.

[0015] By adopting the above technical solution, the metal properties of the activated alloy material are relatively active, and it is easy to spontaneously combust when exposed to air. It cannot be directly exposed to the air for sampling. The configuration of the glove box is conducive to ensuring the quality of the sample. The activated bottle is placed in the glove box, and the glove box is first vacuumed and then filled with inert gas for protection. Then, the screw plug is unscrewed, and the activated alloy material is taken out with the help of a sampling spoon and filled into the filling tube, which facilitates the smooth progress of sampling.

[0016] The beneficial effects of the utility model are:

[0017] 1. The utility model is convenient for providing constant temperature conditions for activation through the setting of high and low temperature integrated machine, and the helium cylinder and hydrogen cylinder are convenient for providing gas source for the activation unit.

[0018] 2. The utility model is provided with a circulating water tank and an activation bottle body. The three-way valve facilitates the distribution control of the hydrogen, helium pipelines and the vacuum pipeline. The vacuum pump facilitates the vacuum treatment of the entire device. The material and volume of the activation bottle body can be designed as needed according to the properties of the alloy material, the activation temperature and the amount of sampling quality. Through the provision of a circulating water tank and circulating water, a water bath is used to provide the temperature conditions for hydrogen absorption and desorption.

[0019] 3. The utility model is provided with a helium cylinder and a hydrogen cylinder. The provision of the helium cylinder facilitates filling helium into the activation unit for a pressure test, which is beneficial to ensuring that the strength of each part of the device is qualified and there is no leakage at the joints. After the pressure test is qualified, the alloy material is loaded, which is convenient for subsequent activation treatment. The main steps of activation are heating, vacuuming, helium filling, vacuuming, hydrogen filling, and vacuuming. Among them, heating and vacuuming are beneficial to increasing the activity of the alloy material and removing moisture from the device and the alloy material. Vacuuming after helium filling is convenient for completely removing the air in the device. Vacuuming after hydrogen filling is convenient for activating the alloy material. The number of hydrogen filling and vacuuming will vary according to the different alloy materials, and the interval time between hydrogen filling and vacuuming will also vary according to the different alloy materials. After the activation of the alloy material is completed, the activation result is tested. First, the activation bottle body is Perform vacuum treatment, then use the high and low temperature integrated machine to lower the water temperature and maintain stable circulation to meet the hydrogen absorption temperature requirements of the alloy material. At this time, turn on the hydrogen source, record the pressure value, and adjust the high-pressure hydrogen to the hydrogen absorption pressure range of the alloy material through the hydrogen pressure reducer. Provide hydrogen, and the alloy material will start to absorb hydrogen. After the pressure stabilizes, record the pressure value again. Calculate the theoretical hydrogen absorption amount based on the filling quality of the alloy material and the hydrogen absorption capacity after complete activation. Calculate the theoretical hydrogen release amount based on the recorded pressure value and the volume parameter of the hydrogen cylinder. Compare the hydrogen absorption amount of the alloy material with the hydrogen release amount of the hydrogen cylinder. When the two are equivalent, the alloy material is successfully activated. Stop providing the gas source, turn off the high and low temperature integrated machine, and adjust the three-way valve to the closed position. At this time, separate the tube body and the stem to facilitate the removal of the activated bottle containing the alloy material from the circulating water tank for the next sampling operation.

[0020] 4. The utility model is equipped with a glove box. The metal properties of the activated alloy material are relatively active and it is easy to spontaneously combust when it comes into contact with air. It cannot be directly exposed to the air for sampling. The configuration of the glove box is conducive to ensuring the quality of the sample. The activated bottle is placed in the glove box. The glove box is first vacuumed and then filled with inert gas for protection. Then, the screw plug is unscrewed, and the activated alloy material is taken out with the help of a sampling spoon and filled into the filling tube, which facilitates the smooth progress of sampling.

[0021] Other features and advantages of the present invention will be described in the following description, and in part will become apparent from the description, or understood by practicing the present invention. The purpose and other advantages of the present invention can be achieved and obtained through the structures particularly pointed out in the description and the drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation of the present invention. In the accompanying drawings:

[0023] Figure 1 This is a schematic structural diagram of the activation unit in an embodiment of the present utility model;

[0024] Figure 2 Schematic diagram of the structure of the sampling unit in the embodiment of the present utility model.

[0025] Figure numerals: 101, activation unit; 102, sampling unit; 1, high and low temperature integrated machine; 2, water inlet pipeline; 3, return pipeline; 4, circulating water tank; 5, helium cylinder; 6, helium pressure reducer; 7, one-way valve three; 8, metal pipeline; 9, hydrogen cylinder; 10, hydrogen pressure reducer; 11, one-way valve one; 12, three-way connector; 13, screw plug; 14, activation bottle body; 15, alloy material; 16, circulating water; 17, filter; 18, tube body; 19, tube stem; 20, threaded joint; 21, three-way valve; 22, hose; 23, one-way valve two; 24, vacuum pump; 25, discharge pipe; 26, filling pipe; 27, glove box. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical solution and advantages of the technical solution of the present invention clearer, the technical solution of the embodiment of the present invention will be clearly and completely described below in conjunction with the drawings of the specific embodiments of the present invention. The same figure marks in the drawings represent the same parts. It should be noted that the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the described embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] Reference Figure 1-2 The embodiment of the present invention proposes a solid-state hydrogen storage alloy material activation sampling device, including an activation unit 101 and a sampling unit 102. The activation unit 101 includes a high and low temperature integrated machine 1, a helium cylinder 5 and a hydrogen cylinder 9. The high and low temperature integrated machine 1 is connected to a water inlet pipeline 2 and a water return pipeline 3, which is convenient for connecting the high and low temperature integrated machine 1 with a circulating water tank 4. The high and low temperature integrated machine 1 is convenient for providing constant temperature conditions for activation, and the helium cylinder 5 and the hydrogen cylinder 9 are convenient for providing a gas source for the activation unit 101.

[0028] The high and low temperature integrated machine 1 is connected to a circulating water tank 4, which is connected to the water inlet pipeline 2, and the circulating water tank 4 is connected to the return water pipeline 3. An activation bottle 14 is placed in the circulating water tank 4, and the lower end of the activation bottle 14 is blocked with a wire plug 13. The activation bottle 14 is filled with an alloy material 15, and the circulating water tank 4 is filled with circulating water 16. The upper end of the activation bottle 14 is fixedly connected to a filter 17, and the upper end of the activation bottle 14 is connected to a tube 18. The other end of the tube 18 is provided with a stem 19, and the other end of the stem 19 is provided with a threaded joint 20. The other end of the threaded joint 20 is connected to The three-way valve 21 is connected to the left end of the three-way valve 21. The hose 22 is provided with a one-way valve 23. The other end of the hose 22 is connected to the vacuum pump 24. The other end of the vacuum pump 24 is connected to the discharge pipe 25. The three-way valve 21 facilitates the distribution control of the hydrogen, helium pipelines and the vacuum pipeline. The vacuum pump 24 facilitates the vacuum treatment of the entire device. The material and volume of the activation bottle 14 can be designed as needed according to the properties of the alloy material, the activation temperature and the quality of the sample. Through the setting of the circulating water tank 4 and the circulating water 16, a water bath is used to provide the temperature conditions for hydrogen absorption and desorption.

[0029] The helium cylinder 5 is connected to a helium pressure reducer 6, the other end of which is connected to a metal pipeline 8, a one-way valve 7 is provided on the metal pipeline 8, the other end of the metal pipeline 8 is connected to a three-way joint 12, and the three-way joint 12 is connected to a three-way valve 21. The provision of the helium cylinder 5 facilitates the filling of helium into the activation unit 101 for a pressure test, which is beneficial to ensuring that the strength of each part of the device is qualified and there is no leakage at the joints. After the pressure test is passed, the alloy material is loaded to facilitate subsequent activation treatment.

[0030] The hydrogen cylinder 9 is connected to a hydrogen pressure reducer 10, and the other end of the hydrogen pressure reducer 10 is connected to the trachea, and a one-way valve 11 is provided on the trachea. The other end of the trachea is connected to a three-way joint 12. The main steps of activation are heating, vacuuming, helium filling, vacuuming, hydrogen filling, and vacuuming. Heating and vacuuming are beneficial to increasing the activity of the alloy material and removing moisture from the device and the alloy material. Vacuuming after helium filling is convenient for completely removing the air in the device. Vacuuming after hydrogen filling is convenient for activating the alloy material. The number of hydrogen filling and vacuuming will vary depending on the alloy material, and the interval time between hydrogen filling and vacuuming will also vary depending on the alloy material. After the activation of the alloy material is completed, the activation result is tested. The activation bottle body 14 is vacuumed first, and then the water temperature is lowered and maintained through the high and low temperature all-in-one machine 1. Stabilize the circulation and meet the hydrogen absorption temperature requirement of the alloy material. At this time, turn on the hydrogen source and record the pressure value. Adjust the high-pressure hydrogen to the hydrogen absorption pressure range of the alloy material through the hydrogen pressure reducer 10, provide hydrogen, and the alloy material starts to absorb hydrogen. After the pressure stabilizes, record the pressure value again. Calculate the theoretical hydrogen absorption amount based on the filling quality of the alloy material and the hydrogen absorption capacity after complete activation. Then calculate the theoretical hydrogen release amount based on the recorded pressure value and the volume parameter of the hydrogen cylinder. Compare the hydrogen absorption amount of the alloy material with the hydrogen release amount of the hydrogen cylinder 9. When the two are equivalent, the alloy material is successfully activated. Stop providing the gas source at this time, turn off the high and low temperature integrated machine 1, and adjust the three-way valve 21 to the closed position. At this time, separate the tube body 18 and the tube stem 19 to facilitate the removal of the activated bottle body 14 containing the alloy material from the circulating water tank 4 for the next sampling operation.

[0031] The sampling unit 102 includes a glove box 27, in which a filling tube 26 is placed. The metal properties of the activated alloy material are relatively active and it is easy to spontaneously combust when exposed to air. It cannot be directly exposed to the air for sampling. The configuration of the glove box 27 is conducive to ensuring the quality of the sample. The activated bottle body 14 is placed in the glove box 27. The glove box 27 is first vacuumed and then filled with inert gas for protection. Then, the screw plug 13 is unscrewed, and the activated alloy material is taken out with the help of a sampling spoon and filled into the filling tube 26 to facilitate the smooth progress of the sampling work.

[0032] The specific implementation method is as follows: when in use, the high and low temperature integrated machine 1 is connected to the circulating water tank 4 by using the water inlet pipeline 2 and the return water pipeline 3. The high and low temperature integrated machine 1 provides constant temperature conditions for activation. The helium cylinder 5 and the hydrogen cylinder 9 are convenient for providing gas source for the activation unit 101. The three-way valve 21 distributes and controls the hydrogen, helium pipelines and vacuum pipelines. The vacuum pump 24 facilitates the vacuum treatment of the entire device. The material and volume of the activation bottle body 14 can be designed as needed according to the properties of the alloy material, the activation temperature and the quality of the sample. Through the setting of the circulating water tank 4 and the circulating water 16, a water bath is used to facilitate the provision of temperature conditions for hydrogen absorption and desorption. The setting of the helium cylinder 5 facilitates the flow of hydrogen toward the activation unit 101. Fill with helium to conduct a pressure test to ensure that the strength of each part of the device is qualified and there is no leakage at the joints. After the pressure test is qualified, the alloy material is loaded for subsequent activation treatment. The main steps of activation are heating, vacuuming, helium filling, vacuuming, hydrogen filling, and vacuuming. Heating and vacuuming are beneficial to increasing the activity of the alloy material and removing moisture from the device and the alloy material. Vacuuming after helium filling is convenient for completely removing the air in the device. Vacuuming after hydrogen filling is convenient for activating the alloy material. The number of hydrogen filling and vacuuming will vary according to the different alloy materials, and the interval time between hydrogen filling and vacuuming will also vary according to the different alloy materials. After the activation of the alloy material is completed, the activated structure is The results are inspected. First, the activation bottle body 14 is vacuumed, and then the water temperature is lowered and a stable cycle is maintained through the high and low temperature integrated machine 1 to meet the hydrogen absorption temperature requirements of the alloy material. At this time, the hydrogen source is turned on, and the pressure value is recorded. The high-pressure hydrogen is adjusted to the hydrogen absorption pressure range of the alloy material through the hydrogen pressure reducer 10. Hydrogen is provided, and the alloy material begins to absorb hydrogen. After the pressure stabilizes, the pressure value is recorded again. The theoretical hydrogen absorption amount is calculated based on the filling quality of the alloy material and the hydrogen absorption capacity after complete activation. The theoretical hydrogen release amount is then calculated based on the recorded pressure value and the volume parameter of the hydrogen bottle. The hydrogen absorption amount of the alloy material is compared with the hydrogen release amount of the hydrogen cylinder 9. When the two are equivalent, the alloy material is activated successfully. Stop providing gas source, turn off high and low temperature all-in-one machine 1, adjust three-way valve 21 to closed position, separate tube body 18 and tube stem 19 at this time, and take out activation bottle body 14 containing alloy material from circulating water tank 4 conveniently, so as to carry out next sampling operation. The metal property of activated alloy material is relatively active, and it is easy to spontaneously combust when it encounters air, so it cannot be directly exposed to air for sampling. The configuration of glove box 27 is conducive to ensuring sample quality. Put the activated bottle body 14 into glove box 27, vacuum the glove box 27 first, and then fill it with inert gas for protection, then unscrew the screw plug 13, use sampling spoon to take out the activated alloy material and fill it into filling tube 26, and the sampling work is completed.

[0033] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions are merely illustrative of the principles of the present invention. Various changes and improvements may be made to the present invention without departing from the spirit and scope of the present invention. Such changes and improvements are intended to fall within the scope of the present invention. The scope of protection claimed in this invention is defined by the appended claims and their equivalents.

Claims

1. A solid hydrogen storage alloy material activation sampling device, comprising an activation unit (101) and a sampling unit (102), characterized in that: The activation unit (101) includes a high-low temperature integrated machine (1), a helium cylinder (5) and a hydrogen cylinder (9); the sampling unit (102) includes a glove box (27); and the high-low temperature integrated machine (1) is connected to a circulating water tank (4).

2. The solid hydrogen storage alloy material activation sampling device according to claim 1, characterized in that: The high and low temperature integrated machine (1) is connected to a water inlet pipeline (2) and a water return pipeline (3).

3. The solid hydrogen storage alloy material activation sampling device according to claim 2, characterized in that: The circulating water tank (4) is connected to the water inlet pipeline (2), and the circulating water tank (4) is connected to the water return pipeline (3). An activation bottle (14) is placed in the circulating water tank (4), the lower end of the activation bottle (14) is blocked with a wire plug (13), the activation bottle (14) is filled with alloy material (15), the circulating water tank (4) is filled with circulating water (16), the upper end of the activation bottle (14) is fixedly connected with a filter plate (17), and the activation bottle (14) is The upper end is connected to a tube body (18), the other end of the tube body (18) is provided with a tube stem (19), the other end of the tube stem (19) is provided with a threaded joint (20), the other end of the threaded joint (20) is connected to a three-way valve (21), the left end of the three-way valve (21) is connected to a hose (22), a one-way valve (23) is provided on the hose (22), the other end of the hose (22) is connected to a vacuum pump (24), and the other end of the vacuum pump (24) is connected to a discharge pipe (25).

4. The solid hydrogen storage alloy material activation sampling device according to claim 3, characterized in that: The helium cylinder (5) is connected to a helium pressure reducer (6), the other end of which is connected to a metal pipeline (8), a one-way valve (7) is provided on the metal pipeline (8), the other end of which is connected to a three-way joint (12), and the three-way joint (12) is connected to the three-way valve (21).

5. The solid hydrogen storage alloy material activation sampling device according to claim 4, characterized in that: The hydrogen cylinder (9) is connected to a hydrogen pressure reducer (10), the other end of which is connected to a gas pipe, a one-way valve (11) is provided on the gas pipe, and the other end of the gas pipe is connected to the three-way joint (12).

6. The solid hydrogen storage alloy material activation sampling device according to claim 1, characterized in that: A filling tube (26) is placed in the glove box (27).

Images