CN115050250B - Experimental device and method for accurately and quantitatively adding hydrogen - Google Patents
Experimental device and method for accurately and quantitatively adding hydrogen Download PDFInfo
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- CN115050250B CN115050250B CN202110249817.2A CN202110249817A CN115050250B CN 115050250 B CN115050250 B CN 115050250B CN 202110249817 A CN202110249817 A CN 202110249817A CN 115050250 B CN115050250 B CN 115050250B
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000001257 hydrogen Substances 0.000 title claims abstract description 65
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000007789 gas Substances 0.000 claims abstract description 70
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000010931 gold Substances 0.000 claims abstract description 62
- 229910052737 gold Inorganic materials 0.000 claims abstract description 62
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 10
- 238000007789 sealing Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 13
- 239000010959 steel Substances 0.000 claims description 13
- 238000002347 injection Methods 0.000 claims description 9
- 239000007924 injection Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000010985 leather Substances 0.000 claims description 7
- 230000002093 peripheral effect Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000002474 experimental method Methods 0.000 claims description 5
- 210000001503 joint Anatomy 0.000 claims description 5
- 238000003466 welding Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000005984 hydrogenation reaction Methods 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 13
- 229930195733 hydrocarbon Natural products 0.000 description 13
- 150000002430 hydrocarbons Chemical class 0.000 description 11
- 239000007788 liquid Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- 238000004088 simulation Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005273 aeration Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09B—EDUCATIONAL OR DEMONSTRATION APPLIANCES; APPLIANCES FOR TEACHING, OR COMMUNICATING WITH, THE BLIND, DEAF OR MUTE; MODELS; PLANETARIA; GLOBES; MAPS; DIAGRAMS
- G09B23/00—Models for scientific, medical, or mathematical purposes, e.g. full-sized devices for demonstration purposes
- G09B23/24—Models for scientific, medical, or mathematical purposes, e.g. full-sized devices for demonstration purposes for chemistry
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Mathematical Physics (AREA)
- Business, Economics & Management (AREA)
- Algebra (AREA)
- Computational Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Mathematical Analysis (AREA)
- Mathematical Optimization (AREA)
- Health & Medical Sciences (AREA)
- Pure & Applied Mathematics (AREA)
- Medicinal Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Educational Administration (AREA)
- Educational Technology (AREA)
- Theoretical Computer Science (AREA)
- Accessories For Mixers (AREA)
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention provides an experimental device and a method for accurately and quantitatively adding hydrogen, wherein the device comprises a gas supply device, and the gas supply device is configured to be capable of supplying hydrogen; and a reaction device connected to the gas supply device; wherein the gas supply means delivers hydrogen to the reaction means at a controlled rate and flow rate. The method includes injecting hydrogen: opening a pressurized air source to inject hydrogen into the gold tube at a certain pressure and keeping the pressure for a certain time; replacement air: closing the first stop valve and simultaneously opening the second stop valve to slowly release the exhaust gas; repeating the steps of injecting hydrogen and replacing air until the air composition in the gold tube reaches the experimental requirement; sealing the gold tube: the golden tube is tightly pressed by a pressure clamp, the air in the golden tube is sealed, and whether the tightness is good is checked.
Description
Technical Field
The invention relates to an experimental device and method for accurately and quantitatively adding hydrogen, and belongs to the field of oil gas geochemistry.
Background
In the global scope, hydrogen-rich fluid is found in a plurality of hydrocarbon-bearing gas basins, and hydrogen-rich substances such as hydrogen are input into the hydrocarbon-bearing gas basins by the hydrogen-rich fluid, so that the hydrogen-rich fluid becomes exogenous hydrogen outside hydrocarbon source rocks, and the exogenous hydrogen has important promotion effect on hydrocarbon production of organic matters. In order to clarify the influence of hydrogen-rich fluid on hydrocarbon production of hydrocarbon source rock and other organic matters, exogenous hydrogen, kerogen and other organic matters are placed in a closed hydrocarbon production reaction system, such as a gold pipe, the reaction process of hydrocarbon production of hydrocarbon source rock is influenced by simulating temperature and pressure conditions in geological environment, external assistance hydrogen is supplied by hydrogen or hydrogen-rich compound pyrolysis, and the potential and evolution process of hydrocarbon production of oil gas in geological exploration are evaluated through the component content, elements and isotope composition characteristics of experimental products. At present, the hydrogen is difficult to accurately and quantitatively add in the experimental modes at home and abroad, mainly because hydrogen molecules have strong dissipation property and are easy to mix with other reaction substances, so that the hydrogen quantitative process is easy to be interfered and difficult to accurately quantify.
At present, in the research of geochemistry experiments, the hydrocarbon generation simulation experiment technical method of the gold pipe and hydrogen is widely applied, is mainly used for the researches of hydrocarbon generation dynamics, hydrocarbon generation thermal evolution and the like, not only provides support for the research of petroleum geology theory, but also provides specific parameters for oil and gas exploration and development practice. However, in the experimental process of a closed reaction system, such as a gold tube, when the solid or liquid state mixture is closed and the reactants are added, the method can quantitatively inject the hydrogen, effectively eliminate the interference of air components, avoid the loss of the solid or liquid state reactants in the reaction kettle, and is always a technical problem of accurately and quantitatively adding the hydrogen in the closed experimental system.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides an experimental device and a method for accurately and quantitatively adding hydrogen, which are suitable for a gold tube closed solid-liquid mixed reaction system. The purpose is to realize accurate quantitative hydrogen addition and Jin Guanna air replacement in the sample loading process of the simulation experiment, ensure that other solid or liquid reactants in the gold tube cannot be subjected to quality loss, and ensure the authenticity and repeatability of the experimental result.
In one aspect of the present invention, an experimental apparatus for accurately and quantitatively adding hydrogen is provided, comprising:
a gas supply device configured to be able to supply hydrogen gas; and
a reaction device connected to the gas supply device;
wherein the gas supply means delivers hydrogen to the reaction means at a controlled rate and flow rate.
The invention is further improved in that the pressurized gas source comprises a pressurized gas source for storing hydrogen, the pressurized gas source is connected with the four-way valve through a first gas pipe,
the first interface of the four-way valve is connected with the first air pipe, the second interface is connected with the reaction device through the second air pipe, and the third interface is connected with the exhaust pipe.
A further improvement of the invention is that a first stop valve is arranged on the first air pipe, and a flowmeter is arranged at the downstream of the stop valve.
The invention further improves that the fourth interface of the four-way valve is connected with a pressure gauge.
The invention further improves that the reaction device comprises a gold pipe, and the inlet end of the gold pipe is connected with the second air pipe through an elastic rubber leather pipe.
The invention is further improved in that the inner side of the butt joint part of the gold pipe and the elastic rubber pipe is provided with a pressure-bearing steel pipe, and the outer side of the butt joint part is provided with a peripheral rigid hoop.
The invention further improves that the exhaust pipe is provided with a second stop valve, and the outlet of the exhaust pipe is provided with a gas collecting tank.
According to another aspect of the invention, an experimental method of the hydrogenation gas is also provided, which is realized by using an experimental device for accurately and quantitatively adding hydrogen; it comprises the following steps:
hydrogen injection: opening a pressurized air source to inject hydrogen into the gold tube at a certain pressure and keeping the pressure for a certain time;
replacement air: closing the first stop valve and simultaneously opening the second stop valve to slowly release the exhaust gas;
repeating the steps of injecting hydrogen and replacing air until the air composition in the gold tube reaches the experimental requirement;
sealing the gold tube: the golden tube is tightly pressed by a pressure clamp, the air in the golden tube is sealed, and whether the tightness is good is checked.
The invention further improves that when the air in the gold tube is sealed, the gold tube wall is clamped by the pressing clamp and then welded by argon arc welding.
The invention further improves that the gold pipe after being welded and sealed is put into hot water with the temperature of more than 60 ℃ to check whether beaded water bubbles are generated or not so as to determine whether the gas tightness in the gold pipe is good or not.
Compared with the prior art, the invention has the advantages that:
the invention provides an experimental device and a method for accurately and quantitatively adding hydrogen, which are suitable for a gold tube closed solid-liquid mixed reaction system and aim at solving the technical problem that the accurate and quantitative hydrogen addition to a closed reaction system is difficult to realize. The purpose is to realize accurate quantitative hydrogen addition and Jin Guanna air replacement in the sample loading process of the simulation experiment, ensure that other solid or liquid reactants in the gold tube cannot be subjected to quality loss, and ensure the authenticity and repeatability of the experimental result.
Drawings
Preferred embodiments of the present invention will be described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic diagram showing the structure of an experimental apparatus for precisely quantitatively adding hydrogen according to an embodiment of the present invention;
FIG. 2 is a schematic view showing the cross section of the joint of a gold tube and an elastic rubber tube according to an embodiment of the present invention;
figure 3 shows a schematic view of a gold tube seal in accordance with one embodiment of the invention.
In the drawings, like parts are designated with like reference numerals. The figures are not drawn to scale.
The meaning of the reference numerals in the drawings is as follows: 10. the device comprises a pressurized air source, 11, a first stop valve, 12, a flowmeter, 13, a pressure gauge, 20, a four-way valve, 21, a first air pipe, 22, a second air pipe, 23, an exhaust pipe, 24, a gas collecting tank, 25, a second stop valve, 30, a gold pipe, 31, a peripheral steel hoop, 32, a pressure clamp, 33, a pressure-bearing steel ring, 34 and an elastic rubber leather pipe.
Detailed Description
In order to make the technical solution and advantages of the present invention more apparent, exemplary embodiments of the present invention will be described in further detail below with reference to the accompanying drawings. It will be apparent that the described embodiments are only some of the embodiments of the present invention and are not exhaustive of all embodiments. And embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Fig. 1 schematically shows an experimental set-up for accurate dosing of hydrogen according to an embodiment of the invention, comprising a gas supply. The gas supply device is configured to be capable of supplying hydrogen gas. The gas supply device is connected with the reaction device and is used for conveying hydrogen to the reaction device. The gas supply means delivers hydrogen gas to the reaction means at a controlled rate and flow rate.
In this embodiment, the gas supply means stores hydrogen gas and has a certain pressure to supply hydrogen gas to the reaction means. The air supply device supplies hydrogen to the reaction device and replaces air in the reaction device. The experimental device described in this example also includes a reaction device. The gas supply means delivers hydrogen gas to the reaction means at a controlled rate and flow rate.
In one embodiment, the pressurized gas source 10 includes a pressurized gas source 10 and a four-way valve 20. The pressurized gas source 10 is used to store hydrogen gas, either as a compressed gas within the pressurized gas source 10 or in a liquid form, which enables the pressurized gas source 10 to have a certain pressure output outwards. The pressurized air source 10 is connected to a four-way valve 20 via a first air line 21. The four interfaces of the four-way valve 20 are a first interface, a second interface, a third interface and a fourth interface respectively, wherein the first interface of the four-way valve 20 is connected with the first air pipe 21, the second interface is connected with the reaction device through the second air pipe 22, and the third interface is connected with the exhaust pipe 23.
In the experimental device for accurately and quantitatively adding hydrogen according to the embodiment, a plurality of groups of channels are formed between the pressurized air source 10 and the reaction device by the four-way valve 20, and the reaction device and the exhaust pipe 23 are respectively connected. The exhaust pipe 23 can discharge the replaced air during the injection of the hydrogen gas to replace the air in the reaction device.
In one embodiment, a first stop valve 11 is provided on the first air pipe 21, and a flow meter 12 is provided downstream of the stop valve. Preferably, the first air pipe 21 is connected with the first stop valve 11 and the pressurized air source 10 to form a flow limiting capillary, and the flow rate of the output air of the pressurized air source 10 can be regulated by opening or closing the first stop valve 11.
In one embodiment, the fourth port of the four-way valve 20 is connected to a pressure gauge 13. The pressure gauge 13 is capable of measuring the pressure output by the pressurized gas source 10, which in combination with the flow meter 12 is capable of measuring the pressure and flow rate, thereby providing a reference for the hydrogen gas output by the control of the first shut-off valve 11.
In one embodiment, the reaction device comprises a gold tube 30, wherein the gold tube 30 has a tubular structure with one end closed and one end open. An elastic rubber leather hose 34 is arranged at the inlet end of the gold hose 30, one end of the elastic rubber leather hose 34 is connected with the gold hose 30, and the other end of the elastic rubber leather hose is connected with the second air pipe 22.
In one embodiment, the gold pipe 30 is provided with a pressure-bearing steel pipe on the inner side and a peripheral steel hoop 3131 on the outer side at the butt joint of the elastic rubber pipe 34.
The elastic rubber hose 34 of the reaction device has the same size as the outer metal Guan Waijing, so that the reaction device is convenient to seal and prevent air leakage. The gold tube 30 is internally provided with the pressure-bearing steel ring 33, the size design of the pressure-bearing steel ring 33 is slightly smaller than that of the gold tube, and the gold tube is convenient to put in and plays a role in pressure-bearing protection of the gold tube and deformation prevention. After the reaction device finishes injecting hydrogen and replacing air, a pressure clamp 32 is needed to press the lower part of the overlapping part of the gold pipe, the peripheral steel hoop 31 and the elastic rubber leather pipe 34 are loosened, the built-in pressure-bearing steel ring 33 is taken out, the gold pipe wall is clamped by the pressure clamp, and then the gold pipe wall is welded and sealed by argon arc welding.
In one embodiment, a second stop valve 25 is arranged on the exhaust pipe 23, and a gas collecting tank 24 is arranged at the outlet of the exhaust pipe 23. The gas collection tank 24 contains a certain amount of water, the gas in the exhaust pipe 23 generates bubbles in the water, so that the displacement of the gas can be conveniently observed, the gas can be collected, and the hydrogen concentration in the gas can be measured.
According to another aspect of the present invention, there is also provided an experimental method of hydrogenation gas, comprising:
hydrogen injection: opening the pressurized gas source 10 to inject hydrogen into the gold tube 30 at a certain pressure and for a certain time;
replacement air: closing the first shut-off valve 11 and simultaneously opening the second shut-off valve 25, slowly releasing the exhaust gas;
repeating the steps of injecting hydrogen and replacing air until the air composition in the gold tube 30 meets the experimental requirements;
sealing the gold tube 30: the gold tube 30 is pressed by the pressure tongs 32 and the air inside the gold tube 30 is sealed, and whether the sealing property is good or not is checked.
In a specific embodiment, the experimental method comprises the steps of:
hydrogen injection: opening the pressurized air source 10 and the first stop valve 11 to enable the first channel and the second channel to be in a conducting state; at the same time, the second shut-off valve 25 and the exhaust pipe 23 connected to the four-way valve 20 are closed. During the hydrogen gas introduction process, the flow rate of the introduced hydrogen gas is judged by the flow meter 12, so that the flow rate is prevented from being too fast; the pressure gauge 13 adjusts the section to be stable at a specific pressure to control the total gas injection volume to be constant and to maintain constant time.
The pressure and constant time of the injected gas are determined according to the capacity of the gold tube 30, and the main purpose thereof is to allow the hydrogen gas to enter the gold tube to be thoroughly mixed with the air in the reaction system.
Replacement air: at the end of the constant time, the second stop valve 25 connected to the four-way valve 20 is opened, the first stop valve 11 connected to the pressurized gas source 10 is closed, and the exhaust gas is slowly released by observing the change of the indication of the flow meter 12.
The above steps of injecting hydrogen and replacing air are repeated in sequence: the repeated air concentration is 1/N (N is the ratio of the pressure of the reaction system to the standard atmospheric pressure in the process of gas injection, and the temperature and pressure conditions are kept constant in the process of gas injection) of the previous air concentration each time, and the experimental requirements are met after repeated times until the air components in the gold tube 30 are removed.
Sealing the gold tube 30: the pressure clamp 32 is used for pressing the lower part of the overlapped part of the gold pipe 30, the gas inside the gold pipe 30 is sealed, the peripheral steel hoop 31 and the elastic rubber pipe 34 are loosened, the built-in pressure-bearing steel ring 33 (shown in figure 2) is taken out, the wall of the gold pipe 30 is clamped by the pressure clamp, then the wall is welded and sealed by argon arc welding, and after the welding is finished, the gold pipe is put into hot water (more than 60 ℃) to check whether beaded bubbles are generated or not, so as to determine whether the gas tightness inside the gold pipe is good.
In the method according to this embodiment, the principle is as follows: the reason for the replacement of air is that after the injection of hydrogen, the hydrogen is fully mixed with air to dilute the air concentration, and the concentration is determined by the multiple n of the atmospheric pressure of the hydrogenated gas and the number m of times of aeration, in theory V air /V in ＝1/n m . For precisely quantifying hydrogen, under the condition of constant temperature, the amount of the substance of the hydrogen to be added is calculated according to the hydrogen charging pressure and the effective volume of the gold tube during loading. From the ideal gas state equation: pv=nrt, the volume V of the gold Guan Lai in The temperature is constant and the P in the system is kept unchanged in In proportion to the number n of moles of air (i.e. the total volume of air injected at p=101.3 kPa). Simulation experiment data (table 1) show that the device and the method can well replace scavenging air and accurately quantify hydrogen under the condition that other solid or liquid reactants in a reaction system are not affected.
Table 1 table for data of air displacement of hydrogenation gas in simulation experiment
Note that: the sample filling and detection temperature is 25 ℃ constant at room temperature, and the inner diameter of the gold tube is 10mm.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiment and all alterations and/or modifications that fall within the scope of the invention, and that are intended to be included within the scope of the invention.
Claims (6)
1. An experimental device for accurate quantitative hydrogen addition, which is characterized by comprising:
a gas supply device configured to be able to supply hydrogen gas; and
a reaction device connected to the gas supply device;
wherein the gas supply means delivers hydrogen gas to the reaction means at a controlled rate and flow rate;
the gas supply device comprises a pressurized gas source (10) for storing hydrogen, the pressurized gas source (10) is connected with a four-way valve (20) through a first gas pipe (21), a first interface of the four-way valve (20) is connected with the first gas pipe (21), a second interface is connected with the reaction device through a second gas pipe (22), and a third interface is connected with a gas exhaust pipe (23);
the reaction device comprises a gold pipe (30), and the inlet end of the gold pipe (30) is connected with the second air pipe (22) through an elastic rubber leather pipe (34);
the inner side of the butt joint part of the gold pipe (30) and the elastic rubber pipe (34) is provided with a pressure-bearing steel pipe, and the outer side of the butt joint part is provided with a peripheral steel hoop (31);
the exhaust pipe (23) is provided with a second stop valve (25), and the outlet of the exhaust pipe (23) is provided with a gas collecting tank (24).
2. The experimental device for accurately and quantitatively adding hydrogen according to claim 1, wherein a first stop valve (11) is arranged on the first air pipe (21), and a flowmeter (12) is arranged downstream of the stop valve.
3. The experimental device for accurately and quantitatively adding hydrogen according to claim 2, wherein a fourth interface of the four-way valve (20) is connected with a pressure gauge (13).
4. An experimental method of a hydrogenation gas, characterized in that it is realized using the experimental device for accurate quantitative hydrogen addition according to any one of claims 1 to 3; it comprises the following steps:
hydrogen injection: opening a pressurized gas source (10) to inject hydrogen into the gold tube (30) at a certain pressure and for a certain time;
replacement air: closing the first stop valve (11) and simultaneously opening the second stop valve (25) to slowly release the exhaust gas;
repeating the steps of injecting hydrogen and replacing air until the air composition in the gold tube (30) meets the experimental requirements;
sealing the gold tube (30): the golden tube (30) is pressed by a pressure clamp (32) and the air inside the golden tube (30) is sealed, and whether the tightness is good or not is checked.
5. The method according to claim 4, wherein the sealing is performed by argon arc welding after clamping the wall of the gold tube (30) by a press clamp while sealing the air inside the gold tube (30).
6. The method according to claim 5, wherein the sealing is checked by placing the sealed gold tube (30) in hot water at a temperature of more than 60 ℃ and checking whether beaded bubbles are generated to determine whether the gas tightness in the gold tube (30) is good.
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| CN202110249817.2A CN115050250B (en) | 2021-03-08 | 2021-03-08 | Experimental device and method for accurately and quantitatively adding hydrogen |
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| CN202110249817.2A CN115050250B (en) | 2021-03-08 | 2021-03-08 | Experimental device and method for accurately and quantitatively adding hydrogen |
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| CN115050250A CN115050250A (en) | 2022-09-13 |
| CN115050250B true CN115050250B (en) | 2024-04-02 |
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