CN103869044A - Testing device and testing method for reaction of carbon dioxide and hot dry rock powder - Google Patents
Testing device and testing method for reaction of carbon dioxide and hot dry rock powder Download PDFInfo
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- CN103869044A CN103869044A CN201410100071.9A CN201410100071A CN103869044A CN 103869044 A CN103869044 A CN 103869044A CN 201410100071 A CN201410100071 A CN 201410100071A CN 103869044 A CN103869044 A CN 103869044A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 147
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 67
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 61
- 238000012360 testing method Methods 0.000 title claims abstract description 61
- 239000000843 powder Substances 0.000 title claims abstract description 40
- 239000011435 rock Substances 0.000 title claims abstract description 34
- 238000001179 sorption measurement Methods 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000005259 measurement Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 230000001502 supplementing effect Effects 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000004364 calculation method Methods 0.000 claims description 7
- 238000001612 separation test Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000013589 supplement Substances 0.000 claims description 2
- 230000000153 supplemental effect Effects 0.000 claims description 2
- 238000010998 test method Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 8
- 230000004069 differentiation Effects 0.000 abstract 1
- 230000010354 integration Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 22
- 238000011161 development Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000009919 sequestration Effects 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
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Abstract
The invention discloses a testing device and a testing method for reaction of carbon dioxide and hot dry rock powder, relating to the testing technology of geological storage of carbon dioxide in deep earthcrust. The testing device is composed of a carbon dioxide gas pressurization system (10), a core reaction system (20), a cold well gas-water separating system (30) and an oil bath constant temperature system (40), wherein the core reaction system (20) comprises a pressure compensating vessel (21), a reaction kettle (22), an adsorption kettle (23), a PID (Proportion Integration Differentiation) automatic pressure control valve (24) and a gas guide pipe (25); and the cold well gas-water separating system (30) comprises a cold well (31), a secondary vacuum buffer container (32), a primary vacuum buffer container (33), a vacuum pump (34) and a common valve (35). Data measurement is simple, the parameters such as temperature and pressure are only recorded, the consumption amount of carbon dioxide in the reaction can be calculated, the testing efficiency can be effectively improved and the device and the method can provide reliable theory and testing basis for the technology of carbon dioxide geological storage.
Description
Technical Field
The invention relates to a test technology for geological storage of carbon dioxide in deep crustal parts, in particular to a test device and a test method for simulating carbon dioxide-hot dry rock powder reaction under the conditions of high temperature and high pressure.
Background
The development and utilization of energy resources not only promote the rapid development of society, but also cause increasingly serious environmental problems. The use of fossil fuel is the largest pollution source of gas at present and also the largest emission source of greenhouse gas carbon dioxide. The emission of carbon dioxide causes global warming, thereby causing negative effects on environment and ecology, so that effective measures must be taken to control the emission of carbon dioxide and slow down the intensification of greenhouse effect. The Enhanced Geothermal System (EGS) using carbon dioxide as working medium can not only extract heat, but also realize the sealing and storage of carbon dioxide, thereby having good development prospect. In an EGS system, carbon dioxide and hot dry rock powder are subjected to chemical reaction under the conditions of high temperature and high pressure, so that the carbon dioxide is solidified and permanently sealed in the deep part of the crust, which is the theoretical basis and key link of the geological sealing technology of the carbon dioxide. The main reason why the optimal temperature and pressure during the reaction of carbon dioxide and dry-hot rock powder are not known uniformly at present is that no test device capable of changing the reaction temperature and pressure in a large range and with high precision is developed at present, the reaction process cannot be measured accurately, the calculation of the carbon dioxide consumed by the actual reaction cannot reach sufficient precision, and the calculation method is not mature.
The reaction test device for carbon dioxide under high temperature and high pressure in the prior art at home and abroad has the temperature change range limited to about 200 ℃, the operation process of the test is more complicated, the safety degree is not high, the test result is rough due to large data metering error, the persuasion is not strong, and the cost is very expensive.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art, and provides a test device and a method for carbon dioxide-dry hot rock powder reaction, which can accurately measure the amount of carbon dioxide consumed by a certain amount of dry hot rock powder in the reaction with carbon dioxide under the conditions of high temperature and high pressure based on the assistance of water vapor, thereby providing reliable theoretical and test basis for the carbon dioxide geological sequestration technology.
The purpose of the invention is realized as follows:
first, design idea
1. A high-temperature oil bath heating system is utilized to keep the reaction kettle and the adsorption kettle in a constant temperature state;
2. a PID automatic pressure control valve is utilized to enable the reaction kettle and the adsorption kettle to be in a constant pressure state;
3. the reaction kettle is provided with a magnetic stirrer, so that reactants are subjected to full contact reaction;
4. the amount of carbon dioxide consumed by the reaction can be calculated by recording parameters such as temperature, pressure and the like.
Second, technical scheme
1. Carbon dioxide-dry heat rock powder reaction test device (device for short)
The device consists of a carbon dioxide gas pressurization system, a core reaction system, a cold well gas-water separation system and an oil bath constant temperature system;
the core reaction system comprises a pressure supplementing container, a reaction kettle, an adsorption kettle, a PID automatic pressure control valve and an air guide pipe; the PID automatic pressure control valve 2 comprises a 1 st PID automatic pressure control valve and a 2 nd PID automatic pressure control valve 2 … … 5;
the cold well gas-water separation system comprises a cold well, a secondary vacuum buffer container, a primary vacuum buffer container, a vacuum pump and a common valve;
the position and connection relation is as follows:
the reaction kettle and the adsorption kettle are arranged in an oil bath constant temperature system;
respectively placing the dry hot rock powder in a reaction kettle and an adsorption kettle;
the carbon dioxide gas pressurization system, the 1 st PID automatic pressure control valve, the pressure supplementing container and the 2 nd PID automatic pressure control valve are sequentially communicated through a gas guide pipe to provide a pressurized carbon dioxide gas;
the 2 nd PID automatic pressure control valve, the 3 rd PID automatic pressure control valve, the reaction kettle, the 4 th PID automatic pressure control valve, the cold well, the secondary vacuum buffer container, the common valve, the primary vacuum buffer container and the vacuum pump 34 are sequentially communicated through the gas guide pipe, so that high-temperature and high-pressure reaction of the dry and hot rock powder in the reaction kettle is realized, and the residual water vapor in the reaction kettle is cooled and metered after a reaction test;
the 2 nd PID automatic pressure control valve, the 5 th PID automatic pressure control valve and the adsorption kettle are sequentially communicated through the air guide pipe, so that the measurement of carbon dioxide adsorbed in the dry hot rock powder G in the adsorption kettle in the reaction test process is realized.
2. Carbon dioxide-dry heat rock powder reaction method (method for short)
The method is based on the carbon dioxide and hot dry rock reaction test device and comprises the following reaction tests, gas-liquid separation tests, adsorption tests and calculation methods:
1) reaction test
Taking volume as V0The dry hot rock powder is weighed and then added into a reaction kettle, and the mass is m0;
② taking enough water, placing it into water storage device (measuring cup) in the reaction kettle, the water volume is Vw;
Thirdly, sealing the reaction kettle, vacuumizing the reaction kettle by using a vacuum pump, heating to the temperature (room temperature to 350 ℃) required by the test, and measuring the pressure P in the reaction kettle after the temperature inside and outside the reaction kettle is stable1;
Fourthly, opening the 2 nd and 3 rd PID automatic pressure control valves, adding the pressure in the reaction kettle to the pressure P (0 to 50 MPa) required by the reaction, and recording the pressure P of the pressure compensation containerb1;
Opening the reaction kettle stirrer to ensure that the reaction kettle is fully reacted, and continuously supplementing pressure through 2 nd and 3 rd PID automatic control pressure valves to keep the pressure in the reaction kettle constant in the reaction process;
closing the 2 nd and 3 rd PID automatic pressure control valves after the reaction is finished, recording the pressure P of the pressure compensating container at the momentb2;
2) Gas-liquid separation test
After the reaction test is finished, opening a cold well at the outlet of the reaction kettle, evacuating gas in the reaction kettle (in the process, the temperature in the reaction kettle is required to be ensured to be higher than the boiling point of water so as to ensure that residual carbon dioxide gas and water vapor in the reaction kettle are completely released), cooling the exhausted gas at the outlet, and metering the amount V of liquid waterwsObtaining the volume of the residual water in the reaction kettle;
3) adsorption test
A. Taking out the residual solid powder V in the reaction kettlesWeighing the materials after drying and vacuumizing, wherein the mass is ms;
B. The weighed solid powder is filled into an adsorption kettle, the temperature required by a reaction test is heated to be between room temperature and 350 ℃, after the temperature inside and outside the adsorption kettle is balanced, a 2 nd PID automatic pressure control valve and a 5 th PID automatic pressure control valve are opened, and the pressure is increased to be the pressure P required by the reaction test;
C. keeping the state and standing for a period of time, namely recording the pressure P' of the adsorption kettle at the moment when the pressure is not changed;
4) calculation method
When the temperature is T and the pressure is P, the volume V of the consumed steam can be obtained according to the data of the reaction test and the gas-liquid separation testwxAnd volume of supplemental carbon dioxide
When the volume of water vapor consumed is converted to the volume of carbon dioxide at the same pressure, it is:
wherein V is the volume of the reaction kettle,
Vbuin order to supplement the volume of the pressure container,
the rest symbols are consistent with those mentioned in the operation steps;
meanwhile, according to an adsorption test, the adsorption quantity of the powder is as follows:
wherein,is the volume of carbon dioxide adsorbed,
Vxis the volume of the adsorption tank,
the rest symbols are consistent with those mentioned in the operation steps;
from the above experiments and calculations, the amount of CO2 consumed during the reaction was knownTotal amount of CO2 to be added to the autoclave for the pressure compensating vesselThe amount of carbon dioxide supplemented by water vapor consumption in the reaction process is subtractedThen subtract the amount of CO2 adsorbed by the powderNamely:
the invention has the following characteristics and positive effects:
1. the whole device adopts a modular design, so that the operation and the maintenance are convenient;
2. the high-temperature part adopts automatic lifting, so that direct operation by people is avoided, and the test is safe and reliable;
3. the carbon dioxide gas pressurization system adopts a booster pump provided with a high-pressure safety valve to control the limit pressure of the system, so that accidents caused by overpressure are avoided;
4. the PID automatic pressure control valve can accurately control the pressure, and the precision reaches 0.1 MPa.
The invention has the following advantages and positive effects:
1. due to the modular design, the high-temperature part adopts automatic lifting, the complicated operation process and maintenance cost in the prior device can be reduced, the test process is safer and more reliable, and the precision of the PID automatic pressure control valve can reach 0.1MPa, so the measurement result of the invention is more accurate.
2. Each system and each part in the whole device are accurately processed and professionally assembled, so that the error sources are reduced, the error size is reduced, and the measurement result is efficiently processed, so that the method has development prospect and other potential application prospects;
3. the data measurement of the invention is very simple, and the carbon dioxide amount consumed by the reaction can be calculated only by recording parameters such as temperature, pressure and the like, so that the test efficiency can be effectively improved;
4. the variable range of the working pressure and the oil bath temperature is larger, the great effect is achieved on directly searching the optimal temperature and pressure when the carbon dioxide reacts with the dry hot rock powder, the magnetic stirrer is arranged in the reaction kettle, the reactants can be fully contacted, the reaction is more complete, and the working effect of the whole device can provide more reliable theoretical and experimental basis for the carbon dioxide geological storage technology;
in a word, the invention has important theoretical research and indoor test values due to low cost, simple operation, safety, reliability and high measurement precision.
Drawings
FIG. 1 is a block diagram showing the structure of a carbon dioxide-hot dry rock reaction test apparatus;
FIG. 2 is a block diagram of the structure of a core reaction system;
FIG. 3 is a block diagram of the structure of a cold well gas-water separation system.
In the figure:
10-carbon dioxide gas pressurization system;
20-a core reaction system, wherein,
21-a pressure compensating container;
22-a reaction kettle;
23-an adsorption kettle;
24-a PID automatic pressure control valve,
241. 242 … … 245-No. 1, 2 … … 5PID automatic pressure control valve;
25-gas-guide tube;
30-a gas-water separation system of a cold well,
31-cold well; 32-a secondary vacuum buffer container; 33-first stage vacuum buffer container;
34-a vacuum pump; 35-a common valve;
t-thermometer;
g-dry hot rock powder.
Detailed Description
The following detailed description is made with reference to the accompanying drawings and examples:
a, device
1. General of
Referring to fig. 1, fig. 2 and fig. 3, the device is composed of a carbon dioxide gas pressurization system 10, a core reaction system 20, a cold well gas-water separation system 30 and an oil bath constant temperature system 40;
the core reaction system 20 comprises a pressure supplementing container 21, a reaction kettle 22, an adsorption kettle 23, a PID automatic pressure control valve 24 and an air duct 25; the PID automatic pressure control valve 24 comprises 1 st and 2 nd 2 … … 5 th PID automatic pressure control valves 241 and 242 … … 245;
the cold well gas-water separation system 30 comprises a cold well 31, a secondary vacuum buffer container 32, a primary vacuum buffer container 33, a vacuum pump 34 and a common valve 35;
the position and connection relation is as follows:
the reaction kettle 22 and the adsorption kettle 23 are arranged in an oil bath constant temperature system 40;
the dry hot rock powder G is respectively placed in a reaction kettle 22 and an adsorption kettle 23;
the carbon dioxide gas pressurization system 10, the 1 st PID automatic pressure control valve 241, the pressure supplementing container 21 and the 2 nd PID automatic pressure control valve 242 are sequentially communicated through the air duct 25 to provide a pressurized carbon dioxide gas;
the 2 nd PID automatic pressure control valve 242, the 3 rd PID automatic pressure control valve 243, the reaction kettle 22, the 4 th PID automatic pressure control valve 244, the cold well 31, the secondary vacuum buffer container 32, the common valve 35, the primary vacuum buffer container 33 and the vacuum pump 34 are sequentially communicated through the air duct 25, so that the high-temperature and high-pressure reaction of the dry hot rock powder G in the reaction kettle 22 is realized, and the residual water vapor in the reaction kettle 22 is cooled and metered after the reaction test;
the 2 nd PID automatic control pressure valve 242, the 5 th PID automatic control pressure valve 245 and the adsorption kettle 23 are sequentially communicated through the gas guide pipe 25, and measurement of carbon dioxide adsorbed by the dry-hot rock powder G in the adsorption kettle 23 in the reaction test process is achieved.
2. Principle of operation
The test of the invention comprises a reaction test, a gas-liquid separation test and an adsorption test which are carried out in a core reaction system 20 and a cold well gas-water separation system 30, a carbon dioxide gas pressurization system 10 and an oil bath constant temperature system 40 are used as auxiliary equipment, and reactants are hot dry rock powder G, carbon dioxide and water vapor.
The carbon dioxide gas pressurization system 10 is used as a pressure source and is directly communicated with the pressure supplementing container 21 and is provided with a high-pressure safety valve for providing the pressure required by the system; after the pressure compensating container 21 is loaded with a PID automatic pressure control valve 24 through a gas guide pipe 25, the pressure compensating container is respectively communicated with the reaction kettle 22 and the adsorption kettle 23, so that the interior of the reaction kettle 22 and the interior of the adsorption kettle 23 are in a constant pressure state in the whole reaction process; the reaction kettle 22 and the adsorption kettle 23 are placed in the oil bath constant temperature system 40 at respective use stages, so that the whole reaction process is in a constant temperature state; the reaction kettle 22 is connected with a cold well gas-water separation system 30 through a gas guide pipe 25, and is provided with a vacuum pump 34 and a vacuum buffer container to fully release the residual water vapor in the reaction kettle 22 after reaction and the water adsorbed by the dry hot rock powder G.
2. Functional component
1) Carbon dioxide gas pressurization system 10
The carbon dioxide gas pressurizing system 10 is composed of a pressurizing pump equipped with a high-pressure safety control valve, which can provide a pressure source for the system and can prevent an overpressure accident.
2) Core reaction system 20
As shown in fig. 2, the core reaction system 20 includes a pressure compensating vessel 21, a reaction kettle 22, an adsorption kettle 23, a PID automatic pressure control valve 24, and an air duct 25, wherein the pressure compensating vessel 21, the reaction kettle 22, and the adsorption kettle 23 are all conventional high-pressure autoclave devices, have high temperature and high pressure resistance, can bear high temperature of about 350 ℃ and pressure of about 50MPa, and are equipped with a thermometer T capable of displaying the temperature inside and outside the vessel in real time; the PID automatic pressure control valve 24 can be used as a switch to control the circulation of high-pressure air flow and can display the pressure in each kettle in real time, and the precision reaches 0.1 MPa.
The pressure compensating vessel 21 stores carbon dioxide gas under high pressure.
② reaction kettle 22
The reaction vessel 22 is used as a reaction vessel for carbon dioxide and dry hot rock powder G, and is provided with a magnetic stirrer so as to fully contact the reactants.
③ adsorption kettle 23
The adsorption kettle 23 is used for measuring the amount of carbon dioxide adsorbed by the dry heat rock powder G in the reaction kettle 22 during the reaction test.
PID automatic pressure control valve 24
The PID automatic pressure control valve 24 is an automatic pressure control valve based on a PID control technology, comprises 1 st and 2 … … 5 th PID automatic pressure control valves 241 and 242 … … 245, can realize automatic pressure control and data output, and has the precision of 0.1 Mpa.
Fifthly, the air duct 25
The air duct 25 is a conventional conduit that serves as a connector for the components on the one hand and as a passage for the high pressure air stream on the other hand.
3) Cold well gas-water separation system 30
As shown in fig. 3, the cold well gas-water separation system 30 includes a cold well 31, a secondary vacuum buffer container 32, a primary vacuum buffer container 33, a vacuum pump 34 and a common valve 35, and is used for cooling and metering residual water vapor in the reaction kettle after a reaction test;
cooling well 31
The cold well 31 is a standard component and has a cooling effect, and the temperature range is-5-10 ℃;
② two-stage vacuum buffer container 32
The secondary vacuum buffer container 32 is a standard component and is used for performing a secondary buffer function during vacuum pumping;
③ Primary vacuum buffer container 33
The first-stage vacuum buffer container 33 is a standard component and is used for playing a buffer role during vacuumizing;
fourthly, the vacuum pump 34
The vacuum pump 34 is a standard component and is used for pumping air so as to enable the reaction kettle 22 to reach the vacuum required by the test;
fifth common valve 35
The ordinary valve 35 is a standard component and plays a control role.
4) Oil bath constant temperature system 40
The oil bath constant temperature system 40 is a standard component to realize constant temperature control of the system, the temperature controllable range is room temperature-350 ℃, the precision can reach +/-0.5 ℃, an automatic heating device is adopted, direct operation of people is avoided, and safety and reliability of the test are ensured.
Through detection, the invention has the following basic performance indexes:
1. working pressure: 0-50 MPa, and the precision is +/-0.1 MPa;
2. oil bath temperature: the room temperature is 350 ℃, and the precision is +/-0.5 ℃;
3. specification of the reaction kettle: magnetically stirring at 50MPa/1L/350 deg.C;
4. temperature of the cold well: -5 to 10 ℃.
Second, application
The traditional reaction test device for carbon dioxide-dry hot rock powder under high temperature and high pressure has the advantages of narrow temperature change range, complex test operation process, low precision and high cost. The invention aims to overcome the defects and shortcomings of the prior art, and provides a test device and a method for carbon dioxide-dry hot rock powder reaction, which can accurately measure the amount of carbon dioxide consumed by a certain amount of dry hot rock powder in the reaction with carbon dioxide under the conditions of high temperature and high pressure based on the assistance of water vapor, thereby providing reliable theoretical and test basis for the carbon dioxide geological sequestration technology.
Claims (2)
1. The utility model provides a test device of carbon dioxide-dry heat rock powder reaction which characterized in that:
the system consists of a carbon dioxide gas pressurization system (10), a core reaction system (20), a cold well gas-water separation system (30) and an oil bath constant temperature system (40);
the core reaction system (20) comprises a pressure supplementing container (21), a reaction kettle (22), an adsorption kettle (23), a PID automatic pressure control valve (24) and an air duct (25); the PID automatic pressure control valve (24) comprises a 1 st PID automatic pressure control valve (241, 242 … … 245) and a 2 nd PID automatic pressure control valve (2, 2 … … 5);
the cold well gas-water separation system (30) comprises a cold well (31), a secondary vacuum buffer container (32), a primary vacuum buffer container (33), a vacuum pump (34) and a common valve (35);
the position and connection relation is as follows:
the reaction kettle (22) and the adsorption kettle (23) are arranged in an oil bath constant temperature system (40);
the dry hot rock powder (G) is respectively placed in a reaction kettle (22) and an adsorption kettle (23);
the carbon dioxide gas pressurization system (10), the 1 st PID automatic pressure control valve (241), the pressure supplementing container (21) and the 2 nd PID automatic pressure control valve (242) are sequentially communicated through a gas guide pipe (25) to provide a pressurized carbon dioxide gas;
the 2 nd PID automatic pressure control valve (242), the 3 rd PID automatic pressure control valve (243), the reaction kettle (22), the 4 th PID automatic pressure control valve (244), the cold well (31), the secondary vacuum buffer container (32), the common valve (35), the primary vacuum buffer container (33) and the vacuum pump (34) are sequentially communicated through the air duct (25), so that high-temperature and high-pressure reaction on dry and hot rock powder (G) in the reaction kettle (22) is realized, and residual steam in the reaction kettle (22) is cooled and metered after a reaction test;
the 2 nd PID automatic pressure control valve (242), the 5 th PID automatic pressure control valve (245) and the adsorption kettle (23) are sequentially communicated through the air duct (25), so that the measurement of carbon dioxide adsorbed in the dry hot rock powder (G) in the adsorption kettle (23) in the reaction test process is realized.
2. The test method of the test device for carbon dioxide-hot dry rock powder reaction according to claim 1, wherein:
1) reaction test
Taking volume as V0The dry hot rock powder is weighed and then added into a reaction kettle, and the mass is m0;
② taking enough water, placing it into water storage device (measuring cup) in the reaction kettle, the water volume is Vw;
Thirdly, sealing the reaction kettle, vacuumizing the reaction kettle by using a vacuum pump, heating to the temperature (room temperature to 350 ℃) required by the test, and measuring the pressure P in the reaction kettle after the temperature inside and outside the reaction kettle is stable1;
Fourthly, opening the 2 nd and 3 rd PID automatic pressure control valves, adding the pressure in the reaction kettle to the pressure P (0 to 50 MPa) required by the reaction, and recording the pressure P of the pressure compensation containerb1;
Opening the reaction kettle stirrer to ensure that the reaction kettle is fully reacted, and continuously supplementing pressure through 2 nd and 3 rd PID automatic control pressure valves to keep the pressure in the reaction kettle constant in the reaction process;
closing the 2 nd and 3 rd PID automatic pressure control valves after the reaction is finished, recording the pressure P of the pressure compensating container at the momentb2;
2) Gas-liquid separation test
After the reaction test is finished, opening a cold well at the outlet of the reaction kettle, evacuating gas in the reaction kettle (in the process, the temperature in the reaction kettle is required to be ensured to be higher than the boiling point of water so as to ensure that residual carbon dioxide gas and water vapor in the reaction kettle are completely released), cooling the exhausted gas at the outlet, and metering the amount V of liquid waterwsObtaining the volume of the residual water in the reaction kettle;
3) adsorption test
A. Taking out the residual solid powder V in the reaction kettlesWeighing the materials after drying and vacuumizing, wherein the mass is ms;
B. The weighed solid powder is filled into an adsorption kettle, the temperature required by a reaction test is heated to be between room temperature and 350 ℃, after the temperature inside and outside the adsorption kettle is balanced, a 2 nd PID automatic pressure control valve and a 5 th PID automatic pressure control valve are opened, and the pressure is increased to be the pressure P required by the reaction test;
C. keeping the state and standing for a period of time, namely recording the pressure P' of the adsorption kettle at the moment when the pressure is not changed;
4) calculation method
When the temperature is T and the pressure is P, the volume V of the consumed steam can be obtained according to the data of the reaction test and the gas-liquid separation testwxAnd volume of supplemental carbon dioxide
When the volume of water vapor consumed is converted to the volume of carbon dioxide at the same pressure, it is:
wherein V is the volume of the reaction kettle,
Vbuin order to supplement the volume of the pressure container,
the rest symbols are consistent with those mentioned in the operation steps;
meanwhile, according to an adsorption test, the adsorption quantity of the powder is as follows:
Vxis the volume of the adsorption tank,
the rest symbols are consistent with those mentioned in the operation steps;
from the above experiments and calculations, the amount of CO2 consumed during the reaction was knownTotal amount of CO2 to be added to the autoclave for the pressure compensating vesselThe amount of carbon dioxide supplemented by water vapor consumption in the reaction process is subtractedThen subtract the amount of CO2 adsorbed by the powderNamely:
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Cited By (2)
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CN109030140A (en) * | 2018-06-30 | 2018-12-18 | 西南石油大学 | A kind of thermal production well Behavior of Hardened Cement Paste high-temperature water wet curing simulation test device and method |
CN113685175A (en) * | 2021-08-18 | 2021-11-23 | 中国科学院武汉岩土力学研究所 | Method and device for underground fixed-depth in-situ comprehensive experiment |
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CN102635468A (en) * | 2012-04-23 | 2012-08-15 | 北京建筑工程学院 | Carbon dioxide fixing device |
CN203732526U (en) * | 2014-03-18 | 2014-07-23 | 中国科学院武汉岩土力学研究所 | Test device for carbon dioxide-hot dry rock powder reaction |
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