CN101149363B - Rock sample hydrocarbon generation kinetics high pressure thermal simulation experimental method and device - Google Patents
Rock sample hydrocarbon generation kinetics high pressure thermal simulation experimental method and device Download PDFInfo
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- CN101149363B CN101149363B CN2007100311157A CN200710031115A CN101149363B CN 101149363 B CN101149363 B CN 101149363B CN 2007100311157 A CN2007100311157 A CN 2007100311157A CN 200710031115 A CN200710031115 A CN 200710031115A CN 101149363 B CN101149363 B CN 101149363B
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Abstract
The invention discloses a hydrocarbon dynamics high pressure thermal simulation experiment method and the device for the rock sample, which belongs to the rock oil and natural gas earth chemical experiment research technology field. The method includes the sealing sample into the gold pipe, putting the gold pipe into the high pressure kettle, putting many high pressure kettle into one pyrolyzing oven, starting the water adding pressure and stabilized voltage system, the pyrolyzing oven, picking out one high-pressure kettle and cooling quickly in different temperature point, closing the pyrolyzing oven and water adding pressure and stabilized voltage system until the high-pressure kettle with sample is picked out, then opening the high-pressure kettle and analysis of the sample; the device is made up of the water adding pressure and stabilized voltage system, the heating system and the controlling system. The water adding pressure and stabilized voltage system includes the water tank, the high pressure water pump and the stabilized voltage valve. The heating system includes the pyrolyzing oven, many high-pressure kettles and circle fan. The controlling system includes the central computer, the pressure controller, the pressure recorder, the temperature controller and multi-way temperature detection recorder. The invention can be used in analysis of the kerogen or rock sample.
Description
Technical field
The present invention relates to petroleum gas geochemistry experiment investigative technique, more particularly, it relates to the hydrocarbon generation kinetics high pressure thermal simulation experimental method of rock sample, the invention still further relates to the experimental provision of realizing said method.
Background technology
In petroleum gas geochemical investigation field, need come the geologize sample under certain temperature, pressure by thermal simulation experiment, the quantity of the hydro carbons that is produced and composition.And in the thermal simulation experiment research of hydrocarbon-generating dynamics, especially need to control accurately the temperature and pressure of experiment.The thermal simulation experiment that surpasses 100MPa pressure is both at home and abroad all realized by the piston type press at present, being about to rock sample is placed among the metallic cylinder, a piston is arranged at sample top, by oil pressure or baric systerm piston is pressurizeed, and piston pressurizes to sample again; Thereby heating produces hydro carbons to the sample among the metallic cylinder with electric tube furnace simultaneously.Such device has following shortcoming: (1) because need prevent gas leakage, the friction force between piston and the metallic cylinder is quite big, causes the pressure that really is applied on the sample on the low side like this; (2) repeatedly in the experiment, because the variation of the friction force between above-mentioned piston and the metallic cylinder, the actual pressure that each laboratory sample is subjected to is not quite identical; (3) for the thermal simulation experiment of hydrocarbon-generating dynamics, a living hydrocarbon curve needs 10 temperature spots, because the piston type compression system can only be adorned a sample, 10 temperature spots will be done 10 experiments, and workload is huge, and efficient is very low.
Summary of the invention
The technical problem to be solved in the present invention is at the deficiencies in the prior art, and the hydrocarbon generation kinetics high pressure thermal simulation experimental method of a kind of pressure, temperature fluctuation is little, simple to operate, efficient is high rock sample is provided.
Another technical matters that the present invention will solve provides a kind of device of realizing said method.
Last technical scheme of the present invention is such: a kind of hydrocarbon generation kinetics high pressure thermal simulation experimental method of rock sample comprises the steps:
(1) under inert gas shielding, be encapsulated in sample to be analyzed in the golden pipe;
(2) the golden pipe that at least one is equipped with sample is positioned in the autoclave that is connected with water pressurization and voltage-stabilizing system;
(3) a plurality of autoclaves are positioned in the same pyrolysis oven;
(4) start water pressurization and voltage-stabilizing system, pressure in whole autoclaves is reached and remain on a predefined numerical value;
(5) start pyrolysis oven work, and carry out heat temperature raising by the programming rate of setting;
(6) when temperature reaches the required temperature spot of certain autoclave, close its pressurization of corresponding water and voltage-stabilizing system valve, this autoclave is taken out from pyrolysis oven, be placed in the cold water and cool off rapidly;
(7) all the other autoclaves continue heating, and take out an autoclave respectively at different temperature spots, and the autoclave that laboratory sample is housed until remainder all after the taking-up, cuts out pressurization of pyrolysis oven and water and voltage-stabilizing system from pyrolysis oven;
(8) open autoclave, take out sample gold pipe, carry out every analyses such as gas yield, composition, isotope.
In the hydrocarbon generation kinetics high pressure thermal simulation experimental method of above-mentioned rock sample, the gold pipe diameter described in the step (1) is 4～6 millimeters, 40～120 millimeters of length; Sample to be analyzed is one of kerogen or protolith, and amount of samples is 3～2000mg; Also in the gold pipe, be added with gas or water or reagent during encapsulation according to the experiment needs.The predefined numerical value of pressure described in the step (4) is 10～300 MPa.Programming rate described in the step (5) be 20 ℃/time or 2 ℃/time.
Back of the present invention one technical scheme is such: a kind of device of hydrocarbon generation kinetics high pressure thermal simulation experiment of rock sample, form by water pressurization and voltage-stabilizing system, heating system and control system, wherein, described water pressurization and voltage-stabilizing system comprise water tank, high-pressure hydraulic pump and pressure maintaining valve, the water inlet pipeline of high-pressure hydraulic pump connects water tank, and pressure maintaining valve is connected on the water output main line of high-pressure hydraulic pump; Described heating system comprises pyrolysis oven, a plurality of autoclaves and circulating fan, a plurality of autoclaves are arranged in the pyrolysis oven ringwise, circulating fan is arranged on the inner underside of pyrolysis oven, described control system comprises central controlling computer, pressure controller, pressure recorder, temperature controller and multipath temperature patrol inspection register, and pressure controller, pressure recorder, temperature controller and multipath temperature patrol inspection register connect with central controlling computer circuit respectively; The water output of described high-pressure hydraulic pump connects each autoclave by parallel pipeline respectively, is respectively equipped with high-pressure solenoid valve on the connecting branch road between high-pressure hydraulic pump and each autoclave; The output control signal circuit of the output pressure signal difference circuit connection pressure controller of high-pressure hydraulic pump and pressure recorder, pressure controller connects high-pressure hydraulic pump; The temperature output signal of described pyrolysis oven circuit respectively connects temperature controller and multipath temperature patrol inspection register, and the output control signal circuit of temperature controller connects pyrolysis oven.
In the device of the hydrocarbon generation kinetics high pressure thermal simulation experiment of above-mentioned rock sample; described water pressurization and voltage-stabilizing system also comprise superpressure cascading water protective valve; superpressure cascading water protective valve connects the water output of high-pressure hydraulic pump to be responsible for; the control input signals circuit of superpressure cascading water protective valve connects central controlling computer, and the fortuitous event that is used for losing efficacy simultaneously at pressure maintaining valve and pressure controller takes place and system protection when causing pressure to be elevated to dangerous values.Described heating system also comprises the overtemperature prote device, and overtemperature prote device circuit connects pyrolysis oven, and the control input signals circuit of overtemperature prote device connects central controlling computer, is used for the system protection when temperature controller lost efficacy.
The present invention compared with prior art has following advantage:
(1) sample is encapsulated in the argon gas case and carries out, and guaranteeing does not have air pollution.
(2) a plurality of autoclaves are positioned in the same pyrolysis oven, and the temperature difference of each autoclave is less than 1 ℃, and pressure can be set arbitrarily at 10～300MPa, and is adjustable continuously, automatically control.
(3) temperature controller can carry out temperature control processes such as constant temperature, temperature programme and curve intensification as required, and temperature range is room temperature～650 ℃, and temperature fluctuation is less than 1 ℃.
(4) efficient height, once experiment can obtain the living hydrocarbon data of 84 samples at 14 temperature/time points.
Description of drawings
Below in conjunction with drawings and Examples the present invention is described in further detail, but does not constitute any limitation of the invention.
Fig. 1 is the structural representation of experimental provision among the present invention.
Among the figure: water tank 10, high-pressure hydraulic pump 11, pressure maintaining valve 12, high-pressure solenoid valve 13, superpressure cascading water protective valve 14, tensimeter 15, pyrolysis oven 20, autoclave 21, circulating fan 22, overtemperature prote device 23, central controlling computer 30, pressure controller 31, pressure recorder 32, temperature controller 33, multipath temperature patrol inspection register 34, sample gold pipe 40.
Embodiment
Consult shown in Figure 1; the device of the hydrocarbon generation kinetics high pressure thermal simulation experiment of rock sample of the present invention; form by water pressurization and voltage-stabilizing system, heating system and control system; water pressurization and voltage-stabilizing system comprise water tank 10, high-pressure hydraulic pump 11, pressure maintaining valve 12, high-pressure solenoid valve 13, superpressure cascading water protective valve 14 and tensimeter 15; the water inlet pipeline of high-pressure hydraulic pump 11 connects water tank 10, and pressure maintaining valve 12, superpressure cascading water protective valve 14 and tensimeter 15 all are connected on the water output main line of high-pressure hydraulic pump 11.
Heating system comprises that vertical electric separates 20, ten five autoclaves 21 of stove, circulating fan 22 and 23, ten five autoclaves 21 of overtemperature prote device and be arranged on ringwise in the pyrolysis oven 20, and circulating fan 22 is arranged on the inner underside of pyrolysis oven 20; Overtemperature prote device 23 circuits connect pyrolysis oven 20.
Control system comprises central controlling computer 30, pressure controller 31, pressure recorder 32, temperature controller 33 and 30 two road temperature patrol inspection registers 34, and pressure controller 31, pressure recorder 32, temperature controller 33 and 30 two road temperature patrol inspection registers 34 connect with central controlling computer 30 circuits respectively; The control input signals circuit of overtemperature prote device 23 connects central controlling computer 30.The control input signals circuit of superpressure cascading water protective valve 14 connects central controlling computer 30.
The temperature output signal of pyrolysis oven 20 circuit respectively connects temperature controller 33 and multipath temperature patrol inspection register 34, and the output control signal circuit of temperature controller 33 connects pyrolysis oven 20.
The water output of high-pressure hydraulic pump 11 connects each autoclave 21 by parallel pipeline respectively, adopt the pressure parallel way, the pressure that can guarantee each autoclave 21 is in full accord, on the connecting branch road between high-pressure hydraulic pump 11 and each autoclave 21, be respectively equipped with high-pressure solenoid valve 13, be used for the water lines switch of each autoclave 21; The output control signal circuit of the output pressure signal difference circuit connection pressure controller 31 of high-pressure hydraulic pump 11 and pressure recorder 32, pressure controller 31 connects high-pressure hydraulic pump 11.
Water pressurization and voltage-stabilizing system are when work, and each autoclave 21 can be placed six sample gold pipes 40 at most, and by 11 pairs of autoclave 21 water-fillings of high-pressure hydraulic pump, water under high pressure is crushed sample gold pipe 40, and then the sample in the sample gold pipe 40 is exerted pressure.The tensimeter 15 that is connected on the high-pressure hydraulic pump 11 water output person in charge is used for observing pressure, and when pressure raise, pressure maintaining valve 12 was opened automatically, and bleed off goes out a spot of water, makes system pressure keep stablizing constant.Cross when low when system pressure, pressure controller 31 output signals make high-pressure hydraulic pump 11 start pressurization, and like this, by the concerted action of pressure maintaining valve 12 and pressure controller 31, making is that pressure remains at a predefined numerical value.The fortuitous event that lost efficacy simultaneously when pressure maintaining valve 12 and pressure controller 31 takes place and when causing pressure to be elevated to dangerous values; superpressure cascading water protective valve 14 is opened, and system pressure is discharged, and protection system is without prejudice; make system cut-off by central controlling computer 30 simultaneously, wait for maintenance.
Heating system is when work, and 15 autoclaves are ring-like and are placed in the electric pyrolysis oven 20, and the circulating fan 22 of electric pyrolysis oven 20 bottoms makes the temperature unanimity at each position in the stove.In 15 autoclaves 21, the center and the outer wall of one of them autoclave 21 are equipped with thermopair, are used for measuring and the control temperature, and the top and the bottom of all the other each autoclaves 21 respectively are equipped with a thermopair and are used for monitor temperature.Temperature controller 33 and overtemperature prote device 23 guarantee that electric pyrolysis oven 20 is by the program run of setting; the temperature signal of 32 thermopairs by 30 two road temperature patrol inspection registers 34, changes into digital signal; be sent to central controlling computer 30, show in real time and record in addition in central controlling computer 30.
Utilize the job step of this system as follows:
(1) the kerogen sample is enclosed gold pipe 40 with argon arc welding under argon shield, 4～6 millimeters of gold pipe diameters, 40～120 millimeters of length.Amount of samples can be selected arbitrarily between 3-2000mg, sample can be kerogen, also can be protolith, can add special gas (as adding gases such as sulfuretted hydrogen, methane, study these gases under High Temperature High Pressure and the interaction of rock), water or other reagent (, study these materials and under High Temperature High Pressure, generate the kinetic parameter of gas and carbon, hydrogen isotope evolution feature) as single chemical substances such as normal hexane, 24 alkane.
(2) six of sample gold pipes 40 will be housed is positioned in the autoclave 21 that is connected with water pressurization and voltage-stabilizing system.
(3) 15 autoclaves 21 are circularized shape and be placed in the electric pyrolysis oven 20, wherein 14 are equipped with gold pipe 40 respectively, and one of them is unkitted.
(4) start water pressurization and voltage-stabilizing system, promptly open each high-pressure solenoid valve 13, start high-pressure hydraulic pump, pressure maintaining valve 12 and pressure controller 31 work, pressure in the whole autoclaves 21 are reached and remain on a predefined numerical value (normally a point between 10～300MPa, as 50MPa).
(5) start electric pyrolysis oven 20 work, and carry out heat temperature raising by the programming rate of setting; Promptly, make the temperature of electric pyrolysis oven 20 be elevated to required temperature by room temperature by temperature controller 33 and overtemperature prote device 23 are set, heating rate be generally 20 ℃/time and 2 ℃/time.
(6) when temperature reaches the required temperature spot of certain autoclave 21, close its pressurization of corresponding water and voltage-stabilizing system high-pressure solenoid valve 13, this autoclave 21 is taken out from pyrolysis oven 20, be placed in the cold water and cool off rapidly.
(7) all the other autoclaves 21 continue heating, and take out (6) operation set by step of an autoclave 21 respectively at different temperature spots, and the autoclave 21 that laboratory sample is housed until remainder all after the taking-up, cuts out pressurization of pyrolysis oven 20 and water and voltage-stabilizing system from pyrolysis oven 20;
(8) open autoclave 21, take out sample gold pipe 40, carry out every analyses such as gas yield, composition, isotope.
Claims (4)
1. the hydrocarbon generation kinetics high pressure thermal simulation experimental method of a rock sample is characterized in that comprising the steps;
(1) under inert gas shielding, be encapsulated in sample to be analyzed in the golden pipe;
(2) the golden pipe that at least one is equipped with sample is positioned in the autoclave that is connected with water pressurization and voltage-stabilizing system;
(3) a plurality of autoclaves are positioned in the same pyrolysis oven;
(4) start water pressurization and voltage-stabilizing system, pressure in whole autoclaves is reached and remain on a predefined numerical value;
(5) start pyrolysis oven work, and carry out heat temperature raising by the programming rate of setting;
(6) when temperature reaches the required temperature spot of certain autoclave, close its pressurization of corresponding water and voltage-stabilizing system valve, this autoclave is taken out from pyrolysis oven, be placed in the cold water and cool off rapidly;
(7) all the other autoclaves continue heating, and take out an autoclave respectively at different temperature spots, after the autoclave that remainder is equipped with laboratory sample all takes out from pyrolysis oven. close pressurization of pyrolysis oven and water and voltage-stabilizing system;
(8) open autoclave, take out sample gold pipe, carry out gas yield, composition, the every analysis of isotope;
Gold pipe diameter described in the step (1) is 4～6 millimeters, 40～120 millimeters of length;
Sample to be analyzed described in the step (1) is one of kerogen or protolith, and amount of samples is 3～2000mg;
Also in the gold pipe, be added with gas or water or reagent during encapsulation described in the step (1) according to the experiment needs:
The predefined numerical value of pressure described in the step (4) is 50～300MPa;
Programming rate described in the step (5) be 20 ℃/time or 2 ℃/time.
2. device of implementing the hydrocarbon generation kinetics high pressure thermal simulation experimental method of the described rock sample of claim 1, form by water pressurization and voltage-stabilizing system, heating system and control system, it is characterized in that, described water pressurization and voltage-stabilizing system comprise water tank (10), high-pressure hydraulic pump (11) and pressure maintaining valve (12), the water inlet pipeline of high-pressure hydraulic pump (11) connects water tank (10), and pressure maintaining valve (12) is connected on the water output main line of high-pressure hydraulic pump (11); Described heating system comprises pyrolysis oven (20), a plurality of autoclaves (21) and circulating fan (22), a plurality of autoclaves (21) are arranged in the pyrolysis oven (20) ringwise, circulating fan (22) is arranged on the inner underside of pyrolysis oven (20), described control system comprises central controlling computer (30), pressure controller (31), pressure recorder (32), temperature controller (33) and multipath temperature patrol inspection register (34), pressure controller (31), pressure recorder (32), temperature controller (33) and multipath temperature patrol inspection register (34) connect with central controlling computer (30) circuit respectively; The water output of described high-pressure hydraulic pump (11) connects each autoclave (21) by parallel pipeline respectively, is respectively equipped with high-pressure solenoid valve (13) on the connecting branch road between high-pressure hydraulic pump (11) and each autoclave (21); The output control signal circuit of the output pressure signal difference circuit connection pressure controller (31) of high-pressure hydraulic pump (11) and pressure recorder (32), pressure controller (31) connects high-pressure hydraulic pump (11); The temperature output signal of described pyrolysis oven (20) circuit respectively connects temperature controller (33) and multipath temperature patrol inspection register (34), and the output control signal circuit of temperature controller (33) connects pyrolysis oven (20).
3. device according to claim 2; it is characterized in that; described water pressurization and voltage-stabilizing system also comprise superpressure cascading water protective valve (14); superpressure cascading water protective valve (14) connects the water output of high-pressure hydraulic pump (11) to be responsible for, and the control input signals circuit of superpressure cascading water protective valve (14) connects central controlling computer (30).
4. device according to claim 2; it is characterized in that; described heating system also comprises overtemperature prote device (23), and overtemperature prote device (23) circuit connects pyrolysis oven (20), and the control input signals circuit of overtemperature prote device (23) connects central controlling computer (30).
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| CN2007100311157A CN101149363B (en) | 2007-10-29 | 2007-10-29 | Rock sample hydrocarbon generation kinetics high pressure thermal simulation experimental method and device |
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| CN2007100311157A CN101149363B (en) | 2007-10-29 | 2007-10-29 | Rock sample hydrocarbon generation kinetics high pressure thermal simulation experimental method and device |
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| CN101149363B true CN101149363B (en) | 2011-09-14 |
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| CN102182911B (en) * | 2011-04-01 | 2014-03-19 | 中国科学研究院广州地球化学研究所 | Device for injecting gas into gold tube and use method thereof |
| RU2485495C2 (en) * | 2011-07-20 | 2013-06-20 | Открытое акционерное общество "Сургутнефтегаз" | Method to determine kerogen content in rocks and its parameters |
| CN102733801B (en) * | 2012-06-26 | 2015-08-05 | 中国石油天然气股份有限公司 | Diagenesis raw hydrocarbon row hydrocarbon overall process heat-press simulation experiment device |
| CN106482924B (en) * | 2015-08-31 | 2019-12-13 | 中国石油化工股份有限公司 | Rock hydrocarbon generation flow simulation device |
| CN105651912A (en) * | 2015-12-30 | 2016-06-08 | 海城市石油化工仪器厂 | Rock pyrologger and pyrolytic analysis method |
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| CN108181138B (en) * | 2017-12-29 | 2019-12-24 | 中国科学院广州地球化学研究所 | Gas taking device of hydrocarbon source rock hydrocarbon generation thermal simulation reaction kettle |
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| CN111173497B (en) * | 2020-01-10 | 2022-03-29 | 中国科学院广州地球化学研究所 | Mobile phase water rock reaction unit |
| CN111812267B (en) * | 2020-08-13 | 2024-04-12 | 西南交通大学 | Multi-field coupling effect dynamic linkage water rock effect experimental device and experimental method thereof |
| CN114441735A (en) * | 2020-11-03 | 2022-05-06 | 中国石油化工股份有限公司 | Hydraulic transmission device of hydrocarbon source rock hydrocarbon generation kettle |
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