CN101231279A - Autoclave for high pressure thermal simulation experiment and high pressure thermal simulation experimental method - Google Patents
Autoclave for high pressure thermal simulation experiment and high pressure thermal simulation experimental method Download PDFInfo
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- CN101231279A CN101231279A CNA2008100263707A CN200810026370A CN101231279A CN 101231279 A CN101231279 A CN 101231279A CN A2008100263707 A CNA2008100263707 A CN A2008100263707A CN 200810026370 A CN200810026370 A CN 200810026370A CN 101231279 A CN101231279 A CN 101231279A
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- autoclave
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Abstract
The invention discloses a high-pressure autoclave used for a high-pressure thermal simulation experiment and a high-pressure thermal simulation experiment method, and belongs to the technical field of the petroleum geochemistry experiment. The high-pressure autoclave has the technical key point that the outer surface of the autoclave body is provided with a plurality of annular grooves, an tubular cavity of the autoclave body is provided with at least one ceramic stick, the outside diameter of which is little smaller than the inside diameter of the tubular cavity. The experiment method includes the steps that: (1) a standard sample is used for measuring the correcting temperature with different rates of temperature rise; (2) three golden tubes packaged with samples are arranged inside the autoclave body in sequence, then the ceramic stick is put in to ensure that the autoclave body is positioned inside a heating furnace chamber and a screw sealed part is positioned outside a heating furnace body, heating experiment begins under the setting rate of temperature rise according to a conventional method; (3) a gas yield curve is obtained and the temperature correction is performed; (4) data through the temperature correction is processed to obtain a nascent hydrocarbon dynamical parameter. The invention is used for the high-pressure thermal simulation experiment.
Description
Technical field
The present invention relates to a kind of device that is used for the petroleum geochemistry experiment, more particularly, it relates to a kind of autoclave that is used for the high pressure thermal simulation experiment, the invention still further relates to and utilizes this autoclave to carry out high pressure thermal simulation experimental method.
Background technology
In the petroleum geochemistry experiment, rock sample need be encapsulated in the gold pipe, and then the gold pipe that sample will be housed puts into high pressure vessel (to call autoclave in the following text), in autoclave, inject water under high pressure by pipeline, water under high pressure flattens the gold pipe of softness, thereby sample is exerted pressure.The autoclave that is placed with the gold pipe is put into electric furnace again and is heated.Because the top of autoclave is the thread seal of cone with the bottom, under the little situation of pressure, the whole electric furnace of putting into of thread seal part can be heated, can make whole autoclave all obtain uniform heating, thereby make the sample on autoclave top and the sample of bottom bear identical temperature, guaranteed experimental precision.But (pressure is greater than 100MP) is if thread seal is partly put into electric furnace to be heated under the situation of high pressure, and during greater than 500 ℃, creep will take place the thread seal part, cause autoclave to be revealed, and make the failure of an experiment in temperature.For above-mentioned reasons, at present in the High Temperature High Pressure thermal cycle simulation of domestic and international existing pressure greater than 50MP, for guaranteeing sealing, it all is the outside that the top of autoclave is placed on electric furnace, but it is more much lower than the temperature of bottom that the consequence of doing like this is exactly the temperature on top of autoclave, through actual measurement, when the temperature on the autoclave top was 500 ℃, the temperature of bottom reached 548 ℃, and this temperature difference is affected by environment bigger, do not fix, thereby also can't be proofreaied and correct, because it is the autoclave temperature difference up and down is very big, inhomogeneous for what keep from heat, can only place a gold pipe during experiment in the bottom, experimental period is prolonged greatly.
Thermograde has two reasons, the heat conduction of (1) autoclave metal kettle itself about causing autoclave; (2) convection current of autoclave inner fluid.For solving the autoclave inconsistent problem of temperature up and down, the designer of the present patent application improves existing autoclave, and has proposed a kind of experimental program that adapts to this autoclave working, can well address the above problem.
Summary of the invention
The technical problem to be solved in the present invention is at the deficiencies in the prior art, and a kind of simple in structure, easy to use, the autoclave that is used for high pressure thermal simulation experiment that can test a plurality of samples simultaneously is provided.
Another technical matters that the present invention will solve provides a kind of efficient height, data high pressure thermal simulation experimental method accurately.
Last technical scheme of the present invention is achieved in that a kind of autoclave that is used for the high pressure thermal simulation experiment, comprises kettle, seal cones, cone pressure cap, feed tube and pipe pressure cap, is provided with unidirectional unlimited tubular cavity in the described kettle; The tapered portion of described seal cones is arranged on the open side of tubular cavity, the cone pressure cap of seal cones by being arranged on the seal cones periphery and the peristome crimping sealing of tubular cavity, and the cone pressure cap is threaded with kettle; Described feed tube passes seal cones and is communicated with tubular cavity, fix by the pipe pressure cap that is connected the seal cones rear portion, between seal cones and pipe pressure cap, be provided with the cydariform sealing ring, wherein, described kettle outside surface is provided with the multiple tracks annular groove, be placed with at least one section ceramic rod in tubular cavity, the external diameter of this ceramic rod is slightly less than the internal diameter of tubular cavity.
Above-mentioned a kind of autoclave that is used for the high pressure thermal simulation experiment, described annular groove is along the circumferential connection of kettle; The external diameter of described ceramic rod is than the little 0.5mm of internal diameter of tubular cavity.
Back of the present invention one technical scheme is achieved in that a kind of high pressure thermal simulation experimental method, comprises the steps: that (1) utilizes standard model to measure the Tc of different heating rates; (2) three gold that will be packaged with sample are managed the tubular cavity of putting into the described kettle of the application successively, put into two ceramic rods then, screw cone pressure cap and pipe pressure cap, and make kettle be positioned at the heating furnace chamber, make thread seal partly be positioned at outside the heating furnace body, in kettle, inject water under high pressure with high-pressure pump, begin the heating experiment according to a conventional method with the heating rate of setting; (3) analyze and to draw the gas yield curve trip temperature of going forward side by side and proofread and correct; (4) data through temperature correction are handled, drawn the hydrocarbon-generating dynamics parameter.
In above-mentioned a kind of high pressure thermal simulation experimental method, the assay method of step (1) is: (A) pressure is set at 50MP, with the autoclave of routine to the standard model experiment that heats up, kettle all is positioned at the heating furnace chamber, draws the relation curve H of the methane production of experimental temperature and crude oil pyrolysis generation; (B) pressure is set at 200MP, utilize the described autoclave of claim 1 to experimentize with same heating rate, and make kettle be positioned at the heating furnace chamber, and thread seal partly is positioned at outside the heating furnace body, draw the relation curve worker of the methane production of experimental temperature and crude oil pyrolysis generation; (C) each temperature spot with curve I correspondence progressively reduces by 1 ℃, overlaps substantially with curve I until curve H, and the temperature that this moment, curve I reduced is a Tc.
The present invention compared with prior art has following advantage:
(1) because the outside a series of annular groove of autoclave makes the heat of bottom be restricted to the process of top conduction; Can guarantee the sealing effectiveness of screw thread, prevent from high temperature, High-Voltage Experimentation to take place to reveal and cause the failure of an experiment.
(2) simultaneously, because ceramic rod is the poor conductor of heat, and because the gap is little between the internal diameter of ceramic rod external diameter and tubular cavity, blocked the passage that the highly pressurised liquid in the autoclave tubular cavity conducts heat to top, make that the temperature difference between gold pipe A and the gold pipe C is very little, thereby three gold pipe A, B, C having guaranteed to contain sample can both be subjected to the heating of basic uniformity.
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 the specific embodiment of the invention;
Fig. 2 is user mode figure of the present invention;
Fig. 3 is the traditional experiment view;
Fig. 4 is an experimental state synoptic diagram of the present invention;
Fig. 5 is the graph of relation of the methane production that two kinds of experimental techniques of standard model generate among the present invention;
Fig. 6 is the graph of relation after the methane production correction that two kinds of experimental techniques of standard model generate among the present invention.
Embodiment
Consult shown in Figure 1ly, the autoclave that is used for high pressure thermal simulation experiment of the present invention comprises kettle 1, seal cones 2, cone pressure cap 3, feed tube 4 and pipe pressure cap 5, is provided with unidirectional unlimited tubular cavity 11 in kettle 1; The tapered portion of described seal cones 2 is arranged on the open side of tubular cavity 11, the peristome crimping sealing of the cone pressure cap 3 of seal cones 2 by being arranged on seal cones 2 peripheries and tubular cavity 11, and cone pressure cap 3 is threaded with kettle 1; Feed tube 4 passes seal cones 2 and is communicated with tubular cavity 11, fixing by the pipe pressure cap 5 that is connected seal cones 2 rear portions, between seal cones 2 and pipe pressure cap 5, be provided with cydariform sealing ring 6, screw pipe pressure cap 5, cydariform sealing ring 6 compressive deformations are inwardly shunk, banding feed tube (stainless-steel tube) 4, and the sealing between assurance feed tube 4 and the seal cones 2; Be provided with multiple tracks annular groove 12 at kettle 1 outside surface, annular groove 12 makes the heat of bottom be restricted to the process of top conduction along the circumferential connection of kettle 1; In tubular cavity 11, be placed with two sections ceramic rods 7, the external diameter of this ceramic rod 7 is than the little 0.5mm of internal diameter of tubular cavity 11, because ceramic rod 7 is poor conductors of heat, and the gap of the external diameter of ceramic rod 7 and tubular cavity 11 is little, blocked the passage of the High-Pressure Water of tubular cavity 11 to the top heat transfer, make that the temperature difference in the tubular cavity 11 is very little, thereby guaranteed a plurality of heating that sample gold pipe can both be subjected to basic uniformity that contain.
High pressure thermal simulation experimental method of the present invention is as follows:
(1) at first determine Tc, concrete grammar is as follows:
(A) pressure is set at 50MP, with conventional autoclave standard model is carried out High Temperature High Pressure pyrolysis experiment, the synoptic diagram of experimental provision is seen shown in Figure 3, with kettle 1 ' all the be positioned at furnace chamber of heating furnace 10; The present invention adopts the crude oil in the ancient area of oil field, Tarim Basin, Xinjiang wheel as standard model, carry out 2 ℃/time the intensification experiment, draw the relation curve of experimental temperature and the methane production of crude oil pyrolysis generation after experiment finishes, see the curve H (solid line) among Fig. 5.
(B) pressure is set at 200MP, utilize autoclave of the present invention to carry out above-mentioned experiment, three gold pipe A, B, the C that will contain sample are placed in the tubular cavity 11 of kettle 1 successively, place two sections ceramic rods 7 then on top, screw cone pressure cap 3 and make the peristome sealing of seal cones 2, screw pipe pressure cap 5 then, cydariform sealing ring 6 compressive deformations are inwardly shunk tubular cavity 11, banding feed tube 4, and the sealing between assurance feed tube 4 and the seal cones 2; Fig. 2 and shown in Figure 4 is seen in the signal of experimental provision, kettle 1 is positioned at the furnace chamber of heating furnace 10, but thread seal is positioned at partly outside the body of heater of heating furnace 10; Draw the relation curve (gold pipe A) of the methane production of experimental temperature and crude oil pyrolysis generation after experiment finishes equally, see the curve I (dotted line) among Fig. 5.
(C) each temperature spot with curve I correspondence progressively reduces by 1 ℃, 2 ℃ ..., be about to curve I and progressively hold level with both hands left and move, overlap substantially with curve I until curve H, see shown in Fig. 6; This moment, the temperature of curve I translation was a Tc; The result shows, for 2 ℃/time the intensification experiment, Tc is 3 ℃.
Equally, gold pipe B, C are taken turns doing above-mentioned demarcation, the result shows, for 2 ℃/time the intensification experiment, the temperature difference of gold pipe A and gold pipe C can satisfy the requirement of experiment of most of sample less than 2 ℃.For the demanding sample of temperature accuracy, can golden temperature of managing A be benchmark, the temperature of order gold pipe B, C is hanged down 1 ℃, 2 ℃ than the temperature of gold pipe A respectively.
With temperature calibration being carried out in the experiment of different heating rates, draw the Tc under the condition of 20 ℃ heating rate with quadrat method.The result shows, for 20 ℃/time the intensification experiment, Tc is 5 ℃.
Measure 20 ℃ and 2 ℃/time heating rate Tc after, can carry out the following experiment of thermal simulation to sample according to the experiment flow of the autoclave of routine.
(2) will be packaged with the tubular cavity 11 that three of sample gold pipe A, B, C put into the described kettle 1 of the application successively, put into two ceramic rods 7 then, screw cone pressure cap 3 and pipe pressure cap 5, and make kettle 1 be positioned at the furnace chamber of heating furnace 10, thread seal partly is positioned at outside the body of heater of heating furnace 10, in kettle 1, inject water under high pressure with high-pressure pump, respectively with 2 ℃/time and 20 ℃/time life temperature speed begin heating experiment.
(3) after heating finishes, take out the gold pipe successively, analyze and draw the gas yield curve trip temperature of going forward side by side and proofread and correct.
(4) data through temperature correction are handled, drawn the hydrocarbon-generating dynamics parameter.
Claims (6)
1. an autoclave that is used for the high pressure thermal simulation experiment comprises kettle (1), seal cones (2), cone pressure cap (3), feed tube (4) and pipe pressure cap (5), is provided with unidirectional unlimited tubular cavity (11) in the described kettle (1); The tapered portion of described seal cones (2) is arranged on the open side of tubular cavity (11), seal cones (2) is by being arranged on the peristome crimping sealing of peripheral cone pressure cap (3) of seal cones (2) and tubular cavity (11), and cone pressure cap (3) is threaded with kettle (1); Described feed tube (4) passes seal cones (2) and is communicated with tubular cavity (11), fixing by the pipe pressure cap (5) that is connected seal cones (2) rear portion, between seal cones (2) and pipe pressure cap (5), be provided with cydariform sealing ring (6), it is characterized in that, described kettle (1) outside surface is provided with multiple tracks annular groove (12), be placed with at least one section ceramic rod (7) in tubular cavity (11), the external diameter of this ceramic rod (7) is slightly less than the internal diameter of tubular cavity (11).
2. a kind of autoclave that is used for the high pressure thermal simulation experiment according to claim 1 is characterized in that described annular groove (12) is along the circumferential connection of kettle (1).
3. a kind of autoclave that is used for the high pressure thermal simulation experiment according to claim 1 is characterized in that the external diameter of described ceramic rod (7) is than the little 0.5mm of internal diameter of tubular cavity (11).
4. a high pressure thermal simulation experimental method is characterized in that comprising the steps: that (1) utilizes standard model to measure the Tc of different heating rates; (2) three gold that will be packaged with sample are managed the tubular cavity that (A, B, C) puts into the described kettle of claim 1 successively, put into two ceramic rods then, screw cone pressure cap and pipe pressure cap, and make kettle be positioned at the heating furnace chamber, make thread seal partly be positioned at outside the heating furnace body, in kettle, inject water under high pressure with high-pressure pump, begin the heating experiment according to a conventional method with the heating rate of setting; (3) analyze and to draw the gas yield curve trip temperature of going forward side by side and proofread and correct; (4) data through temperature correction are handled, drawn the hydrocarbon-generating dynamics parameter.
5. method according to claim 4, the assay method that it is characterized in that step (1) is: (A) pressure is set at 50MP, with the autoclave of routine to the standard model experiment that heats up, kettle all is positioned at the heating furnace chamber, draws the relation curve H of the methane production of experimental temperature and crude oil pyrolysis generation; (2) pressure is set at 200MP, utilize the described autoclave of claim 1 to experimentize with same heating rate, and make kettle be positioned at the heating furnace chamber, and thread seal partly is positioned at outside the heating furnace body, draw the relation curve I of the methane production of experimental temperature and crude oil pyrolysis generation; (3) each temperature spot with curve I correspondence progressively reduces by 1 ℃, overlaps substantially with curve I until curve H, and the temperature that this moment, curve I reduced is a Tc.
6. according to claim 4 or 5 described methods, it is characterized in that described standard model is the crude oil in the ancient area of wheel, oil field, Tarim Basin, Xinjiang.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2008100263707A CN101231279B (en) | 2008-02-19 | 2008-02-19 | Autoclave for high pressure thermal simulation experiment and high pressure thermal simulation experimental method |
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| CN2008100263707A CN101231279B (en) | 2008-02-19 | 2008-02-19 | Autoclave for high pressure thermal simulation experiment and high pressure thermal simulation experimental method |
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| CN101231279A true CN101231279A (en) | 2008-07-30 |
| CN101231279B CN101231279B (en) | 2011-10-05 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102434667A (en) * | 2011-09-06 | 2012-05-02 | 重庆红江机械有限责任公司 | High-pressure test sealing device for fuel pump body local pressure test |
| CN103257217A (en) * | 2013-04-11 | 2013-08-21 | 王思波 | Special sample kettle for superhigh pressure gas adsorption-desorption analyzer |
| CN108181138A (en) * | 2017-12-29 | 2018-06-19 | 中国科学院广州地球化学研究所 | Hydrocarbon primary rock producing hydrocarbon thermal simulation reaction kettle collector |
| CN112509632A (en) * | 2020-12-04 | 2021-03-16 | 中国石油大学(华东) | Multistage micron displacement vertical adjusting device used in high-pressure kettle |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1057159C (en) * | 1993-12-01 | 2000-10-04 | 石油大学(北京) | Complex resistance measuring system for rock sample on condition of simulating high temp. and pressure in strata |
| CN2399726Y (en) * | 1999-10-28 | 2000-10-04 | 沈阳科精石油仪器设备有限公司 | Oil well high temp and high pressure dynamic testing pot |
| JP2004025028A (en) * | 2002-06-25 | 2004-01-29 | Mitsubishi Materials Corp | Reaction treatment apparatus under atmosphere of high temperature and high pressure water |
| FR2856797B1 (en) * | 2003-06-26 | 2005-09-30 | Vinci Technologies | DEVICE AND METHOD FOR THERMODYNAMIC MEASUREMENTS ON PETROLEUM FLUIDS |
| CN100457855C (en) * | 2007-02-28 | 2009-02-04 | 中国科学院广州地球化学研究所 | Pressing open type cracking hydrocarbon simulating device |
| CN201295606Y (en) * | 2008-11-24 | 2009-08-26 | 中国科学院广州地球化学研究所 | A high-pressure autoclave for high pressure simulated experiment |
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2008
- 2008-02-19 CN CN2008100263707A patent/CN101231279B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102434667A (en) * | 2011-09-06 | 2012-05-02 | 重庆红江机械有限责任公司 | High-pressure test sealing device for fuel pump body local pressure test |
| CN102434667B (en) * | 2011-09-06 | 2014-04-09 | 重庆红江机械有限责任公司 | High-pressure test sealing device for fuel pump body local pressure test |
| CN103257217A (en) * | 2013-04-11 | 2013-08-21 | 王思波 | Special sample kettle for superhigh pressure gas adsorption-desorption analyzer |
| CN103257217B (en) * | 2013-04-11 | 2015-09-30 | 王思波 | A kind of extra-high adsorption-desorption analyser Special sample still |
| CN108181138A (en) * | 2017-12-29 | 2018-06-19 | 中国科学院广州地球化学研究所 | Hydrocarbon primary rock producing hydrocarbon thermal simulation reaction kettle collector |
| 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 |
| CN112509632A (en) * | 2020-12-04 | 2021-03-16 | 中国石油大学(华东) | Multistage micron displacement vertical adjusting device used in high-pressure kettle |
| CN112509632B (en) * | 2020-12-04 | 2022-02-22 | 中国石油大学(华东) | Multistage micron displacement vertical adjusting device used in high-pressure kettle |
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| CN101231279B (en) | 2011-10-05 |
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