CN103234871A - A centrifugal analysis method for oil shale samples - Google Patents

A centrifugal analysis method for oil shale samples Download PDF

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Publication number
CN103234871A
CN103234871A CN2013101236394A CN201310123639A CN103234871A CN 103234871 A CN103234871 A CN 103234871A CN 2013101236394 A CN2013101236394 A CN 2013101236394A CN 201310123639 A CN201310123639 A CN 201310123639A CN 103234871 A CN103234871 A CN 103234871A
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oil
centrifuge
rock sample
cup
centrifuge cup
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CN2013101236394A
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宋卫国
蔡建林
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TAICANG JINXUAN LABORATORY EQUIPMENT Co Ltd
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TAICANG JINXUAN LABORATORY EQUIPMENT Co Ltd
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Abstract

The invention discloses a centrifugal analysis method for oil shale samples, and the method comprises the steps of: 1) a prepared shale sample is placed separately into centrifuge cups, and then the centrifuge cups are mounted on the rotor of a centrifuge chamber; 2) the door of the centrifuge chamber is closed, and a vacuum pump is started to make the inside of the centrifuge chamber vacuum; 3) a variable frequency motor is started, and the speed of the variable frequency motor is set, to make the variable frequency motor drive the centrifuge cups in the centrifuge chamber to rotate; 4) a strobe lamp is turned on, wherein the strobe lamp emits synchronous light when each centrifuge cup rotates just above the strobe lamp; and after the synchronous light emitted from the strobe lamp passes through the light transmitting slot of the centrifuge cup and a liquid collection cup, and after a total reflection through a prism, the synchronous light enters into a camera device to complete liquid level collection of the centrifuge cup; 5) oil - water interface image of each centrifuge cup is recorded, and the volume of oil or water of each centrifugal cup is calculated; and 6) based on the volume of oil or water obtained in step 5), the capillary pressure curve of the shale sample is obtained. The method of the present invention has high efficiency and small errors.

Description

A kind of oil rock sample centrifugal analysis method
Technical field
The invention belongs to oil rock sample analysis technical field, relate to a kind of method of capillary pressure curve of continuous coverage rock sample.
Background technology
Petroleum resources occupy extremely important position in national economy, be the indispensable resource of social development and human survival.Along with the raising of the developing rapidly of industry, Increase of population and living standards of the people, energy shortage has become worldwide problem, and energy security is subjected to the attention of more and more national.
At present, in oil field prospecting and exploitation, particularly when the secondary oil recovery in oil field and tertiary oil recovery, must analyze just the rock sample of sampling theoretical foundation can be provided, and in rock sample was analyzed, one of most important rock sample analysis project was exactly the capillary pressure data of measuring rock sample.When immiscible two-phase fluid contacts with each other in blowhole, between the fluid on the interphase pressure of two side liquids be unequal, its pressure differential just is defined as capillary pressure.
The method that mensuration rock sample capillary pressure curve relies on mainly is: mercury intrusion method, baffle method, centrifuge method.Centrifugal measurement method wherein: after a columned little rock sample cleaned oven dry, vacuumize and make the rock sample saturated brine, weigh and determine the weight of its saturated brine, then the rock sample behind the saturated brine is placed (rock sample box) in the special hydro-extractor box, rock sample immerses in the oil phase.
The rock sample box is under action of centrifugal force, and the water in the rock sample is come out by oily displacement, and the oil of equivalent (equal-volume) enters in the rock sample, presses rotating speed from low to high, measures and record the water yield that the rock sample under each rotating speed is discharged.When improving the rotating speed of hydro-extractor again, till the water yield that rock sample is discharged was constant basically, experimental measurements can obtain the water yield that a series of centrifuge speed and corresponding rock sample thereof are discharged, and just can measure the capillary pressure curve of rock sample by this.
When adopting existing centrifuge method to measure the rock sample capillary pressure curve, must stop hydro-extractor at set intervals after, observe the fluid displacement of discharging from rock sample again.This way not only efficient is lower, and error is bigger.
Summary of the invention
The objective of the invention is at above-mentioned the deficiencies in the prior art, a kind of oil rock sample centrifugal analysis method is provided, this method can be measured the capillary pressure curve of rock sample continuously.For achieving the above object, the technical scheme taked of the present invention is as follows.
A kind of oil rock sample centrifugal analysis method comprises the steps:
1) rock sample for preparing is put into Centrifuge Cup respectively, then Centrifuge Cup is installed in the rotary head in the centrifugal chamber;
2) close centrifugal chamber hatch door, open vacuum pump, make centrifugal chamber inner vacuum;
3) start variable-frequency motor, and set the speed of variable-frequency motor, the Centrifuge Cup that variable-frequency motor is driven in the centrifugal chamber rotates;
4) open stroboscopic lamp, in the time of directly over each Centrifuge Cup rotates to stroboscopic lamp, described stroboscopic lamp sends synchronizable optical, and the synchronizable optical that stroboscopic lamp sends is successively by behind the light tank and liquid collecting cup of Centrifuge Cup, after the prism total reflection, enter camera head, finish the liquid level collection of Centrifuge Cup;
5) record oil-water interface image in each Centrifuge Cup, and calculate the volume of oil in each Centrifuge Cup or water;
6) oil that obtains according to step 5) or the volume of water obtain the capillary pressure curve of rock sample.
Further, also comprise step 7): close variable-frequency motor, opened door after being exitted in centrifugal chamber takes out rock sample, finishes analysis.
Further, after described step 5), reset the speed of variable-frequency motor, repeating said steps 4) and described step 5), data acquisition and the calculating of a plurality of speed finished.
Further, described camera head is the CCD camera.
Further, camera head described in the step 4) is taken the oil-water interface image in each Centrifuge Cup, and is sent to computing machine.
Owing to adopt above technical scheme, the invention has the beneficial effects as follows: use oil rock sample centrifugal analysis method of the present invention can the continuous monitoring Centrifuge Cup in the variation of oil-water interface, calculate the water yield or oil mass that rock sample is discharged, measure the capillary pressure curve of rock sample at this point, this method efficient height, error is little, and the total reflection effect by prism, make camera head can be arranged on horizontal direction, it is more reasonable to arrange, reduce the height of hydro-extractor, avoid camera head vertically to settle problems such as caused hydro-extractor volume is excessive.
Description of drawings
Fig. 1 is process flow diagram of the present invention;
Fig. 2 is a kind of one-piece construction synoptic diagram of analysis centrifugal machine.
Fig. 3 is a kind of rotor structure synoptic diagram of analysis centrifugal machine.
Fig. 4 is a kind of structural representation of oily expelling water Centrifuge Cup.
Fig. 5 is a kind of structural representation of water displacing oil Centrifuge Cup.
Fig. 6 is a kind of light path system synoptic diagram.
Fig. 7 is the process flow diagram of embodiment for the present invention one.
Embodiment
For abundant disclosed purpose, below with reference to drawings and Examples the present invention is described in further details.The specific embodiment that should be appreciated that the following stated only is used for explaining the present invention, is not for limiting protection scope of the present invention.
As shown in Figure 1, the invention provides a kind of oil rock sample centrifugal analysis method, comprise the steps: 1) rock sample preparation and placement: the rock sample for preparing is put into Centrifuge Cup (adding oil or water as required) respectively, then Centrifuge Cup is installed in the rotary head in the centrifugal chamber;
2) vacuum environment is prepared: close centrifugal chamber hatch door, open vacuum pump, make centrifugal chamber inner vacuum;
3) parameter is set and start: start variable-frequency motor, and set the speed of variable-frequency motor, the Centrifuge Cup that variable-frequency motor is driven in the centrifugal chamber rotates;
4) data acquisition: open stroboscopic lamp, in the time of directly over each Centrifuge Cup rotates to stroboscopic lamp, described stroboscopic lamp sends synchronizable optical, the synchronizable optical that stroboscopic lamp sends is successively by behind the light tank and liquid collecting cup of Centrifuge Cup, enter camera head after the prism total reflection, (described camera head preferably adopts the CCD camera.Camera head is taken the oil-water interface image in each Centrifuge Cup, and is sent to computing machine.) finish the liquid level collection of Centrifuge Cup;
5) volume calculates: record the oil-water interface image in each Centrifuge Cup, and calculate the volume of oil in each Centrifuge Cup or water;
6) obtain curve: the oil that obtains according to step 5) or the volume of water obtain the capillary pressure curve of rock sample.
7) finish analysis and shutdown: close variable-frequency motor, opened door after being exitted in centrifugal chamber takes out rock sample, finishes analysis.
Wherein, after described step 5), reset the speed of variable-frequency motor, repeating said steps 4) and described step 5), the image acquisition when finishing a plurality of motor speed obtains multi-group data according to a plurality of speed, and curve plotting.
Oil rock sample centrifugal analysis method provided by the invention can adopt analysis centrifugal machine as shown in Figure 2 to realize that it comprises rotating bearing system, vacuum protection system, light path system, computer automatic measurement and control system and electric control box 18.Described rotating bearing system comprises centrifuge rotor 14, flexible shaft, wheel box 15 and variable-frequency motor, centrifuge rotor 14 comprises that rotary head and several are installed in the Centrifuge Cup on the centrifugal rotor, the two ends of described flexible shaft are connected with the tooth axis hole of described rotary head and wheel box 15 respectively, the power that described variable-frequency motor produces is delivered to described rotary head by described flexible shaft and wheel box 15, drives the rotary head rotation.The overcritical operation of flexible shaft, good stability, noise are little.On the tooth axle of wheel box 15 high-speed ball bearing and damping can be housed, make rotating bearing system that stability preferably be arranged.Described vacuum protection system comprises the centrifugal chamber 13 of sealing and the vacuum pump 17 that vacuumizes for centrifugal chamber 13, and centrifuge rotor 14 is arranged in the centrifugal chamber 13, and the bottom in described centrifugal chamber 13 and top are respectively arranged with bottom photic zone and top photic zone.Described light path system comprises stroboscopic lamp, prism 12 and the camera head 11 that is installed in bottom photic zone (being preferably quartz glass) below, described prism 12 is arranged on photic zone top, top, camera head 11 is equipped with prism, receives the total reflection light of prism.Described computer automatic measurement and control system is connected with camera head 11, the host computer that comprises the DSP that is connected with camera head 11 and realize controlling, and PORT COM is RS232.
Fig. 3 is the rotor structure synoptic diagram of a kind of analysis centrifugal machine of realization method shown in the present, and as shown in Figure 3, centrifuge rotor comprises rotary head 21 and 4 Centrifuge Cups 24 that are installed on the centrifugal rotor.Be symmetrically arranged with 4 mounting holes in the rotary head 21, be installed with Centrifuge Cup 21 in each mounting hole respectively, Centrifuge Cup 21 is provided with liquid level light tank 22.Rotary head 21 and Centrifuge Cup 24 can have titanium alloy material to make, and rotary head 21 and 4 Centrifuge Cup 24 preferred employings are threaded.
The Centrifuge Cup of oil rock sample analysis centrifugal machine provided by the invention can be oily expelling water Centrifuge Cup and/or water displacing oil Centrifuge Cup, oil expelling water Centrifuge Cup as shown in Figure 4, the inside of oil expelling water Centrifuge Cup 35 is provided with liquid collecting cup 32 and rock sample cover 36, liquid collecting cup 32 is arranged on the rear end of Centrifuge Cup 35, liquid level light tank 34 is arranged on liquid collecting cup 32 places, rock sample cover 36 is arranged on the front end of oily expelling water Centrifuge Cup 35, the junction of liquid collecting cup 32 and rock sample cover 36 is provided with O-ring seal 31(and is preferably two, sealing is better), and described liquid collecting cup and described rock sample cover are connected.The water displacing oil Centrifuge Cup as shown in Figure 5, the inside of water displacing oil Centrifuge Cup 43 is provided with liquid collecting cup 41 and rock sample cover 45, liquid collecting cup 41 is arranged on the front end of water displacing oil Centrifuge Cup 43, described liquid level light tank 46 is arranged on liquid collecting cup 41 places, the front end of liquid collecting cup 41 is provided with liquid injection hole 47 and sealing-plug 48, the convenient fluid injection in the liquid collecting cup 41 of liquid injection hole 47 is set, and rock sample cover 45 is arranged on the rear end of water displacing oil Centrifuge Cup 43, and liquid collecting cup 41 and rock sample overlap 45 junction and preferably be provided with two O-ring seals 42.
For realizing oil rock sample centrifugal analysis method of the present invention, the analysis centrifugal facility have preferred light path system as shown in Figure 6, comprise the stroboscopic lamp 57 that is installed in photic zone 58 belows, bottom, be installed in the prism 51 of top photic zone 53 tops and the camera head that is equipped with prism 51, stroboscopic lamp 57 passes through coupling and synchronizing strobelight and rotor rotation synchronously, and tells the rock sample numbering.Shown in arrow indication among Fig. 6, synchronizable optical successively by the top photic zone 53 at the bottom photic zone 58 of bottom, centrifugal chamber 56, the light tank of Centrifuge Cup 55, the liquid collecting cup of Centrifuge Cup 55 inside, centrifugal top of chamber 54 places, by entering the camera head (not shown) after prism 51 total reflections, so just can collect oil-water interface and position thereof.Prism 51 is arranged at the top of hydro-extractor by prism fixed mount 52, and prism fixed mount 52 is provided with printing opacity draw-in groove 59.Bottom photic zone 58 and top photic zone 53 can be quartz glass, length and the plane of incidence length of prism 51 and the equal in length of Centrifuge Cup 55 of bottom photic zone 58 and top photic zone 53, even the position of liquid collecting cup is different in the Centrifuge Cup of water displacing oil and oily expelling water like this, also can satisfy the requirement of taking the oil-water interface position, reach general purpose, and prism the installation that can make things convenient for camera head is set, reduce the height of analysis centrifugal machine, volume is littler, operates easier.
Oil rock sample centrifugal analysis method provided by the invention adopts computer automatic measurement and control system to finish, and is finished with the upper and lower computer form by the DSP that is connected with camera head and a computer, and PORT COM adopts RS232.Computer automatic measurement and control system is achieved as follows function: the one, and the programmed control of start, shutdown and correlated condition; The 2nd, setting and the control of machine operational factors such as the speed of motor speed, stroboscopic and time.
The function that computer software in the computer (host computer) is realized in the present invention mainly contains four aspects: control function, set-up function, parameter setting and computing function.The control function comprises open and close, the start-stop of control vacuum pump, the start-stop of control variable-frequency motor, the control stroboscopic lamp switch of the centrifugal chamber of control door.Set-up function mainly is the rotating speed of setting variable-frequency motor.The parameter setting comprises that the setting of rock sample inner rotary radius, two-phase fluid density difference arrange, saturated resident fluid volume arranges, rock sample length arranges, the capillary diameter setting.Computing function by the volume of image calculation oil or water, is calculated capillary pressure curve automatically, and data is deposited in database.
A kind of oil rock sample centrifugal analysis method of the present invention as shown in Figure 7, concrete steps are as follows:
1. the rock sample of preparation is as requested put into Centrifuge Cup respectively, Centrifuge Cup is installed to the correspondence position of the rotary head in the centrifugal chamber.
2. close centrifugal chamber hatch door, click the vacuum pump key point, vacuum pump is started working and is made centrifugal chamber be in vacuum state.
3. opening the page that arranges of software inserts correlation parameter.
4. according to experimental program the speed of first data point is inserted in the velocity window.
5. click the motor open key, equipment will progressively add to speed the speed of first data point.
6. click and open stroboscopic lamp, when each described Centrifuge Cup rotates to the bottom of bottom, centrifugal chamber by directly over distinguishing and when parallel with the bottom photic zone, described stroboscopic lamp sends synchronizable optical, the synchronizable optical that stroboscopic lamp sends is successively by bottom photic zone, the light tank of Centrifuge Cup, liquid collecting cup, top photic zone, by entering camera head after the prism total reflection.
7. select rock sample successively, this moment is because the effect of high speed stroboscopic lamp, the interface image of the oil-water under this speed in four centrifugal chambeies can appear in the area of image of software successively, place respectively with two cursor lines about mouse drag oil-water interface image about end, click then and preserve, software is automatic volume calculated, and deposits velocity amplitude of itself and this moment in database.In flood pot test, cursor line should place the both bounded sides of oil, calculates and record fuel-displaced volume by software.In oily expelling water experiment, cursor line should place the both bounded sides of water, calculates and record the volume of water outlet by software.Rock sample is measured successively to preserve and is finished, and the first data point measurement is finished.
8. according to experimental program the speed of second data point is inserted in the velocity window.
9. click the motor open key, equipment will progressively add to speed the speed of second data point
10. repeating step 7, finish second data point and measure.
11. repeat step 8-10, finish up to the data acquisition of total data point.
12. click the motor close key, equipment will progressively be decelerated to and stop.
13. click venting.
14. the click opened door takes out rock sample.
15. database can be exported with form, the curve map that also can click in the file is checked the curve map that software generates.
By above-mentioned technological means, oil rock sample centrifugal analysis method of the present invention can the continuous monitoring Centrifuge Cup in the variation of oil-water interface, calculate the water yield or oil mass that rock sample is discharged, measure the capillary pressure curve of rock sample at this point.This method is the efficient height not only, and error is little.
The above embodiment has only expressed embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (5)

1. an oil rock sample centrifugal analysis method is characterized in that, comprises the steps:
1) rock sample for preparing is put into Centrifuge Cup respectively, then Centrifuge Cup is installed in the rotary head in the centrifugal chamber;
2) close centrifugal chamber hatch door, open vacuum pump, make centrifugal chamber inner vacuum;
3) start variable-frequency motor, and set the speed of variable-frequency motor, the Centrifuge Cup that variable-frequency motor is driven in the centrifugal chamber rotates;
4) open stroboscopic lamp, in the time of directly over each Centrifuge Cup rotates to stroboscopic lamp, described stroboscopic lamp sends synchronizable optical, and the synchronizable optical that stroboscopic lamp sends is successively by behind the light tank and liquid collecting cup of Centrifuge Cup, after the prism total reflection, enter camera head, finish the liquid level collection of Centrifuge Cup;
5) record oil-water interface image in each Centrifuge Cup, and calculate the volume of oil in each Centrifuge Cup or water;
6) oil that obtains according to step 5) or the volume of water obtain the capillary pressure curve of rock sample.
2. oil rock sample centrifugal analysis method according to claim 1 is characterized in that, also comprises step 7): close variable-frequency motor, opened door after being exitted in centrifugal chamber takes out rock sample, finishes analysis.
3. oil rock sample centrifugal analysis method according to claim 1 is characterized in that, resets the speed of variable-frequency motor after described step 5), repeating said steps 4) and described step 5), data acquisition and the calculating of a plurality of speed finished.
4. according to claim 1 or 2 or 3 described oil rock sample centrifugal analysis methods, it is characterized in that described camera head is the CCD camera.
5. oil rock sample centrifugal analysis method according to claim 1 is characterized in that camera head described in the step 4) is taken the oil-water interface image in each Centrifuge Cup, and is sent to computing machine.
CN2013101236394A 2013-04-10 2013-04-10 A centrifugal analysis method for oil shale samples Pending CN103234871A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111537695A (en) * 2020-05-07 2020-08-14 苏州闪掣智能科技有限公司 Control method for centrifugal analysis of petroleum rock sample
CN113514607A (en) * 2021-04-26 2021-10-19 东北石油大学 Device and method for evaluating performance of microemulsion for oil displacement

Citations (3)

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Publication number Priority date Publication date Assignee Title
US4657373A (en) * 1984-07-25 1987-04-14 Oce-Nederland B.V. Electrophotographic copying device with means to effect uniform aging of photoconductive element
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CN102615000A (en) * 2011-11-29 2012-08-01 太仓金旋实验设备有限公司 Vacuum centrifugal machine for analyzing oil rock samples

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4657373A (en) * 1984-07-25 1987-04-14 Oce-Nederland B.V. Electrophotographic copying device with means to effect uniform aging of photoconductive element
US4740077A (en) * 1985-06-21 1988-04-26 Atlantic Richfield Company Centrifugal measurement of core samples
CN102615000A (en) * 2011-11-29 2012-08-01 太仓金旋实验设备有限公司 Vacuum centrifugal machine for analyzing oil rock samples

Non-Patent Citations (1)

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Title
付先学等: "离心机测控系统中旋转计量柱图像获取方法的研究", 《测控技术》, vol. 22, no. 12, 18 December 2003 (2003-12-18) *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111537695A (en) * 2020-05-07 2020-08-14 苏州闪掣智能科技有限公司 Control method for centrifugal analysis of petroleum rock sample
CN113514607A (en) * 2021-04-26 2021-10-19 东北石油大学 Device and method for evaluating performance of microemulsion for oil displacement
CN113514607B (en) * 2021-04-26 2023-09-08 东北石油大学 Device and method for evaluating performance of microemulsion for oil displacement

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Application publication date: 20130807