CN110715887A - Bituminous sand porosity determination device and method - Google Patents

Bituminous sand porosity determination device and method Download PDF

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CN110715887A
CN110715887A CN201810763149.3A CN201810763149A CN110715887A CN 110715887 A CN110715887 A CN 110715887A CN 201810763149 A CN201810763149 A CN 201810763149A CN 110715887 A CN110715887 A CN 110715887A
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sample
mold
pressurizing
porosity
sample preparation
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CN110715887B (en
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范明
俞凌杰
刘友祥
芮晓庆
陈红宇
鲍芳
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Sinopec Exploration and Production Research Institute
China Petrochemical Corp
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Sinopec Exploration and Production Research Institute
China Petrochemical Corp
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/088Investigating volume, surface area, size or distribution of pores; Porosimetry

Abstract

The invention provides a device and a method for measuring the porosity of bituminous sand, wherein the device comprises: the device comprises a sample mold, a sample preparation mold, a pressurizing and fixing box, two plugs, a pressurizing system and an oil washing instrument, wherein the sample mold is accommodated in the sample preparation mold, the sample preparation mold is accommodated and fixed in the pressurizing and fixing box, the plugs are used for plugging two ends of the sample mold filled with asphalt sand sample particles, an opening is formed in one end of the pressurizing and fixing box, a pressurizing end of the pressurizing system extends into the opening and applies mechanical force to one of the plugs, and the oil washing instrument is used for washing oil to the pressurized asphalt sand sample particles. The invention can accurately obtain the total volume after the bituminous sand (rock) is injection-molded under the formation pressure, can wash oil in batches based on the action of the sample mold, ensures no particle loss, and can obtain the accurate framework volume, thereby providing accurate porosity data, and having high precision and high efficiency.

Description

Bituminous sand porosity determination device and method
Technical Field
The invention belongs to the field of oil-gas exploration, and particularly relates to a device and a method for measuring the porosity of bituminous sand (also applicable to bituminous rock).
Background
Rock porosity refers to the percentage of the pore volume in the total volume of the rock sample, and if any two of the three parameters of the total volume of the rock, the pore volume and the skeleton volume can be measured, the porosity can be calculated.
For rocks with good cementation degree, the porosity can be conveniently obtained by the following main methods: three methods, namely a measurement method, a liquid method and a gas method, are adopted, but loose samples like bituminous sands (rocks) are difficult to obtain the porosity. Bituminous sands (rocks) refer to sands (rocks) formed by the cementation of asphalt-filled pores, the porosity of which is one of the key parameters used to calculate the bitumen reserves. To obtain the porosity parameter, the asphalt in the rock sample must be washed away by an organic solvent, but after the asphalt is washed away, the rock sample becomes loose sand and does not meet the porosity test condition.
At present, the plunger sample of the bituminous sand (rock) is generally obtained by adopting freezing coring, the total volume is calculated according to the length and the diameter, but the sample with a smooth end face is difficult to cut out due to poor consolidation degree of the bituminous sand, so that the total volume error is large, and the porosity has serious deviation. In addition, loose sand after oil washing is easily lost when being transferred to a sample cup, and further contributes to porosity error.
The porosity determination method for loose materials like bituminous sands (rocks) mainly comprises the following steps: microscopic imaging (e.g., patent 201210364652.4) and nuclear magnetic resonance (e.g., patent 201610243039.5). Microscopic imaging methods are limited by image resolution, with large samples resulting in low resolution and small samples resulting in poor representativeness. Although the nuclear magnetic resonance method can obtain the porosity and the oil saturation in one step, the nuclear magnetic resonance method does not directly measure the porosity and the oil saturation, and needs to be converted by an empirical formula, so that a large error still exists.
Therefore, the following two requirements need to be met for solving the problem of accurate testing of the porosity of the bituminous sand (rock):
(1) accurately acquiring the total volume of the bituminous sand (rock);
(2) the oil washing is convenient, and the rock sample after oil washing can be transferred without damage, and the volume of the particle framework can be conveniently tested.
In view of this, the inventor of the present application provides a device and a method for measuring the porosity of tar sand, so as to solve the problem of accurately measuring the porosity of tar sand (rock) with poor cementation degree, and improve the efficiency and the accuracy by optimizing the sample preparation and oil washing steps.
Disclosure of Invention
The invention aims to provide a device and a method for measuring the porosity of bituminous sand (also suitable for bituminous rock) so as to solve the problem of accurately measuring the porosity of bituminous sand (rock) with poor cementation degree and improve the efficiency and the precision by optimizing sample preparation and oil washing steps.
In order to achieve the above object, the present invention provides an apparatus for measuring the porosity of tar sand, comprising: the device comprises a sample mold, a sample preparation mold, a pressurizing and fixing box, two plugs, a pressurizing system and an oil washing instrument, wherein the sample mold is accommodated in the sample preparation mold, the sample preparation mold is accommodated and fixed in the pressurizing and fixing box, the plugs are used for plugging two ends of the sample mold filled with asphalt sand sample particles, an opening is formed in one end of the pressurizing and fixing box, a pressurizing end of the pressurizing system extends into the opening and applies mechanical force to one of the plugs, and the oil washing instrument is used for washing oil to the pressurized asphalt sand sample particles.
The bituminous sand porosity apparatus comprises a sample mold, wherein the sample mold comprises a cylinder and two end covers which are respectively installed at two ends of the cylinder in a matching manner, and an opening is arranged in the center of each end cover.
The bitumen sand porosity measuring device is characterized in that external threads are arranged at two ends of the cylinder, matched internal threads are arranged on the inner side of each end cover, and the two end covers are in threaded connection with the cylinder respectively.
The asphalt sand porosity measuring device is characterized in that the outer surface of the cylinder is engraved with a number for identification.
The asphalt sand porosity measuring device is characterized in that the sample preparation mold is dumbbell-shaped, a hollow cylindrical inner groove is formed in the sample preparation mold along the extending direction of the sample preparation mold, and the diameter of the cylindrical inner groove is equal to the outer diameter of a cylinder of the sample mold.
The asphalt sand porosity measuring device is characterized in that the pressurizing fixing box is a rectangular box body and is provided with a dumbbell-shaped inner groove which is completely matched with the outside of the sample preparation mould.
The asphalt sand porosity measuring device is characterized in that a metal screen and filter paper are sequentially arranged between the end covers at two ends of the sample mold and the sample when oil washing is carried out.
The asphalt sand porosity measuring device is characterized in that the sample module, the sample preparation module and the pressurizing fixing box are all made of stainless steel.
The invention also provides a determination method implemented by adopting the asphalt sand porosity determination device, which comprises the following steps:
firstly, removing end covers at two ends of a sample mould and placing the end covers in a sample preparation mould, filling the sample mould with crushed asphalt sand sample particles, and respectively placing plugs at two ends of the sample mould;
secondly, applying mechanical force to one plug close to the pressurizing end of the pressurizing system by the pressurizing end of the pressurizing system, wherein the other plug extends out of the sample preparation mould and abuts against the other end, far away from the pressurizing system, of the inside of the pressurizing fixing box;
thirdly, releasing pressure after maintaining constant pressure for a preset time, ejecting a sample die, cutting off redundant samples at two ends of the sample die until the end faces are flat, firstly padding filter paper on the end faces of the samples, then installing a metal screen, screwing an end cover, and then putting the samples into an oil washing instrument for washing oil by using an organic solvent;
fourthly, after the oil washing is finished, all samples are taken outAfter the organic solvent is volatilized, taking out the sample mold with the sample particles inside for skeleton volume determination, and determining the porosity
Figure BDA0001728361830000031
And (3) calculating:
wherein the total volume of the sample mold, the metal screen and the filter paper is V0
The internal volume of the sample mold, i.e. the total volume of the bituminous sand (rock), is V1
The volume of the particle skeleton is as follows: v2-V0
In the fourth step, the total volume of the sample mold, the metal screen and the filter paper is measured by using a gas method, and the particle skeleton volume and the total volume of the sample mold, the metal screen and the filter paper are measured by using a gas method.
In conclusion, the beneficial effects of the invention are as follows: the method mainly solves the problem of accurate determination of the porosity of the bituminous sand (rock) with poor cementation degree, and improves the efficiency and the precision through the optimization of sample preparation and oil washing steps. The sample preparation device comprises a sample mold, a sample preparation mold and a pressurizing fixing box, the total volume can be accurately obtained after the bituminous sand (rock) is subjected to injection molding under the formation pressure, oil can be washed in batches based on the effect of the sample mold, no particle loss is guaranteed, the accurate framework volume can be obtained, accurate porosity data can be provided, and the sample preparation device is high in precision and efficiency.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 is a schematic view of the construction of a tar sand porosity measuring apparatus according to the present invention;
fig. 2 is an exploded schematic view of a sample mold.
In the drawings, like parts are provided with like reference numerals. The drawings are not to scale.
Detailed Description
The invention will be further explained with reference to the drawings.
As shown in fig. 1 and 2, which are a schematic structural diagram of a tar sand porosity measuring apparatus according to the present invention and an exploded schematic diagram of a sample mold, respectively. The invention provides a device for measuring the porosity of bituminous sand (also applicable to asphaltite), which mainly comprises: the sample mold 1, the sample preparation mold 2, the pressurizing and fixing box 3, the two plugs 4, the pressurizing system 5 and the oil washing instrument (not shown in the figure).
Wherein the sample mold 1 comprises: a cylinder 11 and two end covers 12 respectively matched and installed at two ends of the cylinder 11. Specifically, both ends of the cylinder 11 are provided with external threads, the inner side of each end cover 12 is provided with matched internal threads, and the two end covers 12 can be respectively in threaded connection with the cylinder 11. The outer surface of the cylinder 11 may be engraved with a number for identification. In addition, each end cap 12 is provided with an opening 121 at the center thereof, so that when filling and pressurizing the crushed sample particles of tar sands (rocks), a part of the sample particles of tar sands (rocks) outside the sample mold 1 can be squeezed into the sample mold 1, and the sample in the sample mold 1 is compacted. Preferably, the sample module 1 can be made of stainless steel. The plugs 4 are used for plugging two ends of the sample mould 1 filled with the asphalt sand (rock) sample particles, and the plugs 4 can also be made of stainless steel,
the sample preparation mold 2 is used for accommodating the sample mold 1. Specifically, the sample preparation mold 2 is dumbbell-shaped, and has a structure with large outer diameters at two ends and a small outer diameter in the middle. The sampling mold 2 has a hollow cylindrical inner groove 21 along its extending direction, and the diameter of the cylindrical inner groove 21 is equal to the outer diameter of the cylinder 11 of the sample mold 1 so that the sample mold 1 can be placed in the sampling mold 2. Preferably, the sample preparation module 2 can also be made of stainless steel.
The pressure fixing box 3 is used for accommodating the sample preparation mold 2 and can fix the sample preparation mold therein. Specifically, the pressurizing fixing box 3 is a rectangular box body, and it has a dumbbell-shaped inner groove 31 completely matching with the outside of the sample-making mold 2, so that when the sample-making mold 2 is loaded into the pressurizing fixing box 3, the sample-making mold 2 can be clamped, preventing the sample-making mold 2 from moving. Preferably, the pressing and fixing box 3 can also be made of stainless steel.
An opening is provided at one of the ends of the pressure fixation capsule 3 for allowing a pressure end of a pressure system 5 (not shown in detail) to extend from the opening and apply a mechanical force to one of the plugs 4.
The working principle of the invention is as follows: the end covers 12 at two ends of the sample mould 1 are detached and placed in the sample preparation mould 2, the sample mould 1 is filled with crushed bituminous sand (rock) sample particles, and the two ends of the sample mould 1 are respectively provided with a plug 4. It should be noted that some of the escaping sample particles 6 may remain between the sample mold 1 and the stopper 4. The pressurizing end of the pressurizing system 5 applies mechanical force to one plug 4 facing the pressurizing system, and the other plug 4 extends out of the sample preparation mold 2 and abuts against the other end, far away from the pressurizing system 5, in the pressurizing fixing box 3. The applied mechanical force is set according to the depth of the formation, the depth of the formation is proportional to the applied mechanical force (for example, when the tar sand (rock) sample is taken 1000 meters under the formation, a pressure of about 15MPa is applied to the tar sand (rock) sample), the pressure is released after maintaining a constant pressure for a predetermined time (for example, 20 minutes to 60 minutes), the sample mold 1 is ejected, the excess sample at both ends of the sample mold 2 is cut off until the end face is flat, filter paper is first laid on the end face of the sample, then a metal screen (preferably a stainless steel screen) is installed, the end cap 12 is screwed on, and then the sample mold is put into an oil washing instrument (not shown in the figure) to be washed with an organic.
After making a plurality of samples, with the help of the serial number sign on sample mould drum surface, can carry out sample oil washing in batches, after waiting to wash oil, take out whole samples, treat that organic solvent volatilizees the back, take out the sample mould that inside was equipped with the sample granule and carry out skeleton volume survey, specifically do:
the total volume of the sample mold, the metal screen and the filter paper is measured to be V by adopting a gas method0The internal volume of the sample mold 1, i.e. the total volume V of the tar sand (rock)1After washing the oil, the particle skeleton volume and V were determined by gas method0Volume V including volume2The volume of the particle skeleton is as follows: v2-V0Then porosity is increased
Figure BDA0001728361830000052
The invention also provides a method for measuring the porosity of the bituminous sand (also applicable to the asphaltite), which mainly comprises the following steps:
firstly, detaching end covers 12 at two ends of a sample mould and placing the end covers in a sample preparation mould 1, filling the sample mould with crushed bituminous sand (rock) sample particles and respectively placing a plug at two ends of the sample mould 1;
secondly, applying mechanical force to one plug 4 close to the pressurizing end of the pressurizing system 5 by the pressurizing end of the pressurizing system 5, wherein the other plug 4 extends out of the sample preparation mould 2 and is propped against the other end, far away from the pressurizing system 5, in the pressurizing fixing box 3;
the applied mechanical force is set according to the depth of the formation, which is proportional to the applied mechanical force (e.g., about 15MPa of pressure is applied to the tar sands sample when it is taken 1000 meters below the formation);
thirdly, releasing pressure after maintaining constant pressure for a period of time, ejecting the sample mold 1, cutting off redundant samples at two ends of the sample mold 2 until the end faces are flat, firstly padding filter paper on the end faces of the samples, then installing a metal screen, screwing an end cover 12, and then putting the samples into an oil washing instrument (not shown in the figure) for washing oil by using an organic solvent;
after a plurality of samples are manufactured, the serial number marks on the surface of the sample mould cylinder can be used for washing oil for the samples in batches;
fourthly, after the oil washing is finished, all samples are taken out, and after the organic solvent is volatilized, the sample mold with the sample particles inside is taken out to measure the volume of the framework, which specifically comprises the following steps:
the total volume of the sample mold, the metal screen and the filter paper is measured to be V by adopting a gas method0Internal volume of sample mold 1, i.e. total volume of tar sand (rock)V1After washing the oil, the particle skeleton volume and V were determined by gas method0Volume V including volume2The volume of the particle skeleton is as follows: v2-V0Then porosity is increased
Figure BDA0001728361830000062
Examples
The sample mould is stainless steel's drum, and external diameter phi 25mm, internal diameter phi 20mm, height 25mm, both ends are M3 external screw thread, and the drum surface is carved with the number that is used for the sign, and the drum is furnished with circular lid, and external diameter phi 25mm, height are 5mm, and processing M3 internal thread has diameter phi 18mm round hole in the middle of the lid processing for organic solvent circulation leaching when washing oil.
The sample preparation mould is made of stainless steel and is a long strip-shaped cylinder, the length of the sample preparation mould is 100mm, the two ends of the outer diameter are thick (phi 80mm), the middle part is thin (phi 50mm), and the inner diameter is consistent (phi 25 mm).
The length of the pressurizing fixing box is 300mm, the inner width of the pressurizing fixing box is consistent with the outer diameters of two ends of the sample preparation mold, two separating blocks are arranged in the middle of the pressurizing fixing box, the height of the pressurizing fixing box is about 15mm, and the pressurizing fixing box is used for clamping the sample preparation mold.
Molding and oil washing:
removing covers at two ends of a sample mould, filling the sample mould into a sample preparation mould, filling crushed sample particles of the bituminous sand (rock) into the sample preparation mould until the sample is full, plugging a stainless steel plunger plug, putting the sample into a pressurizing fixing box, setting applied mechanical force according to the depth of a stratum, maintaining constant pressure for a period of time, releasing pressure, ejecting the sample mould, cutting redundant samples at two ends of the sample until the end surfaces are flat, padding filter paper and a metal screen, screwing the covers, and putting the sample mould into an oil washing instrument for oil washing. After a plurality of samples are manufactured, the serial number marks on the surface of the cylinder of the sample mold are used for washing oil for the samples in batches, after the oil washing is finished, the samples are taken out and are completely dissolved out by the organic solvent, and the sample mold with the sample particles in the samples is taken out for measuring the volume of the framework.
And (3) porosity determination:
measuring the solid volume V of the sample mold, the metal screen and the filter paper by adopting a gas method0Internal volume of mould, sample mould, i.e. total volume V of bituminous sand (rock)1After oil washing, the volume V2 including the volume of the particle skeleton and the volume V0 is measured by a gas method, wherein the volume of the particle skeleton is as follows: v2-V0Then porosity is increased
Figure BDA0001728361830000063
In conclusion, the beneficial effects of the invention are as follows: the method mainly solves the problem of accurate determination of the porosity of the bituminous sand (rock) with poor cementation degree, and improves the efficiency and the precision through the optimization of sample preparation and oil washing steps. The sample preparation device comprises a sample mold, a sample preparation mold and a pressurizing fixing box, the total volume can be accurately obtained after the bituminous sand (rock) is subjected to injection molding under the formation pressure, oil can be washed in batches based on the effect of the sample mold, no particle loss is guaranteed, the accurate framework volume can be obtained, accurate porosity data can be provided, and the sample preparation device is high in precision and efficiency.
While the invention has been described with reference to a preferred embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the technical features mentioned in the embodiments can be combined in any way as long as there is no structural conflict. It is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (10)

1. A tar sand porosity measurement device, comprising: the device comprises a sample mold, a sample preparation mold, a pressurizing and fixing box, two plugs, a pressurizing system and an oil washing instrument, wherein the sample mold is accommodated in the sample preparation mold, the sample preparation mold is accommodated and fixed in the pressurizing and fixing box, the plugs are used for plugging two ends of the sample mold filled with asphalt sand sample particles, an opening is formed in one end of the pressurizing and fixing box, a pressurizing end of the pressurizing system extends into the opening and applies mechanical force to one of the plugs, and the oil washing instrument is used for washing oil to the pressurized asphalt sand sample particles.
2. The apparatus for measuring porosity of tar sand as claimed in claim 1, wherein the sample mold comprises a cylinder and two end caps respectively fitted to both ends of the cylinder, each end cap having an opening at its center.
3. The tar sand porosity measuring device as claimed in claim 2, wherein both ends of the cylinder are provided with external threads, the inner side of each end cap is provided with a matching internal thread, and the two end caps are respectively in threaded connection with the cylinder.
4. The tar sand porosity determination apparatus of claim 2, wherein the outer surface of the cylinder is engraved with a number for identification.
5. The tar sand porosity measuring apparatus according to claim 2, wherein the sample preparation mold has a dumbbell shape, and the sample preparation mold has a hollow cylindrical inner groove along an extending direction thereof, and a diameter of the cylindrical inner groove is equal to an outer diameter of a cylinder of the sample mold.
6. The tar sand porosity measurement device according to claim 1, wherein the pressurizing and fixing case is a rectangular case and has a dumbbell-shaped inner groove that completely matches the outside of the sample preparation mold.
7. The tar sand porosity measuring device according to claim 2, wherein a metal screen and a filter paper are sequentially disposed between the sample and the end caps at both ends of the sample mold during oil washing.
8. The tar sand porosity determination apparatus of claim 2, wherein the sample module, the sample preparation module, and the pressurizing and fixing box are made of stainless steel.
9. A measuring method implemented by using the tar sand porosity measuring apparatus according to any one of claims 1 to 8, comprising the steps of:
firstly, removing end covers at two ends of a sample mould and placing the end covers in a sample preparation mould, filling the sample mould with crushed asphalt sand sample particles, and respectively placing plugs at two ends of the sample mould;
secondly, applying mechanical force to one plug close to the pressurizing end of the pressurizing system by the pressurizing end of the pressurizing system, wherein the other plug extends out of the sample preparation mould and abuts against the other end, far away from the pressurizing system, of the inside of the pressurizing fixing box;
thirdly, releasing pressure after maintaining constant pressure for a preset time, ejecting a sample die, cutting off redundant samples at two ends of the sample die until the end faces are flat, firstly padding filter paper on the end faces of the samples, then installing a metal screen, screwing an end cover, and then putting the samples into an oil washing instrument for washing oil by using an organic solvent;
fourthly, after the oil washing is finished, all samples are taken out, after the organic solvent is volatilized, the sample mold with the sample particles inside is taken out for the determination of the skeleton volume, and the porosity is measured
Figure FDA0001728361820000021
And (3) calculating:
Figure FDA0001728361820000022
wherein the total volume of the sample mold, the metal screen and the filter paper is V0
The internal volume of the sample mold, i.e. the total volume of the bituminous sand (rock), is V1
The volume of the particle skeleton is as follows: v2-V0
10. The measuring method according to claim 9, wherein in the fourth step, the total volume of the sample mold, the metal mesh, and the filter paper is measured by a gas method, and the total volume of the sample mold, the metal mesh, and the filter paper is measured by a gas method.
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CN114112861A (en) * 2021-12-21 2022-03-01 广东石油化工学院 Method and device for measuring porosity of ionic rare earth ore

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