CN113884356A - Method for determining solid asphalt content and distribution characteristics in reservoir based on crude oil cracking - Google Patents
Method for determining solid asphalt content and distribution characteristics in reservoir based on crude oil cracking Download PDFInfo
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Abstract
The invention discloses a method for determining the content and distribution characteristics of solid asphalt in a reservoir based on crude oil cracking. The method comprises the following steps: taking and numbering a plurality of reservoir core samples, drilling 2 plunger samples from each reservoir core sample, and recording the plunger samples as a plunger sample A and a plunger sample B; extracting the plunger sample A and the plunger sample B by using an organic solvent, and drying; preparing a plunger sample A into a casting sheet, and measuring the physical property I of a plunger sample B; placing the plunger sample B in an oil injection system for high-pressure oil injection and saturation, and recording parameters in the oil injection process and after oil injection; placing the plunger sample B in a quartz tube, then placing the quartz tube in a high-pressure kettle for pyrolysis, and measuring the physical property II of the sample subjected to pyrolysis; and preparing the sample subjected to high-temperature cracking into a plurality of casting body slices, observing the asphalt distribution characteristics and quantitatively counting the asphalt content, thereby realizing the solid asphalt content and the distribution characteristics in the reservoir. The invention adopts an experimental simulation method to confirm and test the non-uniform residual characteristics of the solid asphalt in the ancient oil reservoir.
Description
Technical Field
The invention relates to a method for determining the content and distribution characteristics of solid asphalt in a reservoir based on crude oil cracking, and belongs to the field of comprehensive utilization of mineral resources.
Background
Solid bitumen, as a product after crude oil cracking, necessarily remains in the pores of the reservoir and results in a reduction in the porosity and permeability of the previous reservoir, increasing the heterogeneity of the reservoir.
The study by Huc (2000) et al shows that the content of highly evolved pyrobitumen has a negative correlation with total porosity, i.e. small pores are preferentially occupied by bitumen. Li et al (2015), based on systematic studies on the nash group of south-built gas fields, further revealed non-uniform residual characteristics of solid bitumen after crude oil cracking, the residual proportion of bitumen in the pores (bitumen content/(bitumen content + porosity)) being non-uniform, the residual proportion of bitumen in the small pores, or the destruction of the porosity, being greater than the large porosity, making part of the small-pore reservoir ineffective as filled with bitumen. The non-uniform residual phenomenon of the asphalt plays an important role in evaluating reservoirs which take in-situ crude oil pyrolysis gas as a gas source and have a large amount of residual solid asphalt in deep layers of the Sichuan basin and other basins in the world, and the exploration risk can be effectively reduced.
At present, the distribution of solid bitumen in ancient oil reservoirs is known to be non-uniform, but how to confirm the phenomenon of non-uniform distribution through experimental simulation is a difficulty of current research.
Disclosure of Invention
The invention aims to provide a method for determining the content and the distribution characteristics of solid asphalt based on a crude oil cracking experiment.
The method for determining the content and the distribution characteristics of the solid asphalt in the reservoir provided by the invention comprises the following steps:
s1, taking a plurality of reservoir core samples, numbering the reservoir core samples, and drilling 2 plunger samples from each reservoir core sample, wherein the plunger samples are marked as a plunger sample A and a plunger sample B; the number of the selected reservoir core samples can be determined according to actual conditions;
s2, extracting the plunger sample A and the plunger sample B by using an organic solvent, and drying; preparing the plunger sample A into a casting sheet, and measuring the physical property I of the plunger sample B;
s3, placing the plunger sample B in an oil injection system for high-pressure oil injection and saturation, and recording parameters in the oil injection process and after oil injection;
s4, placing the plunger sample B in a quartz tube, placing the quartz tube in an autoclave for pyrolysis, and determining the physical property II of the sample subjected to pyrolysis;
s5, preparing the sample subjected to pyrolysis into a plurality of casting body slices, observing the asphalt distribution characteristics, and quantitatively counting the asphalt content, thereby realizing the solid asphalt content and the distribution characteristics in the reservoir.
In the above method, in step S2, the organic solvent may be a mixture of benzene and ethanol, and the volume ratio of benzene to ethanol is 2-3: 1, removing soluble organic matters in a sample until an extraction solution is colorless and transparent;
and (4) carrying out oil washing and salt washing on the rock core in advance, wherein the oil washing method is carried out according to the regulation of SY/T5336-2006.
In the above method, in step S2, the specifications of the plug sample a and the plug sample B are both: the diameter is 25-30 mm and the length is 25-30 mm.
In the above method, in step S2, property i includes mass, pore volume, porosity and permeability, and the pore volume, porosity and permeability can be determined by using CMS-300 system.
In the method, in step S3, the parameters include the oil injection volume, the oil injection pressure and the sample mass after oil injection, and the oil saturation of the plunger sample B is obtained;
the volume of the injected oil may be recorded using a flow sensor and the pressure of the injected oil may be recorded using a pressure sensor.
In the above method, in step S4, the pyrolysis conditions are as follows:
the confining pressure is 5-10 MPa;
the initial temperature is 25-35 ℃, the heating rate is 20-25 ℃/h, and the temperature is stabilized for 4-6 h after being heated to 600-650 ℃.
The cover of the high-pressure kettle is connected with an air inlet pipeline and an air outlet pipeline, the air inlet pipeline is connected with a high-pressure gas cylinder and a pressure gauge, the air outlet pipeline is connected with a gas storage chamber and an air outlet valve, nitrogen is filled into the high-pressure kettle through the air inlet pipeline to stabilize the ambient pressure of crude oil cracking, the ambient pressure has the function of preventing the crude oil in a rock core from flowing out in the cracking process, and the ambient pressure can be more than 5MPa in the experimental process; after completion of the cracking, the autoclave was cooled and the methane and other gases produced were collected and treated.
In the above method, in step S4, property ii includes weight, porosity, and permeability.
In the method, the sample subjected to pyrolysis is prepared into 1-5 casting body slices for observing asphalt distribution and counting the asphalt content;
observing the distribution characteristics of the asphalt by using a microscope;
and quantitatively counting the asphalt content by adopting Photoshop software.
The core sample injected into a research area of crude oil is subjected to crude oil cracking reaction in an autoclave, and then the reacted sample is made into a casting body slice to observe the distribution characteristics of solid asphalt under a microscope and quantitatively count the asphalt content.
In the method, the crude oil cracking experiment is carried out in the reservoir rock core, so that the cracked product solid asphalt is distributed in the pores of the rock core sample, and the content and the distribution characteristics of the solid asphalt in the rock core sample are further determined.
The invention adopts an experimental simulation method to confirm and test the non-uniform residual characteristics of the solid asphalt in the ancient oil reservoir.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
FIG. 2 is a schematic view of the structure of an autoclave reaction apparatus used in the process of the present invention.
FIG. 3 is a graph of the residual solid bitumen content of samples of injected normal oil and light oil after cracking crude oil in an example of the invention.
FIG. 4 is a comparison of sample porosity before and after cracking of crude oil in an example of the present invention.
FIG. 5 is a comparison of sample permeability before and after cracking of crude oil in an example of the present invention.
FIG. 6 is a slice micrograph of the distribution of residual solid pitch after cracking a dolomite sample crude oil according to an embodiment of the present invention.
The figures are labeled as follows:
1. the device comprises a high-temperature heating furnace, 2, a high-pressure kettle, 3, a quartz tube, 4, an oil-containing plunger sample, 5, a thermometer, 6, a kettle cover, 7, a pressure gauge, 8, a high-pressure gas bottle, 9, a gas storage chamber, 10 and an exhaust valve.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
In the embodiment of the invention, a dolomite sample is taken as an example, crude oil filling and pyrolysis are carried out, and observation and statistics of residual solid asphalt are carried out, wherein the flow is shown in figure 1, and the specific steps are as follows:
first, sample collection and preparation
8 dolomitic samples are collected, and the core sample is cylindrical.
2 Changxing groups from Yuanba gas field (YB123 well, No. 1 and No. 2), 2 Feixian groups from Puguang gas field (Puguan 2 well, No. 3 and No. 4), and 4 Leikou slope groups (No. 5, 6 and 7) from the cross section of the yellow bridgehead of the Sichuan river.
And then drilling 2 plunger samples (with the diameter of 25mm and the length of 25-30 mm) for each sample by using a core drilling machine.
Secondly, extracting the sample and measuring the physical property
8 samples (16 plunger samples) are put into a Soxhlet fat extractor, a mixed solution of benzene and alcohol (the volume ratio of the benzene to the alcohol is 2: 1) is used for extracting the samples, before analysis, oil washing and salt washing are carried out on a rock core, the oil washing method is carried out according to the specification of SY/T5336-2006, and the purpose of extraction is to remove soluble organic matters in the samples.
In order to determine whether the core is completely extracted, the core sample needs to be soaked in water for 48 hours, and if the color of the solvent is not changed, the core sample is completely extracted.
And (3) placing the core sample which is completely extracted at normal temperature to volatilize the solvent, and then placing the sample into a dryer to be dried for 4 hours continuously at the temperature of 120 ℃ after the solvent is volatilized.
One of the columns of the same sample was used to prepare a cast slab in order to again confirm that the sample pores and throat were free of soluble organic matter, and the other column was weighed (m)0) And determination of Pore Volume (PV), porosity with CMS-300 System
And permeability (K1).
Third, filling of crude oil
And (3) putting the sample for measuring the porosity and the permeability into an oil injection system for high-pressure oil injection, wherein the flow sensor can record the volume of the injected oil, and the pressure sensor can record the pressure of the injected oil.
Wherein the samples No. 1, 3 and 7 are injected with normal crude oil (normal crude oil of Changqing oilfield extension group, density is 0.814g/cm3) The oil injection pressure is 2.5 Mpa; 2. samples No. 4, 5, 6 and 8 were injected with light crude oil (light crude oil of the Fujia river group of the Zhongba gas field, density 0.742g/cm3) The oil injection pressure is 1.5 Mpa.
The volume of oil injected (OV) and the mass of the sample after injection (m)1)，
And the saturation (OS) was calculated, and the oil-saturated sample was stored at a low temperature (4 ℃ C.).
Cracking of crude oil
The crude oil-saturated plug sample is loaded into a quartz tube 3 and then into an autoclave 2 for pyrolysis. The autoclave was used in the following manner, and the structure of the autoclave is shown in FIG. 2:
1. the crude oil saturated plug sample is loaded into a quartz tube 3, and then the quartz tube is loaded into an autoclave 2 and is provided with an autoclave cover 6, and the autoclave cover is connected with an air inlet pipeline and an exhaust pipeline.
2. The autoclave was placed in a high temperature furnace 1: the air inlet pipeline is connected with a high-pressure air bottle 8 and a pressure gauge 7; the exhaust pipeline is connected with the air storage chamber 9 and the exhaust valve 10;
3. nitrogen is filled into the autoclave through an air inlet pipeline, so that the ambient pressure of crude oil cracking is stabilized at 5MPa, the ambient pressure has the function of preventing crude oil in the rock core from flowing out in the cracking process, and the ambient pressure can be more than 5MPa in the experimental process;
4. setting the initial cracking temperature at 30 deg.c and the heating rate at 20 deg.c/h, heating to 600 deg.c and stabilizing for 4 hr to crack the crude oil fully.
5. After cracking is complete, the reactor is cooled and the methane and other gases produced are collected and disposed of.
Fifth, content statistics and distribution characteristics of solid asphalt
The samples after lysis are weighed (m)2) The CMS system then measures the porosity of the sample
And permeability (K)2). Thereafter, 4 cast pieces were prepared for each sample, and a total of 32 cast pieces were prepared for 8 samples. Finally, the asphalt distribution characteristics were observed under a microscope and the asphalt content was quantitatively counted using the Photoshop software, as shown in table 1.
TABLE 1 weight, porosity and permeability of samples before and after crude oil cracking, and solid bitumen content of samples after crude oil cracking
The experimental results are as follows:
1. solid asphalt content
For the samples filled with normal crude oil, sample No. 1 and sample No. 7 had porosities of 15.1 and 7.69, respectively, and residual asphalt contents (volume of asphalt) of 1.48 and 0.95, respectively; for the light oil filled samples, sample No. 2 and sample No. 8 had porosities of 14.4 and 2.56, respectively, and residual asphalt contents of 0.49 and 0.22, respectively, as shown in fig. 3.
After cracking of crude oil, the residual asphalt content is generally related to the type of crude oil, and the asphalt content (0.95-1.48) of normal crude oil after filling is higher than the residual asphalt content (0.22-0.49) of light oil. For samples filled with the same type of crude oil, the bitumen content is related to the porosity, with samples with high porosity having a higher residual bitumen content than samples with lower porosity.
After cracking of the crude oil, both the porosity and permeability of the sample decreased, as shown in fig. 4 and 5. However, the samples filled with normal oil had a greater reduction in porosity and permeability than the light oil samples. The asphalt content and the porosity reduction value obtained by the flake are in a similar range, and the permeability is reduced to 9.31-54.85 mD; the permeability of the light oil is reduced to 0.04-16.72 mD.
2. Solid pitch distribution characteristics
FIG. 6 is a microscopic photograph of crude oil after cracking.
It can be seen that samples nos. 1, 3, and 7 (fig. 6A, 6B, and 6C) injected with normal oil had a higher solid pitch content. Some of the smaller pores are completely filled with solid pitch and some of the larger pores are only partially filled with solid pitch. Samples nos. 2, 4, 5, 6, and 8 (fig. 6D, 6E, 6F, 6G, and 6H) were injected with light oil and had a low solid pitch content. That is, the solid asphalt developed mainly in the small pores and throat (sample nos. 1, 4).
In summary, the crude oil cracking experiment and the actual reservoir sample support that asphalt tends to remain at small pores and roars, and the observation of a core slice containing asphalt under a microscope shows that the asphalt is distributed in the small pores and the roars, so that the porosity and the permeability of the reservoir are reduced, and the heterogeneity of the reservoir is increased.
Claims (8)
1. A method for determining solid bitumen content and distribution characteristics in a reservoir, comprising the steps of:
s1, taking and numbering a plurality of reservoir core samples, and drilling 2 plunger samples from each reservoir core sample, wherein the plunger samples are marked as a plunger sample A and a plunger sample B;
s2, extracting the plunger sample A and the plunger sample B by using an organic solvent, and drying; preparing the plunger sample A into a casting sheet, and measuring the physical property I of the plunger sample B;
s3, placing the plunger sample B in an oil injection system for high-pressure oil injection and saturation, and recording parameters in the oil injection process and after oil injection;
s4, placing the plunger sample B in a quartz tube, placing the quartz tube in an autoclave for pyrolysis, and determining the physical property II of the sample subjected to pyrolysis;
s5, preparing the sample subjected to pyrolysis into a plurality of casting body slices, observing the asphalt distribution characteristics and quantitatively counting the asphalt content, thereby realizing the solid asphalt content and the distribution characteristics in the reservoir.
2. The method of claim 1, wherein: in step S2, the organic solvent is a mixed solution of benzene and ethanol, and the volume ratio of benzene to ethanol is 1: 1 to 2.
3. The method according to claim 1 or 2, characterized in that: in step S2, the specifications of the plug sample a and the plug sample B are both: the diameter is 25-30 mm, and the length is 25-30 mm.
4. The method according to any one of claims 1-3, wherein: in step S2, property I includes mass, pore volume, porosity, and permeability.
5. The method according to any one of claims 1-4, wherein: in step S3, the parameters include the oil injection volume, the oil injection pressure, and the sample mass after oil injection, and the oil saturation of the plunger sample B is obtained therefrom.
6. The method according to any one of claims 1-5, wherein: in step S4, the pyrolysis conditions are as follows:
the confining pressure is 5-10 MPa;
the initial temperature is 25-35 ℃, the heating rate is 20-25 ℃/h, and the temperature is stabilized for 4-6 h after being heated to 600-650 ℃.
7. The method according to any one of claims 1-6, wherein: in step S4, property ii includes weight, porosity, and permeability.
8. The method according to any one of claims 1-7, wherein: in step S5, preparing the sample subjected to pyrolysis into 1-5 casting slices;
observing the distribution characteristics of the asphalt by using a microscope;
and quantitatively counting the asphalt content by adopting Photoshop software.
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