CN105548232B - The microcosmic detection method of Polymer Used For Oil Displacement distribution in porous media - Google Patents
The microcosmic detection method of Polymer Used For Oil Displacement distribution in porous media Download PDFInfo
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- CN105548232B CN105548232B CN201510888168.5A CN201510888168A CN105548232B CN 105548232 B CN105548232 B CN 105548232B CN 201510888168 A CN201510888168 A CN 201510888168A CN 105548232 B CN105548232 B CN 105548232B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
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- G01N23/2252—Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
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- G01N2223/079—Investigating materials by wave or particle radiation secondary emission incident electron beam and measuring excited X-rays
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Abstract
The present invention relates to a kind of microcosmic detection method of Polymer Used For Oil Displacement distribution in porous media, comprise the following steps according to sequencing：Complete after polymer displacement of reservoir oil experiment, core is taken out from rock core fastener, core chip sample is prepared；Detect the element species of core chip sample diverse location and the content of each element；Find the distributing position and its corresponding distribution content of " N " element in core chip sample；According to the testing result of " N " element, the regularity of distribution of " N " element is determined in core chip sample.The microcosmic detection method is simple to operate, accuracy rate is high, the novel means of " N " element in electron probe technology for detection Polymer Used For Oil Displacement solution are used first, by carrying out punctuate to exclusive " N " element of polymer, the anti-preservation position for pushing away polymer in porous media and preservation content, the microcosmic occurrence status of polymer can be intuitively provided, so that preservation research of the people to polymer solution in reservoir enters microcosmic mechanism aspect.
Description
Technical field
The invention belongs to oil reservoir production technique field, and in particular to a kind of Polymer Used For Oil Displacement is distributed shape in porous media
The microcosmic detection method of state.
Background technology
Polymer flooding and its derivative binary combination flooding or ternary composite driving, are steady after many water floodings of China
One of production, the important means of volume increase.Polymer solution is added, the viscosity of displacement solution can be effectively improved, in increase injection pressure
Swept volume can be expanded while power, so as to improve the recovery ratio of reservoir crude oil.But with the continuous injection of polymer solution,
Porous media can carry out adsorbing and trapping to it so that the mobility of reservoir declines.If the polymer solution of design is matched somebody with somebody with reservoir
5 property are not good, or even occur that injection of polymer blocks the phenomenon of hole.
Prior art is usual based on Measure macro in the research of reservoir distribution to polymer, such as by molten in polymer
The method that tracer is added in liquid, Study Polymer Melts are in the flow direction of reservoir, flowing velocity and by position etc..Macro -examination
Method is used for produced on-site, if from attachment of the Study Polymer Melts in mechanism in porous media and distribution situation, must be from
Microcosmic angle is studied.Because polymer solution does not have special color or other microscopic characteristics, it is impossible to in rock sample
Water, oil make a distinction, can not be observed by traditional microcosmic means such as light microscope at present.Therefore, it is badly in need of
A kind of new microcosmic detection method is developed, for studying distribution of the Polymer Used For Oil Displacement in porous media.
Application publication number discloses to remain in a kind of polymer flooding reservoir rock for CN102003176A patent of invention to be gathered
The quantitative measuring method of compound, its step is：(1) collection non-polymer drives reservoir rock sample, and grinding is uniform, weighs 5mg and puts
Enter to heat according to certain condition in the oxidation tube of combustion furnace and burn, combustion product purging is then carried to reduction furnace with helium
Reduce, according still further to certain condition separating nitrogen, carbon dioxide and water, examined by elemental analyser according to certain condition in reduction tube
Survey, the data measured are averaged and are used as the nitrogenous background value of polymer flooding reservoir rock sample；(2) collection polymer flooding storage
Layer rock sample, grinding is uniform, weighs 5mg and is put into the oxidation tube of combustion furnace to heat according to certain condition and burn, then uses helium
Combustion product purging is carried in the reduction tube of reduction furnace and reduced according to certain condition by gas, according still further to certain condition separating nitrogen,
Carbon dioxide and water, are detected by elemental analyser, obtain the nitrogenous Value Data of polymer flooding reservoir rock sample；(3) use
The nitrogenous Value Data of polymer flooding reservoir rock sample subtracts the nitrogenous background value of polymer flooding reservoir rock sample, is polymerize
Thing contain values of nitrogen might；(4) polymer is substituted into formula y=0.0003x+0.0142 containing values of nitrogen might, produces polymer flooding reservoir rock
The residual quantity of polymer in stone, wherein x is the values of nitrogen might that contains of polymer, and y is the residual quantity of polymer in polymer flooding reservoir rock.
The technical scheme of the patent of invention is complicated, and the process conditions being related to are more, if the harmony of these process conditions is bad, will produce
Very big error, testing result is inaccurate, needs to use the legacy equipments such as combustion furnace, reduction furnace, elemental analyser in addition, precision compared with
It is low, influence testing result.
The content of the invention
To solve problems of the prior art, the present invention provides a kind of Polymer Used For Oil Displacement and is distributed in porous media
The microcosmic detection method of state, its object is to：A kind of microscopic approach is developed, to point of the Polymer Used For Oil Displacement in porous media
Cloth position is determined, and counts distribution content of the polymer in the position, and then is realized using microcosmic means research polymerization
The purpose of thing adhesion condition in porous media.
To achieve the above object, the technical solution adopted by the present invention is：Polymer Used For Oil Displacement is distributed shape in porous media
The microcosmic detection method of state, comprises the following steps according to sequencing：
Step one：Complete after polymer displacement of reservoir oil experiment, core is taken out from rock core fastener, core chip sample is prepared；
Step 2：Detect the element species of core chip sample diverse location and the content of each element；
Step 3：Find the distributing position and its corresponding distribution content of " N " element in core chip sample；
Step 4：According to the testing result of " N " element, the regularity of distribution of " N " element is determined in core chip sample.
The present invention is detected by " N " element exclusive to polymer, is followed the trail of " N " element in polymer and is situated between porous
Distributing position and its corresponding distribution content in matter, and then judge distributing position of the polymer in porous media and its corresponding
Distribution content.
Due to there is amide groups in Polymer Used For Oil Displacement so that can there is " N " element to be detected in polymer solution,
And " N " element preservation is not present in stratum, this is just the preservation with " N " element standardization Study Polymer Melts in porous media
Position and preservation content provide foundation.The chemical constitution molecular formula of Polymer Used For Oil Displacement is as follows：
The present invention, in combination with electron probe microscope, is probe using the extremely narrow electron beam by accelerating and focusing on,
A certain tiny area in core chip sample is excited, it is sent characteristic X-ray, the wavelength and intensity of the X-ray is determined, you can
Qualitative and quantitative analysis is made to " N " element of the microcell.
Preferably, in the step one, after core is taken out from rock core fastener, with the material without " N " element
Core is coated, horizontal positioned cuts off core top half, then with being free of the material of " N " element by the upper of core the latter half
Surface coating, overturns core, reserves certain thickness core in its bottom, remainder is cut off, then with being free of " N " element
Material coats the upper surface of reserved part core, and core chip sample is made.
Before microcosmic detection is carried out, core chip sample is pre-processed, core is coated with the material without " N " element,
The step such as then cut, overturn, being coated again, final obtained core chip sample integral coating is without " N " element
In material.After the displacement of reservoir oil, the liquid that polymer solution enters in core, core is in flow regime, and form is unstable, if through
Cross and move, place for a long time or external and internal pressure imbalance etc., liquid can ooze out from the hole of core, so as to cause testing result
It is inaccurate, therefore during core thin slice is prepared, just core is progressively pre-processed, it is ensured that it is detected samples met real
Border situation, so as to improve the authenticity of testing result.
In addition in detection process, core chip sample is put into detection chambers, if core chip sample is exposed, very may be used
Sample can be caused to pollute or new " N " element is introduced from extraneous, so as to cause testing result inaccurate.Because experimental facilities is in inspection
When surveying the sample that other contain " N " element, " N " element is evaporated in itself or in forms such as compounds, is adhered to or is trapped in detection
In chamber, even if being cleaned and being handled, it can not also ensure that " N " element is completely absent, when detecting core chip sample, if
Sample is exposed, then extraneous " N " element is likely to and volatilized be attached on core chip sample, so as to cause testing result not
Accurately, therefore when preparing core chip sample pretreatment is needed, sample is coated, it is to avoid new " N " is introduced from extraneous
Element.
In any of the above-described scheme preferably, in the step 2, core thin slice is detected using electron probe microscope
The element species of sample diverse location and the content of each element.
In any of the above-described scheme preferably, in the step 3, core thin slice is detected using electron probe microscope
The distributing position and its corresponding distribution content of " N " element in sample.
In any of the above-described scheme preferably, in the step 4, the regularity of distribution of " N " element in core chip sample
The as regularity of distribution of the Polymer Used For Oil Displacement in porous media.
In any of the above-described scheme preferably, the material without " N " element is aluminium foil.
In any of the above-described scheme preferably, the material thickness without " N " element is 0.05-1.0mm.
In any of the above-described scheme preferably, the thickness of the core chip sample is 15-20mm.
The microcosmic detection method of Polymer Used For Oil Displacement distribution in porous media of the present invention, it is simple to operate, accurately
Rate is high, it is easy to promote.The microcosmic detection method combines electron probe microscope inspection flow measurement according to " N " Element detection law theory
The novel means of " N " element in body, by carrying out punctuate to exclusive " N " element of polymer, the anti-polymer that pushes away is situated between porous
Preservation position and preservation content in matter, can intuitively provide the microcosmic occurrence status of polymer, so that people are to polymerization
Thing solution enters microcosmic mechanism aspect in the preservation research of reservoir.The present invention uses poly- using electron probe technology to the displacement of reservoir oil first
" N " element in polymer solution is detected, and can effectively determine distributing position and its corresponding distribution of the polymer in reservoir
Content.
Brief description of the drawings
Fig. 1 be according to the Polymer Used For Oil Displacement of the present invention in porous media the microcosmic detection method of distribution it is one excellent
Select embodiment process chart；
Fig. 2 is Fig. 1 of Polymer Used For Oil Displacement microcosmic detection method of distribution in porous media according to the present invention
The microcosmic detection result schematic diagram of illustrated embodiment；
Fig. 3 be according to the present invention Polymer Used For Oil Displacement in porous media the microcosmic detection method of distribution it is another
The microcosmic detection result schematic diagram of embodiment；
Fig. 4 be according to the present invention Polymer Used For Oil Displacement in porous media the microcosmic detection method of distribution it is another
The microcosmic detection result schematic diagram of embodiment.
Embodiment
In order to be further understood that the content of the invention of the present invention, the present invention is elaborated below in conjunction with specific embodiment.
Embodiment one：
As shown in figure 1, the microcosmic detection method of Polymer Used For Oil Displacement distribution in porous media according to the present invention
An embodiment, it comprises the following steps according to sequencing：
Step one：Complete after polymer displacement of reservoir oil experiment, core is taken out from rock core fastener, core chip sample is prepared；
Step 2：Detect the element species of core chip sample diverse location and the content of each element；
Step 3：Find the distributing position and its corresponding distribution content of " N " element in core chip sample；
Step 4：According to the testing result of " N " element, the regularity of distribution of " N " element is determined in core chip sample.
The present embodiment detects that " N " element is porous in tracking polymer by " N " element exclusive to polymer
Distributing position and its corresponding distribution content in medium, and then judge distributing position and its phase of the polymer in porous media
The distribution content answered.
Because Polymer Used For Oil Displacement is polyacrylamide, there is " N " element preservation in its solution, and be not present in stratum
" N " element preservation, this is just the preservation position and preservation in porous media with " N " element standardization detection polyacrylamide
Content provides foundation.The chemical constitution molecular formula of polyacrylamide is as follows：
The present embodiment, in combination with electron probe microscope, is spy using the extremely narrow electron beam by accelerating and focusing on
Pin, excites a certain tiny area in core chip sample, it is sent characteristic X-ray, determines the wavelength and intensity of the X-ray,
Qualitative and quantitative analysis can be made to " N " element of the microcell.
In the step one, after core is taken out from rock core fastener, core is coated with the material without " N " element,
Horizontal positioned, core top half is cut off, then is coated the upper surface of core the latter half with the material without " N " element,
Core is overturn, certain thickness core is reserved in its bottom, remainder is cut off, then will be pre- with the material without " N " element
Stay the upper surface of part core to coat, core chip sample is made.The material without " N " element is aluminium foil, and its thickness is
0.05mm.The thickness of the core chip sample is 20mm.
Before microcosmic detection is carried out, core chip sample is pre-processed, core is coated with the material without " N " element,
The step such as then cut, overturn, being coated again, final obtained core chip sample integral coating is without " N " element
In material.After the displacement of reservoir oil, the liquid that polymer solution enters in core, core is in flow regime, and form is unstable, if through
Cross and move, place for a long time or external and internal pressure imbalance etc., liquid can ooze out from the hole of core, so as to cause testing result
It is inaccurate, therefore during core thin slice is prepared, just core is progressively pre-processed, it is ensured that it is detected samples met real
Border situation, so as to improve the authenticity of testing result.
In addition in detection process, core chip sample is put into detection chambers, if core chip sample is exposed, very may be used
Sample can be caused to pollute or new " N " element is introduced from extraneous, so as to cause testing result inaccurate.Because experimental facilities is in inspection
When surveying the sample that other contain " N " element, " N " element is evaporated in itself or in forms such as compounds, is adhered to or is trapped in detection
In chamber, even if being cleaned and being handled, it can not also ensure that " N " element is completely absent, when detecting core chip sample, if
Sample is exposed, then extraneous " N " element is likely to and volatilized be attached on core chip sample, so as to cause testing result not
Accurately, therefore when preparing core chip sample pretreatment is needed, sample is coated, it is to avoid new " N " is introduced from extraneous
Element.
In the step 2, the element species of core chip sample diverse location are detected and each using electron probe microscope
The content of element.
In the step 3, using electron probe microscope detect core chip sample in " N " element distributing position and
Its corresponding distribution content.
In the step 4, the regularity of distribution of " N " element is that Polymer Used For Oil Displacement is situated between porous in core chip sample
The regularity of distribution in matter.
The core chip sample of the present embodiment is hypertonic sample (K=153.5mD), and its microcosmic detection result is as shown in Figure 2.
As shown in Figure 2, polyacrylamide is mainly distributed on hole edge and clay mineral rich region, in main flow duct, does not examine
Polyacrylamide is measured, illustrates that polyacrylamide does not have to block in porous media.
The microcosmic detection method of the Polymer Used For Oil Displacement of the present embodiment distribution in porous media, it is simple to operate, it is accurate
True rate is high, it is easy to promote.The microcosmic detection method combines the detection of electron probe microscope according to " N " Element detection law theory
The novel means of " N " element in fluid, by carrying out punctuate to exclusive " N " element of polymer, the anti-polymer that pushes away is porous
Preservation position and preservation content in medium, can intuitively provide the microcosmic occurrence status of polymer, so that people are to poly-
Polymer solution enters microcosmic mechanism aspect in the preservation research of reservoir.The present embodiment is first using electron probe technology to the displacement of reservoir oil
Detected with " N " element in polymer solution, can effectively determine distributing position of the polymer in reservoir and its corresponding
Distribution content.
Embodiment two：
According to another implementation of Polymer Used For Oil Displacement microcosmic detection method of distribution in porous media of the present invention
, its processing step, principle and beneficial effect etc. are identical with embodiment one, unlike：The material without " N " element
For aluminium foil, its thickness is 1.0mm.The thickness of the core chip sample is 15mm.During the core chip sample of the present embodiment is
Sample (K=87.8mD) is oozed, its microcosmic detection result is as shown in Figure 3.From the figure 3, it may be seen that polyacrylamide is mainly distributed on hole
Edge and clay mineral rich region, detect polyacrylamide in the main flow duct of part, illustrate polyacrylamide in part
Main flow is blocked in duct.
Embodiment three：
According to another implementation of Polymer Used For Oil Displacement microcosmic detection method of distribution in porous media of the present invention
, its processing step, principle and beneficial effect etc. are identical with embodiment one, unlike：The material without " N " element
For aluminium foil, its thickness is 0.5mm.The thickness of the core chip sample is 18mm.The core chip sample of the present embodiment is low
Sample (K=53.3mD) is oozed, its microcosmic detection result is as shown in Figure 4.As shown in Figure 4, polyacrylamide is mainly distributed on hole
Edge and clay mineral rich region, polyacrylamide is detected in all main flow ducts, illustrates polyacrylamide in institute
Have in main flow duct and block.With the decline of permeability, the content of polymer gradually increases in main flow duct, occurs stifled
The situation of plug is also increasingly severe.
It will be apparent to those skilled in the art that the present invention Polymer Used For Oil Displacement in porous media distribution it is microcosmic
Each portion shown by the content of the invention and embodiment part and accompanying drawing of the detection method including the invention described above specification
Any combination divided, is described one by one as space is limited and for each scheme for making specification concise without these combinations are constituted.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc., should be included in the guarantor of the present invention
Within the scope of shield.
Claims (2)
1. a kind of microcosmic detection method of Polymer Used For Oil Displacement distribution in porous media, includes following according to sequencing
Step：
Step one：Complete after polymer displacement of reservoir oil experiment, core is taken out from rock core fastener, core chip sample is prepared；
Step 2：Detect the element species of core chip sample diverse location and the content of each element；
Step 3：Find the distributing position and its corresponding distribution content of " N " element in core chip sample；
Step 4：According to the testing result of " N " element, the regularity of distribution of " N " element is determined in core chip sample；
In step one, after core is taken out from rock core fastener, with without " N " element material coat core, horizontal positioned,
Core top half is cut off, then coated the upper surface of core the latter half with the material without " N " element, core is overturn,
Certain thickness core is reserved in its bottom, remainder is cut off, then with the material without " N " element by reserved part core
Upper surface cladding, core chip sample is made；
In step 2, the element species of core chip sample diverse location and containing for each element are detected using electron probe microscope
Amount；
In step 3, the distributing position of " N " element is detected in core chip sample and its corresponding using electron probe microscope
Distribution content；
In step 4, the regularity of distribution of " N " element is point of the Polymer Used For Oil Displacement in porous media in core chip sample
Cloth rule；
" N " element in polymer solution is directly detected by electron probe, and punctuate is carried out to " N " element in polymer,
Determine the distribution content of distributing position of the polymer in reservoir and polymer in the position；The material without " N " element
Material thickness is 0.05-1.0mm, and the thickness of the core chip sample is 15-20mm；The core chip sample is completely true
Real core.
2. the microcosmic detection method of polymer as claimed in claim 1 distribution in porous media, it is characterised in that：Institute
It is aluminium foil to state the material without " N " element.
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| CN112198184B (en) * | 2020-09-16 | 2022-04-22 | 宁波锦越新材料有限公司 | Analysis method for detecting indium element content and distribution of high-purity aluminum target material after acid washing by EPMA |
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| CN102071929B (en) * | 2010-12-09 | 2013-06-05 | 中国石油天然气股份有限公司 | Dolomite reservoir geochemical plate generation method |
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| JPH09151217A (en) * | 1995-11-29 | 1997-06-10 | Sanyo Chem Ind Ltd | Anionic water-soluble polymer |
| CN102003176A (en) * | 2010-10-19 | 2011-04-06 | 大庆油田有限责任公司 | Quantitative test method for residual polymer in polymer flooding reservoir rocks |
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