Method to detect spatial distribution and concentration of component in pore space of porous material

FIELD: measurement equipment.

SUBSTANCE: application: to detect spatial distribution and concentration of a component in a pore space of a porous material. The invention concept is as follows: it consists in the fact that a contrast X-ray substance is pumped into a sample of a porous material, such as a water-soluble salt of metal with high atomic weight that enters into a selective ion-exchange reaction with a surveyed component, of the common formula: R+M-, where R+ is selected from the group {Ba +; Sr2+; Tl+; Rb+…}, and M- is selected from the group {Cln; NOn; OHn; CH3COO, SO4; …} in accordance with the table of solubility of inorganic substances in water, upon completion of the reaction of selective ion exchange, a non-contrast displacement agent is pumped into a sample, the sample is scanned by means of X-ray microtomography to define spatial distribution and concentration of a surveyed component by means of analysis of the produced computer tomographic image.

EFFECT: higher X-ray contrast of low-contrast components contained in a pore space, when doing computer tomography of porous material samples.

2 cl, 2 dwg

 

The invention relates to methods of non-destructive analysis of samples of porous materials, in particular, it can be used to analyze the distribution of residual oil, and determining the concentration of natural clay in the core sample or clay that has penetrated into the core during the injection of drilling mud.

The spatial distribution of the component (residual water adsorbed film on the surface of the pore, clay or other solid aggregate pore space)contained in the pore space of a porous material, is important information for various technical applications in medicine, petrophysics, civil engineering and materials science, development of oil and gas fields.

So, there is the problem of formation damage under the influence of the drilling fluid (or mud), especially for long horizontal wells since the completion of most of them is in an open state, i.e. without cemented and perforated production string.

Drilling fluids are complex mixtures of clay, fine particles (ranging in size from a few millimeters to less than one micron) and organic additives (polymers, surfactants and so on)contained in the "carrier" fluid "basis" of mud, as the which can be water, oil or any synthetic fluid.

In the process of drilling under the influence of excess pressure of the mud filtrate, and contained fine particles and clay penetrate into kalokairinou zone of the reservoir and cause a significant reduction in its permeability (for characterization of this phenomenon is typically used the term "damage layer zones" or simply "formation damage").

During the process of cleaning procedures well (by the gradual withdrawal of extraction) these components are partially washed away from the vicinity of the zone, and its permeability is partially restored. However, some components remains retained in the pore space of rocks (absorbed on the surface of the pores, are trapped in the pore narrowing and so on), which leads to a considerable difference between the initial permeability and permeability are restored after the technological procedure cleanup (usually restored permeability does not exceed 50-70% of the initial).

Common laboratory method of testing the quality of the drilling fluid is its direct and inverse filtering through the core sample, which measured the dynamics of degradation / restoration of the permeability as a function of the number of injected pore volumes of drilling mud or oil (the latter - p and reverse pumping, modeling the process of cleaning).

However, the distribution and concentration of clay and other components of the drilling fluid, held in the pore space, the length of the core sample represents an important information for understanding the mechanism of formation damage and select the appropriate method of increasing the productivity index of the well (minimizing damage to the bottom-hole formation zone). These parameters are not measured under the above traditional procedures for checking the quality of the mud.

One of the most common non-destructive methods of investigation of the structure of the sample is x-ray computed tomography.

In U.S. patent No. 4540882 describes a method of determining the depth of penetration of the drilling fluid using x-ray computed tomography core with the addition of a contrast agent. The first material is added to the drilling mud to detect a first fluid having an average atomic number, different from the average atomic number of the residual fluid contained in the bottomhole formation zone. Saved the core sample is collected from the wells for scanning x-ray computed axial tomography to determine the absorption coefficients of x-rays in the set of points lying in a transverse slashing the AI of the core sample. the core sample is scanned using x-rays at the first and second energy. Obtained values of the absorption coefficients in the set of points lying on the cross-section at each energy value is used to determine the atomic number of the elements in the image. Then the atomic number of the elements in the image is determined by the penetration depth of the first fluid, and the resulting value is an indicator of the depth of penetration of the drilling fluid into the core sample.

Another method is disclosed in U.S. patent No. 4722095, which is based on the use of high absorption coefficient of x-rays in barite is widely used as weighting additive for drilling mud. First, the mud filtrate is removed from the core sample, and then using x-ray computed tomography is measured and the total pore volume of the core sample, and the amount of particles of barite, penetrated into the sample.

Unfortunately, the use of barite as a contrast agent to assess the depth of penetration of the drilling fluid is not always justified, since the size of these particles is comparable to the size of the pore narrowing and therefore most of them will be trapped in small pores near the entrance to the sample.

Other components of the drilling mud (clay, polymers, the ode, and so on) have generally weak in contrast to x-rays and cannot be spatially resolved with the required precision.

The use of contrast agent that is soluble in the carrier fluid", as suggested in U.S. patent No. 5027379, it is not possible to estimate the penetration depth and the concentration of clay and other low-contrast additives contained in the mud, because the penetration depth of the mud filtrate and these additives are in General different.

The technical result achieved by the invention is to increase the x-ray contrast low-contrast component contained in the pore space, computed tomography (CT) of the samples of porous materials. These components can be either natural (e.g., natural clay, film, oil etc)and implemented in the course of filtration experiments (for example, components of drilling mud).

This technical result is ensured by the fact that in the sample of porous material is injected contrast x-ray of the substance, which is used as a water-soluble salt of a metal of high atomic weight, coming in selective ion-exchange reaction with the test component. In General, the formula for water-soluble metal salt can be recorded is in the form: R +M-where R+chosen from the group {VA2+; Sr2+; TL+; Tb+...}and M-chosen from the group {CLn; NOn; OHn; SNAO, SO4; ...}. Substance R+and M-are selected in accordance with the table of solubility of inorganic substances in water.

Upon completion of the reaction, selective ion exchange in the sample is pumped with no displacing agent, conduct x-ray computer microtomography imaging of the sample and determine the spatial distribution and concentration of the component under consideration by computer analysis of the obtained tomographic image.

The invention is illustrated in the drawing, where figure 1 shows the data computed x-ray microtomography of an aqueous solution of the original clay (before mixing with contrast agent) and an aqueous solution of contrasting clay, and figure 2 - example of computed x-ray microtomography of the sample after application of a contrast agent.

The main criterion for the applicability of the method is the stability of the studied components to the process of injection of contrast agent.

When used as a contrast x-ray of the substance water-soluble salt of a metal of high atomic weight, with the ability to enter into selective ion-exchange reaction with the test component, and the us heavy metals are accumulated at the denoising component, thereby increasing its contrast to the x-ray radiation. In the injection sample contrasty displacing agent upon termination of the reaction selective ion exchange remnants of heavy metal and the reaction products are washed from the sample. From the analysis of the obtained CT image (see, for example, Gonzalez R.., Woods, R.E. Digital Image Processing. Addison-Wessley, New York (1992)determine the spatial distribution and concentration of the considered component.

As a first example implementation of the invention consider the use of the claimed method to increase the contrast to x-ray radiation and the subsequent determination of the concentration of clay, held in the pore space after cycle direct - inverse filtering model mud - 2% aqueous solution of bentonite clay through the core sample.

Perform filtration experiment by injection of 2% aqueous solution of bentonite clay and subsequent washing penetrated clay from the porous medium (backward pumping). After the end of the experiment in the pore space of the sample is retained only clay, firmly held in the narrowing of the pore.

Choose a water-soluble salt of a metal of high atomic weight, coming in selective ion-exchange reaction with the investigated clay.

Taking into account the remaining bentonite clay Al 2[Si4O10](OH)2·nH2O and following the standard table of solubility of inorganic substances in water (e.g., the Handbook of experimental data on the solubility of multicomponent water-salt systems, the State scientific and technical publishing house of the chemical literature. Leningrad, V.1-2, 1954), as a metal salt chosen l2.

For illustration, figure 1 shows data computed x-ray microtomography of an aqueous solution of the original clay (before mixing with contrast agent) and an aqueous solution of contrasting clay (i.e. clay subjected to ion-exchange reactions with salt l2).

Sample saturated aqueous solution of contrast agent (l2and maintain some time, depending on the speed of reaction.

After the reaction through the sample is pumped 3-4 pore volume model non-contrast fluid (saline solution) to remove the reaction products and residues contrast agent.

The rate of injection should not exceed the speed of backward pumping in the filtration experiment.

Examine the sample using computed x-ray microtomography.

An example of computed x-ray microtomography of the sample after application patentable contrast agent is shown in Figure 2. Accumulation of barium ion in the clay, as R is the result of ion-exchange reactions leads to a significant increase in its contrast (modified clay corresponds to the white area in the picture).

Another example implementation of the invention is the study of hydrocarbons in the sample. Alkanes when heated interact with a solution of bromine in an organic solvent, reacting the substitution. It can be shown by the example of the interaction of n-dodecane CH3(CH2)10CH3with bromine dissolved in carbon tetrachloride Cl4.

This reaction can be used for the selective modification of hydrocarbons in porous media. Sample containing hydrocarbons, saturated solution of bromine, then heated and maintained at a given temperature. Temperature and reaction time depend on the composition of the hydrocarbon mixture. After the reaction through the sample it is necessary to pump 3-4 pore volume of the model fluid (saline solution) to remove the reaction products. The introduction of bromine can increase the contrast of hydrocarbons in the pores of the sample under study using computed x-ray microtomography.

1. The method of determining the spatial distribution and concentration of the component in the pore space of a porous material, in accordance with which
in the sample of porous material sakac which provide a contrast x-ray of the substance, which is used as a water-soluble salt of a metal of high atomic weight, coming in selective ion-exchange reaction with the test component, with the General formula: R+M-where R+chosen from the group {VA2+; Sr2+; T1+; Rb+...}, a M-chosen from the group {CLn; NOn; OHn; CH3COO, SO4; ...} in accordance with the table of solubility of inorganic substances in water
after the reaction of selective ion exchange in the sample is pumped with no displacing agent,
- conduct computerized x-ray microtomography imaging of a sample and the
determine the spatial distribution and concentration of the analyzed component by computer analysis of the obtained tomographic image.

2. The method according to claim 1, whereby as the displacing agent using aqueous salt solution.



 

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