Method of determining spatial distribution in core material of effective pore space

FIELD: chemistry.

SUBSTANCE: method includes pumping an X-ray contrast substance into a core sample, scanning the sample by X-ray tomography and obtaining histograms. The method is characterised by that the X-ray contrast substance in the core sample is a mixture of gelatine and an iodine-containing substance in concentration of not less than 10% by weight of the prepared solution.

EFFECT: high accuracy of determining spatial distribution in core material of effective pore space, and enabling investigation of structural features of the core after chemical or physical action.

2 dwg

 

The invention relates to methods of studying the structure of the core before and after physical or chemical effect during testing of drilling fluids, gel-forming formulations, viscoelastic polymer systems, chemical reagents, etc.

Known "Method of preventing drilling mud loss" ("Method of determining drilling fluid invasion, U.S. patent No. 4540882, publication date 10.09.1985), including the definition of the completeness of penetration of mud filtrate into the core with the addition of an agent with a high resistance to the passage of X-rays using microcomputed tomography. The first material is added to the drilling mud for the purpose of detection of the first fluid having an average atomic number that is different from the average atomic number of the residual fluid contained in the borehole zone of the formation. Preserved core samples taken from wells for scanning x-ray computerized axial tomography to determine the absorption coefficients of x-rays in the set of points lying in the cross section of the core sample. The core sample is scanned with the help of x-rays on the first and second energy.

Its disadvantage is the extremely high mobility of the mixture "drilling mud + contrast agent", which makes it impossible for high-quality scan of the sample in microtome�Rafah and to further build three-dimensional models, as for standard scan takes a long time.

Also known "Method of determining the porosity and absorption of drilling mud core sample from the subterranean formations" ("Method for identifying a variety of architectural expressions and drilling mud invasion of a core sample from a subterranean formation", U.S. patent No. 4722095, publication date 26.01.1988), based on the use of high absorption coefficient of x-ray radiation in barite is widely used as the weight 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 volume of barite particles penetrated into the sample.

The disadvantage of this method is the use of barite as a radiopaque material, the large size of the particles which prevents its penetration into small cracks and pores. Clay and other substances included in the composition of drilling fluids, have a weak contrast to x-ray radiation.

Known "Method of determining the penetration of mud filtrate in the core samples of subterranean formations" ("Method for identifying drilling mud filtrate invasion of a core sample from a subterranean formation", U.S. patent No. 5027379, publication date 25.06.1991), including the use of radiopaque additives (as in the method proposed by the authors �patent data).

Its disadvantage is concluded that the use rentgencontrastnoe substances to assess the penetration of mud filtrate is not possible due to the fact that rentgencontrastnoe substance, soluble in water, will penetrate incomparably deeper than the mud filtrate with small particles.

Also known "Method of determining spatial distribution and concentration of clay in the core sample" (patent RF №2467315, publication date 20.11.2012, bull. No. 32), adopted as a prototype, including the determination of the spatial distribution and concentration of clay in the core sample with the addition of a contrast x-ray of the substance, which is used as a water-soluble salt of a metal with high atomic weight, entering into selective ion-exchange reaction with the clay, after the reaction, selective ion exchange in the sample is pumped soft displacing agent, scan the sample by means of x-ray tomography, computed tomographic image of the isolated region of interest and the reference section, get the histogram of a grayscale image in the cross sections of the sample and determine the spatial distribution and concentration of clay in the sample by analyzing the histograms, since the histogram of the reference section.

The disadvantage Yes�tion of this method is the impossibility of its use in the study of structural features of the core before and after chemical or physical methods of influence.

The technical result consists in increasing the accuracy of determining the concentration and spatial distribution of the gel-forming composition based on gelatin in the core sample, improving the quality of research of influence of alkalis, acids, etc. on the porosity, permeability, the number of communicating pores in the core sample, etc., as well as enabling more detailed investigation of the core sample after physical impact.

The technical result is achieved in that as a contrast x-ray of the substance in the core sample is injected a mixture of gelatin and iodine-containing substances in a concentration of at least 10 percent by weight prepared solution, conduct x-ray scan of the sample and produce three-dimensional models of the sample and the pore space by reconstructing the images of x-ray tomography.

The described method is illustrated by the following figures:

Fig. 1 - the effective pore space of the core, saturated radiopaque structure (to chemical exposure);

Fig. 2 - the effective pore space of the core, saturated radiopaque structure (after chemical exposure).

As an example of the invention, consider the use of the claimed method of determining the spatial distribution in to�room material effective pore space when comparing capacitive parameters of the core (rock), scanned before and after chemical exposure.

Example 1. At the initial stage, the preparation of core material, cutting out from the cores of cylindrical samples with a diameter of 3 cm, the grinding of the side faces of the specimen to ensure a tight crimp and uniform injection of the agent, the cleaning of the sample from the residual content of formation fluid through a first extraction with toluene, then with petroleum ether and then with distilled water. Next, the preparation of radiopaque mixture to 62.0 g of fresh water is added 3.0 g of gelatin and 35.0 g of salt KI, heated until dissolved under constant stirring. Receive 100.0 g of a solution containing 3.0 wt. % gelatin, 35.0 wt. % KI and 62.0 wt. % water.

The resulting composition is injected into the sample of porous material. At the next stage, conduct a computer x-ray scan of the sample using x-ray computer tomograph SkyScan 1174 and computer control software. Then perform the reconstruction of the images obtained by using specialized software NRecon, to thereby produce images of cross-sections of the sample in steps of 9 micrometers. Then determine the spatial distribution of the examined structure by 3D analysis in a specialized software about�the sintered material CTAn received reconstructed computer tomographic image, calculate the parameters of the open/closed porosity, anizotropnoi, density, pore volume, volume of rock, the surface area of pores, the size of fractions. At the final stage, the formation of a detailed three-dimensional model of the sample core with the help of specialized software and CTvol CTvox.

An example implementation of the invention is illustrated by the following figures. Fig. 1 shows a three-dimensional image model of the effective pore space of the core sample prior to chemical exposure to saturated radiopaque composition. Fig. 2 shows a three-dimensional image model of the effective pore space of the core sample after chemical exposure to that created new filtration channels. In this case, was built three-dimensional model of the pore space and combined with the original model, shown in Fig. 1. Where alignment of the original model with the resulting't happened have been allocated to the newly formed filtration channels marked in red.

The results presented in the form of three-dimensional models prove the high efficiency of the described method of research to study the cores and substances that affect the breed.

Example 2. Prepare the core material. Then prepare rentgenocontrast�th mixture, what to 81.0 g of fresh water is added 3.0 g of gelatin and 16.0 g of salt KI, heated until dissolved under constant stirring. Receive 100.0 g of a solution containing 3.0 wt. % gelatin, 16.0 masses. % KI and 81.0 masses. % of water. The resulting composition is injected into the sample of porous material. The following stage is carried out x-ray scanning of the sample and produce three-dimensional models of the sample by reconstructing the x-ray tomography images. Then determine the spatial distribution of the examined structure by 3D analysis of the obtained reconstructed image, calculate the parameters of the open/closed porosity, anizotropnoi, density, pore volume, volume of rock, the surface area of pores, the size of fractions. At the concluding stage, the formation of a detailed three-dimensional model of the sample core with the help of specialized software and CTvol CTvox.

Example 3. Prepare the core material. Then prepare radiopaque mixture to 87.0 g of fresh water is added 3.0 g of gelatin and 10.0 g of salt KI, heated until dissolved under constant stirring. Receive 100.0 g of a solution containing 3.0 wt. % gelatin, 10.0 masses. % KI and 87.0 masses. % of water. The resulting composition is injected into the sample of porous material. At the next stage, carry out the whole machine�RNA x-ray scan of the sample. Then perform the reconstruction of the images. Then determine the spatial distribution of the examined structure by 3D analysis of the obtained reconstructed image, calculate the parameters of the open/closed porosity, anizotropnoi, density, pore volume, volume of rock, the surface area of pores, the size of fractions. At the final stage, the formation of a detailed three-dimensional model of the sample core with the help of specialized software and CTvol CTvox.

The method for determining the spatial distribution of the core material in effective pore space, whereby the core sample is injected contrast x-ray substance, scan the sample by means of x-ray tomography, get the histogram, characterized in that as a contrast x-ray of the substance in the core sample is injected a mixture of gelatin and iodine-containing substances in a concentration of at least 10 percent by weight for solution.



 

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