CN111007093B - Novel material composite adjustable tracer and detection method thereof - Google Patents
Novel material composite adjustable tracer and detection method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of energy development and tracing, and particularly relates to a novel material composite adjustable tracer for oil and gas exploitation and a detection method thereof. The invention also provides a series of preparation, detection, use and interpretation methods with system relevance corresponding to related tracers, the material has great significance in the field of tracer materials, is a prediction means for providing effective energy development, has the predictive effect of energy misleading development and environmental pollution development, and has the adjustable and controllable advanced effect in energy development.
Description
Technical Field
The invention belongs to the field of energy development tracing, and particularly relates to a new material tracer for oil and gas exploitation and a detection method thereof.
Background
The new material is an important determinant factor for promoting scientific and technological progress and influencing the improvement of human living standard, the breakthrough of energy development is an important field and a major topic in the current society, the new material for energy development, especially the new tracer material is a prediction means for energy development, has a pilot prejudgment function on the quality of the energy development effect, and the good tracer material is also an important assistant or advanced tool for increasing the environmental protection property of energy development, reducing the energy consumption of energy development and providing the energy development efficiency.
However, most of the existing tracer materials are single in material composition, meanwhile, a single tracer is greatly influenced by formation factors, the tracer monitoring result is available or unavailable, the use is unreliable, the underground tracer monitoring of various parameters can not be adapted, in addition, the existing tracer monitoring is complex, a monitoring instrument is precise and high in cost, the existing tracer monitoring materials can not adapt to various tracer monitoring rapidly and flexibly, the existing other tracer materials also have the defects that the using mode of the tracer is not fixed, the variability of the detection result caused by the using mode is large, the existing tracer materials can not be well combined with underground equipment for use, the time requirement controllability of tracer release is poor, and corresponding tracers, preparation methods and using methods thereof are also lacked. Therefore, a novel tracer and a method thereof have yet to be developed.
Disclosure of Invention
In order to solve one of the problems, the invention provides a novel material composite adjustable tracer, which comprises the components of 5-pyrazolone, diethylenetriamine, bromopentafluorobenzene and a compound of rare earth elements.
Preferably, the components also comprise 128 epoxy resin, polyetheramine d400, urea, micron graphite powder, white granulated sugar and calcium oxide.
Preferably, the rare earth elements include terbium, cerium, samarium and yttrium.
Preferably, the method further comprises the step of matching the components with a modeling structure device to form the mechanical structure material with controllable functional tracing.
Preferably, the modeling structure device is a space shell model, the component is matched with the space shell model to form a mechanical structure material with controllable function tracing, the mechanical structure material with controllable function tracing comprises a surface contact area space part which is formed by matching the bottom end of the space shell model with a tracer component,
the middle of the space shell model is matched with a tracer component to form a central release area space part of the mechanical structure material with controllable function tracing, the middle of the space shell model is matched with the tracer component to form the central release area space part of the mechanical structure material with controllable function tracing, the other end of the space shell model is matched with the tracer component to form a contact connection space part of the mechanical structure material with controllable function tracing, the surface contact area space part is formed by uniformly stirring and mixing 5-pyrazolone, diethylenetriamine, cerium chloride, urea, bromopentafluorobenzene, micron graphite powder, 128 epoxy resin and polyetheramine d400, the central release area space part of the mechanical structure material with controllable tracing is formed by mixing 5-pyrazolone, diethylenetriamine, cerium chloride, bromopentafluorobenzene, micron graphite powder, 128 epoxy resin and polyetheramine d400 and then gradually mixing white granulated sugar aqueous solution, the contact connection space part of the tracing controllable mechanical structure material is composed of 5-pyrazolone, diethylenetriamine, cerium chloride, bromopentafluorobenzene, micron graphite powder, 128 epoxy resin, polyetheramine d400 and gradually reduced mixed calcium oxide.
Preferably, the contact connection space structure is an inlaid type sleeve structure, the mechanical structure material with controllable function tracing further comprises an inlaid type sleeve structure for connecting the inlaid type sleeve structure of the tracer material with one end of a support connection material, the other end of the support connection material is connected with the inlaid type sleeve structure of the same tracer material with controllable modeling structure, the inlaid type sleeve structure is assembled and connected with the support connection material through the inlaid type sleeve structure to form a tracer release device, the tracer release device is clamped or inserted in a groove or a pipe network space of an underground tool, the size of the tracer release device is larger than the size of the clamped groove or the size of the pipe network space, the size of the support connection material cannot exceed the size of the clamped groove or the size of the pipe network space, and the space parts of surface contact areas at two ends of the tracer device are in contact with the clamping groove or the pipe network extrusion pressure by the pipe network, and the supporting connecting materials are matched to transfer pressure from the tracer releasing device to the two ends to realize the extrusion connection of the tracer controllable mechanical structure materials connected with the two ends of the device so as to realize the controlled release of the tracer.
The invention also provides a preparation method of the tracer, which comprises the following steps: weighing 2 parts of 5-pyrazolone, 1 part of diethylenetriamine and 6 parts of cerium chloride or terbium chloride according to molar ratio, dissolving the 5-pyrazolone, the diethylenetriamine and the 6 parts of cerium chloride or terbium chloride in water 2 times of solute, carrying out complexation reaction, adjusting the pH value to 6-8, heating to 60-90 ℃, carrying out nitrogen flushing reaction for 2-6 hours, judging the reaction degree through uniform transparency when observing the reaction liquid is uniform, sequentially adding 2 parts of bromopentafluorobenzene, sequentially adding 400 g of micron graphite powder accounting for 20% of the weight of water to form liquid A, equally dividing the liquid A into three parts, recording the three parts as A1, A2 and A3 for later use, and further controlling the release speed of the components under the condition that a tracing component formed by the reaction is matched with a mechanical structure material;
secondly, adding 2 parts by mole of urea into the A1 in the first step, then adding 500g of 128-epoxy resin, stirring, adding 300g of polyetheramine d400, uniformly stirring, and placing the mixture at the bottom end of the space shell model to form a surface contact area space part of the mechanical structure material with controllable functional tracing;
thirdly, before the epoxy resin in the second step is cured, adding 300g of 128-epoxy resin into the A2 solution in the first step, stirring, adding 180 g of polyetheramine d400, introducing nitrogen, stirring, adding the mixture into the middle of the space shell, slowly adding 10g of white granulated sugar aqueous solution until the reaction integral reaction solution has the viscosity of 5-8Mpa.s, and forming a central release area space part of the functional tracing controllable mechanical structure material;
the fourth step: before the epoxy resin in the third step is cured, adding half of A3 in the first step into the contact connection space part at the other end of the shell model, then adding 7g of calcium oxide, stirring and dissolving uniformly, then adding 100g of 128 epoxy resin, stirring and adding 60g of polyetheramine d400, stirring and reacting for several minutes, then adding the other half of A3 liquid into the rest part at the contact connection space part at the other end of the shell model, then stirring and adding 100g of 128 epoxy resin, stirring and adding 60g of polyetheramine d400, stirring and reacting until the reaction and curing are completed to form the contact connection space part of the functional tracing controllable mechanical structure material.
The invention also provides a method for testing the tracer, which comprises the following steps of firstly, taking the space part of the surface contact area, the space part of the central release area, and the material contacting and connecting the space part, cutting the materials into cubes of 1 cm respectively, marking the cubes a, b and c as the cubes a, b and c, and applying the cubes a, b and c to the pressure of a weight of 30 g; then, the cube slices subjected to the pressure of the 30g weight were observed under an electron microscope, and the respective gaps in the electron microscope images of the cubes a, b, and c were changed, and finally, the dissolution or dispersion rate process in water of the pressure of the 30g weight applied to the cubes a, b, and c was measured in the test environment, and the detected concentration of bromopentafluorobenzene in a certain period of time after the pressure of the 30g weight applied to the cubes a, b, and c was measured by high performance liquid chromatography.
The invention also provides a method for using the tracer, which comprises the first step of designing the size area and the occupied proportion of each part of the space part of the surface contact area of the controllable mechanical structure material, the space part of the central release area and the contact connection space part according to the release speed measured by experiments, and the second step of connecting the parts by using a supporting connection material to form extrusion connection of the mechanical structure material and clamping or inserting the extrusion connection in a downhole tool to realize controllable design and release of the tracer.
The invention also relates to an interpretation method of the tracer, which comprises the process of comprehensively analyzing and interpreting the parameters of the stratum condition by comprehensively utilizing data information obtained by monitoring various modes of rare earth elements, micron graphite powder, 5-pyrazolone and bromopentafluorobenzene.
The invention has the beneficial effects that: through the tracer material that constitutes including multiple component, use and detect simple and convenient nimble, data that can obtain through the monitoring of multiple mode carry out comprehensive analysis explanation seal stratum condition parameter, accommodation is wide, form the controllable mechanical structure material of function spike through different component cooperation molding structure device, can simply effectual card in or insert in the instrument in the pit through this material and realize the tracer and put in the use, also can realize release speed control, simultaneously through the test release speed condition, also can set up regional size of different component parts in the material and shared proportion in order to realize nimble use and control tracer release time length or effect relatively good and bad according to the demand. The invention also provides a series of related preparation, detection, use and interpretation methods with system relevance corresponding to the tracer, the material has great significance in the field of tracer materials, provides a prediction means for effective energy development, and has the effect of predicting and predicting to obtain related information for misleading energy development and environmental pollution development, and the tracer material of the invention can be used for the advanced adjustable and controllable energy development.
Drawings
FIG. 1: the composition structure of the tracer is shown in the figure;
FIG. 2: schematic diagram of the method of using the tracer of the invention;
FIG. 3: the structure performance detection result of the tracer is shown in the figure.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A new material composite adjustable tracer comprises a composite tracer material composed of 5-pyrazolone, diethylenetriamine, bromopentafluorobenzene and rare earth element compound (such as cerium chloride) for tracing detection and realizing comprehensive analysis and explanation of verified underground parameters, if the components of the tracer agent are mixed according to the mol ratio of 1:1 and then injected into the stratum for at least 10ppm, then, the occurrence condition of the tracer is monitored by sampling the stratum to know the geological parameters of the stratum, if a stratum channel exists or not, the tracer can realize the inspection and monitoring of any one or more of fluorescence, rare earth and halogen, the monitoring equipment can be various, the components, the monitoring method and the analysis method of the tracer are adjustable and controllable, the monitoring mode is flexible and changeable, for example, the on-site simple fluorescence halogen monitoring and analysis can be realized, the underground parameter analysis system can be used for indoor precise trace monitoring and analysis, and can comprehensively analyze and explain the verified underground parameters by utilizing various conditions and obtained related data.
Preferably, the tracer also comprises a component 128 of epoxy resin, polyetheramine d400, urea, micron graphite powder, white granulated sugar and calcium oxide, and the component is generated by combining, reacting and mixing. The rare earth elements comprise terbium, cerium, samarium and yttrium.
Preferably, the tracer also comprises a mechanical structure material with controllable functional tracing formed by matching the components with a modeling structure device. As shown in fig. 1, the modeling structure device is a space shell model, as shown in fig. 1, the sectional view of the space shell model is a, the component is matched with the space shell model to form a mechanical structure material with controllable function tracing, (also called modeling structure controllable tracing material) the mechanical structure material with controllable function tracing comprises matching the bottom end of the space shell model with a tracer component to form a surface contact area space part of the mechanical structure material with controllable function tracing, as shown in a in fig. 1, the bottom end of the shell model can be set into different shapes to realize the surface contact area space part 1 for generating tracer materials with different shapes, and the different shapes of the bottom end can be rectangular.
As shown in a in fig. 1, the space shell model is matched with a tracer component to form a central release area space part 2 of the mechanical structural material with controllable function tracer, the other end of the space shell model is matched with the tracer component to form a contact connection space part 3 of the mechanical structural material with controllable function tracer, the other end of the shell model is provided with a contact connection space structure as a force arm material, the contact connection space structure is an inlaid type socket joint structure, and if the contact connection space structure is in the socket joint with a projection 31 as in fig. 1, the contact connection space part of the mechanical structural material can be manufactured by matching the tracer component with the contact connection space structure.
The space part of the surface contact zone is formed by uniformly stirring and mixing 5-pyrazolone, diethylenetriamine, cerium chloride, urea, bromopentafluorobenzene, graphite powder, 128-epoxy resin and polyetheramine d400 so as to realize close contact and a contact point or a force point when the surface contact zone is inserted into a clamping sleeve of an underground tool, and simultaneously achieve the effect of relatively longer tracer release when the surface contact zone is in close contact, the space part of the central release zone of the tracer material is formed by mixing 5-pyrazolone, diethylenetriamine, cerium chloride, bromopentafluorobenzene, micron graphite powder, 128-epoxy resin and polyetheramine d400 and then gradually mixing white granulated sugar aqueous solution, and the space part of the central release zone can be provided with the tracer which is preferentially released compared with the space part of the surface contact zone by arranging the space part component structure of the central release zone.
The contact connection space part of the tracing controllable mechanical structure material or the contact connection space part of the force arm material is composed of 5-pyrazolone, diethylenetriamine, cerium chloride, bromopentafluorobenzene, graphite powder, 128 epoxy resin, polyetheramine d400 and gradually reduced mixed calcium oxide, and the calcium oxide is used to make the material become brittle or easy to age under the oxidation of the whole material and the calcium oxide structure.
The contact connection space structure is an inlaid type sleeve structure, as shown in fig. 1B, the inlaid type sleeve structure is a groove 3 and bump 31 sleeve structure, the mechanical structure material with controllable function tracing further comprises a inlaid type sleeve structure which connects the inlaid type sleeve structure of the tracing material with a controllable modeling structure with one end of a supporting connecting material 4, the supporting connecting material 4 is preferably made into a sleeved model corresponding to the inlaid type sleeve structure with certain strength through a water-soluble curing agent, the other end of the supporting connecting material 4 is connected with the inlaid type sleeve structure of the tracing material with the same controllable modeling structure, and the inlaid type sleeve structure and the supporting connecting material are assembled and connected to form a tracer releasing device (as shown in fig. 1C), the tracer releasing device C is clamped or inserted in a downhole tool, as shown in fig. 2, In fig. 2, D represents a sealer, a bell mouth, a sieve tube, or a groove or a pipe network space, the size of the tracer releasing device C is larger than the size of the groove to be clamped or the pipe network space to be inserted, the size of the supporting connecting material cannot exceed the size of the groove to be clamped or the pipe network space to be inserted, the mechanical structure material comprises various parts (a contact connecting space part, a surface contact area space part, and a central releasing area space part) formed by the modeling of a space shell and the tracer component, and the mechanical structure has the mechanical effects of bending, extrusion, support and rebound and different loose tightness of the structure of each part under the mechanical effect, so as to realize the sequential control of bending or inserting the tracer releasing device C (such as the groove in the packer) and releasing the tracer component of the clamping material, the surface contact area space parts at two ends of the tracer releasing device are in compression contact with the clamping groove or the pipe network to be inserted, and the supporting connecting material is matched to transmit pressure from the tracer releasing device to two ends to realize the extrusion or connection of the tracer controllable mechanical structure materials connected with the two ends of the device, furthermore, because the surface contact area space part, the central releasing area space part and the contact connecting space part in the tracer controllable mechanical structure materials have different components and structures, and then under the condition of combining the pressure action with each different structure space part, the structure of each different structure space part is different in loosening condition, for example, because the contact connecting space part is structurally provided with an inlaid type sleeving structure such as a sleeved groove, or because the whole stress of the contact connecting space part is weaker than that of other parts due to the use of calcium oxide in the component materials, the structure starts to loosen firstly, especially under the condition of water, the tracer is easier to dissolve and loosen firstly to realize the release, and when the tracer in the contact connecting space part is released for a certain time to the end, the space part of the central release area correspondingly starts to loosen the structure or starts to release the tracer agent after a certain time of bearing pressure or continuous bearing pressure in a certain time or combining sugar and the like in the structure in water, oxygen or bacteria, and finally starts to release under the action of combining the structure of the space part of the contact area and component materials with the outside under different conditions or combined action in the same way after a certain time when the space part of the central release area is released quickly, so that the controlled release of the tracer agent is realized.
The following illustrates a method for preparing the tracer of the present invention, comprising a first step of: firstly, weighing 2 parts of 5-pyrazolone, 1 part of diethylenetriamine and 6 parts of cerium chloride or terbium chloride according to molar ratio, dissolving the 5-pyrazolone, the 1 part of diethylenetriamine and the 6 parts of cerium chloride or terbium chloride in water which is 2 times of the solute, carrying out complexation reaction (the mass of the water is 2 times of the mass of the 5-pyrazolone, the diethylenetriamine, the cerium chloride or the terbium chloride, the complexation reaction comprises complexation or complexation reaction), adjusting the pH value to 6-8, heating to 60-90 ℃, flushing nitrogen gas for reaction for 2-6 hours, when the reaction liquid is observed to be uniform, judging the reaction degree through uniform transparency, sequentially adding 2 parts of bromopentafluorobenzene, then adding 400 g of graphite powder (the grain diameter of the graphite powder is 0.8-106 um, selected according to stratum) which is 20% of the weight of water in sequence to form liquid A, dividing the liquid A into three parts, recording the parts as A1, A2 and A3 for later use, the release speed of the components can be further controlled under the condition that the tracer components formed by the reaction are matched with mechanical structure materials;
secondly, adding 2 parts by mole of urea into the A1 in the first step, then adding 500g of 128-epoxy resin, stirring, adding 300g of polyetheramine d400, uniformly stirring, and placing the mixture at the bottom end of the space shell model to form a surface contact area space part of the mechanical structure material with controllable functional tracing;
thirdly, before the epoxy resin in the second step is cured, adding 300g of 128-epoxy resin into the A2 liquid in the first step, stirring, adding 180 g of polyetheramine d400, introducing nitrogen, stirring, adding the mixture into the middle of the space shell model, slowly adding 10g of white granulated sugar water (the concentration of the white granulated sugar is 30%, wherein the white granulated sugar is selected from American chemical products) solution, reacting the whole reaction solution to the viscosity of 5-8Mpa.s, forming a space part of a central release area of the mechanical structure material with controllable function tracing, and adding the affinity of the material and water by using urea;
the fourth step: before the epoxy resin in the third step is cured, half of A3 in the first step is added into the other end of the shell molding, then 7g of calcium oxide is added and stirred to be dissolved uniformly, then 7g of calcium oxide is added to reduce the viscosity of the material, the release rate is increased, 100g of 128 epoxy resin is added, 60g of polyetheramine d400 is added and stirred to react for a plurality of minutes, then the other half of A3 liquid is added into the other end of the shell molding, then 100g of 128 epoxy resin is added and stirred, 60g of polyetheramine d400 is added and stirred to react until the reaction and curing are completed to form a contact connection space part of the mechanical structure material with controllable functional tracing, and the contact connection space part is preferably shaped as a groove, such as 31 in A in figure 1.
In addition, the method also comprises the step of using the modeling structure device of the invention to model the space shell and form a plurality of mechanical structure materials with controllable functional tracing finally after the four steps, and the section of the appearance modeling is shown as a graph in A in figure 1. Then, the first functional tracing controllable mechanical structure material is nested and connected with a supporting connecting material 4 which is made into a sleeved circular groove (shown as 41 in B in figure 1) with certain strength and corresponding to the inlaid type sleeving structure through curing of a water-soluble curing agent, and the sleeved circular groove (shown as 42 in B in figure 1) corresponding to the other end of the supporting connecting material 4 which corresponds to the inlaid type sleeving structure is also nested and connected with another functional tracing controllable mechanical structure material to finally form a preferred tracer releasing device (shown as C in figure 1). In addition, one or two of the chlorides are selected from the above description, and the use of other rare earth chlorides will be known to those skilled in the art.
The invention also provides a method for testing the release speed of the tracer, which is based on the principle that the release speeds of the surface contact area space part, the central release area space part and the contact connection space part in a test environment are different; the specific test method comprises the following steps: firstly, taking a surface contact region space part, a central release region space part and a contact connection space part, cutting materials of the surface contact region space part, the central release region space part and the contact connection space part into cubes of 1 cm, marking the cubes a, b and c as the surface contact region space part cube, the central release region space part cube and the contact connection space part cube, and applying pressures of the cubes a, b and c to a weight of 30g respectively; then, a pressure cube slice applied to a weight of 30g is respectively observed under an electron microscope (preferably, a VHX-7000 series electron microscope), as can be seen from FIG. 3, the change of the respective gaps in the electron microscope images of the cube a, the cube b and the cube c is shown as FIG. 3, and the spatial parts of the materials corresponding to the cube a, the cube b and the cube c are shown as 1, 2 and 3 in the figure, and as can be seen from FIG. 3, the structures of the surface contact region spatial part, the central release region spatial part and the contact connection spatial part become thick, the inside becomes loose, the gaps become large, which shows that the respective structures become loose and loose relatively, and the compactness becomes small; finally, testing the process of dissolving or dispersing speed of the cube 1, the cube b and the cube c in water by applying pressure of 30g weight in a testing environment, specifically comprising the steps of putting the cube a, the cube b and the cube c in formation water at 50 ℃ (the same testing conditions) when the surface contact area space part, the center release area space part and the material contacting and connecting the space part have different dispersing effects or releasing speeds when the material acts with water molecules, applying the pressure of 30g weight on the cube b and the cube c, using the pressure after 1 week, testing the structure of the structure, the tracer was also detected.
Bromopentafluorobenzene, comprising: detecting the bromopentafluorobenzene concentration of the cubes a, b and C in a certain time after applying a pressure of 30g weight by using a high performance liquid chromatography, specifically, adopting the following method in formation water to test by using the following instruments and equipment, including an Agilent 1260 high performance liquid chromatograph, an Agilent ZORBAX eclipse XDB-C18 chromatographic column, and adopting acetonitrile-water (volume ratio is 75: 25); flow rate: 0.5 mL/min; detection wavelength: 254 nm; sample introduction volume: 10 mu L of the solution; column temperature: preparing a standard curve of bromopentafluorobenzene at 40 ℃, and testing the bromopentafluorobenzene by taking a sample of a cube a, a cube b and a cube c in formation water for 1 week and a sample of 6 months after applying a pressure of 30g weight; the results are shown in Table 1 below
TABLE 1
| Bromopentafluorobenzene | Stratum water sample of cube a | Stratum water sample of cube b | Cubic c |
| 1 week | 0.07mg/L | Can not be detected | Can not be detected |
| 6 month | Can not be detected | 1.63 mg/L | Can not be detected |
It can be known from the table that different positions of the mechanical structure material with controllable tracing are different in structure and composition and different in structure loosening change under different forces, and different in time and effect for releasing the tracing agent under the action of water, the structure embodied by the experiment is that the space parts of the materials corresponding to the cube a, the cube b and the cube c become thick, the gap becomes large, and the corresponding release speed after the installation action in the stratum water environment becomes slow and fast.
The present invention also provides a method of using a tracer material, in which the tracer material is used in a tracer release apparatus, in which the ratio of the location and size of the various parts is set to achieve rate control in accordance with the above test.
The method of using the tracer material of the invention is described below. The controllable tracer controlled design and release method comprises the steps of firstly, designing the size area and the occupied proportion of each part of the controllable mechanical structure material surface contact area space part, the central release area space part and the contact connection space part according to the release speed measured by experiments, and secondly, connecting the parts by using a supporting connecting material to form the extrusion connection of the mechanical structure material and clamping or inserting the mechanical structure material in a downhole tool to realize the controllable design and release of the tracer. Preferably, the release speed measured by the above experiment is measured by the experiment that the surface contact area space part, the central release area space part and the contact connection space part are respectively under the shape of the trapezoid, the inlaid type socket joint structure of the contact connection space part is a circular concave nested joint structure, and the contact connection space part is combined with the support connection material to clamp the parts after connection and clamp the parts in the pipe network space of a downhole tool such as a packer sieve pipe to realize the test after extrusion connection and installation, the test method can adopt the method provided by the invention, for example, the surface contact area space part, the central release area space part and the time period for releasing the tracer agent of the contact connection space part are respectively 1 to 5 months, 5 to 12 months and 11 to 20 months, the surface contact area space part, the central release area space part and the area size and the occupied ratio of the contact connection space part are set to be 1:1: 1:1, and the surface contact area space part, the central release area space part and the contact connection space part are made into controllable mechanical structure materials according to the area ratio of the composition areas of 1:1:1, an inlaid type sleeve joint structure of the controllable mechanical structure materials is connected with one end of a supporting connection material in an inlaid type sleeve joint mode, one end of the supporting connection material is connected with an inlaid type sleeve joint structure of a controllable tracer material with the same modeling structure, the inlaid type sleeve joint structure and the supporting connection material are assembled and connected to form a tracer release device, the tracer device is clamped in a groove of a packer or inserted in a net groove of an underground sieve tube, the integral length or size of the tracer device and the supporting connection material does not exceed the length or size of the groove or the size of the underground sieve tube groove, the size of the tracer release device is adjusted through the size of the supporting connection material, and the supporting connection material is a curing agent which has certain strength and is not easy to dissolve in water, such as a curing agent formed from 128 epoxy resin and polyetheramine d400, which does not participate in the other components.
The invention also provides a tracer interpretation method, which is characterized by comprising the following steps: the method comprises the process of comprehensively utilizing data information obtained by monitoring rare earth, micron graphite powder and pyrazolone bromopentafluorobenzene in various modes to comprehensively analyze and explain the evidence.
Further, whether stratum channels exist or not is obtained through analyzing qualitative and quantitative data of rare earth elements by using an inductively coupled plasma mass spectrometry, whether graphite powder appears or not is observed by using a microscope, the size of the stratum rock voidage and the proportion of the voidages in different sizes are judged according to the quantity after the graphite powder appears, and then a chromatograph is used for monitoring the content of fluorobenzene in water and oil to judge the total water-oil ratio of the stratum channels or the voids. The explanation of the condition of the formation channel is that the data information obtained by monitoring the rare earth elements, the micron graphite powder and the pyrazolone bromopentafluorobenzene in various modes is used for carrying out evidence analysis on the related parameters such as the size of the formation channel.
To sum up: through the tracer material that constitutes including multiple component, use and detect simple and convenient nimble, data that can obtain through the monitoring of multiple mode carry out comprehensive analysis explanation seal stratum condition parameter, accommodation is wide, form the controllable mechanical structure material of function spike through different component cooperation molding structure device, can simply effectual card in or insert in the instrument in the pit through this material and realize the tracer and put in the use, also can realize release speed control, simultaneously through the test release speed condition, also can set up regional size of different component parts in the material and shared proportion in order to realize nimble use and control tracer release time length or effect relatively good and bad according to the demand. The material has great significance in the field of tracer materials, so that a prediction means for effective development of energy is provided, and the material has the functions of predicting and understanding the stratum conditions of prediction of energy misleading development and environmental pollution development.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention shall fall within the protection scope defined by the claims of the present invention.
Claims (7)
1. The new material composite adjustable tracer is characterized in that the components comprise 5-pyrazolone, diethylenetriamine, bromopentafluorobenzene and a compound of rare earth elements;
the components also comprise 128 epoxy resin, polyetheramine d400, urea, micron graphite powder, white granulated sugar and calcium oxide;
the rare earth elements comprise terbium, cerium, samarium and yttrium;
the component is matched with a modeling structure device to form a mechanical structure material with controllable functional tracing, the modeling structure device is a space shell model, the component is matched with a space shell model to form a mechanical structure material with controllable functional tracing, and the mechanical structure material with controllable functional tracing comprises a surface contact area space part which is formed by matching the bottom end of the space shell model with a tracer component; the space shell is shaped, the middle of the space shell is matched with the tracer component to form the space part of the central release area of the mechanical structural material with controllable function tracing, and the other end of the space shell is matched with the tracer component to form the space part for contact connection of the mechanical structural material with controllable function tracing.
2. The tracer of claim 1, wherein:
the space part of the surface contact zone is formed by uniformly stirring and mixing 5-pyrazolone, diethylenetriamine, cerium chloride, urea, bromopentafluorobenzene, micron graphite powder, 128-epoxy resin and polyetheramine d400, the space part of the central release zone of the tracing controllable mechanical structure material is formed by mixing 5-pyrazolone, diethylenetriamine, cerium chloride, bromopentafluorobenzene, micron graphite powder, 128-epoxy resin and polyetheramine d400 and then gradually mixing a white granulated sugar aqueous solution, and the contact connection space part of the tracing controllable mechanical structure material is formed by 5-pyrazolone, diethylenetriamine, cerium chloride, bromopentafluorobenzene, micron graphite powder, 128-epoxy resin, polyetheramine d400 and calcium oxide.
3. A tracer according to any of claims 1-2, wherein: but contact space portion is the mosaic type cup joint structure, but the controllable mechanical structure material of function spike still includes can mosaic type cup joint structure and is connected with the one end that supports connecting material, supports connecting material's the other end and connects the same mosaic type cup joint structure, through mosaic type cup joint structure with support connecting material equipment connection and form tracer release, tracer release card in or insert in recess or pipe network space of instrument in the pit, the size of tracer release who props up is greater than by the card recess or inserted pipe network space size, the size that supports connecting material can not exceed by the card recess or inserted pipe network space size, the surface contact area space portion at tracer device both ends with the draw-in groove or by the crowded press contact of intubate net, and the cooperation support connecting material from tracer release to both ends transmission pressure realization to the controllable mechanical structure material of tracer of device both ends connection The connection is pressed to achieve a controlled release of the tracer.
4. A method of producing a tracer according to any of claims 1-2, wherein: the first step is as follows: weighing 2 parts of 5-pyrazolone, 1 part of diethylenetriamine and 6 parts of cerium chloride or terbium chloride according to molar ratio, dissolving the 5-pyrazolone, the 1 part of diethylenetriamine and the 6 parts of cerium chloride or terbium chloride in water 2 times of solute to perform complexation reaction, adjusting the pH value to 6-8, heating to 60-90 ℃, filling nitrogen to react for 2-6 hours, judging the reaction progress degree through uniform transparency when observing the reaction liquid is uniform, sequentially adding 2 parts of bromopentafluorobenzene, then sequentially adding 400 g of micron graphite powder accounting for 20% of the weight of water to form liquid A, and equally dividing the liquid A into three parts, namely liquid A1, liquid A2 and liquid A3 for later use;
secondly, adding 2 parts by mole of urea into the A1 obtained in the first step, then adding 500g of 128-epoxy resin, stirring, adding 300g of polyetheramine d400, uniformly stirring, and placing the mixture at the bottom end of the space shell model to form a surface contact area space part of the mechanical structure material with controllable functional tracing;
thirdly, before the epoxy resin in the second step is cured, adding 300g of 128-epoxy resin into the A2 solution in the first step, stirring, adding 180 g of polyetheramine d400, introducing nitrogen, stirring, adding the mixture into the middle of the space shell, slowly adding 10g of white granulated sugar aqueous solution until the reaction integral reaction solution has the viscosity of 5-8Mpa.s, and forming a space part of a central release area of the mechanical structure material with controllable function tracing;
the fourth step: before the epoxy resin in the third step is cured, adding half of A3 in the first step into the contact connection space part at the other end of the shell model, then adding 7g of calcium oxide, stirring and dissolving uniformly, then adding 100g of 128 epoxy resin, stirring and adding 60g of polyetheramine d400, stirring and reacting for several minutes, then adding the other half of A3 liquid into the rest part of the contact connection space part at the other end of the shell model, then stirring and adding 100g of 128 epoxy resin, stirring and adding 60g of polyetheramine d400, stirring and reacting until the reaction and curing are completed to form the contact connection space part of the functional tracing controllable mechanical structure material.
5. A method of testing a tracer according to any of claims 1-2, wherein: firstly, taking a surface contact region space part, a central release region space part and a contact connection space part, respectively cutting materials into 1 cm cubes, marking as a surface contact region space part cube a, a central release region space part cube b and a contact connection space part cube c, and respectively applying pressures of the cubes a, the cubes b and the cubes c to a weight of 30 g; then, the cube slices subjected to the pressure of the 30g weight were observed under an electron microscope, and the respective gaps in the electron microscope images of the cubes a, b, and c were changed, and finally, the dissolution or dispersion rate process in water of the pressure of the 30g weight applied to the cubes a, b, and c was measured in the test environment, and the detected concentration of bromopentafluorobenzene in a certain period of time after the pressure of the 30g weight applied to the cubes a, b, and c was measured by high performance liquid chromatography.
6. A method of using a tracer according to any of claims 1-2, wherein: the controllable tracer controlled design and release method comprises the steps of firstly, designing the size area and the occupied proportion of each part of the controllable mechanical structure material surface contact area space part, the central release area space part and the contact connection space part according to the release speed measured by experiments, and secondly, connecting the parts by using a supporting connecting material to form the extrusion connection of the mechanical structure material and clamping or inserting the mechanical structure material in a downhole tool to realize the controllable design and release of the tracer.
7. A method of interpreting a tracer according to any of claims 1-2, wherein: the method comprises the process of comprehensively analyzing and explaining the parameters of the verified stratum condition by comprehensively utilizing data information obtained by monitoring various modes of rare earth elements, micron graphite powder, 5-pyrazolone and bromopentafluorobenzene.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101589003A (en) * | 2006-09-21 | 2009-11-25 | 雷恩国家应用科学学院 | Method for labelling a material comprising at least one non-organic matrix and corresponding material |
| CN103588801A (en) * | 2013-12-02 | 2014-02-19 | 天津大港油田圣达科技有限公司 | Trace element well-to-well tracer agent use method |
| CN109667574A (en) * | 2017-10-13 | 2019-04-23 | 中国石油化工股份有限公司 | A kind of multistage pressure break metal ion tracer and its application |
| CN109931052A (en) * | 2019-03-19 | 2019-06-25 | 固安国勘石油技术有限公司 | Utilize the method for effect and production capacity situation after tracer monitoring oil well delamination or staged fracturing |
-
2019
- 2019-12-29 CN CN201911386797.2A patent/CN111007093B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101589003A (en) * | 2006-09-21 | 2009-11-25 | 雷恩国家应用科学学院 | Method for labelling a material comprising at least one non-organic matrix and corresponding material |
| CN103588801A (en) * | 2013-12-02 | 2014-02-19 | 天津大港油田圣达科技有限公司 | Trace element well-to-well tracer agent use method |
| CN109667574A (en) * | 2017-10-13 | 2019-04-23 | 中国石油化工股份有限公司 | A kind of multistage pressure break metal ion tracer and its application |
| CN109931052A (en) * | 2019-03-19 | 2019-06-25 | 固安国勘石油技术有限公司 | Utilize the method for effect and production capacity situation after tracer monitoring oil well delamination or staged fracturing |
Non-Patent Citations (4)
| Title |
|---|
| Experimental research of the tracer characteristic curves for fracture-cave structures in a carbonate oil and gas reservoir;Yuanshuai Rong等;《Journal of Natural Gas Science and Engineering》;20160430;全文 * |
| 油田示踪剂技术;于瑞香等;《工业水处理》;20070831;第13-15页 * |
| 油田示踪剂监测技术;龚山华;《化学工程与装备》;20170331;4示踪剂的检测，5 结语 * |
| 缓释型长效固体示踪剂研究;温守国等;《天津科技》;20180630;全文 * |
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