CN113980675A - Petroleum tracer agent, application thereof and oil field tracing method - Google Patents
Petroleum tracer agent, application thereof and oil field tracing method Download PDFInfo
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Abstract
The invention discloses a petroleum tracer, which is a phosphorescent carbon quantum dot, wherein the phosphorescent carbon quantum dot comprises a carbon quantum dot body and a loading agent, and the phosphorescent carbon quantum dot has a phosphorescent characteristic. The petroleum tracer has the phosphorescence property, the phosphorescence service life of the petroleum tracer reaches millisecond level, and the detection limit of the petroleum tracer can reach 0.3 ppm; the petroleum tracer with the phosphorescence performance is used, so that the interference of petroleum autofluorescence can be effectively avoided, the detection sensitivity is improved, and the environment-friendly effect is achieved; phosphorescent carbon quantum dots with different phosphorescent lifetimes are simultaneously applied to the field of petroleum tracing, and the luminescent peak positions of the phosphorescent carbon quantum dots can be conveniently distinguished, so that the detection efficiency and accuracy are greatly improved; the oil field tracing method can accurately detect the communication condition of the oil well and provide a detection basis for oil well surveying.
Description
Technical Field
The invention belongs to the field of detection and analysis, and particularly relates to a petroleum tracer and application thereof, and an oil field tracing method.
Background
The tracer has great significance for exploitation, design, crosslinking condition and later adjustment of oil fields and water wells, and common tracers in the prior art mainly comprise dye tracers, chemical tracers, radioactive isotopes, trace substances and the like, but have various defects respectively, so that the application of the tracers is limited. For example, the dye tracer has strong adsorbability and large dosage; chemical tracers, such as ammonium nitrate, ammonium thiocyanate and the like, have high cost, are easy to adsorb by rocks, have large detection error, low test resolution, poor adaptability and selectivity and have environmental and safety problems; the radioactive isotope has strong radioactivity, complicated analysis and test means and high cost, and is not beneficial to large-scale popularization and application; the detection requirement is high due to the adoption of trace substances such as gadolinium, high-end analysis equipment such as inductively coupled plasma mass spectrometry is needed, and the cost is overhigh.
In summary, there is a need to find an environmentally friendly petroleum tracer and oil field tracing method with simple preparation method, long service life and strong anti-interference capability.
Disclosure of Invention
In view of the above, the present invention aims to provide a petroleum tracer, an application thereof, and an oil field tracing method, wherein the petroleum tracer has a long service life, a strong anti-interference capability, and is environment-friendly, and the oil field tracing method is simple and easy to operate.
In order to achieve the purpose, the invention adopts the technical scheme that:
the first purpose of the invention is to provide a petroleum tracer, wherein the petroleum tracer is a phosphorescent carbon quantum dot, the phosphorescent carbon quantum dot comprises a carbon quantum dot body and a loading agent, and the phosphorescent carbon quantum dot has a phosphorescent characteristic.
Specifically, the loading agent is a porous material, and the carbon quantum dot body is dispersed in the porous material through physical adsorption.
Preferably, the porous material comprises at least one of a polymer and an inorganic substance;
preferably, the polymer is at least one selected from the group consisting of polyethylene, polypropylene, polystyrene, polyethylene oxide, polysiloxane, polyphenylene, polythiophene, polyphenylene ethylene, polysilane, polyethylene terephthalate and polyphenylethynyl, polymethyl methacrylate, polydodeca methacrylate, polycarbonate and epoxy resin;
preferably, the inorganic substance is at least one selected from the group consisting of silicon oxide, boron-containing inorganic substance, aluminum-containing oxide, zirconium-containing oxide, titanium-containing oxide, hafnium-containing oxide, and yttrium-containing oxide.
Preferably, the loading agent is an intercalation element linked to the carbon quantum dot body by covalent bonds, and the intercalation element includes at least one of N, P, F;
preferably, the intercalation element is at least one selected from phosphoric acid, nitric acid, hydrofluoric acid, ammonium fluoride, ammonium citrate, triethylamine trihydrofluoride.
Specifically, the petroleum tracer comprises at least one of red-light phosphorescent carbon quantum dots, green-light phosphorescent carbon quantum dots and blue-light phosphorescent carbon quantum dots;
preferably, the petroleum tracer is a mixture of red phosphorescent carbon quantum dots, green phosphorescent carbon quantum dots and blue phosphorescent carbon quantum dots.
Specifically, the solubility of the petroleum tracer agent in water at 10-100 ℃ is less than 1 x 10-5g/L, solubility in petroleum greater than 1 x 102g/L。
The characterization mode of the solubility of the phosphorescent carbon quantum dots in the petroleum is similar to the dispersion degree mode, namely the phosphorescent carbon quantum dots are gradually added into a certain volume of the petroleum at normal temperature and normal pressure while stirring is carried out continuously, when the situation that the phosphorescent carbon quantum dots in the petroleum can not be dispersed and precipitates appear is observed, the adding quality of the phosphorescent carbon quantum dots is stopped, and the adding quality is divided by the volume of the petroleum, so that the solubility of the phosphorescent carbon quantum dots in the petroleum under the condition can be obtained.
Specifically, the phosphorescent carbon quantum dots of the petroleum tracer may be excited at 350 nm or more and 450nm or less.
The second purpose of the invention is to provide an application of the petroleum tracer, wherein the petroleum tracer is used for petroleum tracing detection, oil pipe leakage detection and detection of oil well communication conditions.
The third purpose of the invention is to provide an oil field tracing method, which comprises the following steps:
s1, adding the phosphorescent carbon quantum dots into an oil field injection well;
s2, obtaining an oil-water mixture at an oil field production well, and extracting an oil phase in the oil-water mixture;
and S3, detecting whether the oil phase has a phosphorescence signal or phosphorescence service life, and judging whether the oil phase has the phosphorescence carbon quantum dots.
Specifically, the method further comprises the following steps:
s4, establishing a standard curve of the concentration-phosphorescence intensity of the phosphorescent carbon quantum dots in the petroleum;
and S5, detecting the phosphorescence intensity in the oil phase, and obtaining the concentration of the phosphorescent carbon quantum dots in the oil field well corresponding to the standard curve of the concentration-phosphorescence intensity of the phosphorescent carbon quantum dots.
Compared with the prior art, the petroleum tracer and the application thereof and the oil field tracing method have the following advantages:
(1) the petroleum tracer has the phosphorescence property, the phosphorescence service life of the petroleum tracer reaches millisecond level, and the detection limit of the petroleum tracer can reach 0.3 ppm;
(2) the petroleum tracer with the phosphorescence performance is used, so that the interference of petroleum autofluorescence can be effectively avoided, the detection sensitivity is improved, and the environment-friendly effect is achieved;
(3) phosphorescent carbon quantum dots with different phosphorescent lifetimes are simultaneously applied to the field of petroleum tracing, and the luminescent peak positions of the phosphorescent carbon quantum dots can be conveniently distinguished, so that the detection efficiency and accuracy are greatly improved;
(4) the oil field tracing method can accurately detect the communication condition of the oil well and provide a detection basis for oil well surveying.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram relating to example 1:
(a) a graph of the change in phosphorescence intensity of phosphorescent carbon quantum dots with standing time;
(b) a graph of the variation of the phosphorescence intensity of the phosphorescent carbon quantum dots with the irradiation time of the ultraviolet lamp;
(c) a graph of the change of phosphorescence intensity of the mixed phosphorescent carbon quantum dots and petroleum along with heating time;
(d) a standard curve of the concentration value of the phosphorescent carbon quantum dots and the phosphorescent intensity value;
(e) a phosphorescence lifetime map of phosphorescent carbon quantum dots;
FIG. 2 is a schematic diagram relating to example 2:
(a) a graph of the change in phosphorescence intensity of phosphorescent carbon quantum dots with standing time;
(b) a graph of the variation of the phosphorescence intensity of the phosphorescent carbon quantum dots with the irradiation time of the ultraviolet lamp;
(c) a graph of the change of phosphorescence intensity of the mixed phosphorescent carbon quantum dots and petroleum along with heating time;
(d) a standard curve of the concentration value of the phosphorescent carbon quantum dots and the phosphorescent intensity value;
(e) a phosphorescence lifetime map of phosphorescent carbon quantum dots;
FIG. 3 is a diagram relating to example 3:
(a) a graph of the change in phosphorescence intensity of phosphorescent carbon quantum dots with standing time;
(b) a graph of the variation of the phosphorescence intensity of the phosphorescent carbon quantum dots with the irradiation time of the ultraviolet lamp;
(c) a graph of the change of phosphorescence intensity of the mixed phosphorescent carbon quantum dots and petroleum along with heating time;
(d) a standard curve of the concentration value of the phosphorescent carbon quantum dots and the phosphorescent intensity value;
(e) a phosphorescence lifetime map of phosphorescent carbon quantum dots;
FIG. 4 is a diagram relating to example 4:
(a) a graph of the change in phosphorescence intensity of phosphorescent carbon quantum dots with standing time;
(b) a graph of the variation of the phosphorescence intensity of the phosphorescent carbon quantum dots with the irradiation time of the ultraviolet lamp;
(c) a graph of the change of phosphorescence intensity of the mixed phosphorescent carbon quantum dots and petroleum along with heating time;
(d) a standard curve of the concentration value of the phosphorescent carbon quantum dots and the phosphorescent intensity value;
FIG. 5-a is a graph showing the change of the petroleum fluorescence signal before and after the addition of the fluorescent carbon quantum dots in comparative example 1;
FIG. 5-b is a graph of phosphorescence signals for any phosphorescent carbon quantum dot of the present invention mixed with petroleum.
Detailed Description
The technical solutions in the examples will be described in detail below with reference to the embodiments of the present application. It should be noted that this embodiment is only a partial way, not a complete one.
As used herein, a statement such as "at least one (one)" modifies an entire list of elements as it precedes or succeeds the list of elements without modifying individual elements of the list. Unless otherwise defined, all terms (including technical and scientific terms) in the specification may be defined as commonly understood by one of ordinary skill in the art. Terms defined in commonly used dictionaries should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and the present disclosure, and may not be interpreted in an idealized or overly formal sense unless expressly so defined. Furthermore, unless expressly stated to the contrary, the terms "comprises" and "comprising," when used in this specification, specify the presence of stated features, regions, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, regions, integers, steps, operations, elements, components, and/or groups thereof. Thus, the above wording will be understood to mean that the stated elements are included, but not to exclude any other elements.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. The term "or" means "and/or".
It will be understood that, although the terms first, second, third, etc. may be used herein to describe various elements, components, regions, layers and/or sections, these elements, components, regions, layers and/or sections should not be limited by these terms.
As used herein, "about" or "approximately" includes the stated value and is meant to be within an acceptable range of deviation for the particular value as determined by one of ordinary skill in the art in view of the measurement in question and the error associated with measurement of the particular quantity (i.e., limitations of the measurement system). For example, "about" may mean a deviation from the stated value within one or more standard deviation ranges, or within ± 10%, ± 5%.
In order to solve the problems that the petroleum tracer in the prior art is poor in anti-interference capability, high in cost, complex in preparation method, not environment-friendly, incapable of eliminating petroleum autofluorescence interference and the like, the invention researches a petroleum tracer.
The petroleum tracer is a phosphorescent carbon quantum dot which has phosphorescence. The petroleum tracer has phosphorescence characteristics that phosphorescent carbon quantum dots form an excited triplet state (or an excited triplet state) after being excited by radiation, and when the excited triplet state with high energy is transited to a ground state with low energy, energy is released and phosphorescence is emitted, wherein the phosphorescence is afterglow still visible to the naked eye after the radiation is finished. Aromatic carbonyl compounds on the surface of the carbon quantum dot are the origin of triplet excited states, but are easily affected by non-radiative decay caused by thermal and collision processes, and are extremely sensitive to oxygen in the air, and need to participate in a loading agent to show phosphorescent properties.
In order to prevent the quenching effect of the phosphorescent material, the phosphorescent carbon quantum dot comprises a carbon quantum dot body and a loading agent, and the carbon quantum dot can effectively prevent the quenching effect of the petroleum tracer by virtue of the action of the loading agent.
The loading agent can be a porous material or an embedded element connected with the carbon quantum dot body through a covalent bond.
When the loading agent is a porous material, the carbon quantum dot bodies are dispersed in the porous material through physical adsorption. The porous material comprises at least one of polymer and inorganic substance.
The polymer is one or more selected from polyethylene, polypropylene, polystyrene, polyoxyethylene, polysiloxane, polyphenylene, polythiophene, polyphenylene ethylene, polysilane, polyethylene terephthalate and polyphenylethynyl, polymethyl methacrylate, polydodecamethacrylate, polycarbonate and epoxy resin; the inorganic substance is one or more selected from silicon oxide, boron-containing inorganic substance, aluminum-containing oxide, zirconium-containing oxide, titanium-containing oxide, hafnium-containing oxide or yttrium-containing oxide.
When the loading agent is an intercalation element covalently linked to the carbon quantum dot body, the intercalation element includes at least one of N, P, F; the intercalation element is at least one selected from phosphoric acid, nitric acid, hydrofluoric acid, ammonium fluoride, ammonium citrate, triethylamine, and hydrogen trifluoride. The embedding of the embedding element is beneficial to regulating and controlling the triplet state energy level structure of the carbon quantum dot body, so that the phosphorescent carbon quantum dot with stable phosphorescence characteristics is formed.
The solubility of the petroleum tracer in water at 10-100 deg.C is less than 1 × 10-5g/L, solubility in petroleum greater than 1 x 102g/L. The characterization mode of the solubility of the phosphorescent carbon quantum dots in the petroleum is similar to the dispersion degree mode, namely the phosphorescent carbon quantum dots are gradually added into a certain volume of the petroleum at normal temperature and normal pressure while stirring is carried out continuously, when the situation that the phosphorescent carbon quantum dots in the petroleum can not be dispersed and precipitates appear is observed, the adding quality of the phosphorescent carbon quantum dots is stopped, and the adding quality is divided by the volume of the petroleum, so that the solubility of the phosphorescent carbon quantum dots in the petroleum under the condition can be obtained.
The application of the petroleum tracer agent is beneficial to use in the oil phase, can effectively avoid the adsorption interference of water, and improves the accuracy of tracing detection. The petroleum tracer in the application can be used for petroleum tracing detection or oil pipe leakage detection or detection of oil well communication conditions.
In a specific embodiment, the petroleum tracer of the present application can be used for oil phase tracing, oil pipe leak detection or oil well communication detection, and the oil phase of the present application means that the liquid to be detected is petroleum. When the petroleum tracer is used for oil pipe leakage detection, phosphorescent carbon quantum dots are gathered at an oil leakage position, and at the moment, two obvious points can be seen by using illumination, so that the oil leakage position is detected; when the petroleum tracer is used for oil well communication detection, the petroleum tracer is put into any oil well, and after a certain time, the phosphorescent carbon quantum dots are sampled from other oil wells for phosphorescent detection, so that the communication condition among the oil wells is judged.
The petroleum tracer is easily dispersed in petroleum, and can detect the phosphorescence service life and the phosphorescence intensity in a phosphorescence carbon quantum dot flowing area along with the flow of the petroleum, and the flow direction and the flow rate of the petroleum are detected by means of the movement track and the content of the phosphorescence carbon quantum dot.
In one embodiment of the present application, the phosphorescent carbon quantum dots may be excited at 350 nm or more and 450nm or less. The excitable wavelength band can be used for judging the service life of the phosphorus-free optical signal or the phosphorescence by using an instrument. When the blue light phosphorescence carbon quantum dots are used, the phosphorescence service life is longer, the identification time of human eyes is exceeded, phosphorescence signals can be observed by naked eyes, and the operation is more convenient.
The carbon quantum dots can be prepared by a microwave method or a solvothermal method; the preparation of the carbon quantum dots can be realized by adopting a conventional preparation method in the prior art.
The phosphorescent carbon quantum dots include at least one of red phosphorescent carbon quantum dots, green phosphorescent carbon quantum dots, and blue phosphorescent carbon quantum dots. Phosphorescent materials with different colors are excited at different wavelengths, so that the spectrum superposition problem can be effectively eliminated, and the detection efficiency is improved. The red light phosphorescent carbon quantum dots, the green light phosphorescent carbon quantum dots and the blue light phosphorescent carbon quantum dots are simultaneously applied to the petroleum tracing field, the phosphorescent carbon quantum dots with different phosphorescent service lives are simultaneously applied to the petroleum tracing field, the phosphorescent carbon quantum dots are conveniently distinguished from each other in the light-emitting peak position, and the detection efficiency and accuracy are greatly improved.
In addition, the use of the phosphorescent material prolongs the light-emitting time window, and avoids the fluorescent material or the self-fluorescence influence of petroleum; the phosphorescence lifetime value of the phosphorescence material is much longer than the fluorescence lifetime value of the fluorescence material. The two characteristics enable the application of the phosphorescent carbon quantum dots to have wider application fields than the fluorescent carbon quantum dots.
The invention also provides an application of the petroleum tracer, which is used for petroleum tracing detection, oil pipe leakage detection and detection of oil well communication conditions.
The invention provides an oil field tracing method, which comprises the following steps:
s1, adding the phosphorescent carbon quantum dots into an oil field injection well;
s2, obtaining an oil-water mixture at an oil field production well, and extracting an oil phase in the oil-water mixture;
and S3, detecting whether the oil phase has a phosphorescence signal or phosphorescence service life, and judging whether the oil phase has the phosphorescence carbon quantum dots.
The method can be used for oil phase tracing, oil pipe leakage detection and detection of oil well communication conditions. This is a very simple method as a qualitative characterization of oil.
In another embodiment of the present application, the method for oilfield tracing further comprises the steps of:
s4, establishing a standard curve of the concentration-phosphorescence intensity of the phosphorescent carbon quantum dots in the petroleum;
and S5, detecting the phosphorescence intensity in the oil phase, and obtaining the concentration of the phosphorescent carbon quantum dots in the oil field well corresponding to the standard curve of the concentration-phosphorescence intensity of the phosphorescent carbon quantum dots.
The present application will be described in detail below with specific examples and comparative examples:
example 1
1. Preparation of blue light phosphorescent carbon quantum dots (petroleum tracer):
ultrasonically dissolving 1.5g of urea, 0.5g of citric acid, 0.2mL of phosphoric acid and 10mL of water to obtain a mixed solution, then putting the mixed solution into a microwave oven, setting the microwave power to be 800W, reacting for 5min, after the reaction is finished, centrifuging the obtained liquid for 10min at a rotating speed, centrifuging and washing for 3 times under the same condition to obtain a white solid, putting the white solid into a freezer, and finally freeze-drying by using a freeze dryer to obtain the blue light carbon quantum dots of white solid powder.
Dispersing the obtained blue light carbon quantum dots in ethanol again, then adding 2mL of polyethylene glycol 600 and 1.0g of boric acid, then carrying out a dissolution thermal reaction at the temperature of 180 ℃ for 6h, naturally cooling to room temperature after the reaction is finished, carrying out centrifugal treatment on the obtained solution, removing supernatant, collecting bottom sediment, then washing the sediment with distilled water, and finally freeze-drying the obtained substrate to obtain the blue light phosphorescent carbon quantum dots, namely the petroleum tracer.
2. Stability testing of petroleum tracers:
2.1 air stability
The phosphorescent carbon quantum dots are placed in the air, the change of the phosphorescent intensity of the phosphorescent carbon quantum dots along with the placing time is tested under the conditions of room temperature and normal pressure, the phosphorescent intensity of the phosphorescent carbon quantum dots is tested at different times, and the result is shown in figure 1-a. The phosphorescent carbon quantum dots are still found to have the phosphorescence intensity more than 98% of the initial value after being placed for 400 min.
2.2 UV stability
The UV stability of the phosphorescent carbon quantum dots was tested. Placing the phosphorescent carbon quantum dots under an ultraviolet lamp with the power of 20W to continuously irradiate the phosphorescent carbon quantum dots, and testing and recording the phosphorescent intensity at different moments to obtain a graph of the change of the phosphorescent intensity along with the irradiation time of the ultraviolet lamp, as shown in fig. 1-b. And testing the phosphorescence intensity of the phosphorescence carbon quantum dots at different time respectively, wherein the phosphorescence intensity is still kept above 96% of the initial value after the phosphorescence carbon quantum dots are irradiated by an ultraviolet lamp for 400 min.
2.3 internal stability of Petroleum
0.5g of phosphorescent carbon quantum dots and 50mL of petroleum were mixed and stirred at 65 ℃ to measure the change of phosphorescent intensity with heating time, and the results are shown in FIG. 1-c. From the stability test results, the phosphorescence intensity can still maintain more than 95% of the initial value after 168 hours.
3. Standard curve
In order to determine the specific phosphorescent carbon quantum dot concentration value in the petroleum, a standard curve of the petroleum is measured in advance, that is, a petroleum solution with known concentrations of phosphorescent carbon quantum dots is prepared, and then a phosphorescent intensity value is measured to obtain the relationship between the phosphorescent carbon quantum dot concentration value and the phosphorescent intensity value, as shown in table 1, and the obtained standard curve is shown in fig. 1-d. And (3) testing conditions are as follows: excitation wavelength: 370nm, taking 3mL of the reagent as it is, the phosphorescence spectrum is tested.
TABLE 1
From the above, the linear relation of the standard curve of the petroleum tracer of the embodiment is good, R2The value is 0.999, the phosphorescence intensity of the petroleum tracer solution is basically maintained for a long time, the detection limit is as low as 0.36mg/L, and the phosphorescence lifetime of the embodiment is 40ms as seen from FIG. 1-e.
4. The method for using the petroleum tracer to trace the oil field comprises the following steps of assuming the flow velocity when an injection well flows to a production well, ensuring the flow to be consistent, and ensuring that the concentration of the tracer in the production well is stable and does not change when the production well samples:
the method for measuring connectivity among oil wells by using the petroleum tracer of the embodiment comprises the following specific steps: weighing 5kg of petroleum tracer to prepare a petroleum solution with a certain concentration, adding the petroleum solution into an injection well, sampling in the injection well, and measuring the phosphorescence intensity to obtain the concentration of the tracer of 10 ppm; after the petroleum tracer is injected for a period of time, sampling is respectively carried out on the No. 1, No. 2 and No. 3 extraction wells, the phosphorescence intensity of sample liquid in the three extraction wells is measured at regular time, the concentration of the tracer in the No. 1 is finally measured to be 2ppm, no tracer is detected in the No. 2, the concentration of the tracer in the No. 3 is 1ppm, the injection well can be known to be respectively communicated with the No. 1 and No. 3 extraction wells, but not communicated with the No. 2 extraction well, and then the use of the injection well can be reasonably planned as required.
Example 2
1. Preparation of green phosphorescent carbon quantum dots (petroleum tracer):
0.3g of pseudo-boehmite, 0.17g of manganese acetate tetrahydrate and 0.2g of boric acid were dissolved in 20mL of deionized water, and 0.56mL of phosphoric acid and 1.5g of triethylenetetramine were added, followed by placing the mixed solution in a high-temperature reaction vessel and reacting at 180 ℃ for 10 hours. And after the reaction is finished, centrifuging the obtained solution, washing the substrate by using distilled water, and drying at 80 ℃ to obtain green phosphorescent carbon quantum dot powder.
2. Stability testing of petroleum tracers:
2.1 air stability
The phosphorescent carbon quantum dots are placed in the air, and the change of the phosphorescence intensity of the phosphorescent carbon quantum dots along with the placing time under the conditions of room temperature and normal pressure is tested, and the result is shown in figure 2-a. The phosphorescent carbon quantum dots are subjected to a phosphorescence intensity test, and the phosphorescence intensity is still maintained to be more than 94% of the initial value after the phosphorescent carbon quantum dots are placed for 400 min.
2.2 UV stability
And (3) testing the ultraviolet stability of the phosphorescent carbon quantum dots. Placing the phosphorescent carbon quantum dots under an ultraviolet lamp with power of 20W to continuously irradiate the phosphorescent carbon quantum dots, and recording the phosphorescent intensity at different time to obtain a graph of the change of the phosphorescent intensity value along with the irradiation time of the ultraviolet lamp, as shown in fig. 2-b. After the phosphorescent carbon quantum dots are irradiated by an ultraviolet lamp for 400min, the phosphorescence intensity still keeps more than 92% of the initial value.
2.3 internal stability of Petroleum
0.5g of phosphorescent carbon quantum dots and 50mL of petroleum are mixed, stirred at 65 ℃, and the change of the phosphorescent signal intensity value is tested at different heating times, and the result is shown in figure 2-c. From the stability test results, the phosphorescence intensity can still maintain more than 94% of the initial value after 168 hours
3. Standard curve
In order to determine the specific phosphorescent carbon quantum dot concentration value in the petroleum, a standard curve of the petroleum is measured in advance, that is, a petroleum solution with known concentrations of phosphorescent carbon quantum dots is prepared, and then a phosphorescent intensity value is measured to obtain the relationship between the phosphorescent carbon quantum dot concentration value and the phosphorescent intensity value, as shown in table 2, and the obtained standard curve is shown in fig. 2-d. And (3) testing conditions are as follows: excitation wavelength: 450nm, and 3mL of the reagent is taken as the test procedure to carry out the phosphorescence spectrum test.
TABLE 2
| Concentration ppm of | 0.7 | 14 | 70 | 140 | 280 |
| Phosphor intensity a.u. | 15 | 70 | 385 | 763 | 1442 |
From the above, the linear relation of the standard curve of the petroleum tracer of the embodiment is good, R2The value is 0.999, the phosphorescence intensity of the petroleum tracer solution is basically maintained for a long time, the detection limit is as low as 0.3mg/L, and the phosphorescence lifetime of the embodiment is 5.6ms as seen from FIG. 2-e.
4. The method for using the petroleum tracer for oil field tracing comprises the following steps:
utilize the oil tracer of this embodiment to measure connectivity between the oil well, the velocity of flow when supposing injection well flow direction extraction well this moment, the flow is unanimous, and when the extraction well was taken a sample, the concentration of tracer in the extraction well is stable no longer changes, and concrete method is: weighing 5kg of petroleum tracer to prepare a petroleum solution with a certain concentration, adding the petroleum solution into an injection well, sampling in the injection well, and measuring the phosphorescence intensity to obtain the concentration of the tracer of 5 ppm; after the petroleum tracer is injected for a period of time, sampling is respectively carried out on the No. 1, No. 2 and No. 3 production wells, the phosphorescence intensity of sample liquid in the three production wells is measured at regular time, finally, the concentration of the tracer in the No. 1 is measured to be 1ppm, no tracer is detected in the No. 2, no tracer is detected in the No. 3, and the injection well is only communicated with the No. 1 production well.
Example 3
1. Preparation of red light phosphorescent carbon quantum dots (petroleum tracer):
0.3g of pseudo-boehmite, 0.17g of manganese acetate tetrahydrate and 0.2g of boric acid were dissolved in 20mL of deionized water, and 0.56mL of phosphoric acid and 0.8mL of 2,2- (ethylenedioxy) bis (ethylamine) were added, followed by placing the mixed solution in a high-temperature reaction tank to react at 160 ℃ for 12 hours. And after the reaction is finished, centrifuging the obtained solution, washing the substrate by using distilled water, and drying at 80 ℃ to obtain red phosphorescent carbon quantum dot powder.
2. Stability testing of petroleum tracers:
2.1 air stability
The phosphorescent carbon quantum dots were placed in the air, and the change of the phosphorescence intensity of the phosphorescent carbon quantum dots with the time of placement was measured under the conditions of room temperature and normal pressure, and the result is shown in fig. 3-a. The phosphorescence intensity of the phosphorescence carbon quantum dots is tested, and the phosphorescence intensity is still kept to be more than 86% of the initial value after the phosphorescence carbon quantum dots are placed for 400 min.
2.2 UV stability
And (3) testing the ultraviolet stability of the phosphorescent carbon quantum dots. The phosphorescent carbon quantum dots are placed under an ultraviolet lamp with the power of 20W to continuously irradiate the phosphorescent carbon quantum dots, and the phosphorescence intensity is recorded at different time, so that a graph of the change of the phosphorescence intensity value along with the irradiation time of the ultraviolet lamp is obtained, and the result is shown in fig. 3-b. After the phosphorescent carbon quantum dots are irradiated by an ultraviolet lamp for 400min, the phosphorescence intensity still keeps more than 81% of the initial value.
2.3 internal stability of Petroleum
0.5g of phosphorescent carbon quantum dots and 50mL of petroleum are mixed, stirred at 65 ℃, and the change of the phosphorescent signal intensity value is tested at different heating times, and the result is shown in figure 3-c. From the stability test results, the phosphorescence intensity can still maintain more than 86% of the initial value after 168 hours.
3. Standard curve
In order to determine the specific phosphorescent carbon quantum dot concentration value in the petroleum, a standard curve is measured on the petroleum in advance, that is, a petroleum solution with known concentrations of phosphorescent carbon quantum dots is prepared, and then a phosphorescent intensity value is measured on the petroleum solution to obtain the relationship between the phosphorescent carbon quantum dot concentration value and the phosphorescent intensity value, as shown in table 3, and the obtained standard curve is shown in fig. 3-d. And (3) testing conditions are as follows: excitation wavelength: 520nm, and 3mL of reagent is taken as the test procedure to test the phosphorescence spectrum.
TABLE 3
| Concentration ppm of | 1 | 10 | 50 | 100 | 500 |
| PhosphorescenceIntensity a.u. | 18 | 60 | 225 | 403 | 1631 |
From the above, the linear relation of the standard curve of the petroleum tracer of the embodiment is good, R2The value is 0.998, the phosphorescence intensity of the petroleum tracer solution is basically maintained for a long time, the detection limit is as low as 0.32mg/L, and the phosphorescence lifetime of the embodiment is 5.2ms as seen in FIG. 3-e.
4. The method for using the petroleum tracer for oil field tracing comprises the following steps:
the method for measuring connectivity among oil wells by using the petroleum tracer in the embodiment is characterized in that the flow rate and the flow rate of the injection well flowing to the production well are consistent, and the concentration of the tracer in the production well is stable and does not change any more when the production well samples, and the method comprises the following specific steps: weighing 5kg of petroleum tracer to prepare a petroleum solution with a certain concentration, adding the petroleum solution into an injection well, sampling in the injection well, and measuring the phosphorescence intensity to obtain the concentration of the tracer of 15 ppm; after the petroleum tracer is injected for a period of time, the extraction wells 1#, 2# and 3# are respectively sampled, the phosphorescence intensity of sample liquid in the three extraction wells is measured at regular time, finally, the concentration of the petroleum tracer in the extraction well 1# is 1ppm, the concentration of the petroleum tracer in the extraction well 2# is 2ppm, and the concentration of the petroleum tracer in the extraction well 3# is 3ppm, so that the injection well is communicated with the extraction wells 1#, 2# and 3# and the use of the injection well can be reasonably planned as required.
Example 4
1. Ordinary carbon quantum dots (not containing N, P, F) were prepared and loaded in the pores of the inorganic boronic acid.
Dissolving 2g of citric acid in 10mL of deionized water, then placing the solution into a reaction kettle for hydrothermal reaction at 180 ℃ for 5h, carrying out centrifugal separation on the obtained solution after the reaction is finished, collecting supernatant to obtain a carbon quantum dot solution, and removing water in the solution by means of rotary evaporation or freeze drying to obtain carbon quantum dot powder.
Dissolving 2g of boric acid in 20mL of deionized water, then adding the synthesized 3mg of carbon quantum dots, stirring uniformly, then placing the solution into the reaction kettle again for reaction, wherein the reaction temperature is 180 ℃, the reaction time is 6 hours, and then naturally cooling to room temperature to obtain the phosphorescent carbon quantum dots.
2. Stability testing of petroleum tracers:
2.1 air stability
The phosphorescent carbon quantum dots were placed in the air, and the change of the phosphorescence intensity of the phosphorescent carbon quantum dots with the time of placement was measured under the conditions of room temperature and normal pressure, and the result is shown in fig. 4-a. The phosphorescence intensity of the phosphorescence carbon quantum dots is tested, and the phosphorescence intensity is still kept more than 90% of the initial value after the phosphorescence carbon quantum dots are placed for 420 min.
2.2 UV stability
And (3) testing the ultraviolet stability of the phosphorescent carbon quantum dots. The phosphorescent carbon quantum dots are placed under an ultraviolet lamp with the power of 20W to continuously irradiate the phosphorescent carbon quantum dots, and the phosphorescence intensity is recorded at different time, so that a graph of the change of the phosphorescence intensity value along with the irradiation time of the ultraviolet lamp is obtained, and the result is shown in fig. 4-b. After the phosphorescent carbon quantum dots are irradiated by an ultraviolet lamp for 420min, the phosphorescence intensity still keeps more than 89% of the initial value.
2.3 internal stability of Petroleum
0.5g of phosphorescent carbon quantum dots and 50mL of petroleum are mixed, stirred at 65 ℃, and the change of the phosphorescent signal intensity value is tested at different heating times, and the result is shown in figure 4-c. From the stability test results, the phosphorescence intensity can still maintain more than 91% of the initial value after 168 hours.
3. Standard curve
In order to determine the specific phosphorescent carbon quantum dot concentration value in the petroleum, a standard curve of the petroleum is measured in advance, that is, a petroleum solution with known concentrations of phosphorescent carbon quantum dots is prepared, and then a phosphorescent intensity value is measured to obtain the relationship between the phosphorescent carbon quantum dot concentration value and the phosphorescent intensity value, as shown in table 4, and the obtained standard curve is shown in fig. 4-d. And (3) testing conditions are as follows: excitation wavelength: 450nm, and 3mL of the reagent is taken as the test procedure to carry out the phosphorescence spectrum test.
TABLE 3
| Concentration ppm of | 0.5 | 5 | 50 | 250 | 500 |
| Phosphor intensity a.u. | 13 | 61 | 260 | 738 | 1331 |
From the above, the linear relation of the standard curve of the petroleum tracer of the embodiment is good, R2The value is 99.2%, the phosphorescence intensity of the petroleum tracer solution is basically maintained unchanged in a longer time, and the detection limit is as low as 0.3 mg/L.
4. The method for using the petroleum tracer for oil field tracing comprises the following steps:
the method for measuring connectivity among oil wells by using the petroleum tracer of the embodiment comprises the following specific steps: weighing 5kg of petroleum tracer to prepare a petroleum solution with a certain concentration, adding the petroleum solution into an injection well, sampling in the injection well, and measuring the phosphorescence intensity to obtain the concentration of the tracer of 8 ppm; after the petroleum tracer is injected for a period of time, the extraction wells 1#, 2# and 3# are respectively sampled, the phosphorescence intensity of sample liquid in the three extraction wells is measured at regular time, finally, the concentration of the petroleum tracer in the extraction well 1# is 2ppm, the concentration of the petroleum tracer in the extraction well 2# is 2ppm, no petroleum tracer exists in the extraction well 3#, the injection well can be known to be communicated with the extraction wells 1# and 2# and not communicated with the extraction well 3# so as to reasonably plan the use of the injection well as required.
Example 5 three different light phosphorescent carbon quantum dots prepared in examples 1-3 above were mixed for use.
Certain qualities of petroleum tracers A (prepared in blue light-example 1), B (prepared in green light-example 2) and C (prepared in red light-example 3) are respectively added into injection wells 1#, 2# and 3# (three wells are not communicated with each other), and samples are taken in different monitoring wells 4# and 5# (the two wells are not communicated with each other) to measure phosphorescence signals. Monitoring a tracer A, a tracer B and a phosphorescent signal without a tracer C in a monitoring well 4 #; phosphorescent signals of the B tracer, the C tracer and no A tracer are monitored in a monitoring well 5 #.
The following information can thus be obtained:
1. the injection well 1# and the injection well 2# are communicated with the monitoring well 4# at the same time, and the injection well 3# is not communicated with the monitoring well 4# at the same time;
2. the injection well 2# and the injection well 3# are simultaneously communicated with the monitoring well 5 #; injection well # 1 is not in communication with monitoring well # 5.
In embodiment 5, because the lifetimes of the different types of phosphorescent carbon quantum dots are different, the monitoring time for each phosphorescent carbon quantum dot is different, and the peak positions of different types of phosphorescent carbon quantum dots are conveniently distinguished, so as to determine the communication between different injection wells and the same monitoring well.
Comparative example 1 this comparative example provides a conventional method for preparing fluorescent carbon quantum dots, as follows: dissolving 1.2g of citric acid and 0.5g of cysteine in 15mL of deionized water, after the two reagents are completely dissolved, putting the two reagents into a reaction kettle for hydrothermal reaction at the reaction temperature of 150 ℃ for 6 hours, after the reaction is finished, performing centrifugal separation on the obtained solution, collecting supernatant to obtain a fluorescent carbon quantum dot solution, purifying by using a silica gel chromatographic column, and performing rotary evaporation or freeze drying to obtain fluorescent carbon quantum dot powder.
The fluorescent carbon quantum dots obtained by the method are mixed with petroleum, and the change condition of petroleum fluorescent signals before and after the fluorescent carbon quantum dots are added is measured, as shown in figure 5-a, it can be seen that a petroleum sample without the fluorescent carbon quantum dots has a fluorescent emission peak with certain intensity at the wavelength of 430nm, the fluorescent signals in the petroleum sample after the fluorescent carbon quantum dots are added and the fluorescent signals in pure petroleum have certain similarity, and the fluorescent emission peak at the wavelength of 440nm, so that the emission peak of the fluorescent carbon quantum dots is greatly interfered due to the interference of the self-fluorescent signals of petroleum, and errors are easily caused in the process of actually using and detecting petroleum.
FIG. 5-b is a phosphorescence signal diagram of the mixture of phosphorescence carbon quantum dots and petroleum prepared at will in the present application, and the difference between the phosphorescence signals of the two is large, thereby avoiding the influence of fluorescence of fluorescent materials or petroleum and expanding the application range thereof.
Compared with the prior art, the invention relates to a petroleum tracer and a qualitative and quantitative method for petroleum tracing, which have the following advantages:
(1) the petroleum tracer has the phosphorescence property, the phosphorescence service life of the petroleum tracer reaches millisecond level, and the detection limit of the petroleum tracer can reach 0.3 ppm;
(2) the petroleum tracer with the phosphorescence performance is used, so that the interference of petroleum autofluorescence can be effectively avoided, the detection sensitivity is improved, and the environment-friendly effect is achieved;
(3) phosphorescent carbon quantum dots with different phosphorescent lifetimes are simultaneously applied to the field of petroleum tracing, and the luminescent peak positions of the phosphorescent carbon quantum dots can be conveniently distinguished, so that the detection efficiency and accuracy are greatly improved;
(4) the oil field tracing method can accurately detect the communication condition of the oil well and provide a detection basis for oil well surveying.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A petroleum tracer which is characterized in that: the petroleum tracer is a phosphorescent carbon quantum dot, the phosphorescent carbon quantum dot comprises a carbon quantum dot body and a loading agent, and the phosphorescent carbon quantum dot has a phosphorescent characteristic.
2. The petroleum tracer according to claim 1, wherein: the load carrier is a porous material, and the carbon quantum dot body is dispersed in the porous material through physical adsorption.
3. The petroleum tracer according to claim 2, wherein: the porous material comprises at least one of polymer and inorganic matter;
preferably, the polymer is at least one selected from the group consisting of polyethylene, polypropylene, polystyrene, polyethylene oxide, polysiloxane, polyphenylene, polythiophene, polyphenylene ethylene, polysilane, polyethylene terephthalate, polyphenylethynyl, polymethyl methacrylate, polydodecamethacrylate, polycarbonate and epoxy resin;
preferably, the inorganic substance is at least one selected from the group consisting of silicon oxide, boron-containing inorganic substance, aluminum-containing oxide, zirconium-containing oxide, titanium-containing oxide, hafnium-containing oxide and yttrium-containing oxide.
4. The petroleum tracer according to claim 2, wherein: the loading agent is an embedded element connected with the carbon quantum dot body through a covalent bond, and the embedded element comprises N, P, F;
preferably, the intercalation element is at least one selected from phosphoric acid, nitric acid, hydrofluoric acid, ammonium fluoride, ammonium citrate, triethylamine trihydrofluoride.
5. The petroleum tracer according to claim 1, wherein: the petroleum tracer comprises at least one of red-light phosphorescent carbon quantum dots, green-light phosphorescent carbon quantum dots and blue-light phosphorescent carbon quantum dots;
preferably, the petroleum tracer is a mixture of red phosphorescent carbon quantum dots, green phosphorescent carbon quantum dots and blue phosphorescent carbon quantum dots.
6. The petroleum tracer according to claim 1, wherein: the solubility of the petroleum tracer agent in water at 10-100 ℃ is less than 1 x 10-5g/L, solubility in petroleum greater than 1 x 102g/L。
7. The petroleum tracer according to claim 1, wherein: the phosphorescent carbon quantum dots of the petroleum tracer may be excited at 350 nm or more and 450nm or less.
8. The application of the petroleum tracer agent is characterized in that: use of the petroleum tracer according to any one of claims 1 to 7 for petroleum tracer testing, tubing leak testing, detection of well communication conditions.
9. An oil field tracing method is characterized by comprising the following steps:
s1, adding the phosphorescent carbon quantum dots according to any one of claims 1 to 7 into an oil field injection well;
s2, obtaining an oil-water mixture at an oil field production well, and extracting an oil phase in the oil-water mixture;
and S3, detecting whether the oil phase has a phosphorescence signal or phosphorescence service life, and judging whether the oil phase has the phosphorescence carbon quantum dots.
10. The method for oilfield tracing of claim 9, further comprising the steps of:
s4, establishing a standard curve of the concentration-phosphorescence intensity of the phosphorescent carbon quantum dots in the petroleum;
and S5, detecting the phosphorescence intensity in the oil phase, and obtaining the concentration of the phosphorescent carbon quantum dots in the oil field well corresponding to the standard curve of the concentration-phosphorescence intensity of the phosphorescent carbon quantum dots.
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