CN114350344A - Metal tracing and film-covering proppant for fracturing and preparation method and application thereof - Google Patents
Metal tracing and film-covering proppant for fracturing and preparation method and application thereof Download PDFInfo
- Publication number
- CN114350344A CN114350344A CN202210039292.4A CN202210039292A CN114350344A CN 114350344 A CN114350344 A CN 114350344A CN 202210039292 A CN202210039292 A CN 202210039292A CN 114350344 A CN114350344 A CN 114350344A
- Authority
- CN
- China
- Prior art keywords
- fracturing
- metal
- nitrate
- tracing
- proppant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 94
- 239000002184 metal Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000700 radioactive tracer Substances 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229920000642 polymer Polymers 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 23
- 150000003839 salts Chemical class 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- 229910002651 NO3 Inorganic materials 0.000 claims description 14
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 12
- 150000001735 carboxylic acids Chemical class 0.000 claims description 10
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 10
- 238000001953 recrystallisation Methods 0.000 claims description 8
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 6
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 claims description 6
- URXZXNYJPAJJOQ-UHFFFAOYSA-N Erucic acid Natural products CCCCCCC=CCCCCCCCCCCCC(O)=O URXZXNYJPAJJOQ-UHFFFAOYSA-N 0.000 claims description 6
- DPUOLQHDNGRHBS-KTKRTIGZSA-N erucic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-KTKRTIGZSA-N 0.000 claims description 6
- 229960001124 trientine Drugs 0.000 claims description 6
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- YBYGDBANBWOYIF-UHFFFAOYSA-N erbium(3+);trinitrate Chemical compound [Er+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YBYGDBANBWOYIF-UHFFFAOYSA-N 0.000 claims description 5
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 5
- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- DPRMFUAMSRXGDE-UHFFFAOYSA-N ac1o530g Chemical compound NCCN.NCCN DPRMFUAMSRXGDE-UHFFFAOYSA-N 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000007888 film coating Substances 0.000 claims 2
- 238000009501 film coating Methods 0.000 claims 2
- 238000010030 laminating Methods 0.000 claims 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims 1
- 229920001568 phenolic resin Polymers 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 18
- 239000011248 coating agent Substances 0.000 abstract description 9
- 238000000576 coating method Methods 0.000 abstract description 6
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 238000001125 extrusion Methods 0.000 abstract description 4
- 239000012530 fluid Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 239000011550 stock solution Substances 0.000 abstract description 3
- 210000002489 tectorial membrane Anatomy 0.000 abstract description 3
- 230000004071 biological effect Effects 0.000 abstract description 2
- 238000005553 drilling Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 22
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 17
- 230000001186 cumulative effect Effects 0.000 description 12
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 8
- 238000009616 inductively coupled plasma Methods 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 6
- 150000001768 cations Chemical class 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000003129 oil well Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000004843 novolac epoxy resin Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910001960 metal nitrate Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000000763 radioactive isotope labeling Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Images
Abstract
The invention discloses a metal tracer coated proppant for fracturing and a preparation method and application thereof, belongs to the technical field of oil field drilling, and solves the technical problems of short validity period, poor thermal stability, low recovery rate, large stratum adsorption loss, low detection precision and the like of other tracers. According to the preparation method of the metal tracer coated proppant for fracturing, resin polymers are cured to form a coating agent stock solution, so that the extrusion resistance among ceramsite proppants can be improved; after the oil and the water are contacted with the polymer coating on the surface of the proppant, the metal tracer slowly diffuses into the stratum through the pore canal in the polymer framework, so that the slow release is realized, and the accurate detection is achieved. The method is simple to operate, safe and pollution-free, and can be used for industrial production. The metal tracing tectorial membrane proppant for fracturing has the advantages of no radioactivity, no pollution, stable and high chemical and biological properties, high analysis precision, and no limitation of oil reservoir properties, fluid properties and the like due to the excellent tracing capacity.
Description
Technical Field
The invention belongs to the technical field of oil field drilling, and particularly relates to a metal tracer coated proppant for fracturing as well as a preparation method and application thereof.
Background
With the progress of oil exploration technology and the continuous development and utilization of oil resources, low permeability oil reservoirs become the main field of oil field development. The exploitation difficulty of low-permeability oil reservoirs is high, and a fracturing technology is needed to generate a complex artificial fracture network in the reservoir during production and development, so that seepage channels of compact oil gas are increased, and the productivity of oil gas wells is further improved. Therefore, the accurate determination of the fracturing condition of the oil well is very important for the evaluation of the fluid production capacity of the production well. The tracer is used as a key carrier of an oil field tracing and monitoring technology and is the only substance which can enter a reservoir and carry fluid and oil reservoir information. The conventional tracer monitoring technology which is generally adopted at present has the problems of short effective period, poor thermal stability, low recovery rate, large formation adsorption loss, low detection precision and the like. Meanwhile, the tracer after the radioactive isotope labeling has certain radioactivity, so that the tracer has certain damage and pollution to engineering personnel and a shaft.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a metal tracer coated proppant for fracturing as well as a preparation method and application thereof, which are used for solving the technical problems of short validity period, poor thermal stability, low recovery rate, large formation adsorption loss, low detection accuracy and the like of other tracers.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a metal tracing and film-covering proppant for fracturing, which has the following structural formula:
wherein, R represents: ce Er Sm La; r’Represents: c21H41 C17H33 C17H35。
The invention also discloses a preparation method of the metal tracer coated proppant for fracturing, which comprises the following steps:
s1: dripping nitrate into a long-chain carboxylic acid solution for reaction, filtering, washing with water, performing primary recrystallization, stripping off formed upper-layer waxy substances, performing recrystallization, and drying to obtain metal salt powder;
s2: and (3) mixing the resin polymer, the metal salt powder obtained in the step S1 and an acetone solution to obtain a mixture, and adding a curing agent into the mixture to obtain the metal tracer coated proppant for fracturing.
Further, in S1, the nitrate includes lithium nitrate, lanthanum nitrate, cerium nitrate, samarium nitrate, or erbium nitrate; the long-chain carboxylic acid solution comprises an erucic acid solution, a stearic acid solution or an oleic acid solution.
Further, in S1, the molar ratio of the nitrate to the long-chain carboxylic acid solution is 1:1 or 1: 3.
Further, when the nitrate is lithium nitrate, the molar ratio of the nitrate to the long-chain carboxylic acid solution is 1: 1; when the nitrate is cerium nitrate, lanthanum nitrate, samarium nitrate or erbium nitrate, the molar ratio of the nitrate to the long-chain carboxylic acid solution is 1: 3.
Further, in S2, the mass ratio of the resin polymer to the curing agent is 1: 1-1: 1.5; the addition amount of the acetone solution is 10 wt% of the total mass of the resin polymer and the curing agent.
Further, in S2, the resinous polymer is any one of an epoxy resin, a phenol resin, a furfuryl alcohol resin, or an acrylic resin; the curing agent is any one of triethylene tetramine, triethylene diamine, diethylene tetramine or triethanolamine; the solvent is acetone solution; the temperature at the time of the mixing was room temperature.
The invention also discloses an application of the metal tracing and film covering propping agent for fracturing, which is characterized in that the metal tracing and film covering propping agent for fracturing is used for oil field tracing, and the main steps are as follows when the oil field tracing is carried out: soaking the ceramsite in a fracturing metal tracing coated proppant, and drying to obtain coated ceramsite; and soaking the coated ceramsite in water for several times, detecting the concentration of the metal elements released in the water after each soaking, repeating the steps, and observing the change trend of the concentration of the metal elements released in the accumulated water.
Further, the fracturing metal tracing coated proppant is used for oil field tracing, and the time for soaking the coated ceramsite in water each time is more than or equal to 24 hours and less than or equal to 48 hours when the oil field tracing is carried out; the above steps are repeated for 2-3 months.
Further, the fracturing metal tracer coated proppant is used for oil field tracing, and when oil field tracing is carried out, the drying mode is fluidized bed drying, and the drying temperature is 60-90 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a metal tracing coated proppant for fracturing, which is formed by solidifying a resin polymer, is used for carrying synthesized metal nitrate by solidifying the resin polymer, is marked in a stock solution of the resin coated proppant, is adsorbed on the surface of a ceramic particle and other proppants to form a polymer coating, prevents a stratum from consuming metal cations and extruding the ceramic particles, realizes slow release and achieves accurate detection. Compared with the conventional tracer, the metal tracer coated proppant for fracturing has the advantages of no radioactivity, no pollution, stable and high chemical and biological properties, high analysis precision and no limitation of oil reservoir properties, fluid properties and the like due to the excellent tracer capacity.
The application also discloses a preparation method of the metal tracer coated proppant for fracturing, which is characterized in that the resin polymer is cured to form the metal tracer coated proppant for fracturing, so that the anti-extrusion capacity among ceramsite proppants can be improved; in addition, the resin polymer is used for solidifying and carrying the synthesized metal nitrate to mark the metal nitrate in the stock solution of the resin coating agent, the resin coating agent is adsorbed on the surfaces of proppants such as ceramic grains to form a polymer coating to prevent the loss of metal cations and the extrusion between the ceramic grains by a stratum, and after oil and water are contacted with the polymer coating on the surface of the proppants, the metal tracer is slowly diffused into the stratum through a pore channel in a polymer framework to realize slow release so as to achieve accurate detection. The method is simple to operate, safe and pollution-free, and can be used for industrial production.
The invention also discloses the application of the metal tracing tectorial membrane proppant for fracturing in oil field tracing, and the metal element is used as a detection core to accurately depict the fracturing condition of an oil well and determine the influence factors of the effective production condition and the ineffective production of the oil well. And (3) carrying out stratum monitoring by taking the metal element as a detection core and the release concentration variation trend as a basis. The problems of short effective period, poor thermal stability, low recovery rate, large stratum adsorption loss and low detection precision of the conventional tracer are effectively solved, and the conventional tracer plays a role in supporting cracks in fracturing, so that the problem of monitoring an oil well is solved.
Drawings
FIG. 1 is a schematic diagram of the fracturing metal tracer coated proppant prepared by the method provided by the invention used for oilfield tracing.
Detailed Description
To make the features and effects of the present invention comprehensible to those skilled in the art, general description and definitions are made below with reference to terms and expressions mentioned in the specification and claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The theory or mechanism described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features defined herein as numerical ranges or percentage ranges, such as values, amounts, levels and concentrations, are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to cover and specifically disclose all possible subranges and individual numerical values (including integers and fractions) within the range.
Unless otherwise specified herein, "comprising," including, "" containing, "" having, "or the like, means" consisting of … … "and" consisting essentially of … …, "e.g.," a comprises a "means" a comprises a and the other, "and" a comprises a only.
In this context, for the sake of brevity, not all possible combinations of features in the various embodiments or examples are described. Therefore, the respective features in the respective embodiments or examples may be arbitrarily combined as long as there is no contradiction between the combinations of the features, and all the possible combinations should be considered as the scope of the present specification.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or conditions recommended by the manufacturers. The various starting materials used in the examples which follow, unless otherwise indicated, are conventional commercial products having specifications which are conventional in the art. In the description of the present invention and the following examples, "%" represents weight percent, "parts" represents parts by weight, and proportions represent weight ratios, unless otherwise specified.
Fig. 1 is a schematic diagram of the fracturing metal tracer coated proppant used for oilfield tracing, and the concrete principle is as follows: negatively charged minerals exist in the stratum, the cation adsorption is strong, and a large amount of OH exists in the stratum water-、CO3 2-Plasma anions, single metal cations, cause significant losses in the formation due to adsorption and chemical reactions, and therefore the metal elements must be stabilized in the formation to ensure the stability of the metal tracer coated proppant. The prepared metal tracing tectorial membrane proppant for fracturing mainly contains metal elements, mainly lithium elements and rare earth metal elements. The resin is used for solidifying and carrying synthesized metal salt, so that the metal salt is marked in the resin film covering agent, and the resin film covering agent is adsorbed on the surfaces of proppants such as ceramic grains to form a polymer coating, so that the loss of metal cations and the extrusion among the ceramic grains by the stratum are hindered. After the oil and water are contacted with the polymer coating on the surface of the proppant, the fracturing metal tracer coated proppant slowly diffuses into the stratum through the pore channels in the polymer framework, so that the slow release is realized. And (3) carrying out stratum monitoring by taking the metal element as a detection core and the release concentration variation trend as a basis.
Example 1
A preparation method of a metal tracer coated proppant for fracturing comprises the following steps:
s1: 0.2g of lithium nitrate is dripped into 1.0g of erucic acid solution to react at 70 ℃, and then the mixture is filtered, washed by water, recrystallized by acetone, stripped of wax-like substance at the upper layer, recrystallized twice and dried at 70 ℃ in vacuum to obtain metal salt powder.
S2: at 25 ℃, 18g of bisphenol A novolac epoxy resin and 1g S1 obtained metal salt powder are added into a beaker and mixed, 3g of acetone solution is added to dissolve the mixture to obtain a mixture, and 6g of triethylene tetramine is added into the mixture to synthesize the metal tracer coated proppant for fracturing.
Example 2
A preparation method of a metal tracer coated proppant for fracturing comprises the following steps:
s1: 0.2g of lithium nitrate is added dropwise to 0.8g of oleic acid solution, and after reaction at 70 ℃, the mixture is filtered, washed with water, recrystallized by acetone, stripped of wax-like substance at the upper layer, recrystallized twice and dried at 70 ℃ in vacuum to obtain metal salt powder.
S2: at 25 ℃, 18g of acrylic resin and 1g S1 obtained metal salt powder are added into a beaker and mixed, 3g of acetone solution is added to dissolve the mixture to obtain a mixture, and 6g of triethanolamine is added into the mixture to synthesize the metal tracer coated proppant for fracturing.
Example 3
A preparation method of a metal tracer coated proppant for fracturing comprises the following steps:
s1: 0.9g of samarium nitrate is dripped into 2.0g of erucic acid solution to react at 70 ℃, and then the metal salt powder is obtained after filtration, water washing, acetone recrystallization, upper wax stripping, twice recrystallization and vacuum drying at 70 ℃.
S2: at 25 ℃, 18g of bisphenol A novolac epoxy resin and 1g S1 obtained metal salt powder are added into a beaker and mixed, 3g of acetone solution is added to dissolve the mixture to obtain a mixture, and 6g of triethylene tetramine is added into the mixture to synthesize the metal tracer coated proppant for fracturing.
Example 4
A preparation method of a metal tracer coated proppant for fracturing comprises the following steps:
s1: 0.9g of lanthanum nitrate is dripped into 2.1g of erucic acid to react at 70 ℃, and then the mixture is filtered, washed by water, recrystallized by acetone, stripped of wax-like substances on the upper layer, recrystallized twice and dried at 70 ℃ in vacuum to obtain metal salt powder.
S2: at 25 ℃, 18g of bisphenol A novolac epoxy resin and 1g S1 obtained metal salt powder are added into a beaker and mixed, 3g of acetone solution is added to dissolve the mixture to obtain a mixture, and 6g of triethylene tetramine is added into the mixture to synthesize the metal tracer coated proppant for fracturing.
Example 5
A preparation method of a metal tracer coated proppant for fracturing comprises the following steps:
s1: 0.9g of cerium nitrate is dripped into 2.1g of erucic acid solution to react at 70 ℃, and then the mixture is filtered, washed by water, recrystallized by acetone, stripped of wax-like substance at the upper layer, recrystallized twice and dried at 70 ℃ in vacuum to obtain metal salt powder.
S2: at 25 ℃, 18g of bisphenol A novolac epoxy resin and 1g S1 obtained metal salt powder are added into a beaker and mixed, 3g of acetone solution is added to dissolve the mixture to obtain a mixture, and 6g of triethylene tetramine is added into the mixture to synthesize the metal tracer coated proppant for fracturing.
Example 6
A preparation method of a metal tracer coated proppant for fracturing comprises the following steps:
s1: 0.9g of erbium nitrate is dripped into 1.7g of stearic acid solution, after reaction at 80 ℃, filtration and water washing are carried out, acetone is used for recrystallization, wax-like substances on the upper layer are stripped, recrystallization is carried out twice, and drying is carried out at 70 ℃ in vacuum, thus obtaining metal salt powder.
S2: at 25 ℃, 18g of furfuryl alcohol resin and the metal salt powder obtained from 1g S1 are added into a beaker and mixed, 3g of acetone solution is added to dissolve the furfuryl alcohol resin and the metal salt powder to obtain a mixture, and 6g of triethylene diamine is added into the mixture to synthesize the metal tracer coated proppant for fracturing.
Application example 1
Soaking the ceramsite in the fracturing metal tracer coated proppant prepared in the embodiment 1, drying the proppant at 90 ℃ by a fluidized bed, and drying to obtain coated ceramsite; 10.0g of coated ceramsite is soaked in 90.0g of water, the temperature is kept at 80 ℃, and after 24 hours, the concentration of lithium element is detected by using an inductively coupled plasma emission spectrometer. Adding 90.0g of water again, detecting for 24h, repeating the above steps for 3 months, and observing the variation trend of the cumulative release concentration of the lithium element, wherein the detection results are shown in Table 1.
Table 1: application example 1 cumulative release concentration variation tendency of lithium element
Application example 2
Soaking the ceramsite in the fracturing metal tracer coated proppant prepared in the embodiment 2, drying the proppant at 65 ℃ by a fluidized bed, and drying to obtain coated ceramsite; 10.0g of coated ceramsite is soaked in 90.0g of water, the temperature is kept at 70 ℃, and after 24 hours, the concentration of lithium element is detected by using an inductively coupled plasma emission spectrometer. Adding 90.0g of water again, detecting for 24h, repeating the above steps for 3 months, and observing the variation trend of the cumulative release concentration of the lithium element, wherein the detection results are shown in Table 2.
Table 2: application example 2 cumulative release concentration variation tendency of lithium element
Application example 3
Soaking the ceramsite in the fracturing metal tracer coated proppant prepared in the embodiment 3, drying the proppant at 90 ℃ by a fluidized bed, and drying to obtain coated ceramsite; 10.0g of coated ceramsite is soaked in 90.0g of water, the temperature is kept at 80 ℃, and after 24 hours, the concentration of lithium element is detected by using an inductively coupled plasma emission spectrometer. 90.0g of water is added again, and the detection is carried out for 24 hours, the operation is repeated for 2 months, the variation trend of the cumulative release concentration of the lithium element is observed, and the detection results are shown in Table 3.
Table 3: application example 3 cumulative release concentration variation tendency of lithium element
Application example 4
Soaking the ceramsite in the fracturing metal tracer coated proppant prepared in the embodiment 4, drying the proppant at 90 ℃ by a fluidized bed, and drying to obtain coated ceramsite; 10.0g of coated ceramsite is soaked in 90.0g of water, the temperature is kept at 80 ℃, and after 24 hours, the concentration of lithium element is detected by using an inductively coupled plasma emission spectrometer. 90.0g of water is added again, and the detection is carried out for 24 hours, the operation is repeated for 3 months, the variation trend of the cumulative release concentration of the lithium element is observed, and the detection results are shown in Table 4.
Table 4: application example 4 cumulative release concentration variation tendency of lithium element
Application example 5
Soaking the ceramsite in the fracturing metal tracer coated proppant prepared in the embodiment 5, drying the proppant at 60 ℃ by a fluidized bed, and drying to obtain coated ceramsite; 10.0g of coated ceramsite is soaked in 90.0g of water, the temperature is kept at 80 ℃, and after 24 hours, the concentration of lithium element is detected by using an inductively coupled plasma emission spectrometer. 90.0g of water is added again, and the detection is carried out for 24 hours, the operation is repeated for 3 months, the variation trend of the cumulative release concentration of the lithium element is observed, and the detection results are shown in Table 4.
Table 5: application example 5 cumulative lithium release concentration variation tendency
Application example 6
Soaking the ceramsite in the fracturing metal tracer coated proppant prepared in the embodiment 6, drying the proppant at 85 ℃ by a fluidized bed, and drying to obtain coated ceramsite; 10.0g of the lithium ion battery is soaked in 90.0g of water, the temperature is kept at 80 ℃, and after 24 hours, the concentration of the lithium element is detected by using an inductively coupled plasma emission spectrometer. 90.0g of water is added again, and the test is carried out for 24 hours, the operation is repeated for 2 months, the trend of the cumulative release concentration of the lithium element is observed, and the test results are shown in Table 6.
Table 6: application example 6 cumulative lithium release concentration variation tendency
From the above table, it can be known that the metal tracer in the metal tracer coated proppant has low release concentration in the stratum, is slow and durable in release, and plays a role in supporting fractures in fracturing, and simultaneously achieves the effect of monitoring an oil well for a long time. The metal elements are detected by using an inductively coupled plasma emission spectrometer, so that the multi-component simultaneous determination can be realized, the analysis is rapid, the sensitivity and the accuracy are high, and the operation is simple and convenient and is easy to master.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. The metal tracing and film covering propping agent for fracturing is characterized by having the following structural formula:
wherein, R represents: ce Er Sm La; r' represents: c21H41 C17H33 C17H35。
2. The preparation method of the metal tracer coated proppant for fracturing, which is characterized by comprising the following steps:
s1: dripping nitrate into a long-chain carboxylic acid solution for reaction, filtering, washing with water, performing primary recrystallization, stripping off formed upper-layer waxy substances, performing recrystallization, and drying to obtain metal salt powder;
s2: and (3) mixing the resin polymer, the metal salt powder obtained in the step S1 and an acetone solution to obtain a mixture, and adding a curing agent into the mixture to obtain the metal tracer coated proppant for fracturing.
3. The method according to claim 2, wherein in S1, the nitrate comprises lithium nitrate, lanthanum nitrate, cerium nitrate, samarium nitrate or erbium nitrate; the long-chain carboxylic acid solution comprises an erucic acid solution, a stearic acid solution or an oleic acid solution.
4. The method for preparing the metal tracer coated proppant for fracturing as claimed in claim 2, wherein in S1, the molar ratio of the nitrate to the long-chain carboxylic acid solution is 1:1 or 1: 3.
5. The preparation method of the metal tracer coated proppant for fracturing as claimed in claim 3 or 4, wherein when the nitrate is lithium nitrate, the molar ratio of the nitrate to the long-chain carboxylic acid solution is 1: 1; when the nitrate is cerium nitrate, lanthanum nitrate, samarium nitrate or erbium nitrate, the molar ratio of the nitrate to the long-chain carboxylic acid solution is 1: 3.
6. The preparation method of the metal tracer coated proppant for fracturing as claimed in claim 2, wherein in S2, the mass ratio of the resin polymer to the curing agent is 1: 1-1: 1.5; the addition amount of the acetone solution is 10 wt% of the total mass of the resin polymer and the curing agent.
7. The method for preparing the metal tracer coated proppant for fracturing as claimed in claim 2, wherein in S2, the resinous polymer is any one of epoxy resin, phenolic resin, furfuryl alcohol resin or acrylic resin; the curing agent is any one of triethylene tetramine, triethylene diamine, diethylene tetramine or triethanolamine; the solvent is acetone solution; the temperature at the time of the mixing was room temperature.
8. The application of the metal tracing and laminating propping agent for fracturing as claimed in claim 1, wherein the metal tracing and laminating propping agent for fracturing is used for oilfield tracing, and the main steps are as follows: soaking the ceramsite in a fracturing metal tracing coated proppant, and drying to obtain coated ceramsite; and soaking the coated ceramsite in water for several times, detecting the concentration of the metal elements released in the water after each soaking, repeating the steps, and observing the change trend of the concentration of the metal elements released in the accumulated water.
9. The application of the metal tracing and film-coating propping agent for fracturing as claimed in claim 8, wherein the metal tracing and film-coating propping agent for fracturing is used for oilfield tracing, and the time for soaking the film-coated ceramsite in water each time is not less than 24h and not more than 48 h; the above steps are repeated for 2-3 months.
10. The use of the metal tracer coated proppant for fracturing as set forth in claim 8, wherein the metal tracer coated proppant for fracturing is used for oilfield tracing, and the drying mode is fluidized bed drying, and the drying temperature is 60-90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210039292.4A CN114350344A (en) | 2022-01-13 | 2022-01-13 | Metal tracing and film-covering proppant for fracturing and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210039292.4A CN114350344A (en) | 2022-01-13 | 2022-01-13 | Metal tracing and film-covering proppant for fracturing and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114350344A true CN114350344A (en) | 2022-04-15 |
Family
ID=81108593
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210039292.4A Pending CN114350344A (en) | 2022-01-13 | 2022-01-13 | Metal tracing and film-covering proppant for fracturing and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114350344A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000290436A (en) * | 1999-04-09 | 2000-10-17 | Japan Polychem Corp | Polyolefin-based resin composition excellent in extrusion characteristic and molded product |
| US20030196799A1 (en) * | 2002-04-18 | 2003-10-23 | Nguyen Philip D. | Method of tracking fluids produced from various zones in subterranean wells |
| AU2005233531A2 (en) * | 2004-04-05 | 2005-10-27 | Carbo Ceramics Incorporated | Tagged propping agents and related methods |
| US20100307745A1 (en) * | 2009-06-03 | 2010-12-09 | Schlumberger Technology Corporation | Use of encapsulated tracers |
| CA3148911A1 (en) * | 2013-03-15 | 2014-09-18 | Carbo Ceramics Inc. | Dna infused particulates and their use in a proppant composition for hydraulic fracturing |
| US20160230543A1 (en) * | 2013-09-05 | 2016-08-11 | Johnson Matthey Public Limited Company | Tracer and method |
| US20170306217A1 (en) * | 2016-04-20 | 2017-10-26 | Spectrum Tracer Services, Llc | Method and compositions for hydraulic fracturing and for tracing formation water |
| WO2018093272A1 (en) * | 2016-11-18 | 2018-05-24 | Institutt For Energiteknikk | Tracers |
| CN113549444A (en) * | 2021-08-25 | 2021-10-26 | 山东谊星新材料有限公司 | Trace element slow-release tracing proppant and preparation method thereof |
-
2022
- 2022-01-13 CN CN202210039292.4A patent/CN114350344A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000290436A (en) * | 1999-04-09 | 2000-10-17 | Japan Polychem Corp | Polyolefin-based resin composition excellent in extrusion characteristic and molded product |
| US20030196799A1 (en) * | 2002-04-18 | 2003-10-23 | Nguyen Philip D. | Method of tracking fluids produced from various zones in subterranean wells |
| AU2005233531A2 (en) * | 2004-04-05 | 2005-10-27 | Carbo Ceramics Incorporated | Tagged propping agents and related methods |
| US20080210421A1 (en) * | 2004-04-05 | 2008-09-04 | Carbo Ceramics Incorporated | Tagged Propping Agents and Related Methods |
| US20100307745A1 (en) * | 2009-06-03 | 2010-12-09 | Schlumberger Technology Corporation | Use of encapsulated tracers |
| CA3148911A1 (en) * | 2013-03-15 | 2014-09-18 | Carbo Ceramics Inc. | Dna infused particulates and their use in a proppant composition for hydraulic fracturing |
| US20160230543A1 (en) * | 2013-09-05 | 2016-08-11 | Johnson Matthey Public Limited Company | Tracer and method |
| US20170306217A1 (en) * | 2016-04-20 | 2017-10-26 | Spectrum Tracer Services, Llc | Method and compositions for hydraulic fracturing and for tracing formation water |
| WO2018093272A1 (en) * | 2016-11-18 | 2018-05-24 | Institutt For Energiteknikk | Tracers |
| CN113549444A (en) * | 2021-08-25 | 2021-10-26 | 山东谊星新材料有限公司 | Trace element slow-release tracing proppant and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107795310B (en) | Long-term real-time tracking method for staged fracturing effect of horizontal well | |
| Vetter | The chemical squeeze process some new information on some old misconceptions | |
| CN1699998B (en) | Constant quantity substance tracer agent for oilfield monitoring and application in oil deposit dynamic monitoring | |
| Saar et al. | Lead (II) complexation by fulvic acid: how it differs from fulvic acid complexation of copper (II) and cadmium (II) | |
| CN113549444A (en) | Trace element slow-release tracing proppant and preparation method thereof | |
| CN103588801A (en) | Trace element well-to-well tracer agent use method | |
| AU2012203555B2 (en) | Method for determining spatial distribution and concentration of a component in a pore volume of a porous material | |
| CN113980675A (en) | Petroleum tracer agent, application thereof and oil field tracing method | |
| Thomas et al. | Primary migration by diffusion through kerogen: I. Model experiments with organic-coated rocks | |
| CN114350344A (en) | Metal tracing and film-covering proppant for fracturing and preparation method and application thereof | |
| CN103357386B (en) | Preparation method of filter core capable of fast and efficiently adsorbing caesium | |
| CN104402772A (en) | High base and high salinity resistance trace element tracer used for oil field, preparation method and application method thereof | |
| CN114380976B (en) | Sustained-release fluorescent tracing tectorial membrane propping agent for oil field and preparation method and application thereof | |
| CN109628091B (en) | Synthesis method and application of BYC tracer | |
| CN109735336B (en) | Synthetic method and application of BEFC tracer | |
| CN109735338B (en) | Synthetic method and application of NYPP tracer | |
| CN114315652B (en) | Aromatic ring tracing type tectorial membrane propping agent for fracturing and preparation method and application thereof | |
| Granger et al. | Using δ15N and δ18O to evaluate the sources and pathways of NO in rainfall event discharge from drained agricultural grassland lysimeters at high temporal resolutions | |
| CN109735334B (en) | Synthetic method and application method of BYP tracer | |
| CN117865919A (en) | Organic tracer, preparation method thereof, interwell tracing method and application of polycyclic aliphatic ether compound as organic tracer | |
| CN114316120B (en) | Coated propping tracer containing rare earth metal elements and preparation method and application thereof | |
| CN109735335B (en) | Synthetic method and application of BYT tracer | |
| CN102998220A (en) | Method for testing intrinsic viscosity number of polymer | |
| CN109628094B (en) | Synthesis method and application of YYTC tracer | |
| CN112300765A (en) | Organic polymer plugging agent and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220415 |