CN115785928B - Intra-slot tracing temporary plugging agent and preparation method and application thereof - Google Patents
Intra-slot tracing temporary plugging agent and preparation method and application thereof Download PDFInfo
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- CN115785928B CN115785928B CN202211522230.5A CN202211522230A CN115785928B CN 115785928 B CN115785928 B CN 115785928B CN 202211522230 A CN202211522230 A CN 202211522230A CN 115785928 B CN115785928 B CN 115785928B
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- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 88
- 239000000700 radioactive tracer Substances 0.000 claims abstract description 56
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 239000011248 coating agent Substances 0.000 claims abstract description 30
- 238000000576 coating method Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 230000000694 effects Effects 0.000 claims abstract description 19
- 239000000314 lubricant Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000012530 fluid Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims description 39
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- -1 polybutylene butyrate Polymers 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 22
- 239000004576 sand Substances 0.000 claims description 21
- 229920002678 cellulose Polymers 0.000 claims description 19
- 239000001913 cellulose Substances 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000008139 complexing agent Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052693 Europium Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 3
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 3
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 3
- 239000001856 Ethyl cellulose Substances 0.000 claims description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 3
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 3
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- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical group [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 3
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 3
- 229920001249 ethyl cellulose Polymers 0.000 claims description 3
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 3
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 3
- 229920001220 nitrocellulos Polymers 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 3
- 239000004633 polyglycolic acid Substances 0.000 claims description 3
- 239000004626 polylactic acid Substances 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- LQLQDKBJAIILIQ-UHFFFAOYSA-N Dibutyl terephthalate Chemical compound CCCCOC(=O)C1=CC=C(C(=O)OCCCC)C=C1 LQLQDKBJAIILIQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 2
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims description 2
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 2
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 2
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- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
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- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 2
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- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims 1
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- 239000003129 oil well Substances 0.000 abstract 1
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- UJZQBMQZMKFSRV-PHQFMFTGSA-N Lithospermic acid Natural products O([C@@H](C(=O)O)Cc1cc(O)c(O)cc1)C(=O)/C=C/c1c2[C@@H](C(=O)O)[C@H](c3cc(O)c(O)cc3)Oc2c(O)cc1 UJZQBMQZMKFSRV-PHQFMFTGSA-N 0.000 description 2
- NFOCYHUCMXEHDG-UHFFFAOYSA-N Monomethyl lithospermate Natural products COC(=O)C1C(C=2C=C(O)C(O)=CC=2)OC(C(=CC=2)O)=C1C=2C=CC(=O)OC(C(O)=O)CC1=CC=C(O)C(O)=C1 NFOCYHUCMXEHDG-UHFFFAOYSA-N 0.000 description 2
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Landscapes
- Lubricants (AREA)
Abstract
The invention provides an in-seam tracing temporary plugging agent, a preparation method and application thereof, wherein the temporary plugging agent comprises the following raw materials in parts by weight: 100-120 parts of temporary plugging agent, 20-35 parts of coating liquid, 2-3 parts of tracer solution and 1-2 parts of lubricant. The invention is suitable for the temporary plugging and steering transformation process in the oil well seam, the temporary plugging agent is tracked in the seam to combine the tracer and the temporary plugging agent in the seam into a whole, after the temporary plugging and steering is performed in the fracturing, the temporary plugging agent is tracked in the seam to be gradually dissolved in the stratum, the tracer is gradually released, the tracer can be completely dissolved in the fracturing fluid and the stratum water, and the concentration of different types of tracer in the flowback water is detected, so that the production condition of each section of production fluid can be calculated, and the temporary plugging and steering effect in the seam can be determined.
Description
Technical Field
The invention relates to an in-seam tracing temporary plugging agent and a preparation method and application thereof, belonging to the field of petroleum exploitation.
Technical Field
The fracturing means to point to the underground in the oil gas reservoir of several kilometers in depth, inject the high-pressure fluid (namely fracturing fluid) through the oil gas well, in order to form the artificial fracture, utilize fracturing fluid to carry solid propping agent granule (namely propping agent, such as haydite, quartz sand) to enter the artificial fracture that presses open at the same time, in order to form and support, the artificial fracture supported is regarded as the high-speed flow channel of oil gas, realize the high-speed extraction of oil gas; temporary plugging and turning fracturing means that after an artificial fracture is pressed in a reservoir, temporary plugging agent is injected to prevent subsequent fracturing fluid from entering the pressed artificial fracture, so that a new artificial fracture is forced to be formed, and fracture turning is realized.
The fracturing temporary plugging steering technology plays a very important role in realizing the efficient transformation and yield increase of old wells and new wells of oil fields. At present, a microseism monitoring technology and fracturing construction pressure are commonly used for evaluating temporary plugging effects, but after the depth of an oil layer exceeds 3000 meters, the signal to noise ratio of a microseism signal source is low, the monitoring precision is low, and the accuracy for monitoring subsurface microseism events is lowered. The factors influencing the construction pressure, such as increased discharge capacity, increased viscosity of the fracturing fluid and increased sand ratio, are more, so that even if the construction pressure is increased after the temporary plugging agent is added, the temporary plugging agent cannot be completely considered to have a temporary plugging and turning effect, and the temporary plugging and turning effect can be the result caused by various influencing factors.
The prior report adopts the method for evaluating the plugging effect by injecting the tracer, for example, chinese patent document CN 108222922 discloses an oil and gas well reservoir productivity evaluation method based on temporary plugging diversion fracturing technology, when temporary plugging diversion fracturing construction is carried out, a water-soluble tracer is carried into a target oil and gas well by fracturing fluid before temporary plugging each time, a flowback fluid sample is collected and the concentration of the water-soluble tracer in flowback fluid is detected at a flowback test stage after the temporary plugging diversion fracturing construction is completed, so that the temporary plugging effect of each temporary plugging is analyzed, and the productivity contribution of each fracturing stage is calculated. However, when the temporary plugging agent is added, the method also needs to additionally manually operate the metering pump to pump the tracer solution, the temporary plugging agent and the tracer are separately injected, the construction process is complex, the cost is high, and the test result is also influenced by sequential injection.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an in-seam tracing temporary plugging agent, a preparation method and application thereof, the method has the temporary plugging steering function in the joint, the functions of monitoring the liquid production profile and determining the temporary plugging effect of the tracer, and meanwhile, the construction process is simple, the cost is low, and the evaluation of the temporary plugging effect is accurate.
The invention is realized by the following technical scheme:
The temporary plugging agent for in-seam tracing consists of the following raw materials in parts by weight: 100-150 parts of temporary plugging agent, 20-40 parts of coating liquid, 2-10 parts of tracer solution and 1-10 parts of lubricant.
According to the invention, the temporary plugging agent is one or more than two of polylactic acid, polyglycolic acid and polybutylene butyrate, and the particle size of the temporary plugging agent is 0.15-0.85mm.
According to the invention, the coating liquid is cellulose, ethanol and lipid compounds according to the mass ratio of 1: (18-22): (0.1-0.5) a mixture.
Further preferably, the coating liquid is cellulose, ethanol and lipid compounds according to the mass ratio of 1: (18-22): (0.15-0.25).
Most preferably, the coating liquid is cellulose, ethanol and lipid compounds according to the mass ratio of 1:19: (0.15-0.25).
According to the present invention, the cellulose is preferably one or a mixture of two or more of hydroxyethyl cellulose, ethyl cellulose, hydroxymethyl cellulose, methyl cellulose and nitrocellulose.
According to the present invention, the lipid compound is preferably one or a mixture of two or more of dioctyl phthalate, dibutyl phthalate, acetyltributyl citrate and dibutyl terephthalate.
According to the invention, preferably, the tracing solution is rare earth nitrate, complexing agent and distilled water according to the mole ratio (1-2): (1-2): the mixture of (1-2) in a ratio.
Most preferably, the tracer solution is rare earth nitrate, complexing agent and distilled water according to the mole ratio of 1:1:1, and a mixture thereof.
According to the invention, the rare earth element is one or more of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium and yttrium.
According to the invention, the complexing agent is preferably one or more than two of citric acid, lithospermic acid, citric acid and disodium ethylenediamine tetraacetate.
According to a preferred embodiment of the present invention, the lubricant is calcium stearate or zinc stearate.
The preferred technical scheme of the invention is as follows:
the temporary plugging agent for in-seam tracing consists of the following raw materials in parts by weight: 100 parts of temporary plugging agent, 22 parts of coating liquid, 2 parts of tracer solution and 1 part of lubricant.
The preparation method of the temporary plugging agent for in-seam tracing comprises the following steps:
step one, mixing cellulose and ethanol according to a proportion, uniformly stirring, and fully dissolving;
step two, adding the lipid compound into the mixed solution in the step one, and stirring for 20-40 minutes to obtain coating liquid;
Heating the sand mixing pot to 60-80 ℃, adding the temporary plugging agent and the tracer solution into the sand mixing pot according to the proportion, mixing for 5-10 minutes at the rotation speed of 70-90 r/min, adding the coating liquid in the second step, mixing for 60-90 minutes, finally adding the lubricant, mixing for 3-5 minutes, drying, cooling and screening to obtain the in-seam tracing temporary plugging agent.
On the other hand, the invention also provides application of the temporary plugging agent for in-seam tracing, which is applied to temporary plugging steering in the fracture and evaluation of the temporary plugging steering effect in the seam.
The preferred specific application method according to the invention is as follows:
in the fracturing process, the in-seam tracing temporary plugging agent is injected into the seam of the reservoir seam to realize temporary plugging and turning in the seam, the in-seam tracing temporary plugging agent is gradually dissolved and simultaneously gradually released at the reservoir temperature, the tracer is completely dissolved in fracturing fluid and stratum water, and the concentration of different types of tracer in flowback water is detected to calculate the production condition of each section and determine the temporary plugging and turning effect in the seam.
The invention has the technical characteristics and advantages that:
1. The temporary plugging agent for in-seam tracing has the temporary plugging steering function in the seam, the functions of monitoring the liquid production profile and determining the temporary plugging effect of the tracer, and meanwhile, the construction process is simple, the cost is low, and the evaluation of the temporary plugging effect is accurate.
2. When the temporary plugging agent is added in situ for the in-seam tracing, the metering pump is not required to be additionally operated manually to pump the tracer solution, and the construction process is simple.
3. The invention surprisingly discovers that the weight ratio of the coating liquid and the types of the coating liquid can be controlled in the implementation process, the coating effect can be obviously improved, all tracers are wrapped on the surface of the temporary plugging agent, the tracers have no loss, the tracers are completely dissolved in the fracturing liquid and the stratum water after the temporary plugging and turning fracturing construction is completed, the flowback effect is good by detecting the concentration of different types of tracers in flowback water, the temporary plugging effect can be well evaluated, the influence of the depth of an oil layer is avoided, the influence of the discharge capacity, the viscosity of the fracturing liquid and sand ratio factors is avoided, the influence factors are small, and the temporary plugging effect is accurately evaluated by a simple and low-cost process.
Drawings
FIG. 1 is a section 1 fracturing construction curve of a Y930 well;
FIG. 2 is a graph of a Y930 well section 2 fracturing construction;
FIG. 3 is a graph showing the concentration of europium element detected by analysis using the tracer in Experimental example 3.
Fig. 4 is a concentration profile of gadolinium element analyzed and detected using the tracer in experimental example 3.
FIG. 5 is a graph showing the cumulative rate of contribution of each section of the produced fluid in Experimental example 3.
FIG. 6 is a schematic diagram of the temporary plugging agent for in-line tracing obtained in example 1.
Detailed description of the preferred embodiments
For a better understanding of the nature and features of the present invention, reference will now be made in detail to the embodiments of the present invention, examples of which are illustrated in the accompanying drawings.
Example 1
The temporary plugging agent for in-seam tracing consists of the following raw materials in parts by weight: 100 parts of temporary plugging agent, 22 parts of coating liquid, 2 parts of tracer solution and 1 part of lubricant.
The temporary plugging agent is polylactic acid with the grain diameter of 0.15-0.25mm;
the coating liquid is cellulose, ethanol and lipid compounds according to the mass ratio of 1:19:0.15 a mixture of cellulose, hydroxyethyl cellulose and lipid compound, dioctyl phthalate;
the tracing solution is rare earth nitrate, complexing agent and distilled water according to the mol ratio of 1:1:1, wherein the rare earth element is europium and the complexing agent is citric acid;
The lubricant is calcium stearate;
The preparation method of the temporary plugging agent for in-seam tracing comprises the following specific steps:
step one, mixing 1 part of cellulose and 19 parts of ethanol, uniformly stirring, fully dissolving,
And step two, adding 0.15 part of lipid compound into the mixed solution in the step one, and stirring for 30 minutes to obtain coating liquid.
Heating the sand mixing pot to 70 ℃, adding 100 parts of temporary plugging agent and 2 parts of tracer solution into the sand mixing pot, setting the rotation speed of the sand mixing pot to 70 revolutions per minute, mixing for 10 minutes, adding 22 parts of coating liquid in the step two into the sand mixing pot, mixing for 60 minutes, adding 1 part of lubricant into the sand mixing pot, and mixing for 5 minutes to obtain a primary product.
And step four, drying, cooling and screening the primary product in the step three to obtain the in-seam tracing temporary plugging agent, wherein the appearance physical diagram is shown in figure 6.
Example 2
The temporary plugging agent for in-seam tracing consists of the following raw materials in parts by weight: 108 parts of temporary plugging agent, 25 parts of coating liquid, 2.4 parts of tracer solution and 1.5 parts of lubricant.
The temporary plugging agent is polybutyl butyrate with the particle size of 0.25-0.5mm.
The coating liquid is cellulose, ethanol and lipid compounds according to the mass ratio of 1:19:0.25 of a cellulose nitrocellulose, and the lipid compound is dibutyl phthalate.
The tracing solution is rare earth nitrate, complexing agent and distilled water according to the mol ratio of 1:1:1, wherein the rare earth element is gadolinium and the complexing agent is lithospermic acid;
the lubricant is zinc stearate;
The preparation method of the temporary plugging agent for in-seam tracing comprises the following specific steps:
step one, mixing 1 part of cellulose and 19 parts of ethanol, uniformly stirring, and fully dissolving.
And step two, adding 0.25 part of lipid compound into the mixed solution in the step one, and stirring for 30 minutes to obtain coating liquid.
Heating the sand mixing pot to 70 ℃, adding 108 parts of temporary plugging agent and 2.4 parts of tracer solution into the sand mixing pot, setting the rotation speed of the sand mixing pot to 90 r/min, mixing for 10 minutes, adding 25 parts of coating liquid in the second step into the sand mixing pot, mixing for 80 minutes, adding 1.5 parts of lubricant into the sand mixing pot, and mixing for 5 minutes to obtain a primary product;
And step four, drying, cooling and screening the primary product in the step three to obtain the in-seam tracing temporary plugging agent.
Example 3
The temporary plugging agent for in-seam tracing consists of the following raw materials in parts by weight: 120 parts of temporary plugging agent, 35 parts of coating liquid, 3 parts of tracer solution and 2 parts of lubricant;
the temporary plugging agent is polyglycolic acid with the grain diameter of 0.5-0.85mm.
The coating liquid is cellulose, ethanol and lipid compounds according to the mass ratio of 1:19:0.22, wherein the cellulose is ethyl cellulose, and the lipid compound is acetyl tributyl citrate.
The tracing solution is rare earth nitrate, complexing agent and distilled water according to the mol ratio of 1:1:1, wherein the rare earth element is dysprosium, the complexing agent is disodium ethylenediamine tetraacetate,
The lubricant is zinc stearate and the lubricant is zinc stearate,
The preparation method of the temporary plugging agent for in-seam tracing comprises the following specific steps:
step one, mixing 1 part of cellulose and 19 parts of ethanol, uniformly stirring, and fully dissolving.
And step two, adding 0.22 part of lipid compound into the mixed solution in the step one, and stirring for 30 minutes to obtain coating liquid.
Step three, adjusting the temperature of the sand mixing pot to 80 ℃, adding 120 parts of temporary plugging agent and 3 parts of tracer agent solution into the sand mixing pot, setting the rotating speed of the sand mixing pot to 90 r/min, mixing for 8 minutes, then adding the coating liquid in the step two into the sand mixing pot, mixing for 90 minutes, then adding 2 parts of lubricant into the sand mixing pot, mixing for 3 minutes to obtain a primary product,
And step four, drying, cooling and screening the primary product in the step three to obtain the in-seam tracing temporary plugging agent.
Comparative example 1
The same in-seam tracer temporary plugging agent as described in example 1 is different in that: the composite material consists of the following raw materials in parts by weight: 100 parts of temporary plugging agent, 16 parts of coating liquid, 2 parts of tracer solution, 1 part of lubricant and the other parts are carried out according to the embodiment 1.
Comparative example 2
The same in-seam tracer temporary plugging agent as described in example 2 is different in that:
The coating liquid is cellulose, ethanol and lipid compounds according to the mass ratio of 1:19:0.35, otherwise as in example 2.
Comparative example 3
The same in-seam tracer temporary plugging agent as described in example 2 is different in that:
The coating liquid is cellulose, ethanol and lipid compounds according to the mass ratio of 1:19:0.05, and the rest of example 2.
Experimental example 1
The in-seam tracer temporary plugging agents of examples 1 to 3 were evaluated for their properties, and the results were as follows:
(1) Solubility of
The degradation time and degradation rate of 3 in-seam tracer temporary plugging agents in water are tested at 95 ℃ and the results are shown in table 1. As can be seen from Table 1, the products of examples 1 to 3 can be completely dissolved in water within 48 hours, and meet the technical requirements of reservoirs on temporary plugging agents.
TABLE 1
| Project | Example 1 | Example 2 | Example 3 |
| Degradation time, h | 47 | 46 | 46.5 |
| Degradation rate, percent | 100 | 100 | 100 |
(2) Blocking strength
The temporary plugging agent for the in-seam tracing is placed in a steel film with the outer diameter of 2.5cm, the inner diameter of 1.5cm and the thickness of 1cm, the steel film is placed in a baking oven at the temperature of 95 ℃ for standing for 1 hour, the pressure change is measured by clean water in a constant flow mode of 2mL/min, the maximum pressure in the displacement process is recorded, and the pressure measurement result is shown in Table 2. As can be seen from table 2, the products of examples 1 to 3 have high blocking strength, and meet the technical requirements of the reservoir for temporary blocking agents.
TABLE 2
| Project | Example 1 | Example 2 | Example 3 |
| Maximum pressure, MPa | 10.5 | 11.5 | 11.2 |
Experimental example 2
The 3 kinds of the in-seam tracer temporary plugging agents of examples 1 to 3 were taken and placed in water respectively, heated to 95 ℃, after the 3 kinds of the in-seam tracer temporary plugging agents are completely dissolved in water, water was added to dilute to the initial concentration as described in table 3, and the mixture was left standing for 90 days at 95 ℃, and whether the solution was clear or not was observed, and the concentration retention rate of the rare earth element was measured, and the result is shown in table 3. The concentration retention rate of 3 rare earth elements is above 90%, and the solution is clear, so that the technical requirement of a reservoir on the tracer is met.
TABLE 3 Table 3
Experimental example 3
The Y930 well is a straight well, the designed well depth is 3805 meters, the stratum temperature is 125 ℃, the production interval is 2 layers, and repeated fracturing is carried out on the 2 layers. And (3) injecting the embodiment 1 in-seam tracing temporary plugging agent into the 1 st layer in the repeated fracturing process, respectively performing in-seam temporary plugging by injecting the embodiment 2 in-seam tracing temporary plugging agent into the 2 nd layer, designing 185kg of rare earth element europium in-seam tracing temporary plugging agent and 192kg of rare earth element gadolinium in-seam tracing temporary plugging agent, wherein the use amounts of the rare earth elements in the two in-seam tracing temporary plugging agents are the same, and the construction graph is shown in fig. 1 and 2.
FIG. 1 shows that when the rare earth element europium-doped in-slot tracer temporary plugging agent reaches the bottom of a well in the layer 1 fracturing, the ground construction pressure is increased from 50.1MPa to 56.2MPa, and the in-slot temporary plugging diversion pressure reaches 6.1MPa, which shows that in-slot temporary plugging diversion is realized.
FIG. 2 shows that when the rare earth element gadolinium in-seam tracing temporary plugging agent reaches the bottom of the well in the process of fracturing the layer 2, the ground construction pressure is increased from 58.4MPa to 62.3MPa, and the in-seam temporary plugging diversion pressure reaches 3.9MPa, which shows that in-seam temporary plugging diversion is realized.
After fracturing, regularly collecting flowback fluid from a wellhead, detecting the concentration of 2 rare earth elements in the flowback fluid by using a mass spectrometer, accumulating the concentration of the tracer in the monitoring section for days, and further calculating the contribution rate of each rare earth element to the produced fluid of each section. Fig. 3-5 show the concentration results of 2 tracers, and the yield contribution rate curves. The results show that the liquid production contribution rates of the 1 st section and the 2 nd section are respectively, namely the 1 st section is a main production layer, and the 2 nd section is a secondary production layer. The tracer detection result further proves that the temporary plugging steering in the seam is realized after the temporary plugging agent is injected into the seam, and the temporary plugging steering effect in the seam of the 1 st section is better than that of the 2 nd section from the aspect of the liquid production contribution rate.
Comparative experiment example 1
The in-slit tracer temporary plugging agents in example 1 and comparative example 1 were placed in water respectively, and after the in-slit tracer temporary plugging agents were completely dissolved in water at 95 ℃, the concentrations of rare earth elements in the water were directly measured, and the results are shown in table 4. It can be seen that the deviation between the measured value and the theoretical value of the rare earth element in comparative example 1 is 15%, while the deviation between the measured value and the theoretical value of the rare earth element in example 1 is less than 1%, which means that the whole tracer cannot be coated on the surface of the temporary plugging agent in comparative example 1, and a part of tracer is lost.
TABLE 4 Table 4
| Case (B) | Theoretical value of rare earth element (μg/L) | Actual measurement value of rare earth element (μg/L) | Deviation ratio (%) |
| Example 1 | 50 | 49.7 | 0.6％ |
| Comparative example 1 | 50 | 42.5 | 15 |
Comparative experiment example 2
The in-slit tracer temporary plugging agents in example 2 and comparative example 2 were placed in water respectively, and after the in-slit tracer temporary plugging agents were completely dissolved in water at 95 ℃, the concentrations of rare earth elements in the water were directly measured, and the results are shown in table 5. It can be seen that the deviation between the measured value and the theoretical value of the rare earth element in comparative example 2 is 13.6%, while the deviation between the measured value and the theoretical value of the rare earth element in example 2 is less than 1%, which indicates that the whole tracer cannot be coated on the surface of the temporary plugging agent in comparative example 2, and a part of tracer is lost.
TABLE 5
| Case (B) | Theoretical value of rare earth element (μg/L) | Actual measurement value of rare earth element (μg/L) | Deviation ratio (%) |
| Example 2 | 50 | 49.8 | 0.4％ |
| Comparative example 2 | 50 | 43.2 | 13.6 |
Comparative experiment example 3
The in-slit tracer temporary plugging agents in example 3 and comparative example 2 were placed in water respectively, and after the in-slit tracer temporary plugging agents were completely dissolved in water at 95 ℃, the concentrations of rare earth elements in the water were directly measured, and the results are shown in table 6.
TABLE 6
| Case (B) | Theoretical value of rare earth element (μg/L) | Actual measurement value of rare earth element (μg/L) | Deviation ratio (%) |
| Example 2 | 50 | 49.8 | 0.4％ |
| Comparative example 2 | 50 | 41.9 | 16.2 |
It can be seen that the deviation between the measured value and the theoretical value of the rare earth element in comparative example 3 is 16.2%, while the deviation between the measured value and the theoretical value of the rare earth element in example 2 is less than 1%, which means that the whole tracer cannot be wrapped on the surface of the temporary plugging agent in comparative example 3, and a part of tracer is lost.
Claims (4)
1. The temporary plugging agent for in-seam tracing consists of the following raw materials in parts by weight: 100-150 parts of temporary plugging agent, 20-40 parts of coating liquid, 2-10 parts of tracer solution and 1-10 parts of lubricant;
The temporary plugging agent is one or more than two of polylactic acid, polyglycolic acid and polybutylene butyrate, and the particle size of the temporary plugging agent is 0.15-0.85mm;
the coating liquid is prepared from cellulose, ethanol and ester compounds according to the mass ratio of 1:19: (0.15-0.25);
The cellulose is one or more than two of hydroxyethyl cellulose, ethyl cellulose, hydroxymethyl cellulose, methyl cellulose and nitrocellulose;
the ester compound is one or more than two of dioctyl phthalate, dibutyl phthalate, acetyl tributyl citrate and dibutyl terephthalate;
the tracing solution is rare earth nitrate, complexing agent and distilled water according to the mol ratio of 1:1:1, a mixture of the components mixed in proportion;
the rare earth element is one or more of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium and yttrium;
The complexing agent is one or more of citric acid, tartaric acid, citric acid and disodium ethylenediamine tetraacetate, and the lubricant is calcium stearate or zinc stearate.
2. The method for preparing the temporary plugging agent for in-seam tracing as defined in claim 1, comprising the following steps:
step one, mixing cellulose and ethanol according to a proportion, uniformly stirring, and fully dissolving;
Step two, adding an ester compound into the mixed solution in the step one, and stirring for 20-40 minutes to obtain coating liquid;
Heating the sand mixing pot to 60-80 ℃, adding the temporary plugging agent and the tracer solution into the sand mixing pot according to the proportion, mixing for 5-10 minutes at the rotation speed of 70-90 r/min, adding the coating liquid in the second step, mixing for 60-90 minutes, finally adding the lubricant, mixing for 3-5 minutes, drying, cooling and screening to obtain the in-seam tracing temporary plugging agent.
3. The application of the in-seam tracer temporary plugging agent as defined in claim 1, which is applied to temporary plugging steering in a fracture and evaluating the effect of temporary plugging steering in the seam.
4. The use according to claim 3, characterized in that the specific application method is as follows:
in the fracturing process, the in-seam tracing temporary plugging agent is injected into the seam of the reservoir seam to realize temporary plugging and turning in the seam, the in-seam tracing temporary plugging agent is gradually dissolved and simultaneously gradually released at the reservoir temperature, the tracer is completely dissolved in fracturing fluid and stratum water, and the concentration of different types of tracer in flowback water is detected to calculate the production condition of each section and determine the temporary plugging and turning effect in the seam.
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