CN117304913A - Dyeing tracer for fracturing propping agent and preparation method and application thereof - Google Patents
Dyeing tracer for fracturing propping agent and preparation method and application thereof Download PDFInfo
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- CN117304913A CN117304913A CN202311064615.6A CN202311064615A CN117304913A CN 117304913 A CN117304913 A CN 117304913A CN 202311064615 A CN202311064615 A CN 202311064615A CN 117304913 A CN117304913 A CN 117304913A
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- agent
- propping agent
- dye
- proppant
- solution
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 252
- 239000000700 radioactive tracer Substances 0.000 title claims abstract description 52
- 238000004043 dyeing Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 76
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 74
- 239000003086 colorant Substances 0.000 claims abstract description 35
- 229920000642 polymer Polymers 0.000 claims abstract description 17
- -1 cationic quaternary ammonium salt Chemical class 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000000975 dye Substances 0.000 claims description 130
- 235000006708 antioxidants Nutrition 0.000 claims description 72
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 23
- 239000002904 solvent Substances 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 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
- 239000002002 slurry Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 10
- 239000006004 Quartz sand Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 10
- 239000004576 sand Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 239000004814 polyurethane Substances 0.000 claims description 9
- 229920002635 polyurethane Polymers 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000004040 coloring Methods 0.000 claims description 7
- 239000003381 stabilizer Substances 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 241000779819 Syncarpia glomulifera Species 0.000 claims description 5
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 5
- 235000015165 citric acid Nutrition 0.000 claims description 5
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- 239000001739 pinus spp. Substances 0.000 claims description 5
- 229940116411 terpineol Drugs 0.000 claims description 5
- 229940036248 turpentine Drugs 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- 235000009328 Amaranthus caudatus Nutrition 0.000 claims description 4
- 240000001592 Amaranthus caudatus Species 0.000 claims description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 4
- 235000000177 Indigofera tinctoria Nutrition 0.000 claims description 4
- 235000012735 amaranth Nutrition 0.000 claims description 4
- 239000004178 amaranth Substances 0.000 claims description 4
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- ZXJXZNDDNMQXFV-UHFFFAOYSA-M crystal violet Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1[C+](C=1C=CC(=CC=1)N(C)C)C1=CC=C(N(C)C)C=C1 ZXJXZNDDNMQXFV-UHFFFAOYSA-M 0.000 claims description 4
- NJDNXYGOVLYJHP-UHFFFAOYSA-L disodium;2-(3-oxido-6-oxoxanthen-9-yl)benzoate Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C1=C2C=CC(=O)C=C2OC2=CC([O-])=CC=C21 NJDNXYGOVLYJHP-UHFFFAOYSA-L 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 239000005007 epoxy-phenolic resin Substances 0.000 claims description 4
- 230000002209 hydrophobic effect Effects 0.000 claims description 4
- 229940097275 indigo Drugs 0.000 claims description 4
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- VOFUROIFQGPCGE-UHFFFAOYSA-N nile red Chemical compound C1=CC=C2C3=NC4=CC=C(N(CC)CC)C=C4OC3=CC(=O)C2=C1 VOFUROIFQGPCGE-UHFFFAOYSA-N 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 235000013824 polyphenols Nutrition 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 229940099373 sudan iii Drugs 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- JOBXVSNBBMBPGZ-UHFFFAOYSA-N 1-methylpyrrole Chemical compound CN1C=CC=C1.CN1C=CC=C1 JOBXVSNBBMBPGZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004101 4-Hexylresorcinol Substances 0.000 claims description 3
- WFJIVOKAWHGMBH-UHFFFAOYSA-N 4-hexylbenzene-1,3-diol Chemical compound CCCCCCC1=CC=C(O)C=C1O WFJIVOKAWHGMBH-UHFFFAOYSA-N 0.000 claims description 3
- 235000019360 4-hexylresorcinol Nutrition 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- IPMYMEWFZKHGAX-UHFFFAOYSA-N Isotheaflavin Natural products OC1CC2=C(O)C=C(O)C=C2OC1C(C1=C2)=CC(O)=C(O)C1=C(O)C(=O)C=C2C1C(O)CC2=C(O)C=C(O)C=C2O1 IPMYMEWFZKHGAX-UHFFFAOYSA-N 0.000 claims description 3
- 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 description 3
- UXRMWRBWCAGDQB-UHFFFAOYSA-N Theaflavin Natural products C1=CC(C2C(CC3=C(O)C=C(O)C=C3O2)O)=C(O)C(=O)C2=C1C(C1OC3=CC(O)=CC(O)=C3CC1O)=CC(O)=C2O UXRMWRBWCAGDQB-UHFFFAOYSA-N 0.000 claims description 3
- FENRSEGZMITUEF-ATTCVCFYSA-E [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] FENRSEGZMITUEF-ATTCVCFYSA-E 0.000 claims description 3
- 229960001927 cetylpyridinium chloride Drugs 0.000 claims description 3
- YMKDRGPMQRFJGP-UHFFFAOYSA-M cetylpyridinium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 YMKDRGPMQRFJGP-UHFFFAOYSA-M 0.000 claims description 3
- 229960004106 citric acid Drugs 0.000 claims description 3
- 229960003258 hexylresorcinol Drugs 0.000 claims description 3
- 229940083982 sodium phytate Drugs 0.000 claims description 3
- FHNINJWBTRXEBC-HXEHWPEMSA-N sudan iii Chemical compound OC1=CC=C2C=CC=CC2=C1\N=N\C(C=C1)=CC=C1\N=N/C1=CC=CC=C1 FHNINJWBTRXEBC-HXEHWPEMSA-N 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 229960001367 tartaric acid Drugs 0.000 claims description 3
- IPMYMEWFZKHGAX-ZKSIBHASSA-N theaflavin Chemical compound C1=C2C([C@H]3OC4=CC(O)=CC(O)=C4C[C@H]3O)=CC(O)=C(O)C2=C(O)C(=O)C=C1[C@@H]1[C@H](O)CC2=C(O)C=C(O)C=C2O1 IPMYMEWFZKHGAX-ZKSIBHASSA-N 0.000 claims description 3
- 229940026509 theaflavin Drugs 0.000 claims description 3
- 235000014620 theaflavin Nutrition 0.000 claims description 3
- 210000002221 olecranon process Anatomy 0.000 claims description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 13
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 94
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 18
- 239000012530 fluid Substances 0.000 description 17
- 230000032683 aging Effects 0.000 description 13
- 230000000694 effects Effects 0.000 description 12
- 238000005406 washing Methods 0.000 description 10
- 239000007800 oxidant agent Substances 0.000 description 9
- 238000005507 spraying Methods 0.000 description 9
- 230000001590 oxidative effect Effects 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 230000018109 developmental process Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 5
- 230000007774 longterm Effects 0.000 description 4
- 235000013619 trace mineral Nutrition 0.000 description 4
- 239000011573 trace mineral Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000003064 anti-oxidating effect Effects 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005562 fading Methods 0.000 description 2
- 239000007850 fluorescent dye Substances 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- FHNINJWBTRXEBC-UHFFFAOYSA-N Sudan III Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC(C=C1)=CC=C1N=NC1=CC=CC=C1 FHNINJWBTRXEBC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000001045 blue dye Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 231100000045 chemical toxicity Toxicity 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 125000001117 oleyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000941 radioactive substance Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000008093 supporting effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/25—Methods for stimulating production
- E21B43/26—Methods for stimulating production by forming crevices or fractures
- E21B43/267—Methods for stimulating production by forming crevices or fractures reinforcing fractures by propping
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B47/00—Survey of boreholes or wells
- E21B47/10—Locating fluid leaks, intrusions or movements
- E21B47/11—Locating fluid leaks, intrusions or movements using tracers; using radioactivity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mining & Mineral Resources (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Geophysics (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Coloring (AREA)
Abstract
The application relates to the technical field of oilfield chemical products, in particular to a dyeing tracer propping agent for fracturing and a preparation method and application thereof; the raw materials of the dyeing tracing propping agent comprise dye solution, propping agent and antioxidant solution, wherein the mass ratio of the dye solution to the propping agent is 1-100:500; the mass ratio of proppant to antioxidant solution was 50:0.1 to 5; the dye solution comprises a coloring agent and a fixing agent; the color fixing agent comprises a cationic quaternary ammonium salt color fixing agent and/or a polymer color fixing agent; the dye solution is limited to comprise a dye and a color fixing agent, the mass ratio of the dye solution to the propping agent is controlled, the mass ratio of the propping agent to the antioxidant solution is controlled, and the specific types of the color fixing agent are limited, so that the dye tracing propping agent has the advantages of various colors, convenience in detection, capability of meeting simultaneous monitoring of single-well multi-section cracks, good stability, safety and no pollution.
Description
Technical Field
The application relates to the technical field of oilfield chemical products, in particular to a dyeing tracer propping agent for fracturing and a preparation method and application thereof.
Background
The fracturing technology is a key technical means for improving the yield of low-permeability oil and gas wells at present, the technology forces a stratum to generate cracks through high-pressure hydraulic pumping, then adopts sand-carrying fluid to bring proppants such as ceramsite, quartz sand and the like into the cracks, and after the high-pressure hydraulic pumping is withdrawn, the proppants stay in the cracks to support the cracks, so that an oil and gas high-diversion channel is established. However, when the construction is completed, the flowback fluid may carry out part of the propping agent, thereby reducing the crack supporting effect, and the returned propping agent may also block the well bore and damage wellhead equipment. And the backflow of propping agents can be influenced by different fracturing processes, propping agent selection, flowback speed control and the like, so that the propping agent backflow phenomenon is more prominent in the large-scale fracturing of the horizontal well at present (particularly the fracturing with more fine propping agents). Therefore, knowing the specific position of the returned propping agent in the horizontal well fracturing is of great significance to the optimization of the later fracturing construction, and special marking of the propping agent is needed to achieve the purpose, so that the development of the corresponding tracer propping agent has significant engineering value.
The oil field adopts the tracer propping agent to determine the distribution of the propping agent in the underground fracture for a long time, the current commonly used tracer propping agent technology is divided into two main types, one type is that radioactive substances, magnetic substances, conductive substances and the like are used as markers to be added into the propping agent, and the markers reach specific positions of the stratum along with the propping agent and are matched with various logging equipment to monitor the fracture; the other is to load chemical tracers such as fluorescent dye, trace elements, water-soluble inorganic salt, low molecular alcohol and the like on the surface of the propping agent, analyze the concentration of the chemical tracers in flowback fluid by controlling the release of the chemical tracers in the stratum, further obtain crack related information, for example, provide trace element slow release tracers, hydrolyze and release the trace element phthalocyanine in the stratum by taking the trace element phthalocyanine as an effective component, realize the tracing function, but because the phthalocyanine is indissolvable in water and an organic solvent, the phthalocyanine is difficult to remain at the propping agent release position, and a large amount of phthalocyanine damages an oil and gas reservoir, although the trace propping agent with a combined mode is provided at present, for example, the trace propping agent with magnetic and fluorescent dual functions can be enriched in the oilfield by adopting a magnetic field when sampling a produced well, compared with the mode of directly detecting the stock solution, the error of re-detecting after the oilfield tracer is enriched is obviously reduced, higher accuracy is realized, but the whole cost is high, and two times of detection are required by the magnetic field and fluorescent are more inconvenient.
However, the main function of the current tracer proppants is to explain underground cracks, and few reports are made on the tracer proppants with knowledge of proppant return positions. Therefore, how to provide a tracing propping agent which is simple in preparation method, low in cost, convenient in detection technology, nontoxic and harmless so as to realize the determination of the sand discharge position and the sand discharge amount is a technical problem which needs to be solved at present.
Disclosure of Invention
The application provides a dyeing tracing propping agent for fracturing and a preparation method and application thereof, and aims to solve the technical problems that in the prior art, the tracing propping agent has high cost, inconvenient detection and larger pollution in the determination of the tracing propping agent at the propping agent returning position.
In a first aspect, the present application provides a dye tracer proppant for fracturing, wherein the dye tracer proppant comprises a dye solution, a proppant and an antioxidant solution, and the mass ratio between the dye solution and the proppant is 1-100: 500;
the mass ratio of the proppant to the antioxidant solution is 50:0.1 to 5;
wherein the dye solution comprises a coloring agent and a fixing agent; the color fixing agent comprises a cationic quaternary ammonium salt type color fixing agent and/or a polymer type color fixing agent.
Optionally, the dye solution comprises, in parts by weight: dyeing agent: 0.2-20 parts of color fixing agent: 0.5-10 parts of solvent: 100 parts; and/or the number of the groups of groups,
the antioxidant solution comprises the following components in parts by weight: antioxidant: 0.1-5 parts of solvent: 10 parts.
Optionally, the solvent includes at least one of water, methanol, ethanol, n-butanol, terpineol, turpentine, n-octane, white oil, petroleum ether, toluene, and xylene.
Optionally, the particle size of the propping agent is 10-140 meshes; and/or the number of the groups of groups,
the propping agent comprises at least one of quartz sand propping agent, ceramsite propping agent, pre-cured resin coating propping agent, polymer coated self-suspension propping agent and hydrophobic modification propping agent.
Optionally, the cationic quaternary ammonium salt type color fixing agent comprises cetylpyridinium chloride; and/or the number of the groups of groups,
the polymer color fixing agent comprises at least one of high molecular weight aromatic sulfonic acid condensate, phenolic condensate, cellulose, acrylic resin, epoxy resin, phenolic resin and modified polyurethane.
Optionally, the coloring agent comprises at least one of methylene blue, oleyl blue, indigo, fluorescent yellow green, amaranth, sudan iii, nile red, sodium fluorescein, and methyl violet; and/or the number of the groups of groups,
the antioxidant comprises at least one of N-methylpyrrole-1-methylpyrrole, tartaric acid, sodium phytate, theaflavin, 4-hexylresorcinol and citric acid.
In a second aspect, the present application provides a method of preparing the dyed tracer proppant of the first aspect, the method comprising:
pre-cleaning a proppant sample to obtain a proppant;
dissolving a coloring agent in a solvent to obtain a primary dye solution, adding a color fixing agent into the primary dye solution, and adjusting the pH value to a preset pH value to obtain a dye solution;
respectively enabling a coloring agent in the dye solution, a color fixing agent and an antioxidant in the antioxidant solution to be attached to the surface of the propping agent, then heating, and stirring to obtain a dyeing tracing propping agent slurry;
filtering the dyeing tracer proppant slurry, and drying to obtain a dyeing tracer proppant; or alternatively, the first and second heat exchangers may be,
pre-cleaning a proppant sample to obtain a proppant;
mixing the propping agent and the coloring agent, adding a solvent, stirring and filtering to obtain a pre-coloring propping agent;
respectively adding a color fixing agent and an antioxidant into the solvent to obtain a color stabilizer solution;
attaching a fixing agent and an antioxidant in the color stabilizer solution to the surface of the pre-coloring propping agent, heating, and stirring to obtain a dyeing tracing propping agent slurry;
and filtering the dyeing tracer propping agent slurry, and drying to obtain the dyeing tracer propping agent.
Optionally, the preset pH value is 3-12; and/or the number of the groups of groups,
the stirring speed is 30 rpm-60 rpm, and the stirring time is 5 min-30 min.
Optionally, the temperature of the heating end point is 40-60 ℃; and/or the number of the groups of groups,
the temperature of the drying is 30-50 ℃, and the time of the drying is 3-12 h.
In a third aspect, the present application provides the use of a dyed tracer proppant for fracturing, the use comprising the use of a dyed tracer proppant according to the first aspect in determining post-fracturing flowback sand location and sand volume of an oil and gas well.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the dye tracing propping agent for fracturing, the dye solution, the propping agent and the antioxidant solution are used as the dye tracing propping agent, the dye solution is limited to comprise the dyeing agent, the color fixing agent and the antioxidant solution, the specific mass ratio of the dye solution to the propping agent is controlled, the propping agent can be used for adsorbing the dyeing agent, the propping agent is colored, the color fixing agent is limited to comprise the cationic quaternary ammonium salt type color fixing agent and/or the polymer type color fixing agent, the quaternary ammonium salt type color fixing agent is combined with the dye to form insoluble dye salt to be deposited on the skeleton surface of the propping agent, the polymer type color fixing agent is mainly coated on the surface of the dye to form a color fixing layer, the propping agent adsorbed with the dye in the dye is reinforced and protected, the dye is decolorized due to factors such as water washing and friction, the antioxidant solution is added, the color breaking agent, dissolved oxygen and the oxidant of other chemical additives are present in the fracturing fluid, the dye is prevented from being oxidized too fast through the antioxidation effect of the antioxidant solution, and the color fixing agent can be effectively and effectively detected in the fracturing fluid, the well is free of toxicity and stability can be met, the stability of the well is further stable, the stability of the well can be met, and the quality can be well can be stably detected at the same time, and the quality can be well-stable, and stable quality can be well-kept at the stability, and stable quality can be well-stable, and stable.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a schematic structural diagram of a dye tracer proppant for fracturing according to an embodiment of the present application;
fig. 2 is a schematic flow chart of a preparation method of a dye tracer proppant for fracturing according to an embodiment of the present application;
FIG. 3 is a schematic flow chart of another method for preparing a dye tracer proppant for fracturing according to an embodiment of the present disclosure;
wherein, the 1-dyeing layer, the 2-fixation layer, the 3-antioxidant particles, the 4-oxidant particles, the 5-oxidant and the antioxidant are combined.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
Unless specifically indicated otherwise, the various raw materials, reagents, instruments, equipment, and the like used in this application are commercially available or may be prepared by existing methods.
The inventive thinking of this application is:
if the chemical tracer used by the traditional quartz sand proppant is used as the tracer proppant at the proppant return position, as the surface of the quartz sand proppant lacks active groups, the specific surface area is small, and the dye is difficult to be firmly attached to the surface of the proppant by using a conventional dyeing method, then decolorization is carried out in fracturing fluid, so that the fracturing fluid is invalid and pollutes water, the proppant return position is difficult to be stably displayed, and part of fluorescent dye has chemical toxicity, so that the method for preparing the tracer proppant is simple, low in cost, convenient in detection technology, nontoxic and harmless, and capable of determining the sand outlet position and the sand outlet amount is a technical problem which needs to be solved urgently at present.
As shown in fig. 1, an embodiment of the present application provides a dye tracer proppant for fracturing, wherein raw materials of the dye tracer proppant include a dye solution, a proppant and an antioxidant solution, and a mass ratio between the dye solution and the proppant is 1-100:500;
the mass ratio of the proppant to the antioxidant solution is 50:0.1 to 5;
wherein the dye solution comprises a coloring agent and a fixing agent; the color fixing agent comprises a cationic quaternary ammonium salt type color fixing agent and/or a polymer type color fixing agent.
In the embodiment of the application, the working principle of the dyeing tracing propping agent is as follows:
the dye agent is adhered to the surface of the propping agent through adsorption to form a dye layer 1, the fixing agent is used for stabilizing the adhesion of the dye on the surface of the propping agent to form a water-insoluble fixing layer 2, the quaternary ammonium salt type fixing agent in the fixing agent can be combined with the dye to form insoluble dye salt to be deposited on the surface of the propping agent, and the polymer type fixing agent is mainly coated on the surface of the dye to form a film so as to form the fixing layer 2. Because oxidant particles 4 such as gel breaker, dissolved oxygen and other chemical additives exist in the fracturing fluid, antioxidant particles 3 such as antioxidants are added to the surface of the propping agent, and the oxidant existing in the water phase is combined with the antioxidant particles 3 at the joint 5 of the oxidant and the antioxidant and is mutually neutralized, the direct contact of the oxidant with the oxidant to oxidize the dye is avoided, and the dye can be prevented from being oxidized too fast to fade.
The specific mass ratio between the dye solution and the propping agent is controlled, so that the dyeing agent in the dye solution is fully adsorbed by the propping agent, and the propping agent adsorbed with the dye can be reinforced and protected by the color fixing agent, so that the dyeing agent is not decolorized due to factors such as washing, friction and the like, and the stability of the dye in the dyeing agent is improved.
The mass ratio between the dye solution and the proppant may be 1:500, or may be 6:500, or may be 11:500, or may be 16:500, or may be 21:500, or may be 26:500, or may be 31:500, or may be 36:500, or may be 41:500, or may be 46:500, or may be 51:500, or may be 56:500, or may be 61:500, or may be 66:500, or may be 71:500, or may be 76:500, or may be 81:500, or may be 86:500, or may be 91:500, or may be 96:500, or may be 100:500.
The specific mass ratio between the propping agent and the color fixing agent is controlled, the oxidation resistance of the antioxidant in the antioxidant solution can be utilized to prevent the dye from being oxidized too fast to fade, and meanwhile, the curing effect of the color fixing agent is matched, so that the effective substances of the antioxidant can be slowly released even in a high-temperature stratum, and further, the long-term color development of the dye is maintained.
The mass ratio between the dye solution and the propping agent can be 50:0.1, 50:0.3, 50:0.5, 50:0.7, 50:0.9, 50:1.1, 50:1.3, 50:1.5, 50:1.7, 50:1.9, 50:2.1, 50:2.3, 50:2.5, 50:2.9, 50:3.1, 50:3.3, 50:3.5, 50:4.1, 4.1, 4.5, and 4.5.
The specific mass ratio of the dye solution to the antioxidant solution is controlled, and as small molecular particles of the oxidant such as gel breaker, dissolved oxygen, other chemical additives and the like exist in the fracturing fluid, the long-term color development of the dye can be maintained by introducing the antioxidant solution containing the antioxidant to avoid the dye from being oxidized and fading too quickly.
The mass ratio of the dye solution to the antioxidant solution may be 50:0.1, or 50:0.5, or 50:1.0, or 50:1.5, also 50:1.5, also 50:2.0, also 50:2.5, also 50:3.0, also 50:3.5, also 50:4.0, also 50:4.5, and may also be 50:5.0.
the antioxidant means an agent having a function of preventing the surface coloring agent of the proppant from being oxidized, and the antioxidants described in the present application refer to all agents having such a function. The antioxidant solution is specifically an embodiment in which the agent is present in the form of a solution, and the solvent for dissolving the antioxidant may be arbitrarily selected from water, methanol, ethanol, n-butanol, terpineol, turpentine, n-octane, white oil, petroleum ether, toluene and xylene.
In some alternative embodiments, the dye solution comprises, in parts by weight: dyeing agent: 0.2-20 parts of color fixing agent: 0.5-10 parts of solvent: 100 parts; and/or the number of the groups of groups,
the antioxidant solution comprises the following components in parts by weight: antioxidant: 0.1-5 parts of solvent: 10 parts.
In the embodiment of the application, in the dye solution, the specific weight parts of the dye are controlled, so that the dye can be fully absorbed by the propping agent, and the dye in the dye is uniformly distributed on the propping agent.
The specific type fraction of the color fixing agent is controlled, and the color fixing agent can be used for reinforcing and protecting the propping agent adsorbed with the dye, so that the propping agent is not decolorized due to factors such as washing, friction and the like, and the stability of the dye in the dye is improved.
The specific parts by weight of the solvent are controlled, so that the coloring agent and the color fixing agent are uniformly dissolved, the adjustment of the pH value is convenient, the mixing of the dye solution and the propping agent is also uniform, the coloring agent in the dye solution is completely adsorbed by the propping agent, and the propping agent adsorbed with the coloring agent is reinforced and protected through the color fixing agent, so that the coloring agent is not decolorized due to factors such as washing, friction and the like.
In the antioxidant solution, the specific parts by weight of the antioxidant are controlled, so that the dye in the dye solution can be prevented from being quickly oxidized to fade, and the color fixing effect of the color fixing agent can be matched, so that the effective substances of the antioxidant can be slowly released even in a high-temperature stratum, and the long-term color development of the dye is maintained.
The specific weight parts of the solvent are controlled, so that the antioxidant can be uniformly dissolved, the subsequent antioxidant solution can be conveniently and completely adsorbed by the propping agent, and the long-term color development of the dye can be maintained.
In some alternative embodiments, the solvent comprises at least one of water, methanol, ethanol, n-butanol, terpineol, turpentine, n-octane, white oil, petroleum ether, toluene, and xylene.
In this application embodiment, the specific kind of control solvent can further make stain and fixation agent dissolve evenly, can also make things convenient for the adjustment of pH valve simultaneously, can also make the misce bene of dye solution and proppant to make this dyeing tracer proppant can not decolorize because of factors such as washing, friction.
The solvent may be water, methanol, ethanol, n-butanol, terpineol, turpentine, n-octane, white oil, petroleum ether, toluene, or xylene.
In some alternative embodiments, the proppant has a particle size of 10 mesh to 140 mesh; and/or the number of the groups of groups,
the propping agent comprises at least one of quartz sand propping agent, ceramsite propping agent, pre-cured resin coating propping agent, polymer coated self-suspension propping agent and hydrophobic modification propping agent.
In the embodiment of the application, the specific particle size of the propping agent is controlled to be finer, so that the dye in the coloring agent is completely adsorbed by the propping agent; the specific types of proppants are limited, and most proppant products in the prior art can be included, so that the application range of the dyed tracer proppants is improved.
The propping agent can be quartz sand propping agent, ceramsite propping agent, pre-cured resin coating propping agent, polymer coated self-suspension propping agent and hydrophobic modified propping agent.
In some alternative embodiments, the cationic quaternary ammonium salt fixing agent comprises cetylpyridinium chloride; and/or the number of the groups of groups,
the polymer color fixing agent comprises at least one of high molecular weight aromatic sulfonic acid condensate, phenolic condensate, cellulose, acrylic resin, epoxy resin, phenolic resin and modified polyurethane.
The specific types of cationic quaternary ammonium salt type fixing agents and polymer type fixing agents in the fixing agents are controlled, insoluble dye salt formed by combining the quaternary ammonium salt type fixing agents with the dye is deposited on the surface of a framework of the propping agent, and the polymer type fixing agents are mainly coated on the surface of the dye to form a fixing layer, so that the propping agent adsorbed with the dye in the dyeing agent is reinforced and protected, and decolorization caused by factors such as washing, friction and the like is avoided.
The polymer color fixing agent can be a high molecular weight aromatic sulfonic acid condensate, a phenolic condensate, cellulose, acrylic resin, epoxy resin, phenolic resin and modified polyurethane.
In some alternative embodiments, the coloring agent comprises at least one of methylene blue, olecranon, indigo, fluorescent yellow green, amaranth, sudan iii, nile red, sodium fluorescein, and methyl violet; and/or the number of the groups of groups,
the antioxidant comprises at least one of N-methylpyrrole-1-methylpyrrole, tartaric acid, sodium phytate, theaflavin, 4-hexylresorcinol and citric acid.
In this application embodiment, control the specific kind of dyestuff, can make the dyestuff can be by abundant absorption of proppant, simultaneously because the dyestuff that adopts is the harmless dyestuff of low toxicity, consequently make the dyeing tracer proppant have the harmless characteristics of low toxicity to can make things convenient for the dyestuff to consolidate and protect the proppant through the effect of fixation agent.
The dye may be methylene blue, olelan, indigo, fluorescent yellow-green, amaranth, sudan III, nile red, sodium fluorescein, or methyl violet.
As shown in fig. 2, based on one general inventive concept, an embodiment of the present application provides a method of preparing the dye trace proppant, the method comprising:
s1, pre-cleaning a propping agent sample to obtain a propping agent;
s2, dissolving a coloring agent in a solvent to obtain a primary dye solution, adding a color fixing agent into the primary dye solution, and adjusting the pH value to a preset pH value to obtain a dye solution;
s3, respectively enabling a coloring agent in the dye solution, a color fixing agent and an antioxidant in the antioxidant solution to be attached to the surface of the propping agent, heating and stirring to obtain a dyeing tracing propping agent slurry;
and S4, filtering the dyeing tracer propping agent slurry, and drying to obtain the dyeing tracer propping agent.
Or as shown in fig. 3, based on one general inventive concept, the present embodiments provide another method of preparing the dye trace proppant, the method comprising:
s1, pre-cleaning a propping agent sample to obtain a propping agent;
s2, mixing the propping agent and the coloring agent, adding a solvent, stirring and filtering to obtain a pre-coloring propping agent;
s3, respectively adding a color fixing agent and an antioxidant into the solvent to obtain a color stabilizer solution;
s4, attaching a color fixing agent and an antioxidant in the color stabilizer solution to the pre-coloring propping agent, heating and stirring to obtain a dyeing tracing propping agent slurry;
s5, filtering the dyeing tracer propping agent slurry, and drying to obtain the dyeing tracer propping agent.
In this embodiment of the present application, the dye in the dye solution may be attached to the surface of the propping agent through the adsorption of the propping agent, wherein the means for attaching the dye to the surface of the propping agent generally adopts spraying (shown in fig. 2) or soaking (shown in fig. 3), and in order to enhance the dyeing effect, steps of heating, stirring, adjusting the pH value of the dye solution, and the like may be adopted.
The attachment means include, but are not limited to, physical attachment means such as spraying, dipping, and the like.
The method is directed to the preparation method of the dyeing tracing propping agent, the specific composition of the dyeing tracing propping agent can refer to the embodiment, and because the method adopts part or all of the technical schemes of the embodiment, the method at least has all the beneficial effects brought by the technical schemes of the embodiment, and the description is omitted herein.
In some alternative embodiments, the preset ph is 3 to 12; and/or the number of the groups of groups,
the stirring speed is 30 rpm-60 rpm, and the stirring time is 5 min-30 min.
In this application embodiment, control predetermines the pH value, can make the stable distribution of dyestuff and fixation agent in the dyestuff solution, make things convenient for follow-up dyestuff and fixation agent to respectively with the reaction effect of proppant to realize strengthening and protecting the proppant that has adsorbed the dyestuff in the dyestuff through the fixation agent, make it not decolor because of factors such as washing, friction.
In some alternative embodiments, the elevated end point temperature is 40 ℃ to 60 ℃; and/or the number of the groups of groups,
the temperature of the drying is 30-50 ℃, and the time of the drying is 3-12 h.
In the embodiment of the application, the specific end temperature of the heating is controlled, so that the antioxidant in the antioxidant solution is adsorbed by the propping agent, and the antioxidant effect of the coloring agent is improved; when the end point temperature is too high, the oxidation-resistant protection effect of the antioxidant solution is disabled, so that the coloring agent is oxidized to fade; when the end point temperature is too low, the thermodynamic rate of the antioxidant solution is low, so that the antioxidant solution is insufficient to be adsorbed on the proppant surface, thereby the color retention effect is poor.
The specific temperature and specific time of drying are controlled, so that on one hand, moisture in the propping agent can be evaporated completely, and on the other hand, the failure of the antioxidation effect of the antioxidant solution in the propping agent can be avoided, thereby improving the antioxidation effect of the propping agent and further improving the color retention effect.
Based on one general inventive concept, embodiments of the present application provide an application of a dyed tracer proppant for fracturing, the application including using the dyed tracer proppant in a reagent for determining a post-fracturing flowback sand location and sand amount of an oil and gas well.
In the embodiment of the application, the specific process of the application is as follows:
washing the dyed tracing propping agent with clear water, drying at normal temperature, taking the common similar propping agent as a contrast, and identifying the color of the propping agent by using a standard color chart or a special solid particle color identification instrument so as to trace the layer section; the crack monitoring method is simple to operate, the tracer propping agent is free of radioactivity and pollution, and the method is good in safety and stability and has good application prospect.
The application is realized based on the above-mentioned dyeing tracer propping agent, the specific composition of the dyeing tracer propping agent can refer to the above-mentioned embodiment, and because the application adopts some or all of the technical solutions of the above-mentioned embodiment, the application has at least all the beneficial effects brought by the technical solutions of the above-mentioned embodiment, and the detailed description is omitted herein.
The present application is further illustrated below in conjunction with specific examples. It should be understood that these examples are illustrative only of the present application and are not intended to limit the scope of the present application. The experimental procedures, which are not specified in the following examples, are generally determined according to national standards. If the corresponding national standard does not exist, the method is carried out according to the general international standard, the conventional condition or the condition recommended by the manufacturer.
Example 1
The preparation method of the dyeing tracer propping agent for fracturing comprises the following steps:
dissolving 0.5 part of methylene blue coloring agent in 5 parts of clear water, adding 0.5 part of modified waterborne polyurethane color fixing agent, fully stirring until the mixture is completely dissolved, and controlling the pH value of the solution to be 4.0-6.0 to obtain a dye solution.
0.2 part of citric acid antioxidant is dissolved in 5 parts of ethanol to form an antioxidant solution, and the solution is fully stirred until the antioxidant solution is completely dissolved.
1000 parts of 40/70 mesh quartz sand are poured into a mixer and stirred at a speed of 30r/min, and then 5 parts of dye solution and 5 parts of antioxidant solution are added into the propping agent in a spray-coating mode, and stirring is continued for 10min at a constant temperature of 60 ℃. And taking out the stirred propping agent, and drying at 40 ℃ for 12 hours to obtain the dyeing propping agent.
Adding 40 parts of propping agent into 100 parts of fracturing fluid containing gel breaker, aging for 24 hours at 120 ℃ in a closed tank, taking out, washing with clear water, drying at 40 ℃, comparing the color changes before and after aging, and testing the concentration of methylene blue in the water phase by using a spectrophotometer.
Example 2
Dissolving 0.5 part of methylene blue coloring agent in 5 parts of clear water, adding 0.8 part of modified waterborne polyurethane color fixing agent, fully stirring until the mixture is completely dissolved, and controlling the pH value of the solution to be 4.0-6.0 to obtain a dye solution.
0.4 part of citric acid antioxidant is dissolved in 5 parts of ethanol to form an antioxidant solution, and the solution is fully stirred until the antioxidant solution is completely dissolved.
1000 parts of 40/70 mesh ceramsite propping agent is poured into a mixer, stirred at the speed of 30r/min, and then 5 parts of dye solution and 5 parts of antioxidant solution are added into the propping agent in a spraying mode, and stirring is carried out continuously for 10min at the constant temperature of 60 ℃. And taking out the stirred propping agent, and drying at 40 ℃ for 12 hours to obtain the dyeing propping agent.
Adding 40 parts of propping agent into 100 parts of fracturing fluid containing gel breaker, aging for 24 hours at 120 ℃ in a closed tank, taking out, washing with clear water, drying at 40 ℃, comparing the color changes before and after aging, and testing the concentration of methylene blue in the water phase by using a spectrophotometer.
Example 3
1000 parts of proppant and 5 parts of methylene blue dye were added to a stirrer, followed by 1000 parts of clear water, stirred for 30min at 30r/min, and then the solution was filtered off to give a pre-colored proppant. The filtrate is preserved, and the dye can be reused for many times after being supplemented. Dissolving 0.5 part of modified polyurethane color fixing agent and 0.5 part of antioxidant in 5 parts of ethanol to prepare a solution, adding the color stabilizer solution into the propping agent in a spray coating mode, continuously stirring for 10min at 30r/min at 60 ℃, and then drying for 12h at 40 ℃ to obtain the dyed propping agent.
Taking out 40 parts of propping agent, adding the propping agent into 100 parts of fracturing fluid containing the gel breaker, aging for 4 hours at 120 ℃, cleaning the fracturing fluid with clear water after taking out, drying at 40 ℃, comparing the color changes before and after aging, and testing the concentration of methylene blue in the water phase by using a spectrophotometer.
Comparative example 1
0.5 part of methylene blue coloring agent is dissolved in 5 parts of clear water, and the mixture is fully stirred until the methylene blue coloring agent is completely dissolved.
1000 parts of 40/70 mesh quartz sand are poured into a mixer and stirred at a speed of 30r/min, and then 5 parts of dye solution are added to the propping agent in a spray-coating form, and stirring is continued for 10min at a constant temperature of 60 ℃. And taking out the stirred propping agent, and drying at 40 ℃ for 12 hours to obtain the dyeing propping agent.
40 parts of propping agent is taken and added into 100 parts of slickwater fracturing fluid, aging is carried out at 120 ℃ for 24 hours, the propping agent is taken out, washed and dried at 40 ℃, the color change of the propping agent before and after aging is compared, and a spectrophotometer is used for testing the concentration of methylene blue in the water phase.
Comparative example 2
Dissolving 0.5 part of methylene blue coloring agent in 5 parts of clear water to prepare dye; and then 0.5 part of modified polyurethane color fixing agent is dissolved in 5 parts of ethanol, and fully stirred until the modified polyurethane color fixing agent is completely dissolved. 1000 parts of 40/70 mesh quartz sand are poured into a mixer and stirred at a speed of 30r/min, and then 5 parts of dye solution and 5 parts of fixing agent solution are added to the propping agent in a spray-coating form, and stirring is continued for 10min at a constant temperature of 60 ℃. And taking out the stirred propping agent, and drying at 40 ℃ for 12 hours to obtain the dyeing propping agent.
40 parts of propping agent is taken and added into 100 parts of fracturing fluid containing gel breaker, aging is carried out at 120 ℃ for 24 hours, the fracturing fluid is taken out, washed and dried at 40 ℃, the color changes before and after aging are compared, and a spectrophotometer is used for testing the concentration of methylene blue in the water phase.
Comparative example 3
0.5 part of the colorant methylene blue is dissolved in 5 parts of clear water and fully stirred until the colorant methylene blue is completely dissolved. 1000 parts of 40/70 mesh silica sand was poured into a mixer and stirred at a speed of 30r/min, followed by adding 5 parts of the dye solution and 5 parts of the antioxidant solution obtained in example 1 to the proppant in spray form and stirring at a constant temperature of 60℃for 10min. And taking out the stirred propping agent, and drying at 40 ℃ for 12 hours to obtain the dyeing propping agent.
40 parts of propping agent is taken and added into 100 parts of slickwater fracturing fluid, aging is carried out at 120 ℃ for 24 hours, the propping agent is taken out, washed and dried at 40 ℃, the color change of the propping agent before and after aging is compared, and a spectrophotometer is used for testing the concentration of methylene blue in the water phase.
TABLE 1 methylene blue aqueous phase concentration after proppant aging
As can be seen from table 1, the use of both spraying and dipping methods enabled stable coloring of the colorant on the proppant surface according to the data of example 1, example 2 and example 3; comparison of the results of example 1 with comparative example 1 shows that the use of an antioxidant solution and a fixing agent can greatly reduce the dissolution of the proppant in the aqueous phase and prevent the proppant from decolorization; the lower level of aqueous phase solution colorant in comparative example 2, while the lower level of proppant color fading occurred, indicated that the antioxidant solution was able to maintain stable performance of the colorant at high temperature, and the higher concentration of liquid phase was achieved in comparative example 3 because the proppant color was severely faded without the addition of the fixing agent, while the faded colorant was not oxidized in water due to the antioxidant solution.
Therefore, the dye tracing propping agent can be prepared by spraying, soaking and other modes, and in order to achieve the best use effect, the dye is stably adsorbed on the surface of the propping agent through the color fixing agent, and the property of the dye is kept stable through the antioxidant solution.
Various embodiments of the present application may exist in a range format; it should be understood that the description in a range format is merely for convenience and brevity and should not be interpreted as a rigid limitation on the scope of the application. It is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
In this application, unless otherwise indicated, terms of orientation such as "upper" and "lower" are used specifically to refer to the orientation of the drawing in the figures. In addition, in the description of the present application, the terms "include", "comprise", "comprising" and the like mean "including but not limited to". Relational terms such as "first" and "second", and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Herein, "and/or" describing an association relationship of an association object means that there may be three relationships, for example, a and/or B, may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural. Herein, "at least one" means one or more, and "a plurality" means two or more. "at least one", "at least one" or the like refer to any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
The foregoing is merely a specific embodiment of the application to enable one skilled in the art to understand or practice the application. 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 application. Thus, the present application 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. The dyeing tracing propping agent for fracturing is characterized in that the raw materials of the dyeing tracing propping agent comprise dye solution, propping agent and antioxidant solution, and the mass ratio of the dye solution to the propping agent is 1-100:500;
the mass ratio of the proppant to the antioxidant solution is 50:0.1 to 5;
wherein the dye solution comprises a coloring agent and a fixing agent; the color fixing agent comprises a cationic quaternary ammonium salt type color fixing agent and/or a polymer type color fixing agent.
2. The dye tracer proppant of claim 1, wherein the dye solution comprises, in parts by weight: dyeing agent: 0.2-20 parts of color fixing agent: 0.5-10 parts of solvent: 100 parts; and/or the number of the groups of groups,
the antioxidant solution comprises the following components in parts by weight: antioxidant: 0.1-5 parts of solvent: 10 parts.
3. The dye tracery proppant of claim 2, wherein the solvent comprises at least one of water, methanol, ethanol, n-butanol, terpineol, turpentine, n-octane, white oil, petroleum ether, toluene, and xylene.
4. The dye tracer proppant of claim 1, wherein the proppant has a particle size of 10 mesh to 140 mesh; and/or the number of the groups of groups,
the propping agent comprises at least one of quartz sand propping agent, ceramsite propping agent, pre-cured resin coating propping agent, polymer coated self-suspension propping agent and hydrophobic modification propping agent.
5. The dye trace proppant of claim 1, wherein the cationic quaternary ammonium salt fixing agent comprises cetylpyridinium chloride; and/or the number of the groups of groups,
the polymer color fixing agent comprises at least one of high molecular weight aromatic sulfonic acid condensate, phenolic condensate, cellulose, acrylic resin, epoxy resin, phenolic resin and modified polyurethane.
6. The dye tracer proppant of claim 1, wherein the dye agent comprises at least one of methylene blue, olecranon, indigo, fluorescent yellow green, amaranth, sudan iii, nile red, sodium fluorescein, and methyl violet; and/or the number of the groups of groups,
the antioxidant comprises at least one of N-methylpyrrole-1-methylpyrrole, tartaric acid, sodium phytate, theaflavin, 4-hexylresorcinol and citric acid.
7. A method of preparing a dyed tracer proppant as set forth in any one of claims 1-6, said method comprising:
pre-cleaning a proppant sample to obtain a proppant;
dissolving a coloring agent in a solvent to obtain a primary dye solution, adding a color fixing agent into the primary dye solution, and adjusting the pH value to a preset pH value to obtain a dye solution;
respectively enabling a coloring agent in the dye solution, a color fixing agent and an antioxidant in the antioxidant solution to be attached to the surface of the propping agent, then heating, and stirring to obtain a dyeing tracing propping agent slurry;
filtering the dyeing tracer proppant slurry, and drying to obtain a dyeing tracer proppant; or alternatively, the first and second heat exchangers may be,
pre-cleaning a proppant sample to obtain a proppant;
mixing the propping agent and the coloring agent, adding a solvent, stirring and filtering to obtain a pre-coloring propping agent;
respectively adding a color fixing agent and an antioxidant into the solvent to obtain a color stabilizer solution;
attaching a fixing agent and an antioxidant in the color stabilizer solution to the pre-coloring propping agent, heating and stirring to obtain a dyeing tracing propping agent slurry;
and filtering the dyeing tracer propping agent slurry, and drying to obtain the dyeing tracer propping agent.
8. The dye tracer proppant of claim 7, wherein the preset ph is 3-12; and/or the number of the groups of groups,
the stirring speed is 30 rpm-60 rpm, and the stirring time is 5 min-30 min.
9. A dye tracer proppant according to claim 7, wherein,
the temperature of the heating end point is 40-60 ℃; and/or the number of the groups of groups,
the temperature of the drying is 30-50 ℃, and the time of the drying is 3-12 h.
10. Use of a dyed tracer proppant for fracturing, comprising the use of a dyed tracer proppant according to any one of claims 1-6 for determining the position and amount of sand in a post-fracturing flowback of an oil and gas well.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311064615.6A CN117304913A (en) | 2023-08-23 | 2023-08-23 | Dyeing tracer for fracturing propping agent and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311064615.6A CN117304913A (en) | 2023-08-23 | 2023-08-23 | Dyeing tracer for fracturing propping agent and preparation method and application thereof |
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