CN115306376A - Oil-gas well fracturing monitoring reagent, method and application thereof - Google Patents
Oil-gas well fracturing monitoring reagent, method and application thereof Download PDFInfo
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- CN115306376A CN115306376A CN202110502517.0A CN202110502517A CN115306376A CN 115306376 A CN115306376 A CN 115306376A CN 202110502517 A CN202110502517 A CN 202110502517A CN 115306376 A CN115306376 A CN 115306376A
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 19
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 24
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- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 24
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- 238000012360 testing method Methods 0.000 claims abstract description 14
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- 229910052738 indium Inorganic materials 0.000 claims abstract description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052747 lanthanoid Inorganic materials 0.000 claims abstract description 5
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- 229910052702 rhenium Inorganic materials 0.000 claims abstract description 5
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims abstract description 5
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- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims abstract description 5
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- 239000011669 selenium Substances 0.000 claims abstract description 5
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- 239000003921 oil Substances 0.000 claims description 94
- 238000004519 manufacturing process Methods 0.000 claims description 44
- 239000012530 fluid Substances 0.000 claims description 23
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- 229920005989 resin Polymers 0.000 claims description 15
- 239000004576 sand Substances 0.000 claims description 11
- 239000010779 crude oil Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- OSTIHFXUTPZJQL-UHFFFAOYSA-N fluoro benzoate Chemical compound FOC(=O)C1=CC=CC=C1 OSTIHFXUTPZJQL-UHFFFAOYSA-N 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 5
- 239000008139 complexing agent Substances 0.000 claims description 5
- YQUHULOBTDYMAG-UHFFFAOYSA-N methyl 2,4-difluorobenzoate Chemical compound COC(=O)C1=CC=C(F)C=C1F YQUHULOBTDYMAG-UHFFFAOYSA-N 0.000 claims description 4
- QAFJIJWLEBLXHH-UHFFFAOYSA-N methyl 2-fluorobenzoate Chemical compound COC(=O)C1=CC=CC=C1F QAFJIJWLEBLXHH-UHFFFAOYSA-N 0.000 claims description 4
- YXZNVLYXBIIIOB-UHFFFAOYSA-N methyl 3-fluorobenzoate Chemical compound COC(=O)C1=CC=CC(F)=C1 YXZNVLYXBIIIOB-UHFFFAOYSA-N 0.000 claims description 4
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 3
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
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- MAEQYZYOSFAUAF-UHFFFAOYSA-N methyl 2,3,4,5-tetrafluorobenzoate Chemical compound COC(=O)C1=CC(F)=C(F)C(F)=C1F MAEQYZYOSFAUAF-UHFFFAOYSA-N 0.000 claims description 3
- QNPFLTKQLFSKBY-UHFFFAOYSA-N methyl 2,6-difluorobenzoate Chemical compound COC(=O)C1=C(F)C=CC=C1F QNPFLTKQLFSKBY-UHFFFAOYSA-N 0.000 claims description 3
- DWRVHDWKWKFSAI-UHFFFAOYSA-N methyl 3,4-difluorobenzoate Chemical compound COC(=O)C1=CC=C(F)C(F)=C1 DWRVHDWKWKFSAI-UHFFFAOYSA-N 0.000 claims description 3
- MSEBQGULDWDIRW-UHFFFAOYSA-N methyl 4-fluorobenzoate Chemical compound COC(=O)C1=CC=C(F)C=C1 MSEBQGULDWDIRW-UHFFFAOYSA-N 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
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- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 3
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- OPQFYGPAOVCNEQ-UHFFFAOYSA-N ethyl 2,4-difluorobenzoate Chemical compound CCOC(=O)C1=CC=C(F)C=C1F OPQFYGPAOVCNEQ-UHFFFAOYSA-N 0.000 description 2
- RUWPGPOBTHOLHF-UHFFFAOYSA-N ethyl 2-fluorobenzoate Chemical compound CCOC(=O)C1=CC=CC=C1F RUWPGPOBTHOLHF-UHFFFAOYSA-N 0.000 description 2
- SMMIKBXLEWTSJD-UHFFFAOYSA-N ethyl 3-fluorobenzoate Chemical compound CCOC(=O)C1=CC=CC(F)=C1 SMMIKBXLEWTSJD-UHFFFAOYSA-N 0.000 description 2
- UMPRJGKLMUDRHL-UHFFFAOYSA-N ethyl 4-fluorobenzoate Chemical compound CCOC(=O)C1=CC=C(F)C=C1 UMPRJGKLMUDRHL-UHFFFAOYSA-N 0.000 description 2
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- 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 description 1
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- SBHMXBYMQZRRLC-UHFFFAOYSA-N ethyl 2,3,4,5-tetrafluorobenzoate Chemical compound CCOC(=O)C1=CC(F)=C(F)C(F)=C1F SBHMXBYMQZRRLC-UHFFFAOYSA-N 0.000 description 1
- FBQKPNPHWYPJFU-UHFFFAOYSA-N ethyl 2,6-difluorobenzoate Chemical compound CCOC(=O)C1=C(F)C=CC=C1F FBQKPNPHWYPJFU-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- 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
-
- 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
- E21B49/00—Testing the nature of borehole walls; Formation testing; Methods or apparatus for obtaining samples of soil or well fluids, specially adapted to earth drilling or wells
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Mining & Mineral Resources (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides an oil-gas well fracturing monitoring reagent, an oil-gas well fracturing monitoring method and application thereof. The reagent comprises an oil-soluble tracer and a water-soluble tracer, wherein the oil-soluble tracer comprises: a fluorine-containing organic compound, a carrier for loading the fluorine-containing organic compound, and an oil-soluble coating for coating the fluorine-containing organic compound and the carrier; the water-soluble tracer comprises: a water-soluble complex of any one of the trace elements selected from the group consisting of lanthanides and any one of scandium, yttrium, gallium, indium, thallium, germanium, rhenium, selenium and tellurium. Through two kinds of tracer detection, the effect of horizontal well staged fracturing or every layer of fracturing of vertical well of understanding that can be direct knows the productivity condition of every section or every layer, and the test result can provide reliable foundation for the improvement of next step's fracturing scheme.
Description
Technical Field
The invention relates to the field of testing of oil and gas field development, in particular to an oil and gas well fracturing monitoring reagent, an oil and gas well fracturing monitoring method and application of the oil and gas well fracturing monitoring reagent.
Background
In oil field development, oil well fracturing technology is continuously developed to achieve higher productivity. In recent years, the staged fracturing technology of horizontal wells, whether oil wells or gas wells (containing shale gas), has been developed rapidly. But how to evaluate and analyze the fracturing effect and the productivity of each section is very important, which has important guiding significance on the fracturing design and the development and adjustment of the later stage of fracturing. At present, the fracture form of fracturing is monitored by utilizing a microseism technology, but the technology needs complicated equipment and large investment, and the fracturing effect and the capacity condition of each section cannot be distinguished.
Thus, there remains a need for improvements to existing monitoring methods.
Disclosure of Invention
The invention mainly aims to provide an oil-gas well fracturing monitoring reagent, an oil-gas well fracturing monitoring method and application thereof, and aims to solve the problem that the fracturing effect of each section cannot be accurately monitored in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a well fracture monitoring reagent comprising an oil-soluble tracer and a water-soluble tracer, wherein the oil-soluble tracer comprises: a fluorine-containing organic compound, a carrier carrying the fluorine-containing organic compound, and an oil-soluble coating the fluorine-containing organic compound and the carrier; the water-soluble tracer comprises: a water-soluble complex of any one of the following trace elements: lanthanides, scandium, yttrium, gallium, indium, thallium, germanium, rhenium, selenium and tellurium.
Furthermore, in the oil-soluble tracer, the content of the fluorine-containing organic compound is 10-20 wt%, the content of the carrier is 60-70 wt%, and the balance is the oil-soluble coating; preferably, the fluorine-containing organic compound is a fluorobenzoate, and more preferably, the fluorobenzoate is selected from any one or more of the following: methyl o-fluorobenzoate, methyl p-fluorobenzoate, methyl m-fluorobenzoate, methyl 2, 4-difluorobenzoate, methyl 2, 6-difluorobenzoate, methyl 3, 4-difluorobenzoate and methyl 2,3,4, 5-tetrafluorobenzoate.
Further, the carrier is a porous carrier, preferably the porous carrier is in a granular form, and more preferably the porous carrier is an alumina carrier; further preferably porous ceramics, porous ceramisite or porous volcanic rock.
Further, the oil-soluble coating is formed by curing resin, preferably the resin is one or more selected from rosin resin, dammar resin and petroleum resin.
Further, the oil-soluble tracer is in the form of particles, and preferably, the particle size of the oil-soluble tracer is 20 to 40 mesh.
Further, the water-soluble complex of the trace elements is formed by complexing the trace elements and a complexing agent EDTA2Na according to a coordination ratio of 1.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for fracture monitoring of an oil and gas well, the method comprising: in the fracturing process, sequentially injecting a water-soluble tracer into each interval of an oil-gas well along with a pad fluid and a sand carrying fluid, controlling the water-soluble tracer to be injected before a displacement fluid, placing an oil-soluble tracer in the front of fracturing sand, and injecting the oil-soluble tracer into each interval of the oil-gas well along with the sand carrying fluid; after fracturing is finished, respectively detecting the production concentration and time of the water-soluble tracer and the oil-soluble tracer in each layer section in the flowback fluid, and drawing a production curve of the water-soluble tracer and a production curve of the oil-soluble tracer; evaluating the fracturing condition of each interval according to the production curve of the water-soluble tracer, and evaluating the oil production condition of each interval according to the production curve of the oil-soluble tracer; the water-soluble tracer and the oil-soluble tracer are oil-soluble tracer and water-soluble tracer in any one of the oil-gas well fracturing monitoring reagents.
Further, the dosage of the water-soluble tracer is as follows:
A＝Ci*Vp*10 -3 -o-f- -a compound of formula (I),
Vp＝V1+V2，
a represents the dosage of the water-soluble tracer with the unit of g,
ci represents the concentration of water-soluble tracer in ng/ml,
vp represents the volume of fracturing fluid required by the ith interval in m 3 ，
V1 represents the required pad volume of the ith interval in m 3
V2 represents the volume of the sand-carrying fluid required by the ith interval and has the unit of m 3 。
Further, the dosage of the oil-soluble tracer is as follows:
Aij＝Ai*10 3 *Cj*10 -9 10% - - - - - - - - - - - - -formula (II),
wherein Ai =10 4 ，
Ai represents the total amount of crude oil in tons,
aij represents the amount of the oil-soluble tracer required by the ith interval, and the unit is Kg,
cj represents the saturation concentration of the oil soluble tracer in the crude oil in the ith interval in ppb,
10% represents the content of the fluorine-containing organic compound in the oil-soluble tracer.
According to another aspect of the present invention there is provided the use of any one of the above-described well fracture monitoring agents in well fracture monitoring.
And further, detecting the fracturing conditions of each interval of the oil-gas well according to the method, wherein the oil-soluble tracer and the water-soluble tracer used by each interval are different.
By applying the technical scheme of the invention, two tracers with completely different properties are adopted, and different types of tracers are added into different intervals of the horizontal well according to the monitoring purpose, so that the water yield of different intervals is different, and the concentrations of the water-soluble tracers are different; the oil yield is different, the concentration of oil-soluble tracer is different, and different types of tracers are added into different monitoring layers (sections) when fracturing is facilitated, so that the oil yield and the water yield of each layer section can be accurately monitored and evaluated. Through two kinds of tracer detection, the effect of horizontal well staged fracturing or every layer of fracturing of vertical well of understanding that can be direct knows the productivity condition of every section or every layer. The test result provides reliable basis for the improvement of the next fracturing scheme and the taking of measures.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view showing the flow of processing of a prototype in example 1.
Figure 2 shows a graph of water aqua assay data for each stage in example 1.
FIG. 3 is a graph showing the data of the oil assay in each stage of example 1.
FIG. 4 shows a graph of instantaneous water contribution rate in stage 2 of example 1.
Fig. 5 shows a graph of the instantaneous contribution rate of stage 3 water in example 1.
FIG. 6 shows a graph of the transient contribution rate of stage 4 water in example 1.
Fig. 7 shows a graph of the instantaneous contribution rate of stage 5 water in example 1.
Fig. 8 shows a graph of the instantaneous contribution rate of stage 6 water in example 1.
Fig. 9 shows a graph of the instantaneous contribution rate of stage 7 water in example 1.
Fig. 10 shows a graph of the instantaneous contribution rate of water in stage 8 of example 1.
FIG. 11 is a graph showing the instantaneous contribution rate of water in stage 8 of example 1.
FIG. 12 shows a graph of the transient contribution rate of the oil of stage 2 in example 1.
FIG. 13 shows a graph of the transient contribution rate of oil in stage 3 of example 1.
FIG. 14 shows a graph of the transient contribution rate of oil in stage 4 of example 1.
FIG. 15 shows a graph of the transient contribution rate of the oil of paragraph 5 in example 1.
FIG. 16 shows a graph of the transient contribution rate of oil at stage 6 of example 1.
FIG. 17 shows a graph of the instantaneous contribution rate of oil in stage 7 of example 1.
FIG. 18 shows a graph of the instantaneous contribution rate of oil in stage 8 of example 1.
FIG. 19 shows a graph of the transient contribution rate of oil in paragraph 9 of example 1.
Fig. 20 to 24 show the water production profile at different time points and the water production profile during monitoring in example 1, respectively.
Fig. 25 to 28 show the oil production profile at different time points and the oil production profile during monitoring in example 1, respectively.
Figure 29 shows a comparison of water and oil production profiles during monitoring in example 1.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
In an exemplary embodiment of the present application, there is provided a well fracture monitoring reagent comprising an oil-soluble tracer and a water-soluble tracer, wherein the oil-soluble tracer comprises: a fluorine-containing organic compound, a carrier carrying the fluorine-containing organic compound, and an oil-soluble coating the fluorine-containing organic compound and the carrier; the water-soluble tracer comprises: a water-soluble complex of any one of the following trace elements: lanthanides, scandium, yttrium, gallium, indium, thallium, germanium, rhenium, selenium and tellurium.
According to the method, two tracers with completely different properties are adopted, and different types of tracers are added into different intervals of the horizontal well according to the monitoring purpose, so that the water yield of different intervals is different, and the concentrations of water-soluble tracers are different; the oil production quantity is different, the concentration of the oil-soluble tracer is different, and different types of tracers can be added into different monitoring layers (sections) conveniently during fracturing, so that the oil production and the water production of each layer section can be accurately monitored and evaluated. Through two kinds of tracer detection, the effect of horizontal well staged fracturing or every layer of fracturing of vertical well that can be direct is known, the productivity condition of every section or every layer is known. The test result provides reliable basis for the improvement of the next fracturing scheme and the taking of measures.
Trace elements in this application refer to some rare or transition metal elements including lanthanides and scandium, yttrium, gallium, indium, thallium, germanium, rhenium, selenium and tellurium. The term "trace elements" does not include the trace elements that are present in the water-soluble tracer in a small amount. The trace elements in the water-soluble tracer have the advantages of small addition amount, high detection precision, no toxicity, no harm, no radioactivity, safety, environmental protection, good compatibility with the fracturing fluid, and only solubility in water but not oil. It should be noted that the types of trace elements contained in different water-soluble tracers are different, and each water-soluble tracer only contains one trace element and a complexing agent.
The carrier of the oil-soluble tracer is usually a porous carrier, and the adsorbed oil-soluble tracer substance and the oil-soluble coating can be slowly released into crude oil or liquid hydrocarbon products, so that the purpose of long-term monitoring can be achieved. The oil soluble tracer is soluble only in oil and insoluble in water.
In a preferred embodiment, the oil-soluble tracer is prepared as follows: 1. dissolving a fluorine-containing organic compound in an organic solvent, uniformly stirring the fluorine-containing organic compound and a porous carrier material, and drying the mixture in a 65 ℃ drying oven; 2. preheating the mixture to 150 ℃, adding an oil-soluble coating material, rapidly and forcibly stirring, adding a curing agent and a lubricant, stirring for several minutes, and placing the mixture in a drying oven for cooling and drying; 3. and (4) crushing and granulating. The particle size is equivalent to that of the corresponding fracturing propping object (20-40 meshes).
In a preferred embodiment of the present application, in the oil-soluble tracer, the content of the fluorine-containing organic compound is 10 to 20wt%, the content of the carrier is 60 to 70wt%, and the balance is the oil-soluble coating; more preferably, the mass ratio of the three components is 10:70:20. the mixture according to the proportion has the beneficial effects of stable and controllable release speed of the tracer and long validity period.
In the application, the fluorine-containing organic compound is preferably a fluorobenzoate substance, and the fluorine-containing organic compound has the beneficial characteristics of stable property and convenience in detection. More preferably, the fluorobenzoate group is selected from any one or more of: methyl o-fluorobenzoate, methyl p-fluorobenzoate, methyl m-fluorobenzoate, methyl 2, 4-difluorobenzoate, methyl 2, 6-difluorobenzoate, methyl 3, 4-difluorobenzoate and methyl 2,3,4, 5-tetrafluorobenzoate, ethyl o-fluorobenzoate, ethyl m-fluorobenzoate, ethyl p-fluorobenzoate, ethyl 2, 4-difluorobenzoate, ethyl 2, 6-difluorobenzoate and ethyl 2,3,4, 5-tetrafluorobenzoate. The fluorobenzoate compounds in the above category have excellent properties of easy procurement and high detection sensitivity.
The carrier is a porous carrier, and any existing porous carrier can be used as the carrier. The porous carrier is preferably granular, and more preferably, the porous carrier is an alumina carrier; further preferably porous ceramics, porous ceramsites or porous volcanic rocks with low cost and wide sources.
The oil-soluble coating is formed by curing resin, preferably the resin is one or more selected from rosin resin, dammar resin and petroleum resin. The oil-soluble polymer has the function of excellent oil solubility and can be uniformly dissolved in crude oil.
The oil-soluble tracer is granular, and preferably has a particle size of 20-40 meshes, which is equivalent to that of the corresponding fracturing propping object.
The complexing agent in the water-soluble tracer is an EDTA complex system, preferably EDTA and EDTA-2Na. Preferably, the water-soluble complex of the trace elements is formed by complexing the trace elements and a complexing agent EDTA according to a coordination ratio of 1. The two are mixed according to the coordination ratio, so that the advantages of stable property, good compatibility with stratum, reduction of stratum adsorption and the like are achieved.
The synthesis method and the process of the complex are detailed in the application publication number of the early invention of the inventor, namely, the tracer of the constant substance used in oil field monitoring and the use method of the tracer in dynamic monitoring of oil reservoirs: CN 169998.
A water-soluble complex of any trace element formed from the chloride of that element and EDTA in a ratio of 1:1 coordination ratio of
In a second exemplary embodiment of the present application, there is provided a method of monitoring a fracture of an oil or gas well, the method comprising: in the fracturing process, sequentially injecting a water-soluble tracer into each interval of an oil-gas well along with a pad fluid and a sand-carrying fluid, controlling the water-soluble tracer to be injected before a displacement fluid, placing an oil-soluble tracer in the front of fracturing sand, and injecting the oil-soluble tracer into each interval of the oil-gas well along with the sand-carrying fluid; after fracturing is completed, respectively detecting the production concentrations and the time of the water-soluble tracer and the oil-soluble tracer in each interval of the flowback fluid, and drawing a production curve of the water-soluble tracer and a production curve of the oil-soluble tracer; evaluating the fracturing condition of each interval according to the production curve of the water-soluble tracer, and evaluating the oil production condition of each interval according to the production curve of the oil-soluble tracer; the water-soluble tracer and the oil-soluble tracer are oil-soluble tracer and water-soluble tracer in any one of the oil-gas well fracturing monitoring reagents.
Through two kinds of tracer detection, can directly, accurately know the effect of horizontal well staged fracturing or every layer of fracturing of vertical well, know the productivity condition of every section or every layer. And the test result provides reliable basis for the improvement of the next fracturing scheme and the taking of measures.
In a preferred embodiment of the present application, the water-soluble tracer is used in an amount of:
A＝Ci*Vp*10 -3 -o-f- -a compound of formula (I),
Vp＝V1+V2，
a represents the amount of water-soluble tracer in g,
ci represents the concentration of water-soluble tracer (preferably 1000 ng/ml), in ng/ml,
vp represents the volume of fracturing fluid required by the ith interval and is expressed in m 3 ，
V1 represents the required pad volume of the ith interval in m 3
V2 represents the volume of the sand-carrying fluid required by the ith interval and has the unit of m 3 。
In a preferred embodiment of the present application, the oil-soluble tracer is used in the amount of:
Aij＝Ai*10 3 *Cj*10 -9 10% - - - - - - - - - - - - -formula (II),
wherein Ai =10 4 ，
Ai represents the total amount of crude oil in tons,
aij represents the amount of oil soluble tracer required in the ith interval, in Kg,
cj represents the saturation concentration of the oil soluble tracer in the crude oil in the ith interval in ppb,
10% represents the content of the fluorine-containing organic compound in the oil-soluble tracer.
In the above preferred embodiment, the calculation formulas of the amount of the water-soluble tracer and the amount of the oil-soluble tracer are respectively obtained according to the maximum concentration/saturation of the tracer in the fracturing fluid/crude oil, and the calculation of the amount of each layer/section according to the above formulas can be relatively more accurate.
In a third exemplary embodiment of the present application, there is provided the use of any one of the above-described well fracture monitoring agents in well fracture monitoring.
The application comprises the step of detecting the fracturing condition of each interval of the oil-gas well according to any one of the oil-gas well fracturing monitoring methods, wherein the oil-soluble tracer and the water-soluble tracer used by each interval are different.
The following examples are included to further illustrate the benefits of the present application. In the following examples, the oil-soluble tracer and the water-soluble tracer are simply referred to as an oil agent and an aqueous agent, respectively.
1.Oil-gas well fracturing monitoring reagent formula and construction scheme
Construction injection is completed on the south 218-Ping 335 tracer site in the range of 2018-8-4 to 2018-8-7 according to the following scheme, and detailed construction data are shown in Table 1.
TABLE 1 construction injection watch for south 218-Ping 335 tracer
Table 2:
| type of aqueous solution | Tracer substance and concentration | Kind of oil agent | Tracer substance and concentration |
| MT6 | Praseodymium chloride-EDTA complex 5% | ST-02a | P-fluorobenzoic |
| MT3 | Neodymium chloride-EDTA complex 5% | ST- |
2,2,3,4,5-tetrafluorobenzoic |
| MT1 | Lanthanum chloride-EDTA complex 5% | ST-03b | Ethyl m-fluorobenzoate 10% |
| MT2 | Gadolinium chloride-EDTA complex 5% | ST-02b | Ethyl p-fluorobenzoate 10% |
| MT8 | Samarium chloride-EDTA complex 5% | ST- |
2, 4-difluorobenzoic |
| MT11 | Dysprosium chloride-EDTA complex 5% | ST-03a | M-fluorobenzoic |
| MT4 | Erbium chloride-EDTA complex 5% | ST- |
10 percent of ethyl o-fluorobenzoate |
| MT14 | Lutetium chloride-EDTA complex 5% | ST- |
10% of o-fluorobenzoic acid methyl ester |
| MT12 | Ytterbium chloride-EDTA complex 5% | ST- |
2, 4-Difluorobenzoic |
2. Sampling and assaying
1) Sampling
From 2018, 8, 7, 13:00 start sampling by 2018, 10, 6, 14:00, 362 oil-water samples are taken in total, and the sampling frequency is 6 per 1 day;
2) Sample testing
(1) Aqueous phase sample testing
The obtained sample is detected, firstly the sample is subjected to early-stage treatment, organic matters and solid impurities are removed by digestion and filtration, and then the detection is carried out by using an inductive plasma mass spectrometer. The specific test flow is as follows:
a) Pretreatment of samples
And filtering a primary sample (a sample transported to a laboratory from a field), carrying out nitration, evaporation to dryness, cooling and acid dilution to finally obtain a sample to be detected. The detailed process flow is shown in FIG. 1 below.
b) Testing various tracer concentrations
The concentrations of the various tracers were measured via inductively coupled plasma mass spectrometry (ICP-MS). The instrument test principle is as follows: ICP is used as a high-temperature ion source (7000K) of mass spectrum, and the sample is subjected to processes of evaporation, dissociation, atomization, ionization and the like in a channel. Ions enter a high-vacuum MS part through a sample cone interface and an ion transmission system, the MS part is a quadrupole rapid scanning mass spectrometer, all ions are separated and determined through high-speed sequential scanning, the mass number range of scanning elements is from 6 to 260, the ions separated through a high-speed double channel are detected, the linear dynamic range of concentration reaches 9 orders of magnitude, and direct determination is carried out from ppq to ppm.
(2) Oil sample testing
Testing various tracer concentrations
An instrument device: triple quadrupole LC Mass spectrometer (Agilent 6470B);
the obtained sample is firstly subjected to oil-water separation, impurities are removed through filtration, the component to be detected in the oil sample is extracted by using a special organic solvent, the tracer content in the sample is analyzed and detected by adopting a triple quadrupole liquid chromatography-mass spectrometer, and the lowest detection limit of the analyzer can reach the ppq level.
3) Test results
Water samples are assayed for 8 trace elements, data is obtained by 362 × 8=2896, and the period is 20180807 13 from 00 to 20181006 14; oil samples were assayed for 8 oils, giving a data of 251 × 8=2008, see 20180826 2 during oil period from 00 to 20181006 14.
The water assay data of each section is shown in fig. 2, and the oil assay data is shown in fig. 3.
3. Explanation of the invention
1) Analysis of contribution rate
Water/oil contribution rate calculation model for each section:
Pi＝Ci/(C2+C3+…C9)
ci: the assay concentration of the i-stage water/oil phase tracer is ng/ml;
pi is the i-th stage water/oil contribution rate.
(1) Contribution rate of each stage of water
Layer 2: as shown in fig. 4, in the initial stage of flowback, the water contribution rate was high (11%), then slowly decreased to about 20d to 9.31% of monitoring, and then fluctuated about 9.74%, with a maximum of 11.59%, a minimum of 8.75%, and an average of 9.79% during monitoring. Lower than the average contribution rate of each segment.
Layer 3: as shown in fig. 5, the contribution rate of the segment does not slightly rise during the monitoring period, and the contribution rate is 10.92% at most, 8.44% at most and 9.67% on average during the monitoring period. Lower than the average contribution rate of each segment.
Layer 4: referring to fig. 6, in the initial stage of flowback, the water contribution rate is increased in a single-sided and slow manner within 0-20 d; the 20 th d to 45 th d fluctuate up and down by about 12.06%; 45 to 60d fluctuated around 11.48%. The monitoring period was 13.22% maximum, 9.86% minimum, and 11.59% average. Slightly lower than the average contribution rate of each segment.
A 5 th layer section: referring to FIG. 7, the water contribution rate is increased in a single-sided rapid manner from 0d to 12 d; the 12d th to 50d th fluctuates around 11.08%; 50 to 60d fluctuated around 11.91%. The monitoring period was up to 12.66%, minimum 8.0%, average 10.98%. Slightly lower than the average contribution rate of each segment.
The 6 th layer: referring to FIG. 8, the water contribution rate decreases unilaterally and rapidly from 0 to 15 d; the 15 th to 60 th pulses fluctuate around 14.668%. The monitoring period was 18.82% maximum, 12.16% minimum, and 14.66% average. 3 one of the major labor producing layers.
The 7 th layer: referring to FIG. 9, the water contribution rate is increased in a single-sided rapid manner from 0d to 10 d; the 10 th d to 60 th d fluctuated about 16.31% up and down. The monitoring period was 18.27% maximum, 12.50% minimum, and 16.31% average. 3 one of the major water producing layers.
Layer 8: referring to FIG. 10, the water contribution rate is single-sided and rapidly increased from 0 to 13 d; the 13 th to 60 th waves about 11.73%. The monitoring period was 13.09% maximum, 8.03% minimum, and 11.34% average. Lower than average.
Layer 9: referring to FIG. 11, the water contribution rate decreases slowly in a single side from 0d to 30 d; the 30 th to 60 th waves fluctuate around 14.37%. The monitoring period was 22.08% maximum, 12.55% minimum, and 15.67% average. 3 one of the major labor producing layers.
(2) Oil contribution rate of each stage
Layer 2: referring to fig. 12, the oil contribution rate fluctuates around 8.5% up and down during the monitoring period, with a maximum of 9.4%, a minimum of 7.5%, and an average of 8.5% that is much lower than the average, non-prime pay zone.
Layer 3: referring to fig. 13, the oil contribution during monitoring is floating up and down around 13.2%, with a maximum of 14.5%, a minimum of 12.0%, and an average of 13.2% during monitoring, slightly above the average, one of the main force pay zones.
Layer 4: referring to fig. 14, the oil contribution rate in the monitoring period almost has a unilateral descending trend, the descending amplitude of 0-40d is large, the descending amplitude of 40-60d is small, the maximum of 10.9%, the minimum of 6.6% and the average of 8.3% in the monitoring period are far lower than the average value, and the oil contribution rate is not a dominant oil production layer.
A 5 th layer section: referring to fig. 15, the oil contribution rate in the monitoring period almost has a unilateral upward trend, and the maximum in the monitoring period is 18.9%, the minimum in the monitoring period is 14.4%, and the average in the monitoring period is 16.3%, which is far higher than the average value, namely the main pay zone.
Layer 6: referring to fig. 16, the single-edge drop of 0-48d, the drop of 48-60d around 5.3% is small, the maximum 10.9%, the minimum 6.6%, and the average 8.3% during monitoring are far lower than the average value, which is a non-dominant pay zone.
The 7 th layer: referring to FIG. 17, the single-edge rise of 0-42d, fluctuation of 42-60d around 22.3% is up and down, the maximum of 24.2%, the minimum of 17.9%, and the average of 21.4% during monitoring are far higher than the average value, the main pay zone.
Layer 8: referring to fig. 18, during monitoring, the single-edge rise is achieved, and the maximum of the monitoring period is 21.0%, the minimum is 16.5%, and the average is 19.1%, which is far higher than the average value, the main pay zone.
Layer 9: referring to fig. 19, the fluctuation amplitude is small, with a maximum of 7.7%, a minimum of 6.2%, and an average of 6.9%, much lower than the mean, non-dominant reservoir.
2) Water production profile
20180807 15.
20180827 The 14.
20180916 The water production profile at 14.
20181006 The water production profile of 14.
Water production profile during monitoring is shown in figure 24.
And (3) knotting: (1) the contribution rate of each section of water is changed and the change amplitude is different; (2) the difference of the water contribution rate of each section at the initial stage of flowback is serious, and the difference at the later stage is small; (3) the main power water producing layer sections are 9 th, 7 th and 6 th; (4) the interval of the intermediate water producing layer is the 8 th, 5 th and 4 th sections; (5) the poor water producing interval is the 3 rd and 2 nd sections.
3) Oil production profile
20180827 See fig. 25 for a 14.
20180916 The oil production profile of 14.
20181006 The oil production profile of 14.
The oil production profile during monitoring is shown in fig. 28.
And (4) summarizing: (1) the oil contribution rate of each section is changed and the change amplitude is different; (2) the main oil producing layer sections are the 8 th, 7 th, 5 th and 3 rd sections; (3) the middle oil production intervals are 9 th, 6 th, 4 th and 2 th.
4. Comprehensive evaluation
1) Oil and water production evaluation
TABLE 3 evaluation chart of the produced water and oil of each stage of nan 218-ping 335
Oil and water production evaluation description: above 12.5% is the dominant force and below 12.5% is the non-dominant force. The comparison of the water and oil production profiles during the monitoring period is shown in FIG. 29.
(1) Water production evaluation
The main power water producing layer comprises: in the 4 th, 6 th, 7 th and 9 th layer sections, the total contribution rate is 58.9%; the non-principal water producing layer has: in the 2 nd, 3 rd, 5 th and 8 th intervals, the total contribution rate is 41.1%.
(2) Evaluation of oil production
The main oil production layer comprises: in the 3 rd, 5 th, 7 th and 8 th intervals, the total contribution rate is 68.5%; the non-principal oil producing layer comprises: in the 2 nd, 4 th, 6 th and 9 th intervals, the total contribution rate is 31.5%.
2) Evaluation of fracturing Effect
TABLE 4 fracturing effect evaluation table for each section of south 218-Ping 335
Description of the invention: the single sand water/oil/liquid contribution rate is the water/oil/liquid contribution rate of the section divided by the sand adding amount of the section during the monitoring period; the difference/medium/good in the evaluation of the fracturing effect is a relative concept and is divided according to the amount of the single sand liquid. (1) Fractured well interval: paragraphs 4,5, 7 and 8; (2) interval in fracturing: paragraphs 3, 6 and 9; (3) poor fractured interval: stage 2.
5. Conclusion and instructive significance
1) Conclusion
(1) The 2 nd to 9 th sections contribute to the process, and no mechanical blockage exists;
(2) in the 3 rd, 5 th, 7 th and 8 th main force oil production intervals, the oil contribution rates are respectively 12.9%, 16.0%, 21% and 18.7%, the total contribution rate is 68.6%, and the oil contribution rates are all new joint common fracturing;
(3) the water contribution rates of the 3 rd, 5 th, 7 th and 8 th main oil layer sections are respectively 9.5%, 10.8%, 16.0% and 11.2%, the total amount is 47.4%, and 1 high-yield water layer section and 3 low-yield water layer sections;
(4) in the 2 nd, 4 th, 6 th and 9 th intervals which are not the main power oil production intervals, the oil contribution rates are respectively as follows: 8.3%, 8.1%, 8.2%, 6.8% total 31.4%,3 old fractures were fractured repeatedly and 1 new fracture was fractured normally.
(5) The water contribution rates of the 2 nd, 4 th, 6 th and 9 th sections of the non-dominant oil interval are respectively 9.6%, 13.0%, 14.4% and 15.4%, and are 52.4% in total, and 1 low water production interval and 3 high water production intervals are provided.
2) The meaning of the guidance
(1) The water contribution rate of each interval changes along with the change of production time (flow back), and the change range of the water contribution rate at the initial stage of flow back is larger, the change range of the water contribution rate is smaller and smaller along with the time, and the water contribution rate finally tends to be stable;
(2) the oil contribution rate of each interval is not constant, but the change is small relative to the change of water;
(3) the major oil reservoir has relatively large oil contribution rate and relatively small water contribution rate in most of the oil and water, and the oil and water contribution rates of individual wells are large, for example, the oil and water contribution rates of a 7 th layer are large;
(4) most of the non-main oil reservoirs have smaller oil contribution rate and larger water contribution rate, but the 2 nd layer is exceptional;
(5) the main oil layers are all newly fractured and are subjected to common fracturing; and the non-main oil reservoir is only subjected to 1 new fracture and common fracturing, and the other 3 new fractures are all subjected to old fracture repeated fracturing.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: through two kinds of tracer detection, the effect of horizontal well staged fracturing or each layer of fracturing of a vertical well can be directly known, and the productivity condition of each stage or each layer can be directly known. The monitoring result of the application can provide reliable basis for the improvement and the measure of the next fracturing scheme.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (11)
1. An oil and gas well fracturing monitoring reagent, characterized in that the reagent comprises an oil-soluble tracer and a water-soluble tracer, wherein,
the oil-soluble tracer comprises: the coating comprises a fluorine-containing organic compound, a carrier for supporting the fluorine-containing organic compound and an oil-soluble coating for coating the fluorine-containing organic compound and the carrier;
the water-soluble tracer comprises: a water-soluble complex of any one of the following trace elements: lanthanides, scandium, yttrium, gallium, indium, thallium, germanium, rhenium, selenium and tellurium.
2. The reagent as claimed in claim 1, wherein in the oil-soluble tracer, the content of the fluorine-containing organic compound is 10 to 20wt%, the content of the carrier is 60 to 70wt%, and the balance is the oil-soluble coating;
preferably, the fluorine-containing organic compound is a fluorobenzoate,
more preferably, the fluorobenzoate is selected from any one or more of: methyl o-fluorobenzoate, methyl p-fluorobenzoate, methyl m-fluorobenzoate, methyl 2, 4-difluorobenzoate, methyl 2, 6-difluorobenzoate, methyl 3, 4-difluorobenzoate and methyl 2,3,4, 5-tetrafluorobenzoate.
3. The reagent of claim 1, wherein the support is a porous support, preferably the porous support is in the form of particles, more preferably the porous support is an alumina support; further preferably porous ceramics, porous ceramsite or porous volcanic rock.
4. The agent according to claim 1, wherein the oil-soluble coating is obtained by curing a resin, preferably the resin is selected from any one or more of rosin resin, dammar resin and petroleum resin.
5. Reagent according to any one of claims 1 to 4, characterized in that the oil-soluble tracer is in particulate form, preferably the particle size of the oil-soluble tracer is 20-40 mesh.
6. The reagent according to any one of claims 1 to 4, characterized in that the water-soluble complex of the trace element is formed by complexing the trace element with a complexing agent EDTA according to a coordination ratio of 1.
7. A method of monitoring fracturing in an oil or gas well, the method comprising:
in the fracturing process, sequentially injecting a water-soluble tracer into each interval of an oil-gas well along with a pad fluid and a sand carrying fluid, controlling the water-soluble tracer to be injected before a displacement fluid, placing an oil-soluble tracer in the front of fracturing sand, and injecting the oil-soluble tracer into each interval of the oil-gas well along with the sand carrying fluid;
after fracturing is completed, respectively detecting the output concentrations and the time of the water-soluble tracer and the oil-soluble tracer in each interval of the flowback fluid, and drawing an output curve of the water-soluble tracer and an output curve of the oil-soluble tracer; and
evaluating the fracturing condition of each interval according to the production curve of the water-soluble tracer, and evaluating the oil production condition of each interval according to the production curve of the oil-soluble tracer;
wherein the water-soluble tracer and the oil-soluble tracer are the oil-soluble tracer and the water-soluble tracer in the oil and gas well fracturing monitoring reagent of any one of claims 1 to 6.
8. The method of claim 7, wherein the water-soluble tracer is present in an amount of:
A＝Ci*Vp*10 -3 a compound of formula (I),
Vp＝V1+V2，
a represents the dosage of the water-soluble tracer with the unit of g,
ci represents the concentration of the water-soluble tracer in ng/ml,
vp represents the volume of fracturing fluid required by the ith interval and is expressed in m 3 ，
V1 represents the required pad volume of the ith interval in m 3
V2 represents the volume of the sand carrying fluid required by the ith interval and has the unit of m 3 。
9. The method of claim 7, wherein the oil soluble tracer is used in an amount of:
Aij＝Ai*10 3 *Cj*10 -9 10% - - - - - - - - - - - - -formula (II),
wherein Ai =10 4 ，
Ai represents the total amount of crude oil to be marked in the ith interval, in tons,
aij represents the amount of the oil soluble tracer required for the ith interval, in Kg,
cj represents the saturation concentration of the oil soluble tracer in the crude oil in the ith interval in ppb,
10% represents the content of the fluorine-containing organic compound in the oil-soluble tracer.
10. Use of the oil and gas well fracture monitoring agent of any one of claims 1 to 6 in oil and gas well fracture monitoring.
11. Use according to claim 10 for testing the fracturing of intervals in a hydrocarbon well according to the method of any one of claims 7 to 9, wherein the oil-soluble tracer and the water-soluble tracer used in each interval are different.
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