CN115141621A - Oil-based fracturing fluid, multi-stage fracturing method and method for online monitoring productivity of reservoir intervals - Google Patents
Oil-based fracturing fluid, multi-stage fracturing method and method for online monitoring productivity of reservoir intervals Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000012544 monitoring process Methods 0.000 title claims abstract description 20
- DQFBYFPFKXHELB-UHFFFAOYSA-N Chalcone Natural products C=1C=CC=CC=1C(=O)C=CC1=CC=CC=C1 DQFBYFPFKXHELB-UHFFFAOYSA-N 0.000 claims abstract description 34
- 235000005513 chalcones Nutrition 0.000 claims abstract description 34
- 230000011218 segmentation Effects 0.000 claims abstract description 32
- -1 chalcone compound Chemical class 0.000 claims abstract description 30
- 238000001514 detection method Methods 0.000 claims abstract description 20
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- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 24
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- WXPWZZHELZEVPO-UHFFFAOYSA-N (4-methylphenyl)-phenylmethanone Chemical compound C1=CC(C)=CC=C1C(=O)C1=CC=CC=C1 WXPWZZHELZEVPO-UHFFFAOYSA-N 0.000 claims description 10
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- IBRIFDGHXDFGBY-UHFFFAOYSA-N (4-ethoxyphenyl)-phenylmethanone Chemical compound C1=CC(OCC)=CC=C1C(=O)C1=CC=CC=C1 IBRIFDGHXDFGBY-UHFFFAOYSA-N 0.000 claims description 6
- HDXVSZWKIHQDES-LFYBBSHMSA-N (e)-1,3-bis(4-methoxyphenyl)prop-2-en-1-one Chemical compound C1=CC(OC)=CC=C1\C=C\C(=O)C1=CC=C(OC)C=C1 HDXVSZWKIHQDES-LFYBBSHMSA-N 0.000 claims description 6
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- IFQUPKAISSPFTE-UHFFFAOYSA-N 4-benzoylbenzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1C(=O)C1=CC=CC=C1 IFQUPKAISSPFTE-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
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- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
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- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
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- XZNQFPSOLGYVDO-UHFFFAOYSA-N bis(4-ethoxyphenyl)methanone Chemical compound C1=CC(OCC)=CC=C1C(=O)C1=CC=C(OCC)C=C1 XZNQFPSOLGYVDO-UHFFFAOYSA-N 0.000 description 5
- ZWPWLKXZYNXATK-UHFFFAOYSA-N bis(4-methylphenyl)methanone Chemical compound C1=CC(C)=CC=C1C(=O)C1=CC=C(C)C=C1 ZWPWLKXZYNXATK-UHFFFAOYSA-N 0.000 description 5
- LSQARZALBDFYQZ-UHFFFAOYSA-N 4,4'-difluorobenzophenone Chemical compound C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 LSQARZALBDFYQZ-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
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- DTEBZGKINVACPT-FMIVXFBMSA-N (e)-1,3-bis(4-methylphenyl)prop-2-en-1-one Chemical compound C1=CC(C)=CC=C1\C=C\C(=O)C1=CC=C(C)C=C1 DTEBZGKINVACPT-FMIVXFBMSA-N 0.000 description 3
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- AZBVDMNDUOURGI-UHFFFAOYSA-N 1,3-bis(4-fluorophenyl)prop-2-en-1-one Chemical class C1=CC(F)=CC=C1C=CC(=O)C1=CC=C(F)C=C1 AZBVDMNDUOURGI-UHFFFAOYSA-N 0.000 description 2
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Classifications
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- 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
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/64—Oil-based compositions
-
- 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
- E21B49/08—Obtaining fluid samples or testing fluids, in boreholes or wells
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mining & Mineral Resources (AREA)
- Geology (AREA)
- Chemical & Material Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Fluid Mechanics (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to an oil-based fracturing fluid, a multi-stage fracturing method and a method for online monitoring productivity of reservoir intervals. The oil-based fracturing fluid comprises an oil-based base fluid and a segmentation assistant, wherein the segmentation assistant is a chalcone compound and/or a diphenyl ketone compound. The invention also provides a multi-stage fracturing method of the oil-based fracturing fluid and an online productivity monitoring method of an oil reservoir interval. The oil-based fracturing fluid disclosed by the invention is good in stability, good in salt tolerance, less in adhesion with stratum particles and environment-friendly. When the method is used for monitoring the oil production of each layer section in multi-section fracturing, higher detection sensitivity and precision can be obtained under the condition of small using amount of the sectional additives.
Description
Technical Field
The invention belongs to the field of oil reservoir exploration, and particularly relates to an oil-based fracturing fluid, a multi-section fracturing method adopting the oil-based fracturing fluid, and a method for online monitoring of productivity of an oil reservoir interval by adopting the oil-based fracturing fluid.
Background
The fracturing technology is widely applied in China as a common technology for increasing the yield of an oil well, the quality of the fracturing condition directly influences the oil production and the fluid production performance of the well, and the flowback condition of the fracturing fluid is directly related to formation damage. At present, water-based and oil-based fracturing fluids are widely used in China, wherein the oil-based fracturing fluid mainly comprises the following components: 1. oil-based gel fracturing fluids; 2. thickening oil-based fracturing fluid; 3. foam fracturing fluids, and others. The oil-based fracturing fluid is single in functionality and is not as easy and convenient to clean as a water-based fracturing fluid, so that the application range is small. The development of the functional oil-based fracturing fluid can improve the application range of the oil-based fracturing fluid, achieve the aim of one agent with multiple effects, and is one of the research hotspots of the modified fracturing fluid at present. In addition, although the yield is monitored by the online monitoring equipment provided with the induction type flow sensor, the data acquisition card, the signal converter and the like, the equipment device is complicated to set, the monitoring data is easily interfered by electric signals, the monitoring precision is not high, and the real-time online monitoring of different intervals is difficult to realize all the time.
Disclosure of Invention
One of the technical problems to be solved by the invention is that the oil-based fracturing fluid is easy to pollute the environment, and a method for accurately monitoring the productivity of different intervals of an oil reservoir stratum on line in real time is lacked, so that the invention provides the oil-based fracturing fluid, a multi-section fracturing method adopting the oil-based fracturing fluid and a method for monitoring the productivity of the oil reservoir stratum on line by adopting the oil-based fracturing fluid. The oil-based fracturing fluid disclosed by the invention is good in stability and salt tolerance, less in adhesion with stratum particles and environment-friendly. When the method is used for monitoring the oil yield of each layer section in multi-section fracturing, higher detection sensitivity and precision can be obtained under the condition of small using amount of the sectional auxiliary agent.
The invention provides an oil-based fracturing fluid which comprises an oil-based base fluid and a segmentation assistant, wherein the segmentation assistant is a chalcone compound and/or a diphenyl ketone compound.
In some specific embodiments, preferably, the chalcone compound has a structural formula shown in formula (1):
wherein R is saturated or unsaturated C 1 -C 29 An aliphatic carbonyl group; r 1 、R 2 、R 3 、R 4 Each independently selected from H and C 1 ～C 6 Alkyl of (C) 1 ～C 6 And one of alkoxy, nitroso, carboxyl and halogen.
In some embodiments, preferably, in formula (1), R is carbonyl or allylcarbonyl; r 1 、R 2 、R 3 、R 4 Each independently selected from C 1 ～C 6 Alkyl and C 1 ～C 6 One of alkoxy groups of (a).
In some specific embodiments, preferably, the chalcone based compound is selected from one or more of 4,4 '-dimethoxychalcone, 4' -dimethylchalcone, 4 '-difluorochalcone, chalcone, 4-methoxychalcone, 4' -diethylchalcone, 2, 4-dimethylchalcone, 4-methylchalcone, 4 '-methylchalcone, and 4-methoxy-4' methylchalcone.
In some embodiments, preferably, the diphenyl ketone compound has a structural formula represented by formula (2):
wherein R is 1 、R 2 Each independently selected from H and C 1 ～C 12 Alkyl of (C) 1 ～C 12 And one of alkoxy, nitro, nitroso, carboxyl and halogen.
In some embodiments, preferably, the benzophenone compound is selected from one or more of 4,4' -dimethoxybenzophenone, 4' -dimethylbenzophenone, 4' -difluorobenzophenone, benzophenone, 4-methoxybenzophenone, 4' -diethylbenzophenone, 4' -diethoxybenzophenone, 4-methylbenzophenone, 4-diethylbenzophenone, 4-fluorobenzophenone, 4-ethoxybenzophenone, and 4-carboxybenzophenone.
In some embodiments, preferably, R is 1 、R 2 Each independently selected from C 1 ～C 6 Alkyl and C 1 ～C 6 One of alkoxy groups of (a).
In some specific embodiments, it is preferable that the content of the segmentation aid is 0.0001 to 0.01 wt% in the oil-based fracturing fluid.
In some embodiments, preferably, the oil-based base fluid is selected from crude oil and/or finished oil. The product oil is gasoline, kerosene, diesel oil, etc. In the present invention, crude oil, product oil, can be obtained commercially.
In some specific embodiments, preferably, the oil-based fracturing fluid further comprises an auxiliary agent, preferably, the auxiliary agent is selected from one or more of a proppant, a thickener and a cross-linking agent.
In some specific embodiments, preferably, the proppant is selected from one or more of ceramsite, quartz sand, metal aluminum ball, walnut shell, glass bead, plastic ball, steel ball, ceramsite, and resin-coated sand.
In some specific embodiments, preferably, the thickening agent is selected from one or more of vegetable gums or derivatives thereof, cellulose derivatives, biopolysaccharides, polyacrylates, and synthetic polymers, and more preferably, the thickening agent is selected from one or more of guar gum, hydroxypropyl guar gum, fenugreek gum, polyacrylamide, and methylene polyacrylamide.
In some specific embodiments, preferably, the crosslinking agent is a covalent crosslinking agent, more preferably, the crosslinking agent is selected from one or more of polyethylene glycol, diglycidyl ether, maleic anhydride, formaldehyde, glyoxal, glutaraldehyde, toluene diisocyanate, methylene diphenyl diisocyanate, and 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide.
In the present invention, the addition agent, for example, the proppant, thickener and cross-linking agent can be added or not and added according to specific working conditions.
In the present invention, the auxiliary is not limited thereto, and may include a breaker and the like.
In the present invention, "chalcone" is also "chalcone".
In a second aspect, the invention provides a multi-stage fracturing method comprising applying the oil-based fracturing fluid described above to different intervals of a reservoir formation.
The oil-based fracturing fluid may be as desired, and in preferred cases, the oil-based fracturing fluid applied to different intervals will have different staging aids.
In a third aspect of the invention, a method for online monitoring of productivity of an oil reservoir interval is provided, which comprises applying the oil-based fracturing fluid to different intervals of the oil reservoir stratum, wherein the oil-based fracturing fluid applied to different intervals of the oil reservoir stratum has different segmentation aids.
In some specific embodiments, different intervals can be determined according to actual working conditions, and the different intervals are normal operation intervals in the exploration field.
In some embodiments, the method for online monitoring the productivity of the reservoir interval preferably comprises the following steps:
1) Selecting oil-based fracturing fluid, wherein the applied oil-based fracturing fluid has different segmentation aids in different intervals of the oil reservoir stratum;
2) Sampling different intervals of the reservoir formation;
3) Carrying out standardization treatment on the sampled sample;
4) And detecting and calculating the concentration of the sectional aids of different intervals to obtain the productivity of different intervals.
In some embodiments, step 2) may be performed at the monitoring well.
In some embodiments, the sampling period of step 2) may be determined according to the operating conditions, with a wide selection range, the sampling period of step 2) is preferably 15 days to 180 days.
In some specific embodiments, preferably, the normalization processing method in step 3) includes: the sample was dissolved using n-octane and filtered.
In some specific embodiments, preferably, the detecting of step 4) comprises using liquid chromatography-mass spectrometry; preferably, the liquid chromatography uses a normal phase column for the separation detection.
In some specific embodiments, preferably, after step 3) and before step 4), the method further comprises performing filtration. Large-particle suspended matters are filtered out.
In some more specific embodiments, the liquid chromatography detection includes performing separation detection using a positive phase column, performing gradient elution with methanol/ethyl acetate, comparing a peak area of the column with a standard curve, comparing the peak area of the column with the standard curve, calculating concentrations of the segmentation aids in different intervals, and comparing the concentrations with mass spectrum molecular weights to determine productivity between different intervals.
Compared with the prior art, the invention has the following beneficial effects:
(1) The currently applied oil-based fracturing fluid has the problems of poor thermal stability, poor salt resistance and loss caused by adhesion with stratum particles, and the oil-based fracturing fluid disclosed by the invention better solves the problems of the existing oil-based fracturing fluid, has good stability and salt resistance, is less in adhesion with stratum particles and is environment-friendly. The inventive segmentation aids do not interfere with the use of the aid where it is desired to use the aid.
(2) When the oil-based fracturing fluid is used for monitoring the productivity of an oil reservoir interval on line, higher detection sensitivity and detection precision can be obtained under the condition of adding less segmentation aids, the oil reservoir stratum pollution caused by excessive use amount of the segmentation aids is avoided, and the detection method is simple and convenient and is not easily interfered by electric signals.
Detailed Description
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
The raw materials used in the examples and comparative examples are disclosed in the prior art if not particularly limited, and may be, for example, directly purchased or prepared according to the preparation methods disclosed in the prior art. Wherein, the first and the second end of the pipe are connected with each other,
the starting materials used in the syntheses described in the examples are all commercially available,
CAS number for 4,4' -dimethoxychalcone is: 2373-89-9.
CAS number of 4,4' -dimethyl chalcone is: 13565-37-2.
CAS number for 4,4' -difluorochalcone is: 2805-56-3.
CAS number for chalcones is: 94-41-7.
CAS number for 4-methoxychalcone: 959-33-1.
CAS number for 4,4' -diethylchalcone is: 864784-22-5.
CAS number for 2, 4-dimethyl chalcone is: 58764-87-7.
CAS number for 4-methyl chalcone is: 4224-87-7.
CAS number of 4' -methyl chalcone is: 4224-96-8.
CAS number of 4-methoxy-4' methyl chalcone is: 6552-71-2.
CAS number for 4,4' -dimethoxybenzophenone is: 90-96-0.
CAS number for 4,4' -dimethylbenzophenone is: 611-97-2.
CAS number for 4,4' -difluorobenzophenone is: 345-92-6.
The CAS number for benzophenone is: 119-61-9.
The CAS number of 4-methoxybenzophenone is: 611-94-9.
CAS number for 4,4' -diethylbenzophenone is: 21192-56-3.
CAS number for 4,4' -diethoxybenzophenone is: 5032-11-1.
The CAS number of 4-methylbenzophenone is: 134-84-9.
The CAS number of 4-ethyl benzophenone is: 18220-90-1.
CAS number for 4-fluorobenzophenone is: 345-83-5.
The CAS number for 4-ethoxybenzophenone is: 27982-06-5.
The CAS number for 4-carboxybenzophenone is: 1137-42-4.
The performance of the invention was determined as follows:
the percentages and concentrations in the examples and comparative examples are by weight, unless otherwise specified.
The retention rate is calculated by the formula of retention rate = (C) Concentration after aging /C Initial concentration )×100％
[ example 1 ]
The chalcone compounds in table 1 were prepared into n-octane solution with concentration of 50mg/L (the content of the chalcone compounds in the n-octane solution is 50 mg/L), aged at 100 ℃, contained in a 25mL pressure bomb, aged for 30 days, and then sampled for analysis and detection, and concentration and retention rate were calculated. The results of the experiment are shown in table 1:
TABLE 1 thermal stability test of chalcones
| Segmented aid | Retention (%) after 30 days of aging |
| 4,4' -Dimethoxychalcone | 96％ |
| 4,4' -dimethyl chalcone | 99％ |
| 4,4' -difluorochalcones | 98％ |
| Chalcones | 95％ |
| 4-methoxy chalcones | 94％ |
| 4,4' -diethyl chalcone | 95％ |
| 2, 4-dimethyl chalcones | 96％ |
| 4-methyl chalcones | 97％ |
| 4' -methyl chalcones | 98％ |
| 4-methoxy-4' methyl chalcones | 96％ |
[ example 2 ]
Preparing the diphenyl ketone compounds in the table 2 into n-octane solution with the concentration of 50mg/L, aging at 100 ℃, taking 25mL pressure bomb as a container, aging for 30 days, sampling for analysis and detection when aging for 30 days, and calculating the concentration and retention rate, wherein the experimental results are shown in the table 2:
TABLE 2 Heat stability test of Diphenyl ketones
| Segmented aid | Retention (%) after 30 days of aging |
| 4,4' -Dimethoxybenzophenone | 95％ |
| 4,4' -dimethyl benzophenone | 94％ |
| 4,4' -Difluorobenzophenone | 93％ |
| Benzophenones as fungicides | 93％ |
| 4-methoxybenzophenone | 93％ |
| 4,4' -diethyl benzophenone | 95％ |
| 4,4' -diethoxybenzophenone | 93％ |
| 4-firstBenzophenones as herbicides | 97％ |
| 4-ethyl benzophenone | 93％ |
| 4-fluorobenzophenones | 97％ |
[ example 3 ]
The chalcone compounds in table 3 were prepared into n-octane solution with a concentration of 50mg/L, and saline solution with a degree of mineralization of 1000mg/L, 10000mg/L and 50000mg/L, respectively, was added at a volume ratio of 1. Aging is carried out at 100 ℃ in a 25mL pressure vessel for 30 days, then a sample is taken for analysis and detection, and the concentration and retention rate are calculated, and the experimental results are shown in Table 3
TABLE 3 salt tolerance test of chalcones
[ example 4 ]
The diphenyl ketone compound in the table 4 is prepared into n-octane solution with the concentration of 50mg/L, adding saline solution with the mineralization degrees of 5000mg/L, 50000mg/L and 200000mg/L respectively, wherein the volume ratio is 1. Aging at 100 deg.C in 25mL pressure container for 10 days, sampling, analyzing, and calculating concentration and retention rate, and the experimental results are shown in Table 4
TABLE 4 salt tolerance test for diphenylketones
[ example 5 ] A method for producing a polycarbonate
10mg/L of ten chalcone compound mixed solutions in the table 5 are prepared, and static adsorption experiments are carried out, and the results are shown in the table 5.
TABLE 5 anti-adsorption Capacity of chalcones
[ example 6 ] A method for producing a polycarbonate
50mg/L of a mixed solution of twelve benzophenone compound segmentation aids in Table 6 is prepared, and a static adsorption experiment is carried out, and the results are shown in Table 6.
TABLE 6 Diphenyl ketones Compound anti adsorption Capacity
[ example 7 ]
Ten different segmentation aids in table 7 were formulated into a mixed solution using n-octane, and the individual sample concentration was 10mg/L (segmentation aid/n-octane), and the mixed solution was examined using liquid chromatography. And judging whether the segmentation aids of the type interfere with each other or not to influence the detection result. The results are shown in Table 7.
TABLE 7 anti-interference experimental results of chalcone compounds
| Segmented aid | Configured concentration (mg/L) | Detection concentration (mg/L) |
| 4,4' -Dimethoxychalcone | 10.1 | 10.3 |
| 4,4' -dimethyl chalcones | 10.0 | 10.5 |
| 4,4' -difluorochalcones | 10.2 | 10.6 |
| Chalcones | 9.9 | 10.1 |
| 4-methoxy chalcones | 10.4 | 10.1 |
| 4,4' -diethyl chalcones | 9.9 | 10.0 |
| 2, 4-dimethyl chalcones | 10.7 | 10.8 |
| 4-methyl chalcones | 10.9 | 11.2 |
| 4' -methyl chalcones | 10.2 | 10.1 |
| 4-methoxy-4' methyl chalcones | 10.3 | 10.7 |
[ example 8 ]
Twelve different segmentation aids in table 8 were formulated into a mixed solution with a single sample concentration of 50mg/L using n-octane, and the mixed solution was tested using liquid chromatography. And judging whether the segmentation aids of the type interfere with each other or not to influence the detection result. The results are shown in Table 8.
TABLE 8 anti-interference test results of diphenyl ketone compounds
| Segmented aid | Configured concentration (mg/L) | Detection concentration (mg/L) |
| 4,4' -Dimethoxybenzophenone | 51.1 | 51.2 |
| 4,4' -dimethyl benzophenone | 51.2 | 51.3 |
| 4,4' -DifluorodiphenylmethaneKetones | 50.0 | 50.6 |
| Benzophenones as herbicides | 49.9 | 50.2 |
| 4-methoxybenzophenone | 50.4 | 50.3 |
| 4,4' -diethyl benzophenone | 49.9 | 50.6 |
| 4,4' -diethoxybenzophenone | 50.7 | 50.2 |
| 4-methylbenzophenone | 51.9 | 51.2 |
| 4-ethyl benzophenone | 50.2 | 50.1 |
| 4-fluorobenzophenones | 53.3 | 52.7 |
| 4-ethoxy benzophenone | 52.1 | 52.3 |
| 4-carboxybenzophenone | 51.7 | 52.0 |
[ example 9 ] A method for producing a polycarbonate
Preparing a fracturing fluid solution with the concentration of about 50mg/L from the chalcone compound and n-octane, performing a compatibility experiment on the prepared oil-based fracturing fluid, and observing whether the solution precipitates or not at 100 ℃. After 24 hours of high temperature aging, the experimental results are shown in Table 9.
TABLE 9 chalcone compatibility tests
[ example 10 ] A method for producing a polycarbonate
The diphenyl ketone compound is prepared into a fracturing fluid solution with the concentration of about 50mg/L, and whether the solution precipitates or not is observed at 100 ℃. After 24 hours of high temperature aging, the experimental results are shown in Table 10.
TABLE 10 Diphenyl ketones compatibility test
| Segmented aid | Clarity of sample |
| 4,4' -Dimethoxybenzophenone | Clarification |
| 4,4' -dimethyl benzophenone | Clarification |
| 4,4' -difluorobenzophenone | Clarification |
| Benzophenones as herbicides | Clarification |
| 4-methoxybenzophenone | Clarification |
| 4,4' -diethyl benzophenone | Clarification |
| 4,4' -diethoxybenzophenone | Clarification |
| 4-methylbenzophenone | Clarification |
| 4-ethyl benzophenone | Clarification |
| 4-fluorobenzophenones | Clarification |
| 4-ethoxy benzophenone | Clarification |
| 4-carboxybenzophenone | Clarification |
[ example 11 ] A method for producing a polycarbonate
Simulating the use condition of the field fracturing fluid, and carrying out an indoor experiment:
preparing an oil-based fracturing fluid, wherein the oil-based fracturing fluid comprises the following components: kerosene +1.0% thickener (polyacrylate type compound, but molecular weight is not clear, viscosity 80 mPas) +0.5% crosslinker (sodium metaaluminate) +1.0% breaker (sodium acetate).
The prepared oil-based fracturing fluid is mixed with different staging aids (see table 11 specifically) to prepare a 100mg/L (staging aid/fracturing fluid) solution, the temperature of the in-situ fracturing is simulated to be 90 ℃, the pH is =9, and then the concentration detection is carried out. The results are shown in Table 11.
TABLE 11 detection results of the segmentation aid in fracturing fluids
[ example 12 ] A method for producing a polycarbonate
Combining the experimental results in example 11, considering the cost, it was decided to use 4-methyl chalcone, 4-methyl benzophenone, 4-methoxy chalcone, 4-fluoro benzophenone as the segmentation assistant (the initial concentrations of 4-methyl chalcone, 4-methyl benzophenone, 4-methoxy chalcone, 4-fluoro benzophenone in the oil-based fracturing fluid are about 50mg/L, respectively) for field application, add the four assistants to the oil-based base fluid of the four intervals in segments to obtain four fracturing fluids, sample for 30 days, sample different intervals of the oil reservoir stratum (collect crude oil), standardize the collected crude oil obtained by sampling, dissolve 1g of the sample with 10mL of n-octane, filter, then detect the collected crude oil by liquid chromatography mass spectrometry, separate and detect the liquid chromatography detection with a positive phase column, gradient elution with methanol/ethyl acetate, compare the chromatography column with a standard curve by mass spectrometry, compare the chromatography column peak area with the standard curve, calculate the concentration of the segmentation assistant in different intervals, compare the concentration with the molecular weight of the segmentation assistant in the standard column, and finally detect the peak area of the 4-methyl benzophenone, and finally obtain the 4-fluoro benzophenone compound in the oil-4-methyl chalcone and 4-fluoro benzophenone compoundThe oil production condition of each layer of cracks in the multi-section fracturing is obtained through concentration comparison, and a calculation formula n of the oil production ratio of each layer of section is obtained i ＝c i /c Total amount of X100%. The results are shown in Table 12.
TABLE 12 Performance analysis of the in situ experiment
[ example 13 ]
The procedure of example 12 was followed except that 4-methyl chalcone was used for each of the four intervals. As a result, the oil production in each interval and the oil production ratio in each interval cannot be distinguished.
[ example 14 ] A method for producing a polycarbonate
The procedure of example 12 was followed except that 4-methylbenzophenone was used for all four intervals. As a result, the oil production in each interval and the oil production ratio in each interval cannot be distinguished.
[ example 15 ]
The procedure of example 12 was followed except that 4-methoxychalcone was used for each of the four intervals. As a result, the oil production in each interval and the oil production ratio in each interval cannot be distinguished.
[ example 16 ]
The procedure of example 12 was followed except that 4-fluorobenzophenone was used for each of the four intervals. As a result, the oil production in each interval and the oil production ratio in each interval cannot be distinguished.
As can be seen from the thermal stability experiments of examples 1 and 2 and the data in tables 1 and 2, the segmentation aid used in the present invention has better thermal stability.
It can be seen from the salt tolerance tests of examples 3 and 4 and the data in tables 3 and 4 that the segmentation aid used in the present invention has better salt tolerance.
As can be seen from the anti-adsorption capacity experiments of examples 5 and 6 and the data in tables 5 and 6, in the quartz sand or kaolin, the adsorption amounts of the sectional aids adopted by the invention are less than 0.1mg/g, the adsorption amounts are lower, and the larger loss of the stratum is avoided.
As can be seen from the anti-interference tests of examples 7 and 8 and the data in tables 7 and 8, the detection result of the segmentation aid adopted by the invention in the mixed solution is close to the configured concentration, and the mutual interference of the segmentation aids is small.
As can be seen from the compatibility tests of examples 9 and 10 and the data in tables 9 and 10, the segmentation aid used in the present invention has high solubility and does not precipitate. The segmentation assistant has better compatibility with fracturing and can be added into fracturing fluid for use.
As can be seen from the data of example 11 and Table 11, the segmentation aid selected by the invention has better stability under the fracturing condition, and can be used in field fracturing.
It can be seen from the data of example 12 and table 12 that the oil-based fracturing fluid and the method for online monitoring productivity of reservoir intervals can be used for monitoring oil production of each interval in multi-stage fracturing.
Claims (10)
1. The oil-based fracturing fluid comprises an oil-based base fluid and a segmentation assistant, wherein the segmentation assistant is a chalcone compound and/or a diphenyl ketone compound.
2. The oil-based fracturing fluid of claim 1, wherein the chalcone compound has a structural formula represented by formula (1):
wherein R is saturated or unsaturated C 1 -C 29 An aliphatic carbonyl group; r 1 、R 2 、R 3 、R 4 Each independently selected from H, C 1 ～C 6 Alkyl of (C) 1 ～C 6 Alkoxy group of,One of nitroso, carboxyl and halogen;
preferably, R is carbonyl or allylcarbonyl; r is 1 、R 2 、R 3 、R 4 Each independently selected from C 1 ～C 6 Alkyl and C 1 ～C 6 One of alkoxy groups of (a);
more preferably, the chalcone compound is selected from one or more of 4,4 '-dimethoxychalcone, 4' -dimethylchalcone, 4 '-difluorochalcone, chalcone, 4-methoxychalcone, 4' -diethylchalcone, 2, 4-dimethylchalcone, 4-methylchalcone, 4 '-methylchalcone and 4-methoxy-4' methylchalcone.
3. The oil-based fracturing fluid of claim 1, the diphenyl ketone compound has a structural formula shown in a formula (2):
wherein R is 1 、R 2 Each independently selected from H and C 1 ～C 12 Alkyl of (C) 1 ～C 12 One of alkoxy, nitro, nitroso, carboxyl and halogen;
preferably, R 1 、R 2 Each independently selected from C 1 ～C 6 Alkyl and C 1 ～C 6 One of alkoxy groups of (a);
more preferably, the benzophenone-based compound is selected from one or more of 4,4' -dimethoxybenzophenone, 4' -dimethylbenzophenone, 4' -difluorobenzophenone, benzophenone, 4-methoxybenzophenone, 4' -diethylbenzophenone, 4' -diethoxybenzophenone, 4-methylbenzophenone, 4-diethylbenzophenone, 4-fluorobenzophenone, 4-ethoxybenzophenone and 4-carboxybenzophenone.
4. The oil-based fracturing fluid of claim 1, wherein the content of the segmentation aid in the oil-based fracturing fluid is from 0.0001% to 0.01% by weight; and/or the presence of a gas in the gas,
the oil-based base fluid is selected from crude oil and/or finished oil.
5. The oil-based fracturing fluid of any one of claims 1 to 4, further comprising an adjuvant, preferably selected from one or more of proppants, viscosifiers, and cross-linking agents;
preferably, the proppant is selected from one or more of ceramsite, quartz sand, metal aluminum ball, walnut shell, glass bead, plastic ball, steel ball, ceramsite and resin coated sand;
preferably, the thickening agent is selected from one or more of vegetable gum or derivatives thereof, cellulose derivatives, biopolysaccharides, polyacrylates and synthetic polymers, more preferably, the thickening agent is selected from one or more of guar gum, hydroxypropyl guar gum, fenugreek gum, polyacrylamide and methylene polyacrylamide;
preferably, the crosslinking agent is a covalent crosslinking agent, more preferably, the crosslinking agent is selected from one or more of polyethylene glycol, diglycidyl ether, maleic anhydride, formaldehyde, glyoxal, glutaraldehyde, toluene diisocyanate, methylene diphenyl diisocyanate, sodium metaaluminate, and 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide.
6. A multi-stage fracturing method comprising applying the oil-based fracturing fluid of any one of claims 1-5 to different intervals of a reservoir formation.
7. A method for on-line monitoring of productivity of a reservoir interval, comprising applying the oil-based fracturing fluid of any one of claims 1 to 5 to different intervals of a reservoir formation, and applying a different staging aid to the oil-based fracturing fluid at different intervals of the reservoir formation.
8. The method of claim 7, comprising the steps of:
1) Selecting oil-based fracturing fluid, wherein the applied oil-based fracturing fluid has different segmentation aids in different intervals of the reservoir stratum;
2) Sampling different intervals of the reservoir formation;
3) Carrying out standardization treatment on the sampled sample;
4) And detecting and calculating the concentration of the sectional aids of different intervals to obtain the productivity of different intervals.
9. The method according to claim 7 or 8, wherein the sampling period of step 2) is 15 to 180 days;
preferably, the normalization processing method of step 3) includes: the sample was dissolved using n-octane and filtered.
10. The method according to any one of claims 7 to 9, wherein the detecting of step 4) comprises using liquid chromatography-mass spectrometry; preferably, the liquid chromatography uses a normal phase column for the separation detection.
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