CN117986137A - Triarylamine fracturing tracer, tracing method, fracturing fluid and application - Google Patents

Triarylamine fracturing tracer, tracing method, fracturing fluid and application Download PDF

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Publication number
CN117986137A
CN117986137A CN202211325769.1A CN202211325769A CN117986137A CN 117986137 A CN117986137 A CN 117986137A CN 202211325769 A CN202211325769 A CN 202211325769A CN 117986137 A CN117986137 A CN 117986137A
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China
Prior art keywords
tracer
fracturing
triarylamine
fracturing fluid
methoxy
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CN202211325769.1A
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Chinese (zh)
Inventor
张立
李应成
沙鸥
张卫东
张慧
鲍新宁
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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Priority to CN202211325769.1A priority Critical patent/CN117986137A/en
Publication of CN117986137A publication Critical patent/CN117986137A/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C211/00—Compounds containing amino groups bound to a carbon skeleton
    • C07C211/43—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton
    • C07C211/54—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton having amino groups bound to two or three six-membered aromatic rings
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C211/00—Compounds containing amino groups bound to a carbon skeleton
    • C07C211/43—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton
    • C07C211/54—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton having amino groups bound to two or three six-membered aromatic rings
    • C07C211/56—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton having amino groups bound to two or three six-membered aromatic rings the carbon skeleton being further substituted by halogen atoms or by nitro or nitroso groups
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C217/00—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton
    • C07C217/78—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having amino groups and etherified hydroxy groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton
    • C07C217/80—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having amino groups and etherified hydroxy groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton having amino groups and etherified hydroxy groups bound to carbon atoms of non-condensed six-membered aromatic rings
    • C07C217/82—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having amino groups and etherified hydroxy groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton having amino groups and etherified hydroxy groups bound to carbon atoms of non-condensed six-membered aromatic rings of the same non-condensed six-membered aromatic ring
    • C07C217/92—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having amino groups and etherified hydroxy groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton having amino groups and etherified hydroxy groups bound to carbon atoms of non-condensed six-membered aromatic rings of the same non-condensed six-membered aromatic ring the nitrogen atom of at least one of the amino groups being further bound to a carbon atom of a six-membered aromatic ring
    • 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
    • C09K8/66—Compositions based on water or polar solvents
    • C09K8/68—Compositions based on water or polar solvents containing organic compounds
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Geology (AREA)
  • Mining & Mineral Resources (AREA)
  • Physics & Mathematics (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Fluid Mechanics (AREA)
  • Geophysics (AREA)
  • Materials Engineering (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

The invention discloses a triarylamine fracturing tracer, a tracer method, fracturing fluid and application. The triarylamine fracturing tracer has the structural formula: Wherein R 1～R15 is the same or different and is one of H, methyl, methoxy, ethyl, ethoxy and fluorine respectively and independently. The triarylamine fracturing tracer provided by the invention has higher stability under the mineralization degree condition of 0-50000mg/L at room temperature-80 ℃, is suitable for stratum with severe conditions, has small dosage, is environment-friendly, sensitive in detection and low in detection limit, and can be used for multi-stage fracturing tracer technology of oil fields.

Description

Triarylamine fracturing tracer, tracing method, fracturing fluid and application
Technical Field
The invention relates to the technical field of oilfield drilling, in particular to a triarylamine fracturing tracer, a tracer method, fracturing fluid and application.
Background
With the improvement and promotion of multi-stage fracturing technology, the multi-stage fracturing technology has become one of the dominant technologies for improving the development degree of low-permeability reservoirs. Through multistage fracturing technology, can realize the reservoir transformation, promote the seepage flow area, reach the purpose that improves output. The multi-section fracturing tracing technology is an auxiliary technology matched with multi-section fracturing, and mainly aims to judge the seam making condition, the liquid production amount and the oil production condition of each layer section, the capacity contribution rate and the like. The common tracers for oil fields include chemical tracers, radioactive isotope tracers, non-radioactive isotope tracers and trace substance tracers. The traditional chemical tracer has rich types, and has new application potential if the defects of high dosage, large adsorption, easy degradation and high detection limit can be overcome.
Therefore, the chemical tracer with small dosage, small adsorption, difficult degradation and low detection limit is provided, and the technical problem to be solved at present.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a triarylamine fracturing tracer, a tracer method, fracturing fluid and application. The triarylamine fracturing tracer with lower detection limit is suitable for multi-stage fracturing tracing technology, has higher stability under the mineralization degree condition of 0-50000mg/L at room temperature-80 ℃, and is suitable for stratum with harsh conditions. The method has the advantages of less tracer consumption, environment friendliness, sensitive detection, low detection limit, strong temperature resistance and strong adsorption resistance, and each tracer does not interfere with each other, so that the method can be used for the multi-stage fracturing tracing technology of the oil field. The triarylamine fracturing tracer disclosed by the invention exploits a brand-new chemical tracer species, contains aromatic rings, has ultraviolet absorption and other properties, and can be determined by more monitoring methods.
The invention aims to provide a triarylamine fracturing tracer, which has the structural formula:
wherein R 1～R15 is the same or different and is one of H, methyl, methoxy, ethyl, ethoxy and fluorine respectively and independently.
In a preferred embodiment of the present invention,
In the structural formula, R 1～R15 is the same or different and is one of H, methyl, methoxy and fluorine respectively and independently.
In a preferred embodiment of the present invention,
The triarylamine fracturing tracer is at least one of triphenylamine, 4-methyltrianiline, 4-methoxytriphenylamine and 4-fluoro-N, N-diphenylaniline.
The second object of the invention is to provide a multi-stage fracturing tracing method of the triarylamine fracturing tracer adopting one of the objects of the invention, which comprises the steps of adding the triarylamine fracturing tracer from an injection well, sampling in a monitoring well, and drawing a tracer yield curve.
In a preferred embodiment of the present invention,
The triarylamine fracturing tracer is added from an injection well in a single dose or formulated as a tracer solution.
In a preferred embodiment of the present invention,
The concentration of the tracer solution is in the range of 0.1 to 500mg/L, preferably 1 to 500mg/L, more preferably 1 to 50mg/L.
In a preferred embodiment of the present invention,
The method comprises the following steps:
(1) Selecting a tracer conforming to fracturing conditions;
(2) Calculating and determining the tracer dosage according to the minimum detection limit of the instrument, the dosage of the fracturing fluid and the physical properties of the stratum according to the number of the segments to be fractured;
(3) The tracer is injected along with the fracturing fluid in the fracturing process;
(4) Sampling in a monitoring well, wherein the sampling period is 15 days to 60 days;
(5) And carrying out standardized treatment, detection analysis and tracer yield curve drawing on the sample.
In a preferred embodiment of the present invention,
In the step 4), a peristaltic pump can be used in the injection process, and the tracer and the fracturing fluid are injected together.
The invention adopts the following technical scheme:
1) Analyzing the oilfield fracturing fluid and the produced water, and selecting a tracer for the stratum, wherein the tracer for the stratum is selected from compounds which are not contained in the stratum;
2) Design embodiments;
3) Calculating the dosage of the tracer to be added: calculating and determining the tracer dosage according to the minimum detection limit of the instrument, the dosage of the fracturing fluid and the physical properties of the stratum according to the number of the segments to be fractured;
4) Injecting the tracer along with the fracturing fluid in the fracturing process by using a pump truck or other equipment;
5) Sampling in a monitoring well according to a formulated sampling system, wherein the sampling period is 15 days to 60 days;
6) Carrying out standardized treatment on the sample;
7) Detecting and analyzing the produced liquid by utilizing a corresponding analysis means; the analytical means are conventional in the art;
8) Drawing a tracer yield curve;
9) Performing simulation calculation by using conventional tracer digital-analog software;
10 Complete the comprehensive analysis test report.
The invention further provides a fracturing fluid, which comprises the triarylamine fracturing tracer which is one of the purposes.
In a preferred embodiment of the present invention,
The amount of the triarylamine fracturing tracer is 0.0005-0.05 wt% of the fracturing fluid, preferably 0.005-0.01 wt%.
The fourth object of the invention is to provide an application of the fracturing fluid of the third object of the invention in multistage fracturing.
The fifth purpose of the invention is to provide an application of a triarylamine compound as a fracturing tracer, wherein the triarylamine compound has the structural formula:
wherein R 1～R15 is the same or different and is one of H, methyl, methoxy, ethyl, ethoxy and fluorine respectively and independently.
In a preferred embodiment of the present invention,
In the structural formula, R 1～R15 is the same or different and is one of H, methyl, methoxy and fluorine respectively and independently.
In a preferred embodiment of the present invention,
The triarylamine compound is at least one of triphenylamine, 4-methyltrianiline, 4-methoxytriphenylamine and 4-fluoro-N, N-diphenylaniline.
In a preferred embodiment of the present invention,
The application comprises the steps of adding the triarylamine compound as a tracer from an injection well, sampling in a monitoring well, and drawing a tracer yield curve; preferably, the method comprises the steps of,
The triarylamine compound is added from an injection well singly or in the form of a solution; and/or the number of the groups of groups,
The concentration of the solution is in the range of 0.1 to 500mg/L, preferably 1 to 500mg/L, more preferably 1 to 50mg/L.
The invention has the beneficial effects that:
in the triarylamine compound, because amino groups are substituted, the triarylamine compound becomes an inert group, otherwise, the stability is poor, the triarylamine compound is difficult to be applied to tracing technology, for example, pure aniline is easy to oxidize and deteriorate in air and is harmful to the environment; simultaneously, as amino groups are substituted, the water solubility of the compounds is reduced, and the error of monitoring results caused by water dissolution is prevented.
The triarylamine fracturing tracer disclosed by the invention is sensitive in detection, low in detection limit, strong in temperature resistance and strong in adsorption resistance, and each tracer does not interfere with each other, so that the triarylamine fracturing tracer can be used for an oilfield multistage fracturing tracer technology. The required dosage is small, the detection limit can reach 0.1mg/L, the use amount of the oilfield tracer is greatly reduced, and the pollution of the oil reservoir stratum caused by the excessive use amount of the oilfield tracer can be avoided. The triarylamine fracturing tracer disclosed by the invention exploits a brand-new chemical tracer species, contains aromatic rings, has ultraviolet absorption and other properties, and can be determined by more monitoring methods.
Drawings
FIG. 1 is a graph of analysis criteria obtained by selecting triphenylamine for the detection limit experiment in example 6;
Wherein the horizontal scale is the concentration (mg/L) of a single tracer; the ordinate is the liquid chromatography peak area (au×min).
Detailed Description
The present invention will be described in detail with reference to the following specific embodiments and the accompanying drawings, and it is necessary to point out that the following embodiments are merely for further explanation of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adaptations of the invention based on the present disclosure will remain within the scope of the invention.
The raw materials used in the examples are all commercially available, wherein some of the raw materials are derived from the following sources:
Triphenylamine: brand TCI, CAS:603-34-9;
4-methyltrianiline: brand TCI, M1898 CAS:4316-53-4;
4-methoxytriphenylamine: brand: an Naiji chemical CAS 4316-51-2;
4-fluoro-N, N-diphenylaniline: brand milin CAS:437-25-2.
Example 1
The test samples were prepared as n-octane solutions at a concentration of about 100mg/L, aged at 80℃in 50mL pressure bomb, sampled for concentration test at 30 days of aging, and the retention was calculated, and the test results are shown in Table 1:
TABLE 1
Example 2
The experimental samples were prepared as n-octane solutions at a concentration of about 100mg/L, and brine solutions of varying degrees of mineralization were added at a volume ratio of 1:1. Aging is carried out at 80 ℃, the container is 50mL of pressure bomb, aging is carried out for 30 days, sampling is carried out, concentration test is carried out, retention rate is calculated, experimental results are shown in table 2, and the graph shows that the tracer has higher salt tolerance and consistent stability under different salinity.
TABLE 2
Example 3
A100 mg/L mixed solution of four tracers was prepared for static adsorption experiments, and the results are shown in Table 3. In quartz sand, kaolin or montmorillonite, the adsorption capacity of the tracer is smaller than 0.1mg/g, the adsorption capacity is lower, and the large loss of the tracer in the stratum caused by the adsorption problem is avoided.
TABLE 3 Table 3
Example 4
The tracer was formulated as a mixed solution using n-octane at a single sample concentration of 100mg/L, and the mixed solution was detected using liquid chromatography. Judging whether the tracer agents of the type interfere with each other or not, and influencing the detection result. The experimental results are shown in Table 4. The experimental results show that the detection result of the tracer in the mixed solution is close to the configuration concentration, and the mutual interference of the tracer is less.
TABLE 4 Table 4
Example 5
The experimental sample is prepared into n-octane solution with the concentration of about 100mg/L, the displacement experiment is carried out at the temperature of 80 ℃, the artificial rock core with the permeability of 2.5D is used, the solution with the fixed volume is injected into the rock core, the produced liquid is extracted for concentration analysis and detection, and the retention rate of the tracer is calculated in the displacement experiment. The displacement experiment result shows that the tracer has low adsorption amount in the rock core and has the potential of the tracer.
TABLE 5
Example 6
Triphenylamine is selected for detection limit experiments, 8 kinds of tracer solutions with different concentrations are prepared, wherein the concentration of the tracer solutions is 0.1,0.5,1.0,2.5,5, 10, 25 and 50mg/L, detection is carried out by using HPLC-MS, an analysis standard curve of the compound is prepared, and specific test results are shown in figure 1. As can be seen from FIG. 1, the tracer has a good linear relationship in the concentration range of 0.1-50mg/L, can be quantitatively analyzed and monitored, and has a detection limit lower than 0.1mg/L, so that the detection limit of the method is at least 0.1mg/L.
It can be seen from examples 1 to 6 that: the triarylamine fracturing tracer provided by the invention is sensitive in detection, low in detection limit, high in temperature resistance, high in stability and high in adsorption resistance under the mineralization condition of 0-50000 mg/L at room temperature-80 ℃, the detection limit can reach 0.1mg/L, each tracer does not interfere with each other, and the triarylamine fracturing tracer is suitable for stratum with severe conditions and can be well applied to oilfield multistage fracturing tracing technology.
It should be noted that the above-described embodiments are only for explaining the present invention and do not constitute any limitation of the present invention. The invention has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined in the appended claims, and the invention may be modified without departing from the scope and spirit of the invention. Although the invention is described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, as the invention extends to all other means and applications which perform the same function.
All publications, patent applications, patents, and other references mentioned in this specification are incorporated herein by reference in their entirety. Unless defined otherwise, all technical and scientific terms used herein have the meaning commonly understood by one of ordinary skill in the art. In case of conflict, the present specification, definitions, will control.
When the specification derives materials, substances, methods, steps, devices, or elements and the like in the word "known to those skilled in the art", "prior art", or the like, such derived objects encompass those conventionally used in the art as the application suggests, but also include those which are not currently commonly used but which would become known in the art to be suitable for similar purposes.
The endpoints of the ranges and any values disclosed in this document are not limited to the precise range or value, and the range or value should be understood to include values approaching the range or value. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein. In the following, the individual technical solutions can in principle be combined with one another to give new technical solutions, which should also be regarded as specifically disclosed herein.
In the context of this specification, any matters or matters not mentioned are directly applicable to those known in the art without modification except as explicitly stated.
Moreover, any embodiment described herein can be freely combined with one or more other embodiments described herein, and the technical solutions or ideas thus formed are all deemed to be part of the original disclosure or original description of the present invention, and should not be deemed to be a new matter which has not been disclosed or contemplated herein, unless such combination is clearly unreasonable by those skilled in the art.

Claims (14)

1. A triarylamine fracturing tracer has a structural formula:
wherein R 1～R15 is the same or different and is one of H, methyl, methoxy, ethyl, ethoxy and fluorine respectively and independently.
2. The triarylamine fracturing tracer of claim 1 wherein:
In the structural formula, R 1～R15 is the same or different and is one of H, methyl, methoxy and fluorine respectively and independently.
3. The triarylamine fracturing tracer of claim 1 wherein:
the triarylamine fracturing tracer is at least one of triphenylamine, 4-methyltrianiline, 4-methoxytriphenylamine and 4-fluoro-N, N-diphenylaniline.
4. A multi-stage frac tracer method employing a triarylamine frac tracer as claimed in any one of claims 1 to 3, comprising the steps of adding the triarylamine frac tracer from an injection well, then sampling the monitoring well, and drawing a tracer yield curve.
5. The method of claim 4, wherein:
the triarylamine fracturing tracer is added from an injection well in a single dose or formulated as a tracer solution.
6. The method of claim 5, wherein:
the concentration of the tracer solution is in the range of 0.1 to 500mg/L, preferably 1 to 500mg/L, more preferably 1 to 50mg/L.
7. A method according to any one of claims 4 to 6, characterized in that the method comprises:
(1) Selecting a tracer conforming to fracturing conditions;
(2) Calculating and determining the tracer dosage according to the minimum detection limit of the instrument, the dosage of the fracturing fluid and the physical properties of the stratum according to the number of the segments to be fractured;
(3) The tracer is injected along with the fracturing fluid in the fracturing process;
(4) Sampling in a monitoring well, wherein the sampling period is 15 days to 60 days;
(5) And carrying out standardized treatment, detection analysis and tracer yield curve drawing on the sample.
8. A fracturing fluid comprising the triarylamine fracturing tracer of any one of claims 1-3.
9. The fracturing fluid of claim 8, wherein:
the amount of the triarylamine fracturing tracer is 0.0005-0.05 wt% of the fracturing fluid, preferably 0.005-0.01 wt%.
10. Use of a fracturing fluid according to any of claims 8 to 9 in multistage fracturing.
11. An application of a triarylamine compound as a fracturing tracer, wherein the triarylamine compound has a structural formula as follows:
wherein R 1～R15 is the same or different and is one of H, methyl, methoxy, ethyl, ethoxy and fluorine respectively and independently.
12. The use according to claim 11, wherein:
In the structural formula, R 1～R15 is the same or different and is one of H, methyl, methoxy and fluorine respectively and independently.
13. The use according to claim 11, wherein:
The triarylamine compound is at least one of triphenylamine, 4-methyltrianiline, 4-methoxytriphenylamine and 4-fluoro-N, N-diphenylaniline.
14. Use according to any one of claims 11 to 13, comprising the step of adding the triarylamine compound as a tracer from an injection well, subsequently sampling the monitoring well, and plotting the tracer yield curve; preferably, the method comprises the steps of,
The triarylamine compound is added from an injection well singly or in the form of a solution; and/or the number of the groups of groups,
The concentration of the solution is in the range of 0.1 to 500mg/L, preferably 1 to 500mg/L, more preferably 1 to 50mg/L.
CN202211325769.1A 2022-10-27 2022-10-27 Triarylamine fracturing tracer, tracing method, fracturing fluid and application Pending CN117986137A (en)

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