CN112111261B - CO (carbon monoxide) 2 Shale oil-based channeling sealing agent for flooding and preparation method thereof - Google Patents
CO (carbon monoxide) 2 Shale oil-based channeling sealing agent for flooding and preparation method thereof Download PDFInfo
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- CN112111261B CN112111261B CN202010939143.4A CN202010939143A CN112111261B CN 112111261 B CN112111261 B CN 112111261B CN 202010939143 A CN202010939143 A CN 202010939143A CN 112111261 B CN112111261 B CN 112111261B
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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
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/594—Compositions used in combination with injected gas, e.g. CO2 orcarbonated gas
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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
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
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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
- C09K8/602—Compositions for stimulating production by acting on the underground formation containing surfactants
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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
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
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Abstract
The invention relates to CO 2 A shale oil-based channeling sealing agent for flooding and a preparation method thereof. The CO is 2 The preparation method of the shale oil-based channeling sealing agent for flooding comprises the following steps: uniformly mixing the oil shale fines with n-octanoic acid, and standing to obtain a shale oil extracting solution; sulfonating the shale oil extract to obtain CO 2 The shale oil-based channeling sealing agent is used for displacement. The channeling sealing agent obtained by the invention can obviously reduce the surface tension of water without adding a surfactant, a polymer and other additives, has certain temperature and salt resistance, can effectively improve the recovery ratio of crude oil, has stable foam and CO 2 The gas composite displacement effect is good; the method has simple preparation process and low cost, and is favorable for realizing large-scale production.
Description
Technical Field
The invention relates to the technical field of oilfield exploitation, in particular to CO 2 A shale oil-based channeling sealing agent for flooding and a preparation method thereof.
Background
Carbon dioxide flooding, as an effective method for improving recovery efficiency, has been applied to oilfield development practices in the early 60 and 70 s of the 20 th century abroad, and CO injection is particularly performed in the United states 2 The gas drive technology is widely applied, and the gas drive technology is mostly in an indoor research stage in China. In recent years, due to the continuous development of low-permeability reservoirs, neither water flooding nor chemical flooding can meet the exploitation requirements, and injection fluid damage is easily caused. If the low permeability oil holds sufficient CO 2 Gas source, then the use of CO can be considered 2 And (5) driving. However, for heterogeneous reservoirs, CO 2 The flooding is influenced by factors such as the slip effect and viscous finger advance of gas, gas channeling easily occurs, and problems such as large pore channel channeling, high permeable layer bursting and the like generally existTo give a title. CO injection 2 Early breakthrough will result in most reservoirs of the reservoir not being swept, allowing for CO injection 2 The development is difficult to achieve the expected development effect. Thus in CO 2 Before flooding, effective channeling sealing must be performed.
In addition, due to the action of surface molecular force and capillary force inside the oil reservoir, the liquid in the oil reservoir can be driven only when a large displacement pressure is input. The method of reducing the oil-water interfacial tension by adding a surfactant is one of the important ways of forcing the remaining oil retained in the porous medium to flow, thereby enhancing the recovery efficiency.
Therefore, it is important to provide a channeling agent capable of reducing the surface tension of an oil-water interface.
Disclosure of Invention
In view of the above, there is a need to provide a CO 2 A shale oil-based channeling sealing agent for flooding and a preparation method thereof are used for solving the technical problem of low crude oil recovery rate in the prior art.
In a first aspect of the invention there is provided a CO 2 The preparation method of the shale oil-based channeling sealing agent for flooding comprises the following steps:
evenly mixing the oil shale fines with n-caprylic acid, and standing to obtain a shale oil extracting solution;
performing sulfonation reaction on the shale oil extracting solution to obtain CO 2 The shale oil-based channeling sealing agent is used for displacement.
Furthermore, the dosage ratio of the oil shale fines to the n-caprylic acid is 1g (4-6) ml.
Furthermore, the standing time is 12-24 h.
Further, the temperature of the sulfonation reaction is 70-90 ℃, and the time of the sulfonation reaction is 60-120 min.
Further, the sulfonation reaction is carried out in the presence of sulfur trioxide.
Further, the above sulfur trioxide is passed through P 2 O 5 Is obtained by reacting with concentrated sulfuric acid, the reaction temperature is 90-100 ℃, and P is 2 O 5 The dosage ratio of the concentrated sulfuric acid to the concentrated sulfuric acid is 1g: (0.5-1) ml.
Go further forwardIn one step, P is 2 O 5 The dosage ratio of the shale oil extract to the shale oil extract is 1g: (0.5-2) ml.
In a first aspect of the invention there is provided a CO 2 Shale oil-based channeling sealing agent for flooding, the CO 2 Shale oil-based channeling sealing agent for displacement CO provided by first aspect of the invention 2 The shale oil-based channeling sealing agent for the flooding is prepared by a preparation method.
Compared with the prior art, the invention has the beneficial effects that:
the channeling sealing agent can obviously reduce the surface tension of water without adding a surfactant, a polymer and other additives, has certain temperature resistance and salt resistance, can effectively improve the recovery ratio of crude oil, has stable foam, and is compatible with CO 2 The gas composite displacement effect is better;
the method has simple preparation process and low cost, and is beneficial to realizing large-scale production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In a first aspect of the invention there is provided a CO 2 The preparation method of the shale oil-based channeling sealing agent for flooding comprises the following steps:
(1) and (3) uniformly mixing the oil shale fines and n-caprylic acid, and standing to obtain a shale oil extracting solution. In the process, the dosage ratio of the oil shale fines to the n-caprylic acid is 1g (4-6) ml.
And the standing process is carried out at normal temperature, and the standing time is 12-24 h. According to the invention, the shale oil extracting solution is obtained by mixing and standing the oil shale fines and the n-octanoic acid, the shale oil extracting method is simple, heating is not required, and the production cost is favorably reduced. It should be noted that the addition of n-octanoic acid should not be too much or too little, which would result in a low content of shale oil in the shale oil extract and CO obtained after sulfonation 2 Content of sulfonated shale oil in shale oil-based channeling sealing agent for floodingToo low is detrimental to improving oil recovery, too little will result in detrimental extraction of shale oil from the oil shale fines.
(2) Sulfonating the shale oil extract to obtain CO 2 The shale oil base channeling sealing agent is used for displacement. In the process, the temperature of the sulfonation reaction is 70-90 ℃, and the time of the sulfonation reaction is 60-120 min. The invention does not limit the concrete type of the sulfonation reagent used in the sulfonation reaction, and the person skilled in the art can select the reagent according to the actual situation as long as the reagent can ensure the sulfonation reaction with the shale oil extract. In some embodiments of the invention, the sulfonation reaction is carried out in the presence of sulfur trioxide. Further, sulfur trioxide is passed through P 2 O 5 Reacting with concentrated sulfuric acid at 90-100 ℃, wherein P is 2 O 5 The dosage ratio of the concentrated sulfuric acid to the concentrated sulfuric acid is 1g: (0.5-1) ml. Further, P 2 O 5 The dosage ratio of the shale oil extract to the shale oil extract is 1: (0.5 to 2), preferably 1g: 0.5 ml.
In a second aspect of the invention, there is provided a CO 2 Shale oil-based channeling agent for flooding, the CO 2 Shale oil-based channeling sealing agent for displacement CO provided by first aspect of the invention 2 The shale oil-based channeling sealing agent for the displacement is prepared by a preparation method.
To avoid redundancy, the process of extracting shale oil extract and CO in the examples of the present invention will now be described 2 The test procedure for the flooding shale oil-based channeling agent is summarized as follows:
the shale oil extracting solution is obtained by the following steps: 10g of oil shale was ground and dried, and then added to a 250ml beaker, followed by addition of 50ml of n-octanoic acid, stirred with a glass rod for 10min, and then left to stand for 18 hours, to obtain a rock oil extract.
And (3) testing foaming performance: opening the constant temperature water bath box, and circulating hot water in the annular space of the jacket graduated cylinder for about 2min to ensure that the annular space temperature reaches the required experimental temperature; the prepared surfactant solution with the dosage of 100mL is transferred to a beaker and heated to a specified temperature in a constant-temperature water bath kettle; preheating CO 2 Adding the shale oil-based channeling sealing agent solution into an annular measuring cylinder, and opening the measuring cylinder after the temperature reading reaches the specified temperatureOpening a carbon dioxide cylinder switch, quickly opening an annular measuring cylinder switch, adjusting the gas flow to a specified reading, and starting timing; after the ventilation reaches the designated time, the foam volume is quickly recorded, the switch of the annular measuring cylinder is closed firstly, then the switch of the carbon dioxide cylinder is closed, and the foam half-life period is recorded.
And (3) testing the surface tension: 2% of CO is prepared 2 A shale oil base channeling sealing agent solution for flooding; and (4) detecting by adopting a JK99B full-automatic tensiometer, and measuring the surface tension of the distilled water at room temperature. Thereby inspecting and calibrating the instrument; the surface tension of the different solutions was then measured sequentially, with a small amount of the liquid being measured washing the instrument before each measurement.
When the variable is controlled, the conditions of 80 ℃, 400ml/min of air flow, 2min of ventilation and no mineralization are adopted by default.
Simulating tertiary oil recovery test of an oil field:
screening a certain amount of fine sand, cleaning and drying the fine sand, pouring the fine sand into a clean beaker, adding a small amount of resin and acetone solution, uniformly stirring the fine sand by using a glass rod, adding the fine sand into a mounted mould in batches, pressurizing the fine sand to 30kp by using a hydraulic jack, standing the fine sand for about one hour, disassembling the mould to obtain a required core, and putting the core into an oven at 80 ℃ for full drying;
placing a rock core in the middle into a rock core holding device, adding a rock core plug at two ends, screwing an experimental device, pressurizing an annular space of the rock core holding device by using a manual metering pump after screwing to enable annular pressure to reach about 7MP, if the annular pressure is unchanged after standing for a period of time or is unchanged after a little drop, installing a vacuum meter at one end of the rock core holding device after annular pressure, and installing a vacuum pump at the other end of the rock core holding device to pump internal pressure to be below 0.09 MPa;
driving water into the core, and recording the reading of the pressure gauge after the reading of the pressure gauge is stable; driving crude oil of the victory oil field into the core, closing the constant-flow pump when the reading of the pressure gauge is stable and no water flows out for 30min, and aging the oil in the core for 12 h;
after water flooding is carried out until the water content is close to 98 percent, the water flooding agent is replaced by a channeling sealing agent solution with the volume ratio of 2 percent to drive the oil to about 0.5PV, and CO is replaced by CO 2 Data during recording and processing.
After the experiment is finished, the instrument needs to be closed in time, the experiment device is reasonably cleaned, and the equipment is maintained.
Examples
20g P was added to the first three-necked flask 2 O 5 And 10-20 ml of H 2 SO 4 Adding 10ml of shale oil extracting solution prepared in advance into the second three-neck flask, and communicating the first three-neck flask with the second three-neck flask through a gas-guide tube; heating the temperature of the mixed solution in the first three-neck flask to 90 ℃, heating the temperature of the mixed solution in the second three-neck flask to 70-90 ℃, reacting for 60-120 min, and absorbing tail gas by adopting a sodium hydroxide solution in the reaction process. Screening for synthetic CO by orthogonal assays 2 The optimal process conditions of the shale oil-based channeling sealing agent for displacement, the implementation conditions of the examples 1 to 9 are shown in table 1, and the test results are shown in tables 2 to 10.
TABLE 1 sulfonation Process conditions
TABLE 280 ℃ Effect of the amount of channeling-blocking agent added on the foam volume (ml)
TABLE 380 ℃ Effect of the amount of the channeling sealing agent added on the half-life(s) of the foam
Table CO at 480 deg.C 2 Effect of gas flow on foaming volume (ml)
Table CO at 580 deg.C 2 Influence of gas flow on half-life(s)
TABLE 6 temperature effect on foaming volume (ml)
TABLE 7 Effect of temperature on half-life(s)
TABLE influence of degree of mineralization on foaming volume (ml) at 880 ℃
TABLE Effect of mineralization at 980 ℃ on half-life(s)
Surface tension of 2% channeling agent solution at 1025 deg.C
As can be seen from tables 2 and 3, the channeling sealing agent synthesized by the process conditions of groups 1 and 2 has larger foam volume and higher half-life, and although the foam volume and the half-life of the channeling sealing agent synthesized under different process conditions do not change in accordance with the change rule under different channeling sealing agent adding conditions, the foam volume and the half-life of the channeling sealing agent obtained by groups 1 and 2 increase with the increase of the channeling sealing agent adding amount.
As can be seen from tables 4 and 5, the channeling sealing agents synthesized by the processes of groups 1, 2 and 9 have larger foam volume and higher half-life period under different gas flow conditions.
As can be seen from tables 6 and 7, the channeling sealing agents synthesized by the processes of groups 1, 2 and 9 have larger foam volume and higher half-life under different temperature conditions, and the half-life period is reduced along with the increase of the temperature.
As can be seen from tables 8 and 9, the channeling sealing agents synthesized by the processes of groups 1 and 2 have larger foam volume and higher half-life under different mineralization conditions, and the foam volume is in a descending trend along with the increase of the mineralization.
As can be seen from table 10, the channeling agent synthesized by the processes of group 3 and group 4 has the best effect of reducing the surface tension, and then group 1, group 2, group 5, group 6, and group 9 have the worst effect of reducing the surface tension.
Combining the above results, the bottom flooding test was simulated using the channeling agent synthesized by the process of group 3, and the results are shown in table 11.
Table 11 displacement artificial rock core data recording table
It can be seen from Table 11 that the pressure was low at the initial stage and then gradually increased; at about 0.52PV injection, the water content began to rise substantially; when the water content reaches 98%, the extraction degree reaches about 49%, then the channeling sealing agent solution is used for driving, and the pressure rises rapidly; when the process pressure is stable, and aboutStopping the displacement after no crude oil is produced for 30min, and performing secondary displacement by using water, wherein less crude oil is produced in the process; when the pressure is stable and no crude oil is produced for 30min, the displacement is continued to be carried out by using the channeling sealing agent solution, after about 0.5PV sulfonate solution is injected, the surfactant expands swept volume of the displacement fluid, the displacement fluid enters the part which is not swept when water flooding is started, the water content is reduced, the production degree is improved from 49 percent to about 62 percent, and the recovery ratio is improved by about 13 percent; subsequent use of CO 2 The injection pressure and the pressure during the subsequent water flooding are greatly increased by the gas in the compound flooding, and the recovery ratio is increased by about 5.5 percent, which indicates that the surfactant can improve the CO content 2 The gas drive has a certain plugging effect, and the gas drive has considerable application prospect as a channeling sealing agent in subsequent application.
Compared with the prior art, the invention has the beneficial effects that:
the channeling sealing agent can obviously reduce the surface tension of water without adding a surfactant, a polymer and other additives, has certain temperature and salt resistance, can effectively improve the recovery ratio of crude oil, has stable foam and CO 2 The gas composite displacement effect is good;
the method has simple preparation process and low cost, and is beneficial to realizing large-scale production.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (7)
1. CO (carbon monoxide) 2 The preparation method of the shale oil-based channeling sealing agent for flooding is characterized by comprising the following steps of:
uniformly mixing the oil shale fines with n-octanoic acid, and standing to obtain a shale oil extracting solution; the dosage ratio of the oil shale fines to the n-caprylic acid is 1g (4-6) mL;
sulfonating the shale oil extracting solution to obtain CO 2 Shale for drivingAnd (3) an oil-based channeling sealing agent.
2. CO according to claim 1 2 The preparation method of the shale oil-based channeling sealing agent for the flooding is characterized in that the standing time is 12-24 hours.
3. CO according to claim 1 2 The preparation method of the shale oil-based channeling sealing agent is characterized in that the temperature of the sulfonation reaction is 70-90 ℃, and the time of the sulfonation reaction is 60-120 min.
4. CO according to claim 3 2 The preparation method of the shale oil-based channeling sealing agent for flooding is characterized in that the sulfonation reaction is carried out in the presence of sulfur trioxide.
5. CO according to claim 4 2 The preparation method of the shale oil-based channeling sealing agent for flooding is characterized in that sulfur trioxide passes through P 2 O 5 Reacting with concentrated sulfuric acid at 90-100 ℃, wherein P is 2 O 5 The dosage ratio of the concentrated sulfuric acid to the concentrated sulfuric acid is 1g: (0.5-1) mL.
6. CO according to claim 5 2 The preparation method of the shale oil-based channeling sealing agent for flooding is characterized in that P is 2 O 5 The dosage ratio of the shale oil extract to the shale oil extract is 1g: (0.5-2) mL.
7. CO (carbon monoxide) 2 The shale oil base channeling sealing agent for flooding is characterized in that CO is 2 A shale oil-based channeling sealing agent for flooding passing through CO described in any one of claims 1-6 2 The shale oil-based channeling sealing agent for the flooding is prepared by a preparation method.
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