CN114163981B - Expanded graphite fluid composition and preparation method and application thereof - Google Patents
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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Abstract
The invention provides an expanded graphite fluid composition, a preparation method and application thereof. The present invention provides an expanded graphite fluid composition comprising unexpanded expanded graphite and a solution comprising a dispersant and a suspending agent. The expanded graphite fluid composition provided by the invention can be added into conventional water-based drilling fluid, can be used as a plugging agent while drilling and a filtrate reducer of the drilling fluid, and can still have an expansion effect of 2-10 times under the high-temperature condition of a stratum, so that the expanded graphite fluid composition has a better plugging effect on stratum cracks, can also improve the compactness of mud cakes, and can reduce the filtrate loss of the drilling fluid.
Description
Technical Field
The invention relates to an expanded graphite fluid composition, a preparation method and application thereof.
Background
Expandable graphite has been used as an inorganic material with excellent properties in various fields (fire protection, environmental protection, medicine, etc.), its good expansibility, self-lubricity, thermal stability and chemical stability, and environmental friendliness have prompted it to become one of the widely studied materials, which can also be used as a novel drilling fluid well high temperature resistant material.
Among common organic and inorganic drilling fluid high temperature resistant materials, the problems of carbonization, agglomeration and other strength reduction of the organic materials are easy to occur under the high temperature condition, and the inorganic materials have higher rigidity and basically have no expansion performance, so that the inorganic materials can not meet the stable plugging materials of the drilling fluid under the high temperature condition. The general temperature resistance of graphite can reach above 350 ℃, and the temperature resistance of graphite can basically meet the requirement of the vast majority of drilling fluid, but the graphite is basically difficult to disperse in water and fluid due to the inert nature of the graphite surface, so that the graphite cannot realize stable dispersion in the drilling fluid and other fluids, and the wide application of the graphite is limited.
The particle size of the graphite particles themselves can be prepared by physical or chemical methods, respectively, but the dispersibility in water, particularly the suspension stability of the graphite particles in aqueous solution is difficult to solve, and graphite suspensions which are dispersed in water and can expand under high temperature conditions are rarely reported. The nano-micron expanded graphite is prepared by physical means, and is stably dispersed in aqueous solution, so that the nano-micron expanded graphite can be used as a high-temperature resistant plugging and fluid loss reducing material for drilling fluid.
Disclosure of Invention
Aiming at the defect that the expanded graphite material cannot be stably dispersed in water, the invention provides an expanded graphite system which can be stably dispersed in water, and the system can be directly added into a drilling fluid system, so that the problem of the dispersibility of the expanded graphite in water is solved.
In a first aspect the present invention provides an expanded graphite fluid composition comprising unexpanded expanded graphite and a solution comprising a dispersant and a suspending agent.
According to some embodiments of the invention, the mass content of unexpanded expanded graphite in the expanded graphite fluid composition is from 0.1 to 2wt%.
According to some embodiments of the invention, the unexpanded expanded graphite has a particle size of 0.1-200 μm, preferably 0.5-180 μm. In the present invention, the unexpanded expanded graphite refers to expandable graphite capable of being expanded in the art, but which is still in an unexpanded state.
According to some embodiments of the invention, the solution containing the dispersant and the suspending agent is an aqueous solution containing the dispersant and the suspending agent.
According to some embodiments of the invention, the concentration of the dispersant in the expanded graphite fluid composition is from 0.01 to 1.2wt%.
According to some embodiments of the invention, the concentration of the suspending agent in the expanded graphite fluid composition is from 0.01 to 0.5wt%.
According to some embodiments of the invention, the dispersant comprises one or more of an alkyl sulfonate, an alkyl benzene sulfonate, and an alkyl sulfate.
According to some embodiments of the invention, the dispersant comprises one or more of a C8-C20 alkyl sulfonate, a C8-C20 alkylbenzene sulfonate, and a C8-C20 alkyl sulfate.
According to a preferred embodiment of the present invention, the dispersant comprises one or more of dodecylbenzene sulfonate, dodecylsulfonate and dodecylsulfate.
According to a preferred embodiment of the invention, the dispersant is selected from dodecylbenzene sulphonates.
According to some embodiments of the invention, the suspending agent comprises one or more of low viscosity polyanionic cellulose, partially hydrolyzed polyacrylamide, acrylamide copolymer, and hydroxyethylcellulose.
According to a preferred embodiment of the invention, the suspending agent is selected from the group consisting of low viscosity polyanionic celluloses.
According to some embodiments of the invention, the low viscosity polyanionic cellulose has a degree of substitution >95%.
According to some embodiments of the invention, the partially hydrolyzed polyacrylamides have a degree of hydrolysis of 3.5% to 20% and a molecular weight of 5.0X10 5 -6×10 6 g/mol。
According to some embodiments of the invention, the acrylamide copolymer has a molecular weight of 5.0X10 5 -6×10 6 g/mol。
According to some embodiments of the invention, the hydroxyethyl cellulose has a molecular weight of 4.0X10 5 -1.3×10 6 g/mol。
According to some embodiments of the invention, the expanded graphite fluid composition further comprises a pH adjuster.
According to some embodiments of the invention, the pH adjuster comprises NH 3 /NH 4 Cl and Na 2 HPO 4 One or more of the following.
According to some embodiments of the invention, the expanded graphite fluid composition expands in an aqueous system.
According to some embodiments of the invention, the temperature at which expansion occurs is greater than 130 ℃.
According to some embodiments of the invention, the temperature at which the expansion occurs is 130-300 ℃, preferably 130-200 ℃.
According to some embodiments of the invention, the swelling occurs for a period of 3 to 16 hours. According to some embodiments of the present invention, the expanded graphite composition begins to expand at a temperature greater than 130 ℃ for 3-8 hours, and then expands completely for more than 12-16 hours, with higher temperatures and shorter expansion times.
According to some embodiments of the invention, the expansion is 2-10 times, e.g. 2-fold, 3-fold, 4-fold, 5-fold, 6-fold, 7-fold, 8-fold, 9-fold and any value in between.
According to some embodiments of the invention, the expansion is 4-10 times.
A second aspect of the present invention provides a method of preparing an expanded graphite fluid composition according to the first aspect, comprising the steps of:
s1: mixing expanded graphite with a solution containing a dispersing agent and a suspending agent to obtain a mixed solution;
s2: and carrying out ultrasonic dispersion on the mixed solution to obtain the expanded graphite fluid composition.
According to some embodiments of the invention, the method further comprises mixing the mixed solution with a pH adjuster to adjust pH prior to ultrasonic dispersion.
According to some embodiments of the invention, the pH is adjusted to between 5.0 and 11.0, e.g. 6.0, 7.0, 8.0, 9.0, 10.0 and any value in between.
According to a preferred embodiment of the invention, the pH is adjusted to 7.0-10.0.
According to some embodiments of the invention, in step S2, the time of the ultrasonic dispersion is 20-60min, for example 25min, 30min, 35min, 40min, 45min, 50min, 55min and any value in between.
According to some embodiments of the invention, in step S2, the power of the ultrasonic dispersion is 200-500W, such as 250W, 300W, 350W, 400W, 450W and any value in between.
A third aspect of the present invention provides the use of an expanded graphite fluid composition according to the first aspect or an expanded graphite fluid composition obtained according to the method of preparation of the second aspect in the field of drilling fluids.
According to some embodiments of the present invention, the present invention provides the use of the expanded graphite fluid composition in a lost circulation agent and/or a fluid loss additive.
In a fourth aspect the present invention provides a drilling fluid system comprising an expanded graphite fluid composition according to the first aspect or an expanded graphite fluid composition obtainable by the method of preparation according to the second aspect.
According to some embodiments of the invention, the expanded graphite fluid composition comprises 0.1 to 10wt% of the drilling fluid system.
The beneficial technical effects of the invention are as follows:
(1) The expanded graphite fluid composition provided by the invention can be added into conventional water-based drilling fluid, can be used as a plugging agent while drilling and a filtrate reducer of the drilling fluid, and can still have an expansion effect of 2-10 times under the high-temperature condition of a stratum, so that the expanded graphite fluid composition has a better plugging effect on stratum cracks, can also improve the compactness of mud cakes and reduce the filtrate loss of the drilling fluid;
(2) The expanded graphite fluid composition is simple and stable to prepare, can be produced in a large scale and can be applied to a drilling fluid site;
(3) Graphite is chemically inert, does not react with acids, bases, and salts easily, and is corrosion resistant. The increase in mineralization thus has substantially no effect on the expansibility of the expandable graphite, and the expanded graphite particles may be stably present.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to fall within the scope of the present invention.
The raw materials used in the examples are all commercially available. The expandable graphite powder solid is EPS expandable graphite obtained from Qingdao rock sea carbon materials, inc., and is unexpanded expandable graphite powder.
Example 1
0.1% by weight of an expanded graphite powdery solid (average particle diameter: 175 μm) was dispersed in an aqueous solution containing 0.015% by weight of a dispersant dodecyl sulfate and 0.012% of a suspending agent LV-PAC, and passed through a pH regulator Na 2 HPO 4 And regulating the pH value of the system solution to 7.1+/-0.1, and performing ultrasonic dispersion for 20min to obtain the well-dispersed expanded graphite fluid composition.
Example 2
1.9% by weight of an expanded graphite powdery solid (average particle diameter: 0.55 μm) was dispersed in an aqueous solution containing 0.8% by weight of a dispersant dodecylbenzenesulfonate and 0.26% of a partially hydrolyzed polyacrylamide having a degree of hydrolysis of 12% of the suspending agent, and passed through a pH adjustor NH 3 /NH 4 Cl is used for regulating the pH value of the system solution to 9.5+/-0.1, and the system solution is subjected to ultrasonic dispersion for 60 minutes to obtain a well-dispersed expanded graphite fluid composition.
Example 3
1.0% by weight of an expanded graphite powdery solid (average particle diameter 80 μm) was dispersed in an aqueous solution containing 1.2% by weight of a dispersant dodecylsulfonate and 0.48% of a suspending agent acrylamide copolymer, and passed through a pH adjustor Na 2 HPO 4 The pH value of the system solution is regulated to 6.0+/-0.1, and the system solution is subjected to ultrasonic dispersion for 50 minutes, so that a well-dispersed expanded graphite fluid composition is obtained.
Example 4
0.8wt% of an expanded graphite powdery solid (average particle diameter: 50 μm) was dispersed in a dispersion containing 0.5wt%In an aqueous solution of the dispersant dodecyl sulfonate and 0.15% of hydroxyethyl cellulose, and by means of a pH regulator NH 3 /NH 4 Cl is used for regulating the pH value of the system solution to 8.0+/-0.1, and the system solution is subjected to ultrasonic dispersion for 50min to obtain a well-dispersed expanded graphite fluid composition.
Example 5
0.8% by weight of an expanded graphite powdery solid (average particle diameter: 50 μm) was dispersed in an aqueous solution containing 0.5% by weight of a dispersant dodecylsulfonate and 0.15% of hydroxyethylcellulose, and passed through a pH adjustor NH 3 /NH 4 Cl is used for regulating the pH value of the system solution to 5.0+/-0.1, and the system solution is subjected to ultrasonic dispersion for 50min to obtain a well-dispersed expanded graphite fluid composition.
Example 6
0.8% by weight of an expanded graphite powdery solid (average particle diameter: 50 μm) was dispersed in an aqueous solution containing 0.5% by weight of a dispersant dodecylsulfonate and 0.15% of hydroxyethylcellulose, and passed through a pH adjustor NH 3 /NH 4 Cl is used for regulating the pH value of the system solution to 7.0+/-0.1, and the system solution is subjected to ultrasonic dispersion for 50min to obtain a well-dispersed expanded graphite fluid composition.
Example 7
0.8% by weight of an expanded graphite powdery solid (average particle diameter: 50 μm) was dispersed in an aqueous solution containing 0.5% by weight of a dispersant dodecylsulfonate and 0.15% of hydroxyethylcellulose, and passed through a pH adjustor NH 3 /NH 4 Cl is used for regulating the pH value of the system solution to 9.0+/-0.1, and the system solution is subjected to ultrasonic dispersion for 50min to obtain a well-dispersed expanded graphite fluid composition.
Example 8
0.8% by weight of an expanded graphite powdery solid (average particle diameter: 50 μm) was dispersed in an aqueous solution containing 0.5% by weight of a dispersant dodecylsulfonate and 0.15% of hydroxyethylcellulose, and passed through a pH adjustor NH 3 /NH 4 Cl is used for regulating the pH value of the system solution to 11.0+/-0.1, and the system solution is subjected to ultrasonic dispersion for 50min to obtain a well-dispersed expanded graphite fluid composition.
Comparative example 1
Dispersing 0.8wt% of an expanded graphite powdery solid (average particle diameter: 50 μm) in a dispersion medium containing 0.5wt% of dodecaneIn an aqueous solution of a sulfosalt and by means of a pH regulator NH 3 /NH 4 Cl is used for regulating the pH value of the system solution to 8.0+/-0.1, and the system solution is subjected to ultrasonic dispersion for 50min to obtain a well-dispersed expanded graphite fluid composition.
Comparative example 2
0.8% by weight of an expanded graphite powdery solid (average particle diameter: 50 μm) was dispersed in an aqueous solution containing 0.15% of hydroxyethylcellulose, and passed through a pH regulator NH 3 /NH 4 Cl is used for regulating the pH value of the system solution to 8.0+/-0.1, and the system solution is subjected to ultrasonic dispersion for 50min to obtain a well-dispersed expanded graphite fluid composition.
Comparative example 3
Dispersing 0.8wt% of expanded graphite powdery solid (average particle diameter 50 μm, obtained from the product obtained by expanding EPS expandable graphite obtained from Qingdao rock sea carbon Material Co., ltd. In air at 200 ℃ C. For 16 hours) in an aqueous solution containing 0.15% of hydroxyethyl cellulose, and passing through pH regulator NH 3 /NH 4 Cl is used for regulating the pH value of the system solution to 8.0+/-0.1, and the system solution is subjected to ultrasonic dispersion for 50min to obtain a well-dispersed expanded graphite fluid composition.
Test example 1
Medium pressure fluid loss of drilling fluid: according to the medium pressure water loss test method in drilling fluid test standard SY-T-5621-1993, the API fluid loss of the following drilling fluid systems are respectively tested:
common water-based drilling fluid system a:2% bentonite, 3% sulfomethyl phenolic resin, 1% asphalt, barite and water, the density is 1.35g/cm 3 ;
Water-based drilling fluid system B after addition of the expanded graphite fluid composition prepared in example 4 above: 2% bentonite+3% sulfomethylphenol resin+1% pitch+barite+2% of the expanded graphite fluid composition prepared in example 4;
water-based drilling fluid system C after addition of the expanded graphite fluid composition prepared in example 4 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+5% of the expanded graphite fluid composition prepared in example 4;
water-based drilling fluid system D after addition of the expanded graphite fluid composition prepared in example 4 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in example 4;
water-based drilling fluid system E after addition of the expanded graphite fluid composition prepared in example 1 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in example 1;
water-based drilling fluid system F after addition of the expanded graphite fluid composition prepared in example 2 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in example 2;
water-based drilling fluid system G after addition of the expanded graphite fluid composition prepared in example 3 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in example 3;
water-based drilling fluid system H after addition of the expanded graphite fluid composition prepared in example 5 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in example 5;
water-based drilling fluid system I after addition of the expanded graphite fluid composition prepared in example 6 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in example 6;
water-based drilling fluid system J after addition of the expanded graphite fluid composition prepared in example 7 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in example 7;
water-based drilling fluid system K after addition of the expanded graphite fluid composition prepared in example 8 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in example 8;
water-based drilling fluid system L after adding the expanded graphite fluid composition prepared in comparative example 1 above: 2% bentonite+3% sulfomethylphenol resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in comparative example 1;
water-based drilling fluid system M after adding the expanded graphite fluid composition prepared in comparative example 2 above: 2% bentonite+3% sulfomethyl phenolic resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in comparative example 2; and
water-based drilling fluid system N after adding the expanded graphite fluid composition prepared in comparative example 3 above: 2% bentonite+3% sulfomethylphenol resin+1% pitch+barite+8% of the expanded graphite fluid composition prepared in comparative example 3; and
API fluid loss of the above systems after aging at 200℃for 16 hours.
The results are shown in Table 1.
TABLE 1
From the data in table 1, the fluid loss of the fluid composition added with the expanded graphite is significantly reduced, which indicates that the graphite particles have good plugging performance on drilling fluid, and particularly, the reduction effect of graphite after high-temperature aging on the fluid loss of the drilling fluid is more significant.
Test example 2
Characterization method of expansion performance of expandable graphite: 1g of the expanded graphite fluid composition prepared in examples 2 to 4 was weighed, poured into a graduated quartz glass tube, and the graphite volume was recorded as V 1 Then 50g of alkaline water (pH about 9) was added to the glass tube; placing the glass tube into a high-temperature high-pressure kettle at room temperature, sealing the high-temperature high-pressure kettle, heating for a certain time at different temperatures, cooling to room temperature, taking out the quartz glass tube, and recording that the volume of the expanded graphite is V 2 ,V 2 /V 1 The ratio of (2) is expressed as the volume expansion factor of graphite, and the data of the results are shown in Table 2.
TABLE 2
It should be noted that the above-described embodiments are only for explaining the present invention and do not limit the present invention in any way. 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.
Claims (14)
1. An expanded graphite fluid composition comprising unexpanded expanded graphite and a solution comprising a dispersant and a suspending agent; the dispersant comprises one or more of alkyl sulfonate, alkylbenzene sulfonate and alkyl sulfate; the suspending agent comprises one or more of low-viscosity polyanionic cellulose, partially hydrolyzed polyacrylamide, acrylamide copolymer and hydroxyethyl cellulose;
in the expanded graphite fluid composition, the mass content of the unexpanded expanded graphite is 0.1 to 2wt%; the concentration of the dispersing agent is 0.01-1.2wt%; the concentration of the suspending agent is 0.01-0.5wt%;
the expanded graphite fluid composition further comprises a pH adjuster; the expanded graphite fluid composition has a pH of from 5.0 to 11.0.
2. The expanded graphite fluid composition according to claim 1, wherein the solution containing a dispersant and a suspending agent is an aqueous solution containing a dispersant and a suspending agent.
3. The expanded graphite fluid composition according to claim 1 or 2, wherein the unexpanded expanded graphite has a particle size of 0.1-200 μm; and/or
The dispersant comprises C 8 -C 20 Alkyl sulfonate, C 8 -C 20 Alkylbenzene sulfonate and C 8 -C 20 One or more of the alkyl sulfates of (a); and/or
The suspending agent is selected from the group consisting of low viscosity polyanionic celluloses.
4. The expanded graphite fluid composition according to claim 1 or 2, wherein the unexpanded expanded graphite has a particle size of 0.5-180 μm; and/or
The dispersant comprises one or more of dodecyl benzene sulfonate, dodecyl sulfonate and dodecyl sulfate; and/or
Degree of substitution of the low viscosity polyanionic cellulose>95%; the degree of hydrolysis of the partially hydrolyzed polyacrylamide is 3.5% -20%, and the molecular weight is 5.0X10 5 -6.0×10 6 g/mol; the molecular weight of the acrylamide copolymer is 5.0X10 5 -6.0×10 6 g/mol; the molecular weight of the hydroxyethyl cellulose is 4.0X10 5 -1.3×10 6 g/mol。
5. The expanded graphite fluid composition according to claim 1 or 2, wherein the pH adjuster comprises NH 3 /NH 4 Cl and Na 2 HPO 4 One or more of the following.
6. The expanded graphite fluid composition according to claim 1 or 2, wherein the expanded graphite fluid composition expands in an aqueous system.
7. The expanded graphite fluid composition according to claim 6, wherein the temperature at which expansion occurs is greater than 130 ℃ and/or the time for which expansion occurs is from 3 to 16 hours.
8. The expanded graphite fluid composition according to claim 7, wherein the expansion is 2-10 times.
9. A method of preparing an expanded graphite fluid composition according to any one of claims 1-8, comprising the steps of:
s1: mixing the unexpanded expanded graphite with a solution containing a dispersing agent and a suspending agent to obtain a mixed solution;
s2: performing ultrasonic dispersion on the mixed solution to obtain the expanded graphite fluid composition;
the preparation method also comprises the step of mixing the mixed solution with a pH regulator and regulating the pH to 5.0-11.0 before ultrasonic dispersion.
10. The method according to claim 9, wherein the pH is adjusted to 7.0 to 10.0.
11. The method according to claim 9 or 10, wherein in step S2, the time of the ultrasonic dispersion is 20 to 60min; the power of the ultrasonic dispersion is 200-500W.
12. Use of an expanded graphite fluid composition according to any one of claims 1-8 or obtained according to the method of preparation of any one of claims 9-11 in the field of drilling fluids.
13. A drilling fluid system comprising the expanded graphite fluid composition according to any one of claims 1-8 or the expanded graphite fluid composition obtained by the method of preparation according to any one of claims 9-11.
14. The drilling fluid system of claim 13, wherein the expanded graphite fluid composition comprises from 0.1 to 10wt% of the drilling fluid system.
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CN106640000A (en) * | 2016-09-13 | 2017-05-10 | 中国石油大学(华东) | Expandable graphite plugging agent system for deep channel blocking of heavy oil reservoir steam flooding and injection method |
CN111454698A (en) * | 2019-01-20 | 2020-07-28 | 中石化石油工程技术服务有限公司 | Drilling fluid containing plugging particle composition |
CN111188606A (en) * | 2020-01-14 | 2020-05-22 | 中国石油大学(华东) | Low-temperature expandable graphite for steam injection channeling sealing of heavy oil reservoir and preparation method and application thereof |
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