CN108864387B - Drag reducer for carbon dioxide dry fracturing and application thereof - Google Patents

Drag reducer for carbon dioxide dry fracturing and application thereof Download PDF

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CN108864387B
CN108864387B CN201810743824.6A CN201810743824A CN108864387B CN 108864387 B CN108864387 B CN 108864387B CN 201810743824 A CN201810743824 A CN 201810743824A CN 108864387 B CN108864387 B CN 108864387B
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styrene
carbon dioxide
drag reducer
polystyrene
fluorinated acrylate
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CN108864387A (en
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张劲
伊安
祝佳秋
薛振乾
齐璇
陆强民
高源�
宋帅
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Beijing Niuhe Ruichen Energy Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F301/00—Macromolecular compounds not provided for in groups C08F10/00 - C08F299/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F293/00—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule
    • 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
    • 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
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/28—Friction or drag reducing additives

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  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
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  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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Abstract

The invention provides a drag reducer for carbon dioxide dry fracturing and application thereof. The drag reducer of the present invention mainly comprises: the fluorinated acrylate-styrene-sulfonated styrene block copolymer is prepared by polymerization reaction of fluorinated acrylate polymer, sulfonated polystyrene and styrene, wherein the mass ratio of the fluorinated acrylate-styrene-sulfonated styrene block copolymer to the fluorinated acrylate-styrene-sulfonated styrene block copolymer is (55-65) to (20-30) to (10-20). The drag reducer has good compatibility with carbon dioxide, is dissolved in carbon dioxide fracturing fluid, can reduce the frictional resistance during fracturing, further reduce the ground pump pressure, reduce the pressure bearing of a pipeline, ensure that the carbon dioxide dry-method fracturing engineering is safer, the pipeline can better meet the working requirement, improve the speed of injecting liquid carbon dioxide, ensure that the carbon dioxide dry-method fracturing can be used in a deeper reservoir stratum with more extreme conditions, still can keep good drag reduction effect under more extreme conditions, and the drag reduction effect can reach 30-40% in the fracturing operation.

Description

Drag reducer for carbon dioxide dry fracturing and application thereof
Technical Field
The invention relates to the technical field of oilfield chemistry, in particular to a drag reducer for carbon dioxide dry fracturing and application thereof.
Background
The use of the carbon dioxide fracturing fluid can greatly reduce or eliminate the contact chance of water and the stratum in the fracturing construction, thereby greatly reducing the damage of the stratum caused by water lock and water sensitivity. The dry carbon dioxide fracturing technology has wide prospects in development of shale gas, compact oil reservoirs and strong water-sensitive strata, has many advantages compared with the conventional fracturing technology, and mainly comprises the following steps: (1) the water-free phase eliminates the damage caused by water sensitivity and water lock; (2) the fracturing fluid has extremely low interfacial tension, and is directly discharged back without gel breaking after heated and gasified; (3) the oil can be dissolved in the crude oil, so that the viscosity of the crude oil can be reduced, and the fluidity of the crude oil can be improved.
However, the carbon dioxide fracturing fluid simultaneously faces the problem of high friction resistance in fracturing construction, which limits the application range of the carbon dioxide fracturing fluid, so that some low-permeability and strong water-sensitive reservoirs with deeper burial have to use the conventional water-based fracturing fluid, permanent damage is caused to the reservoirs, and the development effect is not ideal.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a drag reducer for carbon dioxide dry fracturing and a preparation method and application thereof. The main component of the drag reducer is fluorinated acrylate-styrene-sulfonated styrene block copolymer, so that the problem of high friction resistance of the carbon dioxide fracturing fluid can be effectively solved.
In order to achieve the above object, the present invention provides a drag reducer for carbon dioxide dry fracturing, the drag reducer comprising: fluorinated acrylate-styrene-sulfonated styrene block copolymer is prepared by polymerization reaction of fluorinated acrylate polymer, sulfonated polystyrene and styrene.
Among the above-mentioned drag reducers, it is preferable that the mass ratio of the fluorinated acrylate polymer, the sulfonated polystyrene and the styrene used is (55-65): (20-30): (10-20), more preferably 60:25: 15.
In the above drag reducer, the reaction temperature of the polymerization reaction is preferably 75 to 80 ℃ and the reaction time is preferably 1 to 2 hours.
According to a particular embodiment of the present invention, preferably, the fluorinated acrylate-styrene-sulfonated styrene block copolymer is prepared by the following steps: (1) mixing and stirring uniformly appropriate amounts of water, fluorinated acrylate polymer and styrene to obtain a mixed solution (the amount of water added in the mixed solution can be adjusted by a person skilled in the art in a conventional way): (2) adjusting the pH value of the mixed solution to 7-10 (the pH value adjusting agent adopted can be conventional in the field, such as ammonia water, sodium hydroxide and monoethanolamine), then adding sulfonated polystyrene and an initiator, and carrying out polymerization reaction for 1-2 hours at 75-80 ℃ to obtain the fluorinated acrylate-styrene-sulfonated styrene block copolymer. The initiator used in the polymerization reaction comprises azobisisobutyronitrile and Na2S2O8And Na2S2O3One or a combination of several of the above; preferably, in the step (2), the total amount of the initiator added is 0.08-0.12% of the total mass of the sulfonated polystyrene and the styrene.
In the above drag reducer, preferably, the fluoroacrylate polymer is prepared by: butyl methacrylate, isobornyl methacrylate and methyl methacrylate are used as mixed monomers to carry out polymerization reaction, and dodecafluoroheptyl methacrylate is added to continue the polymerization reaction to prepare the fluorinated acrylate polymer. Among them, it is preferable that the mass ratio of butyl methacrylate, isobornyl methacrylate, methyl methacrylate and dodecafluoroheptyl methacrylate is 40:10:25: 25. The reaction temperature for the polymerization reaction using butyl methacrylate, isobornyl methacrylate and methyl methacrylate as the mixed monomer may be 75 to 80 ℃ and the reaction time may be 1 to 3 hours, and then the reaction temperature for the polymerization reaction continued by adding dodecafluoroheptyl methacrylate may be 75 to 80 ℃ and the reaction time may be 1 to 3 hours. In addition, the polymerization reaction is carried out in the presence of an initiator, wherein the initiator comprises azodiisobutyronitrile and Na2S2O8And Na2S2O3The addition amount of the initiator is 0.05-0.08%, preferably 0.05-0.06%. Both of the two polymerization steps in the preparation of the fluoroacrylate polymer require the addition of an initiator.
Among the above drag reducers, preferably, the sulfonated polystyrene is prepared by: and mixing and reacting the organic solution of polystyrene with concentrated sulfuric acid to prepare the sulfonated polystyrene. Wherein, the mass ratio of the polystyrene to the concentrated sulfuric acid can be 90: 10. The solvent in the organic solution of polystyrene may include dichloroethane, a mixture of toluene and butanol, and the like. Preferably, the solvent is a mixed solution of toluene and butanol, and the mass ratio of the toluene to the butanol is (30-40): (60-70). The organic solution of polystyrene may be prepared by adding polystyrene to a solvent and stirring at 60 ℃ to completely dissolve the polystyrene. Further, the reaction temperature of mixing and reacting the organic solution of polystyrene with concentrated sulfuric acid is preferably not more than 40 ℃, and the reaction time may be 10 hours. In addition, after the organic solution of polystyrene is mixed with concentrated sulfuric acid and reacted, the obtained precipitate may be washed and dried to prepare sulfonated polystyrene.
The fluorinated acrylate-styrene-sulfonated styrene block copolymer comprised by the drag reducer provided by the present invention may be prepared by:
firstly, butyl methacrylate, isobornyl methacrylate and methyl methacrylate are taken as mixed monomers to carry out polymerization reaction for 1-3 hours at 75-80 ℃, and then dodecafluoroheptyl methacrylate is added to carry out polymerization reaction for 1-3 hours at 75-80 ℃ to prepare the fluorinated acrylate polymer; wherein the mass ratio of the butyl methacrylate to the isobornyl methacrylate to the methyl methacrylate to the dodecafluoroheptyl methacrylate is 40:10:25: 25; mixing organic solution of polystyrene with concentrated sulfuric acid, and reacting at 40 ℃ for 10 hours to prepare sulfonated polystyrene; wherein the mass ratio of the polystyrene to the concentrated sulfuric acid is 90: 10;
mixing and uniformly stirring a proper amount of water, fluorinated acrylate polymer and styrene to obtain a mixed solution: and adjusting the pH value of the mixed solution to 7-10, then adding sulfonated polystyrene and an initiator, and carrying out polymerization reaction for 1-2 hours at the temperature of 75-80 ℃ to obtain the fluorinated acrylate-styrene-sulfonated styrene block copolymer.
In the process of preparing the fluorinated acrylate-styrene-sulfonated styrene block copolymer, the adopted initiator comprises azodiisobutyronitrile and Na2S2O8And Na2S2O3One or a combination of several of the above; preferably Na2S2O8And Na2S2O3The two initiators are combined for redox reaction to form a redox initiation system, OH generated by the redox reaction can abstract hydrogen on a substance to form a new free radical, so that the polymerization effect of the fluorinated acrylate-styrene-sulfonated styrene block copolymer is better; the ratio of the two is preferably (60-70) to (30-40). Wherein the total addition of the initiator is 0.08-0.12% of the total mass of the sulfonated polystyrene and the styrene.
On the other hand, the invention also provides an application of the drag reducer for carbon dioxide dry fracturing in a carbon dioxide fracturing fluid.
In the application, the fluorinated acrylate-styrene-sulfonated styrene block copolymer in the drag reducer for carbon dioxide dry fracturing is preferably added in an amount of 50-80mg/L in the carbon dioxide fracturing fluid. By adopting the smaller dosage, the cost can be well controlled, and the wellhead back pressure of the pipeline can be reduced by 30-40 percentage points in the carbon dioxide dry fracturing process.
The main component of the drag reducer for carbon dioxide dry fracturing provided by the invention is fluorinated acrylate-styrene-sulfonated styrene block copolymerization, and the drag reducer has good compatibility with carbon dioxide; the friction resistance (including the injection process and the friction resistance along the process) during fracturing can be reduced by dissolving the drag reducer in the carbon dioxide fracturing fluid, so that the ground pump pressure is reduced, the pressure bearing of a pipeline is reduced, the carbon dioxide dry fracturing engineering is safer, the pipeline can meet the working requirement, the speed of injecting liquid carbon dioxide is increased, the carbon dioxide dry fracturing can be used in a deeper reservoir with more extreme conditions (such as high temperature and high pressure), a better drag reduction effect can be still kept under the more extreme conditions, and the drag reduction effect in the fracturing operation can reach 30-40%; therefore, the drag reducer provided by the invention can enable the carbon dioxide fracturing fluid to have a wider application range and a more economic development effect.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
This example provides a drag reducer for carbon dioxide dry fracturing, which comprises fluorinated acrylate-styrene-sulfonated styrene block copolymer as the total component, and is prepared by the following steps:
1. preparation of fluorinated acrylate polymer:
(1) adding deionized water, ethanol and concentrated hydrochloric acid with the concentration of 37 wt% in a mass ratio of 50:28:22 into a three-neck flask, and uniformly stirring at room temperature; uniformly mixing butyl methacrylate, isobornyl methacrylate and methyl methacrylate in a mass ratio of 41:35:24 in a mixed solvent of toluene and butyl acetate (wherein the mass ratio of toluene to butyl acetate is 1:2) to obtain a mixed monomer, adding the mixed monomer into a three-neck flask containing a mixed solution of deionized water, ethanol and concentrated hydrochloric acid, adding an initiator of azobisisobutyronitrile, wherein the addition amount of azobisisobutyronitrile is 0.05%, and carrying out polymerization reaction at 75-80 ℃ for 2 hours to obtain a mixed solution containing a first polymer;
(2) uniformly mixing dodecafluoroheptyl methacrylate and an initiator azobisisobutyronitrile, dropwise adding the mixture into a three-neck flask containing the mixed solution containing the first polymer at the temperature of 75-80 ℃ at the speed of 0.05mL/s, and continuing to perform polymerization reaction (namely, completing the reaction after the dropwise adding is finished) for 1.5 hours to obtain a crude product of the fluorinated acrylate polymer; wherein the mass ratio of the dodecafluoroheptyl methacrylate to the methyl methacrylate in the step (1) is 52:48, and the addition amount of the azobisisobutyronitrile adopted in the step is 0.08%;
(3) and refining the crude product of the fluorinated acrylate polymer to obtain the fluorinated acrylate polymer.
2. Preparation of sulfonated polystyrene:
adding polystyrene into dichloroethane, stirring at 60 ℃ to completely dissolve the polystyrene, wherein the ratio of the polystyrene to the dichloroethane is 1g:100mL, cooling, adding concentrated sulfuric acid with the concentration of 98%, and the mass ratio of the concentrated sulfuric acid to the polystyrene is 90:10, reacting at 40 ℃ for 10 hours, separating the obtained precipitate from liquid, washing with distilled water, and drying at 25 ℃ for 4 hours to obtain sulfonated polystyrene.
3. Preparation of fluorinated acrylate-styrene-sulfonated styrene block copolymer:
(1) adding deionized water, fluorinated acrylate polymer and styrene in a mass ratio of 63:25:12 into a polymerization reaction kettle, and uniformly stirring and mixing to obtain a mixed solution:
(2) adjusting the pH value of the mixed solution to 7-10 by using sodium hydroxide, and then adding sulfonated polystyrene and an initiator Na2S2O8-Na2S2O3(the mass ratio of the sulfonated polystyrene to the styrene is 65: 35; the total addition of the initiator is 0.09% of the total mass of the sulfonated polystyrene and the styrene), and the mass ratio of the added sulfonated polystyrene to the styrene is 70:30, and the fluorinated acrylate-styrene-sulfonated styrene block copolymer is obtained after the polymerization reaction is carried out for 1 to 2 hours at the temperature of 75 to 80 ℃.
The drag reducer for carbon dioxide dry fracturing provided in this embodiment is added to pure liquid carbon dioxide, and the addition amount is 60mg/L, so as to obtain a liquid carbon dioxide fracturing fluid containing the drag reducer.
The liquid carbon dioxide fracturing fluid containing the drag reducer is used in the fracturing process, and the whole process is closed to contain liquid CO2Storing in ground, pressurizing and delivering to CO2The liquid inlet system of the sand mixing truck is sealed, and the pressure and the temperature of a plurality of sections (12 places) are carried outAnd (5) monitoring the degree, and finding that the back pressure of the wellhead of the pipeline is reduced by 30-40 percentage points after the construction is finished.
Comparative example 1
Zoihua Huang et al (Enhancement of the vision of Carbon Dioxide Using Styrene/fluoro copolymers, macromolecules [ J].2000, 33(15): 5437-5442) copolymers of fluorinated acrylates and styrene were synthesized to increase the viscosity of liquid carbon dioxide. Styrene was distilled under vacuum before use, HFDA was purified to remove inhibitors before use, HFDA and styrene copolymer monomers were obtained by bulk radical polymerization and used AIBN as initiator. In the presence of inert nitrogen2A50 mL glass bottle was charged with 5.18g of monomer HFDA (0.01mol), 0.42g of styrene (4.0mmol), and 4.6mg of AIBN under the same conditions. Sealing the glass bottle, carrying out water bath at 65 ℃ for 12 hours, cooling the reaction mixture, dissolving the reaction mixture in 1,1, 2-trichlorotrifluoroethane, precipitating the polymer in methanol, washing and drying to finally prepare the copolymer of the fluorinated acrylate and the styrene.
The mixture of polymer and carbon dioxide was tested experimentally at 295K and at pressures from 6.70 to 48.28 MPa. Experiments have shown that the solubility of the polymers decreases with increasing styrene content in the polymer chains, the miscible pressure decreases with decreasing styrene content, and these polymers increase the viscosity of carbon dioxide by about one-fold with increasing molecular weight, with an optimum fluorine-containing mole fraction of 29-71% in the styrene used for viscosification.
The copolymer of fluorinated acrylate and styrene synthesized by Zhuihua Huang and the like adopts AIBN (azobisisobutyronitrile) as an initiator, and can cause the problems of crystallization, reaction residue generation and the like under the condition of unstable experimental conditions, and the copolymer has certain toxicity and certain harm to experimenters. While the preferred initiator of the present invention is Na2S2O8And Na2S2O3The combination of (1) has simple operation and less side reaction, the two initiators are combined to generate redox reaction to form a redox initiation system, OH generated by the redox reaction can abstract hydrogen on a substance to form a new free radical, so that fluorination is realizedThe polymerization effect of the acrylate-styrene-sulfonated styrene block copolymer is better.

Claims (10)

1. A drag reducer for carbon dioxide dry fracturing, the drag reducer comprising: fluorinated acrylate-styrene-sulfonated styrene block copolymer prepared by polymerization reaction of fluorinated acrylate polymer, sulfonated polystyrene and styrene;
wherein the mass ratio of the fluorinated acrylate polymer to the sulfonated polystyrene to the styrene is 60:25: 15;
the fluorinated acrylate-styrene-sulfonated styrene block copolymer is prepared by the following steps:
(1) mixing and uniformly stirring a proper amount of water, fluorinated acrylate polymer and styrene to obtain a mixed solution:
(2) adjusting the pH value of the mixed solution to 7-10, then adding sulfonated polystyrene and an initiator, and carrying out polymerization reaction for 1-2 hours at the temperature of 75-80 ℃ to obtain a fluorinated acrylate-styrene-sulfonated styrene block copolymer; wherein the initiator comprises azobisisobutyronitrile and Na2S2O8And Na2S2O3One or a combination of more of the components, wherein the addition amount of the initiator is 0.05-0.08% by the total mass of the fluorinated acrylate polymer, the sulfonated polystyrene and the styrene;
the fluorinated acrylate polymer is prepared by the following steps: firstly, taking butyl methacrylate, isobornyl methacrylate and methyl methacrylate as mixed monomers to carry out polymerization reaction, and then adding dodecafluoroheptyl methacrylate to continue the polymerization reaction to prepare the fluorinated acrylate polymer; wherein, the reaction temperature of the polymerization reaction of the butyl methacrylate, the isobornyl methacrylate and the methyl methacrylate as the mixed monomers is 75-80 ℃, the reaction time is 1-3 hours, and then the reaction temperature of the polymerization reaction of the dodecafluoroheptyl methacrylate is 75-80 ℃ and the reaction time is 1-3 hours;
the sulfonated polystyrene is prepared by the following steps: mixing and reacting an organic solution of polystyrene with concentrated sulfuric acid to prepare the sulfonated polystyrene; wherein the mass ratio of the polystyrene to the concentrated sulfuric acid is 90: 10; the solvent in the organic solution of polystyrene comprises dichloroethane or a mixed solution of toluene and butanol; the solvent is a mixed solution of toluene and butanol, and the mass ratio of the toluene to the butanol is (30-40): (60-70).
2. The drag reducer of claim 1, wherein the initiator is added in an amount of 0.05% to 0.06%.
3. The drag reducer of claim 1, wherein the mass ratio of butyl methacrylate, isobornyl methacrylate, methyl methacrylate, and dodecafluoroheptyl methacrylate is 40:10:25: 25.
4. The drag reducer of claim 1 or 2, wherein the organic solution of polystyrene is prepared by adding polystyrene to a solvent and stirring at a temperature not exceeding 60 ℃ to completely dissolve the polystyrene.
5. Drag reducer according to claim 1 or 2, characterized in that the organic solution of polystyrene is mixed with concentrated sulfuric acid and reacted at a reaction temperature not exceeding 40 ℃ for a reaction time of 10 hours.
6. The drag reducer of claim 1, wherein the initiator comprises Na2S2O8And Na2S2O3Combinations of (a) and (b).
7. The drag reducer of claim 6, wherein the Na is2S2O8And Na2S2O3The mass ratio of (60-70) to (30-40).
8. The drag reducer of claim 1, wherein the total initiator loading is 0.08% -0.12% of the total mass of sulfonated polystyrene and styrene.
9. Use of a drag reducer for carbon dioxide dry fracturing as claimed in any of claims 1 to 8 as a drag reducer in a carbon dioxide fracturing fluid.
10. The use of claim 9, wherein the fluorinated acrylate-styrene-sulfonated styrene block copolymer in the drag reducer for carbon dioxide dry fracturing is added in an amount of 50-80mg/L in the carbon dioxide fracturing fluid.
CN201810743824.6A 2018-07-09 2018-07-09 Drag reducer for carbon dioxide dry fracturing and application thereof Active CN108864387B (en)

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Publication number Priority date Publication date Assignee Title
CN111019627B (en) * 2019-12-17 2021-11-26 陕西延长石油(集团)有限责任公司研究院 Drag reducer and preparation method and application thereof
CN115873582B (en) * 2022-12-27 2024-07-02 泰坦(天津)能源技术有限公司 Composite carbon dioxide fracturing fluid and preparation method and application thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
SIWEI Meng et.al..《Thickening carbon dioxide by designing new block copolymer》.《Advanced Materials Research (Durnten-Zurich, Switzerland) (2014), 1021(Advanced Research on Structure, Materials, Engineering and Information Technology III)》.2014,第1021卷第20-24页. *
Zhang, J.;Rao, L. Q.;Meng, S. W.;Lu, G. W.;Zhang, R.;Yu, W..《Thickening carbon dioxide with amphiphilic block copolymer》.《WIT Transactions on Ecology and the Environment (2015), 206(Energy and Sustainability V: Special Contributions)》.2015,第206卷第175-182页. *
Zhihua Huang et.al..《Enhancement of the Viscosity of Carbon Dioxide Using Styrene/Fluoroacrylate Copolymer》.《Macromolecules》.2000,第33卷第5437-5442页. *

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