CN108864387A - A kind of carbon dioxide dry method pressure break drag reducer and its application - Google Patents
A kind of carbon dioxide dry method pressure break drag reducer and its application Download PDFInfo
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- CN108864387A CN108864387A CN201810743824.6A CN201810743824A CN108864387A CN 108864387 A CN108864387 A CN 108864387A CN 201810743824 A CN201810743824 A CN 201810743824A CN 108864387 A CN108864387 A CN 108864387A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
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- C09K2208/28—Friction or drag reducing additives
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Abstract
The present invention provides a kind of carbon dioxide dry method pressure break drag reducer and its applications.Drag reducer of the invention mainly includes：Fluorinated acrylic ester-styrene-sulfonated phenylethylene the block copolymer being prepared by fluorinated acrylate polymer, sulfonated polystyrene and styrene by polymerization reaction, wherein the mass ratio of three is (55-65):(20-30):(10-20).The drag reducer and carbon dioxide have preferable compatibility, it is dissolved in carbon dioxide pressure break liquid, it can reduce frictional resistance when pressure break, and then reduce ground pump pressure, reduce the pressure-bearing of pipeline, make that carbon dioxide dry method fracturing engineering is safer, pipeline is more able to satisfy job requirement, improve the speed of injection liquid carbon dioxide, it is able to use carbon dioxide dry method pressure break in reservoir deeper, that condition is more extreme, and it is still able to maintain preferable drag-reduction effect under conditions of more extreme, drag-reduction effect can reach 30%-40% in fracturing work.
Description
Technical field
The present invention relates to technical field of oilfield chemistry, and in particular to carbon dioxide dry method pressure break drag reducer and its application.
Background technique
The use of carbon dioxide pressure break liquid can substantially reduce or eliminate the touch opportunity of water and stratum in pressing crack construction,
Thus greatly reduce formation damage caused by water lock and water-sensitive.Dry method carbon dioxide pressure break technology is in exploitation shale gas, densification
Oil reservoir and strong retraction stratum all have broad prospects, and dry method carbon dioxide pressure break technology has compared to conventional fracturing technology
There are many advantages, mainly includes：(1) it without water phase, eliminates and is injured caused by water-sensitive and water lock；(2) fracturing fluid has extremely low boundary
Face tension is not necessarily to the broken glue directly row of returning by after thermal evaporation；(3) it is dissolved in crude oil, can reduce the viscosity of crude oil, improve crude oil
Mobility.
However, carbon dioxide pressure break liquid faces the higher problem of frictional resistance simultaneously in pressing crack construction, which has limited titanium dioxides
The scope of application of carbon fracturing fluid buries deeper hypotonic, strong retraction reservoir and has to using conventional aqueous fracturing fluid so that some,
Possible permanent damage is caused to reservoir, and development effectiveness is undesirable.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide a kind of carbon dioxide dry method pressure break drag reducer and
Preparation method and application.The main component of drag reducer of the invention is fluorinated acrylic ester-styrene-sulfonated phenylethylene block
Copolymer can effectively solve the higher problem of carbon dioxide pressure break liquid frictional resistance.
In order to achieve the above objectives, present invention firstly provides a kind of carbon dioxide dry method pressure break drag reducer, the drag reducers
Including：The fluorination third being prepared by fluorinated acrylate polymer, sulfonated polystyrene and styrene by polymerization reaction
Olefin(e) acid ester-styrene-sulfonated phenylethylene block copolymer.
In above-mentioned drag reducer, it is preferable that used fluorinated acrylate polymer, sulfonated polystyrene and benzene second
The mass ratio of alkene is (55-65):(20-30):(10-20), more preferably 60:25:15.
In above-mentioned drag reducer, it is preferable that the reaction temperature of polymerization reaction is 75-80 DEG C, and the reaction time is 1-2 hours.
Specific embodiment according to the present invention, it is preferable that fluorinated acrylic ester-styrene-sulfonated phenylethylene block is total
Polymers is through the following steps that be prepared：(1) suitable quantity of water, fluorinated acrylate polymer and styrene are mixed and is stirred
It mixes and uniformly obtains mixed liquor (additional amount of water can be carried out conventional adjusting by those skilled in the art in the mixed liquor)：(2)
Adjusting the pH value of the mixed liquor, (pH adjusting agent used can be that this field is conventional, such as ammonium hydroxide, hydroxide to 7-10
Sodium, monoethanolamine), sulfonated polystyrene and initiator is then added, 75-80 DEG C progress polymerization reaction 1-2 hours, obtain fluorine
Change Acrylate-styrene bipolymer-sulfonated phenylethylene block copolymer.Initiator used by above-mentioned polymerization reaction includes that azo two is different
Butyronitrile, Na2S2O8And Na2S2O3Deng one or more of combination；Preferably, in above-mentioned steps (2), initiator is always added
Amount is the 0.08%-0.12% of sulfonated polystyrene and styrene gross mass.
In above-mentioned drag reducer, it is preferable that the fluorinated acrylate polymer is through the following steps that be prepared：
It is anti-that polymerization first occurs using butyl methacrylate, isobornyl methacrylate and methyl methacrylate as mix monomer
It answers, adds dodecafluoroheptyl methacrylate and continue that polymerization reaction occurs, fluorinated acrylate polymer is prepared.Its
In, it is preferable that butyl methacrylate, ten difluoro of isobornyl methacrylate, methyl methacrylate and methacrylic acid
The mass ratio of heptyl ester is 40:10:25:25.Also, with butyl methacrylate, isobornyl methacrylate and metering system
Sour methyl esters can be 75-80 DEG C as the reaction temperature that polymerization reaction occurs for mix monomer, and the reaction time can be 1-3 hours,
It to be 75-80 DEG C that the reaction temperature that dodecafluoroheptyl methacrylate continues that polymerization reaction occurs is added later, the reaction time
It can be 1-3 hours.In addition, above-mentioned polymerization reaction is carried out in the presence of initiator, which includes that azo two is different
Butyronitrile, Na2S2O8And Na2S2O3One or more of combination, the additive amount of initiator is 0.05%-0.08%, preferably
0.05%-0.06%.The two-stage polymerization reaction during fluorinated acrylate polymer is prepared to be required to that initiator is added.
In the above-mentioned drag reducer, it is preferable that sulfonated polystyrene is through the following steps that be prepared：By polystyrene
Organic solution mix and react with the concentrated sulfuric acid, sulfonated polystyrene is prepared.Wherein, the quality of polystyrene and the concentrated sulfuric acid
Than that can be 90:10.Also, the solvent in the organic solution of polystyrene may include the mixed of dichloroethanes, toluene and butanol
Close liquid etc..Preferably, above-mentioned solvent is the mixed liquor of toluene and butanol, and the mass ratio of the two is (30-40)：(60-70).Polyphenyl
The organic solution of ethylene can be by the way that polystyrene is added in solvent and is prepared and 60 DEG C of stirrings make it completely dissolved
It obtains.In addition, the reaction temperature that the organic solution of polystyrene is mixed and reacted with the concentrated sulfuric acid is preferably more than 40 DEG C, reaction
Time can be 10 hours.In addition, the organic solution of polystyrene is mixed with the concentrated sulfuric acid and after reaction, can will obtain
Sediment washed, dried, so that sulfonated polystyrene be prepared.
Fluorinated acrylic ester-styrene-sulfonated phenylethylene block copolymer that drag reducer provided by the present invention is included
Can with through the following steps that preparation：
First using butyl methacrylate, isobornyl methacrylate and methyl methacrylate as mix monomer in
75-80 DEG C generation polymerization reaction 1-3 hours, add dodecafluoroheptyl methacrylate continue polymerization occurs in 75-80 DEG C it is anti-
It answers 1-3 hours, fluorinated acrylate polymer is prepared；Wherein, the butyl methacrylate, methacrylic acid isoborneol
The mass ratio of ester, methyl methacrylate and dodecafluoroheptyl methacrylate is 40:10:25:25；By the organic of polystyrene
Solution is mixed with the concentrated sulfuric acid, reacts 10 hours in 40 DEG C, sulfonated polystyrene is prepared；Wherein, the polystyrene with it is dense
The mass ratio of sulfuric acid is 90:10；
Suitable quantity of water, fluorinated acrylate polymer and styrene are mixed and stirred for uniformly, to obtain mixed liquor：Adjust institute
The pH value of mixed liquor is stated to 7-10, then addition sulfonated polystyrene and initiator, small in 75-80 DEG C of progress polymerization reaction 1-2
When, obtain fluorinated acrylic ester-styrene-sulfonated phenylethylene block copolymer.
During preparing fluorinated acrylic ester-styrene-sulfonated phenylethylene block copolymer, used initiator
Including azodiisobutyronitrile, Na2S2O8And Na2S2O3Deng one or more of combination；Preferably Na2S2O8And Na2S2O3's
Combination, two kinds of initiators, which are used in combination, occurs redox reactions, forms redox initiation system, redox reaction produce at
OH can capture the hydrogen on substance and form new free radical so that fluorinated acrylic ester-styrene-sulfonated phenylethylene is embedding
The polymerization effect of section copolymer is more preferably；The ratio of the two is preferably (60-70):(30-40).Wherein, the total additional amount of initiator is
The 0.08%-0.12% of sulfonated polystyrene and styrene gross mass.
On the other hand, the present invention also provides a kind of above-mentioned carbon dioxide dry method pressure break drag reducers in carbon dioxide pressure break
As the application of drag reducer in liquid.
In above-mentioned application, it is preferable that fluorinated acrylic ester-benzene second in the carbon dioxide dry method pressure break drag reducer
Additive amount of the alkene-sulfonated phenylethylene block copolymer in the carbon dioxide pressure break liquid is 50-80mg/L.It is lesser using this
Dosage, the available good control of cost, and pipeline wellhead back pressure can be made to drop in carbon dioxide dry method fracturing process
Low 30-40 percentage points.
The main component of carbon dioxide dry method pressure break drag reducer provided by the invention is fluorinated acrylic ester-styrene-
Sulfonated phenylethylene block copolymerization has preferable compatibility with carbon dioxide；The drag reducer is dissolved in carbon dioxide pressure break
In liquid, the frictional resistance (including injection process and along the frictional resistance of journey) when pressure break can reduce, and then reduce ground pump pressure, reduce
The pressure-bearing of pipeline, makes that carbon dioxide dry method fracturing engineering is safer, pipeline is more able to satisfy job requirement, improves injection liquid dioxy
The speed for changing carbon is able to use carbon dioxide dry method pressure break in the reservoir of deeper, condition more extreme (such as high temperature and pressure),
And it is still able to maintain preferable drag-reduction effect under conditions of more extreme, drag-reduction effect can reach 30%- in fracturing work
40%；Therefore, drag reducer provided by the invention enables to carbon dioxide pressure break liquid to have the wider array of scope of application, more economically
Development effectiveness.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention
Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
Embodiment 1
The present embodiment provides a kind of carbon dioxide dry method pressure break drag reducer, whole components are fluorinated acrylic ester-benzene
Ethylene-sulfonated phenylethylene block copolymer, the copolymer is through the following steps that be prepared：
1, the preparation of fluorinated acrylate polymer：
(1) it is 50 that mass ratio is added in three-necked flask:28:22 deionized water, ethyl alcohol and concentration is the dense of 37wt%
Hydrochloric acid stirs evenly at room temperature；It is 41 by mass ratio:35:24 butyl methacrylate, isobornyl methacrylate and
In the mixed solvent of toluene and butyl acetate, (mass ratio of toluene and butyl acetate therein is 1 to methyl methacrylate:2) in
It is uniformly mixed and is used as mix monomer, be added in the three-necked flask for filling deionized water, ethyl alcohol and concentrated hydrochloric acid mixed liquor, add
Initiator azodiisobutyronitrile, and the additional amount of azodiisobutyronitrile is 0.05%, it is small in 75-80 DEG C of progress polymerization reaction 2
When, obtain the mixed liquor containing first polymer；
(2) dodecafluoroheptyl methacrylate is uniformly mixed with initiator azodiisobutyronitrile, 75-80 DEG C with
The speed of 0.05mL/s is added drop-wise in the three-necked flask for filling the mixed liquor containing first polymer, and it is anti-to continue polymerization
It answers and (i.e. end of reaction is added dropwise) 1.5 hours, obtain the crude product of fluorinated acrylate polymer；Wherein, methacrylic acid
The mass ratio of methyl methacrylate in ten difluoro heptyl esters and step (1) is 52:48, the azodiisobutyronitrile that this step uses
Additional amount be 0.08%；
(3) crude product of the fluorinated acrylate polymer is refined, obtains fluorinated acrylate polymer.
2, the preparation of sulfonated polystyrene：
Polystyrene is added in dichloroethanes and is made it completely dissolved in 60 DEG C of stirrings, polystyrene and dichloroethanes
Ratio be 1g:The concentrated sulfuric acid of concentration 98%, and the matter of the used concentrated sulfuric acid and polystyrene is added in 100mL after cooling
Amount is than being 90:10, it reacts 10 hours at 40 DEG C, then separates obtained sediment with liquid, then washed using distilled water
It washs, it is then 4 hours dry in 25 DEG C, obtain sulfonated polystyrene.
3, fluorinated acrylic ester-styrene-sulfonated phenylethylene block copolymer preparation：
(1) it is 63 that mass ratio is added in polymerization reaction kettle:25:12 deionized water, fluorinated acrylate polymer with
And styrene and be uniformly mixed, obtain mixed liquor：
(2) pH value of mixed liquor is adjusted using sodium hydroxide to 7-10, and sulfonated polystyrene and initiator is then added
Na2S2O8-Na2S2O3(mass ratio of the two is 65:35；The total additional amount of initiator is sulfonated polystyrene and styrene gross mass
0.09%), and the mass ratio for the sulfonated polystyrene and styrene being added be 70:30, it carries out polymerizeing at 75-80 DEG C anti-
It answers 1-2 hours, obtains fluorinated acrylic ester-styrene-sulfonated phenylethylene block copolymer.
Carbon dioxide dry method pressure break provided in this embodiment drag reducer is added in pure liquid carbon dioxide, additional amount is
60mg/L obtains the liquid carbon dioxide fracturing fluid containing drag reducer.
The liquid carbon dioxide fracturing fluid that this is contained drag reducer is used in fracturing process, and overall process is closed by liquid
CO2It is preserved on ground, CO is transported to after being pressurized2The feed liquor system of closed fracturing blender truck, and carry out more piece (at 12) point pressure, temperature
Degree monitoring finds that pipeline wellhead back pressure reduces 30-40 percentage points after construction.
Comparative example 1
(the Enhancement of the Viscosity of Carbon Dioxide Using such as Zhihua Huang
Styrene/Fluoroacrylate Copolymers.Macromolecules [J] .2000,33 (15)：5437-5442) close
At the copolymer of fluorinated acrylic ester and styrene to improve viscosity liquid carbon dioxide.Styrene is under using preceding progress vacuum
Distillation, HFDA are purified to remove inhibitor before use, and HFDA and styrol copolymer monomer are polymerize by ontological idea of freedom base
It obtains and uses AIBN as initiator.In inert N2Under the conditions of lower, the monomer HFDA of 5.18g is packed into 50mL vial
(0.01mol), the AIBN of styrene (4.0mmol) and 4.6mg of 0.42g.By vial sealing and water-bath under the conditions of 65 DEG C
12 hours, reaction mixture cooling is then dissolved in 1,1,2- trichorotrifluoroethane, then after polymer is precipitated in methyl alcohol
It washs and is dried, be finally made the copolymer of fluorinated acrylic ester and styrene.
In 295K, pressure tests the mixture of polymer and carbon dioxide under conditions of 6.70-48.28MPa
Test.Experiment show that the solubility of polymer is reduced with the increase of the styrene-content in polymer chain, miscible pressure with
Styrene-content must decline and decline, increase with the increase of molecular weight, these polymer improve about one times of titanium dioxide
The viscosity of carbon is 29%-71% for fluorine-containing molar fraction best in the styrene of thickening.
Zhihua Huang etc. synthesizes fluorinated acrylic ester and the copolymer of styrene uses AIBN (azodiisobutyronitrile)
As initiator, it will cause crystallization in the case that experiment condition is unstable, generate the problems such as reaction residue, and it has one
Fixed toxicity has certain harm to experimenter.And the preferred initiator of the present invention is Na2S2O8And Na2S2O3Combination, behaviour
Work is simple, side reaction is few, and two kinds of initiators, which are used in combination, occurs redox reactions, forms redox initiation system, aoxidizes
The OH that reduction reaction produces can capture the hydrogen on substance and form new free radical, so that fluorinated acrylic ester-styrene-
The polymerization effect of sulfonated phenylethylene block copolymer is more preferably.
Claims (10)
1. a kind of carbon dioxide dry method pressure break drag reducer, the drag reducer include：By fluorinated acrylate polymer, sulfonated polyphenyl
Fluorinated acrylic ester-styrene-sulfonated phenylethylene block copolymer that ethylene and styrene are prepared by polymerization reaction；
Wherein, the mass ratio of the fluorinated acrylate polymer, sulfonated polystyrene and styrene is (55-65):(20-
30):(10-20), preferably 60:25:15.
2. drag reducer according to claim 1, wherein the fluorinated acrylic ester-styrene-sulfonated phenylethylene block is total
Polymers is through the following steps that be prepared：
(1) suitable quantity of water, fluorinated acrylate polymer and styrene are mixed and stirred for uniformly, obtaining mixed liquor：
(2) pH value of the mixed liquor is adjusted to 7-10, and sulfonated polystyrene and initiator is then added, carries out at 75-80 DEG C
Polymerization reaction 1-2 hours, obtain fluorinated acrylic ester-styrene-sulfonated phenylethylene block copolymer.
3. drag reducer according to claim 2, wherein the initiator includes azodiisobutyronitrile, Na2S2O8With
Na2S2O3One or more of combination；
Preferably, in terms of the gross mass of fluorinated acrylate polymer, sulfonated polystyrene and styrene, the addition of initiator
Amount is 0.05%-0.08%, more preferably 0.05%-0.06%.
4. drag reducer according to claim 1 or 2, wherein the fluorinated acrylate polymer through the following steps that
It is prepared：First using butyl methacrylate, isobornyl methacrylate and methyl methacrylate as mix monomer
Polymerization reaction occurs, adds dodecafluoroheptyl methacrylate and continues that polymerization reaction occurs, the fluorination third is prepared
Olefine acid ester polymer；
Preferably, it is sent out using butyl methacrylate, isobornyl methacrylate and methyl methacrylate as mix monomer
The reaction temperature of raw polymerization reaction is 75-80 DEG C, and the reaction time is 1-3 hours, and dodecafluoroheptyl methacrylate is added later
The reaction temperature for continuing that polymerization reaction occurs is 75-80 DEG C, and the reaction time is 1-3 hours.
5. drag reducer according to claim 4, wherein the polymerization reaction is to carry out in the presence of an initiator
's；
Preferably, the initiator includes azodiisobutyronitrile, Na2S2O8And Na2S2O3One or more of combination；
Preferably, in terms of the gross mass of fluorinated acrylate polymer, sulfonated polystyrene and styrene, the addition of initiator
Amount is 0.05%-0.08%, more preferably 0.05%-0.06%.
6. drag reducer according to claim 5, wherein the butyl methacrylate, isobornyl methacrylate, first
The mass ratio of base methyl acrylate and dodecafluoroheptyl methacrylate is 40:10:25:25.
7. drag reducer according to claim 1 or 2, wherein the sulfonated polystyrene is through the following steps that be prepared into
It arrives：The organic solution of polystyrene is mixed and reacted with the concentrated sulfuric acid, the sulfonated polystyrene is prepared；
Preferably, the mass ratio of the polystyrene and the concentrated sulfuric acid is 90:10；
Preferably, the solvent in the organic solution of the polystyrene includes the mixed liquor of dichloroethanes or toluene and butanol；
It is highly preferred that the solvent is the mixed liquor of toluene and butanol, the mass ratio of the two is (30-40)：(60-70)；
Preferably, the organic solution of the polystyrene is by the way that polystyrene is added in solvent and is being no more than 60 DEG C
At a temperature of stirring make it completely dissolved and be prepared；
Preferably, the reaction temperature that the organic solution of the polystyrene is mixed and reacted with the concentrated sulfuric acid is no more than 40 DEG C, instead
It is 10 hours between seasonable.
8. drag reducer according to claim 1-7, through the following steps that preparation：
First using butyl methacrylate, isobornyl methacrylate and methyl methacrylate as mix monomer in 75-80
DEG C occur polymerization reaction 1-3 hour, add dodecafluoroheptyl methacrylate continue in 75-80 DEG C generation polymerization reaction 1-3
Hour, fluorinated acrylate polymer is prepared；Wherein, the butyl methacrylate, isobornyl methacrylate, first
The mass ratio of base methyl acrylate and dodecafluoroheptyl methacrylate is 40:10:25:25；By the organic solution of polystyrene
It is mixed with the concentrated sulfuric acid, is reacted 10 hours in 40 DEG C, sulfonated polystyrene is prepared；Wherein, the polystyrene and the concentrated sulfuric acid
Mass ratio be 90:10；
Suitable quantity of water, fluorinated acrylate polymer and styrene are mixed and stirred for uniformly, to obtain mixed liquor：It adjusts described mixed
The pH value of liquid is closed to 7-10, sulfonated polystyrene and initiator is then added, 75-80 DEG C progress polymerization reaction 1-2 hours, obtain
To fluorinated acrylic ester-styrene-sulfonated phenylethylene block copolymer；
Preferably, the initiator includes azodiisobutyronitrile, Na2S2O8And Na2S2O3One or more of combination；It is more excellent
It is selected as Na2S2O8And Na2S2O3Combination, the ratio of the two is preferably (60-70):(30-40)；
It is highly preferred that the total additional amount of initiator is the 0.08%-0.12% of sulfonated polystyrene and styrene gross mass.
9. the described in any item carbon dioxide dry method pressure breaks of claim 1-8 use drag reducer in carbon dioxide pressure break liquid as subtracting
The application of resist.
10. application according to claim 9, wherein the fluorinated acrylamide in the carbon dioxide dry method pressure break drag reducer
Additive amount of the acid esters-styrene-sulfonated phenylethylene block copolymer in the carbon dioxide pressure break liquid is 50-80mg/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111019627A (en) * | 2019-12-17 | 2020-04-17 | 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 |
| CN115873582A (en) * | 2022-12-27 | 2023-03-31 | 泰坦(天津)能源技术有限公司 | Composite carbon dioxide fracturing fluid and preparation method and application thereof |
-
2018
- 2018-07-09 CN CN201810743824.6A patent/CN108864387B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111019627A (en) * | 2019-12-17 | 2020-04-17 | 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 |
| 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 |
| CN115873582A (en) * | 2022-12-27 | 2023-03-31 | 泰坦(天津)能源技术有限公司 | Composite carbon dioxide fracturing fluid and preparation method and application thereof |
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