CN103881693B - Inverse emulsion resistance reducing agent for fracturing of shale gas slickwater and preparation method thereof - Google Patents
Inverse emulsion resistance reducing agent for fracturing of shale gas slickwater and preparation method thereof Download PDFInfo
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- CN103881693B CN103881693B CN201410101052.8A CN201410101052A CN103881693B CN 103881693 B CN103881693 B CN 103881693B CN 201410101052 A CN201410101052 A CN 201410101052A CN 103881693 B CN103881693 B CN 103881693B
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 54
- 239000000839 emulsion Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000178 monomer Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims description 38
- 239000012071 phase Substances 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 21
- -1 azo diisobutyl amidine Chemical class 0.000 claims description 19
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 18
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 17
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 14
- 239000006184 cosolvent Substances 0.000 claims description 12
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 12
- 239000003995 emulsifying agent Substances 0.000 claims description 12
- 229920003169 water-soluble polymer Polymers 0.000 claims description 12
- 239000008346 aqueous phase Substances 0.000 claims description 11
- 239000003999 initiator Substances 0.000 claims description 11
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 10
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical group CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 10
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 claims description 10
- UWNADWZGEHDQAB-UHFFFAOYSA-N i-Pr2C2H4i-Pr2 Natural products CC(C)CCC(C)C UWNADWZGEHDQAB-UHFFFAOYSA-N 0.000 claims description 10
- 229940047670 sodium acrylate Drugs 0.000 claims description 10
- 235000010265 sodium sulphite Nutrition 0.000 claims description 9
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- CMXPERZAMAQXSF-UHFFFAOYSA-M sodium;1,4-bis(2-ethylhexoxy)-1,4-dioxobutane-2-sulfonate;1,8-dihydroxyanthracene-9,10-dione Chemical compound [Na+].O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=CC=C2O.CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC CMXPERZAMAQXSF-UHFFFAOYSA-M 0.000 claims description 7
- 238000007664 blowing Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 230000001804 emulsifying effect Effects 0.000 claims description 5
- 230000000813 microbial effect Effects 0.000 claims description 5
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- 235000011572 Pyrus ussuriensis Nutrition 0.000 claims 1
- 244000173166 Pyrus ussuriensis Species 0.000 claims 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims 1
- 150000001409 amidines Chemical class 0.000 claims 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims 1
- 238000010276 construction Methods 0.000 abstract description 12
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000012530 fluid Substances 0.000 abstract description 3
- 239000003208 petroleum Substances 0.000 abstract description 3
- 238000006073 displacement reaction Methods 0.000 abstract description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 238000002347 injection Methods 0.000 abstract description 2
- 239000007924 injection Substances 0.000 abstract description 2
- 238000012688 inverse emulsion polymerization Methods 0.000 abstract 1
- 238000010008 shearing Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000001802 infusion Methods 0.000 description 10
- 238000006116 polymerization reaction Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical class OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 3
- 238000006392 deoxygenation reaction Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 1
- 102400000830 Saposin-B Human genes 0.000 description 1
- 101800001697 Saposin-B Proteins 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000555 dodecyl gallate Substances 0.000 description 1
- 229940080643 dodecyl gallate Drugs 0.000 description 1
- 235000010386 dodecyl gallate Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 230000015784 hyperosmotic salinity response Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- PZNOBXVHZYGUEX-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine;hydrochloride Chemical compound Cl.C=CCNCC=C PZNOBXVHZYGUEX-UHFFFAOYSA-N 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- HSFQBFMEWSTNOW-UHFFFAOYSA-N sodium;carbanide Chemical class [CH3-].[Na+] HSFQBFMEWSTNOW-UHFFFAOYSA-N 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002888 zwitterionic surfactant Substances 0.000 description 1
Classifications
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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
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
-
- 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
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/665—Compositions based on water or polar solvents containing inorganic compounds
-
- 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
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/882—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses an inverse emulsion resistance reducer for shale gas slickwater fracturing fluid and a preparation method thereof, and relates to the technical field of petroleum engineering. The drag reducer introduces long-chain hydrophobic monomers, improves the shearing resistance of the drag reducer in the high-displacement pump injection process, is prepared by inverse emulsion polymerization, is liquid and instant, meets the liquid preparation requirement of the shale gas fracturing continuous blending construction process, is used in site with the addition of 0.06-0.8 percent of the mass of clear water, and has the drag reduction rate of 73 percent at most.
Description
Technical field
The present invention relates to petroleum works technical field, be specifically related to a kind of shale gas slippery water pressure break reversed-phase emulsion fall resistance
Agent and preparation method thereof.
Background technology
As the shale gas of unconventional petroleum resources, its reservoir reconstruction technique is very different with conventional gas and oil resource.For
The Fracture System linked up to greatest extent or open in reservoir, shale gas reservoir storey increase design uses big liquid measure, huge discharge pressure break
Technology.For shale gas storey increase design demand, reduce fracturing fluid fluid in pumping procedure because high infusion pressure influence occurs disorderly
The energy loss that stream causes, improves infusion discharge capacity and the liquid injection rate under identical infusion discharge capacity is particularly important.
Publication No. CN1487985A, publication date is that the Chinese patent literature on April 7th, 2004 discloses the work of a kind of surface
Property agent class friction reducer, relate to zwitterionic surfactant and ether sulfate or ether carboxylate surfactant package at water base body
As the application of drag reducer in system.But this kind of drag reducer needs to reach more than the critical micelle concentration of surfactant just can be made
With, concentration is high, is not suitable for shale gas low cost development demand.
Publication No. CN103333672A, publication date is that the Chinese patent literature on October 2nd, 2013 discloses by propylene
Amide and acrylic tri alkyl ammomium chloride or alkyl acryl amido tri alkyl ammomium chloride or dialkyl diallyl ammonium chloride water
The sodium salt friction reducer of application and shale gas reservoir that polymerisation in solution prepares, friction reducer prepared by the method is powder, and powder is inapplicable
In the extensive shale gas pressing crack construction using continuous mixture construction technology.
Publication No. CN102977877A, publication date is that the Chinese patent literature on March 20th, 2013 discloses by propylene
Shale gas pressure break drag reducer that amide, sodium acrylate and 2-acrylamide-2 methyl propane sulfonic acid sodium prepare and preparation method thereof,
The method needs to first pass through aqueous solution polymerization and prepares stabilizer, then prepares drag reducer by dispersin polymerization, simultaneously in preparation process
Nitrogen deoxygenation and preparation time length (total reaction time is at more than 20h), complex manufacturing need to be led to, be unfavorable for industrialized production,
This friction reducer solid content is low simultaneously, and dosage is bigger in use.
Summary of the invention
It is contemplated that for the defect existing for above-mentioned prior art and deficiency, it is provided that a kind of shale gas slippery water pressure break
Use reversed-phase emulsion friction reducer, use the present invention, improve the structural stability under high infusion discharge capacity and resistance-reducing performance, should simultaneously
Friction reducer is product emulsion, it is easy to dosing, it is adaptable to the extensive shale gas pressing crack construction of mixture construction technology continuously.
Meanwhile, present invention also offers the preparation method of shale gas slippery water pressure break reversed-phase emulsion friction reducer, the method
Employing super-concentrated inverse emulsion is polymerized, and aqueous phase accounts for system 70%～80%, and solid content is high, gained friction reducer under the conditions of low dosage just
Can reach good resistance reducing effect, when producing, one-step polymerization obtains product simultaneously, it is not necessary to logical nitrogen deoxygenation, production time section,
Greatly simplify production technology.
The present invention realizes by using following technical proposals:
A kind of shale gas slippery water pressure break reversed-phase emulsion friction reducer, it is characterised in that: by percentage to the quality, each component
Proportioning as follows:
High molecular weight water soluble polymer 30%～37.5%；
Non-polar solven 20%～25%；
Oil soluble emulsifying agent 2.5%～2.75%；
Cosolvent 0.2%～0.3%；
Remaining is water.
Described high molecular weight water soluble polymer is acrylamide, sodium acrylate and three kinds of monomers of lauryl methacrylate
Copolymer, in high molecular weight water soluble polymer, the mass percent of described acrylamide is 65%～70%, described third
The mass percent of olefin(e) acid sodium is 29%～33%；The mass percent of described water lauryl methacrylate is 1%～2%；Water
Initiator in soluble macromolecular polymer is azo diisobutyl amidine hydrochlorate and sodium sulfite composite initiator, wherein,
Azo diisobutyl amidine hydrochlorate accounts for the 0.1%～0.3% of described three kinds of monomer gross masses, and sodium sulfite accounts for described three kinds of monomers
The 0.1%～0.4% of gross mass.
Described non-polar solven is 15# white oil.
Described oil soluble emulsifying agent is sorbitan mono-oleic acid ester and SPAN85 compound emulsifying agent, wherein
The mass ratio of sorbitan mono-oleic acid ester and SPAN85 is 8～9:1～2.
Described cosolvent is sodium bicarbonate.
The preparation method of a kind of shale gas slippery water pressure break reversed-phase emulsion friction reducer, it is characterised in that step is as follows:
1) prepare acrylamide, sodium acrylate and three kinds of monomers of lauryl methacrylate, first will account for three kinds of total matter of monomer
The sodium acrylate of amount 23%～29% is soluble in water, adds and accounts for the acrylamide of three kinds of monomer gross masses 70%～75%, accounts for three kinds
Monomer gross mass 0.1%～0.3% initiator azo diisobutyl amidine hydrochlorate and account for prepared friction reducer gross mass 0.2%～
The cosolvent sodium bicarbonate of 0.3%, stirring and dissolving obtains aqueous phase solution；
2) in the 15# white oil accounting for prepared friction reducer gross mass 20%～25%, addition accounts for the total matter of prepared friction reducer
The emulsifier sorbitol acid anhydride monoleate of amount 2.5%～2.75% and SPAN85, wherein: sorbitan mono-oleic acid ester
It is 8～9:1～2 with the mass ratio of SPAN85；Add in described 15# white oil again and account for three kinds of monomer gross masses 1%
～the lauryl methacrylate of 2%, stirring obtains oil phase；
3) by above-mentioned 1) aqueous phase solution that obtains in step is added dropwise to above-mentioned 2 under continuous stirring state) step obtains
In oil phase, after dropping, emulsifying 30min obtains reversed-phase emulsion；
4) 15～25 DEG C, under continuous stirring state to above-mentioned 3) in the reversed-phase emulsion that obtains of step dropping account for three kinds of monomers
The aqueous solution of sodium bisulfite of gross mass 0.1%～0.4%, stops stirring after dropping and standing and reacting rises to system temperature
Start stirring when 35 DEG C, after being continuously stirring to when temperature no longer changes stop stirring and stand insulation 4 hours, be naturally cooling to ring
Blowing after the temperature of border, obtains reversed-phase emulsion friction reducer.
In described step 1), acrylamide performance prepared by acrylamide selection microbial method is more.
Compared with prior art, what the present invention was reached has the beneficial effect that:
1, " high molecular weight water soluble polymer 30%～37.5% is selected；Non-polar solven 20%～25%；Oil soluble emulsifying agent
2.5%～2.75%；Cosolvent 0.2%～0.3%；Remaining is water " friction reducer of the most specific proportioning, improve in high infusion discharge capacity
Under structural stability and resistance-reducing performance, this friction reducer is product emulsion simultaneously, it is easy to dosing, it is adaptable to continuously mixture construction work
The extensive shale gas pressing crack construction of skill
2, through overtesting, record this reversed-phase emulsion friction reducer when dissolving in water, can viscosify rapidly, solution apparent in 3min
Viscosity can reach stable viscosity more than 90%.Therefore, in shale gas massive hydraulic fracture transformation process, continuous compounding process can be used
Carrying out dosing construction, the friction reducer product of liquid directly can pump into manifold by metering with proportioning pump, reduces construction dosing greatly
Workload, improves efficiency of construction.
3, the reversed-phase emulsion friction reducer that the present invention provides have employed the lauryl methacrylate of chain hydrophobic is function list
Body, utilizes heat resistance and salt tolerance to enhance (5～16 m under the high infusion discharge capacity of friction reducer molecule pressing crack construction at the scene3/ min)
There is good molecular structure stabilized.
4, the reversed-phase emulsion friction reducer that the present invention provides only need to i.e. obtain product in process of production by one-step polymerization, and raw
Products application performance can be reached without being passed through nitrogen deoxygenation during product, the production time short (about 6h), greatly simplify life
Produce operation, reduce production cost.
5, the reversed-phase emulsion friction reducer fall dosage that the present invention provides is low, and resistance reducing effect is good, at the scene the smooth hydraulic pressure of shale gas
Splitting in construction, under the conditions of the friction reducer dosage of 0.05%～0.1%, its resistance-reducing yield is up to more than 70%.
6, providing following contrast experiment's data, illustrate in this preparation method the 4th with this) selection of the parameters of step is then
There is a specific reason:
| Comparative example | Reversed-phase emulsion Temperature (DEG C) | Aqueous solution of sodium bisulfite After dropping, start System temperature during stirring (DEG C) | When standing insulation Between (hour) | Comparing result |
| 1 | 15～25 | 35 | 4 | Steadily, product is placed stable in polymerization, fall resistance Rate is up to more than 70% |
| 2 | 25～30 | 35 | 4 | Steadily, product shelf-stability is poor in polymerization, Easily occur sudden and violent after blowing in 24 hours Gather and breakdown of emulsion caking |
| 3 | 15～25 | 25～30 | 4 | Steadily, product is put at non-lucifuge in polymerization Put poor stability, autohemagglutination caking in 2 days, Place stable at lucifuge, but resistance-reducing yield It is only about 30% |
| 4 | 15～25 | More than 40 | 4 | Early stage polymerization is steady, when temperature rises to 40 After more than DEG C, polymerization temperature climbing speed Drastically accelerate, then open agitator and cooling Water is also difficult to control to drastically going up of temperature Rising, material is sudden and violent coalescence knot in reactor Block |
| 5 | 15～25 | 35 | 1～3 | Steadily, product is put at non-lucifuge in polymerization There is autohemagglutination exothermic phenomenon when putting, but do not go out Existing breakdown of emulsion caking, places steady at lucifuge Fixed, resistance-reducing yield is about 50% |
Accompanying drawing explanation
Below in conjunction with specification drawings and specific embodiments, the present invention is described in further detail, wherein:
Fig. 1 is that the coiled tubing of 375m long internal diameter 25.4mm, 700 type fracturing unit truck infusions, 0.1% reversed-phase emulsion friction reducer add
Friction test curve chart under the conditions of amount.
Fig. 2 be under above-mentioned test condition friction reducer aqueous solution relative to clear water frictional resistance curve chart under different displacements.
Detailed description of the invention
Embodiment 1(is pressed 400kg and is produced)
Add 121.7kg clear water in reactor, add the anionic monomer acrylic acid of 30kg, add 16.7kg sodium hydroxide
And the sodium hydroxide solution of 25kg clear water preparation, regulation pH value, about 6.5, adds the non-ionic monomer microbial method of 98.5kg
Acrylamide, 0.3kg initiator azo diisobutyl amidine hydrochlorate and the cosolvent sodium bicarbonate of 1kg, stirring is to being completely dissolved
Obtain aqueous phase solution；The 15# white oil of 90kg adds 9kg sorbitan mono-oleic acid ester and 1kg SPAN85 and
The oil-soluble monomer lauryl methacrylate of 1.5kg, is uniformly mixing to obtain oil phase；By above-mentioned aqueous phase solution in continuous stirring
Being added dropwise in oil phase under state, after dropping, high speed emulsifying 30min obtains stable inverse emulsion system；Molten with 5kg clear water
Solve 0.3kg sodium sulfite, 20 DEG C, in inverse emulsion system obtained above, drip this sulfurous acid under continuous stirring state
Hydrogen sodium water solution, stops to stir standing and reacting to system temperature and rises to start stirring when 35 DEG C, be continuously stirring to temperature after dropping
Stop being naturally cooling to blowing after ambient temperature after stirring stands insulation 4 hours during degree no longer change, obtain homogeneous, stable anti-phase
Emulsion friction reducer.Take 10kg friction reducer and add 10m3In clear water (friction reducer mass percentage concentration is 0.1%), in using 375m length
The coiled tubing of footpath 25.4mm, with 700 type fracturing unit truck infusion friction reducer solution, records resistance-reducing yield up to 70.7%.
Embodiment 2(is pressed 400kg and is produced)
Add 121.6kg clear water in reactor, add the anionic monomer acrylic acid of 32kg, add 17.8kg sodium hydroxide
And the sodium hydroxide solution of 25kg clear water preparation, regulation pH value, about 6.5, adds the non-ionic monomer microbial method third of 96kg
Acrylamide, 0.15kg initiator azo diisobutyl amidine hydrochlorate and the cosolvent sodium bicarbonate of 1kg, stirring is to being completely dissolved
To aqueous phase solution；9kg sorbitan mono-oleic acid ester and 1kg SPAN85 and 2kg is added in the 15# white oil of 90kg
Oil-soluble monomer lauryl methacrylate, be uniformly mixing to obtain oil phase；By above-mentioned aqueous phase solution in continuous stirring state
Under be added dropwise in oil phase, after dropping, high speed emulsifying 30min obtains stable inverse emulsion system；Dissolve with 5kg clear water
0.45kg sodium sulfite, 20 DEG C, in inverse emulsion system obtained above, drip this sulfurous acid under continuous stirring state
Hydrogen sodium water solution, stops to stir standing and reacting to system temperature and rises to start stirring when 35 DEG C, be continuously stirring to temperature after dropping
Stop being naturally cooling to blowing after ambient temperature after stirring stands insulation 4 hours during degree no longer change, obtain homogeneous, stable anti-phase
Emulsion friction reducer.Take 10kg friction reducer and add 10m3In clear water (friction reducer mass percentage concentration is 0.1%), in using 375m length
The coiled tubing of footpath 25.4mm, with 700 type fracturing unit truck infusion friction reducer solution, records resistance-reducing yield up to 70.2%.
Embodiment 3(is pressed 400kg and is produced)
Add 116.6kg clear water in reactor, add the anionic monomer acrylic acid of 35kg, add 19.5kg sodium hydroxide
And the sodium hydroxide solution of 25kg clear water preparation, regulation pH value, about 6.5, adds the non-ionic monomer microbial method third of 95kg
Acrylamide, 0.3kg initiator azo diisobutyl amidine hydrochlorate and the cosolvent sodium bicarbonate of 1kg, stirring is to being completely dissolved
To aqueous phase solution；8.5kg sorbitan mono-oleic acid ester and 1.5kg SPAN85 is added in the 15# white oil of 90kg
And the oil-soluble monomer lauryl methacrylate of 2kg, it is uniformly mixing to obtain oil phase；By above-mentioned aqueous phase solution in continuous stirring
Being added dropwise in oil phase under state, after dropping, high speed emulsifying 30min obtains stable inverse emulsion system；Molten with 5kg clear water
Solve 0.6kg sodium sulfite, 20 DEG C, in inverse emulsion system obtained above, drip this sulfurous acid under continuous stirring state
Hydrogen sodium water solution, stops to stir standing and reacting to system temperature and rises to start stirring when 35 DEG C, be continuously stirring to temperature after dropping
Stop being naturally cooling to blowing after ambient temperature after stirring stands insulation 4 hours during degree no longer change, obtain homogeneous, stable anti-phase
Emulsion friction reducer.Take 10kg friction reducer and add 10m3In clear water (friction reducer mass percentage concentration is 0.1%), in using 375m length
The coiled tubing of footpath 25.4mm, with 700 type fracturing unit truck infusion friction reducer solution, records resistance-reducing yield up to 68.7%.
Embodiment 4
As a better embodiment of the present invention, its shale gas slippery water pressure break reversed-phase emulsion friction reducer, with quality
Percentages, the proportioning of each component is as follows: high molecular weight water soluble polymer 35%；Non-polar solven 23%；Oil soluble emulsifying agent
2.5%；Cosolvent 0.25%；Remaining is water.Described high molecular weight water soluble polymer is acrylamide, sodium acrylate and methyl-prop
The copolymer of three kinds of monomers of alkene dodecyl gallate, in high molecular weight water soluble polymer, the mass percent of described acrylamide
Being 70%, the mass percent of described sodium acrylate is 29%；The mass percent of described water lauryl methacrylate is
1%；Initiator in high molecular weight water soluble polymer is azo diisobutyl amidine hydrochlorate and sodium sulfite composite initiator,
Wherein, azo diisobutyl amidine hydrochlorate accounts for the 0.2% of described three kinds of monomer gross masses, and sodium sulfite accounts for described three kinds of monomers
The 0.3% of gross mass.Described non-polar solven is 15# white oil.Described oil soluble emulsifying agent be sorbitan mono-oleic acid ester and
SPAN85 compound emulsifying agent, wherein the mass ratio of sorbitan mono-oleic acid ester and SPAN85 is 8
～9:1～2.Described cosolvent is sodium bicarbonate.
Claims (3)
1. a shale gas slippery water pressure break reversed-phase emulsion friction reducer, it is characterised in that: by percentage to the quality, each component
Proportioning is as follows:
High molecular weight water soluble polymer 30%～37.5%；
Non-polar solven 20%～25%；
Oil soluble emulsifying agent 2.5%～2.75%；
Cosolvent 0.2%～0.3%；
Remaining is water；
High molecular weight water soluble polymer is acrylamide, sodium acrylate and the copolymer of three kinds of monomers of lauryl methacrylate,
In high molecular weight water soluble polymer, the mass percent of described acrylamide is 65%～70%, described sodium acrylate
Mass percent is 29%～33%；The mass percent of described lauryl methacrylate is 1%～2%；Water soluble polymer
Initiator in polymer is azo diisobutyl amidine hydrochlorate and sodium sulfite composite initiator, wherein, azo two isobutyl
Base amidine hydrochlorate accounts for the 0.1%～0.3% of described three kinds of monomer gross masses, and sodium sulfite accounts for described three kinds of monomer gross masses
0.1%～0.4%；
Described non-polar solven is 15# white oil；
Described oil soluble emulsifying agent is sorbitan mono-oleic acid ester and SPAN85 compound emulsifying agent, wherein Pyrusussuriensis
The mass ratio of alcohol acid anhydride monoleate and SPAN85 is 8～9:1～2；
Described cosolvent is sodium bicarbonate.
2. the shale gas slippery water pressure break preparation method of reversed-phase emulsion friction reducer, it is characterised in that step is as follows:
1) prepare acrylamide, sodium acrylate and three kinds of monomers of lauryl methacrylate, first will account for three kinds of monomer gross masses 23%
～the sodium acrylate of 29% is soluble in water, adds and account for the acrylamide of three kinds of monomer gross masses 70%～75%, to account for three kinds of monomers total
Quality 0.1%～0.3% initiator azo diisobutyl amidine hydrochlorate and account for prepared friction reducer gross mass 0.2%～0.3%
Cosolvent sodium bicarbonate, stirring and dissolving obtains aqueous phase solution；
2) in the 15# white oil accounting for prepared friction reducer gross mass 20%～25%, addition accounts for prepared friction reducer gross mass
The emulsifier sorbitol acid anhydride monoleate of 2.5%～2.75% and SPAN85, wherein: sorbitan mono-oleic acid ester and
The mass ratio of SPAN85 is 8～9:1～2；Again in described 15# white oil add account for three kinds of monomer gross masses 1%～
The lauryl methacrylate of 2%, stirring obtains oil phase；
3) by above-mentioned 1) aqueous phase solution that obtains in step is added dropwise to above-mentioned 2 under continuous stirring state) oil phase that obtains of step
In, after dropping, emulsifying 30min obtains reversed-phase emulsion；
4) 15～25 DEG C, under continuous stirring state to above-mentioned 3) in the reversed-phase emulsion that obtains of step dropping account for three kinds of total matter of monomer
The aqueous solution of sodium bisulfite of amount 0.1%～0.4%, stops stirring after dropping and standing and reacting to system temperature rises to 35 DEG C
Shi Qidong stirs, and after being continuously stirring to when temperature no longer changes stop stirring and stand insulation 4 hours, is naturally cooling to environment temperature
Blowing after degree, obtains reversed-phase emulsion friction reducer.
The preparation method of shale gas slippery water pressure break reversed-phase emulsion friction reducer the most according to claim 2, its feature exists
In: in described step 1), acrylamide is acrylamide prepared by microbial method.
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| MX2017000553A (en) * | 2014-07-15 | 2017-07-04 | Solvay Usa Inc | Salt tolerant friction reducer. |
| CN105384868B (en) * | 2014-09-05 | 2018-03-02 | 中国石油化工股份有限公司 | Preparation method and pressure break drag reducer of the pressure break with drag reducing agent composition and pressure break with drag reducer |
| EP3262136B1 (en) * | 2015-02-27 | 2020-11-11 | Solvay USA Inc. | Viscosifying friction reducers |
| CN104744630B (en) * | 2015-03-26 | 2017-07-07 | 长江大学 | A kind of hydrophobically modified oil base reversed-phase emulsion Low Damage hydraulic fracturing drag reducer |
| CN105418840B (en) * | 2015-12-04 | 2017-03-08 | 中国石油大学(华东) | Preparation method of hydrophobically associating polymer inverse emulsion |
| CN109135687A (en) * | 2018-08-01 | 2019-01-04 | 四川省威沃敦化工有限公司 | A kind of shale gas fracturing fluid Instant suspension salt resistance friction reducer and preparation method thereof |
| CN109265605B (en) * | 2018-11-26 | 2020-12-04 | 西南石油大学 | Low-adsorption salt-resistant resistance-reducing agent suitable for shale reservoir fracturing transformation |
| CN111763511B (en) * | 2020-06-28 | 2021-07-06 | 中国石油集团长城钻探工程有限公司压裂公司 | Preparation and liquid preparation method of integrated self-crosslinking thickener modified polymer for fracturing |
| CN111748332A (en) * | 2020-07-16 | 2020-10-09 | 陕西万朗石油工程技术服务有限公司 | Multifunctional online emulsified self-crosslinking fracturing fluid and preparation method thereof |
| CN112029491A (en) * | 2020-09-15 | 2020-12-04 | 郑州德融科技有限公司 | Drag reducer for fracturing and production process thereof |
| CN116200183B (en) * | 2023-03-02 | 2024-05-28 | 四川申和新材料科技有限公司 | High-efficiency variable-viscosity fracturing fluid for deep coal bed gas development and integrated construction method |
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