CN117510712A - Drag reducer for fracturing and preparation method thereof - Google Patents
Drag reducer for fracturing and preparation method thereof Download PDFInfo
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- CN117510712A CN117510712A CN202311612567.XA CN202311612567A CN117510712A CN 117510712 A CN117510712 A CN 117510712A CN 202311612567 A CN202311612567 A CN 202311612567A CN 117510712 A CN117510712 A CN 117510712A
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 72
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003999 initiator Substances 0.000 claims abstract description 25
- QUKRIOLKOHUUBM-UHFFFAOYSA-N 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl prop-2-enoate Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCOC(=O)C=C QUKRIOLKOHUUBM-UHFFFAOYSA-N 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- PPBAWVJOPQUAMY-UHFFFAOYSA-N 3-tris(trimethylsilyloxy)silylpropyl prop-2-enoate Chemical compound C[Si](C)(C)O[Si](O[Si](C)(C)C)(O[Si](C)(C)C)CCCOC(=O)C=C PPBAWVJOPQUAMY-UHFFFAOYSA-N 0.000 claims abstract description 16
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 14
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 14
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 14
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 14
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 14
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- 230000001105 regulatory effect Effects 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000337 buffer salt Substances 0.000 claims abstract description 8
- 238000010926 purge Methods 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 66
- 239000000243 solution Substances 0.000 claims description 34
- 150000003839 salts Chemical class 0.000 claims description 15
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 13
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 13
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 11
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 7
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 7
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 7
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 6
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 6
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 6
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 6
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 2
- JMGZBMRVDHKMKB-UHFFFAOYSA-L disodium;2-sulfobutanedioate Chemical compound [Na+].[Na+].OS(=O)(=O)C(C([O-])=O)CC([O-])=O JMGZBMRVDHKMKB-UHFFFAOYSA-L 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- KCXFHTAICRTXLI-UHFFFAOYSA-M propane-1-sulfonate Chemical compound CCCS([O-])(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-M 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000004321 preservation Methods 0.000 abstract description 12
- 239000000047 product Substances 0.000 abstract description 9
- 239000006227 byproduct Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000003208 petroleum Substances 0.000 abstract description 2
- -1 TX-10 Chemical compound 0.000 abstract 1
- 239000012530 fluid Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 11
- 239000007789 gas Substances 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 239000000839 emulsion Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000001965 increasing effect Effects 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 239000004094 surface-active agent Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Classifications
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/22—Esters containing halogen
- C08F220/24—Esters containing halogen containing perhaloalkyl radicals
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
Abstract
The invention belongs to the technical field of petroleum exploitation, and particularly relates to a drag reducer for fracturing and a preparation method thereof. The preparation method comprises the following steps: sequentially adding perfluorooctyl ethyl acrylate, (3-acryloyloxypropyl) tris (trimethylsiloxy) silane, 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonate, butenedioic acid, TX-10, MS-1, carboxymethyl cellulose, buffer salt and distilled water into a reaction kettle, and adjusting pH to 7-8; and (3) purging the reaction kettle and the pipeline with nitrogen, dropwise adding an initiator into the reaction kettle, heating, carrying out heat preservation reaction, continuing the reaction, then raising the temperature, carrying out heat preservation reaction, reducing the temperature to below 40 ℃, and regulating the pH value to 7-8 to obtain the drag reducer for fracturing products. The invention has the advantages of wide raw material sources, simple synthesis process and no byproducts; meanwhile, the invention has the characteristics of high apparent viscosity and high drag reduction rate.
Description
Technical Field
The invention belongs to the technical field of petroleum exploitation, and particularly relates to a drag reducer for fracturing and a preparation method thereof.
Background
With the rapid development of social progress and economy, the modern industry and the oil-gas engineering in life account for a considerable proportion. The unconventional oil and gas resource is deeply valued at home and abroad, shale gas and tight oil exploitation is becoming the weight of the oil and gas field exploitation, the fracturing technology is becoming the main stream reconstruction technology of unconventional oil and gas reservoirs, and is also the key technology for economic development of low-permeability and ultra-low-permeability oil and gas reservoirs, and the fracturing technology is commonly adopted in various oil fields at present, and is to utilize a ground high-pressure pump group to pump fracturing fluid into stratum with a displacement pump which greatly exceeds the stratum absorption capacity, fracture is pressed in stratum, and the fracture is extended so as to adjust the water absorption profile of a well to improve the recovery ratio.
After the fracturing fluid is pressurized by the high-pressure pump injection equipment, the fracturing fluid is pumped into the stratum at a high speed through the pipe column, the turbulence phenomenon of the fluid in the pipe flowing process is serious under the high-pressure and high-speed condition, and large friction resistance exists between the fracturing fluid and the pipe wall, so that the flow of the fluid in the pipeline is limited by the friction resistance of the fluid, the pipeline transmission capacity is reduced, and the energy loss is increased. Therefore, there is a need to reduce the effects of frictional resistance by adding drag reducers to the fluid, thereby improving the efficiency of construction.
The drag reducer is prepared by adding a small amount of high molecular polymer or surfactant into liquid, so that friction resistance is greatly reduced by influencing a turbulent flow structure when the liquid flows in a turbulent flow manner, and energy consumption and equipment requirements in the fracturing process are greatly reduced.
CN103694984a discloses a shale gas acidizing and fracturing drag reducer and a preparation method thereof, the drag reducer is prepared by an inverse emulsion method, a large amount of organic solvent is contained in the inverse emulsion, and the drag reducer of the fracturing fluid can cause pollution of underground water after being injected into a stratum, cause environmental injury and can not meet the requirement of environmental protection.
CN103013488A discloses a drag reducer applicable to slickwater fracturing fluid and a preparation method thereof, wherein an organic salt is added into an aqueous solution of acrylamide and functional monomers to prepare a water phase, the water phase is added into an oil phase system formed by a surfactant and base oil under high-speed stirring to form a stable W/O microemulsion system, nitrogen is introduced to drive oxygen, and an initiator is added to polymerize to form a long-chain structure without branching. The polymer micro emulsion is a transparent or semitransparent thermodynamic stable system, can be quickly swelled in water, can be directly used, and can improve the flow and reduce the energy consumption to a certain extent by adding a small amount of the drag reducer during fluid transportation, and compared with clear water, the drag reduction effect can reach 30-65%. The drag reducer has the characteristics of good stability, high dissolution speed, good dissolution performance, convenient use, remarkable drag reduction effect and the like, is suitable for the slickwater fracturing technology, is applied to field fracturing operation, and achieves good yield increasing effect. But the drag reduction rate of the drag reducer is only 30-60%, and the construction requirement cannot be met.
Disclosure of Invention
The invention provides a drag reducer for fracturing and a preparation method thereof, aiming at the defects of the prior art. The invention has the advantages of wide raw material sources, simple synthesis process and no byproducts; meanwhile, the invention has the characteristics of high apparent viscosity and high drag reduction rate.
In order to achieve the above object, one of the objects of the present invention is to disclose a drag reducer for fracturing, the molecular structural formula of which is as follows:
wherein:
a＝5000-50000；
b＝500-10000；
c＝250-5000；
d＝125-2500。
preferably, the drag reducer for fracturing has a viscosity-average molecular weight of 10000000-20000000.
The invention further discloses a preparation method of the drag reducer for fracturing, which comprises the following specific steps:
(1) Sequentially adding perfluorooctyl ethyl acrylate, (3-acryloyloxypropyl) tris (trimethylsiloxy) silane, 3- [ N, N-dimethyl- [2- (2-methylpropyl-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonate inner salt, butenedioic acid, TX-10 (nonylphenol polyoxyethylene ether), MS-1 (alkylphenol ether sulfosuccinate sodium salt), carboxymethyl cellulose, buffer salt and distilled water into a reaction kettle, stirring, adding a sodium hydroxide solution, and adjusting the pH to 7-8;
(2) The reaction kettle and the pipeline are purged by nitrogen for 3-5min, and the nitrogen atmosphere is maintained for the whole synthesis. Dropwise adding an initiator into the reaction kettle, heating to 50-55 ℃ after the dropwise adding is finished, keeping the temperature for reaction until the solution starts to become viscous, continuing the reaction for 20-30min, then heating to 80-85 ℃, keeping the temperature for reaction for 30-50min, cooling to below 40 ℃, and regulating the pH value to 7-8 by using a sodium hydroxide solution to obtain the drag reducer for fracturing products.
Preferably, the molar ratio of the (3-acryloxypropyl) tris (trimethylsiloxy) silane, 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, butenedioic acid and perfluorooctyl ethyl acrylate is 0.2-0.4:0.1-0.2:0.05-0.1:1.
preferably, the weight ratio of TX-10, MS-1, carboxymethyl cellulose, buffer salt, distilled water and perfluorooctyl ethyl acrylate in the step (1) is 0.2-0.4:0.1-0.2:0.2-0.4:0.1-0.2:6-8:1.
preferably, the buffer salt in the step (1) is one of potassium dihydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, ammonium dihydrogen phosphate and diammonium hydrogen phosphate.
More preferably, the buffer salt is one of potassium dihydrogen phosphate, dipotassium hydrogen phosphate and sodium dihydrogen phosphate.
Preferably, in the step (2), the initiator is a mixed solution of persulfate and sodium bisulfite, and the weight ratio of the initiator to perfluorooctyl ethyl acrylate is 0.2-0.5:1.
more preferably, the concentration of the persulfate is 8 to 10wt% and the concentration of the sodium bisulfite is 4 to 5wt%.
More preferably, the persulfate is one of potassium persulfate, ammonium persulfate and sodium persulfate.
The reaction equation for the synthesis of the drag reducer for fracturing is as follows:
the drag reducer for fracturing is a quaternary high polymer taking perfluorooctyl ethyl acrylate, (3-acryloxypropyl) tris (trimethylsiloxy) silane and 3- [ N, N-dimethyl- [2- (2-methylprop-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonate inner salt and butenedioic acid as monomers. Perfluoro octyl ethyl acrylate, (3-acryloyloxypropyl) tris (trimethylsiloxy) silane belongs to a special surfactant monomer, has low surface tension and interface tension which are incomparable with those of a common surfactant, and can greatly reduce friction resistance in the transportation process of fracturing fluid; 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonate belongs to an amphoteric surfactant monomer, and butenedioic acid can provide two carboxyl groups and belongs to an anionic surfactant monomer, so that the surface tension and the interfacial tension can be greatly reduced, and the friction resistance in the transportation process of the fracturing fluid can be reduced; TX-10 and MS-1 are nonionic and anionic emulsifying agents, and carboxymethyl cellulose belongs to emulsifying dispersing agents, so that the polymerization quality of products can be improved, the molecular weight and the uniformity degree can be improved, the viscosity of the products can be improved, and the drag reduction effect can be further enhanced.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The drag reducer for fracturing is synthesized into a one-pot method, raw materials are easy to obtain, byproducts are avoided, and the method is safe and environment-friendly;
(2) The drag reducer for fracturing has the characteristic of high apparent viscosity, and the apparent viscosity of 0.4 weight percent concentration reaches more than 100 mPa.s;
(3) The drag reducer for fracturing has a good drag reduction effect, and the drag reduction rate of 0.6wt% concentration reaches 75% or more.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments:
example 1
(1) 0.05mol of perfluorooctyl ethyl acrylate, 0.01mol of (3-acryloyloxypropyl) tris (trimethylsiloxy) silane, 0.01mol of 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, 0.005mol of butenedioic acid, 5.18g of TX-10, 4.66g of MS-1, 5.18g of carboxymethyl cellulose, 4.16g of potassium dihydrogen phosphate and 155.4g of distilled water are sequentially added into the reaction kettle, and a sodium hydroxide solution is added while stirring, so that the pH value is adjusted to 7-8;
(2) The reaction kettle and the pipeline are purged with nitrogen for 3min, and the nitrogen atmosphere is maintained for the whole synthesis. And (3) dropwise adding 5.18g of an initiator into the reaction kettle, wherein the initiator contains 10wt% of potassium persulfate and 4wt% of sodium bisulphite, heating to 50 ℃ after the dropwise addition is finished, carrying out heat preservation reaction until the solution starts to become viscous, continuing the reaction for 20min, then heating to 80 ℃, carrying out heat preservation reaction for 30min, cooling to below 40 ℃, and regulating the pH value to 7-8 by using a sodium hydroxide solution to obtain the drag reducer for fracturing.
Example 2
(1) 0.05mol of perfluorooctyl ethyl acrylate, 0.012mol of (3-acryloyloxypropyl) tris (trimethylsiloxy) silane, 0.009mol of 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, 0.005mol of butenedioic acid, 6.47g of TX-10, 2.59g of MS-1, 6.47g of carboxymethyl cellulose, 4.23g of potassium dihydrogen phosphate and 169g of distilled water are sequentially added into the reaction kettle, and a sodium hydroxide solution is added while stirring, so that the pH value is adjusted to 7-8;
(2) The reaction kettle and the pipeline are purged with nitrogen for 3min, and the nitrogen atmosphere is maintained for the whole synthesis. And (3) dropwise adding 6.27g of an initiator into the reaction kettle, wherein the initiator contains 8wt% of potassium persulfate and 5wt% of sodium bisulphite, heating to 55 ℃ after the dropwise addition is finished, carrying out heat preservation reaction until the solution starts to become sticky, continuing the reaction for 30min, then heating to 85 ℃, carrying out heat preservation reaction for 50min, cooling to below 40 ℃, and regulating the pH value to 7-8 by using a sodium hydroxide solution to obtain the drag reducer for fracturing.
Example 3
(1) 0.05mol of perfluorooctyl ethyl acrylate, 0.014mol of (3-acryloxypropyl) tris (trimethylsiloxy) silane, 0.008mol of 3- [ N, N-dimethyl- [2- (2-methylprop-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, 0.0045mol of butenedioic acid, 7.68g of TX-10, 3.77g of MS-1, 9.86g of carboxymethyl cellulose, 5.18g of dipotassium hydrogen phosphate and 182g of distilled water are sequentially added into the reaction kettle, and a sodium hydroxide solution is added while stirring, so that the pH value is adjusted to 7-8;
(2) The reaction kettle and the pipeline are purged with nitrogen for 5min, and the nitrogen atmosphere is maintained for the whole synthesis. 7.86g of initiator is dripped into the reaction kettle, the initiator contains 10wt% of potassium persulfate and 5wt% of sodium bisulphite, the temperature is heated to 50 ℃ after the dripping is finished, the reaction is kept at the temperature until the solution starts to become sticky, the reaction is continued for 25min, the temperature is then increased to 80 ℃, the reaction is kept at the temperature for 40min, the temperature is reduced to below 40 ℃, and the pH value is regulated to 7-8 by using sodium hydroxide solution, so that the drag reducer for fracturing of the product is obtained.
Example 4
(1) 0.05mol of perfluorooctyl ethyl acrylate, 0.016mol of (3-acryloxypropyl) tris (trimethylsiloxy) silane, 0.00758 mol of 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, 0.0045mol of butenedioic acid, 8.19g of TX-10, 4.58g of MS-1, 7.14g of carboxymethyl cellulose, 3.66g of potassium dihydrogen phosphate and 176g of distilled water are sequentially added into the reaction kettle, and a sodium hydroxide solution is added while stirring, so that the pH value is adjusted to 7-8;
(2) The reaction kettle and the pipeline are purged with nitrogen for 5min, and the nitrogen atmosphere is maintained for the whole synthesis. 9.27g of initiator is dripped into the reaction kettle, the initiator contains 9wt% of sodium persulfate and 4wt% of sodium bisulphite, the temperature is raised to 55 ℃ after the dripping is finished, the reaction is kept at the temperature until the solution starts to become sticky, the reaction is continued for 25min, the temperature is raised to 85 ℃, the reaction is kept at the temperature for 35min, the temperature is reduced to below 40 ℃, and the pH value is regulated to 7-8 by using sodium hydroxide solution, so that the drag reducer for fracturing of the product is obtained.
Example 5
(1) 0.05mol of perfluorooctyl ethyl acrylate, 0.016mol of (3-acryloyloxypropyl) tris (trimethylsiloxy) silane, 0.006mol of 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, 0.0045mol of butenedioic acid, 8.32g of TX-10, 5.18g of MS-1, 8.2g of carboxymethyl cellulose, 2.59g of sodium dihydrogen phosphate and 174g of distilled water are sequentially added into a reaction kettle, and a sodium hydroxide solution is added while stirring, so that the pH value is adjusted to 7-8;
(2) The reaction kettle and the pipeline are purged with nitrogen for 4min, and the nitrogen atmosphere is maintained for the whole synthesis. And (3) dropwise adding 8.14g of an initiator into the reaction kettle, wherein the initiator contains 10wt% of sodium persulfate and 4wt% of sodium bisulphite, heating to 52 ℃ after the dropwise addition is finished, carrying out heat preservation reaction until the solution starts to become viscous, continuing the reaction for 22min, then heating to 82 ℃, carrying out heat preservation reaction for 45min, cooling to below 40 ℃, and regulating the pH value to 7-8 by using a sodium hydroxide solution to obtain the drag reducer for fracturing.
Example 6
(1) 0.05mol of perfluorooctyl ethyl acrylate, 0.018mol of (3-acryloyloxypropyl) tris (trimethylsiloxy) silane, 0.006mol of 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, 0.0035mol of butenedioic acid, 9.58g of TX-10, 4.62g of MS-1, 10.1g of carboxymethyl cellulose, 3.44g of disodium hydrogen phosphate and 200g of distilled water are sequentially added into the reaction kettle, and a sodium hydroxide solution is added while stirring, so that the pH value is adjusted to 7-8;
(2) The reaction kettle and the pipeline are purged with nitrogen for 4min, and the nitrogen atmosphere is maintained for the whole synthesis. And (3) dropwise adding 12.95g of an initiator into the reaction kettle, wherein the initiator contains 8wt% of sodium persulfate and 4wt% of sodium bisulphite, heating to 53 ℃ after the dropwise addition is finished, carrying out heat preservation reaction until the solution becomes viscous, continuing the reaction for 26min, then heating to 81 ℃, carrying out heat preservation reaction for 32min, cooling to below 40 ℃, and regulating the pH value to 7-8 by using a sodium hydroxide solution to obtain the drag reducer for fracturing.
Example 7
(1) 0.05mol of perfluorooctyl ethyl acrylate, 0.018mol of (3-acryloxypropyl) tris (trimethylsiloxy) silane, 0.005mol of 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, 0.0035mol of butenedioic acid, 10.36g of TX-10, 5.18g of MS-1, 10.36g of carboxymethyl cellulose, 4.2g of ammonium dihydrogen phosphate and 207.2g of distilled water are sequentially added into the reaction kettle, and a sodium hydroxide solution is added while stirring, so that the pH value is adjusted to 7-8;
(2) The reaction kettle and the pipeline are purged with nitrogen for 3min, and the nitrogen atmosphere is maintained for the whole synthesis. 11.44g of initiator is dripped into the reaction kettle, the initiator contains 10wt% of ammonium persulfate and 5wt% of sodium bisulphite, the temperature is heated to 51 ℃ after the dripping is finished, the reaction is kept at the temperature until the solution starts to become viscous, the reaction is continued for 28min, the temperature is then increased to 82 ℃, the reaction is kept at the temperature for 40min, the temperature is reduced to below 40 ℃, and the pH value is regulated to 7-8 by using sodium hydroxide solution, so that the drag reducer for fracturing of the product is obtained.
Example 8
(1) 0.05mol of perfluorooctyl ethyl acrylate, 0.02mol of (3-acryloyloxypropyl) tris (trimethylsiloxy) silane, 0.005mol of 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, 0.003mol of butenedioic acid, 9.42g of TX-10, 4.9g of MS-1, 9.27g of carboxymethyl cellulose, 4.98g of diammonium hydrogen phosphate and 198g of distilled water are sequentially added into the reaction kettle, and a sodium hydroxide solution is added while stirring, so that the pH value is adjusted to 7-8;
(2) The reaction kettle and the pipeline are purged with nitrogen for 5min, and the nitrogen atmosphere is maintained for the whole synthesis. And (3) dropwise adding 10.28g of initiator into the reaction kettle, wherein the initiator contains 8wt% of ammonium persulfate and 5wt% of sodium bisulphite, heating to 54 ℃ after the dropwise addition is finished, performing heat preservation reaction until the solution starts to become viscous, continuing the reaction for 20min, then heating to 83 ℃, performing heat preservation reaction for 36min, cooling to below 40 ℃, and regulating the pH value to 7-8 by using a sodium hydroxide solution to obtain the drag reducer for fracturing products.
Example 9
(1) 0.05mol of perfluorooctyl ethyl acrylate, 0.02mol of (3-acryloyloxypropyl) tris (trimethylsiloxy) silane, 0.006mol of 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt, 0.0025mol of butenedioic acid, 8.55g of TX-10, 4.77g of MS-1, 8.49g of carboxymethyl cellulose, 4.18g of sodium dihydrogen phosphate and 184g of distilled water are sequentially added into the reaction kettle, and a sodium hydroxide solution is added while stirring, so that the pH value is adjusted to 7-8;
(2) The reaction kettle and the pipeline are purged with nitrogen for 4min, and the nitrogen atmosphere is maintained for the whole synthesis. 9.86g of initiator is dripped into the reaction kettle, the initiator contains 8wt% of ammonium persulfate and 5wt% of sodium bisulphite, the temperature is heated to 52 ℃ after the dripping is finished, the reaction is kept at the temperature until the solution starts to become viscous, the reaction is continued for 30min, the temperature is then increased to 84 ℃, the reaction is kept at the temperature for 43min, the temperature is reduced to below 40 ℃, and the pH value is regulated to 7-8 by using sodium hydroxide solution, so that the drag reducer for fracturing of the product is obtained.
Example 10 apparent viscosity test
The drag reducer for fracturing of the present invention (examples 1-9) was tested for apparent viscosity at a concentration of 0.4wt% with reference to SY/T6376-2008 "general technical Condition for fracturing fluids".
Apparent viscosity comparisons were made with Puyang, sea, source chemical industry Co., ltd, and the test results are shown in Table 1.
As can be seen from table 1: the apparent viscosity of the drag reducer for fracturing (examples 1-9) of the invention at a test concentration of 0.4wt% is greater than 100mPa.s and up to 128mPa.s, whereas the apparent viscosity of the emulsion drag reducer for fracturing of the invention at a comparative experiment Puyang city, source chemical industry, inc. is 53mPa.s, which is significantly lower than the invention.
Example 11 drag reduction rate test
The drag reduction rate of the invention is tested, the testing concentration is 0.2wt%, 0.4wt% and 0.6wt%, and the testing method refers to SY/T6376-2008 general technical Condition for fracturing fluids.
Drag reduction ratio comparison was performed with an emulsion drag reducer from source chemical industry Co., ltd. In Puyang, sea, and the test results are shown in Table 1.
TABLE 1 apparent viscosity, drag reduction test results
As can be seen from table 1:
(1) The drag reduction rate of the drag reducer for fracturing (examples 1-9) is more than or equal to 65% and is up to 70% when the test concentration is 0.2wt%, and the drag reduction rate of the emulsion drag reducer for the source chemical industry limited company of the Puyang city sea is compared to 55%, which is obviously lower than the drag reduction rate of the drag reducer for the fracturing;
(2) The drag reduction rate of the drag reducer for fracturing (examples 1-9) is more than 70% and up to 75% when the test concentration is 0.4wt%, and the drag reduction rate of the emulsion drag reducer for the source chemical industry limited company of the Puyang city sea is 59% in comparison, which is obviously lower than that of the drag reducer for fracturing;
(3) The drag reduction rates of the drag reducer for fracturing (examples 1-9) of the invention are all more than 75% and up to 80% at a test concentration of 0.6wt%, while the drag reduction rate of the emulsion drag reducer of the source chemical industry Co., ltd. In the comparative experimental Puyang city is 62%, which is significantly lower than the drag reduction rate of the invention.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (8)
1. The preparation method of the drag reducer for fracturing is characterized by comprising the following specific steps of:
(1) Sequentially adding perfluorooctyl ethyl acrylate, (3-acryloyloxypropyl) tris (trimethylsiloxy) silane, 3- [ N, N-dimethyl- [2- (2-methylpropyl-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonate inner salt, butenedioic acid, TX-10 (nonylphenol polyoxyethylene ether), MS-1 (alkylphenol ether sulfosuccinate sodium salt), carboxymethyl cellulose, buffer salt and distilled water into a reaction kettle, stirring, adding a sodium hydroxide solution, and adjusting the pH to 7-8;
(2) Purging the reaction kettle and the pipeline for 3-5min by nitrogen, and maintaining the nitrogen atmosphere in the whole synthesis; dropwise adding an initiator into a reaction kettle, heating to 50-55 ℃ after dropwise adding, keeping the temperature for reaction until the solution starts to become viscous, continuing to react for 20-30min, then heating to 80-85 ℃, keeping the temperature for reaction for 30-50min, cooling to below 40 ℃, and regulating the pH value to 7-8 by using a sodium hydroxide solution to obtain the drag reducer for fracturing the product;
the molar ratio of the (3-acryloyloxypropyl) tris (trimethylsiloxy) silane to the 3- [ N, N-dimethyl- [2- (2-methylpropan-2-enoyloxy) ethyl ] ammonium ] propane-1-sulfonic acid inner salt to the butenedioic acid to the perfluorooctyl ethyl acrylate is 0.2-0.4:0.1-0.2:0.05-0.1:1.
2. the method for producing drag reducer for fracturing according to claim 1, wherein the buffer salt in the step (1) is one of potassium dihydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, ammonium dihydrogen phosphate and diammonium hydrogen phosphate.
3. The method for preparing a drag reducer for fracturing according to claim 2, wherein the buffer salt is one of potassium dihydrogen phosphate, dipotassium hydrogen phosphate and sodium dihydrogen phosphate.
4. The method for preparing the drag reducer for fracturing according to claim 1, wherein in the step (2), the initiator is a mixed solution of persulfate and sodium bisulphite, and the weight ratio of the mixed solution to perfluorooctyl ethyl acrylate is 0.2-0.5:1.
5. the method for producing drag reducer for fracturing according to claim 4, wherein the concentration of persulfate is 8-10wt% and the concentration of sodium bisulphite is 4-5wt%.
6. The method for preparing a drag reducer for fracturing according to claim 1, wherein the persulfate is one of potassium persulfate, ammonium persulfate and sodium persulfate.
7. The drag reducer for fracturing is characterized by comprising the following molecular structural formula:
wherein:
a＝5000-50000；
b＝500-10000；
c＝250-5000；
d＝125-2500。
8. the drag reducer for fracturing of claim 7, wherein said drag reducer for fracturing has a viscosity-average molecular weight of 10000000-20000000.
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