CN115477934B - Reusable scale inhibition fracturing fluid and preparation method thereof - Google Patents
Reusable scale inhibition fracturing fluid and preparation method thereof Download PDFInfo
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- CN115477934B CN115477934B CN202110600351.6A CN202110600351A CN115477934B CN 115477934 B CN115477934 B CN 115477934B CN 202110600351 A CN202110600351 A CN 202110600351A CN 115477934 B CN115477934 B CN 115477934B
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- 239000012530 fluid Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000005764 inhibitory process Effects 0.000 title description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000002105 nanoparticle Substances 0.000 claims abstract description 47
- 230000002401 inhibitory effect Effects 0.000 claims abstract description 37
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 37
- 239000002455 scale inhibitor Substances 0.000 claims abstract description 37
- 239000007762 w/o emulsion Substances 0.000 claims abstract description 36
- 239000000654 additive Substances 0.000 claims abstract description 34
- 230000000996 additive effect Effects 0.000 claims abstract description 30
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 23
- 239000004927 clay Substances 0.000 claims abstract description 16
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 14
- 239000003899 bactericide agent Substances 0.000 claims abstract description 13
- 239000003381 stabilizer Substances 0.000 claims abstract description 12
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229940120146 EDTMP Drugs 0.000 claims abstract description 10
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims abstract description 10
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 48
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 38
- 239000000377 silicon dioxide Substances 0.000 claims description 22
- 239000001103 potassium chloride Substances 0.000 claims description 19
- 235000011164 potassium chloride Nutrition 0.000 claims description 19
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 230000001804 emulsifying effect Effects 0.000 claims description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 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
- 239000000839 emulsion Substances 0.000 claims description 10
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- 239000002245 particle Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
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- 238000000034 method Methods 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 5
- 239000005662 Paraffin oil Substances 0.000 claims description 5
- 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 5
- 239000004147 Sorbitan trioleate Substances 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229960000391 sorbitan trioleate Drugs 0.000 claims description 5
- 235000019337 sorbitan trioleate Nutrition 0.000 claims description 5
- TZYULTYGSBAILI-UHFFFAOYSA-M trimethyl(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC=C TZYULTYGSBAILI-UHFFFAOYSA-M 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 4
- 235000019743 Choline chloride Nutrition 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 4
- 229960003178 choline chloride Drugs 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- YIEDHPBKGZGLIK-UHFFFAOYSA-L tetrakis(hydroxymethyl)phosphanium;sulfate Chemical compound [O-]S([O-])(=O)=O.OC[P+](CO)(CO)CO.OC[P+](CO)(CO)CO YIEDHPBKGZGLIK-UHFFFAOYSA-L 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 12
- 230000009467 reduction Effects 0.000 abstract description 11
- 238000001556 precipitation Methods 0.000 abstract description 6
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- 238000004064 recycling Methods 0.000 abstract description 2
- 239000002562 thickening agent Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
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- 241000894006 Bacteria Species 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 230000033558 biomineral tissue development Effects 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 239000008398 formation water Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 241000295146 Gallionellaceae Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000009920 chelation Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 230000006870 function Effects 0.000 description 2
- 230000015784 hyperosmotic salinity response Effects 0.000 description 2
- 238000005213 imbibition Methods 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000003129 oil well Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
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- 230000008961 swelling Effects 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 244000007835 Cyamopsis tetragonoloba Species 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- -1 hydroxypropyl Chemical group 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 239000011591 potassium Substances 0.000 description 1
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- 150000003839 salts Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
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Classifications
-
- 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
- C09K8/84—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
Abstract
The invention provides a recyclable scale-inhibiting fracturing fluid and a preparation method thereof, wherein the preparation raw materials comprise 0.06-0.20% of drag reducer by weight percent; 0.15 to 0.4 percent of cleanup additive; 0.1 to 0.2 percent of bactericide; clay stabilizer in 0.2-0.4 wt%; 0.05 to 0.15% hydrophilic nanoparticles; 0.03 to 0.05 percent of scale inhibitor; the balance being water; wherein the drag reducer is water-in-oil emulsion type zwitterionic polyacrylamide, and the scale inhibitor consists of amino trimethylene phosphonic acid, hydroxy ethylidene diphosphonic acid and ethylenediamine tetramethylene phosphonic acid. According to the invention, by developing a novel drag reducer, by compounding other additives, the generation of precipitation after fluid is retained in the reservoir is inhibited, and by changing the concentration of the thickening agent, the function of a liquid system is switched between sand carrying and renting reduction, so that the low cost, low friction resistance, low harm construction and recycling of flowback fluid of a compact oil-gas reservoir are realized.
Description
Technical Field
The invention belongs to the technical field of oilfield exploitation chemicals, and particularly relates to a recyclable scale-inhibiting fracturing fluid and a preparation method thereof.
Background
The fracturing fluid is a working fluid used for fracturing modification of an oil-gas layer, and has the main functions of injecting the fracturing fluid with certain viscosity into an oil layer by utilizing the principle of liquid pressure transmission, gradually increasing the pressure in a shaft, so that the stratum is broken to form cracks and propping agents are conveyed along the cracks. Slickwater fracturing fluids have been widely used in the development of unconventional tight hydrocarbon reservoirs, and chemical additives for slickwater fracturing fluids typically include friction reducers, clay stabilizers, cleanup additives, and the like.
Currently, 98.0 to 99.5 percent of the slick water fracturing fluid system is sand mixing water, and the resistance reducing agent is a core additive of the system, wherein the polyacrylamide type resistance reducing agent in the synthetic polymer is a main flow resistance reducing agent for domestic and foreign slick water fracturing fluids, but the resistance reducing performance in the slick water prepared by the flowback fluid is seriously influenced due to poor mineralization resistance; in addition, with the large-scale application of the fracturing transformation process of the volume of the tight reservoir, the liquid inflow amount is continuously increased, a large amount of fracturing liquid is lost after fracturing to stay in the reservoir, precipitation is generated and bacteria are bred due to the change of factors such as pH value, ion concentration and environmental temperature after stratum water is encountered, and reservoir damage is caused, so that the development of the scale-inhibiting fracturing liquid capable of being recycled is particularly important.
Disclosure of Invention
In order to solve the problems and the defects in the prior art, the invention provides a recyclable scale-inhibiting fracturing fluid and a preparation method thereof.
The invention is realized by the following technical scheme:
the reusable scale-inhibiting fracturing fluid comprises the following components in percentage by weight: 0.06-0.20% of drag reducer, 0.15-0.4% of cleanup additive, 0.1-0.2% of bactericide, 0.2-0.4% of clay stabilizer, 0.05-0.15% of hydrophilic nano particles, 0.03-0.05% of scale inhibitor and the balance of water.
Further, the drag reducer is water-in-oil emulsion type zwitterionic polyacrylamide.
As a further preferable technical scheme, the preparation method of the water-in-oil emulsion type zwitterionic polyacrylamide comprises the following steps:
s1, adding 40-60 parts of water into 1-5 parts of acrylic acid according to parts by weight, neutralizing to pH=7 by using sodium hydroxide, and adding 10-20 parts of acrylamide and 1-5 parts of allyl trimethyl ammonium chloride to prepare a water phase;
s2, adding 1-5 parts of sorbitan trioleate into 70-100 parts of paraffin oil according to parts by weight to prepare an oil phase;
s3, placing the oil phase into a high-speed emulsifying machine with the rotating speed of 4000-7000 rpm, starting the emulsifying machine, then adding the water phase, and emulsifying for 30 minutes to prepare monomer emulsion;
s4, introducing nitrogen into 100 parts of monomer emulsion for 20min, stirring for 5-6 h at the temperature of 30-40 ℃, then adding 0.004-0.007 part of ammonium persulfate, stirring for 2-3 h at the temperature of 50-60 ℃, and cooling to room temperature to obtain the water-in-oil emulsion type zwitterionic polyacrylamide.
Further, the cleanup additive is prepared from 2 to 6 parts by weight of alkyl polyglycoside, 10 to 20 parts by weight of ethanol and 60 to 80 parts by weight of water.
Further, the bactericide is one or a mixture of more than one of glutaraldehyde, formaldehyde and tetrakis (hydroxymethyl) phosphonium sulfate in any proportion.
As a further preferable technical scheme, the clay stabilizer is one or a mixture of a plurality of potassium chloride, ammonium chloride and choline chloride in any proportion.
As a further preferable technical scheme, the hydrophilic nanoparticle is one or a mixture of several of hydrophilic silica nanoparticle, hydrophilic titanium dioxide nanoparticle, hydrophilic magnesium oxide nanoparticle and hydrophilic zinc oxide nanoparticle in any proportion.
As a further preferable embodiment, the hydrophilic nanoparticles have an average particle diameter of 50 to 100nm.
Further, the scale inhibitor is formed by mixing amino trimethylene phosphonic acid, hydroxy ethylidene diphosphonic acid and ethylenediamine tetramethylene phosphonic acid.
As a further preferable technical scheme, the weight ratio of the amino trimethylene phosphonic acid, the hydroxy ethylidene diphosphonic acid and the ethylenediamine tetramethylene phosphonic acid is (0.8-1.2): (1-1.5): 1.
a preparation method of a recyclable scale-inhibiting fracturing fluid comprises the following specific operation steps: sequentially adding a drag reducer, a cleanup additive, a bactericide, a clay stabilizer, hydrophilic nano particles and a scale inhibitor into water according to the formula amount; and each reagent is added to the next reagent after being stirred uniformly in the container.
By adopting the technical scheme, the invention has the following beneficial effects:
1. the water-in-oil emulsion type zwitterionic polyacrylamide prepared by the invention is used as a drag reducer, so that the excellent drag reduction effect of anions is ensured, and the construction pressure during large-displacement fracturing operation is effectively reduced; the cationic group can obviously enhance the salt tolerance of the fracturing flowback fluid and realize the good performance of the fracturing flowback fluid and the sand carrying fluid.
2. The cleanup additive is prepared from alkyl polyglycoside, ethanol and water, has good solubility and dispersibility, and ensures that the fracturing fluid is discharged back to the ground as much as possible after the fracturing fluid plays a role.
3. The hydrophilic nano particles adopted by the invention can change the wettability of a reservoir, improve the stratum permeability, and drive by capillary force, so that the slickwater fracturing fluid entering a well can enter a fine pore canal of matrix rock through spontaneous imbibition after gel breaking, and crude oil is gradually gathered into a large pore canal and a fracturing main crack by utilizing oil-water displacement, thereby realizing the dual purposes of supplementing stratum energy and improving the oil well yield.
4. The addition of the scale inhibitor can prevent the precipitation of insoluble inorganic salt, because the scale inhibitor is prepared from amino trimethylene phosphonic acid, hydroxy ethylidene diphosphonic acid and ethylenediamine tetramethylene phosphonic acid, has higher stability, acid and alkali resistance and chlorine oxidation resistance, has strong chelation to Ca, mg and Fe and has good scale inhibition effect.
5. The existence of hydrophilic nano particles of silicon dioxide, titanium dioxide, magnesium oxide and zinc oxide in the fracturing fluid can also inhibit the formation of sediment in formation water, thereby improving the scale inhibition capability of the fracturing fluid. The silicon dioxide and titanium dioxide hydrophilic nano particles can be combined with the hydrophilic end of the water-in-oil emulsion type amphoteric ion polyacrylamide, so that the drag reduction effect of the drag reducer is improved.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention will be further described with reference to the preferred embodiments.
Detailed Description
The disclosure of the present invention will be further understood in conjunction with the following detailed description of the preferred embodiments of the invention, including examples. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If the definition of a particular term disclosed in the prior art is inconsistent with any definition provided in the present invention, the definition of the term provided in the present invention controls.
It should be noted that the implementation conditions used in the examples may be further adjusted according to the specific experimental environment, and the implementation conditions that are not noted are generally conditions in the conventional experiments. The preparation methods mentioned in the present invention are all conventional methods unless otherwise specified.
According to the reconstruction requirement of a compact oil and gas reservoir and the problems existing in the current slick water fracturing fluid system, the invention firstly provides a reusable scale inhibition type fracturing fluid, which comprises the following components in percentage by weight: 0.06-0.20% of drag reducer, 0.15-0.4% of cleanup additive, 0.1-0.2% of bactericide, 0.2-0.4% of clay stabilizer, 0.05-0.15% of hydrophilic nano particles, 0.03-0.05% of scale inhibitor and the balance of water.
The drag reducer can reduce friction force of the fracturing fluid and improve rheological property of the fracturing fluid, in some preferred embodiments, the drag reducer is water-in-oil emulsion type zwitterionic polyacrylamide, so that not only is excellent drag reduction effect of the water-in-oil emulsion type zwitterionic polyacrylamide maintained, but also effective power of joint making is improved, and the salt tolerance and compatibility of the fracturing fluid can be obviously enhanced by cationic groups, so that good effects on sand carrying performance and flowback performance of the recovered fracturing fluid are achieved, the fracturing fluid can be reused, and cost is reduced. In addition, the water-in-oil emulsion type zwitterionic polyacrylamide has better compatibility, and can be cooperated with hydrophilic nano particles to improve the wettability of a reservoir.
Further, the preparation method of the water-in-oil emulsion type zwitterionic polyacrylamide comprises the following steps:
s1, adding 40-60 parts of water into 1-5 parts of acrylic acid according to parts by weight, neutralizing to pH=7 by using sodium hydroxide, and adding 10-20 parts of acrylamide and 1-5 parts of allyl trimethyl ammonium chloride to prepare a water phase;
s2, adding 1-5 parts of sorbitan trioleate into 70-100 parts of paraffin oil according to parts by weight to prepare an oil phase;
s3, placing the oil phase into a high-speed emulsifying machine with the rotating speed of 4000-7000 rpm, starting the emulsifying machine, then adding the water phase, and emulsifying for 30 minutes to prepare monomer emulsion;
s4, introducing nitrogen into 100 parts of monomer emulsion for 20min, stirring for 5-6 h at the temperature of 30-40 ℃, then adding 0.004-0.007 part of ammonium persulfate, stirring for 2-3 h at the temperature of 50-60 ℃, and cooling to room temperature to obtain the water-in-oil emulsion type zwitterionic polyacrylamide.
The cleanup additive can help the working fracturing fluid to return to the ground as much as possible, and in some preferred embodiments, the cleanup additive is prepared from 2-6 parts of alkyl polyglycoside, 10-20 parts of ethanol and 60-80 parts of water according to parts by weight, and has the advantages of simple and convenient preparation, low cost, better solubility and dispersibility, improved cleanup efficiency and reduced damage to a reservoir to the greatest extent.
The bactericide is used for killing bacteria in the rock stratum, and in some preferred embodiments, the bactericide is one or a mixture of a plurality of glutaraldehyde, formaldehyde and tetrakis (hydroxymethyl) phosphonium sulfate in any proportion, so that the bactericide has good bactericidal effect, and can prevent bacteria in a reservoir from growing and prevent polymer degradation. The combination of the scale inhibitor and the sulfate reducing bacteria has better inhibition effect on sulfate reducing bacteria and iron bacteria. In addition, the generation of sediment in the formation water can be inhibited.
The clay stabilizer can be adsorbed on the clay surface to prevent the clay from swelling and migration. In some preferred embodiments, the clay stabilizer is one or a mixture of several of potassium chloride, ammonium chloride and choline chloride in any proportion, chloride ions can improve the scale inhibition capability of the fracturing fluid, cations can enter hexagonal spaces of silicon oxygen tetrahedra of clay to prevent the clay from swelling, dispersing and transporting, and the addition of one or a mixture of several of potassium chloride, ammonium chloride and choline chloride can also improve the mineralization of the fracturing fluid to be matched with the mineralization of stratum water.
In order to increase formation permeability to increase well production, in some preferred embodiments, one or a mixture of any proportion of hydrophilic silica nanoparticles, hydrophilic titania nanoparticles, hydrophilic magnesia nanoparticles, and hydrophilic zinc oxide nanoparticles is added. When hydrophilic nano particles are uniformly and dispersedly distributed in the fracturing fluid, the wettability of a reservoir layer can be changed, the stratum permeability is improved, the fracturing fluid entering a well can enter fine pore channels of matrix rock through spontaneous imbibition after gel breaking, crude oil is gradually gathered into large pore channels and a fracturing main crack by utilizing oil-water displacement, and therefore the dual purposes of supplementing stratum energy and improving oil well yield are achieved. The existence of hydrophilic nano particles of silicon dioxide, titanium dioxide, magnesium oxide and zinc oxide in the fracturing fluid can also inhibit the formation of sediment in formation water, thereby improving the scale inhibition capability of the fracturing fluid. The silicon dioxide and titanium dioxide hydrophilic nano particles can be combined with the hydrophilic end of the water-in-oil emulsion type amphoteric ion polyacrylamide, so that the drag reduction effect of the drag reducer is improved.
In some more preferred embodiments, the hydrophilic nanoparticles have an average particle size of 50-100 nm, and if the particle size is less than 50nm, the hydrophilic nanoparticles are easy to agglomerate and difficult to uniformly disperse, and the performance of the fracturing fluid is affected. If the particle diameter is larger than 100nm, the ability to improve wettability decreases.
The addition of the scale inhibitor can prevent precipitation of sparingly soluble inorganic salts, and in some preferred embodiments consists of aminotrimethylene phosphonic acid, hydroxyethylidene diphosphonic acid, ethylenediamine tetramethylene phosphonic acid, and in some more preferred embodiments, aminotrimethylene phosphonic acid, hydroxyethylidene diphosphonic acid, ethylenediamine tetramethylene phosphonic acid in an amount of (0.8 to 1.2): (1-1.5): the scale inhibitor is prepared according to the weight ratio of 1, so that the scale inhibitor has higher stability, acid and alkali resistance and chlorine oxidation resistance, has strong chelation to Ca, mg and Fe, has good scale inhibition effect, reduces the influence of indissolvable inorganic salt on a drag reducer (water-in-oil emulsion type zwitterionic polyacrylamide), and can inhibit the growth of bacteria.
The invention also provides a preparation method of the recyclable scale-inhibiting fracturing fluid, which comprises the following specific operation steps: sequentially adding a drag reducer, a cleanup additive, a bactericide, a clay stabilizer, hydrophilic nano particles and a scale inhibitor into water according to the formula amount; and each reagent is added to the next reagent after being stirred uniformly in the container.
The invention successfully develops a recyclable scale-inhibiting fracturing fluid system by compounding the scale inhibitor and the bactericide, and realizes low-cost and low-damage reconstruction of a compact oil-gas reservoir.
The technical scheme of the present invention is described in detail below by way of examples, but the scope of the present invention is not limited to the examples.
Example 1:
the embodiment provides a recyclable scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0.1% water-in-oil emulsion type zwitterionic polyacrylamide, 0.2% cleanup additive, 0.15% glutaraldehyde, 0.3% potassium chloride, 0.1% hydrophilic silica nanoparticles (available from Beijing Anbiqi biotechnology Co., ltd., brand name DNG-B004, average particle size 70 nm), 0.04% scale inhibitor and 99.11% water.
The preparation method of the recyclable scale-inhibiting fracturing fluid comprises the following steps,
s1, preparing water-in-oil emulsion type zwitterionic polyacrylamide, which comprises the following steps:
s101, adding 50 parts of water into 3 parts of acrylic acid according to parts by weight, neutralizing the mixture to pH=7 by using sodium hydroxide, and adding 15 parts of acrylamide and 3 parts of trimethyl allyl ammonium chloride to prepare a water phase;
s102, adding 3 parts of sorbitan trioleate into 90 parts of paraffin oil to prepare an oil phase;
s103, placing the oil phase in a high-speed emulsifying machine, starting the emulsifying machine, then adding the water phase, and emulsifying for 30 minutes to prepare monomer emulsion;
s104, placing 100 parts of monomer emulsion into a flask, introducing nitrogen for 20min, stirring for 5h at the temperature of 40 ℃, then adding 0.005 part of ammonium persulfate, stirring for 2h at the temperature of 60 ℃, and cooling to room temperature to obtain water-in-oil emulsion type zwitterionic polyacrylamide;
s2, preparing a cleanup additive, which comprises the following specific steps: mixing 5 parts by weight of alkyl polyglycoside (purchased from Shanghai drum ministerial biotechnology Co., ltd.), 15 parts by weight of ethanol and 80 parts by weight of water to prepare a drainage aid;
s3, preparing a scale inhibitor, wherein the specific method comprises the following steps: mixing 1 part of amino trimethylene phosphonic acid, 1.2 parts of hydroxy ethylidene diphosphonic acid and 1 part of ethylenediamine tetramethylene phosphonic acid according to parts by weight to obtain a scale inhibitor;
s4, preparing a recyclable scale-inhibiting fracturing fluid, wherein the specific method comprises the following steps of: 99.11 percent of water, 0.1 percent of water-in-oil emulsion type zwitterionic polyacrylamide, 0.2 percent of cleanup additive, 0.15 percent of glutaraldehyde, 0.3 percent of potassium chloride, 0.1 percent of hydrophilic silicon dioxide nano particles and 0.04 percent of scale inhibitor are sequentially added into a container and uniformly stirred to obtain recyclable scale-inhibiting fracturing fluid; when the above reagents are added, care should be taken: every time one reagent is added, the next reagent can be added after the reagent is uniformly stirred in a container.
Example 2:
the embodiment provides a recyclable scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0.06% water-in-oil emulsion type zwitterionic polyacrylamide, 0.15% cleanup additive, 0.2% glutaraldehyde, 0.2% potassium chloride, 0.05% hydrophilic silica nano-particles, 0.03% scale inhibitor and 99.31% water.
The method for preparing the reusable scale-inhibiting fracturing fluid in the embodiment is the same as that in the embodiment 1.
Example 3:
the embodiment provides a recyclable scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0.2% water-in-oil emulsion type zwitterionic polyacrylamide, 0.4% cleanup additive, 0.2% glutaraldehyde, 0.4% potassium chloride, 0.15% hydrophilic silica nanoparticles, 0.05% scale inhibitor and 98.6% water.
The method for preparing the reusable scale-inhibiting fracturing fluid in the embodiment is the same as that in the embodiment 1.
Comparative example 1:
the embodiment provides a scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0% water-in-oil emulsion type zwitterionic polyacrylamide, 0.2% cleanup additive, 0.15% glutaraldehyde, 0.3% potassium chloride, 0.1% hydrophilic silica nanoparticles, 0.04% scale inhibitor and 99.21% water.
The fracturing fluid of this example was prepared in the same manner as in example 1.
Comparative example 2:
the embodiment provides a scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0.1% water-in-oil emulsion type zwitterionic polyacrylamide, 0.2% cleanup additive, 0% glutaraldehyde, 0.3% potassium chloride, 0.1% hydrophilic silica nanoparticles, 0.04% scale inhibitor and 99.26% water.
The fracturing fluid of this example was prepared in the same manner as in example 1.
Comparative example 3:
the embodiment provides a scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0.1% water-in-oil emulsion type zwitterionic polyacrylamide, 0.2% cleanup additive, 0.15% glutaraldehyde, 0.3% potassium chloride, 0% hydrophilic silica nanoparticles, 0.04% scale inhibitor and 99.21% water.
The fracturing fluid of this example was prepared in the same manner as in example 1.
Comparative example 4:
the embodiment provides a scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0.1% water-in-oil emulsion type zwitterionic polyacrylamide, 0.2% cleanup additive, 0.15% glutaraldehyde, 0.15% hydroxypropyl guar, 0.3% potassium chloride, 0.1% hydrophilic silica nanoparticles, 0% scale inhibitor and 99% water.
The fracturing fluid of this example was prepared in the same manner as in example 1.
Comparative example 5:
the comparative example provides a scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0.1% water-in-oil emulsion type zwitterionic polyacrylamide, 0.2% cleanup additive, 0.15% glutaraldehyde, 0.3% potassium chloride, 0.1% hydrophilic silica nanoparticles (available from Beijing Anbiqi biotechnology Co., ltd., brand name DNG-B004, average particle size 70 nm), 0.04% scale inhibitor and 99.11% water.
The preparation method of the fracturing fluid comprises the following steps,
s1, preparing water-in-oil emulsion type zwitterionic polyacrylamide, which comprises the following steps:
s101, adding 50 parts of water into 3 parts of acrylic acid according to parts by weight, neutralizing the mixture to pH=7 by using sodium hydroxide, and adding 15 parts of acrylamide and 3 parts of trimethyl allyl ammonium chloride to prepare a water phase;
s102, adding 3 parts of sorbitan trioleate into 90 parts of paraffin oil to prepare an oil phase;
s103, placing the oil phase in a high-speed emulsifying machine, starting the emulsifying machine, then adding the water phase, and emulsifying for 30 minutes to prepare monomer emulsion;
s104, placing 100 parts of monomer emulsion into a flask, introducing nitrogen for 20min, stirring for 5h at the temperature of 40 ℃, then adding 0.005 part of ammonium persulfate, stirring for 2h at the temperature of 60 ℃, and cooling to room temperature to obtain water-in-oil emulsion type zwitterionic polyacrylamide;
s2, preparing a cleanup additive, which comprises the following specific steps: mixing 5 parts by weight of alkyl polyglycoside (purchased from Shanghai drum ministerial biotechnology Co., ltd.), 15 parts by weight of ethanol and 80 parts by weight of water to prepare a drainage aid;
s3, preparing a scale inhibitor, wherein the specific method comprises the following steps: according to the weight portions, 1 portion of amino trimethylene phosphonic acid, 0 portion of hydroxy ethylidene diphosphonic acid and 1 portion of ethylenediamine tetramethylene phosphonic acid are mixed to obtain the scale inhibitor;
s4, preparing a scale-inhibiting fracturing fluid, which comprises the following specific steps: 99.11 percent of water, 0.1 percent of water-in-oil emulsion type zwitterionic polyacrylamide, 0.2 percent of cleanup additive, 0.15 percent of glutaraldehyde, 0.3 percent of potassium chloride, 0.1 percent of hydrophilic silicon dioxide nano particles and 0.04 percent of scale inhibitor are sequentially added into a container, and uniformly stirred to obtain scale-inhibiting fracturing fluid; when the above reagents are added, care should be taken: every time one reagent is added, the next reagent can be added after the reagent is uniformly stirred in a container.
The present comparative example differs from example 1 in that: the raw materials and the preparation methods of the scale inhibitor are different.
Comparative example 6:
the comparative example provides a scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0.1% water-in-oil emulsion type zwitterionic polyacrylamide, 0.2% cleanup additive, 0.15% glutaraldehyde, 0.3% potassium chloride, 0.1% hydrophilic silica nanoparticles (available from Beijing Anbiqi Biotech Co., ltd., brand DNG-B006, average particle size 200 nm) with an average particle size of 200nm, 0.04% scale inhibitor and 99.11% water.
The fracturing fluid of this example was prepared in the same manner as in example 1.
Comparative example 7:
the comparative example provides a scale-inhibiting fracturing fluid, which comprises the following raw materials in percentage by mass: 0.1% water-in-oil emulsion type zwitterionic polyacrylamide, 0.2% cleanup additive, 0.15% glutaraldehyde, 0.3% potassium chloride, 0.1% hydrophilic silica nanoparticles (available from Beijing Anbiqi biotechnology Co., ltd., brand DNG-B004, average particle size 70 nm), 0.04% scale inhibitor and 99.11% formation mineralization water.
Specifically, the measurement results of the component content of the mineralized water of the formation are shown in table 1.
TABLE 1
| Composition of the components | Content of | Unit (B) |
| Ferrous iron (II) | 96.7 | mg/L |
| Ferric iron | 49.3 | mg/L |
| Total iron | 146 | mg/L |
| Sulfides | 0.041 | mg/L |
| Sulfate reducing bacteria | 0 | Individual/ml |
| Iron bacteria | 95 | Individual/ml |
| Potassium | 75.6 | mg/L |
| Calcium | 6061 | mg/L |
| Sodium salt | 2967 | mg/L |
| Magnesium (Mg) | 180 | mg/L |
The following related tests were carried out on the fracturing fluid obtained in the above example, and the test methods are as follows:
1. drag reduction rate test: the drag reduction performance of the fracturing fluid is tested by adopting a tubular rheometer, the pressure difference of the fluid when the fluid passes through a tubular column is recorded, the drag reduction rate of the fracturing fluid is calculated, the drag reduction rate eta= x 100%, wherein a is the pressure difference of clear water flowing through the tubular column, b is the pressure difference of slick water flowing through the tubular column under the same condition, and the result is shown in table 2.
2. And (3) scale inhibition rate test: the scale inhibition rate of the fracturing fluid is tested according to GB/T16632-2019 method for measuring scale inhibition performance of water treatment agent by calcium carbonate deposition, and the result is shown in Table 2.
3. Interfacial tension test with aviation kerosene: the surface area interfacial tension of the fracturing fluid was tested according to SY/T5370-2018 surface and interfacial tension determination method, and the results are shown in Table 2.
TABLE 2
It can be seen from examples 1 to 3 and comparative examples 1 to 7 that the invention provides a recyclable scale-inhibiting fracturing fluid and a preparation method thereof, which have high drag reduction rate and scale inhibition rate, and can be recycled.
In conclusion, the water-in-oil emulsion type zwitterionic polyacrylamide disclosed by the invention is a novel low-cost salt-tolerant drag reducer, and has the performances of low-viscosity slickwater and high-viscosity sand-carrying fluid.
The novel drag reducer is developed and other additives are compounded, so that the prepared recyclable scale-inhibiting fracturing fluid system meets the requirements of the reformation of a tight reservoir containing high-mineralization stratum water, the generation of precipitation after fluid is retained in the reservoir is inhibited, the function of the fluid system is switched between sand carrying and renting reduction by changing the concentration of the thickening agent, the low-cost, low-friction and low-damage construction of the tight oil-gas reservoir and the recycling of flowback fluid are realized, and the fracturing fluid system has good reformation effect on the reservoir with obvious calcium chloride water type or scaling trend of other blocks and is good in the early stage of application. Meanwhile, the scale-inhibiting fracturing fluid system can avoid precipitation and bacteria breeding after the retained reservoir fracturing fluid meets stratum water, and realize low-cost and low-damage reconstruction of a tight oil-gas reservoir.
Finally, it should be understood that the foregoing description is merely illustrative of the preferred embodiments of the present invention, and that no limitations are intended to the scope of the invention, as defined by the appended claims.
Claims (6)
1. The reusable scale-inhibiting fracturing fluid is characterized by comprising the following components in percentage by mass: 0.06 to 0.20 percent of drag reducer, 0.15 to 0.4 percent of cleanup additive, 0.1 to 0.2 percent of bactericide, 0.2 to 0.4 percent of clay stabilizer, 0.05 to 0.15 percent of hydrophilic nano particles, 0.03 to 0.05 percent of scale inhibitor and the balance of water;
the drag reducer is water-in-oil emulsion type zwitterionic polyacrylamide;
the preparation method of the water-in-oil emulsion type zwitterionic polyacrylamide comprises the following steps:
s1, adding 40-60 parts of water into 1-5 parts of acrylic acid according to parts by weight, neutralizing to pH=7 by using sodium hydroxide, and adding 10-20 parts of acrylamide and 1-5 parts of allyl trimethyl ammonium chloride to prepare a water phase;
s2, adding 1-5 parts of sorbitan trioleate into 70-100 parts of paraffin oil according to parts by weight to prepare an oil phase;
s3, placing the oil phase into a high-speed emulsifying machine with the rotating speed of 4000-7000 rpm, starting the emulsifying machine, then adding the water phase, and emulsifying for 30 minutes to prepare monomer emulsion;
s4, placing 100 parts of monomer emulsion into a container, introducing nitrogen for 20min, stirring for 5-6 h at the temperature of 30-40 ℃, then adding 0.004-0.007 part of ammonium persulfate, stirring for 2-3 h at the temperature of 50-60 ℃, and cooling to room temperature to obtain the water-in-oil emulsion type zwitterionic polyacrylamide;
the cleanup additive is prepared from 2-6 parts by weight of alkyl polyglycoside, 10-20 parts by weight of ethanol and 60-80 parts by weight of water;
the bactericide is one or a mixture of more than one of glutaraldehyde, formaldehyde and tetrakis (hydroxymethyl) phosphonium sulfate in any proportion;
the scale inhibitor is formed by mixing amino trimethylene phosphonic acid, hydroxy ethylidene diphosphonic acid and ethylenediamine tetramethylene phosphonic acid; the weight ratio of the amino trimethylene phosphonic acid to the hydroxy ethylidene diphosphonic acid to the ethylenediamine tetramethylene phosphonic acid is (0.8-1.2): (1-1.5): 1, a step of;
the hydrophilic nano particles are one or a mixture of a plurality of hydrophilic silicon dioxide nano particles, hydrophilic titanium dioxide nano particles, hydrophilic magnesium oxide nano particles and hydrophilic zinc oxide nano particles in any proportion; the average particle diameter of the hydrophilic nano particles is 50-100 nm.
2. The reusable scale inhibiting fracturing fluid of claim 1, wherein: the clay stabilizer is one or a mixture of a plurality of potassium chloride, ammonium chloride and choline chloride in any proportion.
3. The reusable scale-inhibiting fracturing fluid of claim 1, wherein the reusable scale-inhibiting fracturing fluid comprises the following components in percentage by mass: 0.1% water-in-oil emulsion type zwitterionic polyacrylamide, 0.2% cleanup additive, 0.15% glutaraldehyde, 0.3% potassium chloride, 0.1% hydrophilic silica nanoparticles, 0.04% scale inhibitor and 99.11% water.
4. The reusable scale inhibiting fracturing fluid of claim 1, wherein: the recyclable scale-inhibiting fracturing fluid comprises the following components in percentage by mass: 0.06% water-in-oil emulsion type zwitterionic polyacrylamide, 0.15% cleanup additive, 0.2% glutaraldehyde, 0.2% potassium chloride, 0.05% hydrophilic silica nano-particles, 0.03% scale inhibitor and 99.31% water.
5. The reusable scale inhibiting fracturing fluid of claim 1, wherein: the recyclable scale-inhibiting fracturing fluid comprises the following components in percentage by mass: 0.2% water-in-oil emulsion type zwitterionic polyacrylamide, 0.4% cleanup additive, 0.2% glutaraldehyde, 0.4% potassium chloride, 0.15% hydrophilic silica nanoparticles, 0.05% scale inhibitor and 98.6% water.
6. A method for preparing the recyclable scale-inhibiting fracturing fluid according to any one of claims 1 to 5, characterized in that the specific operation steps of the preparation method are as follows: sequentially adding a drag reducer, a cleanup additive, a bactericide, a clay stabilizer, hydrophilic nano particles and a scale inhibitor into water according to the formula amount; and each reagent is added to the next reagent after being stirred uniformly in the container.
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