CN105462574A - Nanosilicon dioxide oil displacement agent with modified terminated polyether and preparation method thereof - Google Patents
Nanosilicon dioxide oil displacement agent with modified terminated polyether and preparation method thereof Download PDFInfo
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 74
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 229920000570 polyether Polymers 0.000 title claims abstract description 40
- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 38
- 238000006073 displacement reaction Methods 0.000 title abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 72
- 239000000243 solution Substances 0.000 claims abstract description 51
- 239000003921 oil Substances 0.000 claims abstract description 47
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- -1 polyoxy Polymers 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 54
- 230000004048 modification Effects 0.000 claims description 34
- 238000012986 modification Methods 0.000 claims description 31
- 239000001257 hydrogen Substances 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- 238000011084 recovery Methods 0.000 claims description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical compound C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 7
- 229910000077 silane Inorganic materials 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000002459 sustained effect Effects 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 2
- 238000000034 method Methods 0.000 abstract description 8
- 238000010790 dilution Methods 0.000 abstract description 4
- 239000012895 dilution Substances 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract 2
- 239000011863 silicon-based powder Substances 0.000 abstract 2
- HQSLRIXPNFGAQR-UHFFFAOYSA-N [SiH4].Cl Chemical compound [SiH4].Cl HQSLRIXPNFGAQR-UHFFFAOYSA-N 0.000 abstract 1
- 150000005215 alkyl ethers Chemical class 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 abstract 1
- 235000019198 oils Nutrition 0.000 description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 239000013543 active substance Substances 0.000 description 12
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 12
- 239000000377 silicon dioxide Substances 0.000 description 12
- 235000013312 flour Nutrition 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 239000010779 crude oil Substances 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 5
- 239000002585 base Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- DOKHEARVIDLSFF-UHFFFAOYSA-N prop-1-en-1-ol Chemical compound CC=CO DOKHEARVIDLSFF-UHFFFAOYSA-N 0.000 description 5
- 238000010008 shearing Methods 0.000 description 5
- 230000008719 thickening Effects 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002715 modification method Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229920001732 Lignosulfonate Polymers 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005194 fractionation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 235000019357 lignosulphonate Nutrition 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 235000016068 Berberis vulgaris Nutrition 0.000 description 1
- 241000335053 Beta vulgaris Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000412 dendrimer Substances 0.000 description 1
- 229920000736 dendritic polymer Polymers 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002193 fatty amides Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 235000019476 oil-water mixture Nutrition 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- PFIOPNYSBSJFJJ-UHFFFAOYSA-M sodium;2-octylbenzenesulfonate Chemical compound [Na+].CCCCCCCCC1=CC=CC=C1S([O-])(=O)=O PFIOPNYSBSJFJJ-UHFFFAOYSA-M 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012747 synergistic agent Substances 0.000 description 1
- 238000005406 washing Methods 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
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/48—Polymers modified by chemical after-treatment
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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
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/16—Enhanced recovery methods for obtaining hydrocarbons
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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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/10—Nanoparticle-containing well treatment fluids
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Mining & Mineral Resources (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Polyethers (AREA)
- Silicon Polymers (AREA)
Abstract
The invention provides a preparation method of a nanosilicon dioxide oil displacement agent with modified terminated polyether. The method comprises the following steps that metal silicon powder and water are mixed on the basis that the mass ratio is 1:5-1:2, an alkaline agent is added to form a mixing solution with the pH value being 8-10, metal silicon powder is added at the temperature of 60-90 DEG C to be subjected to a continuous reaction to obtain a nanosilicon dioxide solution with the concentration being 1-20 wt%, acid is added to adjust the pH value to be 4.0-5.0, and a first reaction solution is formed; terminated allyl alcohol polyoxy alkyl ether, hexachloroplatinic acid and triethoxy chloride silane are mixed on the basis that the mole ratio is 1:(0.005-0.01):1 to be subjected to a coupled reaction, a silane coupling agent with the concentration being 90-95 wt% is obtained, dilution is performed to make the concentration be 1-20 wt%, and a second reaction solution is obtained; the first reaction solution is added into the second reaction solution to be subjected to a modified reaction, and an oil displacement agent is obtained, wherein the mass ratio of the nanosilicon dioxide to the silane coupling agent is 1:0.05-1:0.1.
Description
Technical field
The invention belongs to the chemical oil displacement agent field in tertiary oil recovery, relate to nano silicon oil-displacing agent of a kind of end capped polyether modification and preparation method thereof.
Background technology
Along with the develop rapidly of economic technology, the demand of crude oil is increasing, and crude oil has become an important factor of restriction China Economic development.Oil reservoir, after experienced by primary oil recovery and secondary oil recovery, still has a large amount of surplus oils cannot be extracted in the earth formation.In this case, tertiary oil recovery becomes gradually and is widely used, and improves a kind of oil production method of recovery ratio.Special in China, current tertiary oil recovery has become maturing field and has reduced one of moisture, major measure improving oil recovery factor.Affect oil recovery factor and have two principal elements, one is sweep efficiency, and another one is displacement efficiency.
Polymer flooding by improving the viscosity of injection liquid, can improve sweep efficiency, thus reaching the object improving recovery ratio.Chinese patent CN1152587A discloses a kind of preparation method of polymer oil-displacing agent, and the homogeneous phase complex oil displacing agent solution that the method obtains has significant Efficient Adhesive Promotion at low concentrations.Chinese patent CN1611562A discloses a kind of ter-polymers oil-displacing agent and its preparation method and application, and the ter-polymers oil-displacing agent of this invention effectively can improve temperature resistance and the salt resistant character of oil-displacing agent in oil recovery process.But polymer oil-displacing agent can only movable oil in extraction surplus oil, does not act on unmobilized oil wherein.And tensio-active agent can reduce the interfacial tension between profit, reducing the retention force of irreducible oil, the recovery ratio of crude oil can be improved by improving displacement efficiency.Chinese patent CN1327026A discloses a kind of chemical oil displacement agent of the sulfonated lignin fatty amide modified containing Long carbon chain, a kind of chemical oil displacement agent of the sulfonated lignin containing Long carbon chain fatty amide is provided, Crude oil-water can be made to have ultra low interfacial tension in wide concentration range.Chinese patent CN1352224A discloses a kind of high-level efficiency oil-displacing agent, it is primarily of sodium octylbenzene sulfonate anion surfactant, surfactant adjuvant, tensio-active agent synergistic agent, surface active agent solubilization agent composition, the structural viscosity of viscous crude can be reduced significantly, reduce oil water interfacial tension, improve displacement efficiency, thus improve recovery ratio.But tensio-active agent is large in stratum Adsorption And Retention amount, and cost is higher, thus limit its application.Document " irreducible oil recovery ratio research after polymkeric substance/beet alkali surface activator raising water drive " (China University Of Petroleum Beijing's journal, 2007,31 (6): 74-78) mention, polymkeric substance/tensio-active agent compound oil displacement agent, although oil-production efficiency can be improved in conjunction with both advantages, but the select and requirement of polymkeric substance/tensio-active agent compound oil displacement agent Surfactant is comparatively harsh, meanwhile, the membership that adds of tensio-active agent reduces the apparent viscosity injecting water.
About the application of nano silicon in the displacement of reservoir oil, Chinese patent application CN102965094A discloses a kind of dendritic polymers/SiO
2nanometer displacement agent and preparation method thereof, this oil-displacing agent can set up higher resistance coefficient and residual resistance factor, thus improves oil recovery factor.Chinese patent CN1818008A discloses a kind of oil-displacing agent and preparation method thereof, and this oil-displacing agent adopts sulfonated petro-leum and improved silica to react in a kettle. and is prepared from, and its product can make oil water interfacial tension be reduced to 1 × 10
-4mNm
-1below, thus improve oil recovery factor.Document " SiO
2the behavior of/PEG dispersion system dynamic shear rheological " (Acta PhySico-Chimica Sinica, 2008,24 (3): 433-436) research discovery, certain density nano silicon system, there will be the phenomenon of thickening under certain shearing condition.If adopt separately nano silicon and the composite of tensio-active agent to improve oil-production efficiency, enter in the process on stratum in system, both separation can be caused due to the chromatographic separation effect of rock stratum.
Summary of the invention
In view of the above problems, the object of the present invention is to provide nano silicon oil-displacing agent of a kind of end capped polyether modification and preparation method thereof, this oil-displacing agent can increase the viscosity of injection liquid, can reduce again the tension force of water-oil interface simultaneously largely, can also avoid the chromatographic fractionation effect of rock stratum.
In order to reach foregoing invention object, the invention provides a kind of preparation method of nano silicon oil-displacing agent of end capped polyether modification, comprising the steps:
By metallic silicon power with water in mass ratio for 1:5-1:2 mixes, then add alkaline agent, forming pH value is the mixed solution of 8-10, then adds metallic silicon power sustained reaction under 60-90 DEG C of condition, obtains the nanosilica solution that mass concentration is 1%-20%;
Acid adding regulates the pH value of described nanosilica solution to 4.0-5.0, forms the first reaction solution;
Blocked allyl alcohol polyoxyalkyl ether and chlordene are closed platinic acid mix, then add three oxygen base hydrogen silanes, carry out linked reaction, obtain the blocked allyl alcohol polyoxyalkyl ether silane coupling agent that mass concentration is 90%-95%;
Described silane coupling agent being diluted to mass concentration is 1%-20%, as the second reaction solution;
Described second reaction solution is slowly added in described first reaction solution and carries out modified-reaction, obtain the nano silicon oil-displacing agent of end capped polyether modification;
Wherein, the mol ratio of described blocked allyl alcohol polyoxyalkyl ether, chlordene conjunction platinic acid and three oxygen base hydrogen silanes is 1:(0.005-0.01): 1; The mass ratio of the silane coupling agent in the nano silicon in described first reaction solution and described second reaction solution is 1:0.05-1:0.1.
In above-mentioned preparation method, preferably, adding after metallic silicon power (in batches adding) sustained reaction terminates, filtered by gained mixture, filter residue is unreacted metallic silicon power, can reuse, and filtrate is nanosilica solution.
In above-mentioned preparation method, preferably, described chlordene closes platinic acid and mixes with blocked allyl alcohol polyoxyalkyl ether with its aqueous isopropanol, then adds three oxygen base hydrogen silanes, carries out linked reaction.Preferred, described linked reaction is carried out under protection gas, and described protection gas is nitrogen; The solvent of diluted silane coupling agent is ethanol.
In above-mentioned preparation method, preferably, described alkaline agent comprises the combination of one or more in sodium hydroxide, potassium hydroxide and ammoniacal liquor; Described acid comprises the combination of one or more in acetic acid, hydrochloric acid and Citric Acid; Described three oxygen base hydrogen silanes comprise trimethoxy hydrogen silane or triethoxy hydrogen silane.
In above-mentioned preparation method, preferably, the end group of described silane coupling agent is blocked allyl alcohol polyoxyalkyl ether; The molecular structural formula of described blocked allyl alcohol polyoxyalkyl ether is: CH
2=CH-CH
2o (CH
2cH
2cH
2o)
m-(CH
2cH
2o)
noR', R' represent-CH
3,-C
2h
5,-OC
2h
4oCH
3,-OSi (CH
3)
3in any one, and 0≤m≤20,0≤n≤20, m+n>=1, m and n is integer;
The structural formula of described three oxygen base hydrogen silanes is:
R represents-CH
3or-C
2h
5.
In above-mentioned preparation method, preferably, the structural formula of described silane coupling agent is:
R represents-CH
3or-C
2h
5, R' represents-CH
3,-C
2h
5,-OC
2h
4oCH
3,-OSi (CH
3)
3in any one, and 0≤m≤20,0≤n≤20, m+n>=1, m and n is integer.
In above-mentioned preparation method, preferably, the structural formula of the nano silicon oil-displacing agent of described end capped polyether modification is:
R' represents-CH
3,-C
2h
5,-OC
2h
4oCH
3,-OSi (CH
3)
3in any one, and 0≤m≤20,0≤n≤20, m+n>=1, m and n is integer.
In above-mentioned preparation method, preferably, the temperature of described linked reaction is 80-95 DEG C, and the time is 3-9 hour.
Preferred, the reaction formula of described linked reaction is:
R represents-CH
3or-C
2h
5, R' represents-CH
3,-C
2h
5,-OC
2h
4oCH
3,-OSi (CH
3)
3in any one, and 0≤m≤20,0≤n≤20, m+n>=1, m and n is integer.
In above-mentioned preparation method, preferably, the temperature of described modified-reaction is 60-90 DEG C, and the time is 3-8 hour.
Preferred, the reaction formula of described modified-reaction is:
R represents-CH
3or-C
2h
5, R' represents-CH
3,-C
2h
5,-OC
2h
4oCH
3,-OSi (CH
3)
3in any one, and 0≤m≤20,0≤n≤20, m+n>=1, m and n is integer.
The preparation method of the nano silicon oil-displacing agent of end capped polyether modification provided by the invention, the nano silicon of the silane coupling agent of end capped polyether to synthesis is utilized to carry out modification, non-ionic tensio-active agent end capped polyether is grafted to the surface of nano silicon, obtains polyether-modified nano silicon oil-displacing agent.
The present invention also provides a kind of nano silicon oil-displacing agent of the end capped polyether modification obtained according to above-mentioned preparation method, and wherein, the particle diameter of described nano silicon is 5-100nm.
The present invention also provides a kind of application of nano silicon oil-displacing agent in tertiary oil recovery of end capped polyether modification, and preferably, the consumption of the nano silicon oil-displacing agent of described end capped polyether modification is more than 0.1%.
Nano silicon oil-displacing agent and traditional oil-displacing agent used for tertiary oil recovery of end capped polyether modification provided by the invention make a big difference, oil-displacing agent of the present invention is that nonionogenic tenside---end group is the silane coupling agent of blocked allyl alcohol polyoxyalkyl ether in the mode grafting of nano-silica surface by chemical bonding, both there is the feature of tensio-active agent in the process of the displacement of reservoir oil, there is again the advantage of nano material, injecting the process of water sport, the viscosity of the aqueous solution can be increased, increase swept volume.In the process that it uses when the concentration of nano silicon is 0.1%, the surface tension of water-oil interface can be made to be reduced to 1 × 10
-3mNm
-1.And this tensio-active agent is not containing aromatic ring, has environment-protecting asepsis, is easy to the advantages such as degraded.The technical maturity simultaneously preparing nanosilica solution is simple, has cheap advantage, the advantages such as therefore oil-displacing agent of the present invention has environmental protection, easily degrades, and price is low.
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and beneficial effect, existing following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.The material adopted in following examples, except indicating, all the other are commercially available.
Embodiment 1
The present embodiment provides a kind of preparation method of nano silicon oil-displacing agent of end capped polyether modification, and it comprises the following steps:
The preparation of the nano silicon aqueous solution: by metallic silicon power and deionized water in mass ratio for 1:4 adds in reactor, then the sodium hydroxide solution prepared in advance is added, make the pH value of whole solution system between 8-10, subsequently under whipped state, reacting by heating still, be warming up to 80 DEG C of reactions, and add silica flour in batches in reaction process, keep reaction to continue to carry out.After question response terminates, gained solution is filtered, remove unreacted silica flour, this filtration silica flour can reuse, and the filtrate obtained is the aqueous solution of nano silicon, wherein, the mass concentration of nano silicon is 16.3%, and size is between 30-60nm.
The preparation of silane coupling agent: get chlordene conjunction platinic acid 0.65 gram and add in three-necked bottle, and with 200 grams of Virahol dissolved dilutions, add methoxy group allyl alcohol polyethenoxy ether 150 grams wherein; Inserted by thermometer in an eck of this three-necked flask, two other eck, one passes into nitrogen, another one access dropping funnel; First logical nitrogen, by the air displacement in this three-necked flask, and heat this three-necked flask, then get 30.5 grams of trimethoxy hydrogen silanes and put into dropping funnel and slowly instill this three-necked flask, controlling temperature of reaction is 85 DEG C, react 6 hours, be cooled to room temperature, carry out underpressure distillation subsequently, removing unreacted reactant and solvent, obtain the methoxy group allyl alcohol polyethenoxy ether silane coupling agent 163 grams that organic chain is methoxy group polyethers, purity 90.3%.
The preparation of oil-displacing agent: getting the nanosilica solution 500 grams that above-mentioned mass concentration is 16.3%, is 4.5 by acetic acid regulator solution pH value, as the first reaction solution; Get the methoxy group allyl alcohol polyethenoxy ether silane coupling agent 4.2 grams of above-mentioned synthesis, be diluted with ethanol to 120 grams, as the second reaction solution; Above-mentioned second reaction solution is dropwise joined in above-mentioned first reaction solution, keep temperature of reaction to be 70 DEG C, react 4.5 hours, obtain the nano silicon oil-displacing agent product of end capped polyether modification.
The molecular structural formula of methoxy group allyl alcohol polyethenoxy ether is: CH
2=CH-CH
2o-(CH
2cH
2o)
12oCH
3, molecular weight is 616.
The structural formula of trimethoxy hydrogen silane is:
R represents-CH
3;
The structural formula of methoxy group allyl alcohol polyethenoxy ether silane coupling agent is:
R represents-CH
3, R' represents-CH
3, and m is 0, n is 12;
The structural formula of the nano silicon oil-displacing agent of end capped polyether modification is:
R' represents-CH
3, and m is 0, n is 12.
The reaction formula of the linked reaction of the present embodiment is:
R represents-CH
3, R' represents-CH
3, and m is 0, n is 12.
The modified-reaction of the present embodiment is:
R represents-CH
3, R' represents-CH
3, and m is 0, n is 12.
The nano silicon oil-displacing agent of the end capped polyether modification that the present embodiment obtains is tested
Testing tool: the MCR101 of Tx-500 interfacial tensimeter, Anton Paar company
Test oil/water sample: profit sample to be measured is Daqing crude oil and grand celebration sewage
Added in oil/water sample to be measured by the nano silicon oil-displacing agent of the end capped polyether modification of the present embodiment and stir, be configured to mixed solution to be measured, wherein, the mass concentration of this oil-displacing agent is 0.1%, i.e. 1000mgL
-1; Tx-500 interfacial tensimeter is heated to 65 DEG C, and rotating speed is set to 5000 revs/min; Drop on the measuring stand of Tx-500 interfacial tensimeter by this mixed solution to be measured, 8 minutes time, the oil water interfacial tension recording this mixed solution is 1.2 × 10
-3mNm
-1.
Adopt the MCR101 of Anton Paar company to carry out the thickening test of this oil-displacing agent, its result is, is 500s at shearing frequency
-1time, the apparent viscosity of this mixed solution can increase to original 3.2 times.
Embodiment 2
The present embodiment provides a kind of preparation method of nano silicon oil-displacing agent of end capped polyether modification, and it comprises the following steps:
The preparation of the nano silicon aqueous solution: by metallic silicon power and deionized water in mass ratio for 1:3 adds in reactor, then the potassium hydroxide solution prepared in advance is added, make the pH value of whole solution system between 8-10, subsequently under whipped state, reacting by heating still, be warming up to 80 DEG C of reactions, and add silica flour in batches in reaction process, keep reaction to continue to carry out.After question response terminates, gained solution is filtered, remove unreacted silica flour, this filtration silica flour can reuse, and the filtrate obtained is the aqueous solution of nano silicon, wherein, the mass concentration of nano silicon is 17.8%, and size is between 50-80nm.
The preparation of silane coupling agent: get chlordene conjunction platinic acid 0.8 gram and add in three-necked bottle, with 200 grams of Virahol dissolved dilutions, add methoxy group allyl alcohol polyethenoxy polyethenoxy ether 300 grams wherein; Inserted by thermometer in an eck of this three-necked flask, two other eck, one passes into nitrogen, another one access dropping funnel; First logical nitrogen, by the air displacement in this three-necked flask, and heat this three-necked flask, then get 30.5 grams of trimethoxy hydrogen silanes and put into dropping funnel and slowly instill this three-necked flask, controlling temperature of reaction is 80 DEG C, react 8 hours, be cooled to room temperature, carry out underpressure distillation subsequently, removing unreacted reactant and solvent, obtain the methoxy group allyl alcohol polyethenoxy polyethenoxy ether silane coupling agent 314 grams that organic chain is methoxy group polyethers, purity 95%.
The preparation of oil-displacing agent: getting the nanosilica solution 500 grams that above-mentioned mass concentration is 17.8%, is 4.8 by acetic acid regulator solution pH value, as the first reaction solution; Get the methoxy group allyl alcohol polyethenoxy polyethenoxy ether silane coupling agent 7.9 grams of above-mentioned synthesis, be diluted with ethanol to 120 grams, as the second reaction solution; Above-mentioned second reaction solution is dropwise joined in above-mentioned first reaction solution, keep temperature of reaction to be 75 DEG C, react 4 hours, obtain the nano silicon oil-displacing agent product of end capped polyether modification.
The molecular structural formula of methoxy group allyl alcohol polyethenoxy polyethenoxy ether is: CH
2=CH-CH
2o (CH
2cH
2cH
2o)
9-(CH
2cH
2o)
13oCH
3weight-average molecular weight is 1182.
The structural formula of trimethoxy hydrogen silane is:
R represents-CH
3;
The structural formula of methoxy group allyl alcohol polyethenoxy polyethenoxy ether silane coupling agent is:
R represents-CH
3, R' represents-CH
3, and m is 9, n is 13;
The structural formula of the nano silicon oil-displacing agent of end capped polyether modification is:
R' represents-CH
3, and m is 9, n is 13.
The reaction formula of the linked reaction of the present embodiment is:
R represents-CH
3, R' represents-CH
3, and m is 9, n is 13.
The modified-reaction of the present embodiment is:
R represents-CH
3, R' represents-CH
3, and m is 9, n is 13.
The nano silicon oil-displacing agent of the end capped polyether modification that the present embodiment obtains is tested
Testing tool: the MCR101 of Tx-500 interfacial tensimeter, Anton Paar company
Test oil/water sample: profit sample to be measured is Daqing crude oil and grand celebration sewage
Added in oil/water sample to be measured by the nano silicon oil-displacing agent of this end capped polyether modification and stir, be configured to mixed solution to be measured, wherein, the mass concentration of this oil-displacing agent is 0.1%, i.e. 1000mgL
-1; Tx-500 interfacial tensimeter is heated to 70 DEG C, and rotating speed is set to 5000 revs/min; Drop on the measuring stand of Tx-500 interfacial tensimeter by this mixed solution to be measured, 6 minutes time, the oil water interfacial tension recording this mixed solution is 1.3 × 10
-3mNm
-1.
Adopt the MCR101 of Anton Paar company to carry out the thickening test of this oil-displacing agent, its result is, is 450s at shearing frequency
-1time, the apparent viscosity of this mixed solution can increase to original 3 times.
Embodiment 3
The present embodiment provides a kind of preparation method of nano silicon oil-displacing agent of end capped polyether modification, and it comprises the following steps:
The preparation of the nano silicon aqueous solution: by metallic silicon power and deionized water in mass ratio for 1:5 adds in reactor, then the ammonia soln prepared in advance is added, make the pH value of whole solution system between 8-10, subsequently under whipped state, reacting by heating still, be warming up to 80 DEG C of reactions, and add silica flour in batches in reaction process, keep reaction to continue to carry out.After question response terminates, gained solution is filtered, remove unreacted silica flour, this filtration silica flour can reuse, and the filtrate obtained is the aqueous solution of nano silicon, wherein, the mass concentration of nano silicon is 15.6%, and size is between 20-60nm.
The preparation of silane coupling agent: get chlordene conjunction platinic acid 1.25 grams and add in three-necked bottle, with 200 grams of Virahol dissolved dilutions, add oxyethyl group terminated propenol polyoxyethylene polyethenoxy ether 400 grams wherein; Inserted by thermometer in an eck of this three-necked flask, two other eck, one passes into nitrogen, another one access dropping funnel; First logical nitrogen, by the air displacement in this three-necked flask, and heat this three-necked flask, then get 41 grams of triethoxy hydrogen silanes and put into dropping funnel and slowly instill this three-necked flask, controlling temperature of reaction is 93 DEG C, react 8 hours, be cooled to room temperature, carry out underpressure distillation subsequently, removing unreacted reactant and solvent, obtain the oxyethyl group terminated propenol polyoxyethylene polyethenoxy ether silane coupling agent 400 grams that organic chain is oxyethyl group end capped polyether, purity 93%.
The preparation of oil-displacing agent: getting the nanosilica solution 500 grams that above-mentioned mass concentration is 15.6%, is 4.6 by acetic acid regulator solution pH value, as the first reaction solution; Get the oxyethyl group terminated propenol polyoxyethylene polyethenoxy ether silane coupling agent 5.5 grams of above-mentioned synthesis, be diluted with ethanol to 120 grams, as the second reaction solution; Above-mentioned second reaction solution is dropwise joined in above-mentioned first reaction solution, keep temperature of reaction to be 80 DEG C, react 3 hours, obtain the nano silicon oil-displacing agent product of end capped polyether modification.
The molecular structural formula of oxyethyl group terminated propenol polyoxyethylene polyethenoxy ether is: CH
2=CH-CH
2o (CH
2cH
2cH
2o)
11-(CH
2cH
2o)
20oC
2h
5weight-average molecular weight is 1620.
The structural formula of triethoxy hydrogen silane is:
R represents-C
2h
5;
The structural formula of oxyethyl group terminated propenol polyoxyethylene polyethenoxy ether silane coupling agent is:
R represents-C
2h
5, R' represents-C
2h
5, and m is 11, n is 20;
The structural formula of the nano silicon oil-displacing agent of end capped polyether modification is:
R' represents-C
2h
5, and m is 11, n is 20.
The reaction formula of the linked reaction of the present embodiment is:
R represents-C
2h
5, R' represents-C
2h
5, and m is 11, n is 20.
The modified-reaction of the present embodiment is:
R represents-C
2h
5, R' represents-C
2h
5, and m is 11, n is 20.
The nano silicon oil-displacing agent of end capped polyether modification
The nano silicon oil-displacing agent of the end capped polyether modification that the present embodiment obtains is tested
Testing tool: the MCR101 of Tx-500 interfacial tensimeter, Anton Paar company
Test oil/water sample: profit sample to be measured is Daqing crude oil and grand celebration sewage
Added in oil/water sample to be measured by the nano silicon oil-displacing agent of this end capped polyether modification and stir, be configured to mixed solution to be measured, wherein, the mass concentration of this oil-displacing agent is 0.1%, i.e. 1000mgL
-1; Tx-500 interfacial tensimeter is heated to 75 DEG C, and rotating speed is set to 5000 revs/min; Drop on the measuring stand of Tx-500 interfacial tensimeter by this mixed solution to be measured, 5 minutes time, the oil water interfacial tension recording this mixed solution is 1.1 × 10
-3mNm
-1.
Adopt the MCR101 of Anton Paar company to carry out the thickening test of this oil-displacing agent, its result is, is 500s at shearing frequency
-1time, the apparent viscosity of this mixed solution can increase to original 2.8 times.
As can be seen from above specific embodiment, oil-displacing agent of the present invention generally can by the interfacial tension lowering of profit to 10
-3mNm
-1the order of magnitude about.Can also under certain shearing frequency, make the apparent viscosity of oil-water mixture increase to original 2 to 3 times simultaneously.
The preparation method of oil-displacing agent provided by the present invention has passed through in the mode grafting of chemical bonding nonionogenic tenside at nano-silica surface, the performance of Properties of Polymer and tensio-active agent has been focused on nano silicon, injecting the process of water sport, both the characteristic of nano silicon thickening under certain condition can have been utilized to improve sweep efficiency, increase the viscosity of the aqueous solution, tensio-active agent can be utilized again to reduce the tension force of water-oil interface largely, reach the object of washing oil, the adverse influence can effectively avoiding the chromatographic fractionation effect on stratum to cause in the process of conveying, thus effectively raise oil recovery factor.
Claims (10)
1. a preparation method for the nano silicon oil-displacing agent of end capped polyether modification, comprises the steps:
By metallic silicon power with water in mass ratio for 1:5-1:2 mixes, then add alkaline agent, forming pH value is the mixed solution of 8-10, then adds metallic silicon power sustained reaction under 60-90 DEG C of condition, obtains the nanosilica solution that mass concentration is 1%-20%;
Acid adding regulates the pH value of described nanosilica solution to 4.0-5.0, forms the first reaction solution;
Blocked allyl alcohol polyoxyalkyl ether and chlordene are closed platinic acid mix, then add three oxygen base hydrogen silanes, carry out linked reaction, obtain the blocked allyl alcohol polyoxyalkyl ether silane coupling agent that mass concentration is 90%-95%;
Described silane coupling agent being diluted to mass concentration is 1%-20%, as the second reaction solution;
Described second reaction solution is slowly added in described first reaction solution and carries out modified-reaction, obtain the nano silicon oil-displacing agent of end capped polyether modification;
Wherein, the mol ratio of described blocked allyl alcohol polyoxyalkyl ether, chlordene conjunction platinic acid and three oxygen base hydrogen silanes is 1:(0.005-0.01): 1; The mass ratio of the silane coupling agent in the nano silicon in described first reaction solution and described second reaction solution is 1:0.05-1:0.1.
2. preparation method according to claim 1, is characterized in that, described alkaline agent comprises the combination of one or more in sodium hydroxide, potassium hydroxide and ammoniacal liquor; Described acid comprises the combination of one or more in acetic acid, hydrochloric acid and Citric Acid; Described three oxygen base hydrogen silanes comprise trimethoxy hydrogen silane or triethoxy hydrogen silane.
3. preparation method according to claim 1 and 2, is characterized in that, the end group of described silane coupling agent is blocked allyl alcohol polyoxyalkyl ether; The molecular structural formula of described blocked allyl alcohol polyoxyalkyl ether is: CH
2=CH-CH
2o (CH
2cH
2cH
2o)
m-(CH
2cH
2o)
noR', R' represent-CH
3,-C
2h
5,-OC
2h
4oCH
3,-OSi (CH
3)
3in any one, and 0≤m≤20,0≤n≤20, m+n>=1, m and n is integer;
The structural formula of described three oxygen base hydrogen silanes is:
R represents-CH
3or-C
2h
5.
4. the preparation method according to any one of claim 1-3, is characterized in that, the structural formula of described silane coupling agent is:
R represents-CH
3or-C
2h
5, R' represents-CH
3,-C
2h
5,-OC
2h
4oCH
3,-OSi (CH
3)
3in any one, and 0≤m≤20,0≤n≤20, m+n>=1, m and n is integer.
5. the preparation method according to any one of claim 1-4, is characterized in that, the structural formula of the nano silicon oil-displacing agent of described end capped polyether modification is:
R' represents-CH
3,-C
2h
5,-OC
2h
4oCH
3,-OSi (CH
3)
3in any one, and 0≤m≤20,0≤n≤20, m+n>=1, m and n is integer.
6. the preparation method according to any one of claim 1-5, is characterized in that, the described temperature preparing nanosilica solution reaction is 60-90 DEG C, and the time is 5-10 hour.
7. the preparation method according to any one of claim 1-6, is characterized in that, the temperature of described linked reaction is 80-95 DEG C, and the time is 3-9 hour.
8. the preparation method according to any one of claim 1-7, is characterized in that, the temperature of described modified-reaction is 60-90 DEG C, and the time is 3-8 hour.
9. the nano silicon oil-displacing agent of the end capped polyether modification that the preparation method according to any one of claim 1-8 obtains, is characterized in that, the particle diameter of described nano silicon is 5-100nm.
10. the application of nano silicon oil-displacing agent in tertiary oil recovery of end capped polyether modification according to claim 9, is characterized in that, the consumption of the nano silicon oil-displacing agent of described end capped polyether modification is more than 0.1%.
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| CN106832417A (en) * | 2017-03-14 | 2017-06-13 | 北京化工大学 | Using aliphatic APEO modified white carbon black and its with rubber combined method |
| CN113136193A (en) * | 2021-04-23 | 2021-07-20 | 西南石油大学 | High-activity nano oil displacement agent and preparation method thereof |
| CN114835866A (en) * | 2022-07-01 | 2022-08-02 | 山东科兴化工有限责任公司 | Nano microemulsion oil displacement agent for low-permeability oil reservoir and preparation method thereof |
| CN115772397A (en) * | 2021-09-08 | 2023-03-10 | 中国石油化工股份有限公司 | Temperature-resistant salt-resistant thick oil viscosity reducer composition and preparation method and application thereof |
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| CN115772397A (en) * | 2021-09-08 | 2023-03-10 | 中国石油化工股份有限公司 | Temperature-resistant salt-resistant thick oil viscosity reducer composition and preparation method and application thereof |
| CN114835866A (en) * | 2022-07-01 | 2022-08-02 | 山东科兴化工有限责任公司 | Nano microemulsion oil displacement agent for low-permeability oil reservoir and preparation method thereof |
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