CN104449636B - Oil displacement agent of recovery ratio and preparation method thereof is improved suitable for high temperature and high salt harshness oil reservoir - Google Patents

Oil displacement agent of recovery ratio and preparation method thereof is improved suitable for high temperature and high salt harshness oil reservoir Download PDF

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CN104449636B
CN104449636B CN201310435366.7A CN201310435366A CN104449636B CN 104449636 B CN104449636 B CN 104449636B CN 201310435366 A CN201310435366 A CN 201310435366A CN 104449636 B CN104449636 B CN 104449636B
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oil
monomer
water
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temperature
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CN104449636A (en
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夏燕敏
许汇
苏智青
于志省
蔡红
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/58Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
    • C09K8/584Compositions 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/58Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
    • C09K8/588Compositions 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

Abstract

The present invention relates to a kind of oil displacement agents that recovery ratio is improved suitable for high temperature and high salt harshness oil reservoir and preparation method thereof, mainly solve the oil displacement agent temperature-resistant anti-salt in the prior art containing polymer and performance steady in a long-term is poor, it is impossible to the problem of meeting tertiary oil recovery requirement.The present invention is by using in displacement of reservoir oil temperature>90 DEG C, total salinity is more than 180000mg/L, under injection water condition of the total amount more than 5000mg/L of calcium ion and magnesium ion, underground dewatered oil is contacted with oil displacement agent, mother oil displacement in rock core is come out, wherein the oil displacement agent is by weight percentage, including following component:(1) 0.01~3.0% both sexes hydrophobically associated polyacrylamide;(2) 0.01~5.0% aliphatic alcohol polyoxyethylene sulfonate surfactant;(3) 92.0~99.98% injection water;Technical solution, preferably resolve the problem, available for high temperature and high salt harshness oil reservoir improve recovery ratio oil displacement agent industrial production and application.

Description

Oil displacement agent of recovery ratio and preparation method thereof is improved suitable for high temperature and high salt harshness oil reservoir
Technical field
The present invention relates to a kind of oil displacement agents that recovery ratio is improved suitable for high temperature and high salt harshness oil reservoir and preparation method thereof.
Background technology
By primary, secondary oil recovery, crude oil water content is continuously increased domestic each elephant, and part elephant successively enters three The secondary oil recovery stage.Polymer flooding is the main technique methods of tertiary oil recovery, and mechanism of oil displacement understands that technique is relatively easy, technology day Become ripe, be an effective raising recovery efficiency technique measure.The mechanism of oil displacement of polymer mainly utilizes water-soluble polypropylene The viscosity of amide molecule chain improves the mobility ratio of displacing fluid, displacement efficiency and swept volume is improved, so as to reach raising recovery ratio Purpose.Since the tertiary oil recovery period is long, deep layer oil temperature is high, and therefore, polymer used for tertiary oil recovery must have good increasing Viscous, heatproof, salt resistance, shear resistant, and performance is steady in a long-term.
Early stage is usually used in enhanced oil recovery(EOR)The industrial products of polymer flooding only have partially hydrolyzed polyacrylamide (PHPA) (PAM), it reaches thickening dependent on the ion in high molecular weight and polymer molecular chain and the repulsive interaction of highly polar side group Effect.But heavy polymer is when by larger stretching and shear stress, it is prone to mechanical degradation and lose viscous Degree, it is particularly evident during injection of polymer in low-permeability rock stratum.Cation in aqueous solution, especially divalent ion can shield The ionic group in polymer is covered, crimps polymer molecular chain, hydrodynamic volume, which reduces, even to be precipitated, so as to make tackifying It substantially reduces.When depth of stratum is up to 20000 feet, reservoir temperature is higher(About 100 DEG C), the acyl in polyacrylamide (PAM) Amido facile hydrolysis in high temperature aqueous solution, makes the salt-resistance of polymer solution drastically decline.In recent years, related temperature-resistant and anti-salt type gathers The research of acrylamide mainly by introduce big side group on main polymer chain or rigid side group improve polymer thermal stability, Introduce the monomer for inhibiting hydrolysis or the monomer insensitive to the salt hydrolysis and anti-salt property that are copolymerized to improve polymer or Improve the temperature-resistant anti-salt performance of polymer by the heat resistance and salt tolerance of hydrophobic grouping.But due to the quality or valency of comonomer Lattice cause polymer to be difficult to reach high molecular weight or product and have higher cost, are answered in industrial production or tertiary oil recovery is practical With can be somewhat limited.At present in tertiary oil recovery, the polymer that can meet temperature-resistant anti-salt requirement is seldom, is not that price is too high It is exactly that performance is unstable, cannot particularly meets more than salinity 100000mg/L, the requirement of 85 DEG C or more high temperature.
Hydrophobic associated water-soluble polymer refers to carry the one of a small amount of hydrophobic grouping on polymer hydrophilicity macromolecular chain Class water-soluble polymer.It, should as novel polymeric oil-displacing agent due to the SOLUTION PROPERTIESs such as its unique thickening, salt resistance, anti-shearing It has a good application prospect for high salt, high shear oil reservoir development.It is given birth to because of hydrophobic grouping is introduced in polymer molecule Into hydrophobic association type copolymer, its hydrophobic chain link is assembled and associates to be similar in a manner of surfactant in aqueous medium, Effective hydrodynamic volume increase of a macromolecular ball of string, aqueous medium viscosity improve, and larger side group plays polymer molecule backbone To shielding action, weaken the p- COO of salt ionThe influence of group;And larger side group also there is certain steric hindrance to imitate Should, enhance chain rigidity.
But it is existing research shows that conflicting between the associative ability and water solubility of such polymer, good water solubility is gathered The carbochain for closing object often hydrophobic monomer is shorter or content is relatively low, associating effect unobvious, need to be under higher polymer concentration It shows certain association effect and meets heat and salinity tolerance performance;And the polymer associate of the hydrophobic monomer containing long-chain or high-content Very capable, heat and salinity tolerance performance is good, but poorly water-soluble, and generally requiring long time can just be completely dissolved, and lose industry Change the value of application.How ideal equalization point is found between, be that can such polymer be widely used in three times The key of oil recovery process.
The country has carried out numerous studies in terms of hydrophobic associated polymer, wherein Southwest Petroleum Institute, Chengdu Univ. of Science & Technology, Petrochina exploration and development research institute, University of Petroleum, Northcentral University etc. achieve preferable progress and achievement.
Feng Rusen etc.(CN1793189A)Using micella copolymerization method synthesized containing acrylamide, sodium acrylate and pi-allyl- The hydrophobic associated polymer of three kinds of structural units of alkyl phenyl ether, although there is preferable Efficient Adhesive Promotion, pi-allyl-alkyl phenyl The synthesis of ether monomer is complex;Zhong Chuanrong etc.(CN101293944A、CN 101148582A)The virtue of condensed ring containing vinyl is synthesized Hydrophobic associated polymer of the hydrocarbon as hydrophobic monomer, the polymerization process time is longer, only have rated at 45 DEG C polymer in fresh water and Efficient Adhesive Promotion in brine, salt resistance effect assessment NaCl concentration<100000mg/L、CaC12Concentration<The situation of 1000mg/L; Ou Yangjian etc.(CN1317501)High-molecular hydrophobic associated polymer, in 75 DEG C of total salinity 12000mg/L, wherein Ca2+With Mg2+For 300mg/L, sample concentration 1500mg/L, using Brookfield viscometer, shear rate 36.7s-1Viscosity for 15.6 ~ 12.4mPa.s;Hole beautiful jade etc.(CN1528734、CN1528797)The super high molecular weight water insoluble hydrophobic containing fluorocarbon group has been synthesized to form Mould assembly polymer has rated it in triumph brine(Total salinity 6000mg/L, calcium ions and magnesium ions 500mg/L)Increasing under the conditions of 70 DEG C Viscosity, wherein fluorinated acrylate hydrophobic monomer is expensive;Jiang Liding(The synthesis of new family hydrophobic association polyacrylamide And its rheological property of aqueous solution, Master's thesis in 2007)Using surface active monomer NaAMC14S and AM aqueous solutions are homogeneously copolymerized The method of conjunction has been successfully prepared the copolymer NaAMC with hydrophobic block structure14S/AM overcomes micellar co-polymerization using general Several shortcomings caused by logical surfactant, copolymer NaAMC14The length of hydrophobic micro- block of S/AM can be outer by adjusting The dosage of electrolyte is added to control, but research work biases toward theory, not the evaluation result under the conditions of practical oil field mineral reserve.
The studies above is made a general survey of, the current synthetizing hydrophobic associated most common method of polymer is micellar free radical copolymerization method, is adopted It needs to add in a large amount of surfactant when with such method being polymerize(Such as SDS)Make hydrophobic monomer solubilising in micella, but poly- Add in a large amount of surfactant during closing has significant impact to the association behavior of polymer, these surfactants are poly- It closes in product and interacts with hydrophobic segment, deteriorate the performance of hydrophobic associated water-soluble polymer.If remove these tables Face activating agent can increase the complexity of the last handling processes such as separation and purifying.In order to simplify last handling process and enhance polymer Dissolubility, can be used inherently have surface-active hydrophobic monomer.This kind of monomer contains hydrophobic grouping and hydrophilic simultaneously Group does not need to additionally incorporate surfactant in combined polymerization, can directly use traditional free yl solution polymerization, and It can make hydrophobic monomer is highly disordered to be irregularly introduced into copolymer.But there are research in foreign countries(Ezzell,S.A.,McCormick, C.L., Macromolecules 1992,25(7), 1881~1886)It was found that the copolymer of this kind of ionic hydrophobic monomer exists Critical association concentration in aqueous solution is the 2 times or more of the identical Hydrophobic chain length of micella copolymer, this point polymerize hydrophobic association The application of object industrially is totally unfavorable.It can be seen that both at home and abroad researcher to the structure of hydrophobic associated water-soluble polymer, Property, viscosifying mechanisms and application have done numerous studies, have explored work, but the evaluation of polymer is essentially according to grand celebration or Shengli Oil Field Certain mineral reserve conditions, temperature and salinity are all not belonging to high temperature and high salt type, for more than salinity 100000mg/L, 85 DEG C or more The condition of high temperature is almost without being related to.
The present invention is to the synthesis of ionic, both sexes hydrophobic associated water-soluble polymer and hydrophobically modified polyelectrolyte, knot It is opposite to that using the monomer with surface-active on the basis of carrying out extensive, in-depth study in terms of structure characterization and SOLUTION PROPERTIES Interaction between the ionic comonomer of charge first, ionic comonomer has solubilization to surface active monomer, is not required to Separately add surfactant during polymerization, second is that both sexes hydrophobic associated polymer can be formed, even if under hydrophobic monomer lower content Polymer also has high-effective viscosity and excellent heatproof, salt resistance and long-time stability, and is not required to rear hydrolytic process, not only helps In long-term ageing property, energy consumption is also reduced, and does not influence the dissolubility of product;It adds in the drying process a certain amount of Steady agent and surfactant are glued, the dissolving of polymer is not only helped and plays collaboration tackifying effect, yet further enhance anti- Ageing properties.Polymer mobility control agent of the present invention suitable for high temperature and high salt harshness oil reservoir has high tackifying, just The quick property of salt(Meet salt retrogradation), a certain range of positive Thermo-sensitive(Heat up retrogradation)With relatively low critical micelle concentration and excellent Long-term ageing is suitable for requirement of the total salinity more than the harsh oil reservoir oil displacement of 100,000 mg/L, temperature more than 85 DEG C, three times It has a good application prospect in petroleum production engineering.The polymer system of the present invention for being just suitable for high temperature and high salt harshness oil reservoir Preparation Method, binary be compound and its application in tertiary oil recovery.
Invention content
The first technical problem to be solved by the present invention is the oil displacement agent high temperature resistant in the prior art containing polymer The problem of anti-high salinity and long-time stability can meet tertiary oil recovery requirement, provides a kind of harsh suitable for high temperature and high salt Oil reservoir improves the oil displacement agent of recovery ratio, which has high-effective viscosity, temperature-resistant anti-salt(A certain range of chance salt retrogradation rises Warm retrogradation), long-time stability the features such as.
The second technical problem to be solved by the present invention is to provide a kind of system for solving the oil displacement agent in one of technical problem Preparation Method, this method have that polymerisation process is simple, without detach, purify and after hydrolyze, reduce cost the advantages of.
One of in order to solve the above-mentioned technical problem, the present invention is as follows using following technical scheme:It is high that one kind is suitable for high temperature Salt harshness oil reservoir improves the oil displacement agent of recovery ratio, in displacement of reservoir oil temperature>90 DEG C, total salinity about 180000mg/L, calcium ion and Under injection water condition of the total amount of magnesium ion more than 5000mg/L, underground dewatered oil is made to be contacted with oil displacement agent, it will be in rock core The abundant displacement of crude oil comes out, wherein the oil displacement agent includes following component by weight percentage:
(1) 0.01~3.0% both sexes hydrophobically associated polyacrylamide;
(2) 0.01~5.0% aliphatic alcohol polyoxyethylene sulfonate surfactant;
(3) 92.0~99.98% injection water;
Wherein (1) component both sexes hydrophobically associated polyacrylamide presses GBT12005.10-92 Molecular Weight for Polyacrylamide Mw It measures(Viscosimetry)Intrinsic viscosity is measured, and by [η]=3.73 × 10-4Mw0.66Molecular weight is calculated between 200-2000 ten thousand, It is 1500mg/L in the aqueous solution of 5700mg/L in the total amount that total salinity is 180000mg/L, wherein calcium ion and magnesium ion Polymer concentration solution is in 95 DEG C, 7.34s-1Under apparent viscosity be 120~780mps.
In above-mentioned technical proposal, displacement of reservoir oil temperature is preferably 85~95 DEG C, and the injection water total salinity is preferably The total amount of 100000~250000 mg/L, calcium ion and magnesium ion preferably 2000~7000 mg/L;Polymer is selected from above-mentioned Both sexes hydrophobically associated polyacrylamide, surfactant are selected from aliphatic alcohol polyoxyethylene sulfonate, and ethoxy group number n is preferred It is 2~18.
This flooding method concrete operation step includes the following steps:
(a) water, nonionic water-soluble monomers, anionic monomer or/and cationic monomer are added in a kettle, are had The auxiliary agents such as the hydrophobic monomer and inorganic matter of surface-active;
(b) composite initiation system of part is added in, is stirred evenly, forms solution;
(c) pH value of solution is adjusted to 7 ~ 10, and is passed through nitrogen, and temperature in the kettle is down to 10 ~ 30 DEG C, then adds in it Remaining composite initiator continues after being passed through nitrogen, sealing;
(d) reaction temperature is gradually increased to 40 ~ 60 DEG C after 0.5 ~ 1 hour, after reacting 2 ~ 8 hours, obtains gel polymerization Product;
(e) cut and add in after glue containing the drying aids for gluing steady agent and aqueous surfactant solution, after stirring evenly 80~ Forced air drying 1~3 hour at 95 DEG C, certain particle size is crushed to pulverizer or roller, obtains being suitable for high temperature and high salt harshness The polymer mobility control agent of oil reservoir.
(f) by the desired amount of both sexes hydrophobic associated polymer, above-mentioned aliphatic alcohol polyoxyethylene sulfonate and injection Water uniformly mixes, and 5 ~ 35 DEG C are stirred 1~3 hour, obtain required composition, by weight percentage, both sexes hydrophobic association type Polymer, aliphatic alcohol polyoxyethylene sulfonate and inject the proportioning of water for 0.01~3.0%: 0.01~5.0%: 92.0~ 99.98;
(g) first using total salinity as 100000~250000mg/L, Ca2++Mg2+Injection water for 2000~7000mg/L By rock core saturation, the pore volume (PV) of rock core is measured, saturation is then carried out with dewatered oil, is carried out at a temperature of 85~95 DEG C Imitation oil displacement experiment is tested:First water drive is to aqueous 92%, the displacement of reservoir oil composition of metaideophone 0.3pv (rock pore volume) step (f) synthesis Afterwards, water drive calculates the percentage for improving oil recovery factor to aqueous 99%.
In above-mentioned technical proposal, preferred embodiment for composite initiator in terms of whole weight percent monomers, comprising with the following group Point:(a) 0.003~0.5% persulfate;(b) 0.003~0.5% sulphite or acid sulphite;(c) 0.003~1% by NR1R2R3Tertiary amine compounds of representative or by N+R4R5R6R7Quaternary ammonium compounds of representative or by NH2R8 The fat amine compound of representative, R in formula1~R7It is selected from C1~C14Linear or branched alkyl group or alkyl derivative, R8Selected from C1~ C18Linear or branched alkyl group or alkyl derivative;(d) 0.005~1% azo compound;(e) 0.01~10% urine Element, thiocarbamide;(f) 0.03~0.5% disodium ethylene diamine tetraacetate or diethylene triamine pentacetic acid (DTPA) sodium;(g) 0.03~0.5% Molecular weight regulator.The drying aids, in terms of association polymer whole weight percent monomer, including following components:(a) 0.1~20% viscous steady agent;(b) 0.1~20% surfactant;(c) 50~99% water.
In above-mentioned technical proposal, the hydrophobic monomer with surface-active for anionic surface activity monomer or sun from Subtype surface active monomer, anionic surface activity monomer are the acrylamide azanyl sulfonic acid that vinyl carbochain number is 8 ~ 18 Sodium, cationic surfactant monomer are the allyl alkyl ammonium chloride that vinyl carbochain number is 12 ~ 22;With surface-active Hydrophobic monomer is the mono-vinyl class compound selected from 8-22 carbon atom;The surfactant is lived selected from anionic surface At least one of property agent, cationic surface active agent, nonionic surface active agent, anionic surfactant is C8-16 sodium alkyl sulfates, C8-16 sodium alkyl benzene sulfonates;The cationic surface active agent is C8-16 alkyl trimethyl bromines (Chlorine)Change ammonium;Non-ionic is alkyl phenol polyoxyethylene ether(EO=4~30);Composite hydrolysis agent, the Compound Water can also be added in Agent is solved, in terms of association polymer whole weight percent monomer, including following components:
(a) at least one of 0~20% sodium hydroxide or sodium carbonate;
(b) 0.5 ~ 50% surfactant;The surfactant is selected from anionic surfactant, cationic table At least one of face activating agent, nonionic surface active agent, anionic surfactant for C8-16 sodium alkyl sulfates, C8-16 sodium alkyl benzene sulfonates;The cationic surface active agent is C8-16 alkyl trimethyl bromines(Chlorine)Change ammonium;It is non-ionic For alkyl phenol polyoxyethylene ether(EO=4~30).
Oil displacement agent of the present invention that recovery ratio is improved suitable for high temperature and high salt harshness oil reservoir and preparation method thereof, due to The ion monomer opposite with having surface active monomer ion characteristic is employed, the interaction of the two has surface active monomer Solubilization is not required to separately add surfactant in polymerization;And even if obtained both sexes hydrophobic association polymerize in hydrophobic monomer Polymer also has excellent temperature-resistant anti-salt, thermostabilization and anti-shear performance under lower content;And employ composite initiation System, it is and matched with preferred technique, therefore reacting balance, be conducive to chain growth, molecular weight of product is controllable, and is not required to rear water Solution preocess not only helps long-term ageing property, also reduces energy consumption, and does not influence the dissolubility of product;Dried A certain amount of viscous steady agent and surfactant are added in journey, the dissolving of polymer is not only helped and plays collaboration tackifying effect, Yet further enhance anti-aging property.It is harsh oily using high temperature and high salt is suitable for made from preparation process provided by the present invention Both sexes hydrophobically associated polyacrylamide of Tibetan and preparation method thereof, molecular weight is adjustable between 200 ~ 20,000,000, in high temperature height Excellent tackifying effect is shown under salinity, the dense curve that glues of polymer is shown, both sexes hydrophobic associated polymer compound tool Have a stronger association, viscosity amplification up to two to three orders of magnitude, and critical micelle concentration appear in 2000mg/L with Under;Polymer under salinity there is salt to viscosify effect more than 100,000, and viscosity-temperature curve shows polymer viscosity at 60~80 DEG C Significantly increase, though have later decline but still it is higher than the viscosity before 60 DEG C;By polymer with still having after surfactant compound Thickening, drop tension, temperature-resistant anti-salt and long-term anti-ageing performance.
It is using the present invention suitable for raising recovery ratio oil displacement agent of high temperature and high salt harshness oil reservoir and preparation method thereof, can use In formation temperature 85~95, total salinity be 100000~250000 mg/L, the total amount of calcium ion and magnesium ion for 2000~ The crude oil and water of the Zhongyuan Oil Field of 7000 mg/L etc., with dosage 0.1~0.3wt% both sexes hydrophobically associated polyacrylamide with 0.1~0.3wt% aliphatic alcohol polyoxyethylene sulfonates formed above-mentioned composition oil displacement agent, determine the oil displacement agent aqueous solution with Dynamical interfacial tension value between the Pu xi Area crude oil of Zhongyuan Oil Field, up to 10-3~10-4The ultralow interfacial tension of mN/m, through object The oil displacement agent can (water drive improves crude oil and adopts reason simulation displacement experiment Lab-evaluation on the basis of water drive on high temperature, high salinity reservoir Yield achieves preferable technique effect up to oil recovery factor 43.6%) is improved up to 16.8%.
Below by specific embodiment, the present invention will be further elaborated.
Specific embodiment
【Embodiment 1】
(1)It first adds in 2500g deionized waters in a kettle, adds in 430g acrylamides(AM), 2- acrylamidos- 2- methyl propane sulfonic acids(AMPS)150g, 3.5g2- acrylamido myristyl sodium sulfonate(NaAMC14S), 4.5g acryloyl-oxy second Base trimethyl ammonium chloride(DAC), neutrality is neutralized to NaOH, then adds in disodium ethylene diamine tetraacetate 0.04g, urea 7g, different Propyl alcohol 0.07g, stirring is to being completely dissolved.With NaOH pH value is adjusted to 8.9, and start to be passed through high pure nitrogen, it will be in kettle after 30min Temperature is down to 15 DEG C, then sequentially adds 0.2% aqueous solution of sodium bisulfite 10g, 0.5% methacrylic acid N, N- dimethylamino Ethyl ester(DMAEMA)Aqueous solution 10g, 0.5% azo diisobutyl amidine hydrochloride 10g, 0.3% persulfate aqueous solution 10g, It is sealed after continuing logical nitrogen 30min.Reaction temperature is gradually increased to 52 DEG C after 1 hour, reaction obtains gel after 3.5 hours and gathers Product is closed, cuts the drying aids 300g aqueous solutions of addition lauryl sodium sulfate containing 25g and 30g thiocarbamides after glue, the drum under 90 oC Dry 1.5h is air-dried, sampling analysis after smashing screening with pulverizer.By GB/T12005.2-89 polyacrylamides determination of solid content side Method test solid content is 89.9%, when testing dissolving by GB/T12005.8-89 powdered polypropylene amide measuring of dissolution velocity method Jian≤90min is measured by GB/T12005.10-92 Molecular Weight for Polyacrylamide(Viscosimetry)Measure intrinsic viscosity, and by [η]= 3.73×10-4Mw0.66It is 8,320,000 to calculate molecular weight.Apparent viscosity is in 95 DEG C, brine total salinity 180000mg/L, Ca2++Mg2 +:1500mg/L polymer concentrations solution under 5700 mg/L, using Haake torque rheometer, concentric drums shear rate 7.34s-1Under Apparent viscosity is 180mPas.
By synthesized both sexes hydrophobically associated polyacrylamide 0.10wt%, above-mentioned fatty alcohol polyoxyethylene ether sulfonic acid Salt(n=14)0.30wt% and 99.6wt% Zhongyuan Oil Fields Pu xi Areas injection water uniformly mixes, and 20 DEG C are stirred 2 hours, obtain institute The oil displacement agent needed.In 95 DEG C of temperature, salinity 180000mg/L, Ca2++Mg2+In the water of 5700mg/L, this composition is measured Apparent viscosity is 126mPa.s.;The super of 0.0065mN/m is formed between the composition and Zhongyuan Oil Field Pu xi Area dewatered oils Low interfacial tension.Apparent viscosity is by the III type rheometer measurements of MARS of German Haake companies, and interfacial tension is by U.S. De Kesa The TX500 types rotating interfacial tensimeter of this university production measures.
First with salinity 180000mg/L, Ca2++Mg2+By rock core, (length is 30 centimetres to the injection water of 5700mg/L, directly Diameter is 2.5 centimetres, and permeability is 1.5 microns2) saturation, the pore volume (PV) for measuring rock core is 16.2%, then with Crude Oil Field Pu xi Areas dewatered oil carries out saturation, and imitation oil displacement experiment experiment is carried out under 95 DEG C of constant temperature:First water drive is measured to aqueous 92% After water drive improves oil recovery factor 48.6%, then the displacement of reservoir oil composition of metaideophone 0.3pv (rock pore volume) step (f) synthesis, For water drive to aqueous 99%, oil recovery factor 15.9% can be improved again on the basis of water drive by measuring.
【Embodiment 2】
It first adds in 2600g deionized waters in a kettle, adds in 480g acrylamides(AM), 2- acrylamidos -2- Methyl propane sulfonic acid(AMPS)130g, 4.0g2- acrylamido dodecyl sodium sulfate(NaAMC12S), 7.8g methacryloxypropyls Ethyl-trimethyl salmiac(DMC)With 5.0g nitrogen vinyl pyrrolidones(NVP), neutrality is neutralized to NaOH, then adds in second Edetate disodium 0.045g, urea 7.0g, isopropanol 0.06g, stirring is to being completely dissolved.PH value is adjusted to 9.0 with NaOH, And start to be passed through high pure nitrogen, temperature in the kettle is down to 16 DEG C after 30min, then sequentially add 0.2% sodium hydrogensulfite it is water-soluble Liquid 10.2g, 0.5% acrylic acid N, N- dimethylaminoethyl(DA)Aqueous solution 11g, 0.5% azo diisobutyl amidine hydrochloride 11.9g, 0.3% persulfate aqueous solution 11.2g are sealed after continuing logical nitrogen 30min.Reaction temperature is gradually risen after 1 hour To 58 DEG C, reaction obtains gel polymerizate after 3 hours, and neopelex containing 51g, 6g isopropanols are added in after cutting glue With the 300g aqueous solutions of 45g sodium sulfites, the forced air drying 1h under 95oC, sampling analysis after smashing screening with pulverizer.By GB/ T12005.2-89 polyacrylamide determination of solid content method test solid content is 88.7%, is gathered by GB/T12005.8-89 powderies Acrylamide measuring of dissolution velocity method test Rong solution Shi Jian≤90min, by GB/T12005.10-92 Molecular Weight for Polyacrylamide It measures(Viscosimetry)Intrinsic viscosity is measured, and by [η]=3.73 × 10-4Mw0.66It is 8,460,000 to calculate molecular weight.Apparent viscosity is 95 DEG C, brine total salinity 180000mg/L, Ca2++Mg2+:1500mg/L polymer concentrations solution under 5700 mg/L, using Haake Rheometer, concentric drums shear rate 7.34s-1Under apparent viscosity be 165Pas.
By synthesized both sexes hydrophobically associated polyacrylamide 0.10wt%, above-mentioned fatty alcohol polyoxyethylene ether sulfonic acid Salt(n=14)0.30wt% and 99.6wt% Zhongyuan Oil Fields Pu xi Areas injection water uniformly mixes, and 20 DEG C are stirred 2 hours, obtain institute The oil displacement agent needed.In 95 DEG C of temperature, salinity 180000mg/L, Ca2++Mg2+In the water of 5700mg/L, this composition is measured Apparent viscosity is 112mPa.s.;The super of 0.0073mN/m is formed between the composition and Zhongyuan Oil Field Pu xi Area dewatered oils Low interfacial tension.Apparent viscosity is by the III type rheometer measurements of MARS of German Haake companies, and interfacial tension is by U.S. De Kesa The TX500 types rotating interfacial tensimeter of this university production measures.
First with salinity 180000mg/L, Ca2++Mg2+By rock core, (length is 30 centimetres to the injection water of 5700mg/L, directly Diameter is 2.5 centimetres, and permeability is 1.5 microns2) saturation, the pore volume (PV) for measuring rock core is 15.5%, then with Crude Oil Field Pu xi Areas dewatered oil carries out saturation, and imitation oil displacement experiment experiment is carried out under 95 DEG C of constant temperature:First water drive is measured to aqueous 92% After water drive improves oil recovery factor 43.7%, then the displacement of reservoir oil composition of metaideophone 0.3pv (rock pore volume) step (f) synthesis, For water drive to aqueous 99%, oil recovery factor 15.4% can be improved again on the basis of water drive by measuring.
【Embodiment 3】
It first adds in 2700g deionized waters in a kettle, adds in 500g acrylamides(AM), 2- acrylamidos -2- Methyl propane sulfonic acid(AMPS)150g, 5.2g2- acrylamido sodium cetanesulfonate(NaAMC16S)With 9.4g dimethyl diene Propyl ammonium chloride(DMDAAC), neutrality is neutralized to NaOH, then adds in disodium ethylene diamine tetraacetate 0.05g, urea 8.0g, different Propyl alcohol 0.07g, stirring is to being completely dissolved.With NaOH pH value is adjusted to 9.5, and start to be passed through high pure nitrogen, it will be in kettle after 30min Temperature is down to 20 DEG C, then sequentially adds 0.2% aqueous solution of sodium bisulfite 10.2g, 0.5% acrylic acid N, N- dimethylamino second Ester(DA)Aqueous solution 12.1g, 0.5% 2,2'- azos [2- (2- imidazoline -2- bases) propane] dihydrochloride 12g, 0.3% mistake Potassium sulfate solution 11g is sealed after continuing logical nitrogen 30min.Reaction temperature is gradually increased to 55 DEG C after 1 hour, reaction 2.5 is small When after obtain gel polymerizate, cut and the 300g water containing 38gOP-20,20g thiocarbamide and 5g 1-hydroxy ethylidene-1,1-diphosphonic acids added in after glue Solution, the forced air drying 2h under 85oC, sampling analysis after smashing screening with pulverizer.By GB/T12005.2-89 polyacrylamides Determination of solid content method test solid content is 90.3%, by GB/T12005.8-89 powdered polypropylene amides measuring of dissolution velocity side Method test Rong solution Shi Jian≤90min, are measured by GB/T12005.10-92 Molecular Weight for Polyacrylamide(Viscosimetry)Characteristic is measured to glue Number, and by [η]=3.73 × 10-4Mw0.66It is 9,060,000 to calculate molecular weight.Apparent viscosity is in 95 DEG C, brine total salinity 180000mg/L, Ca2++Mg2+:1500mg/L polymer concentrations solution under 5700 mg/L, using Haake torque rheometer, concentric drums Shear rate 7.34s-1Under apparent viscosity be 156Pas.
By synthesized both sexes hydrophobically associated polyacrylamide 0.10wt%, above-mentioned fatty alcohol polyoxyethylene ether sulfonic acid Salt(n=16)0.30wt% and 99.6wt% Zhongyuan Oil Fields Pu xi Areas injection water uniformly mixes, and 20 DEG C are stirred 2 hours, obtain institute The oil displacement agent needed.In 95 DEG C of temperature, salinity 180000mg/L, Ca2++Mg2+In the water of 5700mg/L, this composition is measured Apparent viscosity is 112mPa.s.;The super of 0.0058mN/m is formed between the composition and Zhongyuan Oil Field Pu xi Area dewatered oils Low interfacial tension.Apparent viscosity is by the III type rheometer measurements of MARS of German Haake companies, and interfacial tension is by U.S. De Kesa The TX500 types rotating interfacial tensimeter of this university production measures.
First with salinity 180000mg/L, Ca2++Mg2+By rock core, (length is 30 centimetres to the injection water of 5700mg/L, directly Diameter is 2.5 centimetres, and permeability is 1.5 microns2) saturation, the pore volume (PV) for measuring rock core is 16.6%, then with Crude Oil Field Pu xi Areas dewatered oil carries out saturation, and imitation oil displacement experiment experiment is carried out under 95 DEG C of constant temperature:First water drive is measured to aqueous 92% After water drive improves oil recovery factor 43.6%, then the displacement of reservoir oil composition of metaideophone 0.3pv (rock pore volume) step (f) synthesis, For water drive to aqueous 99%, oil recovery factor 16.8% can be improved again on the basis of water drive by measuring.
【Embodiment 4】
It first adds in 2600g deionized waters in a kettle, adds in 510g acrylamides(AM), 2- acrylamidos -2- Methyl propane sulfonic acid(AMPS)170g, 5.0g hexadecyldimethyl benzyl ammonium allyl ammonium chloride(C16DMAAC)With 7.8g methacrylic acids (MAA), neutrality is neutralized to NaOH, then adds in disodium ethylene diamine tetraacetate 0.048g, urea 7.5g, tert-butyl alcohol 0.08g are stirred It mixes to being completely dissolved.PH value is adjusted to 8.7 with NaOH, and starts to be passed through high pure nitrogen, and temperature in the kettle is down to 12 after 30min DEG C, then sequentially add 0.2% aqueous solution of sodium bisulfite 11.2g, 0.5% methacrylic acid N, N- dimethylaminoethyl (DMAEMA)Aqueous solution 12.6g, 0.5% azo diisobutyl amidine hydrochloride 12g, 0.3% persulfate aqueous solution 10.9g, It is sealed after continuing logical nitrogen 30min.Reaction temperature is gradually increased to 52 DEG C after 1 hour, reaction obtains gel polymerization after 3 hours Product cuts the 300g aqueous solutions of addition thiocarbamide containing 42gOP-1020g and 4g methenamines after glue, the forced air drying under 90oC 1.5h, sampling analysis after smashing screening with pulverizer.
It is 92.4% by GB/T12005.2-89 polyacrylamide determination of solid content method test solid content, by GB/ T12005.8-89 powdered polypropylene amide measuring of dissolution velocity method test Rong solution Shi Jian≤90min, by GB/T12005.10- 92 Molecular Weight for Polyacrylamide measure(Viscosimetry)Intrinsic viscosity is measured, and by [η]=3.73 × 10-4Mw0.66Calculating molecular weight is 8290000.Apparent viscosity is in 95 DEG C, brine total salinity 180000mg/L, Ca2++Mg2+:1500mg/L polymerize under 5700 mg/L Object strength solution, using Haake torque rheometer, concentric drums shear rate 7.34s-1Under apparent viscosity be 283Pas.
By synthesized both sexes hydrophobically associated polyacrylamide 0.10wt%, above-mentioned fatty alcohol polyoxyethylene ether sulfonic acid Salt(n=18)0.30wt% and 99.6wt% Zhongyuan Oil Fields Pu xi Areas injection water uniformly mixes, and 20 DEG C are stirred 2 hours, obtain institute The oil displacement agent needed.In 95 DEG C of temperature, salinity 180000mg/L, Ca2++Mg2+In the water of 5700mg/L, this composition is measured Apparent viscosity is 178mPa.s.;The super of 0.0082mN/m is formed between the composition and Zhongyuan Oil Field Pu xi Area dewatered oils Low interfacial tension.Apparent viscosity is by the III type rheometer measurements of MARS of German Haake companies, and interfacial tension is by U.S. De Kesa The TX500 types rotating interfacial tensimeter of this university production measures.
First with salinity 180000mg/L, Ca2++Mg2+By rock core, (length is 30 centimetres to the injection water of 5700mg/L, directly Diameter is 2.5 centimetres, and permeability is 1.5 microns2) saturation, the pore volume (PV) for measuring rock core is 12.9%, then with Crude Oil Field Pu xi Areas dewatered oil carries out saturation, and imitation oil displacement experiment experiment is carried out under 95 DEG C of constant temperature:First water drive is measured to aqueous 92% After water drive improves oil recovery factor 45.9%, then the displacement of reservoir oil composition of metaideophone 0.3pv (rock pore volume) step (f) synthesis, For water drive to aqueous 99%, oil recovery factor 14.8% can be improved again on the basis of water drive by measuring.
【Comparative example 1】
By 650g acrylamide monomers, disodium ethylene diamine tetraacetate 0.04g, urea 7g, isopropanol 0.07g adds in 2500g In deionized water, after stirring evenly dissolving completely, pH value is adjusted to 8.5 with NaOH solution.Then lead to nitrogen 30min, and by water Bath temperature is adjusted to 15 DEG C, then sequentially adds 0.2% aqueous solution of sodium bisulfite 10g, 0.5% methacrylic acid N, N- diformazan ammonia Base ethyl ester(DMAEMA)Aqueous solution 10g, 0.5% azo diisobutyl amidine hydrochloride 10g, 0.3% persulfate aqueous solution 10g is sealed after continuing logical nitrogen 30min.Reaction temperature is gradually increased to 50 DEG C after 1 hour, reaction obtains gel after 3 hours Polymerizate is cut and the hydrolytic reagent 730g aqueous solutions containing 37gNaOH is added in after glue, in 90 oC hydrolysis 2 hours, then 75 5h is dried in vacuo at DEG C, sampling analysis after smashing screening with pulverizer.
It is 88.92% by GBT12005.2-89 polyacrylamide determination of solid content method test solid content, presses GBT12005.6-89 partially hydrolyzed polyacrylamide (PHPA) degree of hydrolysis assay method test degree of hydrolysis is 11.3%, is pressed GBT12005.10-92 Molecular Weight for Polyacrylamide measures(Viscosimetry)Intrinsic viscosity is measured, and by [η]=3.73 × 10-4Mw0.66 It is 19,630,000 to calculate molecular weight.Apparent viscosity is in 95 DEG C, brine total salinity 180000mg/L, Ca2++Mg2+:Under 5700 mg/L 1500mg/L polymer concentration solution, using Haake torque rheometer, concentric drums shear rate 7.34s-1Under apparent viscosity be 2.5Pa·s。
Together【Embodiment 1】, measure water drive and improve oil recovery factor 48.6%, after the above-mentioned displacement of reservoir oil composition of metaideophone, measure Oil recovery factor 5.7% can be improved on the basis of water drive again.
【Comparative example 2】
By 450g acrylamides(AM), 200g2- acrylamido -2- methyl propane sulfonic acids(AMPS), ethylenediamine tetra-acetic acid two Sodium 0.04g, urea 7g, isopropanol 0.07g are added in 2500g deionized waters, after stirring evenly dissolving completely, are adjusted with NaOH PH value is to 9.0.Then lead to nitrogen 30min, and bath temperature is adjusted to 15 DEG C, then sequentially add 0.2% sodium hydrogensulfite water Solution 10g, 0.5% methacrylic acid N, N- dimethylaminoethyl(DMAEMA)Aqueous solution 10g, 0.5% azo diisobutyl amidine Hydrochloride 10g, 0.3% persulfate aqueous solution 10g are sealed after continuing logical nitrogen 30min.It is after 1 hour that reaction temperature is gradual 50 DEG C are risen to, reaction obtains gel polymerizate after 3 hours, and the hydrolytic reagent 500g aqueous solutions containing 25gNaOH are added in after cutting glue, In 90 oC hydrolysis 2 hours, 5h then is dried in vacuo at 75 DEG C, sampling analysis after smashing screening with pulverizer.
It is 87.34% by GBT12005.2-89 polyacrylamide determination of solid content method test solid content, presses GBT12005.6-89 partially hydrolyzed polyacrylamide (PHPA) degree of hydrolysis assay method test degree of hydrolysis is 12.6%, is pressed GBT12005.10-92 Molecular Weight for Polyacrylamide measures(Viscosimetry)Intrinsic viscosity is measured, and by [η]=3.73 × 10-4Mw0.66 It is 13,650,000 to calculate molecular weight.Apparent viscosity is in 95 DEG C, brine total salinity 180000mg/L, Ca2++Mg2+:Under 5700 mg/L 1500mg/L polymer concentration solution, using Haake torque rheometer, concentric drums shear rate 7.34s-1Under apparent viscosity be 7.6Pa·s。
Together【Embodiment 1】, measure water drive and improve oil recovery factor 43.7%, after the above-mentioned displacement of reservoir oil composition of metaideophone, measure Oil recovery factor 8.2% can be improved on the basis of water drive again.

Claims (3)

1. the oil displacement agent of recovery ratio is improved suitable for high temperature and high salt harshness oil reservoir, by the oil displacement agent in displacement of reservoir oil temperature>90 DEG C, total ore deposit Change degree is more than 180000mg/L, under injection water condition of the total amount more than 5000mg/L of calcium ion and magnesium ion, is dehydrated underground Crude oil is contacted with oil displacement agent, the abundant displacement of crude oil in rock core is come out, wherein the oil displacement agent wraps by weight percentage Include following component:
(1) 0.01~3.0% both sexes hydrophobically associated polyacrylamide;
(2) 0.01~5.0% aliphatic alcohol polyoxyethylene sulfonate surfactant;
(3) 92.0~99.98% injection water;
Wherein (1) component both sexes hydrophobically associated polyacrylamide is measured by GBT12005.10-92 Molecular Weight for Polyacrylamide Mw (viscosimetry) measures intrinsic viscosity, and by [η]=3.73 × 10-4Mw0.66Molecular weight is calculated between 200-2000 ten thousand, Total salinity is in the aqueous solution that the total amount of 180000mg/L, wherein calcium ion and magnesium ion is 5700mg/L, and 1500mg/L gathers Object strength solution is closed in 95 DEG C, 7.34s-1Under apparent viscosity be 150~780mps;Described is suitable for the harsh oil of high temperature and high salt The preparation method for the oil displacement agent for improving recovery ratio is hidden, is included the following steps:
(a) water, nonionic water-soluble monomers, anionic monomer or/and cationic monomer are added in a kettle, there is surface to live The hydrophobic monomer of property;
(b) composite initiation system of part is added in, is stirred evenly, forms solution;
(c) pH value of solution is adjusted to 7~10, and is passed through nitrogen, and temperature in the kettle is down to 10~30 DEG C, then adds in remaining Composite initiator continues after being passed through nitrogen, sealing;
(d) reaction temperature is gradually increased to 40~60 DEG C after 0.5~1 hour, after reacting 2~8 hours, obtains gel polymerization production Object;
(e) it is added in after cutting glue containing the drying aids for gluing steady agent and aqueous surfactant solution, at 80~95 DEG C after stirring evenly Lower forced air drying 1~3 hour, certain particle size is crushed to pulverizer or roller, obtains being suitable for high temperature and high salt harshness oil reservoir Both sexes hydrophobically associated polyacrylamide;
(f) it is the desired amount of both sexes hydrophobic associated polymer, above-mentioned aliphatic alcohol polyoxyethylene sulfonate and injection water is equal Even mixing, 5~35 DEG C are stirred 1~3 hour, obtain required composition, by weight percentage, the polymerization of both sexes hydrophobic association type The proportioning of object, aliphatic alcohol polyoxyethylene sulfonate and injection water is 0.01~3.0%: 0.01~5.0%: 92.0~99.98; Wherein, the both sexes hydrophobically associated polyacrylamide by the solution that following monomer or auxiliary agent form composite initiator presence Lower reaction is made;The solution of the monomer composition includes following components in terms of parts by weight:
A) 5~99.9 parts of nonionic water-soluble monomers;
B) 0~50 and more than 0 part of anionic monomer or/and cationic monomer;
C) 0.1~10 part of the hydrophobic monomer with surface-active;
D) 200~2000 parts of water;
Wherein, the composite initiator in terms of above-mentioned whole weight percent monomers, includes following components:(a) 0.003~ 0.5% persulfate;(b) 0.003~0.5% sulphite or acid sulphite;(c) 0.003~1% by NR1R2R3Tertiary amine compounds of representative or by N+R4R5R6R7Quaternary ammonium compounds of representative or by NH2R8The fatty amines of representative Compound, R in formula1~R7It is selected from C1~C14Linear or branched alkyl group or alkyl derivative, R8Selected from C1~C18Linear chain or branch chain Alkyl or alkyl derivative;(d) 0.005~1% azo compound;(e) 0.01~10% urea, thiocarbamide;(f)0.03 ~0.5% disodium ethylene diamine tetraacetate or diethylene triamine pentacetic acid (DTPA) sodium;(g) 0.03~0.5% molecular weight regulator;Institute Drying aids are stated, in terms of association polymer whole weight percent monomer, including following components:(a) 0.1~20% it is viscous steady Agent;(b) 0.1~20% surfactant;(c) 50~99% water;The hydrophobic monomer with surface-active is anion Type surface active monomer or cationic surfactant monomer, wherein, the anionic surface activity monomer is vinyl carbon Chain number is 8~18 acrylamide azanyl sodium sulfonate, and cationic surfactant monomer is that vinyl carbochain number is 12~22 Allyl alkyl ammonium chloride.
2. the oil displacement agent according to claim 1 that recovery ratio is improved suitable for high temperature and high salt harshness oil reservoir, it is characterised in that The surfactant is selected from aliphatic alcohol polyoxyethylene sulfonate type the moon-non-surface-active agent, general molecular formula RO (CH2CH2O)nCH2CH2SO3M, M are any one metal ion in potassium, sodium or lithium, R C9~C17Alkyl, n is second The adduction number of oxygen groups EO, value range are any one integer in 2~18.
3. the preparation method of the oil displacement agent described in claim 1 that recovery ratio is improved suitable for high temperature and high salt harshness oil reservoir, including Following steps:
(a) water, nonionic water-soluble monomers, anionic monomer or/and cationic monomer are added in a kettle, there is surface to live The hydrophobic monomer of property;
(b) composite initiation system of part is added in, is stirred evenly, forms solution;
(c) pH value of solution is adjusted to 7~10, and is passed through nitrogen, and temperature in the kettle is down to 10~30 DEG C, then adds in remaining Composite initiator continues after being passed through nitrogen, sealing;
(d) reaction temperature is gradually increased to 40~60 DEG C after 0.5~1 hour, after reacting 2~8 hours, obtains gel polymerization production Object;
(e) it is added in after cutting glue containing the drying aids for gluing steady agent and aqueous surfactant solution, at 80~95 DEG C after stirring evenly Lower forced air drying 1~3 hour, certain particle size is crushed to pulverizer or roller, obtains being suitable for high temperature and high salt harshness oil reservoir Both sexes hydrophobically associated polyacrylamide;
(f) it is the desired amount of both sexes hydrophobic associated polymer, above-mentioned aliphatic alcohol polyoxyethylene sulfonate and injection water is equal Even mixing, 5~35 DEG C are stirred 1~3 hour, obtain required composition, by weight percentage, the polymerization of both sexes hydrophobic association type The proportioning of object, aliphatic alcohol polyoxyethylene sulfonate and injection water is 0.01~3.0%: 0.01~5.0%: 92.0~99.98.
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