CN104449636A - Oil-displacing agent applied to high-temperature high-salt harsh oil deposit for improving oil recovery and preparation method of oil-displacing agent - Google Patents
Oil-displacing agent applied to high-temperature high-salt harsh oil deposit for improving oil recovery and preparation method of oil-displacing agent Download PDFInfo
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Abstract
The invention relates to an oil-displacing agent applied to high-temperature high-salt harsh oil deposit for improving oil recovery and a preparation method of the oil-displacing agent. The problems in the prior art that a polymer-containing oil-displacing agent is poor in temperature resistance, salt resistance and long-term stability and the tertiary oil recovery requirement cannot be met are mainly solved. With the adoption of the technical scheme, under the injected water conditions that the oil displacement temperature is higher than 90 DEG C, the total salinity is larger than 180000mg/L, and the total amount of calcium ions and magnesium ions is larger than 5000mg/L, the underground dehydrated crude oil comes into contact with the oil-displacing agent, and crude oil in the rock core is displaced. The oil-displacing agent comprises the following components in percentage by weight: (1) 0.01-3.0 percent of amphoteric hydrophobically associating polyacrylamide; (2) 0.01-5.0 percent of aliphatic alcohol polyoxyethylene ether sulfonate surfactant; and (3) 92.0-99.98 percent of injected water. The problems are well solved, and the preparation method can be applied to industrial production and application of oil-displacing agents in the high-temperature high-salt harsh oil deposit for improving oil recovery.
Description
Technical field
The present invention relates to a kind of harsh oil reservoir of high temperature and high salt that is applicable to and improve oil-displacing agent of recovery ratio and preparation method thereof.
Background technology
Domestic each elephant through once, secondary oil recovery, crude oil water content constantly increases, and part elephant successively enters tertiary phase.Polymer flooding is the main technique methods of tertiary oil recovery, and oil-displacement mechanism is clear, and technique is relatively simple, and technology reaches its maturity, and is one and effectively improves recovery efficiency technique measure.The oil-displacement mechanism of polymkeric substance mainly utilizes the viscosity of water-soluble polyacrylamide molecular chain, improves the mobility ratio of displacing fluid, improves efficiency of displacement and swept volume, thus reaches the object improving recovery ratio.Because the tertiary oil recovery cycle is long, deep layer oil temperature is high, and therefore, polymkeric substance used for tertiary oil recovery must have good thickening, heatproof, anti-salt, shear resistant, and performance is steady in a long-term.
The Industrial products being usually used in the polymer flooding of enhanced oil recovery (EOR) in early days only have partially hydrolyzed polyacrylamide (PAM), and it depends on the repulsive interaction of ion on high molecular and polymer molecular chain and strong polarity side base and reaches Efficient Adhesive Promotion.But high-molecular weight polymer, when being subject to larger stretching and shear-stress, is easy to mechano-degradation and loses viscosity occur, particularly evident during injection of polymer in low permeability rock stratum.Positively charged ion in the aqueous solution, especially divalent ion, the ionic group in meeting shielded polymer, makes polymer molecular chain curling, and hydrodynamic volume reduces even to precipitate, thus tackifying is reduced greatly.When depth of stratum reaches 20000 feet, reservoir temperature higher (about 100 DEG C), the facile hydrolysis in high-temperature water solution of the amide group in polyacrylamide (PAM), makes the salt resistance of polymers soln sharply decline.In recent years, about the research of temperature-resistant and anti-salt type polyacrylamide mainly through introducing the thermostability of large side base or rigidity side base raising polymkeric substance, the monomer of introducing suppression hydrolysis or carrying out copolymerization to improve hydrolysis and the anti-salt property of polymkeric substance to the insensitive monomer of salt on main polymer chain, or improve the temperature resistant antisalt performance of polymkeric substance by the heat resistance and salt tolerance of hydrophobic grouping.But make polymkeric substance be difficult to reach high molecular due to the quality of comonomer or price or product has higher cost, in industrial production or some restrictions can be subject in tertiary oil recovery practical application.In current tertiary oil recovery, the polymkeric substance that can meet temperature resistant antisalt requirement is little, be not price too higher position be unstable properties, particularly can not meet more than salinity 100000mg/L, the requirement of more than 85 DEG C high temperature.
Hydrophobic associated water-soluble polymer refers to the class water-soluble polymers with a small amount of hydrophobic grouping on polymer hydrophilicity macromolecular chain.Due to the thickening of its uniqueness, anti-salt, the SOLUTION PROPERTIES such as anti-shearing, be applied to high salt as novel polymeric oil-displacing agent, high-shear oil reservoir development has a good application prospect.The hydrophobic association type multipolymer generated because of introducing hydrophobic grouping in polymer molecule, in water medium, its hydrophobic chain link is assembled to be similar to tensio-active agent mode and to associate, effective hydrodynamic volume of a macromole ball of string increases, water medium viscosity improves, larger side base plays shielding effect to polymer molecule backbone, weakens the p-COO of salt ion
-the impact of group; And larger side base also has certain space steric effect, strengthen chain rigidity.
But now there are some researches show this base polymer associative ability and water-soluble between conflicting, the carbochain of the polymkeric substance of good water solubility often hydrophobic monomer is shorter or content is lower, associating effect is not obvious, just need show certain association effect and meet heat and salinity tolerance performance under higher polymer concentration; And the polymer associate containing the hydrophobic monomer of long-chain or high-content is very capable, heat and salinity tolerance performance is good, but poorly water-soluble, often need long time to dissolve completely, lose the value of industrial applications.How can find desirable trim point between, be the key that can this base polymer be widely used in tertiary oil recovery process.
Domesticly in hydrophobic associated polymer, carried out large quantity research, wherein Southwest Petroleum Institute, Chengdu Univ. of Science & Technology, exploratory development research institute of PetroChina Company Limited., University of Petroleum, Northcentral University etc. all achieve progress and achievement preferably.
Feng Rusen etc. (CN1793189A) have adopted micella copolymerization method to synthesize containing the hydrophobic associated polymer of acrylamide, sodium acrylate and allyl group-alkyl phenyl ether three kinds of structural units, although there is good Efficient Adhesive Promotion, the synthesis of allyl group-alkyl phenyl ether monomer is comparatively complicated; Zhong Chuanrong etc. (CN101293944A, CN 101148582A) have synthesized containing the hydrophobic associated polymer of vinyl condensed-nuclei aromatics as hydrophobic monomer, the polymerization process time is longer, only have rated the Efficient Adhesive Promotion of polymkeric substance in fresh water and salt solution at 45 DEG C, anti-salt effect assessment NaCl concentration <100000mg/L, CaC1
2the situation of concentration <1000mg/L; Ou Yangjian etc. (CN1317501) high-molecular hydrophobic associated polymkeric substance, at 75 DEG C of total mineralization 12000mg/L, wherein Ca
2+and Mg
2+for 300mg/L, sample concentration is 1500mg/L, and adopt Brookfield viscometer, shearing rate is 36.7s
-1viscosity is 15.6 ~ 12.4mPa.s; Kong Ying etc. (CN1528734, CN1528797) have synthesized the water-soluble hydrophobic associated type polymkeric substance of ultra-high molecular weight containing fluorocarbon group, have rated it at triumph salt solution (total mineralization 6000mg/L, calcium ions and magnesium ions 500mg/L) tackifying under 70 DEG C of conditions, wherein fluorinated acrylate hydrophobic monomer is expensive; Jiang Liding (synthesis of new gang hydrophobic association polyacrylamide and the rheological property of the aqueous solution thereof, Master's thesis in 2007) adopts surface active monomer NaAMC
14the method of S and AM aqueous solution homogeneous phase copolymerization has successfully prepared the multipolymer NaAMC with hydrophobic block structure
14s/AM, overcomes some shortcomings that micellar co-polymerization uses conventional surfactants to bring, multipolymer NaAMC
14the length of hydrophobic micro-block of S/AM can control by regulating additional electrolytical consumption, but research work biases toward theory, the evaluation result not under the mineral reserve condition of actual oil field.
Make a general survey of above-mentioned research, the most frequently used method of current synthetizing hydrophobic associated polymkeric substance is micellar free radical copolymerization method, needing to add a large amount of tensio-active agents (as SDS) when adopting this kind of method to be polymerized makes hydrophobic monomer solubilising in micella, but add the association behavior of a large amount of tensio-active agents on polymkeric substance in the course of the polymerization process and have significant impact, these tensio-active agents interact with hydrophobic segment in polymerisate, deteriorate the performance of hydrophobic associated water-soluble polymer.If remove these tensio-active agents, the complicacy of the last handling processes such as separation and purifying can be increased.In order to simplify last handling process and strengthen structure adaptability, can adopt and inherently there is surface-active hydrophobic monomer.This kind of monomer containing hydrophobic grouping and hydrophilic radical, does not need when copolymerization to add tensio-active agent in addition, can directly adopt traditional free yl solution polymerization simultaneously, and can make in hydrophobic monomer height unordered irregularly introducing multipolymer.But there is research (Ezzell abroad, S.A., McCormick, C.L., Macromolecules 1992,25 (7), 1881 ~ 1886) find, the multipolymer critical association concentration in aqueous of this kind of ionic hydrophobic monomer is more than 2 times of the identical Hydrophobic chain length of micella multipolymer, and this is totally unfavorable to hydrophobic associated polymer application industrially.As can be seen here, domestic and international researchist is to structure, character, the viscosifying mechanisms of hydrophobic associated water-soluble polymer and should be used as large quantity research, exploration work, but the evaluation of polymkeric substance is substantially according to grand celebration or some mineral reserve condition of Shengli Oil Field, temperature and salinity do not belong to high temperature and high salt type, for more than salinity 100000mg/L, the condition of more than 85 DEG C high temperature does not almost relate to.
The present invention is to ionic, the synthesis of both sexes hydrophobic associated water-soluble polymer and hydrophobically modified polyelectrolyte, structural characterization and SOLUTION PROPERTIES aspect are carried out extensively, on deep Research foundation, utilize the interaction had between surface-active monomer and the ionic comonomer of its opposite charges, one is that ionic comonomer effects on surface reactive monomer has solublization, separately tensio-active agent need not be added when being polymerized, two is to form both sexes hydrophobic associated polymer, even if polymkeric substance also has high-effective viscosity and excellent heatproof under hydrophobic monomer lower aq, anti-salt and permanent stability, and do not need rear hydrolytic process, not only contribute to long-term ageing property, also reduce production energy consumption, do not affect again the solvability of product, in drying process, add a certain amount of sticky steady agent and tensio-active agent, not only contribute to structure adaptability and play collaborative viscosifying action, yet further enhances ageing resistance.The polymkeric substance mobility control agent being applicable to the harsh oil reservoir of high temperature and high salt of the present invention has high tackifying, normal salt sensitivity (meeting salt retrogradation), the positive Thermo-sensitive (intensification retrogradation) of certain limit and lower micelle-forming concentration, and excellent long-term aging, be suitable for total mineralization is greater than the harsh oil reservoir oil displacement of 85 DEG C requirement more than 100,000 mg/L, temperature, have a good application prospect in tertiary oil recovery engineering.Of the present invention be suitable for the harsh oil reservoir of high temperature and high salt just method for producing polymer, binary compound and the application in tertiary oil recovery thereof.
Summary of the invention
One of technical problem to be solved by this invention be exist in prior art can meet containing the high temperature resistant anti-high salinity of oil-displacing agent of polymkeric substance and permanent stability the problem that tertiary oil recovery requires, there is provided a kind of and be applicable to the oil-displacing agent that the harsh oil reservoir of high temperature and high salt improves recovery ratio, this oil-displacing agent has the features such as high-effective viscosity, temperature resistant antisalt (the chance salt retrogradation of certain limit, intensification retrogradation), permanent stability.
Two of technical problem to be solved by this invention is to provide the preparation method of the oil-displacing agent in one of a kind of technical solution problem, and it is simple that the method has polymerisation process, without the need to steps such as separation, purifying and rear hydrolysis, and the advantage reduced costs.
In order to one of solve the problems of the technologies described above, the present invention is as follows by the following technical solutions: a kind of oil-displacing agent being applicable to high temperature and high salt harsh oil reservoir raising recovery ratio, at displacement of reservoir oil temperature >90 DEG C, the about 180000mg/L of total mineralization, under the total amount of calcium ion and magnesium ion is greater than the injection water condition of 5000mg/L, underground dewatered oil is contacted with oil-displacing agent, and by abundant for the crude oil in rock core displacement out, wherein said oil-displacing agent comprises following component by weight percentage:
The both sexes hydrophobically associated polyacrylamide of (1) 0.01 ~ 3.0%;
The aliphatic alcohol polyoxyethylene sulfonate tensio-active agent of (2) 0.01 ~ 5.0%;
The injection water of (3) 92.0 ~ 99.98%;
Wherein (1) component both sexes hydrophobically associated polyacrylamide measures (viscosimetry) by GBT12005.10-92 Molecular Weight for Polyacrylamide Mw and measures intrinsic viscosity, and by [η]=3.73 × 10
-4mw
0.66calculate molecular weight between 200-2000 ten thousand, the total amount being 180000mg/L, wherein calcium ion and magnesium ion in total mineralization is in the aqueous solution of 5700mg/L, and 1500mg/L polymer concentration solution is at 95 DEG C, 7.34s
-1under apparent viscosity be 120 ~ 780mps.
In technique scheme, displacement of reservoir oil temperature is preferably 85 ~ 95 DEG C, and described injection water total mineralization is preferably 100000 ~ 250000 mg/L, total amount preferably 2000 ~ 7000 mg/L of calcium ion and magnesium ion; Polymkeric substance is selected from above-mentioned both sexes hydrophobically associated polyacrylamide, and tensio-active agent is selected from aliphatic alcohol polyoxyethylene sulfonate, and ethoxy group number n is preferably 2 ~ 18.
This flooding method concrete operation step comprises the following steps:
A () adds water, nonionic water-soluble monomers, anionic monomer in a kettle. or/and cationic monomer, have the auxiliary agents such as surface-active hydrophobic monomer and inorganics;
B () adds the composite initiation system of part, stir, and forms solution;
PH value to 7 ~ 10 of (c) regulator solution, and pass into nitrogen, temperature in the kettle is down to 10 ~ 30 DEG C, then adds remaining composite initiator, after continuing to pass into nitrogen, sealing;
D temperature of reaction was risen to 40 ~ 60 DEG C after 0.5 ~ 1 hour by () gradually, react after 2 ~ 8 hours, obtain gel polymerisate;
E () adds the drying aids containing sticky steady agent and water phase surfactant mixture after cutting glue, forced air drying 1 ~ 3 hour at 80 ~ 95 DEG C after stirring, be crushed to certain particle size with pulverizer or rolling machine, obtain the polymkeric substance mobility control agent being applicable to the harsh oil reservoir of high temperature and high salt.
F () is by the both sexes hydrophobic associated polymer of aequum, above-mentioned aliphatic alcohol polyoxyethylene sulfonate and inject water Homogeneous phase mixing, 5 ~ 35 DEG C are stirred 1 ~ 3 hour, obtain required composition, by weight percentage, the proportioning of both sexes hydrophobic associated polymer, aliphatic alcohol polyoxyethylene sulfonate and injection water is 0.01 ~ 3.0%: 0.01 ~ 5.0%: 92.0 ~ 99.98;
G () is first is 100000 ~ 250000mg/L, Ca with total mineralization
2++ Mg
2+the injection water being 2000 ~ 7000mg/L is saturated by rock core, measure the volume of voids (PV) of rock core, then carry out saturated with dewatered oil, imitation oil displacement experiment test is carried out: first water drive is to moisture 92% at 85 ~ 95 DEG C of temperature, after the displacement of reservoir oil composition that metaideophone 0.3pv (rock pore volume) step (f) is synthesized, water drive, to moisture 99%, calculates the percentage ratio improving oil recovery factor.
In technique scheme, preferred version be composite initiator in whole weight percent monomer, comprise following component: the persulphate of (a) 0.003 ~ 0.5%; The sulphite of (b) 0.003 ~ 0.5% or bisul-phite; (c) 0.003 ~ 1% by NR
1r
2r
3representative tertiary amine compounds or by N
+r
4r
5r
6r
7representative quaternary ammonium compounds or by NH
2r
8the fat amine compound of representative, R in formula
1~ R
7all be selected from C
1~ C
14straight or branched alkyl or alkyl derivative, R
8be selected from C
1~ C
18straight or branched alkyl or alkyl derivative; The azo compound of (d) 0.005 ~ 1%; The urea of (e) 0.01 ~ 10%, thiocarbamide; The disodium ethylene diamine tetraacetate of (f) 0.03 ~ 0.5% or diethylene triamine pentacetic acid (DTPA) sodium; The molecular weight regulator of (g) 0.03 ~ 0.5%.Described drying aids, in the whole weight percent monomer of association polymer, comprises following component: the sticky steady agent of (a) 0.1 ~ 20%; (b) 0.1 ~ 20% tensio-active agent; The water of (c) 50 ~ 99%.
In technique scheme, it is described that to have surface-active hydrophobic monomer be anionic surface activity monomer or cationic surfactant monomer, anionic surface activity monomer to be vinyl carbochain number be 8 ~ 18 acrylamide azanyl sodium sulfonate, cationic surfactant monomer to be vinyl carbochain number be 12 ~ 22 allyl alkyl ammonium chloride; Having surface-active hydrophobic monomer is the mono-vinyl compounds being selected from 8-22 carbon atom; Described tensio-active agent is selected from least one in aniorfic surfactant, cationic surfactant, nonionic surface active agent, and aniorfic surfactant is C8-16 sodium alkyl sulfate, C8-16 sodium alkyl benzene sulfonate; Described cationic surfactant is that C8-16 alkyl trimethyl bromine (chlorine) changes ammonium; Non-ionic type is alkylphenol polyoxyethylene (EO=4 ~ 30); Composite hydrolysis agent can also be added, described composite hydrolysis agent, in the whole weight percent monomer of association polymer, comprise following component:
At least one in the sodium hydroxide of (a) 0 ~ 20% or sodium carbonate;
(b) 0.5 ~ 50% tensio-active agent; Described tensio-active agent is selected from least one in aniorfic surfactant, cationic surfactant, nonionic surface active agent, and aniorfic surfactant is C8-16 sodium alkyl sulfate, C8-16 sodium alkyl benzene sulfonate; Described cationic surfactant is that C8-16 alkyl trimethyl bromine (chlorine) changes ammonium; Non-ionic type is alkylphenol polyoxyethylene (EO=4 ~ 30).
The harsh oil reservoir of high temperature and high salt that is applicable to that the present invention relates to improves oil-displacing agent of recovery ratio and preparation method thereof, owing to have employed the ion monomer contrary with having surface active monomer ion characteristic, both interaction effects on surface reactive monomers have solublization, separately need not add tensio-active agent when being polymerized; Even and if the both sexes hydrophobic association polymerization polymkeric substance under hydrophobic monomer lower aq obtained also has excellent temperature resistant antisalt, thermally-stabilised and anti-shear performance; And have employed composite initiation system, and supporting with it with preferred technique, therefore reacting balance, be conducive to chainpropagation, molecular weight of product is controlled, and does not need rear hydrolytic process, not only contributes to long-term ageing property, also reduce production energy consumption, do not affect again the solvability of product; In drying process, add a certain amount of sticky steady agent and tensio-active agent, not only contribute to structure adaptability and play collaborative viscosifying action, yet further enhances ageing resistance.What use preparation technology provided by the present invention to obtain is applicable to both sexes hydrophobically associated polyacrylamide of the harsh oil reservoir of high temperature and high salt and preparation method thereof, molecular weight is adjustable between 200 ~ 2,000 ten thousand, excellent viscosifying action is shown under high temperature and high salinity, the sticky dense curve display of polymkeric substance, this both sexes hydrophobic associated polymer mixture has stronger association, viscosity amplification can reach two to three orders of magnitude, and micelle-forming concentration appears at below 2000mg/L; Polymkeric substance has salt thickening effect more than 100,000 under salinity, viscosity-temperature curve shows, polymkeric substance viscosity 60 ~ 80 DEG C time obviously increases, and to decline but still higher than the viscosity before 60 DEG C though have afterwards; By still having thickening after polymkeric substance and surfactant compound, tension force falls, temperature resistant antisalt and resisting ageing for long time performance.
Adopt and be of the present inventionly applicable to raising recovery ratio oil-displacing agent of the harsh oil reservoir of high temperature and high salt and preparation method thereof, can be used for formation temperature 85 ~ 95, total mineralization is 100000 ~ 250000 mg/L, the total amount of calcium ion and magnesium ion is crude oil and the water of the Zhongyuan Oil Field of 2000 ~ 7000 mg/L etc., above-mentioned composition oil-displacing agent is formed with consumption 0.1 ~ 0.3wt% both sexes hydrophobically associated polyacrylamide and 0.1 ~ 0.3wt% aliphatic alcohol polyoxyethylene sulfonate, determine the dynamical interfacial tension value between this oil-displacing agent aqueous solution and Zhongyuan Oil Field Pu xi Area crude oil, can 10 be reached
-3~ 10
-4the ultra low interfacial tension of mN/m, on water drive basis, can reach 16.8% by (water drive improves oil recovery factor and reaches 43.6%) raising oil recovery factor through physical simulation displacement test Lab-evaluation this oil-displacing agent on high temperature, high salinity reservoir, achieve good technique effect.
Below by specific embodiment, the present invention will be further elaborated.
Embodiment
[embodiment 1]
(1) first add in 2500g deionized water in a kettle., add 430g acrylamide (AM), 2-acrylamido-2-methyl propane sulfonic acid (AMPS) 150g, 3.5g2-acrylamido tetradecyl sodium sulfonate (NaAMC
14s), 4.5g acrylyl oxy-ethyl-trimethyl salmiac (DAC), be neutralized to neutrality with NaOH, add disodium ethylene diamine tetraacetate 0.04g, urea 7g, Virahol 0.07g subsequently, be stirred to and dissolve completely.By NaOH adjust ph to 8.9, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then the aqueous solution of sodium bisulfite 10g of 0.2% is added successively, 0.5% methacrylic acid N, N-dimethylaminoethyl (DMAEMA) aqueous solution 10g, the azo diisobutyl amidine hydrochloride 10g of 0.5%, the persulfate aqueous solution 10g of 0.3%, seals after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 52 DEG C gradually, react and obtain gel polymerisate after 3.5 hours, add the drying aids 300g aqueous solution containing 25g sodium lauryl sulphate and 30g thiocarbamide after cutting glue, forced air drying 1.5h under 90 oC, smash the rear sampling analysis of screening with pulverizer.Testing solid content by GB/T12005.2-89 polyacrylamide determination of solid content method is 89.9%, Shi Jian≤90min is separated by GB/T12005.8-89 powdered polypropylene acid amides measuring of dissolution velocity method test Rong, measure (viscosimetry) by GB/T12005.10-92 Molecular Weight for Polyacrylamide and measure intrinsic viscosity, and by [η]=3.73 × 10
-4mw
0.66calculating molecular weight is 8,320,000.Apparent viscosity is at 95 DEG C, salt solution total mineralization 180000mg/L, Ca
2++ Mg
2+: 1500mg/L polymer concentration solution under 5700 mg/L, adopts Haake torque rheometer, concentric drums shearing rate 7.34s
-1under apparent viscosity be 180mPas.
Synthesized both sexes hydrophobically associated polyacrylamide 0.10wt%, above-mentioned aliphatic alcohol polyoxyethylene sulfonate (n=14) 0.30wt% and 99.6wt% Zhongyuan Oil Field Pu xi Area are injected water Homogeneous phase mixing, 20 DEG C are stirred 2 hours, obtain required oil-displacing agent.At temperature 95 DEG C, salinity 180000mg/L, Ca
2++ Mg
2+in the water of 5700mg/L, the apparent viscosity recording this composition is 126mPa.s.; The ultra low interfacial tension of 0.0065mN/m is formed between said composition and Zhongyuan Oil Field Pu xi Area dewatered oil.Apparent viscosity is by the MARS III type rheometer measurement of German Haake company, and the TX500 type that interfacial tension is produced by Texas ,Usa university rotates and drips interfacial tensimeter mensuration.
First with salinity 180000mg/L, Ca
2++ Mg
2+by rock core, (length is 30 centimetres to the injection water of 5700mg/L, and diameter is 2.5 centimetres, and rate of permeation is 1.5 microns
2) saturated, the volume of voids (PV) measuring rock core is 16.2%, then carry out saturated with Zhongyuan Oil Field Pu xi Area dewatered oil, imitation oil displacement experiment test is carried out: first water drive is to moisture 92% under 95 DEG C of constant temperature, record water drive and improve oil recovery factor 48.6%, after the displacement of reservoir oil composition that metaideophone 0.3pv (rock pore volume) step (f) is synthesized again, water drive, to moisture 99%, records and can improve oil recovery factor 15.9% again on water drive basis.
[embodiment 2]
First add in 2600g deionized water in a kettle., add 480g acrylamide (AM), 2-acrylamido-2-methyl propane sulfonic acid (AMPS) 130g, 4.0g2-acrylamido sodium laurylsulfonate (NaAMC
12s), 7.8g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) and 5.0g nitrogen vinyl pyrrolidone (NVP), neutrality is neutralized to NaOH, add disodium ethylene diamine tetraacetate 0.045g, urea 7.0g, Virahol 0.06g subsequently, be stirred to and dissolve completely.By NaOH adjust ph to 9.0, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 16 DEG C, then the aqueous solution of sodium bisulfite 10.2g of 0.2% is added successively, 0.5% vinylformic acid N, N-dimethylaminoethyl (DA) aqueous solution 11g, the azo diisobutyl amidine hydrochloride 11.9g of 0.5%, the persulfate aqueous solution 11.2g of 0.3%, seals after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 58 DEG C gradually, react and obtain gel polymerisate after 3 hours, add the 300g aqueous solution containing 51g Sodium dodecylbenzene sulfonate, 6g Virahol and 45g S-WAT after cutting glue, forced air drying 1h under 95oC, smash the rear sampling analysis of screening with pulverizer.Testing solid content by GB/T12005.2-89 polyacrylamide determination of solid content method is 88.7%, Shi Jian≤90min is separated by GB/T12005.8-89 powdered polypropylene acid amides measuring of dissolution velocity method test Rong, measure (viscosimetry) by GB/T12005.10-92 Molecular Weight for Polyacrylamide and measure intrinsic viscosity, and by [η]=3.73 × 10
-4mw
0.66calculating molecular weight is 8,460,000.Apparent viscosity is at 95 DEG C, salt solution total mineralization 180000mg/L, Ca
2++ Mg
2+: 1500mg/L polymer concentration solution under 5700 mg/L, adopts Haake torque rheometer, concentric drums shearing rate 7.34s
-1under apparent viscosity be 165Pas.
Synthesized both sexes hydrophobically associated polyacrylamide 0.10wt%, above-mentioned aliphatic alcohol polyoxyethylene sulfonate (n=14) 0.30wt% and 99.6wt% Zhongyuan Oil Field Pu xi Area are injected water Homogeneous phase mixing, 20 DEG C are stirred 2 hours, obtain required oil-displacing agent.At temperature 95 DEG C, salinity 180000mg/L, Ca
2++ Mg
2+in the water of 5700mg/L, the apparent viscosity recording this composition is 112mPa.s.; The ultra low interfacial tension of 0.0073mN/m is formed between said composition and Zhongyuan Oil Field Pu xi Area dewatered oil.Apparent viscosity is by the MARS III type rheometer measurement of German Haake company, and the TX500 type that interfacial tension is produced by Texas ,Usa university rotates and drips interfacial tensimeter mensuration.
First with salinity 180000mg/L, Ca
2++ Mg
2+by rock core, (length is 30 centimetres to the injection water of 5700mg/L, and diameter is 2.5 centimetres, and rate of permeation is 1.5 microns
2) saturated, the volume of voids (PV) measuring rock core is 15.5%, then carry out saturated with Zhongyuan Oil Field Pu xi Area dewatered oil, imitation oil displacement experiment test is carried out: first water drive is to moisture 92% under 95 DEG C of constant temperature, record water drive and improve oil recovery factor 43.7%, after the displacement of reservoir oil composition that metaideophone 0.3pv (rock pore volume) step (f) is synthesized again, water drive, to moisture 99%, records and can improve oil recovery factor 15.4% again on water drive basis.
[embodiment 3]
First add in 2700g deionized water in a kettle., add 500g acrylamide (AM), 2-acrylamido-2-methyl propane sulfonic acid (AMPS) 150g, 5.2g2-acrylamido sodium cetanesulfonate (NaAMC
16s) and 9.4g dimethyl diallyl ammonium chloride (DMDAAC), be neutralized to neutrality with NaOH, add disodium ethylene diamine tetraacetate 0.05g, urea 8.0g, Virahol 0.07g subsequently, be stirred to and dissolve completely.By NaOH adjust ph to 9.5, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 20 DEG C, then the aqueous solution of sodium bisulfite 10.2g of 0.2% is added successively, 0.5% vinylformic acid N, N-dimethylaminoethyl (DA) aqueous solution 12.1g, 0.5% 2,2'-azo [2-(2-tetrahydroglyoxaline-2-base) propane] dihydrochloride 12g, the persulfate aqueous solution 11g of 0.3%, seal after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 55 DEG C gradually, react and obtain gel polymerisate after 2.5 hours, add the 300g aqueous solution containing 38gOP-20,20g thiocarbamide and 5g 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid after cutting glue, forced air drying 2h under 85oC, smash the rear sampling analysis of screening with pulverizer.Testing solid content by GB/T12005.2-89 polyacrylamide determination of solid content method is 90.3%, Shi Jian≤90min is separated by GB/T12005.8-89 powdered polypropylene acid amides measuring of dissolution velocity method test Rong, measure (viscosimetry) by GB/T12005.10-92 Molecular Weight for Polyacrylamide and measure intrinsic viscosity, and by [η]=3.73 × 10
-4mw
0.66calculating molecular weight is 9,060,000.Apparent viscosity is at 95 DEG C, salt solution total mineralization 180000mg/L, Ca
2++ Mg
2+: 1500mg/L polymer concentration solution under 5700 mg/L, adopts Haake torque rheometer, concentric drums shearing rate 7.34s
-1under apparent viscosity be 156Pas.
Synthesized both sexes hydrophobically associated polyacrylamide 0.10wt%, above-mentioned aliphatic alcohol polyoxyethylene sulfonate (n=16) 0.30wt% and 99.6wt% Zhongyuan Oil Field Pu xi Area are injected water Homogeneous phase mixing, 20 DEG C are stirred 2 hours, obtain required oil-displacing agent.At temperature 95 DEG C, salinity 180000mg/L, Ca
2++ Mg
2+in the water of 5700mg/L, the apparent viscosity recording this composition is 112mPa.s.; The ultra low interfacial tension of 0.0058mN/m is formed between said composition and Zhongyuan Oil Field Pu xi Area dewatered oil.Apparent viscosity is by the MARS III type rheometer measurement of German Haake company, and the TX500 type that interfacial tension is produced by Texas ,Usa university rotates and drips interfacial tensimeter mensuration.
First with salinity 180000mg/L, Ca
2++ Mg
2+by rock core, (length is 30 centimetres to the injection water of 5700mg/L, and diameter is 2.5 centimetres, and rate of permeation is 1.5 microns
2) saturated, the volume of voids (PV) measuring rock core is 16.6%, then carry out saturated with Zhongyuan Oil Field Pu xi Area dewatered oil, imitation oil displacement experiment test is carried out: first water drive is to moisture 92% under 95 DEG C of constant temperature, record water drive and improve oil recovery factor 43.6%, after the displacement of reservoir oil composition that metaideophone 0.3pv (rock pore volume) step (f) is synthesized again, water drive, to moisture 99%, records and can improve oil recovery factor 16.8% again on water drive basis.
[embodiment 4]
First add in 2600g deionized water in a kettle., add 510g acrylamide (AM), 2-acrylamido-2-methyl propane sulfonic acid (AMPS) 170g, 5.0g hexadecyldimethyl benzyl ammonium allyl ammonium chloride (C
16dMAAC) and 7.8g methacrylic acid (MAA), be neutralized to neutrality with NaOH, add disodium ethylene diamine tetraacetate 0.048g, urea 7.5g subsequently, trimethyl carbinol 0.08g, is stirred to and dissolves completely.By NaOH adjust ph to 8.7, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 12 DEG C, then the aqueous solution of sodium bisulfite 11.2g of 0.2% is added successively, 0.5% methacrylic acid N, N-dimethylaminoethyl (DMAEMA) aqueous solution 12.6g, the azo diisobutyl amidine hydrochloride 12g of 0.5%, the persulfate aqueous solution 10.9g of 0.3%, seals after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 52 DEG C gradually, react and obtain gel polymerisate after 3 hours, add the 300g aqueous solution containing 42gOP-1020g thiocarbamide and 4g urotropine after cutting glue, forced air drying 1.5h under 90oC, smash the rear sampling analysis of screening with pulverizer.
Testing solid content by GB/T12005.2-89 polyacrylamide determination of solid content method is 92.4%, Shi Jian≤90min is separated by GB/T12005.8-89 powdered polypropylene acid amides measuring of dissolution velocity method test Rong, measure (viscosimetry) by GB/T12005.10-92 Molecular Weight for Polyacrylamide and measure intrinsic viscosity, and by [η]=3.73 × 10
-4mw
0.66calculating molecular weight is 8,290,000.Apparent viscosity is at 95 DEG C, salt solution total mineralization 180000mg/L, Ca
2++ Mg
2+: 1500mg/L polymer concentration solution under 5700 mg/L, adopts Haake torque rheometer, concentric drums shearing rate 7.34s
-1under apparent viscosity be 283Pas.
Synthesized both sexes hydrophobically associated polyacrylamide 0.10wt%, above-mentioned aliphatic alcohol polyoxyethylene sulfonate (n=18) 0.30wt% and 99.6wt% Zhongyuan Oil Field Pu xi Area are injected water Homogeneous phase mixing, 20 DEG C are stirred 2 hours, obtain required oil-displacing agent.At temperature 95 DEG C, salinity 180000mg/L, Ca
2++ Mg
2+in the water of 5700mg/L, the apparent viscosity recording this composition is 178mPa.s.; The ultra low interfacial tension of 0.0082mN/m is formed between said composition and Zhongyuan Oil Field Pu xi Area dewatered oil.Apparent viscosity is by the MARS III type rheometer measurement of German Haake company, and the TX500 type that interfacial tension is produced by Texas ,Usa university rotates and drips interfacial tensimeter mensuration.
First with salinity 180000mg/L, Ca
2++ Mg
2+by rock core, (length is 30 centimetres to the injection water of 5700mg/L, and diameter is 2.5 centimetres, and rate of permeation is 1.5 microns
2) saturated, the volume of voids (PV) measuring rock core is 12.9%, then carry out saturated with Zhongyuan Oil Field Pu xi Area dewatered oil, imitation oil displacement experiment test is carried out: first water drive is to moisture 92% under 95 DEG C of constant temperature, record water drive and improve oil recovery factor 45.9%, after the displacement of reservoir oil composition that metaideophone 0.3pv (rock pore volume) step (f) is synthesized again, water drive, to moisture 99%, records and can improve oil recovery factor 14.8% again on water drive basis.
[comparative example 1]
By 650g acrylamide monomer, disodium ethylene diamine tetraacetate 0.04g, urea 7g, Virahol 0.07g, adds in 2500g deionized water, stirs and dissolves completely, by NaOH solution adjust ph to 8.5.Then logical nitrogen 30min, and bath temperature is adjusted to 15 DEG C, then the aqueous solution of sodium bisulfite 10g of 0.2% is added successively, 0.5% methacrylic acid N, N-dimethylaminoethyl (DMAEMA) aqueous solution 10g, the azo diisobutyl amidine hydrochloride 10g of 0.5%, the persulfate aqueous solution 10g of 0.3%, seal after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 50 DEG C gradually, react and obtain gel polymerisate after 3 hours, after cutting glue, add the hydrolytic reagent 730g aqueous solution containing 37gNaOH, 90 oC hydrolysis reaction 2 hours, then vacuum-drying 5h at 75 DEG C, smashes the rear sampling analysis of screening with pulverizer.
Testing solid content by GBT12005.2-89 polyacrylamide determination of solid content method is 88.92%, testing degree of hydrolysis by GBT12005.6-89 partially hydrolyzed polyacrylamide degree of hydrolysis measuring method is 11.3%, measure (viscosimetry) by GBT12005.10-92 Molecular Weight for Polyacrylamide and measure intrinsic viscosity, and by [η]=3.73 × 10
-4mw
0.66calculating molecular weight is 1,963 ten thousand.Apparent viscosity is at 95 DEG C, salt solution total mineralization 180000mg/L, Ca
2++ Mg
2+: 1500mg/L polymer concentration solution under 5700 mg/L, adopts Haake torque rheometer, concentric drums shearing rate 7.34s
-1under apparent viscosity be 2.5Pas.
With [embodiment 1], record water drive and improve oil recovery factor 48.6%, after the above-mentioned displacement of reservoir oil composition of metaideophone, record and can improve oil recovery factor 5.7% again on water drive basis.
[comparative example 2]
By 450g acrylamide (AM), 200g2-acrylamido-2-methyl propane sulfonic acid (AMPS), disodium ethylene diamine tetraacetate 0.04g, urea 7g, Virahol 0.07g, add in 2500g deionized water, stir and dissolve completely, by NaOH adjust ph to 9.0.Then logical nitrogen 30min, and bath temperature is adjusted to 15 DEG C, then the aqueous solution of sodium bisulfite 10g of 0.2% is added successively, 0.5% methacrylic acid N, N-dimethylaminoethyl (DMAEMA) aqueous solution 10g, the azo diisobutyl amidine hydrochloride 10g of 0.5%, the persulfate aqueous solution 10g of 0.3%, seal after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 50 DEG C gradually, react and obtain gel polymerisate after 3 hours, after cutting glue, add the hydrolytic reagent 500g aqueous solution containing 25gNaOH, 90 oC hydrolysis reaction 2 hours, then vacuum-drying 5h at 75 DEG C, smashes the rear sampling analysis of screening with pulverizer.
Testing solid content by GBT12005.2-89 polyacrylamide determination of solid content method is 87.34%, testing degree of hydrolysis by GBT12005.6-89 partially hydrolyzed polyacrylamide degree of hydrolysis measuring method is 12.6%, measure (viscosimetry) by GBT12005.10-92 Molecular Weight for Polyacrylamide and measure intrinsic viscosity, and by [η]=3.73 × 10
-4mw
0.66calculating molecular weight is 1,365 ten thousand.Apparent viscosity is at 95 DEG C, salt solution total mineralization 180000mg/L, Ca
2++ Mg
2+: 1500mg/L polymer concentration solution under 5700 mg/L, adopts Haake torque rheometer, concentric drums shearing rate 7.34s
-1under apparent viscosity be 7.6Pas.
With [embodiment 1], record water drive and improve oil recovery factor 43.7%, after the above-mentioned displacement of reservoir oil composition of metaideophone, record and can improve oil recovery factor 8.2% again on water drive basis.
Claims (10)
1. be applicable to the oil-displacing agent that the harsh oil reservoir of high temperature and high salt improves recovery ratio, by this oil-displacing agent at displacement of reservoir oil temperature >90 DEG C, total mineralization is greater than 180000mg/L, under the total amount of calcium ion and magnesium ion is greater than the injection water condition of 5000mg/L, underground dewatered oil is contacted with oil-displacing agent, by abundant for the crude oil in rock core displacement out, wherein said oil-displacing agent comprises following component by weight percentage:
The both sexes hydrophobically associated polyacrylamide of (1) 0.01 ~ 3.0%;
The aliphatic alcohol polyoxyethylene sulfonate tensio-active agent of (2) 0.01 ~ 5.0%;
The injection water of (3) 92.0 ~ 99.98%;
Wherein (1) component both sexes hydrophobically associated polyacrylamide measures (viscosimetry) by GBT12005.10-92 Molecular Weight for Polyacrylamide Mw and measures intrinsic viscosity, and by [η]=3.73 × 10
-4mw
0.66calculate molecular weight between 200-2000 ten thousand, the total amount being 180000mg/L, wherein calcium ion and magnesium ion in total mineralization is in the aqueous solution of 5700mg/L, and 1500mg/L polymer concentration solution is at 95 DEG C, 7.34s
-1under apparent viscosity be 150 ~ 780mps.
2. the oil-displacing agent being applicable to high temperature and high salt harsh oil reservoir raising recovery ratio according to claim 1, it is characterized in that described tensio-active agent is selected from aliphatic alcohol polyoxyethylene sulfonate type the moon-nonsurfactant, general molecular formula is RO (CH
2cH
2o)
ncH
2cH
2sO
3m, M are any one metal ion be selected from potassium, sodium or lithium, and R is C
9~ C
17alkyl, n is the adduction number of ethoxy group EO, and its span is any one integer in 2 ~ 18.
3. the preparation method being applicable to the oil-displacing agent of high temperature and high salt harsh oil reservoir raising recovery ratio according to claim 1, comprises the following steps:
A () adds water, nonionic water-soluble monomers, anionic monomer in a kettle. or/and cationic monomer, have surface-active hydrophobic monomer;
B () adds the composite initiation system of part, stir, and forms solution;
PH value to 7 ~ 10 of (c) regulator solution, and pass into nitrogen, temperature in the kettle is down to 10 ~ 30 DEG C, then adds remaining composite initiator, after continuing to pass into nitrogen, sealing;
D temperature of reaction was risen to 40 ~ 60 DEG C after 0.5 ~ 1 hour by () gradually, react after 2 ~ 8 hours, obtain gel polymerisate;
E () adds the drying aids containing sticky steady agent and water phase surfactant mixture after cutting glue, forced air drying 1 ~ 3 hour at 80 ~ 95 DEG C after stirring, be crushed to certain particle size with pulverizer or rolling machine, obtain the both sexes hydrophobically associated polyacrylamide being applicable to the harsh oil reservoir of high temperature and high salt;
F () is by the both sexes hydrophobic associated polymer of aequum, above-mentioned aliphatic alcohol polyoxyethylene sulfonate and inject water Homogeneous phase mixing, 5 ~ 35 DEG C are stirred 1 ~ 3 hour, obtain required composition, by weight percentage, the proportioning of both sexes hydrophobic associated polymer, aliphatic alcohol polyoxyethylene sulfonate and injection water is 0.01 ~ 3.0%: 0.01 ~ 5.0%: 92.0 ~ 99.98.
4. the preparation method being applicable to the oil-displacing agent of high temperature and high salt harsh oil reservoir raising recovery ratio according to claim 3, it is characterized in that, the solution that described both sexes hydrophobically associated polyacrylamide is made up of following monomer or auxiliary agent reacts obtained under the existence of composite initiator; The solution of described monomer composition, with weight parts, comprises following component:
A) nonionic water-soluble monomers of 5 ~ 99.9 parts;
B) 0 ~ 50 part of anionic monomer is or/and cationic monomer;
C) 0.1 ~ 10 part there is surface-active hydrophobic monomer;
D) water of 200 ~ 2000 parts;
Wherein, described composite initiator, in above-mentioned whole weight percent monomer, comprises following component: the persulphate of (a) 0.003 ~ 0.5%; The sulphite of (b) 0.003 ~ 0.5% or bisul-phite; (c) 0.003 ~ 1% by NR
1r
2r
3representative tertiary amine compounds or by N
+r
4r
5r
6r
7representative quaternary ammonium compounds or by NH
2r
8the fat amine compound of representative, R in formula
1~ R
7all be selected from C
1~ C
14straight or branched alkyl or alkyl derivative, R
8be selected from C
1~ C
18straight or branched alkyl or alkyl derivative; The azo compound of (d) 0.005 ~ 1%; The urea of (e) 0.01 ~ 10%, thiocarbamide; The disodium ethylene diamine tetraacetate of (f) 0.03 ~ 0.5% or diethylene triamine pentacetic acid (DTPA) sodium; The molecular weight regulator of (g) 0.03 ~ 0.5%; Described drying aids, in the whole weight percent monomer of association polymer, comprises following component: the sticky steady agent of (a) 0.1 ~ 20%; (b) 0.1 ~ 20% tensio-active agent; The water of (c) 50 ~ 99%.
5. the preparation method being applicable to the oil-displacing agent of high temperature and high salt harsh oil reservoir raising recovery ratio according to claim 3, having surface-active hydrophobic monomer described in it is characterized in that is anionic surface activity monomer or cationic surfactant monomer.
6. the preparation method being applicable to the oil-displacing agent of high temperature and high salt harsh oil reservoir raising recovery ratio according to claim 3, having surface-active hydrophobic monomer described in it is characterized in that is the mono-vinyl compounds being selected from 8-22 carbon atom.
7. be according to claim 3ly applicable to the preparation method that the harsh oil reservoir of high temperature and high salt improves the oil-displacing agent of recovery ratio, it is characterized in that described anionic surface activity monomer to be vinyl carbochain number be the acrylamide azanyl sodium sulfonate of 8 ~ 18; Cationic surfactant monomer to be vinyl carbochain number be 12 ~ 22 allyl alkyl ammonium chloride.
8. the preparation method being applicable to the oil-displacing agent of high temperature and high salt harsh oil reservoir raising recovery ratio according to claim 3, it is characterized in that, also add composite hydrolysis agent, described composite hydrolysis agent, in the whole weight percent monomer of association polymer, comprise following component:
At least one in the sodium hydroxide of (a) 0 ~ 20% or sodium carbonate;
(b) 0.5 ~ 50% tensio-active agent.
9. the preparation method being applicable to the oil-displacing agent of high temperature and high salt harsh oil reservoir raising recovery ratio according to claim 4 or 8, it is characterized in that, described tensio-active agent is selected from least one in aniorfic surfactant, cationic surfactant, nonionic surface active agent.
10. the preparation method being applicable to the oil-displacing agent of high temperature and high salt harsh oil reservoir raising recovery ratio according to claim 9, it is characterized in that, described aniorfic surfactant is C8-16 sodium alkyl sulfate, C8-16 sodium alkyl benzene sulfonate; Described cationic surfactant is that C8-16 alkyl trimethyl bromine (chlorine) changes ammonium; Non-ionic type is alkylphenol polyoxyethylene (EO=4 ~ 30).
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