CN104448128B - Polymer mobility control agent suitable for high-temperature and high-salinity harsh reservoir and preparation method of polymer mobility control agent - Google Patents

Polymer mobility control agent suitable for high-temperature and high-salinity harsh reservoir and preparation method of polymer mobility control agent Download PDF

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CN104448128B
CN104448128B CN201310435350.6A CN201310435350A CN104448128B CN 104448128 B CN104448128 B CN 104448128B CN 201310435350 A CN201310435350 A CN 201310435350A CN 104448128 B CN104448128 B CN 104448128B
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monomer
polymer
mobility control
acid
control agent
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CN104448128A (en
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夏燕敏
苏智青
于志省
宋晓芳
许汇
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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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Abstract

The invention relates to a polymer mobility control agent suitable for a high-temperature and high-salinity harsh reservoir and a preparation method of the polymer mobility control agent, and the polymer mobility control agent is mainly used for solving the problems that the polymer in the prior art is poor in heat and salt resistance and long-term stability, and cannot meet the requirements of tertiary oil recovery. In order to better solve the problems, the technical scheme adopted by the invention is as follows: an amphoteric hydrophobic association polymer is prepared from the following raw materials in parts by weight: 5-99.9 parts of a non-ionic water-soluble monomer, 0-50 parts of an anionic monomer or/and cationic monomer, 0.1-10 parts of a hydrophobic monomer with surface activity, 0-20 parts of a viscosity stabilizer and 0-20 parts of a surfactant. The preparation method can be applied to industrial production and application of the polymer mobility control agent for the high-temperature and high-salinity harsh reservoir.

Description

Polymer mobility control agent suitable for high temperature and high salt harshness oil reservoir and preparation method thereof
Technical field
The present invention relates to a kind of polymer mobility control agent suitable for high temperature and high salt harshness oil reservoir and preparation method thereof.
Background technology
Domestic each elephant through once, secondary oil recovery, crude oil water content is continuously increased, 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 one and effectively improve recovery efficiency technique measure.The mechanism of oil displacement of polymer mainly uses 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.Because the tertiary oil recovery cycle is long, deep layer oil temperature is high, 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 depends on the repulsive interaction of the ion on HMW and polymer molecular chain and highly polar side base and reaches thickening Effect.But, heavy polymer is when by larger stretching and shear stress, it is easy to mechanical degradation occurs and loses viscous Degree, it is particularly evident during injection of polymer in low-permeability rock stratum.Cation in the aqueous solution, especially divalent ion, can shield The ionic group in polymer is covered, polymer molecular chain is crimped, hydrodynamic volume reduces even precipitation, so that tackifying Substantially reduce.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 the high temperature aqueous solution, the salt-resistance for making polymer solution drastically declines.In recent years, relevant temperature-resistant and anti-salt type gathers The research of acrylamide mainly by introduce big side base on main polymer chain or rigid side base improve polymer heat endurance, Introduce and suppress the monomer or the monomer insensitive to salt of hydrolysis to carry out copolymerization to improve the hydrolysis and anti-salt property of 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 that polymer is difficult to reach HMW or product has higher cost, answer in industrial production or tertiary oil recovery is actual With can be somewhat limited.In tertiary oil recovery at present, the polymer of temperature-resistant anti-salt requirement can be met seldom, not be that price is too high It is exactly unstable properties, particularly can not meets more than salinity 100000mg/L, the requirement of 85 DEG C of high temperature above.
Hydrophobic associated water-soluble polymer is referred to a small amount of hydrophobic grouping one on polymer hydrophilicity macromolecular chain Class water-soluble polymer.Due to the SOLUTION PROPERTIES such as the thickening of its uniqueness, salt resistance, anti-shearing, should as novel polymeric oil-displacing agent Have a good application prospect for high salt, high shear oil reservoir development.Give birth to because of hydrophobic grouping is introduced in polymer molecule Into hydrophobic association type copolymer, in aqueous medium its hydrophobic chain link to assemble and associate similar to surfactant mode, Effective hydrodynamic volume increase of a macromolecular ball of string, aqueous medium viscosity is improved, and larger side base rises to polymer molecule backbone To shielding action, weaken the p- COO of salt ionThe impact of group;And larger side base also has certain sterically hindered effect Should, strengthen chain rigidity.
But now there are some researches show it is conflicting between the associative ability of such polymer and water solubility, good water solubility it is poly- The carbochain of compound often hydrophobic monomer is shorter or content is relatively low, and associating effect is not obvious, need to be under higher polymer concentration Show certain association effect and meet heat and salinity tolerance performance;And the polymer associate containing long-chain or the hydrophobic monomer of high-load Very capable, heat and salinity tolerance performance is good, but poorly water-soluble, and generally requiring long time just can be completely dissolved, and lose industry Change the value of application.How preferable 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 preferably progress and achievement.
Feng Rusen etc.(CN1793189A)Using micella copolymerization method synthesized containing acrylamide, PAA and pi-allyl- The hydrophobic associated polymer of three kinds of construction units of alkyl phenyl ether, although have preferable Efficient Adhesive Promotion, but 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 Hydrocarbon is used as the hydrophobic associated polymer of hydrophobic monomer, and the polymerization process time is longer, at only have rated 45 DEG C polymer in fresh water and Efficient Adhesive Promotion in salt solution, 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 salinities 12000mg/L, wherein Ca2+With Mg2+For 300mg/L, sample concentration is 1500mg/L, and using Brookfield viscometer, shear rate is 36.7s-1Viscosity be 15.6 ~ 12.4mPa.s;Kong Ying etc.(CN1528734、CN1528797)Synthesize the super high molecular weight water insoluble hydrophobic containing fluorocarbon group to form Mould assembly polymer, have rated it in triumph salt solution(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 the aqueous solution, Master's thesis in 2007)Using surface active monomer NaAMC14S and the homogeneous copolymerization of the AM aqueous solution The method of conjunction has been successfully prepared the copolymer NaAMC with hydrophobic block structure14S/AM, overcome micellar co-polymerization use it is general Some shortcomings that logical surfactant is brought, copolymer NaAMC14The length of hydrophobic micro- block of S/AM can be outer by adjusting Plus the consumption of electrolyte is controlling, but research work biases toward theory, without the evaluation result under the conditions of actual oil field mineral reserve.
The studies above is made a general survey of, at present synthetizing hydrophobic associated polymer most common method is micellar free radical copolymerization method, is adopted Need to add substantial amounts of surfactant when being polymerized with this kind of method(Such as SDS)Hydrophobic monomer solubilising is made in micella, but is being gathered Substantial amounts of surfactant is added to have significant impact to the association behavior of polymer during conjunction, these surfactants are poly- Close in product and interacted with hydrophobic segment, deteriorate the performance of hydrophobic associated water-soluble polymer.If removing these tables Face activating agent, can increase the complexity of the last handling process such as separation and purifying.In order to simplify last handling process and strengthen polymer Dissolubility, can adopt inherently with surface-active hydrophobic monomer.This kind of monomer is simultaneously containing hydrophobic grouping and hydrophilic Group, surfactant need not be it is possible to additionally incorporate in combined polymerization, can directly adopt traditional free yl solution polymerization, and Can make that hydrophobic monomer is highly unordered to be irregularly introduced in 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 the aqueous solution is more than 2 times of the identical Hydrophobic chain length of micella copolymer, and this point is polymerized to hydrophobic association Thing application industrially is totally unfavorable.As can be seen here, domestic and international 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 Some mineral reserve conditions, temperature and salinity are all not belonging to high temperature and high salt type, more than salinity 100000mg/L, more than 85 DEG C The condition of high temperature almost without reference to.
The present invention is to ionic, the synthesis of both sexes hydrophobic associated water-soluble polymer and hydrophobically modified polyelectrolyte, knot Structure is characterized and SOLUTION PROPERTIES aspect is carried out on the basis of extensive, in-depth study, opposite to that using the monomer with surface-active Interaction between the ionic comonomer of electric charge, one is that ionic comonomer has solubilization to surface active monomer, is not required to Separately add surfactant during polymerization, two can be to form both sexes hydrophobic associated polymer, 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 do not affect the dissolubility of product;Add in dry run a certain amount of Steady agent and surfactant are glued, the dissolving of polymer is not only helped and is played collaboration viscosifying action, be yet further enhances anti- Ageing properties.Polymer mobility control agent suitable for high temperature and high salt harshness oil reservoir of the present invention has high tackifying, just The quick property of salt(Meet salt retrogradation), a range of positive Thermo-sensitive(Intensification retrogradation)With relatively low critical micelle concentration, it is and excellent Long-term ageing, is suitable for the requirement of harsh oil reservoir oil displacement of the total salinity more than 100,000 mg/L, temperature more than 85 DEG C, at three times Have a good application prospect in petroleum production engineering.
The content of the invention
One of the technical problem to be solved is the anti-high salinity of polymer high temperature resistant present in prior art And long-time stability can meet the problem of tertiary oil recovery requirement, there is provided a kind of polymerization suitable for high temperature and high salt harshness oil reservoir Thing mobility control agent, the polymer has high-effective viscosity, temperature-resistant anti-salt(The salt retrogradation of a range of chance, intensification retrogradation), it is long The features such as phase stability.
The two of the technical problem to be solved are to provide the system of the polymer in a kind of one of solution technical problem Preparation Method, the method has polymerisation process simple, without the need for the steps such as separation, purifying and rear hydrolysis, the advantage of reduces cost.
In order to solve one of above-mentioned technical problem, the present invention employs the following technical solutions as follows:It is high that one kind is applied to high temperature Salt harshness oil reservoir polymer mobility control agent, the molecular weight of the polymer between 200-2000 ten thousand, by following monomer composition Solution react in the presence of composite initiator be obtained;The solution of described monomer composition in terms of parts by weight, comprising following Component:
A) 5 ~ 99.9 parts of nonionic water-soluble monomers;
B) 0 ~ 50 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, comprising following components:
The persulfate of (a) 0.003~0.5%;
The sulphite or acid sulphite of (b) 0.003~0.5%;
(c) 0.003~1% by NR1R2R3Tertiary amine compounds of representative or by N+R4R5R6R7The quaternary amines of representative Compound or by NH2R8The fat amine compound of representative, R in formula1~R7It is selected from C1~C14Straight or branched alkyl or alkyl derivative Thing, R8Selected from C1~C18Straight 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 or diethylene triamine pentacetic acid (DTPA) sodium of (f) 0.03~0.5%;
The molecular weight regulator of (g) 0.03~0.5%.
In above-mentioned technical proposal, the nonionic water-soluble monomers preferred version is selected from water-soluble vinyl monomer, institute Vinyl monomer is stated selected from acrylamide, Methacrylamide, NIPA, N-N- DMAAs, N- N- acrylamides and N hydroxymethyl acrylamide, N- vinyl formamides, N- vinyl acetamides, N- vinylpyridines And at least one in NVP.The anionic monomer preferred version is selected from 2- acrylamido -2- first Base propane sulfonic acid, acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid, crotonic acid, vinylbenzenesulfonic acid, vinyl sulphur In acid, vinyl phosphonate, allyl sulphonic acid, allyl phosphonic acid and/or its water-soluble alkali, alkaline-earth metal and ammonium salt at least It is a kind of;Cationic monomer is selected from dimethyl diallyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, methacryloxypropyl At least one in ethyl-trimethyl salmiac and 2- acrylamido -2- trimethoxysilyl propyl methacrylate ammonium chlorides.
The hydrophobic monomer preferred version with surface-active is anionic surface activity monomer or cationic table Face activated monomer.The hydrophobic monomer with surface-active more preferably scheme is the mono-vinyl class selected from 8-22 carbon atom Compound.Preferred technical scheme, the anionic surface activity monomer is the acrylamide that vinyl carbochain number is 8 ~ 18 Azanyl sodium sulfonate;Cationic surfactant monomer is the allyl alkyl ammonium chloride that vinyl carbochain number is 12 ~ 22.
Persulfate preferred version is selected from potassium peroxydisulfate, sodium peroxydisulfate or ammonium persulfate;Sulphite is selected from sulfurous acid Sodium or potassium sulfite, acid sulphite is selected from sodium hydrogensulfite or potassium bisulfite;Tertiary amine compounds preferred version is choosing From methacrylic acid N, N- dimethylaminoethyls, acrylic acid N, N- dimethylaminoethyls, β-dimethylaminopropionitrile, tetramethyl second two Amine, hexa etc.;Quaternary ammonium compoundses are selected from N, N- dimethyl diallyl ammonium chlorides, N, N- diethyl diallyls Ammonium chloride;Fat amine compound is selected from methylamine, ethylenediamine, 1,3- propane diamine, 1,4- butanediamine, N, N- dimethyl -1,3- third Diamines etc.;Azo compound is selected from azo diisobutyl amidine hydrochloride, 2,2'- azos [2- (2- imidazoline -2- bases) propane] Dihydrochloride etc.;Molecular weight regulator preferred version is selected from isopropanol, the tert-butyl alcohol, isobutanol, pentaerythrite or a contracting dipropyl At least one in glycol.
In order to solve the two of above-mentioned technical problem, the present invention employs the following technical solutions as follows:It is high that one kind is applied to high temperature The preparation method of the polymer mobility control agent of salt harshness oil reservoir, successively including following step:
A () adds in a kettle. water, nonionic water-soluble monomers, anionic monomer or/and cationic monomer, has The auxiliary agents such as the hydrophobic monomer and inorganic matter of surface-active;
B () adds the composite initiation system of part, stir, and forms solution;
C () adjusts the pH value of solution to 7 ~ 10, and be passed through nitrogen, and temperature in the kettle is down to into 10 ~ 30 DEG C, is subsequently adding it Remaining composite initiator, continues to be passed through after nitrogen, sealing;
D reaction temperature is gradually increased to 40 ~ 60 DEG C by () after 0.5 ~ 1 hour, after reacting 2 ~ 8 hours, obtain gel polymerization Product;
E () is cut and add after glue containing the drying aids for gluing steady agent and aqueous surfactant solution, after stirring 80~ Forced air drying 1~3 hour at 95 DEG C, with pulverizer or roller certain particle size is crushed to, and obtains being applied to high temperature and high salt harshness The polymer mobility control agent of oil reservoir.
In above-mentioned technical proposal, preferred technical scheme, the drying aids, with association polymer whole monomer weight hundred Divide than meter, including following components:The viscous steady agent of (a) 0.1~20%;(b) 0.1~20% surfactant;(c) 50~99% Water.
It is described to glue steady agent selected from free radical resistant type such as sodium sulfite, phenol/quinones etc., reduced form for example sodium thiosulfate, thiocarbamide, Sodium hydrogensulfite, tetraethyl amylamine, hydrazine etc., high-valency metal particle complexing agent such as arabo-ascorbic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid etc., Alcohol, amine such as isopropanol, the tert-butyl alcohol, methenamine etc., one or more in polymer electrolyte such as PVA;Surfactant is selected From anionic surfactant such as C8-16Sodium alkyl sulfate, C8-16Sodium alkyl benzene sulfonate etc., cationic surface active agent is such as C8-16Alkyl trimethyl bromine(Chlorine)Change ammonium etc., nonionic such as APES(EO=4~30)Or theirs is any Mixture.
In above-mentioned technical proposal, polymer mobility control agent and preparation method thereof of high temperature and high salt harshness oil reservoir, including with Lower step:A certain amount of deionized water is initially charged in a kettle., then puts into acrylamide, surface active monomer and anion And/or cationic monomer and other auxiliary agents are stirred to being completely dissolved.PH value is adjusted to 7 ~ 10, and start to be passed through height with NaOH solution Pure nitrogen gas, set point of temperature is down to after 10 ~ 60min by temperature in the kettle(10~30℃), composite initiator is then sequentially added, continue Seal after logical 10 ~ 60min of nitrogen.Reaction temperature is gradually increased to into set point of temperature after 0.5 ~ 2 hour(40~60℃), react 2 ~ 8 little When after obtain gel polymerizate, cut and add after glue containing the drying aids for gluing steady agent and aqueous surfactant solution, stirring After uniform at 80~95 DEG C forced air drying 1~3 hour, be crushed to certain particle size with pulverizer or roller, be applied to The polymer mobility control agent of high temperature and high salt harshness oil reservoir.
It is by using 5 ~ 99.9 parts of nonionics suitable for the polymer mobility control agent of high temperature and high salt harshness oil reservoir oil reservoir Water-soluble monomer, 0 ~ 50 part of anion or/and cationic monomer, 0.1 ~ 10 part of hydrophobic monomer with surface-active;Compound In the presence of initiator system, cause the aqueous solution polymerization of comonomer, then add drying aids to carry out forced air drying as needed, Certain particle size is finally ground into, solid content 90% or so the, polymer of molecular weight 200-2000 ten thousand is obtained, in high temperature and high salt condition There is down high-effective viscosity and the quick property of normal salt(Meet salt retrogradation), a range of positive Thermo-sensitive(Intensification retrogradation)It is critical with relatively low Micellar concentration, and with preferable dissolubility, long-term thermal stability and anti-shear performance, 100,000 mg/ are met in tertiary oil recovery The requirement of L, temperature more than more than 85 DEG C salinity high temperature and high salt harshness oil reservoir oil displacement polymer.The process is simple is easy to operate, It is adapted to large-scale production.
Polymer mobility control agent suitable for high temperature and high salt harshness oil reservoir according to the present invention and preparation method thereof, due to Employ with the contrary ion monomer of surface active monomer ion characteristic, both interactions have to surface active monomer Solubilization, is not required to separately add surfactant in polymerization;Even and if the both sexes hydrophobic association for obtaining is polymerized in hydrophobic monomer Polymer also has excellent temperature-resistant anti-salt, thermally-stabilised 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 to increase, 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 affect the dissolubility of product;Dried A certain amount of viscous steady agent and surfactant are added in journey, the dissolving of polymer are not only helped and is played collaboration viscosifying action, Yet further enhances ageing resistace.It is harsh oily using high temperature and high salt is applied to obtained in preparation technology provided by the present invention Polymer mobility control agent of Tibetan and preparation method thereof, molecular weight is adjustable between 200 ~ 20,000,000, under high temperature and high salinity Excellent viscosifying action is shown, the viscous dense curve of polymer shows, the both sexes hydrophobic associated polymer compound has stronger Association, viscosity amplification is up to two to three orders of magnitude, and critical micelle concentration occurs in below 2000mg/L;Polymer There is salt to viscosify effect more than 100,000, viscosity-temperature curve shows that polymer viscosity at 60~80 DEG C substantially increases under salinity, Though there is decline afterwards but still higher than 60 DEG C of viscosity before;The resisting ageing for long time and anti-shear performance of polymer is good, can use In the tertiary oil recovery of high temperature and high salt harshness oil reservoir.
Below by specific embodiment, the present invention will be further elaborated.
Specific embodiment
【Embodiment 1】
In being initially charged 2500g deionized waters in a kettle., 430g acrylamides are added(AM), 2- acrylamido -2- Methyl propane sulfonic acid(AMPS)150g, 3.5g2- acrylamido myristyl sodium sulfonate(NaAMC14S), 4.5g acrylyl oxy-ethyls Trimethyl ammonium chloride(DAC), neutrality is neutralized to NaOH, it is subsequently added disodium ethylene diamine tetraacetate 0.04g, urea 7g, isopropyl Alcohol 0.07g, stirs to being completely dissolved.PH value is adjusted to 8.9, and start to be passed through high pure nitrogen, with NaOH by kettle interior temperature after 30min Degree is down to 15 DEG C, then sequentially adds 0.2% aqueous solution of sodium bisulfite 10g, 0.5% methacrylic acid N, N- dimethylamino second Ester(DMAEMA)Aqueous solution 10g, 0.5% azo diisobutyl amidine hydrochloride 10g, 0.3% persulfate aqueous solution 10g, after Seal after continuous logical nitrogen 30min.Reaction temperature is gradually increased to into 52 DEG C after 1 hour, reaction obtains gel polymerization after 3.5 hours Product, cuts the drying aids 300g aqueous solution that lauryl sodium sulfate containing 25g and 30g thiocarbamides are added after glue, the air blast under 90 C 1.5h is dried, with pulverizer sample analysis after screening are smashed.
(1)It is 89.9% by GB/T12005.2-89 polyacrylamide determination of solid content method test solid content, by GB/ T12005.8-89 powdered polypropylene acid amides measuring of dissolution velocity method test Rong solution Shi Jian≤90min, by GB/T12005.10- 92 Molecular Weight for Polyacrylamide are determined(Viscosimetry)Intrinsic viscosity is determined, and by [η]=3.73 × 10-4Mw0.66Calculating molecular weight is 8320000.Apparent viscosity is in 95 DEG C, salt solution total salinity 180000mg/L, Ca2++Mg2+:1500mg/L polymerizations under 5700 mg/L Thing strength solution, using Haake torque rheometer, concentric drums shear rate 7.34s-1Under apparent viscosity be 180mPas.95℃ Viscosity retention ratio is respectively 102% after aging 30 days.
【Embodiment 2】
(2)In being initially charged 2600g deionized waters in a kettle., 480g acrylamides are added(AM), 2- acrylamidos- 2- methyl propane sulfonic acids(AMPS)130g, 4.0g2- acrylamido dodecyl sodium sulfate(NaAMC12S), 7.8g methacryls Oxy-ethyl-trimethyl salmiac(DMC)With 5.0g nitrogen vinyl pyrrolidones(NVP), neutrality is neutralized to NaOH, it is subsequently added Disodium ethylene diamine tetraacetate 0.045g, urea 7.0g, isopropanol 0.06g, stir to being completely dissolved.With NaOH adjust pH value to 9.0, and start to be passed through high pure nitrogen, temperature in the kettle is down to into 16 DEG C after 30min, then sequentially add 0.2% sodium hydrogensulfite Aqueous solution 10.2g, 0.5% acrylic acid N, N- dimethylaminoethyls(DA)Aqueous solution 11g, 0.5% azo diisobutyl amidine hydrochloric acid Salt 11.9g, 0.3% persulfate aqueous solution 11.2g, continue to be sealed after logical nitrogen 30min.After 1 hour by reaction temperature gradually 58 DEG C are risen to, reaction obtains gel polymerizate after 3 hours, cut and add after glue neopelex containing 51g, 6g isopropyls The 300g aqueous solution of alcohol and 45g sodium sulfites, the forced air drying 1h under 95 C smashes sample analysis after screening with pulverizer.
It is 88.7% by GB/T12005.2-89 polyacrylamide determination of solid content method test solid content, by GB/ T12005.8-89 powdered polypropylene acid amides measuring of dissolution velocity method test Rong solution Shi Jian≤90min, by GB/T12005.10- 92 Molecular Weight for Polyacrylamide are determined(Viscosimetry)Intrinsic viscosity is determined, and by [η]=3.73 × 10-4Mw0.66Calculating molecular weight is 8460000.Apparent viscosity is in 95 DEG C, salt solution total salinity 180000mg/L, Ca2++Mg2+:1500mg/L polymerizations under 5700 mg/L Thing strength solution, using Haake torque rheometer, concentric drums shear rate 7.34s-1Under apparent viscosity be 165Pas.95 DEG C old Viscosity retention ratio is respectively 117% after changing 30 days.
【Embodiment 3】
In being initially charged 2700g deionized waters in a kettle., 500g acrylamides are added(AM), 2- acrylamido -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, it is subsequently added disodium ethylene diamine tetraacetate 0.05g, urea 8.0g, different Propyl alcohol 0.07g, stirs to being completely dissolved.PH value is adjusted to 9.5, and start to be passed through high pure nitrogen, with NaOH by 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, continues to be sealed after logical nitrogen 30min.Reaction temperature is gradually increased to into 55 DEG C after 1 hour, reaction 2.5 is little When after obtain gel polymerizate, cut and add after glue the 300g water containing 38gOP-20,20g thiocarbamide and 5g 1-hydroxy ethylidene-1,1-diphosphonic acids Solution, the forced air drying 2h under 85 C smashes sample analysis after screening with pulverizer.
It is 90.3% by GB/T12005.2-89 polyacrylamide determination of solid content method test solid content, by GB/ T12005.8-89 powdered polypropylene acid amides measuring of dissolution velocity method test Rong solution Shi Jian≤90min, by GB/T12005.10- 92 Molecular Weight for Polyacrylamide are determined(Viscosimetry)Intrinsic viscosity is determined, and by [η]=3.73 × 10-4Mw0.66Calculating molecular weight is 9060000.Apparent viscosity is in 95 DEG C, salt solution total salinity 180000mg/L, Ca2++Mg2+:1500mg/L polymerizations under 5700 mg/L Thing strength solution, using Haake torque rheometer, concentric drums shear rate 7.34s-1Under apparent viscosity be 156Pas.95 DEG C old Viscosity retention ratio is respectively 107% after changing 30 days.
【Embodiment 4】
In being initially charged 2600g deionized waters in a kettle., 510g acrylamides are added(AM), 2- acrylamido -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, disodium ethylene diamine tetraacetate 0.048g, urea 7.5g are subsequently added, tert-butyl alcohol 0.08g is stirred Mix to being completely dissolved.PH value being adjusted to 8.7, and starting to be passed through high pure nitrogen, temperature in the kettle is down to into 12 after 30min with NaOH DEG C, then sequentially add 0.2% aqueous solution of sodium bisulfite 11.2g, 0.5% methacrylic acid N, N- dimethylaminoethyls (DMAEMA)Aqueous solution 12.6g, 0.5% azo diisobutyl amidine hydrochloride 12g, 0.3% persulfate aqueous solution 10.9g, Continue to be sealed after logical nitrogen 30min.Reaction temperature is gradually increased to into 52 DEG C after 1 hour, reaction obtains gel polymerization after 3 hours Product, cuts the 300g aqueous solution that thiocarbamide containing 42gOP-1020g and 4g methenamines are added after glue, the forced air drying under 90 C 1.5h, with pulverizer sample analysis after screening are smashed.
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 acid amides measuring of dissolution velocity method test Rong solution Shi Jian≤90min, by GB/T12005.10- 92 Molecular Weight for Polyacrylamide are determined(Viscosimetry)Intrinsic viscosity is determined, and by [η]=3.73 × 10-4Mw0.66Calculating molecular weight is 8290000.Apparent viscosity is in 95 DEG C, salt solution total salinity 180000mg/L, Ca2++Mg2+:1500mg/L polymerizations under 5700 mg/L Thing strength solution, using Haake torque rheometer, concentric drums shear rate 7.34s-1Under apparent viscosity be 283Pas.95 DEG C old Viscosity retention ratio is respectively 123% after changing 30 days.
【Comparative example 1】
By 650g acrylamide monomers, disodium ethylene diamine tetraacetate 0.04g, urea 7g, isopropanol 0.07g, 2500g is added In deionized water, after the dissolving completely that stirs, pH value is adjusted to 8.5 with NaOH solution.Then nitrogen 30min is led to, 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, continues to be sealed after logical nitrogen 30min.Reaction temperature is gradually increased to into 50 DEG C after 1 hour, reaction obtains gel after 3 hours Polymerizate, cuts and add after glue the hydrolytic reagent 730g aqueous solution containing 37gNaOH, in 90 C hydrolysis 2 hours, then 75 5h is vacuum dried at DEG C, with pulverizer sample analysis after screening are smashed.
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 is determined(Viscosimetry)Intrinsic viscosity is determined, and by [η]=3.73 × 10-4Mw0.66 It is 19,630,000 to calculate molecular weight.Apparent viscosity is in 95 DEG C, salt solution 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.95 DEG C of viscosity retention ratios after aging 30 days are respectively 46%.
【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 in adding 2500g deionized waters, stirs after dissolving completely, is adjusted with NaOH PH value is to 9.0.Then lead to nitrogen 30min, and bath temperature is adjusted to into 15 DEG C, then sequentially add 0.2% sodium hydrogensulfite water Solution 10g, 0.5% methacrylic acid N, N- dimethylaminoethyls(DMAEMA)Aqueous solution 10g, 0.5% azo diisobutyl amidine Hydrochloride 10g, 0.3% persulfate aqueous solution 10g, continue to be sealed after logical nitrogen 30min.After 1 hour by reaction temperature gradually 50 DEG C are risen to, reaction obtains gel polymerizate after 3 hours, cut and add after glue the hydrolytic reagent 500g aqueous solution containing 25gNaOH, In 90 C hydrolysis 2 hours, then 5h is vacuum dried at 75 DEG C, with pulverizer sample analysis after screening are smashed.
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 is determined(Viscosimetry)Intrinsic viscosity is determined, and by [η]=3.73 × 10-4Mw0.66 It is 13,650,000 to calculate molecular weight.Apparent viscosity is in 95 DEG C, salt solution 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.95 DEG C of viscosity retention ratios after aging 30 days are respectively 54%.

Claims (12)

1. it is a kind of suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent, the molecular weight of the polymer is in 200-2000 Between ten thousand, the solution being made up of following monomer and auxiliary agent reacts in the presence of composite initiator and is obtained;Described monomer composition Solution in terms of parts by weight, comprising following components:
A) 5~99.9 parts of nonionic water-soluble monomers;
B) 0~50 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, comprising following components:
The persulfate of (a) 0.003~0.5%;
The sulphite or acid sulphite of (b) 0.003~0.5%;
(c) 0.003~1% by NR1R2R3Tertiary amine compounds of representative or by N+R4R5R6R7The quaternary ammonium compoundses of representative or By NH2R8The fat amine compound of representative, R in formula1~R7It is selected from C1~C14Straight or branched alkyl or alkyl derivative, R8 Selected from C1~C18Straight 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 or diethylene triamine pentacetic acid (DTPA) sodium of (f) 0.03~0.5%;
The molecular weight regulator of (g) 0.03~0.5%;
Wherein, the polymer mobility control agent adds drying aids, the drying aids, to form in the dry run for preparing Close polymer whole weight percent monomer meter, including following components:
The viscous steady agent of (a) 0.1~20%;
(b) 0.1~20% surfactant;
The water of (c) 50~99%;Wherein, it is described glue steady agent be selected from free radical resistant type, reduced form, high volence metal ion complexing agent, Alcohol, amine, one or more in polymer electrolyte;Surfactant is selected from anionic surfactant, cationic Activating agent, nonionic surface active agent or their any mixture.
2. it is according to claim 1 suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent, it is characterised in that The free radical resistant type is selected from sodium sulfite, phenol/quinones, and reduced form is selected from sodium thiosulfate, thiocarbamide, sodium hydrogensulfite, tetrem Base amylamine, hydrazine, high volence metal ion complexing agent be selected from arabo-ascorbic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, alcohol, amine selected from isopropanol, The tert-butyl alcohol, methenamine, polymer electrolyte is selected from PVA;The anionic surfactant is selected from C8-16Sodium alkyl sulfate, C8-16 Sodium alkyl benzene sulfonate, cationic surface active agent is selected from C8-16Alkyl trimethyl bromine (chlorine) changes ammonium, non-ionic surfactant APES of the agent selected from EO=4~30.
3. it is according to claim 1 suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent, it is characterised in that The nonionic water-soluble monomers are selected from water-soluble vinyl monomer, and the vinyl monomer is selected from acrylamide, metering system Acid amides, NIPA, N-N- DMAAs, N-N- acrylamides and N- methylol acryloyls At least one in amine, N- vinyl formamides, N- vinyl acetamides, N- vinylpyridines and NVP.
4. it is according to claim 1 suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent, it is characterised in that The anionic monomer selected from 2- acrylamide-2-methylpro panesulfonic acids, acrylic acid, methacrylic acid, itaconic acid, maleic acid, Fumaric acid, crotonic acid, vinylbenzenesulfonic acid, vinyl sulfonic acid, vinyl phosphonate, allyl sulphonic acid, allyl phosphonic acid and/or its At least one in water-soluble alkali, alkaline-earth metal and ammonium salt;Cationic monomer selected from dimethyl diallyl ammonium chloride, third Alkene acyloxyethyl trimethyl ammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and 2- acrylamido -2- methyl-propyls At least one in trimethyl ammonium chloride.
5. it is according to claim 1 suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent, it is characterised in that The hydrophobic monomer with surface-active is anionic surface activity monomer or cationic surfactant monomer.
6. it is according to claim 5 suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent, it is characterised in that The hydrophobic monomer with surface-active is the mono-vinyl class compound selected from 8-22 carbon atom.
7. it is according to claim 5 suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent, it is characterised in that The anionic surface activity monomer is the acrylamide azanyl sodium sulfonate that vinyl carbochain number is 8~18;Cationic Surface active monomer is the allyl alkyl ammonium chloride that vinyl carbochain number is 12~22.
8. it is according to claim 1 suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent, it is characterised in that Persulfate is selected from potassium peroxydisulfate, sodium peroxydisulfate or ammonium persulfate;Sulphite is selected from sodium sulfite or potassium sulfite, and acid is sub- Sulfate is selected from sodium hydrogensulfite or potassium bisulfite;Tertiary amine compounds be selected from methacrylic acid N, N- dimethylaminoethyls, Acrylic acid N, N- dimethylaminoethyl, β-dimethylaminopropionitrile, tetramethylethylenediamine, hexa;Quaternary ammonium compoundses Selected from N, N- dimethyl diallyl ammonium chlorides, N, N- diethyl diallyl ammonium chlorides;Fat amine compound selected from methylamine, Ethylenediamine, 1,3- propane diamine, 1,4- butanediamine, N, N- dimethyl -1,3- propane diamine;Azo compound is selected from the isobutyl of azo two Base amidine hydrochloride, 2,2'- azos [2- (2- imidazoline -2- bases) propane] dihydrochloride;Molecular weight regulator is selected from isopropanol, uncle At least one in butanol, isobutanol, pentaerythrite or dipropylene glycol.
9. described in claim 1 suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent preparation method, successively Including following step:
A () adds in a kettle. water, nonionic water-soluble monomers, anionic monomer or/and cationic monomer, lives with surface The hydrophobic monomer of property;
B () adds the composite initiation system of part, stir, and forms solution;
C () adjusts the pH value of solution to 7~10, and be passed through nitrogen, and temperature in the kettle is down to into 10~30 DEG C, is subsequently adding remaining Composite initiator, continues to be passed through after nitrogen, sealing;
D reaction temperature is gradually increased to 40~60 DEG C by () after 0.5~1 hour, after reacting 2~8 hours, obtain gel polymerization and produce Thing;
E () is cut and added containing the drying aids for gluing steady agent and aqueous surfactant solution, at 80~95 DEG C after stirring after glue Lower forced air drying 1~3 hour, with pulverizer or roller certain particle size is crushed to, and obtains being applied to high temperature and high salt harshness oil reservoir Polymer mobility control agent.
10. it is according to claim 9 suitable for high temperature and high salt harshness oil reservoir polymer mobility control agent preparation method, Characterized in that, the drying aids, in terms of association polymer whole weight percent monomer, including following components:
The viscous steady agent of (a) 0.1~20%;
(b) 0.1~20% surfactant;
The water of (c) 50~99%.
The preparation side of the 11. polymer mobility control agents suitable for high temperature and high salt harshness oil reservoir according to claim 10 Method, it is characterised in that described to glue steady agent selected from free radical resistant type, reduced form, high volence metal ion complexing agent, alcohol, amine, high score One or more in subtype;Surfactant is selected from anionic surfactant, cationic surface active agent, nonionic Type or their any mixture.
The preparation side of the 12. polymer mobility control agents suitable for high temperature and high salt harshness oil reservoir according to claim 11 Method, it is characterised in that the free radical resistant type is selected from sodium sulfite, phenol/quinones, reduced form is selected from sodium thiosulfate, thiocarbamide, Asia Niter cake, tetraethyl amylamine, hydrazine, high volence metal ion complexing agent is selected from arabo-ascorbic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, alcohol, amine Class is selected from isopropanol, the tert-butyl alcohol, methenamine, and polymer electrolyte is selected from PVA;The anionic surfactant is selected from C8-16Alkane Base sodium sulphate, C8-16Sodium alkyl benzene sulfonate, cationic surface active agent is selected from C8-16Alkyl trimethyl bromine (chlorine) change ammonium, it is non-from APES of the subtype selected from EO=4~30.
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