CN113736039B - Thick oil activator and preparation method thereof - Google Patents
Thick oil activator and preparation method thereof Download PDFInfo
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- 239000012190 activator Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 14
- 239000000178 monomer Substances 0.000 claims abstract description 87
- 239000003921 oil Substances 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000003999 initiator Substances 0.000 claims abstract description 30
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 15
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010526 radical polymerization reaction Methods 0.000 claims abstract description 13
- 229920001577 copolymer Polymers 0.000 claims abstract description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 67
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 63
- 239000000243 solution Substances 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 230000000977 initiatory effect Effects 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000012544 monitoring process Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- YYROPELSRYBVMQ-UHFFFAOYSA-N 4-toluenesulfonyl chloride Chemical compound CC1=CC=C(S(Cl)(=O)=O)C=C1 YYROPELSRYBVMQ-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 229940125753 fibrate Drugs 0.000 claims description 8
- 238000006116 polymerization reaction Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- MBYLVOKEDDQJDY-UHFFFAOYSA-N tris(2-aminoethyl)amine Chemical compound NCCN(CCN)CCN MBYLVOKEDDQJDY-UHFFFAOYSA-N 0.000 claims description 7
- 239000004115 Sodium Silicate Substances 0.000 claims description 6
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 150000003512 tertiary amines Chemical class 0.000 claims description 6
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000011668 ascorbic acid Substances 0.000 claims description 5
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- MQSGEIOQMQPUMJ-UHFFFAOYSA-N 1-benzyl-4-(2-chloroethenyl)benzene Chemical compound C(C1=CC=CC=C1)C1=CC=C(C=CCl)C=C1 MQSGEIOQMQPUMJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 4
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000295 fuel oil Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- DYUWTXWIYMHBQS-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCNCC=C DYUWTXWIYMHBQS-UHFFFAOYSA-N 0.000 claims description 4
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 4
- 238000005956 quaternization reaction Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical compound NCCS(O)(=O)=O XOAAWQZATWQOTB-UHFFFAOYSA-N 0.000 claims description 4
- VJISAEASWJKEQR-UHFFFAOYSA-N 2-methyl-n-(3-triethoxysilylpropyl)prop-2-enamide Chemical compound CCO[Si](OCC)(OCC)CCCNC(=O)C(C)=C VJISAEASWJKEQR-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 3
- UOKUUKOEIMCYAI-UHFFFAOYSA-N trimethoxysilylmethyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)COC(=O)C(C)=C UOKUUKOEIMCYAI-UHFFFAOYSA-N 0.000 claims description 3
- 238000002347 injection Methods 0.000 abstract description 26
- 239000007924 injection Substances 0.000 abstract description 26
- 238000006073 displacement reaction Methods 0.000 abstract description 14
- 239000010779 crude oil Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 9
- 230000001603 reducing effect Effects 0.000 abstract description 9
- 230000001954 sterilising effect Effects 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 description 25
- 230000009467 reduction Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000010008 shearing Methods 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000001804 emulsifying effect Effects 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000004945 emulsification Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- AUZRCMMVHXRSGT-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CC(C)CS(O)(=O)=O AUZRCMMVHXRSGT-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 229920000891 common polymer Polymers 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
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- 239000007764 o/w emulsion Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
- C08F290/06—Polymers provided for in subclass C08G
- C08F290/062—Polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a thick oil activator, which comprises a copolymer, wherein the copolymer is prepared by carrying out free radical polymerization on acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, a monomer I, a monomer II and a monomer III under the conditions of inert atmosphere, initiator existence and alkalinity; the monomer I is selected from one or more polymerizable silane coupling agents; the monomer II is shown in a formula 1, and the monomer III is shown in a formula 2. The thick oil activator provided by the invention has the functions and effects of increasing the water phase viscosity at the injection end, adjusting the water injection section, adjusting the deep profile, sterilizing, slowly releasing, reducing the crude oil viscosity at the injection distal end, increasing the mobility of the mixed phase flow, improving the displacement capacity and the like.
Description
Technical Field
The invention belongs to the field of oilfield polymer materials, and particularly relates to a thick oil activator and a preparation method thereof.
Background
The thick oil is a strategic raw material for national defense and military industry and major engineering construction, the detected reserve of the world thick oil is about 8150 hundred million tons, and the thick oil accounts for 70% of the residual reserve of the global petroleum, and is an important petroleum taking-over resource. The countries rich in thickened oil resources are Canadian, venezuela, america, china, indonesia, etc. China is the fourth largest thickened oil production country in the world, and is mainly distributed in the oil fields of Bohai sea, victory, liaohe, henan, xinjiang and the like. The reservoir of the heavy oil reservoir has loose cementation, high permeability and serious non-uniformity, and the water invasion phenomenon is serious due to the fact that the side water and the bottom water are active. Therefore, the combined technical measures of profile control, water shutoff and viscosity reduction are required to be adopted, the injection water and side bottom water are prevented from being suddenly introduced, the viscosity of the thickened oil is reduced, the fluidity is improved, and the oil washing efficiency is improved. Compared with thermal viscosity reduction and dilution viscosity reduction, the chemical viscosity reduction technology is relatively simple and has good economic benefit, and can realize multifunctional integration in a combined application mode, thereby avoiding chromatographic separation effect and realizing effective recovery of thickened oil. However, the current chemical viscosity reduction technology has certain limitations to different degrees. For example, the viscosity reducing technology of adding the emulsifier has a lot of formulas, low emulsification temperature (more than 50 ℃) and good viscosity reducing effect (the viscosity reducing rate reaches 99.85%), and can greatly improve the lifting and gathering efficiency of crude oil. However, each emulsifying viscosity-reducing agent is always effective only for one thick oil, i.e. has strong selectivity. Therefore, the thick oil has different properties, the types of the emulsifying and viscosity reducing agents which are suitable for the thick oil are different, and few emulsifying and viscosity reducing agent products with excellent temperature resistance and salt resistance are produced. In addition, the viscous oil emulsification viscosity-reducing technology has a key problem that the single viscous oil viscosity-reducing can aggravate the reservoir heterogeneity, so that an oil displacement agent integrating multiple functions of increasing the water phase viscosity at the injection end, adjusting the water injection profile, adjusting the deep profile, sterilizing and slowly releasing, reducing the crude oil viscosity at the injection distal end, increasing the mixed phase fluidity and improving the displacement capacity is needed.
Disclosure of Invention
The invention aims to provide a thickened oil activator and a preparation method thereof, and the thickened oil activator provided by the invention can realize that the injection end increases the viscosity of water phase, adjusts the water injection section, deep profile control, sterilizes and slowly releases, the injection distal end reduces the viscosity of crude oil, increases the fluidity of mixed phase and improves the displacement capability, thereby realizing the combination of profile control, water shutoff and viscosity reduction effects.
The invention provides a thick oil activator, which comprises a copolymer, wherein the copolymer is obtained by carrying out free radical polymerization on acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, a monomer I, a monomer II and a monomer III under inert atmosphere, initiator existence and alkaline conditions; the monomer I is selected from one or more polymerizable silane coupling agents;
the monomer II is shown in a formula 1:
the monomer III is shown as a formula 2:
wherein R is 1 Is that
m and n are positive integers and m+n=12-18, p=5-50.
According to an embodiment of the present invention, the total mass of the copolymer is from 74% to 90% by mass of acrylamide, the mass of 2-acrylamide-2-methylpropanesulfonic acid is from 4% to 25% by mass, the mass of monomer I is from 5% to 20% by mass, the mass of monomer II is from 0.1% to 1% by mass, and the mass of monomer III is from 0.01% to 0.5% by mass.
According to another embodiment of the invention, the monomer I is selected from one or more of vinyltrimethoxysilane, methacryloxymethyltrimethoxysilane, (3-methacrylamidopropyl) triethoxysilane.
The invention also provides a preparation method of the thick oil activator, which comprises the following steps: s1, adding acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, the monomer I, the monomer II and the monomer III into water to form a solution, and regulating the pH value of the solution to 7-11 by utilizing sodium silicate; s2, controlling the temperature of the solution to be 3-10 ℃, and adding the initiator to perform the free radical polymerization reaction; s3, the heat released by the free radical polymerization reaction increases the temperature of the reaction system, and the reaction is continued for 2 to 6 hours after the temperature of the reaction system reaches the highest point.
According to an embodiment of the invention, the initiator is a composite system comprising a redox system initiator and an azo initiation system initiator; the redox system initiator consists of potassium persulfate, ascorbic acid and white suspending block; the azo initiation system initiator is a mixture of azo diisobutylamidine hydrochloride and azo diiso Ding Mi-hydrochloride; the redox system and the quality of the azo initiation system initiatorThe addition amounts are respectively 10×10 of the total mass of the reactant system -6 ～120×10 -6 The method comprises the steps of carrying out a first treatment on the surface of the Preferably, tertiary amine and urea are also added to the reaction system.
According to another embodiment of the present invention, in the system for radical polymerization, the total mass concentration of the reaction monomers is 19 to 35%.
According to another embodiment of the invention, the maximum temperature reached by the reaction system is 55-70 ℃.
According to another embodiment of the invention, the preparation of monomer II comprises: s11, maintaining the toluene solution of cyanuric chloride at 0-5 ℃, dropwise adding the toluene solution of n-octylamine under stirring, and continuously dropwise adding a sodium hydroxide solution after the dropwise adding is finished so as to maintain the pH value of the system to be 8 in the reaction process, and monitoring the reaction to an end point by using a toluene and acetone mixed solution with the volume ratio of 1:1; s12, heating the reaction system to 45-50 ℃, dropwise adding an aqueous solution of aminoethanesulfonic acid, dropwise adding a sodium hydroxide solution in the reaction process to maintain the pH value of the system to be 8-9, and monitoring the reaction to an end point by using a mixed solution of acetone, toluene and water in a volume ratio of 6:1:0.5; s13, heating the reaction system to 90 ℃, dropwise adding an aqueous solution of tri (2-aminoethyl) amine, dropwise adding a sodium carbonate solution in the reaction process to maintain the pH value of the system to be about 9, and monitoring the reaction to an end point by using a mixed solution of methanol and toluene with the volume ratio of 6:1; preferably, the molar ratio of the added amount of the aqueous solution of tris (2-aminoethyl) amine to the product of the S12 step is 1.1:1, a step of; s14, carrying out quaternization reaction on the reaction product obtained in the step S13 and 4-benzyl chlorostyrene in an equimolar ratio to obtain the monomer II.
According to another embodiment of the invention, the monomer III is prepared by reacting a Bei Techun polyoxyethylene ether with p-toluenesulfonyl chloride and then with diallylamine.
According to another embodiment of the invention, the fibrate alcohol is one or more of fibrate dodecanol, tetradecanol, hexadecanol and octadecanol, and the polyoxyethylene ether has a polymerization degree of 5-50.
The thick oil activator provided by the invention has the functions and effects of increasing the water phase viscosity at the injection end, adjusting the water injection section, adjusting the deep profile, sterilizing, slowly releasing, reducing the crude oil viscosity at the injection distal end, increasing the mobility of the mixed phase flow, improving the displacement capacity and the like.
Drawings
FIG. 1 is a schematic flow chart of a process for preparing a thickened oil activator of the present invention.
FIG. 2 is a schematic flow chart of the process for the preparation of monomer II.
FIG. 3 shows the variation of pressure, water content and recovery ratio of the thick oil activator prepared by the embodiment of the invention in an oil displacement experiment.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The thick oil activator comprises a copolymer, wherein the copolymer is prepared by carrying out free radical polymerization on acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, a monomer I, a monomer II and a monomer III under inert atmosphere, the existence of an initiator and alkaline conditions.
The monomer I is selected from one or more polymerizable silane coupling agents.
Monomer II is shown in formula 1:
monomer III is shown in formula 2:
wherein R is 5 Is that
m and n are positive integers and m+n=12-18, p=5-50.
In the monomer for forming the thick oil activator, the acrylamide can ensure the molecular weight and the water phase tackifying effect of the formed activator. The acrylamide-2-methylpropanesulfonic acid has the functions of temperature resistance and salt resistance. The monomer I plays roles of water phase adhesion promotion and deep profile control. The monomer II plays roles in viscosity reduction and sterilization of the oil phase. The monomer III can play a role in water phase adhesion, and meanwhile, the monomer III not only has super-strong surface-to-surface activity, but also can be used for adjusting the molecular weight of the polymer and has a slow release effect. Therefore, the polymer formed by copolymerizing the five monomers can realize the effects of increasing the water phase viscosity at the injection end, adjusting the water injection section, adjusting the profile of the deep part, sterilizing and slowly releasing, reducing the viscosity of crude oil at the injection end, increasing the fluidity of mixed phase, improving the displacement capability and realizing the combination of profile control, water shutoff and viscosity reduction.
As shown in fig. 1, the thick oil activator of the present invention may be prepared by the following method, the preparation steps comprising: s1, adding acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, a monomer I, a monomer II and a monomer III into water to form a solution, and regulating the pH value of the solution to 7-11 by utilizing sodium silicate; s2, controlling the temperature of the solution to be 3-10 ℃, and adding an initiator to perform free radical polymerization reaction; s3, raising the temperature of the reaction system by heat released by the free radical polymerization reaction, and continuing to react for 2-6 hours after the temperature of the reaction system reaches the highest point.
In the step S1, the pH value of the solution is regulated to 7-11 by sodium silicate, so that the solubility of the polymer can be ensured.
The general formula of the polymer formed by the method is shown in the formula 3:
wherein R is 1 Is that
R 2 Is->
R 3 Is a group formed after polymerization of a polymerizable silane coupling agent (e.g., R when the polymerizable silane coupling agent is selected from one or more of vinyltrimethoxysilane, methacryloxymethyltrimethoxysilane, (3-methacrylamidopropyl) triethoxysilane) 3 Can be correspondingly
One or more of them), R 4 Is->
R 5 Is that
(m and n are positive integers and m+n=12-18, p=5-50).
Based on 100% of the total mass of the copolymer, the mass percentage of the acrylamide is 74% -94%, the mass percentage of the 2-acrylamide-2-methylpropanesulfonic acid is 5% -25%, the mass percentage of the monomer I is 5% -20%, the mass percentage of the monomer II is 0.1% -1%, and the mass percentage of the monomer III is 0.1% -1%. That is, a, b, x, y and z in formula 3 represent the mass percentage of the repeating units corresponding thereto, a=0.74 to 0.94, b=0.05 to 0.25, x=0.05 to 0.2, y=0.001 to 0.01, z=0.001 to 0.01, a+b+x+y+z=1.
In an alternative embodiment, the initiator is a composite system including a redox system initiator and an azo initiation system initiator. The redox system initiator consists of potassium persulfate, ascorbic acid and white suspended block. The azo initiation system initiator is a mixture of azobisisobutyrimidine hydrochloride and azobisiso Ding Mi hydrochloride. Preferably, the molar amount of potassium persulfate is equal to or greater than the molar total amount of the ascorbic acid and the clod. The azo initiation system initiator plays a role of a high-temperature section initiator, and improves the monomer conversion rate. The mass addition amount of the redox system and the azo initiation system initiator is 10 multiplied by 10 respectively of the total mass of the reactant system -6 ～120×10 -6 . When the initiator is added in an amount to ensure the molecular weight of the polymer, the amount is less than 10X 10 -6 At this time, polymerization cannot be initiated or the conversion rate of the monomer is low; the addition amount is higher than 120 multiplied by 10 -6 The molecular weight of the polymer is low.Preferably, tertiary amine and urea are also added into the reaction system, the tertiary amine is a part of an initiator system, and the urea is used for assisting dissolution, so that the solubility of the macromolecular polymer can be improved.
In an alternative embodiment, the total mass concentration of the reactive monomers in the system of the free radical polymerization reaction is 19 to 35%. The total mass concentration of the reaction monomers refers to the percentage of the sum of the mass of acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, monomer I, monomer II and monomer III to the total mass of the reaction system. The concentration of the reaction monomer is less than 19 percent, so that the molecular weight of the polymer formed by low concentration of the monomer is small; if the amount is more than 35%, the polymer formed with a high monomer concentration has poor solubility.
In alternative embodiments, appropriate conditions may be selected, such as the initial temperature, the system concentration, the type and amount of initiator, etc., to control the maximum temperature of the reaction system. The maximum temperature of the system is preferably controlled to 55-70 ℃. The highest temperature of the system is lower than 55 ℃, and the monomer polymerization is not completely converted; the temperature is higher than 70℃and the solubility of the polymer formed is poor.
In an alternative embodiment, monomer II may be prepared by the following steps. As shown in fig. 2, the specific steps include: s11, maintaining the toluene solution of cyanuric chloride at 0-5 ℃, dropwise adding the toluene solution of n-octylamine under stirring, and continuously dropwise adding a sodium hydroxide solution after the dropwise adding is finished so as to maintain the pH value of the system to be 8 in the reaction process, and monitoring the reaction to an end point by using a toluene and acetone mixed solution with the volume ratio of 1:1; s12, heating the reaction system to 45-50 ℃, dropwise adding an aqueous solution of aminoethanesulfonic acid, dropwise adding a sodium hydroxide solution in the reaction process to maintain the pH value of the system to be 8-9, and monitoring the reaction to an end point by using a mixed solution of acetone, toluene and water in a volume ratio of 6:1:0.5; s13, heating the reaction system to 90 ℃, dropwise adding an aqueous solution of tri (2-aminoethyl) amine, dropwise adding a sodium carbonate solution in the reaction process to maintain the pH value of the system to be about 9, and monitoring the reaction to an end point by using a mixed solution of methanol and toluene with the volume ratio of 6:1; preferably, the molar ratio of the amount of aqueous solution of tris (2-aminoethyl) amine added to the product of step S12 is 1.1:1; s14, carrying out quaternization reaction on the reaction product obtained in the step S13 and 4-benzyl chlorostyrene in an equimolar ratio to obtain a monomer II.
In an alternative embodiment, monomer III is prepared by reacting a polyoxyethylene ether of Bei Techun with p-toluenesulfonyl chloride and then with diallylamine.
In an alternative embodiment, the fibrate alcohol is one or more of fibrate dodecanol, tetradecanol, hexadecanol and octadecanol, and the polyoxyethylene ether has a polymerization degree of 5-50.
The heavy oil activator formed by the method has a weight average molecular weight of 600-2000 ten thousand. The viscous oil activator has low molecular weight, so that the water phase tackifying effect is poor; the solubility of the polymer is poor when the molecular weight is high.
When the concentration of the thick oil activator is 400-3000 mg/L, the viscosity is 10-100 mPa.s, the retention rate of shear viscosity is 70-90%, the retention rate of 90-day aging viscosity is 80%, and the thick oil activator has good salt resistance. The mineralization degree is 10000-20000 mg/L, the viscosity reduction rate of the thick oil activator is lower than 5%, and the oil-water interfacial tension is 0.1-1 multiplied by 10 -1 mN/m. For thick oil with viscosity of 1500-2000 mPa.s, the viscosity reduction rate is 95%; for thick oil with viscosity of 600-1000 mPa.s, the viscosity reduction rate is 80-92%; for thick oil with viscosity of 200-350 mPa.s, the viscosity reduction rate is 60-75%. The volume ratio of oil to water between activated polymer and thick oil is less than 9:1, forming a substantially oil-in-water emulsion.
The thick oil activator is suitable for oil field reservoir layers with crude oil viscosity of 1-5000 mPa.s and permeability level difference of 0.1-10D, and can be used according to the following steps:
and injecting the thick oil activator when the oil field starts to be mined or when the water content of water flooding is 0-80%, and injecting the thick oil activator in a pressurizing mode of an injection pump. The method comprises the following steps: firstly, preparing high-concentration mother liquor by rapidly dissolving activator polymer dry powder by water injection, diluting the mother liquor into an activated water flooding system with target concentration, pressurizing by an injection pump, and injecting the activated water flooding system into a target oil layer from an injection well according to the set daily injection amount of a single well. The concentration of the mother solution is 4000-5000 mg/L, and the target concentration is 400-3000 mg/L. Daily injection quantity of single well is 200-3000 m 3 。
Compared with common polymers, high viscosity polymers, surface polymerization agents and conventional viscosity reducing agents with the same cost, the thickened oil activating agent can improve the recovery ratio by 10-20%.
The inventive concept of the present invention is explained below by means of specific examples. The experimental methods used in the examples are conventional methods unless otherwise specified. The percentages in the examples are by weight unless otherwise indicated. Materials, reagents and the like used in the examples are commercially available unless otherwise specified.
Example 1
(1) Preparation of monomer II
36.88g of cyanuric chloride (0.2 mol) and 200ml of toluene are added into a four-necked flask, the temperature is maintained at 0-5 ℃ by an ice bath, 25.85g of toluene solution of n-octylamine (0.2 mol, dissolved in 100ml of toluene) is dropwise added under stirring, and after the dropwise addition, sodium hydroxide solution is continuously dropwise added to maintain the pH value of the system in the reaction process at 8, and the reaction end point is monitored by TIC (toluene: acetone=1:1, volume ratio). Heating to 45-50 ℃, slowly dropwise adding an aqueous solution with 20.5g of aminoethanesulfonic acid (0.2 mol) dissolved therein, continuously dropwise adding a sodium hydroxide solution, maintaining the pH value of the system in the reaction process to be 8-9, and monitoring the reaction to an end point by using TIC (acetone: toluene: water-6:1:0.5 by volume). Then heating to 90 ℃, slowly dripping 0.22mol of aqueous solution of tri (2-amino ethyl) amine, and then slowly dripping sodium carbonate solution, wherein the pH value of the system is maintained to be about 9 in the reaction process. The reaction was monitored by TLC (methanol: toluene=6:1, volume ratio) to endpoint. Adjusting pH to 2 with hydrochloric acid, filtering, repeatedly washing filter cake with water to neutrality, and oven drying.
And (3) carrying out quaternization reaction on the reaction product of the last step and 4-benzyl chlorostyrene in an equimolar ratio, wherein the reaction temperature is 75 ℃, and acetonitrile is used as a solution. To obtain the polymerizable target monomer II.
(2) Preparation of monomer III
Adding 0.45mol of fibrate dodecanol into a high-pressure reactor, heating to 110 ℃ with 0.32g of anhydrous potassium hydroxide, vacuumizing to replace nitrogen three times, removing air each time for 30 minutes, adding ethylene oxide into a reaction device, controlling the temperature to be 110-120 ℃ and the pressure to be less than 0.4MPa in the reaction process, reacting to negative pressure after the dripping is finished, cooling to 50 ℃ and discharging to obtain the yellow oily fibrate dodecanol-epoxy adduct.
Reacting the adduct with 0.5mol of p-toluenesulfonyl chloride, introducing a highly active leaving group; and then reacted with 0.45mol of diallylamine to prepare the polymerizable bezate dodecanol polyether.
(3) Preparation of activator copolymer
Adding acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, a monomer I, a monomer II and a monomer III into a reaction kettle according to a polymerization reaction liquid formula, and stirring until the acrylamide, the 2-acrylamide-2-methylpropanesulfonic acid, the monomer I, the monomer II and the monomer III are completely dissolved, wherein the feeding amounts of the acrylamide, the 2-acrylamide-2-methylpropanesulfonic acid, the monomer I, the monomer II and the monomer III are respectively 90wt%, 4.89wt%, 5wt%, 0.1wt% and 0.01wt% of the total monomer amount, and the mass concentration of the total monomer content in a reaction system is 23wt%. The pH value of the reaction solution is regulated to 8 by adopting sodium silicate, and then nitrogen is introduced for 10min so as to remove oxygen in the reaction system. The temperature of the reaction system is reduced to 3 ℃ by using an ice salt water bath, then an initiating system is added under the protection of nitrogen, the initiating system is a composite system, and consists of potassium persulfate, ascorbic acid, sodium silicate, azo diiso Ding Mi hydrochloride and tertiary amine, and the addition amounts of the initiator system and the tertiary amine are 110 multiplied by 10 respectively -6 。
Urea is added in the reaction process for dissolution assistance, and the addition amount is 1wt% of the reaction system.
The reaction heat is continuously released, the temperature of the reaction system is increased, and the reaction is continued for 2 hours after the system temperature reaches the highest point (67 ℃). And after the reaction is finished, granulating, drying and screening the jelly in the reaction kettle to obtain an activated polymer oil-displacing agent granular product.
Performance evaluation of heavy oil activator
Preparing a solution according to the standard of SY/T5862-2008 polymer technical requirement for oil displacement, and preparing water into simulated mineralized water of a certain oil field of the Bohai sea, wherein the ion composition is Na + +K + 2360.09、Ca 2+ 115.53、Mg 2+ 52.29、HCO 3 - 619.22、SO 4 2- 11.16、Cl - 3689.88. The crude oil in the experiment is the crude oil of a certain oil field of Bohai sea,the formation viscosity was 450mPa.s (65 ℃).
(1) Dissolution time
The thick oil dismantling agent mother liquor with the mass concentration of 5000mg/L is prepared by using simulated water, stirred at the rotating speed of 400r/min and the temperature of 45 ℃ by using an overhead stirrer, and filtered by using a stainless steel net with the aperture of 149 mu m under the pressure difference of 0.05MPa, wherein the time required for the residue content to reach less than 2 percent.
(2) Viscosity-concentration relationship
A1200 mg/L polymer solution was prepared and tested for viscosity before and after shearing using BROOKFIELD DV-III. Shearing by using a Waring stirrer is carried out, wherein the shearing standard is that the shearing strength is 1 grade and the shearing time is 20s. The rotation speed was set to 6r/min (7.34 s) -1 ) And (3) performing an apparent viscosity test, and obtaining a viscosity curve of the activated water flooding system at a test temperature of 65 ℃.
The main system is obviously different from other oil displacement systems in that the polymer prepared by the method contains an active siloxy structure and has the in-situ tackifying capability of a polymer solution. The testing method is that the polymer solution sheared by the Waring stirrer is deoxidized, aged for 5 hours at 65 ℃, and tested for viscosity recovery.
(3) Viscosity reducing performance
Preparing activated polymer solutions with different concentrations, mixing thick oil to be tested with the activated polymer solutions according to an oil-water ratio of 1:1, and keeping the temperature at 65 ℃ for 1h. Mechanical stirring was carried out for 1min (600 r/min). The viscosity test was rapidly performed using BROOKFIELD DV-III at 65℃and the results are shown in Table 1.
(4) Oil displacement performance
Selecting core of target oil reservoir according to experimental requirement, or making artificial three-layer heterogeneous Fang Yanxin (size 45×45×300mm, gas measurement 500/1500/2500 μm) 2 ) Washing or drying the core, measuring the size of the core, and weighing the weight M of the core after drying 0 . Evacuating saturated simulated water (maintaining pressure about-0.09 MPa, and evacuating for more than 2 hr), placing saturated core on electronic balance, and weighing its weight M 1 . The pore volume of the porous medium was calculated (pv=m 1 -M 0 ). Saturated simulated oil, the water yield is recorded as saturated oil quantityAging for 72h at the experimental temperature, and then carrying out a water flooding experiment. Performing displacement at a flow rate of 1mL/min, collecting liquid at an outlet end, changing a liquid collecting test tube every 5min (or determining interval time according to actual conditions), respectively reading the volumes of water, oil and total liquid, and calculating the instantaneous water content (the oil and water are mixed and are easy to be emulsified, the test tube is required to be placed in a constant-temperature water bath kettle, and the number is read after heating and demulsification); when the water drives to three continuous instant water content points reach 95% of the water content set by the scheme, the activated water starts to be injected.
Preparing 1200mg/L polymer solution, closing a water injection valve, performing displacement at a flow rate of 0.5mL/min, and recording the injection time; when the polymer flooding starts, the accumulated liquid outlet amount of the outlet (or the injection amount is recorded, the total amount of the solution injected with the dismantling agent is calculated), and when the accumulated liquid outlet amount of the injected polymer solution reaches the injection amount required by the experiment, the method immediately shifts to the subsequent water flooding. The subsequent water flooding displacement can be stopped until the instantaneous water content reaches more than 98% at three continuous points.
The test results are shown in tables 1 and 2.
TABLE 1
TABLE 2
FIG. 3 is a graph showing the comprehensive capacity test of the thick oil activator prepared by the embodiment of the invention by taking the oil displacement performance test as an index. As can be seen from tables 1, 2 and 3, the thickened oil activator prepared in the example 1 has higher water phase tackifying capability and thickened oil viscosity reducing capability under lower use concentration, and the recovery ratio increase can reach more than 17.4%.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (11)
1. The thick oil activator comprises a copolymer, and is characterized in that the copolymer is obtained by free radical polymerization of acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, a monomer I, a monomer II and a monomer III under the conditions of inert atmosphere, initiator existence and alkalinity;
the monomer I is selected from one or more polymerizable silane coupling agents;
the monomer II is shown in a formula 1:
the monomer III is shown as a formula 2:
wherein R is 5 Is that
m and n are positive integers and m+n=12-18, p=5-50;
based on 100% of the total mass of the copolymer, the mass percentage of the acrylamide is 74% -90%, the mass percentage of the 2-acrylamide-2-methylpropanesulfonic acid is 4% -25%, the mass percentage of the monomer I is 5% -20%, the mass percentage of the monomer II is 0.1% -1%, and the mass percentage of the monomer III is 0.01% -0.5%.
2. The thick oil activator according to claim 1, wherein the monomer I is selected from one or more of vinyltrimethoxysilane, methacryloxymethyltrimethoxysilane, (3-methacrylamidopropyl) triethoxysilane.
3. A process for the preparation of the heavy oil activator of claim 1, comprising:
s1, adding acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, the monomer I, the monomer II and the monomer III into water to form a solution, and regulating the pH value of the solution to 7-11 by utilizing sodium silicate;
s2, controlling the temperature of the solution to be 3-10 ℃, and adding the initiator to perform the free radical polymerization reaction;
s3, the heat released by the free radical polymerization reaction increases the temperature of the reaction system, and the reaction is continued for 2 to 6 hours after the temperature of the reaction system reaches the highest point.
4. The method of claim 3, wherein the initiator is a complex system comprising a redox system initiator and an azo initiation system initiator; the redox system initiator consists of potassium persulfate, ascorbic acid and white suspending block; the azo initiation system initiator is a mixture of azo diisobutylamidine hydrochloride and azo diiso Ding Mi-hydrochloride;
the mass addition amount of the redox system and the azo initiation system initiator is 10 multiplied by 10 respectively of the total mass of the reaction system -6 ～120×10 -6 。
5. The method according to claim 4, wherein a tertiary amine and urea are further added to the reaction system.
6. The process according to claim 3, wherein the total mass concentration of the reaction monomers in the radical polymerization system is 19 to 35%.
7. A process according to claim 3, wherein the maximum temperature reached by the reaction system is 55-70 ℃.
8. A process according to claim 3, wherein the preparation of monomer II comprises:
s11, maintaining the toluene solution of cyanuric chloride at 0-5 ℃, dropwise adding the toluene solution of n-octylamine under stirring, and continuously dropwise adding a sodium hydroxide solution after the dropwise adding is finished so as to maintain the pH value of the system to be 8 in the reaction process, and monitoring the reaction to an end point by using a toluene and acetone mixed solution with the volume ratio of 1:1;
s12, heating the reaction system to 45-50 ℃, dropwise adding an aqueous solution of aminoethanesulfonic acid, dropwise adding a sodium hydroxide solution in the reaction process to maintain the pH value of the system to be 8-9, and monitoring the reaction to an end point by using a mixed solution of acetone, toluene and water in a volume ratio of 6:1:0.5;
s13, heating the reaction system to 90 ℃, dropwise adding an aqueous solution of tri (2-aminoethyl) amine, dropwise adding a sodium carbonate solution in the reaction process to maintain the pH value of the system to be 9, and monitoring the reaction to an end point by using a mixed solution of methanol and toluene with the volume ratio of 6:1;
s14, carrying out quaternization reaction on the reaction product obtained in the step S13 and 4-benzyl chlorostyrene in an equimolar ratio to obtain the monomer II.
9. The method according to claim 8, wherein the molar ratio of the aqueous solution of tris (2-aminoethyl) amine to the product of the step S12 is 1.1:1.
10. The process according to claim 3, wherein the monomer III is obtained by reacting a polyoxyethylene ether of Bei Techun with p-toluenesulfonyl chloride and then with diallylamine.
11. The preparation method according to claim 10, wherein the fibrate alcohol is one or more of fibrate dodecanol, tetradecanol, hexadecanol and octadecanol, and the polyoxyethylene ether has a polymerization degree of 5-50.
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| CN110591012A (en) * | 2019-09-09 | 2019-12-20 | 中海石油(中国)有限公司 | Water-soluble hyperbranched polymer thickened oil viscosity reducer and preparation method thereof |
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| CN107383273A (en) * | 2017-08-04 | 2017-11-24 | 中国海洋石油总公司 | A kind of viscous crude activator and preparation method thereof |
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