CN114380946A - Self-tackifying steering acid liquid thickener and preparation method and application thereof - Google Patents
Self-tackifying steering acid liquid thickener and preparation method and application thereof Download PDFInfo
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- CN114380946A CN114380946A CN202011137159.XA CN202011137159A CN114380946A CN 114380946 A CN114380946 A CN 114380946A CN 202011137159 A CN202011137159 A CN 202011137159A CN 114380946 A CN114380946 A CN 114380946A
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- 239000002253 acid Substances 0.000 title claims abstract description 91
- 239000002562 thickening agent Substances 0.000 title claims abstract description 84
- 239000007788 liquid Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title abstract description 28
- 239000000178 monomer Substances 0.000 claims abstract description 69
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 5
- 125000001165 hydrophobic group Chemical group 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims description 10
- AVWKSSYTZYDQFG-UHFFFAOYSA-M dimethyl-octadecyl-prop-2-enylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CC=C AVWKSSYTZYDQFG-UHFFFAOYSA-M 0.000 claims description 10
- 239000003999 initiator Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000012966 redox initiator Substances 0.000 claims description 9
- XLPJNCYCZORXHG-UHFFFAOYSA-N 1-morpholin-4-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCOCC1 XLPJNCYCZORXHG-UHFFFAOYSA-N 0.000 claims description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- DJEHXEMURTVAOE-UHFFFAOYSA-M potassium bisulfite Chemical compound [K+].OS([O-])=O DJEHXEMURTVAOE-UHFFFAOYSA-M 0.000 claims description 8
- 229940099427 potassium bisulfite Drugs 0.000 claims description 8
- 235000010259 potassium hydrogen sulphite Nutrition 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 239000007800 oxidant agent Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- -1 alkyl dimethyl allyl ammonium chloride Chemical compound 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 239000003002 pH adjusting agent Substances 0.000 claims description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000004280 Sodium formate Substances 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 2
- ACWKAVFAONSRKJ-UHFFFAOYSA-M hexadecyl-dimethyl-prop-2-enylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)CC=C ACWKAVFAONSRKJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims description 2
- 235000019254 sodium formate Nutrition 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- FZGFBJMPSHGTRQ-UHFFFAOYSA-M trimethyl(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCOC(=O)C=C FZGFBJMPSHGTRQ-UHFFFAOYSA-M 0.000 claims description 2
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 2
- 230000000638 stimulation Effects 0.000 claims 1
- 230000020477 pH reduction Effects 0.000 abstract description 8
- 238000010276 construction Methods 0.000 abstract description 6
- 230000009467 reduction Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 79
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 230000000977 initiatory effect Effects 0.000 description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 12
- 239000000843 powder Substances 0.000 description 11
- 238000001035 drying Methods 0.000 description 8
- 238000007873 sieving Methods 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- DIHKMUNUGQVFES-UHFFFAOYSA-N n,n,n',n'-tetraethylethane-1,2-diamine Chemical compound CCN(CC)CCN(CC)CC DIHKMUNUGQVFES-UHFFFAOYSA-N 0.000 description 1
- QJFMXJDSWJZAAL-UHFFFAOYSA-N n,n,n',n'-tetrakis(prop-2-enyl)ethane-1,2-diamine Chemical compound C=CCN(CC=C)CCN(CC=C)CC=C QJFMXJDSWJZAAL-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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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
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
-
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/72—Eroding chemicals, e.g. acids
- C09K8/74—Eroding chemicals, e.g. acids combined with additives added for specific purposes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Detergent Compositions (AREA)
- Lubricants (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides a self-thickening acid-diverting thickener, and a preparation method and application thereof. The self-tackifying to acid liquid thickener is a quaternary polymer which is formed by copolymerizing quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide monomers and rigid monomers, takes acrylamide as a main chain and contains hydrophobic groups. The invention also provides a preparation method of the self-tackifying steering acid liquid thickener, which comprises the step of carrying out polymerization reaction on the quaternary ammonium salt unsaturated monomer, the long-chain unsaturated monomer, the acrylamide and the rigid monomer serving as raw materials at a temperature of between 5 ℃ below zero and 5 ℃ for 3 to 5 hours to obtain the self-tackifying steering acid liquid thickener. The invention also provides application of the self-tackifying steering acid liquid thickener in acidification or acid fracturing yield increase construction. The self-viscosity-increasing acid-liquid-turning thickening agent provided by the invention has the advantages of low concentration, friction resistance reduction and high temperature resistance when being applied to acidification or acid fracturing production increase construction.
Description
Technical Field
The invention relates to the technical field of carbonate oil and gas field development acidification or acid fracturing yield increase, in particular to a self-viscosifying and acid-diverting viscosifier and a preparation method and application thereof.
Background
The carbonate reservoir has the characteristics of universal crack development, strong heterogeneity and the like. In the acidification or acid fracturing process, acid liquor easily enters a large pore channel or a high permeability layer preferentially, and due to the corrosion action of the acid liquor, the large pore channel or the high permeability layer is further expanded to form an acid liquor action dominant channel in a stratum, so that the transformation efficiency of a low permeability compact layer is low, and the phenomenon is particularly prominent in a naked eye horizontal section.
In order to achieve the purpose of uniform and deep reconstruction, a VDA (vertical double-diffused vertical double-acting absorption enhancer) diversion acid liquor system is usually adopted, the system mainly comprises one or more surfactants with certain hydrophobic property, along with the reaction of the acid liquor and the stratum, the mineralization degree of the solution is increased, the critical micelle concentration of surfactant molecules in the solution is reduced, and single surfactant molecules are subjected to multi-stage association to finally form gel, so that the effect of blocking a high-depth reconstructed low-permeability layer section is realized, and the purpose of increasing the yield of an oil-gas well is achieved.
However, the current self-diverting acid liquid systems still have certain problems: (1) the concentration of the diverter is generally about 4-8 percent, so that the effect of effective tackifying can be achieved; (2) the temperature resistance has certain defects, and the common use temperature is lower than 120 ℃; (3) the friction resistance of the steering acid liquid system in a shaft is large, and the injection and discharge capacity of the acid liquid is limited under the condition of pressure limitation. Therefore, it is necessary to provide a self-diverting acid liquid system which is resistant to high temperature, has a low use concentration and has a function of reducing friction resistance.
Disclosure of Invention
In order to solve the above problems, the present invention aims to provide a self-thickening acid-to-acid thickener, and a preparation method and an application thereof. The self-tackifying steering acid liquid thickener is a quadripolymer, and has the characteristics of low concentration, friction resistance reduction and high temperature resistance when applied and constructed; the preparation method of the acid thickener is simple in process and convenient to popularize and use.
In order to achieve the purpose, the invention provides a self-viscosity-increasing acid-liquid-changing thickener which is a quaternary polymer which is formed by copolymerizing quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide monomers and rigid monomers, takes acrylamide as a main chain and contains hydrophobic groups.
In the above self-viscosifying acid-diverting acid viscosifier, the self-viscosifying acid-diverting viscosifier is generally a water-soluble high polymer.
The existing acid liquid system mainly uses a long-chain surfactant as a thickening agent, the molecular weight of the system is small, so that the tackifying capability is weak, and the molecular chain is seriously bent due to the large molecular weight, so that the friction resistance can be increased; compared with the prior art, the self-tackifying steering acid solution densifier provided by the invention has larger molecular weight, so that the self-tackifying steering acid solution densifier can achieve a tackifying effect under the condition of reducing concentration, and meanwhile, as the molecular chain of the self-tackifying steering acid solution densifier contains a rigid monomer, the molecular chain is relatively difficult to bend, and the friction resistance can be reduced. Preferably, the viscosity average molecular weight of the self-viscosifying acid-diverting acid viscosifier is 20-80 ten thousand.
In a specific embodiment of the invention, the molecule of the self-viscosity increasing acid-liquid thickener can be composed of four units of quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide and rigid monomers. In particular embodiments of the present invention, the molecular structure of the self-viscosifying to acid viscosifier includes, but is not limited to, the following:
1. a molecular structure obtained by cross arrangement and polymerization of four monomers, namely quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide and rigid monomers;
2. the same monomers are polymerized first, and then the polymers of all the monomers are copolymerized to obtain a molecular structure;
3. the molecular structure is obtained by the random combination and copolymerization of the four monomers.
In the self-viscosifying acid-diverting acid thickener, the solid content of the self-viscosifying acid-diverting acid thickener is generally above 85%, and preferably, the solid content of the acid thickener is greater than or equal to 90%.
In the above self-viscosifying acid-diverting acid thickener, preferably, the self-viscosifying acid-diverting acid thickener is formed by copolymerizing raw material compositions, wherein the raw material compositions comprise, in parts by mass: 20-80 parts of quaternary ammonium salt unsaturated monomer, 1-5 parts of long-chain unsaturated monomer, more than 0 part and less than or equal to 40 parts of acrylamide monomer and 5-20 parts of rigid monomer.
In a specific embodiment of the invention, the mass ratio of the quaternary ammonium salt unsaturated monomer, the long-chain unsaturated monomer, the acrylamide monomer and the rigid monomer can be controlled to be (20-80): (1-5): (20-40): (5-20)
In a specific embodiment of the present invention, the mass ratio of the acrylamide in the raw material composition can be controlled to be greater than 0% and less than or equal to 40%, based on 100% of the total weight of the raw materials.
In the self-tackifying steering acid solution thickener, the quaternary ammonium salt unsaturated monomer can provide hydrophobic groups for the self-tackifying steering acid solution thickener and can improve the temperature resistance and salt resistance of the self-tackifying steering acid solution thickener. Preferably, the quaternary ammonium salt type unsaturated monomer comprises dimethyldiallylammonium chloride and/or acryloyloxyethyltrimethylammonium chloride, more preferably dimethyldiallylammonium chloride.
In the self-tackifying steering acid solution thickener, the non-polarity of the long-chain alkyl in the long-chain unsaturated monomer is strong, and the long-chain alkyl can be associated and tackified in a polar solution, so that the viscoelasticity and the hydrophobic association of the self-tackifying steering acid solution thickener are improved. The long-chain unsaturated monomer may include long-chain alkyl dimethyl allyl ammonium chloride, and the carbon number of the long chain in the long-chain unsaturated monomer may be 12 to 20. For example, the long chain alkyl dimethyl allyl ammonium chloride monomer may include octadecyl dimethyl allyl ammonium chloride and/or hexadecyl dimethyl allyl ammonium chloride, preferably octadecyl dimethyl allyl ammonium chloride.
In the self-tackifying steering acid solution thickener, the rigid monomer can improve the temperature resistance and salt resistance of the self-tackifying steering acid solution thickener. In some embodiments, the rigid monomer may be a monomer having a molecular structure that is not easily twisted, such as a cycloalkyl group, and preferably, the rigid monomer includes acryloyl morpholine and/or vinyl pyrrolidone.
The invention also provides a preparation method of the self-tackifying acid-turning thickener, which comprises the following steps: the self-tackifying turning acid liquid thickener is prepared by carrying out polymerization reaction on quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide and rigid monomers serving as raw materials at a temperature of between 5 ℃ below zero and 5 ℃ for 3 to 5 hours.
In a specific embodiment of the present invention, the preparation method of the self-viscosifying to acid viscosifier may comprise the following processes:
dissolving quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide and rigid monomers in water to obtain an intermediate solution;
and step two, adding a low-temperature initiator, a molecular weight regulator and a redox initiator into the intermediate solution in a nitrogen atmosphere and/or an inert atmosphere, and carrying out polymerization reaction for 3-5h at the temperature of-5 ℃ to obtain the self-thickening diverting acid thickener.
In the above preparation method, the low-temperature initiator is used to lower the temperature at which polymerization reaction occurs. Preferably, the low-temperature initiator comprises one or a combination of more than two of ethylenediamine, triethylenetetramine, N, N, N ', N' -tetraethylethylenediamine and N, N, N ', N' -tetraallylethylenediamine.
In the preparation method, the molecular weight regulator can realize the adjustment of the molecular weight of the self-tackifying acid liquid thickener. Preferably, the molecular weight regulator comprises one or a combination of two or more of potassium formate, sodium formate and mercaptoethanol.
In the above production method, the redox initiator generally includes an oxidizing agent which may include one or a combination of two or more of potassium persulfate, sodium persulfate, and ammonium persulfate, and a reducing agent which may include sodium bisulfite and/or potassium bisulfite. The low-temperature initiator and the redox initiator form a low-temperature initiation system.
In the above preparation method, preferably, the mass concentration of the intermediate solution is 25% to 40%.
In the above production method, preferably, the mass of the low-temperature initiator is 0.005 to 0.03% of the total mass of the intermediate solution.
In the above production method, preferably, the mass of the molecular weight modifier is 0.01 to 0.05% of the total mass of the intermediate solution.
In the above production method, preferably, the mass of the redox initiator is 0.015 to 0.09% of the total mass of the intermediate solution. More preferably, the mass of the oxidizing agent is 0.01 to 0.06% of the total mass of the intermediate solution, and the mass of the reducing agent is 0.005 to 0.03% of the total mass of the intermediate solution.
According to a specific embodiment of the present invention, in the first step, the pH of the intermediate solution may be controlled to 5 to 7 (preferably 6 to 6.5). In some embodiments, step one may include adjusting the pH of the intermediate solution with a pH adjuster, which may include one or a combination of two or more of sodium hydroxide, potassium carbonate, sodium bicarbonate, potassium bicarbonate, glacial acetic acid, and hydrochloric acid.
According to the specific embodiment of the invention, in the second step, nitrogen is firstly introduced into the intermediate solution for 20-40min, then the low-temperature initiator and the molecular weight regulator are added, then nitrogen is introduced for 10-20min, and the redox initiator is added to carry out the polymerization reaction.
According to a specific embodiment of the present invention, in the second step, the reaction temperature of the polymerization reaction is preferably-5 ℃ to 0 ℃.
In a specific embodiment of the present invention, the preparation method may include the following processes: dissolving quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide and rigid monomers in water to form an intermediate solution, adjusting the temperature of the intermediate solution to the polymerization reaction temperature, introducing nitrogen or inert gas, removing oxygen in the reaction environment, adding a low-temperature initiator, a molecular weight regulator and a redox initiator, and carrying out polymerization reaction for 3-5 hours at the temperature of-5 ℃ to obtain the self-thickening to acid liquid thickener.
In the above preparation method, the acid thickener obtained in step two is generally in the form of gel. When acid thickener powder needs to be obtained, the preparation method can further comprise the following operation of carrying out post-treatment on the self-viscosifying diversion acid thickener: the method comprises the steps of granulating, drying, crushing, drying and sieving the acid liquid thickener prepared in the step two to obtain the self-tackifying turning acid liquid thickener powder.
The invention provides an application of the self-tackifying steering acid solution thickener in acidification or acid fracturing yield increase construction, and preferably, the use concentration of the self-tackifying steering acid solution thickener is 2-4 wt%.
The beneficial effects of the invention include:
1. the self-viscosity-increasing diverting acid liquid thickener provided by the invention has the advantages of low concentration, friction resistance reduction and high temperature resistance when being applied to acidification or acid fracturing production increase construction, and can reduce the cost and damage to stratum, reduce ground pumping pressure during construction and enlarge the application range of the acid liquid thickener.
2. The self-viscosity-increasing acid-changing thickener provided by the invention is prepared at 150 ℃ for 170s-1The viscosity retention rate after shearing for 60min is not lower than 80%, which is beneficial to increasing the effective acid solution action distance and improving the acidification effect of the high-temperature deep well of the carbonate reservoir.
3. The preparation method of the self-viscosity-increasing acid liquid thickener provided by the invention is simple in process and convenient to popularize and use.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
The embodiment provides a preparation method of a self-viscosity-increasing acid-liquid thickener, which specifically comprises the following steps:
1. fully mixing dimethyldiallylammonium chloride, octadecyl dimethyl allylammonium chloride, acrylamide and acryloyl morpholine in distilled water according to the mass ratio of 7:0.2:2:0.8 to prepare an intermediate solution with the mass concentration of 30%, adding glacial acetic acid and sodium carbonate as pH regulators until the pH of the intermediate solution reaches 6.3, and placing the intermediate solution in an oil bath pan for temperature control.
2. Adjusting the temperature of an oil bath kettle to be-3 ℃, continuously introducing 99.999% high-purity nitrogen into the intermediate solution, adding a low-temperature initiation system formed by ethylenediamine, ammonium persulfate and potassium bisulfite with the mass ratio of 5.5:3:1.5 after 30min, adding potassium formate serving as a molecular weight regulator, sealing after 20min, and reacting for 4 h to obtain a self-thickening-acid-liquid-thickener gel block;
wherein the low-temperature initiation system accounts for 0.02 percent of the total mass of the intermediate solution, and the potassium formate accounts for 0.02 percent of the total mass of the intermediate solution.
3. Granulating the self-tackifying turning acid liquid thickener gel block, drying for 7h at 70 ℃, and then crushing and sieving to obtain self-tackifying turning acid liquid thickener powder, which is marked as SW-1.
Example 2
The embodiment provides a preparation method of a self-viscosity-increasing acid-liquid thickener, which is different from the embodiment 1 in that the mass concentration of an intermediate solution is different, and the preparation method specifically comprises the following steps:
1. fully mixing dimethyldiallylammonium chloride, octadecyl dimethyl allylammonium chloride, acrylamide and acryloyl morpholine in distilled water according to the mass ratio of 7:0.2:1.8:1 to prepare an intermediate solution with the mass concentration of 40%, adding glacial acetic acid and sodium carbonate as pH regulators until the pH of the intermediate solution reaches 6.3, and placing the intermediate solution in an oil bath pan for temperature control.
2. Adjusting the temperature of an oil bath kettle to be-3 ℃, continuously introducing 99.999% high-purity nitrogen into the intermediate solution, adding a low-temperature initiation system formed by ethylenediamine, ammonium persulfate and potassium bisulfite with the mass ratio of 5.5:3:1.5 after 30min, adding potassium formate serving as a molecular weight regulator, sealing after 20min, and reacting for 4 h to obtain a self-thickening-acid-liquid-thickener gel block;
wherein the low-temperature initiation system accounts for 0.02 percent of the total mass of the intermediate solution, and the potassium formate accounts for 0.02 percent of the total mass of the intermediate solution.
3. Granulating the self-tackifying turning acid liquid thickener gel block, drying for 7h at 70 ℃, and then crushing and sieving to obtain self-tackifying turning acid liquid thickener powder, which is marked as SW-2.
Example 3
The embodiment provides a preparation method for a self-viscosity-increasing acid-liquid thickener, which is different from the preparation method in embodiment 1 in that the mass ratio between solutes in an intermediate solution and the mass concentration of the intermediate solution are different, and the preparation method specifically comprises the following steps:
1. fully mixing dimethyldiallylammonium chloride, octadecyl dimethyl allylammonium chloride, acrylamide and acryloyl morpholine in distilled water according to the mass ratio of 8:0.2:0.8:1 to prepare an intermediate solution with the mass concentration of 40%, adding glacial acetic acid and sodium carbonate as pH regulators until the pH of the intermediate solution reaches 6.3, and placing the intermediate solution in an oil bath pan for temperature control.
2. Adjusting the temperature of an oil bath kettle to be-3 ℃, continuously introducing 99.999% high-purity nitrogen into the intermediate solution, adding a low-temperature initiation system formed by ethylenediamine, ammonium persulfate and potassium bisulfite with the mass ratio of 5.5:3:1.5 after 30min, adding potassium formate serving as a molecular weight regulator, sealing after 20min, and reacting for 4 h to obtain a self-thickening-acid-liquid-thickener gel block;
wherein the low-temperature initiation system accounts for 0.02 percent of the total mass of the intermediate solution, and the potassium formate accounts for 0.02 percent of the total mass of the intermediate solution.
3. Granulating the self-tackifying turning acid liquid thickener gel block, drying for 7h at 70 ℃, and then crushing and sieving to obtain self-tackifying turning acid liquid thickener powder, which is marked as SW-3.
Example 4
The embodiment provides a preparation method of a self-viscosity-increasing acid-liquid thickener, which is different from the preparation method of embodiment 1 in the mass concentration of an intermediate solution, the mass ratio between solutes of the intermediate solution, the dosage of a low-temperature initiation system and the dosage of a molecular weight regulator, and specifically comprises the following steps:
1. fully mixing dimethyldiallylammonium chloride, octadecyl dimethyl allylammonium chloride, acrylamide and acryloyl morpholine in distilled water according to the mass ratio of 8:0.2:0.8:1 to prepare an intermediate solution with the mass concentration of 40%, adding glacial acetic acid and sodium carbonate as pH regulators until the pH of the intermediate solution reaches 6.3, and placing the intermediate solution in an oil bath pan for temperature control.
2. Adjusting the temperature of an oil bath kettle to be-3 ℃, continuously introducing 99.999% high-purity nitrogen into the intermediate solution, adding a low-temperature initiation system formed by ethylenediamine, ammonium persulfate and potassium bisulfite with the mass ratio of 5.5:3:1.5 after 30min, adding potassium formate serving as a molecular weight regulator, sealing after 20min, and reacting for 4 h to obtain a self-thickening-acid-liquid-thickener gel block;
wherein the low-temperature initiation system accounts for 0.04 percent of the total mass of the intermediate solution, and the potassium formate accounts for 0.04 percent of the total mass of the intermediate solution.
3. Granulating the self-tackifying turning acid liquid thickener gel block, drying for 7h at 70 ℃, and then crushing and sieving to obtain self-tackifying turning acid liquid thickener powder, which is marked as SW-4.
Example 5
The embodiment provides a preparation method of a self-viscosity-increasing acid-liquid thickener, which is different from the preparation method of embodiment 1 in the mass concentration of an intermediate solution, the mass ratio between solutes of the intermediate solution, the dosage of a low-temperature initiation system and the dosage of a molecular weight regulator, and specifically comprises the following steps:
1. fully mixing dimethyldiallylammonium chloride, octadecyl dimethyl allylammonium chloride, acrylamide and acryloyl morpholine in distilled water according to the mass ratio of 8:0.2:0.8:1 to prepare an intermediate solution with the mass concentration of 25%, adding glacial acetic acid and sodium carbonate as pH regulators until the pH of the intermediate solution reaches 6.3, and placing the intermediate solution in an oil bath pan for temperature control.
2. Adjusting the temperature of an oil bath kettle to be-3 ℃, continuously introducing 99.999% high-purity nitrogen into the intermediate solution, adding a low-temperature initiation system formed by ethylenediamine, ammonium persulfate and potassium bisulfite with the mass ratio of 5.5:3:1.5 after 30min, adding potassium formate serving as a molecular weight regulator, sealing after 20min, and reacting for 4 h to obtain a self-thickening-acid-liquid-thickener gel block;
wherein the low-temperature initiation system accounts for 0.04 percent of the total mass of the intermediate solution, and the potassium formate accounts for 0.04 percent of the total mass of the intermediate solution.
3. Granulating the self-tackifying turning acid liquid thickener gel block, drying for 7h at 70 ℃, and then crushing and sieving to obtain self-tackifying turning acid liquid thickener powder, which is marked as SW-5.
Example 6
The embodiment provides a preparation method of a self-viscosity-increasing acid-liquid thickener, which is different from the preparation method of embodiment 1 in the mass concentration of an intermediate solution, the mass ratio between solutes of the intermediate solution, the dosage of a low-temperature initiation system and the dosage of a molecular weight regulator, and specifically comprises the following steps:
1. fully mixing dimethyldiallylammonium chloride, octadecyl dimethyl allylammonium chloride, acrylamide and acryloyl morpholine in distilled water according to the mass ratio of 7.5:0.2:1.5:0.8 to prepare an intermediate solution with the mass concentration of 40%, adding glacial acetic acid and sodium carbonate as pH regulators until the pH of the intermediate solution reaches 6.3, and placing the intermediate solution in an oil bath pan for controlling the temperature.
2. Adjusting the temperature of an oil bath kettle to be-3 ℃, continuously introducing 99.999% high-purity nitrogen into the intermediate solution, adding a low-temperature initiation system formed by ethylenediamine, ammonium persulfate and potassium bisulfite with the mass ratio of 5.5:3:1.5 after 30min, adding potassium formate serving as a molecular weight regulator, sealing after 20min, and reacting for 4 h to obtain a self-thickening-acid-liquid-thickener gel block;
wherein the low-temperature initiation system accounts for 0.04 percent of the total mass of the intermediate solution, and the potassium formate accounts for 0.04 percent of the total mass of the intermediate solution.
3. Granulating the self-tackifying turning acid liquid thickener gel block, drying for 7h at 70 ℃, and then crushing and sieving to obtain self-tackifying turning acid liquid thickener powder, which is marked as SW-6.
Test example 1
The present test example provides a test of the molecular weight, solid content and dissolution time in hydrochloric acid of 20% mass concentration of the self-thickening diverting acid thickener powder prepared in examples 1-6. The molecular weight test method of the self-viscosity-increasing diverting acid liquid thickener powder is based on the national industry standard GB 17514-2008-water treatment agent polyacrylamide; the test method of the hydrochloric acid dissolution time is summarized in Table 1 according to the oil industry standard SY/T6214-2016-thickening agent for thickening acid, and the test results and the appearance of the sample.
TABLE 1
As can be seen from the data in table 1, the self-viscosity increasing acid solution thickener prepared in examples 1 to 6 has a solid content of more than 90%, a viscosity average molecular weight of 20 to 65 ten thousand, and a dissolution time in 20% hydrochloric acid of 5 to 19min, which proves that the dissolution speed of the acid solution thickener provided by the present invention in hydrochloric acid is overall faster, the field construction is facilitated, and the adjustment of the dissolution speed of the acid solution thickener in hydrochloric acid can be realized by adjusting the monomer composition in the acid solution thickener.
The test example also provides a temperature resistance and shear resistance test for the above samples, the mass concentration of each sample is 1.5%, and the temperature is 150 ℃ for 170s-1Conditions (3) viscosity was determined after 60min of shearing, the test being carried out according to the oil industry Standard SY/T6214-2016-thickener for thickening acids, the test results being summarized in Table 2.
TABLE 2
As can be seen from the data in Table 2, the self-viscosifying to acid viscosifier powders prepared in examples 1-6 were prepared at 150 ℃ for 170s-1The apparent viscosity after shearing for 60min is still more than 40mPa.s, and the retention rate of the apparent viscosity is more than 80%, which proves that the self-thickening acid-to-acid thickener can be widely applied to high-temperature carbonate acidification or acid fracturing。
Claims (15)
1. The self-viscosity-increasing acid-liquid-changing thickener is a quaternary polymer which is formed by copolymerizing quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide monomers and rigid monomers, takes acrylamide as a main chain and contains hydrophobic groups.
2. The self-viscosifying to acid viscosifying agent of claim 1, wherein the self-viscosifying to acid viscosifying agent has a viscosity average molecular weight of 20 to 80 ten thousand.
3. The self-thickening acid-diverting acid thickener according to claim 1 or 2, wherein the solids content of the acid thickener is 90% or more.
4. The self-viscosifying acid-diverting agent according to any one of claims 1 to 3, wherein the self-viscosifying acid-diverting agent is formed by copolymerization of a raw material composition comprising, in parts by mass: 20-80 parts of quaternary ammonium salt unsaturated monomer, 1-5 parts of long-chain unsaturated monomer, more than 0 part and less than or equal to 40 parts of acrylamide monomer and 5-20 parts of rigid monomer;
preferably, the mass ratio of the quaternary ammonium salt unsaturated monomer, the long-chain unsaturated monomer, the acrylamide monomer and the rigid monomer is (20-80): (1-5): (20-40): (5-20);
preferably, the mass ratio of the acrylamide in the raw material composition is more than 0% and not more than 40% based on 100% of the total mass of the raw material composition.
5. A self-thickening acid-diverting thickener according to any of claims 1 to 4, wherein the unsaturated monomer of the quaternary ammonium salt type comprises dimethyldiallylammonium chloride and/or acryloyloxyethyltrimethylammonium chloride, preferably dimethyldiallylammonium chloride.
6. The self-viscosifying acid-diverting agent according to any one of claims 1 to 5, wherein the long chain unsaturated monomer comprises a long chain alkyl dimethyl allyl ammonium chloride;
preferably, the carbon number of the long chain in the long-chain unsaturated monomer is 12-20;
more preferably, the long-chain alkyl dimethyl allyl ammonium chloride monomer comprises octadecyl dimethyl allyl ammonium chloride and/or hexadecyl dimethyl allyl ammonium chloride, and further preferably octadecyl dimethyl allyl ammonium chloride.
7. A self-thickening acid-diverting thickener according to any of claims 3 to 6, wherein the rigid monomer comprises acryloyl morpholine and/or vinyl pyrrolidone.
8. A method of making a self-thickening acid-diverting acid thickener according to any of claims 1 to 7, comprising: carrying out polymerization reaction on quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide and rigid monomers serving as raw materials at a temperature of between 5 ℃ below zero and 5 ℃ for 3 to 5 hours to obtain the self-tackifying turning acid liquid thickener.
9. The production method according to claim 8, wherein the production method comprises:
dissolving quaternary ammonium salt unsaturated monomers, long-chain unsaturated monomers, acrylamide and rigid monomers in water to obtain an intermediate solution;
and step two, adding a low-temperature initiator, a molecular weight regulator and a redox initiator into the intermediate solution in a nitrogen atmosphere and/or an inert atmosphere, and carrying out polymerization reaction for 3-5 hours at the temperature of-5 ℃ to obtain the self-thickening diverting acid thickener.
10. The production method according to claim 8 or 9, wherein the reaction temperature of the polymerization reaction is from-5 ℃ to 0 ℃.
11. The production method according to claim 9, wherein the intermediate solution has a mass concentration of 25% to 40%.
12. The production method according to claim 9, wherein the low-temperature initiator includes one or a combination of two or more of ethylenediamine, triethylenetetramine, N '-tetraethylethylenediamine, and N, N' -tetraallylethylenediamine;
the molecular weight regulator comprises one or the combination of more than two of potassium formate, sodium formate and mercaptoethanol;
the redox initiator comprises an oxidizing agent and a reducing agent, wherein the oxidizing agent comprises one or a combination of more than two of potassium persulfate, sodium persulfate and ammonium persulfate, and the reducing agent comprises sodium bisulfite and/or potassium bisulfite.
13. The production method according to claim 9 or 12, wherein the mass of the low-temperature initiator is 0.005 to 0.03% of the total mass of the intermediate solution;
the mass of the molecular weight regulator is 0.01-0.05% of the total mass of the intermediate solution;
the mass of the redox initiator is 0.015-0.09% of the total mass of the intermediate solution;
preferably, the mass of the oxidizing agent is 0.01-0.06% of the total mass of the intermediate solution, and the mass of the reducing agent is 0.005-0.03% of the total mass of the intermediate solution.
14. The method according to claim 9, wherein in the first step, the pH of the intermediate solution is 5 to 7; preferably, the pH of the intermediate solution is 6-6.5;
preferably, the first step includes the operation of adjusting the pH value of the intermediate solution by using a pH adjusting agent, wherein the pH adjusting agent includes one or a combination of two or more of sodium hydroxide, potassium carbonate, sodium bicarbonate, potassium bicarbonate, glacial acetic acid and hydrochloric acid.
15. Use of the self-viscosifying to acid viscosifying agent of any one of claims 1 to 7 in acidizing or acid fracturing stimulation operations; preferably, the concentration of the self-thickening acid-diverting thickener is 2-4 wt%.
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