CN115785937A - Acid-resistant waterproof locking agent for low-permeability gas well and preparation method thereof - Google Patents
Acid-resistant waterproof locking agent for low-permeability gas well and preparation method thereof Download PDFInfo
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 55
- 239000002253 acid Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- -1 quaternary ammonium halide Chemical class 0.000 claims abstract description 88
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 39
- 230000007797 corrosion Effects 0.000 claims abstract description 37
- 238000005260 corrosion Methods 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000003112 inhibitor Substances 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 18
- 150000003512 tertiary amines Chemical class 0.000 claims description 16
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 13
- 230000035699 permeability Effects 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 5
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 4
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 4
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 150000003841 chloride salts Chemical group 0.000 claims 1
- 239000011435 rock Substances 0.000 abstract description 7
- 150000001768 cations Chemical class 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 41
- 239000007789 gas Substances 0.000 description 34
- 239000000243 solution Substances 0.000 description 23
- ULTHEAFYOOPTTB-UHFFFAOYSA-N 1,4-dibromobutane Chemical group BrCCCCBr ULTHEAFYOOPTTB-UHFFFAOYSA-N 0.000 description 19
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 14
- 235000019441 ethanol Nutrition 0.000 description 13
- 239000004094 surface-active agent Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000002981 blocking agent Substances 0.000 description 7
- 239000012530 fluid Substances 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000006378 damage Effects 0.000 description 5
- 239000002736 nonionic surfactant Substances 0.000 description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- KJDRSWPQXHESDQ-UHFFFAOYSA-N 1,4-dichlorobutane Chemical compound ClCCCCCl KJDRSWPQXHESDQ-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 229940077388 benzenesulfonate Drugs 0.000 description 2
- SRSXLGNVWSONIS-UHFFFAOYSA-M benzenesulfonate Chemical compound [O-]S(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-M 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 239000002888 zwitterionic surfactant Substances 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- WESZRJDUYAKEOH-UHFFFAOYSA-N FC=1C(=C(C(=C(C=1F)F)F)O)C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F Chemical compound FC=1C(=C(C(=C(C=1F)F)F)O)C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F WESZRJDUYAKEOH-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 1
- RULGYZBKEXOMGE-UHFFFAOYSA-N O=S(C(C=CC=C1)=C1OC1=CC=CC=C1)(OC(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)=O Chemical compound O=S(C(C=CC=C1)=C1OC1=CC=CC=C1)(OC(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)=O RULGYZBKEXOMGE-UHFFFAOYSA-N 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 150000001669 calcium Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 150000001805 chlorine compounds Chemical group 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 1
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VHDPPDRSCMVFAV-UHFFFAOYSA-N n,n-dimethylhexadecan-1-amine;hydrobromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH+](C)C VHDPPDRSCMVFAV-UHFFFAOYSA-N 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 1
- RRRXPPIDPYTNJG-UHFFFAOYSA-N perfluorooctanesulfonamide Chemical compound NS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F RRRXPPIDPYTNJG-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920006027 ternary co-polymer Polymers 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an acid-resistant waterproof locking agent for a low-permeability gas well and a preparation method thereof, wherein the acid-resistant waterproof locking agent comprises the following components in percentage by weight: 5-20% of gemini quaternary ammonium halide, 10-20% of low-carbon chain alcohol, 2-5% of cationic surfactant, 0.5-1% of corrosion inhibitor and the balance of water. The gemini quaternary ammonium salt halide disclosed by the invention is a cation containing double chains, has a lower CMC value and adsorption performance, can be adsorbed on the surface of a rock when being contacted with the surface of the rock, so that the hydrophilicity is changed into weak lipophilicity, the adhesion work is effectively reduced, the flow resistance is reduced, and the waterproof locking agent is environment-friendly and has lower cost.
Description
Technical Field
The invention relates to the technical field of oil and gas exploitation, in particular to an acid-resistant waterproof locking agent for a low-permeability gas well and a preparation method thereof.
Background
In the process of natural gas development, a horizontal well-digging fracturing synergistic technology is generally implemented, and the flow-back amount of fracturing fluid in fracturing construction is an important factor influencing the fracturing construction effect and oil gas yield increase. Because the permeability of the low-permeability gas-permeable well is low, when external fluid in the gas well reaches a certain condition, the permeability in the gas well can be linearly reduced, so that a water lock effect occurs in a reservoir of the gas well, and the production yield is influenced, therefore, the water lock-preventing agent is an important auxiliary agent in oil and gas production. The acid pretreatment technology before fracturing can reduce the damage in the fracturing process, improve the fracturing effect and improve the permeability of the rock core.
The existing waterproof locking agent added into the fracturing fluid mainly comprises a surfactant, modified organic silicon and fluorocarbon. The low-permeability oil-gas reservoir waterproof locking agent disclosed in the publication No. CN113462373A is composed of ternary copolymer block silicone oil, glacial acetic acid and a defoaming agent. The publication No. CN113308236A discloses a temperature-resistant, efficient and compact waterproof locking agent for gas reservoir fracturing and an application thereof, wherein a fluorocarbon nonionic surfactant, perfluorononyl phenoxybenzene sulfonate, branched-chain dodecylbenzene sulfonate, short-chain alcohol and organic carboxylate are adopted, and the technical scheme mainly improves the temperature resistance of the fracturing fluid. The waterproof locking agent disclosed in publication No. CN114316924A consists of a cation and anion pair, a zwitterionic surfactant and short-chain alcohol, and the technical problems solved by the technical scheme are mainly the technical problems of high foamability and low wettability. The publication No. CN113528099A discloses a waterproof locking agent and a preparation method thereof, wherein the waterproof locking agent is composed of nonionic surfactant isomeric fatty alcohol polyoxyethylene ether, an anionic surfactant, a zwitterionic surfactant (betaine) and a low-carbon alcohol, and the technical scheme mainly reduces low surface tension and oil-water interfacial tension and improves neutral wetting. The publication No. CN104927830A discloses a waterproof lock fracturing fluid and a preparation method thereof, wherein the waterproof lock agent is composed of a cationic surfactant cetyl dimethyl ammonium bromide, a nonionic surfactant octylphenol polyoxyethylene ether and a fluorocarbon surfactant, and the technical problems of low drainage rate and great damage to rocks are solved. Publication No. CN114958330A discloses a waterproof locking agent for fracturing and a preparation method thereof, which is prepared from sodium p-perfluorononenoxybenzene sulfonate, perfluorooctylsulfonyl polyoxyethylene ether and sodium dodecyl benzene sulfonate. Publication No. CN110387218A discloses a modified calcium brine workover fluid and a preparation method thereof, wherein the adopted waterproof locking agent is a cationic fluorocarbon surfactant, a non-ionic fluorocarbon surfactant, a foaming agent and octadecyl trimethyl ammonium chloride.
In summary, the existing water-proof locking agent for fracturing fluid mainly adopts fluorocarbon, modified silicon and nonionic surfactant which are used singly or in a mixed way. Most fluorocarbon surfactants adopt perfluorononyl-enoxy benzene sulfonate, perfluorooctyl sulfonamide polyoxyethylene ether nonionic surfactants and the like, and the fluorocarbon surfactants contain PFOS, are not easy to degrade and are forbidden at present. Pure fluorocarbon has a low surface tension but is costly.
Disclosure of Invention
In order to solve the problems, the invention provides an acid-resistant waterproof locking agent for a low-permeability gas well, which takes a cationic surfactant as a main waterproof locking agent, has low surface tension, shortens the liquid drainage time and lightens the damage of water lock; the wettability is changed, the adhesion work is effectively reduced, and the flow resistance is reduced. And the method is environment-friendly, has lower cost and good strong acid resistance.
In order to achieve the purpose, the invention is realized by the following technical scheme:
an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following components in percentage by weight: 5-20% of gemini quaternary ammonium halide, 10-20% of low-carbon chain alcohol, 2-5% of cationic surfactant, 0.5-1% of corrosion inhibitor and the balance of water.
It is further noted that said gemini quaternary ammonium bromide or gemini quaternary ammonium chloride is used.
Further, the gemini quaternary ammonium salt bromide or chloride is obtained by reacting dihalogenated alkane with tertiary amine.
It needs to be further explained that the preparation method of the gemini quaternary ammonium salt bromide or chloride comprises the following steps: tertiary amine and dihaloalkane are mixed according to the molar ratio of 1.8-2.2: 1 and reacted in an organic solvent.
It is further noted that the molar ratio of tertiary amine to dihaloalkane is 2.
Further, the alkyl chain length of the tertiary amine is C8-C18.
Further, the tertiary amine is one or two of dodecyl tertiary amine, tetradecyl tertiary amine, hexadecyl tertiary amine and octadecyl tertiary amine. If one tertiary amine is used, a symmetrical gemini quaternary ammonium halide is formed. If there are two types of tertiary amines, an asymmetric gemini quaternary ammonium halide is formed.
It is further noted that the dihaloalkane is 1, 4-dibromobutane or 1, 4-dichlorobutane.
Further, the low carbon chain alcohol is one or more of methanol, ethylene glycol, ethanol, isopropanol and butanediol.
Further, the cationic surfactant is chloride or sulfate with alkyl chain length of C12-C18.
Further, the cationic surfactant is any one or a combination of dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, dodecyl trimethyl sulfate, hexadecyl trimethyl sulfate and octadecyl trimethyl sulfate.
The invention also discloses a preparation method of the acid-resistant waterproof locking agent for the low-permeability gas well, which comprises the following steps: adding water into a reaction kettle, slowly heating to 40-60 ℃, sequentially adding C8-C18 gemini quaternary ammonium halide and a cationic surfactant, and stirring for 3-4 hours; then adding low carbon chain alcohol and corrosion inhibitor, stirring evenly, and adjusting the pH value to 1-2 by adopting a pH regulator.
The acid-resistant waterproof locking agent for the low-permeability gas well and the preparation method have the beneficial effects that:
(1) The gemini quaternary ammonium salt halide provided by the invention is a cation containing double chains, has a lower CMC value and adsorption performance, and can be adsorbed on the surface of rock when contacting with the surface of the rock, so that the hydrophilicity is changed into weak lipophilicity, the adhesion work is effectively reduced, and the flow resistance is reduced.
(2) After the gemini quaternary ammonium salt halide and the cationic surfactant are compounded, the adsorption effect is increased, the interfacial activity is improved, and the effect of the waterproof locking agent is better.
(3) The water-proof locking agent is cationic, has good acid resistance, can obviously reduce the surface tension in acid liquor, change the wettability of a reservoir, reduce the water-locking damage and the capillary resistance of the reservoir, has effect on the reconstruction of the strong water-locking reservoir, has certain corrosion inhibition performance and small corrosion performance to equipment.
(4) The gemini quaternary ammonium salt and the cationic surfactant are compounded, so that the gemini quaternary ammonium salt and the cationic surfactant have good biodegradability. Compared with the existing fluorocarbon surfactants, the waterproof locking agent is environment-friendly, and the cost is reduced by about 10-15% compared with fluorocarbon or organosilicon.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
An acid-resistant waterproof locking agent for a low-permeability gas well comprises the following components in percentage by weight: 5-20% of gemini quaternary ammonium halide, 10-20% of low-carbon chain alcohol, 2-5% of cationic surfactant, 0.5-1% of corrosion inhibitor and the balance of water.
It is worth mentioning that the gemini quaternary ammonium salt halide is obtained by reacting dihalogenated alkane with tertiary amine.
The specific preparation method of the gemini quaternary ammonium salt halide comprises the following steps:
(1) Adding an organic solvent into a reaction kettle, and mixing tertiary amine and dihalogenated alkane in the reaction kettle according to the molar ratio of 2.01;
(2) Heating the temperature in the reaction kettle to 70-80 ℃, refluxing for 4-6h under the protection of nitrogen, removing the crude solvent, adding ethyl acetate, pulping at 70 ℃, then cooling to room temperature, filtering, leaching the solid with ethyl acetate for several times, and then drying the solid to obtain white solid powder, namely the gemini quaternary ammonium halide;
the reaction equation is:
wherein R is a C12 or C14 or C16 or C18 straight chain alkyl group.
In the preparation method of the gemini quaternary ammonium salt halide, the reaction temperature in the step (2) is set to be 70-80 ℃, preferably 80 ℃, the reaction can be promoted and the reaction process can be accelerated under the condition of increasing the temperature, and when the reaction temperature is too high, side reaction is easy to occur and the yield of the gemini quaternary ammonium salt halide is reduced, so that the reaction rate can be improved and the yield of the gemini quaternary ammonium salt halide can be improved by adopting a specific temperature.
In the preparation method of the gemini quaternary ammonium salt halide, the organic amine is easy to oxidize, so the nitrogen is adopted for protection in the whole process.
The dihaloalkane is 1, 4-dibromobutane or 1, 4-dichlorobutane. 1, 4-dibromobutane is adopted to react with tertiary amine to obtain gemini quaternary ammonium salt bromide. If 1, 4-dichlorobutane reacts with amine, gemini quaternary ammonium salt chloride is obtained.
The organic solvent is an aprotic polar solvent, which can promote the reaction. The organic solvent is selected from anhydrous alcohol, ether, and ethylene glycol. Preferably, absolute ethanol, which promotes the reaction.
The tertiary amine is one or two of dodecyl tertiary amine, tetradecyl tertiary amine, hexadecyl tertiary amine and octadecyl tertiary amine. If the tertiary amine is one, a symmetrical gemini quaternary ammonium halide is formed. If there are two types of tertiary amines, an asymmetric gemini quaternary ammonium halide is formed.
The low carbon chain alcohol is one or more of methanol, ethylene glycol, ethanol, isopropanol and butanediol.
The cationic surfactant is any one or combination of dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, dodecyl trimethyl sulfate, hexadecyl trimethyl sulfate and octadecyl trimethyl sulfate. Dodecyl trimethyl sulfate is obtained by reacting alkyl with dimethyl sulfate, thus showing the performance of the cationic surfactant.
The corrosion inhibitor is pyridine, naphthene, imidazoline or derivatives thereof, such as imidazoline quaternary ammonium salt, mannich base and/or pyridine. The corrosion inhibitor can effectively relieve the corrosion rate of the fracturing equipment in the using process.
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: adding water into a reaction kettle, slowly heating to 40-60 ℃, sequentially adding C8-C18 gemini quaternary ammonium halide and a cationic surfactant, and stirring for 3-4 hours; then adding low carbon chain alcohol and corrosion inhibitor, stirring uniformly, and adjusting the pH value to 1-2 by adopting a pH regulator.
The pH regulator is acidic pH regulator, and comprises any one of hydrochloric acid, sulfuric acid, and citric acid.
In the following embodiments of the invention, a preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: adding water into a reaction kettle, slowly heating to 40-60 ℃, sequentially adding C8-C18 gemini quaternary ammonium halide and a cationic surfactant, and stirring for 3-4 hours; then adding low carbon chain alcohol and corrosion inhibitor, stirring uniformly, and adjusting the pH value to 1-2 by adopting a pH regulator.
Example 1
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 7% of 12-4-14 Gemini quaternary ammonium salt dibromide, 10% of isopropanol, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 0.5% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 12-4-14 Gemini quaternary ammonium salt dibromide is obtained by reacting dodecyl tertiary amine, tetradecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 2
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 10% of 12-4-14 gemini quaternary ammonium salt dibromide, 10% of ethylene glycol, 2% of cationic surfactant cetyl trimethyl ammonium chloride, 0.5% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 12-4-14 Gemini quaternary ammonium salt dibromide is obtained by reacting dodecyl tertiary amine, tetradecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 3
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 10% of 12-4-14 Gemini quaternary ammonium salt dibromide, 10% of methanol, 2% of cationic surfactant octadecyl trimethyl ammonium chloride, 0.5% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 12-4-14 Gemini quaternary ammonium salt dibromide is obtained by reacting dodecyl tertiary amine, tetradecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 4
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 10% of 12-4-14 gemini quaternary ammonium salt dibromide, 10% of methanol, 2% of cationic surfactant dodecyl trimethyl sulfate, 0.5% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 12-4-14 Gemini quaternary ammonium salt dibromide is obtained by reacting dodecyl tertiary amine, tetradecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 5
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 10% of 12-4-14 Gemini quaternary ammonium salt dibromide, 10% of isopropanol, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 1% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 12-4-14 gemini quaternary ammonium salt dibromide is obtained by reacting dodecyl tertiary amine, tetradecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 6
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 15% of 12-4-14 Gemini quaternary ammonium salt dibromide, 15% of isopropanol, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 1% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 12-4-14 Gemini quaternary ammonium salt dibromide is obtained by reacting dodecyl tertiary amine, tetradecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 7
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 15% of 16-4-18 Gemini quaternary ammonium salt dibromide, 15% of isopropanol, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 1% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 16-4-18 gemini quaternary ammonium salt dibromide is obtained by reacting hexadecyl tertiary amine, octadecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 8
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 10% of 16-4-18 Gemini quaternary ammonium salt dibromide, 15% of ethylene glycol, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 1% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 16-4-18 gemini quaternary ammonium salt dibromide is obtained by reacting hexadecyl tertiary amine, octadecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 9
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 20% of 16-4-18 Gemini quaternary ammonium salt dibromide, 15% of butanediol, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 1% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 16-4-18 gemini quaternary ammonium salt dibromide is obtained by reacting hexadecyl tertiary amine, octadecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 10
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 15% of 14-4-16 gemini quaternary ammonium salt dibromide, 15% of isopropanol, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 1% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 14-4-16 gemini quaternary ammonium salt dibromide is obtained by reacting tetradecyl tertiary amine, hexadecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 11
A preparation method of an acid-resistant waterproof locking agent for a low permeability gas well comprises the following steps: 14-4-16 Gemini quaternary ammonium salt dibromide 10%, isopropanol 10%, cationic surfactant dodecyl trimethyl ammonium chloride 2%, corrosion inhibitor imidazoline quaternary ammonium salt 1%, and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 14-4-16 gemini quaternary ammonium salt dibromide is obtained by reacting tetradecyl tertiary amine, hexadecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 12
A preparation method of an acid-resistant waterproof locking agent for a low permeability gas well comprises the following steps: 14-4-16 Gemini quaternary ammonium salt dibromide 20%, isopropanol 10%, cationic surfactant dodecyl trimethyl ammonium chloride 2%, corrosion inhibitor imidazoline quaternary ammonium salt 1%, and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 14-4-16 gemini quaternary ammonium salt dibromide is obtained by reacting tetradecyl tertiary amine, hexadecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 1.
Example 13
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 12-4-12 Gemini quaternary ammonium salt dibromide 15%, isopropanol 10%, cationic surfactant dodecyl trimethyl ammonium chloride 2%, corrosion inhibitor imidazoline quaternary ammonium salt 1%, and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, 12-4-12 gemini quaternary ammonium salt dibromide is obtained by reacting dodecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 2.
Example 14
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 14-4-14 Gemini quaternary ammonium salt dibromide 15%, isopropanol 10%, cationic surfactant dodecyl trimethyl ammonium chloride 2%, corrosion inhibitor imidazoline quaternary ammonium salt 1%, and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 14-4-14 gemini quaternary ammonium salt dibromide is obtained by reacting tetradecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 2.
Example 15
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 15% of 16-4-16 Gemini quaternary ammonium salt dibromide, 10% of isopropanol, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 1% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 16-4-16 gemini quaternary ammonium salt dibromide is obtained by reacting hexadecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 2 to 1 in the presence of absolute ethyl alcohol.
Example 16
A preparation method of an acid-resistant waterproof locking agent for a low-permeability gas well comprises the following steps: 15% of 18-4-18 Gemini quaternary ammonium salt dibromide, 10% of isopropanol, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 1% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water. In this example, the pH of the solution was adjusted to 2.
In the embodiment, the 18-4-18 gemini quaternary ammonium salt dibromide is obtained by reacting octadecyl tertiary amine and 1, 4-dibromobutane according to the proportion of 2.
Comparative example 1
Example 1 was repeated, with the difference that the composition of the water-blocking agent was changed to: 9 percent of 12-4-14 Gemini quaternary ammonium salt dibromide, 10 percent of isopropanol, 0.5 percent of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water
Comparative example 2
Example 1 was repeated with the difference that the composition of the water-blocking agent was changed to: 10% of isopropanol, 9% of cationic surfactant dodecyl trimethyl ammonium chloride, 0.5% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water.
Comparative example 3
Example 1 was repeated, with the difference that the composition of the water-blocking agent was changed to: 7% of 12-4-14 Gemini quaternary ammonium salt dibromide, 2% of cationic surfactant dodecyl trimethyl ammonium chloride, 0.5% of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water.
Comparative example 4
Example 1 was repeated, with the difference that the composition of the water-blocking agent was changed to: 9 percent of perfluoro nonylenyloxy benzene sulfonate, 0.5 percent of corrosion inhibitor imidazoline quaternary ammonium salt and the balance of water.
Comparative example 5
Example 1 was repeated with the difference that the composition of the water-blocking agent was changed to: 9 percent of perfluorooctyl phenol polyoxyethylene ether, 0.5 percent of imidazoline quaternary ammonium salt as a corrosion inhibitor and the balance of water.
Performance detection
The contact angle test and the surface tension test were carried out on the aqueous solution having a mass percentage concentration of 0.5% of the water-resistant locking agent in each of the above examples and comparative examples.
Contact angle test: and (3) soaking the glass slide or the field core in the solution for 2h at room temperature, taking out and airing, and testing the contact angle of the glass slide or the field core by using a contact angle tester.
And (3) testing the surface tension: refer to the standard SY/T5370-1999 surface and interfacial tension determination method.
And (3) corrosion inhibition rate determination: the method refers to a corrosion inhibitor performance test method for standard acidification and an evaluation index standard SY/T5405-1996. The test data are shown in table 1:
TABLE 1
As can be seen from examples 1-16, the contact angle of the waterproof locking agent of the invention on a glass slide is 80-95 degrees, the surface tension is 20-25mN/m, and the corrosion inhibition rate is 0.9-1.5g/m 2 H. The water-blocking agent has a large contact angle in acid liquor and low surface tension, and can effectively solve the water-blocking effect of a low-permeability gas well.
Compared with comparative examples 4 and 5, the surface tension of the invention is not much different from that of the fluorocarbon surfactant, which means that the invention can achieve the same excellent water-locking resistance as the fluorocarbon surfactant. The fluorocarbon surfactant can not increase the contact angle, but the invention can increase the contact angle, so that the range of the contact angle is increased to 80-95 degrees, the wetting reversibility of the waterproof locking agent is greatly improved, and meanwhile, the gemini quaternary ammonium salt and the cationic surfactant are more environment-friendly, have little harm to groundwater environment, rock surface layers and equipment, and have lower cost.
From comparative examples 1 to 3, it can be seen that in the components of the present invention, the gemini quaternary ammonium halide, the cationic surfactant and the lower chain alcohol act synergistically, and the surface tension and the contact angle of the water-blocking agent are affected in the absence of any one of the formulations.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the invention. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.
Finally, it should be noted that: the embodiment of the present invention is disclosed only as a preferred embodiment of the present invention, which is only used for illustrating the technical solutions of the present invention and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art; the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. The acid-resistant waterproof locking agent for the low-permeability gas well is characterized in that: comprises the following components in percentage by weight: 5-20% of gemini quaternary ammonium halide, 10-20% of low-carbon chain alcohol, 2-5% of cationic surfactant, 0.5-1% of corrosion inhibitor and the balance of water.
2. The acid-resistant and waterproof locking agent for the low permeability gas well, according to claim 1, is characterized in that: the gemini quaternary ammonium salt halide is obtained by reacting dihalogenated alkane with tertiary amine.
3. The acid-resistant and waterproof locking agent for the low permeability gas well, according to claim 2, is characterized in that: the tertiary amine has an alkyl chain length of C8-C18.
4. The acid-resistant and water-resistant locking agent for the low permeability gas well according to claim 3, which is characterized in that: the tertiary amine is one or two of dodecyl tertiary amine, tetradecyl tertiary amine, hexadecyl tertiary amine and octadecyl tertiary amine.
5. The acid-resistant and waterproof locking agent for the low permeability gas well, according to claim 1, is characterized in that: the low carbon chain alcohol is one or more of methanol, ethylene glycol, ethanol, isopropanol and butanediol.
6. The acid-resistant and water-resistant locking agent for the low permeability gas well according to claim 1, which is characterized in that: the cationic surfactant is chloride or sulfate with alkyl chain length of C12-C18.
7. The acid-resistant and waterproof locking agent for the low permeability gas well, according to claim 6, is characterized in that: the cationic surfactant is any one or combination of dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, dodecyl trimethyl sulfate, hexadecyl trimethyl sulfate and octadecyl trimethyl sulfate.
8. The preparation method of the acid-resistant and water-proof locking agent for the low-permeability gas well is characterized by comprising the following steps of: the method comprises the following steps: adding water into a reaction kettle, slowly heating to 40-60 ℃, sequentially adding C8-C18 gemini quaternary ammonium halide and a cationic surfactant, and stirring for 3-4 hours; then adding low carbon chain alcohol and corrosion inhibitor, stirring uniformly, and adjusting the pH value to 1-2 by adopting a pH regulator.
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