CN116333695A - Shale inhibitor and preparation method thereof - Google Patents
Shale inhibitor and preparation method thereof Download PDFInfo
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- CN116333695A CN116333695A CN202111593413.1A CN202111593413A CN116333695A CN 116333695 A CN116333695 A CN 116333695A CN 202111593413 A CN202111593413 A CN 202111593413A CN 116333695 A CN116333695 A CN 116333695A
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- shale inhibitor
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- potassium hydroxide
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- 239000003112 inhibitor Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 55
- 239000004111 Potassium silicate Substances 0.000 claims abstract description 40
- BHGADZKHWXCHKX-UHFFFAOYSA-N methane;potassium Chemical compound C.[K] BHGADZKHWXCHKX-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052913 potassium silicate Inorganic materials 0.000 claims abstract description 40
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000000203 mixture Substances 0.000 claims abstract description 34
- 238000005553 drilling Methods 0.000 claims abstract description 30
- 239000012530 fluid Substances 0.000 claims abstract description 28
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims abstract description 18
- 150000001350 alkyl halides Chemical class 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 136
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 63
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 41
- 229920002050 silicone resin Polymers 0.000 claims description 41
- 238000001704 evaporation Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 239000005457 ice water Substances 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 5
- HLVFKOKELQSXIQ-UHFFFAOYSA-N 1-bromo-2-methylpropane Chemical compound CC(C)CBr HLVFKOKELQSXIQ-UHFFFAOYSA-N 0.000 claims description 2
- MNDIARAMWBIKFW-UHFFFAOYSA-N 1-bromohexane Chemical compound CCCCCCBr MNDIARAMWBIKFW-UHFFFAOYSA-N 0.000 claims description 2
- MJMQIMYDFATMEH-UHFFFAOYSA-N 2-chloro-2,4,4-trimethylpentane Chemical compound CC(C)(C)CC(C)(C)Cl MJMQIMYDFATMEH-UHFFFAOYSA-N 0.000 claims description 2
- MPPPKRYCTPRNTB-UHFFFAOYSA-N 1-bromobutane Chemical compound CCCCBr MPPPKRYCTPRNTB-UHFFFAOYSA-N 0.000 claims 1
- VMKOFRJSULQZRM-UHFFFAOYSA-N 1-bromooctane Chemical compound CCCCCCCCBr VMKOFRJSULQZRM-UHFFFAOYSA-N 0.000 claims 1
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 claims 1
- MLRVZFYXUZQSRU-UHFFFAOYSA-N 1-chlorohexane Chemical compound CCCCCCCl MLRVZFYXUZQSRU-UHFFFAOYSA-N 0.000 claims 1
- CNDHHGUSRIZDSL-UHFFFAOYSA-N 1-chlorooctane Chemical compound CCCCCCCCCl CNDHHGUSRIZDSL-UHFFFAOYSA-N 0.000 claims 1
- NZWIYPLSXWYKLH-UHFFFAOYSA-N 3-(bromomethyl)heptane Chemical compound CCCCC(CC)CBr NZWIYPLSXWYKLH-UHFFFAOYSA-N 0.000 claims 1
- QTBFPMKWQKYFLR-UHFFFAOYSA-N isobutyl chloride Chemical compound CC(C)CCl QTBFPMKWQKYFLR-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000005764 inhibitory process Effects 0.000 abstract description 19
- 238000005187 foaming Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 17
- 238000010438 heat treatment Methods 0.000 description 8
- 229920005989 resin Polymers 0.000 description 8
- 239000011347 resin Substances 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- 238000005096 rolling process Methods 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 239000000440 bentonite Substances 0.000 description 5
- 229910000278 bentonite Inorganic materials 0.000 description 5
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 4
- 229920000768 polyamine Polymers 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IZUOFDKRBUHNPE-UHFFFAOYSA-N 2-methylpropane hydrochloride Chemical compound CC(C)C.Cl IZUOFDKRBUHNPE-UHFFFAOYSA-N 0.000 description 2
- QBNJPSHRAWSBDW-UHFFFAOYSA-N 2-methylpropane;hydrobromide Chemical compound Br.CC(C)C QBNJPSHRAWSBDW-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 2
- BWUHFJZNEUYVKM-UHFFFAOYSA-N CC(C)CC(C)(C)C.Br Chemical compound CC(C)CC(C)(C)C.Br BWUHFJZNEUYVKM-UHFFFAOYSA-N 0.000 description 2
- VZMQPBMPUPSQDJ-UHFFFAOYSA-N CC(C)CC(C)(C)C.Cl Chemical compound CC(C)CC(C)(C)C.Cl VZMQPBMPUPSQDJ-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- VFEVXBKBGMAKME-UHFFFAOYSA-N butane;hydrobromide Chemical compound Br.CCCC VFEVXBKBGMAKME-UHFFFAOYSA-N 0.000 description 2
- IODDQGMEFSNLGV-UHFFFAOYSA-N butane;hydrochloride Chemical compound Cl.CCCC IODDQGMEFSNLGV-UHFFFAOYSA-N 0.000 description 2
- WTVNABTWDZCYCN-UHFFFAOYSA-N hexane;hydrobromide Chemical compound Br.CCCCCC WTVNABTWDZCYCN-UHFFFAOYSA-N 0.000 description 2
- HJLHTTJLVALHOP-UHFFFAOYSA-N hexane;hydron;chloride Chemical compound Cl.CCCCCC HJLHTTJLVALHOP-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- BDDIUTHMWNWMRJ-UHFFFAOYSA-N octane;hydrobromide Chemical compound Br.CCCCCCCC BDDIUTHMWNWMRJ-UHFFFAOYSA-N 0.000 description 2
- ZHVULPDNOFUIML-UHFFFAOYSA-N octane;hydrochloride Chemical compound Cl.CCCCCCCC ZHVULPDNOFUIML-UHFFFAOYSA-N 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XTIIITNXEHRMQL-UHFFFAOYSA-N tripotassium methoxy(trioxido)silane Chemical compound [K+].[K+].[K+].CO[Si]([O-])([O-])[O-] XTIIITNXEHRMQL-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 101000832669 Rattus norvegicus Probable alcohol sulfotransferase Proteins 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 239000010428 baryte Substances 0.000 description 1
- 229910052601 baryte Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
-
- 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
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/22—Synthetic organic compounds
- C09K8/24—Polymers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a preparation method of a shale inhibitor, which comprises the following steps: a) Stirring N-methylimidazole and haloalkane for reaction to obtain a first mixture; b) And mixing the first mixture with a multi-chain methyl potassium silicate solution, and reacting to obtain the shale inhibitor. The shale inhibitor provided by the invention has good shale inhibition capability, high temperature resistance, no tackifying in the use process, and especially the high-density drilling fluid is beneficial to regulating flow pattern and no foaming; the preparation method of the shale inhibitor provided by the invention is simple and mild, and three wastes are not generated.
Description
Technical Field
The invention relates to the technical field of drilling fluid, in particular to a shale inhibitor and a preparation method thereof.
Background
With the continuous exploitation of unconventional oil and gas resources, deep wells, ultra-deep wells, ocean wells and complex section wells, when shale formations are encountered in the drilling process, the hydration expansion and dispersion of the shale can cause a series of problems such as instability of the well wall, bit balling, borehole purification and the like, the drilling difficulty is increased, and higher requirements are put forward on a drilling fluid system, particularly shale inhibitors.
The shale inhibitors are mainly polymers, inorganic salts, asphalt, polyamine and the like, and have the defects of poor environmental protection, high cost, easy viscosity increase, flocculation, foaming and the like when the dosage is high.
Therefore, the development of the shale inhibitor with low cost, high temperature resistance and strong collapse prevention capability has important significance.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a preparation method of shale inhibitor, which has the advantages of high temperature resistance, low cost, good compatibility with drilling fluid, no foaming, high inhibition rate and viscosity reduction capability.
The invention provides a preparation method of a shale inhibitor, which comprises the following steps:
a) Stirring N-methylimidazole and haloalkane for reaction to obtain a first mixture;
b) And mixing the first mixture with a multi-chain methyl potassium silicate solution, and reacting to obtain the shale inhibitor.
Preferably, the molar ratio of N-methylimidazole to haloalkane in step a) is 1: (1.0-1.2).
Preferably, the stirring speed in the step A) is 200-300 r/min; the reaction temperature is 80-90 ℃; the reaction time is 18-24 h.
Preferably, the alkyl halide is one of n-butane bromide, isobutane bromide, n-hexane bromide, n-octane bromide, isooctane bromide, n-butane chloride, isobutane chloride, n-hexane chloride, n-octane chloride or isooctane chloride.
Preferably, in the step B), the first mixture and the multi-chain methyl potassium silicate solution are mixed in a mass ratio of 10 (10-15).
Preferably, the temperature of the reaction in the step B) is 40-50 ℃; the reaction time is 2-3 h.
Preferably, the preparation method of the multi-chain methyl potassium silicate in the step B) specifically comprises the following steps:
dissolving methyl silicone resin in a solvent to obtain a methyl silicone resin solution;
dropwise adding the potassium hydroxide solution into the methyl silicone resin solution for reaction, continuously stirring after the dropwise adding is finished, and evaporating to remove the solvent to obtain the multi-chain methyl potassium silicate.
Preferably, the solvent is absolute ethyl alcohol, the reaction is carried out in an ice-water bath, and the reaction temperature is 0 ℃; the dripping time is 2min; the stirring time is 2-3 h; the mass fraction of potassium hydroxide in the potassium hydroxide solution is 40% -50%; the mole fraction ratio of the potassium hydroxide to the methyl silicone resin is 1 (1-3).
The invention provides a shale inhibitor which is prepared by the preparation method according to any one of the technical schemes.
The invention provides a drilling fluid, which comprises the shale inhibitor prepared by the preparation method according to any one of the technical schemes or the shale inhibitor.
Compared with the prior art, the invention provides a preparation method of a shale inhibitor, which comprises the following steps: a) Stirring N-methylimidazole and haloalkane for reaction to obtain a first mixture; b) And mixing the first mixture with a multi-chain methyl potassium silicate solution, and reacting to obtain the shale inhibitor. The shale inhibitor provided by the invention has good shale inhibition capability, high temperature resistance, no tackifying in the use process, and especially the high-density drilling fluid is beneficial to regulating flow pattern and no foaming; the preparation method of the shale inhibitor provided by the invention is simple and mild, and three wastes are not generated.
Detailed Description
The invention provides a shale inhibitor and a preparation method thereof, and a person skilled in the art can refer to the content of the shale inhibitor and properly improve the technological parameters. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and they are intended to be within the scope of the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that the invention can be practiced and practiced with modification and alteration and combination of the methods and applications herein without departing from the spirit and scope of the invention.
The invention provides a preparation method of a shale inhibitor, which comprises the following steps:
a) Stirring N-methylimidazole and haloalkane for reaction to obtain a first mixture;
b) And mixing the first mixture with a multi-chain methyl potassium silicate solution, and reacting to obtain the shale inhibitor.
The preparation method of the shale inhibitor comprises the steps of firstly stirring N-methylimidazole and haloalkane for reaction to obtain a first mixture.
The haloalkane is preferably one of n-butane bromide, isobutane bromide, n-hexane bromide, n-octane bromide, isooctane bromide, n-butane chloride, isobutane chloride, n-hexane chloride, n-octane chloride or isooctane chloride. The source of the haloalkane is not limited and may be known to those skilled in the art.
According to the invention, the molar ratio of N-methylimidazole to haloalkane is preferably 1: (1.0-1.2).
The present invention is not limited to the specific reaction vessel, and may be a three-necked flask equipped with a condenser.
The reaction is carried out under the condition of stirring, and the stirring speed is preferably 200-300 r/min; more preferably 210 to 290r/min; most preferably 220 to 280r/min.
The reaction temperature is preferably 80-90 ℃; more preferably 82 to 88 ℃; the reaction time is preferably 18 to 24 hours; more preferably 19 to 23 hours.
And mixing the first mixture with a multi-chain methyl potassium silicate solution, and reacting to obtain the shale inhibitor.
According to the invention, the mass ratio of the first mixture to the multi-chain methyl potassium silicate solution is preferably 10 (10-15); more preferably 10 (11) to 14).
The reaction is preferably carried out at 40-50 ℃ for 2-3 hours; more preferably 42 to 48 ℃, and the reaction is continued for 2 to 3 hours.
According to the invention, the preparation method of the multi-chain methyl potassium silicate specifically comprises the following steps:
dissolving methyl silicone resin in a solvent to obtain a methyl silicone resin solution;
dropwise adding the potassium hydroxide solution into the methyl silicone resin solution for reaction, continuously stirring after the dropwise adding is finished, and evaporating to remove the solvent to obtain the multi-chain methyl potassium silicate.
Dissolving methyl silicone resin in a solvent to obtain a methyl silicone resin solution; the solvent is absolute ethyl alcohol, and the absolute ethyl alcohol is stirred to be uniformly dispersed.
Dropwise adding potassium hydroxide solution into methyl silicone resin solution for reaction. The ethanol solution in which the methyl silicone resin was dissolved was poured into a three-necked flask, and a potassium hydroxide solution was dropwise added thereto with stirring.
The mass fraction of potassium hydroxide in the potassium hydroxide solution is preferably 40% -50%; more preferably 45%.
The reaction is carried out in ice-water bath, and the reaction temperature is 0 ℃; the dropping time is 2min.
Stirring is continued after the dripping is finished, and stirring is continued for 2-3 hours after the dripping of the potassium hydroxide is finished, so that the methyl silicone resin and the potassium hydroxide fully react.
The mole fraction ratio of the potassium hydroxide to the methyl silicone resin is 1 (1-3).
Evaporating to remove the solvent to obtain the multi-chain methyl potassium silicate. The present invention is not limited to the specific manner in which the solvent is evaporated, and may be well known to those skilled in the art.
The shale inhibitor has the advantages of high temperature resistance, low cost, good compatibility with drilling fluid, no foaming, strong collapse prevention inhibition capability and viscosity reduction effect, and is suitable for various water-based drilling fluids.
The invention provides a shale inhibitor which is prepared by the preparation method according to any one of the technical schemes.
The shale inhibitor provided by the invention has the temperature resistance reaching 260 ℃, the relative inhibition rate of 0.3 percent of addition is 98.5-99.5 percent, the primary shale rolling recovery rate is more than or equal to 98.8 percent, and the secondary shale rolling recovery rate is more than or equal to 98.2 percent.
The invention provides a drilling fluid, which comprises the shale inhibitor prepared by the preparation method according to any one of the technical schemes or the shale inhibitor.
The shale inhibitor of the present invention is preferably added in an amount of 1wt%.
The shale inhibitor prepared by the invention has the shale inhibitor capacity equivalent to that of the traditional polyamine and polyether amine shale inhibitor, has almost no influence on rheological property, fluid loss and other performances of drilling fluid, does not increase viscosity and resist high temperature, and is particularly favorable for adjusting flow patterns in high-density drilling fluid without foaming. The shale inhibitor provided by the invention has the advantages of mild and simple preparation process and no generation of three wastes.
In order to further illustrate the present invention, the following describes in detail a shale inhibitor and a preparation method thereof provided by the present invention in connection with examples.
The methyl silicone resin related by the invention is purchased from Shenzhen Jinbo Cheng technology Co., ltd, and N-methylimidazole, haloalkane and the like are all purchased from Ara Ding Shiji Co.
The relative inhibition rate of the embodiment of the invention is measured according to the standard Q/SH0323-2009 technical requirement of shale inhibitor for drilling fluid. Shale rolling recovery rate is measured according to standard Q/SH 1500 0032-2013 technical requirement of polyamine of anti-collapse agent for drilling fluid.
Example 1
Adding 1 mol of N-methylimidazole and 1.0 mol of N-butane bromide into a three-neck flask with a condenser, and reacting for 18 hours at 80 ℃ at a stirring speed of 200r/min to obtain a mixture 1; then, 10 parts by mass of mixture 1 and 10 parts by mass of multi-chain methyl potassium silicate solution are added into another three-neck flask with a condenser, and the reaction is continued for 2 hours at 40 ℃ to obtain the shale inhibitor.
The preparation method of the multi-chain methyl potassium silicate solution comprises the following steps: 1 mol of methyl silicone resin is taken and dissolved in 500mL of absolute ethyl alcohol, and the mixture is stirred to be uniformly dispersed; then pouring the ethanol solution dissolved with the methyl silicone resin into a three-neck flask, dropwise adding potassium hydroxide solution (the mole number of the potassium hydroxide is 1 mole, and the mass fraction of the potassium hydroxide is 45%) into the three-neck flask under stirring, and reacting to keep an ice water bath; after the completion of the dropwise addition of potassium hydroxide, stirring was continued for 3 hours to allow the methylsilicone resin and potassium hydroxide to react sufficiently. Finally, heating and evaporating ethanol in the solution to obtain the multi-chain methyl potassium silicate solution.
Example 2
Adding 1 mol of N-methylimidazole and 1.2 mol of bromoisobutane into a three-neck flask with a condenser, controlling the stirring speed to 300r/min, and reacting at 90 ℃ for 24 hours to obtain a mixture 1; then, 10 parts by mass of mixture 1 and 15 parts by mass of multi-chain methyl potassium silicate solution are added into another three-neck flask with a condenser, and the reaction is continued for 3 hours at 50 ℃ to obtain the shale inhibitor.
The preparation method of the multi-chain methyl potassium silicate solution comprises the following steps: dissolving 2 moles of methyl silicone resin in 500mL of absolute ethyl alcohol, and stirring to uniformly disperse the methyl silicone resin; then pouring the ethanol solution dissolved with the methyl silicone resin into a three-neck flask, dropwise adding potassium hydroxide solution (the mole number of the potassium hydroxide is 1 mole, and the mass fraction of the potassium hydroxide is 45%) into the three-neck flask under stirring, and reacting to keep an ice water bath; after the completion of the dropwise addition of potassium hydroxide, stirring was continued for 3 hours to allow the methylsilicone resin and potassium hydroxide to react sufficiently. Finally, heating and evaporating ethanol in the solution to obtain the multi-chain methyl potassium silicate solution.
Example 3
Adding 1 mol of N-methylimidazole and 1.1 mol of bromohexane into a three-neck flask with a condenser, controlling the stirring speed to be 250r/min, and reacting at 85 ℃ for 21 hours to obtain a mixture 1; then, 10 parts by mass of mixture 1 and 13 parts by mass of multi-chain methyl potassium silicate solution are added into another three-neck flask with a condenser, and the reaction is continued for 2.5 hours at 45 ℃ to obtain the shale inhibitor.
The preparation method of the multi-chain methyl potassium silicate solution comprises the following steps: dissolving 3 moles of methyl silicone resin in 500mL of absolute ethyl alcohol, and stirring to uniformly disperse the methyl silicone resin; then pouring the ethanol solution dissolved with the methyl silicone resin into a three-neck flask, dropwise adding potassium hydroxide solution (the mole number of the potassium hydroxide is 1 mole, and the mass fraction of the potassium hydroxide is 45%) into the three-neck flask under stirring, and reacting to keep an ice water bath; after the completion of the dropwise addition of potassium hydroxide, stirring was continued for 3 hours to allow the methylsilicone resin and potassium hydroxide to react sufficiently. Finally, heating and evaporating ethanol in the solution to obtain the multi-chain methyl potassium silicate solution.
Example 4
Adding 1 mol of N-methylimidazole and 1.05 mol of N-octane bromide into a three-neck flask with a condenser, controlling the stirring speed to be 280r/min, and reacting at 80 ℃ for 24 hours to obtain a mixture 1; then, 10 parts by mass of mixture 1 and 10 parts by mass of multi-chain methyl potassium silicate solution are added into another three-neck flask with a condenser, and the reaction is continued for 3 hours at 50 ℃ to obtain the shale inhibitor.
The preparation method of the multi-chain methyl potassium silicate solution comprises the following steps: dissolving 2 moles of methyl silicone resin in 500mL of absolute ethyl alcohol, and stirring to uniformly disperse the methyl silicone resin; then pouring the ethanol solution dissolved with the methyl silicone resin into a three-neck flask, dropwise adding potassium hydroxide solution (the mole number of the potassium hydroxide is 1 mole, and the mass fraction of the potassium hydroxide is 45%) into the three-neck flask under stirring, and reacting to keep an ice water bath; after the completion of the dropwise addition of potassium hydroxide, stirring was continued for 3 hours to allow the methylsilicone resin and potassium hydroxide to react sufficiently. Finally, heating and evaporating ethanol in the solution to obtain the multi-chain methyl potassium silicate solution.
Example 5
1 mol of N-methylimidazole and 1.15 mol of N-butane chloride are added into a three-neck flask with a condenser, the stirring speed is controlled to be 300r/min, and the reaction is carried out for 20 hours at 80 ℃ to obtain a mixture 1; then, 10 parts by mass of the mixture 1 and 12 parts by mass of the multi-chain methyl potassium silicate solution are added into another three-neck flask with a condenser, and the reaction is continued for 3 hours at 45 ℃ to obtain the shale inhibitor.
The preparation method of the multi-chain methyl potassium silicate solution comprises the following steps: dissolving 3 moles of methyl silicone resin in 500mL of absolute ethyl alcohol, and stirring to uniformly disperse the methyl silicone resin; then pouring the ethanol solution dissolved with the methyl silicone resin into a three-neck flask, dropwise adding potassium hydroxide solution (the mole number of the potassium hydroxide is 1 mole, and the mass fraction of the potassium hydroxide is 45%) into the three-neck flask under stirring, and reacting to keep an ice water bath; after the completion of the dropwise addition of potassium hydroxide, stirring was continued for 3 hours to allow the methylsilicone resin and potassium hydroxide to react sufficiently. Finally, heating and evaporating ethanol in the solution to obtain the multi-chain methyl potassium silicate solution.
Example 6
Adding 1 mol of N-methylimidazole and 1.0 mol of chloro-N-hexane into a three-neck flask with a condenser, controlling the stirring speed to 300r/min, and reacting at 90 ℃ for 24 hours to obtain a mixture 1; then, 10 parts by mass of the mixture 1 and 14 parts by mass of the multi-chain methyl potassium silicate solution are added into another three-neck flask with a condenser, and the reaction is continued for 2 hours at 48 ℃ to obtain the shale inhibitor.
The preparation method of the multi-chain methyl potassium silicate solution comprises the following steps: dissolving 3 moles of methyl silicone resin in 500mL of absolute ethyl alcohol, and stirring to uniformly disperse the methyl silicone resin; then pouring the ethanol solution dissolved with the methyl silicone resin into a three-neck flask, dropwise adding potassium hydroxide solution (the mole number of the potassium hydroxide is 1 mole, and the mass fraction of the potassium hydroxide is 45%) into the three-neck flask under stirring, and reacting to keep an ice water bath; after the completion of the dropwise addition of potassium hydroxide, stirring was continued for 3 hours to allow the methylsilicone resin and potassium hydroxide to react sufficiently. Finally, heating and evaporating ethanol in the solution to obtain the multi-chain methyl potassium silicate solution.
Example 7
Adding 1 mol of N-methylimidazole and 1.2 mol of N-chlorooctane into a three-neck flask with a condenser, controlling the stirring speed to be 220r/min, and reacting at 82 ℃ for 21 hours to obtain a mixture 1; then, 10 parts by mass of mixture 1 and 15 parts by mass of multi-chain methyl potassium silicate solution are added into another three-neck flask with a condenser, and the reaction is continued for 3 hours at 40 ℃ to obtain the shale inhibitor.
The preparation method of the multi-chain methyl potassium silicate solution comprises the following steps: dissolving 3 moles of methyl silicone resin in 500mL of absolute ethyl alcohol, and stirring to uniformly disperse the methyl silicone resin; then pouring the ethanol solution dissolved with the methyl silicone resin into a three-neck flask, dropwise adding potassium hydroxide solution (the mole number of the potassium hydroxide is 1 mole, and the mass fraction of the potassium hydroxide is 45%) into the three-neck flask under stirring, and reacting to keep an ice water bath; after the completion of the dropwise addition of potassium hydroxide, stirring was continued for 3 hours to allow the methylsilicone resin and potassium hydroxide to react sufficiently. Finally, heating and evaporating ethanol in the solution to obtain the multi-chain methyl potassium silicate solution.
Example 8
Adding 1 mol of N-methylimidazole and 1.1 mol of chloroisooctane into a three-neck flask with a condenser, controlling the stirring speed to 300r/min, and reacting at 90 ℃ for 24 hours to obtain a mixture 1; then, 10 parts by mass of mixture 1 and 10 parts by mass of multi-chain methyl potassium silicate solution are added into another three-neck flask with a condenser, and the reaction is continued for 2 hours at 50 ℃ to obtain the shale inhibitor.
The preparation method of the multi-chain methyl potassium silicate solution comprises the following steps: dissolving 3 moles of methyl silicone resin in 500mL of absolute ethyl alcohol, and stirring to uniformly disperse the methyl silicone resin; then pouring the ethanol solution dissolved with the methyl silicone resin into a three-neck flask, dropwise adding potassium hydroxide solution (the mole number of the potassium hydroxide is 1 mole, and the mass fraction of the potassium hydroxide is 45%) into the three-neck flask under stirring, and reacting to keep an ice water bath; after the completion of the dropwise addition of potassium hydroxide, stirring was continued for 3 hours to allow the methylsilicone resin and potassium hydroxide to react sufficiently. Finally, heating and evaporating ethanol in the solution to obtain the multi-chain methyl potassium silicate solution.
The relative inhibition rate, the primary shale rolling recovery rate and the secondary shale rolling recovery rate of the shale inhibitors prepared in the embodiments 1 to 8 are detected, and the detection results are shown in table 1.
Table 1 shale inhibitor performance test
As is clear from Table 1, the shale inhibitors prepared in examples 1 to 8 have a relative inhibition rate of 98.5% to 99.5%, a primary shale rolling recovery rate of 98.8% to 99.4%, and a secondary shale rolling recovery rate of 98.2% to 99.2%, indicating excellent inhibition ability.
In order to show the temperature resistance of the shale inhibitor prepared by the invention, the relative inhibition rate after 1 percent (mass fraction) of the product of the invention is added into the base slurry at different temperatures is further examined, and the results after continuous aging for 16 hours are shown in Table 2.
Determination of relative inhibition Rate in base slurry according to Q/SHCG 99001-2017 general detection evaluation method for oilfield chemical Agents section 1: the drilling fluid was measured using the method of chemistry set forth in 7.1.3.
Relative inhibition ratio calculation:
X＝(Ф-Ф 1 )/Ф×100％
wherein: x-relative inhibition,%;
stabilizing reading when the rotating speed of the phi-blank rotary viscometer is 100 r/min;
Ф 1 -stable reading at rotational speed of the rotational viscometer of 100r/min after addition of the sample.
Comparative example 1:
the relative inhibition was tested by adding 1% potassium methyl silicate to the base slurry.
Comparative example 2:
the relative inhibition was tested by adding 1% polyamine to the base slurry.
Table 2 temperature resistance test of shale inhibitors
As shown in Table 2, the prepared shale inhibitor is continuously aged for 16 hours at the temperature of 120-260 ℃, and the relative inhibition rate is basically unchanged, which indicates that the temperature resistance is strong.
Comparative example 1 shows that only potassium methyl silicate is used as an inhibitor, and has the problem of insufficient inhibition and insufficient temperature resistance; comparative example 2 shows that the inhibition performance at low temperature is strong, the product temperature resistance is poor and the inhibition performance is reduced with the increase of temperature.
The compatibility of the shale inhibitor and the drilling fluid provided by the invention is further examined.
Pre-hydrating bentonite: 400mL of water is added into a stirring cup, 0.56g of anhydrous sodium carbonate and 16g of bentonite are added while stirring, the mixture is stirred at a high speed for 20min at 11000r/min, and the mixture is maintained for 24h in a sealing manner at room temperature, so as to obtain pre-hydrated bentonite slurry.
Based on the total volume of the pre-hydrated bentonite slurry: adding 4% of SMP-2, 4% of SMC and 3% of FT-1 in a mass-volume ratio into bentonite slurry in turn, and stirring at a high speed for 5min; then adding 601 with the mass volume ratio of 0.2% and LV-PAC with the mass volume ratio of 0.7%, and stirring at a high speed for 10min; then adding 0.5% sodium hydroxide in mass-volume ratio, and stirring at high speed for 5min; finally, adding barite to adjust the density of the drilling fluid to 1.5g/cm 3 And 2.5g/cm 3 Stirring at high speed for 20min to obtain drilling fluid.
Examples 9 to 16
The drilling fluid was obtained according to the above preparation method, and shale inhibitors prepared in examples 1 to 8 were added in an amount of 1% to each of examples 9 to 16, and their properties in the drilling fluid were evaluated.
The drilling fluids prepared in examples 9 to 16 were charged into an aging kettle, placed in a roller furnace, rolled at 180℃for 16 hours, and then the properties of the drilling fluids were measured according to the method described above, and the performance measurement method was according to national standard GB/T16783.1-2014, section 1 of Petroleum and Natural gas industry drilling fluid field test: water-based drilling fluid, and the detection results are shown in Table 3.
Table 3 properties of drilling fluids formulated in examples 9 to 16
Wherein AV is apparent viscosity, PV is plastic viscosity, YP is dynamic shear force, Q 10s /Q 10min For initial final cut, FL is API fluid loss.
As shown in Table 3, the shale inhibitor prepared by the invention has a certain viscosity reducing effect in a system, particularly has little influence on shear force and fluid loss on high-density drilling fluid, and the drilling fluid hardly foams after the shale inhibitor is added, and the foaming rate is less than 1.6% even when the shale inhibitor is added by 1%. Therefore, the shale inhibitor prepared by the invention has good compatibility with drilling fluid.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A method of preparing a shale inhibitor, comprising:
a) Stirring N-methylimidazole and haloalkane for reaction to obtain a first mixture;
b) And mixing the first mixture with a multi-chain methyl potassium silicate solution, and reacting to obtain the shale inhibitor.
2. The process according to claim 1, wherein the molar ratio of N-methylimidazole to haloalkane in step a) is 1: (1.0-1.2).
3. The method according to claim 1, wherein the stirring speed in step a) is 200 to 300r/min; the reaction temperature is 80-90 ℃; the reaction time is 18-24 h.
4. The method according to claim 1, wherein the haloalkane is one of bromo-n-butane, bromo-isobutane, bromo-n-hexane, bromo-n-octane, bromo-isooctane, chloro-n-butane, chloro-isobutane, chloro-n-hexane, chloro-n-octane, or chloro-isooctane.
5. The method according to claim 1, wherein the first mixture and the multi-chain methyl potassium silicate solution are mixed in the step B) at a mass ratio of 10 (10-15).
6. The process according to claim 1, wherein the temperature of the reaction in step B) is 40 to 50 ℃; the reaction time is 2-3 h.
7. The preparation method according to claim 1, wherein the preparation method of the multi-chain methyl potassium silicate in the step B) specifically comprises the following steps:
dissolving methyl silicone resin in a solvent to obtain a methyl silicone resin solution;
dropwise adding the potassium hydroxide solution into the methyl silicone resin solution for reaction, continuously stirring after the dropwise adding is finished, and evaporating to remove the solvent to obtain the multi-chain methyl potassium silicate.
8. The method according to claim 7, wherein the solvent is absolute ethanol, the reaction is performed in an ice-water bath, and the reaction temperature is 0 ℃; the dripping time is 2min; the stirring time is 2-3 h; the mass fraction of potassium hydroxide in the potassium hydroxide solution is 40% -50%; the mole fraction ratio of the potassium hydroxide to the methyl silicone resin is 1 (1-3).
9. A shale inhibitor prepared by the preparation method of any one of claims 1 to 8.
10. A drilling fluid comprising the shale inhibitor produced by the production method of any one of claims 1 to 8 or the shale inhibitor of claim 9.
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