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CN114381282B - Surfactant and preparation method thereof, microemulsion plugging agent and preparation method thereof, and water-based drilling fluid - Google Patents

Surfactant and preparation method thereof, microemulsion plugging agent and preparation method thereof, and water-based drilling fluid Download PDF

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CN114381282B
CN114381282B CN202111552870.6A CN202111552870A CN114381282B CN 114381282 B CN114381282 B CN 114381282B CN 202111552870 A CN202111552870 A CN 202111552870A CN 114381282 B CN114381282 B CN 114381282B
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surfactant
microemulsion
water
drilling fluid
based drilling
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CN114381282A (en
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钟汉毅
蔡文明
邱正松
高文龙
董兵强
黄维安
管颖
牟庭波
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China University of Petroleum East China
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
    • C07C213/04—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reaction of ammonia or amines with olefin oxides or halohydrins
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
    • C07C213/08—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions not involving the formation of amino groups, hydroxy groups or etherified or esterified hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/26—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfonic acids
    • C07C303/28—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfonic acids by reaction of hydroxy compounds with sulfonic acids or derivatives thereof
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    • 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
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    • 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
    • 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
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504—Compositions based on water or polar solvents
    • C09K8/506—Compositions based on water or polar solvents containing organic compounds
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    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/10—Nanoparticle-containing well treatment fluids
    • 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
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating

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  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
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Abstract

The invention relates to the field of petroleum engineering, and discloses a surfactant and a preparation method thereof, a microemulsion plugging agent and a preparation method thereof, and water-based drilling fluid. The preparation method of the surfactant comprises the following steps: (1) Carrying out ring opening reaction on amine hydrochloride and epoxy chloropropane to obtain a first intermediate; (2) Quaternizing the first intermediate with dodecyl dimethyl tertiary amine to obtain a second intermediate; (3) And (3) carrying out sulfonation reaction on the second intermediate, sultone and MH to obtain the surfactant. The preparation method of the microemulsion blocking agent comprises the following steps: mixing an oil phase, saline, a first surfactant, a second surfactant and a cosurfactant to obtain the microemulsion blocking agent; the first surfactant is the surfactant prepared by the method, and the water activity of the brine is not more than 0.85. The microemulsion plugging agent for the water-based drilling fluid has good well wall stabilizing effect, and realizes the unification of strong inhibition and strong plugging performance.

Description

Surfactant and preparation method thereof, microemulsion plugging agent and preparation method thereof, and water-based drilling fluid
Technical Field
The invention relates to the field of petroleum engineering, in particular to a surfactant and a preparation method thereof, a microemulsion plugging agent and a preparation method thereof, and water-based drilling fluid.
Background
Since the first discovery of microemulsions (microemulsions/microemulsion/ME) by Hoar and Schulman in 1943, the theoretical and application studies have been greatly advanced, and after the world petroleum crisis occurs in the 20 th century 70, the development of climax has been pursued because microemulsion systems show great potential in tertiary oil recovery technology. After 90 s, the application field of the microemulsion is rapidly expanded, and besides the 3 times oil extraction technology, the microemulsion is penetrated into the fields of daily chemical industry, fine chemical industry, material science, biotechnology, environmental science, analytical chemistry and the like at present, and becomes a research field with huge potential in the world at present.
Since the beginning of the new century, more and more petroleum companies began to pay attention to the great value of microemulsions, and intensive research into microemulsions was conducted and the application fields thereof were widened. The Halebgton energy company develops a microemulsion technology, which can remove emulsion blockage, so that the wettability of a reservoir is reversed to be water-wet again, and the aim of effectively repairing stratum injury is fulfilled. The Bekkes company also performs the study of microemulsion unblocking, and the microemulsion is adopted to solubilize the solvent oil in the well wall mud cake, so that the particles in the mud cake are reversed to be hydrophilic, thereby achieving the purpose of eliminating the skin injury. The emulsion technology is used for plugging the micro/nano pores of shale in a TERRA-MAXHPWBM (high-performance water-based drilling fluid) system constructed by Bekkes, so that good well wall stability and clay dispersion inhibition are achieved, torque and friction resistance can be reduced, drilling speed is improved, and the aim of reducing total cost is fulfilled.
The microemulsion reservoir protecting agent is developed at home abroad, has been successfully applied to shale gas drilling and production increasing measures, and is beneficial to improving the yield of a gas well. However, research in domestic related aspects is still in the beginning stage, and conventional microemulsions generally adopt fresh water or low-concentration saline water, and it is difficult to form the microemulsions under high-concentration saline water.
Disclosure of Invention
The invention aims to solve the problems that the existing microemulsion system is poor in salt tolerance and inapplicable to a low-activity drilling fluid system, and the like, and provides a surfactant and a preparation method thereof, a microemulsion plugging agent and a preparation method thereof, and a water-based drilling fluid.
In order to achieve the above object, the first aspect of the present invention provides a surfactant, wherein the structure of the surfactant is shown in the structural formula I.
Wherein R 1 is-CH 3、-CH2CH3 or-CH 2CH2CH3,R2 is-CH 3、-CH2CH3 or-CH 2CH2CH3,R3 is- (CH 2)3 -or- (CH 2)4-,R4 is- (CH 2)3 -or- (CH 2)4-,M1) is Li, na or K, and M 2 is Li, na or K).
The second aspect of the invention provides a preparation method of the surfactant. The method comprises the following steps:
(1) Carrying out ring-opening reaction on amine hydrochloride shown in a formula II and epichlorohydrin to obtain a first intermediate;
Wherein R 1 is-CH 3、-CH2CH3 or-CH 2CH2CH3,R2 is-CH 3、-CH2CH3 or-CH 2CH2CH3;
(2) Quaternizing the first intermediate with dodecyl dimethyl tertiary amine to obtain a second intermediate;
(3) The second intermediate is sulfonated with sultone shown in a formula III and a compound shown in a general formula MH to obtain the surfactant,
Wherein R 3 is- (CH 2)3 -or- (CH 2)4 -, MH is one or two of LiH, naH and KH).
In a third aspect the present invention provides a surfactant obtainable by the process according to the second aspect.
The fourth aspect of the invention provides a method for preparing a microemulsion plugging agent for water-based drilling fluid, which comprises the following steps: mixing an oil phase, saline, a first surfactant, a second surfactant and a cosurfactant to obtain the microemulsion blocking agent; wherein the first surfactant is the surfactant of the first aspect; the brine has an aqueous activity of no greater than 0.85.
In a fifth aspect, the present invention provides a microemulsion plugging agent for water-based drilling fluids prepared by the method of the fourth aspect. The average particle size of the microemulsion blocking agent is 10-60nm.
In a sixth aspect, the present invention provides a water-based drilling fluid, comprising the microemulsion blocking agent for a water-based drilling fluid according to the fifth aspect.
Through the technical scheme, the invention can obtain the following beneficial effects:
(1) The microemulsion plugging agent for the water-based drilling fluid can be used for plugging micro-nano cracks with different sizes, and has good plugging performance;
(2) Compared with the prior art, the microemulsion plugging agent for the water-based drilling fluid is prepared by adopting high-concentration brine, and the prepared microemulsion is used in the drilling fluid, so that the drilling fluid has strong inhibition.
(3) The microemulsion liquid drops for the water-based drilling fluid can be quickly adsorbed on the surface of the core, so that the wettability of the core is changed from hydrophilic to hydrophobic, and the affinity to water molecules is reduced. Once the microemulsion drops are demulsified, the internal saline is released, so that the hydration and dispersion of clay can be further inhibited, and the microemulsion drops have good inhibition performance.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the present invention, the "first" and "second" do not limit the present inventors, but only to distinguish different materials.
In a first aspect, the present invention provides a surfactant having a structure according to formula I.
Wherein R 1 is-CH 3、-CH2CH3 or-CH 2CH2CH3,R2 is-CH 3、-CH2CH3 or-CH 2CH2CH3,R3 is- (CH 2)3 -or- (CH 2)4-,R4 is- (CH 2)3 -or- (CH 2)4-,M1) is Li, na or K, and M 2 is Li, na or K).
In some embodiments of the invention, R 1 and R 2 may be the same or different, depending primarily on the amine hydrochloride used in the preparation process.
In some embodiments of the invention, R 3 and R 4 may be the same or different, depending primarily on the sultone used in the preparation process.
In some embodiments of the invention, M 1 and M 2 may be different or identical, preferably identical.
The second aspect of the invention provides a preparation method of the surfactant. The method comprises the following steps:
(1) Carrying out ring opening reaction on amine hydrochloride and epoxy chloropropane to obtain a first intermediate; the amine hydrochloride is shown as a formula II, The reaction process of the ring-opening reaction is as follows:
Wherein R 1 is-CH 3、-CH2CH3 or-CH 2CH2CH3,R2 is-CH 3、-CH2CH3 or-CH 2CH2CH3;
(2) Quaternizing the first intermediate with dodecyl dimethyl tertiary amine to obtain a second intermediate; the quaternization reaction comprises the following reaction processes:
(3) The second intermediate is sulfonated with sultone and a compound represented by a general formula MH to obtain the surfactant, the sultone is shown as a formula III, The sulfonation reaction comprises the following reaction processes:
Wherein R 3 is- (CH 2)3 -or- (CH 2)4 -, MH is one or two of LiH, naH and KH).
In some embodiments of the invention, the ring-opening reaction is performed in the presence of a first solvent; preferably, step (1) further comprises: dissolving amine hydrochloride and epichlorohydrin in the first solvent; and decompressing and steaming the product solution obtained by the ring-opening reaction to remove the first solvent to obtain the first intermediate.
The first solvent is not particularly limited as long as it can dissolve amine hydrochloride and epichlorohydrin. Preferably, the first solvent is selected from methanol, ethanol, acetone, toluene, preferably ethanol.
The amount of ethanol used as a solvent for dissolving the amine hydrochloride and epichlorohydrin is not particularly limited in the present invention, as long as the amine hydrochloride and epichlorohydrin can be completely dissolved. Preferably, the mass ratio of amine hydrochloride to ethanol in the ethanol solution of amine hydrochloride is 1:5-1:20, preferably 1:8-1:15, more preferably 1:8-1:12; in the ethanol solution of the epichlorohydrin, the mass ratio of the epichlorohydrin to the ethanol is 1:0.5-1:5, preferably 1:0.5-1:3, and more preferably 1:0.5-1:1.2.
In some embodiments of the invention, the amine hydrochloride is selected from one or more of dimethylamine hydrochloride, diethylamine hydrochloride, and dipropylamine hydrochloride.
In some embodiments of the present invention, to ensure adequate reaction of the amine hydrochloride and epichlorohydrin, the mass ratio of amine hydrochloride to epichlorohydrin is from 1:1 to 1:5, preferably from 1:1 to 1:4, more preferably from 1:1.3 to 1:3.
In some embodiments of the invention, the quaternization reaction is carried out in the presence of a second solvent; preferably, step (2) further comprises: dissolving the first intermediate and dodecyl dimethyl tertiary amine in the second solvent; and evaporating the second solvent under reduced pressure to obtain oily liquid, and recrystallizing the oily liquid to obtain the second intermediate.
The second solvent is not particularly limited as long as the first intermediate and the dodecyldimethyl tertiary amine can be dissolved. Preferably, the second solvent is selected from methanol, ethanol, acetone, toluene, preferably ethanol.
In some embodiments of the present invention, to ensure that the first intermediate and the dodecyldimethyl tertiary amine are sufficiently reacted, the mass ratio of the first intermediate to the dodecyldimethyl tertiary amine is 1:1 to 1:5, preferably 1:1.5 to 1:4, more preferably 1:1.5 to 1:2.5.
In some embodiments of the invention, preferably, the oily liquid is recrystallized from an ethanol/acetone mixed solvent; the mass ratio of the ethanol to the acetone in the ethanol/acetone mixed solvent is 1:1.5-1:3, preferably 1:1.5-1:2.5, and more preferably 1:1.5-1:2.
In some embodiments of the invention, the sulfonation reaction is performed in the presence of tetrahydrofuran; preferably, step (3) further comprises: dissolving a second intermediate, sultone and MH in tetrahydrofuran, refluxing, mixing the solution obtained after refluxing with ethanol, evaporating the tetrahydrofuran and ethanol solvent under reduced pressure to obtain oily liquid, and recrystallizing the oily liquid to obtain the surfactant.
In some embodiments of the invention, the moisture content in the tetrahydrofuran should be less than 1wt%. The tetrahydrofuran may be purified by water removal using methods conventional in the art. Preferably, the water removal and purification process comprises the following steps: adding anhydrous CaCl 2 into tetrahydrofuran, filtering to obtain a reaction solvent I, adding sodium strips into the reaction solvent I, refluxing, adding benzophenone, and if the solution turns blue, indicating that the water content in the tetrahydrofuran meets the requirements, otherwise, the tetrahydrofuran is incompletely dehydrated.
In some embodiments of the present invention, the mass ratio of tetrahydrofuran to anhydrous calcium chloride is 20:1 to 50:1, preferably 20:1 to 40:1, more preferably 25:1 to 30:1, in order to more completely and thoroughly remove water from the tetrahydrofuran. The mass ratio of the anhydrous CaCl 2 to the sodium rod is 5:1-1:1, preferably 4:1-1:1, more preferably 3:1-2:1.
In some embodiments of the invention, benzophenone is used as an indicator to show whether the tetrahydrofuran is completely dehydrated. Therefore, the amount of the benzophenone is not particularly limited in the present invention, and it is preferably 0.5 to 1.5g, more preferably 0.5 to 1.2g, and still more preferably 0.5 to 1g, relative to 300g of tetrahydrofuran.
In some embodiments of the invention, preferably, the sultone is selected from propane sultone and/or butane sultone.
In some embodiments of the invention, to ensure that the hydroxyl groups in the second intermediate are fully substituted, the mass ratio of the second intermediate to the sultone is from 1:1 to 4:1, preferably from 1:1 to 3:1, more preferably from 1.5:1 to 3:1. The mass ratio of the second intermediate to the MH is 15:1-5:1, preferably 10:1-5:1, more preferably 10:1-6:1.
In some embodiments of the invention, to remove MH from the post reflux solution, ethanol is added. The amount of ethanol used in the present invention is not particularly limited as long as the excess MH in the solution after reflux can be completely removed. Preferably, the mass ratio of the ethanol to the MH is 100:3.
In the present invention, the choice of M in MH can correspond to M 1 and M 2 in formula I. Preferably corresponding M 1 is the same as M 2.
In some embodiments of the invention, preferably, the oily liquid is recrystallized from n-hexane.
In a third aspect the present invention provides a surfactant obtainable by the process according to the second aspect.
The fourth aspect of the invention provides a method for preparing a microemulsion plugging agent for water-based drilling fluid, which comprises the following steps: mixing an oil phase, saline, a first surfactant, a second surfactant and a cosurfactant to obtain the microemulsion blocking agent; wherein the first surfactant is the surfactant of the first aspect; the brine has an aqueous activity of no greater than 0.85.
The inventors of the present invention have found in the study that by adding the first surfactant during the preparation of the microemulsion, the prepared microemulsion can be made more stable, and the high-concentration brine can be made more easily to form the microemulsion. In addition, the high-concentration brine is selected in the preparation process of the microemulsion, so that the prepared microemulsion has better inhibition performance.
In the invention, the forming principle of the microemulsion blocking agent is as follows: in the presence of surfactant, the oil-water interfacial tension is greatly reduced, so that a common emulsion is formed, but the microemulsion is not formed enough, and the addition of the cosurfactant can form a mixed adsorption film with the surfactant molecules at the oil-water interface. With further addition of the cosurfactant, the oil-water interfacial tension can drop to zero or even a negative value at a certain moment, and at the moment, the system can generate more emulsion particles to enlarge the oil-water interfacial area so as to offset the negative value of the interfacial tension, so that emulsion drops become very small, and microemulsion is formed. If the emulsion droplets coalesce, the interfacial tension then becomes negative again, which in turn promotes dispersion of the emulsion droplets into finer microemulsion droplets.
In some embodiments of the invention, the second surfactant is selected from one or more of cocamidopropyl hydroxysulfobetaine, bromohexadecyl trimethylamine, perfluoroalkyl polyether phosphate, tween 80 and span 80, preferably span 80.
In some embodiments of the present invention, preferably, the cosurfactant is selected from one or more of n-pentanol, n-propanol, n-hexanol, n-heptanol, 1, 3-propanediol, n-butanol, and polyethylene glycol, preferably one or more of n-pentanol, n-butanol, n-hexanol, and n-heptanol.
In some embodiments of the invention, the oil phase is preferably selected from one of 3 # white oil, 5 # white oil, 0 # diesel, 5 # diesel, n-octane and n-decane, preferably one of 3 # white oil, 5 # white oil, 0 # diesel and 5 # diesel.
In some embodiments of the invention, preferably, the brine is selected from one or more of sodium chloride brine, potassium chloride brine, calcium chloride brine, potassium formate brine, and sodium formate brine, preferably one of sodium chloride and potassium chloride.
In the prior art, the microemulsion is generally fresh water or low-concentration brine, and is difficult to form under high-concentration brine. The microemulsion plugging agent for the water-based drilling fluid is prepared by adopting high-concentration brine, and the prepared microemulsion is used in the drilling fluid, so that the drilling fluid has strong inhibition.
In some embodiments of the invention, the brine has an aqueous activity of no greater than 0.85. The water activity of the brine can be measured using a water activity meter conventional in the art, for example, a portable water activity meter model LabSwift-aw from Novasina, switzerland.
In some embodiments of the invention, since the water activity of brine is directly related to concentration, the water activity of brine is no greater than 0.85 when the concentration of brine meets the following conditions;
The sodium chloride salt water concentration is selected from 10-30wt%, preferably 15-27wt%, more preferably 18-24wt%;
the concentration of the potassium chloride salt water is selected from 20-40wt%, preferably 20-35wt%, more preferably 25-30wt%;
The calcium chloride brine concentration is selected from 25-40wt%, preferably 30-38wt%, more preferably 30-35wt%;
the concentration of the potassium formate brine is selected from 25-40wt%, preferably 30-38wt%, more preferably 30-35wt%;
the sodium formate brine concentration is selected from 25 to 40wt%, preferably 25 to 35wt%, more preferably 30 to 35wt%.
In some embodiments of the invention, the mass ratio of the first surfactant, the second surfactant, the cosurfactant, the oil phase and the brine is 8-20:1-6:2-4:15-25:15-25. When the content ranges are satisfied, the blocking performance and the inhibition performance of the prepared microemulsion blocking agent can be improved.
In a fifth aspect, the present invention provides a microemulsion plugging agent for water-based drilling fluids prepared by the method of the third aspect. The average particle size of the microemulsion blocking agent is 10-60nm. The microemulsion plugging agent for the water-based drilling fluid has good well wall stabilizing effect, and realizes the unification of strong inhibition and strong plugging performance.
In a sixth aspect, the present invention provides a water-based drilling fluid, comprising the microemulsion blocking agent for a water-based drilling fluid according to the fourth aspect. The microemulsion plugging agent provided by the invention is applied to water-based drilling fluid, and the prepared water-based drilling fluid has strong plugging property and inhibition property.
In some embodiments of the invention, the microemulsion blocking agent is present in an amount of 0.5 to 5wt%, preferably 0.5 to 3wt%, based on the total amount of water-based drilling fluid.
According to the invention, when the microemulsions with different concentrations are added into the drilling fluid, the microemulsions are diluted to form the nanoemulsions, and the particle sizes of the droplets of the nanoemulsions diluted by the microemulsions with different concentrations are different, so that the micro-nano cracks with different sizes can be plugged.
In some embodiments of the present invention, bentonite, conventional treatments, flow modifiers and weighting materials may also be included in the water-based drilling fluid. The types and amounts of bentonite, conventional treating agent, flow pattern modifier and weighting material may be selected as is conventional in the art, and the present invention is not limited herein.
The present invention will be described in detail by examples. In the following examples and comparative examples:
Dimethylamine hydrochloride, diethylamine hydrochloride and dipropylamine hydrochloride were purchased from Shanghai Yu Kagaku Co., ltd;
dodecyl dimethyl tertiary amine, propane sultone and butane sultone are purchased from national pharmaceutical chemicals company, ltd.
Example 1
Preparation of a surfactant:
(1) Dissolving 4.1g of dimethylamine hydrochloride in 40g of ethanol, dissolving 10.18g of epichlorohydrin in 12g of ethanol, slowly adding the epichlorohydrin solution into dimethylamine hydrochloride solution, stopping reacting for 48 hours at 50 ℃, and evaporating the solvent under reduced pressure to obtain colorless viscous liquid, namely a first intermediate;
(2) Dissolving 10g of a first intermediate in 85g of ethanol, slowly adding 20g of dodecyl dimethyl tertiary amine, reacting for 48 hours at the temperature of 60 ℃, stopping reacting, evaporating the solvent under reduced pressure to obtain pale yellow oily liquid, recrystallizing with 40g of ethanol/acetone mixed solvent, and standing for 5 hours at the temperature of 4 ℃ to obtain white powdery solid, namely a second intermediate;
(3) Dissolving 2g of the second intermediate obtained in the step (2) in 200g of tetrahydrofuran (the water content is lower than 1 wt%) and introducing N 2, adding 0.3g of NaH, adding 1g of propane sultone, carrying out reflux reaction for 48h, adding 10g of ethanol, decompressing and steaming to remove the solvent (tetrahydrofuran and ethanol) when no bubbles are generated, obtaining pale yellow oily liquid, and recrystallizing with N-hexane at 3 ℃ for 4h to obtain white solid, namely the target product surfactant which is marked as DMS-1.
Preparation of microemulsion plugging agent for water-based drilling fluid:
Mixing and shaking 10g of 3 # white oil, 10g of 21% sodium chloride brine, 6.88g of DMS-1 and 1.12g of span 80 at 25 ℃; then 1.5g of n-butanol was slowly added dropwise thereto; after slight shaking, the mixture was allowed to stand for 24 hours to form a microemulsion, which was designated CDMS-1.
Example 2
Preparation of a surfactant:
A surfactant was prepared as in example 1, except that in step (1), "dimethylamine hydrochloride" was modified to "diethylamine hydrochloride", and the addition of amine hydrochloride was modified from "4.1g" to "5.5g", and the surfactant thus prepared was designated as DMS-2.
Preparation of microemulsion plugging agent for water-based drilling fluid:
Mixing 10g of 5 # white oil, 10g of 25% potassium chloride brine, 6.88g of DMS-2 and 1.12g of span 80 at 25 ℃ and shaking uniformly; then 1.5g of n-amyl alcohol is slowly added dropwise thereto; after slight shaking, the mixture was allowed to stand for 24 hours to form a microemulsion, which was designated CDMS-2.
Example 3
Preparation of a surfactant:
a surfactant was prepared as in example 1, except that in step (1), "dimethylamine hydrochloride" was modified to "dipropylamine hydrochloride", and the addition amount of amine hydrochloride was modified from "4.1g" to "6.9g", and the surfactant thus prepared was designated as DMS-3.
Preparation of microemulsion plugging agent for water-based drilling fluid:
Mixing 10g of 0 # diesel oil, 10g of 24% sodium chloride brine, 5.76g of DMS-3 and 2.24g of span 80 at 25 ℃ and shaking uniformly; then 1.5g of n-hexanol was slowly added dropwise thereto; after slight shaking, the mixture was allowed to stand for 24 hours to form a microemulsion, which was designated CDMS-3.
Example 4
Preparation of a surfactant:
a surfactant was prepared in the same manner as in example 1 except that in step (3), propane sultone was modified to "butane sultone", and the amount of the added sultone was modified from "1g" to "1.1g", and the surfactant thus prepared was designated as DMS-4.
Preparation of microemulsion plugging agent for water-based drilling fluid:
Mixing 10g of 5 # diesel oil, 10g of 28% potassium chloride brine, 5.76g of DMS-4 and 2.24g of span 80 at 25 ℃ and shaking uniformly; then 1.5g of n-heptanol was slowly added dropwise thereto; after slight shaking, the mixture was allowed to stand for 24 hours to form a microemulsion, which was designated CDMS-4.
Example 5
Preparation of microemulsion plugging agent for water-based drilling fluid:
mixing 10g of 3 # white oil, 10g of 21% sodium chloride brine, 5.76g of DMS-4 and 2.24g of span 80 at 25 ℃ and shaking uniformly; then 1.5g of n-butanol was slowly added dropwise thereto; after slight shaking, the mixture was allowed to stand for 24 hours to form a microemulsion, which was designated CDMS-5.
Test example 1
The surface tension of the surfactants prepared in examples 1-4 at room temperature was measured using DCAT table/interfacial tension meter at different concentrations and the test results are shown in table 1.
TABLE 1
As can be seen from the results in table 1, as the mass concentration of the surfactant increases, the surface tension of the solution gradually decreases, which indicates that the surfactant provided by the invention can effectively reduce the surface tension of the solution, and when the mass concentration of the surfactant solution is 0.5%, the surface tension of the solution is about 30mN/m, and the effect of reducing the surface tension is remarkable.
Test example 2
The microemulsion blocking agents for water-based drilling fluids prepared in examples 1 to 5 were tested for emulsifying property and stability.
Emulsifying property test
The microemulsions prepared in examples 1-5 were each taken and the volume average particle size of the microemulsion was determined using a Zetasizer Nano S90 malvern nanosize meter with the following parameters: universal mode (Default); the refractive index of the particles was 1.520; the refractive index of the dispersant is 1.330; rotational speed of the pump: 2050r/min. Average 3 determinations for each sample were averaged. The test results are shown in Table 2.
Stability determination
20G of the microemulsion prepared in examples 1 to 5 was placed in a centrifuge tube, and centrifuged at 7000rpm for 10min by a high-speed centrifuge, and the layering condition of the emulsion was observed. The test results are shown in Table 2.
TABLE 2
CDMS-1 CDMS-2 CDMS-3 CDMS-4 CDMS-5
Particle size (nm) 22.3 31.2 28.5 30.4 38.8
Stability of Not layered Not layered Not layered Not layered Not layered
As shown in the data in Table 2, the particle size of the microemulsion prepared by the invention is smaller than 50nm, which indicates that the surfactant prepared by the invention has very good emulsifying property, and the result of centrifugal stability measurement further proves that the microemulsion prepared by the invention has higher stability.
Test example 3
The clay-free phase water-based drilling fluid is prepared using methods conventional in the art. Taking the total amount of drilling fluid as a reference, the formula of the clay-free phase water-based drilling fluid comprises the following components: 400mL of water+0.2 wt% NaOH+0.3wt% PAC-HV+0.3wt% XCD+1wt% polyamine SDJA-1+3wt% ultrafine calcium carbonate (ASP-1250) +3wt% ASR-1+100g barite. The water-based drilling fluid is prepared according to the adding sequence in the formula, and the specific operation process comprises the following steps: the treatment agent was added while homogenizing at 10000rpm using a high-speed homogenizer. After each treatment agent was added at intervals of 10min, stirring was continued for 20min using a high-speed homogenizer at 10000 rpm. The prepared clay-free phase water-based drilling fluid is recorded as a basic formula.
3Wt% of the microemulsion blocking agents CDMS-1, CDMS-2, CDMS-3, CDMS-4 and CDMS-5 for the water-based drilling fluid prepared in examples 1-5 are respectively added into the basic formula, and the rheological parameters and the fluid loss of the drilling fluid before and after hot rolling at 90 ℃ for 16 hours are measured, and the results are shown in Table 3.
Wherein the rheological parameters are tested by a ZNN-D6 six-speed viscometer and a cloth-type viscometer, and the rheological parameters comprise apparent viscosity AV, plastic viscosity PV and dynamic shear force YP.
The filtrate loss was tested by a ZNS-2 type medium pressure filtrate instrument.
TABLE 3 Table 3
As can be seen from the test results in Table 3, after the microemulsion plugging agent for water-based drilling fluid provided by the invention is added into the basic formula, the rheological parameter of the drilling fluid is little changed, FL API (i.e. medium pressure filtration vector) is reduced, and the rheological parameter and API filtration loss before and after hot rolling are little different, which indicates that the drilling fluid system after the microemulsion plugging agent for water-based drilling fluid is added has good temperature resistance, and the formed mud cake has good quality, can be effectively plugged, and reduces the penetration of filtrate.
The plugging effect of each drilling fluid was evaluated at 120 ℃/3.5MPa using a high temperature high pressure infiltration plugging instrument (PPT), and the test results are shown in table 4.
TABLE 4 Table 4
As can be seen from the test results of Table 4, the water-based drilling fluid has a smaller HTHP/FL after the microemulsion plugging agent for the water-based drilling fluid is added into the basic formula, which indicates that the plugging effect of the water-based drilling fluid provided by the invention is better.
Test example 4
The inhibition performance of the microemulsion plugging agent for the water-based drilling fluid is evaluated by 2 indexes of shale expansion rate and shale recovery rate.
Shale expansion experiment:
10g of standard lime clay is put into a self-made mould and pressed for 5min under the pressure of 10MPa by using a press to obtain an artificial rock core, and the linear expansion rates of the artificial rock core in clear water, a drilling fluid basic formula and a drilling fluid containing a microemulsion plugging agent are measured by using an intelligent shale expander, and the results are shown in table 5.
TABLE 5
As can be seen from the results in Table 5, the expansion rate of the artificial core in clear water is 10.48%, the expansion rate of the artificial core in the water-based drilling fluid base slurry is 1.64%, and the expansion rate of the artificial core is only 1.22% -1.45% after the microemulsion plugging agent is added into the water-based drilling fluid base slurry, so that the inhibition performance of the microemulsion provided by the invention is better.
Shale rolling dispersion experiment:
50g of mud shale with the grain size of 5-10 meshes and used for sand river street group of victory oil fields is taken and respectively put into water-based drilling fluid containing 350mL of clear water, a drilling fluid basic formula and a microemulsion plugging agent, and the water-based drilling fluid is heated and rolled for 16 hours at 100 ℃ and then passes through a 40-target standard sieve, and after the screen residue is dried at 105 ℃, the recovery rate of rock debris is measured, and the result is shown in Table 6.
TABLE 6
As can be seen from the results in Table 6, after 3wt% of the microemulsion blocking agent for water-based drilling fluid is added, the recovery rate of rock debris reaches more than 90%, which shows that the microemulsion blocking agent for water-based drilling fluid has strong shale hydration dispersion inhibition performance.
In conclusion, the average particle size of the microemulsion blocking agent for the water-based drilling fluid provided by the invention is 10-60nm, and the microemulsion blocking agent has good stability. The microemulsion plugging agent provided by the invention is applied to water-based drilling fluid, and the prepared water-based drilling fluid has strong plugging property and inhibition property.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (29)

1. The preparation method of the microemulsion plugging agent for the water-based drilling fluid is characterized by comprising the following steps of: mixing an oil phase, saline, a first surfactant, a second surfactant and a cosurfactant to obtain the microemulsion blocking agent; the brine has an aqueous activity of no greater than 0.85;
The structure of the first surfactant is shown as a structural formula I
Wherein R 1 is-CH 3、-CH2CH3 or-CH 2CH2CH3,R2 is-CH 3、-CH2CH3 or-CH 2CH2CH3,R3 is- (CH 2)3 -or- (CH 2)4-,R4 is- (CH 2)3 -or- (CH 2)4-,M1) is Li, na or K, and M 2 is Li, na or K).
2. The method of claim 1, wherein the method of preparing the first surfactant comprises the steps of:
(1) Carrying out ring-opening reaction on amine hydrochloride shown in a formula II and epichlorohydrin to obtain a first intermediate;
Wherein R 1 is-CH 3、-CH2CH3 or-CH 2CH2CH3,R2 is-CH 3、-CH2CH3 or-CH 2CH2CH3;
(2) Quaternizing the first intermediate with dodecyl dimethyl tertiary amine to obtain a second intermediate;
(3) Sulfonation reaction is carried out on the second intermediate, sultone shown in a formula III and a compound shown in a general formula MH, so as to obtain the first surfactant,
Wherein R 3 is- (CH 2)3 -or- (CH 2)4 -, MH is one or two of LiH, naH and KH).
3. The method of claim 2, wherein the ring-opening reaction is performed in the presence of a first solvent.
4. A method according to claim 3, wherein step (1) further comprises: dissolving amine hydrochloride and epichlorohydrin in the first solvent; and decompressing and steaming the product solution obtained by the ring-opening reaction to remove the first solvent to obtain the first intermediate.
5. The method of claim 4, wherein the amine hydrochloride is selected from one or more of dimethylamine hydrochloride, diethylamine hydrochloride, and dipropylamine hydrochloride.
6. The method of claim 5, wherein the mass ratio of amine hydrochloride to epichlorohydrin is from 1:1 to 1:5.
7. The method of claim 6, wherein the mass ratio of amine hydrochloride to epichlorohydrin is from 1:1 to 1:4.
8. The method of claim 7, wherein the mass ratio of amine hydrochloride to epichlorohydrin is from 1:1.3 to 1:3.
9. The method of claim 2, wherein the quaternizing reaction is performed in the presence of a second solvent.
10. The method of claim 9, wherein step (2) further comprises: dissolving the first intermediate and dodecyl dimethyl tertiary amine in the second solvent; and evaporating the second solvent under reduced pressure to obtain oily liquid, and recrystallizing the oily liquid to obtain the second intermediate.
11. The process according to claim 2 or 9, wherein the mass ratio of the first intermediate to dodecyl dimethyl tertiary amine is 1:1-1:5.
12. The process of claim 11, wherein the mass ratio of the first intermediate to dodecyl dimethyl tertiary amine is from 1:1.5 to 1:4.
13. The process of claim 12, wherein the mass ratio of the first intermediate to dodecyl dimethyl tertiary amine is from 1:1.5 to 1:2.5.
14. The process of claim 2, wherein the sulfonation reaction is carried out in the presence of tetrahydrofuran.
15. The method of claim 14, wherein step (3) further comprises: dissolving a second intermediate, sultone and MH in tetrahydrofuran, refluxing, mixing the solution obtained after refluxing with ethanol, evaporating the tetrahydrofuran and ethanol solvent under reduced pressure to obtain oily liquid, and recrystallizing the oily liquid to obtain the surfactant.
16. A method according to claim 2 or 15, wherein the sultone is selected from propane sultone and/or butane sultone.
17. The process of claim 16, wherein the mass ratio of the second intermediate to sultone is 1:1-4:1.
18. The process of claim 17, wherein the mass ratio of the second intermediate to sultone is 1:1-3:1.
19. The process of claim 18, wherein the mass ratio of the second intermediate to sultone is 1.5:1-3:1.
20. The method of claim 1, wherein the second surfactant is selected from one or more of cocamidopropyl hydroxysulfobetaine, bromohexadecyl trimethylamine, perfluoroalkyl polyether phosphates, tween 80, and span 80.
21. The method of claim 20, wherein the second surfactant is span 80.
22. The method of claim 1, wherein the cosurfactant is selected from one or more of n-pentanol, n-propanol, n-hexanol, n-heptanol, 1, 3-propanediol, n-butanol, and polyethylene glycol.
23. The method of claim 1, wherein the oil phase is selected from one of 3 # white oil, 5 # white oil, 0 # diesel, 5 # diesel, n-octane, and n-decane.
24. The method of claim 1, wherein the brine is selected from one or more of sodium chloride brine, potassium chloride brine, calcium chloride brine, potassium formate brine, and sodium formate brine.
25. The method of claim 1, wherein the mass ratio of the first surfactant, the second surfactant, the cosurfactant, the oil phase and the brine is 8-20:1-6:2-4:15-25:15-25.
26. A microemulsion blocking agent for water-based drilling fluids prepared by the method of any one of claims 1 to 25, wherein the microemulsion blocking agent has an average particle size of 10 to 60nm.
27. A water-based drilling fluid comprising the microemulsion plugging agent for a water-based drilling fluid of claim 26.
28. The water-based drilling fluid of claim 27, wherein the microemulsion blocking agent is present in an amount of 0.5 to 5wt% based on the total amount of the water-based drilling fluid.
29. The water-based drilling fluid of claim 28, wherein the microemulsion blocking agent is present in an amount of 0.5 to 3wt% based on the total amount of the water-based drilling fluid.
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