CN107603576A - A kind of well cementation oil-based mud flushing liquor and its preparation and evaluation method - Google Patents

A kind of well cementation oil-based mud flushing liquor and its preparation and evaluation method Download PDF

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Publication number
CN107603576A
CN107603576A CN201710624393.7A CN201710624393A CN107603576A CN 107603576 A CN107603576 A CN 107603576A CN 201710624393 A CN201710624393 A CN 201710624393A CN 107603576 A CN107603576 A CN 107603576A
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China
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oil
flushing liquor
mud
based mud
well cementation
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CN201710624393.7A
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CN107603576B (en
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张福铭
赵琥
王雪山
代丹
孟佳佳
符军放
薛雷
陈凡斌
宋茂林
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China Oilfield Services Ltd
China National Offshore Oil Corp CNOOC
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China Oilfield Services Ltd
China National Offshore Oil Corp CNOOC
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Abstract

A kind of well cementation oil-based mud flushing liquor and its preparation and evaluation method, the flushing liquor includes solvent, nonionic surfactant, zwitterionic surfactant, polymer and water, the polymer is by selected from N, N DMAAs, acrylic acid, propylene are fine, a kind of or more kinds of monomer in the methyl propane sulfonic acid of 2 acrylamide 2, acrylamide is polymerized;The preparation method includes dissolving a polymer in water, and nonionic surfactant and zwitterionic surfactant are dissolved in solvent, the aqueous solution containing polymer is added in the solvent dissolved with surfactant, stirred;The evaluation method includes the performance that comprehensive well cementation oil-based mud flushing liquor judges the developing result of oil-base mud, water wettability, three evaluation indexes of compatibility to oil-base mud and cement mortar well cementation oil-based mud flushing liquor.The oil-based mud flushing liquor of the application has excellent developing result, good with oil-base mud, cement mortar compatibility.

Description

A kind of well cementation oil-based mud flushing liquor and its preparation and evaluation method
Technical field
The application relates to, but are not limited to a kind of well cementation oil-based mud flushing liquor and preparation method thereof, and a kind of evaluation oil base The method of mud fluid.
Background technology
One layer of slurry oil, oil film are adhering in oil-base mud finishing drilling well section, the borehole wall and casing wall, it will cause cement sheath Interface agglutination poor-performing.Laboratory test shows that the interface cementing strength of Behavior of Hardened Cement Paste is zero in this case, and this is by serious shadow Ring cementing quality.Therefore, it is successfully to cement the well to clean slurry oil, the oil film being adhered on down-hole annular interface before cementing with flushing liquor Key measure.
External oil company mainly adds among separating liquid system can make the surface of oil-base mud wettability reversal live Property agent carry out operation, such as the D607 of Schlumberger, S-5, MCS-GS of Bake Hughes, be primarily upon insulating liquid and oil-base mud The characteristic of compatibility and surfactant to oil-base mud wettability reversal.Home products single varieties, washability is poor, main to close The cleaning to cement plane oil film is noted, the measure and compatibility concern for oil-base mud wettability reversal (electrical conductivity method) are less.
Patent CN 103642475A disclose a kind of washing oil irrigation, there is good flushing effect to all kinds of oil base drilling fluids Fruit and wettability reversal effect, the insulating liquid prepared using the irrigation can solve oilwell drilling liquid and water-based insulating liquid, cement mortar Incompatibility problem.The irrigation is mainly by soap base, sodium sulfate of polyethenoxy ether of fatty alcohol, AEO, alkyl Phenol polyethenoxy ether, sorbitan monooleate and water are formed, main to be stained with oil-base mud under 300rpm/min using rotor and use 6% washing oil irrigation rinses 5min, and flush efficiency is evaluated using weight method, is stained with steel disc after oil-base mud rinses with flushing liquor Measurement angle of wetting acts on to determine wettability reversal.
Patent CN 1405265A disclose a kind of oil-based mud flushing liquor, the flushing liquor mainly by lauryl sodium sulfate, AEO, oleic acid, sodium hydroxide, ethylenediamine tetra-acetic acid, water are formed.With the work for separating drilling fluid and cement mortar With, contact stain can be prevented, it is good with the compatibility of drilling fluid, the viscosity and shear force of drilling fluid can be reduced, can be more effectively Second interface is rinsed, improves cementing strength.The main work data with scene is evaluated effect, such as cementing quality.
Patent CN 1329126A disclose a kind of oil base mud well-cementing flushing fluid, and the flushing liquor is by lard acid polyoxy second Alkene fat, diesel oil, APES are formed.The flushing liquor has preferable developing result to oil-base mud and mud cake, together When to oil-base mud have preferably dilution viscosity reduction effect.One or two cement planes are simulated with steel pipe and rock core, again by being stained with oil base The method that mud is rinsed with flushing liquor tests developing result, and the steel pipe cleaned and rock core and blank are placed in certain mould In, cement mortar is poured into, tests cementing strength.
Patent CN 106367050A disclose a kind of high density oil base drilling fluid superhigh temperature resistant flushing liquor and its preparation side Method, the flushing liquor is by cocoanut fatty acid diethanolamide, alkyl benzene sulphonate triethanolamine salt, ethylene glycol monobutyl ether, maleic acid Acrylic copolymer, water composition, temperature resistance is up to 190 DEG C, flush efficiency more than 90%.Only oil is stained with the outer barrel of six fast rotation viscometers Base mud carries out simulation flushing, calculates flush efficiency with this, does not refer to the test of other performances.
Patent CN 105419758A disclose a kind of suitable for the well cementation flushing liquor system of oil base drilling fluid and its preparation side Method, the flushing liquor system by anion surfactant, nonionic surfactant, cosurfactant, oil phase, salt aqueous phase, Polymer, heavy weight additive, water, salt etc. form, 20 DEG C~130 DEG C of Applicable temperature.Valuation of patent flushing liquor and oil-base mud Compatibility, and immersed after oil base drilling fluid by mould and rinsed with flushing liquor to test flush efficiency, utilize contact angle Method of testing have rated wettability reversal performance, and test second interface cementing strength.
Patent CN103555304B discloses a kind of oil base flushing spacer fluid and preparation method thereof, and the insulating liquid is mainly by clear Water, surfactant, chelating agent, suspension stabilizer, tackifier, carry cutting and put forward the groups such as stick, heavy weight additive, pH adjusting agent, defoamer Into.The insulating liquid has the double action rinsed and isolated, and has good stability.Being simple test in CN103555304B should The stability and rheological parameter of system, the performances such as the developing result to oil-base mud, wettability reversal are not evaluated.
Patent CN104140798A discloses a kind of anti-freezing type flushing liquor for being used to clean oil base drilling fluid, flushing liquor master To be made up of nonionic surfactant, anion surfactant and freezing point depressant, lowest construction temperature reaches -15 DEG C.Comment Angle of wetting is tested with steel disc in valency experiment, while tests the mobility under low temperature, does not test and oil-base mud is rushed Wash effect and compatibility.
Patent CN103849364B discloses a kind of oil base drilling fluid well cementation flushing liquor and preparation method, flushing liquor master Will be by xanthans, hydroxyethyl cellulose, xanthans, polyvinylpyrrolidone, sodium polyphosphate, NPE, ten Dialkyl benzene sulfonic acids sodium, water, solid phase particles etc. form.In evaluation experimental, using six fast rotation viscometer outer barrels in oil-base mud Middle stirring immersion, then rinses 3~10min to evaluate flush efficiency, and test flushing liquor and oil-base mud with flushing liquor Compatibility.
Patent CN103555306B discloses a kind of oil-based mud flushing liquor suitable for high temperature and high salt environment and its preparation Method, the flushing liquor are made up of calcium chloride, AES, ethoxylated dodecyl alcohol, clear water.It is viscous using six speed rotations in evaluation experimental Degree meter outer barrel is rinsed after being soaked in oil-base mud with flushing liquor, while tests angle of wetting with steel disc method.
Patent CN105315979A discloses a kind of well cementation oil-based mud flushing liquor and preparation method thereof, the flushing liquor by Water, polymeric surfactant, nano-attapulgite powder composition.Flush efficiency data are only gived in evaluation experimental, but are not said It is bright which kind of method to test flush efficiency with.
Patent CN105315978A discloses a kind of well cementation oil-based mud flushing liquor and preparation method thereof, the flushing liquor by Water, nonionic surfactant, anion surfactant, zwitterionic surfactant, sorbester p17, Tween 80, carry viscous carry Cut agent composition.Flush efficiency data are only gived in evaluation experimental, but which kind of method flush efficiency is tested with without explanation.
US6686323 discloses a kind of oil-based mud flushing liquor, and the flushing liquor is mainly by alkyl poly glucoside class surface Activating agent, the mixed liquor of esters solvent are formed.
Above-mentioned oil-based mud flushing liquor largely includes water and surfactant, some additions carry viscous extracting and cutting agent, salt solution, Polymer etc., whole flushing liquor are water base state, and such flushing liquor is limited to the flushing action of oil-base mud, for viscous The oil-base mud being attached on 100 mesh sand paper (using the 100 mesh sand paper simulation borehole wall, more convincing than being stained with oil-base mud with rotor) Developing result it is poor.
And by above-mentioned disclosure from the point of view of, the evaluation for oil-based mud flushing liquor is excessively simple, and It is not rigorous, it is impossible to simulate the real conditions of underground.
The content of the invention
It is the general introduction of the theme to being described in detail herein below.It is to limit the protection model of claim that this general introduction, which is not, Enclose.
This application provides a kind of with good developing result, the oil-base mud punching that wettability reversal ability is strong, compatibility is good Washing lotion and preparation method thereof, and a kind of rigorous, accurate evaluation oil-based mud flushing liquor method.
Specifically, this application provides a kind of well cementation oil-based mud flushing liquor, the flushing liquor to include solvent, nonionic Surfactant, zwitterionic surfactant, polymer and water, wherein, the polymer is by selected from N, N- dimethyl allenes Acid amides, acrylic acid, propylene are fine, a kind of or more kinds of monomer polymerization in 2- acrylamide-2-methyl propane sulfonics, acrylamide Form.
Alternatively, the polymer can be by N,N-DMAA, 2- acrylamide-2-methyl propane sulfonics and third Acrylamide is polymerized.
In presently filed embodiment, the solvent can be selected from hydrocarbon-type oil, oleic acid, ketone, C6~C7 alkane, benzene Two kinds in class, alcohols, turpentine oil and ethers.
Alternatively, the solvent is hydrocarbon-type oil and diethylene glycol monobutyl ether.
Alternatively, in the solvent being made up of hydrocarbon-type oil and diethylene glycol monobutyl ether, hydrocarbon-type oil and diethylene glycol monobutyl ether Weight ratio be (50~70):(5~20).
Alternatively, flash-point >=60 DEG C of the hydrocarbon-type oil.
Alternatively, the ketone is selected from acetone, ring ethyl ketone.
Alternatively, C6~C7 alkane is selected from hexamethylene, n-hexane, isohexane, heptane.
Alternatively, the benzene class is selected from toluene, dimethylbenzene.
Alternatively, the alcohols is selected from isopropanol, butanol, amylalcohol.
Alternatively, the ethers is selected from ethylene glycol monobutyl ether, diethylene glycol monobutyl ether.
In presently filed embodiment, the nonionic surfactant can be selected from AEO, fat Fat alcohol polyoxyalkyl ether, aliphatic acid polyethenoxy fat, APES, castor oil polyoxyethylene ether, fatty amine polyoxy One or more in vinethene, polyethers.
Alternatively, the nonionic surfactant is aliphatic amine polyoxyethylene ether and castor oil polyoxyethylene ether.
Alternatively, in the nonionic surfactant being made up of aliphatic amine polyoxyethylene ether and castor oil polyoxyethylene ether In, the weight ratio of aliphatic amine polyoxyethylene ether and castor oil polyoxyethylene ether is 1:3~3:1.
Alternatively, the molecular formula of the AEO is RO (CH2CH2O)nH, wherein n=4~9, R C8~ C18Alkyl.
Alternatively, the molecular formula of the fatty alcohol polyoxyalkyl ether is RO (CH2CH2O)n(CH2CH2CH2O)mH, wherein n= 1~9, m=1~9, R C8~C18Alkyl.
Alternatively, the molecular formula of the aliphatic acid polyethenoxy fat is RCOO (CH2CH2O)nH, wherein n=4~9, R C8 ~C18Alkyl.
Alternatively, the molecular formula of the APES is RCO (CH2CH2O)nH, wherein n=5~10, R C12 ~C18Alkyl.
Alternatively, the castor oil polyoxyethylene ether is EL-n, wherein n=10~130.
Alternatively, the molecular formula of the aliphatic amine polyoxyethylene ether is RN [(CH2CH2O)nH]2, wherein n=1~15, R are C8~C18Alkyl.
Alternatively, the molecular formula of the polyethers is HO (C2H4O)m(C3H6O)nH, wherein m=1~30, n=1~30.
In presently filed embodiment, the zwitterionic surfactant can be betaine type amphoteric ion surface Activating agent.
Alternatively, the zwitterionic surfactant is selected from one or both of carboxylic acid glycine betaine, sulfobetaines.
Alternatively, the molecular formula of the carboxylic acid glycine betaine is RN+(CH3)2(CH2)mCOO-, wherein m=1~3, R C8~ C18Alkyl.
Alternatively, the molecular formula of the sulfobetaines is RN+(CH3)2(CH2)mSO3 -, wherein m=1~3, R C8~ C18Alkyl.
In presently filed embodiment, the polymer can be prepared by following methods:N, N- dimethyl will be selected from Acrylamide, acrylic acid, propylene are fine, a kind of or more kinds of monomer in 2- acrylamide-2-methyl propane sulfonics, acrylamide It is 40wt% to be adjusted to concentration with water;40 DEG C~60 DEG C are warming up to, initiator, reducing agent and chain-transferring agent is added and polymerize instead Should;Dry, crush after completion of the reaction
Alternatively, the monomer is N,N-DMAA, 2- acrylamide-2-methyl propane sulfonics and acryloyl Amine, and the weight ratio of N,N-DMAA, 2- acrylamide-2-methyl propane sulfonics and acrylamide for (10~ 30):(40~80):(10~30).
Alternatively, the initiator is (NH4)2S2O8
Alternatively, the reducing agent is NaHSO3
Alternatively, the chain-transferring agent is HCOONa.
In presently filed embodiment, the viscosity average molecular weigh of the polymer can be below 100,000.
In presently filed embodiment, the water can be fresh water.
In presently filed embodiment, counted using the weight of the well cementation oil-based mud flushing liquor as 100%, it is described molten The content of agent can be 60%~80%, and the content of the nonionic surfactant can be 10%~25%, both sexes The content of ionic surface active agent can be that 1%-5%, the content of the polymer can be 1%~3%, the content of the water Can be 7%~10%.
Present invention also provides a kind of method for preparing well cementation oil-based mud flushing liquor as described above, methods described bag Include:
Dissolve a polymer in water;
Nonionic surfactant and zwitterionic surfactant are dissolved in solvent;
The aqueous solution containing polymer is added in the solvent dissolved with surfactant, stirred.
Present invention also provides a kind of method of evaluating cementing oil-based mud flushing liquor, methods described includes comprehensive cement the well With oil-based mud flushing liquor to the developing result of oil-base mud, water wettability, the compatibility three to oil-base mud and cement mortar Individual evaluation index judges the performance of well cementation oil-based mud flushing liquor.
In presently filed embodiment, the borehole wall is simulated with sand paper, utilizes what is prepared by cementing the well with oil-based mud flushing liquor Flushing liquor system reflects the flushing liquor system to being adhered to the borehole wall to the developing result for the oil-base mud being adhered on sand paper On oil-base mud developing result.
Alternatively, the water wettability of well cementation oil-based mud flushing liquor is tested using electrical conductivity method.
Alternatively, the method according to specified in GB/T 19139-2012 tests well cementation oil-based mud flushing liquor to oil base The compatibility of mud and cement mortar.
Alternatively, the oil-base mud is the oil-base mud after live shaft bottom is circulated.
Alternatively, the well cementation is well cementation oil-based mud flushing liquor as described above with oil-based mud flushing liquor.
In presently filed embodiment, using by cementing the well with the flushing liquor system that oil-based mud flushing liquor is prepared to adhesion The developing result of oil-base mud on sand paper can comprise the steps:
Fritter sand paper is fixed on rotation viscometer outer barrel;
The rotation viscometer outer barrel is immersed in oil-base mud, the oil-base mud is flooded the bottom of the sand paper Point, simulate wall building;
The rotation viscometer outer barrel is taken out from oil-base mud, is put into what is prepared by cementing the well with oil-based mud flushing liquor In flushing liquor system, the flushing liquor system is set to flood the lower part of the sand paper, simulation flushing liquor rinses the process of the borehole wall, seen Examine and record experimental phenomena;
After flushing terminates, sand paper is removed into tiling on the table, the wettability of rinsing area, contaminated area is tested with water droplet.
In presently filed embodiment, the oil-base mud can be made to flood lower 2/3 part of the sand paper;Make described Flushing liquor system floods lower 1/3 part of the sand paper.
In presently filed embodiment, the rotating speed of rotation viscometer can be 600r/min when simulating wall building, and simulation is made The time of wall can be 10min.
In presently filed embodiment, the rotating speed of rotation viscometer can be 200r/ when simulation flushing liquor rinses the borehole wall Min, the time for simulating flushing can be 5min.
In presently filed embodiment, developing result, water wettability and the rheology phase with oil-base mud and cement mortar The qualified flushing liquor system of three indexs of capacitive is qualified products, wherein, the qualified evaluation criterion of developing result is to rinse Fall more than 90% oil-base mud, and flushing interface is changed into water wetting, the qualified evaluation criterion of water wettability is to make oil Volume fraction≤75% of oil-based mud flushing liquor system of the base mud completely needed for reversion, closed with the rheological compatibility of cement mortar The evaluation criterion of lattice is R≤0, and qualified evaluation criterion is R≤0 with the rheological compatibility of oil-base mud.
The oil-based mud flushing liquor of the application is in integrally oil phase state, is added to the water with certain proportion during use, to viscous The oil-base mud being attached on sand paper has obvious developing result, and it is in water wetting state to rinse interface;Moistened with electrical conductivity method test water Wet ability meets condition;It is good with oil-base mud, cement mortar compatibility.The Applicable temperature model of the oil-based mud flushing liquor of the application Enclose for 25 DEG C~200 DEG C.
The oil-based mud flushing liquor of the application dissolves first, viscosity reduction oil-base mud;Subsequent complexed surfactant oozes rapidly The Water-In-Oil state of oil-base mud is destroyed thoroughly, and the oleophylic chain of surfactant is adsorbed onto on the material that interface is oil phase, hydrophilic group Around being centered around, mineral oil, the oiliness additive prepared used in oil-base mud are changed into oil-in-water state, and then be dissolved in water base In system;By dissolving, permeating, being demulsified, wettability reversal four steps, the oil film, slurry oil on cement plane can be eliminated rapidly, and will Cement plane is changed into water wetting state.
More it is essential that the polymer in the oil-based mud flushing liquor of the application is not only with after suspending stabilized exacerbation The effect of oil-based mud flushing liquor system, and the function with chelating and auxiliary cleaning.Because the polymerization in flushing liquor Thing can chelate high volence metal ion, generate complex compound stablize, being dissolved in water or colloidal suspension state, have to solids foul Anti-coagulation and peptizaiton, prevent soil redeposition.Furthermore metal ion " constraint " is lived, avoids metal ion from being lived with surface Property agent reaction and reduce surfactant activity, so as to improve the developing result of oil-based mud flushing liquor.
The method of the evaluating cementing oil-based mud flushing liquor of the application, while with well cementation oil-based mud flushing liquor to oil Developing result, water wettability, three indexs of compatibility to oil-base mud and cement mortar of base mud carry out evaluating cementing oil The performance of base mud fluid, evaluation procedure is more rigorous, as a result more accurate.And the roughness of the borehole wall is simulated using sand paper, than It is stained with that oil-base mud is more convincing with rotor, the sample of oil-base mud on rotor can be easily washed away in experiment, on sand paper Oil-base mud does not have effect but.
The flushing liquor for the oil-base mud generally prepared in energy purge chamber, returns oil-base mud for scene and does not act on, it is necessary to Increase dosage or change composition can be only achieved effect.In order to solve this problem, the evaluating cementing oil-base mud of the application The method of flushing liquor, the oil-base mud used in evaluation procedure is sample representative, after live shaft bottom is circulated Product, closer to the scene of field application, make evaluation result closer to truth.
Other features and advantage will illustrate in the following description, also, partly become from specification Obtain it is clear that or being understood by implementing the application.The purpose of the application and other advantages can be by specification, rights Specifically noted structure is realized and obtained in claim and accompanying drawing.
Brief description of the drawings
Accompanying drawing is used for providing further understanding technical scheme, and a part for constitution instruction, with this The embodiment of application is used for the technical scheme for explaining the application together, does not form the limitation to technical scheme.
Fig. 1 is the developing result comparison diagram of the embodiment of the present application 5.
Fig. 2 is the water wettability measurement result figure of the embodiment of the present application 5.
Fig. 3 is the conductance profile of the embodiment of the present application 6.
Fig. 4 is the mixed liquor water wetting effect test result figure after the embodiment of the present application 6 is rinsed.
Fig. 5 is the developing result figure of the embodiment of the present application 8.
Fig. 6 is the water wettability measurement result figure of the embodiment of the present application 8.
Fig. 7 is the conductance profile of the embodiment of the present application 8.
Fig. 8 is the mixed liquor water wetting effect test result figure after the embodiment of the present application 8 is rinsed.
Fig. 9 is the developing result of the embodiment of the present application 9 with the variation diagram of polymer volume.
Embodiment
For the purpose, technical scheme and advantage of the application are more clearly understood, below in conjunction with accompanying drawing to the application Embodiment be described in detail.It should be noted that in the case where not conflicting, in the embodiment and embodiment in the application Feature can mutually be combined.
Raw material and reagent used in following examples, it is ordinary commercial products unless otherwise instructed.
Polymer is prepared by the following method:
Weigh 20g N, N- DMAAs, 70g 2- acrylamide-2-methyl propane sulfonics, 10g acrylamide lists Body is placed in there-necked flask, is adjusted to 40wt% concentration with distilled water, is warming up to 40 DEG C;Sequentially add the initiator of Sq (NH4)2S2O8, reducing agent NaHSO3With chain-transferring agent HCOONa.Dry, crush after completion of the reaction.
Embodiment 1
15g polymer is weighed, is dissolved in 100g fresh water;Weigh 90g aliphatic amine polyoxyethylene ethers (n=5, R C12Alkyl), It is 60 DEG C de- that 90g castor oil polyoxyethylene ethers (n=40), 20g cocamidopropyl propyl amide hydroxy sulfo lycines, which are dissolved in 600g flash-points, In aromatic solvent naphtha, 100g diethylene glycol monobutyl ethers are added;The aqueous solution containing polymer is slowly added under stirring Enter in the double solvents dissolved with surfactant, be well mixed.
Embodiment 2
15g polymer is weighed, is dissolved in 100g fresh water;Weigh 60g isomerous tridecanol polyoxyethylene ethers (n=6), 120g fat Fat amine APEO (n=5, R C12Alkyl), 20g cocamidopropyl propyl amide hydroxy sulfo lycines be dissolved in 600g flash-points for 60 DEG C Porous deproteinized bone solvent naphtha in, add 100g ethylene glycol monobutyl ethers;By the aqueous solution containing polymer under stirring slowly Add dissolved with the double solvents of surfactant, be well mixed.
Embodiment 3
15g polymer is weighed, is dissolved in 100g fresh water;Weigh 120g aliphatic amine polyoxyethylene ethers (n=5, R C12Alkane Base), 60g castor oil polyoxyethylene ethers (n=40), 20g cocamidopropyl propyl amide hydroxy sulfo lycines be dissolved in 600g flash-points for 60 DEG C Porous deproteinized bone solvent naphtha in, add 100g isopropanols;The aqueous solution containing polymer is slowly added under stirring molten Have in the double solvents of surfactant, be well mixed.
Embodiment 4
20g polymer is weighed, is dissolved in 100g fresh water;Weigh 90g aliphatic amine polyoxyethylene ethers (n=5, R C12Alkyl), It is 60 DEG C that 90g isomerous tridecanol polyoxyethylene ethers (n=6), 20g cocamidopropyl propyl amide hydroxy sulfo lycines, which are dissolved in 600g flash-points, In Porous deproteinized bone solvent naphtha, 100g ethylene glycol monobutyl ethers are added;The aqueous solution containing polymer is slowly added under stirring Enter in the double solvents dissolved with surfactant, be well mixed.
The performance evaluation of oil-based mud flushing liquor
Oil-base mud punching is prepared by formula " 300g fresh water+105g oil-based mud flushing liquor (embodiment 1)+137g barites " Washing lotion system.
Oil-base mud sample source is in live WZ6-9-A platforms.
Cement-slurry method is:Dehydration drops in the defoamer+5% of+47.83% fresh water of+35% silica flour of 100% Shandong cement+0.2% The retarder of the anti-channeling of agent+5% reinforcing agent+1%.
Embodiment 5
The developing result of oil-based mud flushing liquor prepared by the present embodiment evaluation embodiment 1, evaluation method are as follows:
At (1) 200 DEG C by oil-based mud flushing liquor system in ageing can aging 4h, pour out after cooling and conserved at 90 DEG C Developing result test is carried out after 20min.
If bottom hole temperature (BHT) be higher than 90 DEG C, should by oil-based mud flushing liquor system in ageing can according to bottom hole temperature (BHT) aging 4h, poured out after its cooling and carry out other test (developing result, water wettability, phases after stirring maintenance 20min at 90 DEG C Capacitive);If bottom hole temperature (BHT)≤90 DEG C, without aging, the stirring maintenance 20min directly under bottom hole temperature (BHT).
(2) 100 mesh sand paper are cut into 132mm × 55mm fritter, and be fixed on six fast rotation viscometer outer barrels.
(3) measure the oil-base mud 300mL after stirring maintenance to pour into six fast rotary viscosity measuring cups, measuring cup is put In lower 2/3 part on test desk, flooding sand paper.Open motor and oil-base mud wall building, wall building are simulated with 600r/min speed Time 10min;
(4) after shutting down, the measuring cup equipped with oil-base mud is removed, while being prepared by embodiment 1 after conserving will be stirred The flushing liquor system prepared of oil-based mud flushing liquor measure 300ml and pour into another clean measuring cup, measuring cup is placed in survey Measure on platform, flood lower 1/3 part of sand paper.The process that motor rinses the borehole wall with 200r/min speed simulation flushing liquor is opened, Washing time 5min.If developing result is good, it is seen that a large amount of greasy dirts are dissolved among flushing liquor system;
(5) after flushing experiment terminates, sand paper is gently removed into tiling on the table, and rinsing area (i.e. sand is tested with water droplet Lower 1/3 part of paper), contaminated area (i.e. by oil-base mud pollute part) wettability.
It will be seen from figure 1 that the oil-base mud on six fast rotation viscometer outer barrels cleans up completely, illustrate the application reality Applying the oil-based mud flushing liquor system that oil-based mud flushing liquor prepared by example 1 is prepared has good developing result, and can With resistance to 200 DEG C of high temperature.Figure it is seen that it is in water droplet state that water droplet is rear on contaminated area, and drops in and rinse interface (i.e. quilt The surface of flushing) on after can scatter rapidly, illustrate rinse interface be water wetting.
Qualified oil-based mud flushing liquor system should be able to rinse out the most of oil-base mud being attached on sand paper, and will punching Wash interface and be changed into water wetting state.
Embodiment 6
The water wettability of oil-based mud flushing liquor prepared by the present embodiment evaluation embodiment 1, evaluation method are as follows:
At (1) 200 DEG C by oil-based mud flushing liquor system in ageing can aging 4h, pour out after cooling and conserved at 90 DEG C The laggard water-filling wettability tests of 20min.
(2) tested by GB/T 19139-2012 " oil-well cement test method ", and calculate oil-based mud flushing liquor system and account for The volume fraction of the mixed liquor of oil-base mud/oil-based mud flushing liquor system
In formula:
VP--- from the volume that oily continuous phase transistion is the oil-based mud flushing liquor system needed for water continuous phase, unit is milliliter (mL);
Vm--- initial oil-base mud volume in jar, unit are milliliter (mL).
Example, in order to obtain full scale reading, in the oil base drilling fluid that initial volume is 200mL, 150mL oil should be added Base mud flush liquid system, it as a result should be reported as 43% (150mL divided by 350mL).
(3) after the completion of testing, jar is rinsed, and observe whether wall of cup has residual oil film.Water is instilled to final oil base The mixed liquor surface of mud/oil-based mud flushing liquor system, observation experiment phenomenon, if water droplet quickly sinks to disperseing, illustrate mixed Conjunction liquid is water wetting state, if water droplet is at random to be dispersed in surface, it is glossy wet condition to illustrate mixed liquor.
Test result is see Fig. 3-4.From figure 3, it can be seen that oil-based mud flushing liquor prepared by the embodiment of the present application 1 can Make oil-base mud invert completely required oil-based mud flushing liquor system volume fraction be 64.91%.From fig. 4, it can be seen that Mixed liquor after flushing is water wetting state.
For qualified oil-based mud flushing liquor system, oil-base mud is inverted required oil-base mud completely and rinse The volume fraction of liquid system answers≤75%.
Embodiment 7
Oil-based mud flushing liquor prepared by the present embodiment evaluation embodiment 1 is compatible with the rheology of oil-base mud or cement mortar Property, evaluation method is as follows:
At (1) 200 DEG C by oil-based mud flushing liquor system in ageing can aging 4h, pour out after cooling and conserved at 90 DEG C Rheological compatibility test is carried out after 20min.
(2) tested by GB/T 19139-2012 " oil-well cement test method " at 90 DEG C, and calculate R values.
The definition of R values is in the application:Different proportion mixed liquor (oil-base mud/oil-based mud flushing liquor system or cement Slurry/oil-based mud flushing liquor system) 300 turns of tidal stream become reading subtract pure liquid (oil-based mud flushing liquor system, oil-base mud or cement Slurry) in 300 turns of tidal stream become larger one group of reading numerical value.If R≤0, represent that compatibility is very good;If 0 < R < 40, represent slight It is incompatible;If 40≤R < 70, represent incompatible;If R >=70, represent extremely incompatible.
Rheological compatibility evaluation result is respectively as shown in table 1, table 2.
The rheological compatibility of the oil-based mud flushing liquor system of table 1 and oil-base mud
The rheological compatibility of the oil-based mud flushing liquor system of table 2 and cement mortar
Oil-based mud flushing liquor and cement mortar, the rheological compatibility data R < 0 of oil-base mud are can be seen that from table 1-2, Illustrate that compatibility is very good.
Embodiment 8
At 25 DEG C, with reference to the flushing effect of the oil-based mud flushing liquor of the embodiment 5-7 method evaluation preparation of embodiment 1 Fruit, water wettability and with oil-base mud, the rheological compatibility of cement mortar.
(1) developing result is evaluated
Evaluation result is see Fig. 5-6.
From Fig. 5-6 as can be seen that the oil-base mud that oil-based mud flushing liquor prepared by the embodiment of the present application 1 is prepared rinses Liquid system has good developing result at 25 DEG C, and the interface after flushing soaks for water, and developing result is qualified.
(2) water wettability is evaluated
Evaluation result is see Fig. 7-8.
From figure 7 it can be seen that oil-based mud flushing liquor prepared by the embodiment of the present application 1 can be such that oil-base mud inverts completely The volume fraction of required oil-based mud flushing liquor system is 61.54%.From figure 8, it is seen that the mixed liquor after rinsing is water Wetting state.
(3) rheological compatibility is evaluated
Evaluation result is see table 3-4.
The rheological compatibility of the oil-based mud flushing liquor system of table 3 and oil-base mud
The rheological compatibility of the oil-based mud flushing liquor system of table 4 and cement mortar
It is can be seen that from table 3-4 at 25 DEG C, oil-based mud flushing liquor and cement mortar, the rheological compatibility of oil-base mud It is all very good.
Embodiment 9
The present embodiment investigates influence of the dosage of polymer to developing result.
By taking WZ6-9-A platform oil-base mud as an example, influence of the dosage of Study Polymer Melts to developing result at 70 DEG C.Press It is formulated " oil-based mud flushing liquor+137g barites of 300g fresh water+105g embodiments 1 " and prepares oil-based mud flushing liquor system.
From fig. 9, it can be seen that increase to 3 weight % from 0 weight % with the dosage of polymer in oil-based mud flushing liquor, The developing result of oil-based mud flushing liquor is become better and better, but after the dosage of polymer reaches 2 weight %, the use of polymer Measure the influence unobvious to developing result.
Embodiment 10
Oil-based mud flushing liquor prepared by the present embodiment evaluation embodiment 1 is to cement slurry thickening time and the shadow of compression strength Ring, test and carried out according to GB/T 19139-2012 " oil-well cement test method ".
Test result is see table 5.
Table 5
Test condition:120℃@60min@60Mpa
As can be seen from Table 5, the oil-based mud flushing liquor that the oil-based mud flushing liquor that prepared by the embodiment of the present application 1 is prepared For system to thickening time of cement mortar without being obviously prolonged or shortening acts on, the influence to intensity also complies with requirement.
Although the embodiment disclosed by the application is as above, described content is only to readily appreciate the application and use Embodiment, it is not limited to the application.Technical staff in any the application art, is taken off not departing from the application On the premise of the spirit and scope of dew, any modification and change, but the application can be carried out in the form and details of implementation Scope of patent protection, still should be subject to the scope of the claims as defined in the appended claims.

Claims (12)

1. a kind of well cementation oil-based mud flushing liquor, the flushing liquor include solvent, nonionic surfactant, amphion table Face activating agent, polymer and water, wherein, the polymer by selected from N,N-DMAA, acrylic acid, propylene be fine, 2- A kind of or more kinds of monomer in acrylamide-2-methyl propane sulfonic, acrylamide is polymerized.
2. well cementation oil-based mud flushing liquor according to claim 1, wherein, the solvent is selected from hydrocarbon-type oil, oleic acid, ketone Two kinds in class, C6~C7 alkane, benzene class, alcohols, turpentine oil and ethers;
Alternatively,
Flash-point >=60 DEG C of the hydrocarbon-type oil;
The ketone is selected from acetone, ring ethyl ketone;
C6~C7 alkane is selected from hexamethylene, n-hexane, isohexane, heptane;
The benzene class is selected from toluene, dimethylbenzene;
The alcohols is selected from isopropanol, butanol, amylalcohol;
The ethers is selected from ethylene glycol monobutyl ether, diethylene glycol monobutyl ether.
3. well cementation oil-based mud flushing liquor according to claim 1, wherein, the nonionic surfactant is selected from fat Fat alcohol APEO, fatty alcohol polyoxyalkyl ether, aliphatic acid polyethenoxy fat, APES, castor oil polyoxy One or more in vinethene, aliphatic amine polyoxyethylene ether, polyethers;
Alternatively,
The molecular formula of the AEO is RO (CH2CH2O)nH, wherein n=4~9, R C8~C18Alkyl;
The molecular formula of the fatty alcohol polyoxyalkyl ether is RO (CH2CH2O)n(CH2CH2CH2O)mH, wherein n=1~9, m=1~ 9, R C8~C18Alkyl;
The molecular formula of the aliphatic acid polyethenoxy fat is RCOO (CH2CH2O)nH, wherein n=4~9, R C8~C18Alkyl;
The molecular formula of the APES is RCO (CH2CH2O)nH, wherein n=5~10, R C12~C18Alkyl;
The castor oil polyoxyethylene ether is EL-n, wherein n=10~130;
The molecular formula of the aliphatic amine polyoxyethylene ether is RN [(CH2CH2O)nH]2, wherein n=1~15, R C8~C18Alkyl;
The molecular formula of the polyethers is HO (C2H4O)m(C3H6O)nH, wherein m=1~30, n=1~30.
4. well cementation oil-based mud flushing liquor according to claim 1, wherein, the zwitterionic surfactant is sweet tea Dish alkaline zwitterionic surfactant;Alternatively, the zwitterionic surfactant is selected from carboxylic acid glycine betaine, sulfobetaines One or both of alkali;Alternatively, the molecular formula of the carboxylic acid glycine betaine is RN+(CH3)2(CH2)mCOO-, wherein m=1~ 3, R C8~C18Alkyl;The molecular formula of the sulfobetaines is RN+(CH3)2(CH2)mSO3 -, wherein m=1~3, R C8~ C18Alkyl.
5. well cementation oil-based mud flushing liquor according to claim 1, wherein, the polymer passes through following method systems It is standby:
N will be selected from, N- DMAAs, acrylic acid, propylene are fine, in 2- acrylamide-2-methyl propane sulfonics, acrylamide A kind of or more kinds of monomer to be adjusted to concentration with water be 40wt%;40 DEG C~60 DEG C are warming up to, adds initiator, reducing agent Polymerisation is carried out with chain-transferring agent;Dry, crush after completion of the reaction;
Alternatively,
The monomer is N,N-DMAA, 2- acrylamide-2-methyl propane sulfonics and acrylamide, and N, N- bis- The weight ratio of Methacrylamide, 2- acrylamide-2-methyl propane sulfonics and acrylamide is (10~30):(40~80):(10 ~30);
The initiator is (NH4)2S2O8
The reducing agent is NaHSO3
The chain-transferring agent is HCOONa;
The viscosity average molecular weigh of the polymer is below 100,000.
6. the well cementation oil-based mud flushing liquor according to any one of claim 1-5, wherein, with the well cementation oil base The weight of mud fluid is 100% meter, and the content of the solvent is 60%~80%, and the nonionic surfactant contains The content measured as 10%~25%, the zwitterionic surfactant is 1%-5%, the content of the polymer be 1%~ 3%, the content of the water is 7%~10%.
7. a kind of method for preparing the well cementation oil-based mud flushing liquor according to any one of claim 1-6, the side Method includes:
Dissolve a polymer in water;
Nonionic surfactant and zwitterionic surfactant are dissolved in solvent;
The aqueous solution containing polymer is added in the solvent dissolved with surfactant, stirred.
8. a kind of method of evaluating cementing oil-based mud flushing liquor, methods described includes comprehensive well cementation oil-based mud flushing liquor Developing result, water wettability to oil-base mud, three evaluation indexes judgements of compatibility to oil-base mud and cement mortar are solid The performance of well oil-based mud flushing liquor.
9. according to the method for claim 8, wherein, the borehole wall is simulated with sand paper, using by well cementation oil-based mud flushing liquor The flushing liquor system of preparation reflects the flushing liquor system to adhesion to the developing result for the oil-base mud being adhered on sand paper The developing result of oil-base mud on the borehole wall;
Alternatively,
Using the water wettability of electrical conductivity method test well cementation oil-based mud flushing liquor;
Well cementation oil-based mud flushing liquor is tested to oil-base mud and cement mortar according to method specified in GB/T 19139-2012 Compatibility;
The oil-base mud is the oil-base mud after live shaft bottom is circulated;
The well cementation is that well cementation according to any one of claim 1-7 is rinsed with oil-base mud with oil-based mud flushing liquor Liquid.
10. according to the method for claim 9, wherein, utilize the flushing liquid prepared by cementing the well with oil-based mud flushing liquor The developing result of oil-base mud of the system to being adhered on sand paper comprises the steps:
Fritter sand paper is fixed on rotation viscometer outer barrel;
The rotation viscometer outer barrel is immersed in oil-base mud, the oil-base mud is flooded the lower part of the sand paper, mould Intend wall building;
The rotation viscometer outer barrel is taken out from oil-base mud, is put into the flushing prepared by cementing the well with oil-based mud flushing liquor In liquid system, the flushing liquor system is set to flood the lower part of the sand paper, simulation flushing liquor rinses the process of the borehole wall, and observation is simultaneously Record experimental phenomena;
After flushing terminates, sand paper is removed into tiling on the table, the wettability of rinsing area, contaminated area is tested with water droplet.
11. according to the method for claim 10, wherein, the oil-base mud is set to flood lower 2/3 part of the sand paper;Make The flushing liquor system floods lower 1/3 part of the sand paper;
Alternatively,
The rotating speed of rotation viscometer is 600r/min when simulating wall building, and the time for simulating wall building is 10min;
The rotating speed for simulating rotation viscometer when flushing liquor rinses the borehole wall is 200r/min, and the time for simulating flushing is 5min.
12. according to the method for claim 8, wherein, developing result, water wettability and with oil-base mud and cement mortar The qualified flushing liquor system of three indexs of rheological compatibility is qualified products, wherein, the qualified evaluation criterion of developing result is More than 90% oil-base mud can be rinsed out, and flushing interface is changed into water wetting, the qualified evaluation criterion of water wettability It is volume fraction≤75% for making oil-base mud invert required oil-based mud flushing liquor system completely, the rheology phase with cement mortar The qualified evaluation criterion of capacitive is R≤0, and qualified evaluation criterion is R≤0 with the rheological compatibility of oil-base mud.
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CN112834626A (en) * 2019-11-22 2021-05-25 中国海洋石油集团有限公司 Method for measuring pollution degree of oil-based mud in crude oil
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CN108975646A (en) * 2018-09-11 2018-12-11 浙江奇彩环境科技股份有限公司 A kind of greasy filth demulsifier and its preparation method and application
CN109337661B (en) * 2018-11-19 2022-12-06 安东石油技术(集团)有限公司 Low-foam oil displacement type flushing agent and preparation method and application thereof
CN109337661A (en) * 2018-11-19 2019-02-15 安东石油技术(集团)有限公司 Low bubble displacement of reservoir oil type irrigation of one kind and its preparation method and application
CN109652044A (en) * 2019-01-02 2019-04-19 中国石油集团川庆钻探工程有限公司工程技术研究院 A kind of compound Cementing system and its purging method
CN110484221A (en) * 2019-09-16 2019-11-22 中国石油集团西部钻探工程有限公司 Consolidate well oil-base mud insulating liquid and preparation method thereof
CN112834626A (en) * 2019-11-22 2021-05-25 中国海洋石油集团有限公司 Method for measuring pollution degree of oil-based mud in crude oil
CN112834626B (en) * 2019-11-22 2022-08-02 中国海洋石油集团有限公司 Method for measuring pollution degree of oil-based mud in crude oil
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CN116064017A (en) * 2022-11-30 2023-05-05 中国石油天然气集团有限公司 Oil displacement flushing fluid and preparation method and application thereof
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