CN116854868A - Ultra-high temperature-resistant and brine-resistant fluid loss additive for drilling fluid and preparation method thereof - Google Patents
Ultra-high temperature-resistant and brine-resistant fluid loss additive for drilling fluid and preparation method thereof Download PDFInfo
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- 239000012267 brine Substances 0.000 title claims abstract description 72
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 72
- 238000005553 drilling Methods 0.000 title claims abstract description 29
- 239000012530 fluid Substances 0.000 title claims abstract description 19
- 239000000654 additive Substances 0.000 title claims description 53
- 230000000996 additive effect Effects 0.000 title claims description 51
- 238000002360 preparation method Methods 0.000 title claims description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 114
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 104
- 239000000178 monomer Substances 0.000 claims description 84
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 52
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 24
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 23
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 14
- 125000000217 alkyl group Chemical group 0.000 claims description 13
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000003999 initiator Substances 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000010526 radical polymerization reaction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 abstract description 17
- 230000000694 effects Effects 0.000 abstract description 15
- 238000010276 construction Methods 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 description 119
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 74
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 67
- 229910052757 nitrogen Inorganic materials 0.000 description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 33
- 239000011780 sodium chloride Substances 0.000 description 33
- 239000013505 freshwater Substances 0.000 description 32
- 238000012360 testing method Methods 0.000 description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 18
- 229920000642 polymer Polymers 0.000 description 17
- 230000032683 aging Effects 0.000 description 15
- 239000012065 filter cake Substances 0.000 description 15
- 239000002245 particle Substances 0.000 description 14
- 239000000203 mixture Substances 0.000 description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 description 10
- WHNPOQXWAMXPTA-UHFFFAOYSA-N 3-methylbut-2-enamide Chemical compound CC(C)=CC(N)=O WHNPOQXWAMXPTA-UHFFFAOYSA-N 0.000 description 9
- 238000000746 purification Methods 0.000 description 9
- XCEHVMVAFZVMOI-UHFFFAOYSA-N 2-methyl-3-(prop-2-enoylamino)butane-2-sulfonic acid Chemical compound OS(=O)(=O)C(C)(C)C(C)NC(=O)C=C XCEHVMVAFZVMOI-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000000518 rheometry Methods 0.000 description 7
- 239000004927 clay Substances 0.000 description 5
- 230000036571 hydration Effects 0.000 description 5
- 238000006703 hydration reaction Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000008186 active pharmaceutical agent Substances 0.000 description 4
- 238000005098 hot rolling Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000000440 bentonite Substances 0.000 description 3
- 229910000278 bentonite Inorganic materials 0.000 description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- DBMBAVFODTXIDN-UHFFFAOYSA-N 2-methylbutane-2-sulfonic acid Chemical compound CCC(C)(C)S(O)(=O)=O DBMBAVFODTXIDN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- CHDKQNHKDMEASZ-UHFFFAOYSA-N n-prop-2-enoylprop-2-enamide Chemical compound C=CC(=O)NC(=O)C=C CHDKQNHKDMEASZ-UHFFFAOYSA-N 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- -1 -CH 3 Chemical compound 0.000 description 1
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- NZQQFMVULBBDSP-FPLPWBNLSA-N bis(4-methylpentan-2-yl) (z)-but-2-enedioate Chemical compound CC(C)CC(C)OC(=O)\C=C/C(=O)OC(C)CC(C)C NZQQFMVULBBDSP-FPLPWBNLSA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010850 salt effect Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/06—Clay-free compositions
- C09K8/12—Clay-free compositions containing synthetic organic macromolecular compounds or their precursors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses an ultra-high temperature resistant brine-based drilling fluid filtrate reducer, the structural formula of which is shown as formula 1, the filtrate reducer can resist ultra-high temperature of 260 ℃, has excellent salt resistance effect in a high-temperature environment of 230 ℃, and can well meet the requirements of high-temperature construction.
Description
Technical Field
The invention relates to the technical field of petroleum drilling engineering, in particular to an ultra-high temperature resistant and brine-resistant base drilling fluid filtrate reducer and a preparation method thereof.
Background
The drilling fluid has excellent performances of bearing and suspending rock debris, cooling and lubricating a drill bit, stabilizing a well wall, controlling the underground pressure, transmitting hydrodynamic force and the like, and is known as 'blood' of drilling. As drilling depths increase and bottom hole temperatures increase, water-based drilling fluids present significant challenges in high temperature, high salt environments. Under the drilling condition, the rheological property, viscosity, stability and the like of the water-based drilling fluid are changed, the fluid loss is increased to different degrees, and the drilling efficiency and the safety are seriously affected. Therefore, how to effectively control the fluid loss of the water-based drilling fluid and ensure the stability and the safety of the well wall is a problem that the drilling industry must be studied deeply.
The filtrate reducer is used as one of the indispensable treatment agents in the drilling process, and can be adsorbed on the surfaces of bentonite particles through physical actions such as hydrogen bonds, electrostatic force and the like to form a bentonite-polymer-water layered structure, so that the filtrate reducer has important significance on rheological property and filtrate performance of drilling fluid.
However, the existing filtrate reducer can not well meet the requirement of high-temperature construction, and at present, two main problems exist: 1. the high temperature resistance is poor, the existing filtrate reducer can only resist 240 ℃ high temperature at the highest, and when facing to severe environments with ultra-high temperature above 260 ℃, the polymer filtrate reducer is easy to degrade, flocculate or desorb, the protection capability of clay particles is weakened, the rheological property, stability and other properties of drilling fluid are out of control, and the treating agent fails to play the role. 2. Most filtrate reducers can resist high temperature, but cannot achieve the effect of resisting salt at high temperature (T >220 ℃).
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides an ultra-high temperature resistant and brine-based drilling fluid filtrate reducer and a preparation method thereof, which can resist ultra-high temperature of 260 ℃ and also has an anti-salt effect in a high-temperature environment of 230 ℃.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
in a first aspect, the invention provides an ultra-high temperature resistant and brine resistant drilling fluid filtrate reducer, wherein the structural formula of the filtrate reducer is shown as formula 1:
wherein v, w, x, y, z is a natural number;
the R is 1 And R is 2 Is hydrogen or alkyl; and R3, R4, R5, R6 and R7 are alkyl.
Preferably, the molecular weight of the filtrate reducer is 30-300 ten thousand.
Preferably, the filtrate reducer is prepared by taking five monomers of the following formulas 2,3, 4, 5 and 6 as raw materials and carrying out free radical polymerization:
r1 and R2 are hydrogen or alkyl; and R3, R4, R5, R6 and R7 are alkyl.
Preferably, the monomer of formula 2: monomers of formula 3: monomers of formula 4: monomers of formula 5: the mass ratio of the monomer of the formula 6 is (6-9): (1-4): (3-4): (2-3): (0.1-0.5).
In a second aspect, the invention provides a method for preparing the fluid loss additive, comprising the following steps:
s1, after dissolving the monomer of the formula 3 in a solvent, regulating the pH value to be neutral;
s2, adding monomers shown in formulas 2, 4, 5 and 6 into the solution obtained in the step S1, and stirring and dissolving;
and S3, adding an initiator into the solution obtained in the step S2 in an oxygen-free environment for reaction, purifying and drying the reacted substance to obtain the catalyst.
Preferably, in S1, the mass ratio of the monomer of formula 3 to the solvent is 1: (10-50).
Preferably, in S2, the monomer of formula 2: monomers of formula 3: monomers of formula 4: monomers of formula 5: the mass ratio of the monomer of the formula 6 is (6-9): (1-4): (3-4): (2-3): (0.1-0.5).
Preferably, in the step S3, the reaction temperature is 70-90 ℃ and the reaction time is 5-8 h.
Preferably, in S3, the initiator is selected from one or more of ammonium persulfate, sodium bisulphite and potassium persulfate.
Preferably, the initiator is ammonium persulfate and sodium bisulphite, the total mass of the ammonium persulfate and the sodium bisulphite accounts for 0.3-0.4% of the total monomer mass, and the mass ratio of the ammonium persulfate to the sodium bisulphite is 2:1.
Preferably, the drying is such that the total content of purified solvent and solvent as described in S1 is less than 5%.
The beneficial effects of the invention are as follows:
the filtrate reducer can resist ultra-high temperature of 260 ℃, has excellent salt resistance effect in a high-temperature environment of 230 ℃, and can well meet the requirement of high-temperature construction.
The filtrate reducer is mainly prepared by free polymerization of 5 monomers, wherein the monomer of the formula 2 contains amide groups, is an adsorption group, can improve the adsorption capacity of a polymer, the monomer of the formula 3 contains sulfonic groups, is a hydration group, can improve the hydration capacity of the polymer, the monomer of the formula 4 is a cationic monomer, can reduce electrostatic repulsion on the surfaces of clay particles, reduce Zeta potential, can improve the viscosity of drilling fluid, the monomer of the formula 5 has a benzene ring structure, can improve the temperature resistance and salt resistance of the polymer, the monomer of the formula 6 is silica modified by KH570, can improve the overall suspension stability and thermal stability, and the addition of KH-570 also introduces an organosilicon group into a side chain, so that the temperature resistance and salt resistance of the polymer are further improved, and the filtrate reducer can provide technical support for further drilling deep wells and ultra-deep wells in a water-based drilling fluid system.
Drawings
FIG. 1 is an infrared spectrum of the filtrate reducer obtained in example 8;
FIG. 2 is a graph of filter cakes (examples 1,2,3 in order from left to right) of examples 1-3 after aging at 260℃for 16 hours;
FIG. 3 is a graph of filter cakes (examples 1,2,3 in order from left to right) of examples 1-3 after aging for 16 hours at 220℃with 5% NaCl;
FIG. 4 is a graph of filter cakes (examples 4, 5, 6, 7, 8) of examples 4-8 after aging for 16h at 220℃with 5% NaCl, in order from left to right;
FIG. 5 is a HTHP cake plot of example 3 (HTHP cake plot aged at 260℃on the left, HTHP cake plot aged at 220℃5% NaCl on the right);
FIG. 6 is a graph of filter cakes of example 8 under different salinity conditions at different temperatures (220 ℃ C., 10% NaCl for 16h in the middle, 220 ℃ C., 15% NaCl for 16h, 230 ℃ C., 5% NaCl for 16 h).
Detailed Description
The present invention will be described in further detail with reference to specific embodiments thereof in order to enable those skilled in the art to better understand the technical aspects of the invention.
In order to enable the filtrate reducer to resist ultra-high temperature of 260 ℃ and also have salt resistance effect in a high-temperature environment of 230 ℃, the invention firstly provides the ultra-high temperature resistant brine-based drilling fluid filtrate reducer, and the structural formula of the filtrate reducer is shown as formula 1:
wherein v, w, x, y, z is a natural number;
the R is 1 And R is 2 Is hydrogen or alkyl, e.g. -CH 3 、(-CH 2 -) n Wherein n is 1,2,3, … and other natural numbers;
the R3, R4, R5, R6 and R7 groups are alkyl groups, such as-CH 3 、(-CH 2 -) n Wherein n is a natural number such as 1,2,3 or ….
Preferably, the molecular weight of the filtrate reducer is 80-300 ten thousand.
Preferably, the filtrate reducer is prepared by taking five monomers of the following formulas 2,3, 4, 5 and 6 as raw materials and carrying out free radical polymerization:
r1 and R2 are hydrogen or alkyl, and the alkyl is such as-CH 3, (-CH 2-) n, wherein n is 1,2,3 … and other natural numbers;
r3, R4, R5, R6 and R7 are alkyl groups, such as-CH 3, (-CH 2-) n, wherein n is a natural number such as 1,2,3 …, etc.
The above substituents can achieve the effects of the invention, and the embodiment of the invention only selects one monomer form of five compounds, and the invention is not limited by the embodiment, and other limited substituents can achieve the same technical effects.
Preferably, the monomer of formula 2: monomers of formula 3: monomers of formula 4: monomers of formula 5: the mass ratio of the monomer of the formula 6 is (6-9): (1-4): (3-4): (2-3): (0.1-0.5).
The invention aims to synthesize an ultrahigh temperature-resistant and brine-resistant drilling fluid filtrate reducer, wherein a monomer of a formula 2 contains amide groups, is an adsorption group, can improve the adsorption capacity of a polymer, a monomer of a formula 3 contains sulfonic groups, is a hydration group, can improve the hydration capacity of the polymer, a monomer of a formula 4 is a cationic monomer, can be adsorbed on the surface of clay through electrostatic action, neutralizes negative charges on the surface of clay particles, thereby reducing electrostatic repulsion on the surface of the clay particles, reducing Zeta potential, enhancing the viscosity of the drilling fluid, and has a benzene ring structure, can improve the rigidity and steric hindrance effect of a molecular chain, thereby improving the temperature-resistant and salt-resistant performance of the polymer, and a monomer of a formula 6 is silica modified by KH570, has good dispersibility, improved hydrophobicity, has small particle size, large specific surface area, dominant surface force, van der Waals force and molecular force, is favorable for interaction between nano particles or between nano particles and a medium, has the obtained characteristics, and can improve the overall suspension stability and thermal stability. In addition, the side chain of the filtrate reducer is introduced with an adsorption group, a hydration group and a rigid group, and the addition of KH-570 also introduces an organosilicon group into the side chain, so that the temperature resistance and salt resistance of the polymer are further improved, and technical support can be provided for further drilling deep wells and ultra-deep wells of a water-based drilling fluid system.
In a second aspect, the invention provides a method for preparing the fluid loss additive, comprising the following steps:
s1, after dissolving the monomer of the formula 3 in a solvent, regulating the pH value to be neutral;
s2, adding monomers shown in formulas 2, 4, 5 and 6 into the solution obtained in the step S1, and stirring and dissolving;
and S3, adding an initiator into the solution obtained in the step S2 in an oxygen-free environment for reaction, purifying and drying the reacted substance to obtain the catalyst.
In the S1, the mass ratio of the monomer of the formula 3 to the solvent is 1: (10-50). The solvent may be any solvent capable of dissolving the 5 monomers of the present invention. In some embodiments of the invention, the solvent is water. Illustratively, the mass ratio of monomer of formula 3 to solvent is a value between any one or both of 1:10, 1:17, 1:46.
The pH value regulating agent provided by the invention is a reagent which is conventional in the art and can regulate the pH value. In an embodiment of the invention, the pH adjustor is sodium hydroxide solution.
In the S2 of the present invention, the monomer of formula 2: monomers of formula 3: monomers of formula 4: monomers of formula 5: the mass ratio of the monomer of the formula 6 is (6-9): (1-4): (3-4): (2-3): (0.1-0.5). In some embodiments of the invention, the monomer of formula 2: monomers of formula 3: monomers of formula 4: monomers of formula 5: the mass ratio of the monomer of the formula 6 is (6.4-8.6): (1.45-4): (3.5-3.9): (2.7-3) (0.17-0.45).
In some embodiments of the present invention, the anaerobic environment is specifically: nitrogen is introduced to drive oxygen so as to maintain an anaerobic environment.
In the S3, the reaction temperature is 70-90 ℃ and the reaction time is 5-8 h.
In the S3 of the invention, the initiator is one or more selected from ammonium persulfate, sodium bisulphite and potassium persulfate. In some embodiments of the invention, the initiator is ammonium persulfate and sodium bisulfite. The solubility of ammonium persulfate in water is greater than that of potassium persulfate, the initiation efficiency is high, and the cost of ammonium persulfate is lower than that of potassium persulfate, and although the ammonium persulfate can be independently used as an initiator, the ammonium persulfate can form a redox system after being combined with sodium bisulphite to be used for polymerization, so that the activation energy of free radical generation reaction can be reduced, and the polymerization rate can be improved. Wherein the total mass of the ammonium persulfate and the sodium bisulphite accounts for 0.3-0.4% of the total monomer mass, and the mass ratio of the ammonium persulfate to the sodium bisulphite is 2:1.
The purification according to the invention may be carried out using an acetone solution.
The drying according to the invention is such that the total content of purified solvent and solvent as described in S1 is less than 5%.
The foregoing is a detailed description of the invention and the following examples of the invention.
The starting materials used in the examples:
pure water (made by laboratory), N-N dimethylacrylamide (from damas-beta), diacrylamide-based dimethylpropanesulfonic acid (from Allatin), dimethyldiallylammonium chloride (from Allatin), sodium p-styrenesulfonate (from damas-beta), KH570 modified SiO 2 Analytically pure (from exploration platform), sodium hydroxide (from GENERAL-regent company), ammonium persulfate (from damas-beta company), sodium bisulphite (from adzuki company).
Example 1
The structural formulas of the five reaction monomers are respectively as follows:
the preparation method of the filtrate reducer comprises the following steps:
into a three-necked flask equipped with a stirrer, a thermometer and a heating device, 73.164g of pure water and 3g of 2-acrylamido-dimethylpropanesulfonic acid were sequentially added, the pH was adjusted to 7.0 with 0.58g of NaOH, and 7.902g N-N dimethylacrylamide, 2.988g of sodium p-styrenesulfonate, 3.9014g of dimethyldiallylammonium chloride and 0.45g of KH570-modified SiO were further added 2 Stirring until all monomers are dissolved, introducing nitrogen to drive oxygen for 30min, then continuously introducing nitrogen while heating, adding 0.03768g ammonium persulfate and 0.01719g sodium bisulfite when the temperature is raised to 90 ℃, continuously introducing nitrogen for half an hour, and stopping introducing nitrogen; the reaction lasts for 8 hours, after 8 hours, the polymer is poured into acetone solution for purification, sheared and granulated, and then is put into a 60 ℃ oven for drying, and white particles are obtained after drying, namely the filtrate reducer A.
Example 2
The structural formula of the five reaction monomers is the same as that of example 1.
The preparation method of the filtrate reducer comprises the following steps:
into a three-necked flask equipped with a stirrer, a thermometer and a heating device, 69.689g of pure water and 1.5g of 2-acrylamido-dimethylpropanesulfonic acid were sequentially added, the pH was adjusted to 7.0 with 0.3g of NaOH, and 8.620g N-N dimethylacrylamide, 2.988g of sodium p-styrenesulfonate, 3.901g of dimethyldiallylammonium chloride and 0.43g of KH570-modified SiO were further added 2 Stirring until all monomers are dissolved, introducing nitrogen to drive oxygen for 30min, then continuously introducing nitrogen while heating, adding 0.03589g ammonium persulfate and 0.01637g sodium bisulfite when the temperature is raised to 90 ℃, continuously introducing nitrogen for half an hour, and stopping introducing nitrogen; the reaction lasts for 8 hours, after 8 hours, the polymer is poured into acetone solution for purification, sheared and granulated, and then is put into a 60 ℃ oven for drying, and white particles are obtained after drying, namely the filtrate reducer B.
Example 3
The structural formula of the five reaction monomers is the same as that of example 1.
The preparation method of the filtrate reducer comprises the following steps:
into a three-necked flask equipped with a stirrer, a thermometer and a heating device, 67.636g of pure water and 4g of 2-acrylamido-dimethylpropanesulfonic acid were sequentially added, the pH was adjusted to 7.0 with 0.78g of NaOH, and 6.385g N-N dimethylacrylamide, 2.656g of sodium p-styrenesulfonate, 3.468g of dimethyldiallylammonium chloride and 0.41g of KH570-modified SiO were further added 2 Stirring until all monomers are dissolved, introducing nitrogen to drive oxygen for 30min, then continuously introducing nitrogen while heating, adding 0.03484g ammonium persulfate and 0.01589g sodium bisulfite when the temperature is raised to 90 ℃, continuously introducing nitrogen for half an hour, and stopping introducing nitrogen; the reaction lasts for 8 hours, after 8 hours, the polymer is poured into acetone solution for purification, sheared and granulated, and then is put into a 60 ℃ oven for drying, and white particles are obtained after drying, namely the filtrate reducer C.
Example 4
The structural formula of the five reaction monomers is the same as that of example 1.
The preparation method of the filtrate reducer comprises the following steps:
into a three-necked flask equipped with a stirrer, a thermometer and a heating device, 66.44g of pure water and 1.45g of 2-acrylamido-dimethylpropanesulfonic acid were sequentially added, the pH was adjusted to 7 with 0.282g of NaOH, and 8.333 and g N-N dimethylacrylamide, 2.889g of sodium p-styrenesulfonate, 3.771g of dimethyldiallylammonium chloride and 0.167g of KH570 modified SiO were further added 2 Stirring until all monomers are dissolved, introducing nitrogen to drive oxygen for 30min, then continuously introducing nitrogen while heating, adding 0.03422g ammonium persulfate and 0.01561g sodium bisulfite when the temperature is raised to 70 ℃, continuously introducing nitrogen for half an hour, and stopping introducing nitrogen; the reaction lasts for 5 hours, after 5 hours, the polymer is poured into acetone solution for purification, sheared and granulated, and then is put into a 60 ℃ oven for drying, and white particles are obtained after drying, namely the filtrate reducer D.
Example 5
The structural formula of the five reaction monomers is the same as that of example 1.
The preparation method of the filtrate reducer comprises the following steps:
66.4 parts of a three-necked flask equipped with a stirrer, a thermometer and a heating device were successively charged in the flask4g of pure water and 1.45g of 2-acrylamido-dimethylpropanesulfonic acid, adjusting the pH to 7 with 0.282g of NaOH, adding 8.333g N-N dimethylacrylamide, 2.889g of sodium p-styrenesulfonate, 3.771g of dimethyl diallyl ammonium chloride, 0.167g of KH570 modified SiO 2 Stirring until all monomers are dissolved, introducing nitrogen to drive oxygen for 30min, then continuously introducing nitrogen while heating, adding 0.03422g ammonium persulfate and 0.01561g sodium bisulfite when the temperature is raised to 75 ℃, continuously introducing nitrogen for half an hour, and stopping introducing nitrogen; the reaction lasts for 5 hours, after 5 hours, the polymer is poured into acetone solution for purification, sheared and granulated, and then is put into a 60 ℃ oven for drying, and white particles are obtained after drying, namely the filtrate reducer E.
Example 6
The structural formula of the five reaction monomers is the same as that of example 1.
The preparation method of the filtrate reducer comprises the following steps:
into a three-necked flask equipped with a stirrer, a thermometer and a heating device, 66.44g of pure water and 1.45g of 2-acrylamido-dimethylpropanesulfonic acid were sequentially added, the pH was adjusted to 7 with 0.282g of NaOH, and 8.333 and g N-N dimethylacrylamide, 2.889g of sodium p-styrenesulfonate, 3.771g of dimethyldiallylammonium chloride and 0.167g of KH570 modified SiO were further added 2 Stirring until all monomers are dissolved, introducing nitrogen to drive oxygen for 30min, then continuously introducing nitrogen while heating, adding 0.03422g ammonium persulfate and 0.01561g sodium bisulfite when the temperature is raised to 80 ℃, continuously introducing nitrogen for half an hour, and stopping introducing nitrogen; the reaction lasts for 5 hours, after 5 hours, the polymer is poured into acetone solution for purification, sheared and granulated, and then is put into a 60 ℃ oven for drying, and white particles are obtained after drying, namely the filtrate reducer F.
Example 7
The structural formula of the five reaction monomers is the same as that of example 1.
The preparation method of the filtrate reducer comprises the following steps:
into a three-necked flask equipped with a stirrer, a thermometer and a heating device, 66.44g of pure water and 1.45g of 2-acrylamido-dimethylpropanesulfonic acid were successively added, the pH was adjusted to 7 with 0.282g of NaOH, and 8.333/g N-N-dimethylacrylamide, 2.889g sodium p-styrenesulfonate, 3.771g dimethyl diallyl ammonium chloride, 0.167g KH570 modified SiO 2 Stirring until all monomers are dissolved, introducing nitrogen to drive oxygen for 30min, then continuously introducing nitrogen while heating, adding 0.03422g ammonium persulfate and 0.01561g sodium bisulfite when the temperature is raised to 85 ℃, continuously introducing nitrogen for half an hour, and stopping introducing nitrogen; the reaction lasts for 5 hours, after 5 hours, the polymer is poured into acetone solution for purification, sheared and granulated, and then is put into a 60 ℃ oven for drying, and white particles are obtained after drying, namely the filtrate reducer G.
Example 8
The structural formula of the five reaction monomers is the same as that of example 1.
The preparation method of the filtrate reducer comprises the following steps:
into a three-necked flask equipped with a stirrer, a thermometer and a heating device, 66.44g of pure water and 1.45g of 2-acrylamido-dimethylpropanesulfonic acid were sequentially added, the pH was adjusted to 7 with 0.282g of NaOH, and 8.333 and g N-N dimethylacrylamide, 2.889g of sodium p-styrenesulfonate, 3.771g of dimethyldiallylammonium chloride and 0.167g of KH570 modified SiO were further added 2 Stirring until all monomers are dissolved, introducing nitrogen to drive oxygen for 30min, then continuously introducing nitrogen while heating, adding 0.03422g ammonium persulfate and 0.01561g sodium bisulfite when the temperature is raised to 90 ℃, continuously introducing nitrogen for half an hour, and stopping introducing nitrogen; the reaction lasts for 5 hours, after 5 hours, the polymer is poured into acetone solution for purification, sheared and granulated, and then is put into a 60 ℃ oven for drying, and white particles are obtained after drying, namely the filtrate reducer H.
Comparative example 1
67.63g of pure water and 4g of diacrylamide-based dimethylpropanesulfonic acid were sequentially added to a three-necked flask equipped with a stirrer, a thermometer and a heating device, the pH was adjusted to 7 with 0.78g of NaOH, and 6.385g N-N dimethylacrylamide, 2.656g of sodium p-styrenesulfonate, 3.468g of dimethyldiallylammonium chloride and 0.41g of KH570-modified SiO were further added 2 Stirring until all monomers are dissolved, introducing nitrogen to drive oxygen for 30min, continuously introducing nitrogen and heating until the temperature is raised to 65 ℃, adding 0.03484g of ammonium persulfate and 0.01589g of sodium bisulfite, and nitrogen was continuously introduced thereinto, and after half an hour, the introduction of nitrogen was stopped.
Results: it was found that the reaction monomer could not polymerize at this temperature and the desired filtrate reducer could not be obtained.
Effect example 1 fluid loss additive fresh water slurry Performance test
Preparing fresh water-based slurry: 400g of tap water is added into an enamel cup, 16g of bentonite and 0.8g of sodium carbonate are added under continuous stirring, the mixture is stirred at the speed of 600r/min for 30min, then the mixture is transferred into a high-stirring cup, the mixture is stirred at the speed of 12000r/min for 10min, and the mixture is maintained for 24h at room temperature, so that the dilute water-based slurry is obtained.
The experimental process comprises the following steps: 9 parts of pre-hydrated fresh water-based slurry are taken, 1% of the filtrate reducer prepared in examples 1-8 is added to 8 parts of the fresh water-based slurry under the condition of continuous stirring, and the mixture is stirred uniformly at a high speed and is respectively marked as filtrate reducer A fresh water-based slurry, filtrate reducer B fresh water-based slurry, filtrate reducer C fresh water-based slurry, filtrate reducer D fresh water-based slurry, filtrate reducer E fresh water-based slurry, filtrate reducer F fresh water-based slurry, filtrate reducer G fresh water-based slurry and filtrate reducer H fresh water-based slurry, and fresh water-based slurry without filtrate reducer is used as a control group. The rheology test and the fluid loss test were performed on each of the fresh water-based slurries, respectively, and the results are shown in table 1.
TABLE 1 fluid loss additive fresh water based slurry rheology and fluid loss test table
| Experimental pulp | AV(mPa·s) | PV(mPa.s) | YP(Pa) | FL API (mL) |
| Fresh water-based slurry | 9 | 5 | 4 | 26 |
| Fluid loss additive A dilute water-based slurry | 56 | 48 | 8 | 2.3 |
| Fluid loss additive B dilute water-based slurry | 45.5 | 37 | 8.5 | 1.8 |
| Fluid loss additive C dilute water-based slurry | 28 | 16 | 12 | 1.7 |
| Fluid loss additive D dilute water-based slurry | 18.5 | 15 | 3.5 | 2.4 |
| Fluid loss additive E dilute aqueous slurry | 13.5 | 12 | 1.5 | 2.0 |
| Fluid loss additive F dilute water-based slurry | 23.5 | 18 | 5.5 | 3.2 |
| Fluid loss agent G dilute water-based slurry | 27 | 21 | 6 | 2.8 |
| Fluid loss additive H dilute water-based slurry | 39 | 33 | 6 | 2.6 |
In Table 1, AV is apparent viscosity, PV is plastic viscosity, YP is dynamic shear force, and FLAPI is normal temperature and pressure drilling fluid loss. As can be seen from Table 1, the fluid loss additives prepared in examples 1 to 8 of the present invention have good fluid loss properties.
Effect example 2 fluid loss additive brine-based slurry Performance test
Preparation of brine-based slurry: 400g of tap water is added into an enamel cup, 16g of bentonite, 0.8g of sodium carbonate, 5% of NaCl, 10% of NaCl or 15% of NaCl are added under continuous stirring, the mixture is stirred at 600r/min for 30min, then the mixture is transferred into a high stirring cup, the mixture is stirred at 12000r/min for 10min, and the mixture is maintained for 24h at room temperature, so that 5% of NaCl brine-based slurry, 10% of NaCl brine-based slurry or 15% of NaCl brine-based slurry is obtained.
The experimental process comprises the following steps: 9 parts of pre-hydrated 5% NaCl brine-based slurry are taken, 3% filtrate reducer of examples 1-8 is added to 8 parts of the slurry under the condition of continuous stirring, and the slurry is stirred uniformly at a high speed and is respectively marked as filtrate reducer A brine-based slurry, filtrate reducer B brine-based slurry, filtrate reducer C brine-based slurry, filtrate reducer D brine-based slurry, filtrate reducer E brine-based slurry, filtrate reducer F brine-based slurry, filtrate reducer G brine-based slurry and filtrate reducer H brine-based slurry, and brine-based slurries without filtrate reducer are used as control groups. The rheology test and the fluid loss test were performed on each of the brine-based slurries, respectively, and the results are shown in table 2.
Table 2 fluid loss additive brine-based slurry rheology and fluid loss test table
| Experimental pulp | AV(mPa·s) | PV(mPa.s) | YP(Pa) | FL API (mL) |
| Brine-based slurry | 15 | 10 | 5 | 64 |
| Fluid loss additive A brine-based slurry | 66.5 | 52 | 14.5 | 4.6 |
| Fluid loss additive B brine-based slurry | 43.5 | 36 | 7.5 | 3.6 |
| Fluid loss additive C brine-based slurry | 28 | 18 | 10 | 3.0 |
| Fluid loss additive D brine-based slurry | 67 | 51 | 16 | 5.6 |
| Fluid loss additive E brine-based slurry | 40 | 31 | 11 | 4.4 |
| Fluid loss additive F brine-based slurry | 67.5 | 51 | 16.5 | 6.0 |
| Fluid loss additive G brine-based slurry | 73.5 | 57 | 16.5 | 6.2 |
| Fluid loss additive H salt water-based slurry | 51.5 | 37 | 14.5 | 4.8 |
As can be seen from Table 2, the fluid loss additive brine-based slurries prepared in examples 1-8 of the present invention have good fluid loss properties, indicating that the fluid loss additives prepared in examples have good salt resistance.
Effect example 3 high temperature drop out fluid loss agent fresh water based slurry Performance test
The fresh water-based slurry was prepared as in effect example 1.
The experimental process comprises the following steps: 9 parts of pre-hydrated fresh water base slurry are taken, 1% of filtrate reducer (examples 1-8) by mass fraction is added to 8 parts of fresh water base slurry respectively under the condition of continuous stirring, and the mixture is stirred uniformly at high speed and is marked as filtrate reducer A fresh water base slurry, filtrate reducer B fresh water base slurry, filtrate reducer C fresh water base slurry, filtrate reducer D fresh water base slurry, filtrate reducer E fresh water base slurry, filtrate reducer F fresh water base slurry, filtrate reducer G fresh water base slurry and filtrate reducer H fresh water base slurry, and fresh water base slurry without filtrate reducer is used as a control group. And respectively carrying out a heat rolling aging experiment at 260 ℃ on each dilute water-based slurry, taking out each dilute water-based slurry after the experiment, and carrying out a rheological property test, a filtration loss test and a high-temperature high-pressure test at 180 ℃, wherein the results are shown in Table 3.
TABLE 3 Table for testing rheology and fluid loss of fluid loss additive fresh water based slurry at high temperature
| Experimental pulp | AV(mPa·s) | PV(mPa.s) | YP(Pa) | FL API (mL) | HTHP(mL) |
| Fresh water-based slurry | 21 | 12 | 9 | 61 | 162 |
| Fluid loss additive A dilute water-based slurry | 45 | 37 | 8 | 9.2 | 18 |
| Fluid loss additive B dilute water-based slurry | 38.5 | 29 | 9.5 | 7.2 | 12 |
| Fluid loss additive C dilute water-based slurry | 26 | 11 | 5 | 6.0 | 19 |
| Fluid loss additive D dilute water-based slurry | 38.5 | 31 | 7.5 | 11.2 | 32 |
| Fluid loss additive E dilute aqueous slurry | 42 | 32 | 10 | 13.6 | 36 |
| Fluid loss additive F dilute water-based slurry | 27 | 25 | 2 | 9.6 | 26 |
| Fluid loss agent G dilute water-based slurry | 28.5 | 25 | 3.5 | 7.4 | 27 |
| Fluid loss additive H dilute water-based slurry | 32 | 28 | 4 | 6.8 | 24 |
As shown in Table 3, the filtrate reducer of the embodiment of the invention still has good filtrate reduction performance under the conditions of fresh water base slurry and 260 ℃, which indicates that the filtrate reducer has good temperature resistance.
Effect example 4 high temperature fluid loss additive brine-based slurry Performance test
The brine-based slurry was prepared as in effect example 2.
The experimental process comprises the following steps: 9 parts of pre-hydrated brine-based slurry containing 5% NaCl is taken, 3% filtrate reducer (examples 1-8) is added to 8 parts of the pre-hydrated brine-based slurry under the condition of continuous stirring, and the pre-hydrated brine-based slurry is uniformly stirred at a high speed and is respectively marked as filtrate reducer A brine-based slurry, filtrate reducer B brine-based slurry, filtrate reducer C brine-based slurry, filtrate reducer D brine-based slurry, filtrate reducer E brine-based slurry, filtrate reducer F brine-based slurry, filtrate reducer G brine-based slurry and filtrate reducer H brine-based slurry, and brine-based slurry without filtrate reducer is used as a control group. And respectively carrying out a 220 ℃ hot rolling aging experiment on each brine-based slurry, taking out each brine-based slurry after the experiment, and carrying out a rheological property test, a fluid loss test and a 180 ℃ high-temperature high-pressure test, wherein the results are shown in table 4.
TABLE 4 Table for testing rheology and fluid loss after high temperature of fluid loss additive brine-based slurry
| Experimental pulp | AV(mPa·s) | PV(mPa.s) | YP(Pa) | FL API (mL) | HTHP(mL) |
| Brine-based slurry | 13 | 7.5 | 6.5 | 96 | 186 |
| Fluid loss additive A brine-based slurry | 31.5 | 23 | 8.5 | 5.2 | 21 |
| Fluid loss additive B brine-based slurry | 22.5 | 18 | 4.5 | 5.0 | 17 |
| Fluid loss additive C brine-based slurry | 28 | 20 | 8 | 7.6 | 22 |
| Fluid loss additive D brine-based slurry | 37 | 15 | 22 | 9.6 | 29 |
| Fluid loss additive E brine-based slurry | 32 | 22 | 10 | 10.4 | 34 |
| Fluid loss additive F brine-based slurry | 23 | 18 | 5 | 5.2 | 24 |
| Fluid loss additive G brine-based slurry | 31 | 23 | 8 | 5.8 | 25 |
| Fluid loss additive H salt water-based slurry | 20.5 | 17 | 3.5 | 4.4 | 23 |
As shown in Table 4, the filtrate reducer of the invention still has good filtrate reduction performance under the conditions of 220 ℃ and 5% NaCl, which indicates that the filtrate reducer has good temperature resistance and salt resistance.
Performance test of the fluid loss additive of example 8 at different salinity:
3 parts of pre-hydrated 5% NaCl brine-based slurry, 10% NaCl brine-based slurry and 15% NaCl brine-based slurry are taken, 3% of the filtrate reducer of the example 8 is respectively added under the condition of continuous stirring, and the mixture is stirred uniformly at a high speed and is marked as filtrate reducer H-10% NaCl brine-based slurry, filtrate reducer H-15% NaCl brine-based slurry and filtrate reducer H-5% NaCl brine-based slurry. Respectively carrying out 220 ℃ hot rolling aging experiments on H-10% NaCl brine-based slurry and filtrate reducer H-15% NaCl brine-based slurry, and taking out each brine-based slurry after the experiments to carry out rheological property test, filtrate loss test and 180 ℃ high-temperature high-pressure test; carrying out a hot rolling aging experiment at 230 ℃ on the filtrate reducer H-5% NaCl brine-based slurry, taking out the slurry after the experiment, and carrying out a rheological property test, a filtrate loss test and a high-temperature high-pressure test at 180 ℃; a hot rolling aging test at 230 ℃ was carried out using a brine-based slurry without filtrate reducer as a control, and after the test, the test was taken out to carry out a rheological test, a filtrate loss test and a high-temperature high-pressure test at 180 ℃, and the results of the rheological test and the filtrate loss test are shown in Table 5.
Table 5 fluid loss additive brine-based slurry rheology and fluid loss test table
As shown in Table 5, the filtrate reducer of the invention still has good filtrate reduction performance under the conditions of 220 ℃,10% NaCl,220 ℃,15% NaCl,230 ℃ and 5% NaCl, which proves that the filtrate reducer of the invention has good salt resistance.
Effect example 5 characterization of fluid loss agent by IR spectrum
FIG. 1 is an infrared spectrum of a filtrate reducer obtained in example 8, in which the peak value is 3422cm -1 And 3342cm -1 N-H stretching vibration is respectively corresponding to DMAM and AMPS,2981cm -1 Is a characteristic peak of-CH 3, 1652cm -1 Characteristic absorption peak of c=o, 1404cm -1 For C-H bending vibration in DMDAAC 1224cm -1 And 1045cm -1 For a tensile vibration of s=o in SSS, 769cm -1 Benzene ring flexural vibration at SSS 1186cm -1 ，842cm -1 ，468cm -1 The analysis shows that the filtrate reducer is successfully synthesized as the characteristic absorption peak of Si-O-Si.
Effect example 6 cake pattern of fluid loss additive
Fig. 2 is a graph of filter cakes (examples 1,2 and 3 from left to right) of examples 1 to 3 after aging at 260 ℃ for 16 hours, and it can be seen that filter cakes formed by using the filtrate reducer synthesized from five monomers are compact, have a temperature resistance up to 260 ℃, and have excellent temperature resistance.
FIG. 3 is a graph of filter cakes (examples 1,2,3 in order from left to right) of examples 1-3 after aging for 16 hours at 220℃with 5% NaCl; fig. 4 is a graph of filter cakes (examples 4, 5, 6, 7 and 8 from left to right) of examples 4 to 8 after aging at 220 ℃ for 16 hours with 5% nacl, and it can be seen that the filtrate reducer obtained by the invention can effectively control the filtrate loss after aging at 220 ℃ and the formed filter cakes are thin and compact, thus indicating that the prepared filtrate reducer has excellent salt resistance.
FIG. 5 is a HTHP cake plot of example 3, wherein the left is an HTHP cake plot of example 3 aged at 260℃and the right is an HTHP cake plot aged at 220℃with 5% NaCl. It can be seen that the filter cake formed by HTHP has proper thickness and smooth and uniform surface, can effectively control the filtration loss, and can resist HTHP. Taken together, the prepared filtrate reducer has excellent temperature resistance and salt resistance.
FIG. 6 is a graph of filter cakes of example 8 at different temperatures and different salinity, wherein the left side is a graph of filter cakes after aging for 16 hours at 220 ℃ and 10% NaCl, the middle is a graph of filter cakes after aging for 16 hours at 220 ℃ and 15% NaCl, and the right side is a graph of filter cakes after aging for 16 hours at 230 ℃ and 5% NaCl. It can be seen that the prepared filtrate reducer can form a compact and smooth filter cake on the surface under the conditions of different temperatures and different salts, and has small filtrate loss, and can resist 230 ℃ and 5% NaCl.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (10)
1. The ultra-high temperature resistant and brine resistant drilling fluid filtrate reducer is characterized in that the structural formula of the filtrate reducer is shown as formula 1:
wherein v, w, x, y, z is a natural number;
the R is 1 And R is 2 Is hydrogen or alkyl; and R3, R4, R5, R6 and R7 are alkyl.
2. The fluid loss additive of claim 1, wherein the fluid loss additive has a molecular weight of 30 to 300 tens of thousands.
3. The fluid loss additive according to claim 1, wherein the fluid loss additive is prepared by radical polymerization of five monomers of the following formulas 2,3, 4, 5 and 6:
r1 and R2 are hydrogen or alkyl; and R3, R4, R5, R6 and R7 are alkyl.
4. A fluid loss additive according to claim 3 wherein the monomer of formula 2: monomers of formula 3: monomers of formula 4: monomers of formula 5: the mass ratio of the monomer of the formula 6 is (6-9): (1-4): (3-4): (2-3): (0.1-0.5).
5. A method of preparing the fluid loss additive of claim 3 or 4, comprising the steps of:
s1, after dissolving the monomer of the formula 3 in a solvent, regulating the pH value to be neutral;
s2, adding monomers shown in formulas 2, 4, 5 and 6 into the solution obtained in the step S1, and stirring and dissolving;
and S3, adding an initiator into the solution obtained in the step S2 in an oxygen-free environment for reaction, purifying and drying the reacted substance to obtain the catalyst.
6. The method according to claim 5, wherein in S1, the mass ratio of the monomer of formula 3 to the solvent is 1: (10-50).
7. The method of claim 5, wherein in S2, the monomer of formula 2: monomers of formula 3: monomers of formula 4: monomers of formula 5: the mass ratio of the monomer of the formula 6 is (6-9): (1-4): (3-4): (2-3): (0.1-0.5).
8. The method according to claim 5, wherein in S3, the reaction temperature is 70 to 90℃and the reaction time is 5 to 8 hours.
9. The method according to claim 5, wherein in S3, the initiator is one or more selected from the group consisting of ammonium persulfate, sodium bisulphite and potassium persulfate.
10. The preparation method according to claim 5, wherein the initiator is ammonium persulfate and sodium bisulphite, wherein the total mass of the ammonium persulfate and the sodium bisulphite is 0.3-0.4% of the total monomer mass, and the mass ratio of the ammonium persulfate to the sodium bisulphite is 2:1.
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