CN115873577B - Wettability regulator composition and preparation method and application thereof - Google Patents
Wettability regulator composition and preparation method and application thereof Download PDFInfo
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- CN115873577B CN115873577B CN202110988632.3A CN202110988632A CN115873577B CN 115873577 B CN115873577 B CN 115873577B CN 202110988632 A CN202110988632 A CN 202110988632A CN 115873577 B CN115873577 B CN 115873577B
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- 239000000203 mixture Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 118
- 229920000570 polyether Polymers 0.000 claims abstract description 118
- -1 hydrocarbyl amide Chemical class 0.000 claims abstract description 62
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 42
- 239000002253 acid Substances 0.000 claims abstract description 39
- 150000003839 salts Chemical class 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 125000001183 hydrocarbyl group Chemical group 0.000 claims abstract description 26
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 125000000217 alkyl group Chemical group 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 125000002947 alkylene group Chemical group 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 15
- 239000003513 alkali Substances 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 7
- 150000001768 cations Chemical class 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 4
- 150000001450 anions Chemical group 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 3
- 230000021523 carboxylation Effects 0.000 claims description 3
- 238000006473 carboxylation reaction Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 125000002091 cationic group Chemical group 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 125000000547 substituted alkyl group Chemical group 0.000 claims description 2
- 238000006277 sulfonation reaction Methods 0.000 claims description 2
- 230000035699 permeability Effects 0.000 abstract description 10
- 238000006073 displacement reaction Methods 0.000 abstract description 8
- 238000005213 imbibition Methods 0.000 abstract description 8
- 239000011435 rock Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 229920006395 saturated elastomer Polymers 0.000 abstract description 5
- 239000004094 surface-active agent Substances 0.000 description 27
- 239000003921 oil Substances 0.000 description 25
- 239000007864 aqueous solution Substances 0.000 description 19
- 239000000243 solution Substances 0.000 description 18
- 229910001425 magnesium ion Inorganic materials 0.000 description 17
- 239000002736 nonionic surfactant Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 14
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 13
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 13
- 230000033558 biomineral tissue development Effects 0.000 description 13
- 239000011575 calcium Substances 0.000 description 13
- 229910001424 calcium ion Inorganic materials 0.000 description 13
- 239000010779 crude oil Substances 0.000 description 12
- 238000000502 dialysis Methods 0.000 description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- 230000003068 static effect Effects 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 239000008398 formation water Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000029936 alkylation Effects 0.000 description 2
- 238000005804 alkylation reaction Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000001160 methoxycarbonyl group Chemical group [H]C([H])([H])OC(*)=O 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 description 1
- BVIXLMYIFZGRBH-UHFFFAOYSA-M sodium;2-chloroethanesulfonate Chemical compound [Na+].[O-]S(=O)(=O)CCCl BVIXLMYIFZGRBH-UHFFFAOYSA-M 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A10/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE at coastal zones; at river basins
- Y02A10/40—Controlling or monitoring, e.g. of flood or hurricane; Forecasting, e.g. risk assessment or mapping
Abstract
The invention provides a wettability regulator composition, a preparation method and application thereof, wherein the wettability regulator composition comprises the following components: a hydrocarbyl polyether quaternary ammonium salt shown as a formula (1), a hydrocarbyl amide polyether acid salt shown as a formula (2) and a hydrocarbyl amide polyether shown as a formula (3). The wettability regulator composition can regulate the oil-wet saturated rock core into weak water wet, promote the imbibition and oil displacement effects, and greatly improve the recovery ratio of the ultralow permeability reservoir.
Description
Technical Field
The invention relates to the technical field of oil extraction in oil fields, in particular to a wettability regulator composition, a preparation method and application thereof.
Background
The low permeability oil field in China has rich resources, the relative proportion of low permeability reserves in newly ascertained reserves in recent years is larger and larger, accounting for 60 percent to 70 percent, and the national low permeability oil reservoir reserves reach 210.7X10 percent 8 t. The low permeability oil reservoir is the main resource base for increasing the up-production of the oil reservoir in a quite period in the future, so that the recovery ratio of the low permeability oil field is improved, and the method is suitable for the prior artThe oil field development in China has important significance. For an ultralow permeability oil reservoir, the wettability of the ultralow permeability oil reservoir is researched to have an important influence on the oil gas extraction stage, and the wettability of a tight reservoir influences the entry and flowback of fracturing fluid in the fracturing construction stage, so that the method has a very important meaning on the output after the reservoir is laminated.
Imbibition is a common natural phenomenon and is widely used in engineering and life. Imbibition refers to the process of spontaneously drawing in a wetting phase fluid in a porous medium and displacing a non-wetting phase fluid. The small pore throat determines that the imbibition effect of low permeability dense reservoirs is more pronounced than conventional reservoirs, and data shows that twenty percent of the total recovery may be contributed from imbibition. Aiming at unconventional imbibition oil-water displacement research is one of the current foreign research hotspots, but shale is mostly used as a matrix and is in an indoor experimental simulation stage, and the improvement of the oil-water imbibition displacement efficiency is one of important technical means for improving the recovery ratio of crude oil in a reservoir by developing a wettability regulator formula with special properties.
The wettability regulator can effectively change the wettability of oil reservoirs, reduce the tension of oil-water interfaces, emulsify and solubilize crude oil and reduce the viscosity of the crude oil. Some wettability regulator compound systems have more excellent performance due to the synergistic effect. CN105884255a reports a method for controlling wettability of artificial sandstone core by converting the wettability of artificial sandstone core by nonionic surfactant OP-10 from neutral lipophilicity to hydrophilicity. Patent CN111635476A discloses an oil reservoir wettability improver and a preparation method thereof, wherein the oil reservoir wettability improver comprises a hydrophilic unsaturated monomer, a nitrogen-containing heterocyclic unsaturated monomer, a hydrophobic unsaturated monomer, a phase transfer agent and a solvent, and is suitable for low-permeability and ultra-low-permeability oil reservoirs with the temperature of 105 ℃.
In conclusion, although the wettability regulator in the prior art can reduce the surface area of an oil-water interface, the wettability regulator in the prior art has the problems of high use concentration, low dialysis oil displacement efficiency and the like.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a wettability regulator composition, a preparation method and application thereof, and the wettability regulator composition can regulate an oil-wet saturated rock core into weak water wet, promote the imbibition and displacement effects and greatly improve the recovery ratio of an ultralow permeability reservoir.
The first aspect of the present invention provides a wettability modulator composition,
comprising the following steps: hydrocarbyl polyether quaternary ammonium salts, hydrocarbyl amide polyether acid salts, and hydrocarbyl amide polyether;
the hydrocarbyl polyether quaternary ammonium salt satisfies formula (1):
wherein R is 1 Is C 1 ～C 30 At least one of the alkyl groups of (a);
R 2 、R 3 、R 4 each independently is substituted and unsubstituted C 1 ～C 4 At least one of the alkyl groups of (a);
x is an anion which makes the hydrocarbyl polyether quaternary ammonium salt molecule electrically neutral, j is the reciprocal of the absolute value of the valence state of X;
a is any number from 0 to 10;
b is any number from 1 to 10;
the hydrocarbyl amide polyether acid salt satisfies formula (2):
wherein R is 5 Is substituted and unsubstituted C 1 ～C 30 At least one of the alkyl groups of (a);
R 6 is substituted and unsubstituted C 2 ～C 8 At least one of alkylene groups of (a);
R 7 is substituted and unsubstituted C 1 ～C 4 At least one of alkylene groups of (a);
y is-SO 3 At least one of M and COON, wherein M and N are the same or different and are the same or different, and wherein M and N are the same or different and are the same or differentThe polyether acid salt molecule presents a cation or a cation group which is electrically neutral;
the sum of m1 and m2 is any number from 0 to 20;
the sum of n1 and n2 is any number from 0 to 20;
the hydrocarbyl amide polyether satisfies formula (3):
wherein R is 8 Is C 1 ～C 30 Alkyl, C of (2) 1 ～C 30 At least one of the substituted alkyl groups;
R 9 is substituted and unsubstituted C 2 ～C 8 At least one of alkylene groups of (a);
R 10 is substituted and unsubstituted C 1 ～C 4 At least one of alkylene groups of (a);
the sum of m3 and m4 is any number from 0 to 20;
the sum of n3 and n4 is any number from 0 to 20.
The invention adopts the anionic-nonionic and cationic-nonionic surfactant composition, and after the anionic-nonionic and cationic-nonionic surfactants are compounded, the problems of loose interfacial film arrangement and the like caused by electrostatic repulsive force among the same kind of charges of the traditional surfactants can be avoided, so that the interfacial activity of the compound agent is enhanced, and the oil displacement efficiency is improved. Meanwhile, the anti-adsorption and anti-calcium-magnesium ion capabilities of the surfactant composition are enhanced, so that the surfactant composition has the possibility of being applied to high-mineralization oil reservoirs.
Further, the hydrocarbyl polyether quaternary ammonium salt satisfies formula (1A):
wherein R is 1 Is C 1 ～C 30 At least one of the alkyl groups of (2), preferably R 1 Is C 1 ～C 22 At least one of the alkyl groups of (2), more preferably R 1 Is C 8 ～C 22 At least one of the alkyl groups of (a); and/or R 2 、R 3 、R 4 Each independently is substituted and unsubstituted C 1 ～C 4 At least one of the alkyl groups of (2), preferably R 2 、R 3 、R 4 Each independently is substituted and unsubstituted C 1 ～C 3 At least one of the alkyl groups of (a) may be a hydroxy group; and/or X is an anion which renders the hydrocarbyl polyether quaternary ammonium molecule electrically neutral, preferably X is at least one of the halide ions, more preferably X is-Cl - 、-Br - 、-I - At least one of (a) and (b); j is the reciprocal of the absolute value of the X valence; and/or a is the sum of the propoxy groups, a is any number from 0 to 10, preferably a is any number from 0 to 5; and/or b is the sum of the ethoxy groups, b is any number from 1 to 10, preferably b is any number from 5 to 8.
Further, X in the formula (1) and the formula (1A) may be selected as-Cl - 。
According to some embodiments of the wettability modulator composition of the present invention, the hydrocarbyl amide polyether acid salt satisfies R in formula (2) 5 Is substituted and unsubstituted C 1 ～C 20 At least one of the alkyl groups of (2), preferably R 5 Is substituted and unsubstituted C 8 ～C 20 At least one of the alkyl groups of (a) may be a hydroxy group; and/or R 6 Is C 2 ～C 8 At least one of the substituted and unsubstituted alkylene groups, the substituent may be a hydroxy group, preferably R 6 Is C 2 ～C 4 At least one of alkylene groups of (a); and/or R 7 Is substituted and unsubstituted C 1 ～C 4 At least one of the alkylene groups of (a) may be a hydroxy group, preferably R 7 Is C 1 ～C 2 At least one of alkylene groups of (a); and/or Y is-SO 3 At least one of M and COON, wherein M and N are cations or cationic groups that render the hydrocarbyl amide polyether acid salt molecule electrically neutral; and/or the sum of m1 and m2 is any number from 0 to 20, preferably the sum of m1 and m2 is any number from 0 to 10; and/or the sum of n1 and n2 is 0 to 20Any number, preferably the sum of n1 and n2 is any number from 2 to 10.
According to some embodiments of the wettability modulator composition of the present invention, the hydrocarbyl amide polyether of formula (3) is R 8 Is substituted and unsubstituted C 1 ～C 20 At least one of the alkyl groups of (2), preferably R 8 Is substituted and unsubstituted C 8 ～C 20 At least one of the alkyl groups of (a) may be a hydroxy group; and/or R 9 Is substituted and unsubstituted C 2 ～C 8 At least one of the alkylene groups of (a) may be a hydroxy group, preferably R 9 Is C 2 ～C 4 At least one of alkylene groups of (a); and/or R 10 Is substituted and unsubstituted C 1 ～C 4 At least one of the alkylene groups of (a) may be a hydroxy group, preferably R 10 Is C 1 ～C 2 At least one of alkylene groups of (a); and/or the sum of m3 and m4 is any number from 0 to 20, preferably the sum of m3 and m4 is any number from 0 to 10; and/or the sum of n3 and n4 is any number from 0 to 20, preferably the sum of n3 and n4 is any number from 2 to 10.
According to some embodiments of the wettability modulator composition of the present invention, the molar ratio of the hydrocarbyl amide polyether acid salt, the hydrocarbyl amide polyether and the hydrocarbyl polyether quaternary ammonium salt is 1: (0.01-1): (0.01-100).
According to some embodiments of the wettability modulator composition of the present invention, the wettability modulator composition further comprises water in an amount of 98% to 99.98% based on the total mass of the surfactant composition.
Further, the total mineralization degree of the water injection is preferably 10000-30000 mg/L, ca 2+ +Mg 2+ Preferably 0 to 1000mg/L.
In a second aspect, the present invention provides a method for preparing a wettability modulator composition as described above, comprising the steps of: mixing alkyl polyether quaternary ammonium salt, alkyl amide polyether acid salt and alkyl amide polyether with water, and regulating pH value; wherein the molar ratio of the hydrocarbyl amide polyether acid salt, the hydrocarbyl amide polyether and the hydrocarbyl polyether quaternary ammonium salt is 1: (0.01-1): (0.01-100); preferably, the valence pH is adjusted to 7 to 10, more preferably 8 to 9.5.
According to some embodiments of the method of preparing a wettability modulator composition of the present invention, the method of preparing a hydrocarbylamide polyether comprises: alkoxylating a hydrocarbyl amide with propylene oxide and ethylene oxide in the presence of a basic catalyst; preferably, the alkaline catalyst is used in an amount of 1 to 3wt% based on the mass of the hydrocarbylamide; preferably, the alkylation conditions include: the temperature is 100-180 ℃, the pressure is less than 0.60MPa, and the time is 30 minutes-2 hours.
Further, the hydrocarbylamide may be prepared by the steps of:
methyl alkyl acid ester R 5 COOMe(R 5 The molar ratio of the alkali catalyst to the short-chain alcohol amine is 1 (1-1.5), the dosage of the alkali catalyst is 0.5-3 wt% of the mass of methyl alkyl acid, the reaction time is preferably 2-10 hours at 60-80 ℃, and the reaction pressure is preferably less than 0.5MPa gauge pressure.
Further, the basic catalyst of the present invention may be various basic catalysts commonly used in the art for alkoxylation reactions, such as, but not limited to, alkali metal hydroxides.
According to some embodiments of the method of preparing a wettability modulator composition of the present invention, the method of preparing a hydrocarbyl amide polyether acid salt comprises the steps of:
step I) selecting a hydrocarbyl amide polyether, preferably a hydrocarbyl amide polyether as described hereinabove; step II) carrying out an alkalization reaction on the hydrocarbylamide polyether selected in the step I) and alkali, then carrying out a reaction I with a sulfonation reagent or a carboxylation reagent, regulating the pH value, carrying out oil-water separation, and adding alkali liquor for neutralization after evaporating the solvent from the oil phase; preferably, in step II) the pH is adjusted to less than 3, and in the alkalization reaction and reaction I, the molar ratio of the hydrocarbylamide polyether, the base and the sulphonating or carboxylating agent is 1: (3-6): (3-6).
More preferably, the alkalization reaction temperature in step II) is 45 to 80 ℃ for 1 to 5 hours, and the reaction temperature in reaction I is 70 to 90 ℃ for 5 to 15 hours.
Further, the sulfonating agent in said step II) is preferably Z-R 6 SO 3 H, wherein Z is halogen; the carboxylation reagent is preferably Z-R 6 COOH, Z is halogen.
According to a third aspect of the present invention there is provided the use of a wettability modulator composition as described above or a method of preparing a wettability modulator composition as described above in oil recovery in an oilfield.
Further, one skilled in the art may utilize, in accordance with the prior art, for example, but not limited to, injecting a solution of the wettability modulator composition into an oil reservoir for contact with the subterranean crude oil to displace the subterranean crude oil; or is compounded with other oil extraction agents for use, etc.
According to the application of the invention, the preferable range of the alkyl amide polyether acid salt is 0.1-0.3 wt% and the preferable range of the alkyl polyether quaternary ammonium salt is 0.02-0.15 wt% based on the mass percentage of the total system.
The invention has the beneficial effects that:
the wettability regulator composition can avoid the problems of loose arrangement of interfacial films and the like caused by electrostatic repulsive force among the same kind of charges of the traditional wettability regulator, further enhance the interfacial activity of the compound agent and improve the oil displacement efficiency. Meanwhile, the wettability regulator composition has enhanced capabilities of resisting adsorption and calcium and magnesium ions, so that the wettability regulator composition has the possibility of being applied to high-mineralization oil reservoirs.
The wettability regulator composition capable of improving the recovery ratio can be used for the water and crude oil of the north-critical stratum with the stratum temperature of 30 ℃, the mineralization degree of 35000mg/L and the calcium-magnesium ion of 1000mg/L, and the wettability regulator composition is formed by 0.1-0.3 wt% of alkyl amide polyether acid salt, 0.01-0.03wt% of nonionic surfactant (alkyl amide polyether) and 0.02-0.15 wt% of alkyl polyether quaternary ammonium salt, so that the water drop contact angle of the north-critical stratum after the crude oil aging after the water drop contact angle of the north-critical stratum core is soaked in the wettability regulator composition is measured, and a static dialysis test is carried out. The wettability of the saturated core is weak hydrophilic under the action of the wettability regulator, the dialysis recovery ratio can reach 10-20%, and a better technical effect is obtained.
Detailed Description
In order that the invention may be more readily understood, the invention will be described in detail below with reference to the following examples, which are given by way of illustration only and are not limiting of the scope of application of the invention.
[ Performance test of wettability controlling agent ]
1. Wettability modifier composition interfacial wettability modification capability test
Cutting the rock core into slices with the thickness of 3-4mm, and soaking with petroleum ether to remove residual oil in the rock core. And taking out the core slice, drying, pumping the saturated crude oil by using a vacuum pump, immersing the saturated crude oil in the Weibei crude oil for 40 hours, taking out, and wiping the crude oil on the surface. The core after saturating the crude oil was immersed in the 0.1% concentration wettability modifier composition solution described in examples 2-10, immersed for 24 hours, taken out, and the contact angle was measured after wiping off the surface liquid.
2. Static dialysis test
And (3) cutting, measuring, drying and weighing the rock core taken by the stratum in the static dialysis test, and carrying out a rock core saturation test by using a rock core saturator. The cores after saturating the crude were immersed in a 0.5% strength solution of the wettability modulator composition described in examples 1-9 for static dialysis testing.
[ preparation of wettability control agent composition ]
It should be noted that the raw materials selected in the examples of the present invention are commercially available conventional products, and the purity is chemically pure/analytically pure, and the present invention is not limited thereto.
Step a), adding a certain amount of methyl alkyl acid, short-chain alcohol amine and 0.5% NaOH by weight into a polymerization reaction kettle, heating the system to 70-75 ℃ under stirring, starting a vacuum system, then purging 3-4 times with nitrogen to remove air in the system, controlling the reaction pressure to be less than 0.30MPa, reacting for 3-4 hours, vacuumizing, condensing, recovering methanol, and reacting to obtain the alkyl alcohol amide.
Step b), adding a certain amount of alkyl alcohol amide and 1% KOH by weight of the alkyl alcohol amide into a polymerization reaction kettle, heating the system to 80-90 ℃ under stirring, starting a vacuum system, dehydrating under high vacuum for 1 hour, then purging with nitrogen for 3-4 times to remove air in the system, then slowly introducing calculated amount of propylene oxide to control the reaction pressure to be less than 0.40MPa after the reaction temperature of the system is adjusted to 130 ℃ for propoxylation and alkylation, continuously slowly introducing calculated amount of ethylene oxide after the reaction is finished, purging with nitrogen to remove unreacted ethylene oxide, and neutralizing, decolorizing, filtering and dehydrating after cooling to obtain the alkyl alcohol amide polyether with different polymerization degrees.
Step c), placing the alkyl alcohol amide polyether synthesized in the step b), an organic solvent with the weight being 2-4 times that of the alkyl alcohol amide polyether and NaOH in a reactor (the molar ratio is 1:4-5), starting stirring and heating to 50-80 ℃, performing alkalization reaction for 1-4 hours, then slowly adding 4-6 mol of sodium chloroethyl sulfonate or sodium chloroacetate at 70-90 ℃, after the addition is finished, continuing to perform reaction for 5-10 hours in a reflux state, and after the conversion rate is detected to be qualified, acidifying, washing, evaporating the solvent from the organic phase, adding alkali liquor and neutralizing to obtain the alkyl alcohol amide polyether acid salt.
Preparation of the wettability modulator composition of step d)
And c) uniformly mixing the alkylamide polyether acid salt and the alkyl polyether quaternary ammonium salt synthesized in the step c) with the calculated alkali liquor and water at 50-60 ℃ according to the required proportion to obtain the wettability regulator product with the required content.
[ example 1 ]
The alkylamide polyether acid salt and the nonionic surfactant (R) are prepared by the experimental steps of the preparation of the wettability regulator composition 5 ＝C 11 H 23 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝3，n1+n2＝7，Y＝CH 2 COONa，R 8 、R 9 、R 10 Respectively with R 5 、R 6 、R 7 Similarly, m1+m2=m3+m4, n1+n2=n3+n4) and an alkyl polyether quaternary ammonium salt (R 1 ＝C 18 H 37 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=2 and b=9) the surfactant is respectively dissolved in stratum water with the mineralization degree of 35000mg/L and the calcium and magnesium ion of 1000mg/L, stirred for 30 minutes to prepare 0.1-0.5% wt of aqueous solution, and then the aqueous solution is prepared according to the following steps: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.05:1 mixing the surface active agents uniformly to obtain a wettability regulator composition product solution 1a.
[ example 2 ]
Using a procedure similar to example 1, alkylamide polyether acid salt, nonionic surfactant (R 5 ＝C 15 H 31 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝0，n1+n2＝5，Y＝CH 2 COONa，R 8 、R 9 、R 10 Respectively with R 5 、R 6 、R 7 Similarly, m1+m2=m3+m4, n1+n2=n3+n4) and an alkyl polyether quaternary ammonium salt (R 1 ＝C 16 H 33 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=3 and b=5) the surfactant is respectively dissolved in stratum water with the mineralization degree of 35000mg/L and the calcium and magnesium ion of 1000mg/L, stirred for 30 minutes to prepare 0.1-0.5% wt of aqueous solution, and then the aqueous solution is prepared according to the following steps: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.05:1.2 mixing the above surfactants uniformly to obtain a wettability control agent composition product solution 2a.
[ example 3 ]
Using a procedure similar to example 1, alkylamide polyether acid salt, nonionic surfactant (R 5 ＝C 16 H 33 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝2，n1+n2＝5，Y＝CH 2 COONa，R 8 、R 9 、R 10 Respectively with R 5 、R 6 、R 7 Similarly, m1+m2=m3+m4, n1+n2=n3+n4) and an alkyl polyether quaternary ammonium salt (R 1 ＝C 16 H 33 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=3 and b=5) the surfactant is respectively dissolved in stratum water with the mineralization degree of 35000mg/L and the calcium and magnesium ion of 1000mg/L, stirred for 30 minutes to prepare 0.1-0.5% wt of aqueous solution, and then the aqueous solution is prepared according to the following steps: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.05: and 0.8, uniformly mixing the surfactants to obtain a wettability regulator composition product solution 3a.
[ example 4 ]
Using a procedure similar to example 1, alkylamide polyether acid salt, nonionic surfactant (R 5 ＝C 8 H 7 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝0，n1+n2＝8，Y＝CH 2 COONa，R 8 、R 9 、R 10 Respectively with R 5 、R 6 、R 7 Similarly, m1+m2=m3+m4, n1+n2=n3+n4) and an alkyl polyether quaternary ammonium salt (C 22 H 45 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=3 and b=6) the surfactant is respectively dissolved in stratum water with the mineralization degree of 35000mg/L and the calcium and magnesium ion of 1000mg/L, stirred for 30 minutes to prepare 0.1-0.5% wt of aqueous solution, and then the aqueous solution is prepared according to the following steps: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.08:1.6 mixing the above surfactants uniformly to obtain a wettability control agent composition product solution 4a.
[ example 5 ]
Using a procedure similar to example 1, alkylamide polyether acid salt, nonionic surfactant (R 5 ＝C 17 H 35 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝9，n1+n2＝4，Y＝CH 2 COONa，R 8 、R 9 、R 10 Respectively with R 5 、R 6 、R 7 Similarly, m1+m2=m3+m4, n1+n2=n3+n4) and an alkyl polyether quaternary ammonium salt (R 1 ＝C 12 H 25 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=0, b=7) surface active agentThe sex agent is respectively dissolved in stratum water with the mineralization degree of 35000mg/L and the calcium and magnesium ion of 1000mg/L, stirred for 30 minutes to prepare 0.1 to 0.5 percent by weight of aqueous solution, and then the aqueous solution is prepared according to the alkyl amide polyether acid salt: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.03:1.6 mixing the above surfactants uniformly to obtain a wettability control agent composition product solution 5a.
[ example 6 ]
Using a procedure similar to example 1, alkylamide polyether acid salt, nonionic surfactant (R 5 ＝C 15 H 31 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 CH 2 ，m1+m2＝0，n1+n2＝5，Y＝CH 2 COONa，R 8 、R 9 、R 10 Respectively with R 5 、R 6 、R 7 Similarly, m1+m2=m3+m4, n1+n2=n3+n4) and an alkyl polyether quaternary ammonium salt (R 1 ＝C 18 H 37 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH 2 CH 3 A=0, b=5) the surfactant is respectively dissolved in stratum water with the mineralization degree of 35000mg/L and the calcium-magnesium ion of 1000mg/L, stirred for 30 minutes to prepare 0.1-0.5%wt water solution, and then the water solution is prepared according to the following steps: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.05: and 0.8, uniformly mixing the surfactants to obtain a wettability regulator composition product solution 6a.
[ example 7 ]
Using a procedure similar to example 1, alkylamide polyether acid salt, nonionic surfactant (R 5 ＝C 16 H 33 ，R 6 ＝CH 2 CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝3，n1+n2＝7，Y＝CH 2 COONa，R 8 、R 9 、R 10 Respectively with R 5 、R 6 、R 7 Similarly, m1+m2=m3+m4, n1+n2=n3+n4) and an alkyl polyether quaternary ammonium salt (R 1 ＝C 14 H 29 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=2 and b=6) the surfactant is respectively dissolved in 35000mg/L of stratum water with 1000mg/L of calcium and magnesium ions, stirred for 30 minutes to prepare 0.1-0.5% wt of aqueous solution, and then the aqueous solution is prepared according to the following steps: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.09:2.2 mixing the above surfactants uniformly to obtain a wettability control agent composition product solution 7a.
[ example 8 ]
Using a procedure similar to example 1, alkylamide polyether acid salt, nonionic surfactant (R 5 ＝C 17 H 35 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝0，n1+n2＝7，Y＝CH 2 SO 3 Na，R 8 、R 9 、R 10 Respectively with R 5 、R 6 、R 7 Similarly, m1+m2=m3+m4, n1+n2=n3+n4) and an alkyl polyether quaternary ammonium salt (R 1 ＝C 16 H 33 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=3 and b=5) the surfactant is respectively dissolved in 35000mg/L of stratum water with 1000mg/L of calcium and magnesium ions, stirred for 30 minutes to prepare 0.1-0.5% wt of aqueous solution, and then the aqueous solution is prepared according to the following steps: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.05:1 mixing the surfactants uniformly to obtain a wettability regulator composition product solution 8a.
[ example 9 ]
Using a procedure similar to example 1, alkylamide polyether acid salt, nonionic surfactant (R 5 ＝C 13 H 27 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝3，n1+n2＝7，Y＝CH 2 SO 3 Na，R 8 、R 9 、R 10 Respectively with R 5 、R 6 、R 7 Similarly, m1+m2=m3+m4, n1+n2=n3+n4) and an alkyl polyether quaternary ammonium salt (R 1 ＝C 18 H 37 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=2 and b=9) surfactant is respectively dissolved in 35000mg/L of stratum water with 1000mg/L of calcium and magnesium ions, stirred for 30 minutes to prepare 0.1-0.5% wt of aqueous solution, and then the aqueous solution is prepared according to the following steps: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.1:0.4 mixing the above surfactants uniformly to obtain a wettability control agent composition product solution 9a.
[ example 10 ]
Using a procedure similar to example 1, alkylamide polyether acid salt, nonionic surfactant (R 5 ＝C 15 H 31 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝0，n1+n2＝5，Y＝CH 2 COONa，R 8 ＝C 16 H 33 ，R 9 ＝CH 2 CH 2 ，R 10 ＝CH 2 M3+m4=2, n3+n4=5) with an alkyl polyether quaternary ammonium salt (R 1 ＝C 16 H 33 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=3 and b=5) the surfactant is respectively dissolved in stratum water with the mineralization degree of 35000mg/L and the calcium and magnesium ion of 1000mg/L, stirred for 30 minutes to prepare 0.1-0.5% wt of aqueous solution, and then the aqueous solution is prepared according to the following steps: hydrocarbyl amide polyether: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1:0.05:1.2 mixing the above surfactants uniformly to obtain a wettability control agent composition product solution 10a.
Comparative example 1
The nonionic surfactant OP-10 was dissolved in formation water having a mineralization of 35000mg/L and a calcium magnesium ion of 1000mg/L to prepare a 0.5% wt aqueous solution according to the method of patent CN 105884255A. Stirring for 30 min, and mixing to obtain reference wettability regulator composition 1b.
Comparative example 2
Alkyl amide polyether acid salt (R) 5 ＝C 16 H 33 ，R 6 ＝CH 2 CH 2 ，R 7 ＝CH 2 ，m1+m2＝2，n1+n2＝5，Y＝CH 2 COONa) surfactant and alkyl polyether quaternary ammonium salt (R) 1 ＝C 16 H 33 ，R 2 ＝CH 3 ，R 3 ＝CH 3 ，R 4 ＝CH(OH)CH 3 A=3 and b=5) the surfactant is respectively dissolved in formation water with the mineralization degree of 35000mg/L and the calcium and magnesium ion of 1000mg/L, and stirred for 30 minutes to prepare 0.1 percent weight water solution, and then the water solution is prepared according to the following steps: the molar ratio of the hydrocarbyl polyether quaternary ammonium salt is 1: and 0.8, uniformly mixing the surfactants to obtain a wettability regulator composition product solution 2b.
Examples 1-9 were tested for contact angle measurements using the wettability modifier composition interface wettability modification capability test above, with the results shown in table 1:
TABLE 1
Wherein, test temperature: 30 ℃; formation water mineralization 35000mg/L and calcium and magnesium ions 1000mg/L.
The results of the tests for examples 1-9 using the above wettability modulator static dialysis test are shown in table 2:
TABLE 2
Using the above wettability modulator composition static dialysis test, the contact angle measurements were performed for the test of example 3, comparative examples 1-2, and the results are shown in table 3:
TABLE 3 Table 3
| Component (A) | Before soaking | 3a | 1b | 2b |
| Replacement efficiency | 4％ | 17％ | 7％ | 9％ |
Wherein, test temperature: 30 ℃; formation water mineralization 35000mg/L and calcium and magnesium ions 1000mg/L.
As can be seen from tables 1-3, example 3 has a higher dialysis displacement efficiency relative to the respective comparative examples. The invention uses the compositions of 0.1-0.3 wt% of alkyl amide polyether acid salt, 0.01-0.03wt% of nonionic surfactant (alkyl amide polyether) and 0.02-0.15 wt% of alkyl polyether quaternary ammonium salt to form a wettability regulator composition, which has smaller water drop contact angle than the wettability regulator formed by the nonionic surfactant or the surfactant formed by anions and cations in the prior art, and can achieve dialysis recovery ratio of 10-20% in static dialysis test.
What has been described above is merely a preferred example of the present invention. It should be noted that other equivalent modifications and improvements will occur to those skilled in the art, and are intended to be within the scope of the present invention, as a matter of common general knowledge in the art, in light of the technical teaching provided by the present invention.
Claims (19)
1. A wettability modulator composition comprising: hydrocarbyl polyether quaternary ammonium salts, hydrocarbyl amide polyether acid salts, and hydrocarbyl amide polyether;
the hydrocarbyl polyether quaternary ammonium salt satisfies formula (1):
wherein R is 1 Is C 8 ～C 22 At least one of the alkyl groups of (a);
R 2 、R 3 、R 4 each independently is substituted and unsubstituted C 1 ～C 4 At least one of the alkyl groups of (a);
x is an anion which makes the hydrocarbyl polyether quaternary ammonium salt molecule electrically neutral, j is the reciprocal of the absolute value of the valence state of X;
a is any number from 0 to 10;
b is any number from 1 to 10;
the hydrocarbyl amide polyether acid salt satisfies formula (2):
wherein R is 5 Is C 8 ～C 20 Alkyl, C of (2) 8 ～C 20 At least one of the substituted alkyl groups;
R 6 is substituted and unsubstituted C 2 ～C 8 At least one of alkylene groups of (a);
R 7 is substituted and unsubstituted C 1 ～C 4 At least one of alkylene groups of (a);
y is-SO 3 At least one of M and COON, wherein M and N are cations or cationic groups that render the hydrocarbyl amide polyether acid salt molecule electrically neutral;
the sum of m1 and m2 is any number from 0 to 10;
the sum of n1 and n2 is any number from 2 to 10;
the hydrocarbyl amide polyether satisfies formula (3):
wherein the method comprises the steps of，R 8 Is substituted and unsubstituted C 8 ～C 20 At least one of the alkyl groups of (a);
R 9 is substituted and unsubstituted C 2 ～C 8 At least one of alkylene groups of (a);
R 10 is substituted and unsubstituted C 1 ～C 4 At least one of alkylene groups of (a);
the sum of m3 and m4 is any number from 0 to 10;
the sum of n3 and n4 is any number from 2 to 10.
2. The wettability control agent composition according to claim 1, wherein R in the quaternary ammonium salt of a hydrocarbyl polyether represented by the formula (1) 2 、R 3 、R 4 Each independently is substituted and unsubstituted C 1 ～C 3 At least one of the alkyl groups of (a); and/or
a is any number from 0 to 5; and/or
b is any number from 5 to 8.
3. The wettability control agent composition according to claim 1 or 2, wherein R in the hydrocarbylamide polyether acid salt represented by the formula (2) 6 Is C 2 ～C 4 At least one of alkylene groups of (a); and/or
R 7 Is C 1 ～C 2 At least one of alkylene groups of (a).
4. The wettability control agent composition according to claim 1 or 2, wherein R in the hydrocarbylamide polyether represented by the formula (3) 9 Is C 2 ～C 4 At least one of alkylene groups of (a); and/or
R 10 Is C 1 ～C 2 At least one of alkylene groups of (a).
5. The wettability control composition according to claim 1 or 2, characterized in that the molar ratio of the hydrocarbyl amide polyether acid salt, the hydrocarbyl amide polyether and the hydrocarbyl polyether quaternary ammonium salt is (0.01 to 1): (0.01-1): (0.001-0.1).
6. The wettability modulator composition of claim 5 wherein the molar ratio of said hydrocarbyl amide polyether acid salt, said hydrocarbyl amide polyether and said hydrocarbyl polyether quaternary ammonium salt is 1: (0.02-0.5): (1-10).
7. The wettability modulator composition of claim 1 or 2 wherein the wettability modulator composition further comprises water.
8. The wettability modulator composition of claim 7 wherein the water content is 98% to 99.98% based on the total mass of the wettability modulator composition.
9. The method of preparing a wettability modulator composition according to any one of claims 1 to 8, comprising the steps of:
mixing alkyl polyether quaternary ammonium salt, alkyl amide polyether acid salt and alkyl amide polyether with water, and regulating pH value;
wherein the molar ratio of the hydrocarbyl amide polyether acid salt, the hydrocarbyl amide polyether and the hydrocarbyl polyether quaternary ammonium salt is 1: (0.02-0.5): (1-10).
10. The method according to claim 9, wherein the pH is adjusted to 7 to 10.
11. The method according to claim 10, wherein the pH is adjusted to 8 to 9.5.
12. The preparation method according to any one of claims 9 to 11, characterized in that the preparation method of the hydrocarbylamide polyether comprises the following steps:
alkoxylation of hydrocarbylamides with propylene oxide and ethylene oxide in the presence of a basic catalyst.
13. The preparation method according to claim 12, wherein the basic catalyst is used in an amount of 1 to 3wt% based on the mass of the hydrocarbylamide.
14. The method of claim 12, wherein the alkoxylation conditions comprise: the temperature is 100-180 ℃, the pressure is less than 0.60MPa, and the time is 30 minutes-2 hours.
15. The preparation method according to any one of claims 9 to 11, characterized in that the preparation method of the hydrocarbylamide polyether acid salt comprises the steps of:
step I) selecting alkyl amide polyether;
step II) carrying out an alkalization reaction on the alkyl amide polyether selected in the step I) and alkali, then carrying out a reaction I with a sulfonation reagent or a carboxylation reagent, regulating the pH value, carrying out oil-water separation, evaporating the oil phase to remove the solvent, and then adding alkali liquor for neutralization.
16. The process according to claim 15, wherein in step II) the pH is adjusted to less than 3, and the molar ratio of the hydrocarbylamide polyether, base and sulphonating or carboxylating agent in the alkalisation reaction and reaction I is 1: (3-6): (3-6).
17. The process according to claim 15, wherein the alkalization reaction temperature in step II) is 45 to 80 ℃ for 1 to 5 hours; and/or the reaction temperature of the reaction I is 70-90 ℃ and the time is 5-15 hours.
18. The method of claim 15, wherein the hydrocarbyl amide polyether of claim 12 is selected.
19. Use of the wettability modulator composition according to any one of claims 1 to 8 or the method for preparing a wettability modulator composition according to any one of claims 9 to 18 in oil recovery in an oilfield.
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