CN115261005A - Modifying and flooding agent and preparation method thereof - Google Patents
Modifying and flooding agent and preparation method thereof Download PDFInfo
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- CN115261005A CN115261005A CN202110480525.XA CN202110480525A CN115261005A CN 115261005 A CN115261005 A CN 115261005A CN 202110480525 A CN202110480525 A CN 202110480525A CN 115261005 A CN115261005 A CN 115261005A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 90
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 44
- 239000002131 composite material Substances 0.000 claims abstract description 42
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 36
- 239000003381 stabilizer Substances 0.000 claims abstract description 27
- 238000004132 cross linking Methods 0.000 claims abstract description 21
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003623 enhancer Substances 0.000 claims abstract description 17
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000007062 hydrolysis Effects 0.000 claims abstract description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 61
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 46
- 238000003756 stirring Methods 0.000 claims description 45
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 43
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 40
- 238000006243 chemical reaction Methods 0.000 claims description 39
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000008098 formaldehyde solution Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 20
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical group C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 20
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 20
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 10
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 10
- 208000004761 Supernumerary Tooth Diseases 0.000 claims description 9
- 210000004357 third molar Anatomy 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 230000001965 increasing effect Effects 0.000 abstract description 15
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 125000003368 amide group Chemical group 0.000 abstract description 4
- 239000000178 monomer Substances 0.000 abstract description 4
- 230000003335 steric effect Effects 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 10
- 239000005011 phenolic resin Substances 0.000 description 10
- 229920001568 phenolic resin Polymers 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000005465 channeling Effects 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- 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
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/06—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
- C08F226/10—N-Vinyl-pyrrolidone
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The application discloses a profile control agent and a preparation method thereof, belonging to the technical field of oilfield chemistry. The modifying and flooding agent provided by the embodiment of the application comprises modified polyacrylamide, a composite cross-linking agent, a cross-linking enhancer and a stabilizing agent, wherein acrylamide is modified by introducing a functional monomer N-vinyl pyrrolidone, so that the side chain steric effect is increased, the hydrolysis of an amide group in the acrylamide is inhibited, and the stability of the modifying and flooding agent is favorably improved; the complexity of the network structure of the profile control agent is increased by adding the composite cross-linking agent; by adding the stabilizer, the degradation process of the modifying and flooding agent is slowed down. The components play a synergistic cooperation role, so that the high temperature resistance of the profile control agent is improved.
Description
Technical Field
The application relates to the technical field of oilfield chemistry. In particular to a profile control agent and a preparation method thereof.
Background
The deep profile control technology is an important means for improving the water drive development effect, and the technology injects a profile control agent into an oil reservoir to block a high-permeability channeling channel and force subsequent fluid to be diverted to a low-permeability area, so that the swept volume is effectively enlarged. And part of the oil reservoir is buried deeply and has higher temperature, so the injected profile control agent also has good high-temperature resistance, and the failure at high temperature is avoided, and the plugging effect and the profile control benefit are not influenced.
The profile control agent in the related technology mainly comprises a polymer and a cross-linking agent, wherein the polymer is a product obtained by the reaction of acrylamide, 2-acrylamide sodium dodecyl sulfate and 2-acrylamide-2-phenyl ethanesulfonic acid, and the cross-linking agent is a mixture composed of a phenolic resin prepolymer and polyethyleneimine.
However, the profile control agent in the related art can only be applied to water-drive reservoirs below 110 ℃, and cannot meet the profile control requirements of reservoirs above 110 ℃, so that the high temperature resistance is poor.
Disclosure of Invention
The embodiment of the application provides a profile control agent and a preparation method thereof, which can improve the high temperature resistance of the profile control agent. The specific technical scheme is as follows:
in one aspect, an embodiment of the present application provides a profile control agent, where the profile control agent includes the following components in percentage by mass: 0.15 to 0.3 percent of modified polyacrylamide, 0.15 to 0.35 percent of composite cross-linking agent, 0.1 to 0.2 percent of cross-linking enhancer, 0.02 to 0.05 percent of stabilizer and the balance of water;
the modified polyacrylamide is a product obtained by the reaction of acrylamide and N-vinyl pyrrolidone.
In one possible implementation mode, the modified polyacrylamide is prepared according to the following preparation method:
dissolving acrylamide and N-vinyl pyrrolidone in a deionized water-ethanol solution, adding an initiator, and reacting in a constant-temperature water bath at 70 ℃ for 8 hours to obtain a reaction solution;
and adding isopropanol into the reaction solution to generate a precipitate, and filtering and drying to obtain the modified polyacrylamide.
In another possible implementation, the acrylamide has a degree of hydrolysis of 23 to 30% and a molecular weight of not less than 2500 ten thousand.
In another possible implementation manner, the composite cross-linking agent is prepared according to the following preparation method:
adding phenol with a first molar weight into a three-neck flask, heating to 50 ℃ in a constant-temperature water bath kettle, adding a first mass of 40% sodium hydroxide solution under a stirring state, and reacting at the constant temperature of 50 ℃ for 20min to obtain a first solution;
preparing a second molar mass of 36% formaldehyde solution to obtain a second mass of formaldehyde solution, adding a third mass of 36% formaldehyde solution into the three-neck flask within 20min, heating to 65 ℃, and stirring at a constant temperature for 30min to obtain a second solution, wherein the third mass is 80% of the second mass;
adding a sodium hydroxide solution with the concentration of 40% in a fourth mass into the second solution, heating to 75 ℃, stirring at a constant temperature for 15min, adding a formaldehyde solution with the concentration of 36% in a fifth mass, heating to 85-88 ℃, reacting at a constant temperature for 1-2 h, and cooling to room temperature to obtain a third solution, wherein the fifth mass is 20% of the second mass;
and adding a third solution with a third molar weight into the two-neck flask, adding a phenol solution with a concentration of 40% with a fourth molar weight under a stirring state, and continuously stirring for 10min to obtain the composite crosslinking agent.
In another possible implementation manner, the ratio of the first molar amount, the second molar amount, the third molar amount and the fourth molar amount is 1.
In another possible implementation, the first mass is 3.5% of the sum of a sixth mass and a seventh mass, the sixth mass being the mass corresponding to the first molar amount of phenol, the seventh mass being the mass corresponding to the second molar amount of formaldehyde;
the fourth mass is 1.5% of the sum of the sixth mass and the seventh mass.
In another possible implementation, the crosslinking enhancer is hexamethylenetetramine.
In another possible implementation, the stabilizer includes at least one of thiourea and sodium thiosulfate.
In another possible implementation, if the stabilizer comprises thiourea and sodium thiosulfate, the mass ratio of the thiourea to the sodium thiosulfate is 1.
In another aspect, an embodiment of the present application provides a preparation method of a profile control agent, where the preparation method includes:
adding 70% by volume of water into a reaction vessel according to the mass fraction of each component;
sequentially adding a stabilizer, a crosslinking enhancer and modified polyacrylamide into the reaction container, and adding the remaining 30% by volume of water into the reaction container after all the components are completely dissolved;
adding a composite cross-linking agent into the reaction container, and obtaining a mixed solution after the composite cross-linking agent is completely dissolved;
and (3) placing the mixed solution in a thermostat with the temperature of 100-130 ℃ for reaction for 5d to obtain the profile control and flooding agent.
The technical scheme provided by the embodiment of the application has the following beneficial effects:
the modifying and flooding agent provided by the embodiment of the application comprises modified polyacrylamide, a composite cross-linking agent, a cross-linking enhancer and a stabilizing agent, wherein acrylamide is modified by introducing a functional monomer N-vinyl pyrrolidone, so that the side chain steric effect is increased, the hydrolysis of an amide group in the acrylamide is inhibited, and the stability of the modifying and flooding agent is favorably improved; the complexity of the network structure of the profile control agent is increased by adding the composite cross-linking agent; by adding the stabilizer, the degradation process of the modifying and flooding agent is slowed down. The components play a synergistic cooperation role, so that the high temperature resistance of the profile control agent is improved.
Drawings
FIG. 1 is a schematic diagram of a production relationship curve of a 62-block retention block after adding a profile control agent according to an embodiment of the present application.
Detailed Description
In order to make the technical solutions and advantages of the present application more clear, the following describes the embodiments of the present application in further detail.
The embodiment of the application provides a profile control agent, which comprises the following components in percentage by mass: 0.15 to 0.3 percent of modified polyacrylamide, 0.15 to 0.35 percent of composite cross-linking agent, 0.1 to 0.2 percent of cross-linking enhancer, 0.02 to 0.05 percent of stabilizer and the balance of water;
the modified polyacrylamide is a product obtained by the reaction of acrylamide and N-vinyl pyrrolidone.
The modifying and flooding agent provided by the embodiment of the application comprises modified polyacrylamide, a composite cross-linking agent, a cross-linking enhancer and a stabilizing agent, wherein acrylamide is modified by introducing a functional monomer N-vinyl pyrrolidone, so that the side chain steric effect is increased, the hydrolysis of an amide group in the acrylamide is inhibited, and the stability of the modifying and flooding agent is favorably improved; the complexity of the network structure of the profile control agent is increased by adding the composite cross-linking agent; by adding the stabilizer, the degradation process of the modifying and flooding agent is slowed down. The components play a synergistic cooperation role, so that the high temperature resistance of the profile control agent is improved.
In the embodiment of the present application, the mass fraction of the modified polyacrylamide may be 0.15%, 0.18%, 0.2%, 0.22%, 0.25%, 0.28%, or 0.3%, the mass fraction of the composite crosslinking agent may be 0.15%, 0.18%, 0.2%, 0.25%, 0.28%, 0.3%, or 0.35%, the mass fraction of the crosslinking reinforcing agent may be 0.1%, 0.12%, 0.15%, 0.16%, 0.18%, or 0.2%, and the mass fraction of the stabilizer may be 0.02%, 0.025%, 0.03%, 0.04%, 0.045%, or 0.05%.
Introduction of modified Polyacrylamide: in one possible implementation mode, the modified polyacrylamide can be prepared according to the following preparation method:
(1) Dissolving acrylamide and N-vinyl pyrrolidone in a deionized water-ethanol solution, adding an initiator, and reacting in a constant-temperature water bath at 70 ℃ for 8 hours to obtain a reaction solution.
In this step, the molar ratio of acrylamide to N-vinylpyrrolidone can be set and changed as needed, for example, the molar ratio is 1.
The initiator can be set and changed according to the needs, for example, the initiator can be ammonium persulfate, potassium persulfate or dimethyl azodiisobutyrate. In the embodiments of the present application, this is not particularly limited.
(2) Adding isopropanol into the reaction solution to generate a precipitate, filtering and drying to obtain the modified polyacrylamide.
In this step, isopropanol may be mixed with water in an arbitrary ratio, and water in the reaction solution may be deprived by adding isopropanol to the reaction solution, so that the modified polyacrylamide may aggregate to form a precipitate. Wherein the yield of the modified polyacrylamide can be increased by adding isopropanol to the reaction solution a plurality of times and performing filtration a plurality of times.
In the examples of the application, the content of the effective component in the modified polyacrylamide prepared by the method is not less than 88%. And the N-vinyl pyrrolidone is introduced into the acrylamide, so that the side chain steric effect is increased, and the long-term stability of the profile control agent and the flooding agent can be improved.
Introduction of composite crosslinking agent: in the examples of the present application, the composite crosslinking agent can be prepared according to the following preparation method:
step 1: adding phenol with a first molar weight into a three-neck flask, heating to 50 ℃ in a constant-temperature water bath kettle, adding a first mass of 40% sodium hydroxide solution under a stirring state, and reacting at the constant temperature of 50 ℃ for 20min to obtain a first solution.
In this step, the three-necked flask was a flask equipped with a thermometer, a condenser and a stirrer. The volume of the three-neck flask can be set and changed according to needs, for example, the volume of the three-neck flask is 250mL.
The first molar amount may be set and changed as needed, for example, the first molar amount is 1mol or 2mol. The first mass was 3.5% of the sum of the sixth mass and the seventh mass, the sixth mass was the mass corresponding to the first molar amount of phenol, and the seventh mass was the mass corresponding to the second molar amount of formaldehyde. In the present example, the mass of phenol in step 1 and the mass of formaldehyde in step 2 may be determined in advance, and the first mass may be determined based on the total mass of the two.
If the first molar amount is 1mol, the step may be: adding 1mol of phenol into a 250mL three-neck flask with a thermometer, a condenser and a stirrer, and heating the mixture to 50 ℃ by using a constant-temperature water bath kettle to melt the mixture into liquid; starting stirring, slowly adding a 40% sodium hydroxide solution, wherein the mass of the sodium hydroxide is 3.5% of the total mass of the phenol and the formaldehyde, keeping the temperature at 50 ℃, and reacting for 20min to obtain a first solution.
Step 2: preparing a second molar amount of 36% formaldehyde solution to obtain a second mass of formaldehyde solution, adding a third mass of 36% formaldehyde solution into a three-neck flask within 20min, heating to 65 ℃, and stirring at constant temperature for 30min to obtain a second solution.
In this step, the third mass is 80% of the second mass. The second molar amount may also be set and changed as necessary, for example, the second molar amount is 1mol, 2mol, or 3mol. For example, when 3mol of a 36% formaldehyde solution is prepared and the mass of the obtained formaldehyde solution is 250g, 200g of the formaldehyde solution is added to a three-neck flask within 20min, the temperature is raised to 65 ℃, and the mixture is stirred at a constant temperature for 30min to obtain a second solution.
For example, if the first and second molar amounts are 1mol and 3mol, respectively, the mass of phenol added in step 1 is 94.11g, and if the mass of formaldehyde in the formaldehyde solution prepared in step 2 is 90g, the sum of the masses of phenol and formaldehyde is 184.11g, the first mass is 184.11g × 3.5%, that is, 6.44g, and 6.44g of a 40% sodium hydroxide solution is weighed.
And step 3: adding a fourth 40% sodium hydroxide solution into the second solution, heating to 75 ℃, stirring at a constant temperature for 15min, adding a fifth 36% formaldehyde solution, heating to 85-88 ℃, reacting at a constant temperature for 1-2 h, and cooling to room temperature to obtain a third solution.
In this step, the fourth mass is 1.5% of the total mass of phenol and formaldehyde, and the fifth mass is 20% of the second mass. If the first molar amount and the second molar amount are 1mol and 3mol, respectively, the fourth mass in this step is 184.11g × 1.5%, that is, 2.76g, and 2.76g of a 40% sodium hydroxide solution is weighed.
The third solution obtained in the step is a brownish red transparent liquid completely dissolved in water, and the brownish red transparent liquid is water-soluble phenolic resin.
And 4, step 4: and adding a third solution with a third molar weight into the two-neck flask, adding a phenol solution with a concentration of 40% with a fourth molar weight under the stirring state, and continuously stirring for 10min to obtain the composite crosslinking agent.
In this step, the third molar amount may be set and changed as needed, for example, the third molar amount may be 1mol or 2mol. The fourth molar amount may also be set and changed as necessary, for example, the fourth molar amount is 1mol or 2mol. The two-neck flask can be a flask with a stirrer.
If the third molar amount is 1mol and the fourth molar amount is 2mol, the step may be: adding 1mol of phenolic resin into a two-neck flask with a stirrer, slowly adding 2mol of 40% phenol solution under stirring, continuing stirring for 10min, and finishing stirring to obtain the composite crosslinking agent.
In the examples of the present application, the ratio of the first molar amount to the second molar amount to the third molar amount to the fourth molar amount is 1.
It should be noted that the phenolic resin can resist high temperature, and the composite crosslinking agent prepared from the phenolic resin can resist high temperature even if the structural integrity and dimensional stability of the phenolic resin can be maintained at very high temperature. The composite cross-linking agent is mainly used for increasing the complexity of a profile control agent network structure.
Introduction of a crosslinking enhancer: in one possible implementation, the crosslinking enhancer is hexamethylenetetramine.
In the embodiment of the application, the hexamethylenetetramine is mainly used for enhancing the crosslinking reaction of the modified polyacrylamide and the composite crosslinking agent, so that the reaction is more complete.
Introduction of stabilizers: in one possible implementation, the stabilizer includes at least one of thiourea and sodium thiosulfate.
In this implementation, the stabilizer may be thiourea, sodium thiosulfate, or a mixture of thiourea and sodium thiosulfate. If the stabilizer is a mixture of thiourea and sodium thiosulfate, that is, the stabilizer comprises thiourea and sodium thiosulfate, the mass ratio of thiourea to sodium thiosulfate can be set and changed as required, for example, the mass ratio of thiourea to sodium thiosulfate is 1.
In the embodiment of the application, the thiourea and/or the sodium thiosulfate are mainly used for slowing down the degradation process of the profile control and flooding agent, prolonging the service life of the profile control and flooding agent and enhancing the plugging effect and the profile control and flooding benefit of the profile control and flooding agent.
In summary, the modifying and flooding agent provided by the embodiment of the application modifies polyacrylamide by introducing the functional monomer N-vinyl pyrrolidone, so that the steric hindrance effect of a side chain is increased, hydrolysis of an amide group in the polyacrylamide is inhibited, and the stability of the modifying and flooding agent is favorably improved; the complexity of a profile control agent network structure is increased by adding the composite cross-linking agent; by adding the stabilizer, the degradation process of the modifying and flooding agent is slowed down. The components play a synergistic cooperation role, so that the high temperature resistance of the profile control agent is improved.
The embodiment of the application provides a preparation method of a profile control agent, which comprises the following steps:
(1) According to the mass fraction of each component, 70% by volume of water is added into a reaction vessel.
The mass fraction of the modified polyacrylamide is 0.15% to 0.3%, for example, the mass fraction of the modified polyacrylamide is 0.2% to 0.3%. The mass fraction of the composite crosslinking agent is 0.15 to 0.35%, for example, the mass fraction of the composite crosslinking agent is 0.25 to 0.35%. The mass fraction of the crosslinking enhancer is 0.1% to 0.2%, for example, the mass fraction of the crosslinking enhancer is 0.12% to 0.2%. The mass fraction of the stabilizer is 0.02% to 0.05%, for example, the mass fraction of the stabilizer is 0.03% to 0.05%, and the balance is water.
(2) And (3) sequentially adding a stabilizer, a crosslinking enhancer and modified polyacrylamide into the reaction vessel, and adding the rest 30% by volume of water into the reaction vessel when all the components are completely dissolved.
In the step, firstly, adding the stabilizer into the reaction vessel, stirring until the stabilizer is completely dissolved, continuously adding the crosslinking enhancer into the reaction vessel, stirring until the crosslinking enhancer is completely dissolved, continuously adding the modified polyacrylamide into the reaction vessel while stirring until the modified polyacrylamide is completely dissolved, and then adding the water with the volume of the rest 30%.
(3) And adding the composite cross-linking agent into the reaction vessel, and obtaining a mixed solution after the composite cross-linking agent is completely dissolved.
And adding the composite cross-linking agent into the reaction vessel, and stirring until the composite cross-linking agent is completely dissolved to obtain a mixed solution.
(4) And (3) placing the mixed solution in a constant temperature box with the temperature of 100-130 ℃ for reaction for 5d to obtain the profile control and flooding agent.
And (3) placing the mixed solution in a constant temperature oven at 100-130 ℃ for 5 days to fully react to obtain the modifying and driving agent, wherein the modifying and driving agent is a yellowish, flowable and reboundable uniform gel-like agent.
The profile control agent provided by the embodiment of the application can be applied to oil reservoirs with the temperature not higher than 130 ℃, and particularly can ensure excellent gel forming strength, long-term stability and good injectability under the condition that the temperature is 100-130 ℃, so that the aim of improving the water drive development effect of high-temperature and ultrahigh-temperature oil reservoirs is fulfilled. The time of the cross-linking reaction is 72-120 h, and can be adjusted(ii) a The solution viscosity is 80-240 mPa.s, the viscosity is low, the fluidity is good, and the pump injection is easy; after being gelled at 100-130 ℃,7.34S-1The viscosity is 1500-3000 mPa.s under the shearing rate, the plugging capability is excellent, and the deep migration can be realized. In addition, the plugging agent can be placed at a constant temperature of 100-130 ℃, can be stabilized for 60-90 days, has a viscosity retention rate of 75% -95%, and can ensure a longer validity period, thereby improving the plugging effect and the profile control and flooding benefits.
The technical solution of the present application will be described in detail by specific embodiments below.
In the following examples, the operations referred to are those without the indications of conditions, and are carried out according to conventional conditions or conditions recommended by the manufacturer. The raw materials are conventional products which can be obtained commercially by manufacturers and specifications.
Example 1
1. Preparation of composite crosslinking agent
(1) Adding 1mol of phenol into a 250nL three-neck flask with a thermometer, a condenser pipe and a stirrer, and heating the mixture to 50 ℃ by using a constant-temperature water bath kettle to melt the mixture into liquid; starting stirring, slowly adding 40% sodium hydroxide solution with the mass of 1mol of phenol and 3mol of formaldehyde which is 3.5% of the total mass, keeping the temperature at 50 ℃, and reacting for 20min to obtain a first solution.
(2) Preparing 3mol of 36% formaldehyde solution, slowly dripping 80% of 36% formaldehyde solution into a three-neck flask within 20min, heating to 65 ℃, and stirring at constant temperature for 30min to obtain a second solution.
(3) And adding a 40% sodium hydroxide solution into the second solution, wherein the mass of the sodium hydroxide solution is 1.5% of the sum of the mass of 1mol of phenol and the mass of 3mol of formaldehyde, heating to 75 ℃, stirring at a constant temperature for reaction for 15min, adding the remaining 20% mass of 36% formaldehyde solution, slowly heating to 85-88 ℃, continuing the reaction at the constant temperature for 1-2 h, and cooling to room temperature to obtain a brownish red transparent liquid completely dissolved in water, namely the water-soluble phenolic resin.
(4) Adding 1mol of water-soluble phenolic resin into a 250mL two-neck flask with a stirrer, slowly adding 1mol of 40% phenol solution under stirring, continuing stirring for 10min, and obtaining the composite crosslinking agent after the stirring is finished.
2. Preparing profile control agent
(1) 70mL of clear water was added to the beaker and 0.03g of thiourea, or 0.03g of sodium thiosulfate, or 0.015g of thiourea and 0.015g of sodium thiosulfate were added.
(2) Adding 0.12g of hexamethylenetetramine, stirring until the hexamethylenetetramine is completely dissolved, slowly adding 0.2g of modified polyacrylamide into the water while stirring until the modified polyacrylamide is completely dissolved, adding 30mL of clear water again, and stirring uniformly.
(3) 0.25g of composite cross-linking agent is added and stirred evenly to obtain a mixed solution.
(4) And (3) placing the mixed solution in a constant temperature box at 100 ℃ for 5 days to fully react to finally obtain the profile control and flooding agent.
Example 2
1. Preparation of composite crosslinking agent
The preparation method of the composite cross-linking agent in this embodiment is the same as that of the composite cross-linking agent in embodiment 1, and is not described herein again.
2. Preparing profile control agent
(1) 70mL of clear water was added to the beaker and 0.03g of thiourea, alternatively 0.03g of sodium thiosulfate, alternatively 0.015g of thiourea and 0.015g of sodium thiosulfate were added.
(2) Adding 0.12g of hexamethylenetetramine, stirring until the hexamethylenetetramine is completely dissolved, slowly adding 0.2g of modified polyacrylamide into water while stirring until the modified polyacrylamide is completely dissolved, adding 30mL of clear water again, and stirring uniformly.
(3) 0.25g of composite cross-linking agent is added and stirred evenly to obtain a mixed solution.
(4) And (3) placing the mixed solution in a thermostat with the temperature of 115 ℃ for 5d to enable the mixed solution to react fully, and finally obtaining the profile control agent.
Example 3
1. Preparation of composite crosslinking agent
(1) Adding 1mol of phenol into a 250nL three-neck flask with a thermometer, a condenser and a stirrer, heating to 50 ℃ by using a constant-temperature water bath kettle, and melting into liquid; starting stirring, slowly adding 40% sodium hydroxide solution with the mass being 3.5% of the sum of 1mol of phenol and 3mol of formaldehyde, keeping the temperature at 50 ℃, and reacting for 20min to obtain a first solution.
(2) Preparing 3mol of 36% formaldehyde solution, slowly dripping 80% of 36% formaldehyde solution into a three-neck flask within 20min, heating to 65 ℃, and stirring at constant temperature for 30min to obtain a second solution.
(3) And adding a 40% sodium hydroxide solution into the second solution, wherein the mass of the sodium hydroxide solution is the sum of the mass of 1mol of phenol and the mass of 3mol of formaldehyde, heating to 75 ℃, stirring at constant temperature for reaction for 15min, adding the remaining 20% mass of 36% formaldehyde solution, slowly heating to 85-88 ℃, continuing the reaction at constant temperature for 1-2 h, and cooling to room temperature to obtain a brownish red transparent liquid completely dissolved in water, namely the water-soluble phenolic resin.
(4) Adding 1mol of water-soluble phenolic resin into a 250mL two-neck flask with a stirrer, slowly adding 2mol of 40% phenol solution under stirring, continuing stirring for 10min, and obtaining the composite crosslinking agent after the stirring is finished.
2. Preparing profile control agent
(1) 70mL of clear water was added to the beaker, and 0.05g of thiourea, alternatively 0.05g of sodium thiosulfate, alternatively 0.025g of thiourea and 0.025g of sodium thiosulfate were added.
(2) Adding 0.2g of hexamethylenetetramine, stirring until the hexamethylenetetramine is completely dissolved, slowly adding 0.3g of modified polyacrylamide into water while stirring until the modified polyacrylamide is completely dissolved, adding 30mL of clear water again, and stirring uniformly.
(3) And adding 0.35g of composite cross-linking agent, and uniformly stirring to obtain a mixed solution.
(4) And (3) placing the mixed solution in a constant temperature box at 130 ℃ for 5d to fully react to finally obtain the profile control agent.
Application example 1
This application example was conducted mainly to evaluate the viscosity of the flooding agent provided in examples 1 to 3.
Referring to tables 1-3, respectively, table 1 shows the viscosity of the profile control agent provided in example 1 as a function of time at 100 deg.C, table 2 shows the viscosity of the profile control agent provided in example 2 as a function of time at 115 deg.C, and Table 3 shows the viscosity of the profile control agent provided in example 3 as a function of time at 130 deg.C.
TABLE 1 viscosity of the profile control agent provided in example 1 as a function of time at 100 deg.C
TABLE 2 viscosity of the profile control agent provided in example 2 as a function of time at 115 deg.C
TABLE 3 viscosity of the profile control agent provided in example 3 as a function of time at 130 deg.C
The viscosity change of the profile control agent can be seen from tables 1 to 3: the profile control agent prepared in the examples 1-3 can be suitable for profile control treatment of oil reservoirs at 100-130 ℃, and the profile control agent has good gelling performance under high temperature. Moreover, the initial viscosity of the profile control agent is not more than 240 mPas, and the fluidity is excellent. The viscosity rises slowly in 24h and rises rapidly in the range of 72-120 h, and the good injection property and deep migration capability of the profile control agent can be ensured. In addition, the profile control agent can be effectively crosslinked under high temperature, the viscosity is 1900-2600 mPa.s after complete crosslinking, the strength is enough to block a high-seepage channel, and the profile control agent can continuously move to a deep part along with the injection of subsequent fluid, so that the deep treatment of an oil reservoir is realized. Moreover, the profile control agent can be stabilized for 60-90 days at 100-130 ℃, the viscosity retention rate is more than 75%, and the high-permeability channel can be effectively blocked for a long time, so that the fluid is forced to turn to a low-permeability area to displace residual oil.
Application example 2
The application example mainly evaluates the application of the profile control agent provided in example 3 in 62 fault blocks left in the north China oilfield.
The 62 broken blocks left in the North China oilfield are multilayer, high-temperature (115-120 ℃) and low-permeability (12-41 multiplied by 10)-3μm2) The main oil-containing layer of the complex sandstone reservoir is from three sections of the lower third series Dongying group to one section of the sandstone river street group. The oil layer distribution in the longitudinal direction is dispersed, the heterogeneity in the layer and the plane is strong, the difference of permeability is large, and the extraction degree is high (31.5%). After water injection development for many years, the reserved 62 broken blocks enter the development stage of high water content and high extraction, a large amount of injected water is washed in the stratum for a long time to form a water channeling large pore passage, the water content rises quickly, and the yield decreases quickly.
On site, 5-mouth water well is used for cumulatively injecting the profile control agent 44150m provided in example 33. After the profile control is carried out for 2 months, the trend of rapid yield decline is gradually inhibited. Referring to table 4, table 4 shows the oil and water production of each well after the profile control agent was added.
TABLE 4 oil and Water production for each well after addition of profile control agent
As can be seen from table 4: corresponding to 16 mouths of an oil well, the efficiency is 100%, daily oil production is increased from 41.6t to 65.8t, comprehensive water content is reduced from 89.3% to 81.4%, and oil is increased by 16603t. The effective period reaches 24 months, and the medicine is still in a continuous effective stage at present.
Referring to fig. 1, the shaded area in fig. 1 is the stage of adding the profile control agent, and it can be seen from fig. 1 that: in the stage of adding the profile control agent, the daily injection amount is basically kept unchanged, the daily oil yield is increased, and the water content is reduced, which shows that the oil yield is really increased after the profile control agent is added, and simultaneously shows that the profile control agent can effectively block a high-permeability channeling passage, so that the subsequent fluid is diverted to a low-permeability area, and the swept volume is enlarged.
The above description is only for facilitating the technical solution of the present application to be understood by those skilled in the art, and is not intended to limit the present application. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. The modifying and flooding agent is characterized by comprising the following components in parts by mass: 0.15 to 0.3 percent of modified polyacrylamide, 0.15 to 0.35 percent of composite cross-linking agent, 0.1 to 0.2 percent of cross-linking enhancer, 0.02 to 0.05 percent of stabilizer and the balance of water;
the modified polyacrylamide is a product obtained by the reaction of acrylamide and N-vinyl pyrrolidone.
2. The profile-controlling agent according to claim 1, wherein the modified polyacrylamide is prepared according to the following preparation method:
dissolving acrylamide and N-vinyl pyrrolidone in a deionized water-ethanol solution, adding an initiator, and reacting in a constant-temperature water bath at 70 ℃ for 8 hours to obtain a reaction solution;
adding isopropanol into the reaction solution to generate a precipitate, filtering and drying to obtain the modified polyacrylamide.
3. The profile control agent and flooding agent according to claim 2, characterized in that the acrylamide has a degree of hydrolysis of 23-30% and a molecular weight of not less than 2500 ten thousand.
4. The profile control agent and flooding agent according to claim 1, wherein the composite cross-linking agent is prepared according to the following preparation method:
adding phenol with a first molar weight into a three-neck flask, heating to 50 ℃ in a constant-temperature water bath kettle, adding a first mass of 40% sodium hydroxide solution under a stirring state, and reacting at the constant temperature of 50 ℃ for 20min to obtain a first solution;
preparing a second molar mass of 36% formaldehyde solution to obtain a second mass of formaldehyde solution, adding a third mass of 36% formaldehyde solution into the three-neck flask within 20min, heating to 65 ℃, and stirring at a constant temperature for 30min to obtain a second solution, wherein the third mass is 80% of the second mass;
adding a sodium hydroxide solution with the concentration of 40% in a fourth mass into the second solution, heating to 75 ℃, stirring at constant temperature for 15min, adding a formaldehyde solution with the concentration of 36% in a fifth mass, heating to 85-88 ℃, reacting at constant temperature for 1-2 h, and cooling to room temperature to obtain a third solution, wherein the fifth mass is 20% of the second mass;
and adding a third solution with a third molar weight into the two-neck flask, adding a phenol solution with a concentration of 40% with a fourth molar weight under a stirring state, and continuously stirring for 10min to obtain the composite crosslinking agent.
5. The profile control agent according to claim 4, wherein the ratio of the first molar amount, the second molar amount, the third molar amount and the fourth molar amount is 1.
6. The profile-controlling agent according to claim 4, wherein said first mass is 3.5% of the sum of a sixth mass and a seventh mass, said sixth mass being the mass corresponding to said first molar amount of phenol, and said seventh mass being the mass corresponding to said second molar amount of formaldehyde;
the fourth mass is 1.5% of the sum of the sixth mass and the seventh mass.
7. The profile-controlling agent according to claim 1, wherein said crosslinking enhancer is hexamethylenetetramine.
8. The profile control agent according to claim 1, wherein said stabilizer comprises at least one of thiourea and sodium thiosulfate.
9. The profile-controlling agent according to claim 8, wherein if the stabilizer comprises thiourea and sodium thiosulfate, the mass ratio of the thiourea to the sodium thiosulfate is 1.
10. The method for preparing the profile-controlling agent of any one of claims 1 to 9, wherein the preparation method comprises the following steps:
adding 70% by volume of water into a reaction vessel according to the mass fraction of each component;
sequentially adding a stabilizer, a crosslinking enhancer and modified polyacrylamide into the reaction container, and adding the rest 30% by volume of water into the reaction container when all the components are completely dissolved;
adding a composite cross-linking agent into the reaction container, and obtaining a mixed solution after the composite cross-linking agent is completely dissolved;
and placing the mixed solution in a thermostat with the temperature of 100-130 ℃ for reaction for 5d to obtain the profile control agent.
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