CN113201105B - Interface active type core-shell microsphere for oil extraction and preparation method thereof - Google Patents
Interface active type core-shell microsphere for oil extraction and preparation method thereof Download PDFInfo
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- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/584—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 surfactants
Abstract
The invention discloses an interface active type core-shell microsphere for oil extraction and a preparation method thereof2The core-shell structure (inorganic SiO) with interface activity is prepared by the dispersion polymerization of an alcohol-water system as a raw material2Core/copolymer shell) microspheres. The microsphere is nano-scale, can be expanded by 5-6 times to micron scale when meeting water, and can be used for profile control and flooding of oil fields.
Description
Technical Field
The invention belongs to the technical field of petroleum industry, and particularly relates to an interface active type core-shell microsphere for oil extraction and a preparation method thereof.
Background
In the long-term water injection development process of the oil field, due to the fact that underground crude oil is large in viscosity and the stratum is serious in heterogeneity, the water injection effect of a part of water injection development well groups is poor, and contradictions between layers in the stratum are increasingly prominent. In order to improve the water injection development effect in these areas and increase the injection water spread coefficient, deep profile control and flooding of the water injection well are required. The polymer microsphere is an elastic microsphere synthesized by a specific polymerization technology, and is used for deep profile control and flooding of an oil field to expand injected water wave and volume, block large pore channels formed in the middle and later stages of development of the oil field, change the direction of liquid flow, improve the utilization rate of injected water and improve the development effect of water flooding due to the characteristics of controllable size, good dispersibility in water, easy access to deep stratum, water swelling at oil reservoir temperature and the like. The main polymerization modes for preparing the polymer microspheres at present are inverse emulsion polymerization and dispersion polymerization, the particle size of the microspheres can be regulated and controlled within the range from nanometer to millimeter, but the prepared microspheres are expanded in water to form polymer gel, and the compression strength or the shear strength is not enough, and the functions of the microspheres are single. Therefore, the research on the core-shell microspheres with higher strength and certain functions has important production significance for oil field profile control and flooding.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an interface active type core-shell microsphere for oil extraction and a preparation method thereof.
The invention is realized by the following technical scheme:
an interface active type core-shell microsphere for oil extraction is prepared by the following steps:
preparation of block polyether macromonomer
Adding isobutene alcohol and a catalyst potassium hydroxide into a closed high-temperature high-pressure reaction kettle, starting stirring, heating to 120 ℃, stopping heating, dropwise adding ethylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be below 0.4MPa, and reacting for 30min after the pressure returns after the materials are reacted to reduce the pressure to 0 MPa; then, dripping propylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be less than 0.4MPa, reacting for 30min after the pressure is returned after the materials are reacted, reducing the pressure to be 0MPa, and finally cooling, opening the kettle and discharging to obtain the diblock polyether macromonomer taking the isobutenol as an initiator.
Second, modified nano SiO2Preparation of
Preparing ethanol/water mixed solvent, and then preparing 0.05g/mL hydrophilic nano SiO by using the mixed solvent2Carrying out ultrasonic dispersion on the solution for 1 h; then adding a silane coupling agent with the mass ratio of 1:2 to the silicon dioxide, reacting for 12 hours at 80 ℃, and then performing centrifugal separation; washing with ethanol for more than 3 times, removing, and vacuum drying to obtain modified nanometer SiO2。
Preparation of interface active type core-shell structure microsphere
Firstly, weighing ethanol/water solution in a beaker, adding modified nano SiO2Ultrasonic dispersion for 30 min; then, weighing dispersant polyvinylpyrrolidone and cross-linking agent N, N-methylene bisacrylamide, adding the mixture into a beaker, and uniformly stirring; pouring the solution in the beaker into a three-necked bottle, heating to 55 ℃, adding acrylamide and a block polyether macromonomer, stirring for dissolving, and introducing nitrogen to remove oxygen; and finally, weighing initiator ammonium persulfate, dissolving the initiator ammonium persulfate by using a small amount of water, adding the initiator ammonium persulfate into a three-necked bottle, starting timing, and reacting for 10 hours. After the reaction, a white emulsion sample is obtained。
In the technical scheme, in the first step, nitrogen is used for purging and replacing before temperature rising, then vacuum pumping is carried out, and the operations of purging and replacing with nitrogen and then vacuum pumping are repeated at least twice.
In the technical scheme, in the first step, the mass ratio of the isobutylene alcohol to the ethylene oxide is 1:50, the mass ratio of the isobutylene alcohol to the propylene oxide is 1:32.5, and the addition amount of the potassium hydroxide is 0.3 percent of the total mass of the ethylene oxide and the propylene oxide.
In the above technical solution, in the second step, the pH of the ethanol/water mixed solvent is 5, and the volume ratio of ethanol to water is 99: 1.
In the above technical scheme, in the second step, the silane coupling agent used is KH 570.
In the technical scheme, in the third step, the volume ratio of the ethanol to the water in the ethanol/water solution is 1: 1.
In the technical scheme, in the third step, the mass ratio of the acrylamide to the block polyether macromonomer is in the range of 9:1 to 6:4, and preferably 7: 3.
In the technical scheme, in the third step, the total mass fraction of the acrylamide and the block polyether macromonomer is within the range of 12 wt% -20 wt%, and 16 wt% is preferred.
In the technical scheme, in the third step, the mass fraction of the addition amount of the cross-linking agent is in the range of 0.024 wt% to 0.054 wt%, and is preferably 0.048 wt%.
In the technical scheme, in the third step, SiO is modified2The amount added is in the range of 0.1 to 0.5 wt%, preferably 0.3 wt%.
In the technical scheme, in the third step, the mass fraction of the added modified dispersant is 2.4 wt%, and the added amount of the initiator is 0.8 wt% of the total mass of all monomers.
The invention has the advantages and beneficial effects that: the invention uses acrylamide, block polyether macromonomer and modified SiO with double bond on the surface2The core-shell structure (inorganic SiO) with interface activity is prepared by the dispersion polymerization of an alcohol-water system as a raw material2Core/copolymer shell) microspheres. The microsphere of the invention is nano-scale, and can be expanded when meeting water 56 times to micron level, and can be used for profile control and flooding of oil fields.
Drawings
FIG. 1 shows the reaction scheme of the present invention.
FIG. 2a is a transmission electron microscope observation image of core-shell microspheres (I).
FIG. 2b is the transmission electron microscope observation image of the core-shell microsphere (II).
FIG. 3a is a microscope picture of core-shell microspheres expanded for 0 day.
FIG. 3b is a microscope picture of core-shell microspheres expanded for 18 days.
FIG. 4 is a schematic diagram showing the measurement results of the interfacial activity of the interfacial-active core-shell microspheres.
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
EXAMPLE 1 preparation of Block polyether macromonomer
10g of isobutene alcohol and 2.4g of potassium hydroxide are added into a high-temperature high-pressure reaction kettle, and the reaction kettle is sealed. Purging and replacing by using nitrogen before heating, vacuumizing by using a vacuum pump, repeating twice, starting stirring and heating, stopping heating when the temperature is raised to 120 ℃, opening a feed valve, dropwise adding 500g of ethylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be below 0.4MPa, and reacting for 30min after the pressure is returned after the materials are reacted to reduce the pressure to 0 MPa; then 325g of propylene oxide is dripped, the reaction temperature is controlled not to exceed 140 ℃, the pressure is controlled to be below 0.4MPa, and the reaction is carried out for 30min after the pressure returns after the materials are reacted, so that the pressure is reduced to 0 MPa; finally cooling and opening the kettle, and discharging to obtain the block polyether macromonomer.
Example 2 modified SiO2Preparation of
Preparing 200mL of ethanol/water mixed solvent with pH of 5 (the volume ratio of ethanol to water is 99: 1); 10g of hydrophilic nano SiO is added into the mixture2Ultrasonically dispersing for 1 h; then adding 5g of silane coupling agent, reacting for 12h at 80 ℃, and then performing centrifugal separation; washing with ethanol for more than 3 times, removing, and vacuum drying to obtain modified nanometer SiO2。
EXAMPLE 3 preparation of interface-active core-Shell microspheres
Firstly, 75g of ethanol/water solution with the volume ratio of 1:1 is weighed into a beaker, and 0.3g of modified SiO is added2Ultrasonic dispersion for 30 min; then, 2.4g of polyvinylpyrrolidone and 0.128g of N, N-methylene bisacrylamide are weighed and added into a beaker to be uniformly stirred; pouring the solution in the beaker into a three-necked bottle, heating to 55 ℃, adding 14.4g of AM and 1.6g of PEP (the mass ratio of AM to PEP is 9:1), supplementing water until the total mass is 100g, stirring for dissolving, and introducing nitrogen for 10min to remove oxygen; finally, 0.128g of APS was weighed into a three-necked flask, and the reaction was started for 10 hours. After the reaction was complete, a white emulsion sample was obtained.
Example 4 preparation of interface-active core-shell microspheres
Firstly, 75g of ethanol/water solution with the volume ratio of 1:1 is weighed into a beaker, and 0.3g of modified SiO is added2Ultrasonic dispersion for 30 min; then, 2.4g of polyvinylpyrrolidone and 0.128g of N, N-methylene bisacrylamide are weighed and added into a beaker to be uniformly stirred; pouring the solution in the beaker into a three-necked bottle, heating to 55 ℃, adding 12.8g of AM and 3.2g of PEP (the mass ratio of AM to PEP is 8:2), supplementing water to 100g of total mass, stirring for dissolving, and introducing nitrogen for 10min to remove oxygen; finally, 0.128g of APS was weighed into a three-necked flask, and the reaction was started for 10 hours. After the reaction was complete, a white emulsion sample was obtained.
Example 5 preparation of interface-active type core-shell microspheres
Firstly, 75g of ethanol/water solution with the volume ratio of 1:1 is weighed into a beaker, and 0.3g of modified SiO is added2Ultrasonic dispersion for 30 min; then, 2.4g of polyvinylpyrrolidone and 0.128g of N, N-methylene bisacrylamide are weighed and added into a beaker to be uniformly stirred; put in a beakerPouring the solution into a three-necked bottle, heating to 55 ℃, adding 11.2g of AM and 4.8g of PEP (the mass ratio of AM to PEP is 7:3), supplementing water until the total mass is 100g, stirring for dissolving, and introducing nitrogen for 10min to remove oxygen; finally, 0.128g of APS was weighed into a three-necked flask, and the reaction was started for 10 hours. After the reaction was complete, a white emulsion sample was obtained.
Example 6 preparation of interface-active core-shell microspheres
Firstly, 75g of ethanol/water solution with the volume ratio of 1:1 is weighed into a beaker, and 0.3g of modified SiO is added2Ultrasonic dispersion for 30 min; then, 2.4g of polyvinylpyrrolidone and 0.128g of N, N-methylene bisacrylamide are weighed and added into a beaker to be uniformly stirred; pouring the solution in the beaker into a three-necked bottle, heating to 55 ℃, adding 12.6g of AM and 5.4g of PEP (monomer concentration is 18%), supplementing water to 100g of total mass, stirring for dissolving, and introducing nitrogen for 10min to remove oxygen; finally, 0.128g of APS was weighed into a three-necked flask, and the reaction was started for 10 hours. After the reaction was complete, a white emulsion sample was obtained.
Example 7 preparation of interface-active core-shell microspheres
Firstly, 75g of ethanol/water solution with the volume ratio of 1:1 is weighed into a beaker, and 0.3g of modified SiO is added2Ultrasonic dispersion for 30 min; then, 2.4g of polyvinylpyrrolidone and 0.128g of N, N-methylene bisacrylamide are weighed and added into a beaker to be uniformly stirred; pouring the solution in the beaker into a three-necked bottle, heating to 55 ℃, adding 14g of AM and 6g of PEP (monomer concentration is 18%), supplementing water to 100g of total mass, stirring for dissolving, and introducing nitrogen for 10min to remove oxygen; finally, 0.128g of APS was weighed into a three-necked flask, and the reaction was started for 10 hours. After the reaction was complete, a white emulsion sample was obtained.
Example 8 measurement of particle diameter of interface-active core-shell microspheres
The samples of examples 3 to 6 were dispersed in pure water and their median particle size was determined by dynamic light scattering, the results of which are shown in the following table. The results show that the nano-scale microspheres can be prepared.
| Sample (I) | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 |
| Median particle size (nm) | 1231 | 719 | 646 | 752 | 1211 |
Example 9 measurement of interfacial Activity of interface-active core-shell microspheres
Solutions of microspheres (example 5) of different concentrations were prepared and the oil-water interfacial tension (crude oil density 0.9365 g/cm) was measured at 55 ℃3) The results are shown in FIG. 4 below. The result shows that the microsphere can reduce the oil-water interfacial tension to 10-1And (4) stage.
In conclusion, acrylamide, a block polyether macromonomer and modified SiO with double bonds on the surface2The interface active type core-shell structure (inorganic SiO) can be prepared by the dispersion polymerization of an alcohol-water system as a raw material2Core/copolymer shell) microspheres.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (8)
1. An interface active type core-shell microsphere for oil extraction is characterized by being prepared by the following steps:
preparation of block polyether macromonomer
Adding isobutene alcohol and a catalyst potassium hydroxide into a closed high-temperature high-pressure reaction kettle, starting stirring, heating to 120 ℃, stopping heating, dropwise adding ethylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be below 0.4MPa, and reacting for 30min after the pressure returns after the materials are reacted to reduce the pressure to 0 MPa; then dripping propylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be less than 0.4MPa, reacting for 30min after the pressure is returned after the materials are reacted, reducing the pressure to 0MPa, and finally cooling, opening the kettle and discharging to obtain the diblock polyether macromonomer taking the isobutenol as an initiator;
second, modified nano SiO2Preparation of
Preparing ethanol/water mixed solvent, and then preparing 0.05g/mL hydrophilic nano SiO by using the mixed solvent2Carrying out ultrasonic dispersion on the solution for 1 h; then adding a silane coupling agent with the mass ratio of 1:2 to the silicon dioxide, wherein the silane coupling agent is KH570, reacting for 12 hours at the temperature of 80 ℃, and then performing centrifugal separation; washing with ethanol for more than 3 times, removing, and vacuum drying to obtain modified nanometer SiO2；
Preparation of interface active type core-shell structure microsphere
Firstly, weighing ethanol/water solution in a beaker, adding the modified nano SiO2Ultrasonic dispersion for 30 min; then, weighing dispersant polyvinylpyrrolidone and cross-linking agent N, N-methylene bisacrylamide, adding the mixture into a beaker, and uniformly stirring; pouring the solution in the beaker into a three-necked bottle, heating to 55 ℃, adding acrylamide and the block polyether macromonomer, stirring for dissolving, and introducing nitrogen to remove oxygen; and finally, weighing initiator ammonium persulfate, dissolving the initiator ammonium persulfate by using a small amount of water, adding the initiator ammonium persulfate into a three-necked bottle, starting timing, reacting for 10 hours, and obtaining a white emulsion sample after the reaction is finished.
2. The interface active type core-shell microsphere for oil recovery according to claim 1, characterized in that: in the first step, nitrogen is used for purging and replacing before temperature rising, then vacuum pumping is carried out, and the operations of purging and replacing with nitrogen and then vacuum pumping are repeated for at least two times; the mass ratio of the isobutylene alcohol to the ethylene oxide was 1:50, the mass ratio of the isobutylene alcohol to the propylene oxide was 1:32.5, and the amount of potassium hydroxide added was 0.3% of the total mass of the ethylene oxide and the propylene oxide.
3. The interface active type core-shell microsphere for oil recovery according to claim 1, characterized in that: in the second step, the ethanol/water mixed solvent has a pH of 5, and the volume ratio of ethanol to water is 99: 1.
4. The interface active type core-shell microsphere for oil recovery according to claim 1, characterized in that: in the third step, the volume ratio of the ethanol to the water in the ethanol/water solution is 1: 1; the mass ratio of acrylamide to block polyether macromonomer is in the range of 9:1 to 6: 4.
5. A preparation method of interface active type core-shell microspheres for oil extraction is characterized by comprising the following steps:
preparation of block polyether macromonomer
Adding isobutene alcohol and a catalyst potassium hydroxide into a closed high-temperature high-pressure reaction kettle, starting stirring, heating to 120 ℃, stopping heating, dropwise adding ethylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be below 0.4MPa, and reacting for 30min after the pressure returns after the materials are reacted to reduce the pressure to 0 MPa; then, dripping propylene oxide, controlling the reaction temperature to be not more than 140 ℃ and the pressure to be below 0.4MPa, reacting for 30min after the pressure returns after the materials are reacted, reducing the pressure to 0MPa, and finally cooling and opening the kettle for discharging to obtain a diblock polyether macromonomer taking the isobutenol as an initiator;
second, modified nano SiO2Preparation of
Preparing ethanol/water mixed solvent, and then preparing 0.05g/mL hydrophilic nano SiO by using the mixed solvent2Carrying out ultrasonic dispersion on the solution for 1 h; then adding a silane coupling agent with the mass ratio of 1:2 to the silicon dioxide, wherein the silane coupling agent is KH570, reacting at 80 ℃ for 12H, and then performing centrifugal separation; washing with ethanol for more than 3 times, removing, and vacuum drying to obtain modified nanometer SiO2；
Preparation of interface active type core-shell structure microsphere
Firstly, weighing ethanol/water solution in a beaker, adding the modified nano SiO2Ultrasonic dispersion for 30 min; then, weighing dispersant polyvinylpyrrolidone and cross-linking agent N, N-methylene bisacrylamide, adding the mixture into a beaker, and uniformly stirring; pouring the solution in the beaker into a three-necked bottle, heating to 55 ℃, adding acrylamide and the block polyether macromonomer, stirring for dissolving, and introducing nitrogen to remove oxygen; and finally, weighing initiator ammonium persulfate, dissolving the initiator ammonium persulfate by using a small amount of water, adding the initiator ammonium persulfate into a three-necked bottle, starting timing, reacting for 10 hours, and obtaining a white emulsion sample after the reaction is finished.
6. The preparation method of the interface active type core-shell microsphere for oil recovery according to claim 1, characterized in that: in the first step, nitrogen is used for purging and replacing before temperature rising, then vacuum pumping is carried out, and the operations of purging and replacing with nitrogen and then vacuum pumping are repeated for at least two times; the mass ratio of the isobutylene alcohol to the ethylene oxide was 1:50, the mass ratio of the isobutylene alcohol to the propylene oxide was 1:32.5, and the amount of potassium hydroxide added was 0.3% of the total mass of the ethylene oxide and the propylene oxide.
7. The preparation method of the interface active type core-shell microsphere for oil recovery according to claim 1, characterized in that: in the second step, the ethanol/water mixed solvent has a pH of 5, and the volume ratio of ethanol to water is 99: 1.
8. The preparation method of the interface active type core-shell microsphere for oil recovery according to claim 1, characterized in that: in the third step, the volume ratio of the ethanol to the water in the ethanol/water solution is 1: 1; the mass ratio of acrylamide to block polyether macromonomer is in the range of 9:1 to 6: 4.
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| CN106833575A (en) * | 2016-12-28 | 2017-06-13 | 浙江海洋大学 | A kind of composition polymer microballoon of core shell structure and preparation method thereof |
| CN110041474A (en) * | 2019-04-15 | 2019-07-23 | 中国海洋石油集团有限公司 | A kind of hybrid cation reverse-phase emulsifier and the preparation method and application thereof |
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| CN106833575A (en) * | 2016-12-28 | 2017-06-13 | 浙江海洋大学 | A kind of composition polymer microballoon of core shell structure and preparation method thereof |
| CN110041474A (en) * | 2019-04-15 | 2019-07-23 | 中国海洋石油集团有限公司 | A kind of hybrid cation reverse-phase emulsifier and the preparation method and application thereof |
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