CN110980718A - Modified graphene oxide and preparation method and application thereof - Google Patents
Modified graphene oxide and preparation method and application thereof Download PDFInfo
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Abstract
The application discloses a modified graphene oxide, a preparation method and an application thereof. The modified graphene oxide is obtained by chemically grafting an amphiphilic polymer and graphene oxide. According to the invention, an amphiphilic polymer is grafted to one end of graphene oxide by a one-step method to obtain graphene oxide with good amphiphilic performance, the graphene oxide has lower surface tension, the interfacial tension between water and kerosene is reduced, the emulsifying effect is good, and the average oil displacement rate is 10%.
Description
Technical Field
The application relates to modified graphene oxide, and belongs to the technical field of thickened oil exploitation.
Background
After primary oil recovery and secondary oil recovery, over 50% of the oil reserves are still reserved underground. China is the market with the greatest global demand for petrochemical products, and the dependence on imported products is higher and higher due to the capacity limitation of China; the development of an efficient and environment-friendly oil displacement agent for three-extraction of petroleum is an urgent strategic demand for realizing national energy safety in China.
With the less and less recoverable amount of the conventional oil reservoir, the oil extraction direction gradually develops towards the direction of unconventional oil reservoirs such as high-temperature high-salinity, ultra-low permeability and heavy oil. For heavy oil reservoirs, the steam huff and puff technology mainly adopted at present has high cost (more than 80 ten thousand yuan) in a single measure, and after multiple rounds of huff and puff, the oil reservoir has serious steam channeling, the water content is increased, the oil extraction yield is reduced rapidly, and the oil extraction effect is obviously reduced.
The thick oil component contains a plurality of heavy components, and the mutual force among the heavy components makes the viscosity reduction difficult to realize in the prior art. The chemical flooding is generally compounded by adopting various surfactants, so that the cost is higher, and the chemical flooding is easy to precipitate under the condition of high salt. Therefore, the development of a novel viscosity reducer for thick oil is a problem which needs to be solved urgently at present.
Disclosure of Invention
According to one aspect of the application, the modified graphene oxide is a nano material with a large specific surface area, the surface of the modified graphene oxide contains various polar functional groups, and amphiphilic modification can be performed on the graphene oxide, so that the effects of improving the oil quality of thick oil and emulsifying and viscosity reduction are achieved, and the recovery ratio of the thick oil is further improved.
The modified graphene oxide is obtained by chemically grafting an amphiphilic polymer and graphene oxide.
Optionally, the amphiphilic polymer chains are grafted on both sides of the graphene oxide layer.
According to another aspect of the present application, there is also provided a preparation method of any one of the above modified graphene oxides, wherein a mixture containing graphene oxide and an amphiphilic polymer is reacted in the presence of a carboxyl activating agent to obtain the modified graphene oxide.
The carboxyl activator is used for activating carboxyl in graphene oxide.
Optionally, the amphiphilic polymer comprises at least one of rhamnolipids, polyoxyethylene polyoxypropylene ether block copolymers, polyoxypropylene polyoxyethylene block copolymers.
Optionally, the carboxyl activating agent comprises at least one of carbodiimide, 4-dimethylaminopyridine, dicyclohexylcarbodiimide.
Optionally, the carboxyl activating agent is a mixture of carbodiimide and 4-dimethylaminopyridine;
the mass ratio of the carbodiimide to the 4-dimethylaminopyridine is 2.5-10.
Specifically, the upper limit of the mass ratio of carbodiimide to 4-dimethylaminopyridine is independently selected from 3, 5, 7, 10; the lower limit of the mass ratio of carbodiimide to 4-dimethylaminopyridine is independently selected from 2.5, 3, 5, 7.
Optionally, the reaction conditions are: the reaction temperature is 15-30 ℃; the reaction time is 3-5 h.
Specifically, the upper limit of the reaction temperature is independently selected from 20 ℃, 25 ℃, 30 ℃; the lower limit of the reaction temperature is independently selected from 15 ℃, 20 ℃, 25 ℃.
The upper limit of the reaction time is independently selected from 4h, 5 h; the lower limit of the reaction time is independently selected from 3h and 5 h.
Optionally, the preparation method comprises at least the following steps:
a) obtaining graphene oxide with the particle size of 50-150 nm;
b) obtaining a mixture containing the graphene oxide and an amphiphilic polymer;
c) and adding a carboxyl activating agent into the mixture, and reacting to obtain the modified graphene oxide.
Optionally, the step a) comprises: and ultrasonically shearing and centrifuging the graphene oxide dispersion liquid I to obtain the graphene oxide with the particle size of 50-150 nm.
Specifically, the upper limit of the particle size of the graphene oxide is independently selected from 60nm, 80nm, 100nm, 130nm, 150 nm; the lower limit of the particle size of the graphene oxide is independently selected from 50nm, 60nm, 80nm, 100nm and 130 nm.
Optionally, the concentration of the graphene oxide dispersion liquid I is 2-3 mg/mL;
the ultrasonic shearing time is 3-5 h;
the centrifugal speed is 3000-5000 rpm;
the centrifugation time is 10-30 min.
Optionally, the step b) comprises: dissolving the graphene oxide obtained in the step a) in water to obtain a graphene oxide dispersion liquid II, adding an amphiphilic polymer into the graphene oxide dispersion liquid II, and performing ultrasonic stirring in a water bath to obtain the mixture.
Optionally, the concentration of the graphene oxide dispersion liquid II is 1-2 mg/mL;
the mass ratio of the graphene oxide to the amphiphilic polymer is 0.01-0.1;
and the water bath ultrasonic stirring time is 30-60 min.
Specifically, the upper limit of the mass ratio of graphene oxide to amphiphilic polymer is independently selected from 0.05, 0.075, 0.1; the lower limit of the mass ratio of graphene oxide to amphiphilic polymer is independently selected from 0.01, 0.02, 0.03.
Optionally, in the step c), the mass ratio of the carboxyl activating agent to the graphene oxide in the step b) is 3-12.
Specifically, the upper limit of the mass ratio of the carboxyl activating agent to the graphene oxide is independently selected from 5, 7, 10, 12; the lower limit of the mass ratio of the carboxyl activating agent to the graphene oxide is independently selected from 3, 5, 7, 10.
According to another aspect of the application, an oil displacement agent is also provided, and the oil displacement agent comprises the modified graphene oxide described in any one of the above and/or the modified graphene oxide obtained by the preparation method described in any one of the above.
In this application, "carbodiimide" is abbreviated as EDC; "4-dimethylaminopyridine" is abbreviated DMAP;
"polyoxyethylene polyoxypropylene ether block copolymer" is abbreviated as F127;
"polyoxypropylene polyoxyethylene block copolymers" are abbreviated as F108;
"rhamnolipid" is Rha.
The beneficial effects that this application can produce include:
1) according to the preparation method, the amphiphilic polymer is grafted to one end of the graphene oxide by a one-step method, so that the graphene oxide with good amphiphilic performance is obtained, the graphene oxide has low surface tension, the interfacial tension between water and kerosene is reduced, the good emulsification effect is achieved, and the average oil displacement rate is 10%;
2) the modified graphene oxide provided by the application can form a good interface film at an oil-water interface, can form a stable emulsion in an oil layer after shaking, and has good amphiphilic performance;
3) the surface tension of the modified graphene oxide provided by the application is 30-35 mN/m;
4) the modified graphene oxide provided by the application has a viscosity reduction rate of 40% on petroleum.
Drawings
Fig. 1 is an AFM image of graphene oxide in example 1;
fig. 2 is an infrared spectrum of the modified graphene oxide in example 1;
fig. 3 is an oil film experimental graph of the modified graphene oxide in example 1.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
Graphene was purchased from sennito corporation, changzhou, model SE 3122.
AFM test adopts Bruker Dimension Edge instrument/model;
infrared was measured using a Nicolet iS50 Fourier transform infrared spectrometer (available from Saimer Feishell science, Inc.);
the surface tension meter is a German KRUSS surface tension tester model;
the viscometer is a boehler fly DV2TLV model.
One possible implementation is described below:
the invention aims to provide a common thickened oil viscosity-reducing modified graphene oxide oil displacement agent and a preparation method thereof, which can be used for emulsifying and viscosity-reducing thickened oil, improving the oil quality of the thickened oil and effectively realizing yield increase and consumption reduction.
The invention provides a common thickened oil viscosity-reducing modified graphene oxide oil displacement agent and a preparation method thereof, and the preparation method comprises the following steps:
step (1): diluting the purchased graphene oxide with deionized water, and centrifuging by adopting an ultrasonic shearing method to obtain graphene oxide with a smaller particle size;
step (2) diluting the graphene with smaller particle size in the step (1) again, adding a certain amount of amphiphilic polymer, and continuously stirring in a water bath and ultrasonic manner;
and (3) adding a certain amount of EDC/DMAP as a carboxyl activating agent in the step (2), magnetically stirring at normal temperature, and naming for later use after ultrasonic stirring in a water bath.
Step (4), dropwise adding the modified graphene oxide dispersion liquid obtained in the step (3) to an oil-water section, and carrying out apparent amphipathy test;
step (5) carrying out surface tension test on the modified graphene oxide dispersion liquid in the step (3);
step (6) dropwise adding the modified graphene oxide dispersion liquid obtained in the step (3) into petroleum, and performing a viscous oil viscosity reduction test;
step (6) carrying out a displacement test on the modified graphene oxide dispersion liquid in the step (3);
the relevant content in the technical scheme of the preparation method is explained as follows:
1. in the scheme, the concentration of the diluted graphene oxide in the step (1) is 2-3mg/ml, the ultrasonic shearing time is 3-5h, the centrifugation speed is 3000-5000rpm, the centrifugation time is 10-30min, and the particle size of the centrifuged graphene oxide is 50-150 nm;
2. in the scheme, the concentration of the graphene oxide in the step (2) is 1-2mg/mL, the amount of the graphene oxide is 50-100mg, the amphiphilic polymer is rhamnolipid, F127, F108 and the like, the addition amount is 0.5-1g, and the water bath ultrasonic time is 30-1 h;
3. in the scheme, the content of EDC in the step (3) is 0.25-0.5g, the content of DMAP is 0.05-0.1g, the stirring time at normal temperature is 3-5h, and the water bath ultrasound is carried out for 30-60 min;
4. in the scheme, the addition amount of the modified graphene oxide in the step (4) is 0.5-1mL, the mineralization degree of the saline is 3000ppm-5000ppm, and the oil is one of cyclohexane, n-heptane, kerosene and the like;
5. in the scheme, the surface tension meter used in the step (5) is that the concentration of the modified graphene oxide is 0.05-0.1mg/mL, and the dosage is 20-40 mL;
6. in the scheme, the using amount of the petroleum used in the step (6) is 21-42g, the using amount of the modified graphene oxide is 1-2ml, and the using amount of the water is 7-14 g;
7. the modified graphene oxide can form a good interface film at an oil-water interface, and can form a stable emulsion in an oil layer after shaking;
8. wherein the surface tension of the modified graphene oxide dispersion liquid is 30-35 mN/m;
9. wherein the viscosity of the crude oil and the water at 70 ℃ is 380-400cP, the viscosity of the amphiphilic graphene/crude oil/water at 70 ℃ is 240-250cP, and the viscosity reduction rate reaches 40%;
10. wherein the average oil displacement rate of the modified graphene oxide dispersion liquid reaches 10%.
Example 1 preparation of modified graphene oxide
a) Dissolving graphene oxide in deionized water, preparing a graphene oxide dispersion liquid I with the concentration of 2mg/ml, carrying out ultrasonic shearing for 3 hours, and centrifuging at the speed of 3000rpm for 10min to obtain the graphene oxide with the particle size of 50-150 nm;
b) diluting the obtained 50mg of graphene oxide with deionized water to obtain a graphene oxide dispersion liquid II with the concentration of 1mg/ml, adding 0.5g of rhamnolipid, and carrying out ultrasonic stirring in a water bath for 30min to obtain a mixture containing the graphene oxide and amphiphilic polymer rhamnolipid;
c) adding 0.25g EDC and 0.05g DMAP into the mixture, stirring for 3h at 20 ℃, and carrying out water bath ultrasound for 30min to obtain a dispersion liquid containing the modified graphene oxide, wherein the dispersion liquid is marked as sample No. 1.
The morphology of the graphene oxide obtained in step a) of this embodiment is tested, fig. 1 is an AFM image thereof, and as can be seen from fig. 1, the particle size of the graphene oxide is50 to 150 nm.
Example 2 preparation of modified graphene oxide
a) Dissolving graphene oxide in deionized water, preparing a graphene oxide dispersion liquid I with the concentration of 2.5mg/ml, ultrasonically shearing for 4 hours, and centrifuging at the speed of 4000rpm for 20min to obtain the graphene oxide with the particle size of 50-150 nm;
b) diluting the obtained 75mg of graphene oxide with deionized water to obtain a graphene oxide dispersion liquid II with the concentration of 1mg/ml, adding 0.75g of F108, and performing ultrasonic stirring in a water bath for 45min to obtain a mixture containing the graphene oxide and the amphiphilic polymer F108;
c) adding 0.4g EDC and 0.08g DMAP into the mixture, stirring for 4h at 25 ℃, and carrying out water bath ultrasound for 45min to obtain a dispersion liquid containing the modified graphene oxide, wherein the dispersion liquid is marked as sample No. 2.
Example 3 preparation of modified graphene oxide
a) Dissolving graphene oxide in deionized water, preparing a graphene oxide dispersion liquid I with the concentration of 3mg/ml, carrying out ultrasonic shearing for 5 hours, and centrifuging at the speed of 5000rpm for 30min to obtain the graphene oxide with the particle size of 50-150 nm;
b) diluting the obtained 100mg of graphene oxide with deionized water to obtain a graphene oxide dispersion liquid II with the concentration of 1mg/ml, adding 1g of F127, and carrying out ultrasonic stirring in a water bath for 60min to obtain a mixture containing the graphene oxide and the amphiphilic polymer F127;
c) adding 0.5g EDC and 0.1g DMAP into the mixture, stirring for 5h at 30 ℃, and carrying out water bath ultrasound for 60min to obtain a dispersion liquid containing the modified graphene oxide, wherein the dispersion liquid is marked as a sample No. 3.
Example 4 structural characterization of modified graphene oxide
Fourier infrared spectrum tests are respectively carried out on the modified graphene oxides in the embodiments 1# to 3#, and test results show that the amphiphilic polymer is grafted to two sides of the graphene oxide.
Typically, the sample is example 1, and 1456cm is shown in FIG. 2-1，1541cm-1The new appearance of characteristic absorption peak after reaction indicates the success of grafting.
Example 5 parental Performance test
The test method comprises the following steps: 0.5ml of the modified graphene oxide dispersion liquid in each of examples 1# to 3# was added dropwise to the cross section of oil and water, and an apparent amphiphilicity test was performed, in which the degree of mineralization of the saline was 3000ppm and the oil was cyclohexane.
Taking sample # 1 as a typical representative, fig. 3 is an oil film experimental diagram of the modified graphene oxide in example 1, and a test result shows that the modified graphene oxide can form a good interfacial film at an oil-water interface, and a stable emulsion can be formed in an oil layer after shaking.
Example 6 surface tension test
The test method comprises the following steps: respectively carrying out surface tension tests on the modified graphene oxide dispersion liquid in the embodiment 1# to 3#, wherein the concentration of the dispersion liquid is 0.05ml/ml, and the dosage is 20 ml;
and (3) testing results: the surface tension of the modified graphene oxide dispersion liquid is 30-35 mN/m;
the surface tension of the sample No. 1 is typically 30 mN/m.
Example 7 viscosity reduction test for thickened oils
The test method comprises the following steps: respectively dripping the modified graphene oxide dispersion liquid in the embodiment 1# to 3# into petroleum to perform a viscous oil viscosity reduction test; wherein the test oil is purchased from medium sea oil; the using amount of petroleum is 21g, the concentration of the modified graphene oxide dispersion liquid is 1mg/ml, the using amount of the modified graphene oxide dispersion liquid is 1ml, and the using amount of water is 7 g.
And (3) testing results: the viscosity of the crude oil and the water at 70 ℃ is 380-400cP, the viscosity of the modified graphene oxide/crude oil/water at 70 ℃ is 240-250cP, and the viscosity reduction rate reaches 40%.
Example 8 Displacement testing
The test method comprises the following steps: the modified graphene oxide dispersions of examples 1# to 3# were each subjected to a displacement test at 70 ℃ using a Nantong Huaxing DNQP-1 apparatus.
The test result shows that: the average oil displacement rate of the modified graphene oxide dispersion liquid reaches 10%.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. The modified graphene oxide is characterized in that the modified graphene oxide is obtained by chemically grafting an amphiphilic polymer and graphene oxide.
2. The modified graphene oxide of claim 1, wherein the amphiphilic polymer is grafted on both sides of the graphene oxide.
3. The method for preparing modified graphene oxide according to any one of claims 1 to 2, wherein a mixture containing graphene oxide and an amphiphilic polymer is reacted in the presence of a carboxyl activating agent to obtain the modified graphene oxide.
4. The method for preparing according to claim 3, wherein the amphiphilic polymer comprises at least one of rhamnolipid, polyoxyethylene polyoxypropylene ether block copolymer, and polyoxypropylene polyoxyethylene block copolymer.
5. The production method according to claim 3, wherein the carboxyl activating agent comprises at least one of carbodiimide, 4-dimethylaminopyridine and dicyclohexylcarbodiimide.
6. The production method according to claim 3, wherein the carboxyl activating agent is a mixture of carbodiimide and 4-dimethylaminopyridine;
the mass ratio of the carbodiimide to the 4-dimethylaminopyridine is 2.5-10.
7. The method according to claim 3, wherein the reaction conditions are as follows: the reaction temperature is 15-30 ℃; the reaction time is 3-5 h.
8. The method according to claim 3, characterized in that it comprises at least the following steps:
a) obtaining graphene oxide with the particle size of 50-150 nm;
b) obtaining a mixture containing the graphene oxide and an amphiphilic polymer;
c) and adding a carboxyl activating agent into the mixture, and reacting to obtain the modified graphene oxide.
9. The method for preparing according to claim 8, wherein the step a) comprises: ultrasonically shearing and centrifuging the graphene oxide dispersion liquid I to obtain graphene oxide with the particle size of 50-150 nm;
preferably, the concentration of the graphene oxide dispersion liquid I is 2-3 mg/mL;
the ultrasonic shearing time is 3-5 h;
the centrifugal speed is 3000-5000 rpm;
centrifuging for 10-30 min;
preferably, the step b) includes: dissolving the graphene oxide in the step a) in water to obtain a graphene oxide dispersion liquid II, adding an amphiphilic polymer into the graphene oxide dispersion liquid II, and performing ultrasonic stirring in a water bath to obtain the mixture;
preferably, the concentration of the graphene oxide dispersion liquid II is 1-2 mg/mL;
the mass ratio of the graphene oxide to the amphiphilic polymer is 0.01-0.1;
the water bath ultrasonic stirring time is 30-60 min;
preferably, in the step c), the mass ratio of the carboxyl activating agent to the graphene oxide in the mixture is 3-12.
10. A viscosity-reducing oil-displacing agent, which is characterized by comprising the modified graphene oxide of any one of claims 1 to 2 and/or the modified graphene oxide obtained by the preparation method of any one of claims 3 to 9.
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| CN113355064A (en) * | 2021-06-22 | 2021-09-07 | 西南石油大学 | Strong-adsorption salt-resistant plugging agent based on elastic graphite and water-based drilling fluid |
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| CN113355064A (en) * | 2021-06-22 | 2021-09-07 | 西南石油大学 | Strong-adsorption salt-resistant plugging agent based on elastic graphite and water-based drilling fluid |
| CN113355063A (en) * | 2021-06-22 | 2021-09-07 | 西南石油大学 | Elastic graphite strong-adsorption salt-resistant plugging agent and oil-based drilling fluid |
| CN113355063B (en) * | 2021-06-22 | 2022-05-24 | 西南石油大学 | Elastic graphite strong-adsorption salt-resistant plugging agent and oil-based drilling fluid |
| CN113881414A (en) * | 2021-09-29 | 2022-01-04 | 宁波锋成先进能源材料研究院有限公司 | Preparation method and application of amphiphilic graphene oxide heavy oil viscosity reducer |
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