CN117142465A - Amphiphilic graphene oxide and preparation method and application thereof - Google Patents
Amphiphilic graphene oxide and preparation method and application thereof Download PDFInfo
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- CN117142465A CN117142465A CN202311113482.7A CN202311113482A CN117142465A CN 117142465 A CN117142465 A CN 117142465A CN 202311113482 A CN202311113482 A CN 202311113482A CN 117142465 A CN117142465 A CN 117142465A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000006185 dispersion Substances 0.000 claims abstract description 128
- 239000007788 liquid Substances 0.000 claims abstract description 126
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 81
- 229920002472 Starch Polymers 0.000 claims abstract description 30
- 235000019698 starch Nutrition 0.000 claims abstract description 30
- 239000008107 starch Substances 0.000 claims abstract description 30
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000005406 washing Methods 0.000 claims abstract description 25
- 235000019441 ethanol Nutrition 0.000 claims abstract description 21
- -1 alkylamine modified graphene Chemical class 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 150000003973 alkyl amines Chemical class 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000012153 distilled water Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 15
- 238000006073 displacement reaction Methods 0.000 claims description 11
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 5
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 5
- 125000001165 hydrophobic group Chemical group 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 8
- 230000005660 hydrophilic surface Effects 0.000 description 8
- 230000005661 hydrophobic surface Effects 0.000 description 8
- 238000003760 magnetic stirring Methods 0.000 description 8
- 238000009210 therapy by ultrasound Methods 0.000 description 7
- 239000010410 layer Substances 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- RRQQLCXFGWWLPQ-UHFFFAOYSA-N ethanol;octadecan-1-amine Chemical compound CCO.CCCCCCCCCCCCCCCCCCN RRQQLCXFGWWLPQ-UHFFFAOYSA-N 0.000 description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000008034 disappearance Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- 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
Abstract
The invention discloses amphiphilic graphene oxide and a preparation method and application thereof. The preparation method comprises the following steps: adding graphene oxide dispersion liquid into starch dispersion liquid to obtain dispersion liquid A, and then centrifugally washing the dispersion liquid A and dispersing the dispersion liquid A in absolute ethyl alcohol to obtain dispersion liquid B; adding alkylamine ethanol solution into the dispersion liquid B to obtain a dispersion liquid C, centrifugally washing the dispersion liquid C, and dispersing the dispersion liquid C in absolute ethanol to obtain a dispersion liquid D; separating the starch from the graphene oxide by mechanical force action of the dispersion liquid D at constant temperature, and taking the upper dispersion liquid to obtain alkylamine modified graphene oxide dispersion liquid; and dissolving ethanolamine in the alkylamine modified graphene oxide dispersion liquid, fully stirring, washing and drying to obtain the amphiphilic graphene oxide. The invention provides the preparation method of the amphiphilic graphene oxide, which has high synthesis efficiency, is environment-friendly and is suitable for large-scale economic production.
Description
Technical Field
The invention relates to the technical field of oil displacement agents for oil extraction in oil fields, in particular to amphiphilic graphene oxide, and a preparation method and application thereof.
Background
With the development of nano technology, the nano oil displacement agent is widely concerned, and the nano material shows excellent performance in the oil displacement technology by virtue of the characteristics of unique surface effect, small-size effect and the like. The nano oil displacement agent is used as a novel oil displacement agent, and has great advantages compared with the traditional chemical oil displacement agent, such as: the size is small, and the micro-pore of the oil reservoir can be accessed; the specific surface area is large, and the surface energy is high; the oil-water interfacial tension can be effectively reduced, the displacement of crude oil is facilitated, and the recovery ratio of crude oil is obviously improved.
Graphene oxide is a derivative of a graphene nanomaterial, has a unique two-dimensional lamellar structure, and has proved to be an oil displacement material with great application potential. The graphene oxide sheet layer contains a plurality of oxygen-containing groups, has higher specific surface energy, good hydrophilicity and surface activity, and has good dispersion stability in water and most polar organic solvents, so that the graphene oxide sheet layer is researched and applied to the field of petroleum exploitation. However, pure graphene oxide tends to have a single hydrophilicity, and its interfacial activity is low, which results in an undesirable effect of improving recovery.
When the graphene oxide nano-sheet is endowed with different oleophilic-hydrophilic properties on both sides, the graphene oxide has amphiphilic properties similar to those of a surfactant, a stable interfacial film can be formed at an oil-water contact position, and the application of the graphene oxide nano-sheet in improving the recovery ratio can be greatly improved. Therefore, amphiphilic graphene oxide with good interfacial activity capable of stabilizing the oil-water interface is attracting wide attention of technological workers. For example, luo et al (D.Luo et al PNAS,2016,113 (28): 7711-7716.) synthesized graphene oxide nanoplatelets with amphiphilic properties by a wax-in-water emulsion templating method, and the main principle is to utilize alkylamine to carry out unilateral hydrophobic modification on graphene oxide. The modified nano-sheet shows good interface performance, but the method has lower synthesis efficiency and is not beneficial to large-scale production. In addition, the organic solvents used in paraffin removal, such as chloroform or toluene, can cause some environmental damage. Therefore, the preparation method of the amphiphilic graphene oxide, which is efficient, environment-friendly and supports large-scale production, has important significance for improving the recovery ratio of the oil field.
Disclosure of Invention
In order to achieve the above purpose, the invention provides amphiphilic graphene oxide, and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
an amphiphilic graphene oxide, wherein both sides of the amphiphilic graphene oxide are respectively grafted with alkylamine providing a hydrophobic group and ethanolamine providing a hydrophilic group.
Further, the alkylamine is one or more than two of tetradecylamine, hexadecylamine or octadecylamine.
The preparation method of any one of the amphiphilic graphene oxide comprises the following steps:
(1) Dispersing graphene oxide powder in distilled water to obtain graphene oxide dispersion liquid; dispersing starch in distilled water to obtain starch dispersion liquid;
(2) Adding the graphene oxide dispersion liquid into the starch dispersion liquid, fully stirring to obtain a mixed dispersion liquid A, centrifuging the mixed dispersion liquid A, washing with water, and dispersing in absolute ethyl alcohol to obtain a mixed dispersion liquid B;
(3) Dissolving alkylamine in ethanol to obtain a solution a, adding the solution a into the mixed dispersion liquid B, fully stirring to obtain a mixed dispersion liquid C, centrifuging the mixed dispersion liquid C, washing with ethanol, and dispersing in absolute ethanol to obtain a mixed dispersion liquid D;
(4) Heating the mixed dispersion liquid D at a preset temperature for a preset time, then separating starch from graphene oxide under the action of mechanical force, taking an upper dispersion liquid after the dispersion liquid is layered to obtain an alkylamine modified graphene oxide dispersion liquid, and cooling the alkylamine modified graphene oxide dispersion liquid to room temperature;
(5) And dissolving ethanolamine in the alkylamine modified graphene oxide dispersion liquid, fully stirring, washing and drying to obtain the amphiphilic graphene oxide.
Preferably, in the step (1), the mass concentration of the graphene oxide dispersion liquid is 0.2-2 mg/mL, and the mass concentration of the starch dispersion liquid is 80-200 mg/mL.
Preferably, in the step (2), the mass ratio of the graphene oxide dispersion liquid to the starch dispersion liquid is 1:2-5.
Preferably, in the step (3), the mass concentration of the solution a is 1-10 mg/mL, and the mass ratio of the solution a to the mixed dispersion liquid B is 1:2-10.
Preferably, in the step (4), the predetermined temperature is 50 to 100 ℃, and the predetermined time is 10 to 30 minutes.
Preferably, in step (4), the mechanical force is ultrasonic vibration or mechanical stirring.
Preferably, in the step (5), the mass ratio of the ethanolamine to the alkylamine modified graphene oxide dispersion is 1:20-100.
Any one of the amphiphilic graphene oxide is used as an oil displacement agent for oil extraction in an oil field.
The invention has the beneficial effects that:
1. the preparation method has the characteristics of high synthesis efficiency, environment friendliness, suitability for industrial mass production and the like.
2. According to the amphiphilic graphene oxide prepared by the invention, through double-sided modification of alkylamine and ethanolamine, the oil-water amphiphilic structure characteristics are outstanding, excellent interfacial activity and interfacial stability are shown, the amphiphilic graphene oxide is easier to adsorb on an oil-water interface, and the amphiphilic graphene oxide has more excellent oil displacement performance.
Drawings
Fig. 1 is a schematic diagram of a preparation flow of amphiphilic graphene oxide according to the present invention.
Fig. 2 is an X-ray diffraction (XRD) pattern of graphene oxide used in example 2 and amphiphilic graphene oxide prepared.
FIG. 3 (a) is a Scanning Electron Microscope (SEM) image of graphene oxide used in examples 1-4.
Fig. 3 (b) is a Scanning Electron Microscope (SEM) image of the amphiphilic graphene oxide prepared in example 2.
Fig. 4 is a water contact angle of a hydrophilic surface and a hydrophobic surface of the amphiphilic graphene oxide prepared in example 2.
Fig. 5 (a) and 5 (b) are interfacial behavior diagrams of the amphiphilic graphene oxide prepared in example 2 at an oil-water interface.
Fig. 6 is a water contact angle of a hydrophilic surface and a hydrophobic surface of the amphiphilic graphene oxide prepared in example 3.
Fig. 7 is a water contact angle of a hydrophilic surface and a hydrophobic surface of the amphiphilic graphene oxide prepared in example 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solution of the present invention will be clearly and completely described with reference to the accompanying drawings and a preferred embodiment.
Example 1
The preparation method of the amphiphilic graphene oxide comprises the following steps:
(1) 180mg of graphene oxide powder is dispersed in 120mL of distilled water, the graphene oxide dispersion liquid is obtained after ultrasonic treatment is carried out for 30min, 39g of starch is dispersed in 300mL of distilled water, and the starch dispersion liquid is obtained after magnetic stirring is carried out for 30min.
(2) And (3) dropwise adding graphene oxide dispersion liquid into starch dispersion liquid, magnetically stirring for 7 hours to obtain mixed dispersion liquid A, washing the mixed dispersion liquid A with distilled water and ethanol once respectively, wherein the washing mode is centrifugal washing, the rotating speed is 3000r/min, the time is 30min, and the washed product is dispersed in 200mL of absolute ethanol to obtain mixed dispersion liquid B.
(3) 250mg of octadecylamine is dissolved in 50mL of absolute ethyl alcohol to obtain octadecylamine ethanol solution with the mass concentration of 5mg/mL, the obtained octadecylamine ethanol solution is dripped into the mixed dispersion liquid B, the mixed dispersion liquid C is obtained after magnetic stirring for 12h, then the mixed dispersion liquid C is centrifugally washed twice by the ethanol solution at the rotating speed of 3000r/min for 30min, and the washed product is dispersed in 200mL of absolute ethyl alcohol to prepare mixed dispersion liquid D.
(4) Heating the mixed dispersion liquid D at 60 ℃ for 10min, then carrying out ultrasonic treatment for 10min, repeating for three times, taking the upper dispersion liquid when starch falls off from the surface of the graphene oxide and is settled to the bottom layer of the dispersion liquid, obtaining the octadecylamine modified graphene oxide dispersion liquid, and cooling to room temperature.
(5) And (3) dissolving ethanolamine in the cooled octadecylamine modified graphene oxide dispersion liquid by mass fraction of 3.5%, magnetically stirring at room temperature for 18h, after the reaction is finished, sequentially centrifugally washing with distilled water and ethanol at the rotating speed of 3000r/min for 30min, and finally drying at the temperature of 60 ℃ for 24h to obtain the amphiphilic graphene oxide A.
The preparation flow is shown in figure 1.
Example 2
(1) 100mg of graphene oxide powder is dispersed in 100mL of distilled water, the graphene oxide dispersion liquid is obtained after ultrasonic treatment is carried out for 30min, 40g of starch is dispersed in 250mL of distilled water, and the starch dispersion liquid is obtained after magnetic stirring is carried out for 30min.
(2) And (3) dropwise adding graphene oxide dispersion liquid into starch dispersion liquid, magnetically stirring for 7 hours to obtain mixed dispersion liquid A, washing the mixed dispersion liquid once by distilled water and ethanol respectively, wherein the washing mode is centrifugal washing, the rotating speed is 3000r/min, the time is 30min, and the washed product is dispersed in 200mL of absolute ethanol to obtain mixed dispersion liquid B.
(3) 300mg of octadecylamine is dissolved in 50mL of absolute ethyl alcohol to obtain octadecylamine ethanol solution, the octadecylamine ethanol solution is dripped into the mixed dispersion liquid B, the mixed dispersion liquid C is obtained after magnetic stirring for 12 hours, then the mixed dispersion liquid C is centrifugally washed twice by the ethanol solution at the rotating speed of 3000r/min for 30min, and the washed product is dispersed in 200mL of absolute ethyl alcohol to prepare mixed dispersion liquid D.
(4) Heating the mixed dispersion liquid D at 70 ℃ for 10min, then carrying out ultrasonic treatment for 10min, repeating for three times, taking the upper dispersion liquid when starch falls off from the surface of the graphene oxide and is settled to the bottom layer of the dispersion liquid, obtaining the octadecylamine modified graphene oxide dispersion liquid, and cooling to room temperature.
(5) And (3) dissolving ethanolamine in the cooled octadecylamine modified graphene oxide dispersion liquid according to the mass fraction of 3%, magnetically stirring for 18 hours at room temperature, after the reaction is finished, sequentially centrifugally washing with distilled water and ethanol, wherein the rotating speed is 3000r/min, the time is 30min, and finally drying at 60 ℃ for 24 hours to obtain the amphiphilic graphene oxide B.
XRD of graphene oxide and amphiphilic graphene oxide B is shown in figure 2. As shown in fig. 2, the graphene oxide has a characteristic diffraction peak at 2θ= 9.861 °, the corresponding interlayer spacing is 0.8967nm, the disappearance of the characteristic peak of the amphiphilic graphene oxide B at 2θ= 9.861 ° represents the disappearance of the oxygen-containing functional group of the graphene oxide, and a wide and low-intensity diffraction peak appears in the 2θ range of 10-25 ° to indicate successful grafting of octadecylamine and ethanolamine.
SEM of graphene oxide and amphiphilic graphene oxide B is shown in fig. 3 (a) and 3 (B). As shown in fig. 3 (a), the surface of the graphene oxide under the transmission electron microscope is transparent, the periphery is folded towards the middle, and the phenomenon of wrinkling is presented, which indicates that the epoxy group content of the graphene oxide is higher. As shown in FIG. 3 (b), after both sides of ethanolamine and octadecylamine were modified, the dents were significantly removed, and significant wrinkles were generated on the surface, and the transmittance was also reduced. The above results indicate that double sided modification achieves the expected expectations.
The water contact angles of the hydrophilic surface and the hydrophobic surface of the amphiphilic graphene oxide B are shown in fig. 4. As shown in fig. 4, the contact angle of the hydrophilic surface of the amphiphilic graphene oxide B is 52.8 °, and the contact angle of the hydrophobic surface is 94.6 °, which indicates that the amphiphilic modification of the graphene oxide is successful, the contact angle is reduced due to the addition of more hydroxyl groups on the hydrophilic surface, and the hydrophobic surface is added with a carbon chain, so that the hydrophobicity is enhanced and the contact angle is increased.
The interfacial behavior of the amphiphilic graphene oxide B at the oil-water interface is shown in fig. 5 (a) and 5 (B). And injecting the amphiphilic graphene oxide B nano dispersion liquid into a dyed two-phase system of n-heptane and distilled water, and observing the interface condition, so as to explore the interface activity of the particles. As shown in fig. 5 (a), in the initial state, the oil-water interface is in a concave shape, which indicates that the interfacial tension is higher; as shown in fig. 5 (b), after the amphiphilic graphene oxide nano dispersion liquid is injected, the mixture is mixed uniformly and kept still, the interface becomes smoother, and particles appear on the interface, which indicates that the interfacial tension is reduced, and the amphiphilic modification of graphene oxide is successful.
Example 3
The preparation method of the amphiphilic graphene oxide comprises the following steps:
(1) 50mg of graphene oxide powder is dispersed in 100mL of distilled water, the graphene oxide dispersion liquid is obtained after ultrasonic treatment is carried out for 30min, 30g of starch is dispersed in 300mL of distilled water, and the starch dispersion liquid is obtained after magnetic stirring is carried out for 30min.
(2) And (3) dropwise adding graphene oxide dispersion liquid into starch dispersion liquid, magnetically stirring for 7 hours to obtain mixed dispersion liquid A, washing the mixed dispersion liquid once by distilled water and ethanol respectively, wherein the washing mode is centrifugal washing, the rotating speed is 3000r/min, the time is 30min, and the washed product is dispersed in 200mL of absolute ethanol to obtain mixed dispersion liquid B.
(3) 300mg of tetradecylamine is dissolved in 50mL of absolute ethyl alcohol to obtain an ethanol solution containing tetradecylamine, the ethanol solution containing tetradecylamine is dripped into the mixed dispersion liquid B, the mixed dispersion liquid C is obtained after magnetic stirring for 12 hours, then the mixed dispersion liquid C is centrifugally washed twice by the ethanol solution at the rotating speed of 3000r/min for 30min, and the washed product is dispersed in 200mL of absolute ethyl alcohol to obtain a mixed dispersion liquid D.
(4) Heating the mixed dispersion liquid D at 60 ℃ for 30min, magnetically stirring for 20min, repeating for three times, taking the upper dispersion liquid when starch falls off from the surface of the graphene oxide and is settled to the bottom layer of the dispersion liquid, obtaining the tetradecylamine modified graphene oxide dispersion liquid, and cooling to room temperature.
(5) Dissolving ethanolamine in a mass fraction of 2.5% in a tetradecylamine modified graphene oxide dispersion liquid, magnetically stirring at room temperature for 18 hours, after the reaction is finished, sequentially centrifugally washing with distilled water and ethanol, wherein the rotating speed is 3000r/min, the time is 30min, and finally drying at 60 ℃ for 24 hours to obtain amphiphilic graphene oxide C.
As shown in fig. 6, the hydrophilic surface contact angle of the prepared amphiphilic graphene oxide C was 59.3 °, and the hydrophobic surface contact angle was 91.3 °.
Example 4
The preparation method of the amphiphilic graphene oxide comprises the following steps:
(1) 100mg of graphene oxide powder is dispersed in 100mL of distilled water, the graphene oxide dispersion liquid is obtained after ultrasonic treatment is carried out for 30min, 26g of starch is dispersed in 300mL of distilled water, and the starch dispersion liquid is obtained after magnetic stirring is carried out for 30min.
(2) And (3) dropwise adding graphene oxide dispersion liquid into starch dispersion liquid, magnetically stirring for 7 hours to obtain mixed dispersion liquid A, washing the mixed dispersion liquid once by distilled water and ethanol respectively, wherein the washing mode is centrifugal washing, the rotating speed is 3000r/min, the time is 30min, and the washed product is dispersed in 200mL of absolute ethanol to obtain mixed dispersion liquid B.
(3) 250mg of hexadecylamine is dissolved in 50mL of absolute ethyl alcohol to obtain an ethanol solution containing hexadecylamine, the ethanol solution containing hexadecylamine is dripped into the mixed dispersion liquid B, the mixed dispersion liquid C is obtained after magnetic stirring for 12 hours, then the mixed dispersion liquid C is centrifugally washed twice by the ethanol solution at the rotating speed of 3000r/min for 30min, and the washed product is dispersed in 200mL of absolute ethyl alcohol to obtain a mixed dispersion liquid D.
(4) And heating the mixed dispersion liquid D at 80 ℃ for 20min, then carrying out ultrasonic treatment for 10min, repeating for three times, taking the upper dispersion liquid when starch falls off from the surface of the graphene oxide and is settled to the bottom layer of the dispersion liquid, obtaining the hexadecylamine modified graphene oxide dispersion liquid, and cooling to room temperature.
(5) Dissolving ethanolamine in a hexadecylamine modified graphene oxide dispersion liquid by mass fraction of 5%, magnetically stirring for 18 hours at room temperature, after the reaction is finished, sequentially centrifugally washing with distilled water and ethanol, wherein the rotating speed is 3000r/min, the time is 30min, and finally drying at 60 ℃ for 24 hours to obtain the amphiphilic graphene oxide D.
As shown in fig. 7, the hydrophilic surface contact angle of the prepared amphiphilic graphene oxide D was 51.5 °, and the hydrophobic surface contact angle was 105.6 °. Compared with octadecylamine and tetradecylamine modified graphene oxide, hexadecylamine modified graphene oxide has better amphiphilic property.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention and remain within the scope of the invention.
Claims (10)
1. The amphiphilic graphene oxide is characterized in that alkylamine providing hydrophobic groups and ethanolamine providing hydrophilic groups are respectively grafted on two sides of the amphiphilic graphene oxide.
2. The amphiphilic graphene oxide of claim 1, wherein the alkylamine is one or more of tetradecylamine, hexadecylamine, or octadecylamine.
3. The method for preparing the amphiphilic graphene oxide according to claim 1 or 2, which is characterized by comprising the following steps:
(1) Dispersing graphene oxide powder in distilled water to obtain graphene oxide dispersion liquid; dispersing starch in distilled water to obtain starch dispersion liquid;
(2) Adding the graphene oxide dispersion liquid into the starch dispersion liquid, fully stirring to obtain a mixed dispersion liquid A, centrifuging the mixed dispersion liquid A, washing with water, and dispersing in absolute ethyl alcohol to obtain a mixed dispersion liquid B;
(3) Dissolving alkylamine in ethanol to obtain a solution a, adding the solution a into the mixed dispersion liquid B, fully stirring to obtain a mixed dispersion liquid C, centrifuging the mixed dispersion liquid C, washing with ethanol, and dispersing in absolute ethanol to obtain a mixed dispersion liquid D;
(4) Heating the mixed dispersion liquid D at a preset temperature for a preset time, then separating starch from graphene oxide under the action of mechanical force, taking an upper dispersion liquid after the dispersion liquid is layered to obtain an alkylamine modified graphene oxide dispersion liquid, and cooling the alkylamine modified graphene oxide dispersion liquid to room temperature;
(5) And dissolving ethanolamine in the alkylamine modified graphene oxide dispersion liquid, fully stirring, washing and drying to obtain the amphiphilic graphene oxide.
4. The method for preparing amphiphilic graphene oxide according to claim 1, wherein the method comprises the following steps: in the step (1), the mass concentration of the graphene oxide dispersion liquid is 0.2-2 mg/mL, and the mass concentration of the starch dispersion liquid is 80-200 mg/mL.
5. The method for preparing amphiphilic graphene oxide according to claim 1, wherein the method comprises the following steps: in the step (2), the mass ratio of the graphene oxide dispersion liquid to the starch dispersion liquid is 1:2-5.
6. The method for preparing amphiphilic graphene oxide according to claim 1, wherein the method comprises the following steps: in the step (3), the mass concentration of the solution a is 1-10 mg/mL, and the mass ratio of the solution a to the mixed dispersion liquid B is 1:2-10.
7. The method for preparing amphiphilic graphene oxide according to claim 1, wherein the method comprises the following steps: in the step (4), the preset temperature is 50-100 ℃, and the preset time is 10-30 min.
8. The method for preparing amphiphilic graphene oxide according to claim 1, wherein the method comprises the following steps: in the step (4), the mechanical force is ultrasonic vibration or mechanical stirring.
9. The method for preparing amphiphilic graphene oxide according to claim 1, wherein the method comprises the following steps: in the step (5), the mass ratio of the ethanolamine to the alkylamine modified graphene oxide dispersion liquid is 1:20-100.
10. An amphiphilic graphene oxide as claimed in claim 1 or 2 as an oil displacement agent for oil recovery in an oilfield.
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