CN110371963A - A kind of preparation method and application of parental graphite oxide alkene nano material - Google Patents
A kind of preparation method and application of parental graphite oxide alkene nano material Download PDFInfo
- Publication number
- CN110371963A CN110371963A CN201910537963.8A CN201910537963A CN110371963A CN 110371963 A CN110371963 A CN 110371963A CN 201910537963 A CN201910537963 A CN 201910537963A CN 110371963 A CN110371963 A CN 110371963A
- Authority
- CN
- China
- Prior art keywords
- substrate
- parental
- nano material
- graphite oxide
- graphene oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
This application discloses a kind of preparation methods of parental graphite oxide alkene nano material, which comprises (1) by graphene oxide-loaded in the substrate on substrate, obtaining being loaded with graphene oxide；(2) substrate for being loaded with graphene oxide is placed in the solution containing dressing agent, obtains the substrate for being loaded with the graphene oxide after modification, removes substrate, obtain the parental graphite oxide alkene nano material.Method modifying process described herein is easier to control, and reacts more abundant, so that yield can be improved.Entire substrate method preparation process is considerably less than template using the amount of organic solvent, plays the role of to environmental protection very useful.
Description
Technical field
This application involves a kind of preparation method and applications of parental graphite oxide alkene nano material, belong to nano material neck
Domain.
Background technique
Graphene oxide is the oxide of graphene, is the two-dimensional material of single layer, and size has very big in nanoscale
Specific surface area.After peroxidating, surface of graphene oxide makes there is oxygen-containing functional groups such as a large amount of epoxy group, hydroxyl, carboxyls
Obtaining graphene oxide, dispersibility is fine in water, and the functionalization of various ways may be implemented in the presence of a variety of oxygen-containing functional groups
It is modified.Due to these excellent performances, graphene oxide and its derivative are in electronic device, the energy, environment, pharmacy, environment guarantor
The fields such as shield are got the attention.
Graphene oxide composite material due to its surface oxygen-containing functional group abundant so that graphene oxide two sides all present it is excellent
Hydrophilicity.And lipophilic group is connected on one side by what the modifying and decorating of single side made graphene oxide, to make this be on one side
Existing excellent oleophylic performance, it will be able to obtain the different parental graphite oxide alkene nanometer sheet material in two sides.This parents aoxidize stone
Black alkene nanometer sheet material has broad application prospects in fields such as novel oil displacement agent, environment-friendly type surfactant, oily waste treatments.
The single side method of modifying of parental graphite oxide alkene is all template at present, there are it is complicated for operation, be difficult to finely control,
It isolates and purifies difficulty greatly and there are problems that yield is more low and be unfavorable for actual production, it is therefore desirable to it is raw to develop a kind of industry
Produce the preparation method for the parental graphite oxide alkene for being easy to control and realizing.
Summary of the invention
According to the one aspect of the application, a kind of preparation method of parental graphite oxide alkene nano material, the party are provided
Method is easy to operate, and industrial application is wider.
The preparation method of the parental graphite oxide alkene nano material, which is characterized in that the described method includes:
(1) by graphene oxide-loaded in the substrate on substrate, obtaining being loaded with graphene oxide；
(2) substrate for being loaded with graphene oxide is placed in the solution containing dressing agent, obtains being loaded with the oxidation after modification
The substrate of graphene removes substrate, obtains the parental graphite oxide alkene nano material.
Optionally, the parental graphite oxide alkene nano material is nano lamellar material.
Optionally, the size of the parental graphite oxide alkene nano material is 10~1000nm.
Optionally, substrate described in step (1) carries out hydrophilic treated.
Optionally, the hydrophilic treated includes: gas plasma processing；Or
Substrate is soaked in hydrophilic processing liquid.
As one of specific embodiment, the method that the substrate carries out hydrophilic treated includes: to place substrate
It is taken out after being soaked for a period of time in hydrophilic processing liquid.
Optionally, the time of the gas plasma processing is 0.5-2 hours；
It is 2-24 hours that substrate, which is soaked in the soaking time in hydrophilic processing liquid,.
Optionally, the time upper limit of the gas plasma processing is selected from 0.8 hour, 1 hour, 1.5 hours, 1.8 hours
Or 2 hours；Lower limit is selected from 0.5 hour, 0.8 hour, 1 hour, 1.5 hours or 1.8 hours.
Optionally, by substrate be soaked in the soaking time upper limit in hydrophilic processing liquid be selected from 5 hours, 8 hours, 10 hours,
12 hours, 15 hours, 18 hours, 20 hours or 24 hours；Lower limit be selected from 2 hours, 5 hours, 8 hours, 10 hours, 12 hours,
15 hours, 18 hours or 20 hours.
Optionally, the hydrophilic processing liquid is that sulfuric acid-hydrogen peroxide mixed solution or sodium hydroxide-potassium peroxydisulfate mixing are molten
Liquid.
Optionally, the volume ratio of sulfuric acid and hydrogen peroxide is 1~5:1 in the sulfuric acid-hydrogen peroxide mixed solution；
The mass ratio of sodium hydroxide and potassium peroxydisulfate is 2~6:1 in the sodium hydroxide-potassium peroxydisulfate mixed solution.
Optionally, the concentration of the sulfuric acid is 98wt%；The concentration of the hydrogen peroxide is 30wt%.
Optionally, the volume ratio upper limit of sulfuric acid and hydrogen peroxide is selected from 5:1,4 in the sulfuric acid-hydrogen peroxide mixed solution:
1,3:1 or 2:1；Lower limit is selected from 1:1,2:1,3:1 or 4:1.
Optionally, in the sodium hydroxide-potassium peroxydisulfate mixed solution on the mass ratio of sodium hydroxide and potassium peroxydisulfate
Limit is selected from 6:1,5:1,4:1 or 3:1；Lower limit is selected from 2:1,3:1,4:1 or 5:1.
Optionally, mode of loading described in step (1) includes:
Dispersant liquid drop containing graphene oxide is added on substrate；Or
On substrate by the dispersion liquid spin coating containing graphene oxide；Or
Substrate is immersed in the dispersion liquid containing graphene oxide.
As one of specific embodiment, the mode of the load includes: that graphene oxide dispersion is added dropwise
Or on the substrate after the hydrophilic treated being spun on, or hydrophilic treated back substrate is immersed in one in graphene oxide dispersion
It is taken out after the section time.
Optionally, the concentration of the dispersion liquid containing graphene oxide is 0.005mg/mL-10.0mg/mL；
Dispersing agent includes at least one of water, ethyl alcohol in the dispersion liquid.
Optionally, the dispersion liquid concentration upper limit containing graphene oxide be selected from 0.01mg/mL, 0.02mg/mL,
0.1mg/mL, 0.2mg/mL, 0.5mg/mL, 1mg/mL, 2mg/mL, 5mg/mL, 8mg/mL or 10mg/mL；Lower limit is selected from
0.005mg/mL、0.01mg/mL、0.02mg/mL、0.1mg/mL、0.2mg/mL、0.5mg/mL、1mg/mL、2mg/mL、5mg/
ML or 8mg/mL.
Optionally, the partial size of graphene oxide is 10~1000nm in the dispersion liquid containing graphene oxide.
Optionally, soaking time substrate being immersed in the dispersion liquid containing graphene oxide is 2-24 hours.
Optionally, substrate is immersed in the immersion in the dispersion liquid containing graphene oxide time upper limit be selected from 5 hours,
8 hours, 10 hours, 12 hours, 15 hours, 20 hours or 24 hours；Lower limit is selected from 2 hours, 5 hours, 8 hours, 10 hours, 12
Hour, 15 hours or 20 hours.
Optionally, dressing agent described in step (2) is hydrophobing agent；
Solvent is selected from ethyl alcohol, chloroform, acetone, benzene, toluene, carbon tetrachloride, tetrahydro furan in the solution containing dressing agent
It mutters, at least one of ether, hexamethylene.
Optionally, the hydrophobing agent is selected from least one of alkylamine, long-chain alcohol, halogenated hydrocarbons, long chain acid.
Optionally, the hydrophobing agent is selected from lauryl amine, cetylamine, octadecylamine, lauryl alcohol, hexadecanol, dodecyl iodides, bromine
For at least one of hexadecane, certain herbaceous plants with big flowers acid, palmitinic acid, stearic acid.
Optionally, the concentration of dressing agent is 0.01~20.0mol/L in the solution containing dressing agent.
Optionally, the substrate for being loaded with graphene oxide is placed in the mode in dressing agent described in step (2) includes impregnating；
The time of the immersion is 0.5~48 hour；
The temperature of the immersion is 10~40 DEG C.
Optionally, the time upper limit of immersion be selected from 1 hour, 5 hours, 10 hours, 12 hours, 15 hours, 20 hours, it is 25 small
When, 30 hours, 35 hours, 40 hours or 48 hours；Lower limit is selected from 0.5 hour, 1 hour, 5 hours, 10 hours, 12 hours, 15
Hour, 20 hours, 25 hours, 30 hours, 35 hours or 40 hours.
Optionally, the temperature upper limit of the immersion is selected from 15 DEG C, 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C or 40 DEG C；Lower limit is selected from
10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C, 30 DEG C or 35 DEG C.
Optionally, it states substrate and is selected from one of nonmetallic substrate, metal substrate, metallic compound substrate.
Optionally, the nonmetallic substrate includes one kind of glass, silicon wafer, sapphire, SiC, ito glass, FTO glass；
The metal substrate includes one of copper substrate, aluminium substrate；
The metallic compound substrate includes GaN substrate, Ga2O3One of substrate.
Preferably, the substrate is glass or silicon wafer.
Substrate of the present invention includes but is not limited to glass, can also be silicon wafer, sapphire, SiC, ito glass,
The non-metal plates such as FTO glass, the sheet metals such as copper, aluminium, the metal-semiconductor compounds such as GaN, Ga2O3, it is all can in the present invention
The substrate for playing phase same-action should be within the scope of the present invention.
As one of specific embodiment, the acquisition pattern packet of the substrate of the graphene oxide after being loaded with modification
It includes: the substrate for being loaded with graphene oxide being immersed in modification liquid after a period of time and is taken out.
Optionally, the mode of the removal substrate includes: peeling liner bottom.
Optionally, the peeling liner bottom includes: that the substrate for being loaded with the graphene oxide after modifying is soaked in stripper,
Separation, obtains the parental graphite oxide alkene nano material.
Optionally, during peeling liner bottom the immersion condition are as follows:
The time of the immersion is 0.5~48 hour；
The temperature of the immersion is 10 DEG C~40 DEG C.
Optionally, during peeling liner bottom the immersion time upper limit be selected from 1 hour, 5 hours, 10 hours, 12 hours,
15 hours, 20 hours, 25 hours, 30 hours, 35 hours, 40 hours or 48 hours；Lower limit be selected from 0.5 hour, 1 hour, it is 5 small
When, 10 hours, 12 hours, 15 hours, 20 hours, 25 hours, 30 hours, 35 hours or 40 hours.
Optionally, during peeling liner bottom the immersion temperature upper limit be selected from 15 DEG C, 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C or
40℃；Lower limit is selected from 10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C, 30 DEG C or 35 DEG C.
Optionally, the separation process are as follows: stand or stir first or ultrasound, parental graphite oxide alkene nano material is from lining
It falls off, is dispersed in stripper on bottom；
Using centrifugation, filtering, suction filtration, film filtering one of by parental graphite oxide alkene nano material from stripper
Separation.
Optionally, the stripper is selected from least one of at least one of acid or lye.
Optionally, the concentration of the acid is 0.1~10.0mol/L；The concentration of the lye is 0.1~10.0mol/L.
As one of specific embodiment, the stripper is dilute hydrochloric acid or sodium hydroxide solution.
The stripper that the present invention uses includes but is not limited to dilute hydrochloric acid or sodium hydroxide solution, can also be dilute sulfuric acid, phosphorus
The solution of acid, acetic acid, potassium hydroxide, lithium hydroxide, all removings that substrate and graphene oxide may be implemented belongs to this hair
Bright protection scope.
Optionally, the parental graphite oxide alkene nano material is in oil displacement agent, environment-friendly type surfactant, oily waste treatment
Application.
The another aspect of the application provides the preparation side of parental graphite oxide alkene nano material described in any of the above embodiments
The parental graphite oxide alkene nano material that method is prepared.
In the application, " long-chain alcohol, long chain acid " refers to that carbon atom number is 10~20 alcohol or acid.
The beneficial effect that the application can generate includes:
(1) easier in preparation method provided herein operation, the industrial substrate method for being easier to realize is next real
The single side modification of existing parental graphite oxide alkene material；Implementation by the method for the invention, the yield of parental graphite oxide alkene material
It can be improved, decrease the use of organic solvent in preparation process, play the role of to environmental protection very useful.
(2) parental graphite oxide alkene material is prepared by the method for the invention, is not needed preparation template, is connected template, removing
The tedious steps of template, the acquisition of substrate facilitate than the preparation of template it is very much, the removing of substrate also it is more convenient than the removing of template very
It is more；The preparation of substrate method is prepared compared to template, and modifying process is easier to control, and reacts more abundant, so that yield energy
Access raising.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of raw material graphene oxide in the embodiment of the present application 1；
Fig. 2 is the infrared spectrogram of parental graphite oxide alkene material in the embodiment of the present application 1；
Fig. 3 is the infrared spectrogram of parental graphite oxide alkene material in the embodiment of the present application 2；
Fig. 4 is the infrared spectrogram of parental graphite oxide alkene material in the embodiment of the present application 3；
Fig. 5 is the grain size distribution of parental graphite oxide alkene material in the embodiment of the present application 1.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material in embodiments herein is bought by commercial sources, wherein
Graphene oxide is purchased from Changzhou No.6 Element Material Technology Co., Ltd. (model SE3122).
Glass slide be purchased from Aladdin reagent (Shanghai) Co., Ltd., model P3963, size 25.4mm × 76.2mm,
Thickness 1.0-1.2mm, core Silicon Valley brand.
Silicon wafer be purchased from Kunshan Xiao Fei photovoltaic Science and Technology Ltd., 4 inches.
Copper sheet is purchased from Aladdin reagent (Shanghai) Co., Ltd., and analysis is pure, and 99.5%.
Gallium nitride is purchased from Aladdin reagent (Shanghai) Co., Ltd., and analysis is pure, and 99.99%.
The reagents such as lauryl amine, cetylamine, hexadecanol, hydrochloric acid, sodium hydroxide are purchased from Aladdin reagent (Shanghai) Co., Ltd.,
It analyzes pure.
Ethyl alcohol, acetone equal solvent are purchased from Aladdin reagent (Shanghai) Co., Ltd., analyze pure.
Analysis method is as follows in embodiments herein:
Materials chemistry structural analysis is carried out using Fourier transform infrared spectroscopy.
Granularmetric analysis is carried out using Malvern laser particle analyzer.
Embodiment 1
(1) substrate processing: glass slide is soaked in 12 small in sulfuric acid-hydrogen peroxide mixed solution (volume ratio 4:1)
When.Wherein the concentration of sulfuric acid is 98wt%, and the concentration of hydrogen peroxide is 30wt%.Glass slide is taken out after 12 hours, is put into baking
105 DEG C of case drying；
(2) substrate coats: the glass slide Jing Guo hydrophilic treated is soaked in 0.01mg/mL graphene oxide ethyl alcohol point
12 hours in dispersion liquid, taking-up is put into 60 DEG C of dryings of baking oven；
(3) single side is modified: the glass slide that step (2) obtains being soaked in decorating liquid 12 hours, soaking temperature is
30 DEG C, decorating liquid is the chloroformic solution of cetylamine, concentration 0.2mol/L.Glass slide is taken out after 12 hours, is put into baking oven
60 DEG C of drying；
(4) substrate desquamation: the glass slide that step (3) obtains is soaked in stripper, and soaking temperature is 30 DEG C, leaching
Bubble 1 hour, removes parental graphite oxide alkene from substrate by ultrasound, after ultrasonic time 30 minutes, takes out glass slide.
Stripper containing parental graphite oxide alkene is put into centrifuge tube, is centrifuged to obtain lower sediment by centrifuge, 5000 turns of revolving speed
Per minute, centrifugation time 30 minutes.Centrifugation is taken out, 60 DEG C of baking oven obtained by drying to parental graphite oxide ene product, produces
Rate reaches 95%, and products therefrom is labeled as C1.
Stripper is 0.1mol/L sodium hydrate aqueous solution.
Fig. 1 is the graphene oxide infrared spectrogram before modification, and Fig. 2 is the parental graphite oxide alkene after modification, can be seen
There is strong methyl (1376cm after to modification on infrared spectroscopy-1And 2954cm-1), methylene (1456cm-1, 2851cm-1With
2922cm-1) infrared signature absorption peak, it was demonstrated that cetylamine is grafted successfully on graphene oxide.
Ethyl alcohol, chloroform used in whole process only have tens milliliters, and can be evaporated under reduced pressure recycling.
Embodiment 2
By in embodiment 1 step (2) replacement are as follows: by 0.01mg/mL graphene oxide alcohol dispersion liquid be spin-coated on by
In the glass slide of hydrophilic treated, it is then placed in 60 DEG C of dryings of baking oven；Remaining condition is same as Example 1, the product of acquisition
Labeled as C2；
Infrared analysis is carried out to C2, and is compared with Fig. 1, identical as 1 conclusion of embodiment: cetylamine is in graphene oxide
It is upper to be grafted successfully.
Ethyl alcohol, chloroform used in whole process only have tens milliliters, and can be evaporated under reduced pressure recycling.
Embodiment 3
By step (2) replacement in embodiment 1 are as follows: passing through the dropwise addition of 0.01mg/mL graphene oxide alcohol dispersion liquid
In the glass slide of hydrophilic treated, it is then placed in 60 DEG C of dryings of baking oven；Remaining condition is same as Example 1, the product of acquisition
Labeled as C3；
Infrared analysis is carried out to C3, and is compared with Fig. 1, identical as 1 conclusion of embodiment: cetylamine is in graphene oxide
It is upper to be grafted successfully.
Ethyl alcohol, chloroform used in whole process only have tens milliliters, and can be evaporated under reduced pressure recycling.
Embodiment 4
Cetylamine in embodiment 1 is replaced with into 1- bromohexadecane；Remaining condition is same as Example 1, the production of acquisition
Substance markers are C4；
Infrared analysis is carried out to C4, and is compared with Fig. 1, obtain conclusion: 1- bromohexadecane is on graphene oxide
It is grafted successfully.
Ethyl alcohol, chloroform used in whole process only have tens milliliters, and can be evaporated under reduced pressure recycling.
Embodiment 5
(1) copper sheet substrate processing: is soaked in sodium hydroxide-potassium peroxydisulfate mixed solution (mass ratio 5:1, solvent are water)
In 10 hours.Wherein the concentration of sodium hydroxide is 10mg/mL, and the concentration of potassium peroxydisulfate is 2mg/mL.Copper is taken out after 10 hours
Piece is put into 105 DEG C of baking oven drying；
(2) substrate coats: the copper sheet Jing Guo hydrophilic treated is soaked in 12 in 0.02mg/mL graphene oxide aqueous dispersions
Hour, taking-up is put into 60 DEG C of dryings of baking oven；
(3) single side is modified: the copper sheet that step (2) obtains being soaked in decorating liquid 12 hours, soaking temperature is 25 DEG C, is repaired
Adorn the ethanol solution that liquid is lauryl amine, concentration 0.3mol/L.Copper sheet is taken out after 12 hours, is put into 60 DEG C of baking oven drying；
(4) substrate desquamation: the copper sheet that step (3) obtains is soaked in stripper, and soaking temperature is 35 DEG C, and it is small to impregnate 2
When, parental graphite oxide alkene is removed from substrate by stirring, after stirring 1 hour, takes out copper sheet.Stone will be aoxidized containing parents
The stripper of black alkene obtains filter cake by filtering, and 60 DEG C of filter cake baking oven obtained by drying to arrive parental graphite oxide ene product, and yield reaches
To 97%, products therefrom is labeled as C5.
Stripper is 0.1mol/L dilute hydrochloric acid.
Fig. 1 is the graphene oxide infrared spectrogram before modification, and Fig. 3 is the parental graphite oxide alkene parents oxidation after modification
Graphene, it can be seen that have strong methyl (1376cm after modification on infrared spectroscopy-1And 2951cm-1), methylene (2851cm-1
And 2921cm-1) infrared signature absorption peak, it was demonstrated that lauryl amine is grafted successfully on graphene oxide.
Ethyl alcohol used in whole process only has tens milliliters, and can be evaporated under reduced pressure recycling.
Embodiment 6
Cetylamine in embodiment 1 is replaced with into lauryl alcohol；Remaining condition is same as Example 1, the Product Labeling of acquisition
For C6；
Infrared analysis is carried out to C6, and is compared with Fig. 1, obtains conclusion: lauryl alcohol be grafted on graphene oxide at
Function.
Ethyl alcohol, chloroform used in whole process only have tens milliliters, and can be evaporated under reduced pressure recycling.
Embodiment 7
(1) substrate processing: by silicon wafer by being taken out after argon gas-helium corona treatment 30 minutes；
(2) substrate coats: the silicon wafer Jing Guo hydrophilic treated is soaked in 0.1mg/mL graphene oxide alcohol dispersion liquid
12 hours, taking-up was put into 60 DEG C of dryings of baking oven；
(3) single side is modified: the silicon wafer that step (2) obtains being soaked in decorating liquid 12 hours, soaking temperature is 20 DEG C, is repaired
Adorn the chloroformic solution that liquid is palmitinic acid, concentration 0.5mol/L.Silicon wafer is taken out after 12 hours, is put into 60 DEG C of baking oven drying；
(4) substrate desquamation: the silicon wafer that step (3) obtains is soaked in stripper, and soaking temperature is 30 DEG C, and it is small to impregnate 2
When, parental graphite oxide alkene is removed from substrate by stirring, after stirring 1 hour, takes out silicon wafer.Stone will be aoxidized containing parents
The stripper of black alkene obtains filter cake by filtering, and 60 DEG C of filter cake baking oven obtained by drying to arrive parental graphite oxide ene product, and yield reaches
To 93%, products therefrom is labeled as C7.
Stripper is 0.1mol/L dilute hydrochloric acid.
Fig. 1 is the graphene oxide infrared spectrogram before modification, and Fig. 4 is the parental graphite oxide alkene parents oxidation after modification
Graphene, it can be seen that have strong methyl (1368cm after modification on infrared spectroscopy-1And 2961cm-1), methylene (1455cm-1, 2850cm-1, 2922cm-1) infrared signature absorption peak, it was demonstrated that lauryl amine is grafted successfully on graphene oxide.
Ethyl alcohol, chloroform used in whole process only have tens milliliters, and can be evaporated under reduced pressure recycling.
Embodiment 8
Silicon wafer in embodiment 7 is replaced with into gallium nitride GaN substrate；Remaining condition is same as Example 7, the product of acquisition
Labeled as C8；
Infrared analysis is carried out to C8, and is compared with Fig. 1, obtains conclusion with embodiment 7.
9 granularmetric analysis of embodiment
Granularmetric analysis is carried out to the sample C1~C8 obtained in embodiment using Malvern laser particle analyzer, typical consequence is such as
It is the test result that sample C1 is obtained shown in Fig. 5, from figure 5 it can be seen that the average grain diameter of C1 is 70nm；Other samples
Test result is similar to the above, and the partial size of sample is in the range of 10~1000nm.
The analysis of 10 contact angle of embodiment
It is commercially available before not being modified the parental graphite oxide alkene sample C1~C8 being prepared in embodiment 1-8 and
Graphene oxide is dispersed with deionized water, be added drop-wise to hydrophilic treated glass slide, oleophylic processing glass slide on, baking oven drying after, benefit
The contact angle test of water and oil is carried out with JC2000D3 contact angle measurement, typical consequence is shown in Table 1, the test result of other samples
It is similar to the above.Wherein, when measuring the contact angle with oil, agents useful for same is hexadecane.
The test result of contact angle shows that graphene oxide two sides is all hydrophily, and parental graphite oxide alkene unilateralis
Water, a face oleophylic.
Table 1
The test result of other samples is similar to the above, obtains a face oleophylic, on one side hydrophilic parental graphite oxide
Alkene.
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to
Case study on implementation is imitated, is belonged in technical proposal scope.
Claims (10)
1. a kind of preparation method of parental graphite oxide alkene nano material, which is characterized in that the described method includes:
(1) by graphene oxide-loaded in the substrate on substrate, obtaining being loaded with graphene oxide；
(2) substrate for being loaded with graphene oxide is placed in the solution containing dressing agent, obtains being loaded with the graphite oxide after modification
The substrate of alkene removes substrate, obtains the parental graphite oxide alkene nano material.
2. the preparation method of parental graphite oxide alkene nano material according to claim 1, which is characterized in that step (1)
Described in substrate carry out hydrophilic treated；
Preferably, the hydrophilic treated includes: gas plasma processing；Or
Substrate is soaked in hydrophilic processing liquid；
Preferably, the time of the gas plasma processing is 0.5-2 hours；
It is 2-24 hours that substrate, which is soaked in the soaking time in hydrophilic processing liquid,；
Preferably, the hydrophilic processing liquid is sulfuric acid-hydrogen peroxide mixed solution or sodium hydroxide-potassium peroxydisulfate mixed solution；
Preferably, the volume ratio of sulfuric acid and hydrogen peroxide is 1~5:1 in the sulfuric acid-hydrogen peroxide mixed solution；
The ratio of the quality of sodium hydroxide and potassium peroxydisulfate is 2~6:1 in the sodium hydroxide-potassium peroxydisulfate mixed solution.
3. the preparation method of parental graphite oxide alkene nano material according to claim 1, which is characterized in that step (1)
Described in mode of loading include:
Dispersant liquid drop containing graphene oxide is added on substrate；Or
On substrate by the dispersion liquid spin coating containing graphene oxide；Or
Substrate is immersed in the dispersion liquid containing graphene oxide；
Preferably, the concentration of the dispersion liquid containing graphene oxide is 0.005mg/mL-10.0mg/mL；
Dispersing agent includes at least one of water, ethyl alcohol in the dispersion liquid；
Preferably, soaking time substrate being immersed in the dispersion liquid containing graphene oxide is 2-24 hours.
4. the preparation method of parental graphite oxide alkene nano material according to claim 1, which is characterized in that step (2)
Described in dressing agent be hydrophobing agent；
Solvent is selected from ethyl alcohol, chloroform, acetone, benzene, toluene, carbon tetrachloride, tetrahydrofuran, second in the solution containing dressing agent
At least one of ether, hexamethylene；
Preferably, the hydrophobing agent is selected from least one of alkylamine, long-chain alcohol, halogenated hydrocarbons, long chain acid.
5. the preparation method of parental graphite oxide alkene nano material according to claim 1, which is characterized in that step (2)
Described in by the substrate for being loaded with graphene oxide be placed in the mode in dressing agent include impregnate；
The time of the immersion is 0.5~48 hour；
The temperature of the immersion is 10 DEG C~40 DEG C.
6. the preparation method of parental graphite oxide alkene nano material according to claim 1, which is characterized in that the substrate
Selected from one of nonmetallic substrate, metal substrate, metallic compound substrate；
Preferably, the nonmetallic substrate includes one kind of glass, silicon wafer, sapphire, SiC, ito glass, FTO glass；
The metal substrate includes one of copper substrate, aluminium substrate；
The metallic compound substrate includes GaN substrate, Ga2O3One of substrate.
7. the preparation method of parental graphite oxide alkene nano material according to claim 1, which is characterized in that the removal
The mode of substrate includes: peeling liner bottom；
Preferably, the peeling liner bottom includes: that the substrate for being loaded with the graphene oxide after modifying is soaked in stripper, point
From obtaining the parental graphite oxide alkene nano material；
Preferably, the stripper is selected from least one of at least one of acid or lye.
8. the preparation method of parental graphite oxide alkene nano material according to claim 7, which is characterized in that the immersion
Condition are as follows:
The time of the immersion is 0.5~48 hour；
The temperature of the immersion is 10 DEG C~40 DEG C；
The separation process are as follows: it stands or stirs first or ultrasound, parental graphite oxide alkene nano material fall off from substrate, point
It is dispersed in stripper；
Parental graphite oxide alkene nano material is divided from stripper using one of centrifugation, filtering, suction filtration, film filtering
From.
9. the preparation method of parental graphite oxide alkene nano material according to any one of claims 1 to 8, feature exist
In application of the parental graphite oxide alkene nano material in oil displacement agent, environment-friendly type surfactant, oily waste treatment.
10. the parents that the preparation method of the described in any item parental graphite oxide alkene nano materials of claim 1 to 8 is prepared
Stannic oxide/graphene nano material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910537963.8A CN110371963A (en) | 2019-06-20 | 2019-06-20 | A kind of preparation method and application of parental graphite oxide alkene nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910537963.8A CN110371963A (en) | 2019-06-20 | 2019-06-20 | A kind of preparation method and application of parental graphite oxide alkene nano material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110371963A true CN110371963A (en) | 2019-10-25 |
Family
ID=68249120
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910537963.8A Pending CN110371963A (en) | 2019-06-20 | 2019-06-20 | A kind of preparation method and application of parental graphite oxide alkene nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110371963A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110860273A (en) * | 2019-11-08 | 2020-03-06 | 宁波锋成纳米科技有限公司 | Preparation method and application of magnetic graphene oxide nanoparticles |
| CN110980718A (en) * | 2019-11-08 | 2020-04-10 | 宁波锋成先进能源材料研究院 | Modified graphene oxide and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849732A (en) * | 2012-09-18 | 2013-01-02 | 北京大学 | Method for realizing double-surface asymmetric modification of single-layer graphene |
| CN102887507A (en) * | 2012-09-28 | 2013-01-23 | 上海理工大学 | Simple preparation method of amphipathic graphene |
| CN103818896A (en) * | 2013-11-21 | 2014-05-28 | 太原理工大学 | Method for asymmetrically modifying grapheme or oxidized grapheme |
| CN104386672A (en) * | 2014-10-22 | 2015-03-04 | 复旦大学 | Preparation method of graphite oxide alkene materials in dissymmetrical structure |
| CN104909580A (en) * | 2015-05-20 | 2015-09-16 | 苏州大学 | Transparent hydrophobic grating glass and preparation method thereof |
| CN106587043A (en) * | 2016-12-20 | 2017-04-26 | 哈尔滨工业大学 | Preparation method of amphiphilically reinforced graphene oxide |
-
2019
- 2019-06-20 CN CN201910537963.8A patent/CN110371963A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849732A (en) * | 2012-09-18 | 2013-01-02 | 北京大学 | Method for realizing double-surface asymmetric modification of single-layer graphene |
| CN102887507A (en) * | 2012-09-28 | 2013-01-23 | 上海理工大学 | Simple preparation method of amphipathic graphene |
| CN103818896A (en) * | 2013-11-21 | 2014-05-28 | 太原理工大学 | Method for asymmetrically modifying grapheme or oxidized grapheme |
| CN104386672A (en) * | 2014-10-22 | 2015-03-04 | 复旦大学 | Preparation method of graphite oxide alkene materials in dissymmetrical structure |
| CN104909580A (en) * | 2015-05-20 | 2015-09-16 | 苏州大学 | Transparent hydrophobic grating glass and preparation method thereof |
| CN106587043A (en) * | 2016-12-20 | 2017-04-26 | 哈尔滨工业大学 | Preparation method of amphiphilically reinforced graphene oxide |
Non-Patent Citations (2)
| Title |
|---|
| DAN LUO ET AL.: "Synthesis of graphene-based amphiphilic janus nanosheets via manipulation of hydrogen bonding", 《CARBON》 * |
| 高党鸽等: "Janus纳米材料可控制备的研究进展", 《高分子材料科学与工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110860273A (en) * | 2019-11-08 | 2020-03-06 | 宁波锋成纳米科技有限公司 | Preparation method and application of magnetic graphene oxide nanoparticles |
| CN110980718A (en) * | 2019-11-08 | 2020-04-10 | 宁波锋成先进能源材料研究院 | Modified graphene oxide and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109095462A (en) | A kind of graphene and its preparation method and application | |
| CA2999904C (en) | Industrial method for preparing large-sized graphene | |
| CN108192138B (en) | Modification method of carbon nano tube used as rubber filler | |
| CN104085882B (en) | A kind of few layer is containing the preparation method of oxygen fluorinated graphene | |
| CN106629659A (en) | Preparation method of fluorescent carbon quantum dots employing algae as carbon sources and application | |
| CN110371963A (en) | A kind of preparation method and application of parental graphite oxide alkene nano material | |
| CN108393501B (en) | Preparation method of Cu nanowire with controllable diameter | |
| CN110296973B (en) | SiO2@ Ag @ ZrO2 multilayer core-shell structure nano material and preparation method and application thereof | |
| CN104030290A (en) | Method for producing nanometer silicon by adopting rice hull | |
| CN107282940B (en) | Method for preparing gold nanoparticles by using pseudo-ginseng extracting solution | |
| CN107244697A (en) | A kind of preparation method of individual layer molybdenum disulfide nano sheet | |
| CN108970592B (en) | Preparation method and application of sulfonic acid type silver porous adsorbent for ion adsorption | |
| CN105779096A (en) | Recovery treatment method of waste lubrication oil | |
| CN104986802B (en) | Platy nanometer material and preparation method thereof | |
| CN109569494A (en) | A kind of MXene-Ti3C2The preparation method and applications of nanometer sheet | |
| CN108192143B (en) | Method for modifying carbon nano tube used as rubber filler | |
| CN108468071B (en) | Method for preparing inorganic non-metallic material quantum dots by electrochemical ion impact and application thereof | |
| CN105776200B (en) | A kind of photo catalytic reduction continuously prepares the device and method of graphene | |
| CN110031448B (en) | Preparation method of nano tin dioxide/carbon base point/nano silver surface enhanced Raman substrate | |
| CN104028772B (en) | A kind of preparation method of nickel nano particle | |
| CN109626363A (en) | The method for preparing graphene quantum dot using maltose | |
| CN105800673B (en) | A kind of In4SnS8The preparation method of ultrathin membrane | |
| CN110124705B (en) | Preparation method and application of defective few-layer boron carbide | |
| CN114735685A (en) | Preparation method of fluorinated graphene | |
| CN114160806A (en) | Core-shell structure silver nanoparticles prepared by biomass reduction and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191025 |