CN110950332A - Oil-soluble modified graphene and preparation method thereof - Google Patents
Oil-soluble modified graphene and preparation method thereof Download PDFInfo
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- CN110950332A CN110950332A CN201911313129.7A CN201911313129A CN110950332A CN 110950332 A CN110950332 A CN 110950332A CN 201911313129 A CN201911313129 A CN 201911313129A CN 110950332 A CN110950332 A CN 110950332A
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Abstract
The invention provides oil-soluble modified graphene and a preparation method thereof, wherein the oil-soluble modified graphene comprises the following components in parts by weight: 1-5 parts of thermal reduction graphene, 2-10 parts of surfactant, 5-10 parts of initiator and 75-92 parts of deionized water. According to the invention, the organic modification is carried out on the middle defects of the thermal reduction graphene, the graphene and a surfactant form emulsion micelles in deionized water, the emulsion micelles are decomposed into free radicals by an initiator at 60-80 ℃ and enter the emulsion micelles, then the middle defects of the thermal reduction graphene are attacked to carry out organic modification reaction, and after the reaction is finished, the emulsion is demulsified by using absolute ethyl alcohol to obtain the organic modification graphene.
Description
Technical Field
The invention relates to the field of graphene nano materials, in particular to oil-soluble modified graphene and a preparation method thereof.
Background
Graphene has a unique two-dimensional structure and excellent properties, and is widely used in various fields. When the graphene is applied, the graphene is often dispersed in a matrix by a liquid phase method, but due to the special electronic structure of large pi bond conjugation of graphene, large van der waals force exists between the graphene layers, and the van der waals force between the graphene layers inevitably enables the graphene sheet layers to be agglomerated and stacked again, so that the graphene sheet layers are difficult to disperse to form a stable solution.
In the field of mechanical lubrication, graphene is favored as a nano-scale lubricating oil solid additive, and the unique two-dimensional lamellar structure of the graphene can be cooperated with an oil film between friction pairs to form a lubricating oil film with stronger bearing capacity and better antifriction effect. However, the problems of easy dispersion and agglomeration of graphene in the base oil and the like result in deposition of the prepared base oil containing graphene after storage for a period of time, and the performance of the graphene cannot be embodied at all.
At present, two methods of physically assisting dispersion and chemically modifying graphene by using a surfactant are mainly used for improving the continuous and stable dispersion of graphene in an oily liquid. According to the modified graphene lubricating oil with the patent number of CN108913277A and the preparation method thereof, a potassium nitrate crystal compound coated with a biomass carbon source needs to be carbonized at a high temperature under the protection of argon, the heating rate is guaranteed to be 1 ℃/min, and then the compound is subjected to ultrasonic centrifugation and drying to obtain the modified graphene. The method changes the compatibility of graphene in base oil by grafting affinity oily functional groups to the graphene, thereby realizing the continuous and stable dispersion of the graphene in oily liquid. However, the whole preparation process needs to strictly limit the reaction temperature and the heating rate, the requirement of reaction control on equipment is relatively high, and the large-scale industrial production is not easy to realize.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides oil-soluble modified graphene to solve the problem that the existing graphene is poor in long-term dispersion stability in an oily liquid.
In order to achieve the purpose, the invention adopts the following technical scheme:
the oil-soluble modified graphene comprises, by weight, 1-5 parts of thermally reduced graphene, 2-10 parts of a surfactant, 5-10 parts of an initiator and 75-90 parts of deionized water.
Preferably, the graphene/deionized water composite material comprises 1-3 parts of graphene, 2-3 parts of surfactant, 5-6 parts of initiator and 85-90 parts of deionized water.
Preferably, the surfactant is one of sodium dodecyl sulfate, cetyl trimethyl ammonium bromide and sodium lauryl sulfate.
Preferably, the initiator is one of dibenzoyl peroxide, azobisisobutyronitrile and lauroyl peroxide.
The invention also provides a method for preparing the oil-soluble modified graphene, which is used for solving the problems that the existing graphene preparation process is complicated and the reaction conditions are difficult to control.
The method comprises the following steps:
1) reducing the graphite oxide to obtain thermally reduced graphene;
2) adding graphene and a surfactant into deionized water, and stirring for 1 hour to obtain emulsion A;
3) adding dibenzoyl peroxide into the emulsion A, and stirring for 8-15 hours at the temperature of 60-80 ℃;
4) filtering the solution after reaction, and washing with absolute ethyl alcohol until the filtrate is clear to obtain a filter cake;
5) and drying and collecting the filter cake, and grinding the filter cake into powder to obtain the oil-soluble modified graphene.
Preferably, the graphite oxide is reduced in step 1): weighing a proper amount of graphite oxide, placing the graphite oxide in a tubular furnace, introducing nitrogen into the tubular furnace for protection, reacting for 1 hour at 800 ℃, adding the obtained product into absolute ethyl alcohol, stirring, filtering and drying to obtain the thermal reduction graphene.
Preferably, the stirring temperature in the step 3) is 70 ℃, and the stirring time is 11 hours.
Compared with the prior art, the invention has the following beneficial effects:
the oil-soluble modified graphene is generated by adopting the reaction of thermal reduction graphene, a surfactant, dibenzoyl peroxide, deionized water and the like, and the prepared oil-soluble modified graphene still has good dispersion performance after standing in an oil-soluble solution for a long time, so that the graphene oil solution can have good bearing capacity and antifriction effect for a long time. According to the preparation method of the oil-soluble modified graphene, the middle defects of the thermal reduction graphene are organically modified, the graphene and a surfactant form emulsion micelles in deionized water, the free radicals are decomposed into free radicals through dibenzoyl peroxide at the temperature of 60-80 ℃ and enter the emulsion micelles, then the middle defects of the thermal reduction graphene are attacked to carry out organic modification reaction, and after the reaction is finished, the emulsion is demulsified by using absolute ethyl alcohol to obtain the organic oil-soluble modified graphene.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic diagram of the reaction of the present invention;
FIG. 2 is a transmission electron microscope topography of graphene A of the present invention;
fig. 3 is a resting picture of graphene A, B, C of the present invention in base oil.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the functions of the invention clearer and easier to understand, the invention is further explained by combining the drawings and the detailed implementation mode:
weighing a proper amount of graphite oxide, placing the graphite oxide in a tubular furnace, introducing nitrogen into the tubular furnace for protection, reacting for 1 hour at 800 ℃ to obtain a reaction product, placing the reaction product in a beaker, adding sufficient absolute ethyl alcohol into the reaction product until the reaction product is immersed, stirring for 60min, filtering, and drying for 16 hours at 60 ℃ in vacuum to obtain the thermally reduced graphene.
Thermally reducing graphene prepared by a thermal reduction method into defective graphene, wherein the number of graphene layers is controlled to be below 5, and the transverse size is 1-10 um; the graphene is basically free of functional groups in the plane and contains a large number of holes; the edge contains a small amount of carbonyl functionality. The prepared thermal reduction graphene has huge specific surface area, a large number of defects are formed on the edge and the surface of the graphene, active sites are numerous, more organic functional groups can be bonded in the subsequent grafting reaction, and the lipophilicity of the modified graphene can be improved.
The reaction principle schematic diagram of the invention is shown in fig. 1, when the ionic surfactant peels off graphite, the hydrophobic tail group is adsorbed to the surface of a graphite flake due to van der waals force, the hydrophilic head group tends to be dissolved in water to generate effective charges, the graphite flake interlayer spacing is expanded and the aggregation is hindered through electrostatic repulsion, and graphene is effectively peeled off and stably dispersed; through the stirring effect, the surfactant wraps the graphene and forms micelles in the aqueous solution to form emulsion, then the emulsion is changed into emulsion, the free radical initiator is added to generate free radicals at 60-80 ℃, and the free radicals penetrate through the micelles to attack the graphene, so that the graphene is successfully modified and grafted.
Example 1:
adding 91 parts of deionized water into a beaker, weighing 1 part of thermally reduced graphene and 3 parts of sodium dodecyl sulfate, adding into the beaker, and stirring for 1 hour to obtain emulsion A; adding 5 parts of dibenzoyl peroxide into the emulsion A, and stirring for 10 hours at 60 ℃; the reacted solution was filtered and washed with absolute ethanol until the filtrate was clear. And taking out the filter cake, drying, collecting and grinding the filter cake into powder to obtain the oil-soluble modified graphene A.
Example 2:
adding 90 parts of deionized water into a beaker, weighing 2 parts of thermally reduced graphene and 3 parts of hexadecyl trimethyl ammonium bromide, adding into the beaker, and stirring for 1 hour to obtain emulsion B; adding 5 parts of dibenzoyl peroxide into the emulsion B, and stirring for 11 hours at 70 ℃; the reacted solution was filtered and washed with absolute ethanol until the filtrate was clear. And taking out the filter cake, drying, collecting and grinding the filter cake into powder to obtain the oil-soluble modified graphene B.
Example 3:
adding 87 parts of deionized water into a beaker, weighing 5 parts of thermally reduced graphene and 3 parts of sodium lauryl sulfate, adding into the beaker, and stirring for 1 hour to obtain emulsion C; adding 5 parts of dibenzoyl peroxide into the emulsion C, and stirring for 10 hours at 65 ℃; the reacted solution was filtered and washed with absolute ethanol until the filtrate was clear. And taking out the filter cake, drying, collecting and grinding the filter cake into powder to obtain the oil-soluble modified graphene C.
Example 4:
adding 88 parts of deionized water into a beaker, weighing 3 parts of thermally reduced graphene and 2 parts of hexadecyl trimethyl ammonium bromide, adding into the beaker, and stirring for 1 hour to obtain emulsion D; adding 7 parts of dibenzoyl peroxide into the emulsion D, and stirring for 11 hours at 70 ℃; the reacted solution was filtered and washed with absolute ethanol until the filtrate was clear. And taking out the filter cake, drying, collecting and grinding the filter cake into powder to obtain the oil-soluble modified graphene D.
Example 5:
adding 88 parts of deionized water into a beaker, weighing 4 parts of thermally reduced graphene and 3 parts of hexadecyl trimethyl ammonium bromide, adding into the beaker, and stirring for 1 hour to obtain emulsion E; adding 5 parts of azobisisobutyronitrile into the emulsion E, and stirring at 75 ℃ for 11 hours; the reacted solution was filtered and washed with absolute ethanol until the filtrate was clear. And taking out the filter cake, drying, collecting and grinding the filter cake into powder to obtain the oil-soluble modified graphene E.
Example 6:
adding 91 parts of deionized water into a beaker, weighing 1 part of thermally reduced graphene and 3 parts of hexadecyl trimethyl ammonium bromide, adding into the beaker, and stirring for 1 hour to obtain emulsion F; adding 5 parts of lauroyl peroxide into the emulsion F, and stirring at 80 ℃ for 11 hours; the reacted solution was filtered and washed with absolute ethanol until the filtrate was clear. And taking out the filter cake, drying, collecting and grinding the filter cake into powder to obtain the oil-soluble modified graphene F.
Example 7:
adding 91 parts of deionized water into a beaker, weighing 1 part of thermally reduced graphene and 3 parts of hexadecyl trimethyl ammonium bromide, adding into the beaker, and stirring for 1 hour to obtain emulsion G; adding 5 parts of dibenzoyl peroxide into the emulsion G, and stirring at 80 ℃ for 11 hours; the reacted solution was filtered and washed with absolute ethanol until the filtrate was clear. And taking out the filter cake, drying, collecting and grinding the filter cake into powder to obtain the oil-soluble modified graphene G.
Example 8:
adding 91 parts of deionized water into a beaker, weighing 1 part of thermally reduced graphene and 3 parts of hexadecyl trimethyl ammonium bromide, adding into the beaker, and stirring for 1 hour to obtain emulsion G; adding 5 parts of dibenzoyl peroxide into the emulsion G, and stirring at 80 ℃ for 11 hours; the reacted solution was filtered and washed with absolute ethanol until the filtrate was clear. And taking out the filter cake, drying, collecting and grinding the filter cake into powder to obtain the oil-soluble modified graphene G.
Transmission electron microscopy analysis:
as shown in fig. 2(a), the transmission electron microscope of the thermally reduced graphene has a flat lamellar structure, a few folds, and almost a single layer.
Transmission electron microscopy of oil-soluble modified graphene a as shown in fig. 2(b, c, d) showed slightly more rugosities than the thermally reduced graphene. In FIG. 2, b, c and d represent transmission electron micrographs of oil-soluble modified graphene A at 2 μm, 500nm and 5nm, respectively. From fig. 2(c, d) with higher magnification, the number of layers of the edge of the oil-soluble modified graphene a is small, the number of layers is also almost a single layer, the whole is a semitransparent sheet, and the large and thin lamellar structure of typical graphene is met, and good graphene properties are still maintained.
The dispersion test of the oil-soluble modified graphene in the base oil comprises the following steps:
selecting an oil-soluble modified graphene sample A, B, C and graphene obtained by a conventional thermal reduction method to perform a dissolution and dispersion test on 350N base oil and 500N base oil respectively, adding 2mg of thermal reduced graphene or oil-soluble modified graphene and 20mL of 350N base oil or 500N base oil into an observation bottle, sealing, performing ultrasonic treatment for 1h, and standing. The appearance of the mixed solution after standing for 60 days is shown in FIG. 3; then, a visible light spectrophotometry full-scan test is adopted, and the absorbance value at the 660nm wavelength is calculated, wherein the data is as follows:
as can be seen from the experimental data, after sixty days of standing, the thermally reduced graphene was almost completely precipitated in the 350N base oil and the 500N base oil, and the concentration of the graphene in the upper layer solution was 0 mg/L. After 60 days of standing, the concentrations of the oil-soluble modified graphene A to H in 350N base oil are respectively 38.1mg/L, 43.8mg/L, 29.4mg/L, 27.5mg/L, 24.3mg/L, 21.5mg/L, 17.8mg/L and 13.4mg/L, and the concentrations of the oil-soluble modified graphene A to H in 500N base oil are respectively 40.9mg/L, 45.7mg/L, 34.5mg/L, 31.7mg/L, 28.6mg/L, 25.3mg/L, 23.2mg/L and 19.7 mg/L. Therefore, the graphene prepared by organic modification has a quite good long-term stable dispersion effect in the base oil.
The BPO organically modified graphene provided by the invention greatly improves the oleophylic property of graphene, can improve the dispersing capacity of graphene in base oil, and simultaneously increases the stability of a modified graphene dispersion system in oil. The preparation method for the oil-soluble modified graphene by using the emulsion micelle as the microreactor has the advantages of simple process, low cost and easiness in large-scale industrial production.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (8)
1. The oil-soluble modified graphene is characterized by comprising the following components in parts by weight: 1-5 parts of thermal reduction graphene, 2-10 parts of surfactant, 5-10 parts of initiator and 75-92 parts of deionized water.
2. The oil-soluble modified graphene according to claim 1, comprising the following components in parts by weight: 1-3 parts of thermal reduction graphene, 2-3 parts of surfactant, 5-6 parts of initiator and 88-92 parts of deionized water.
3. The oil-soluble modified graphene according to claim 1, wherein the surfactant is one of sodium dodecyl sulfate, cetyl trimethyl ammonium bromide and sodium lauryl sulfate.
4. The oil-soluble modified graphene according to claim 1, wherein the initiator is one of dibenzoyl peroxide, azobisisobutyronitrile and lauroyl peroxide.
5. The oil-soluble modified graphene according to claim 1 or 2, wherein the thermally reduced graphene is a defective graphene having a large number of defects on the surface.
6. A method for preparing the oil-soluble modified graphene according to claims 1 to 4, comprising the steps of:
1) reducing the graphite oxide to obtain thermally reduced graphene;
2) adding the thermally reduced graphene obtained in the step 2) and a surfactant into deionized water, and stirring for 1 hour to obtain emulsion A;
3) adding an initiator into the emulsion A, and stirring for 8-15 hours at the temperature of 60-80 ℃;
4) filtering the solution after reaction, and washing with absolute ethyl alcohol until the filtrate is clear to obtain a filter cake;
5) and drying and collecting the filter cake, and grinding the filter cake into powder to obtain the oil-soluble modified graphene.
7. The method for preparing oil-soluble modified graphene according to claim 6, wherein the step 1) is to reduce graphite oxide: weighing a proper amount of graphite oxide, placing the graphite oxide in a tubular furnace, introducing nitrogen into the tubular furnace for protection, reacting for 1 hour at 800 ℃, adding the obtained product into absolute ethyl alcohol, stirring, filtering and drying to obtain the thermal reduction graphene.
8. The method for preparing oil-soluble modified graphene according to claim 6, wherein the stirring temperature in the step 3) is 70 ℃ and the stirring time is 11 hours.
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| CN112429719A (en) * | 2020-10-30 | 2021-03-02 | 重庆交通大学 | Lipophilic graphene nanosheet and preparation method thereof |
| CN113072064A (en) * | 2021-04-02 | 2021-07-06 | 中国科学院上海高等研究院 | Modified graphene, graphene film, preparation method and application thereof |
| CN114572976A (en) * | 2022-02-28 | 2022-06-03 | 重庆交通大学 | Functionalized graphene and preparation method thereof |
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