CN109337120B - Graphene oxide composite material and preparation method and application thereof - Google Patents
Graphene oxide composite material and preparation method and application thereof Download PDFInfo
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- CN109337120B CN109337120B CN201811146814.0A CN201811146814A CN109337120B CN 109337120 B CN109337120 B CN 109337120B CN 201811146814 A CN201811146814 A CN 201811146814A CN 109337120 B CN109337120 B CN 109337120B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Abstract
The invention discloses a graphene oxide composite material and a preparation method and application thereof. The preparation method of the graphene oxide composite material comprises the following steps: adding isopropanol, aluminum isopropoxide and graphene oxide into deionized water; and then carrying out hydrothermal reaction to obtain the graphene oxide composite material. The preparation method of the graphene oxide composite material can simply and quickly prepare the graphene oxide composite material, and the prepared graphene oxide composite material has the characteristic of high flame retardant efficiency, can be used as a flame retardant of a polymer material, can reduce the damage to the mechanical property of the polymer material, and can improve the dispersibility of the graphene oxide in the polymer material.
Description
Technical Field
The invention relates to the field of graphene, in particular to a graphene oxide composite material and a preparation method and application thereof.
Background
Due to the unique two-dimensional carbon atom lamellar structure of the graphene material, the graphene material has excellent thermal conductivity, electric conductivity and good barrier property, and can be used as a flame retardant to improve the flame retardant property of a polymer material. Inorganic compounds such as aluminum hydroxide and magnesium hydroxide can also play roles of flame retardance, synergistic flame retardance and smoke suppression when being used as common inorganic flame retardants in a polymer formula, are non-toxic and non-corrosive, but need to be added in large quantities and can greatly damage the mechanical properties of polymer materials.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the present invention aims to provide a graphene oxide composite material, a preparation method and a use thereof, and aims to solve the problems that inorganic flame retardants need to be added in a large amount and the mechanical properties of polymer materials are greatly damaged in the prior art.
A preparation method of a graphene oxide composite material comprises the following steps:
adding isopropanol, aluminum isopropoxide and graphene oxide into deionized water;
and then carrying out hydrothermal reaction to obtain the graphene oxide composite material.
The preparation method of the graphene oxide composite material comprises the following steps of:
and washing and drying a product obtained by the hydrothermal reaction to obtain the graphene oxide composite material.
The preparation method of the graphene oxide composite material comprises the following step of mixing isopropanol, aluminum isopropoxide and graphene oxide according to a mass ratio of 100-20:80-5: 5-0.1.
The preparation method of the graphene oxide composite material comprises the step of preparing the graphene oxide composite material, wherein the mass ratio of isopropanol to aluminum isopropoxide to graphene oxide is 70-30: 25-15: 1.
The preparation method of the graphene oxide composite material comprises the step of carrying out hydrothermal reaction at the temperature of 100-300 ℃.
The preparation method of the graphene oxide composite material comprises the step of carrying out hydrothermal reaction for 6-48 h.
The preparation method of the graphene oxide composite material comprises the step of carrying out hydrothermal reaction at the temperature of 150-220 ℃.
The preparation method of the graphene oxide composite material comprises the step of carrying out hydrothermal reaction for 20-25 h.
The graphene oxide composite material comprises graphene oxide and pseudo-boehmite coated on the surface of the graphene oxide.
Use of the graphene oxide composite material as described above, wherein the graphene oxide composite material is used as a flame retardant for a polymer material.
Has the advantages that: the preparation method of the graphene oxide composite material can be used for simply and quickly preparing the graphene oxide composite material. The graphene oxide composite material prepared by the invention has the characteristic of high flame retardant efficiency, can be used as a flame retardant of a polymer material, can reduce the damage to the mechanical property of the polymer material, and improves the dispersibility of the graphene oxide in the polymer material.
Drawings
Fig. 1 is an infrared spectrum of the graphene oxide composite material and graphene oxide prepared by the present invention.
Fig. 2 is an XRD pattern of the graphene oxide composite material prepared by the present invention.
Fig. 3 is a scanning electron micrograph of graphene oxide.
Fig. 4 is a scanning electron microscope image of the graphene oxide composite material prepared by the present invention.
Fig. 5 is another scanning electron microscope image of the graphene oxide composite material prepared by the present invention.
Fig. 6 is another scanning electron microscope image of the graphene oxide composite material prepared by the present invention.
Detailed Description
The invention provides a graphene oxide composite material and a preparation method and application thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and more clear and definite. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A preparation method of a graphene oxide composite material comprises the following steps:
adding isopropanol, aluminum isopropoxide and graphene oxide into deionized water;
and then carrying out hydrothermal reaction to obtain the graphene oxide composite material.
The preparation method of the graphene oxide composite material is a method for synthesizing pseudo-boehmite on the surface of graphene oxide in situ through a hydrothermal reaction, and the obtained graphene oxide composite material is the graphene oxide coated by the pseudo-boehmite. According to the invention, the pseudo-boehmite-coated graphene oxide (graphene oxide composite material) can be simply and rapidly prepared by a hydrothermal method. The preparation method of the graphene oxide composite material is simple in process and suitable for large-scale industrial production.
Preferably, the hydrothermal reaction further comprises:
and washing and drying a product obtained by the hydrothermal reaction to obtain the graphene oxide composite material.
According to the invention, the product obtained after the hydrothermal reaction is washed and dried, so that impurities in the product can be removed, and the purity of the product is improved.
Preferably, the mass ratio of the isopropanol to the aluminum isopropoxide to the graphene oxide is 100-20:80-5: 5-0.1. The preferable mass ratio is favorable for improving the yield and the coating effect of the pseudo-boehmite coated graphene oxide. More preferably, the mass ratio of the isopropanol to the aluminum isopropoxide to the graphene oxide is 70-30: 25-15: 1.
Preferably, the temperature of the hydrothermal reaction is 100-300 ℃. The optimal hydrothermal reaction temperature is beneficial to improving the yield and the reaction rate of the product, thereby reducing the production cost. More preferably, the temperature of the hydrothermal reaction is 150-220 ℃.
Preferably, the hydrothermal reaction time is 6-48 h. The preferred hydrothermal reaction time of the present invention is a period of time in which the product is produced at a faster rate and with a higher yield, relatively speaking. More preferably, the hydrothermal reaction time is 20-25 h.
The invention provides a graphene oxide composite material, wherein the graphene oxide composite material comprises graphene oxide and pseudo-boehmite coated on the surface of the graphene oxide. The pseudo-boehmite has the characteristics of good peptization performance, strong caking property, high specific surface, large pore volume and the like. The graphene has a continuous and dense lamellar structure, and when the polymer material added with the graphene is subjected to high temperature or open fire, the continuous and dense lamellar structure of the graphene can prevent oxygen from entering the interior of the material. The excellent thermal conductivity of graphene can quickly conduct local over-high heat to the rest of the material, so that the heat is quickly dispersed, and the spread of fire is delayed. And the graphene material has large surface area and is easier to adsorb organic volatile matters generated in the combustion process. The graphene oxide is prepared by oxidizing graphene, the graphene oxide still maintains the layered structure of graphite, and a plurality of oxygen-based functional groups are introduced into each layer of graphene single sheet. The graphene oxide composite material is a flame retardant integrating pseudo-boehmite and graphene oxide, and can exert the respective advantages of the pseudo-boehmite and the graphene oxide, so that the flame retardant efficiency of the product is synergistically improved.
The invention also provides application of the graphene oxide composite material, wherein the graphene oxide composite material is used as a flame retardant of a polymer material. The graphene oxide composite material is pseudo-boehmite-coated graphene oxide, can reduce damage to the mechanical property of a polymer material, and improves the dispersibility of the graphene oxide in the polymer material.
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
Adding 100g of isopropanol, 5g of aluminum isopropoxide and 5g of graphene oxide into deionized water;
and then, carrying out hydrothermal reaction for 48h at 100 ℃, washing and drying a product obtained after the hydrothermal reaction, and finally obtaining the graphene oxide composite material.
Example 2
Adding 100g of isopropanol, 80g of aluminum isopropoxide and 5g of graphene oxide into deionized water;
and then, carrying out hydrothermal reaction for 24h at 200 ℃, washing and drying a product obtained after the hydrothermal reaction, and finally obtaining the graphene oxide composite material.
Example 3
Adding 20g of isopropanol, 5g of aluminum isopropoxide and 0.1g of graphene oxide into deionized water;
and then, carrying out hydrothermal reaction for 48h at 200 ℃, washing and drying a product obtained after the hydrothermal reaction, and finally obtaining the graphene oxide composite material.
Example 4
Adding 20g of isopropanol, 80g of aluminum isopropoxide and 4g of graphene oxide into deionized water;
and then, carrying out hydrothermal reaction for 6h at 300 ℃, washing and drying a product obtained after the hydrothermal reaction, and finally obtaining the graphene oxide composite material.
Example 5
Adding 60g of isopropanol, 5g of aluminum isopropoxide and 5g of graphene oxide into deionized water;
and then, carrying out hydrothermal reaction for 6h at 300 ℃, washing and drying a product obtained after the hydrothermal reaction, and finally obtaining the graphene oxide composite material.
Example 6
Adding 40g of isopropanol, 5g of aluminum isopropoxide and 0.1g of graphene oxide into deionized water;
and then, carrying out hydrothermal reaction for 48h at 100 ℃, washing and drying a product obtained after the hydrothermal reaction, and finally obtaining the graphene oxide composite material.
And detecting the prepared graphene oxide composite material.
Fig. 1 is an infrared spectrum of a graphene oxide composite material (GO-AlOOH) and Graphene Oxide (GO) prepared by the present invention. As shown in the infrared spectrum of the graphene oxide composite material in FIG. 1, the infrared spectrum is 3281cm-1The sharp absorption peak is asymmetric stretching vibration of Al-O-H group, 3089cm-1The sharp absorption peak is the symmetric stretching vibration of the Al-O-H group; at 1063cm-1Sharp absorption peak and 1155cm-1The shoulder peaks near the bending vibration are symmetric bending vibration and asymmetric bending vibration of Al-O-H group, and the vibration length is 729cm-1Distortion vibration of Al-O group appearing nearby 1620cm-1And 1464 cm-1The absorption peaks at (b) are respectively the absorption peaks of C = C and CO-H in graphene oxide, indicating that pseudo-boehmite is generated on graphene oxide. In addition, the infrared spectrogram of the graphene oxide is compared at 1720cm-1The absorption peak of C = O at the position substantially disappears, it is inferred that a reduction reaction occurs in the reaction process, and a part of carbonyl groups on the surface of the graphene oxide is reduced by aluminum isopropoxide.
Fig. 2 is an XRD pattern of the graphene oxide composite material prepared by the present invention. As can be seen from FIG. 2, the pseudoboehmite characteristic diffraction peaks appear at positions with 2 theta of 13.933, 28.332, 38.477, 49.214 and the like, and the base line is relatively flat, the peak intensity is high, the peak shape is sharp, which indicates that the generated pseudoboehmite is well crystallized.
Fig. 3 is a scanning electron microscope image (magnification is 1 k) of graphene oxide, and fig. 4, 5 and 6 are scanning electron microscope images of the graphene oxide composite material prepared by the present invention at magnifications of 5k, 30k and 30k, respectively. As can be seen from the scanning electron microscope image, compared with the untreated graphene oxide, the graphene oxide composite material of the invention has the advantage that the pseudoboehmite is completely coated on the surface of the graphene oxide.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (7)
1. The preparation method of the graphene oxide composite material is characterized by comprising the following steps:
adding isopropanol, aluminum isopropoxide and graphene oxide into deionized water;
then carrying out hydrothermal reaction to obtain a graphene oxide composite material;
the temperature of the hydrothermal reaction is 100-300 ℃;
the time of the hydrothermal reaction is 6-48 h;
the mass ratio of the isopropanol to the aluminum isopropoxide to the graphene oxide is 100-20:80-5: 5-0.1;
in the hydrothermal reaction process, part of carbonyl on the surface of the graphene oxide is reduced by aluminum isopropoxide;
in the graphene oxide composite material, pseudo-boehmite is completely coated on the surface of the graphene oxide.
2. The method for preparing a graphene oxide composite material according to claim 1, wherein the hydrothermal reaction further comprises:
and washing and drying a product obtained by the hydrothermal reaction to obtain the graphene oxide composite material.
3. The method for preparing the graphene oxide composite material according to claim 2, wherein the mass ratio of the isopropanol to the aluminum isopropoxide to the graphene oxide is 70-30: 25-15: 1.
4. The method for preparing the graphene oxide composite material according to claim 1, wherein the temperature of the hydrothermal reaction is 150-220 ℃.
5. The method for preparing the graphene oxide composite material according to claim 1, wherein the hydrothermal reaction time is 20-25 h.
6. The graphene oxide composite material prepared by the preparation method of the graphene oxide composite material according to any one of claims 1 to 5, wherein the graphene oxide composite material comprises graphene oxide and pseudo-boehmite coated on the surface of the graphene oxide; the graphene oxide composite material is used as a flame retardant for reducing damage to mechanical properties of polymer materials.
7. Use of the graphene oxide composite material according to claim 6, wherein the graphene oxide composite material is used as a flame retardant for a polymer material, and the damage to the mechanical properties of the polymer material is reduced.
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Address after: 518117 Longgang Road, Longgang District, Shenzhen, Guangdong (No. 1001) Patentee after: Shenzhen Lihe Technology Innovation Co.,Ltd. Patentee after: Beijing University of Chemical Technology Address before: 518117 Longgang Road, Longgang District, Shenzhen, Guangdong (No. 1001) Patentee before: SHENZHEN BEAUTY STAR Co.,Ltd. Patentee before: Beijing University of Chemical Technology |
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Effective date of registration: 20220107 Address after: No. 1001, Longgang Avenue, Pingxi community, Pingdi street, Longgang District, Shenzhen, Guangdong 518000 Patentee after: Shenzhen TONGCHAN Lixing Technology Group Co.,Ltd. Patentee after: Beijing University of Chemical Technology Address before: 518117 Longgang Road, Longgang District, Shenzhen, Guangdong (No. 1001) Patentee before: Shenzhen Lihe Technology Innovation Co.,Ltd. Patentee before: Beijing University of Chemical Technology |
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