CN113897101A - Graphene oxide sealing and protecting method for iron cultural relics - Google Patents
Graphene oxide sealing and protecting method for iron cultural relics Download PDFInfo
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- CN113897101A CN113897101A CN202111175295.2A CN202111175295A CN113897101A CN 113897101 A CN113897101 A CN 113897101A CN 202111175295 A CN202111175295 A CN 202111175295A CN 113897101 A CN113897101 A CN 113897101A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Abstract
The invention relates to a graphene oxide sealing and protecting method for an iron cultural relic, and belongs to the technical field of sealing and protecting of iron cultural relics. The method adopts a modified graphene oxide/acrylic resin coating B72 composite coating for sealing and protecting, wherein the modified graphene oxide is an acrylate grafted modified graphene oxide nanosheet; ultrasonically dispersing the modified graphene oxide in an acrylic resin coating B72/acetone solution to obtain modified graphene oxide/acrylic resin coating B72 slurry; uniformly coating the modified graphene oxide/acrylic resin coating B72 slurry on the surface of an iron cultural relic to be sealed and protected to form a protective film, and volatilizing acetone to obtain the modified graphene oxide/acrylic resin coating B72 composite protective coating. The modified graphene oxide/acrylic resin coating B72 composite protective coating is transparent and easy to remove by organic solvent, meets the principle that the cultural relics can be reprocessed, and does not affect the original appearance of the cultural relics; the modified graphene oxide labyrinth barrier function effectively blocks corrosion factors such as oxygen, moisture and the like.
Description
Technical Field
The invention relates to a graphene oxide sealing and protecting method for an iron cultural relic, and belongs to the technical field of sealing and protecting of iron cultural relics.
Background
The iron cultural relics have important historical, artistic and scientific values and account for a large proportion of cultural relics collected in the library in China. However, if the chemical activity of iron and the structural characteristics of rusty objects are not protected under the condition of collection, further deterioration corrosion and even mineralization disintegration can be generated.
The protection process of the iron cultural relics generally comprises cleaning, derusting, desalting, inhibiting corrosion, reinforcing and sealing protection. The sealing and protecting layer improves the mechanical strength of the irony cultural relics to a certain extent and has extremely high strengthGreatly slows down the speed of oxygen, moisture and other corrosion factors reaching the surface of the steel plate, and avoids or delays the steel plate from being continuously corroded. Therefore, the selection and optimization of the containment material is critical. The wax such as microcrystalline paraffin, insect white wax and the like is earlier and more widely applied to the protection of iron cultural relics, but is only suitable for small utensils and is difficult to operate and use on large utensils due to process limitation. In addition, synthetic polymer materials such as nitro varnish, polyurethane, acrylic resin, fluorocarbon resin and the like are also applied to the sealing protection of iron cultural relics, but all have defects and cannot well meet the cultural relic protection principle. For example, the nitro varnish is fast to dry, hard and wear-resistant, but has poor adhesion; the polyurethane has good weather resistance and aging resistance, but is difficult to remove after curing; acrylic resin has good film forming property but insufficient corrosion resistance; the fluorocarbon resin has good corrosion resistance, but can generate glare after film forming. In order to promote the development of iron cultural relic protection materials, researchers apply organosilicon materials with excellent hydrophobicity to the sealing and protection of iron cultural relics, but the organosilicon film layer often contains micropores and has poor corrosion resistance. Meanwhile, the addition of the nano-filler in the original sealing and protecting material also becomes a research trend, and researchers have put nano-SiO into consideration2TiO 2 nanoparticles2The powder is added into the acrylic emulsion, so that the hydrophobicity, the acid and alkali resistance and the like of the sealing layer can be improved, but the unmodified nano powder is directly added into the coating, so that the dispersion is not uniform, and the sealing and protecting effect is greatly reduced.
Disclosure of Invention
The invention provides a graphene oxide sealing and protecting method for an iron cultural relic, which aims at the problem of sealing and protecting the iron cultural relic in the prior art, namely modified graphene oxide nanosheets are used as fillers, transparent acrylic resin coating B72 which is easy to remove by an organic solvent is used as a base material, the iron cultural relic is sealed and protected to form a modified graphene oxide/acrylic resin coating B72 composite protective coating on the surface of the iron cultural relic, the labyrinth distribution effect and excellent isolation performance of the modified graphene oxide can effectively prevent corrosion factors such as oxygen and moisture from reaching the surface of the iron cultural relic, so that the corrosion resistance and ageing resistance of the modified graphene oxide/acrylic resin coating B72 composite protective coating are enhanced, meanwhile, the glossiness is reduced, and the cultural relic protection requirement is better met.
A graphene oxide sealing and protecting method for an iron cultural relic adopts a modified graphene oxide/acrylic resin coating B72 composite coating for sealing and protecting, wherein the modified graphene oxide is an acrylate grafted modified graphene oxide nanosheet.
The graphene oxide sealing and protecting method comprises the specific steps of
(1) Ultrasonically dispersing the modified graphene oxide in an acrylic resin coating B72/acetone solution to obtain modified graphene oxide/acrylic resin coating B72 slurry;
(2) uniformly coating the modified graphene oxide/acrylic resin coating B72 slurry on the surface of an iron cultural relic to be sealed and protected to form a protective film, and volatilizing acetone to obtain a modified graphene oxide/acrylic resin coating B72 composite protective coating;
further, the mass fraction of the acrylic resin coating B72 in the acrylic resin coating B72/acetone solution in the step (1) is 1-50%, and the modified graphene oxide accounts for 0.1-3% of the total mass of the modified graphene oxide/acrylic resin coating B72;
further, the coating method is spraying, coating by a coating machine or dipping and pulling;
the preparation method of the modified graphene oxide comprises the following specific steps:
1) ultrasonically dispersing graphene oxide nano sheets in N, N-dimethylformamide DMF to obtain a graphene oxide/DMF solution A, and concentrating to obtain a graphene oxide/DMF solution B;
2) adding thionyl chloride into the graphene oxide/DMF solution B, uniformly mixing, heating and refluxing for 2-12 h, centrifugally separating to remove thionyl chloride, and washing with N, N-dimethylformamide DMF to obtain an acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid;
3) adding triethylamine and hydroxyethyl acrylate into the acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid, and stirring and reacting for 2-48 h at room temperature to obtain an acrylate grafted graphene oxide nanosheet/DMF dispersion liquid;
further, the concentration of the graphene oxide in the graphene oxide/DMF solution B in the step 1) is 10-50 mg/mL, preferably 15-35 mg/mL; the centrifugal concentration rotating speed is 5000-15000 rpm, preferably 8000-12000 rpm;
further, the mass ratio of the graphene oxide in the step 2) to the thionyl chloride is 1: 100-1: 800, preferably 1: 150-1: 500;
preferably, the heating reflux reaction time in the step 2) is 4-8 h;
further, the mass ratio of the triethylamine in the step 3) to the graphene oxide is 6-35: 1, preferably 10-30: 1; the mass ratio of the hydroxyethyl acrylate to the graphene oxide is 3-25: 1, preferably 5-20: 1;
preferably, the stirring reaction time in the step 3) is 6-24 h.
The invention has the beneficial effects that:
(1) according to the invention, the transparent acrylic resin B72 coating which is easy to form a film is taken as a base material, the modified graphene oxide is taken as a filler, and an iron cultural relic is sealed and protected to form a modified graphene oxide/acrylic resin coating B72 composite protective coating on the surface, so that the composite protective coating is easy to remove, and the reprocessable principle in cultural relic protection is met; the modified graphene oxide can solve the glare problem of a pure acrylic resin B72 coating;
(2) the modified graphene oxide nanosheets are obtained by chemically modifying and grafting acrylic ester bonds, can be uniformly dispersed in the acrylic resin coating B72, and can effectively prevent corrosion factors such as oxygen, moisture and the like from reaching the surface of an iron cultural relic due to the labyrinth distribution effect and excellent isolation performance of the modified graphene oxide, so that the corrosion resistance and ageing resistance of the modified graphene oxide/acrylic resin coating B72 composite protective coating are enhanced;
(3) the modification method of the graphene oxide nanosheet is simple, mild and controllable in reaction condition, low in energy consumption and suitable for large-scale production; the modified graphene oxide/acrylic resin coating B72 slurry can be formed into a film on the surface of an iron cultural relic by brushing, spraying or dipping and pulling and other methods, has no requirements on the shape and size of the iron cultural relic, and has strong operability.
Drawings
Fig. 1 is a microscopic morphology of modified graphene oxide nanoplatelets of example 1;
FIG. 2 is a surface micro-topography of the modified graphene oxide/acrylic resin coating B72 composite protective coating of example 1;
FIG. 3 is a cross-sectional micro-topography of a modified graphene oxide/acrylic resin coating B72 composite protective coating of example 1;
FIG. 4 is a cross-sectional micro-topography of a modified graphene oxide/acrylic resin coating B72 composite protective coating of example 2;
FIG. 5 is a sample object of a sample iron sealed with graphene oxide according to example 3;
FIG. 6 is a sample object of the iron sample sealed and protected by graphene oxide in example 3.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a graphene oxide sealing and protecting method for an iron cultural relic comprises the following specific steps: sealing and protecting by adopting a modified graphene oxide/acrylic resin coating B72 composite coating, wherein the modified graphene oxide is an acrylate grafted modified graphene oxide nanosheet;
the graphene oxide sealing and protecting method comprises the specific steps of
(1) Ultrasonically dispersing the modified graphene oxide in an acrylic resin coating B72/acetone solution to obtain modified graphene oxide/acrylic resin coating B72 slurry; wherein the mass fraction of the acrylic resin coating B72 in the acrylic resin coating B72/acetone solution is 5%, and the modified graphene oxide accounts for 0.5% of the total mass of the modified graphene oxide/acrylic resin coating B72;
(2) uniformly spraying the modified graphene oxide/acrylic resin coating B72 slurry on the surface of an iron cultural relic to be sealed and protected through a spray gun to form a protective film, drying for 12 hours at room temperature until acetone is completely volatilized to obtain a modified graphene oxide/acrylic resin coating B72 composite protective coating;
the preparation method of the modified graphene oxide comprises the following specific steps:
1) ultrasonically dispersing 50mg of graphene oxide nanosheets in 50mLN, N-dimethylformamide DMF to obtain a graphene oxide/DMF solution A, and centrifuging and concentrating for 3 times by adopting a centrifuge at the rotating speed of 10000rpm/min to obtain a graphene oxide/DMF solution B, wherein the concentration of graphene oxide in the graphene oxide/DMF solution B is 20 mg/mL;
2) adding 25mL of thionyl chloride into 2mL of graphene oxide/DMF solution B, uniformly mixing, heating to 70 ℃, carrying out reflux reaction for 6h, carrying out centrifugal separation to remove thionyl chloride, and washing with N, N-dimethylformamide DMF to obtain an acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid;
3) adding 1.4g of triethylamine and 1.0g of hydroxyethyl acrylate into the acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid, stirring and reacting for 8 hours at room temperature, and centrifugally washing to remove redundant triethylamine and hydroxyethyl acrylate to obtain an acrylate grafted graphene oxide nanosheet/DMF dispersion liquid; wherein the mass ratio of triethylamine to graphene oxide is 35:1, and the mass ratio of hydroxyethyl acrylate to graphene oxide is 25: 1;
the microscopic morphology of the modified graphene oxide nanosheet is shown in fig. 1, and as can be seen from fig. 1, the modified graphene oxide is in a stretched lamellar shape, does not have the conditions of agglomeration and severe wrinkling, and still maintains the original two-dimensional thin-layer structure;
the surface microscopic morphology of the modified graphene oxide/acrylic resin coating B72 composite protective coating in the embodiment is shown in FIG. 2, and it can be seen from FIG. 2 that the surface of the coating formed after spraying is relatively flat and dense, and the damage of the surface layer of the coating is caused by the relatively fast volatilization of the surface layer solvent in the spraying process, so that the sealing performance of the inner layer is not affected;
the cross-sectional micro-morphology of the modified graphene oxide/acrylic resin coating B72 composite protective coating in this example is shown in FIG. 3, and it can be seen from FIG. 3 that, from the cross section of the coating, the whole coating is uniform and dense, and there is no situation of non-uniform structure due to the addition of graphene oxide lamella, and there is no situation of damage to the strength of the coating due to fast solvent evaporation, such as dry cracking.
Example 2: a graphene oxide sealing and protecting method for an iron cultural relic comprises the following specific steps: sealing and protecting by adopting a modified graphene oxide/acrylic resin coating B72 composite coating, wherein the modified graphene oxide is an acrylate grafted modified graphene oxide nanosheet;
the graphene oxide sealing and protecting method comprises the specific steps of
(1) Ultrasonically dispersing the modified graphene oxide in an acrylic resin coating B72/acetone solution to obtain modified graphene oxide/acrylic resin coating B72 slurry; wherein the mass fraction of the acrylic resin coating B72 in the acrylic resin coating B72/acetone solution is 2%, and the modified graphene oxide accounts for 0.8% of the total mass of the modified graphene oxide/acrylic resin coating B72;
(2) uniformly coating the modified graphene oxide/acrylic resin coating B72 slurry on the surface of an iron cultural relic to be sealed and protected by a coating machine to form a protective film, drying for 8 hours at room temperature until acetone is completely volatilized to obtain a modified graphene oxide/acrylic resin coating B72 composite protective coating;
the preparation method of the modified graphene oxide comprises the following specific steps:
1) ultrasonically dispersing 60mg of graphene oxide nanosheets in 100mLN, N-dimethylformamide DMF to obtain a graphene oxide/DMF solution A, and centrifuging and concentrating for 6 times by adopting a centrifuge at the rotating speed of 12000rpm/min to obtain a graphene oxide/DMF solution B, wherein the concentration of graphene oxide in the graphene oxide/DMF solution B is 35 mg/mL;
2) adding 28mL of thionyl chloride into 1mL of graphene oxide/DMF solution B, uniformly mixing, heating to 50 ℃, carrying out reflux reaction for 8 hours, carrying out centrifugal separation to remove thionyl chloride, and washing with N, N-dimethylformamide DMF to obtain an acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid;
3) adding 0.28g of triethylamine and 0.105g of hydroxyethyl acrylate into the acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid, stirring and reacting for 2 hours at room temperature, and centrifugally washing to remove redundant triethylamine and hydroxyethyl acrylate to obtain an acrylate grafted graphene oxide nanosheet/DMF dispersion liquid; wherein the mass ratio of triethylamine to graphene oxide is 8:1, and the mass ratio of hydroxyethyl acrylate to graphene oxide is 3: 1;
the cross-sectional micro-morphology of the modified graphene oxide/acrylic resin coating B72 composite protective coating in the embodiment is shown in FIG. 4, and as can be seen from FIG. 4, the modified graphene oxide added into B72 is tightly bonded with the B72 matrix, and the original two-dimensional lamellar insertion into the matrix is still maintained.
Example 3: a graphene oxide sealing and protecting method for an iron cultural relic comprises the following specific steps: sealing and protecting by adopting a modified graphene oxide/acrylic resin coating B72 composite coating, wherein the modified graphene oxide is an acrylate grafted modified graphene oxide nanosheet;
the graphene oxide sealing and protecting method comprises the specific steps of
(1) Ultrasonically dispersing the modified graphene oxide in an acrylic resin coating B72/acetone solution to obtain modified graphene oxide/acrylic resin coating B72 slurry; wherein the mass fraction of the acrylic resin coating B72 in the acrylic resin coating B72/acetone solution is 2%, and the modified graphene oxide respectively accounts for 0, 0.5%, 1.0%, 1.5%, 2.0%, 2.5% and 3.0% of the total mass of the modified graphene oxide/acrylic resin coating B72;
(2) coating the modified graphene oxide/acrylic resin coating B72 slurry on the surface of an iron cultural relic to be sealed and protected to form a protective film, drying for 8 hours at room temperature until acetone is completely volatilized to obtain a modified graphene oxide/acrylic resin coating B72 composite protective coating;
taking modified graphene oxide accounting for 0.5% of the total mass of the modified graphene oxide/acrylic resin coating B72 as a modified graphene oxide/acrylic resin coating B72 slurry sample, adopting an iron sample for coating on a sample wafer in a dipping and pulling mode as shown in figure 5, and adopting a spray gun spraying mode as shown in figure 6, wherein as can be seen from figures 5 and 6, the dipping and pulling mode is easy to generate slurry accumulation at the edge of the sample, the edge is thicker, and the spraying can ensure that the slurry is uniformly spread on the surface of the sample;
the preparation method of the modified graphene oxide comprises the following specific steps:
1) ultrasonically dispersing 100mg of graphene oxide nanosheets in 120mLN, N-dimethylformamide DMF to obtain a graphene oxide/DMF solution A, and centrifuging and concentrating for 4 times by adopting a centrifuge at the rotating speed of 10000rpm/min to obtain a graphene oxide/DMF solution B, wherein the concentration of graphene oxide in the graphene oxide/DMF solution B is 25 mg/mL;
2) adding 20mL of thionyl chloride into 2mL of graphene oxide/DMF solution B, uniformly mixing, heating to 70 ℃, carrying out reflux reaction for 6h, carrying out centrifugal separation to remove thionyl chloride, and washing with N, N-dimethylformamide DMF to obtain an acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid;
3) adding 1.0g of triethylamine and 0.75g of hydroxyethyl acrylate into the acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid, stirring and reacting for 6 hours at room temperature, and centrifugally washing to remove redundant triethylamine and hydroxyethyl acrylate to obtain an acrylate grafted graphene oxide nanosheet/DMF dispersion liquid; wherein the mass ratio of triethylamine to graphene oxide is 20:1, and the mass ratio of hydroxyethyl acrylate to graphene oxide is 5: 1;
the iron sample sprayed with the modified graphene oxide/acrylic resin coating B72 slurry to form a film in the embodiment is placed in a salt spray corrosion box for simulation experiments, and the salt spray corrosion test results are shown in Table 1,
TABLE 1 salt spray Corrosion test results for different surface treatment samples
As can be seen from table 1, the modified graphene oxide nanosheets obtained by chemically modifying and grafting the acrylic ester bonds with the graphene oxide nanosheets can be uniformly dispersed in the acrylic resin coating B72, and the labyrinth distribution effect and excellent isolation performance of the modified graphene oxide can effectively prevent corrosion factors such as oxygen and moisture from reaching the surface of an iron cultural relic, so that the corrosion resistance and the aging resistance of the modified graphene oxide/acrylic resin coating B72 composite protective coating are enhanced.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (8)
1. A graphene oxide sealing and protecting method for an iron cultural relic is characterized by comprising the following steps: and sealing and protecting by adopting a modified graphene oxide/acrylic resin coating B72 composite coating, wherein the modified graphene oxide is an acrylate grafted modified graphene oxide nanosheet.
2. The graphene oxide sealing and protecting method for the iron cultural relics, which is characterized by comprising the following steps: the graphene oxide sealing and protecting method comprises the specific steps of
(1) Ultrasonically dispersing the modified graphene oxide in an acrylic resin coating B72/acetone solution to obtain modified graphene oxide/acrylic resin coating B72 slurry;
(2) uniformly coating the modified graphene oxide/acrylic resin coating B72 slurry on the surface of an iron cultural relic to be sealed and protected to form a protective film, and volatilizing acetone to obtain the modified graphene oxide/acrylic resin coating B72 composite protective coating.
3. The graphene oxide sealing and protecting method for the iron cultural relics, which is characterized in that the preparation method for the modified graphene oxide comprises the following specific steps:
1) ultrasonically dispersing graphene oxide nano sheets in N, N-dimethylformamide DMF to obtain a graphene oxide/DMF solution A, and concentrating to obtain a graphene oxide/DMF solution B;
2) adding thionyl chloride into the graphene oxide/DMF solution B, uniformly mixing, heating and refluxing for 2-12 h, centrifugally separating to remove thionyl chloride, and washing with N, N-dimethylformamide DMF to obtain an acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid;
3) and adding triethylamine and hydroxyethyl acrylate into the acyl chloride group grafted graphene oxide nanosheet/DMF dispersion liquid, and stirring and reacting for 2-48 h at room temperature to obtain the acrylate grafted graphene oxide nanosheet/DMF dispersion liquid.
4. The graphene oxide sealing and protecting method for the iron cultural relics, which is characterized by comprising the following steps: the concentration of graphene oxide in the graphene oxide/DMF solution B in the step 1) is 10-50 mg/mL.
5. The graphene oxide sealing and protecting method for the iron cultural relics, which is characterized by comprising the following steps: and 2) the mass ratio of the graphene oxide to the thionyl chloride in the step 2) is 1: 100-1: 800.
6. The graphene oxide sealing and protecting method for the iron cultural relics, which is characterized by comprising the following steps: and 3) the mass ratio of triethylamine to graphene oxide is 6-35: 1, and the mass ratio of hydroxyethyl acrylate to graphene oxide is 3-25: 1.
7. The graphene oxide sealing and protecting method for the iron cultural relics, which is characterized by comprising the following steps: in the step (1), the mass fraction of the acrylic resin coating B72 in the acrylic resin coating B72/acetone solution is 1-50%, and the modified graphene oxide accounts for 0.1-3% of the total mass of the modified graphene oxide/acrylic resin coating B72.
8. The graphene oxide sealing and protecting method for the iron cultural relics, which is characterized by comprising the following steps: the coating method is spraying, coater coating or dipping and pulling.
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