CN111662584A - Application of graphene quantum dot/polyphenylene sulfide composite material as preservative - Google Patents
Application of graphene quantum dot/polyphenylene sulfide composite material as preservative Download PDFInfo
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- CN111662584A CN111662584A CN202010664990.4A CN202010664990A CN111662584A CN 111662584 A CN111662584 A CN 111662584A CN 202010664990 A CN202010664990 A CN 202010664990A CN 111662584 A CN111662584 A CN 111662584A
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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
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- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
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Abstract
The invention provides an application of a graphene quantum dot/polyphenylene sulfide composite material as a preservative, and belongs to the technical field of material application. The graphene quantum dots in the graphene quantum dot/polyphenylene sulfide composite material are not only coated on the surface of the flower-shaped polyphenylene sulfide sheet layer, but also effectively filled between the sheet layers, so that the composite material has a more compact structure, and the hydrophobicity and the corrosion resistance of the composite material can be improved; and the graphene quantum dot/polyphenylene sulfide composite material is dispersed in the epoxy resin, so that the hydrophobicity and viscosity of the epoxy resin can be obviously improved, the anticorrosion performance of the coating obtained by dispersing the graphene quantum dot/polyphenylene sulfide composite material and the film-forming assistant in the epoxy resin and curing the film-forming assistant is obviously improved, and the high-performance protection effect on the metal surface is achieved.
Description
Technical Field
The invention relates to an application of a graphene quantum dot/polyphenylene sulfide composite material as a preservative, and belongs to the technical field of material application.
Background
The graphene quantum dots have the advantages of good water solubility, low toxicity, environmental friendliness, strong biocompatibility, rich surface activity, easy functionalization and the like, become a material capable of being doped with a high-performance polymer, can improve the performance of a composite material, and attract wide attention of various social circles. In addition, due to the self-assembly characteristic of the graphene quantum dots, when the graphene quantum dots react with other polymers, the self-assembly of products can be promoted and promoted, and the graphene quantum dots are stacked into nano structures with different dimensions. The method can be used for preparing Nano graphene oxide (Nano-GO) particles with multi-scale structures, and the Nano graphene oxide particles are tightly stacked on the surfaces and in the pore channels of the polyphenylene sulfide, so that the problems of large graphene oxide sheet layers, accumulation and aggregation are solved, and the defect of poor compatibility with polymers is overcome.
Polyphenylene sulfide (abbreviated as PPS) is a polymer containing a p-phenylene sulfide repeating structural unit in a molecule, is a novel functional engineering plastic, and is widely applied to the fields of electronics, automobiles, machinery and chemical engineering. The microscopic form of the polyphenylene sulfide has the structures of lamellar, hollow spherical, rod-shaped, flower-shaped and the like, the size span is large and controllable, the structures have hyperbranched and pure linear types, and the typical polymerization degree of common chemical materials is spanned. Polyphenylene sulfide is known as a non-traditional novel universal material, and has many advantages: such as stable mechanical size, high insulation, high toughness, solvent resistance, high temperature resistance, etc., but also because of stable properties and difficult handling, the application is not wide enough. Fortunately, the polyphenylene sulfide can also be directly used as a substrate of a catalyst or a substrate of a composite material, and can be compounded with a carbon-based material with a specific function, so that a high-quality composite material is obtained and is used in the field of coatings with anticorrosion performance.
Disclosure of Invention
The invention aims to provide an application of a graphene quantum dot/polyphenylene sulfide composite material as a preservative.
Preparation of graphene quantum dot/polyphenylene sulfide composite material and anticorrosive paint
Preparing a graphene quantum dot/polyphenylene sulfide composite material: mixing flower-shaped polyphenylene sulfide and graphene quantum dots, adding the mixture into an organic solvent NMP, stirring and reacting for 3.5-4 h at 220-225 ℃, heating to 270-275 ℃, and continuing stirring and reacting for 1.5-2 h to obtain a gray precipitate; cooling to room temperature, filtering, repeatedly washing with ethanol, acetone and the like, and freeze-drying to obtain the graphene quantum dot/polyphenylene sulfide composite material; the flower-shaped polyphenyl ether and the graphene quantum dots are mixed according to the following mass percentage: 93-99% (preferably 95-97%) of flower-shaped polyphenylene sulfide, and 1-7% (preferably 3-5%) of graphene quantum dots; the freeze drying is carried out at the temperature of-50 to-60 ℃ for 12 to 24 hours.
Preparing an anticorrosive coating: dispersing the graphene quantum dot/polyphenylene sulfide composite material and the film-forming additive into epoxy resin, and uniformly mixing to obtain the anticorrosive paint; the addition amount of the graphene quantum dot/polyphenylene sulfide composite material is 9-12% of the mass of the epoxy resin; the addition amount of the film-forming additive is 2-2.5% of the mass of the epoxy resin.
Second, structure of graphene quantum dot/polyphenylene sulfide composite material
1. Infrared and XRD analysis
FIG. 1 is an infrared spectrum and XRD diagram of polyphenylene sulfide, graphene quantum dots and graphene quantum dot/polyphenylene sulfide composite material. Fig. 1A shows infrared spectra of polyphenylene sulfide, graphene quantum dots, and a graphene quantum dot/polyphenylene sulfide composite material, and characteristic peaks of GQDs and PPS appear in XRD patterns of the Graphene Quantum Dots (GQDs) and the polyphenylene sulfide (PPS), which proves that the GQDs and the PPS are successfully prepared. In the figure, all characteristic peaks of polyphenylene sulfide and graphene quantum dots exist in a graphene quantum dot/polyphenylene sulfide composite material sample, and the positions of the peaks are not changed and are 3000 cm−1The peaks become more pronounced, indicating the successful preparation of the composite. Fig. 1B is an XRD chart in which the mass percentages of the polyphenylene sulfide, the graphene quantum dots and the GQDs/PPS composite material are 0.5%, 1%, 3% and 5%, and in XRD charts of the GQDs and the PPS, corresponding characteristic peaks respectively appear, and compared with the crystallization peaks of pure PPS and the GQDs/PPS composite material, it is found that no new crystallization peak appears on the XRD chart, and the characteristic peaks of the GQDs do not disappear. It can be judged that GQDs are present on the surface of the polyphenylene sulfide sheet layer having a flower bunch-like structure. No impurity peaks were observed, confirming that the GQDs/PPS composite was of good quality.
2. Micro-topography analysis
Fig. 2 is a scanning electron microscope image of the prepared sample, and fig. 2A shows that the prepared polyphenylene sulfide is in a flower bunch shape, the flower bunch is formed by stacking PPS with thin layers and large sizes, and the ordered arrangement structure has a large specific surface area and can provide rich sites for subsequent material compounding. FIG. 2B is a scanning electron microscope image of the GQDs/PPS composite material under low magnification, and it can be seen in the image that the GQDs/PPS composite material has very good dispersibility, substantially uniform particle size, and uniform dispersion. From the high magnification diagram of the CGQDs/PPS composite material shown in FIG. 2, it can be seen that the sheet layer gaps of the composite material structure become smaller and compact and full, and mainly after the graphene quantum dots are subjected to in-situ self-assembly on the surface of polyphenylene sulfide, the graphene quantum dots not only coat the surface of the sheet layer, but also fill the gaps between the sheet layers, so that the composite material can better resist corrosion agents and protect industrial equipment and the like from corrosion of acid, alkali and salt. The GQDs layer with the polyphenylene sulfide surface uniformly distributed through self-assembly can be obviously seen in the enlarged image 2D of the GQDs/PPS composite material, so the success of the preparation of the composite material is also proved from the aspects of micro morphology and structure, which is also consistent with the FTIR characterization result.
Third, the performance of the graphene quantum dot/polyphenylene sulfide composite coating
FIG. 3 shows zeta potential polarization curves of GQDs/PPS composite coatings at different GQDs contents. The test solution was a 3.5% NaCl solution, and the test items were: polarization curve, corrosion potential, corrosion current. Data results were obtained as shown in FIG. 3The corrosion potential Ec = -478mV for pure PPS and the corrosion current ic = 9.789 × 10 when no GQDs are doped-4A/cm2The GQDs/PPS composite coating has the corrosion potential of Ec = -451mV when the GQDs doping with 3.0 percent is contained, and the corrosion current is ic = 1.417 × 10-4A/cm2The GQDs/PPS composite coating has the highest corrosion potential with Ec = -427 mV and the lowest corrosion current with ic =1.258 × 10 when the GQDs is doped with 5.0 percent of the GQDs-4A/cm2The addition of the GQDs is shown to remarkably improve the corrosion resistance of the GQDs/PPS composite coating, and the composite coating added with 5.0 percent of the GQDs also shows the best corrosion resistance, the content of the GQDs is 1.0 percent and 7.0 percent, the corrosion rate of the GQDs/PPS composite coating is greatly influenced, and the sample shows a higher ic value (7.619 × 10)-4A/cm2、8.705×10-4A/cm2) The reason why the content of the corrosion rate GQDs is increased by 5.0% is that the GQDs are not formed into films or uniformly dispersed on the surface of PPS, which not only reduces the adhesion to base materials such as metals and the like to cause the reduction of protection effect, but also creates new reactive active sites on the surface of the base to enhance the corrosion to the base materials.
In conclusion, the graphene quantum dot/polyphenylene sulfide composite material is successfully prepared in a simple physical doping mode, and the doped graphene quantum dots not only coat the surface of the flower-shaped polyphenylene sulfide sheet layer, but also are effectively filled between the sheet layers, so that the composite material has a more compact structure, and the hydrophobicity and the corrosion resistance of the composite material can be improved; and the graphene quantum dot/polyphenylene sulfide composite material is dispersed in the epoxy resin, so that the hydrophobicity and viscosity of the epoxy resin can be obviously improved, the anticorrosion performance of the coating obtained by dispersing the graphene quantum dot/polyphenylene sulfide composite material and the film-forming assistant in the epoxy resin and curing the film-forming assistant is obviously improved, and the high-performance protection effect on the metal surface is achieved.
Drawings
FIG. 1 is an infrared spectrum and XRD diagram of polyphenylene sulfide, graphene quantum dots and graphene quantum dot/polyphenylene sulfide composite material.
FIG. 2 is a scanning electron micrograph of the prepared sample.
FIG. 3 shows zeta potential polarization curves of GQDs/PPS composite coatings at different GQDs contents.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1
(1) Preparation of flower-like polyphenylene sulfide
Weighing 79.5 g of sodium sulfide nonahydrate, adding the sodium sulfide nonahydrate into 200 ml of N-methylpyrrolidone (NMP) solution, continuously introducing nitrogen into a three-neck flask to remove oxygen in the flask because the sodium sulfide is very easy to absorb moisture, stirring and heating the three-neck flask at 160 ℃ for 1 hour to perform dehydration reaction to obtain dark green anhydrous sodium sulfide-NMP solution, cooling, and pouring the solution into a reaction kettle; 6.225 g of anhydrous lithium chloride is taken as a catalyst and added into a high-temperature high-pressure reaction kettle to be mixed uniformly, strong alkali sodium hydroxide is added under the conditions of room temperature and stirring (the stirring speed is 40 r/min), the solution is adjusted to be alkaline to promote the nucleophilic substitution reaction, the temperature of a reaction system is slowly increased, and 44.1 g of p-dichlorobenzene is added under the stirring condition; after the reaction kettle is sealed, the stirring speed is adjusted to 900 r/min for continuous stirring, and simultaneously nitrogen is introduced to replace the air in the reaction kettle so as to prevent S2-Oxidized; then the temperature is raised to 220 ℃ and 270 ℃, and the temperature is kept for reaction for 2.5 h. After the reaction is finished, cooling to room temperature, adding distilled water in a ratio of 1:1 for dilution to obtain turbid solution with white precipitate; repeatedly washing with a mixed solution of deionized water and ethanol for several times, filtering, and drying in an air-blast drying oven at 60 ℃ after washing to obtain flower-shaped polyphenylene sulfide.
(2) Preparation of graphene quantum dots
Dispersing 0.1g of network-like reduced graphene oxide in 100mL of concentrated nitric acid, magnetically stirring, heating to 150 ℃ in an oil bath, simultaneously condensing circulating water, and reacting at constant temperature for 12 h; then removing the condensed water, and continuing to evaporate for 2-3 h at constant temperature; cooling to room temperature, adding ultrapure water into the mixture, and performing ultrasonic dispersion for 10-15 min; filtering, concentrating the obtained filtrate to 10-30 mL by rotary evaporation, and putting into a 3000-8000 Da dialysis bag for dialysis for 1-2 days; performing rotary evaporation and concentration on the obtained dialysate again to obtain high-concentration nitrogen-doped graphene quantum dots; and (5) performing vacuum freeze drying to obtain the light yellow nitrogen-doped graphene quantum dots.
(3) Preparation of graphene quantum dot/polyphenylene sulfide composite material
Mixing 0.99g of flower-shaped polyphenylene sulfide and 0.01g of graphene quantum dots, adding the mixture into an organic solvent NMP, stirring and reacting for 4 hours at 220 ℃, and stirring and reacting for 2 hours at 270-275 ℃ to obtain a gray precipitate; and cooling to room temperature, filtering, repeatedly washing with ethanol, acetone and the like, and freeze-drying to obtain the graphene quantum dot/polyphenylene sulfide composite material with the graphene quantum dot content of 1%.
(4) Testing of Corrosion protection
The coating of the composite coating is carried out according to GB/T1727--4A/cm2。
Example 2
(1) Preparing flower-shaped polyphenylene sulfide: as in example 1.
(2) Preparing graphene quantum dots: as in example 1.
(3) Preparing a graphene quantum dot/polyphenylene sulfide composite material: mixing 0.97g of flower-shaped polyphenylene sulfide and 0.03g of graphene quantum dots, adding the mixture into an organic solvent NMP, stirring and reacting for 4 hours at 220 ℃, and stirring and reacting for 2 hours at 270-275 ℃ to obtain a gray precipitate; and cooling to room temperature, filtering, repeatedly washing with ethanol, acetone and the like, and freeze-drying to obtain the graphene quantum dot/polyphenylene sulfide composite material with the graphene quantum dot content of 3%.
(4) The operation is the same as example 1, and the corrosion resistance is shown in FIG. 3, wherein the corrosion potential Ec = -451mV, the corrosion current is ic = 1.417 × 10-4A/cm2。
Example 3
(1) Preparing flower-shaped polyphenylene sulfide: as in example 1.
(2) Preparing graphene quantum dots: as in example 1.
(3) Preparing a graphene quantum dot/polyphenylene sulfide composite material: mixing 0.95g of flower-shaped polyphenylene sulfide and 0.05g of graphene quantum dots, adding the mixture into an organic solvent NMP, stirring and reacting for 4 hours at 220 ℃, and stirring and reacting for 2 hours at 270-275 ℃ to obtain a gray precipitate; and cooling to room temperature, filtering, repeatedly washing with ethanol, acetone and the like, and freeze-drying to obtain the graphene quantum dot/polyphenylene sulfide composite material with the graphene quantum dot content of 5%.
(4) The operation is the same as example 1, and the corrosion resistance is measured as shown in FIG. 3, wherein the corrosion potential Ec = 427 mV, and the corrosion current ic =1.258 × 10-4A/cm2。
Example 4
(1) Preparing flower-shaped polyphenylene sulfide: as in example 1.
(2) Preparing graphene quantum dots: as in example 1.
(3) Preparing a graphene quantum dot/polyphenylene sulfide composite material: mixing 0.93g of flower-shaped polyphenylene sulfide and 0.07g of graphene quantum dots, adding the mixture into an organic solvent NMP, stirring and reacting for 4 hours at 220 ℃, and stirring and reacting for 2 hours at 270-275 ℃ to obtain a gray precipitate; and cooling to room temperature, filtering, repeatedly washing with ethanol, acetone and the like, and freeze-drying to obtain the graphene quantum dot/polyphenylene sulfide composite material with the graphene quantum dot content of 7%.
(4) The operation is the same as example 1, and the corrosion resistance is measured as shown in FIG. 3, wherein the corrosion potential Ec = 434 mV, and the corrosion current ic = 8.705 × 10-4A/cm2。
Claims (7)
1. An application of a graphene quantum dot/polyphenylene sulfide composite material as a preservative.
2. The application of the graphene quantum dot/polyphenylene sulfide composite material as a preservative according to claim 1, wherein the graphene quantum dot/polyphenylene sulfide composite material is characterized in that: preparation of the anticorrosive paint: and dispersing the graphene quantum dot/polyphenylene sulfide composite material and the film-forming additive into epoxy resin, and uniformly mixing to obtain the anticorrosive paint.
3. The application of the graphene quantum dot/polyphenylene sulfide composite material as a preservative according to claim 2, wherein the graphene quantum dot/polyphenylene sulfide composite material is characterized in that: the addition amount of the graphene quantum dot/polyphenylene sulfide composite material is 9-12% of the mass of the epoxy resin.
4. The application of the graphene quantum dot/polyphenylene sulfide composite material as a preservative according to claim 2, wherein the graphene quantum dot/polyphenylene sulfide composite material is characterized in that: the addition amount of the film-forming additive is 2-2.5% of the mass of the epoxy resin.
5. The use of the graphene quantum dot/polyphenylene sulfide composite material as a preservative according to claims 1-4, wherein: preparing a graphene quantum dot/polyphenylene sulfide composite material: mixing flower-shaped polyphenylene sulfide and graphene quantum dots, adding the mixture into an organic solvent NMP, stirring and reacting for 3.5-4 h at 220-225 ℃, heating to 270-275 ℃, and continuing stirring and reacting for 1.5-2 h to obtain a gray precipitate; and cooling to room temperature, filtering, repeatedly washing with ethanol, acetone and the like, and freeze-drying to obtain the graphene quantum dot/polyphenylene sulfide composite material.
6. The application of the graphene quantum dot/polyphenylene sulfide composite material as a preservative according to claim 5, wherein the graphene quantum dot/polyphenylene sulfide composite material is characterized in that: the flower-shaped polyphenyl ether and the graphene quantum dots are mixed according to the following mass percentage: 93-99% of flower-shaped polyphenylene sulfide and 1-7% of graphene quantum dots.
7. The application of the graphene quantum dot/polyphenylene sulfide composite material as a preservative according to claim 5, wherein the graphene quantum dot/polyphenylene sulfide composite material is characterized in that: the freeze drying is carried out at the temperature of-50 to-60 ℃ for 12 to 24 hours.
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| CN117511391A (en) * | 2024-01-08 | 2024-02-06 | 浙江德力装备有限公司 | Electrostatic spraying composition and preparation method and application thereof |
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Application publication date: 20200915 |