CN111704821A - Graphene oxide grafting-based composite antirust pigment and application thereof in anticorrosive paint - Google Patents
Graphene oxide grafting-based composite antirust pigment and application thereof in anticorrosive paint Download PDFInfo
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D5/082—Anti-corrosive paints characterised by the anti-corrosive pigment
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- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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Abstract
The invention relates to the field of antirust pigments and anticorrosive coatings, in particular to a graphene oxide grafting-based composite antirust pigment and application thereof in anticorrosive coatings. Graphene oxide is used as a barrier type two-dimensional flaky nano material, and the high surface energy of the graphene oxide enables the graphene oxide to be easily agglomerated when the graphene oxide is applied to a coating. The novel antirust pigment is obtained by using the aqueous dispersion of graphene oxide as a raw material and silane as a grafting intermediate to successfully graft the organic acid corrosion inhibitor onto the graphene oxide. By utilizing the instability of the chemical bond Si-O-C generated after grafting, the grafted product is easy to generate hydrolysis reaction to release the silane-organic acid corrosion inhibitor part, and the latter can have obvious corrosion inhibition effect on steel. And drying the grafted product to obtain the antirust pigment product. The novel antirust pigment has the shielding effect of graphene oxide and the antirust effect of an organic acid corrosion inhibitor. The epoxy resin is added into the epoxy coating in a proportion of 0.1-0.5 wt.% and can be used for corrosion protection of steel base materials.
Description
Technical Field
The invention relates to a preparation technology and a coating technology for preparing a novel pigment by utilizing graphene modification, in particular to a composite antirust pigment based on graphene oxide grafting and application thereof in an anticorrosive coating.
Background
The organic coating is widely used for protecting a steel structure, provides barrier protection for the steel structure, and prolongs the service life of the steel structure. In the organic coating, substances with barrier capability such as fillers and anti-rust pigments need to be added to realize the barrier effect of the organic coating, and meanwhile, the anti-rust pigments can also provide a corrosion inhibition effect for the steel substrate and provide passivation protection for the steel substrate under the condition that a corrosive medium completely permeates in the coating.
As a novel flaky two-dimensional material consisting of carbon atoms, the graphene has many excellent optical, electrical and mechanical properties, and has a wide application prospect in the fields of electronics, chemical engineering, biomedicine, energy and the like. The graphene has the advantages of high specific surface area, high conductivity, high chemical stability, high thermal stability, good shielding performance and outstanding mechanical properties. In recent years, graphene coatings have also become an important application research field of graphene. Graphene has been shown to greatly improve the overall performance of coatings in coating systems such as conductive coatings, anticorrosive coatings, flame retardant coatings, and the like. At present, most of the graphene is applied to the anticorrosive paint as a functional filler. Due to the high surface activity of graphene, graphene is very prone to self-agglomeration. If the paint is directly added into the coating without treatment, the mechanical property and the corrosion resistance of the coating are reduced. One key problem caused by this is how to solve the problem of dispersion stability of graphene, and in practice, a dispersion of graphene is usually prepared to solve this problem.
Graphene oxide is an oxidized derivative of graphene, the surface of graphene oxide has rich functional groups (hydroxyl, carboxyl and epoxy), and the existence of oxygen-containing groups provides an effective way for surface modification of graphene oxide. The modified graphene oxide can improve the dispersion performance and compatibility of the graphene oxide in the coating, so that the shielding performance of the graphene oxide for the coating can be improved. Abundant functional groups on the graphene oxide provide possibility for grafting other organic or inorganic materials and preparing the composite material based on the graphene oxide. For example, Pourhashem et al successfully grafted and coated graphene oxide with two silanes, 3-Aminopropyltriethoxysilane (APTES) and gamma- (2, 3-Glycidoxy) Propyltrimethoxysilane (GPTMS). Researches find that the dispersity of the modified graphene oxide is greatly improved. In addition, the graphene oxide can also be used as a corrosion inhibitor carrier. For example, Bahar Nikpour et al studied the adsorption behavior of nettle leaf juice on graphene oxide nanoplatelets (gos).
The experiment result shows that when the pH value of the acid solution is 2, the adsorption of the nettle leaf juice on the graphene oxide sheet is improved, and the corrosion inhibition effect of the nettle leaf juice on carbon steel in the sodium chloride solution can be enhanced. However, Bahar Nikpour utilizes the adsorption effect of graphene oxide, and the organic corrosion inhibitor nettle leaf juice does not form a bonding effect with graphene oxide. If the organic corrosion inhibitor can be grafted to the graphene oxide, the organic corrosion inhibitor can be released through hydrolysis reaction, so that the composite type antirust pigment with the barrier and corrosion inhibition dual functions is expected to be obtained, and the composite type antirust pigment has better dispersibility than the common graphene oxide due to grafting of other molecules. The composite antirust pigment is added into a coating, and is expected to provide excellent corrosion protection capability for a steel substrate.
Disclosure of Invention
The invention aims to provide a graphene oxide grafting-based composite antirust pigment and application thereof in an anticorrosive coating, and the composite antirust pigment realizes two functions of shielding and passivating in a coating. The problem to be solved is to graft organic molecules with a corrosion inhibition effect on steel by utilizing functional groups on the surface of graphene oxide to prepare the composite antirust pigment. And adding the composite type antirust pigment into the paint to form the paint based on the graft modified graphene oxide antirust pigment.
The technical scheme of the invention is as follows:
the composite antirust pigment based on graphene oxide grafting is prepared by carrying out chemical grafting modification on graphene oxide, wherein the graphene oxide is 30-60 parts by weight, silane is 5-30 parts by weight, and an organic acid corrosion inhibitor is 20-60 parts by weight.
The preparation method of the composite anti-rust pigment based on graphene oxide grafting comprises the following steps:
(1) ultrasonically dispersing graphene oxide by using deionized water to prepare a graphene oxide dispersion liquid, wherein the concentration of the dispersion liquid is 0.1-0.5 wt.%, and thus obtaining a first component;
(2) dissolving silane, an organic acid corrosion inhibitor and a catalyst into ethanol, and stirring and dispersing at constant temperature to obtain a second component;
(3) and mixing the component I and the component II, adjusting the pH value to be acidic, stirring at constant temperature for 6-18 h, grafting an organic acid corrosion inhibitor onto graphene oxide by a chemical method, washing with ethanol, and drying to obtain the modified graphene oxide of the chemical grafted organic acid corrosion inhibitor, namely the composite type antirust pigment.
According to the preparation method of the composite anti-rust pigment based on graphene oxide grafting, in the raw materials used for chemical grafting, silane is one of 3-Aminopropyltriethoxysilane (APTES), 3-Aminopropyltrimethoxysilane (APMS), 3- (2-aminoethylamino) propyltrimethoxysilane (AEAPTMS) and aminomethyl trimethylsilane (AMTMS); the organic acid corrosion inhibitor is one of caffeic acid, 3-indolebutyric acid and polyepoxysuccinic acid; the catalyst is one of Dicyclohexylcarbodiimide (DCC) and N, N-Dimethylformamide (DMF).
According to the preparation method of the graphene oxide grafting-based composite anti-rust pigment, in the step (2), the temperature for constant-temperature stirring and dispersion is 15-30 ℃, and the time is 4-8 hours.
The preparation method of the composite anti-rust pigment based on graphene oxide grafting comprises the step (3) of stirring at a constant temperature of 55-75 ℃.
The composite anti-rust pigment based on graphene oxide grafting is applied to an anti-corrosion coating, wherein 0.1-0.5 wt.% of chemical grafting modified graphene oxide is added into the anti-corrosion coating, and the mixture is ground by a ball mill for 4-8 hours to obtain the anti-corrosion coating based on the chemical grafting modified graphene oxide anti-rust pigment.
The design idea of the invention is as follows:
according to the method, the functional group of the graphene oxide is fully utilized, the organic acid corrosion inhibitor is grafted to the surface of the graphene oxide by utilizing the bridging effect of silane, and a combination of the graphene oxide-silane-organic acid corrosion inhibitor is synthesized. On one hand, through graft modification, the functional groups of the graphene oxide are reduced, the activity is reduced, and the agglomeration tendency in the coating is reduced. On the other hand, organic molecules with corrosion inhibition are grafted on the surface through modification, and the organic molecules can be dissociated and released through hydrolysis to form 'graphene oxide' and a transferable 'silane-organic acid corrosion inhibitor' which are remained in the coating. The former can play a role of a barrier, and the latter can play a role of corrosion inhibition on a steel substrate, so that the composite antirust pigment can play a role of shielding and passivating in a coating layer simultaneously.
The invention has the following advantages and beneficial effects:
1. graphene oxide is used as a barrier type two-dimensional flaky nano material, and the high surface energy of the graphene oxide enables the graphene oxide to be easily agglomerated when the graphene oxide is applied to a coating. The novel antirust pigment is obtained by using the aqueous dispersion of graphene oxide as a raw material and silane as a grafting intermediate to successfully graft the organic acid corrosion inhibitor onto the graphene oxide. By utilizing the instability of the chemical bond Si-O-C generated after grafting, the grafted product is easy to generate hydrolysis reaction to release the silane-organic acid corrosion inhibitor part, and the latter can have obvious corrosion inhibition effect on steel. And drying the grafted product to obtain an antirust pigment product, wherein the novel antirust pigment has the shielding effect of graphene oxide and the antirust effect of an organic acid corrosion inhibitor.
2. The composite antirust pigment can be added into an epoxy coating in a proportion of 0.1-0.5 wt.% by releasing an organic acid corrosion inhibitor effective on a steel substrate, and the coating can be used for corrosion protection of the steel substrate.
Description of the drawings:
FIG. 1: (A1) (B1) adding a NaCl aqueous solution with the molar concentration of 0.01M into the modified graphene oxide to form a leaching solution, and soaking the leaching solution for 3 hours to obtain the surface appearance of the Q235 steel; (A2) and (B2) the surface appearance of Q235 steel after being soaked in NaCl aqueous solution with the molar concentration of 0.01M for 3 hours; wherein the pH of the leachate of (a1) and (a2) is 4, and the pH of the NaCl aqueous solution of (B1) and (B2) is 6.7.
FIG. 2: electrochemical impedance spectroscopy of Q235 surface epoxy coating soaked in 0.6M NaCl aqueous solution at molar concentration: (a) epoxy varnish; (b) epoxy varnish +0.1 wt.% graphite oxideAn alkene; (c) epoxy varnish +0.1 wt.% graft modified graphene oxide; in the figure, the abscissa Frequency represents Frequency (Hz), and the left ordinate Module represents the impedance Modulus (ohm cm)2) The right ordinate Phase angle represents the Phase angle (Deg.).
FIG. 3: the appearance of the Q235 surface epoxy coating after 240h of salt spray test is as follows: (a) epoxy varnish; (b) epoxy varnish +0.1 wt.% graphene oxide; (c) epoxy varnish +0.1 wt.% graft modified graphene oxide.
Detailed Description
The technical solution of the present invention is further described below with reference to the following examples, but is not limited to these examples.
Example 1
In this embodiment, the preparation method of the composite anti-rust pigment and the anti-corrosion coating based on graphene oxide grafting is as follows:
taking 1g of graphene oxide, adding the graphene oxide into 500ml of deionized water, and performing ultrasonic dispersion for 8 hours to obtain a component I. 0.3g of 3-Aminopropyltrimethoxysilane (APMS), 1g of polyepoxysuccinic acid and 0.2g of N, N-dimethylformamide are added into 500mL of ethanol for sealing, and the mixture is stirred and dispersed for 8 hours at the constant temperature of 20 ℃ water bath to obtain a second component. And mixing the component I and the component II, adjusting the pH value to 4.5, carrying out constant-temperature water bath at 70 ℃ for 12h, washing the product with ethanol for 3 times, and drying to obtain the graphene oxide grafted with polyepoxysuccinic acid, namely the composite antirust pigment. According to the weight ratio, the graphene oxide: silane: 35-50% of organic acid corrosion inhibitor: 10-15: 35 to 50.
0.1g of grafted and modified graphene oxide is added into the component A of the solvent type epoxy varnish formula according to 0.1 wt% of the solvent type epoxy varnish formula. The solvent type epoxy varnish comprises the following components in parts by weight:
the component A comprises: 50 parts of bisphenol A epoxy resin (NPSN-901-75X), 23 parts of solvent xylene, 1.0 part of dispersant (BYK110), 0.6 part of flatting agent (BYK306), 0.4 part of anti-settling agent (moderate 229), and grinding for 6 hours by a ball mill; and B component: and 25 parts of 650# polyamide curing agent.
And mixing the component A and the component B to obtain the anticorrosive paint based on the chemically grafted and modified graphene oxide antirust pigment. The coating is applied to the surface of Q235 steel (150mm × 70mm × 2mm for salt spray test), and the dry film thickness is 45 + -5 μm.
Example 2
In this embodiment, the preparation method of the composite anti-rust pigment and the anti-corrosion coating based on graphene oxide grafting is as follows:
taking 1g of graphene oxide, adding the graphene oxide into 500ml of deionized water, and performing ultrasonic dispersion for 8 hours to obtain a component I. 0.5g of 3- (2-aminoethylamino) propyltrimethoxysilane (AEAPTMS), 0.5g of 3-indolebutyric acid and 0.6g of dicyclohexylcarbodiimide are added into 500mL of ethanol for sealing, and the mixture is stirred and dispersed for 8 hours at the constant temperature of 25 ℃ in a water bath to obtain a component II. And mixing the component I and the component II, adjusting the pH value to 3.5, carrying out constant-temperature water bath at 65 ℃ for 12h, washing the product with ethanol for 3 times, and drying to obtain the graphene oxide grafted with the 3-indolebutyric acid, namely the composite antirust pigment. According to the weight ratio, the graphene oxide: silane: and (3) organic acid corrosion inhibitor is 45-55: 20-30: 20 to 30.
Adding the grafted and modified graphene oxide into a NaCl aqueous solution with the molar concentration of 0.01M, stirring for 24h, filtering to form a NaCl leaching solution, soaking a sample of Q235 steel by using the leaching solution, wherein the surface morphology of the sample after 3h is as shown in A1 and B1 of the attached drawing 1, and it can be seen that no matter the pH value is 4(A1) or 6.7(B1), the silane-organic acid corrosion inhibitor generated in the precipitation solution has an obvious corrosion inhibition effect on the Q235 steel, and the surface of the Q235 steel is not obviously corroded. On the other hand, as shown in a2 and B2 of fig. 1, Q235 steel directly immersed in an aqueous solution of NaCl (pH 4, a 2; pH 6.7, B2) having a molar concentration of 0.01M showed significant corrosion.
0.1g of grafted and modified graphene oxide is added into the component A of the solvent type epoxy varnish formula according to 0.1 wt% of the solvent type epoxy varnish formula. The solvent type epoxy varnish comprises the following components in parts by weight:
the component A comprises: 50 parts of bisphenol A epoxy resin (NPSN-901-75X), 23 parts of solvent xylene, 1.0 part of dispersant (BYK110), 0.6 part of flatting agent (BYK306), 0.4 part of anti-settling agent (moderate 229), and grinding for 6 hours by a ball mill; and B component: and 25 parts of 650# polyamide curing agent.
And mixing the component A and the component B to obtain the anticorrosive paint based on the chemically grafted and modified graphene oxide antirust pigment. The coating is applied to the surface of Q235 steel (150mm multiplied by 70mm multiplied by 2mm is used for a salt spray test, and 50mm multiplied by 2mm is used for an electrochemical alternating current impedance spectroscopy test), and the thickness of a dry film is 45 +/-5 mu m. The electrochemical ac impedance spectrum of the coating is shown in fig. 2 c. The coating salt spray test 240h morphology is shown in FIG. 3 c.
Example 3
In this embodiment, the preparation method of the composite anti-rust pigment and the anti-corrosion coating based on graphene oxide grafting is as follows:
and taking 0.6g of graphene oxide, adding the graphene oxide into 500ml of deionized water, and performing ultrasonic dispersion for 6 hours to obtain the component I. 0.3g of 3-Aminopropyltriethoxysilane (APTES), 0.4g of caffeic acid and 0.4g of N, N-Dimethylformamide (DMF) are added into 500mL of ethanol for sealing, and the mixture is stirred and dispersed for 6 hours at the constant temperature of 15 ℃ water bath to obtain a component II. And mixing the component I and the component II, adjusting the pH value to 4.0, carrying out constant-temperature water bath at 60 ℃ for 18h, washing the product with ethanol for 3 times, and drying to obtain the caffeic acid grafted graphene oxide, namely the composite antirust pigment. According to the weight ratio, the graphene oxide: silane: 40-50% of organic acid corrosion inhibitor: 20-25: 25 to 35.
0.3g of grafted and modified graphene oxide is added into the component A of the solvent type epoxy varnish formula according to 0.3 wt% of the solvent type epoxy varnish formula. The solvent type epoxy varnish comprises the following components in parts by weight:
the component A comprises: 50 parts of bisphenol A epoxy resin (NPSN-901-75X), 23 parts of solvent xylene, 1.0 part of dispersant (BYK110), 0.6 part of flatting agent (BYK306), 0.4 part of anti-settling agent (moderate 229), and grinding for 6 hours by a ball mill; and B component: and 25 parts of 650# polyamide curing agent.
And mixing the component A and the component B to obtain the anticorrosive paint based on the chemically grafted and modified graphene oxide antirust pigment. The coating is applied to the surface of Q235 steel (150mm multiplied by 70mm multiplied by 2mm is used for a salt spray test, and 50mm multiplied by 2mm is used for an electrochemical alternating current impedance spectroscopy test), and the thickness of a dry film is 45 +/-5 mu m.
Comparative example 1
The same solvent-based epoxy varnish formulation as in example 1 and example 2 was used, with unmodified graphene oxide added in a proportion of 0.1 wt.%, and the resultant was coated onto a surface of Q235 steel (150 mm. times.70 mm. times.2 mm for salt spray testing and 50 mm. times.50 mm. times.2 mm for electrochemical AC impedance spectroscopy) to a dry film thickness of 45. + -. 5. mu.m. The electrochemical ac impedance spectrum of the coating is shown in fig. 2 b. The coating salt spray test 240h morphology is shown in FIG. 3 b.
Comparative example 2
The same solvent-borne epoxy varnish formulation as in example 1 and example 2 was applied to the surface of Q235 steel (150 mm. times.70 mm. times.2 mm for salt spray test 50 mm. times.50 mm. times.2 mm for electrochemical AC impedance spectroscopy) to a dry film thickness of 45. + -.5. mu.m. The electrochemical ac impedance spectrum of the coating is shown in fig. 2 a. The coating salt spray test 240h morphology is shown in FIG. 3 a.
As can be seen from a1, B1, a2 and B2 in fig. 1, after soaking in neutral (pH 6.7) and acidic (pH 4) composite pigment leachate (0.01M NaCl), the corrosion degree of Q235 steel is significantly reduced more than that in an aqueous solution of NaCl with a molar concentration of 0.01M, which indicates that the composite pigment has a significant corrosion inhibition effect on steel.
As shown in FIG. 2, the | Z! Z0.01Hz is significantly higher than epoxy coatings and epoxy varnishes (fig. 2a) with the addition of 0.1 wt.% graphene oxide (fig. 2b) and in the low frequency region (10)-2Hz to 10Hz) has high resistance value, which indicates that the added composite pigment has excellent shielding and corrosion inhibition capability on the coating.
The results of the salt spray tests of the examples and comparative examples are shown in table 1:
TABLE 1 salt spray test 240h test results
| Average rust width (mm) | |
| Example 1 | 3.12 |
| Example 2 | 2.83 |
| Example 3 | 2.91 |
| Comparative example 1 | 4.01 |
| Comparative example 2 | 4.49 |
As shown in Table 1, the results of the examples and the comparative examples show that after 240 hours of salt spray test, the corrosion width of the composite pigment based on graphene oxide added to the epoxy paint on the surface of Q235 steel is obviously reduced compared with the corrosion width of the coating added with unmodified graphene oxide and epoxy varnish, which shows that the corrosion rate of steel is inhibited by the release of corrosion inhibitor, and the feasibility of the application of the composite pigment is also proved.
Claims (6)
1. The composite antirust pigment based on graphene oxide grafting is characterized by being prepared from 30-60 parts by weight of graphene oxide, 5-30 parts by weight of silane and 20-60 parts by weight of an organic acid corrosion inhibitor, wherein the graphene oxide is subjected to chemical grafting modification.
2. The preparation method of the composite antirust pigment based on graphene oxide grafting according to claim 1, characterized by comprising the following steps:
(1) ultrasonically dispersing graphene oxide by using deionized water to prepare a graphene oxide dispersion liquid, wherein the concentration of the dispersion liquid is 0.1-0.5 wt.%, and thus obtaining a first component;
(2) dissolving silane, an organic acid corrosion inhibitor and a catalyst into ethanol, and stirring and dispersing at constant temperature to obtain a second component;
(3) and mixing the component I and the component II, adjusting the pH value to be acidic, stirring at constant temperature for 6-18 h, grafting an organic acid corrosion inhibitor onto graphene oxide by a chemical method, washing with ethanol, and drying to obtain the modified graphene oxide of the chemical grafted organic acid corrosion inhibitor, namely the composite type antirust pigment.
3. The preparation method of the composite anti-rust pigment based on graphene oxide grafting according to claim 2, characterized in that in the raw materials used for chemical grafting, silane is one of 3-Aminopropyltriethoxysilane (APTES), 3-Aminopropyltrimethoxysilane (APMS), 3- (2-aminoethylamino) propyltrimethoxysilane (AEAPTMS) and aminomethyl trimethylsilane (AMTMS); the organic acid corrosion inhibitor is one of caffeic acid, 3-indolebutyric acid and polyepoxysuccinic acid; the catalyst is one of Dicyclohexylcarbodiimide (DCC) and N, N-Dimethylformamide (DMF).
4. The preparation method of the composite anti-rust pigment based on graphene oxide grafting according to claim 2, characterized in that in the step (2), the temperature for constant-temperature stirring and dispersion is 15-30 ℃ and the time is 4-8 h.
5. The preparation method of the composite anti-rust pigment based on graphene oxide grafting according to claim 2, characterized in that in the step (3), the temperature of constant-temperature stirring is 55-75 ℃.
6. The application of the composite anti-corrosive pigment based on graphene oxide grafting in the anti-corrosive paint is characterized in that 0.1-0.5 wt.% of chemically grafted and modified graphene oxide is added into the anti-corrosive paint, and the mixture is ground for 4-8 hours by a ball mill, so that the anti-corrosive paint based on the chemically grafted and modified graphene oxide anti-corrosive pigment is obtained.
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| CN115820019A (en) * | 2022-12-26 | 2023-03-21 | 河南大学 | Low-porosity low-thickness magnesium alloy composite coating and preparation method and application thereof |
| CN115820019B (en) * | 2022-12-26 | 2024-02-09 | 河南大学 | Low-porosity low-thickness magnesium alloy composite coating and preparation method and application thereof |
| CN117050570A (en) * | 2023-08-31 | 2023-11-14 | 江西省科学院应用化学研究所 | Star-shaped organosiloxane modified graphene filler and preparation method of reinforced anticorrosive paint thereof |
| CN117050570B (en) * | 2023-08-31 | 2024-05-17 | 江西省科学院应用化学研究所 | Star-shaped organosiloxane modified graphene filler and preparation method of reinforced anticorrosive paint thereof |
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