CN109777253B - Graphene modified epoxy anticorrosive paint and preparation method thereof - Google Patents
Graphene modified epoxy anticorrosive paint and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of epoxy anticorrosive coatings, and particularly relates to a graphene modified epoxy anticorrosive coating. The graphene modified epoxy anticorrosive paint is mainly prepared from a component A and a component B, wherein the component A mainly comprises epoxy resin, pigment, filler, an auxiliary agent and a graphene dispersion liquid, the component B is a curing agent, the mass ratio of the graphene dispersion liquid to the component A is 6-12: 100, the mass ratio of the component A to the component B is 6-8: 1, the graphene dispersion liquid is obtained by compounding graphene, a mixed solvent and a dispersing agent B, and the mixed solvent is a mixture of xylene, cyclohexanone, butanol, ethylene glycol ethyl ether and ethylene glycol ethyl ether acetate. According to the invention, the mixed solvent is adopted to uniformly disperse the graphene in the coating, so that the prepared coating has good stability and good corrosion resistance.
Description
Technical Field
The invention relates to the field of epoxy anticorrosive paint, and particularly relates to graphene modified epoxy anticorrosive paint and a preparation method thereof.
Background
The epoxy anticorrosive paint is a common anticorrosive paint and is generally used as a primer to be coated on the surface of metal, but the traditional epoxy anticorrosive paint has generally insufficient anticorrosive performance and needs to be improved.
Graphene is a carbon nano material with a regular two-dimensional structure newly found in recent years, and the huge specific surface area, chemical stability, and excellent barrier property and adsorption property make the graphene become a research hotspot of an anticorrosive coating addition material in recent years. However, the dispersibility of graphene in the coating is very poor, the large surface tension of the graphene brings strong van der waals force and pi-pi bond effect, so that the graphene is easy to agglomerate, the agglomeration can not improve the corrosion resistance, but a permeation channel can be formed at the agglomeration position, the diffusion rate of water molecules or chloride ions and the like in the coating is accelerated, and the mechanical property and the corrosion resistance of the coating are reduced.
The current application of graphene in the coating field mostly adopts a surface grafting or in-situ polymerization method in order to obtain a good effect, and although the problem of dispersibility can be partially solved, the application of graphene in the anti-corrosion coating field is greatly limited due to the problems of troublesome operation process, easy uneven grafting in large-scale production, production and application habits different from the conventional coating and the like.
Disclosure of Invention
The invention aims to provide a graphene modified epoxy anticorrosive paint which has excellent dispersibility and corrosion resistance.
The second purpose of the invention is to provide a preparation method of the graphene modified epoxy anticorrosive paint.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the graphene modified epoxy anticorrosive paint is mainly prepared from a component A and a component B, wherein the component A mainly comprises epoxy resin, pigment, filler, an auxiliary agent and a graphene dispersion liquid, the graphene dispersion liquid is obtained by compounding graphene, a mixed solvent and a dispersing agent B, the mixed solvent is a mixture of xylene, cyclohexanone, butanol, ethylene glycol ethyl ether and ethylene glycol ethyl ether acetate, and the mass ratio of the xylene, the cyclohexanone, the butanol, the ethylene glycol ethyl ether and the ethylene glycol ethyl ether acetate is 4-5: 1.1-1.3: 1-1.3: 2-3: 1-2; the mass ratio of the graphene dispersion liquid to the component A is 6-12: 100; the component B is a curing agent, and the mass ratio of the component A to the component B is 6-8: 1.
The mass ratio of the graphene to the dispersant B to the mixed solvent is 1: 0.5-1: 10-20.
The mass ratio of the graphene to the dispersant B to the mixed solvent is 1:1: 20.
The mass ratio of the epoxy resin, the pigment, the filler, the auxiliary agent and the component A is 30-32: 25-28.3: 28.6-33.3: 1.1-1.3: 100.
The epoxy resin is any one or more of epoxy resin 901, epoxy resin E44 and epoxy resin E51.
The pigment is any one or more of titanium dioxide, zinc phosphate and carbon black.
The filler is any one or more of talcum powder, barium sulfate and mica powder.
The auxiliary agent is one or two of a leveling agent or a dispersing agent A.
The dispersant A is one or two of BYK161 and BYK180, and the flatting agent is one or two of AFCONA3777 and BYK 331.
The dispersant B is one or two of Luborun 32500 or Orna F410.
The curing agent is any one or more of polyamide curing agent, phenolic aldehyde amine curing agent and fatty amine curing agent.
The preparation method of the graphene modified epoxy anticorrosive paint comprises the following steps:
1) preparing a premix: uniformly mixing epoxy resin, pigment, filler and an auxiliary agent to prepare a premix;
2) preparing a graphene dispersion liquid: adding graphene into a mixed solvent, soaking for 10-13 h, performing ultrasonic dispersion to obtain a pre-dispersion liquid, dropwise adding a dispersing agent B into the pre-dispersion liquid while stirring, and performing ultrasonic dispersion to form a stable graphene dispersion liquid;
3) preparing a component A: doping the graphene dispersion liquid prepared in the step 2) into the premix prepared in the step 1) to obtain a component A;
4) preparing the graphene modified epoxy anticorrosive paint: uniformly mixing the component A and the component B prepared in the step 3) to obtain the graphene modified epoxy anticorrosive paint.
The graphene dispersion liquid is a black transparent liquid.
And 3) doping the graphene dispersion liquid into the premix by adopting a high-speed stirring mode, wherein the high-speed stirring speed is 600-1200 rpm, and the time is 10-20 min.
The invention has the beneficial effects that:
the graphene modified epoxy anticorrosive paint is mainly prepared from a component A and a component B, wherein the component A mainly comprises epoxy resin, pigment, filler, an auxiliary agent and a graphene dispersion liquid, the graphene dispersion liquid is obtained by compounding graphene, a mixed solvent and a dispersing agent B, and the viscosity of the mixed solvent adopted by the invention is lower than that of an active diluent adopted by the prior art, so that the dispersion expansion of the graphene is not easily influenced by the environmental temperature, and the dispersion effect of the anticorrosive paint prepared by the invention is better than that of the paint prepared by the active diluent.
Cyclohexanone in the special solvent adopted by the invention has strong solubility, so that graphene can be easily and uniformly dispersed in the mixed solvent, and the surfaces of butanol, ethylene glycol monoethyl ether and ethylene glycol monoethyl ether acetate in the mixed solvent contain hydrogen bonds which can act with a small amount of polar functional groups on the surface of the graphene, so that the combination of the butanol, ethylene glycol monoethyl ether and ethylene glycol monoethyl ether acetate solvents and the graphene is realized; xylene in the mixed solvent does not contain hydrogen bonds and cannot be combined with graphene, so that the graphene sheets can be isolated, and the graphene sheets are separated to form a certain distance and are not agglomerated; the mixed solvent system adopted by the invention is superior to the common solvent system.
The method adopts an ultrasonic dispersion mode in the process of preparing the graphene dispersion liquid, and has better ultrasonic dispersion effect, so that the pre-dispersion liquid formed by adding the graphene into the mixed solvent has better dispersibility, and the pre-dispersion liquid is more stable.
The graphene modified epoxy anticorrosive paint is mainly prepared from graphene dispersion liquid with good dispersibility, epoxy resin, pigment, filler, auxiliaries and the like, uniformly dispersed graphene is added into an epoxy resin coating, and graphene microparticles are filled into holes of the epoxy resin coating and play a role in blocking corrosive media, so that the anticorrosive performance of the prepared graphene modified epoxy anticorrosive paint is improved.
Drawings
The invention is further illustrated with reference to the following figures and examples.
Fig. 1 is a picture of a graphene-modified epoxy anticorrosive paint prepared in the first embodiment of the present invention after a salt spray experiment;
fig. 2 is a picture of the graphene-modified epoxy anticorrosive paint prepared in example two of the present invention after a salt spray experiment;
fig. 3 is a picture of the graphene modified epoxy anticorrosive paint prepared in the third embodiment of the invention after a salt spray experiment;
FIG. 4 is a picture of the graphene modified epoxy anticorrosive paint prepared by the comparative example of the present invention after a salt spray experiment.
Detailed Description
In the following examples, cold rolled steel sheets were selected as the metal substrate, which was first subjected to sand blasting or polishing treatment to achieve a surface roughness of ra2.5 grade, and the surface was wiped with xylene after the treatment.
Example one
The graphene modified epoxy anticorrosive paint is mainly prepared from 60g of a component A and 10g of a component B, wherein the component A mainly comprises 19.2g of epoxy resin 901, 16.6g of titanium dioxide, 20g of talcum powder, 0.6g of BYK180 and 3.6g of graphene dispersion liquid, the component B is 10g of polyamide curing agent, and the mass ratio of the graphene dispersion liquid to the component A is 6: 100.
The graphene dispersion liquid is obtained by compounding 20g of graphene, 200g of mixed solvent and 10g of Luborun 32500, wherein the mixed solvent is a mixture of 80g of dimethylbenzene, 20g of cyclohexanone, 20g of butanol, 50g of ethylene glycol ethyl ether and 30g of ethylene glycol ethyl ether acetate.
The preparation method of the graphene modified epoxy anticorrosive paint in the embodiment comprises the following steps:
1) preparing a premix: uniformly mixing 19.2g of epoxy resin 901, 16.6g of titanium dioxide, 20g of talcum powder and 0.6g of BYK180 to prepare a premix;
2) preparing a graphene dispersion liquid: adding 20g of graphene into 200g of mixed solvent, soaking for 10 hours, and performing ultrasonic dispersion to form pre-dispersion liquid; the ultrasonic power is 300W, and the ultrasonic time is 30 min; dropwise adding 10g Luobu 32500 into the pre-dispersion liquid while stirring at the speed of 1-2 drops/second, wherein the dispersion speed is 500rpm, and performing ultrasonic dispersion again to form a stable graphene dispersion liquid, wherein the ultrasonic power is 300W, and the ultrasonic time is 20 min;
3) preparing a component A: weighing 3.6g of the graphene dispersion liquid prepared in the step 2) and doping the graphene dispersion liquid into 56.4g of the premix prepared in the step 1) while stirring at a high speed of 600rpm for 10min to obtain a component A;
4) preparing the graphene modified epoxy anticorrosive paint: weighing 60g of the component A prepared in the step 3) and 10g of polyamide curing agent, and uniformly mixing to obtain the graphene modified epoxy anticorrosive paint.
The application of the graphene modified epoxy anticorrosive paint in the embodiment is as follows:
adding 20g of a matched diluent (the mass ratio of xylene to butanol is 4:1) into 70g of the graphene modified epoxy anticorrosive paint obtained in the embodiment, adjusting the viscosity until the paint is easily sprayed on the cold-rolled steel plate, controlling the thickness of the paint film to be 20-40 mu m, drying the sprayed cold-rolled steel plate at 80 +/-5 ℃ for 2h, and putting the sprayed cold-rolled steel plate into a circulating salt spray box for a salt spray experiment.
Example two
The graphene modified epoxy anticorrosive paint is mainly prepared from 70g of a component A and 10g of a component B, wherein the component A mainly comprises 21g of epoxy resin E44, 19.83g of zinc phosphate, 20g of barium sulfate, 0.77g of AFCONA3777 and 8.4g of graphene dispersion liquid, the component B is 10g of phenolic aldehyde amine curing agent, and the mass ratio of the graphene dispersion liquid to the component A is 12: 100.
The graphene dispersion liquid is mainly obtained by compounding 20g of graphene, 300g of mixed solvent and 16g of olna F410, wherein the mixed solvent is a mixture of 144g of dimethylbenzene, 32g of cyclohexanone, 37g of butanol, 58g of ethylene glycol ethyl ether and 29g of ethylene glycol ethyl ether acetate.
The preparation method of the graphene modified epoxy anticorrosive paint in the embodiment comprises the following steps:
1) preparing a premix: uniformly mixing 21g of epoxy resin E44, 19.83g of zinc phosphate, 20g of barium sulfate and 0.77g of AFCONA3777 to prepare a premix;
2) preparing a graphene dispersion liquid: adding 20g of graphene into 300g of mixed solvent, soaking for 12 hours, and performing ultrasonic dispersion to form pre-dispersion liquid; the ultrasonic power is 450W, and the ultrasonic time is 30 min; dropwise adding 16g of sodium F410 into the pre-dispersion liquid while stirring at the speed of 1-2 drops/second, wherein the dispersion speed is 550rpm, and performing ultrasonic dispersion again to form a stable graphene dispersion liquid, wherein the ultrasonic power is 450W, and the ultrasonic time is 20 min;
3) preparing a component A: weighing 8.4g of the graphene dispersion liquid prepared in the step 2) and doping the graphene dispersion liquid into 61.6g of the premix prepared in the step 1) while stirring at a high speed of 900rpm for 15min to obtain a component A;
4) preparing the graphene modified epoxy anticorrosive paint: weighing 70g of the component A prepared in the step 3) and 10g of the phenolic aldehyde amine curing agent, and uniformly mixing to obtain the graphene modified epoxy anticorrosive paint.
The application of the graphene modified epoxy anticorrosive paint in the embodiment is as follows:
adding 20g of a matched diluent (the mass ratio of xylene to butanol is 4:1) into 70g of the graphene modified epoxy anticorrosive paint obtained in the embodiment, adjusting the viscosity until the paint is easily sprayed on the cold-rolled steel plate, controlling the thickness of the paint film to be 20-40 mu m, drying the sprayed cold-rolled steel plate at 80 +/-5 ℃ for 2h, and putting the sprayed cold-rolled steel plate into a circulating salt spray box for a salt spray experiment.
EXAMPLE III
The graphene modified epoxy anticorrosive paint is mainly prepared from 80g of a component A and 10g of a component B, wherein the component A is mainly composed of 25.2g of epoxy resin E51, 20g of carbon black, 25.76g of mica powder, 1.04g of BYK161 and 8g of graphene dispersion liquid, the component B is 10g of aliphatic amine curing agent, and the mass ratio of the graphene dispersion liquid to the component A is 10: 100.
The graphene dispersion liquid is obtained by compounding 20g of graphene, 400g of mixed solvent and 20g of Luborun 32500, wherein the mixed solvent is a mixture of 150g of dimethylbenzene, 43g of cyclohexanone, 40g of butanol, 100g of ethylene glycol ethyl ether and 67g of ethylene glycol ethyl ether acetate.
The preparation method of the graphene modified epoxy anticorrosive paint in the embodiment comprises the following steps:
1) preparing a premix: uniformly mixing 25.2g of epoxy resin E51, 20g of carbon black, 25.76g of mica powder and 1.04g of BYK161 to prepare a premix;
2) preparing a graphene dispersion liquid: adding 20g of graphene into 400g of mixed solvent, soaking for 13h, and performing ultrasonic dispersion to form pre-dispersion liquid; the ultrasonic power is 600W, and the ultrasonic time is 30 min; dropwise adding 20g Luobu 32500 into the pre-dispersion liquid while stirring at the speed of 1-2 drops/second, wherein the dispersion speed is 600rpm, and performing ultrasonic dispersion again to form a stable graphene dispersion liquid, wherein the ultrasonic power is 600W and the ultrasonic power is 20 min;
3) preparing a component A: weighing 8g of the graphene dispersion liquid prepared in the step 2) and doping the graphene dispersion liquid into 72g of the premix prepared in the step 1) while stirring at a high speed of 1200rpm for 20min to obtain a component A;
4) preparing the graphene modified epoxy anticorrosive paint: weighing 80g of the component A prepared in the step 3) and 10g of the aliphatic amine curing agent, and uniformly mixing to obtain the graphene modified epoxy anticorrosive paint.
The application of the graphene modified epoxy anticorrosive paint in the embodiment is as follows:
adding 20g of a matched diluent (the mass ratio of xylene to butanol is 4:1) into 70g of the graphene modified epoxy anticorrosive paint obtained in the embodiment, adjusting the viscosity until the paint is easily sprayed on the cold-rolled steel plate, controlling the thickness of the paint film to be 20-40 mu m, drying the sprayed cold-rolled steel plate at 80 +/-5 ℃ for 2h, and putting the sprayed cold-rolled steel plate into a circulating salt spray box for a salt spray experiment.
Comparative example
The graphene modified epoxy anticorrosive paint is mainly prepared from 70g of A component and 10g of B component, wherein the A component is mainly prepared from 21.7g of epoxy resin 901, 22.35g of zinc phosphate, 20g of talcum powder, 1.05g of BYK180 and 4.9g of graphene dispersion liquid, the B component is 10g of polyamide curing agent, the mass ratio of the graphene dispersion liquid to the A component is 7:100, the mass ratio of the A component to the B component is 7:1, and the graphene dispersion liquid is prepared by compounding 20g of graphene, 200g of tert-butyl phenol glycidyl ether and 10g of Luobu borun 32500.
The preparation method of the graphene modified epoxy anticorrosive paint comprises the following steps:
1) preparing a premix: uniformly mixing 21.7g of epoxy resin 901, 22.35g of zinc phosphate, 20g of talcum powder and 1.05g of BYK180 to prepare a premix;
2) preparing a graphene dispersion liquid: adding 20g of graphene into 200g of tert-butyl phenol glycidyl ether, and mixing to obtain a pre-dispersion liquid; adding 10g of Luobu 32500 into the pre-dispersion liquid, and uniformly mixing to obtain a graphene dispersion liquid;
3) preparing a component A: weighing 4.9g of the graphene dispersion liquid prepared in the step 2), stirring and doping the graphene dispersion liquid into 65.9g of the premix prepared in the step 1), and stirring to obtain a component A;
4) preparing the graphene modified epoxy anticorrosive paint: weighing 70g of the component A prepared in the step 3) and 10g of polyamide curing agent, and uniformly mixing to obtain the graphene modified epoxy anticorrosive paint.
The application of the graphene modified epoxy anticorrosive paint in the comparative example is as follows:
adding 20g of a matched diluent (xylene: butanol is 4:1) into 70g of the graphene modified epoxy anticorrosive paint obtained in the comparative example, adjusting the viscosity until the paint is easily sprayed on the cold-rolled steel plate, controlling the thickness of the paint film to be 20-40 mu m, drying the sprayed cold-rolled steel plate at 80 +/-5 ℃ for 2h, and putting the sprayed cold-rolled steel plate into a circulating salt spray box for carrying out a salt spray experiment.
Examples of the experiments
Examples one to three and comparative example spray-coated cold rolled steel sheets were put in a circulating salt spray box for 1000 hours of salt spray test, and the test results are shown in fig. 1 to 4.
As can be seen from fig. 1 to 4, the cold-rolled steel sheets sprayed according to the comparative example have very severe surface corrosion after the salt spray test for 1000 hours compared to the cold-rolled steel sheets sprayed according to the first to third examples, while the samples sprayed according to the first to third examples have relatively light surface corrosion, and the third example has substantially no significant corrosion. The anti-corrosion performance of the epoxy zinc phosphate coating is greatly improved through electrochemical barrier and chloride ion permeation resistance after the graphene dispersion liquid with better dispersion performance is added.
In light of the foregoing description of preferred embodiments in accordance with the invention, it is to be understood that numerous changes and modifications may be made by those skilled in the art without departing from the scope of the invention. The technical scope of the present invention is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (7)
1. The graphene modified epoxy anticorrosive paint is characterized in that: the graphene composite coating is mainly prepared from a component A and a component B, wherein the component A mainly comprises epoxy resin, pigment, filler, an auxiliary agent and graphene dispersion liquid, and the mass ratio of the epoxy resin, the pigment, the filler and the auxiliary agent to the component A is 30-32: 25-28.3: 28.6-33.3: 1.1-1.3: 100;
the graphene dispersion liquid is obtained by compounding graphene, a mixed solvent and a dispersing agent B, wherein the mixed solvent is a mixture of xylene, cyclohexanone, butanol, ethylene glycol monoethyl ether and ethylene glycol monoethyl ether acetate, and the mass ratio of the xylene, the cyclohexanone, the butanol, the ethylene glycol monoethyl ether and the ethylene glycol monoethyl ether acetate is 4-5: 1.1-1.3: 1-1.3: 2-3: 1-2; the mass ratio of the graphene dispersion liquid to the component A is 6-12: 100; the component B is a curing agent, the mass ratio of the component A to the component B is 6-8: 1, the mass ratio of the graphene to the dispersant B to the mixed solvent is 1: 0.5-1: 10-20, and the dispersant B is any one or two of Luoborun 32500 or OnalF 410;
the preparation method of the graphene modified epoxy anticorrosive paint comprises the following steps:
1) preparing a premix: uniformly mixing epoxy resin, pigment, filler and an auxiliary agent to prepare a premix;
2) preparing a graphene dispersion liquid: adding graphene into a mixed solvent, soaking for 10-13 h, performing ultrasonic dispersion to obtain a pre-dispersion liquid, dropwise adding a dispersing agent B into the pre-dispersion liquid while stirring, and performing ultrasonic dispersion to form a stable graphene dispersion liquid;
3) preparing a component A: doping the graphene dispersion liquid prepared in the step 2) into the premix prepared in the step 1) to obtain a component A;
4) preparing the graphene modified epoxy anticorrosive paint: uniformly mixing the component A and the component B prepared in the step 3) to obtain the graphene modified epoxy anticorrosive paint.
2. The graphene-modified epoxy anticorrosive paint according to claim 1, characterized in that: the epoxy resin is any one or more of epoxy resin 901, epoxy resin E44 and epoxy resin E51.
3. The graphene-modified epoxy anticorrosive paint according to claim 1, characterized in that: the pigment is any one or more of titanium dioxide, zinc phosphate and carbon black.
4. The graphene-modified epoxy anticorrosive paint according to claim 1, characterized in that: the filler is any one or more of talcum powder, barium sulfate and mica powder.
5. The graphene-modified epoxy anticorrosive paint according to claim 1, characterized in that: the auxiliary agent is one or two of a leveling agent or a dispersing agent A; the dispersant A is one or two of BYK161 and BYK180, and the flatting agent is one or two of AFCONA3777 and BYK 331.
6. The graphene-modified epoxy anticorrosive paint according to claim 1, characterized in that: the curing agent is any one or more of polyamide curing agent, phenolic aldehyde amine curing agent and fatty amine curing agent.
7. The preparation method of the graphene-modified epoxy anticorrosive paint according to claim 1, characterized by comprising the following steps: and 3) doping the graphene dispersion liquid into the premix in a high-speed stirring manner, wherein the high-speed stirring speed is 600-1200 rpm, and the time is 10-20 min.
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| CN110845934A (en) * | 2019-09-25 | 2020-02-28 | 苏州吉人高新材料股份有限公司 | Two-dimensional nano low-surface-treatment graphene anti-corrosion primer and preparation method thereof |
| CN111471345A (en) * | 2020-04-23 | 2020-07-31 | 大厂金隅涂料有限责任公司 | Solvent type anticorrosive coating graphene dispersion liquid and preparation method thereof |
| CN112457744A (en) * | 2020-12-01 | 2021-03-09 | 四川科嘉能源科技有限公司 | Graphene modified anticorrosive paint and preparation method thereof |
| CN114032009A (en) * | 2021-12-23 | 2022-02-11 | 陕西煤业化工技术研究院有限责任公司 | Graphene stealth skin primer as well as preparation method and application thereof |
| CN114231100B (en) * | 2021-12-23 | 2023-08-29 | 陕西煤业化工技术研究院有限责任公司 | Skin finishing paint for airplane and preparation method and application thereof |
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