CN108485495B - Method for preparing self-detection anticorrosive paint containing nano-carrier - Google Patents
Method for preparing self-detection anticorrosive paint containing nano-carrier Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 31
- 239000002539 nanocarrier Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000011259 mixed solution Substances 0.000 claims abstract description 38
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 37
- 239000000126 substance Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 13
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 10
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- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- 229920005749 polyurethane resin Polymers 0.000 claims description 4
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 6
- GNBHRKFJIUUOQI-UHFFFAOYSA-N fluorescein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 GNBHRKFJIUUOQI-UHFFFAOYSA-N 0.000 abstract description 3
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- PRZSXZWFJHEZBJ-UHFFFAOYSA-N thymol blue Chemical group C1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C(=CC(O)=C(C(C)C)C=2)C)=C1C PRZSXZWFJHEZBJ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000004925 Acrylic resin Substances 0.000 abstract description 2
- 229920000178 Acrylic resin Polymers 0.000 abstract description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003822 epoxy resin Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 2
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- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 2
- XSFVQEHUVOVFOW-UHFFFAOYSA-N 1,10-phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1.C1=CN=C2C3=NC=CC=C3C=CC2=C1 XSFVQEHUVOVFOW-UHFFFAOYSA-N 0.000 description 2
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- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
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- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
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- 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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- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- 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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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The method for preparing the self-detection anticorrosive paint containing the nano-carrier comprises the following steps: step one, preparing a nano carrier and preparing a nano carrier aqueous solution with a certain proportional concentration; mixing the nano-carrier aqueous solution and the self-detection chromogenic substance in proportion to obtain a first mixed solution; step three, performing ultrasonic dispersion on the first mixed solution to obtain a second mixed solution; step four, removing unreacted solution in the second mixed solution by suction filtration to obtain solid substances, and adding water to the solid substances to prepare a third mixed solution in a certain proportion; step five, mixing the third mixed solution with a film-forming substrate, wherein the nano carrier is graphene, nano boron nitride, nano clay and a layered double hydroxide sheet layer, the self-detection chromogenic substance is thymol blue, fluorescein, hydroxyquinoline, 1,10 phenanthroline pentaamino and phenolphthalein, the film-forming substrate is water-based organic resin, and the water-based organic resin is water-based polyurethane, water-based acrylic resin and water-based epoxy resin.
Description
Technical Field
The invention relates to a preparation method of an anticorrosive coating, and belongs to the field of chemical industry.
Background
Organic coatings are currently the most common method of corrosion protection of metal surfaces in production. However, after a long period of use, the organic coating on the metal surface is corroded to protect the substrate, so that peeling occurs between the substrate and the coating, and the protection function of the organic coating is further disabled. When macroscopic corrosion products are generated in the corrosion process of the metal surface, the corrosion degree is very serious, so if a coating which can carry out self detection and can warn in the early stage of corrosion is provided, the coating can greatly improve the corrosion prevention effect of the metal when applied to the corrosion prevention of the metal surface.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide a method for preparing a self-inspecting anticorrosive paint containing a nanocarrier.
The invention provides a method for preparing a self-detection anticorrosive paint containing a nano-carrier, which is characterized by comprising the following steps: step one, preparing a nano carrier and preparing a nano carrier aqueous solution with a certain proportional concentration; mixing the nano-carrier aqueous solution and the self-detection chromogenic substance in proportion to obtain a first mixed solution; step three, performing ultrasonic dispersion on the first mixed solution to obtain a second mixed solution; step four, removing unreacted solution in the second mixed solution by suction filtration to obtain solid substances, and adding water to the solid substances to prepare a third mixed solution in a certain proportion; and step five, mixing the third mixed solution with a film-forming substrate to obtain the anticorrosive paint, wherein the nano carrier is any one or a mixture of graphene, nano boron nitride, nano clay and a layered double hydroxide sheet layer, the mass percent of the nano carrier is 0.4% -4%, the self-detection chromogenic substance is any one or a mixture of thymol blue, fluorescein, hydroxyquinoline, 1,10-Phenanthroline (1,10-Phenanthroline), 1,10-Phenanthroline pentaamino (1,10-Phenanthroline-5-amine) and phenolphthalein, the film-forming substrate is a water-based organic resin, the water-based organic resin is any one or a mixture of water-based polyurethane, water-based acrylic resin and water-based epoxy resin, and the mass percent of the water-based organic resin is more than or equal to 94%.
In the method for preparing the self-detection anticorrosive paint containing the nano-carrier, the method can also have the following characteristics: wherein the mass percentage of the self-detection chromogenic substance is 0.2-2%.
In the method for preparing the self-detection anticorrosive paint containing the nano-carrier, the method can also have the following characteristics: wherein, in the first step, the nano-carrier is prepared and prepared into a nano-carrier water solution with the standard concentration of 1mg/ml to 5 mg/ml; in the second step, the nano carrier solution and the self-detection chromogenic substance are mixed according to the mass ratio of 0.9-3.5: mixing at a ratio of 0.3-1.8 to obtain a first mixed solution; in the fourth step, the solid substance is added with water to prepare a third mixed solution with the proportion of 1 mg/ml-5 mg/ml.
Action and Effect of the invention
According to the method for preparing the self-detection anticorrosive coating containing the nano-carrier, which is related by the invention, a nano loading technology is adopted to prepare an intelligent coating which is used as a carrier of a self-detection chromogenic substance and has the function of loading and timely releasing a color developing agent, so that the color developing agent is uniformly mixed in the coating by the method for preparing the self-detection anticorrosive coating containing the nano-carrier, the color change which is visible to naked eyes occurs at the initial stage of the corrosion reaction of a steel plate, the functions of automatic detection and early warning are realized, in addition, the coating prepared by the method has excellent anticorrosive performance, and volatile organic matters are not used in the whole preparation process of the coating prepared by the method, so that the method belongs to an environment-friendly coating.
Drawings
FIG. 1 is a photograph showing the self-color development function of the coating layer upon corrosion of the surface of the iron plate in the first embodiment of the present invention;
FIG. 2 is a photograph of the coating after an extended etching time according to the first embodiment of the present invention;
FIG. 3 shows examples I, II, and III of the present invention without Fe2+A photograph of the color of the coating before ionization; and
FIG. 4 shows examples of the present invention in which Fe is added2+Photograph of the color of the coating after ionization.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the following embodiments are combined with the accompanying drawings to specifically describe the method for preparing the self-detection anticorrosive paint containing the nano-carrier.
< example one >
The preparation method and application of the self-detection anticorrosive paint containing the nano-carrier comprise the following steps:
step one, preparing graphene oxide by using an improved Hummer's method, and preparing a graphene oxide aqueous solution with the concentration of 2 mg/ml.
Step two, mixing the graphene oxide aqueous solution and 1,10 phenanthroline according to a mass ratio of 2: 1 to obtain a first mixed solution.
And step three, performing ultrasonic dispersion on the first mixed solution in an ultrasonic instrument with the ultrasonic power of 300W for 10 minutes to obtain a second mixed solution.
And step four, removing unreacted solution in the second mixed solution by suction filtration to obtain solid substances, and adding water to the solid substances to prepare a third mixed solution of 2 mg/ml.
And step five, mixing the third mixed solution with the waterborne polyurethane resin to obtain the anticorrosive paint, wherein the resin mass percent of the total solid matters of the paint is 99.4%, the graphene oxide mass percent is 0.4%, and the 1,10 phenanthroline mass percent is 0.2%.
Step six, adding deionized water into the anticorrosive paint to adjust the mass percent of the total solid matters of the paint to 20%.
And step seven, coating the coating added with the deionized water in the step six on the surface of the iron plate by using a bar coating method to form a film, putting the film into an oven, drying the film at the temperature of 110 ℃, and taking out the film after 30 minutes to obtain the coating formed on the surface of the iron plate.
< example two >
The preparation method and application of the self-detection anticorrosive paint containing the nano-carrier comprise the following steps:
step one, preparing graphene oxide by using an improved Hummer's method, and preparing a graphene oxide aqueous solution with the concentration of 2 mg/ml.
Step two, mixing the graphene oxide aqueous solution and 1,10 phenanthroline pentaamino according to a mass ratio of 2: 1 to obtain a first mixed solution.
And step three, performing ultrasonic dispersion on the first mixed solution in an ultrasonic instrument with the ultrasonic power of 300W for 10 minutes to obtain a second mixed solution.
And step four, removing unreacted solution in the second mixed solution by suction filtration to obtain solid substances, and adding water to the solid substances to prepare a third mixed solution of 2 mg/ml.
And step five, mixing the third mixed solution with the waterborne polyurethane resin to obtain the anticorrosive paint, wherein the resin mass percent in the total solid matters of the paint is 94%, the graphene oxide mass percent is 4%, and the phenanthroline pentaamino mass percent is 1, 10% is 2%.
Step six, adding deionized water into the anticorrosive paint to adjust the mass percent of the total solid matters of the paint to 20%.
And step seven, coating the paint added with the deionized water in the step six on the surface of an iron plate by using a bar coating method to form a film, then putting the film into an oven, drying the film at the temperature of 110 ℃, and taking the film out after 30 minutes to obtain the coating formed on the surface of the iron plate.
< example three >
The preparation method and application of the self-detection anticorrosive paint containing the nano-carrier comprise the following steps:
step one, preparing graphene oxide by using an improved Hummer's method, preparing a graphene oxide aqueous solution with the concentration of 2mg/ml, and adding hydrazine hydrate which is not more than 0.3 times of the mass of the graphene to obtain the graphene aqueous solution after the graphene oxide is partially reduced.
Step two, mixing the partially reduced graphene aqueous solution and 1,10 phenanthroline according to a mass ratio of 2: 1 to obtain a first mixed solution.
And step three, performing ultrasonic dispersion on the first mixed solution in an ultrasonic instrument with the ultrasonic power of 300W for 10 minutes to obtain a second mixed solution.
And step four, removing unreacted solution in the second mixed solution by suction filtration to obtain solid substances, and adding water to the solid substances to prepare a third mixed solution of 2 mg/ml.
And step five, mixing the third mixed solution with the waterborne polyurethane resin to obtain the anticorrosive paint, wherein the resin mass percent of the total solid matters of the paint is 97%, the graphene oxide mass percent is 2%, and the phenanthroline mass percent is 1, 10%.
Step six, adding deionized water into the anticorrosive paint to adjust the mass percent of the total solid matters of the paint to 20%.
And step seven, coating the paint added with the deionized water in the step six on the surface of an iron plate by using a bar coating method to form a film, then putting the film into an oven, drying the film at the temperature of 110 ℃, and taking the film out after 30 minutes to obtain the coating formed on the surface of the iron plate.
The chemical properties of the composite aqueous solutions formed by the graphene with different reduction degrees and the self-detection coloring substances prepared according to the first to third embodiments are very stable, and no obvious delamination phenomenon is observed after the composite aqueous solutions are placed for 48 hours. Meanwhile, the chemical property of the prepared coating loaded with graphene formed by self-detection color development and mixed with waterborne polyurethane is very stable, and no obvious layering phenomenon is observed after the coating is placed for 48 hours.
FIG. 1 is a photograph showing the self-color-developing function of the coating layer upon corrosion of the surface of the iron plate in the first embodiment of the present invention.
As shown in FIG. 1, it can be seen that the iron plate has good transparency after being bar-coated at room temperature, and the color change visible to the naked eye is generated at the initial stage of corrosion of the iron plate, and the color reaction of the paint is sensitive.
FIG. 2 is a photograph of the coating after an extended etching time according to the first embodiment of the present invention.
As shown in fig. 2, the iron plate in the figure is the iron plate after the rod is coated with the paint in example one and then soaked in the 3.5% NaCl aqueous solution for 1 day, and it can be seen that the iron plate has obvious discoloration phenomenon on the coating layer, which indicates that the base metal has large-area corrosion, and the paint prepared in example one has the self-detection and coloration function.
FIG. 3 shows examples I, II, and III of the present invention without Fe2+Photograph of the color of the coating before ionization.
As shown in FIG. 3, the first, second and third embodiments of FIG. 3 are without Fe added sequentially from left to right2+The coating containing the self-detection chromogenic substance before ionization can be seen to be very stable, and the intelligent coating containing the self-detection chromogenic substance loaded by the nano carrier is also shown to not change the stability of the coating.
FIG. 4 shows examples of the present invention in which Fe is added2+Photograph of the color of the coating after ionization.
As shown in FIG. 4, Fe is added to the first embodiment, the second embodiment and the third embodiment sequentially from left to right in the drawing of FIG. 42+The ionized coating containing the self-detecting chromogenic substance produces obvious color change. The intelligent coating containing the self-detection chromogenic substance prepared by the nano loading technology effectively solves the problems of loading, dispersion, release and the like of the chromogenic agent in the coating, simultaneously retains the characteristics of the chromogenic agent, and can be used for preparing the coating with the self-detection chromogenic function and good corrosion resistance and a coating thereof.
Effects and effects of the embodiments
In a preferred embodiment of the present invention, the nano-carrier in the preparation method is selected from graphene. The graphene may be selected from graphene oxide, partially reduced graphene oxide, and chemically surface modified graphene. In a more preferred embodiment, the graphene is graphene oxide, which may be in the form of a graphene oxide solution prepared by a modified Hummer's method, for example. The functional group on the surface of the graphene is regulated and controlled by partially reducing or chemically modifying the surface of the graphene, so that the load function of the nano carrier on the self-detection chromogenic molecule is controlled. In a preferred embodiment of the present invention, the partially reduced graphene oxide may be prepared by using a reducing agent. The reducing agent may be selected from hydrazine and its derivatives, vitamin C and glucose. In the case where the graphene is in the form of a graphene oxide solution prepared by the modified Hummer's method, the reducing agent is preferably hydrazine hydrate in a trace amount (less than the mass of the graphene oxide). The graphene and the derivatives thereof have good physical barrier property and ultra-large specific surface area. On one hand, the coating can be used as a barrier in the coating to enhance the corrosion resistance of the coating; on the other hand, the carrier can be used as a carrier for self-detection of the color developing molecules, and has the functions of loading and timely releasing the color developing agent.
In addition, in a preferred embodiment of the present invention, the self-detecting chromogenic molecule in the preparation method may be one selected from the group consisting of 1,10-Phenanthroline (1,10-Phenanthroline), 1,10-Phenanthroline pentaamino (1,10-Phenanthroline-5-amine) phenolphthalein, thymol blue, fluorescein, and hydroxyquinoline. In a more preferred embodiment, the self-detecting chromogenic molecule can employ 1,10 phenanthroline, which provides self-detecting color by providing 1,10 phenanthroline.
Further, in the preferred embodiment of the present invention, the preparation method allows the solid content to be controlled to about 20% to obtain the best film formability and the flatness of the coating surface.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
Claims (1)
1. A method for preparing a self-detection anticorrosive paint containing a nano-carrier is characterized by comprising the following steps:
step one, preparing graphene oxide by using an improved Hummer's method, preparing a graphene oxide aqueous solution with the concentration of 2mg/ml,
step two, mixing the graphene oxide aqueous solution and 1,10 phenanthroline according to a mass ratio of 2: 1 to obtain a first mixed solution,
step three, performing ultrasonic dispersion on the first mixed solution in an ultrasonic instrument with the ultrasonic power of 300W for 10 minutes to obtain a second mixed solution,
step four, removing unreacted solution in the second mixed solution by suction filtration to obtain solid substances, adding water into the solid substances to prepare a third mixed solution of 2mg/ml,
and step five, mixing the third mixed solution with the waterborne polyurethane resin to obtain the anticorrosive paint, wherein the resin mass percent of the total solid matters of the paint is 99.4%, the graphene oxide mass percent is 0.4%, and the 1,10 phenanthroline mass percent is 0.2%.
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| CN201810256020.3A CN108485495B (en) | 2016-07-19 | 2016-07-19 | Method for preparing self-detection anticorrosive paint containing nano-carrier |
| CN201610566796.6A CN106189771B (en) | 2016-07-19 | 2016-07-19 | A kind of self-test anticorrosive paint containing nano-carrier and its preparation method and application |
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| CN201810256033.0A Expired - Fee Related CN108485496B (en) | 2016-07-19 | 2016-07-19 | Application of self-detection anticorrosive paint containing nano-carrier on metal surface |
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| CN108485495B (en) * | 2016-07-19 | 2020-02-18 | 上海理工大学 | Method for preparing self-detection anticorrosive paint containing nano-carrier |
| CN106634422B (en) * | 2016-12-14 | 2019-01-08 | 中国科学院过程工程研究所 | A kind of polymeric coating material and preparation method thereof for detecting metal erosion |
| CN108300141A (en) * | 2017-07-04 | 2018-07-20 | 河北晨阳工贸集团有限公司 | Sealing wax and its preparation method and application |
| CN107446464B (en) * | 2017-07-20 | 2019-07-19 | 中国科学院过程工程研究所 | Polymeric coating material and preparation method with Corrosion monitoring and self-repair function |
| CN110183569B (en) * | 2019-05-30 | 2020-12-29 | 江南大学 | Metal corrosion early warning polymer coating material and preparation method thereof |
| US11236195B2 (en) * | 2020-02-24 | 2022-02-01 | Saudi Arabian Oil Company | Corrosion-indicating materials and methods of making and using the same |
| CN112175498A (en) * | 2020-10-06 | 2021-01-05 | 青岛羚智涂料科技有限责任公司 | Self-detection water-based self-repairing anticorrosive coating and preparation method thereof |
| CN112403409A (en) * | 2020-10-06 | 2021-02-26 | 青岛羚智涂料科技有限责任公司 | Self-detection capsule for water-based anticorrosive paint and preparation method thereof |
| CN114574977A (en) * | 2022-02-24 | 2022-06-03 | 中国海洋大学 | Self-early-warning coaxial electrostatic spinning fiber and preparation method and application thereof |
| CN116004093B (en) * | 2022-12-26 | 2023-10-03 | 中国科学院福建物质结构研究所 | Anticorrosive coating and preparation method thereof |
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| CN108485496A (en) | 2018-09-04 |
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| CN106189771B (en) | 2018-06-19 |
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