CN110878184A - Graphene modified epoxy zinc-rich primer and preparation method thereof - Google Patents
Graphene modified epoxy zinc-rich primer and preparation method thereof Download PDFInfo
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- CN110878184A CN110878184A CN201910977159.1A CN201910977159A CN110878184A CN 110878184 A CN110878184 A CN 110878184A CN 201910977159 A CN201910977159 A CN 201910977159A CN 110878184 A CN110878184 A CN 110878184A
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
- C09D5/002—Priming paints
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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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0893—Zinc
Abstract
The invention discloses a graphene modified epoxy zinc-rich primer and a preparation method thereof, wherein the primer comprises a primer, a curing agent and a diluent, and the primer comprises the following components in parts by mass:
Description
Technical Field
The invention belongs to the field of coatings, and particularly relates to a graphene modified epoxy zinc-rich primer and a preparation method thereof.
Background
The zinc-rich primer is a common heavy-duty anticorrosive coating, has excellent physical and mechanical properties and corrosion resistance, is widely applied to ships, marine facilities, bridges, large-scale equipment and various large-scale building steel components, and has the corrosion resistance principle that metal zinc powder in the primer plays a role in cathodic protection on steel. The existing zinc-rich primer has the following defects because of high zinc powder content (60-85 percent):
1. the severe bottom sinking phenomenon occurs in the storage process of the zinc-rich primer;
2. the part coated with the zinc-rich primer generates zinc oxide smoke dust and zinc steam during hot processing such as welding, cutting and the like, and can harm human bodies;
3. the zinc-rich primer has higher density which is 2 times of the density of the common epoxy primer, and cannot be applied to special equipment.
Graphene has excellent mechanical properties, high electrical conductivity and thermal conductivity. By utilizing the excellent conductivity and shielding property of the graphene, the zinc powder content can be reduced and the performance of the zinc-rich primer can be improved by using a small amount of graphene to replace part of zinc powder. However, due to the large surface area of graphene, agglomeration is likely to occur, thereby affecting the performance of the primer.
Disclosure of Invention
The invention aims to provide the graphene modified epoxy zinc-rich primer with good graphene dispersibility, which has good water resistance, wear resistance and corrosion resistance.
In order to solve the technical problems, the invention adopts the following technical scheme:
the graphene modified epoxy zinc-rich primer comprises a primer, a curing agent and a diluent, and is characterized in that: the primer comprises the following components in parts by weight:
the epoxy resin is mainly used as a main film-forming material. Xylene and n-butanol are used as solvents, propylene glycol methyl ether is used as a cosolvent to form a solvent system, and graphene can be uniformly dispersed. The organic bentonite can form gel under the action of high-speed dispersion, is used as a rheological aid, and can improve the water resistance and chemical resistance of the primer. The antirust ferrophosphorus powder can replace a part of zinc powder, further reduce the content of the zinc powder and improve the hardness and wear resistance of a paint film. The anti-settling agent is used for enabling the primer to have thixotropy and improving the viscosity. The rust inhibitive pigment increases the color of the primer. The defoamer controls the surface tension of the primer and prevents the generation of foam.
Preferably, the curing agent comprises the following components in parts by weight:
65030-50 parts of low-molecular polyamide
35-55 parts of dimethylbenzene
10-20 parts of n-butyl alcohol
The curing agent is used for curing the primer, and the primer is formed into a film through the reaction of the polyamide and the epoxy resin. Xylene and n-butanol as solvents.
Preferably, the diluent comprises the following components in parts by weight:
60-80 parts of dimethylbenzene
20-40 parts of n-butanol
Xylene and n-butanol can be used as solvents to dilute the viscosity of the primer, so that the viscosity of the primer is adjusted to a certain range, and the primer is convenient to use.
Preferably, the primer: curing agent: the mass part ratio of the diluent is 10:1 (0.1-10). The proportion of the primer and the curing agent needs to be strictly controlled, the toughness of the paint film is reduced due to excessive curing agent, the service life of the paint film is affected, and the primer is cured slowly and even can be dare for a long time due to insufficient curing agent. Primer coating: the optimal weight ratio of the curing agent is 10: 1. The thinner is used for reducing the viscosity of the primer and preventing the primer from being higher in viscosity and incapable of being coated. The viscosity of the primer is dependent on the environment, so the dosage of the thinner can be adjusted according to the environment.
Preferably, the epoxy resin solution comprises the following components in parts by weight: 75 parts of bisphenol A type epoxy resin, 17 parts of dimethylbenzene and 8 parts of butanol.
The epoxy resin is bisphenol A epoxy resin, and xylene and butanol are used as solvents.
A preparation method of a graphene modified epoxy zinc-rich primer is characterized by comprising the following steps:
(1) adding propylene glycol methyl ether, n-butanol and xylene into a paint mixing tank, uniformly stirring, adding graphene, and continuously stirring and dispersing;
(2) pouring the epoxy resin solution into a paint mixing tank, and uniformly stirring;
(3) adding rust-proof phosphorus iron powder, zinc powder, rust-proof pigment, organic bentonite, anti-settling agent and defoaming agent into a paint mixing tank, and uniformly stirring;
(4) preparing a curing agent from low-molecular polyamide 650, xylene and n-butanol, adding the curing agent into a paint mixing tank, and uniformly stirring;
(5) measuring the viscosity of the primer in the paint mixing tank, adding a diluent prepared from dimethylbenzene and n-butyl alcohol, filtering by using a filter screen, and packaging.
The anti-settling agent is preferably E-200, and the defoaming agent is preferably 241.
Since graphene is easily adsorbed by epoxy resin, the graphene is easily unevenly distributed in the epoxy resin when directly added into the epoxy resin, so that the graphene is firstly added into a mixed solvent consisting of a solvent and a cosolvent before the epoxy resin is added, and is evenly distributed after being stirred, thereby avoiding the phenomenon of agglomeration. Then adding epoxy resin, adding the rest components and fully stirring. And then adding the prepared curing agent, measuring the current viscosity after fully stirring, and adding a diluent according to the viscosity condition to reduce the viscosity of the primer.
Preferably, before the step (1), placing graphene oxide powder into a mixed solvent composed of n-butanol and xylene, performing ultrasonic dispersion for 0.5-5h, transferring the dispersion liquid into a reaction stirring kettle, adding catechol dissolved in the mixed solvent into the reaction stirring kettle, keeping the temperature of the reaction stirring kettle at 100-200 ℃, continuously stirring for 4-12h, filtering, washing and drying the sample to obtain graphene; and (2) putting 5-20 parts by mass of the prepared graphene, 0.5-5 parts by mass of a silane coupling agent and 1-10 parts by mass of a dispersing agent into 30-60 parts by mass of a mixed solvent, and performing ultrasonic dispersion for 0.5-5h to obtain a graphene solution. The dispersant is preferably N-methylpyrrolidone.
Graphene with high purity is prepared by reducing graphene oxide with catechol, and then the graphene is uniformly dispersed in a mixed solvent through a silane coupling agent and a dispersing agent, so that the compatibility between the graphene and an epoxy resin solution is enhanced, and the dispersibility of the graphene is improved.
Preferably, before the step (2), 10-20 parts by mass of organosilicon monomer and 1-5 parts by mass of catalyst dibutyltin dilaurate are added into 50-80 parts by mass of epoxy resin solution, the temperature is raised to 120-200 ℃, and the reaction time is 5-10h, so as to obtain organosilicon modified epoxy resin solution.
The compatibility between the primer and the finish paint is enhanced by the organosilicon modified epoxy resin solution, so that the adhesion between the primer and the finish paint is better, and the weather resistance of the primer is improved.
Preferably, the stirring speed in the step (1) is 100-500r/min, and the stirring time is 5-30 minutes; in the step (2), the stirring speed is 500-. When the graphene is stirred, the stirring speed is not high easily, and the phenomenon that the temperature of the solvent is increased due to stirring heat generation is avoided, so that the graphene is agglomerated. After the epoxy resin is added, the graphene is adsorbed on the epoxy resin, and the agglomeration phenomenon can not occur any more, so that the stirring speed can be increased, and the graphene and the epoxy resin are uniformly mixed. In the step (3), the stirring speed is 1000-; after stirring uniformly, putting the raw materials into a grinder for grinding until the fineness is less than 50 mu m, and pouring the ground raw materials into a paint mixing tank. And adding the rest components, and stirring at a high speed to uniformly mix all the components in the primer. Due to the presence of such particles in the primer, the primer needs to be ground by a grinder to increase the fineness of the primer. In the step (4), the stirring speed is 100-. Adding the curing agent, stirring to uniformly mix the primer and the curing agent, and drying, curing and uniformly mixing the primer.
Preferably, in the step (5), when the viscosity of the primer in the paint mixing tank reaches 90-100KU, the diluent is stopped to be added. The addition of the diluent is related to viscosity, and the viscosity is related to temperature and humidity, so that the viscosity of the primer needs to be monitored in real time, and the diluent is added according to conditions.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
according to the invention, a small amount of graphene replaces part of zinc powder, so that the content of the zinc powder in the primer is reduced, zinc oxide smoke and zinc vapor generated during welding are reduced, the density of the primer is reduced, the conductivity, the water resistance and the corrosion resistance of the primer are improved, the surface of the primer is more compact after the primer is dried, and the primer has a good corrosion prevention effect.
According to the invention, xylene and n-butanol are used as solvents, propylene glycol methyl ether is used as a cosolvent to form a solvent system, and graphene can be uniformly dispersed. Epoxy resins are mainly used as the main film-forming material. The organic bentonite is added to form gel under the action of high-speed dispersion, and the gel is used as a rheological aid and can improve the water resistance and chemical resistance of the primer. The antirust ferrophosphorus powder can replace a part of zinc powder, further reduce the content of the zinc powder and improve the hardness and wear resistance of a paint film. The anti-settling agent is used for enabling the primer to have thixotropy and improving the viscosity. The rust inhibitive pigment increases the color of the primer. The defoamer controls the surface tension of the primer and prevents the generation of foam.
When the primer is prepared, in order to prevent uneven stirring after the graphene is added with the epoxy resin, the graphene with high purity is prepared by reducing and oxidizing the graphene through catechol, and then the graphene is uniformly dispersed in a mixed solvent through a silane coupling agent and a dispersing agent, so that the compatibility between the graphene and the epoxy resin solution is enhanced, and the dispersibility of the graphene is improved. The compatibility between the primer and the finish paint is enhanced by the organosilicon modified epoxy resin solution, so that the adhesion between the primer and the finish paint is better, and the weather resistance of the primer is improved.
Detailed Description
The present invention is further illustrated by the following examples.
Preparing a graphene solution:
putting 10 parts by mass of graphene oxide powder into a mixed solvent composed of 100 parts by mass of n-butanol and xylene, performing ultrasonic dispersion for 3 hours, transferring the dispersion liquid into a reaction stirring kettle, adding catechol dissolved in the mixed solvent and having a mass concentration of 1g/mL into the reaction stirring kettle, keeping the temperature of the reaction stirring kettle at 100-200 ℃, continuously stirring for 10 hours, filtering, washing and drying the sample to obtain the graphene.
And putting 15 parts by mass of the prepared graphene, 3 parts by mass of a silane coupling agent and 5 parts by mass of a dispersing agent into a mixed solvent composed of 50 parts by mass of n-butyl alcohol and xylene, and performing ultrasonic dispersion for h to obtain a graphene solution.
Preparing an organic silicon modified epoxy resin solution:
adding 15 parts by mass of organic silicon monomer and 3 parts by mass of catalyst dibutyltin dilaurate into 70 parts by mass of epoxy resin solution, heating to 180 ℃, and reacting for 10 hours to obtain the organic silicon modified epoxy resin solution.
Examples 1 to 5
A preparation method of graphene modified epoxy zinc-rich primer comprises the following steps:
(1) adding propylene glycol methyl ether, n-butanol and xylene into a paint mixing tank, uniformly stirring, adding graphene, continuously stirring and dispersing at the stirring speed of 200r/min for 30 minutes;
(2) pouring the organosilicon modified epoxy resin solution into a paint mixing tank, and uniformly stirring at the stirring speed of 2000r/min for 60 minutes;
(3) adding rust-proof phosphorus iron powder, zinc powder, rust-proof pigment, organic bentonite, an anti-settling agent and a defoaming agent into a paint mixing tank, and uniformly stirring at the stirring speed of 3000r/min for 45 minutes;
(4) preparing a curing agent from low-molecular-weight polyamide 650, xylene and n-butanol, adding the curing agent into a paint mixing tank, and uniformly stirring at a stirring speed of 500r/min for 45 minutes;
(5) measuring the viscosity of the primer in the paint mixing tank, adding a diluent prepared from dimethylbenzene and n-butyl alcohol, stopping adding the diluent when the viscosity of the primer in the paint mixing tank reaches 90-100KU, filtering by using a filter screen, and packaging.
The mass parts ratios of the components in examples 1 to 5 are shown in Table 1.
The prepared graphene modified epoxy zinc-rich primer is subjected to performance detection, and the performance is shown in table 2.
Comparative examples 1 to 2
The preparation process is as in examples 1-5, except that no graphene is added in comparative example 1, and no graphene and antirust ferrophosphorus powder are added in comparative example 2, and the mass parts of the components are shown in table 1.
Table 1: components in examples 1-5 and comparative example 1 (in parts by mass).
Table 2: the performance index of the primers obtained in examples 1 to 5 and comparative example 1.
Compared with the comparative examples 1-5 and 1-2, the dry film thickness of the primer after the addition of the graphene is obviously smaller than that of the primer without the addition of the graphene, and the salt spray resistance of the primer after the addition of the graphene is excellent, and the primer has no change after more than 1000 hours in a salt spray test. Comparative example 1 has no graphene but contains rust-proof ferrous phosphorus powder to replace part of zinc powder, so that no change is caused in the salt spray test for more than 600h, while comparative example 2 has no graphene and rust-proof ferrous phosphorus powder, the content of the zinc powder is higher, and the foaming phenomenon appears in the salt spray test for 300 h.
The above is only a specific embodiment of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions or modifications made on the basis of the present invention to solve the same technical problems and achieve the same technical effects are all covered in the protection scope of the present invention.
Claims (10)
1. The graphene modified epoxy zinc-rich primer comprises a primer, a curing agent and a diluent, and is characterized in that: the primer comprises the following components in parts by weight:
2. the graphene-modified epoxy zinc-rich primer according to claim 1, wherein: the curing agent comprises the following components in parts by weight:
65030-50 parts of low-molecular polyamide
35-55 parts of dimethylbenzene
10-20 parts of n-butyl alcohol.
3. The graphene-modified epoxy zinc-rich primer according to claim 1, wherein: the diluent comprises the following components in parts by weight:
60-80 parts of dimethylbenzene
20-40 parts of n-butyl alcohol.
4. The graphene-modified epoxy zinc-rich primer according to claim 1, wherein: the primer comprises the following components: curing agent: the mass part ratio of the diluent is 10:1 (0.1-10).
5. The graphene-modified epoxy zinc-rich primer according to claim 1, wherein: the epoxy resin solution comprises the following components in parts by weight: 75 parts of bisphenol A type epoxy resin, 17 parts of dimethylbenzene and 8 parts of butanol.
6. A preparation method of the graphene-modified epoxy zinc rich primer according to any one of claims 1 to 5, comprising the following steps:
(1) adding propylene glycol methyl ether, n-butanol and xylene into a paint mixing tank, uniformly stirring, adding graphene, and continuously stirring and dispersing;
(2) pouring the epoxy resin solution into a paint mixing tank, and uniformly stirring;
(3) adding rust-proof phosphorus iron powder, zinc powder, rust-proof pigment, organic bentonite, anti-settling agent and defoaming agent into a paint mixing tank, and uniformly stirring;
(4) preparing a curing agent from low-molecular polyamide 650, xylene and n-butanol, adding the curing agent into a paint mixing tank, and uniformly stirring;
(5) measuring the viscosity of the primer in the paint mixing tank, adding a diluent prepared from dimethylbenzene and n-butyl alcohol, filtering by using a filter screen, and packaging.
7. The preparation method of the graphene-modified epoxy zinc-rich primer according to claim 6, wherein the preparation method comprises the following steps: before the step (1), placing graphene oxide powder into a mixed solvent composed of n-butyl alcohol and xylene, performing ultrasonic dispersion for 0.5-5h, transferring a dispersion liquid into a reaction stirring kettle, adding catechol dissolved in the mixed solvent and having a mass concentration of 1g/mL into the reaction stirring kettle, keeping the temperature of the reaction stirring kettle at 100-200 ℃, continuously stirring for 4-12h, filtering, washing and drying a sample to obtain graphene; and (2) putting 5-20 parts by mass of the prepared graphene, 0.5-5 parts by mass of a silane coupling agent and 1-10 parts by mass of a dispersing agent into 30-60 parts by mass of a mixed solvent, and performing ultrasonic dispersion for 0.5-5h to obtain a graphene solution.
8. The preparation method of the graphene-modified epoxy zinc-rich primer according to claim 6, wherein the preparation method comprises the following steps: before the step (2), adding 10-20 parts by mass of organic silicon monomer and 1-5 parts by mass of catalyst dibutyltin dilaurate into 50-80 parts by mass of epoxy resin solution, heating to 120-200 ℃, and reacting for 5-10h to obtain the organic silicon modified epoxy resin solution.
9. The preparation method of the graphene-modified epoxy zinc-rich primer according to claim 6, wherein the preparation method comprises the following steps: the stirring speed in the step (1) is 100-500r/min, and the stirring time is 5-30 minutes; the stirring speed in the step (2) is 500-5000r/min, and the stirring time is 30-60 minutes; the stirring speed in the step (3) is 1000-; after stirring uniformly, putting the raw materials into a grinder for grinding until the fineness is less than 50 mu m, and pouring the ground raw materials into a paint mixing tank; the stirring speed in the step (4) is 100-1000r/min, and the stirring time is 30-60 minutes.
10. The graphene-modified epoxy zinc-rich primer according to claim 6, wherein: and (5) stopping adding the diluent when the viscosity of the primer in the paint mixing tank reaches 90-100 KU.
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| CN112680056A (en) * | 2020-12-10 | 2021-04-20 | 珠海复旦创新研究院 | Anticorrosive paint and preparation method and application thereof |
| CN114702881A (en) * | 2022-04-20 | 2022-07-05 | 湖南省德谦新材料有限公司 | Solvent-free epoxy graphene zinc powder coating and preparation method thereof |
| CN114989699A (en) * | 2022-06-20 | 2022-09-02 | 紫荆花涂料（上海）有限公司 | Solvent type graphene epoxy zinc-rich primer and preparation process thereof |
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