CN113801539A - Preparation method of graphene epoxy resin coating - Google Patents
Preparation method of graphene epoxy resin coating Download PDFInfo
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- CN113801539A CN113801539A CN202111185194.3A CN202111185194A CN113801539A CN 113801539 A CN113801539 A CN 113801539A CN 202111185194 A CN202111185194 A CN 202111185194A CN 113801539 A CN113801539 A CN 113801539A
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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
- C09D5/08—Anti-corrosive 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
- 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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- Engineering & Computer Science (AREA)
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Abstract
The invention relates to the technical field of high polymer materials, in particular to a preparation method of a graphene epoxy resin coating.
Description
Technical Field
The invention relates to the technical field of high molecular functions, in particular to a preparation method of a graphene epoxy resin coating.
Background
The graphene has good mechanical properties, and can improve the mechanical properties of the coating, but the graphene is easy to self-agglomerate, and the dispersibility of the graphene in a matrix is poor, so that the properties of the coating are difficult to improve.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the preparation method of the graphene epoxy resin coating, which is simple and safe to operate and low in cost, and can improve the physical property and the mechanical property of the coating when the graphene epoxy resin coating is applied to the coating.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a graphene epoxy resin coating comprises the following steps:
(1) surface modification of graphene:
(1.1) weighing a quantitative modifier in a beaker, and adding a solvent to dissolve the quantitative modifier to obtain a modified solution;
(1.2) weighing raw material graphene in a mixing barrel, adding the modification solution, and adding deionized water;
(1.3) stirring and sanding, and after sanding for a certain time, spray drying to obtain modified graphene;
(2) preparing a graphene/epoxy resin coating:
(2.1) weighing quantitative epoxy resin, placing the epoxy resin in a dispersion machine, and starting the dispersion machine to rotate and stir at the rotating speed of 400-600 rpm;
(2.2) adding the modified graphene, increasing the rotating speed of a dispersion machine after the addition is finished, and sequentially adding a diluent, a defoaming agent, a leveling agent and a dispersing agent;
(2.3) continuously stirring for 15-25 min after the addition is finished; then, uniformly dispersing the modified graphene in a matrix by sanding to obtain a component A;
(2.4) diluting a curing agent phenol aldehyde amine by using a diluent to obtain a component B, weighing a quantitative component B, putting the quantitative component B into the component A, and stirring at the rotating speed of 800-;
and (2.5) brushing the paint on the base material, and drying the base material in a constant temperature and humidity chamber with the temperature of 23 ℃ and the relative humidity of 50% for 6-8 days to obtain the graphene/epoxy resin coating.
Preferably, the modifier in the step (1.1) is one or a mixture of more of (E) -cyclooct-2-en-1-yl (4-nitrophenyl) carbonate, PEDOT, potassium pentyltrichloroborate, NP-40, n-butyl thiophosphoric triamide, aminotrimethylene phosphonic acid, an antioxidant 350, 3' -dithiobis (propane-1-ol), and tetraisopropyl methylenediphosphate.
Preferably, the mass ratio of the modifying solution to the deionized water in the step (1.2) is 0.3/3-2.0/3, and the sanding rotating speed is 800-1100 rpm.
Preferably, in the step (2.3), the rotation speed of the sand mill is 1600-2100 rpm, and the time is 25-45 min.
Preferably, the thickness of the coating in the step (2.5) is 20-100 μm.
Preferably, the amount of the modified graphene in the step (2.2) is 0.3% -0.6%.
Preferably, the mass ratio of the diluent to the curing agent of the component B in the step (2.4) is 0.5-0.9.
Compared with the prior art, the invention has the beneficial effects that: the surface of the graphene is modified, so that the surface energy of the graphene can be reduced, and the agglomeration phenomenon of the graphene is reduced; the surface of the graphene is grafted with a group capable of being combined with a matrix, so that the compatibility of the modified graphene and epoxy resin can be improved, and the mixing degree between the coating and the filler can be greatly improved by a sand milling mixing method, so that the excellent performance of the graphene can be better exerted.
Through the sanding mode, the modifier is used as a bridge, the compatibility of the graphene and the water-based acrylic resin can be improved, the dispersion of the graphene in a matrix is increased, and the high-water-resistance graphene/epoxy resin coating is obtained.
The coating obtained by the invention has good physical property and mechanical property and better application prospect.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: a preparation method of a graphene epoxy resin coating is characterized by comprising the following steps: the method comprises the following steps:
(1) surface modification of graphene:
(1.1) weighing a quantitative modifier in a beaker, and adding a solvent to dissolve the quantitative modifier to obtain a modified solution;
(1.2) weighing raw material graphene in a mixing barrel, adding the modification solution, and adding deionized water;
(1.3) stirring and sanding, and after sanding for a certain time, spray drying to obtain modified graphene;
(2) preparing a graphene/epoxy resin coating:
(2.1) weighing quantitative epoxy resin, placing the epoxy resin in a dispersing machine, and starting the dispersing machine to rotate and stir at the rotating speed of 400-600rpm (specifically 500 rpm);
(2.2) adding the modified graphene, increasing the rotating speed of a dispersion machine after the addition is finished, and sequentially adding a diluent, a defoaming agent, a leveling agent and a dispersing agent;
(2.3) continuously stirring for 15-25 min (specifically 20 min) after the addition is finished; then, uniformly dispersing the modified graphene in a matrix by sanding to obtain a component A;
(2.4) diluting a curing agent phenol aldehyde amine by using a diluent to obtain a component B, weighing a quantitative component B, putting the quantitative component B into the component A, and stirring at the rotating speed of 800-;
and (2.5) brushing the paint on the base material, and drying the base material in a constant temperature and humidity chamber with the temperature of 23 ℃ and the relative humidity of 50% for 6-8 (specifically 7 days) days to obtain the graphene/epoxy resin coating.
In the step (1.1), the modifier is one or a mixture of more of (E) -cycloocta-2-ene-1-yl (4-nitrophenyl) carbonate, PEDOT, potassium amyl trichloroborate, NP-40, n-butyl thiophosphoric triamide, aminotrimethylene phosphonic acid, an antioxidant 350, 3' -dithiobis (propane-1-ol) and tetraisopropyl methylene diphosphate.
In the step (1.2), the mass ratio of the modifying solution to the deionized water is 0.3/3-2.0/3, and the sanding rotating speed is 800-1100 rpm.
In the step (2.3), the rotation speed of the sand mill is 1600-2100 rpm, and the time is 25-45 min.
The thickness of the coating in the step (2.5) is 20-100 μm.
The using amount of the modified graphene in the step (2.2) is 0.3-0.6%.
In the step (2.4), the mass ratio of the diluent to the curing agent of the component B is 0.5-0.9.
Through the adoption of the technical scheme, the device,
example 1
Surface modification of graphene: 1.5 g of modifier is weighed into a beaker, 300 g of absolute ethyl alcohol is added, and the mixture is stirred and dissolved to obtain a modified solution. 50 g of raw material graphene is weighed in a mixing barrel, the prepared modification solution is added, and 3000 g of deionized water is added. The high speed stirrer is started, and the rotating speed is 650 rpm. After 5 min, the sand mill was started at 1000rpm with the mass of the rhenium zirconium being 2.0 kg and the sand milling time being 15 min. And (3) carrying out spray drying on the obtained slurry to obtain the modified graphene, wherein the spray drying parameters are as follows: inlet temperature 170 ℃ and wind speed 80 m3·h-1Creep speed 500 mL. h-1。
Preparing a graphene/epoxy resin coating: weighing 80 g of epoxy resin (E42), slowly adding 0.24 g of modified graphene into the resin at the rotation speed of 500rpm of a multipurpose dispersion machine, increasing the rotation speed to 1000rpm after the addition is finished, and sequentially adding 8 g of diluent, 0.10 g of defoaming agent, 0.10 g of flatting agent and 0.10 g of dispersing agent. Stirring for 20min after the addition is completed; and then sanding for 30 min at the rotating speed of 2000 rpm to uniformly disperse the graphene in the matrix to obtain the component A. Diluting curing agent phenol aldehyde amine with diluent to obtain component B, weighing 103.9 g of component B (the ratio of the diluent to the phenol aldehyde amine curing agent is 0.77), putting the weighed component B into the component A, and stirring at 1000rpm for 3min to obtain the coating. According to the test requirements, the coating is coated on a base material in a spraying mode, and the base material is placed in a constant temperature and humidity room with the temperature of 23 ℃ and the relative humidity of 50% to be dried for 7 days, so that the anticorrosive coating can be obtained.
Example 2
Surface modification of graphene: 1.5 g of modifier is weighed into a beaker, 400 g of absolute ethyl alcohol is added, and the mixture is stirred and dissolved to obtain a modified solution. Weighing 50 g of crude drugAnd putting the graphene into a mixing barrel, adding the prepared modified solution, and adding 3000 g of deionized water. The high speed stirrer is started, and the rotating speed is 650 rpm. After 5 min, the sand mill was started at 1000rpm with the mass of the rhenium zirconium being 2.0 kg and the sand milling time being 20 min. And (3) carrying out spray drying on the obtained slurry to obtain the modified graphene, wherein the spray drying parameters are as follows: inlet temperature 170 ℃ and wind speed 80 m3·h-1Creep speed 500 mL. h-1。
Preparing a graphene/epoxy resin coating: weighing 80 g of epoxy resin (E42), slowly adding 0.32 g of modified graphene into the resin at the rotation speed of 500rpm of a multipurpose dispersion machine, increasing the rotation speed to 1000rpm after the addition is finished, and sequentially adding 8 g of diluent, 0.10 g of defoaming agent, 0.10 g of flatting agent and 0.10 g of dispersing agent. Stirring for 20min after the addition is completed; and then sanding for 35 min at the rotating speed of 1800 rpm to uniformly disperse the graphene in the matrix to obtain the component A. Diluting curing agent phenol aldehyde amine with diluent to obtain component B, weighing 103.9 g of component B (the ratio of the diluent to the phenol aldehyde amine curing agent is 0.77), putting the weighed component B into the component A, and stirring at 1000rpm for 3min to obtain the coating. According to the test requirements, the coating is coated on a base material in a spraying mode, and the base material is placed in a constant temperature and humidity room with the temperature of 23 ℃ and the relative humidity of 50% to be dried for 7 days, so that the anticorrosive coating can be obtained.
Comparative example a
Weighing 80 g of epoxy resin (E42), slowly adding 0.15 g of raw material graphene into the resin at the rotation speed of 500rpm of a multipurpose dispersion machine, increasing the rotation speed to 1000rpm after the addition is finished, and sequentially adding 8 g of diluent, 0.10 g of defoaming agent, 0.10 g of flatting agent and 0.10 g of dispersing agent. And continuously stirring for 20min after the addition is finished, so that the graphene is uniformly dispersed in the matrix to obtain the component A. Diluting curing agent phenol aldehyde amine with diluent to obtain component B, weighing 103.9 g of component B (the ratio of the diluent to the phenol aldehyde amine curing agent is 0.77), putting the weighed component B into the component A, and stirring at 1000rpm for 3min to obtain the coating. And (3) coating the coating on a substrate in a spraying manner, and drying the substrate in a constant-temperature and constant-humidity chamber with the temperature of 23 ℃ and the relative humidity of 50% to obtain the graphene/epoxy resin coating.
Comparative example b
80 g of epoxy resin (E42) is weighed, and 8 g of diluent, 0.10 g of defoaming agent, 0.10 g of flatting agent and 0.10 g of dispersing agent are sequentially added at the rotation speed of 500rpm of a multipurpose dispersing machine. After the addition is completed, stirring is continued for 20min to obtain a component A. Diluting phenolic aldehyde amine serving as a curing agent by using a diluent to obtain a component B (the ratio of the diluent to the phenolic aldehyde amine curing agent is 0.77), weighing 103.9 g of the component B, putting the weighed component B into the component A, and stirring at the rotating speed of 1000rpm for 3min to obtain the coating. And (3) coating the coating on a substrate in a spraying manner, and drying the substrate in a constant-temperature and constant-humidity chamber with the temperature of 23 ℃ and the relative humidity of 50% to obtain the graphene/epoxy resin coating.
The experimental tests of example 1, example 2 and comparative examples a and b gave the following comparative data in tables 1 to 3:
TABLE 1 neutral salt spray time data
| Example 1 | Example 2 | Comparative example a | Comparative example b | |
| Time/h | 950 | 1000 | 700 | 400 |
TABLE 2 coating Water absorption data
| Example 1 | Example 2 | Comparative example a | Comparative example b | |
| Water absorption/%) | 0.7 | 0.5 | 1.7 | 3.3 |
TABLE 3 wear resistance data of the coatings
| Example 1 | Examples2 | Comparative example a | Comparative example b | |
| Abrasion mass/g | 18 | 20 | 50 | 66 |
Through the sanding mode, the modifier is used as a bridge, the compatibility of the graphene and the water-based acrylic resin can be improved, the dispersion of the graphene in a matrix is increased, and the high-water-resistance graphene/epoxy resin coating is obtained.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of a graphene epoxy resin coating is characterized by comprising the following steps: the method comprises the following steps:
(1) surface modification of graphene:
(1.1) weighing a quantitative modifier in a beaker, and adding a solvent to dissolve the quantitative modifier to obtain a modified solution;
(1.2) weighing raw material graphene in a mixing barrel, adding the modification solution, and adding deionized water;
(1.3) stirring and sanding, and after sanding for a certain time, spray drying to obtain modified graphene;
(2) preparing a graphene/epoxy resin coating:
(2.1) weighing quantitative epoxy resin, placing the epoxy resin in a dispersion machine, and starting the dispersion machine to rotate and stir at the rotating speed of 400-600 rpm;
(2.2) adding the modified graphene, increasing the rotating speed of a dispersion machine after the addition is finished, and sequentially adding a diluent, a defoaming agent, a leveling agent and a dispersing agent;
(2.3) continuously stirring for 15-25 min after the addition is finished; then, uniformly dispersing the modified graphene in a matrix by sanding to obtain a component A;
(2.4) diluting a curing agent phenol aldehyde amine by using a diluent to obtain a component B, weighing a quantitative component B, putting the quantitative component B into the component A, and stirring at the rotating speed of 800-;
and (2.5) brushing the paint on the base material, and drying the base material in a constant temperature and humidity chamber with the temperature of 23 ℃ and the relative humidity of 50% for 6-8 days to obtain the graphene/epoxy resin coating.
2. The preparation method of the graphene epoxy resin coating according to claim 1, characterized in that: in the step (1.1), the modifier is one or a mixture of more of (E) -cycloocta-2-ene-1-yl (4-nitrophenyl) carbonate, PEDOT, potassium amyl trichloroborate, NP-40, n-butyl thiophosphoric triamide, aminotrimethylene phosphonic acid, an antioxidant 350, 3' -dithiobis (propane-1-ol) and tetraisopropyl methylene diphosphate.
3. The preparation method of the graphene epoxy resin coating according to claim 1, characterized in that: in the step (1.2), the mass ratio of the modifying solution to the deionized water is 0.3/3-2.0/3, and the sanding rotating speed is 800-1100 rpm.
4. The preparation method of the graphene epoxy resin coating according to claim 1, characterized in that: in the step (2.3), the rotation speed of the sand mill is 1600-2100 rpm, and the time is 25-45 min.
5. The preparation method of the graphene epoxy resin coating according to claim 1, characterized in that: the thickness of the coating in the step (2.5) is 20-100 μm.
6. The preparation method of the graphene epoxy resin coating according to claim 1, characterized in that: the using amount of the modified graphene in the step (2.2) is 0.3-0.6%.
7. The preparation method of the graphene epoxy resin coating according to claim 1, characterized in that: in the step (2.4), the mass ratio of the diluent to the curing agent of the component B is 0.5-0.9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449248A (en) * | 2022-10-14 | 2022-12-09 | 山东京博装备制造安装有限公司 | Graphene heavy-duty anticorrosive paint for outer wall of earthing storage tank |
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| CN108929616A (en) * | 2018-07-16 | 2018-12-04 | 广东绿色大地化工有限公司 | Modified long-effective corrosion paint of a kind of metal base graphene and preparation method thereof |
| CN109354967A (en) * | 2018-09-10 | 2019-02-19 | 成都紫苑华光新材料科技有限公司 | A kind of graphene anticorrosive paint and preparation method thereof |
| CN110982389A (en) * | 2019-11-26 | 2020-04-10 | 厦门双瑞船舶涂料有限公司 | High-solid-content heavy-duty anticorrosive paint and preparation method thereof |
| CN113462202A (en) * | 2021-06-24 | 2021-10-01 | 浙江工业大学 | Method for improving dispersion effect of graphene in acrylic emulsion |
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2021
- 2021-10-12 CN CN202111185194.3A patent/CN113801539A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108929616A (en) * | 2018-07-16 | 2018-12-04 | 广东绿色大地化工有限公司 | Modified long-effective corrosion paint of a kind of metal base graphene and preparation method thereof |
| CN109354967A (en) * | 2018-09-10 | 2019-02-19 | 成都紫苑华光新材料科技有限公司 | A kind of graphene anticorrosive paint and preparation method thereof |
| CN110982389A (en) * | 2019-11-26 | 2020-04-10 | 厦门双瑞船舶涂料有限公司 | High-solid-content heavy-duty anticorrosive paint and preparation method thereof |
| CN113462202A (en) * | 2021-06-24 | 2021-10-01 | 浙江工业大学 | Method for improving dispersion effect of graphene in acrylic emulsion |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115449248A (en) * | 2022-10-14 | 2022-12-09 | 山东京博装备制造安装有限公司 | Graphene heavy-duty anticorrosive paint for outer wall of earthing storage tank |
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