CN111100493B - Graphene anti-corrosion-thermal control-anti-static integrated functional coating and preparation method thereof - Google Patents
Graphene anti-corrosion-thermal control-anti-static integrated functional coating and preparation method thereof Download PDFInfo
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Classifications
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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
-
- 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
-
- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
- C09D5/24—Electrically-conducting paints
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention relates to a graphene anti-corrosion-thermal control-anti-static integrated functional coating and a preparation method thereof, relates to a preparation method of a three-layer structure composite coating aiming at the requirements of thermal control, corrosion prevention and static prevention of an aircraft, and belongs to the technical field of surface engineering. The invention designs a preparation method of an anticorrosion-thermal control-antistatic integrated functional coating. The coating adopts a three-layer composite structure, conductive mica and zinc yellow epoxy resin are used as a bottom anti-corrosion layer, modified graphene and polyurethane are used as a middle conductive layer, silicon, fluorine modified polyurethane, nano zinc oxide and modified graphene are used as a surface thermal control layer, and a spraying mode is adopted to prepare the multifunctional integrated coating which has excellent anti-corrosion, anti-static and thermal control performances. The coating has good bonding force with a base material and low curing temperature, and can be used for various types of aircrafts.
Description
Technical Field
The invention relates to a graphene anti-corrosion-thermal control-anti-static integrated functional coating and a preparation method thereof, relates to a preparation method of a three-layer structure composite coating aiming at the requirements of thermal control, corrosion prevention and static prevention of an aircraft, and belongs to the technical field of surface engineering.
Background
High bearing capacity, long service life and long distance become important development trends of satellite platforms and weaponry in China. With the development of spacecrafts such as space-based radar satellites, military communication satellites and military reconnaissance satellites and the continuous deepening of asteroid exploration and manned lunar landing projects, the requirement of the spacecrafts on the light weight of the structure is more urgent.
However, the problem of poor corrosion resistance of the novel low-density light alloy and the light metal matrix composite material is solved, and the bottleneck of light application of structures of spacecrafts and new-generation weaponry is formed; with the construction and the use of the Hainan emission field and the continuous development of the deep blue navy, higher requirements are provided for corrosion protection of novel light alloy materials (magnesium alloy, magnesium-lithium alloy, aluminum-based silicon carbide, aluminum-lithium alloy and the like); meanwhile, in order to meet the requirements of heat dissipation and electrostatic protection of the high orbit spacecraft under the high vacuum condition, a novel light alloy material surface high-performance anti-corrosion-thermal control-anti-electrostatic multifunctional integrated coating needs to be developed urgently.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a graphene anticorrosion-thermal control-antistatic integrated functional coating and a preparation method thereof.
The technical solution of the invention is as follows:
a graphene anticorrosion-thermal control-antistatic integrated functional coating comprises a bottom layer, a middle layer and a surface layer;
the raw materials of the bottom layer comprise zinc yellow epoxy resin and conductive mica, wherein the mass ratio of the zinc yellow epoxy resin to the conductive mica is 1-2: 1;
the raw material of the middle layer comprises polyurethane and graphene; the mass ratio of the polyurethane to the graphene is 1-2: 1;
the raw materials of the surface layer comprise polyurethane fluorocarbon paint, graphene and nano zinc oxide; the mass ratio of the polyurethane fluorocarbon paint to the graphene and the nano zinc oxide is 1-2:0.5-1: 1.
A preparation method of a graphene anticorrosion-thermal control-antistatic integrated functional coating comprises the following steps:
(1) mixing the raw materials of the bottom layer, the silane coupling agent, the butyl acetate and the glass beads, stirring for 1-3h, filtering to remove the glass beads, adding the curing agent A, stirring and curing for 20-30min to obtain a bottom layer coating;
(2) mixing the raw material, the diluent and the glass beads of the middle layer, stirring for 1-3h, filtering to remove the glass beads, adding the curing agent B, stirring and curing for 20-30min to obtain a middle layer coating;
(3) mixing the raw materials of the surface layer, the diluent and the glass beads, stirring for 1-3h, filtering to remove the glass beads, adding the curing agent C, stirring and curing for 20-30min to obtain a surface layer coating;
(4) spraying the primer obtained in the step (1) on the surface of a spacecraft to obtain a primer, wherein the thickness of the single spraying is 15-20 mu m, the thickness of the obtained primer is 40-60 mu m, and the obtained primer is dried for 24-36h at room temperature;
(5) spraying the middle layer coating obtained in the step (2) on the surface of the base coating obtained in the step (4) to obtain a middle coating, wherein the thickness of single spraying is 15-20 mu m, and the sum of the thicknesses of the obtained base coating and the middle coating is 60-80 mu m; drying the intermediate coating at room temperature for 24-36 h;
(6) spraying the surface layer paint obtained in the step (3) on the surface of the intermediate coating obtained in the step (5) to obtain a surface coating, wherein the thickness of single spraying is 15-20 mu m, and the sum of the thicknesses of the obtained primer coating, the intermediate coating and the surface coating is 80-150 mu m; drying for 24-36h at room temperature after obtaining a surface coating;
(7) and curing the spacecraft with the bottom coating, the middle coating and the surface coating at the temperature of 80-150 ℃ for 1-3h to obtain the spacecraft with the graphene anti-corrosion-thermal control-anti-static integrated functional coating.
In the step (1), the purity of the conductive mica is more than 99%, the silane coupling agent is KH550, KH560 or the mixture of the two, and the butyl acetate is analytically pure; the curing agent A is at least one of triethylamine, triethylene tetramine and tetraethylene pentamine; the mass ratio of the zinc yellow epoxy resin to the conductive mica is 1-2:1, the mass ratio of the conductive mica to the silane coupling agent is 10:1-2, and the mass ratio of the zinc yellow epoxy resin to the butyl acetate and the glass beads is 1:10-15: 5-6; the mass ratio of the zinc yellow epoxy resin to the curing agent A is 1: 0.2-0.25; in the step (1), the stirring speed at the early stage is 1000r/min, and the stirring speed after the curing agent A is added is 600 r/min;
in the step (2), the diluent is one or a mixture of butyl acetate and xylene, and the curing agent B is an isocyanate curing agent; the mass ratio of the polyurethane to the graphene (in the raw material of the middle layer) is 1-2:1, and the mass ratio of the polyurethane to the diluent to the glass beads is 1:10-15: 5-8; the mass ratio of the polyurethane to the curing agent B is 1: 1-1.5; the early-stage stirring speed in the step (4) is 1000 r/min; the stirring speed is 600r/min after the curing agent is added.
The purity of the nano zinc oxide in the step (3) is more than 99%, the particle size of the nano zinc oxide is 0.5-0.8 mu m, the diluent is one or a mixture of butyl acetate and xylene, and the curing agent C adopts an isocyanate curing agent; the mass ratio of the polyurethane fluorocarbon paint to graphene (graphene in the raw materials of the surface layer) and the nano zinc oxide is 1-2:0.5-1:1, and the mass ratio of the polyurethane fluorocarbon paint to the diluent and the glass beads is 1:10-15: 5-8; the mass ratio of the polyurethane fluorocarbon paint to the curing agent is 1: 1-1.5; the early-stage stirring speed in the step (4) is 1000 r/min; the stirring speed is 600r/min after the curing agent is added.
Advantageous effects
(1) The invention designs a preparation method of an anticorrosion-thermal control-antistatic integrated functional coating. The coating adopts a three-layer composite structure, conductive mica and zinc yellow epoxy resin are used as a bottom anti-corrosion layer, modified graphene and polyurethane are used as a middle conductive layer, silicon, fluorine modified polyurethane, nano zinc oxide and modified graphene are used as a surface thermal control layer, and a spraying mode is adopted to prepare the multifunctional integrated coating which has excellent anti-corrosion, anti-static and thermal control performances. The coating has good bonding force with a base material and low curing temperature, and can be used for various types of aircrafts.
(2) The volume resistivity of the anti-corrosion-thermal control-antistatic integrated functional coating prepared by the invention is 1 multiplied by 106Ω·m～1×107Omega.m; the neutral salt spray corrosion resistance is more than or equal to 800 h; the damp and heat resistance is more than or equal to 240 h; the hemispherical emissivity of the coating is more than or equal to 0.90; under the condition of normal atmospheric pressure, the appearance is unchanged after 100 times of thermal cycles at the temperature of-196 ℃ (keeping for 2min) to 100 ℃ (keeping for 4min), the bonding force is intact, and the change of the hemispherical emissivity is less than or equal to 0.02.
(3) The preparation method of the anticorrosion-thermal control-antistatic integrated functional coating is provided, and a three-layer composite structure of an anticorrosion base coat, an antistatic intermediate coat and an antistatic thermal control coating is designed. The anticorrosive bottom layer of the composite coating consists of zinc yellow epoxy resin and conductive mica; the middle antistatic layer takes polyurethane as a binder and takes graphene as a main functional filler; the anti-static thermal control layer on the surface layer takes fluorine modified polyurethane as a binder, and graphene and nano zinc oxide filler are added to realize anti-static and thermal control performances.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
(1) Weighing 5g of zinc yellow epoxy resin (H06-2), 3.8g of conductive mica powder, 0.8g of silane coupling agent (KH550), 60g of butyl acetate and 25g of glass beads, mixing, and stirring for 3 hours at the rotating speed of 1000 r/min; filtering the obtained mixed solution to remove glass beads, adding 2g of triethylene tetramine, stirring and curing for 20min, wherein the rotating speed is 600 r/min;
(2) preparing a coating by adopting a spraying method, spraying for 1-2 times, and spraying for 15-20 mu m in a single time;
(3) mixing 5g of graphene, 10g of polyurethane (TS01-3), 100g of butyl acetate and 60g of glass beads, and stirring for 3 hours at the rotating speed of 1000 r/min; filtering the obtained mixed solution to remove glass beads, adding 11.2g of isocyanate curing agent (N3390), stirring and curing for 20min at the rotating speed of 600 r/min;
(4) spraying 3-4 times on the coating prepared in the step (2) by adopting a spraying method, wherein the spraying time is 15-20 mu m;
(5) mixing 5g of graphene, 10g of nano zinc oxide, 10g of polyurethane fluorocarbon paint, 150g of butyl acetate and 60g of glass beads, and stirring for 3 hours at the rotating speed of 1000 r/min; filtering the obtained mixed solution to remove glass beads, adding 11.2g of isocyanate curing agent (N3390), stirring and curing for 20min at the rotating speed of 600 r/min;
(6) spraying 3-4 times by a spraying method on the coating prepared in the step (4), wherein the spraying time is 15-20 mu m, and the total thickness of the coating is controlled to be 120 mu m;
(7) after drying at room temperature, curing for 3h at the temperature of 100 ℃ to obtain the anticorrosion-thermal control-antistatic integrated functional coating.
The specific technical indexes of the anticorrosive, thermal control and antistatic coating prepared by the embodiment are as follows: volume resistivity of 5.3X 106Omega.m; the coating does not foam and fall off under neutral salt spray corrosion for 800h and a damp and hot environment for 240 h; the hemispherical emissivity of the coating is 0.90; under the condition of normal atmospheric pressure, the appearance is unchanged after 100 times of thermal cycles at the temperature of-196 ℃ (keeping for 2min) to 100 ℃ (keeping for 4min), the bonding force is intact, and the change of the hemispherical emissivity is less than or equal to 0.02.
Example 2
(1) Weighing 5g of zinc yellow epoxy resin (H06-2), 5g of conductive mica powder, 0.5g of silane coupling agent (KH560), 0.5g of silane coupling agent (KH550), 85g of butyl acetate and 30g of glass beads, mixing, and stirring for 3H at the rotating speed of 1000 r/min; filtering the obtained mixed solution to remove glass beads, adding 1.8g of triethylene tetramine and 0.8g of tetraethylenepentamine, stirring and curing for 20min, wherein the rotating speed is 600 r/min;
(2) preparing a coating by adopting a spraying method, spraying for 1-2 times, and spraying for 15-20 mu m in a single time;
(3) mixing 8g of graphene, 10g of polyurethane (TS01-3), 120g of butyl acetate and 80g of glass beads, and stirring for 3 hours at the rotating speed of 1000 r/min; filtering the obtained mixed solution to remove glass beads, adding 12g of isocyanate curing agent (N3390), stirring and curing for 20min at the rotating speed of 600 r/min;
(4) spraying 3-4 times on the coating prepared in the step (2) by adopting a spraying method, wherein the spraying time is 15-20 mu m;
(5) mixing 10g of modified graphene, 10g of nano zinc oxide, 10g of polyurethane fluorocarbon paint, 150g of butyl acetate and 80g of glass beads, and stirring for 3 hours at the rotating speed of 1000 r/min; filtering the obtained mixed solution to remove glass beads, adding 13.5g of isocyanate curing agent (N3390), stirring and curing for 20min at the rotating speed of 600 r/min;
(6) spraying the coating prepared in the step (4) for 3-4 times by adopting a spraying method, wherein the spraying time is 15-20 mu m, and the total thickness of the coating is controlled to be 80-150 mu m;
(7) after drying at room temperature, curing for 3h at the temperature of 100 ℃ to obtain the anticorrosion-thermal control-antistatic integrated functional coating.
The specific technical indexes of the anticorrosive, thermal control and antistatic coating prepared by the embodiment are as follows: bulk resistivity of 1.5X 106Omega.m; the coating does not foam and fall off under neutral salt spray corrosion for 800h and a damp and hot environment for 240 h; the hemispherical emissivity of the coating is 0.91; under the condition of normal atmospheric pressure, the appearance is unchanged after 100 times of thermal cycles at the temperature of-196 ℃ (keeping for 2min) to 100 ℃ (keeping for 4min), the bonding force is intact, and the change of the hemispherical emissivity is less than or equal to 0.02.
Claims (6)
1. The graphene anticorrosion-thermal control-antistatic integrated functional coating is characterized in that: the coating comprises a bottom layer, a middle layer and a surface layer;
the preparation method of the graphene anticorrosion-thermal control-antistatic integrated functional coating comprises the following steps:
(1) mixing zinc yellow epoxy resin, conductive mica, a silane coupling agent, butyl acetate and glass beads, stirring, filtering to remove the glass beads, adding a curing agent A, stirring and curing to obtain a primer;
(2) mixing polyurethane, graphene, a diluent and glass beads, stirring, filtering to remove the glass beads, adding a curing agent B, stirring and curing to obtain a middle-layer coating;
(3) mixing polyurethane fluorocarbon paint, graphene, nano zinc oxide, a diluent and glass beads, stirring, filtering to remove the glass beads, adding a curing agent C, stirring and curing to obtain a surface coating;
(4) spraying the primer obtained in the step (1) on the surface of a spacecraft to obtain a primer, wherein the thickness of the single spraying is 15-20 mu m, the thickness of the obtained primer is 40-60 mu m, and the obtained primer is dried for 24-36h at room temperature;
(5) spraying the middle layer coating obtained in the step (2) on the surface of the base coating obtained in the step (4) to obtain a middle coating, wherein the thickness of single spraying is 15-20 mu m, and the sum of the thicknesses of the obtained base coating and the middle coating is 60-80 mu m; drying the intermediate coating at room temperature for 24-36 h;
(6) spraying the surface layer paint obtained in the step (3) on the surface of the intermediate coating obtained in the step (5) to obtain a surface coating, wherein the thickness of single spraying is 15-20 mu m, and the sum of the thicknesses of the obtained primer coating, the intermediate coating and the surface coating is 80-150 mu m; drying for 24-36h at room temperature after obtaining a surface coating;
(7) curing the spacecraft with the bottom coating, the middle coating and the surface coating at the temperature of 80-150 ℃ for 1-3h to obtain the spacecraft with the graphene anticorrosion-thermal control-antistatic integrated functional coating;
in the step (1), the curing agent A is at least one of triethylamine, triethylene tetramine and tetraethylene pentamine;
in the step (1), the mass ratio of the zinc yellow epoxy resin to the conductive mica is 1-2:1, the mass ratio of the conductive mica to the silane coupling agent is 10:1-2, and the mass ratio of the zinc yellow epoxy resin to the butyl acetate and the glass beads is 1:10-15: 5-6; the mass ratio of the zinc yellow epoxy resin to the curing agent A is 1: 0.2-0.25;
in the step (2), the curing agent B is an isocyanate curing agent; the mass ratio of the polyurethane to the graphene is 1-2:1, and the mass ratio of the polyurethane to the diluent to the glass beads is 1:10-15: 5-8; the mass ratio of the polyurethane to the curing agent B is 1: 1-1.5;
in the step (3), the purity of the nano zinc oxide is more than 99%, the particle size of the nano zinc oxide is 0.5-0.8 μm, the diluent is one or a mixture of butyl acetate and xylene, and the curing agent C adopts an isocyanate curing agent; the mass ratio of the polyurethane fluorocarbon paint to the graphene and the nano zinc oxide is 1-2:0.5-1:1, and the mass ratio of the polyurethane fluorocarbon paint to the diluent and the glass beads is 1:10-15: 5-8; the mass ratio of the polyurethane fluorocarbon paint to the curing agent C is 1: 1-1.5.
2. The graphene anticorrosion-thermal control-antistatic integrated functional coating as claimed in claim 1, wherein: in the step (1), butyl acetate is analytically pure; the purity of the conductive mica is more than 99 percent.
3. The graphene anticorrosion-thermal control-antistatic integrated functional coating as claimed in claim 1, wherein: in the step (1), the silane coupling agent is KH550, KH560 or a mixture of the two.
4. The graphene anticorrosion-thermal control-antistatic integrated functional coating as claimed in claim 1, wherein: in the step (1), the early-stage stirring speed is 1000r/min, and the stirring speed is 600r/min after the curing agent A is added.
5. The graphene anticorrosion-thermal control-antistatic integrated functional coating as claimed in claim 1, wherein: in the step (2), the diluent is one or a mixture of butyl acetate and xylene.
6. A preparation method of the graphene anticorrosion-thermal control-antistatic integrated functional coating as claimed in any one of claims 1 to 5, characterized in that the method comprises the following steps:
(1) mixing zinc yellow epoxy resin, conductive mica, a silane coupling agent, butyl acetate and glass beads, stirring, filtering to remove the glass beads, adding a curing agent A, stirring and curing to obtain a primer;
(2) mixing polyurethane, graphene, a diluent and glass beads, stirring, filtering to remove the glass beads, adding a curing agent B, stirring and curing to obtain a middle-layer coating;
(3) mixing polyurethane fluorocarbon paint, graphene, nano zinc oxide, a diluent and glass beads, stirring, filtering to remove the glass beads, adding a curing agent C, stirring and curing to obtain a surface coating;
(4) spraying the primer obtained in the step (1) on the surface of a spacecraft to obtain a primer, wherein the thickness of the single spraying is 15-20 mu m, the thickness of the obtained primer is 40-60 mu m, and the obtained primer is dried for 24-36h at room temperature;
(5) spraying the middle layer coating obtained in the step (2) on the surface of the base coating obtained in the step (4) to obtain a middle coating, wherein the thickness of single spraying is 15-20 mu m, and the sum of the thicknesses of the obtained base coating and the middle coating is 60-80 mu m; drying the intermediate coating at room temperature for 24-36 h;
(6) spraying the surface layer paint obtained in the step (3) on the surface of the intermediate coating obtained in the step (5) to obtain a surface coating, wherein the thickness of single spraying is 15-20 mu m, and the sum of the thicknesses of the obtained primer coating, the intermediate coating and the surface coating is 80-150 mu m; drying for 24-36h at room temperature after obtaining a surface coating;
(7) and curing the spacecraft with the bottom coating, the middle coating and the surface coating at the temperature of 80-150 ℃ for 1-3h to obtain the spacecraft with the graphene anti-corrosion-thermal control-anti-static integrated functional coating.
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