CN113004762A - Electromagnetic shielding coating - Google Patents
Electromagnetic shielding coating Download PDFInfo
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- CN113004762A CN113004762A CN201911317061.XA CN201911317061A CN113004762A CN 113004762 A CN113004762 A CN 113004762A CN 201911317061 A CN201911317061 A CN 201911317061A CN 113004762 A CN113004762 A CN 113004762A
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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
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- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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 invention relates to an electromagnetic shielding coating which is prepared from the following raw materials in parts by weight: 35-55 parts of resin, 30-60 parts of solvent, 10-25 parts of oxide in-situ modified graphene oxide and 1-10 parts of auxiliary agent; wherein the oxide is ferric oxide, and nickel oxide and/or cobalt oxide. The electromagnetic shielding coating has the advantages of good stability, difficult delamination or sedimentation, good electromagnetic shielding effect, low density, strong adhesive force, corrosion resistance, simple preparation process and convenient large-scale production and application.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to an electromagnetic shielding coating.
Background
With the development of science and technology, human beings have entered the electronic information age, and more electric and electronic devices have penetrated into every corner of society. The rapid development of the electronic, electrical, communication and information industries brings great convenience to the life and work of people, and brings invisible pollution, namely electromagnetic wave pollution, which not only causes serious interference to daily communication equipment, computers and other electronic systems of people and serious threat to information safety, but also brings immeasurable damage to human health. Electromagnetic radiation pollution has been classified as a fourth major environmental nuisance and the "united nations meeting of human environments" has placed electromagnetic radiation pollution as one of the major pollutants that must be controlled.
At present, electromagnetic shielding materials are widely used to prevent electromagnetic pollution, and can maximally block electromagnetic waves, so that targets are prevented from being interfered by the electromagnetic waves. The electromagnetic shielding paint combines an electromagnetic control technology and a paint production process, is applied to the civil field, becomes the most widely applied electromagnetic shielding material at home and abroad at present by the advantages of simple operation, convenient construction, lower cost and the like, and accounts for more than 70 percent of the whole shielding material. With the rapid development of modern high and new technologies and the improvement of human health quality, higher requirements are put forward on the performances of the electromagnetic shielding coating, such as absorption strength, corrosion resistance, density and the like. Therefore, research and development of novel electromagnetic shielding coatings have been the focus of extensive attention of researchers.
The traditional electromagnetic shielding coating mainly comprises a film-forming substance, a conductive filler, a diluent, an auxiliary agent and the like. The conductive filler is the most core component, and is usually a metal and metal-based composite material, usually silver powder, copper powder, nickel powder, silver-coated copper and the like, and the coating prepared from the conductive filler has the problems of easy environmental influence, such as attenuation or failure of shielding effectiveness, high density, high price, poor environmental adaptability, poor compatibility, poor stability and the like. In other documents, graphene, carbon nanotubes and the like are used as conductive fillers, or aniline is used for modifying the conductive fillers, but the problems of poor shielding efficiency, poor coating dispersibility, poor stability, easy delamination or sedimentation and the like are still not solved.
Disclosure of Invention
Based on this, there is a need to provide an electromagnetic shielding coating. The electromagnetic shielding coating has the advantages of good stability, difficult delamination or sedimentation, good electromagnetic shielding effect, low density, strong adhesive force, corrosion resistance, simple preparation process and convenient large-scale production and application.
The electromagnetic shielding coating is prepared from the following raw materials in parts by weight:
35-55 parts of resin,
30-60 parts of solvent,
10-25 parts of oxide in-situ modified graphene oxide, and
1-10 parts of an auxiliary agent;
wherein the oxide is ferric oxide, and nickel oxide and/or cobalt oxide.
In one embodiment, the preparation method of the iron oxide in-situ modified graphene oxide comprises the following steps:
(1) dissolving ferric chloride and nickel chloride and/or cobalt chloride in water, then adding graphene oxide, and dispersing;
(2) and (2) adjusting the reaction liquid obtained in the step (1) to be alkaline, adding a reducing agent to carry out reduction reaction, and collecting a solid product.
In one embodiment, the molar ratio of the oxide to the graphene oxide is 1: 0.4-1.
In one embodiment, the molar ratio of the ferric chloride to the nickel chloride and/or cobalt chloride is 1: 0.5-1.
In one embodiment, the reduction reaction is carried out under hydrothermal conditions at 100-200 ℃ for 15-42 hours.
In one embodiment, the solvent is a mixture of water and ethylene glycol.
In one embodiment, the resin is an epoxy resin; the aid comprises a polyethersulfone non-stick aid.
In one embodiment, the electromagnetic shielding coating comprises the following components in parts by weight of the raw materials:
1-3 parts of polyether sulfone non-stick auxiliary agent,
0.05 to 0.10 portion of defoaming agent,
0.1 to 0.15 portion of wetting agent,
2 to 5 parts of a dispersant, and
1-1.5 parts of a rheological additive.
In one embodiment, the dispersant is a polyamide-based dispersant.
In one embodiment, the defoamer is a mixture of mineral oil and silicone containing paraffin.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the oxide, namely iron oxide, and the nickel oxide and/or cobalt oxide in-situ modified graphene oxide are used as the conductive filler, and the weight parts of the raw material components are reasonably controlled, so that the prepared electromagnetic shielding coating has good stability, is not easy to delaminate or settle, has obviously reduced density, and has good electromagnetic shielding effect and strong adhesive force.
In addition, the electromagnetic shielding coating is low in raw material cost, easy to prepare and convenient for large-scale production and application.
Detailed Description
The electromagnetic shielding paint of the present invention will be described in further detail with reference to specific examples.
The invention provides an electromagnetic shielding coating which comprises the following components in parts by weight:
35-55 parts of resin,
30-60 parts of solvent,
0-25 parts of oxide in-situ modified graphene oxide (conductive filler), and
1-10 parts of an auxiliary agent;
wherein the oxide is ferric oxide, and nickel oxide and/or cobalt oxide.
Graphene oxide is a conductive material with good conductivity, a conductive network can be constructed in the coating to shield electromagnetic waves, but the graphene oxide serving as a conductive filler is very easy to agglomerate and precipitate in the coating, so that the excellent performance of the graphene cannot be fully exerted. According to the electromagnetic shielding coating, the surface of graphene is modified with iron oxide and nickel oxide and/or cobalt oxide, so that the conductive filler has the magnetic loss of the oxide and the electrical loss of graphene oxide, the electromagnetic shielding effect is greatly improved, more importantly, the oxide is used for coating the surface of graphene oxide, the dispersibility of graphene oxide can be improved, the storage stability of graphene oxide is improved, the excellent electromagnetic shielding effect of the conductive filler can be fully exerted by reasonably matching the weight parts of the raw material components, the good electromagnetic shielding effect is realized, compared with the traditional metal electromagnetic shielding coatings such as silver and copper, the surface density of the coating is greatly reduced, the electromagnetic shielding effect is stronger compared with the pure graphene electromagnetic shielding coating, and the formed coating has better mechanical property and weather resistance.
In one specific embodiment, the preparation method of the iron oxide in-situ modified graphite oxide comprises the following steps:
(1) dissolving ferric chloride and nickel chloride and/or cobalt chloride in water, then adding graphene oxide, and dispersing;
(2) and (2) adjusting the reaction liquid obtained in the step (1) to be alkaline, adding a reducing agent to carry out reduction reaction, and collecting a solid product.
The stable micro-nano conductive filler can be formed by using ferric chloride and nickel chloride and/or cobalt chloride to modify graphene oxide in situ, has stable performance and is not easy to settle, and can be reasonably compatible with other raw material components, so that the stability of the electromagnetic shielding coating can be optimized, and the lower areal density of the system can be kept.
In a specific embodiment, the molar ratio of the oxide to the graphene oxide is 1: 0.4-1.
In one specific embodiment, the molar ratio of the ferric chloride to the nickel chloride and/or cobalt chloride is 1: 0.5-1. Wherein, when nickel chloride and cobalt chloride are adopted simultaneously, the molar ratio between the nickel chloride and the cobalt chloride can be arbitrarily combined. More specifically, the molar ratio of nickel chloride to cobalt chloride is 2:0.8: 0.2.
In one embodiment, the reduction reaction is carried out under hydrothermal conditions at 100-200 ℃ for 15-42 hours. Preferably, the reduction reaction is carried out under hydrothermal conditions, the temperature is 140-160 ℃, and the time is 25-35 h.
Hydrothermal conditions are conditions of hydrothermal reaction, and hydrothermal reaction refers to a method for preparing a material by dissolving and recrystallizing powder in a sealed pressure vessel using water as a solvent. By reasonably controlling the temperature in the hydrothermal condition, specific iron oxide and the modification form of nickel oxide and/or cobalt oxide on graphene oxide can be formed, and the performance of the electromagnetic shielding coating is improved.
In one specific embodiment, the preparation method further comprises: drying the solid product under the following conditions: baking for 3-6 h at 75-85 ℃.
In one specific embodiment, the solvent is a mixture of water and ethylene glycol. The mixture of water and glycol is used as a solvent, which is beneficial to the full dispersion of the raw material components. More specifically, the volume ratio of the water to the glycol is 8-10: 1.
Further, in one particular embodiment, the resin is an epoxy resin; the aid comprises a polyethersulfone non-stick aid. By adopting the epoxy resin as the base resin, the dispersion of the conductive filler is facilitated, and meanwhile, the aging resistance is good, so that the electromagnetic shielding performance is better ensured. Meanwhile, the polyether sulfone non-stick auxiliary agent is matched and adopted, and the polyether sulfone non-stick auxiliary agent can be cooperated with the resin and the conductive filler to play a good self-cleaning capability, and can be applied to parts or occasions which are not easily contacted by workers, such as high towers and the interior of pipelines, so that the later maintenance cost of the coating can be reduced. More specifically, the epoxy resin is organosilicon modified waterborne epoxy resin.
It is understood that the auxiliary may further include one or more of a defoaming agent, a wetting agent, a dispersing agent, and a rheological auxiliary according to workability of the coating. When a plurality of auxiliary agents are adopted, the auxiliary agents can be added according to experience in the preparation process of the electromagnetic shielding coating.
In one specific embodiment, the auxiliary comprises the following components in parts by weight of the raw materials:
1-3 parts of polyether sulfone non-stick auxiliary agent,
0.05 to 0.10 portion of defoaming agent,
0.1 to 0.15 portion of wetting agent,
2 to 5 parts of a dispersant, and
1-1.5 parts of a rheological additive.
It should be noted that, the weight parts of the above-mentioned additives are the weight parts of the respective additives in the electromagnetic shielding coating, not the weight parts of the additives. That is, in the above specific embodiment, the electromagnetic shielding paint includes, by weight:
35-55 parts of resin,
30-60 parts of solvent,
10-25 parts of oxide in-situ modified graphene oxide, and
1-3 parts of polyether sulfone non-stick auxiliary agent,
0.05 to 0.10 portion of defoaming agent,
0.1 to 0.15 portion of wetting agent,
2 to 5 parts of a dispersant, and
1-1.5 parts of a rheological additive.
Preferably, the dispersant is a polyamide-based dispersant. The dispersing agent can form a stable double electric layer structure with hydroxyl on the surface of the oxide in-situ modified graphene oxide, so that the oxide in-situ modified graphene oxide can be stably dispersed in a solution, and the construction and storage stability of a coating is further ensured.
Preferably, the defoamer is a mixture of mineral oil containing paraffin and silicone. The defoaming agent is a defoaming agent which is universal for water and oil, can effectively reduce surface tension in a mixed solvent system, thereby eliminating foaming in the grinding and stirring processes, continuously inhibiting foaming in the system, being beneficial to reducing the defects of a coating obtained by construction and ensuring the conductivity and the electromagnetic shielding effect of the coating.
In addition, the preparation method of the electromagnetic shielding coating can comprise the following steps:
s1: adding the dispersing agent and the defoaming agent into the solvent, and stirring and mixing (for example, for 5min) to form a stable and uniform solution;
s2: adding the oxide in-situ modified graphene oxide under the stirring condition, and stirring and mixing (for example, 10min) to form a stable and uniform dispersion liquid;
s3: adding the resin, the wetting agent, the polyether sulfone non-stick additive and the rheological additive under the stirring condition, and dispersing at a high speed until the mixture is uniform, and has no powder balls and no caking (such as 2500 revolutions per minute and 5 minutes); grinding to ensure the fineness to be less than or equal to 15 μm (such as grinding for 1 hour by using a basket type sand mill with 2000 revolutions), and filling and sealing.
Before use, the construction viscosity can be adjusted by using a solvent according to requirements.
Hereinafter, specific examples are described, and the raw materials used in the examples are all commercially available unless otherwise specified.
The resin used in the examples is Doukang
RSN-6018 resin, which is an organosilicon modified epoxy resin;
the non-stick auxiliary agent is P628 polyether sulfone non-stick auxiliary agent in merck chemistry;
the defoaming agent is a bike chemical BYK-034 defoaming agent which is a mixture of mineral oil of paraffin, organic silicon and hydrophobic components;
the wetting agent is a core chemical F-40 base material wetting agent;
the dispersant is a core chemical polyamide dispersant S-3040 or a polycarboxylic acid type dispersant TY-5040;
the rheological additive is a Gekko chemical JCR-8935 thickener.
Example 1
The embodiment is an electromagnetic shielding coating, and the preparation method comprises the following steps:
(1) preparing the conductive filler: 0.001mol of FeCl3·6H2O，0.0005molNiCl2·6H2Dissolving O in 30mL of water to prepare a solution, adding 4mL of graphene oxide solution with the concentration of 10mg/mL, performing ultrasonic treatment for 30 minutes, adjusting the pH value to 10.5 by using sodium hydroxide solution (2M), and finally adding a reducing agent Na2S2O30.05 g; adding the solution into a 60mL polytetrafluoroethylene reaction kettleSealing and carrying out hydrothermal synthesis reaction for 30h at the temperature of 150 ℃ under the condition of no stirring; and collecting the solid product in a centrifuge tube, washing the sample with deionized water and ethanol respectively, separating with a high-speed centrifuge, repeatedly washing for three times, drying the washed and separated sample in an oven at 80 ℃ for 6 hours, and fully grinding the product into powder after drying is finished to obtain the conductive filler.
(2) Preparing the electromagnetic shielding coating: adding 4 parts of polyamide dispersant S-3040 and 0.1 part of defoaming agent into 36.8 parts of solvent, stirring and mixing for 5min to form a stable and uniform solution; adding 25.0 parts of conductive filler into water under the stirring condition, and stirring and mixing for 10min to form stable and uniform dispersion liquid; adding 30.0 parts of resin, 0.1 part of wetting agent, 3.0 parts of non-stick additive and 1.0 part of rheological additive into water under the condition of stirring, and dispersing at high speed for 5min until the mixture is uniform, free of powder balls and free of caking; grinding for 1 hour by basket type sand mill at 2000 rpm to ensure fineness of less than or equal to 15 μm, and filling and sealing.
Example 2
The embodiment is an electromagnetic shielding coating, and the preparation method comprises the following steps:
(1) preparing the conductive filler: 0.001mol of FeCl3·6H2O，0.0005molCoCl2·6H2Dissolving O in 30mL of water to prepare a solution, adding 4mL of graphene oxide solution with the concentration of 50mg/mL, performing ultrasonic treatment for 30 minutes, adjusting the pH to 10.5 by using sodium hydroxide solution (2M), and finally adding a reducing agent Na2S2O30.15 g; adding the solution into a 60mL polytetrafluoroethylene reaction kettle, sealing and carrying out hydrothermal synthesis reaction for 30h at the temperature of 150 ℃ under the condition of no stirring; and collecting the solid product in a centrifuge tube, washing the sample with deionized water and ethanol respectively, separating with a high-speed centrifuge, repeatedly washing for three times, drying the washed and separated sample in an oven at 80 ℃ for 6 hours, and fully grinding the product into powder after drying is finished to obtain the conductive filler.
(2) Preparing the electromagnetic shielding coating: adding 2 parts of polyamide dispersant S-3040 and 0.2 part of defoaming agent into 45.5 parts of solvent, stirring and mixing for 5min to form a stable and uniform solution; adding 10.0 parts of conductive filler into water under the stirring condition, and stirring and mixing for 10min to form stable and uniform dispersion liquid; adding 40.0 parts of resin, 0.3 part of wetting agent, 1.0 part of non-stick additive and 1.0 part of rheological additive into water under the condition of stirring, and dispersing at high speed for 5min until the mixture is uniform, free of powder balls and free of caking; grinding for 1 hour by basket type sand mill at 2000 rpm to ensure fineness of less than or equal to 15 μm, and filling and sealing. Before use, the construction viscosity can be adjusted by using a solvent according to requirements;
example 3
The embodiment is an electromagnetic shielding coating, and the preparation method comprises the following steps:
(1) preparing the conductive filler: 0.001mol of FeCl3·6H2O、0.0005molNiCl2·6H2O and 0.0005mol CoCl2·6H2O was dissolved in 30mL of water to prepare a solution. Adding 4mL of graphene oxide solution with the concentration of 25mg/mL, performing ultrasonic treatment for 30 minutes, adjusting the pH to 10.5 by using sodium hydroxide solution (2M), and finally adding a reducing agent Na2S2O30.10g, adding the solution into a 60mL polytetrafluoroethylene reaction kettle, sealing and carrying out hydrothermal synthesis reaction for 30h at the temperature of 150 ℃ without stirring; and collecting the solid product in a centrifuge tube, washing the sample with deionized water and ethanol respectively, separating with a high-speed centrifuge, repeatedly washing for three times, drying the washed and separated sample in an oven at 80 ℃ for 6 hours, and fully grinding the product into powder after drying is finished to obtain the conductive filler.
(2) Preparing the electromagnetic shielding coating: adding 3 parts of polyamide dispersant S-3040 and 0.15 part of defoaming agent into 42.65 parts of solvent, stirring and mixing for 5min to form a stable and uniform solution; adding 15.0 parts of conductive filler into water under the stirring condition, and stirring and mixing for 10min to form stable and uniform dispersion liquid; adding 35.0 parts of resin, 0.2 part of wetting agent, 2.0 parts of non-stick additive and 2.0 parts of rheological additive into water under the condition of stirring, and dispersing at high speed for 5min until the mixture is uniform, free of powder balls and free of caking; grinding for 1 hour by basket type sand mill at 2000 rpm to ensure fineness of less than or equal to 15 μm, and filling and sealing.
Example 4
The present embodiment is an electromagnetic shielding coating, and the preparation method thereof is the same as that of embodiment 1, except that: the temperature of the hydrothermal synthesis reaction is 200 ℃.
Specifically, the preparation method comprises the following steps:
(1) preparing the conductive filler: 0.001mol of FeCl3·6H2O，0.0005molNiCl2·6H2Dissolving O in 30mL of water to prepare a solution, adding 4mL of graphene oxide solution with the concentration of 10mg/mL, performing ultrasonic treatment for 30 minutes, adjusting the pH value to 10.5 by using sodium hydroxide solution (2M), and finally adding a reducing agent Na2S2O30.05 g; adding the solution into a 60mL polytetrafluoroethylene reaction kettle, sealing and carrying out hydrothermal synthesis reaction for 30h at 200 ℃ without stirring; and collecting the solid product in a centrifuge tube, washing the sample with deionized water and ethanol respectively, separating with a high-speed centrifuge, repeatedly washing for three times, drying the washed and separated sample in an oven at 80 ℃ for 3 hours, and fully grinding the product into powder after drying is finished to obtain the conductive filler.
(2) Preparing the electromagnetic shielding coating: adding 4 parts of polyamide dispersant S-3040 and 0.1 part of defoaming agent into 36.8 parts of solvent, stirring and mixing for 5min to form a stable and uniform solution; adding 25.0 parts of conductive filler into water under the stirring condition, and stirring and mixing for 10min to form stable and uniform dispersion liquid; adding 30.0 parts of resin, 0.1 part of wetting agent, 3.0 parts of non-stick additive and 1.0 part of rheological additive into water under the condition of stirring, and dispersing at high speed for 5min until the mixture is uniform, free of powder balls and free of caking; grinding for 1 hour by basket type sand mill at 2000 rpm to ensure fineness of less than or equal to 15 μm, and filling and sealing.
Example 5
The present embodiment is an electromagnetic shielding coating, and the preparation method thereof is the same as that of embodiment 1, except that: the resin was replaced with an acrylic resin.
Specifically, the preparation method comprises the following steps:
(1) preparing the conductive filler: 0.001mol of FeCl3·6H2O，0.0005molNiCl2·6H2Dissolving O in 30mL of water to prepare a solution, adding 4mL of graphene oxide solution with the concentration of 10mg/mL, performing ultrasonic treatment for 30 minutes, adjusting the pH value to 10.5 by using sodium hydroxide solution (2M), and finally adding a reducing agent Na2S2O30.05 g; adding the solution into a 60mL polytetrafluoroethylene reaction kettle, sealing and carrying out hydrothermal synthesis reaction for 30h at the temperature of 150 ℃ under the condition of no stirring; and collecting the solid product in a centrifuge tube, washing the sample with deionized water and ethanol respectively, separating with a high-speed centrifuge, repeatedly washing for three times, drying the washed and separated sample in an oven at 80 ℃ for 3 hours, and fully grinding the product into powder after drying is finished to obtain the conductive filler.
(2) Preparing the electromagnetic shielding coating: adding 4 parts of polyamide dispersant S-3040 and 0.1 part of defoaming agent into 36.8 parts of solvent, stirring and mixing for 5min to form a stable and uniform solution; adding 25.0 parts of conductive filler into water under the stirring condition, and stirring and mixing for 10min to form stable and uniform dispersion liquid; adding 30.0 parts of resin (acrylic resin), 0.1 part of wetting agent, 3.0 parts of non-stick additive and 1.0 part of rheological additive into water under the condition of stirring, and dispersing at high speed for 5min until the mixture is uniform, free of powder balls and free of caking; grinding for 1 hour by basket type sand mill at 2000 rpm to ensure fineness of less than or equal to 15 μm, and filling and sealing.
Example 6
The present embodiment is an electromagnetic shielding coating, and the preparation method thereof is the same as that of embodiment 1, except that: the non-stick auxiliary agent is replaced by fluorine-containing silicone oil.
Specifically, the preparation method comprises the following steps:
(1) preparing the conductive filler: 0.001mol of FeCl3·6H2O，0.0005molNiCl2·6H2Dissolving O in 30mL of water to prepare a solution, adding 4mL of graphene oxide solution with the concentration of 10mg/mL, performing ultrasonic treatment for 30 minutes, adjusting the pH value to 10.5 by using sodium hydroxide solution (2M), and finally adding a reducing agent Na2S2O30.05 g; adding the solution into a 60mL polytetrafluoroethylene reaction kettle, sealing and carrying out hydrothermal synthesis reaction for 30h at the temperature of 150 ℃ under the condition of no stirring; and collecting the solid product in a centrifuge tube, washing the sample with deionized water and ethanol respectively, separating with a high-speed centrifuge, repeatedly washing for three times, drying the washed and separated sample in an oven at 80 ℃ for 3 hours, and fully grinding the product into powder after drying is finished to obtain the conductive filler.
(2) Preparing the electromagnetic shielding coating: adding 4 parts of polyamide dispersant S-3040 and 0.1 part of defoaming agent into 36.8 parts of solvent, stirring and mixing for 5min to form a stable and uniform solution; adding 25.0 parts of conductive filler into water under the stirring condition, and stirring and mixing for 10min to form stable and uniform dispersion liquid; adding 30.0 parts of resin 0, 0.1 part of wetting agent, 3.0 parts of non-stick additive (fluorine-containing silicone oil) and 1.0 part of rheological additive into water under the condition of stirring, and dispersing at high speed for 5min until the mixture is uniform, free of powder balls and free of agglomeration; grinding for 1 hour by basket type sand mill at 2000 rpm to ensure fineness of less than or equal to 15 μm, and filling and sealing.
Example 7
The present embodiment is an electromagnetic shielding coating, and the preparation method thereof is the same as that of embodiment 1, except that: the polyamide dispersant S-3040 is replaced by a polycarboxylic acid type dispersant TY-5040.
Specifically, the preparation method comprises the following steps:
(1) preparing the conductive filler: 0.001mol of FeCl3·6H2O，0.0005molNiCl2·6H2Dissolving O in 30mL of water to prepare a solution, adding 4mL of graphene oxide solution with the concentration of 10mg/mL, performing ultrasonic treatment for 30 minutes, adjusting the pH value to 10.5 by using sodium hydroxide solution (2M), and finally adding a reducing agent Na2S2O30.05 g; adding the solution into a 60mL polytetrafluoroethylene reaction kettle, sealing and carrying out hydrothermal synthesis reaction for 30h at the temperature of 150 ℃ under the condition of no stirring; and collecting the solid product in a centrifuge tube, washing the sample with deionized water and ethanol respectively, separating with a high-speed centrifuge, repeatedly washing for three times, drying the washed and separated sample in an oven at 80 ℃ for 6 hours, and fully grinding the product into powder after drying is finished to obtain the conductive filler.
(2) Preparing the electromagnetic shielding coating: adding 4 parts of polycarboxylic acid type dispersing agent TY-5040 and 0.1 part of defoaming agent into 36.8 parts of solvent, stirring and mixing for 5min to form a stable and uniform solution; adding 25.0 parts of conductive filler into water under the stirring condition, and stirring and mixing for 10min to form stable and uniform dispersion liquid; adding 30.0 parts of resin, 0.1 part of wetting agent, 3.0 parts of non-stick additive and 1.0 part of rheological additive into water under the condition of stirring, and dispersing at high speed for 5min until the mixture is uniform, free of powder balls and free of caking; grinding for 1 hour by basket type sand mill at 2000 rpm to ensure fineness of less than or equal to 15 μm, and filling and sealing.
Comparative example 1
The comparative example is an electromagnetic shielding coating, and the preparation method is the same as that of example 1, except that: the conductive filler is replaced by 67 parts of iron oxide, 16 parts of nickel oxide and 17 parts of graphene oxide which have the same total mass and are physically blended.
Comparative example 2
The comparative example is an electromagnetic shielding coating, and the preparation method is the same as that of example 1, except that: the conductive filler is replaced by copper powder.
Comparative example 3
The comparative example is an electromagnetic shielding coating, and the preparation method is the same as that of example 1, except that: the conductive filler is replaced by graphene oxide.
The examples 1 to 7 and comparative examples 1 to 3 were subjected to performance tests:
(1) the test method comprises the following steps:
and (3) electromagnetic shielding test: electromagnetic shielding adopts a coaxial method to measure the electromagnetic shielding effectiveness of the material, and the GB/T6113-1995 refers to an original factory electromagnetic shielding effectiveness testing device: type DN 1015;
coating density test standard: GB/T6750-2007;
coating storage stability test standard: GB/T6753.3-1986;
coating adhesion test standard: GB/T5210-2006;
the artificial aging resistance test standard of the coating is as follows: GB/T1766-2008;
coating contact angle test standard: ASTM D7334-2008 (R2013).
(2) The test results are shown in table 1 below:
TABLE 1
As can be seen from table 1, the electromagnetic shielding coatings of examples 1 to 7 can achieve better storage stability and electromagnetic shielding effectiveness than the schemes of comparative examples 1 to 3 in which physical blending, metal powder or pure graphene oxide is used as a conductive filler, and have the advantages of low density, strong adhesion, good corrosion resistance, and excellent self-cleaning function.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The electromagnetic shielding coating is characterized by comprising the following components in parts by weight:
35-55 parts of resin,
30-60 parts of solvent,
10-25 parts of oxide in-situ modified graphene oxide, and
1-10 parts of an auxiliary agent;
wherein the oxide is ferric oxide, and nickel oxide and/or cobalt oxide.
2. The electromagnetic shielding coating of claim 1, wherein the preparation method of the iron oxide in-situ modified graphene oxide comprises the following steps:
(1) dissolving ferric chloride and nickel chloride and/or cobalt chloride in water, then adding graphene oxide, and dispersing;
(2) and (2) adjusting the reaction liquid obtained in the step (1) to be alkaline, adding a reducing agent to carry out reduction reaction, and collecting a solid product.
3. The electromagnetic shielding paint according to claim 2, wherein the molar ratio of the oxide to the graphene oxide is 1: 0.4-1.
4. The electromagnetic shielding paint according to claim 2, wherein the molar ratio of the ferric chloride to the nickel chloride and/or the cobalt chloride is 1: 0.5-1.
5. The electromagnetic shielding coating of claim 2, wherein the reduction reaction is carried out under hydrothermal conditions at a temperature of 100 to 200 ℃ for 15 to 42 hours.
6. The electro-magnetic shielding paint of claim 1, wherein the solvent is water or a mixture of water and an organic solvent.
7. The electro-magnetic shielding paint as claimed in any one of claims 1 to 6, wherein the resin is an epoxy resin; the aid comprises a polyethersulfone non-stick aid.
8. The electromagnetic shielding paint according to claim 7, wherein the auxiliary comprises the following components in parts by weight of the raw materials:
1-3 parts of polyether sulfone non-stick auxiliary agent,
0.05 to 0.10 portion of defoaming agent,
0.1 to 0.15 portion of wetting agent,
2 to 5 parts of a dispersant, and
1-1.5 parts of a rheological additive.
9. The electro-magnetic shielding coating of claim 8, wherein the dispersant is a polyamide-based dispersant.
10. The electro-magnetic shielding paint according to claim 8, wherein the defoaming agent is a mixture of mineral oil containing paraffin and silicone.
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| CN201911317061.XA CN113004762A (en) | 2019-12-19 | 2019-12-19 | Electromagnetic shielding coating |
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| CN201911317061.XA CN113004762A (en) | 2019-12-19 | 2019-12-19 | Electromagnetic shielding coating |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115746684A (en) * | 2022-11-28 | 2023-03-07 | 昆山汉品电子有限公司 | Anti-static high-shielding conductive material for screen film, preparation method of anti-static high-shielding conductive material and screen film |
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| CN109836975A (en) * | 2017-11-24 | 2019-06-04 | 洛阳尖端技术研究院 | A kind of corrosion-resistant conductive coating and its preparation method and application |
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| CN109836975A (en) * | 2017-11-24 | 2019-06-04 | 洛阳尖端技术研究院 | A kind of corrosion-resistant conductive coating and its preparation method and application |
| CN107892747A (en) * | 2017-12-05 | 2018-04-10 | 佛山市珀力玛高新材料有限公司 | Water-based non-stick polyether sulphone coating without perfluoro caprylic acid |
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