CN113698837B - Preparation method of single-component water-based hybrid electromagnetic shielding coating - Google Patents
Preparation method of single-component water-based hybrid electromagnetic shielding coating Download PDFInfo
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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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
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- 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
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
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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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
Abstract
The invention discloses a preparation method of a single-component aqueous hybrid electromagnetic shielding coating. And mixing the initiator with deionized water to obtain a catalyst solution. Adding deionized water, a buffering agent and an emulsifying agent into a reaction kettle according to the formula amount, introducing inert gas for protection, stirring for 20 minutes to 1 hour, then heating to 78 to 82 ℃, simultaneously dropwise adding a mixed monomer and a catalyst solution, finishing dripping within 2 to 3.5 hours, heating to 82 to 90 ℃, preserving heat for 2 to 3 hours, cooling, discharging, and obtaining the aqueous coating matrix resin emulsion. And adding the aqueous graphene dispersoid into the aqueous coating matrix resin emulsion in proportion to obtain the single-component aqueous hybrid electromagnetic shielding coating. The single-component water-based hybrid electromagnetic shielding coating prepared by the invention has excellent conductivity, electromagnetic shielding performance and corrosion resistance.
Description
Technical Field
The invention relates to a preparation method of a water-based hybrid electromagnetic shielding coating, which is a method for physically adding a functional filler by emulsion polymerization and belongs to the field of coating preparation.
Background
The epoxy resin has the advantages of excellent chemical corrosion resistance, excellent adhesion, low shrinkage rate, low price and the like, and is an excellent matrix of the electromagnetic shielding material. However, epoxy resin is brittle, and the hardness and corrosion resistance of the epoxy resin are reduced in the ordinary curing process, so that ideal physical and chemical properties can be obtained by structural modification. In general, the use of soft and hard monomers, thermoplastic polymers, synthetic rubbers, and nanomaterials to modify epoxy resins can achieve desirable properties. Graphene has a peculiar structure, good physical and chemical stability, special electronic properties, surface properties, adsorption characteristics and confinement effects, and is one of the electromagnetic shielding materials considered to be the most ideal by far. Researches on graphene-based electromagnetic shielding composite materials are very active, but the existing research work has two problems: on one hand, graphene is used as a filler, and the addition amount of the graphene is limited; and on the other hand, the graphene has poor dispersibility. A large amount of delocalized pi electrons exist on the surface of graphene, and the large amount of delocalized pi electrons can also adsorb molecules containing aromatic ring structures or molecules with strong pi electron conjugation through a pi-pi stacking effect. Theoretically, graphene has a complete structure, is inert on the surface, is easy to agglomerate, and is difficult to combine with a polymer, so that graphene functionalization is a key for solving the application bottleneck of the graphene.
The epoxy-acrylate hybrid polymer emulsion combines the advantages of epoxy resin and acrylate resin, has outstanding advantages in the field of practical application, and is an important emulsion type which is always concerned by academia and industry. However, the poor stability of the epoxy-acrylate hybrid emulsion has been a pain point in the industry and a research hotspot in academia.
Although much research is currently done on electromagnetic shielding coatings, it is mainly directed to solvent-based coatings. Compared with solvent-based coatings, the technical defects of water resistance, corrosion resistance and electric conductivity of the existing waterborne electromagnetic shielding coatings are not effectively solved.
Disclosure of Invention
The invention aims to provide a preparation method of a single-component water-based hybrid electromagnetic shielding coating aiming at the defects of the prior art, so as to solve the technical defects of water-based electromagnetic shielding coatings in the aspects of water resistance, corrosion resistance and conductivity.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a single-component water-based hybrid electromagnetic shielding coating is characterized by comprising the following steps: the method comprises the following steps:
a step of preparing a mixed monomer and a step of preparing a catalyst solution; the mixed monomer comprises epoxy resin, silane coupling agent modified aqueous graphene dispersoid and acrylic monomer;
adding deionized water, a buffering agent and a surfactant into a reaction kettle, introducing inert gas for protection, heating to a dropwise adding temperature, dropwise adding the mixed monomer and a catalyst solution, heating to a reaction temperature after dropwise adding, carrying out heat preservation reaction, cooling after the reaction is finished to obtain a water-based paint matrix resin emulsion, and adding a water-based graphene dispersion into the water-based paint matrix resin emulsion in proportion to obtain the single-component water-based hybrid electromagnetic shielding paint.
Preferably, the epoxy resin is: e51, E44 or a mixture of E51 and E44, etc.
The catalyst solution is deionized water solution of initiator; preferably, the initiator is potassium persulfate, ammonium persulfate or a mixture of potassium persulfate and ammonium persulfate.
The surfactant can be used as an emulsifier: a complex product of one or more than two surfactants of an anionic surfactant, a cationic surfactant, a reactive surfactant, an amphoteric surfactant and a neutral surfactant.
Preferably, the surfactants are: sodium vinyl sulfonate surfactant.
Further, in the step of preparing the mixed monomer, the epoxy resin, the silane coupling agent modified aqueous graphene dispersion and the acrylic monomer are added into a four-neck flask according to a set proportion, and the mixture is uniformly stirred to obtain the mixed monomer.
Further, the initial stability is to 78-82 ℃ and the reaction temperature is 82-90 ℃.
The single-component water-based hybrid electromagnetic shielding coating prepared by the preparation method has the square resistance value of 5-200k omega/\9633underthe condition of the film thickness of 30 micrometers. The total addition amount of the aqueous graphene dispersion in the prepared single-component aqueous hybrid electromagnetic shielding coating is 5-50%.
The invention has the beneficial effects that: 1. according to the invention, graphene and acrylic monomers can be grafted and copolymerized on epoxy resin, and the high hardness, the corrosion resistance and the conductivity of the hybrid resin are realized by adding the aqueous graphene dispersoid in combination with physical mixing. The sodium vinyl sulfonate in the invention overcomes the defects of the traditional non-reactive emulsifier, is a reactant of emulsion polymerization on one hand, and is an emulsifier of synthetic resin on the other hand, so that the synthesized product has better water solubility and water resistance, and the synthetic resin has outstanding water-based and water-resistant properties.
According to the invention, the addition amount of graphene is greatly increased by a method of combining synthesis copolymerization and physical addition, the defects of poor stability and the like of an epoxy-acrylate hybrid polymer emulsion are solved by optimizing synthesis conditions, and the single-component water-based graphene/epoxy acrylic acid electromagnetic shielding coating with excellent performance is prepared, and has the characteristics of high hardness, good water resistance, excellent corrosion resistance, good conductivity and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 shows the IR spectrum of the one-component aqueous hybrid electromagnetic shielding coating prepared in example 1. It can be seen that a certain amount of epoxy groups are present in the emulsion.
Fig. 3-1 and 3-2 are the micro-morphologies of the surface and the interface of the one-component aqueous hybrid electromagnetic shielding coating prepared in example 1, respectively. The graphene lamellar structure is evident from the figure.
Detailed Description
The preparation method of the single-component water-based hybrid electromagnetic shielding coating is described in detail below with reference to the examples.
Example 1:
a single-component water-based hybrid electromagnetic shielding coating adopts an emulsion synthesis method and comprises the following specific steps:
(1) Adding 25 parts by weight of epoxy resin, 10 parts by weight of silane coupling agent modified aqueous graphene dispersoid and 65 parts by weight of acrylic monomer into a four-neck flask, and uniformly stirring to obtain a mixed monomer;
(2) 1.5 parts by weight of initiator was mixed with 20 parts of deionized water to obtain a catalyst solution.
(3) Adding 100 parts by weight of deionized water, 6 parts by weight of buffering agent and 1.5 parts by weight of emulsifying agent into a reaction kettle, introducing nitrogen for protection, stirring for 20 minutes to 1 hour, heating to 78 to 82 ℃, simultaneously dropwise adding the mixed monomer and the catalyst solution, completing dripping within 2 to 3.5 hours, heating to 82 to 90 ℃, preserving heat for 2 to 3 hours, cooling, and discharging to obtain the aqueous coating matrix resin emulsion.
And adding the aqueous graphene dispersoid into the aqueous coating matrix resin emulsion, wherein the addition amount is 50 mass percent of the aqueous coating matrix resin emulsion, so as to obtain the one-component aqueous hybrid electromagnetic shielding coating, and the aqueous graphene dispersoid is a commercially available product. The main properties of the coating (film thickness 30 microns) are: adhesion rating of 0, water resistance of 25 ℃ for 7 days without abnormality, 3.5% NaCl resistance with brine at 25 ℃ for 7 days without abnormality, hardness of 3-4H, impact resistance of 50cm pass, flexibility of T bend of 2mm pass, conductivity: the square resistance value is 5k omega/\9633.
Comparative example 1:
a single-component water-based hybrid electromagnetic shielding coating adopts an emulsion synthesis method and comprises the following specific steps:
(1) Adding 25 parts by weight of epoxy resin, 10 parts by weight of silane coupling agent modified aqueous graphene dispersoid and 65 parts by weight of acrylic monomer into a four-neck flask, and uniformly stirring to obtain a mixed monomer;
(2) 1.5 parts by weight of initiator was mixed with 20 parts of deionized water to obtain a catalyst solution.
(3) Adding 100 parts by weight of deionized water, 6 parts by weight of buffering agent and 1.5 parts by weight of emulsifying agent into a reaction kettle, introducing nitrogen for protection, stirring for 20 minutes to 1 hour, then heating to 78 to 82 ℃, simultaneously dropwise adding a mixed monomer and a catalyst solution, completing dripping within 2 to 3.5 hours, heating to 82 to 90 ℃, preserving heat for 2 to 3 hours, cooling, discharging, and obtaining the aqueous coating matrix resin emulsion.
And adding the aqueous graphene dispersoid into the aqueous coating matrix resin emulsion, wherein the adding amount is 25 mass percent of the aqueous coating matrix resin emulsion, so as to obtain the one-component aqueous hybrid electromagnetic shielding coating, and the aqueous graphene dispersoid is a commercially available product. The main properties of the coating (film thickness 30 microns) are: adhesion rating 0, water resistance no anomaly for 7 days at 25 ℃, resistance to 3.5% NaCl brine, slight whitening for 7 days at 25 ℃, hardness 4H, impact resistance 50cm pass, flexibility T bend 2mm pass, conductivity: the square resistance value is 100k omega/\9633.
Comparative example 2:
a single-component water-based hybrid electromagnetic shielding coating adopts an emulsion synthesis method and comprises the following specific steps:
(1) Adding 25 parts by weight of epoxy resin, 10 parts by weight of silane coupling agent modified aqueous graphene dispersoid and 65 parts by weight of acrylic monomer into a four-neck flask, and uniformly stirring to obtain a mixed monomer;
(2) 1.5 parts by weight of initiator was mixed with 20 parts of deionized water to obtain a catalyst solution.
(3) Adding 100 parts by weight of deionized water, 6 parts by weight of buffering agent and 1.5 parts by weight of emulsifier into a reaction kettle, introducing nitrogen for protection, stirring for 20 minutes to 1 hour, then heating to 78 to 82 ℃, simultaneously dropwise adding a mixed monomer and a catalyst solution, finishing dripping within 2 to 3.5 hours, heating to 82 to 90 ℃, preserving heat for 2 to 3 hours, cooling, discharging to obtain a water-based paint matrix resin single-component emulsion, and directly using the water-based paint matrix resin single-component emulsion as a water-based hybrid electromagnetic shielding paint without adding a water-based graphene dispersion. The main properties of the coating (film thickness 30 microns) are: adhesion rating of 0, water resistance of 7 days mild whitening without abnormality at 25 ℃, 3.5% resistance of NaCl brine of 25 ℃ for 7 days obvious whitening, hardness of 2-3H, impact resistance of 50cm pass, flexibility of T bend of 2mm pass, conductivity: the square resistance value is out of range (very poor conductivity).
Comparative example 3:
a single-component water-based hybrid electromagnetic shielding coating adopts an emulsion synthesis method and comprises the following specific steps:
(1) Adding 25 parts by weight of epoxy resin and 65 parts by weight of acrylic monomer into a four-neck flask, and uniformly stirring to obtain a mixed monomer;
(2) 1.5 parts by weight of initiator was mixed with 20 parts of deionized water to obtain a catalyst solution.
(3) Adding 100 parts by weight of deionized water, 6 parts by weight of buffering agent and 1.5 parts by weight of emulsifying agent into a reaction kettle, introducing nitrogen for protection, stirring for 20 minutes to 1 hour, then heating to 78 to 82 ℃, simultaneously dropwise adding a mixed monomer and a catalyst solution, completing dripping within 2 to 3.5 hours, heating to 82 to 90 ℃, preserving heat for 2 to 3 hours, cooling, discharging, and obtaining the aqueous coating matrix resin emulsion.
And adding the aqueous graphene dispersoid into the aqueous coating matrix resin emulsion, wherein the adding amount is 50 mass percent of the aqueous coating matrix resin emulsion, so as to obtain the single-component aqueous hybrid electromagnetic shielding coating, and the aqueous graphene dispersoid is a commercially available product. And adding aqueous graphene dispersoid which accounts for 50 percent of the matrix resin emulsion to obtain the single-component aqueous hybrid electromagnetic shielding coating. The main properties of the coating (film thickness 30 microns) are: adhesion level 0, water resistance of 25 ℃ for 7 days without abnormality, 3.5% NaCl brine resistance of 25 ℃ for 7 days without abnormality, hardness of 3-4H, impact resistance of 50cm pass, flexibility T bend of 2mm pass, conductivity: the square resistance value is 11k omega/9633g.
And (4) conclusion: the single-component water-based hybrid electromagnetic shielding coating prepared by the preparation method has the square resistance value of 5-200k omega/\9633underthe condition that the film thickness is 30 micrometers. The total addition amount of the aqueous graphene dispersion in the prepared single-component aqueous hybrid electromagnetic shielding coating is 5-50%. According to the invention, graphene and acrylic monomers can be grafted and copolymerized on epoxy resin, and the high hardness, the corrosion resistance and the conductivity of the hybrid resin are realized by adding the aqueous graphene dispersoid in combination with physical mixing.
Claims (1)
1. A preparation method of a single-component water-based hybrid electromagnetic shielding coating is characterized by comprising the following steps: the method comprises the following specific steps:
(1) Adding 25 parts by weight of epoxy resin, 10 parts by weight of silane coupling agent modified aqueous graphene dispersion and 65 parts by weight of acrylic monomer into a four-neck flask, and uniformly stirring to obtain a mixed monomer;
(2) Mixing 1.5 parts by weight of initiator and 20 parts by weight of deionized water to obtain a catalyst solution;
(3) Adding 100 parts by weight of deionized water, 6 parts by weight of buffering agent and 1.5 parts by weight of surfactant into a reaction kettle, introducing nitrogen for protection, stirring for 20 minutes to 1 hour, heating to 78 to 82 ℃, simultaneously dropwise adding a mixed monomer and a catalyst solution, completing dripping within 2 to 3.5 hours, heating to 82 to 90 ℃, preserving heat for 2 to 3 hours, cooling, discharging, and obtaining a water-based paint matrix resin emulsion;
the addition amount of the water-based graphene is 50 mass percent of the water-based paint matrix resin emulsion;
the surfactant is as follows: sodium vinyl sulfonate; the epoxy resin is E51, E44 or a mixture of E51 and E44; the catalyst solution is deionized water solution of initiator; the initiator is potassium persulfate, ammonium persulfate or a mixture of the potassium persulfate and the ammonium persulfate;
the prepared single-component water-based hybrid electromagnetic shielding coating has the square resistance value of 5k omega/\ 9633under the condition that the film thickness is 30 micrometers.
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| CN107353773B (en) * | 2017-07-14 | 2021-08-31 | 湖南沃特邦恩新材料有限公司 | Graphene-containing waterborne epoxy anticorrosive paint and preparation method and application thereof |
| CN109554055B (en) * | 2018-08-21 | 2020-09-04 | 成都虹润制漆有限公司 | Aqueous thick-coating type aqueous acrylic acid hybrid epoxy floor paint and preparation method thereof |
| CN110054965B (en) * | 2019-04-23 | 2020-07-28 | 华南理工大学 | Modified graphene oxide co-cured waterborne epoxy resin coating and preparation method thereof |
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| CN110776802A (en) * | 2019-12-02 | 2020-02-11 | 湖南太子化工涂料有限公司 | Epoxy modified acrylic acid environment-friendly paint for hardware parts and preparation method thereof |
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