CN112126268A - Preparation method of water-based graphene slurry for electromagnetic shielding coating - Google Patents
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Abstract
The electromagnetic shielding coating aims at the problems that the graphene oxide is too expensive, the graphene powder and the nano ferrite are not uniformly dispersed in the formula, and the graphene powder with chemical inertia is not easy to be chemically compounded with other materials. The invention provides a preparation method of aqueous graphene slurry for an electromagnetic shielding coating, which is characterized in that an active carbon layer is formed on the surface of graphene by chemically treating graphene powder, and ferroferric oxide nano particles uniformly grow on the surface of the graphene to form pretreated graphene, so that the electromagnetic shielding performance of the graphene is improved.
Description
Technical Field
The invention relates to the field of preparation of graphene slurry, and particularly relates to a preparation method of aqueous graphene slurry for an electromagnetic shielding coating.
Background
Electromagnetic waves are shocking particle waves which are derived and emitted in space by electric and magnetic fields which are in the same direction and perpendicular to each other, and are a form of energy propagating in space, which is also called electromagnetic radiation. Electromagnetic radiation cannot be seen or discovered, most of devices generating the electromagnetic radiation are common electrical appliances in daily life, such as mobile phones, electric blankets, electromagnetic ovens, medical instruments, electronic instruments and the like, and electromagnetic waves with various wavelength frequencies generated when high-voltage transmission lines, communication base stations, broadcast televisions and the like work fill spaces, and when the intensity of the electromagnetic radiation exceeds the limit which can be borne by a human body or can be allowed by instruments and devices, electromagnetic pollution is generated.
The graphene is a two-dimensional plane structure formed by single-layer carbon atoms, has excellent physical properties such as high thermal conductivity, high strength, high visible light transmittance, high specific surface area and extremely low resistivity, and has the characteristics of chemical inertness and the like, so that the graphene has potential application in the fields of energy storage, heat conduction, electric conduction, electromagnetic shielding and the like. Aiming at the fields of application of graphene in lithium batteries, supercapacitors, heat-conducting coatings, anticorrosive coatings and the like, the problems of graphene agglomeration and non-uniform dispersion can occur when graphene is directly added into an application formula. Generally, graphene needs to be dispersed in a solvent in advance to prepare a slurry, and then the slurry is added into an application formula. Although the conductivity of graphene is excellent, more insulating polymer materials such as polymethyl pyrrolidone are often added to prepare aqueous slurry from graphene, which affects the conductivity of graphene, for example, chinese patent CN105895870A discloses a high-concentration and high-purity graphene slurry, a preparation method and an application thereof, and the content of the anti-aliasing cleavage assistant is 0.1-20% (one or a combination of organic components such as polyvinyl chloride and polyethylene). Due to the chemical inertia of graphene, the electromagnetic shielding performance of graphene is improved, and graphene oxide is generally adopted to compound some ferrite materials. For example, chinese patents CN108251053A, CN103641488B, etc. adopt graphene oxide and nano ferrite to be compounded, and then reduce graphene for electromagnetic shielding. After the graphite oxide is reduced, the defect exists, the electric conductivity is reduced, the price of the graphene oxide in the market is high, the selling price of 1g of the graphene oxide is about 900 yuan, and the price is far higher than that of graphene powder (1-2 yuan/g). If the graphene and the nano ferrite material are directly mixed, the phenomenon that the graphene loads the nano ferrite material unevenly occurs, the nano material is easy to agglomerate and is not easy to disperse evenly, and the electromagnetic shielding effect is affected. Therefore, the graphene powder is directly compounded with the uniform ferrite material, and the method has great significance.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to provide a preparation method of an aqueous graphene slurry for an electromagnetic shielding coating.
In order to achieve the purpose, the invention discloses a preparation method of aqueous graphene slurry for an electromagnetic shielding coating, which comprises the following steps:
a, dispersing graphene powder, glucose and polyethylene glycol in water according to a mass ratio of 1-4: 6:0.1, and fully stirring to obtain a solution A with the graphene content of 1-4 wt%;
b, mixing ferrous salt and ferric salt according to a mass ratio of 1:1, dissolving in water to obtain a B solution with the total iron salt content of 1-4 wt%;
c, adding a certain amount of the solution B into the solution A, stirring, heating to 40 ℃ after 10 minutes, adding a certain amount of catalyst, and continuously stirring for 10 minutes to obtain solution C;
d, sealing the solution C, keeping the temperature for a period of time at a certain temperature, cooling, centrifuging and washing with deionized water for multiple times until the conductivity of the supernatant is less than 12us/cm, and drying the precipitate in an oven at 80 ℃ for 12 hours to obtain pretreated graphene powder;
and E, dispersing 1-4 parts of the pretreated graphene powder and 0.2-0.4 part of polyvinylpyrrolidone in water, transferring the mixture into a sand mill, adding 0.1-0.2 part of stabilizer after sand milling for 6 hours, and uniformly stirring to obtain the water-based graphene slurry for the electromagnetic shielding paint.
The graphene powder is specifically liquid-phase-stripped graphene powder, the content of surface functional groups is less than 0.1wt%, and the thickness is 0.35-1 nm; the size is 1-15 microns.
Wherein the ferrous salt is one or more of ferrous sulfate, ferrous nitrate, ferrous chloride and potassium ferrocyanide.
Wherein the ferric salt is one or a combination of ferric chloride, ferric sulfate and ferric nitrate.
Adding a certain amount of liquid B into liquid A, wherein the mass ratio of the content of graphene powder in the liquid A to the total mass of ferric salt in the liquid B is 1:1 to 2.
Wherein the catalyst is boric acid or borate, and accounts for 0.3% of the mass fraction of the solution C.
Wherein the temperature under the closed condition is 60-180 ℃, and the heat preservation time is 1-24 hours.
Wherein the stabilizer is prepared from hydroxymethyl cellulose and polyaniline in a mass ratio of 1: 5 compounded mixture.
The electromagnetic shielding coating aims at the problems that the graphene oxide is too expensive, the graphene powder and the nano ferrite are not uniformly dispersed in the formula, and the graphene powder with chemical inertia is not easy to be chemically compounded with other materials. According to the method, graphene powder is chemically treated, an activated carbon layer is formed on the surface of graphene, and ferroferric oxide nano particles grow on the surface of the activated carbon layer to form pretreated graphene; the invention relates to a method for preparing polyaniline/hydroxymethyl cellulose composite material, which comprises the following steps of mixing conductive polymer polyaniline and hydroxymethyl cellulose according to the mass ratio of 1: and 5, compounding is carried out, so that the using amount of the insulating material is greatly reduced, and the insulating material is added into the electromagnetic shielding coating, so that the graphene can be mutually connected to form a conductive path, and the electromagnetic shielding performance of the graphene is improved. The aqueous graphene slurry prepared by the invention is used for the electromagnetic shielding coating, can solve the problem of uneven addition of graphene powder, reduces the cost of adding an auxiliary agent into the coating, is more uniform in compounding with the nano ferrite, and improves the electromagnetic shielding performance of the coating.
Drawings
Fig. 1 is a TEM image of graphene powder in example 1 of the present invention.
Fig. 2 is a TEM image of the pretreated graphene of example 1 of the present invention.
Fig. 3 is a TEM image of comparative example 1 graphene of the present invention.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention without limiting its scope. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available.
Example 1
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 2 parts of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 1 part of ferric chloride and 1 part of ferrous chloride are dissolved in water to obtain a B solution with the total ferric salt content of 2 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 120 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 4 parts of pretreated graphene and 0.2 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.1 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding.
The drawings illustrate: a transmission electron microscope JEM2100 is used to obtain a transmission electron microscope image of the graphene, and fig. 1 shows that before pretreatment, the surface of the graphene is free of other particles in the TEM; FIG. 2 is a TEM of pretreated graphene, and nano ferroferric oxide particles are uniformly distributed on the surface of the pretreated graphene; the viscosity of the aqueous graphene slurry was measured to be 1200 mPa · s with a digital viscometer SNB-2.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK190 (German Bike) 0.5 parts
Leveling agent MOK-2017 (German Merck chemical) 0.5 part
Defoaming agent BYK024 (German bike) 1 portion.
Firstly, uniformly shearing and mixing water-based acrylic resin, water-based graphene slurry, cyanote 325 amino resin, a dispersing agent and a flatting agent at a high speed, then adding a defoaming agent BYK024, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 1.0S/cm, and the maximum value of the electromagnetic shielding effectiveness is 32dB (1 GHz-20 GHz).
Comparative example 1
Dispersing 4 parts of graphene powder, 1 part of nano ferroferric oxide (the average particle size is 30 nm) and 0.2 part of polyvinylpyrrolidone in water, and sanding for 6 hours by using a sand mill to obtain the aqueous graphene slurry. A transmission electron microscope JEM2100 is adopted to obtain a transmission electron microscope image of graphene, and how to show in FIG. 3, nano ferroferric oxide on the surface of the graphene is seriously adhered and is unevenly distributed on the surface of the graphene.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing the water-based acrylic resin, the water-based graphene slurry, the cyanote 325 amino resin, the dispersing agent and the flatting agent at a high speed, then adding the defoaming agent, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 0.05S/cm, and the maximum value of the electromagnetic shielding effectiveness is 10dB (1 GHz-20 GHz).
Example 2
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 1 part of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 1 part of ferric chloride and 1 part of ferrous chloride are dissolved in water to obtain a B solution with the total ferric salt content of 2 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 120 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 4 parts of pretreated graphene and 0.2 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.1 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding, wherein the viscosity of the aqueous graphene slurry is 1120 mPa & s.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing the water-based acrylic resin, the water-based graphene slurry, the cyanote 325 amino resin, the dispersing agent and the flatting agent at a high speed, then adding the defoaming agent, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 0.8S/cm, and the maximum value of the electromagnetic shielding effectiveness is 26dB (1 GHz-20 GHz).
Example 3
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 1 part of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 1 part of ferric chloride and 1 part of ferrous chloride are dissolved in water to obtain a B solution with the total ferric salt content of 2 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 120 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 1 part of pretreated graphene and 0.2 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.1 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding, wherein the viscosity of the aqueous graphene slurry is 606 mPa & s.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing water-based acrylic resin, water-based graphene slurry, cyanote 325 amino resin, a dispersing agent and a flatting agent at a high speed, then adding a defoaming agent BYK024, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 0.5S/cm, and the maximum value of the electromagnetic shielding effectiveness is 21dB (1 GHz-20 GHz).
Example 4
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 1 part of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 2 parts of ferric chloride and 2 parts of ferrous chloride are dissolved in water to obtain a B solution with the total ferric salt content of 4 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 120 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 1 part of pretreated graphene and 0.2 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.1 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding, wherein the viscosity of the aqueous graphene slurry is 482 mPa & s.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing the water-based acrylic resin, the water-based graphene slurry, the cyanote 325 amino resin, the dispersing agent and the flatting agent at a high speed, then adding the defoaming agent, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 0.2S/cm, and the maximum value of the electromagnetic shielding effectiveness is 15dB (1 GHz-20 GHz).
Example 5
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 2 parts of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 2 parts of ferric chloride and 2 parts of ferrous chloride are dissolved in water to obtain a B solution with the total ferric salt content of 4 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 120 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 1 part of pretreated graphene and 0.2 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.1 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding, wherein the viscosity of the aqueous graphene slurry is 753 mPa & s.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing water-based acrylic resin, water-based graphene slurry, cyanote 325 amino resin, a dispersing agent and a flatting agent at a high speed, then adding a defoaming agent BYK024, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 0.6S/cm, and the maximum value of the electromagnetic shielding effectiveness is 23dB (1 GHz-20 GHz).
Example 6
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 2 parts of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 2 parts of ferric chloride and 2 parts of ferrous chloride are dissolved in water to obtain a B solution with the total ferric salt content of 4 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 120 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 1 part of pretreated graphene and 0.4 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.1 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding, wherein the viscosity of the aqueous graphene slurry is 936 mPa & s.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing the water-based acrylic resin, the water-based graphene slurry, the cyanote 325 amino resin, the dispersing agent and the flatting agent at a high speed, then adding the defoaming agent, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 0.1S/cm, and the maximum value of the electromagnetic shielding effectiveness is 12dB (1 GHz-20 GHz).
Example 7
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 2 parts of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 2 parts of ferric chloride and 2 parts of ferrous chloride are dissolved in water to obtain a B solution with the total ferric salt content of 4 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 60 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 1 part of pretreated graphene and 0.4 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.1 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding, wherein the viscosity of the aqueous graphene slurry is 1264 mPa & s.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing the water-based acrylic resin, the water-based graphene slurry, the cyanote 325 amino resin, the dispersing agent and the flatting agent at a high speed, then adding the defoaming agent, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 0.01S/cm, and the maximum value of the electromagnetic shielding effectiveness is 6dB (1 GHz-20 GHz).
Example 8
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 2 parts of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 2 parts of ferric chloride and 2 parts of ferrous chloride are dissolved in water to obtain a B solution with the total ferric salt content of 4 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 180 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 4 parts of pretreated graphene and 0.4 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.1 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding, wherein the viscosity of the aqueous graphene slurry is 1140 mPa & s.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing the water-based acrylic resin, the water-based graphene slurry, the cyanote 325 amino resin, the dispersing agent and the flatting agent at a high speed, then adding the defoaming agent, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 0.9S/cm, and the maximum value of the electromagnetic shielding effectiveness is 22dB (1 GHz-20 GHz).
Example 9
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 2 parts of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 2 parts of ferric chloride and 2 parts of ferrous chloride are dissolved in water to obtain a B solution with the total ferric salt content of 4 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 180 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 4 parts of pretreated graphene and 0.4 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.2 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding, wherein the viscosity of the aqueous graphene slurry is 1640 mPa & s.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing the water-based acrylic resin, the water-based graphene slurry, the cyanote 325 amino resin, the dispersing agent and the flatting agent at a high speed, then adding the defoaming agent, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 1.1S/cm, and the maximum value of the electromagnetic shielding effectiveness is 34dB (1 GHz-20 GHz).
Example 10
Firstly, dissolving 6 parts of glucose and 0.1 part of polyethylene glycol in water, uniformly stirring, then adding 2 parts of graphene powder, and stirring for half an hour to obtain a solution A with the graphene content of 1 wt%; then 2 parts of ferric sulfate and 2 parts of ferrous sulfate are dissolved in water to obtain a B solution with the total ferric salt content of 4 wt%. Mixing the solution A and the solution B according to the mass ratio of 1:1, heating to 40 ℃, adding 0.3 part of sodium borate, and continuously stirring for 10 minutes to obtain solution C. Sealing the solution C, placing the solution C in an oven at 180 ℃, and preserving the heat for 12 hours. And after cooling, centrifugally washing the precipitate for multiple times by using deionized water until the conductivity of the filtrate is less than 12us/cm, and drying the precipitate in an oven at the temperature of 80 ℃ for 12 hours to obtain the pretreated graphene powder. Finally, 4 parts of pretreated graphene and 0.4 part of polyvinylpyrrolidone are dispersed in water. And meanwhile, transferring the slurry to a sand mill for sanding for 6 hours, adding 0.2 part of stabilizer in the stirring process, and stirring for 1 hour to obtain the aqueous graphene slurry for electromagnetic shielding, wherein the viscosity of the aqueous graphene slurry is 1588 mPa & s.
The water-based electromagnetic shielding coating comprises the following components in percentage by weight:
38 parts of waterborne acrylic resin
40 parts of water-based graphene slurry
20 parts of cyanite 325 amino resin
Dispersant BYK 1900.5 parts
Flatting agent MOK-20170.5 parts
Defoaming agent BYK 0241 parts.
Firstly, uniformly shearing and mixing the water-based acrylic resin, the water-based graphene slurry, the cyanote 325 amino resin, the dispersing agent and the flatting agent at a high speed, then adding the defoaming agent, continuously stirring for a period of time, and standing for defoaming. Finally, the coating was applied to an epoxy resin substrate, and after drying at 160 ℃, the film thickness was 30 μm. The conductivity is 1.1S/cm, and the maximum value of the electromagnetic shielding effectiveness is 33dB (1 GHz-20 GHz).
The foregoing has described the general principles, principal features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that various changes and modifications may be made to the invention which fall within the scope of the invention as claimed.
Claims (9)
1. The preparation method of the water-based graphene slurry for the electromagnetic shielding coating is characterized by comprising the following steps of:
A) dispersing graphene powder, glucose and polyethylene glycol in water according to the mass ratio of 1-4: 6:0.1, and fully stirring to obtain a solution A with the graphene content of 1-4 wt%;
B) mixing ferrous salt and ferric salt according to a mass ratio of 1:1, dissolving in water to obtain a solution B with the total iron salt content of 1-4 wt%;
C) mixing the solution B and the solution A, heating to 30-50 ℃, adding a catalyst, and uniformly stirring to obtain solution C;
D) sealing the solution C, keeping the temperature for a period of time at a certain temperature, cooling, centrifuging and washing with deionized water for multiple times until the conductivity of the supernatant is less than 12us/cm, taking the precipitate, and drying in an oven at 80 ℃ for 12 hours to obtain pretreated graphene powder;
E) dispersing 1-4 parts of pretreated graphene powder and 0.2-0.4 part of polyvinylpyrrolidone in water, transferring the mixture into a sand mill, sanding for 6 hours, then adding 0.1-0.2 part of stabilizer, and uniformly stirring to obtain the aqueous graphene slurry for the electromagnetic shielding paint.
2. The graphene slurry preparation method according to claim 1, wherein the graphene in the step a), specifically, the liquid-phase exfoliated graphene powder has a surface functional group content of less than 0.1wt% and a thickness of 0.35 nm to 1 nm; the size is 1-15 microns.
3. The graphene slurry preparation method according to claim 1-2, wherein the ferrous salt in the step B) is one or a combination of ferrous sulfate, ferrous nitrate, ferrous chloride and potassium ferrocyanide.
4. The graphene slurry preparation method according to claim 1-2, wherein the ferric salt in step B) is one or a combination of ferric chloride, ferric sulfate and ferric nitrate.
5. The graphene slurry preparation method according to claims 1-2, wherein the liquid B and the liquid A in the step C) are uniformly mixed in a mass ratio of 1:1, specifically, the mass ratio of the content of graphene powder in the liquid A to the total mass of iron salt in the liquid B is 1:1 to 2.
6. The graphene slurry preparation method according to claim 1-2, wherein the catalyst in the step C) is boric acid or borate, and the mass fraction of the boric acid or borate in the solution C is 0.1-0.5%.
7. The graphene slurry preparation method according to claim 1-2, wherein the temperature in the closed condition in the step D) is 60-180 ℃, and the holding time is 1-24 hours.
8. The graphene slurry preparation method according to claim 1, wherein the stabilizer in the step E) is hydroxymethylcellulose and polyaniline in a mass ratio of 1: 5 compounded mixture.
9. Graphene slurry prepared according to claims 1-8 and application thereof in the field of electromagnetic shielding.
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Application publication date: 20201225 Assignee: GUANGZHOU KING POWDER TECHNOLOGY CO.,LTD. Assignor: Jiangxi Liankai Technology Co.,Ltd. Contract record no.: X2023980037194 Denomination of invention: Preparation method of water-borne Graphene slurry for electromagnetic shielding coating Granted publication date: 20221223 License type: Common License Record date: 20230628 Application publication date: 20201225 Assignee: Shanghai Liankai New Material Co.,Ltd. Assignor: Jiangxi Liankai Technology Co.,Ltd. Contract record no.: X2023980037177 Denomination of invention: Preparation method of water-borne Graphene slurry for electromagnetic shielding coating Granted publication date: 20221223 License type: Common License Record date: 20230627 |