CN111548713A - High-temperature-resistant coating with electromagnetic shielding performance and preparation method thereof - Google Patents
High-temperature-resistant coating with electromagnetic shielding performance and preparation method thereof Download PDFInfo
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- CN111548713A CN111548713A CN202010436854.XA CN202010436854A CN111548713A CN 111548713 A CN111548713 A CN 111548713A CN 202010436854 A CN202010436854 A CN 202010436854A CN 111548713 A CN111548713 A CN 111548713A
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Abstract
The invention relates to a high-temperature-resistant coating with electromagnetic shielding performance and a preparation method thereof, belonging to the technical field of high-temperature-resistant coatings. Comprises the following components in parts by weight: 200-300 parts of polyesterimide resin, 80-160 parts of cresol I, 1-2 parts of cresol II, 18-28 parts of cresol III, 100-200 parts of cresol IV, 20-60 parts of polyol, 22-66 parts of isocyanate, 2-30 parts of graphene solution, 0.2-1.8 parts of stannous octoate and 20-80 parts of xylene I; 30-60 parts of dimethylbenzene II. According to the invention, the polyurethane is modified, and the graphene component is added, so that the high temperature resistance, the voltage resistance and the anti-interference performance of the polyurethane are obviously improved.
Description
Technical Field
The invention belongs to the technical field of high-temperature-resistant coatings, and particularly relates to a high-temperature-resistant coating with electromagnetic shielding performance and a preparation method thereof
Background
The enameled wire is the main raw material of products such as motors, electrical appliances, household electrical appliances and the like, and particularly, the power industry is continuously and rapidly increased in recent years, and the requirements on the quality and the quantity of the enameled wire are greatly improved along with the rapid development of the household electrical appliances.
At present, the types of enameled wires are mainly classified into the following seven major types: acetals, polyesters, polyurethanes, polyesterimines, polyamideimides, polyimides, and composite enameled wires. In order to improve the temperature resistance level and develop special-purpose enameled wires, a more common method is to use a composite insulating layer. Composite coated enameled wires have many advantages over single coated enameled wires in that: can meet a plurality of special requirements, such as can be made into self-adhesive enameled wires which are used in refrigerant-resistant enameled wires for refrigerators and air conditioners; and the service performance can be improved by compounding with various insulating layers.
The polyurethane insulating paint has unique direct welding property, so that the application range of the polyurethane insulating paint is wide, but the use of the polyurethane insulating paint has the limitation that the heat level of a polyurethane coating film is difficult to increase due to the lower inflection point temperature of a dielectric loss curve of the film, and the high-end application of the polyurethane coating film is further influenced. At present, the electromagnetic shielding performance of the metal wire is mainly studied on the outer insulating skin of the wire or the finished packaging shell, and the electromagnetic shielding effect of the method is general and volatile for the special complexity of precise instruments.
Disclosure of Invention
Aiming at the problems of poor heat resistance, poor electromagnetic shielding effect and the like of a single polyurethane paint film in the prior art, the invention provides the electromagnetic shielding paint and the preparation method thereof, so as to solve the problems. According to the invention, the polyurethane is modified, and the graphene component is added, so that the high temperature resistance, the voltage resistance and the anti-interference performance of the polyurethane are obviously improved.
A high-temperature resistant coating with electromagnetic shielding performance comprises the following components in parts by weight: 200-300 parts of polyesterimide resin, 80-160 parts of cresol I, 1-2 parts of cresol II, 18-28 parts of cresol III, 100-200 parts of cresol IV, 20-60 parts of polyol, 22-66 parts of isocyanate, 2-30 parts of graphene solution, 0.2-1.8 parts of stannous octoate and 20-80 parts of xylene I; 30-60 parts of dimethylbenzene II.
Preferably, the composition comprises the following components in parts by weight: 220-250 parts of polyesterimide resin, 100-120 parts of cresol I, 1-2 parts of cresol II, 20-24 parts of cresol III, 100-200 parts of cresol IV, 30-40 parts of polyol, 35-45 parts of isocyanate, 5-12 parts of graphene solution, 0.6-1.0 part of stannous octoate, 30-40 parts of xylene I and 30-60 parts of xylene II.
Preferably, the polyester-imide resin is prepared from trimellitic anhydride, 4 '-diaminodiphenylmethane, dimethyl terephthalate and aliphatic triol, and the molar ratio of the trimellitic anhydride to the 4, 4' -diaminodiphenylmethane to the dimethyl terephthalate to the aliphatic triol is 2:1:1.3: 1.4.
Preferably, the graphene solution comprises at least one of graphene, graphene oxide and multilayer graphene; the graphene solution is prepared in a particle form; the solvent in the graphene solution is one or a combination of several of ethanol, methanol, acetone, n-butanol, toluene and xylene.
Preferably, the particle size of the graphene solution is less than 200 μm; the preferred particle size is less than 100 um; more preferably the particle size is less than 50 um; more preferably the particle size is less than 20 um.
Preferably, the mass percentage of the particles in the graphene solution is more than 0.2%; preferably 0.2 to 15%, more preferably 1 to 5%.
Preferably, the polyol is one or a combination of more of polyester polyol, neopentyl glycol, ethylene glycol and glycerol, and the hydroxyl value of the polyol is 20-45 mgKOH/g, preferably 35 mgKOH/g.
Preferably, the isocyanate is 2, 4-toluene diisocyanate and/or 2, 6-toluene diisocyanate, and the content of-NCO is 10-50%.
Preferably, the weight ratio of the fed amount of the polyol to the fed amount of the isocyanate is 1-5: 1.1 to 10.
The invention also aims to provide a preparation method of the high-temperature-resistant coating with the electromagnetic shielding property, which comprises the following specific steps:
(1) heating the polyester-imide resin to 150 ℃, and adding cresol III for dilution to obtain a polyester-imide solution for later use;
(2) uniformly mixing polyol and isocyanate at 20-30 ℃ to obtain a mixed solution;
(3) mixing the graphene solution, the polyester imide solution prepared in the step (1) and the mixed solution prepared in the step (2), and controlling the mixing temperature to be 80-120 ℃;
(4) and (3) adding stannous octoate into the reaction liquid obtained in the step (3), adding a mixed solvent of cresol IV and xylene II, and diluting the reaction liquid until the solid content of the polyesterimide is 10-40 wt%, thereby obtaining the high-temperature resistant coating with the electromagnetic shielding performance.
Preferably, the preparation method of the polyester-imide resin is as follows:
a. adding cresol I into a reactor, controlling the stirring speed to be 2500-5000 r/min, heating to 60 ℃ under stirring, adding trimellitic anhydride and 4, 4' -diaminodiphenylmethane, slowly heating to 120 ℃, and keeping the temperature for 30 min; then heating to 145 ℃, and preserving heat for 3 hours; finally, cooling to 130 ℃;
b. controlling the stirring speed to be 3000-6000 r/min, sequentially adding a cresol II solution of dimethyl terephthalate, aliphatic trihydric alcohol, ethylene glycol and n-butyl titanate into a reactor, heating to 150 ℃, and keeping the temperature and stirring for 2 hours; then sequentially heating to 150-170 ℃, and preserving heat for 1 h; keeping the temperature at 170-190 ℃ for 2 h; and finally, controlling the reaction temperature to be 190-200 ℃ for reaction until the reaction system becomes transparent, and then preserving the heat for 2 hours.
c. Adding xylene I, volatilizing xylene I by using residual heat, taking away redundant solvent, cooling to room temperature, sealing and storing to obtain the polyester-imide resin.
Preferably, the aliphatic triol is one of glycerol or tris (2-hydroxyethyl) isocyanurate.
Preferably, the feeding amount of the n-butyl titanate is 0.013g/g based on the feeding amount of the 4, 4' -diaminodiphenylmethane.
The invention has the beneficial effects that:
(1) in order to improve the performance of the coating in terms of heat resistance and impact resistance, tris (2-hydroxyethyl) isocyanurate is used in the synthesis of the polyesterimide resin. The tris (2-hydroxyethyl) isocyanurate contains triazine ring with high heat resistance, so that the softening breakdown temperature and the thermal shock resistance of the enameled wire are improved; the larger the amount of the mosaic in the polyester-imide resin, the larger the crosslinking degree of the paint film, the larger the volume of the crosslinking unit, the more the polymer network chain relaxes, the easier the movement of the chain segment, the higher the elasticity of the polymer chain, and the improved hot-stamping performance of the paint film. Meanwhile, the modified polyurethane keeps the characteristics of wide margin and good stripping property of the original polyurethane coating, and graphene is introduced as a lamellar carbon material with a hexagonal structure, so that the molecular rigidity factor is increased, the activity of macromolecules is reduced, and the toughness of a paint film is increased.
(2) The invention adopts the n-butyl titanate modifier as the cross-linking agent to coat the polyesterimide, so that the coated thread sample has smooth surface, uniform paint film, no particles and bubbles and wider thread coating process range.
(3) On the one hand, the viscosity of the paint is sharply reduced when the temperature of the paint is raised and the solvent is not evaporated. Under the action of gravity, the paint liquid will flow or run off rapidly, so that the paint layer becomes thin or eccentric, and the like, so that the temperature is matched, and the solvent is evaporated gradually. The solvent adopted by the invention is dimethylbenzene and cresol, which are both very volatile, so that the method is very important for controlling the temperature, and the reflux time can be increased by gradually heating in sections, so that the change of the solvent in the system is stable; on the other hand, the polyester-imide is very easy to be polymerized violently in the polymerization process, particularly at the temperature of more than 170 ℃, the system reaction is violent, the viscosity is rapidly increased, the color of the solution is darkened, the multi-stage heating is utilized, the reflux device is introduced, and the rotating speed is improved, so that the problem is solved.
(4) According to the invention, the thermal stability of the coating is further improved by controlling the adding time and the adding form of the graphene solution. The traditional graphene solution is difficult to disperse in water, and with the increase of temperature and the increase of viscosity of a high molecular system, the graphene solution is difficult to disperse and causes agglomeration, so that the electromagnetic shielding performance of the graphene solution is reduced and the toughness of the graphene solution after film forming is greatly reduced. The particle size of the graphene solution is screened and regulated by heating in sections, the dispersion of the surface of graphene is controlled without using a surfactant, and toluene, xylene and the like required in the polyurethane/polyimide reaction are adopted, so that the introduction of a new solvent is avoided, the method is more environment-friendly and economical, the operation is more convenient, and the finished paint is more stable. On the other hand, solvents such as toluene, xylene and the like can be inserted between solvent molecules to be intercalated into the graphite layers to obtain a graphite interlayer compound, so that the interlayer aggregation of graphene sheets can be better avoided, and groups in the solvents are used as intermediates, can be uniformly dispersed among chemical bonds of polyimide/polyurethane, and have higher thermal stability and better performance.
(5) According to the invention, the graphene component is added into the coating component, the graphene is a two-dimensional carbon nano-structure material formed by single-layer graphite flakes, and the graphene has excellent mechanical, electrical and thermal properties, particularly, the mobility of the graphene can reach 2 × 104cm2The resistivity of the graphene can reach 10 at room temperature in V × s8S/m, tolerable 108A/cm2The current of (2). The graphene is added into the conductive paste, so that the conductivity can be improved, the use amount of noble metals such as Ag and Cu can be reduced under the condition of ensuring the same conductive performance, and the cost is reduced. Further, due to the advantages of inertia, low density and the like of graphene, the addition of graphene can prolong the service life of the conductive paste and reduce the density of the paste. However, graphene is inThe defects of easy irreversible stacking, poor dispersibility and the like in the processing process limit the exertion of excellent performance of the graphene in the conductive paste. The invention utilizes the synergistic effect of the conjugated structure in the graphene and the polyester imide resin to form a complete conductive path, and overcomes the defects of high cost and poor oxidation resistance of metal synergistic effect.
Detailed description of the preferred embodiments
In order to make those skilled in the art better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a high-temperature resistant coating with electromagnetic shielding performance comprises the following specific steps:
(1) preparation of polyesterimide resins
a. Adding 110 parts of cresol into a reactor, controlling the stirring speed to be 2500-5000 r/min, heating to 60 ℃ under stirring, adding 29.1 parts of trimellitic anhydride and 15.1 parts of 4, 4' -diaminodiphenylmethane, slowly heating to 120 ℃, and keeping the temperature for 30 min; then heating to 145 ℃, and preserving heat for 3 hours; finally, cooling to 130 ℃;
b. controlling the stirring speed to be 3000-6000 r/min, sequentially adding 19.6 parts of dimethyl terephthalate, 28.2 parts of tris (2-hydroxyethyl) isocyanurate, 5.5 parts of ethylene glycol and cresol solution of n-butyl titanate (0.2 part of n-butyl titanate and 1 part of cresol) into a reactor, heating to 150 ℃, and keeping the temperature and stirring for 2 hours; then sequentially heating to 160 ℃, and preserving heat for 1 h; keeping the temperature at 170 ℃ for 2 h; and finally, controlling the reaction temperature at 190 ℃ to react until the reaction system becomes transparent, and then preserving the heat for 2 hours.
c. Adding 21 parts of dimethylbenzene, volatilizing the dimethylbenzene by using waste heat, taking away redundant solvent, cooling to room temperature, and sealing for storage to obtain the polyester-imide resin.
(2) And (2) taking 200 parts of the polyesterimide resin prepared in the step (1), heating to 150 ℃, and adding 18 parts of cresol for dilution to obtain a polyesterimide solution for later use.
(3) And (2) uniformly mixing 20 parts of mixed solvent of polyester polyol, glycerol, neopentyl glycol and ethylene glycol and 22 parts of 2, 4-toluene diisocyanate at the temperature of 20-30 ℃ to obtain a mixed solution.
(4) 5 parts of a xylene solution containing 1% of graphene particles, the polyester imide solution prepared in the step (1) and the mixed solution prepared in the step (2) are mixed, and the mixing temperature is controlled to be 80-90 ℃;
(5) and (3) adding 0.2 part of stannous octoate into the reaction liquid obtained in the step (3), adding 120 parts of cresol and 30 parts of xylene mixed solvent, and diluting the reaction liquid until the solid content of the polyesterimide is 10 wt% to obtain the high-temperature-resistant coating with the electromagnetic shielding performance.
Example 2
A preparation method of a high-temperature resistant coating with electromagnetic shielding performance comprises the following specific steps:
(1) preparation of polyesterimide resins
a. Adding 110 parts of cresol into a reactor, controlling the stirring speed to be 2500-5000 r/min, heating to 60 ℃ under stirring, adding 29.1 parts of trimellitic anhydride and 15.1 parts of 4, 4' -diaminodiphenylmethane, slowly heating to 120 ℃, and keeping the temperature for 30 min; then heating to 145 ℃, and preserving heat for 3 hours; finally, cooling to 130 ℃;
b. controlling the stirring speed to be 3000-6000 r/min, sequentially adding 19.6 parts of dimethyl terephthalate, 28.2 parts of tris (2-hydroxyethyl) isocyanurate, 6 parts of ethylene glycol and cresol solution of n-butyl titanate (0.2 part of n-butyl titanate and 1.5 parts of cresol) into a reactor, heating to 150 ℃, and keeping the temperature and stirring for 2 hours; then sequentially heating to 160 ℃, and preserving heat for 1 h; keeping the temperature at 170 ℃ for 2 h; and finally, controlling the reaction temperature at 190 ℃ to react until the reaction system becomes transparent, and then preserving the heat for 2 hours.
c. Adding 25 parts of dimethylbenzene, volatilizing the dimethylbenzene by using waste heat, taking away redundant solvent, cooling to room temperature, and sealing for storage to obtain the polyester-imide resin.
(2) And (2) taking 200 parts of the polyesterimide resin prepared in the step (1), heating to 150 ℃, and adding 18 parts of cresol for dilution to obtain a polyesterimide solution for later use.
(3) And uniformly mixing 30 parts of mixed solvent of polyester polyol, glycerol, neopentyl glycol and ethylene glycol and 36 parts of 2, 6-toluene diisocyanate at the temperature of 20-30 ℃ to obtain mixed liquid.
(4) Mixing 7 parts of a dimethylbenzene solution containing 2% of graphene particles, the polyesterimide solution prepared in the step (1) and the mixed solution prepared in the step (2), and controlling the mixing temperature to be 80-90 ℃;
(5) and (3) adding 0.6 part of stannous octoate into the reaction liquid obtained in the step (3), adding 160 parts of cresol and 45 parts of xylene mixed solvent, and diluting the reaction liquid until the solid content of the polyesterimide is 15 wt% to obtain the high-temperature-resistant coating with the electromagnetic shielding performance.
Example 3
A preparation method of a high-temperature resistant coating with electromagnetic shielding performance comprises the following specific steps:
(1) preparation of polyesterimide resins
a. Adding 110 parts of cresol into a reactor, controlling the stirring speed to be 2500-5000 r/min, heating to 60 ℃ under stirring, adding 29.1 parts of trimellitic anhydride and 15.1 parts of 4, 4' -diaminodiphenylmethane, slowly heating to 120 ℃, and keeping the temperature for 30 min; then heating to 145 ℃, and preserving heat for 3 hours; finally, cooling to 130 ℃;
b. controlling the stirring speed to be 3000-6000 r/min, sequentially adding 19.6 parts of dimethyl terephthalate, 28.2 parts of tris (2-hydroxyethyl) isocyanurate, 5.5 parts of ethylene glycol and cresol solution of n-butyl titanate (0.2 part of n-butyl titanate and 1 part of cresol) into a reactor, heating to 150 ℃, and keeping the temperature and stirring for 2 hours; then sequentially heating to 160 ℃, and preserving heat for 1 h; keeping the temperature at 180 ℃ for 2 h; and finally, controlling the reaction temperature at 190 ℃ to react until the reaction system becomes transparent, and then preserving the heat for 2 hours.
c. Adding 30 parts of dimethylbenzene, volatilizing the dimethylbenzene by using waste heat, taking away redundant solvent, cooling to room temperature, and sealing for storage to obtain the polyester-imide resin.
(2) And (2) taking 220 parts of the polyesterimide resin prepared in the step (1), heating to 150 ℃, and adding 20 parts of cresol for dilution to obtain a polyesterimide solution for later use.
(3) And (2) uniformly mixing 32 parts of mixed solvent of polyester polyol, glycerol, neopentyl glycol and ethylene glycol and 48 parts of 2, 4-toluene diisocyanate at the temperature of 20-30 ℃ to obtain a mixed solution.
(4) Mixing 8 parts of a xylene solution containing 3% graphene particles, the polyesterimide solution prepared in the step (1) and the mixed solution prepared in the step (2), and controlling the mixing temperature to be 90-100 ℃;
(5) and (3) adding 0.8 part of stannous octoate into the reaction liquid obtained in the step (3), adding 160 parts of cresol and 50 parts of xylene mixed solvent, and diluting the reaction liquid until the solid content of the polyesterimide is 20 wt% to obtain the high-temperature-resistant coating with the electromagnetic shielding performance.
Example 4
A preparation method of a high-temperature resistant coating with electromagnetic shielding performance comprises the following specific steps:
(1) preparation of polyesterimide resins
a. Adding 120 parts of cresol into a reactor, controlling the stirring speed to be 2500-5000 r/min, heating to 60 ℃ under stirring, adding 32 parts of trimellitic anhydride and 16.6 parts of 4, 4' -diaminodiphenylmethane, slowly heating to 120 ℃, and keeping the temperature for 30 min; then heating to 145 ℃, and preserving heat for 3 hours; finally, cooling to 130 ℃;
b. controlling the stirring speed to be 3000-6000 r/min, sequentially adding 21.6 parts of dimethyl terephthalate, 31 parts of tris (2-hydroxyethyl) isocyanurate, 6 parts of ethylene glycol and cresol solution of n-butyl titanate (0.22 part of n-butyl titanate and 1 part of cresol) into a reactor, heating to 150 ℃, and keeping the temperature and stirring for 2 hours; then sequentially heating to 160 ℃, and preserving heat for 1 h; keeping the temperature at 180 ℃ for 2 h; and finally, controlling the reaction temperature at 190 ℃ to react until the reaction system becomes transparent, and then preserving the heat for 2 hours.
c. Adding 35 parts of dimethylbenzene, volatilizing the dimethylbenzene by using waste heat, taking away redundant solvent, cooling to room temperature, and sealing for storage to obtain the polyester-imide resin.
(2) And (2) taking 230 parts of the polyesterimide resin prepared in the step (1), heating to 150 ℃, and adding 21 parts of cresol for dilution to obtain a polyesterimide solution for later use.
(3) And uniformly mixing 36 parts of glycerol and 50 parts of 2, 4-toluene diisocyanate at the temperature of 20-30 ℃ to obtain a mixed solution.
(4) Mixing 8 parts of a xylene solution containing 3% graphene particles, the polyesterimide solution prepared in the step (1) and the mixed solution prepared in the step (2), and controlling the mixing temperature to be 90-100 ℃;
(5) and (3) adding 1.0 part of stannous octoate into the reaction liquid obtained in the step (3), adding 160 parts of cresol and 60 parts of xylene mixed solvent, and diluting the reaction liquid until the solid content of the polyesterimide is 20 wt% to obtain the high-temperature-resistant coating with the electromagnetic shielding performance.
Example 5
A preparation method of a high-temperature resistant coating with electromagnetic shielding performance comprises the following specific steps:
(1) preparation of polyesterimide resins
a. Adding 140 parts of cresol into a reactor, controlling the stirring speed to be 2500-5000 r/min, heating to 60 ℃ under stirring, adding 36.8 parts of trimellitic anhydride and 19.1 parts of 4, 4' -diaminodiphenylmethane, slowly heating to 120 ℃, and keeping the temperature for 30 min; then heating to 145 ℃, and preserving heat for 3 hours; finally, cooling to 130 ℃;
b. controlling the stirring speed to be 3000-6000 r/min, sequentially adding 23.2 parts of dimethyl terephthalate, 35.6 parts of tri (2-hydroxyethyl) isocyanurate, 7 parts of ethylene glycol and cresol solution of n-butyl titanate (0.25 part of n-butyl titanate and 2 parts of cresol) into a reactor, heating to 150 ℃, and keeping the temperature and stirring for 2 hours; then sequentially heating to 160 ℃, and preserving heat for 1 h; keeping the temperature at 180 ℃ for 2 h; and finally, controlling the reaction temperature at 190 ℃ to react until the reaction system becomes transparent, and then preserving the heat for 2 hours.
c. Adding 60 parts of dimethylbenzene, volatilizing the dimethylbenzene by using waste heat, taking away redundant solvent, cooling to room temperature, and sealing for storage to obtain the polyester-imide resin.
(2) And (2) taking 250 parts of the polyesterimide resin prepared in the step (1), heating to 150 ℃, and adding 22 parts of cresol for dilution to obtain a polyesterimide solution for later use.
(3) And (2) uniformly mixing 50 parts of glycerol and 60 parts of 2, 6-toluene diisocyanate at the temperature of 20-30 ℃ to obtain a mixed solution.
(4) Mixing 12 parts of a xylene solution containing 5% of graphene particles, the polyesterimide solution prepared in the step (1) and the mixed solution prepared in the step (2), and controlling the mixing temperature to be 90-100 ℃;
(5) and (3) adding 1.5 parts of stannous octoate into the reaction liquid obtained in the step (3), adding a mixed solvent of 180 parts of cresol and 60 parts of xylene, and diluting the reaction liquid until the solid content of the polyesterimide is 30 wt% to obtain the high-temperature-resistant coating with the electromagnetic shielding performance.
Example 6
A preparation method of a high-temperature resistant coating with electromagnetic shielding performance comprises the following specific steps:
(1) preparation of polyesterimide resins
a. Adding 160 parts of cresol into a reactor, controlling the stirring speed to be 2500-5000 r/min, heating to 60 ℃ under stirring, adding 42.3 parts of trimellitic anhydride and 22.0 parts of 4, 4' -diaminodiphenylmethane, slowly heating to 120 ℃, and keeping the temperature for 30 min; then heating to 145 ℃, and preserving heat for 3 hours; finally, cooling to 130 ℃;
b. controlling the stirring speed to be 3000-6000 r/min, sequentially adding 28.5 parts of dimethyl terephthalate, 41.0 parts of tris (2-hydroxyethyl) isocyanurate, 7 parts of ethylene glycol and cresol solution of n-butyl titanate (0.29 part of n-butyl titanate and 2 parts of cresol) into a reactor, heating to 150 ℃, and keeping the temperature and stirring for 2 hours; then sequentially heating to 170 ℃, and preserving heat for 1 h; keeping the temperature at 190 ℃ for 2 h; and finally, controlling the reaction temperature at 195 ℃ until the reaction system becomes transparent, and then preserving the temperature for 2 h.
c. Adding 80 parts of dimethylbenzene, volatilizing the dimethylbenzene by using waste heat, taking away redundant solvent, cooling to room temperature, and sealing for storage to obtain the polyester-imide resin.
(2) And (2) taking 300 parts of the polyester imide resin prepared in the step (1), heating to 150 ℃, and adding 28 parts of cresol for dilution to obtain a polyester imide solution for later use.
(3) And uniformly mixing 60 parts of glycerol and 66 parts of 2, 6-toluene diisocyanate at the temperature of 20-30 ℃ to obtain a mixed solution.
(4) Mixing 30 parts of a dimethylbenzene solution containing 3% of graphene particles, the polyesterimide solution prepared in the step (1) and the mixed solution prepared in the step (2), and controlling the mixing temperature to be 90-100 ℃;
(5) and (3) adding 1.8 parts of stannous octoate into the reaction liquid obtained in the step (3), adding a mixed solvent of 200 parts of cresol and 60 parts of xylene, and diluting the reaction liquid until the solid content of the polyesterimide is 40 wt%, thereby obtaining the high-temperature resistant coating with electromagnetic shielding performance.
After the coating prepared in examples 1 to 6 and the wire are prepared into the enameled wire, the enameled wire is subjected to performance test, and the specific results are shown in tables 1 to 3 below:
TABLE 1-enameled wire withstand voltage test results (leakage current setting 2mA)
| Sample (I) | Solid content of polyesterimide | voltage/V | Average voltage/V |
| Example 1 | 10％ | 6.18/3.58/3.29/2.22 | 3.81 |
| Example 2 | 15％ | 1.36/1.29/1.20/1.12 | 1.24 |
| Example 3 | 20％ | 0.83/0.91/1.30/0.87 | 0.98 |
| Example 4 | 25％ | 1.63/1.56/1.86/1.60 | 1.66 |
| Example 5 | 30％ | 1.70/1.85/1.75.1.81 | 1.78 |
| Example 6 | 40％ | 4.54/4.22/3.93/3.79 | 4.12 |
From the data in Table 1, it is clear that the voltage resistance of the paint film tends to increase with increasing content of the polyesterimide. The reason is that the content of imine groups and graphene in the polyester imide resin is increased, the rigid structure of a macromolecular structure is increased, and the activity of a macromolecular motion unit is reduced, so that the toughness of a paint film is increased, the using amount of imine is increased, the distance between crosslinking points of macromolecules is increased, the chain segment activity is easier, the adaptability to deformation is higher, the strength and the elasticity of the paint film are obviously improved, and the voltage resistance value is further increased.
TABLE 2 dielectric loss Property test results for enameled wires
| Sample (I) | Solid content of polyesterimide | Temperature of onset/. degree.C | TgD1/℃ | C/(pF) |
| Example 1 | 10％ | 51 | 126 | 373.15 |
| Example 2 | 15％ | 50 | 128 | 190.35 |
| Example 3 | 20％ | 50 | 126 | 187.80 |
| Example 4 | 25％ | 55 | 133 | 208.87 |
| Example 5 | 30％ | 55 | 141 | 209.96 |
| Example 6 | 40％ | 55 | 153 | 210 |
The data in table 2 show that there are more benzene rings and imine rings in the main chain structure of the polyesterimide molecule, and graphene can be independently dispersed in a solvent system to form a two-dimensional nano structure of graphene oxide colloidal solution, so that the molecular chain is endowed with greater rigidity, the transition temperature (TgD1) of the structure motion in the molecule is higher, the capacitance (C) is increased, and a new method is provided for developing the weldable high-temperature-resistant coating with high dielectric loss inflection point temperature.
TABLE 3 electromagnetic shielding effectiveness test results
| Sample (I) | Solid content of polyesterimide | Electromagnetic shielding rate (dB) |
| Example 1 | 10％ | ≥73 |
| Example 2 | 15％ | ≥75 |
| Example 3 | 20％ | ≥77 |
| Example 4 | 25％ | ≥78 |
| Example 5 | 30％ | ≥90 |
| Example 6 | 40％ | ≥85 |
As can be seen from the data in table 3, in the case of high polyimide solid content, through the preparation process of the present invention, graphene particles can be uniformly dispersed into a single-layer structure, agglomeration is effectively prevented, a honeycomb two-dimensional article composed of single-layer hexagonal cell carbon atoms is maintained, and the characteristics of high mechanical strength, excellent conductivity, high chemical stability and the like are maintained.
Selecting a section of paint film with the length of 2-3 cm, coating a better thick line, completely immersing the paint film in a test tube filled with a DMF solvent, placing the test tube on a test tube rack, carefully observing and recording the time for the paint film to crack for the first time, continuously observing until the paint film is completely cracked, and recording the time. The specific test results are shown in table 4:
TABLE 4 influence of the solid content of the polyesterimide paints on the solvent resistance
As can be seen from the data in Table 4, the system formed by the functional additive and the solvent in the invention does not cause cracks, has good solvent resistance, and the aqueous electromagnetic shielding coating has good workability, good leveling effect and uniform arrangement.
Although the present invention has been described in detail by way of preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. The high-temperature-resistant coating with the electromagnetic shielding performance is characterized by comprising the following components in parts by weight: 200-300 parts of polyesterimide resin, 80-160 parts of cresol I, 1-2 parts of cresol II, 18-28 parts of cresol III, 100-200 parts of cresol IV, 20-60 parts of polyol, 22-66 parts of isocyanate, 2-30 parts of graphene solution, 0.2-1.8 parts of stannous octoate and 20-80 parts of xylene I; 30-60 parts of dimethylbenzene II.
2. The high-temperature-resistant coating with electromagnetic shielding property as claimed in claim 1, which comprises the following components in parts by weight: 220-250 parts of polyesterimide resin, 100-120 parts of cresol I, 1-2 parts of cresol II, 20-24 parts of cresol III, 100-200 parts of cresol IV, 30-40 parts of polyol, 35-45 parts of isocyanate, 5-12 parts of graphene solution, 0.6-1.0 part of stannous octoate, 30-40 parts of xylene I and 30-60 parts of xylene II.
3. The high-temperature-resistant coating with electromagnetic shielding property of claim 1, wherein the polyester-imide resin is prepared from trimellitic anhydride, 4' -diaminodiphenylmethane, dimethyl terephthalate and aliphatic trihydric alcohol; the molar ratio of the trimellitic anhydride to the 4, 4' -diaminodiphenylmethane to the dimethyl terephthalate to the aliphatic triol is 2:1:1.3: 1.4.
4. The high-temperature-resistant coating with electromagnetic shielding property of claim 1, wherein the graphene solution comprises at least one of graphene, graphene oxide, and multi-layer graphene; the graphene solution is prepared in a particle form; the solvent in the graphene solution is one or a combination of several of ethanol, methanol, acetone, n-butanol, toluene and xylene.
5. The high-temperature-resistant coating with electromagnetic shielding property of claim 1, wherein the particle size of the graphene solution is less than 200 μm; the preferred particle size is less than 100 um; more preferably the particle size is less than 50 um; more preferably the particle size is less than 20 um.
6. The high-temperature-resistant coating with electromagnetic shielding performance of claim 1, wherein the mass percentage of particles in the graphene solution is more than 0.2%; preferably 0.2 to 15%, more preferably 1 to 5%.
7. The high-temperature-resistant coating with electromagnetic shielding property of claim 1, wherein the polyol is one or a combination of polyester polyol, neopentyl glycol, ethylene glycol and glycerol, and the hydroxyl value of the polyol is 20-45 mgKOH/g, preferably 35 mgKOH/g.
8. The high-temperature-resistant coating with electromagnetic shielding property as claimed in claim 1, wherein the isocyanate is 2, 4-toluene diisocyanate and/or 2, 6-toluene diisocyanate, and the content of-NCO is 10-50%;
preferably, the weight ratio of the fed amount of the polyol to the fed amount of the isocyanate is 1-5: 1.1 to 10.
9. A preparation method of a high-temperature-resistant coating with electromagnetic shielding performance is characterized by comprising the following specific steps:
(1) heating the polyester-imide resin to 150 ℃, and adding cresol III for dilution to obtain a polyester-imide solution for later use;
(2) uniformly mixing polyol and isocyanate at 20-30 ℃ to obtain a mixed solution;
(3) mixing the graphene solution, the polyester imide solution prepared in the step (1) and the mixed solution prepared in the step (2), and controlling the mixing temperature to be 80-120 ℃;
(4) and (3) adding stannous octoate into the reaction liquid obtained in the step (3), adding a mixed solvent of cresol IV and xylene II, and diluting the reaction liquid until the solid content of the polyesterimide is 10-40 wt%, thereby obtaining the high-temperature resistant coating with the electromagnetic shielding performance.
10. The method for preparing the high-temperature-resistant coating with electromagnetic shielding property of claim 9, wherein the method for preparing the polyester-imide resin comprises the following steps:
a. adding cresol I into a reactor, controlling the stirring speed to be 2500-5000 r/min, heating to 60 ℃ under stirring, adding trimellitic anhydride and 4, 4' -diaminodiphenylmethane, slowly heating to 120 ℃, and keeping the temperature for 30 min; then heating to 145 ℃, and preserving heat for 3 hours; finally, cooling to 130 ℃;
b. controlling the stirring speed to be 3000-6000 r/min, sequentially adding a cresol II solution of dimethyl terephthalate, aliphatic trihydric alcohol, ethylene glycol and n-butyl titanate into a reactor, heating to 150 ℃, and keeping the temperature and stirring for 2 hours; then sequentially heating to 150-170 ℃, and preserving heat for 1 h; keeping the temperature at 170-190 ℃ for 2 h; finally, controlling the reaction temperature at 190-200 ℃ to react until the reaction system becomes transparent, and then preserving the heat for 2 hours;
c. adding xylene I, volatilizing xylene I by using residual temperature, taking away redundant solvent, cooling to room temperature, and sealing for storage to obtain polyesterimide resin;
preferably, the aliphatic triol is one of glycerol or tris (2-hydroxyethyl) isocyanurate;
preferably, the feeding amount of the n-butyl titanate is 0.013g/g based on the feeding amount of the 4, 4' -diaminodiphenylmethane.
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