CN115572529A - Wear-resistant nano coating for magnetic material product and preparation method thereof - Google Patents
Wear-resistant nano coating for magnetic material product and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a wear-resistant nano coating for a magnetic material product and a preparation method thereof, and relates to the technical field of magnetic materials. According to the invention, the modified polyurethane is prepared by using trifluoroacetic acid, diethylenetriamine, 4-chloro-3, 6-dihydroxypyridazine, polytetrahydrofuran and 4-chloro-6-methyl m-phenylene diisocyanate, and has a good salt mist resistant effect; and then carrying out deposition treatment on graphite-phase carbon nitride to form alumina aerogel, inhibiting tunnel current between carbon nitride sheets, carrying out heat treatment to form a micro-nano lapped network structure, improving the voltage resistance of the coating, and modifying by utilizing 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone, tetramethyldiethoxydisilane, octamethylcyclotetrasiloxane and aminopropylmethyldimethoxysilane to form the insulating protective film. The wear-resistant nano coating prepared by the invention has the effects of voltage resistance and salt mist resistance.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a wear-resistant nano coating for a magnetic material product and a preparation method thereof.
Background
Magnetic materials, which react in some way to magnetic fields, are commonly used in magnetic storage devices, magnetic cards, microwave components, etc., and are mainly classified into soft magnetic materials, permanent magnetic materials, magnetic recording materials, etc. The magnetic material product is easy to corrode and rust in the salt fog environment, so that the performance of the magnetic material product is reduced, and the service life is seriously influenced. At present, a teflon coating and a polyurethane coating are commonly used as protective means, but the teflon coating and the polyurethane coating still have respective defects. For example, the teflon coating has a high baking temperature, which has a large influence on the magnetic attenuation of magnetic materials, and the high baking temperature has high requirements on the environment, equipment, safety and other aspects of spraying construction, while the polyurethane coating has poor salt spray resistance and cannot meet the requirement of long design life.
With the development of magnetic materials, the magnetic materials gradually extend to special industries such as automobiles, high-voltage electrical appliances and the like, so that the magnetic materials have good insulating property, but the existing protective coatings have poor insulating property, are easy to generate negative effects in actual use, are easy to cause voltage breakdown, generate short-circuit phenomena and influence the safe and stable operation of the electrical appliances.
Disclosure of Invention
The invention aims to provide a wear-resistant nano coating for a magnetic material product and a preparation method thereof, and aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: the wear-resistant nano coating for the magnetic material product mainly comprises modified polyurethane, self-made filler, a closed isocyanate curing agent and a polyethylene glycol solution.
Further, the modified polyurethane is prepared from trifluoroacetic acid, diethylenetriamine, 4-chloro-3, 6-dihydroxypyridazine, polytetrahydrofuran and 4-chloro-6-methyl m-phenylene diisocyanate.
Further, the self-made filler is prepared by a method of depositing graphite phase nitrogen carbide to obtain a filler precursor; the deposition treatment comprises the steps of dispersing graphite phase nitrogen carbide in absolute ethyl alcohol, adjusting the pH value, adding aluminum sec-butoxide, n-butanol, ethyl acetate and deionized water, stirring, cooling to room temperature, standing for aging, placing in an autoclave, reacting at high temperature and high pressure in the nitrogen atmosphere, purging with nitrogen and annealing; then carrying out heating treatment to obtain composite particles; the heating treatment is that the self-made filler precursor is subjected to high-temperature heat treatment for a period of time under the protection of nitrogen; then, 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone, tetramethyldiethoxydisilane, octamethylcyclotetrasiloxane and aminopropylmethyldimethoxysilane were used for modification.
Further, the blocked isocyanate curing agent is one or a mixture of hexamethylene diisocyanate trimer, isophorone diisocyanate trimer or hexamethylene diisocyanate biuret.
Further, a preparation method of the wear-resistant nano coating for the magnetic material product comprises the following preparation steps:
(1) Mixing polytetrahydrofuran 1000, N-dimethylformamide and a corrosion inhibitor according to a mass ratio of 1.2;
(2) Carrying out deposition treatment on graphite phase nitrogen carbide to obtain a filler precursor; then carrying out heating treatment to obtain composite particles;
(3) Mixing the pretreated composite particles, tetramethyldiethoxydisilane, monobutyltin oxide and N, N-dimethylformamide according to a mass ratio of 1.001;
(4) Mixing modified polyurethane, self-made filler and polyethylene glycol solution according to the mass ratio of 1.2.
Further, the preparation method of the corrosion inhibitor in the step (1) is characterized by comprising the following steps: mixing trifluoroacetic acid, diethylenetriamine and xylene according to a mass ratio of 1.3.
Further, the deposition treatment in the step (2) is characterized by comprising the following specific steps: dispersing graphite phase nitrogen carbide in absolute ethyl alcohol with the mass of 3-9 times of that of the graphite phase nitrogen carbide, adding sodium hydroxide until the pH value of the solution is 10-11, stirring the mixture for 60-72 min at the mass ratio of 1.
Further, the heating treatment in the step (2) is characterized by comprising the following specific steps: and (3) carrying out heat treatment on the self-made filler precursor for 56-70 min at 900-1000 ℃ under the protection of nitrogen.
Further, the preparation method of the pretreated composite particles in the step (3) is characterized by comprising the following steps: dispersing the composite particles in absolute ethyl alcohol with the mass of 26-38 times of that of the composite particles, stirring at 1000-1200 rpm for 60-88 min, adding 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone with the mass of 0.08-0.2 time of that of the composite particles, stirring at 1500-2000 rpm for 60-90 min at 60-80 ℃, performing suction filtration, washing with absolute ethyl alcohol for 3-5 times, and drying at 60-70 ℃ for 3-6 h.
Further, the concentration of the polyethylene glycol solution in the step (4) is 0.05-0.2 g/mL.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts modified polyurethane, curing agent, self-made filler and the like to compound and form the coating so as to realize the effects of salt mist resistance and voltage resistance.
Firstly, carboxyl of trifluoroacetic acid reacts with amino of diethylenetriamine to form an imidazoline compound, then the imidazoline compound and chloride ions of 4-chloro-3, 6-dihydroxypyridazine undergo quaternization to form a corrosion inhibitor, so that the coating has a salt mist resistant effect, hydroxyl of the coating is polymerized with hydroxyl of polytetrahydrofuran and diisocyanate of 4-chloro-6-methyl m-phenylene diisocyanate to obtain modified polyurethane, and after the coating is cured, a fluorine-containing side chain is unfolded towards an air contact interface to form a coating with low surface energy, so that salt mist cannot stay on the surface of the coating for a long time, and the corrosion speed is delayed; in addition, the modified polyurethane contains high-activity carbon-nitrogen double bonds and a cation structure, is easy to interact with the surface of a metal magnetic material, is adsorbed on the surface of the metal magnetic material to form a stable protective film, improves the salt fog resistance of the coating, can perform high-temperature curing reaction with an isocyanate curing agent to form a compact reticular interpenetrating structure, and improves the stability and the salt fog resistance of the coating.
Secondly, the graphite-phase carbon nitride is used as a raw material, plasma treatment is carried out, and trimethyl aluminum and oxygen plasmas are used and distributed among carbon nitride sheets to inhibit tunnel current between the carbon nitride sheets, so that the volume resistance of the coating is improved, the voltage resistance of the coating is enhanced, and the coated carbon nitride is further grown; then, heat treatment is carried out, so that carbon nitride is reduced and hybridized and can be more compactly inserted among alumina to form micro-nano lapped composite particles with a network structure, and the voltage resistance of the coating is improved; then 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone is grafted on the surface of the composite particle by utilizing a silicon-oxygen bond, the hydroxyl group of the benzophenone is reacted with the ethoxy group of tetramethyl diethoxy disilane, then the tetramethyl diethoxy disilane is polymerized with octamethyl cyclotetrasiloxane and aminopropyl methyl dimethoxy silane, an insulating protective film is formed on the surface of the composite particle, the voltage resistance of the coating is improved, in addition, the side chain amino group of the film can also react with the chloride ion of the modified polyurethane, and the mutual crosslinking combination is realized, so that the insulating defect is reduced, the voltage resistance is improved, and the wear resistance of the coating can also be improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for detailed description, and the index testing method for the wear-resistant nano coating of the magnetic material product manufactured in the following examples is as follows:
coating the coatings of the embodiment and the comparative example on a metal magnetic material to the same thickness, and carrying out salt spray resistance and voltage resistance effect tests after curing;
salt spray resistance: carrying out continuous neutral salt spray test according to GB/T1771, requiring the test for 400h, and observing the surface condition;
voltage resistance: attaching a circular electrode plate to the upper and lower surfaces of a metal magnetic material with double-sided coatings, and applying 2N/mm to the electrode plate 2 The pressure of the coating is recorded by adopting a direct current power supply to supply power to the electrode plate, displaying the current magnitude in real time through an ammeter connected in series in the circuit, adjusting the voltage to gradually increase, and when the current is monitored to have sudden change, namely the coating insulation breakdown pointThe breakdown voltage value of time.
Example 1
(1) Mixing trifluoroacetic acid, diethylenetriamine and xylene according to a mass ratio of 1:0.3, reacting at 140 ℃ for 2h, heating to 190 ℃, reacting for 2h, cooling to 90 ℃, slowly dropwise adding 4-chloro-3, 6-dihydroxypyridazine with the mass of 0.3 time of that of the trifluoroacetic acid, and reacting for 2h to obtain the corrosion inhibitor; mixing polytetrahydrofuran 1000, N-dimethylformamide and a corrosion inhibitor according to a mass ratio of 1: 0.1, vacuumizing for 3 times, adding 4-chloro-6-methyl m-phenylene diisocyanate, N-dimethylformamide, dibutyltin dilaurate, 4-chloro-6-methyl m-phenylene diisocyanate and polytetrahydrofuran 1000 according to a mass ratio of 1;
(2) Dispersing graphite phase nitrogen carbide in absolute ethyl alcohol with the mass of 3 times of that of the graphite phase nitrogen carbide, adding sodium hydroxide until the pH of the solution is 10, adding aluminum sec-butoxide, n-butanol, ethyl acetate and deionized water according to the mass ratio of 1; carrying out heat treatment on the self-made filler precursor for 56min at 900 ℃ under the protection of nitrogen to obtain composite particles;
(3) Dispersing the composite particles in absolute ethyl alcohol with the mass 26 times that of the composite particles, stirring at 1000rpm for 60min, adding 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone with the mass 0.08 time that of the composite particles, stirring at 60 ℃ and 1500rpm for 60min, then performing suction filtration, washing with absolute ethyl alcohol for 3 times, and drying at 60 ℃ for 3h to obtain pretreated composite particles; mixing the pretreated composite particles, tetramethyldiethoxydisilane, monobutyltin oxide and N, N-dimethylformamide according to a mass ratio of 1.2;
(4) Mixing modified polyurethane, self-made filler and 0.05g/mL polyethylene glycol solution according to a mass ratio of 1.2.
Example 2
(1) Mixing trifluoroacetic acid, diethylenetriamine and xylene according to a mass ratio of 1.45; mixing polytetrahydrofuran 1000, N-dimethylformamide and a corrosion inhibitor according to a mass ratio of 1.3;
(2) Dispersing graphite phase nitrogen carbide in absolute ethyl alcohol with 6 times of the mass of the graphite phase nitrogen carbide, adding sodium hydroxide until the pH of the solution is 10.5, adding aluminum sec-butoxide, n-butanol, ethyl acetate and deionized water according to a mass ratio of 1; carrying out heat treatment on the self-made filler precursor for 63min at 950 ℃ under the protection of nitrogen to obtain composite particles;
(3) Dispersing the composite particles in absolute ethyl alcohol with the mass 32 times that of the composite particles, stirring at 1100rpm for 74min, adding 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone with the mass 0.14 time that of the composite particles, stirring at 70 ℃ and 1750rpm for 75min, performing suction filtration, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 4.5h to obtain pretreated composite particles; mixing the pretreated composite particles, tetramethyldiethoxydisilane, monobutyltin oxide and N, N-dimethylformamide according to a mass ratio of 1: 0.002;
(4) Mixing modified polyurethane, self-made filler and 0.13g/mL polyethylene glycol solution according to the mass ratio of 1.
Example 3
(1) Mixing trifluoroacetic acid, diethylenetriamine and xylene according to a mass ratio of 1.6; mixing polytetrahydrofuran 1000, N-dimethylformamide and a corrosion inhibitor according to a mass ratio of 1.4;
(2) Dispersing graphite phase nitrogen carbide in absolute ethyl alcohol with the mass of 9 times of that of the graphite phase nitrogen carbide, adding sodium hydroxide until the pH of the solution is 11, adding aluminum sec-butoxide, n-butanol, ethyl acetate and deionized water according to a mass ratio of 1.2; carrying out heat treatment on the self-made filler precursor for 70min at 1000 ℃ under the protection of nitrogen to obtain composite particles;
(3) Dispersing the composite particles in absolute ethyl alcohol with the mass 38 times that of the composite particles, stirring at 1200rpm for 88min, adding 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone with the mass 0.2 time that of the composite particles, stirring at 80 ℃ and 2000rpm for 90min, then performing suction filtration, washing 5 times with absolute ethyl alcohol, and drying at 70 ℃ for 6h to obtain pretreated composite particles; mixing the pretreated composite particles, tetramethyldiethoxydisilane, monobutyltin oxide and N, N-dimethylformamide according to a mass ratio of 1.4;
(4) Mixing the modified polyurethane, the self-made filler and a polyethylene glycol solution with the concentration of 0.2g/mL according to the mass ratio of 1.
Comparative example 1
Comparative example 1 differs from example 2 in that step (1) is different, step (1) being changed to: mixing diethylenetriamine, xylene, 4-chloro-3, 6-dihydroxypyridazine according to the mass ratio of 1: 0.45; mixing polytetrahydrofuran 1000, N-dimethylformamide and a corrosion inhibitor according to a mass ratio of 1.3, vacuumizing for 4 times, adding 4-chloro-6-methyl m-phenylene diisocyanate, N-dimethylformamide, dibutyltin dilaurate, and 4-chloro-6-methyl m-phenylene diisocyanate to polytetrahydrofuran 1000 according to a mass ratio of 1.003. The rest of the preparation method is the same as the example 2.
Comparative example 2
Comparative example 2 differs from example 2 in that step (1) is different, step (1) being changed to: mixing trifluoroacetic acid, diethylenetriamine and xylene according to a mass ratio of 1.45; the modified polyurethane is prepared by mixing polytetrahydrofuran 1000, N-dimethylformamide and a corrosion inhibitor according to a mass ratio of 1:0.2, vacuumizing for 4 times, adding 4-chloro-6-methyl-m-phenylene diisocyanate, N-dimethylformamide, dibutyltin dilaurate, 4-chloro-6-methyl-m-phenylene diisocyanate and polytetrahydrofuran 1000 according to a mass ratio of 1: 0.003. The rest of the preparation method is the same as example 2.
Comparative example 3
Comparative example 3 differs from example 2 in that there is no step (2) and step (3) is changed to: dispersing graphite phase carbon nitride in absolute ethyl alcohol with the mass 32 times that of the graphite phase carbon nitride, stirring at 1100rpm for 74min, adding 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone with the mass 0.14 time that of the graphite phase carbon nitride, stirring at 1750rpm for 75min at 70 ℃, performing suction filtration, washing for 4 times by using the absolute ethyl alcohol, and drying at 65 ℃ for 4.5h to obtain pretreated carbon nitride; mixing the pretreated carbon nitride, the tetramethyldiethoxydisilane, the monobutyltin oxide and the N, N-dimethylformamide according to a mass ratio of 1. The rest of the preparation method is the same as the example 2.
Comparative example 4
Comparative example 4 differs from example 2 in that step (3) is different, step (3) being changed to: mixing the composite particles, tetramethyl diethoxy disilane, monobutyl tin oxide and N, N-dimethylformamide according to a mass ratio of 1. The rest of the preparation method is the same as example 2.
Comparative example 5
Comparative example 5 differs from example 2 in that step (3) is different, step (3) being changed to: dispersing the composite particles in absolute ethyl alcohol with the mass 32 times that of the composite particles, stirring at 1100rpm for 74min, adding 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone with the mass 0.14 time that of the composite particles, stirring at 70 ℃ and 1750rpm for 75min, performing suction filtration, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 4.5h to obtain pretreated composite particles; mixing the pretreated composite particles, tetramethyldiethoxydisilane, monobutyltin oxide and N, N-dimethylformamide according to a mass ratio of 1.3. The rest of the preparation method is the same as the example 2.
Examples of effects
The following table 1 shows the performance analysis results of the wear-resistant nano-coating for magnetic material products using examples 1 to 3 and comparative examples 1 to 5 of the present invention.
TABLE 1
Comparing the surface condition data of the embodiment with that of the comparative example, the invention utilizes trifluoroacetic acid, diethylenetriamine and 4-chloro-3, 6-dihydroxypyridazine to form a corrosion inhibitor, so that the coating has salt fog resistance, and then the corrosion inhibitor is polymerized with polytetrahydrofuran and 4-chloro-6-methyl m-phenylene diisocyanate to obtain the modified polyurethane, after the coating is cured, a coating with low surface energy is formed, so that the salt fog cannot stay on the surface of the coating for a long time, in addition, the modified polyurethane can be adsorbed on the surface of a metal magnetic material to form a stable protective film, so that the salt fog resistance of the coating is enhanced; the comparison of the experimental data of the voltage breakdown resistance of the embodiment and the comparative example shows that the graphite-phase carbon nitride is used as the raw material, the deposition treatment is carried out, the alumina is uniformly distributed among the carbon nitride sheet layers and is condensed to form alumina aerogel, the tunnel current between the carbon nitride sheets is inhibited, and the voltage resistance of the coating is improved; then carrying out heat treatment to form micro-nano lapped network structure composite particles, and improving the voltage resistance of the coating; then 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone, tetramethyl diethoxydisilane, octamethylcyclotetrasiloxane and aminopropyl methyldimethoxysilane are subjected to polymerization modification on the surface to form an insulating protective film, so that the voltage resistance of the coating is improved, and the coating can be combined with modified polyurethane through mutual crosslinking, so that the insulating defect is reduced, and the voltage resistance is improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The wear-resistant nano coating for the magnetic material product is characterized by mainly comprising modified polyurethane, self-made filler, closed isocyanate curing agent and polyethylene glycol solution.
2. The wear-resistant nano coating for the magnetic material products as claimed in claim 1, wherein the modified polyurethane is prepared from trifluoroacetic acid, diethylenetriamine, 4-chloro-3, 6-dihydroxypyridazine, polytetrahydrofuran, 4-chloro-6-methyl m-phenylene diisocyanate.
3. The wear-resistant nano coating for the magnetic material product as claimed in claim 1, wherein the self-made filler is prepared by a method comprising the steps of performing deposition treatment on graphite-phase nitrogen carbide to obtain a precursor of the self-made filler; dispersing graphite phase nitrogen carbide in absolute ethyl alcohol, adjusting pH, adding aluminum sec-butoxide, n-butanol, ethyl acetate and deionized water, stirring, cooling to room temperature, standing for aging, placing in a high-pressure kettle, reacting at high temperature and high pressure in a nitrogen atmosphere, purging with nitrogen, and annealing; then carrying out heating treatment to obtain composite particles; the heating treatment is to carry out high-temperature heat treatment on the self-made filler precursor for a period of time under the protection of nitrogen; then, 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone, tetramethyldiethoxydisilane, octamethylcyclotetrasiloxane and aminopropylmethyldimethoxysilane were used for modification.
4. The wear-resistant nano coating for the magnetic material products as claimed in claim 1, wherein the blocked isocyanate curing agent is one or more of hexamethylene diisocyanate trimer, isophorone diisocyanate trimer or hexamethylene diisocyanate biuret.
5. A preparation method of the wear-resistant nano coating for the magnetic material product is characterized by comprising the following preparation steps of:
(1) Polytetrahydrofuran 1000, N-dimethylformamide and corrosion inhibitor are mixed according to the mass ratio
1, the ratio of the components is as follows, namely, 0.1-0.2;
(2) Carrying out deposition treatment on graphite phase nitrogen carbide to obtain a filler precursor; then carrying out heating treatment to obtain composite particles;
(3) Mixing the pretreated composite particles, tetramethyldiethoxydisilane, monobutyltin oxide and N, N-dimethylformamide according to a mass ratio of 1.001;
(4) Mixing the modified polyurethane, the self-made filler and the polyethylene glycol solution according to the mass ratio of 1: 0.002-1: 0.04.
6. The method for preparing the wear-resistant nano coating for the magnetic material product according to claim 5, wherein the preparation method of the corrosion inhibitor in the step (1) comprises the following steps: mixing trifluoroacetic acid, diethylenetriamine and xylene according to a mass ratio of 1.3.
7. The method for preparing the wear-resistant nano coating for the magnetic material product according to claim 5, wherein the deposition treatment of the step (2) comprises the following specific steps: dispersing graphite phase nitrogen carbide in absolute ethyl alcohol with the mass of 3-9 times of that of the graphite phase nitrogen carbide, adding sodium hydroxide until the pH value of the solution is 10-11, stirring at the mass ratio of 1.
8. The preparation method of the wear-resistant nano coating for the magnetic material product according to claim 5, wherein the heating treatment in the step (2) comprises the following specific steps: and (3) carrying out heat treatment on the self-made filler precursor for 56-70 min at 900-1000 ℃ under the protection of nitrogen.
9. The method for preparing the wear-resistant nano coating for the magnetic material product according to claim 5, wherein the preparation method of the pre-treated composite particles in the step (3) is as follows: dispersing the composite particles in absolute ethyl alcohol with the mass of 26-38 times of that of the composite particles, stirring at 1000-1200 rpm for 60-88 min, adding 2-hydroxy-4- (3-triethoxysilylpropoxy) benzophenone with the mass of 0.08-0.2 time of that of the composite particles, stirring at 1500-2000 rpm for 60-90 min at 60-80 ℃, performing suction filtration, washing with absolute ethyl alcohol for 3-5 times, and drying at 60-70 ℃ for 3-6 h.
10. The method for preparing the wear-resistant nano coating for the magnetic material product according to claim 5, wherein the concentration of the polyethylene glycol solution in the step (4) is 0.05-0.2 g/mL.
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| CN117924909A (en) * | 2023-02-08 | 2024-04-26 | 苏州赛荣建筑装饰工程有限公司 | Wave-absorbing insulating foam plastic and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117924909A (en) * | 2023-02-08 | 2024-04-26 | 苏州赛荣建筑装饰工程有限公司 | Wave-absorbing insulating foam plastic and preparation method thereof |
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