CN117165152A - Preparation method of neodymium-iron-boron magnet anticorrosive paint with high surface tension - Google Patents
Preparation method of neodymium-iron-boron magnet anticorrosive paint with high surface tension Download PDFInfo
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- CN117165152A CN117165152A CN202311063654.4A CN202311063654A CN117165152A CN 117165152 A CN117165152 A CN 117165152A CN 202311063654 A CN202311063654 A CN 202311063654A CN 117165152 A CN117165152 A CN 117165152A
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 45
- 239000003973 paint Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000000576 coating method Methods 0.000 claims abstract description 43
- 239000011248 coating agent Substances 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 26
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000004593 Epoxy Substances 0.000 claims abstract description 22
- 239000003822 epoxy resin Substances 0.000 claims abstract description 20
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003377 acid catalyst Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 229910000077 silane Inorganic materials 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 25
- 238000005507 spraying Methods 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000000049 pigment Substances 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- 239000011260 aqueous acid Substances 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims description 2
- 239000004035 construction material Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 claims 1
- 239000006087 Silane Coupling Agent Substances 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 125000003700 epoxy group Chemical group 0.000 abstract description 5
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 238000004132 cross linking Methods 0.000 abstract description 2
- 238000004513 sizing Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- -1 phenolic amine Chemical class 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 238000011160 research Methods 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 238000009832 plasma treatment Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- GTMJWNJPVRGQIH-UHFFFAOYSA-N [Ni].[Cu].[Ni].[B].[Fe].[Nd] Chemical compound [Ni].[Cu].[Ni].[B].[Fe].[Nd] GTMJWNJPVRGQIH-UHFFFAOYSA-N 0.000 description 2
- OPXJEFFTWKGCMW-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Ni].[Cu] OPXJEFFTWKGCMW-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229920006334 epoxy coating Polymers 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Abstract
The invention relates to the technical field of paint, and aims to provide a preparation method of a high-surface-tension neodymium-iron-boron magnet anticorrosive paint. Comprising the following steps: adding epoxy silane and propylene glycol methyl ether into a reaction kettle, and stirring and uniformly mixing under a heating condition; dissolving an acid catalyst in deionized water to obtain an acid catalyst aqueous solution; adding an acid catalyst aqueous solution into a reaction kettle, and stirring and reacting at 30 ℃ to obtain a modified dispersion liquid; adding silicon dioxide into a reaction kettle, stirring for 2 hours at 30 ℃, and cooling to normal temperature to obtain modified hydrophilic silicon dioxide dispersion liquid; and adding the epoxy resin and the sizing agent into the dispersion liquid, and stirring and dispersing for 2 hours to obtain the neodymium-iron-boron anticorrosive paint. The invention fully plays the characteristic that the surface of the hydrophilic silicon dioxide contains hydrophilic functional groups, and can generate crosslinking reaction with epoxy resin to form a network structure after being modified by the silane coupling agent with epoxy groups. Not only effectively improves the surface tension of the coating, but also improves the corrosion resistance of the coating.
Description
Technical Field
The invention belongs to the technical field of paint, and relates to a preparation method of a high-surface-tension neodymium-iron-boron magnet anticorrosive paint.
Background
The neodymium-iron-boron permanent magnet material has high remanence and maximum magnetic energy product, good dynamic recovery characteristic and high cost performance, and is widely applied to the fields of rail transit, energy conservation, new energy automobiles, permanent magnet motors and the like. The neodymium-iron-boron magnet microstructure consists of a main phase, a crystal boundary neodymium-rich phase, a boron-rich phase and the like, wherein the neodymium-rich phase is easily corroded by water vapor and oxygen of air, so that the magnetic performance is invalid, and a protective layer is required to be formed on the surface of the magnet, so that the service life is prolonged. Organic corrosion protection coatings are currently the dominant application technology, with epoxy-based materials being the most common.
An adhesion process is required in the production process of the permanent magnet motor to ensure the mechanical reliability of the rotor at high speed rotation (12000 r/min). However, the surface of the epoxy coating contains hydrophobic functional groups and has a relatively low surface tension (typically 28-30 mN/m); the phenomena of infirm and even degumming easily occur during bonding, and great potential safety hazards exist.
Researchers have conducted researches on the surface hydrophilicity of a coating/a plating layer on a neodymium iron boron magnet, and reported research results are shown as Chinese patent document CN 116037431A, and a method for improving the surface tension of the coating is described, wherein the coating with the surface tension of more than or equal to 50mN/m can be obtained under plasma treatment, but the surface tension of the coating after the plasma treatment gradually decreases along with the time, and a new technological process is needed to be added for the plasma treatment. As another example, the "increase in surface tension of NdFeB Nickel copper Nickel coating" by Gao Zhong et al (contemporary chemical research, 2021, 12:167-169); the control method provided by the document can improve the surface tension of the nickel-copper-nickel coating, the initial surface tension is more than or equal to 42mN/m, and the initial surface tension is more than or equal to 36mN/m after being stored for four months, but the report is only limited to an electroplating coating system.
Therefore, the preparation method of the high-surface-tension neodymium-iron-boron magnet anticorrosive paint is provided, high surface tension is realized at the source of coating preparation, so that the phenomena of infirm and even degumming easily occur when the neodymium-iron-boron magnet is bonded, and the preparation method has a real demand.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and providing a preparation method of a neodymium iron boron magnet anticorrosive paint with high surface tension.
In order to solve the technical problems, the invention adopts the following solutions:
the preparation method of the neodymium-iron-boron magnet anticorrosive paint with high surface tension comprises the following steps:
(1) Taking pigment, filler and ether solvent according to the mass ratio of 1:1:2, and uniformly mixing; after sand grinding treatment, slurry is obtained;
(2) Epoxy silane and propylene glycol methyl ether are taken according to the mass ratio of 1-2:200-400 and added into a reaction kettle; stirring under heating condition, and mixing completely and uniformly to obtain mixed solution A;
(3) Dissolving an acid catalyst in deionized water to obtain an acid catalyst aqueous solution with the mass percent of 10-20%;
(4) Adding the aqueous acid catalyst solution into a reaction kettle according to the mass ratio of the aqueous acid catalyst solution to the mixed solution A of 1-2:1000, and mixing with the mixed solution A; then stirring and reacting for 20min at 30 ℃ to obtain modified dispersion liquid;
(5) Taking silicon dioxide particles and modified dispersion liquid according to the mass ratio of 4-8:100-200, mixing and stirring for 2h at 30 ℃; cooling to normal temperature to obtain modified hydrophilic silica dispersion liquid;
(6) And mixing epoxy resin, slurry and modified hydrophilic silica dispersion liquid according to the mass ratio of 100-200:100-200, and stirring and dispersing for 2 hours to obtain the neodymium-iron-boron magnet anticorrosive paint with high surface tension.
In the step (1), pigment, filler and ether solvent are stirred and mixed uniformly in a mixing bucket, and then the mixture is moved into a sanding tank to be sanded for 10 hours to obtain slurry.
As a preferred embodiment of the present invention, in the step (1), the pigment is at least one of iron oxide red, chrome yellow or cobalt blue; the filler is at least one of calcium carbonate, mica or talcum powder; the ether solvent is propylene glycol methyl ether.
In the preferred embodiment of the present invention, in the step (2), the epoxysilane is one of γ - (2, 3-glycidoxy) propyltrimethoxysilane and γ - (2, 3-glycidoxy) propyltriethoxysilane; the heating temperature is controlled to be 30 ℃, and the stirring time is controlled to be 20min.
As a preferred embodiment of the present invention, in the step (3), the acid catalyst is one or more of acetic acid, formic acid or hydrochloric acid solution.
As a preferable mode of the invention, in the step (5), the silica particles are hydrophilic silica, and the particle diameter is less than or equal to 100nm.
In the preferred embodiment of the present invention, in the step (6), the epoxy resin is one or a combination of two of E44 epoxy resin and E51 epoxy resin.
The invention further provides a use method of the neodymium iron boron anticorrosive paint with high surface tension, which comprises the following steps:
(1) Mixing the anticorrosive paint with the epoxy curing agent according to the mass ratio of 100:6.5-15; stirring uniformly to obtain a material for construction;
(2) Spraying the construction material on the surface of the neodymium-iron-boron magnet, and curing to form a coating after drying treatment; the spraying dosage is controlled to ensure that the thickness of the coating is 25-35 mu m.
As a preferable scheme of the invention, the spraying is performed by using compressed air which is dried and cooled, and the spraying pressure is controlled to be 0.5MPa.
As a preferable scheme of the invention, the drying treatment is to send the sprayed neodymium-iron-boron magnet into a baking oven, heat the neodymium-iron-boron magnet to 80 ℃ for 30min, and then cool the neodymium-iron-boron magnet naturally.
Description of the inventive principles:
1. hydrophilic silicon dioxide is added into the coating, so that the surface tension of the coating can be improved after the hydrophilic silicon dioxide is cured, and the corrosion resistance can be enhanced. The existing common technology is to disperse the silicon dioxide into the paint directly by a mechanical way, but the dispersion way is easy to cause agglomeration of silicon dioxide powder, and is difficult to achieve even nano-level dispersion in the true sense.
2. In the prior art, the usual methods of application for hydrophilic silica are: it is added to aqueous systems to improve the flowability of the aqueous coating and to enhance the mechanical properties of the coating. However, in organic systems, hydrophilic silica does not disperse well after addition. According to the invention, the hydrophilic silicon dioxide is modified by using the silane coupling agent, so that the hydrophilic silicon dioxide can be well dispersed in the solvent-based epoxy paint.
3. The hydrophilic silicon dioxide can improve the corrosion resistance, weather resistance, strength, hardness, ultraviolet resistance and the like of the coating. In addition, in the film forming process, the nano silicon dioxide particles can effectively improve the interfacial bonding tension between the high polymers and the filler, and achieve the effects of enhancing and repairing defects, thereby effectively improving the mechanical properties of the coating after film forming. Hydrophilic silica is therefore widely used in coating preparation techniques, but generally only the properties mentioned above are exploited.
The prior art discloses no use of hydrophilic silica as a means for increasing the surface tension of a coating, and in particular, there is no description of the use of a silane coupling agent to modify silica to thereby increase the surface tension of a coating.
4. According to the invention, silicon dioxide is dispersed in the epoxy paint by a silane coupling agent method. So that the bonding of chemical bonds between the silica and the interface of the epoxy polymer can be formed instead of a simple intermixing of the two components. The specific implementation process can be described as follows: under the action of an acid catalyst, the silane with epoxy groups can be hydrolyzed to generate silanol to be combined with inorganic silicon dioxide, and meanwhile, the epoxy groups in the silane can be combined with organic matters in a reaction way. Therefore, a molecular bridge is erected between the interfaces of the inorganic matters and the organic matters through the silane coupling agent, and the neodymium-iron-boron magnet anticorrosive paint with high surface tension is prepared.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention fully plays the characteristic that the surface of the hydrophilic silicon dioxide contains hydrophilic functional groups, and can generate crosslinking reaction with epoxy resin to form a reticular structure after being modified by the silane coupling agent with epoxy groups. Not only effectively improves the surface tension of the coating, but also improves the corrosion resistance of the coating.
2. After the hydrophilic silicon dioxide is modified by the silane coupling agent with epoxy groups, the modified silicon dioxide is not only applicable to aqueous systems, but also applicable to organic solvent systems, and can be compounded with other organic resins, so that more preferable scheme combinations are realized.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present invention, which is described by the following specific examples. The example embodiments may be embodied in many forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the example embodiments to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Example 1:
1. preparation of the slurry
Taking iron oxide red, calcium carbonate powder and propylene glycol methyl ether according to the mass ratio of 1:1:2, and uniformly stirring and mixing in a mixing barrel; then, the slurry was transferred to a sand tank and sand-ground for 10 hours to obtain a slurry.
2. Preparation of high-surface-tension neodymium-iron-boron magnet anticorrosive paint
(1) Taking epoxy silane and propylene glycol methyl ether according to the mass ratio of 1:400, and adding the epoxy silane and the propylene glycol methyl ether into a reaction kettle; stirring at 30deg.C for 20min, and mixing completely to obtain mixed solution A; the epoxy silane is selected from gamma- (2, 3-glycidoxy) propyl trimethoxy silane;
(2) Dissolving formic acid into deionized water to obtain a formic acid aqueous solution with the mass percent of 10%;
(3) Adding the aqueous solution of hydrochloric acid into a reaction kettle filled with the mixed solution A according to the mass ratio of 1:1000, and stirring and reacting for 20min at 30 ℃ to obtain modified dispersion liquid;
(4) Adding hydrophilic silicon dioxide (particle size is less than or equal to 100 nm) into the reaction kettle filled with the modified dispersion liquid in the step (3) according to the mass ratio of 8:100, stirring for 2h at 30 ℃, and cooling to normal temperature to obtain the modified hydrophilic silicon dioxide dispersion liquid;
(5) And (3) adding E44 epoxy resin and slurry into the modified hydrophilic silicon dioxide dispersion liquid according to the mass ratio of 150:150:150, stirring and dispersing for 2 hours to obtain the neodymium-iron-boron magnet anticorrosive paint with high surface tension.
3. Compounding and coating
(1) Uniformly stirring and mixing the neodymium-iron-boron magnet anticorrosive paint with high surface tension with a phenolic amine epoxy curing agent (T31) according to the ratio of 100:8;
(2) Spraying the mixed coating on the surface of the neodymium-iron-boron magnet, wherein compressed air subjected to drying and cooling is used in spraying, and the spraying pressure is 0.5MPa;
(3) Feeding the sprayed neodymium-iron-boron magnet into a baking furnace, heating to 80 ℃ and keeping for 30min; and after natural cooling, solidifying on the surface of the NdFeB magnet to form a coating with high surface tension. The spraying dosage in the last step is controlled to ensure that the thickness of the film formed after drying is 25-35 mu m.
Example 2:
1. preparation of the slurry
Taking medium chrome yellow, calcium carbonate, mica powder and propylene glycol methyl ether according to the mass ratio of 1:0.5:0.5:2, and uniformly stirring and mixing in a mixing barrel; then, the slurry was transferred to a sand tank and sand-ground for 10 hours to obtain a slurry.
2. Preparation of high-surface-tension neodymium-iron-boron magnet anticorrosive paint
(1) Epoxy silane and propylene glycol methyl ether are taken according to the mass ratio of 2:200 and added into a reaction kettle; stirring at 30deg.C for 20min, and mixing completely to obtain mixed solution A; the epoxy silane is selected from gamma- (2, 3-glycidoxy) propyl triethoxy silane;
(2) Dissolving hydrochloric acid into deionized water to obtain a hydrochloric acid aqueous solution with the mass percent of 20%;
(3) Adding formic acid aqueous solution into a reaction kettle filled with mixed solution A according to the mass ratio of 2:1000, and stirring and reacting for 20min at 30 ℃ to obtain modified dispersion liquid;
(4) Adding hydrophilic silicon dioxide (particle size is less than or equal to 100 nm) into the reaction kettle filled with the modified dispersion liquid in the step (3) according to the mass ratio of 4:200, stirring for 2h at 30 ℃, and cooling to normal temperature to obtain the modified hydrophilic silicon dioxide dispersion liquid;
(5) And (3) adding E51 epoxy resin and slurry into the modified hydrophilic silicon dioxide dispersion liquid according to the mass ratio of 100:100:100, and stirring and dispersing for 2 hours to obtain the neodymium-iron-boron magnet anticorrosive paint with high surface tension.
3. Compounding and coating
(1) Uniformly stirring and mixing the neodymium-iron-boron magnet anticorrosive paint with high surface tension with a phenolic amine epoxy curing agent (T31) according to the ratio of 100:6.5;
(2) Spraying the mixed coating on the surface of the neodymium-iron-boron magnet, wherein compressed air subjected to drying and cooling is used in spraying, and the spraying pressure is 0.5MPa;
(3) Feeding the sprayed neodymium-iron-boron magnet into a baking furnace, heating to 80 ℃ and keeping for 30min; and after natural cooling, solidifying on the surface of the NdFeB magnet to form a coating with high surface tension. The spraying dosage in the last step is controlled to ensure that the thickness of the film formed after drying is 25-35 mu m.
Example 3:
1. preparation of the slurry
Taking cobalt blue, iron oxide red, calcium carbonate, talcum powder and propylene glycol methyl ether according to the mass ratio of 0.5:0.5:0.5:0.5:2, and uniformly stirring and mixing in a mixing barrel; then, the slurry was transferred to a sand tank and sand-ground for 10 hours to obtain a slurry.
2. Preparation of high-surface-tension neodymium-iron-boron magnet anticorrosive paint
(1) Epoxy silane and propylene glycol methyl ether are taken according to the mass ratio of 1.5:225 and added into a reaction kettle; stirring at 30deg.C for 20min, and mixing completely to obtain mixed solution A; the epoxy silane is selected from gamma- (2, 3-glycidoxy) propyl triethoxy silane;
(2) Mixing hydrochloric acid and acetic acid according to the mass ratio of 1:2, and dissolving the mixture in deionized water to obtain an acid catalyst aqueous solution with the mass percentage of 15%;
(3) Adding an acid catalyst aqueous solution into a reaction kettle filled with a mixed solution A according to the mass ratio of 1.5:1000, and stirring and reacting for 20min at 30 ℃ to obtain a modified dispersion liquid;
(4) Adding hydrophilic silicon dioxide (particle size is less than or equal to 100 nm) into the reaction kettle filled with the modified dispersion liquid in the step (3) according to the mass ratio of 6:150, stirring for 2h at 30 ℃, and cooling to normal temperature to obtain the modified hydrophilic silicon dioxide dispersion liquid;
(5) And adding the E51 epoxy resin, the E44 epoxy resin and the sizing agent into the modified hydrophilic silicon dioxide dispersion liquid according to the mass ratio of 100:100:200:200, and stirring and dispersing for 2 hours to obtain the neodymium-iron-boron magnet anticorrosive paint with high surface tension.
3. Compounding and coating
(1) Uniformly stirring and mixing the neodymium-iron-boron magnet anticorrosive paint with high surface tension with a phenolic amine epoxy curing agent (T31) according to the ratio of 100:15;
(2) Spraying the mixed coating on the surface of the neodymium-iron-boron magnet, wherein compressed air subjected to drying and cooling is used in spraying, and the spraying pressure is 0.5MPa;
(3) Feeding the sprayed neodymium-iron-boron magnet into a baking furnace, heating to 80 ℃ and keeping for 30min; and after natural cooling, solidifying on the surface of the NdFeB magnet to form a coating with high surface tension. The spraying dosage in the last step is controlled to ensure that the thickness of the film formed after drying is 25-35 mu m.
Comparative example 1
E44 epoxy resin without adding high-surface Zhang Lijiang material is taken, stirred and mixed uniformly with phenolic amine epoxy curing agent (T31) according to a ratio of 100:8, and then directly sprayed on the surface of the same substrate according to the method of the example 1.
Comparative example 2
E51 epoxy resin without adding high surface Zhang Lijiang material is taken, stirred and mixed uniformly with phenolic amine epoxy curing agent (T31) according to a ratio of 100:6.5, and then directly sprayed on the same surface of a substrate according to the method of the example 1.
Comparative example 3
100 parts by mass of E44 epoxy resin and 100 parts by mass of E51 epoxy resin without adding high-surface Zhang Lijiang materials are taken, uniformly mixed with phenolic amine epoxy curing agent (T31) according to a ratio of 100:15, and then directly sprayed on the surface of the same substrate according to the method of example 1.
Comparative example 4
According to patent CN202310062584, the dyne value of untreated NdFeB surfaces is generally 28-30mN/m.
Comparative example 5
According to the article about the improvement of the surface tension of the neodymium-iron-boron nickel-copper-nickel coating in journal of modern chemical engineering research, the initial surface dyne value after the neodymium-iron-boron nickel-copper-nickel coating is more than or equal to 42mN/m, and the surface dyne value after 4 months of storage is more than or equal to 36mN/m.
The surface dyne value of the magnet surface coating in each of examples and comparative examples was tested by the following method:
the test ink (surface tension test range 28-72 mN/m) produced by Plasmamat corporation, germany, is applied to the surface of the coating, if the liquid wets the surface (i.e. the liquid spreads continuously over the surface), the surface tension of the tested coating is higher than the nominal surface tension of the test ink, the above process is repeated with a higher grade of test ink until the liquid no longer wets the surface (i.e. the liquid shrinks at the surface), the nominal surface tension on the last package of test ink which wets at the surface and retains 2S of non-shrinkage being the surface tension of the tested coating. The test results are shown in Table 1.
TABLE 1
| Paint sample | Surface dyne value (mN/m) |
| Example 1 | 54-56 |
| Example 2 | 46-48 |
| Example 3 | 50-52 |
| Comparative example 1 | 30-32 |
| Comparative example 2 | 30-32 |
| Comparative example 3 | 30-32 |
| Comparative example 4 | 28-30 |
| Comparative example 5 | 36 |
As can be seen from the test data in table 1, the present invention is based on an epoxy resin film forming material that has been treated with a modified hydrophilic silica. The surface tension of the coating formed after solidification of the finally obtained neodymium-iron-boron magnet anticorrosive coating product can reach 46-52 mN/m, and the requirement of the adhesive surface tension can be met (generally more than 36mN/m is required).
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (10)
1. The preparation method of the high-surface-tension neodymium-iron-boron magnet anticorrosive paint is characterized by comprising the following steps of:
(1) Taking pigment, filler and ether solvent according to the mass ratio of 1:1:2, and uniformly mixing; after sand grinding treatment, slurry is obtained;
(2) Epoxy silane and propylene glycol methyl ether are taken according to the mass ratio of 1-2:200-400 and added into a reaction kettle; stirring under heating condition, and mixing completely and uniformly to obtain mixed solution A;
(3) Dissolving an acid catalyst in deionized water to obtain an acid catalyst aqueous solution with the mass percent of 10-20%;
(4) Adding the aqueous acid catalyst solution into a reaction kettle according to the mass ratio of the aqueous acid catalyst solution to the mixed solution A of 1-2:1000, and mixing with the mixed solution A; then stirring and reacting for 20min at 30 ℃ to obtain modified dispersion liquid;
(5) Taking silicon dioxide particles and modified dispersion liquid according to the mass ratio of 4-8:100-200, mixing and stirring for 2h at 30 ℃; cooling to normal temperature to obtain modified hydrophilic silica dispersion liquid;
(6) And mixing epoxy resin, slurry and modified hydrophilic silica dispersion liquid according to the mass ratio of 100-200:100-200, and stirring and dispersing for 2 hours to obtain the neodymium-iron-boron magnet anticorrosive paint with high surface tension.
2. The method according to claim 1, wherein in the step (1), the pigment, the filler and the ether solvent are stirred and mixed uniformly in a mixing drum, and then the mixture is moved to a sanding tank for sanding for 10 hours to obtain the slurry.
3. The method of claim 1, wherein in step (1), the pigment is at least one of iron red, chrome yellow, or cobalt blue; the filler is at least one of calcium carbonate, mica or talcum powder; the ether solvent is propylene glycol methyl ether.
4. The method according to claim 1, wherein in the step (2), the epoxysilane is one of γ - (2, 3-glycidoxy) propyltrimethoxysilane and γ - (2, 3-glycidoxy) propyltriethoxysilane; the heating temperature is controlled to be 30 ℃, and the stirring time is controlled to be 20min.
5. The method of claim 1, wherein in step (3), the acid catalyst is one or a combination of acetic acid, formic acid, or hydrochloric acid solutions.
6. The method according to claim 1, wherein in the step (5), the silica particles are hydrophilic silica having a particle diameter of 100nm or less.
7. The method of claim 1, wherein in step (6), the epoxy resin is one or a combination of two of E44 epoxy resin and E51 epoxy resin.
8. The method for using the high-surface-tension neodymium iron boron anticorrosive paint prepared by the method of claim 1, which is characterized by comprising the following steps:
(1) Mixing the anticorrosive paint with the epoxy curing agent according to the mass ratio of 100:6.5-15; stirring uniformly to obtain a material for construction;
(2) Spraying the construction material on the surface of the neodymium-iron-boron magnet, and curing to form a coating after drying treatment; the spraying dosage is controlled to ensure that the thickness of the coating is 25-35 mu m.
9. The method according to claim 8, wherein the spraying is performed using compressed air that is dried and cooled, and the spraying pressure is controlled to be 0.5MPa.
10. The method according to claim 8, wherein the drying treatment is that the sprayed neodymium iron boron magnet is sent to a baking oven, heated to 80 ℃ for 30min, and then naturally cooled.
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| CN116285590A (en) * | 2023-04-24 | 2023-06-23 | 陕西科技大学 | Fluorinated silica/water-based epoxy resin composite anticorrosive paint and preparation method thereof |
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| US20020177646A1 (en) * | 2001-03-15 | 2002-11-28 | Cabot Corporation | Corrosion-resistant coating composition |
| US20120034458A1 (en) * | 2010-02-09 | 2012-02-09 | Vacuumschmelze Gmbh & Co. Kg | Lacquer Composition and Use Thereof |
| KR102051586B1 (en) * | 2019-03-07 | 2019-12-05 | 한토산업(주) | Paint composition for waterproof, anticorrosion and reinforcement including ceramic, fiber and polymer resin, and method for surface protection, repair and reinforcement using the same |
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