CN117995473A - Wear-resistant corona-resistant enamelled copper round wire - Google Patents
Wear-resistant corona-resistant enamelled copper round wire Download PDFInfo
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- CN117995473A CN117995473A CN202410287878.1A CN202410287878A CN117995473A CN 117995473 A CN117995473 A CN 117995473A CN 202410287878 A CN202410287878 A CN 202410287878A CN 117995473 A CN117995473 A CN 117995473A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 34
- 239000010949 copper Substances 0.000 title claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 111
- 239000007788 liquid Substances 0.000 claims abstract description 64
- 239000011248 coating agent Substances 0.000 claims abstract description 58
- 238000000576 coating method Methods 0.000 claims abstract description 58
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000002131 composite material Substances 0.000 claims abstract description 37
- 239000004962 Polyamide-imide Substances 0.000 claims abstract description 32
- 229920002312 polyamide-imide Polymers 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000003973 paint Substances 0.000 claims abstract description 22
- 229920000728 polyester Polymers 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 548
- 239000000243 solution Substances 0.000 claims description 348
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 96
- 238000003756 stirring Methods 0.000 claims description 95
- 239000007790 solid phase Substances 0.000 claims description 79
- 239000006185 dispersion Substances 0.000 claims description 73
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 54
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 54
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 54
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 54
- QTKPMCIBUROOGY-UHFFFAOYSA-N 2,2,2-trifluoroethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)F QTKPMCIBUROOGY-UHFFFAOYSA-N 0.000 claims description 48
- 239000008367 deionised water Substances 0.000 claims description 45
- 229910021641 deionized water Inorganic materials 0.000 claims description 45
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 45
- 239000012279 sodium borohydride Substances 0.000 claims description 45
- 239000002253 acid Substances 0.000 claims description 42
- 238000009413 insulation Methods 0.000 claims description 39
- OEIMLTQPLAGXMX-UHFFFAOYSA-I tantalum(v) chloride Chemical compound Cl[Ta](Cl)(Cl)(Cl)Cl OEIMLTQPLAGXMX-UHFFFAOYSA-I 0.000 claims description 38
- 239000002904 solvent Substances 0.000 claims description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 29
- 239000007864 aqueous solution Substances 0.000 claims description 27
- 239000007787 solid Substances 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 230000001681 protective effect Effects 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 11
- 238000010790 dilution Methods 0.000 claims description 9
- 239000012895 dilution Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000007872 degassing Methods 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 55
- 230000000052 comparative effect Effects 0.000 description 15
- 238000000926 separation method Methods 0.000 description 12
- 238000009849 vacuum degassing Methods 0.000 description 7
- BQJKTUVYRXYWTJ-UHFFFAOYSA-I ethanol;pentachlorotantalum Chemical compound CCO.Cl[Ta](Cl)(Cl)(Cl)Cl BQJKTUVYRXYWTJ-UHFFFAOYSA-I 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 239000013068 control sample Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- RMKZLFMHXZAGTM-UHFFFAOYSA-N [dimethoxy(propyl)silyl]oxymethyl prop-2-enoate Chemical compound CCC[Si](OC)(OC)OCOC(=O)C=C RMKZLFMHXZAGTM-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- ULFQGKXWKFZMLH-UHFFFAOYSA-N iridium tantalum Chemical compound [Ta].[Ir] ULFQGKXWKFZMLH-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/06—Insulating conductors or cables
- H01B13/065—Insulating conductors with lacquers or enamels
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/06—Insulating conductors or cables
- H01B13/16—Insulating conductors or cables by passing through or dipping in a liquid bath; by spraying
- H01B13/165—Insulating conductors or cables by passing through or dipping in a liquid bath; by spraying by spraying
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/30—Drying; Impregnating
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/02—Disposition of insulation
- H01B7/0208—Cables with several layers of insulating material
- H01B7/0216—Two layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/02—Disposition of insulation
- H01B7/0291—Disposition of insulation comprising two or more layers of insulation having different electrical properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/18—Protection against damage caused by wear, mechanical force or pressure; Sheaths; Armouring
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Paints Or Removers (AREA)
Abstract
本发明公开了一种耐磨抗电晕漆包铜圆线,制备步骤包括:(1)制备溶胶;(2)制备复合物;(3)制备改性粉末;(4)在铜圆线表面涂覆一层聚酯漆作为打底层,然后将所述改性粉末加入水性聚酰胺酰亚胺中形成涂覆液;涂覆液涂覆在所述打底层上,在打底层外部形成抗电晕层,获得所述耐磨抗电晕漆包铜圆线。本发明所述方法制备的漆包铜圆线具有良好的耐电晕效果,且耐刮力较高,漆膜在漆包线上的附着力度良好。The invention discloses a wear-resistant and anti-corona enameled copper round wire, the preparation steps of which include: (1) preparing a sol; (2) preparing a composite; (3) preparing a modified powder; (4) coating a layer of polyester paint on the surface of the copper round wire as a primer layer, and then adding the modified powder into water-based polyamide-imide to form a coating liquid; coating the coating liquid on the primer layer, forming an anti-corona layer outside the primer layer, and obtaining the wear-resistant and anti-corona enameled copper round wire. The enameled copper round wire prepared by the method of the invention has good corona resistance, high scratch resistance, and good adhesion of the paint film on the enameled wire.
Description
技术领域Technical Field
本发明涉及漆包线技术领域,特别涉及一种耐磨抗电晕漆包铜圆线。The invention relates to the technical field of enameled wires, in particular to a wear-resistant and corona-resistant enameled round copper wire.
背景技术Background technique
金属导线的表面绝缘处理方式一般有绕包薄膜、绕包云母带及表面涂覆绝缘漆等。金属导线表面的漆包线漆经高温烘焙后在金属丝表面形成绝缘保护层,由于该工艺制造简便,绝缘厚度适中,成型方面有优势等,在电工、电子、电器等领域具有广泛的应用。近年来,随着电机电器向大功率的方向发展以及我国高速铁路的快速发展,对高性能漆包线的需求日益增加。为了适应高瞬时功率、高功率密度、变速工况、强过载能力和大启动转矩等要求,对漆包线的耐电晕性能提出了更高的要求。漆包线的耐电晕能力是由绝缘层材料的耐电晕性能决定的,提升绝缘层材料的耐电晕性能是解决变频电机技术难题的关键。The surface insulation treatment methods of metal conductors generally include wrapping film, wrapping mica tape and coating insulating paint on the surface. After high-temperature baking, the enameled wire paint on the surface of the metal conductor forms an insulating protective layer on the surface of the metal wire. Due to the simple manufacturing process, moderate insulation thickness, and advantages in molding, it is widely used in electrical, electronic, and electrical fields. In recent years, with the development of motors and electrical appliances towards high power and the rapid development of high-speed railways in my country, the demand for high-performance enameled wires has increased. In order to adapt to the requirements of high instantaneous power, high power density, variable speed conditions, strong overload capacity and large starting torque, higher requirements are placed on the corona resistance of enameled wires. The corona resistance of enameled wires is determined by the corona resistance of the insulating layer material. Improving the corona resistance of the insulating layer material is the key to solving the technical problems of variable frequency motors.
发明内容Summary of the invention
为此,本发明提供了一种耐磨抗电晕漆包铜圆线,制备步骤包括:To this end, the present invention provides a wear-resistant and corona-resistant enameled copper round wire, the preparation steps of which include:
(1)配置硫酸氧钛的水溶液;搅拌所述硫酸氧钛的水溶液,搅拌状态下向溶液中加入氨水,加料完成后溶液水浴恒温至85±5℃,到温后保温搅拌溶液2h以上,然后固液分离,固相用去离子水洗涤,洗涤后的固相加入反应釜中的双氧水溶液中,超声搅拌溶液2h以上,然后加水稀释溶液,密封反应釜,加热至120℃水热保温处理8h以上,保温结束后空冷至常温,打开反应釜,获得溶胶;(1) preparing an aqueous solution of titanyl sulfate; stirring the aqueous solution of titanyl sulfate, adding aqueous ammonia to the solution under stirring, and after the addition is completed, the solution is kept at a constant temperature of 85±5° C. in a water bath, and after reaching the temperature, the solution is kept and stirred for more than 2 hours, and then the solid and liquid are separated, the solid phase is washed with deionized water, and the washed solid phase is added to the hydrogen peroxide solution in the reactor, and the solution is ultrasonically stirred for more than 2 hours, and then water is added to dilute the solution, the reactor is sealed, and heated to 120° C. for hydrothermal insulation treatment for more than 8 hours, and after the insulation is completed, the solution is air-cooled to room temperature, and the reactor is opened to obtain a sol;
(2)配置氯铱酸的乙醇溶液,配置五氯化钽的乙醇溶液;搅拌所述溶胶,然后在搅拌状态下向溶胶中同时加入所述氯铱酸的乙醇溶液和五氯化钽的乙醇溶液,加料完成后继续搅拌溶液50min以上,然后向溶液中加入硼氢化钠溶液,加料完成后搅拌溶液20min以上,然后向溶液中加入氨水将溶液的pH调节至10,然后搅拌溶液1h以上,固液分离,固相用去离子水洗涤3次以上,60℃烘干30min以上,获得复合物;(2) preparing an ethanol solution of chloroiridic acid and an ethanol solution of tantalum pentachloride; stirring the sol, and then adding the ethanol solution of chloroiridic acid and the ethanol solution of tantalum pentachloride to the sol while stirring, and continuing to stir the solution for more than 50 minutes after the addition is completed, and then adding sodium borohydride solution to the solution, and stirring the solution for more than 20 minutes after the addition is completed, and then adding ammonia water to the solution to adjust the pH of the solution to 10, and then stirring the solution for more than 1 hour, separating the solid and the liquid, washing the solid phase with deionized water for more than 3 times, and drying at 60° C. for more than 30 minutes to obtain a composite;
(3)配置γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液;配置甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液;将所述复合物分散在乙醇溶液中形成醇分散液,所述醇分散液水浴恒温至50±2℃保温,保温过程中搅拌醇分散液,冷凝回流,然后在搅拌状态下向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液,加料完成后50±2℃恒温搅拌醇分散液20min,然后向醇分散液中加入去离子水,加料完成后继续50±2℃恒温搅拌2h以上,然后固液分离,固相用乙醇洗涤2次,60℃烘干30min以上,烘干后的固相在氮气保护氛围内加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中形成混合物,混合物在氮气保护氛围中水浴恒温至70±3℃保温10h以上,然后固液分离,固相用乙醇洗涤3次,60℃烘干1h以上,获得改性粉末;(3) preparing an ethanol solution of γ-methacryloxypropyltrimethoxysilane; preparing a mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile; dispersing the composite in the ethanol solution to form an alcohol dispersion, keeping the alcohol dispersion in a water bath at a constant temperature of 50±2° C., stirring the alcohol dispersion during the insulation process, condensing and refluxing, and then adding the ethanol solution of γ-methacryloxypropyltrimethoxysilane to the alcohol dispersion under stirring, and stirring the alcohol dispersion at a constant temperature of 50±2° C. for 20 minutes after the addition is completed. , then add deionized water to the alcohol dispersion, continue to stir at a constant temperature of 50±2°C for more than 2h after the addition is completed, then separate the solid and liquid, wash the solid phase with ethanol twice, and dry it at 60°C for more than 30min, add the dried solid phase to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a nitrogen protective atmosphere to form a mixture, and keep the mixture in a water bath at a constant temperature of 70±3°C in a nitrogen protective atmosphere for more than 10h, then separate the solid and liquid, wash the solid phase with ethanol three times, and dry it at 60°C for more than 1h to obtain a modified powder;
(4)在铜圆线表面涂覆一层聚酯漆作为打底层,然后将所述改性粉末加入水性聚酰胺酰亚胺中形成涂覆液,涂覆液磁力搅拌40min以上,搅拌过程中超声处理,搅拌结束后抽真空除气,然后涂覆在所述打底层上,涂覆完成后70℃保温1h,再150℃保温2h,再210℃保温2h,保温结束后以10℃/min冷却至常温,获得所述耐磨抗电晕漆包铜圆线。(4) coating a layer of polyester paint on the surface of the copper round wire as a base layer, then adding the modified powder into water-based polyamide-imide to form a coating liquid, magnetically stirring the coating liquid for more than 40 minutes, ultrasonically treating during the stirring process, vacuuming and degassing after the stirring is completed, and then coating on the base layer, keeping the temperature at 70°C for 1 hour, then keeping the temperature at 150°C for 2 hours, and then keeping the temperature at 210°C for 2 hours after the coating is completed, and cooling to room temperature at 10°C/min after the insulation is completed to obtain the wear-resistant and corona-resistant enameled copper round wire.
进一步地,所述步骤(1)中,所述硫酸氧钛的水溶液中,硫酸氧钛的浓度为6~8g/L;所述氨水中溶质的质量百分数为20%,向硫酸氧钛的溶液中加入氨水的体积比为硫酸氧钛的溶液:氨水=10:3~4。Furthermore, in the step (1), the concentration of titanyl sulfate in the aqueous solution of titanyl sulfate is 6-8 g/L; the mass percentage of the solute in the ammonia water is 20%, and the volume ratio of ammonia water added to the titanyl sulfate solution is titanyl sulfate solution: ammonia water = 10:3-4.
进一步地,所述步骤(1)中,洗涤后的固相加入反应釜中的双氧水溶液中的质量比为固相:双氧水溶液=1:30;所述双氧水溶液中溶质的质量百分数为30%;超声波功率为200W,频率为30kHz;加水稀释溶液至稀释前溶液体积的5倍。Furthermore, in the step (1), the washed solid phase is added to the hydrogen peroxide solution in the reactor in a mass ratio of solid phase: hydrogen peroxide solution = 1:30; the mass percentage of the solute in the hydrogen peroxide solution is 30%; the ultrasonic power is 200 W and the frequency is 30 kHz; water is added to dilute the solution to 5 times the volume of the solution before dilution.
进一步地,所述步骤(2)中,所述氯铱酸的乙醇溶液中,氯铱酸的浓度为0.8~1.4g/L,溶剂为乙醇;所述五氯化钽的乙醇溶液中,五氯化钽的浓度为12~14g/L,溶剂为乙醇;所述硼氢化钠溶液中,硼氢化钠的浓度为1.4~1.7g/L,溶剂为水;向溶胶中加入所述氯铱酸的乙醇溶液、五氯化钽的乙醇溶液、硼氢化钠溶液的体积比为溶胶:氯铱酸的乙醇溶液:五氯化钽的乙醇溶液:硼氢化钠溶液=10:1~2:1~4:0.6~0.8;所述氨水中溶质的质量百分数为20%。Furthermore, in the step (2), in the ethanol solution of chloroiridic acid, the concentration of chloroiridic acid is 0.8-1.4 g/L, and the solvent is ethanol; in the ethanol solution of tantalum pentachloride, the concentration of tantalum pentachloride is 12-14 g/L, and the solvent is ethanol; in the sodium borohydride solution, the concentration of sodium borohydride is 1.4-1.7 g/L, and the solvent is water; the volume ratio of the ethanol solution of chloroiridic acid, the ethanol solution of tantalum pentachloride, and the sodium borohydride solution added to the sol is sol: ethanol solution of chloroiridic acid: ethanol solution of tantalum pentachloride: sodium borohydride solution = 10:1-2:1-4:0.6-0.8; the mass percentage of the solute in the ammonia water is 20%.
进一步地,所述步骤(3)中,所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液中,γ-甲基丙烯酰氧基丙基三甲氧基硅烷的质量百分数为2%~3%,溶剂为乙醇;甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中,混合质量比为甲基丙烯酸三氟乙酯:偶氮二异丁腈:乙醇=2.6~3.2:0.8~0.9:100;所述复合物分散在乙醇溶液中的固液质量比为复合物:乙醇=1:50;向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液和所述去离子水的体积比为醇分散液:γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液:去离子水=10:2~4:1。Furthermore, in the step (3), in the ethanol solution of γ-methacryloxypropyltrimethoxysilane, the mass percentage of γ-methacryloxypropyltrimethoxysilane is 2% to 3%, and the solvent is ethanol; in the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile, the mixing mass ratio is trifluoroethyl methacrylate: azobisisobutyronitrile: ethanol = 2.6 to 3.2: 0.8 to 0.9: 100; the solid-liquid mass ratio of the composite dispersed in the ethanol solution is composite: ethanol = 1:50; the volume ratio of the ethanol solution of γ-methacryloxypropyltrimethoxysilane and the deionized water added to the alcohol dispersion is alcohol dispersion: ethanol solution of γ-methacryloxypropyltrimethoxysilane: deionized water = 10:2 to 4:1.
进一步地,所述步骤(3)中,烘干后的固相加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中的质量比为固相:甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液=1:100。Furthermore, in the step (3), the dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a mass ratio of solid phase: mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile = 1:100.
进一步地,所述步骤(4)中,所述改性粉末加入水性聚酰胺酰亚胺中的质量比为改性粉末:水性聚酰胺酰亚胺=9~10:100。Furthermore, in the step (4), the mass ratio of the modified powder added to the water-based polyamide-imide is modified powder: water-based polyamide-imide = 9 to 10:100.
本发明的有益效果在于:本发明所述方法制备的漆包铜圆线具有良好的耐电晕效果,且耐刮力较高,漆膜在漆包线上的附着力度良好。The beneficial effects of the present invention are as follows: the enameled round copper wire prepared by the method of the present invention has good corona resistance and high scratch resistance, and the adhesion of the paint film on the enameled wire is good.
具体实施方式Detailed ways
下面结合实施例对本发明做进一步的说明。The present invention will be further described below in conjunction with the embodiments.
实施例1Example 1
一种耐磨抗电晕漆包铜圆线,制备步骤包括:A wear-resistant and corona-resistant enameled round copper wire, the preparation steps comprising:
(1)配置硫酸氧钛的水溶液;所述硫酸氧钛的水溶液中,硫酸氧钛的浓度为6g/L;搅拌所述硫酸氧钛的水溶液,搅拌状态下向溶液中加入氨水,所述氨水中溶质的质量百分数为20%,向硫酸氧钛的溶液中加入氨水的体积比为硫酸氧钛的溶液:氨水=10:3;加料完成后溶液水浴恒温至85±5℃,到温后保温搅拌溶液2h,然后固液分离,固相用去离子水洗涤2次,洗涤后的固相加入反应釜中的双氧水溶液中,洗涤后的固相加入反应釜中的双氧水溶液中的质量比为固相:双氧水溶液=1:30;所述双氧水溶液中溶质的质量百分数为30%;超声搅拌溶液2h,超声波功率为200W,频率为30kHz;然后加水稀释溶液,加水稀释溶液至稀释前溶液体积的5倍;密封反应釜,加热至120℃水热保温处理8h,保温结束后空冷至常温,打开反应釜,获得溶胶;(1) preparing an aqueous solution of titanyl sulfate; in the aqueous solution of titanyl sulfate, the concentration of titanyl sulfate is 6 g/L; stirring the aqueous solution of titanyl sulfate, adding ammonia water to the solution under stirring, wherein the mass percentage of the solute in the ammonia water is 20%, and the volume ratio of ammonia water added to the solution of titanyl sulfate is titanyl sulfate solution: ammonia water = 10:3; after the addition is completed, the solution is kept at a constant temperature of 85±5° C. in a water bath, and after reaching the temperature, the solution is kept at a constant temperature and stirred for 2 hours, and then the solid-liquid separation is carried out, and the solid phase is washed twice with deionized water. The solid phase after washing is added to the hydrogen peroxide solution in the reactor, and the mass ratio of solid phase to hydrogen peroxide solution is 1:30; the mass percentage of the solute in the hydrogen peroxide solution is 30%; the solution is ultrasonically stirred for 2 hours, the ultrasonic power is 200W, and the frequency is 30kHz; then water is added to dilute the solution, and the volume of the solution before dilution is 5 times; the reactor is sealed, heated to 120°C for hydrothermal insulation treatment for 8 hours, and air-cooled to room temperature after the insulation is completed, and the reactor is opened to obtain a sol;
(2)配置氯铱酸的乙醇溶液,所述氯铱酸的乙醇溶液中,氯铱酸的浓度为0.8g/L,溶剂为乙醇;配置五氯化钽的乙醇溶液;所述五氯化钽的乙醇溶液中,五氯化钽的浓度为12g/L,溶剂为乙醇;搅拌所述溶胶,然后在搅拌状态下向溶胶中同时加入所述氯铱酸的乙醇溶液和五氯化钽的乙醇溶液,加料完成后继续搅拌溶液50min,然后向溶液中加入硼氢化钠溶液,所述硼氢化钠溶液中,硼氢化钠的浓度为1.4g/L,溶剂为水;向溶胶中加入所述氯铱酸的乙醇溶液、五氯化钽的乙醇溶液、硼氢化钠溶液的体积比为溶胶:氯铱酸的乙醇溶液:五氯化钽的乙醇溶液:硼氢化钠溶液=10:1:1:0.6;加料完成后搅拌溶液20min,然后向溶液中加入氨水(氨水中溶质的质量百分数为20%)将溶液的pH调节至10,然后搅拌溶液1h,固液分离,固相用去离子水洗涤3次,60℃烘干30min,获得复合物;(2) preparing an ethanol solution of chloroiridic acid, wherein the concentration of chloroiridic acid in the ethanol solution is 0.8 g/L, and the solvent is ethanol; preparing an ethanol solution of tantalum pentachloride, wherein the concentration of tantalum pentachloride in the ethanol solution is 12 g/L, and the solvent is ethanol; stirring the sol, and then adding the ethanol solution of chloroiridic acid and the ethanol solution of tantalum pentachloride to the sol under stirring, and continuing to stir the solution for 50 minutes after the addition is completed, and then adding a sodium borohydride solution to the solution, wherein the concentration of sodium borohydride in the sodium borohydride solution is 1 .4g/L, the solvent is water; the volume ratio of the ethanol solution of chloroiridic acid, the ethanol solution of tantalum pentachloride and the sodium borohydride solution is added to the sol: the ethanol solution of chloroiridic acid: the ethanol solution of tantalum pentachloride: the sodium borohydride solution = 10:1:1:0.6; after the addition is completed, the solution is stirred for 20 minutes, and then ammonia water (the mass percentage of the solute in the ammonia water is 20%) is added to the solution to adjust the pH of the solution to 10, and then the solution is stirred for 1 hour, the solid-liquid separation is carried out, the solid phase is washed with deionized water for 3 times, and dried at 60°C for 30 minutes to obtain a composite;
(3)配置γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液;所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液中,γ-甲基丙烯酰氧基丙基三甲氧基硅烷的质量百分数为2%,溶剂为乙醇;配置甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液;甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中,混合质量比为甲基丙烯酸三氟乙酯:偶氮二异丁腈:乙醇=2.6:0.8:100;将所述复合物分散在乙醇溶液中形成醇分散液,所述复合物分散在乙醇溶液中的固液质量比为复合物:乙醇=1:50;所述醇分散液水浴恒温至50±2℃保温,保温过程中搅拌醇分散液,冷凝回流,然后在搅拌状态下向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液,加料完成后50±2℃恒温搅拌醇分散液20min,然后向醇分散液中加入去离子水,向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液和所述去离子水的体积比为醇分散液:γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液:去离子水=10:2:1;加料完成后继续50±2℃恒温搅拌2h,然后固液分离,固相用乙醇洗涤2次,60℃烘干30min,烘干后的固相在氮气保护氛围内加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中形成混合物,烘干后的固相加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中的质量比为固相:甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液=1:100;混合物在氮气保护氛围中水浴恒温至70±3℃保温10h,然后固液分离,固相用乙醇洗涤3次,60℃烘干1h,获得改性粉末;(3) preparing an ethanol solution of γ-methacryloxypropyl trimethoxysilane; in the ethanol solution of γ-methacryloxypropyl trimethoxysilane, the mass percentage of γ-methacryloxypropyl trimethoxysilane is 2%, and the solvent is ethanol; preparing a mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile; in the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile, the mixing mass ratio is trifluoroethyl methacrylate: azobisisobutyronitrile: ethanol = 2.6:0.8:100; dispersing the composite in the ethanol solution to form an alcohol dispersion, the solid-liquid mass ratio of the composite dispersed in the ethanol solution is composite: ethanol = 1:50; the alcohol dispersion is kept at a constant temperature of 50±2° C. in a water bath, the alcohol dispersion is stirred during the insulation process, condensed and refluxed, and then the ethanol solution of γ-methacryloxypropyl trimethoxysilane is added to the alcohol dispersion under stirring, and after the addition is completed, the alcohol dispersion is stirred at a constant temperature of 50±2° C. for 20 min. in, then add deionized water to the alcohol dispersion, add the ethanol solution of γ-methacryloxypropyltrimethoxysilane and the deionized water to the alcohol dispersion in a volume ratio of alcohol dispersion: ethanol solution of γ-methacryloxypropyltrimethoxysilane: deionized water = 10:2:1; after the addition is completed, continue to stir at a constant temperature of 50±2°C for 2h, then separate the solid and liquid, wash the solid phase with ethanol twice, and dry it at 60°C for 30min. The dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a nitrogen protective atmosphere to form a mixture, and the dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a mass ratio of solid phase: mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile = 1:100; the mixture is kept constant temperature at 70±3°C in a water bath in a nitrogen protective atmosphere for 10h, then separate the solid and liquid, wash the solid phase with ethanol 3 times, and dry it at 60°C for 1h to obtain a modified powder;
(4)在铜圆线表面涂覆一层聚酯漆作为打底层(10μm),然后将所述改性粉末加入水性聚酰胺酰亚胺中形成涂覆液,所述改性粉末加入水性聚酰胺酰亚胺中的质量比为改性粉末:水性聚酰胺酰亚胺=9:100;涂覆液磁力搅拌40min,搅拌过程中超声处理,超声波功率为200W,频率为30kHz;搅拌结束后抽真空除气,然后涂覆在所述打底层上,涂覆完成后70℃保温1h,再150℃保温2h,再210℃保温2h,保温结束后以10℃/min冷却至常温,在打底层外部形成抗电晕层,抗电晕层厚度为20μm,获得所述耐磨抗电晕漆包铜圆线。(4) A layer of polyester paint is coated on the surface of the copper round wire as a primer layer (10 μm), and then the modified powder is added to water-based polyamide-imide to form a coating liquid, wherein the mass ratio of the modified powder to the water-based polyamide-imide is modified powder: water-based polyamide-imide = 9:100; the coating liquid is magnetically stirred for 40 minutes, and ultrasonic treatment is performed during the stirring process, with an ultrasonic power of 200 W and a frequency of 30 kHz; after the stirring is completed, vacuum degassing is performed, and then the coating is applied on the primer layer. After the coating is completed, the coating is kept at 70°C for 1 hour, then at 150°C for 2 hours, and then at 210°C for 2 hours. After the insulation is completed, the coating is cooled to room temperature at a rate of 10°C/min to form an anti-corona layer on the outside of the primer layer. The thickness of the anti-corona layer is 20 μm, and the wear-resistant and anti-corona enameled copper round wire is obtained.
实施例2Example 2
一种耐磨抗电晕漆包铜圆线,制备步骤包括:A wear-resistant and corona-resistant enameled round copper wire, the preparation steps comprising:
(1)配置硫酸氧钛的水溶液;所述硫酸氧钛的水溶液中,硫酸氧钛的浓度为7g/L;搅拌所述硫酸氧钛的水溶液,搅拌状态下向溶液中加入氨水,所述氨水中溶质的质量百分数为20%,向硫酸氧钛的溶液中加入氨水的体积比为硫酸氧钛的溶液:氨水=10:3;加料完成后溶液水浴恒温至85±5℃,到温后保温搅拌溶液2h,然后固液分离,固相用去离子水洗涤2次,洗涤后的固相加入反应釜中的双氧水溶液中,洗涤后的固相加入反应釜中的双氧水溶液中的质量比为固相:双氧水溶液=1:30;所述双氧水溶液中溶质的质量百分数为30%;超声搅拌溶液2h,超声波功率为200W,频率为30kHz;然后加水稀释溶液,加水稀释溶液至稀释前溶液体积的5倍;密封反应釜,加热至120℃水热保温处理8h,保温结束后空冷至常温,打开反应釜,获得溶胶;(1) preparing an aqueous solution of titanyl sulfate; in the aqueous solution of titanyl sulfate, the concentration of titanyl sulfate is 7 g/L; stirring the aqueous solution of titanyl sulfate, adding ammonia water to the solution under stirring, wherein the mass percentage of the solute in the ammonia water is 20%, and the volume ratio of ammonia water added to the solution of titanyl sulfate is titanyl sulfate solution: ammonia water = 10:3; after the addition is completed, the solution is kept at a constant temperature of 85±5° C. in a water bath, and after reaching the temperature, the solution is kept at a constant temperature and stirred for 2 hours, and then the solid and liquid are separated, and the solid phase is washed twice with deionized water. The solid phase after washing is added to the hydrogen peroxide solution in the reactor, and the mass ratio of solid phase to hydrogen peroxide solution is 1:30; the mass percentage of the solute in the hydrogen peroxide solution is 30%; the solution is ultrasonically stirred for 2 hours, the ultrasonic power is 200W, and the frequency is 30kHz; then water is added to dilute the solution, and the volume of the solution before dilution is 5 times; the reactor is sealed, heated to 120°C for hydrothermal insulation treatment for 8 hours, and air-cooled to room temperature after the insulation is completed, and the reactor is opened to obtain a sol;
(2)配置氯铱酸的乙醇溶液,所述氯铱酸的乙醇溶液中,氯铱酸的浓度为1g/L,溶剂为乙醇;配置五氯化钽的乙醇溶液;所述五氯化钽的乙醇溶液中,五氯化钽的浓度为13g/L,溶剂为乙醇;搅拌所述溶胶,然后在搅拌状态下向溶胶中同时加入所述氯铱酸的乙醇溶液和五氯化钽的乙醇溶液,加料完成后继续搅拌溶液50min,然后向溶液中加入硼氢化钠溶液,所述硼氢化钠溶液中,硼氢化钠的浓度为1.5g/L,溶剂为水;向溶胶中加入所述氯铱酸的乙醇溶液、五氯化钽的乙醇溶液、硼氢化钠溶液的体积比为溶胶:氯铱酸的乙醇溶液:五氯化钽的乙醇溶液:硼氢化钠溶液=10:1:2:0.7;加料完成后搅拌溶液20min,然后向溶液中加入氨水(氨水中溶质的质量百分数为20%)将溶液的pH调节至10,然后搅拌溶液1h,固液分离,固相用去离子水洗涤3次,60℃烘干30min,获得复合物;(2) preparing an ethanol solution of chloroiridic acid, wherein the concentration of chloroiridic acid in the ethanol solution is 1 g/L and the solvent is ethanol; preparing an ethanol solution of tantalum pentachloride, wherein the concentration of tantalum pentachloride in the ethanol solution is 13 g/L and the solvent is ethanol; stirring the sol, and then adding the ethanol solution of chloroiridic acid and the ethanol solution of tantalum pentachloride to the sol simultaneously under stirring, and continuing to stir the solution for 50 minutes after the addition is completed, and then adding a sodium borohydride solution to the solution, wherein the concentration of sodium borohydride in the sodium borohydride solution is 1. 5g/L, the solvent is water; the volume ratio of the chloroiridic acid ethanol solution, the tantalum pentachloride ethanol solution and the sodium borohydride solution is added to the sol: the chloroiridic acid ethanol solution: the tantalum pentachloride ethanol solution: the sodium borohydride solution = 10:1:2:0.7; after the addition is completed, the solution is stirred for 20 minutes, and then ammonia water (the mass percentage of the solute in the ammonia water is 20%) is added to the solution to adjust the pH of the solution to 10, and then the solution is stirred for 1 hour, the solid-liquid separation is carried out, the solid phase is washed with deionized water for 3 times, and dried at 60°C for 30 minutes to obtain a composite;
(3)配置γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液;所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液中,γ-甲基丙烯酰氧基丙基三甲氧基硅烷的质量百分数为2%,溶剂为乙醇;配置甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液;甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中,混合质量比为甲基丙烯酸三氟乙酯:偶氮二异丁腈:乙醇=2.8:0.8:100;将所述复合物分散在乙醇溶液中形成醇分散液,所述复合物分散在乙醇溶液中的固液质量比为复合物:乙醇=1:50;所述醇分散液水浴恒温至50±2℃保温,保温过程中搅拌醇分散液,冷凝回流,然后在搅拌状态下向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液,加料完成后50±2℃恒温搅拌醇分散液20min,然后向醇分散液中加入去离子水,向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液和所述去离子水的体积比为醇分散液:γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液:去离子水=10:3:1;加料完成后继续50±2℃恒温搅拌2h,然后固液分离,固相用乙醇洗涤2次,60℃烘干30min,烘干后的固相在氮气保护氛围内加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中形成混合物,烘干后的固相加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中的质量比为固相:甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液=1:100;混合物在氮气保护氛围中水浴恒温至70±3℃保温10h,然后固液分离,固相用乙醇洗涤3次,60℃烘干1h,获得改性粉末;(3) preparing an ethanol solution of γ-methacryloxypropyl trimethoxysilane; in the ethanol solution of γ-methacryloxypropyl trimethoxysilane, the mass percentage of γ-methacryloxypropyl trimethoxysilane is 2%, and the solvent is ethanol; preparing a mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile; in the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile, the mixing mass ratio is trifluoroethyl methacrylate: azobisisobutyronitrile: ethanol = 2.8:0.8:100; dispersing the composite in the ethanol solution to form an alcohol dispersion, the solid-liquid mass ratio of the composite dispersed in the ethanol solution is composite: ethanol = 1:50; the alcohol dispersion is kept at a constant temperature of 50±2° C. in a water bath, the alcohol dispersion is stirred during the insulation process, condensed and refluxed, and then the ethanol solution of γ-methacryloxypropyl trimethoxysilane is added to the alcohol dispersion under stirring, and after the addition is completed, the alcohol dispersion is stirred at a constant temperature of 50±2° C. for 20 min. in, then add deionized water to the alcohol dispersion, add the ethanol solution of γ-methacryloxypropyltrimethoxysilane and the deionized water to the alcohol dispersion in a volume ratio of alcohol dispersion: ethanol solution of γ-methacryloxypropyltrimethoxysilane: deionized water = 10:3:1; after the addition is completed, continue to stir at a constant temperature of 50±2°C for 2h, then separate the solid and liquid, wash the solid phase with ethanol twice, and dry it at 60°C for 30min. The dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a nitrogen protective atmosphere to form a mixture, and the dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a mass ratio of solid phase: mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile = 1:100; the mixture is kept constant at 70±3°C in a water bath in a nitrogen protective atmosphere for 10h, then separate the solid and liquid, wash the solid phase with ethanol 3 times, and dry it at 60°C for 1h to obtain a modified powder;
(4)在铜圆线表面涂覆一层聚酯漆作为打底层(10μm),然后将所述改性粉末加入水性聚酰胺酰亚胺中形成涂覆液,所述改性粉末加入水性聚酰胺酰亚胺中的质量比为改性粉末:水性聚酰胺酰亚胺=9:100;涂覆液磁力搅拌40min,搅拌过程中超声处理,超声波功率为200W,频率为30kHz;搅拌结束后抽真空除气,然后涂覆在所述打底层上,涂覆完成后70℃保温1h,再150℃保温2h,再210℃保温2h,保温结束后以10℃/min冷却至常温,在打底层外部形成抗电晕层,抗电晕层厚度为20μm,获得所述耐磨抗电晕漆包铜圆线。(4) A layer of polyester paint is coated on the surface of the copper round wire as a primer layer (10 μm), and then the modified powder is added to water-based polyamide-imide to form a coating liquid, wherein the mass ratio of the modified powder to the water-based polyamide-imide is modified powder: water-based polyamide-imide = 9:100; the coating liquid is magnetically stirred for 40 minutes, and ultrasonic treatment is performed during the stirring process, with an ultrasonic power of 200 W and a frequency of 30 kHz; after the stirring is completed, vacuum degassing is performed, and then the coating is applied on the primer layer. After the coating is completed, the coating is kept at 70° C. for 1 hour, then at 150° C. for 2 hours, and then at 210° C. for 2 hours. After the insulation is completed, the coating is cooled to room temperature at a rate of 10° C./min to form an anti-corona layer on the outside of the primer layer. The thickness of the anti-corona layer is 20 μm, and the wear-resistant and anti-corona enameled copper round wire is obtained.
实施例3Example 3
一种耐磨抗电晕漆包铜圆线,制备步骤包括:A wear-resistant and corona-resistant enameled round copper wire, the preparation steps comprising:
(1)配置硫酸氧钛的水溶液;所述硫酸氧钛的水溶液中,硫酸氧钛的浓度为7g/L;搅拌所述硫酸氧钛的水溶液,搅拌状态下向溶液中加入氨水,所述氨水中溶质的质量百分数为20%,向硫酸氧钛的溶液中加入氨水的体积比为硫酸氧钛的溶液:氨水=10:4;加料完成后溶液水浴恒温至85±5℃,到温后保温搅拌溶液2h,然后固液分离,固相用去离子水洗涤2次,洗涤后的固相加入反应釜中的双氧水溶液中,洗涤后的固相加入反应釜中的双氧水溶液中的质量比为固相:双氧水溶液=1:30;所述双氧水溶液中溶质的质量百分数为30%;超声搅拌溶液2h,超声波功率为200W,频率为30kHz;然后加水稀释溶液,加水稀释溶液至稀释前溶液体积的5倍;密封反应釜,加热至120℃水热保温处理8h,保温结束后空冷至常温,打开反应釜,获得溶胶;(1) preparing an aqueous solution of titanyl sulfate; in the aqueous solution of titanyl sulfate, the concentration of titanyl sulfate is 7 g/L; stirring the aqueous solution of titanyl sulfate, adding ammonia water to the solution under stirring, wherein the mass percentage of the solute in the ammonia water is 20%, and the volume ratio of ammonia water added to the solution of titanyl sulfate is titanyl sulfate solution: ammonia water = 10:4; after the addition is completed, the solution is kept at a constant temperature of 85±5° C. in a water bath, and after reaching the temperature, the solution is kept at a constant temperature and stirred for 2 hours, and then the solid-liquid separation is carried out, and the solid phase is washed twice with deionized water. The solid phase after washing is added to the hydrogen peroxide solution in the reactor, and the mass ratio of solid phase to hydrogen peroxide solution is 1:30; the mass percentage of the solute in the hydrogen peroxide solution is 30%; the solution is ultrasonically stirred for 2 hours, the ultrasonic power is 200W, and the frequency is 30kHz; then water is added to dilute the solution, and the volume of the solution before dilution is 5 times; the reactor is sealed, heated to 120°C for hydrothermal insulation treatment for 8 hours, and air-cooled to room temperature after the insulation is completed, and the reactor is opened to obtain a sol;
(2)配置氯铱酸的乙醇溶液,所述氯铱酸的乙醇溶液中,氯铱酸的浓度为1.2g/L,溶剂为乙醇;配置五氯化钽的乙醇溶液;所述五氯化钽的乙醇溶液中,五氯化钽的浓度为13g/L,溶剂为乙醇;搅拌所述溶胶,然后在搅拌状态下向溶胶中同时加入所述氯铱酸的乙醇溶液和五氯化钽的乙醇溶液,加料完成后继续搅拌溶液50min,然后向溶液中加入硼氢化钠溶液,所述硼氢化钠溶液中,硼氢化钠的浓度为1.6g/L,溶剂为水;向溶胶中加入所述氯铱酸的乙醇溶液、五氯化钽的乙醇溶液、硼氢化钠溶液的体积比为溶胶:氯铱酸的乙醇溶液:五氯化钽的乙醇溶液:硼氢化钠溶液=10:2:3:0.7;加料完成后搅拌溶液20min,然后向溶液中加入氨水(氨水中溶质的质量百分数为20%)将溶液的pH调节至10,然后搅拌溶液1h,固液分离,固相用去离子水洗涤3次,60℃烘干30min,获得复合物;(2) preparing an ethanol solution of chloroiridic acid, wherein the concentration of chloroiridic acid in the ethanol solution is 1.2 g/L, and the solvent is ethanol; preparing an ethanol solution of tantalum pentachloride, wherein the concentration of tantalum pentachloride in the ethanol solution is 13 g/L, and the solvent is ethanol; stirring the sol, and then adding the ethanol solution of chloroiridic acid and the ethanol solution of tantalum pentachloride to the sol while stirring, and continuing to stir the solution for 50 minutes after the addition is completed, and then adding a sodium borohydride solution to the solution, wherein the concentration of sodium borohydride in the sodium borohydride solution is 1 .6g/L, the solvent is water; the volume ratio of the ethanol solution of chloroiridic acid, the ethanol solution of tantalum pentachloride and the sodium borohydride solution is added to the sol: the ethanol solution of chloroiridic acid: the ethanol solution of tantalum pentachloride: the sodium borohydride solution = 10:2:3:0.7; after the addition is completed, the solution is stirred for 20 minutes, and then ammonia water (the mass percentage of the solute in the ammonia water is 20%) is added to the solution to adjust the pH of the solution to 10, and then the solution is stirred for 1 hour, the solid-liquid separation is carried out, the solid phase is washed with deionized water for 3 times, and dried at 60°C for 30 minutes to obtain a composite;
(3)配置γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液;所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液中,γ-甲基丙烯酰氧基丙基三甲氧基硅烷的质量百分数为3%,溶剂为乙醇;配置甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液;甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中,混合质量比为甲基丙烯酸三氟乙酯:偶氮二异丁腈:乙醇=2.8:0.9:100;将所述复合物分散在乙醇溶液中形成醇分散液,所述复合物分散在乙醇溶液中的固液质量比为复合物:乙醇=1:50;所述醇分散液水浴恒温至50±2℃保温,保温过程中搅拌醇分散液,冷凝回流,然后在搅拌状态下向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液,加料完成后50±2℃恒温搅拌醇分散液20min,然后向醇分散液中加入去离子水,向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液和所述去离子水的体积比为醇分散液:γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液:去离子水=10:3:1;加料完成后继续50±2℃恒温搅拌2h,然后固液分离,固相用乙醇洗涤2次,60℃烘干30min,烘干后的固相在氮气保护氛围内加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中形成混合物,烘干后的固相加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中的质量比为固相:甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液=1:100;混合物在氮气保护氛围中水浴恒温至70±3℃保温10h,然后固液分离,固相用乙醇洗涤3次,60℃烘干1h,获得改性粉末;(3) preparing an ethanol solution of γ-methacryloxypropyl trimethoxysilane; in the ethanol solution of γ-methacryloxypropyl trimethoxysilane, the mass percentage of γ-methacryloxypropyl trimethoxysilane is 3%, and the solvent is ethanol; preparing a mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile; in the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile, the mixing mass ratio is trifluoroethyl methacrylate: azobisisobutyronitrile: ethanol = 2.8:0.9:100; dispersing the composite in the ethanol solution to form an alcohol dispersion, the solid-liquid mass ratio of the composite dispersed in the ethanol solution is composite: ethanol = 1:50; the alcohol dispersion is kept at a constant temperature of 50±2° C. in a water bath, the alcohol dispersion is stirred during the insulation process, condensed and refluxed, and then the ethanol solution of γ-methacryloxypropyl trimethoxysilane is added to the alcohol dispersion under stirring, and after the addition is completed, the alcohol dispersion is stirred at a constant temperature of 50±2° C. for 20 min. in, then add deionized water to the alcohol dispersion, add the ethanol solution of γ-methacryloxypropyltrimethoxysilane and the deionized water to the alcohol dispersion in a volume ratio of alcohol dispersion: ethanol solution of γ-methacryloxypropyltrimethoxysilane: deionized water = 10:3:1; after the addition is completed, continue to stir at a constant temperature of 50±2°C for 2h, then separate the solid and liquid, wash the solid phase with ethanol twice, and dry it at 60°C for 30min. The dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a nitrogen protective atmosphere to form a mixture, and the dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a mass ratio of solid phase: mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile = 1:100; the mixture is kept constant at 70±3°C in a water bath in a nitrogen protective atmosphere for 10h, then separate the solid and liquid, wash the solid phase with ethanol 3 times, and dry it at 60°C for 1h to obtain a modified powder;
(4)在铜圆线表面涂覆一层聚酯漆作为打底层(10μm),然后将所述改性粉末加入水性聚酰胺酰亚胺中形成涂覆液,所述改性粉末加入水性聚酰胺酰亚胺中的质量比为改性粉末:水性聚酰胺酰亚胺=10:100;涂覆液磁力搅拌40min,搅拌过程中超声处理,超声波功率为200W,频率为30kHz;搅拌结束后抽真空除气,然后涂覆在所述打底层上,涂覆完成后70℃保温1h,再150℃保温2h,再210℃保温2h,保温结束后以10℃/min冷却至常温,在打底层外部形成抗电晕层,抗电晕层厚度为20μm,获得所述耐磨抗电晕漆包铜圆线。(4) A layer of polyester paint is coated on the surface of the copper round wire as a primer layer (10 μm), and then the modified powder is added to water-based polyamide-imide to form a coating liquid, wherein the mass ratio of the modified powder to the water-based polyamide-imide is modified powder: water-based polyamide-imide = 10:100; the coating liquid is magnetically stirred for 40 minutes, and ultrasonic treatment is performed during the stirring process, with an ultrasonic power of 200 W and a frequency of 30 kHz; after the stirring is completed, vacuum degassing is performed, and then the coating is applied on the primer layer. After the coating is completed, the coating is kept at 70°C for 1 hour, then at 150°C for 2 hours, and then at 210°C for 2 hours. After the insulation is completed, the coating is cooled to room temperature at a rate of 10°C/min to form an anti-corona layer on the outside of the primer layer. The thickness of the anti-corona layer is 20 μm, and the wear-resistant and anti-corona enameled copper round wire is obtained.
实施例4Example 4
一种耐磨抗电晕漆包铜圆线,制备步骤包括:A wear-resistant and corona-resistant enameled round copper wire, the preparation steps comprising:
(1)配置硫酸氧钛的水溶液;所述硫酸氧钛的水溶液中,硫酸氧钛的浓度为8g/L;搅拌所述硫酸氧钛的水溶液,搅拌状态下向溶液中加入氨水,所述氨水中溶质的质量百分数为20%,向硫酸氧钛的溶液中加入氨水的体积比为硫酸氧钛的溶液:氨水=10:4;加料完成后溶液水浴恒温至85±5℃,到温后保温搅拌溶液2h,然后固液分离,固相用去离子水洗涤2次,洗涤后的固相加入反应釜中的双氧水溶液中,洗涤后的固相加入反应釜中的双氧水溶液中的质量比为固相:双氧水溶液=1:30;所述双氧水溶液中溶质的质量百分数为30%;超声搅拌溶液2h,超声波功率为200W,频率为30kHz;然后加水稀释溶液,加水稀释溶液至稀释前溶液体积的5倍;密封反应釜,加热至120℃水热保温处理8h,保温结束后空冷至常温,打开反应釜,获得溶胶;(1) preparing an aqueous solution of titanyl sulfate; in the aqueous solution of titanyl sulfate, the concentration of titanyl sulfate is 8 g/L; stirring the aqueous solution of titanyl sulfate, adding ammonia water to the solution under stirring, wherein the mass percentage of the solute in the ammonia water is 20%, and the volume ratio of ammonia water added to the solution of titanyl sulfate is titanyl sulfate solution: ammonia water = 10:4; after the addition is completed, the solution is kept at a constant temperature of 85±5° C. in a water bath, and after reaching the temperature, the solution is kept at a constant temperature and stirred for 2 hours, and then the solid-liquid separation is carried out, and the solid phase is washed twice with deionized water. The solid phase after washing is added to the hydrogen peroxide solution in the reactor, and the mass ratio of solid phase to hydrogen peroxide solution is 1:30; the mass percentage of the solute in the hydrogen peroxide solution is 30%; the solution is ultrasonically stirred for 2 hours, the ultrasonic power is 200W, and the frequency is 30kHz; then water is added to dilute the solution, and the volume of the solution before dilution is 5 times; the reactor is sealed, heated to 120°C for hydrothermal insulation treatment for 8 hours, and air-cooled to room temperature after the insulation is completed, and the reactor is opened to obtain a sol;
(2)配置氯铱酸的乙醇溶液,所述氯铱酸的乙醇溶液中,氯铱酸的浓度为1.4g/L,溶剂为乙醇;配置五氯化钽的乙醇溶液;所述五氯化钽的乙醇溶液中,五氯化钽的浓度为14g/L,溶剂为乙醇;搅拌所述溶胶,然后在搅拌状态下向溶胶中同时加入所述氯铱酸的乙醇溶液和五氯化钽的乙醇溶液,加料完成后继续搅拌溶液50min,然后向溶液中加入硼氢化钠溶液,所述硼氢化钠溶液中,硼氢化钠的浓度为1.7g/L,溶剂为水;向溶胶中加入所述氯铱酸的乙醇溶液、五氯化钽的乙醇溶液、硼氢化钠溶液的体积比为溶胶:氯铱酸的乙醇溶液:五氯化钽的乙醇溶液:硼氢化钠溶液=10:2:4:0.8;加料完成后搅拌溶液20min,然后向溶液中加入氨水(氨水中溶质的质量百分数为20%)将溶液的pH调节至10,然后搅拌溶液1h,固液分离,固相用去离子水洗涤3次,60℃烘干30min,获得复合物;(2) preparing an ethanol solution of chloroiridic acid, wherein the concentration of chloroiridic acid in the ethanol solution is 1.4 g/L, and the solvent is ethanol; preparing an ethanol solution of tantalum pentachloride, wherein the concentration of tantalum pentachloride in the ethanol solution is 14 g/L, and the solvent is ethanol; stirring the sol, and then adding the ethanol solution of chloroiridic acid and the ethanol solution of tantalum pentachloride to the sol while stirring, and continuing to stir the solution for 50 minutes after the addition is completed, and then adding a sodium borohydride solution to the solution, wherein the concentration of sodium borohydride in the sodium borohydride solution is 1 .7g/L, the solvent is water; the volume ratio of the chloroiridic acid ethanol solution, the tantalum pentachloride ethanol solution and the sodium borohydride solution is added to the sol: the chloroiridic acid ethanol solution: the tantalum pentachloride ethanol solution: the sodium borohydride solution = 10:2:4:0.8; after the addition is completed, the solution is stirred for 20 minutes, and then ammonia water (the mass percentage of the solute in the ammonia water is 20%) is added to the solution to adjust the pH of the solution to 10, and then the solution is stirred for 1 hour, the solid-liquid separation is carried out, the solid phase is washed with deionized water for 3 times, and dried at 60°C for 30 minutes to obtain a composite;
(3)配置γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液;所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液中,γ-甲基丙烯酰氧基丙基三甲氧基硅烷的质量百分数为3%,溶剂为乙醇;配置甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液;甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中,混合质量比为甲基丙烯酸三氟乙酯:偶氮二异丁腈:乙醇=3.2:0.9:100;将所述复合物分散在乙醇溶液中形成醇分散液,所述复合物分散在乙醇溶液中的固液质量比为复合物:乙醇=1:50;所述醇分散液水浴恒温至50±2℃保温,保温过程中搅拌醇分散液,冷凝回流,然后在搅拌状态下向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液,加料完成后50±2℃恒温搅拌醇分散液20min,然后向醇分散液中加入去离子水,向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液和所述去离子水的体积比为醇分散液:γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液:去离子水=10:4:1;加料完成后继续50±2℃恒温搅拌2h,然后固液分离,固相用乙醇洗涤2次,60℃烘干30min,烘干后的固相在氮气保护氛围内加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中形成混合物,烘干后的固相加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中的质量比为固相:甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液=1:100;混合物在氮气保护氛围中水浴恒温至70±3℃保温10h,然后固液分离,固相用乙醇洗涤3次,60℃烘干1h,获得改性粉末;(3) preparing an ethanol solution of γ-methacryloxypropyl trimethoxysilane; in the ethanol solution of γ-methacryloxypropyl trimethoxysilane, the mass percentage of γ-methacryloxypropyl trimethoxysilane is 3%, and the solvent is ethanol; preparing a mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile; in the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile, the mixing mass ratio is trifluoroethyl methacrylate: azobisisobutyronitrile: ethanol = 3.2:0.9:100; dispersing the composite in the ethanol solution to form an alcohol dispersion, the solid-liquid mass ratio of the composite dispersed in the ethanol solution is composite: ethanol = 1:50; the alcohol dispersion is kept at a constant temperature of 50±2° C. in a water bath, the alcohol dispersion is stirred during the insulation process, condensed and refluxed, and then the ethanol solution of γ-methacryloxypropyl trimethoxysilane is added to the alcohol dispersion under stirring, and after the addition is completed, the alcohol dispersion is stirred at a constant temperature of 50±2° C. for 20 min. in, then add deionized water to the alcohol dispersion, add the ethanol solution of γ-methacryloxypropyltrimethoxysilane and the deionized water to the alcohol dispersion in a volume ratio of alcohol dispersion: ethanol solution of γ-methacryloxypropyltrimethoxysilane: deionized water = 10:4:1; after the addition is completed, continue to stir at a constant temperature of 50±2°C for 2h, then separate the solid and liquid, wash the solid phase with ethanol twice, and dry it at 60°C for 30min. The dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a nitrogen protective atmosphere to form a mixture, and the dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a mass ratio of solid phase: mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile = 1:100; the mixture is kept constant temperature at 70±3°C in a water bath in a nitrogen protective atmosphere for 10h, then separate the solid and liquid, wash the solid phase with ethanol 3 times, and dry it at 60°C for 1h to obtain a modified powder;
(4)在铜圆线表面涂覆一层聚酯漆作为打底层(10μm),然后将所述改性粉末加入水性聚酰胺酰亚胺中形成涂覆液,所述改性粉末加入水性聚酰胺酰亚胺中的质量比为改性粉末:水性聚酰胺酰亚胺=10:100;涂覆液磁力搅拌40min,搅拌过程中超声处理,超声波功率为200W,频率为30kHz;搅拌结束后抽真空除气,然后涂覆在所述打底层上,涂覆完成后70℃保温1h,再150℃保温2h,再210℃保温2h,保温结束后以10℃/min冷却至常温,在打底层外部形成抗电晕层,抗电晕层厚度为20μm,获得所述耐磨抗电晕漆包铜圆线。(4) A layer of polyester paint is coated on the surface of the copper round wire as a primer layer (10 μm), and then the modified powder is added to water-based polyamide-imide to form a coating liquid, wherein the mass ratio of the modified powder to the water-based polyamide-imide is modified powder: water-based polyamide-imide = 10:100; the coating liquid is magnetically stirred for 40 minutes, and ultrasonic treatment is performed during the stirring process, with an ultrasonic power of 200 W and a frequency of 30 kHz; after the stirring is completed, vacuum degassing is performed, and then the coating is applied on the primer layer. After the coating is completed, the coating is kept at 70°C for 1 hour, then at 150°C for 2 hours, and then at 210°C for 2 hours. After the insulation is completed, the coating is cooled to room temperature at a rate of 10°C/min to form an anti-corona layer on the outside of the primer layer. The thickness of the anti-corona layer is 20 μm, and the wear-resistant and anti-corona enameled copper round wire is obtained.
对比例1Comparative Example 1
一种作为对比的漆包铜圆线,制备步骤包括:A comparative enameled round copper wire, the preparation steps include:
(1)配置硫酸氧钛的水溶液;所述硫酸氧钛的水溶液中,硫酸氧钛的浓度为7g/L;搅拌所述硫酸氧钛的水溶液,搅拌状态下向溶液中加入氨水,所述氨水中溶质的质量百分数为20%,向硫酸氧钛的溶液中加入氨水的体积比为硫酸氧钛的溶液:氨水=10:4;加料完成后溶液水浴恒温至85±5℃,到温后保温搅拌溶液2h,然后固液分离,固相用去离子水洗涤2次,洗涤后的固相加入反应釜中的双氧水溶液中,洗涤后的固相加入反应釜中的双氧水溶液中的质量比为固相:双氧水溶液=1:30;所述双氧水溶液中溶质的质量百分数为30%;超声搅拌溶液2h,超声波功率为200W,频率为30kHz;然后加水稀释溶液,加水稀释溶液至稀释前溶液体积的5倍;密封反应釜,加热至120℃水热保温处理8h,保温结束后空冷至常温,打开反应釜,获得溶胶;(1) preparing an aqueous solution of titanyl sulfate; in the aqueous solution of titanyl sulfate, the concentration of titanyl sulfate is 7 g/L; stirring the aqueous solution of titanyl sulfate, adding ammonia water to the solution under stirring, wherein the mass percentage of the solute in the ammonia water is 20%, and the volume ratio of ammonia water added to the solution of titanyl sulfate is titanyl sulfate solution: ammonia water = 10:4; after the addition is completed, the solution is kept at a constant temperature of 85±5° C. in a water bath, and after reaching the temperature, the solution is kept at a constant temperature and stirred for 2 hours, and then the solid-liquid separation is carried out, and the solid phase is washed twice with deionized water. The solid phase after washing is added to the hydrogen peroxide solution in the reactor, and the mass ratio of solid phase to hydrogen peroxide solution is 1:30; the mass percentage of the solute in the hydrogen peroxide solution is 30%; the solution is ultrasonically stirred for 2 hours, the ultrasonic power is 200W, and the frequency is 30kHz; then water is added to dilute the solution, and the volume of the solution before dilution is 5 times; the reactor is sealed, heated to 120°C for hydrothermal insulation treatment for 8 hours, and air-cooled to room temperature after the insulation is completed, and the reactor is opened to obtain a sol;
(2)配置五氯化钽的乙醇溶液;所述五氯化钽的乙醇溶液中,五氯化钽的浓度为13g/L,溶剂为乙醇;搅拌所述溶胶,然后在搅拌状态下向溶胶中加入所述五氯化钽的乙醇溶液,加料完成后继续搅拌溶液50min,然后向溶液中加入硼氢化钠溶液,所述硼氢化钠溶液中,硼氢化钠的浓度为1.6g/L,溶剂为水;向溶胶中加入五氯化钽的乙醇溶液、硼氢化钠溶液的体积比为溶胶:五氯化钽的乙醇溶液:硼氢化钠溶液=10:3:0.7;加料完成后搅拌溶液20min,然后向溶液中加入氨水(氨水中溶质的质量百分数为20%)将溶液的pH调节至10,然后搅拌溶液1h,固液分离,固相用去离子水洗涤3次,60℃烘干30min,获得复合物;(2) preparing an ethanol solution of tantalum pentachloride; in the ethanol solution of tantalum pentachloride, the concentration of tantalum pentachloride is 13 g/L, and the solvent is ethanol; stirring the sol, and then adding the ethanol solution of tantalum pentachloride to the sol under stirring, and continuing to stir the solution for 50 minutes after the addition is completed, and then adding a sodium borohydride solution to the solution, wherein the concentration of sodium borohydride in the sodium borohydride solution is 1.6 g/L, and the solvent is water; adding the ethanol solution of tantalum pentachloride and the sodium borohydride solution to the sol in a volume ratio of sol: ethanol solution of tantalum pentachloride: sodium borohydride solution = 10:3:0.7; after the addition is completed, stirring the solution for 20 minutes, and then adding ammonia water (the mass percentage of the solute in the ammonia water is 20%) to adjust the pH of the solution to 10, and then stirring the solution for 1 hour, separating the solid and the liquid, washing the solid phase with deionized water for 3 times, and drying at 60° C. for 30 minutes to obtain a composite;
(3)配置γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液;所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液中,γ-甲基丙烯酰氧基丙基三甲氧基硅烷的质量百分数为3%,溶剂为乙醇;配置甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液;甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中,混合质量比为甲基丙烯酸三氟乙酯:偶氮二异丁腈:乙醇=2.8:0.9:100;将所述复合物分散在乙醇溶液中形成醇分散液,所述复合物分散在乙醇溶液中的固液质量比为复合物:乙醇=1:50;所述醇分散液水浴恒温至50±2℃保温,保温过程中搅拌醇分散液,冷凝回流,然后在搅拌状态下向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液,加料完成后50±2℃恒温搅拌醇分散液20min,然后向醇分散液中加入去离子水,向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液和所述去离子水的体积比为醇分散液:γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液:去离子水=10:3:1;加料完成后继续50±2℃恒温搅拌2h,然后固液分离,固相用乙醇洗涤2次,60℃烘干30min,烘干后的固相在氮气保护氛围内加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中形成混合物,烘干后的固相加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中的质量比为固相:甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液=1:100;混合物在氮气保护氛围中水浴恒温至70±3℃保温10h,然后固液分离,固相用乙醇洗涤3次,60℃烘干1h,获得改性粉末;(3) preparing an ethanol solution of γ-methacryloxypropyl trimethoxysilane; in the ethanol solution of γ-methacryloxypropyl trimethoxysilane, the mass percentage of γ-methacryloxypropyl trimethoxysilane is 3%, and the solvent is ethanol; preparing a mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile; in the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile, the mixing mass ratio is trifluoroethyl methacrylate: azobisisobutyronitrile: ethanol = 2.8:0.9:100; dispersing the composite in the ethanol solution to form an alcohol dispersion, the solid-liquid mass ratio of the composite dispersed in the ethanol solution is composite: ethanol = 1:50; the alcohol dispersion is kept at a constant temperature of 50±2° C. in a water bath, the alcohol dispersion is stirred during the insulation process, condensed and refluxed, and then the ethanol solution of γ-methacryloxypropyl trimethoxysilane is added to the alcohol dispersion under stirring, and after the addition is completed, the alcohol dispersion is stirred at a constant temperature of 50±2° C. for 20 min. in, then add deionized water to the alcohol dispersion, add the ethanol solution of γ-methacryloxypropyltrimethoxysilane and the deionized water to the alcohol dispersion in a volume ratio of alcohol dispersion: ethanol solution of γ-methacryloxypropyltrimethoxysilane: deionized water = 10:3:1; after the addition is completed, continue to stir at a constant temperature of 50±2°C for 2h, then separate the solid and liquid, wash the solid phase with ethanol twice, and dry it at 60°C for 30min. The dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a nitrogen protective atmosphere to form a mixture, and the dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a mass ratio of solid phase: mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile = 1:100; the mixture is kept constant at 70±3°C in a water bath in a nitrogen protective atmosphere for 10h, then separate the solid and liquid, wash the solid phase with ethanol 3 times, and dry it at 60°C for 1h to obtain a modified powder;
(4)在铜圆线表面涂覆一层聚酯漆作为打底层(10μm),然后将所述改性粉末加入水性聚酰胺酰亚胺中形成涂覆液,所述改性粉末加入水性聚酰胺酰亚胺中的质量比为改性粉末:水性聚酰胺酰亚胺=10:100;涂覆液磁力搅拌40min,搅拌过程中超声处理,超声波功率为200W,频率为30kHz;搅拌结束后抽真空除气,然后涂覆在所述打底层上,涂覆完成后70℃保温1h,再150℃保温2h,再210℃保温2h,保温结束后以10℃/min冷却至常温,在打底层外部形成抗电晕层,抗电晕层厚度为20μm,获得本对比例所述漆包铜圆线。(4) A layer of polyester paint is coated on the surface of the copper round wire as a primer layer (10 μm), and then the modified powder is added to the aqueous polyamide-imide to form a coating liquid, wherein the mass ratio of the modified powder to the aqueous polyamide-imide is modified powder: aqueous polyamide-imide = 10:100; the coating liquid is magnetically stirred for 40 min, and ultrasonically treated during the stirring process, with an ultrasonic power of 200 W and a frequency of 30 kHz; after the stirring is completed, vacuum degassing is performed, and then the coating is applied on the primer layer. After the coating is completed, the coating is kept at 70° C. for 1 h, then at 150° C. for 2 h, and then at 210° C. for 2 h. After the insulation is completed, the coating is cooled to room temperature at a rate of 10° C./min to form an anti-corona layer on the outside of the primer layer. The thickness of the anti-corona layer is 20 μm, and the enameled copper round wire described in this comparative example is obtained.
对比例2Comparative Example 2
一种作为对比的漆包铜圆线,制备步骤包括:A comparative enameled round copper wire, the preparation steps include:
(1)配置硫酸氧钛的水溶液;所述硫酸氧钛的水溶液中,硫酸氧钛的浓度为7g/L;搅拌所述硫酸氧钛的水溶液,搅拌状态下向溶液中加入氨水,所述氨水中溶质的质量百分数为20%,向硫酸氧钛的溶液中加入氨水的体积比为硫酸氧钛的溶液:氨水=10:4;加料完成后溶液水浴恒温至85±5℃,到温后保温搅拌溶液2h,然后固液分离,固相用去离子水洗涤2次,洗涤后的固相加入反应釜中的双氧水溶液中,洗涤后的固相加入反应釜中的双氧水溶液中的质量比为固相:双氧水溶液=1:30;所述双氧水溶液中溶质的质量百分数为30%;超声搅拌溶液2h,超声波功率为200W,频率为30kHz;然后加水稀释溶液,加水稀释溶液至稀释前溶液体积的5倍;密封反应釜,加热至120℃水热保温处理8h,保温结束后空冷至常温,打开反应釜,获得溶胶;(1) preparing an aqueous solution of titanyl sulfate; in the aqueous solution of titanyl sulfate, the concentration of titanyl sulfate is 7 g/L; stirring the aqueous solution of titanyl sulfate, adding ammonia water to the solution under stirring, wherein the mass percentage of the solute in the ammonia water is 20%, and the volume ratio of ammonia water added to the solution of titanyl sulfate is titanyl sulfate solution: ammonia water = 10:4; after the addition is completed, the solution is kept at a constant temperature of 85±5° C. in a water bath, and after reaching the temperature, the solution is kept at a constant temperature and stirred for 2 hours, and then the solid-liquid separation is carried out, and the solid phase is washed twice with deionized water. The solid phase after washing is added to the hydrogen peroxide solution in the reactor, and the mass ratio of solid phase to hydrogen peroxide solution is 1:30; the mass percentage of the solute in the hydrogen peroxide solution is 30%; the solution is ultrasonically stirred for 2 hours, the ultrasonic power is 200W, and the frequency is 30kHz; then water is added to dilute the solution, and the volume of the solution before dilution is 5 times; the reactor is sealed, heated to 120°C for hydrothermal insulation treatment for 8 hours, and air-cooled to room temperature after the insulation is completed, and the reactor is opened to obtain a sol;
(2)配置氯铱酸的乙醇溶液,所述氯铱酸的乙醇溶液中,氯铱酸的浓度为1.2g/L,溶剂为乙醇;搅拌所述溶胶,然后在搅拌状态下向溶胶中加入所述氯铱酸的乙醇溶液,加料完成后继续搅拌溶液50min,然后向溶液中加入硼氢化钠溶液,所述硼氢化钠溶液中,硼氢化钠的浓度为1.6g/L,溶剂为水;向溶胶中加入所述氯铱酸的乙醇溶液、硼氢化钠溶液的体积比为溶胶:氯铱酸的乙醇溶液:硼氢化钠溶液=10:2:0.7;加料完成后搅拌溶液20min,然后向溶液中加入氨水(氨水中溶质的质量百分数为20%)将溶液的pH调节至10,然后搅拌溶液1h,固液分离,固相用去离子水洗涤3次,60℃烘干30min,获得复合物;(2) preparing an ethanol solution of chloroiridic acid, wherein the concentration of chloroiridic acid in the ethanol solution of chloroiridic acid is 1.2 g/L, and the solvent is ethanol; stirring the sol, then adding the ethanol solution of chloroiridic acid to the sol under stirring, and continuing to stir the solution for 50 min after the addition is completed, and then adding a sodium borohydride solution to the solution, wherein the concentration of sodium borohydride in the sodium borohydride solution is 1.6 g/L, and the solvent is water; adding the ethanol solution of chloroiridic acid and the sodium borohydride solution to the sol in a volume ratio of sol: ethanol solution of chloroiridic acid: sodium borohydride solution = 10:2:0.7; stirring the solution for 20 min after the addition is completed, and then adding ammonia water (the mass percentage of the solute in the ammonia water is 20%) to adjust the pH of the solution to 10, and then stirring the solution for 1 h, separating the solid and the liquid, washing the solid phase with deionized water for 3 times, and drying at 60° C. for 30 min to obtain a composite;
(3)配置γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液;所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液中,γ-甲基丙烯酰氧基丙基三甲氧基硅烷的质量百分数为3%,溶剂为乙醇;配置甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液;甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中,混合质量比为甲基丙烯酸三氟乙酯:偶氮二异丁腈:乙醇=2.8:0.9:100;将所述复合物分散在乙醇溶液中形成醇分散液,所述复合物分散在乙醇溶液中的固液质量比为复合物:乙醇=1:50;所述醇分散液水浴恒温至50±2℃保温,保温过程中搅拌醇分散液,冷凝回流,然后在搅拌状态下向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液,加料完成后50±2℃恒温搅拌醇分散液20min,然后向醇分散液中加入去离子水,向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液和所述去离子水的体积比为醇分散液:γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液:去离子水=10:3:1;加料完成后继续50±2℃恒温搅拌2h,然后固液分离,固相用乙醇洗涤2次,60℃烘干30min,烘干后的固相在氮气保护氛围内加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中形成混合物,烘干后的固相加入所述甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液中的质量比为固相:甲基丙烯酸三氟乙酯、偶氮二异丁腈的混合乙醇溶液=1:100;混合物在氮气保护氛围中水浴恒温至70±3℃保温10h,然后固液分离,固相用乙醇洗涤3次,60℃烘干1h,获得改性粉末;(3) preparing an ethanol solution of γ-methacryloxypropyl trimethoxysilane; in the ethanol solution of γ-methacryloxypropyl trimethoxysilane, the mass percentage of γ-methacryloxypropyl trimethoxysilane is 3%, and the solvent is ethanol; preparing a mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile; in the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile, the mixing mass ratio is trifluoroethyl methacrylate: azobisisobutyronitrile: ethanol = 2.8:0.9:100; dispersing the composite in the ethanol solution to form an alcohol dispersion, the solid-liquid mass ratio of the composite dispersed in the ethanol solution is composite: ethanol = 1:50; the alcohol dispersion is kept at a constant temperature of 50±2° C. in a water bath, the alcohol dispersion is stirred during the insulation process, condensed and refluxed, and then the ethanol solution of γ-methacryloxypropyl trimethoxysilane is added to the alcohol dispersion under stirring, and after the addition is completed, the alcohol dispersion is stirred at a constant temperature of 50±2° C. for 20 min. in, then add deionized water to the alcohol dispersion, add the ethanol solution of γ-methacryloxypropyltrimethoxysilane and the deionized water to the alcohol dispersion in a volume ratio of alcohol dispersion: ethanol solution of γ-methacryloxypropyltrimethoxysilane: deionized water = 10:3:1; after the addition is completed, continue to stir at a constant temperature of 50±2°C for 2h, then separate the solid and liquid, wash the solid phase with ethanol twice, and dry it at 60°C for 30min. The dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a nitrogen protective atmosphere to form a mixture, and the dried solid phase is added to the mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile in a mass ratio of solid phase: mixed ethanol solution of trifluoroethyl methacrylate and azobisisobutyronitrile = 1:100; the mixture is kept constant at 70±3°C in a water bath in a nitrogen protective atmosphere for 10h, then separate the solid and liquid, wash the solid phase with ethanol 3 times, and dry it at 60°C for 1h to obtain a modified powder;
(4)在铜圆线表面涂覆一层聚酯漆作为打底层(10μm),然后将所述改性粉末加入水性聚酰胺酰亚胺中形成涂覆液,所述改性粉末加入水性聚酰胺酰亚胺中的质量比为改性粉末:水性聚酰胺酰亚胺=10:100;涂覆液磁力搅拌40min,搅拌过程中超声处理,超声波功率为200W,频率为30kHz;搅拌结束后抽真空除气,然后涂覆在所述打底层上,涂覆完成后70℃保温1h,再150℃保温2h,再210℃保温2h,保温结束后以10℃/min冷却至常温,在打底层外部形成抗电晕层,抗电晕层厚度为20μm,获得本对比例所述漆包铜圆线。(4) A layer of polyester paint is coated on the surface of the copper round wire as a primer layer (10 μm), and then the modified powder is added to the aqueous polyamide-imide to form a coating liquid, wherein the mass ratio of the modified powder to the aqueous polyamide-imide is modified powder: aqueous polyamide-imide = 10:100; the coating liquid is magnetically stirred for 40 min, and ultrasonically treated during the stirring process, with an ultrasonic power of 200 W and a frequency of 30 kHz; after the stirring is completed, vacuum degassing is performed, and then the coating is applied on the primer layer. After the coating is completed, the coating is kept at 70° C. for 1 h, then at 150° C. for 2 h, and then at 210° C. for 2 h. After the insulation is completed, the coating is cooled to room temperature at a rate of 10° C./min to form an anti-corona layer on the outside of the primer layer. The thickness of the anti-corona layer is 20 μm, and the enameled copper round wire described in this comparative example is obtained.
对比例3Comparative Example 3
一种作为对比的漆包铜圆线,制备步骤包括:A comparative enameled round copper wire, the preparation steps include:
(1)配置硫酸氧钛的水溶液;所述硫酸氧钛的水溶液中,硫酸氧钛的浓度为7g/L;搅拌所述硫酸氧钛的水溶液,搅拌状态下向溶液中加入氨水,所述氨水中溶质的质量百分数为20%,向硫酸氧钛的溶液中加入氨水的体积比为硫酸氧钛的溶液:氨水=10:4;加料完成后溶液水浴恒温至85±5℃,到温后保温搅拌溶液2h,然后固液分离,固相用去离子水洗涤2次,洗涤后的固相加入反应釜中的双氧水溶液中,洗涤后的固相加入反应釜中的双氧水溶液中的质量比为固相:双氧水溶液=1:30;所述双氧水溶液中溶质的质量百分数为30%;超声搅拌溶液2h,超声波功率为200W,频率为30kHz;然后加水稀释溶液,加水稀释溶液至稀释前溶液体积的5倍;密封反应釜,加热至120℃水热保温处理8h,保温结束后空冷至常温,打开反应釜,获得溶胶;(1) preparing an aqueous solution of titanyl sulfate; in the aqueous solution of titanyl sulfate, the concentration of titanyl sulfate is 7 g/L; stirring the aqueous solution of titanyl sulfate, adding ammonia water to the solution under stirring, wherein the mass percentage of the solute in the ammonia water is 20%, and the volume ratio of ammonia water added to the solution of titanyl sulfate is titanyl sulfate solution: ammonia water = 10:4; after the addition is completed, the solution is kept at a constant temperature of 85±5° C. in a water bath, and after reaching the temperature, the solution is kept at a constant temperature and stirred for 2 hours, and then the solid-liquid separation is carried out, and the solid phase is washed twice with deionized water. The solid phase after washing is added to the hydrogen peroxide solution in the reactor, and the mass ratio of solid phase to hydrogen peroxide solution is 1:30; the mass percentage of the solute in the hydrogen peroxide solution is 30%; the solution is ultrasonically stirred for 2 hours, the ultrasonic power is 200W, and the frequency is 30kHz; then water is added to dilute the solution, and the volume of the solution before dilution is 5 times; the reactor is sealed, heated to 120°C for hydrothermal insulation treatment for 8 hours, and air-cooled to room temperature after the insulation is completed, and the reactor is opened to obtain a sol;
(2)配置氯铱酸的乙醇溶液,所述氯铱酸的乙醇溶液中,氯铱酸的浓度为1.2g/L,溶剂为乙醇;配置五氯化钽的乙醇溶液;所述五氯化钽的乙醇溶液中,五氯化钽的浓度为13g/L,溶剂为乙醇;搅拌所述溶胶,然后在搅拌状态下向溶胶中同时加入所述氯铱酸的乙醇溶液和五氯化钽的乙醇溶液,加料完成后继续搅拌溶液50min,然后向溶液中加入硼氢化钠溶液,所述硼氢化钠溶液中,硼氢化钠的浓度为1.6g/L,溶剂为水;向溶胶中加入所述氯铱酸的乙醇溶液、五氯化钽的乙醇溶液、硼氢化钠溶液的体积比为溶胶:氯铱酸的乙醇溶液:五氯化钽的乙醇溶液:硼氢化钠溶液=10:2:3:0.7;加料完成后搅拌溶液20min,然后向溶液中加入氨水(氨水中溶质的质量百分数为20%)将溶液的pH调节至10,然后搅拌溶液1h,固液分离,固相用去离子水洗涤3次,60℃烘干30min,获得复合物;(2) preparing an ethanol solution of chloroiridic acid, wherein the concentration of chloroiridic acid in the ethanol solution is 1.2 g/L, and the solvent is ethanol; preparing an ethanol solution of tantalum pentachloride, wherein the concentration of tantalum pentachloride in the ethanol solution is 13 g/L, and the solvent is ethanol; stirring the sol, and then adding the ethanol solution of chloroiridic acid and the ethanol solution of tantalum pentachloride to the sol while stirring, and continuing to stir the solution for 50 minutes after the addition is completed, and then adding a sodium borohydride solution to the solution, wherein the concentration of sodium borohydride in the sodium borohydride solution is 1 .6g/L, the solvent is water; the volume ratio of the ethanol solution of chloroiridic acid, the ethanol solution of tantalum pentachloride and the sodium borohydride solution is added to the sol: the ethanol solution of chloroiridic acid: the ethanol solution of tantalum pentachloride: the sodium borohydride solution = 10:2:3:0.7; after the addition is completed, the solution is stirred for 20 minutes, and then ammonia water (the mass percentage of the solute in the ammonia water is 20%) is added to the solution to adjust the pH of the solution to 10, and then the solution is stirred for 1 hour, the solid-liquid separation is carried out, the solid phase is washed with deionized water for 3 times, and dried at 60°C for 30 minutes to obtain a composite;
(3)配置γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液;所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液中,γ-甲基丙烯酰氧基丙基三甲氧基硅烷的质量百分数为3%,溶剂为乙醇;将所述复合物分散在乙醇溶液中形成醇分散液,所述复合物分散在乙醇溶液中的固液质量比为复合物:乙醇=1:50;所述醇分散液水浴恒温至50±2℃保温,保温过程中搅拌醇分散液,冷凝回流,然后在搅拌状态下向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液,加料完成后50±2℃恒温搅拌醇分散液20min,然后向醇分散液中加入去离子水,向所述醇分散液中加入所述γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液和所述去离子水的体积比为醇分散液:γ-甲基丙烯酰氧基丙基三甲氧基硅烷的乙醇溶液:去离子水=10:3:1;加料完成后继续50±2℃恒温搅拌2h,然后固液分离,固相用乙醇洗涤3次,60℃烘干1h,获得本对比例的改性粉末;(3) preparing an ethanol solution of γ-methacryloxypropyltrimethoxysilane; in the ethanol solution of γ-methacryloxypropyltrimethoxysilane, the mass percentage of γ-methacryloxypropyltrimethoxysilane is 3%, and the solvent is ethanol; dispersing the composite in the ethanol solution to form an alcohol dispersion, wherein the solid-liquid mass ratio of the composite dispersed in the ethanol solution is composite:ethanol=1:50; the alcohol dispersion is kept at a constant temperature of 50±2° C. in a water bath, the alcohol dispersion is stirred during the insulation process, condensed and refluxed, and then the γ-methacryloxypropyltrimethoxysilane is added to the alcohol dispersion under stirring. The ethanol solution of acryloxypropyltrimethoxysilane, after the addition is completed, the alcohol dispersion is stirred at a constant temperature of 50±2°C for 20 minutes, and then deionized water is added to the alcohol dispersion, and the volume ratio of the ethanol solution of γ-methacryloxypropyltrimethoxysilane and the deionized water is added to the alcohol dispersion in an alcohol dispersion: ethanol solution of γ-methacryloxypropyltrimethoxysilane: deionized water = 10:3:1; after the addition is completed, the constant temperature stirring is continued at 50±2°C for 2 hours, and then the solid-liquid separation is carried out, the solid phase is washed with ethanol 3 times, and dried at 60°C for 1 hour to obtain the modified powder of this comparative example;
(4)在铜圆线表面涂覆一层聚酯漆作为打底层(10μm),然后将所述改性粉末加入水性聚酰胺酰亚胺中形成涂覆液,所述改性粉末加入水性聚酰胺酰亚胺中的质量比为改性粉末:水性聚酰胺酰亚胺=10:100;涂覆液磁力搅拌40min,搅拌过程中超声处理,超声波功率为200W,频率为30kHz;搅拌结束后抽真空除气,然后涂覆在所述打底层上,涂覆完成后70℃保温1h,再150℃保温2h,再210℃保温2h,保温结束后以10℃/min冷却至常温,在打底层外部形成抗电晕层,抗电晕层厚度为20μm,获得本对比例所述漆包铜圆线。(4) A layer of polyester paint is coated on the surface of the copper round wire as a primer layer (10 μm), and then the modified powder is added to the aqueous polyamide-imide to form a coating liquid, wherein the mass ratio of the modified powder to the aqueous polyamide-imide is modified powder: aqueous polyamide-imide = 10:100; the coating liquid is magnetically stirred for 40 min, and ultrasonically treated during the stirring process, with an ultrasonic power of 200 W and a frequency of 30 kHz; after the stirring is completed, vacuum degassing is performed, and then the coating is applied on the primer layer. After the coating is completed, the coating is kept at 70° C. for 1 h, then at 150° C. for 2 h, and then at 210° C. for 2 h. After the insulation is completed, the coating is cooled to room temperature at a rate of 10° C./min to form an anti-corona layer on the outside of the primer layer. The thickness of the anti-corona layer is 20 μm, and the enameled copper round wire described in this comparative example is obtained.
实施例5Example 5
在漆包线耐电晕测试仪上测试上述各实施例和对比例所述方法制备的漆包铜圆线的耐电晕性能,另外测试对照试样作为对照组。对照试样的制备方法为:在铜圆线表面涂覆一层聚酯漆作为打底层(10μm),然后将水性聚酰胺酰亚胺涂覆在所述打底层上,涂覆完成后70℃保温1h,再150℃保温2h,再210℃保温2h,保温结束后以10℃/min冷却至常温,在打底层外部形成对照组层,对照组层厚度为20μm,获得对照试样。测试条件为:155℃测试温度,脉冲频率为20kHz,占空比为50%,脉冲电压的峰值设定为3kV,脉冲波形为方波。另外采用智能单向刮漆试验仪对上述各实施例和对比例所述方法制备的漆包铜圆线进行耐刮测试,结果如表1所示。The corona resistance of the enameled copper round wire prepared by the methods described in the above embodiments and comparative examples was tested on an enameled wire corona resistance tester, and a control sample was tested as a control group. The preparation method of the control sample is as follows: a layer of polyester paint is applied on the surface of the copper round wire as a primer layer (10 μm), and then a water-based polyamide-imide is applied on the primer layer. After the coating is completed, it is kept at 70°C for 1 hour, then kept at 150°C for 2 hours, and then kept at 210°C for 2 hours. After the insulation is completed, it is cooled to room temperature at 10°C/min to form a control group layer outside the primer layer. The thickness of the control group layer is 20 μm, and a control sample is obtained. The test conditions are: 155°C test temperature, pulse frequency of 20kHz, duty cycle of 50%, peak value of pulse voltage set to 3kV, and pulse waveform is square wave. In addition, an intelligent unidirectional paint scraping tester is used to carry out a scratch resistance test on the enameled copper round wire prepared by the methods described in the above embodiments and comparative examples, and the results are shown in Table 1.
由表1可知,本发明所述方法制备的漆包铜圆线具有良好的耐电晕效果,且耐刮力较高,漆膜在漆包线上的附着力度良好。这主要是由于本发明制备的改性粉末具有较大的比表面积,掺杂铱钽活性物质后,高压环境下,能够在聚酰胺酰亚胺漆膜内形成电荷弥散保护层,减少绝缘材料内部局部放电的强度,进而提高漆层的耐电晕效果;同时改性后的粉末提高了粉末在聚酰胺酰亚胺漆膜中的分散性,增强了粉末与基体的结合强度,一方面更加削弱了局部放电的可能性,另一方面提高了漆膜的强度,改善了聚酰胺酰亚胺漆膜的耐用性。As can be seen from Table 1, the enameled copper round wire prepared by the method of the present invention has good corona resistance, high scratch resistance, and good adhesion of the paint film on the enameled wire. This is mainly because the modified powder prepared by the present invention has a large specific surface area. After being doped with iridium tantalum active material, it can form a charge dispersion protection layer in the polyamide-imide paint film under high pressure, reduce the intensity of local discharge inside the insulating material, and thus improve the corona resistance of the paint layer; at the same time, the modified powder improves the dispersibility of the powder in the polyamide-imide paint film, enhances the bonding strength between the powder and the substrate, on the one hand, further weakens the possibility of local discharge, and on the other hand, improves the strength of the paint film and improves the durability of the polyamide-imide paint film.
表1Table 1
以上对本发明所提供的技术方案进行了详细介绍,对于本领域的一般技术人员,依据本发明实施例的思想,在具体实施方式及应用范围上均会有改变之处,综上所述,本说明书内容不应理解为对本发明的限制。The technical solution provided by the present invention is introduced in detail above. For those skilled in the art, according to the ideas of the embodiments of the present invention, there may be changes in the specific implementation methods and application scopes. In summary, the content of this specification should not be understood as limiting the present invention.
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