CN117854847A - Production process of anti-aging enameled rectangular copper wire - Google Patents
Production process of anti-aging enameled rectangular copper wire Download PDFInfo
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- CN117854847A CN117854847A CN202311852717.4A CN202311852717A CN117854847A CN 117854847 A CN117854847 A CN 117854847A CN 202311852717 A CN202311852717 A CN 202311852717A CN 117854847 A CN117854847 A CN 117854847A
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- Prior art keywords
- aging
- titanium dioxide
- nano titanium
- modified
- copper wire
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- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 86
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 78
- QUWAJPZDCZDTJS-UHFFFAOYSA-N 2-(2-hydroxyphenyl)sulfonylphenol Chemical compound OC1=CC=CC=C1S(=O)(=O)C1=CC=CC=C1O QUWAJPZDCZDTJS-UHFFFAOYSA-N 0.000 claims abstract description 70
- 238000002156 mixing Methods 0.000 claims abstract description 53
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000012964 benzotriazole Substances 0.000 claims abstract description 30
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000178 monomer Substances 0.000 claims abstract description 28
- 239000003973 paint Substances 0.000 claims abstract description 27
- ZAZINVQEIDWJRC-UHFFFAOYSA-N 1-(2,4-difluorophenyl)pyrrole Chemical compound FC1=CC(F)=CC=C1N1C=CC=C1 ZAZINVQEIDWJRC-UHFFFAOYSA-N 0.000 claims abstract description 25
- LEBRCVXHIFZXEM-UHFFFAOYSA-N 4-(benzotriazol-2-yl)benzene-1,3-diol Chemical compound OC1=CC(O)=CC=C1N1N=C2C=CC=CC2=N1 LEBRCVXHIFZXEM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052802 copper Inorganic materials 0.000 claims abstract description 22
- 239000010949 copper Substances 0.000 claims abstract description 22
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims abstract description 18
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims abstract description 14
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- FPZQYYXSOJSITC-UHFFFAOYSA-N 1-(4-chlorophenyl)pyrrole-2,5-dione Chemical compound C1=CC(Cl)=CC=C1N1C(=O)C=CC1=O FPZQYYXSOJSITC-UHFFFAOYSA-N 0.000 claims abstract description 12
- WCJYTPVNMWIZCG-UHFFFAOYSA-N xylylcarb Chemical compound CNC(=O)OC1=CC=C(C)C(C)=C1 WCJYTPVNMWIZCG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000008021 deposition Effects 0.000 claims abstract description 7
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims description 58
- 238000003756 stirring Methods 0.000 claims description 58
- 238000010438 heat treatment Methods 0.000 claims description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 239000008367 deionised water Substances 0.000 claims description 33
- 229910021641 deionized water Inorganic materials 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 28
- 239000011259 mixed solution Substances 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide Chemical compound CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 claims description 14
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 14
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 12
- 150000004985 diamines Chemical class 0.000 claims description 10
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 7
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 7
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 7
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 206010051246 Photodermatosis Diseases 0.000 abstract description 10
- 230000008845 photoaging Effects 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 12
- 238000005457 optimization Methods 0.000 description 8
- 239000004642 Polyimide Substances 0.000 description 7
- 229920001721 polyimide Polymers 0.000 description 7
- 230000032683 aging Effects 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 210000003298 dental enamel Anatomy 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 125000000168 pyrrolyl group Chemical group 0.000 description 4
- 230000002441 reversible effect Effects 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000006352 cycloaddition reaction Methods 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- 241001391944 Commicarpus scandens Species 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- DLINORNFHVEIFE-UHFFFAOYSA-N hydrogen peroxide;zinc Chemical compound [Zn].OO DLINORNFHVEIFE-UHFFFAOYSA-N 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 125000005439 maleimidyl group Chemical group C1(C=CC(N1*)=O)=O 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004962 Polyamide-imide Substances 0.000 description 1
- -1 [1,2,3] triazole-2-yl Chemical group 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- YCIMNLLNPGFGHC-UHFFFAOYSA-N o-dihydroxy-benzene Natural products OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 229920003055 poly(ester-imide) Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 1
- 229960001755 resorcinol Drugs 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000010998 test method Methods 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/303—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups H01B3/38 or H01B3/302
- H01B3/306—Polyimides or polyesterimides
-
- 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
-
- 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
- H01B7/28—Protection against damage caused by moisture, corrosion, chemical attack or weather
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses a production process of an anti-aging enameled rectangular copper wire, and relates to the technical field of wires and cables. When the anti-aging enameled rectangular copper wire is prepared, 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol and crotonyl chloride are reacted to obtain a benzotriazole monomer containing double bonds; the method comprises the steps of carrying out deposition polymerization on a benzotriazole monomer containing double bonds, methyl acrylate and acrylamide on the surface of nano titanium dioxide, and then reacting with N- (4-chlorophenyl) -maleimide to obtain modified nano titanium dioxide; then reacting 1- (2, 4-difluorophenyl) -1H-pyrrole with sulfonyl diphenol to obtain modified sulfonyl diphenol, reacting the modified sulfonyl diphenol with pyromellitic dianhydride and 4,4' -diaminodiphenyl ether, and blending the modified sulfonyl diphenol with modified nano titanium dioxide to obtain the anti-aging paint; finally, the anti-aging paint is soaked on the copper flat wire and imidized, so that the anti-aging enameled copper flat wire is manufactured. The anti-aging enameled rectangular copper wire prepared by the invention has excellent corona resistance, photo-aging resistance, insulating property and self-repairing property.
Description
Technical Field
The invention relates to the technical field of wires and cables, in particular to a production process of an anti-aging enameled rectangular copper wire.
Background
With the improvement of economic and civil living standards, the demands of wire enamels in the military and civil fields are rapidly increasing. As a coating material excellent in electrical insulation properties, wire enamel is an indispensable material for electrical equipment. The quality of the product is directly related to the economic and technical index and the service life of the electrical equipment. Because the motor electrical appliance always tends to be small in size and large in power, the coil can generate very large heat in the running process, so that the heat-resistant grade of the insulating material is required to be higher and higher, the development of nuclear power and space technology further provides severe high-temperature resistant requirements for the winding wire, and meanwhile, the winding wire is required to have good surface properties in the mechanized and high-speed processes of the winding.
Polyimide has excellent mechanical property, heat resistance, ageing resistance, dimensional stability and chemical stability, and is one of wires and cables with highest thermal stability. Polyimide is therefore widely used as a film, an insulating coating, a structural adhesive, a resin matrix, and wire enamel in the fields of electronics, nuclear power, aerospace, information industry, and automobile manufacturing. Compared with the traditional coatings for enamelled wires, such as polyurethane, polyester imide, polyamide imide, polyester, acetal and the like, polyimide has more excellent thermal performance, and the comprehensive performance of the coating is better than that of other traditional coatings. However, polyimide wire enamel is subject to wear, aging, and the like during actual use. Therefore, the anti-aging enameled rectangular copper wire with excellent corona resistance, photo-aging resistance, insulating property and self-repairing property is prepared.
Disclosure of Invention
The invention aims to provide a production process of an anti-aging enameled rectangular copper wire, which aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the production process of the anti-aging enameled rectangular copper wire is characterized in that the anti-aging enameled rectangular copper wire is obtained by carrying out imidization after the anti-aging enameled rectangular copper wire is soaked by the anti-aging paint.
As optimization, the anti-aging paint is obtained by mixing modified sulfonyl diphenol, pyromellitic dianhydride and 4,4' -diaminodiphenyl ether after reaction with modified nano titanium dioxide.
Preferably, the modified sulfonyl diphenol is obtained by reacting 1- (2, 4-difluorophenyl) -1H-pyrrole with sulfonyl diphenol.
As optimization, the modified nano titanium dioxide is obtained by carrying out deposition polymerization on a benzotriazole monomer containing double bonds, methyl acrylate and acrylamide on the surface of the nano titanium dioxide and then reacting with N- (4-chlorophenyl) -maleimide.
As optimization, the model of the nano titanium dioxide is CY-J25, which is obtained from Shanghai long trade chemical industry Co.
Preferably, the benzotriazole monomer containing a double bond is obtained by reacting 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol with crotonyl chloride.
The production process of the anti-aging enameled rectangular copper wire comprises the following preparation steps:
(1) Uniformly mixing 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, crotonyl chloride, triethylamine and tetrahydrofuran according to the mass ratio of 1 (0.8-1): (0.6-0.7): (6-8), stirring at 100-200 rpm for 10-30 min, adding a developing agent 3-5 times the mass of 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, continuing to react at 1-5 ℃ for 4-6H, adding a sodium bicarbonate solution with the mass ratio of 10-12 times that of 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, standing for 10-14H, taking an upper layer solution, evaporating and drying for 6-8H, recrystallizing with absolute ethyl alcohol, and drying for 10-12H at 40-50 ℃ to obtain a benzotriazole monomer containing double bonds;
(2) The benzotriazole monomer containing double bonds, methyl acrylate, acrylamide, N-dimethylformamide, benzoyl peroxide and deionized water are mixed according to the mass ratio
1 (1-1.2): 0.2-0.4): 4-6): 0.01-0.02): 10-12, stirring for 20-30 min at 200-300 rpm to prepare a mixed solution; uniformly mixing nano titanium dioxide and deionized water according to a mass ratio of 1 (10-12), stirring for 10-30 min at 20-30 ℃ at 200-300 rpm, dripping mixed solution with the mass 2-4 times of the nano titanium dioxide at uniform speed within 20-30 min, continuously stirring for 30-40 min, reacting for 5-15 min at 45-55 ℃, heating to 115-125 ℃ for continuously reacting for 10-20 min, cooling to room temperature, filtering, washing for 3-5 times with acetone, and drying for 16-20 h at 55-65 ℃ to obtain the pre-modified nano titanium dioxide; uniformly mixing pre-modified nano titanium dioxide and dimethyl sulfoxide according to the mass ratio of 1 (10-12), performing ultrasonic dispersion for 20-40 min at 20-30 ℃, heating to 90-100 ℃, adding N- (4-chlorophenyl) -maleimide with the mass of 2-4 times of that of the pre-modified nano titanium dioxide, continuously reacting for 8-10 h, adding deionized water with the mass of 20-30 times of that of the pre-modified nano titanium dioxide, standing for 4-8 h at 50-60 ℃, filtering, washing for 3-5 times by using the deionized water, and drying for 10-12 h at 55-65 ℃ to obtain modified nano titanium dioxide;
(3) Uniformly mixing 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfonyl diphenol according to a molar ratio of 1:2, adding 0.01-0.02 times of anhydrous potassium carbonate and 10-12 times of sulfolane of 1- (2, 4-difluorophenyl) -1H-pyrrole, stirring for 10-30 min at 100-200 rpm, reacting for 1-3H at 110-130 ℃ and 200-300 rpm in a nitrogen environment, taking out all water generated by the reaction, heating to 220-240 ℃ to continue the reaction for 2-4H, respectively washing 3-5 times by using methanol and deionized water, and drying for 8-10H at 95-105 ℃ to obtain modified sulfonyl diphenol;
(4) Uniformly mixing 4,4' -diaminodiphenyl ether and N, N-dimethylacetamide according to the mass ratio of 1 (4-5), and stirring at 100-300 rpm for 30-50 min to obtain diamine mixed solution; uniformly mixing modified sulfonyl diphenol, 4-dimethylaminopyridine, 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide and N, N-dimethylformamide according to the mass ratio of 1 (0.01-0.02) (10-14), stirring at 100-200 rpm for 10-30 min under the nitrogen environment at 20-30 ℃, heating to 140-160 ℃, adding pyromellitic dianhydride which is 0.5-1.5 times of the mass of the modified sulfonyl diphenol every 20-40 min, reacting for 3-5 h, adding a diammine mixed solution which is 5-15 times of the mass of the modified sulfonyl diphenol, continuously reacting for 3-5 h, adding modified nano titanium dioxide which is 0.6-0.7 times of the mass of the modified sulfonyl diphenol, stirring at 100-200 rpm for 10-20 min, and obtaining anti-aging paint;
(5) And (3) soaking the copper flat wire in anti-aging paint, taking out, drying at 75-85 ℃ under 0.05-0.15 MPa for 1-3 hours, soaking again, repeating for 2-4 times, heating to 115-125 ℃ and continuously drying for 0.5-1.5 hours, heating to 145-155 ℃ and drying for 0.5-1.5 hours, transferring into a muffle furnace, standing for 2-4 hours at 170-190 ℃, heating to 290-310 ℃ and continuously standing for 2-4 hours to obtain the anti-aging enameled copper flat wire.
As optimization, the developing agent in the step (1) is obtained by uniformly mixing ethyl acetate and petroleum ether according to a mass ratio of 1:8.
As an optimization, the reaction equation of the benzotriazole monomer containing double bonds in the step (1) is as follows:
as an optimization, the reaction equation of the modified nano titanium dioxide in the step (2) is as follows:
as an optimization, the reaction equation of the modified sulfonyl diphenol in the step (3) is as follows:
as optimization, the reaction equation of the anti-aging enameled rectangular copper wire in the step (5) is as follows:
compared with the prior art, the invention has the following beneficial effects:
when the anti-aging enameled rectangular copper wire is prepared, 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol and crotonyl chloride are reacted to obtain a benzotriazole monomer containing double bonds; the method comprises the steps of carrying out deposition polymerization on a benzotriazole monomer containing double bonds, methyl acrylate and acrylamide on the surface of nano titanium dioxide, and then reacting with N- (4-chlorophenyl) -maleimide to obtain modified nano titanium dioxide; then reacting 1- (2, 4-difluorophenyl) -1H-pyrrole with sulfonyl diphenol to obtain modified sulfonyl diphenol, reacting the modified sulfonyl diphenol with pyromellitic dianhydride and 4,4' -diaminodiphenyl ether, and blending the modified sulfonyl diphenol with modified nano titanium dioxide to obtain the anti-aging paint; and finally, carrying out imidization on the anti-aging paint soaked copper flat wire to prepare the anti-aging enameled copper flat wire.
Firstly, reacting 4- (2H-benzo [ d ] [1,2,3] triazole-2-yl) benzene-1, 3-diol and crotonyl chloride to obtain a benzotriazole monomer containing double bonds; the method comprises the steps of carrying out deposition polymerization on a benzotriazole monomer containing double bonds, methyl acrylate and acrylamide on the surface of nano titanium dioxide, and then reacting with N- (4-chlorophenyl) -maleimide to obtain modified nano titanium dioxide; the benzotriazole monomer containing double bonds, methyl acrylate and acrylamide are subjected to deposition polymerization on the surface of nano titanium dioxide, so that the dispersibility of the nano titanium dioxide is improved, and the corona resistance and the photo-aging resistance of the anti-aging enameled rectangular copper wire are enhanced; simultaneously introducing a benzotriazole and an amino structure, wherein a hydrogen bond in the benzotriazole structure is easy to break after being irradiated by ultraviolet light to form an unstable tautomer, and the absorbed ultraviolet light energy is converted into heat energy, so that the anti-photoaging performance of the anti-aging enameled rectangular copper wire is further enhanced; the introduced amino reacts with chlorine atoms on N- (4-chlorophenyl) -maleimide, and the maleimide structure is grafted on the surface of nano titanium dioxide, so that the nano titanium dioxide can be subjected to thermal reversible cycloaddition reaction with pyrrole on modified sulfonyl diphenol, and the self-repairing performance of the anti-aging enameled rectangular copper wire is improved.
Secondly, reacting 1- (2, 4-difluorophenyl) -1H-pyrrole with sulfonyl diphenol to obtain modified sulfonyl diphenol, reacting the modified sulfonyl diphenol with pyromellitic dianhydride and 4,4' -diaminodiphenyl ether, and blending the modified sulfonyl diphenol with modified nano titanium dioxide to obtain the anti-aging paint; then, carrying out imidization on the anti-aging paint soaked copper flat wire to prepare an anti-aging enameled copper flat wire; 1- (2, 4-difluorophenyl) -1H-pyrrole is grafted on sulfonyl diphenol to participate in the copolymerization of polyimide, so that the self-repairing performance of the anti-aging enameled rectangular copper wire is improved by introducing a pyrrole structure on a main chain and performing a thermal reversible cycloaddition reaction with maleimide on the surface of modified nano zinc dioxide.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for describing the detailed description, and the test method of each index of the anti-aging enameled rectangular copper wire manufactured in the following examples is as follows:
corona resistance: the anti-aging enameled rectangular copper wire obtained in each example is the same as that of the comparative example, a round electrode with the diameter of 2mm is used for clamping the electrode on the surface of a film, a WPT type corona aging instrument of the Wifar company in Changzhou is used for carrying out corona treatment at 30 ℃, 3kV and 20kHz, the corona aging time is measured, and corona resistance is judged.
Anti-photoaging properties: the anti-aging enameled rectangular copper wire obtained in each example and the comparative example material are taken as samples with the same size, placed into a photo-oxidation aging test box, irradiated for 400 hours under the ultraviolet wavelength of 400nm, and the tensile strength retention rate is calculated to judge the photo-aging resistance.
Insulation properties: the anti-aging enameled rectangular copper wire obtained in each embodiment is the same as the comparative example in size, and the volume resistance of a paint film is measured under the condition of 100V voltage by using a YH-8200 type digital insulation resistance tester to judge the insulation performance.
Self-repairing performance: the results of the examples were obtainedThe anti-aging enameled rectangular copper wire and the comparative example material are taken to have the same size, the tensile strength is tested according to GB/T13022, a cutter mark is drawn at 110 ℃, the tensile strength is tested again after standing for 24 hours at 60 ℃, and the repair efficiency = sigma is calculated Rear part (S) /σ Front part 。
Example 1
The production process of the anti-aging enameled rectangular copper wire comprises the following preparation steps:
(1) Uniformly mixing 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, crotonyl chloride, triethylamine and tetrahydrofuran according to the mass ratio of 1:0.8:0.6:6, stirring for 30min at 100rpm, adding a developing agent 3 times the mass of 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, continuously reacting at 1 ℃ for 6H, adding a sodium bicarbonate solution with the mass ratio of 10 times the mass of 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol of 6%, standing for 10H, taking an upper solution, evaporating and drying for 6H, recrystallizing with absolute ethyl alcohol, and drying for 12H at 40 ℃ to obtain a benzotriazole monomer containing double bonds;
(2) Uniformly mixing a benzotriazole monomer containing double bonds, methyl acrylate, acrylamide, N-dimethylformamide, benzoyl peroxide and deionized water according to the mass ratio of 1:1:0.2:4:0.01:10, and stirring at 200rpm for 30min to prepare a mixed solution; uniformly mixing nano titanium dioxide and deionized water according to a mass ratio of 1:10, stirring for 30min at 20 ℃ and 200rpm, uniformly dripping mixed solution with the mass 2 times of the nano titanium dioxide in the 20min, continuously stirring for 30min, reacting for 15min at 45 ℃, heating to 115 ℃ for continuously reacting for 20min, cooling to room temperature, filtering, washing for 3 times by acetone, and drying for 20h at 55 ℃ to obtain the pre-modified nano titanium dioxide; uniformly mixing pre-modified nano titanium dioxide and dimethyl sulfoxide according to a mass ratio of 1:10, performing ultrasonic dispersion for 40min at 20 ℃, heating to 90 ℃, adding N- (4-chlorophenyl) -maleimide with the mass 2 times that of the pre-modified nano titanium dioxide, continuously reacting for 10h, adding deionized water with the mass 20 times that of the pre-modified nano titanium dioxide, standing for 8h at 50 ℃, filtering, washing for 3 times with the deionized water, and drying for 12h at 55 ℃ to obtain modified nano titanium dioxide;
(3) Uniformly mixing 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfonyl diphenol according to a molar ratio of 1:2, adding anhydrous potassium carbonate with the mass of 0.01 times that of 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfolane with the mass of 10 times that of 1- (2, 4-difluorophenyl) -1H-pyrrole, stirring for 30min at 100rpm, reacting for 3H at 110 ℃ under a nitrogen environment at 200rpm, taking out all water generated by the reaction, heating to 220 ℃ for continuous reaction for 4H, washing for 3 times respectively by using methanol and deionized water, and drying for 10H at 95 ℃ to obtain modified sulfonyl diphenol;
(4) Uniformly mixing 4,4' -diaminodiphenyl ether and N, N-dimethylacetamide according to a mass ratio of 1:4, and stirring at 100rpm for 50min to obtain diamine mixed solution; uniformly mixing modified sulfonyl diphenol, 4-dimethylaminopyridine, 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide and N, N-dimethylformamide according to the mass ratio of 1:0.01:0.01:10, stirring for 30min at 100rpm at 20 ℃ under a nitrogen environment, heating to 140 ℃, adding pyromellitic dianhydride with the mass of 0.5 times of the modified sulfonyl diphenol every 20min for reacting for 5h, adding a diammine mixed solution with the mass of 5 times of the modified sulfonyl diphenol, adding pyromellitic dianhydride with the mass of 1 time of the modified sulfonyl diphenol at constant speed within 40min, continuing to react for 5h, adding modified nano titanium dioxide with the mass of 0.6 times of the modified sulfonyl diphenol, and stirring for 20min at 100rpm to obtain anti-aging paint;
(5) And (3) taking out the copper flat wire after being soaked in the anti-aging paint, drying at 75 ℃ under 0.05MPa for 3 hours, soaking again, repeating for 2 times, heating to 115 ℃ and continuously drying for 1.5 hours, heating to 145 ℃ and drying for 1.5 hours, transferring into a muffle furnace, standing for 4 hours at 170 ℃, heating to 290 ℃ and continuously standing for 4 hours, and thus obtaining the anti-aging enameled copper flat wire.
Example 2
The production process of the anti-aging enameled rectangular copper wire comprises the following preparation steps:
(1) Uniformly mixing 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, crotonyl chloride, triethylamine and tetrahydrofuran according to the mass ratio of 1:0.9:0.65:7, stirring for 20min at 150rpm, adding a developing agent which is 4 times the mass of the 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, continuously reacting for 5H at 3 ℃, adding a sodium bicarbonate solution which is 11 times the mass of the 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol and has the mass ratio of 6.5%, standing for 12H, taking an upper solution, evaporating and drying for 7H, recrystallizing with absolute ethyl alcohol, and drying for 11H at 45 ℃ to obtain a benzotriazole monomer containing double bonds;
(2) Uniformly mixing a benzotriazole monomer containing double bonds, methyl acrylate, acrylamide, N-dimethylformamide, benzoyl peroxide and deionized water according to the mass ratio of 1:1.1:0.3:5:0.015:11, and stirring at 250rpm for 25min to prepare a mixed solution; uniformly mixing nano titanium dioxide and deionized water according to a mass ratio of 1:11, stirring at 25 ℃ for 20min at 250rpm, uniformly dripping mixed solution with the mass 3 times of the nano titanium dioxide in 25min, continuously stirring for 35min, reacting at 50 ℃ for 10min, heating to 120 ℃ for continuously reacting for 15min, cooling to room temperature, filtering, washing with acetone for 4 times, and drying at 60 ℃ for 18h to obtain the pre-modified nano titanium dioxide; uniformly mixing pre-modified nano titanium dioxide and dimethyl sulfoxide according to a mass ratio of 1:11, performing ultrasonic dispersion for 30min at 25 ℃, heating to 95 ℃, adding N- (4-chlorophenyl) -maleimide with 3 times of the mass of the pre-modified nano titanium dioxide, continuously reacting for 9h, adding deionized water with 25 times of the mass of the pre-modified nano titanium dioxide, standing for 6h at 55 ℃, filtering, washing for 4 times with the deionized water, and drying for 11h at 60 ℃ to obtain modified nano titanium dioxide;
(3) Uniformly mixing 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfonyl diphenol according to a molar ratio of 1:2, adding anhydrous potassium carbonate with the mass of 0.015 times of that of 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfolane with the mass of 11 times of that of 1- (2, 4-difluorophenyl) -1H-pyrrole, stirring for 20min at 150rpm, reacting for 2H at 120 ℃ in a nitrogen environment at 250rpm, taking out all water generated by the reaction, heating to 230 ℃ for continuous reaction for 3H, washing for 4 times respectively by using methanol and deionized water, and drying for 9H at 100 ℃ to obtain modified sulfonyl diphenol;
(4) Uniformly mixing 4,4' -diaminodiphenyl ether and N, N-dimethylacetamide according to a mass ratio of 1:4.5, and stirring at 200rpm for 40min to obtain diamine mixed solution; uniformly mixing modified sulfonyl diphenol, 4-dimethylaminopyridine, 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide and N, N-dimethylformamide according to the mass ratio of 1:0.015:0.015:12, stirring for 20min at 25 ℃ and 150rpm under a nitrogen environment, heating to 150 ℃, adding pyromellitic dianhydride with the mass 1 time of the modified sulfonyl diphenol every 30min, reacting for 4h, adding a diamine mixed solution with the mass 10 times of the modified sulfonyl diphenol, adding pyromellitic dianhydride with the mass 2 times of the modified sulfonyl diphenol at a constant speed within 50min, continuously reacting for 4h, adding modified nano titanium dioxide with the mass 0.65 time of the modified sulfonyl diphenol, and stirring for 15min at 150rpm to obtain the anti-aging paint;
(5) And taking out the copper flat wire after soaking in the anti-aging paint, drying at 80 ℃ under 0.1MPa for 2 hours, soaking again, repeating for 3 times, heating to 120 ℃ and continuously drying for 1 hour, heating to 150 ℃ and drying for 1 hour, transferring into a muffle furnace, standing for 3 hours at 180 ℃, heating to 300 ℃ and continuously standing for 3 hours to obtain the anti-aging enameled copper flat wire.
Example 3
The production process of the anti-aging enameled rectangular copper wire comprises the following preparation steps:
(1) Uniformly mixing 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, crotonyl chloride, triethylamine and tetrahydrofuran according to the mass ratio of 1:1:0.7:8, stirring for 10min at 200rpm, adding a developing agent which is 5 times the mass of the 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, continuing to react for 4H at 5 ℃, adding a sodium bicarbonate solution with the mass fraction of 12 times that of the 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol of 7%, standing for 14H, taking an upper solution, evaporating and drying for 8H, recrystallizing with absolute ethyl alcohol, and drying for 10H at 50 ℃ to obtain a benzotriazole monomer containing double bonds;
(2) Uniformly mixing a benzotriazole monomer containing double bonds, methyl acrylate, acrylamide, N-dimethylformamide, benzoyl peroxide and deionized water according to the mass ratio of 1:1.2:0.4:6:0.02:12, and stirring at 300rpm for 20min to prepare a mixed solution; uniformly mixing nano titanium dioxide and deionized water according to a mass ratio of 1:12, stirring for 10min at 30 ℃ and 300rpm, uniformly dripping mixed solution with the mass 4 times of the nano titanium dioxide in 30min, continuously stirring for 40min, reacting for 5min at 55 ℃, heating to 125 ℃ for continuously reacting for 10min, cooling to room temperature, filtering, washing for 5 times by acetone, and drying for 16h at 65 ℃ to obtain the pre-modified nano titanium dioxide; uniformly mixing pre-modified nano titanium dioxide and dimethyl sulfoxide according to a mass ratio of 1:12, performing ultrasonic dispersion for 20min at 30 ℃, heating to 100 ℃, adding N- (4-chlorophenyl) -maleimide with the mass 4 times that of the pre-modified nano titanium dioxide, continuously reacting for 8h, adding deionized water with the mass 30 times that of the pre-modified nano titanium dioxide, standing for 4h at 60 ℃, filtering, washing for 5 times with deionized water, and drying for 10h at 65 ℃ to obtain modified nano titanium dioxide;
(3) Uniformly mixing 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfonyl diphenol according to a molar ratio of 1:2, adding anhydrous potassium carbonate with the mass of 0.02 times of that of 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfolane with the mass of 12 times of that of 1- (2, 4-difluorophenyl) -1H-pyrrole, stirring for 10min at 200rpm, reacting for 1H at 130 ℃ under nitrogen environment and 300rpm, taking out all water generated by the reaction, heating to 240 ℃ for continuous reaction for 2H, washing for 5 times respectively by using methanol and deionized water, and drying for 8H at 105 ℃ to obtain modified sulfonyl diphenol;
(4) Uniformly mixing 4,4' -diaminodiphenyl ether and N, N-dimethylacetamide according to a mass ratio of 1:5, and stirring at 300rpm for 30min to obtain diamine mixed solution; uniformly mixing modified sulfonyl diphenol, 4-dimethylaminopyridine, 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide and N, N-dimethylformamide according to the mass ratio of 1:0.02:0.02:14, stirring for 10min at 200rpm at 30 ℃ under a nitrogen environment, heating to 160 ℃, adding pyromellitic dianhydride with the mass of 1.5 times of that of the modified sulfonyl diphenol every 40min for reaction for 3h, adding a diammine mixed solution with the mass of 15 times of that of the modified sulfonyl diphenol, adding pyromellitic dianhydride with the mass of 3 times of that of the modified sulfonyl diphenol at constant speed within 60min, continuing to react for 3h, adding modified nano titanium dioxide with the mass of 0.7 times of that of the modified sulfonyl diphenol, and stirring for 10min at 200rpm to obtain anti-aging paint;
(5) And taking out the copper flat wire after being soaked in the anti-aging paint, drying at 85 ℃ and 0.15MPa for 1h, soaking again, repeating for 4 times, heating to 125 ℃ and continuously drying for 0.5h, heating to 155 ℃ and drying for 0.5h, transferring into a muffle furnace, standing at 190 ℃ for 2h, heating to 310 ℃ and continuously standing for 2h, and thus obtaining the anti-aging enameled copper flat wire.
Comparative example 1
The production process of the anti-aging enameled rectangular copper wire comprises the following preparation steps:
(1) Uniformly mixing 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, crotonyl chloride, triethylamine and tetrahydrofuran according to the mass ratio of 1:0.9:0.65:7, stirring for 20min at 150rpm, adding a developing agent which is 4 times the mass of the 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, continuously reacting for 5H at 3 ℃, adding a sodium bicarbonate solution which is 11 times the mass of the 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol and has the mass ratio of 6.5%, standing for 12H, taking an upper solution, evaporating and drying for 7H, recrystallizing with absolute ethyl alcohol, and drying for 11H at 45 ℃ to obtain a benzotriazole monomer containing double bonds;
(2) Uniformly mixing a benzotriazole monomer containing double bonds, methyl acrylate, acrylamide, N-dimethylformamide, benzoyl peroxide and deionized water according to the mass ratio of 1:1.1:0.3:5:0.015:11, and stirring at 250rpm for 25min to prepare a mixed solution; uniformly mixing nano titanium dioxide and deionized water according to a mass ratio of 1:11, stirring at 25 ℃ for 20min at 250rpm, uniformly dripping mixed solution with the mass 3 times of the nano titanium dioxide in 25min, continuously stirring for 35min, reacting at 50 ℃ for 10min, heating to 120 ℃ for continuously reacting for 15min, cooling to room temperature, filtering, washing with acetone for 4 times, and drying at 60 ℃ for 18h to obtain modified nano titanium dioxide;
(3) Uniformly mixing 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfonyl diphenol according to a molar ratio of 1:2, adding anhydrous potassium carbonate with the mass of 0.015 times of that of 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfolane with the mass of 11 times of that of 1- (2, 4-difluorophenyl) -1H-pyrrole, stirring for 20min at 150rpm, reacting for 2H at 120 ℃ in a nitrogen environment at 250rpm, taking out all water generated by the reaction, heating to 230 ℃ for continuous reaction for 3H, washing for 4 times respectively by using methanol and deionized water, and drying for 9H at 100 ℃ to obtain modified sulfonyl diphenol;
(4) Uniformly mixing 4,4' -diaminodiphenyl ether and N, N-dimethylacetamide according to a mass ratio of 1:4.5, and stirring at 200rpm for 40min to obtain diamine mixed solution; uniformly mixing modified sulfonyl diphenol, 4-dimethylaminopyridine, 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide and N, N-dimethylformamide according to the mass ratio of 1:0.015:0.015:12, stirring for 20min at 25 ℃ and 150rpm under a nitrogen environment, heating to 150 ℃, adding pyromellitic dianhydride with the mass 1 time of the modified sulfonyl diphenol every 30min, reacting for 4h, adding a diamine mixed solution with the mass 10 times of the modified sulfonyl diphenol, adding pyromellitic dianhydride with the mass 2 times of the modified sulfonyl diphenol at a constant speed within 50min, continuously reacting for 4h, adding modified nano titanium dioxide with the mass 0.65 time of the modified sulfonyl diphenol, and stirring for 15min at 150rpm to obtain the anti-aging paint;
(5) And taking out the copper flat wire after soaking in the anti-aging paint, drying at 80 ℃ under 0.1MPa for 2 hours, soaking again, repeating for 3 times, heating to 120 ℃ and continuously drying for 1 hour, heating to 150 ℃ and drying for 1 hour, transferring into a muffle furnace, standing for 3 hours at 180 ℃, heating to 300 ℃ and continuously standing for 3 hours to obtain the anti-aging enameled copper flat wire.
Comparative example 2
The production process of the anti-aging enameled rectangular copper wire comprises the following preparation steps:
(1) Uniformly mixing 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfonyl diphenol according to a molar ratio of 1:2, adding anhydrous potassium carbonate with the mass of 0.015 times of that of 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfolane with the mass of 11 times of that of 1- (2, 4-difluorophenyl) -1H-pyrrole, stirring for 20min at 150rpm, reacting for 2H at 120 ℃ in a nitrogen environment at 250rpm, taking out all water generated by the reaction, heating to 230 ℃ for continuous reaction for 3H, washing for 4 times respectively by using methanol and deionized water, and drying for 9H at 100 ℃ to obtain modified sulfonyl diphenol;
(2) Uniformly mixing 4,4' -diaminodiphenyl ether and N, N-dimethylacetamide according to a mass ratio of 1:4.5, and stirring at 200rpm for 40min to obtain diamine mixed solution; uniformly mixing modified sulfonyl diphenol, 4-dimethylaminopyridine, 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide and N, N-dimethylformamide according to the mass ratio of 1:0.015:0.015:12, stirring for 20min at 25 ℃ and 150rpm under a nitrogen environment, heating to 150 ℃, adding pyromellitic dianhydride with the mass 1 time of the modified sulfonyl diphenol every 30min, reacting for 4h, adding a diamine mixed solution with the mass 10 times of the modified sulfonyl diphenol, adding pyromellitic dianhydride with the mass 2 times of the modified sulfonyl diphenol at a constant speed within 50min, continuously reacting for 4h, adding nano titanium dioxide with the mass 0.65 time of the modified sulfonyl diphenol, and stirring for 15min at 150rpm to obtain the anti-aging paint;
(3) And taking out the copper flat wire after soaking in the anti-aging paint, drying at 80 ℃ under 0.1MPa for 2 hours, soaking again, repeating for 3 times, heating to 120 ℃ and continuously drying for 1 hour, heating to 150 ℃ and drying for 1 hour, transferring into a muffle furnace, standing for 3 hours at 180 ℃, heating to 300 ℃ and continuously standing for 3 hours to obtain the anti-aging enameled copper flat wire.
Comparative example 3
The production process of the anti-aging enameled rectangular copper wire comprises the following preparation steps:
(1) Uniformly mixing 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, crotonyl chloride, triethylamine and tetrahydrofuran according to the mass ratio of 1:0.9:0.65:7, stirring for 20min at 150rpm, adding a developing agent which is 4 times the mass of the 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, continuously reacting for 5H at 3 ℃, adding a sodium bicarbonate solution which is 11 times the mass of the 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol and has the mass ratio of 6.5%, standing for 12H, taking an upper solution, evaporating and drying for 7H, recrystallizing with absolute ethyl alcohol, and drying for 11H at 45 ℃ to obtain a benzotriazole monomer containing double bonds;
(2) Uniformly mixing a benzotriazole monomer containing double bonds, methyl acrylate, acrylamide, N-dimethylformamide, benzoyl peroxide and deionized water according to the mass ratio of 1:1.1:0.3:5:0.015:11, and stirring at 250rpm for 25min to prepare a mixed solution; uniformly mixing nano titanium dioxide and deionized water according to a mass ratio of 1:11, stirring at 25 ℃ for 20min at 250rpm, uniformly dripping mixed solution with the mass 3 times of the nano titanium dioxide in 25min, continuously stirring for 35min, reacting at 50 ℃ for 10min, heating to 120 ℃ for continuously reacting for 15min, cooling to room temperature, filtering, washing with acetone for 4 times, and drying at 60 ℃ for 18h to obtain the pre-modified nano titanium dioxide; uniformly mixing pre-modified nano titanium dioxide and dimethyl sulfoxide according to a mass ratio of 1:11, performing ultrasonic dispersion for 30min at 25 ℃, heating to 95 ℃, adding N- (4-chlorophenyl) -maleimide with 3 times of the mass of the pre-modified nano titanium dioxide, continuously reacting for 9h, adding deionized water with 25 times of the mass of the pre-modified nano titanium dioxide, standing for 6h at 55 ℃, filtering, washing for 4 times with the deionized water, and drying for 11h at 60 ℃ to obtain modified nano titanium dioxide;
(3) Uniformly mixing 4,4 '-diaminodiphenyl ether, pyromellitic dianhydride and N, N-dimethylacetamide according to a mass ratio of 1:1:4.5, stirring and reacting for 4 hours at 150 ℃ under a nitrogen environment, adding modified nano titanium dioxide with the mass of 0.325 times that of the 4,4' -diaminodiphenyl ether, and stirring for 15 minutes at 150rpm to obtain anti-aging paint;
(4) And taking out the copper flat wire after soaking in the anti-aging paint, drying at 80 ℃ under 0.1MPa for 2 hours, soaking again, repeating for 3 times, heating to 120 ℃ and continuously drying for 1 hour, heating to 150 ℃ and drying for 1 hour, transferring into a muffle furnace, standing for 3 hours at 180 ℃, heating to 300 ℃ and continuously standing for 3 hours to obtain the anti-aging enameled copper flat wire.
Effect example
The following table 1 shows the analysis results of corona resistance, photo aging resistance, insulation and self-repairing properties of the anti-aging enameled rectangular copper wire according to examples 1 to 3 and comparative examples 1 to 3.
TABLE 1
From comparison of experimental data of examples 1 to 3 and comparative examples 1 to 3 in Table 1, it can be found that the anti-aging enameled rectangular copper wire prepared by the invention has good corona resistance, photo-aging resistance, insulating property and self-repairing property.
By comparison, the repairing efficiency of the examples 1,2 and 3 is high compared with that of the comparative example 1, and the fact that the maleimide structure is grafted on the surface of the nano titanium dioxide can carry out a thermal reversible cycloaddition reaction with the pyrrole structure on the polyimide main chain, so that the self-repairing performance of the anti-aging enameled rectangular copper wire is improved.
By comparison, examples 1,2 and 3 have high corona resistance time and high tensile strength retention rate compared with comparative example 2, which illustrates that the benzotriazole monomer containing double bonds, methyl acrylate and acrylamide are subjected to deposition polymerization on the surface of nano titanium dioxide, so that the dispersibility of the nano titanium dioxide is improved, and the corona resistance and the photo-aging resistance of the anti-aging enameled rectangular copper wire are enhanced; and simultaneously, benzotriazole and amino structures are introduced, and hydrogen bonds in the benzotriazole structures are easy to break after being irradiated by ultraviolet light to form unstable tautomers, so that absorbed ultraviolet light energy is converted into heat energy, and the anti-photoaging performance of the anti-aging enameled rectangular copper wire is further enhanced.
By comparison, the volume resistance and repair efficiency of examples 1,2 and 3 compared with comparative example 3 are high, which shows that the addition of modified sulfonyl diphenol in the copolymerization reaction of polyimide enhances the insulation performance of the anti-aging enameled rectangular copper wire; meanwhile, a pyrrole structure is introduced into the main chain, and a thermal reversible cyclization addition reaction is carried out on the pyrrole structure and the maleimide on the surface of the modified nano zinc dioxide, so that the self-repairing performance of the anti-aging enameled rectangular copper wire is improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The production process of the anti-aging enameled rectangular copper wire is characterized in that the anti-aging enameled rectangular copper wire is obtained by carrying out imidization after the anti-aging enameled rectangular copper wire is soaked by the anti-aging paint.
2. The process for producing the anti-aging enameled rectangular copper wire according to claim 1, wherein the anti-aging paint is obtained by blending modified nano titanium dioxide after reaction of modified sulfonyl diphenol, pyromellitic dianhydride and 4,4' -diaminodiphenyl ether.
3. The process for producing an anti-aging enameled rectangular copper wire according to claim 2, wherein the modified sulfonyl diphenol is obtained by reacting 1- (2, 4-difluorophenyl) -1H-pyrrole with sulfonyl diphenol.
4. The production process of the anti-aging enameled rectangular copper wire, according to claim 2, is characterized in that the modified nano titanium dioxide is obtained by carrying out deposition polymerization on a benzotriazole monomer containing double bonds, methyl acrylate and acrylamide on the surface of the nano titanium dioxide and then reacting with N- (4-chlorophenyl) -maleimide.
5. The process for producing an anti-aging enameled rectangular copper wire according to claim 4 wherein the benzotriazole monomer containing double bonds is obtained by reacting 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol with crotonyl chloride.
6. The production process of the anti-aging enameled rectangular copper wire is characterized by comprising the following preparation steps of:
(1) Uniformly mixing 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, crotonyl chloride, triethylamine and tetrahydrofuran according to the mass ratio of 1 (0.8-1): (0.6-0.7): (6-8), stirring at 100-200 rpm for 10-30 min, adding a developing agent 3-5 times the mass of 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, continuing to react at 1-5 ℃ for 4-6H, adding a sodium bicarbonate solution with the mass ratio of 10-12 times that of 4- (2H-benzo [ d ] [1,2,3] triazol-2-yl) benzene-1, 3-diol, standing for 10-14H, taking an upper layer solution, evaporating and drying for 6-8H, recrystallizing with absolute ethyl alcohol, and drying for 10-12H at 40-50 ℃ to obtain a benzotriazole monomer containing double bonds;
(2) The benzotriazole monomer containing double bonds, methyl acrylate, acrylamide, N-dimethylformamide, benzoyl peroxide and deionized water are mixed according to the mass ratio
1 (1-1.2): 0.2-0.4): 4-6): 0.01-0.02): 10-12, stirring for 20-30 min at 200-300 rpm to prepare a mixed solution; uniformly mixing nano titanium dioxide and deionized water according to a mass ratio of 1 (10-12), stirring for 10-30 min at 20-30 ℃ at 200-300 rpm, dripping mixed solution with the mass 2-4 times of the nano titanium dioxide at uniform speed within 20-30 min, continuously stirring for 30-40 min, reacting for 5-15 min at 45-55 ℃, heating to 115-125 ℃ for continuously reacting for 10-20 min, cooling to room temperature, filtering, washing for 3-5 times with acetone, and drying for 16-20 h at 55-65 ℃ to obtain the pre-modified nano titanium dioxide; uniformly mixing pre-modified nano titanium dioxide and dimethyl sulfoxide according to the mass ratio of 1 (10-12), performing ultrasonic dispersion for 20-40 min at 20-30 ℃, heating to 90-100 ℃, adding N- (4-chlorophenyl) -maleimide with the mass of 2-4 times of that of the pre-modified nano titanium dioxide, continuously reacting for 8-10 h, adding deionized water with the mass of 20-30 times of that of the pre-modified nano titanium dioxide, standing for 4-8 h at 50-60 ℃, filtering, washing for 3-5 times by using the deionized water, and drying for 10-12 h at 55-65 ℃ to obtain modified nano titanium dioxide;
(3) Uniformly mixing 1- (2, 4-difluorophenyl) -1H-pyrrole and sulfonyl diphenol according to a molar ratio of 1:2, adding 0.01-0.02 times of anhydrous potassium carbonate and 10-12 times of sulfolane of 1- (2, 4-difluorophenyl) -1H-pyrrole, stirring for 10-30 min at 100-200 rpm, reacting for 1-3H at 110-130 ℃ and 200-300 rpm in a nitrogen environment, taking out all water generated by the reaction, heating to 220-240 ℃ to continue the reaction for 2-4H, respectively washing 3-5 times by using methanol and deionized water, and drying for 8-10H at 95-105 ℃ to obtain modified sulfonyl diphenol;
(4) Uniformly mixing 4,4' -diaminodiphenyl ether and N, N-dimethylacetamide according to the mass ratio of 1 (4-5), and stirring at 100-300 rpm for 30-50 min to obtain diamine mixed solution; uniformly mixing modified sulfonyl diphenol, 4-dimethylaminopyridine, 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide and N, N-dimethylformamide according to the mass ratio of 1 (0.01-0.02) (10-14), stirring at 100-200 rpm for 10-30 min under the nitrogen environment at 20-30 ℃, heating to 140-160 ℃, adding pyromellitic dianhydride which is 0.5-1.5 times of the mass of the modified sulfonyl diphenol every 20-40 min, reacting for 3-5 h, adding a diammine mixed solution which is 5-15 times of the mass of the modified sulfonyl diphenol, continuously reacting for 3-5 h, adding modified nano titanium dioxide which is 0.6-0.7 times of the mass of the modified sulfonyl diphenol, stirring at 100-200 rpm for 10-20 min, and obtaining anti-aging paint;
(5) And (3) soaking the copper flat wire in anti-aging paint, taking out, drying at 75-85 ℃ under 0.05-0.15 MPa for 1-3 hours, soaking again, repeating for 2-4 times, heating to 115-125 ℃ and continuously drying for 0.5-1.5 hours, heating to 145-155 ℃ and drying for 0.5-1.5 hours, transferring into a muffle furnace, standing for 2-4 hours at 170-190 ℃, heating to 290-310 ℃ and continuously standing for 2-4 hours to obtain the anti-aging enameled copper flat wire.
7. The process for producing an anti-aging enameled rectangular copper wire according to claim 6, wherein the reaction equation of the benzotriazole monomer containing double bonds in the step (1) is as follows:
8. the process for producing an anti-aging enameled rectangular copper wire according to claim 6, wherein the reaction equation of the modified nano titanium dioxide in the step (2) is as follows:
9. the process for producing an anti-aging enameled rectangular copper wire according to claim 6, wherein the reaction equation of the modified sulfonyl diphenol in the step (3) is as follows:
10. the process for producing an anti-aging enameled rectangular copper wire according to claim 6, wherein the reaction equation of the anti-aging enameled rectangular copper wire in the step (5) is as follows:
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| CN114015349A (en) * | 2021-12-21 | 2022-02-08 | 东莞宇隆电工材料有限公司 | Enameled wire anti-aging coating |
| US20230047864A1 (en) * | 2021-08-12 | 2023-02-16 | Shanghai XPT Technology Limited | Corona-resistant enameled round wire and preparation method therefor |
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