CN112592653A - Preparation method of high-temperature-resistant polyimide wire enamel - Google Patents
Preparation method of high-temperature-resistant polyimide wire enamel Download PDFInfo
- Publication number
- CN112592653A CN112592653A CN202011392954.3A CN202011392954A CN112592653A CN 112592653 A CN112592653 A CN 112592653A CN 202011392954 A CN202011392954 A CN 202011392954A CN 112592653 A CN112592653 A CN 112592653A
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- CN
- China
- Prior art keywords
- graphene oxide
- nano graphene
- wire enamel
- dianhydride
- polyimide wire
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Classifications
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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
- 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
-
- 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
Abstract
A preparation method of high-temperature-resistant polyimide wire enamel comprises the following steps: (1) preparing surface modified nano graphene oxide: (1a) ultrasonically dispersing nano graphene oxide in DMF, adding NaOH and citric acid, controlling the reaction temperature to be 60-85 ℃, and reacting for 2-3h to obtain carboxylated nano graphene oxide; (1b) preparing surface modified nano graphene oxide; (2) weighing a proper amount of surface modified nano graphene oxide, adding a proper amount of diamine and dianhydride, adding a diluent and a film forming additive after the reaction is finished, and stirring to obtain polyimide wire enamel; the production process is simple, graphene oxide and a polyimide system are compounded, and the amino-functionalized gamma-aminopropyl silsesquioxane and the carboxyl and epoxy groups of the carboxylated nano graphene oxide form a conjugated structure, so that the heat resistance and the mechanical strength of the polyester wire enamel are greatly improved.
Description
Technical Field
The invention relates to the technical field of wire enamel preparation, in particular to a preparation method of high-temperature-resistant polyimide wire enamel.
Background
The enameled wire is an electrical material and consists of a conductor and an insulating layer, a thin high-strength insulating layer is processed on the surface of a round copper wire to play a role of insulating the round copper wire from the outside, and the enameled wire is a necessary insulating material for producing the enameled wire; in recent years, widely used high-temperature-resistant insulating coatings mainly include polyimides and polyamideimide resins; polyimide is a special engineering plastic with excellent performance. The main chain of the material contains an imide structure, has excellent non-toxicity, and is widely applied to the fields of aviation, aerospace, microelectronics, separation membranes, lasers, liquid crystals and the like. At present, with the development of scientific technology and the requirement of national production, polyimide materials with more excellent high temperature resistance, chemical corrosion resistance, lower dielectric constant, better mechanical properties, excellent tensile modulus and tensile strength performance have larger demand, and the formula and production process of the wire enamel need to be improved to further improve the performance of the enamel.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a preparation method of high-temperature-resistant polyimide wire enamel, so as to improve the heat resistance and the mechanical property of the polyimide wire enamel.
The technical route for solving the problems is that graphene oxide is prepared firstly, then carboxylation and surface silanization are respectively carried out on the graphene oxide, then polyimide resin is synthesized in a binary network consisting of the graphene, and finally a solvent and a film-forming assistant are added to obtain the product.
The method specifically comprises the following steps:
(1) preparing surface modified nano graphene oxide: (1a) carrying out ultrasonic crushing on graphene oxide for 2-3h, processing the graphene oxide into nano graphene oxide by an ultrasonic probe, filtering the nano graphene oxide by a filter membrane to remove large-size graphene oxide, then ultrasonically dispersing the nano graphene oxide in DMF, adding NaOH and citric acid, continuing to carry out ultrasonic treatment, controlling the reaction temperature to be 60-85 ℃ under the reflux condition, reacting for 2-3h, carrying out suction filtration washing on the obtained product, and drying the product in an oven to obtain carboxylated nano graphene oxide; (1b) adding the carboxylated nano graphene oxide into a reaction kettle, then adding gamma-aminopropyl silsesquioxane, and stirring for 4-6h at 70-90 ℃ to obtain silsesquioxane-grafted carboxylated nano graphene oxide, namely the surface-modified nano graphene oxide; wherein the molar ratio of the gamma-aminopropyl silsesquioxane to the carboxylated nano graphene oxide is 1 (0.2-0.6);
(2) preparing polyimide wire enamel: weighing a proper amount of surface modified nano graphene oxide, placing the nano graphene oxide in a reaction kettle, adding a solvent, heating to 80-90 ℃, adding a proper amount of diamine and dianhydride, heating to 120-140 ℃, cooling the material to 60-80 ℃ after the reaction time is 6-12h, adding a diluent and a film-forming assistant, and stirring to obtain the polyimide wire enamel.
In the step (1a), the graphene oxide is prepared from natural graphite powder by using a modified Hummers method, and the product is golden yellow.
In the step (2) above, the diluent is xylene.
In the step (2), the diamine is at least one of diphenyl ether diamine, p-phenylenediamine, m-phenylenediamine 2- (4-aminophenyl) -5-aminobenzimidazole and 4, 4' -diaminobenzanilide; the dianhydride is at least one of pyromellitic dianhydride, biphenyl dianhydride, cyclohexane tetracarboxylic dianhydride, diphenyl sulfide dianhydride and bisphenol A diether dianhydride.
In the step (2), the molar ratio of the surface modified nano graphene oxide to the diamine to the dianhydride to the diluent to the film-forming assistant is 1 (0.8-0.9) to (3.5-5) to (0.05-0.15).
Has the advantages that: the production process is simple, graphene oxide and a polyimide system are compounded, and the surface of the graphene oxide is modified, so that the graphene oxide has an ultrahigh specific surface area and a two-dimensional planar nanostructure, and the possibility of high heat resistance and mechanical property by compounding the graphene oxide and the polyimide system is realized; and the dispersibility of the graphene oxide in the matrix is crucial to the interface interaction between the graphene oxide and the polyimide and the mechanical property of the composite material, so that the surface of the graphene oxide is carboxylated to provide more carboxyl reaction sites for the reaction of a graphene oxide matrix and the matrix material, then the graphene oxide is modified by adopting gamma-aminopropyl silsesquioxane, and the amino-functionalized gamma-aminopropyl silsesquioxane and the carboxyl and epoxy groups of the carboxylated nano graphene oxide form a conjugated structure, thereby improving the dispersibility of the graphene oxide in a polyimide system from the chemical structure and greatly improving the heat resistance and the mechanical strength of the polyester wire enamel.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
Example 1
A preparation method of high-temperature-resistant polyimide wire enamel comprises the following steps:
(1) preparing surface modified nano graphene oxide: (1a) carrying out ultrasonic crushing on graphene oxide for 2.5h, processing the graphene oxide into nano graphene oxide by an ultrasonic probe, filtering the nano graphene oxide by a filter membrane to remove large-size graphene oxide, then ultrasonically dispersing the nano graphene oxide in DMF, adding NaOH and citric acid, continuing to carry out ultrasonic treatment, controlling the reaction temperature to be 60-85 ℃ under the reflux condition, reacting for 2h, carrying out suction filtration washing on the obtained product, and drying the product in an oven to obtain carboxylated nano graphene oxide; (1b) adding the carboxylated nano graphene oxide into a reaction kettle, then adding gamma-aminopropyl silsesquioxane, and stirring for 5 hours at 70-90 ℃ to obtain silsesquioxane-grafted carboxylated nano graphene oxide, namely the surface-modified nano graphene oxide; wherein the molar ratio of the gamma-aminopropyl silsesquioxane to the carboxylated nano graphene oxide is 1: 0.4;
(2) preparing polyimide wire enamel: weighing a proper amount of surface modified nano graphene oxide, placing the nano graphene oxide in a reaction kettle, adding a solvent, heating to 80-90 ℃, adding a proper amount of diamine and dianhydride, heating to 120-140 ℃, cooling the material to 60-80 ℃ after the reaction time is 8 hours, adding a diluent and a film forming auxiliary agent, and stirring to obtain the polyimide wire enamel.
Example 2
A preparation method of high-temperature-resistant polyimide wire enamel comprises the following steps:
(1) preparing surface modified nano graphene oxide: (1a) carrying out ultrasonic crushing treatment on graphene oxide for 3 hours, treating the graphene oxide into nano graphene oxide by an ultrasonic probe, removing large-size graphene oxide by a filtering membrane, then ultrasonically dispersing the nano graphene oxide in DMF, adding NaOH and citric acid, continuing ultrasonic treatment, controlling the reaction temperature to be 60-85 ℃ under the reflux condition, reacting for 2 hours, carrying out suction filtration washing on the obtained product, and drying the product in an oven to obtain carboxylated nano graphene oxide; (1b) adding the carboxylated nano graphene oxide into a reaction kettle, then adding gamma-aminopropyl silsesquioxane, and stirring for 4 hours at 70-90 ℃ to obtain silsesquioxane-grafted carboxylated nano graphene oxide, namely the surface-modified nano graphene oxide; wherein the molar ratio of the gamma-aminopropyl silsesquioxane to the carboxylated nano graphene oxide is 1: 0.5;
(2) preparing polyimide wire enamel: weighing a proper amount of surface modified nano graphene oxide, placing the nano graphene oxide in a reaction kettle, adding a solvent, heating to 80-90 ℃, adding a proper amount of diamine and dianhydride, heating to 120-140 ℃, cooling the material to 60-80 ℃ after the reaction time is 10 hours, adding a diluent and a film forming auxiliary agent, and stirring to obtain the polyimide wire enamel.
Example 3
A preparation method of high-temperature-resistant polyimide wire enamel comprises the following steps:
(1) preparing surface modified nano graphene oxide: (1a) carrying out ultrasonic crushing treatment on graphene oxide for 3 hours, treating the graphene oxide into nano graphene oxide by an ultrasonic probe, removing large-size graphene oxide by a filtering membrane, then ultrasonically dispersing the nano graphene oxide in DMF, adding NaOH and citric acid, continuing ultrasonic treatment, controlling the reaction temperature to be 60-85 ℃ under the reflux condition, reacting for 2.5 hours, carrying out suction filtration washing on the obtained product, and drying the product in an oven to obtain carboxylated nano graphene oxide; (1b) adding the carboxylated nano graphene oxide into a reaction kettle, then adding gamma-aminopropyl silsesquioxane, and stirring for 5 hours at 70-90 ℃ to obtain silsesquioxane-grafted carboxylated nano graphene oxide, namely the surface-modified nano graphene oxide; wherein the molar ratio of the gamma-aminopropyl silsesquioxane to the carboxylated nano graphene oxide is 1: 0.6;
(2) preparing polyimide wire enamel: weighing a proper amount of surface modified nano graphene oxide, placing the nano graphene oxide in a reaction kettle, adding a solvent, heating to 80-90 ℃, adding a proper amount of diamine and dianhydride, heating to 120-140 ℃, cooling the material to 60-80 ℃ after the reaction time is 12 hours, adding a diluent and a film forming auxiliary agent, and stirring to obtain the polyimide wire enamel.
Performance testing
According to GB/T6109.22QY-1/240, a general enameled wire painting machine is adopted to coat a copper wire by using the products of examples 1-3 to prepare an enameled wire, and the main technical indexes of the enameled wire are shown in Table 1;
TABLE 1
| Index performance | Example 1 | Example 2 | Example 3 |
| Conductor diameter (mm) | 0.200 | 0.200 | 0.200 |
| Maximum outer diameter (mm) | 0.224 | 0.222 | 0.221 |
| Maximum paint film thickness (mm) | 0.028 | 0.031 | 0.029 |
| Heat resistance | Does not crack at 200 ℃/2d | Does not crack at 200 ℃/2d | Does not crack at 200 ℃/2d |
| Breakdown voltage (kv) | 5.9 | 6.4 | 6.5 |
| Corona withstand life (h) | 358 | 362 | 360 |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. The preparation method of the high-temperature-resistant polyimide wire enamel is characterized by comprising the following steps of:
(1) preparing surface modified nano graphene oxide: (1a) carrying out ultrasonic crushing on graphene oxide for 2-3h, processing the graphene oxide into nano graphene oxide by an ultrasonic probe, filtering the nano graphene oxide by a filter membrane to remove large-size graphene oxide, then ultrasonically dispersing the nano graphene oxide in DMF, adding NaOH and citric acid, continuing to carry out ultrasonic treatment at the reaction temperature of 60-85 ℃ for 2-3h, carrying out suction filtration washing on the obtained product, and drying the product in an oven to obtain carboxylated nano graphene oxide; (1b) adding the carboxylated nano graphene oxide into a reaction kettle, then adding gamma-aminopropyl silsesquioxane, and stirring for 4-6h at 70-90 ℃ to obtain silsesquioxane-grafted carboxylated nano graphene oxide, namely the surface-modified nano graphene oxide; wherein the molar ratio of the gamma-aminopropyl silsesquioxane to the carboxylated nano graphene oxide is 1 (0.2-0.6);
(2) preparing polyimide wire enamel: weighing a proper amount of surface modified nano graphene oxide, placing the nano graphene oxide in a reaction kettle, adding a solvent, heating to 80-90 ℃, adding a proper amount of diamine and dianhydride, heating to 120-140 ℃, cooling the material to 60-80 ℃ after the reaction time is 6-12h, adding a diluent and a film-forming assistant, and stirring to obtain the polyimide wire enamel.
2. The high-temperature-resistant polyimide wire enamel according to claim 1, wherein the graphene oxide is prepared from natural graphite powder by using a modified Hummers method, and the product is golden yellow.
3. The high temperature resistant polyimide wire enamel of claim 1 wherein said diluent is xylene.
4. The high temperature resistant polyimide wire enamel of claim 1 wherein said diamine is diphenyl ether diamine, is at least one of p-phenylenediamine, m-phenylenediamine 2- (4-aminophenyl) -5-aminobenzimidazole, and 4, 4' -diaminobenzanilide; the dianhydride is at least one of pyromellitic dianhydride, biphenyl dianhydride, cyclohexane tetracarboxylic dianhydride, diphenyl sulfide dianhydride and bisphenol A diether dianhydride.
5. The high temperature resistant polyimide wire enamel of claim 1, wherein the molar ratio of the surface modified nano graphene oxide to the diamine to the dianhydride to the diluent to the film forming aid is 1 (0.8-0.9) to (3.5-5) to (0.05-0.15).
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| CN202011392954.3A CN112592653A (en) | 2020-12-02 | 2020-12-02 | Preparation method of high-temperature-resistant polyimide wire enamel |
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| CN202011392954.3A CN112592653A (en) | 2020-12-02 | 2020-12-02 | Preparation method of high-temperature-resistant polyimide wire enamel |
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Cited By (1)
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| CN115926615A (en) * | 2022-11-24 | 2023-04-07 | 江苏四达特材科技有限公司 | High-wear-resistance polyimide wire enamel and preparation method thereof |
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