CN116478616A - Preparation method of polyamide imide electromagnetic wire paint - Google Patents

Preparation method of polyamide imide electromagnetic wire paint Download PDF

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Publication number
CN116478616A
CN116478616A CN202310045259.7A CN202310045259A CN116478616A CN 116478616 A CN116478616 A CN 116478616A CN 202310045259 A CN202310045259 A CN 202310045259A CN 116478616 A CN116478616 A CN 116478616A
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China
Prior art keywords
polyamide
electromagnetic wire
paint
imide
preparation
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CN202310045259.7A
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CN116478616B (en
Inventor
郑一帆
秦臻
朱宝阳
浦思伟
李召鹏
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Suzhou Guanlong Electromagnetic Wire Co ltd
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Suzhou Guanlong Electromagnetic Wire Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D179/00Coating 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
    • C09D179/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C09D179/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30Insulators 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
    • H01B3/308Wires with resins

Abstract

According to the preparation method of the polyamide imide electromagnetic wire paint, the polyamide imide electromagnetic wire paint can be prepared by only three steps of stirring, dispersing, heating, polymerizing and freeze drying through the preparation raw materials of the mixed solution including nonylphenol polyoxyethylene ether NP-10, tween 80, N-isopropyl acrylamide, ammonium persulfate and deionized water, and the preparation method is convenient to operate, high in yield and easy to implement; the polyamide-imide electromagnetic wire paint prepared by the method has the advantages that polyamide-imide insulating paint particles are wrapped in a shell formed by high polymers, the wrapping rate is high, the contact between the polyamide-imide insulating paint particles and the outside can be isolated, no pungent smell is generated, the safety is good, the paint is transported and stored only by conventional packaging, the storage stability is good, the cost is low, the cost performance is high, the shell can be damaged by utilizing the film forming process of the traditional electromagnetic wire paint, the polyamide-imide insulating paint particles overflow and form a uniform paint film, the paint film is easy to introduce into the production system of the existing electromagnetic wire, and the application range is wide.

Description

Preparation method of polyamide imide electromagnetic wire paint
Statement of divisional application
The application is a divisional application of China patent application with the application number 202210366541.0, and the name of the patent is polyamide imide electromagnetic wire paint submitted by 2022, 04 and 08.
Technical Field
The invention relates to the technical field of electromagnetic wire production, in particular to a preparation method of polyamide imide electromagnetic wire paint.
Background
The electromagnetic wire is an insulated wire for manufacturing coils or windings in electrical products, also called winding wire, and is divided into enameled wires, lapped wires, enameled wires, inorganic insulated wires and the like according to insulating materials and manufacturing modes used for an electrical insulating layer, and is widely used in the fields of motors, electric appliances, instruments, transformers, electronic components, new energy automobiles, wind power generation and the like.
Because of the specificity of the working environment, the electromagnetic wire must meet various requirements in terms of use and manufacturing processes, including its shape, specification, ability to operate at high temperatures for short and long periods of time, and to withstand strong vibrations and centrifugal forces at high speeds in certain situations, corona and breakdown resistance at high voltages, chemical corrosion resistance under special atmospheres, and the like; the latter include the requirements of being subjected to stretching, bending and abrasion during winding and wire embedding, as well as swelling, erosion during impregnation and drying, etc.
Along with the development of modern industry, the requirements of safety, high efficiency, energy conservation and light weight of electronic and electric equipment are higher and higher, and high-performance insulating materials are generated, so that polyamide imide is an amorphous high-temperature resistant engineering thermoplastic resin, has heat-resistant aromatic hetero-imide groups and flexible amide groups in molecules, has good dimensional stability and creep resistance, excellent heat resistance, radiation resistance, dielectric property, mechanical property and chemical stability, is an engineering material with excellent performance, can generate a good insulating layer in a winding of a metal wire if used as an electromagnetic wire paint, improves and stabilizes the performance of the electromagnetic wire, but the traditional polyamide imide electromagnetic wire paint needs to use volatile organic solvents when being prepared, is not friendly to human bodies and environment, has larger pungent smell, has the characteristics of flammability, explosiveness and the like, has high danger, can be suitable for long-distance transportation and long-term storage only by special packaging, and has high production cost, logistics and storage cost and poor cost performance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides the preparation method of the polyamide imide electromagnetic wire paint, which is convenient to operate, high in yield and easy to implement.
In order to achieve the above purpose, the technical scheme provided by the invention is that the preparation method of the polyamide imide electromagnetic wire paint comprises the following steps:
A. adding the polyamide-imide insulating varnish in an oil phase into the mixed liquid in a water phase, and stirring to enable the polyamide-imide insulating varnish to be emulsified and dispersed into particles, so that monomers in the mixed liquid are uniformly dispersed to obtain a suspension;
B. heating the suspension to polymerize the monomer on the surface of the particles to form a shell;
C. cooling and drying, and removing water in the mixed solution to obtain the polyamide imide electromagnetic wire paint;
the preparation raw materials of the mixed solution in the step A comprise nonylphenol polyoxyethylene ether NP-10, tween 80, N-isopropyl acrylamide, ammonium persulfate and deionized water, wherein the weight ratio of the nonylphenol polyoxyethylene ether NP-10, the Tween 80, the N-isopropyl acrylamide, the ammonium persulfate and the deionized water in the preparation raw materials of the polyamideimide electromagnetic wire paint is 0.5-1%, 5-7%, 0.1-0.2% and 69.3-81.9% respectively;
and C, the entrapment rate of the polyamide-imide electromagnetic wire paint is more than or equal to 96%.
Preferably, the stirring speed in the step A is not less than 20000 revolutions per minute, and the stirring time is not less than 10 minutes.
Preferably, the temperature at which the temperature is raised in step B is 80 ℃ + -2 ℃, and the polymerization time of the monomer is not less than 4 hours.
Preferably, the preparation raw materials of the polyamide imide insulating varnish in the step A comprise 4,4 '-diphenylmethane diisocyanate, 3' -dimethyl-4, 4 '-biphenyl diisocyanate, trimellitic anhydride, N-methylpyrrolidone, N-dimethylacetamide, toluene and xylene, wherein the weight ratio of the 4,4' -diphenylmethane diisocyanate, the 3,3 '-dimethyl-4, 4' -biphenyl diisocyanate, the trimellitic anhydride, the N-methylpyrrolidone, the N, N-dimethylacetamide, the toluene and the xylene in the preparation raw materials of the polyamide imide electromagnetic wire varnish is 1% -2%, 2% -4%, 2.5% -4%, 2% -3%, 0.5% -1.5% and 3% -5% respectively.
Preferably, the preparation method of the polyamide-imide insulating varnish comprises the steps of mixing the 4,4' -diphenylmethane diisocyanate, the 3,3' -dimethyl-4, 4' -biphenyl diisocyanate, the trimellitic anhydride, the N-methylpyrrolidone and the N, N-dimethylacetamide, stirring at room temperature for at least 30min to obtain a homogeneous solution, adding the trimellitic anhydride into the homogeneous solution, stirring and heating to 155+/-2 ℃, keeping constant temperature for reacting for at least 4 hours to obtain a dark red viscous solution, continuously stirring and cooling to 60+/-2 ℃, adding the toluene and the xylene, and keeping constant temperature for reacting for at least 40 min to obtain the polyamide-imide insulating varnish.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the preparation method of the polyamide imide electromagnetic wire paint, the polyamide imide electromagnetic wire paint can be prepared by only three steps of stirring, dispersing, heating, polymerizing and freeze drying through the preparation raw materials of the mixed solution including nonylphenol polyoxyethylene ether NP-10, tween 80, N-isopropyl acrylamide, ammonium persulfate and deionized water, and the preparation method is convenient to operate, high in yield and easy to implement; the polyamide-imide electromagnetic wire paint prepared by the method has the advantages that polyamide-imide insulating paint particles are wrapped in a shell formed by high polymers, the wrapping rate is high, the contact between the polyamide-imide insulating paint particles and the outside can be isolated, no pungent smell is generated, the safety is good, the paint is transported and stored only by conventional packaging, the storage stability is good, the cost is low, the cost performance is high, the shell can be damaged by utilizing the film forming process of the traditional electromagnetic wire paint, the polyamide-imide insulating paint particles overflow and form a uniform paint film, the paint film is easy to introduce into the production system of the existing electromagnetic wire, and the application range is wide.
Drawings
FIG. 1 is a graph showing performance index of a polyamideimide magnet wire paint prepared in accordance with one embodiment of the present invention.
FIG. 2 is an optical microscope characterization of a polyamideimide magnet wire paint prepared in accordance with an embodiment of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the attached drawings so that the advantages and features of the present invention will be more readily understood by those skilled in the art, thereby making clear and defining the scope of the present invention.
The invention provides polyamide imide electromagnetic wire paint, which comprises a plurality of microscopic units, wherein the microscopic units comprise polyamide imide insulating paint particles and shells wrapped on the surfaces of the particles, the particles are formed by emulsifying and dispersing the polyamide imide insulating paint in mixed liquid, the shells are high polymers formed by polymerizing monomers in the mixed liquid on the surfaces of the particles, and specifically, the polyamide imide electromagnetic wire paint is prepared from raw materials including 4,4 '-diphenylmethane diisocyanate, 3' -dimethyl-4, 4 '-biphenyl diisocyanate, trimellitic anhydride, N-methylpyrrolidone, N-dimethylacetamide, toluene, xylene, nonylphenol polyoxyethylene ether NP-10, tween 80, N-isopropyl acrylamide, ammonium persulfate and deionized water, wherein 4,4' -diphenylmethane diisocyanate, 3 '-dimethyl-4, 4' -biphenyl diisocyanate, trimellitic anhydride, N-methylpyrrolidone, N-dimethylacetamide, toluene and xylene are used for preparing the polyamide imide insulating paint; the nonylphenol polyoxyethylene ether NP-10, tween 80, N-isopropyl acrylamide, ammonium persulfate and deionized water are used for preparing a mixed solution.
The device has the advantages that the device can isolate the contact of the polyamide-imide insulating paint particles with the outside through the shell, has no pungent smell and good safety, is transported and stored only by conventional packaging, is convenient to operate, has low cost and high cost performance, can not react with the polyamide-imide insulating paint particles in the process of polymerizing the shell, the monomer and the monomer into the shell, has obvious interfaces between the shell and the particles, can well retain the characteristics of the polyamide-imide insulating paint particles (polyamide-imide insulating paint), can damage the shell by utilizing the film forming process (mainly heating) of the traditional electromagnetic wire paint, overflows the polyamide-imide insulating paint particles and forms a uniform paint film, is easy to introduce into the production system of the existing electromagnetic wire, and has wide application range.
Further, the polyamide imide electromagnetic wire paint comprises the following components in percentage by weight: 1 to 2 percent of 4,4' -diphenylmethane diisocyanate, 1 to 2 percent of 3,3' -dimethyl-4, 4' -biphenyl diisocyanate, 2 to 4 percent of trimellitic anhydride, 2.5 to 4 percent of N-methylpyrrolidone, 2 to 3 percent of N, N-dimethylacetamide, 0.5 to 1.5 percent of toluene, 3 to 5 percent of dimethylbenzene, 0.5 to 1 percent of nonylphenol polyoxyethylene ether NP-10, 0.5 to 1 percent of tween 80, 5 to 7 percent of N-isopropyl acrylamide, 0.1 to 0.2 percent of ammonium persulfate and 69.3 to 81.9 percent of deionized water.
The preparation method has the advantages that the prepared polyamide-imide electromagnetic wire paint has high entrapment rate (entrapment rate is more than or equal to 96 percent) and good storage stability (room temperature is more than 8 months), and meanwhile, the production cost can be controlled in a lower range.
The preparation method for preparing the polyamide imide electromagnetic wire paint provided by the invention comprises the following steps:
adding the polyamide-imide insulating varnish in the oil phase into the mixed liquid in the water phase, and stirring to disperse the polyamide-imide insulating varnish into particles, so that monomers in the mixed liquid are uniformly dispersed to obtain a suspension;
heating the suspension to polymerize the monomer on the surface of the particles to form a shell;
and C, cooling and drying, and removing water in the mixed solution to obtain the polyamide imide electromagnetic wire paint.
The setting has the advantages that only three steps of stirring and dispersing, heating and polymerizing and freeze drying are needed, the working procedure is simple, the operation is convenient, the yield is high, and the implementation is easy.
The polyamideimide magnet wire paint and the method for preparing the same provided by the present invention are described below in specific examples so that advantages and features of the present invention will be more easily understood by those skilled in the art.
Example 1
The polyamide imide electromagnetic wire paint of the embodiment comprises the following raw materials in percentage by mass: 1% of 4,4' -diphenylmethane diisocyanate, 1% of 3,3' -dimethyl-4, 4' -biphenyl diisocyanate, 2% of trimellitic anhydride, 2.5% of N-methylpyrrolidone, 2% of N, N-dimethylacetamide, 0.5% of toluene, 3% of xylene, 0.5% of nonylphenol polyoxyethylene ether NP-10.5%, 0.5% of tween 80, 5% of N-isopropylacrylamide, 0.1% of ammonium persulfate, and the balance of deionized water, wherein the total is 100%.
The preparation method comprises the following steps:
the above-mentioned mass ratio of 4,4' -diphenylmethane diisocyanate, 3' -dimethyl-4, 4' -biphenyl diisocyanate, N-methylpyrrolidone and N, N-dimethylacetamide were added to a four-necked flask equipped with a stirrer, a thermometer, a water separator and a nitrogen inlet, and stirred at room temperature (25 ℃) for 30 minutes to obtain a homogeneous solution, which, of course, was a laboratory method, and in industrial production, a large-scale reaction vessel such as a reaction vessel was used.
And adding quantitative trimellitic anhydride according to the proportion, heating to 155 ℃ under stirring, and keeping constant temperature for reaction for 4 hours to obtain dark red viscous solution.
Then stirring and cooling to 60 ℃, adding toluene and dimethylbenzene according to the proportion, keeping the constant temperature for reaction for 40 minutes, and stopping the reaction to obtain the polyamide-imide insulating varnish, wherein the main performance indexes of the polyamide-imide insulating varnish are shown in figure 1.
Then, the insulating paint is added into a mixed solution composed of nonylphenol polyoxyethylene ether NP-10, tween 80, N-isopropyl acrylamide, ammonium persulfate and deionized water according to the proportion, and the mixture is stirred at a high speed (20000 revolutions per minute) and kept for 10 minutes, so that the mixture is subjected to emulsification and dispersion reaction, and a stable suspension is obtained.
The suspension is heated to 80 ℃ to react for 4 hours, cooled and dried to obtain the polyamideimide electromagnetic wire paint, and the optical microscope characterization diagram of the polyamideimide electromagnetic wire paint is shown in figure 2.
Example two
The preparation method of the second embodiment is the same as that of the first embodiment, and the difference is that the mass ratio of the raw material components in the second embodiment is as follows: 2% of 4,4' -diphenylmethane diisocyanate, 2% of 3,3' -dimethyl-4, 4' -biphenyl diisocyanate, 4% of trimellitic anhydride, 4% of N-methylpyrrolidone, 3% of N, N-dimethylacetamide, 1.5% of toluene, 5% of xylene, 10% of nonylphenol polyoxyethylene ether NP-10, 80% of Tween, 7% of N-isopropylacrylamide, 0.2% of ammonium persulfate, and the balance of deionized water, wherein the total is 100%.
Example III
The preparation method of the third embodiment is the same as that of the first embodiment, and the difference is that the mass ratio of the raw material components in the third embodiment is as follows: 1.5% of 4,4' -diphenylmethane diisocyanate, 1.5% of 3,3' -dimethyl-4, 4' -biphenyl diisocyanate, 3% of trimellitic anhydride, 3% of N-methylpyrrolidone, 2.5% of N, N-dimethylacetamide, 1% of toluene, 4% of xylene, NP-101% of nonylphenol polyoxyethylene ether, 0.5% of tween 80, 6% of N-isopropylacrylamide, 0.15% of ammonium persulfate and the balance of deionized water, wherein the total is 100%.
Example IV
The preparation method of the fourth embodiment is the same as that of the first embodiment, and the difference is that the mass ratio of the raw material components in the fourth embodiment is as follows: 1% of 4,4' -diphenylmethane diisocyanate, 2% of 3,3' -dimethyl-4, 4' -biphenyl diisocyanate, 2.5% of trimellitic anhydride, 2.5% of N-methylpyrrolidone, 3% of N, N-dimethylacetamide, 1% of toluene, 3.5% of xylene, NP-101% of nonylphenol polyoxyethylene ether, 0.5% of tween 80, 6% of N-isopropylacrylamide, 0.2% of ammonium persulfate and the balance of deionized water, wherein the total is 100%.
Example five
The preparation method of the fifth embodiment is the same as that of the first embodiment, and the difference is that the mass ratio of the raw material components in the fifth embodiment is as follows: 2% of 4,4' -diphenylmethane diisocyanate, 1% of 3,3' -dimethyl-4, 4' -biphenyl diisocyanate, 3.5% of trimellitic anhydride, 3.5% of N-methylpyrrolidone, 2% of N, N-dimethylacetamide, 1% of toluene, 4.5% of xylene, 100.5% of nonylphenol polyoxyethylene ether NP-100, 80% of tween, 7% of N-isopropylacrylamide, 0.2% of ammonium persulfate and the balance of deionized water, wherein the total is 100%.
In the second to fifth embodiments, the electrical performance index and the shell thickness of the polyamideimide electromagnetic wire paint can be adjusted by changing the content of each raw material component, so that the electromagnetic wire paint film forming process is suitable for different customer demands and different electromagnetic wire paint film forming processes.
The invention adopts a mode of loading the polyamide-imide insulating varnish particles into the high polymer shell material, and can keep the polyamide-imide insulating varnish from the external environment before use, thereby effectively solving the problems of large smell, heavy pollution and the like of the electromagnetic wire varnish, endowing the electromagnetic wire varnish with better storage stability and carrying safety, adapting to the requirements of safety and environmental protection, and achieving the same film forming effect as the traditional electromagnetic wire varnish after use without influencing the production of the electromagnetic wire.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and to implement the same, but are not intended to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.

Claims (3)

1. The preparation method of the polyamideimide electromagnetic wire paint is characterized by comprising the following steps of:
A. adding the polyamide-imide insulating varnish in an oil phase into the mixed liquid in a water phase, and stirring to enable the polyamide-imide insulating varnish to be emulsified and dispersed into particles, so that monomers in the mixed liquid are uniformly dispersed to obtain a suspension;
B. heating the suspension to polymerize the monomer on the surface of the particles to form a shell;
C. cooling and drying, and removing water in the mixed solution to obtain the polyamide imide electromagnetic wire paint;
the preparation raw materials of the mixed solution in the step A comprise nonylphenol polyoxyethylene ether NP-10, tween 80, N-isopropyl acrylamide, ammonium persulfate and deionized water, wherein the weight ratio of the nonylphenol polyoxyethylene ether NP-10, the Tween 80, the N-isopropyl acrylamide, the ammonium persulfate and the deionized water in the preparation raw materials of the polyamideimide electromagnetic wire paint is 0.5-1%, 5-7%, 0.1-0.2% and 69.3-81.9% respectively; and C, the entrapment rate of the polyamide-imide electromagnetic wire paint is more than or equal to 96%.
2. The method of manufacturing according to claim 1, characterized in that: the stirring speed in the step A is not lower than 20000 revolutions per minute, and the stirring time is not less than 10 minutes.
3. The method of manufacturing according to claim 1, characterized in that: the temperature in the step B is 80+/-2 ℃, and the polymerization reaction time of the monomer is not less than 4 hours.
CN202310045259.7A 2022-04-08 2022-04-08 Preparation method of polyamide imide electromagnetic wire paint Active CN116478616B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2096625A (en) * 1981-04-11 1982-10-20 Sumitomo Electric Industries Magnet wire
JP2008233341A (en) * 2007-03-19 2008-10-02 Canon Inc Magnetic material dispersed resin carrier
CN102099400A (en) * 2008-05-21 2011-06-15 东丽株式会社 Method for producing polymer fine particle
US20120152590A1 (en) * 2010-12-15 2012-06-21 Weijun Yin High Temperature High Frequency Magnet Wire and Method of Making
CN106675388A (en) * 2016-12-16 2017-05-17 上海裕生特种线材有限公司 Nano self-lubricating insulating paint as well as preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5098531B2 (en) * 2007-09-13 2012-12-12 東レ株式会社 Method for producing polyamideimide fine particles
JP2009149757A (en) * 2007-12-20 2009-07-09 Sumitomo Electric Wintec Inc Polyamide imide and production method thereof, polyamide imide-based insulating coating, and insulated wire
CN106811112A (en) * 2016-12-29 2017-06-09 天恒达电工科技股份有限公司 A kind of preparation method of Inverter fed motor polyamide-imide enamelled wire varnishes

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2096625A (en) * 1981-04-11 1982-10-20 Sumitomo Electric Industries Magnet wire
JP2008233341A (en) * 2007-03-19 2008-10-02 Canon Inc Magnetic material dispersed resin carrier
CN102099400A (en) * 2008-05-21 2011-06-15 东丽株式会社 Method for producing polymer fine particle
US20120152590A1 (en) * 2010-12-15 2012-06-21 Weijun Yin High Temperature High Frequency Magnet Wire and Method of Making
CN106675388A (en) * 2016-12-16 2017-05-17 上海裕生特种线材有限公司 Nano self-lubricating insulating paint as well as preparation method and application thereof

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