CN109337428A - A kind of fire resistant polyimide insulating impregnating varnish and its preparation method and application - Google Patents

A kind of fire resistant polyimide insulating impregnating varnish and its preparation method and application Download PDF

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Publication number
CN109337428A
CN109337428A CN201811210869.3A CN201811210869A CN109337428A CN 109337428 A CN109337428 A CN 109337428A CN 201811210869 A CN201811210869 A CN 201811210869A CN 109337428 A CN109337428 A CN 109337428A
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impregnating varnish
fire resistant
paint
resistant polyimide
preparation
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淡宏斌
冯华
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Shaanxi Aero Electric Co Ltd
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Shaanxi Aero Electric 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
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular 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 C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003Preparatory processes
    • C08G73/1007Preparatory processes from tetracarboxylic acids or derivatives and diamines
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular 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 C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1067Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular 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 C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1067Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
    • C08G73/1071Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
    • 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Insulating Materials (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
  • Manufacture Of Motors, Generators (AREA)

Abstract

The present invention proposes a kind of fire resistant polyimide insulating impregnating varnish and its preparation method and application, and for the polyimide insulative impregnating varnish solid content in (45 ± 1) %, viscosity is 60s~90s (25 ± 1 DEG C, No. 4 agar diffusion methods).Tg (glass transition temperature) is greater than 240 DEG C after polyimide insulative impregnating varnish solidification provided by the invention.Polyimide insulative impregnating varnish provided by the invention, viscosity is low under construction temperature, wellability is good, vacuum pressure impregnation number is twice, make insulated paint filled between electrical-coil conducting wire it is full, be evenly distributed, surface of the paint film is smooth, it is continuous it is fine and close, pin hole is few, heat resistance, thermal conductivity, mechanical strength and the humidity resistance of motor product can be improved, extend motor service life.

Description

A kind of fire resistant polyimide insulating impregnating varnish and its preparation method and application
Technical field
The invention belongs to the insulation processing fields of the preparation of insulating impregnating varnish and electrical-coil, more particularly to a kind of resistance to height Warm polyimide insulative impregnating varnish and preparation method and its application in insulating motor coil processing technique.
Background technique
Impregnating varnish is mainly used to carry out insulation impregnating processing to electrical equipment and electrical coil, to fill coil, wire casing or other quilts It is whole to be connected in insulation, and is formed on its surface continuous insulating coating by the hole and stomata of insulant for winding wire insulating sticky, To improve the electricapparatus performance of entire insulation system, heating conduction and to the protective performance of environment.
As electrical equipment and electrical product is towards the development in high-power small size direction, the temperature resistant grade of product is caused gradually to mention Height, in the heat resisting motor that the means of transports such as Aeronautics and Astronautics, navigation and electric locomotive use, winding temperature has been up to 240 DEG C More than, in order to meet the fixation of machine winding, reinforcing insulation and improve thermal conductivity, generally impregnated using fire resistant polyimide Paint carries out insulation processing.
The preparation method of fire resistant polyimide impregnating varnish has at present:
The Pyre-ML insulated paint of nineteen sixty-five E.I.Du Pont Company production, is existed using pyromellitic acid anhydride and diaminodiphenyl ether Reaction generates PAA solution (polyamic acid solution) in N-Methyl pyrrolidone or dimethylformamide, and solid content is in 16..5% ~25%, viscosity is 7.0Pas~8.0Pas (viscosity at 20 DEG C).190 polyimides impregnating varnishes of domestic production, base This group becomes reaction in pyromellitic acid anhydride and diaminodiphenyl ether dimethylformamide and generates PAA solution, and solid content exists 8%~12%, viscosity is 2.0~4.0 minutes (25 ± 1 DEG C, No. 4 agar diffusion methods)
Chinese invention patent CN 1718658A discloses polyimide/inorganic nano-composite insulating varnish and preparation method thereof, The insulated paint is by polyamic acid 3.0%~10% (weight percent), (weight hundred of inorganic nanometer powder 0.5%~15% Point ratio), solvent 75%~90% (weight percent) composition.Preparation method are as follows: solvent is added in reaction kettle, binary is added Amine;Dibasic acid anhydride is added portionwise, stirs 3~5 hours at room temperature;50~85 DEG C of degradations are risen to, until material viscosity drops to 2.0 Until~4.0 minutes (23 ± 2 DEG C, No. 4 agar diffusion methods), polyamic acid solution is obtained;At room temperature, in above-mentioned polyimides acid resin Middle addition inorganic non-metallic nano-powder.
Guilin Inst. of Electrical Equipment Science Liu Ye has carried out by force the research of Modified Polyimide Impregnating Varnish, preparation method be In four-hole boiling flask, the diaminodiphenyl ether, modifier A and dimethyl acetamide of formula ratio is added, starts stirring, is dissolved to system After transparent, end-capping reagent and pyromellitic dianhydride is added portionwise, setting at a temperature of react 4~5 hours, when viscosity reaches requirement Dimethylbenzene is added afterwards to adjust to suitable viscosity, a kind of Modified Polyimide Impregnating Varnish of brown color can be obtained, the impregnating varnish Solid content is 28%, viscosity be 69s (25 ± 1 DEG C, No. 4 agar diffusion methods), storage period 6 months.
Institutes Of Technology Of Nanjing Yang Yu has carried out preparation and the performance study of low viscosity polyimide wire coating enamel and its paint film, The viscous of the PAA solution (polyamic acid solution) of different formulations is prepared by the different dianhydride monomers of research and diamine monomer combination first Secondly the performance comparison of degree and paint film introduces end-capping reagent phthalic anhydride, norbornene acid anhydrides and 3- respectively when synthesizing PAA Aminostyryl studies the viscosity of PAA solution and the performance of paint film.
The bright development for having carried out aero dynamo fire resistant polyimide impregnating varnish of Harbin Research Inst. of Chemical Industry Su Gui, it is described Aero dynamo with fire resistant polyimide impregnating varnish by diaminodiphenyl ether, diaminodiphenyl sulfide, pyromellitic acid anhydride React synthesis PAA solution at 45 ± 5 DEG C with solvent with diphenyl ether tetracid dianhydride.
But the fire resistant polyimide impregnating varnish of above method preparation has that solid content is low, viscosity is high, need to carry out more Secondary vacuum pressure impregnation and Vacuum Heat curing process keep the winding paint film of insulation processing loose, and high-temperature insulation processing is not achieved Purpose.In order to meet the requirement of heat resisting motor winding insulation processing, it is necessary under the premise of meeting insulating impregnating varnish heatproof, The solid content of polyimides impregnating varnish is improved, viscosity is reduced, reduces dipping time.
Summary of the invention
In order to solve the problems existing in the prior art, the present invention proposes a kind of fire resistant polyimide insulating impregnating varnish and its system Preparation Method and application.
The technical solution of the present invention is as follows:
A kind of fire resistant polyimide insulating impregnating varnish, it is characterised in that: including four acid diesters of aromatic series, aromatic series Diamines and solvent, the solvent use methanol and N-Methyl pyrrolidone.
Further preferred embodiment, a kind of fire resistant polyimide insulating impregnating varnish, it is characterised in that: aromatic series four The molar ratio of acid diesters and aromatic diamine is (0.95~1.05): 1.
A kind of preparation method of the fire resistant polyimide insulating impregnating varnish, it is characterised in that: the following steps are included:
Step 1: aromatic series tetracid dianhydride and anhydrous methanol being heated to reflux 5h~6h in N-Methyl pyrrolidone, obtained Faint yellow four acid diesters solution of aromatic series, by temperature and is down to room temperature;
Step 2: aromatic diamine being dissolved in and is added in N-Methyl pyrrolidone, the aromatic series four of step 1 preparation is added Acid diesters solution, is stirred at room temperature 3h~5h, obtains the fire resistant polyimide insulating impregnating varnish of brown.
Further preferred embodiment, a kind of preparation method of fire resistant polyimide insulating impregnating varnish, feature exist In: aromatic series tetracid dianhydride described in step 1 uses 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides.
Further preferred embodiment, a kind of preparation method of fire resistant polyimide insulating impregnating varnish, feature exist In: the molar ratio of aromatic series tetracid dianhydride described in step 1 and anhydrous methanol is 1:2.5.
Further preferred embodiment, a kind of preparation method of fire resistant polyimide insulating impregnating varnish, feature exist In: the mass ratio of aromatic series tetracid dianhydride described in step 1 and N-Methyl pyrrolidone is 1:1.
Further preferred embodiment, a kind of preparation method of fire resistant polyimide insulating impregnating varnish, feature exist In: aromatic diamine described in step 2 is the one or two of 4,4 '-diaminodiphenylmethane and 4,4 '-diaminodiphenyl ethers Mixture.
Further preferred embodiment, a kind of preparation method of fire resistant polyimide insulating impregnating varnish, feature exist In: the mass ratio of aromatic diamine described in step 2 and N-Methyl pyrrolidone is 1:1.
A kind of application method of fire resistant polyimide insulating impregnating varnish, it is characterised in that: the following steps are included:
Step 1: by winding coil in (120 ± 5) DEG C preheating 2 hours, being cooled to 50 DEG C~60 DEG C with baking oven;
Step 2: impregnating vessel being warming up to 30 DEG C~40 DEG C, the winding coil after preheating is transferred to impregnating vessel from baking oven; Impregnating vessel cover is closed, vacuum valve is opened, starts vacuum pump, so that residual compression in tank is lower than 670Pa, keeps the vacuum degree at least 15min;
Step 3: keeping the vacuum in impregnating vessel, open defeated paint valve, paint solution is slowly injected in impregnating vessel, when paint solution liquid level When height is no less than 5mm higher than spare part surface, defeated paint valve is closed, residual compression is lower than dipping lacquer 15min under 670Pa in tank;
Step 4: closing vacuum valve, open intake valve, close intake valve after reaching normal pressure, keep 5min under normal pressure;
Step 5: opening pressurizing valve, be forced into 0.3MPa~0.5MPa, keep pressure 15min;
Step 6: closing pressurizing valve, open back paint valve, paint solution is drained back into storage from impregnating vessel using the overbottom pressure in impregnating vessel In paint can, until paint solution empties, back paint valve is closed, opens relief valve;
Step 7: opening dipping lacquer cover, the winding drop paint 1h after dipping lacquer is placed in baking oven, by 90 DEG C of ± 2 DEG C/1h+ 120 DEG C of ± 2 DEG C/9h+170 DEG C ± 2 DEG C/5h are solidified, and are cooled to 50 DEG C~60 DEG C with baking oven later,
Step 8: repeating step 2~step 6 and carry out secondary dipping lacquer, open dipping lacquer cover, by the winding drop paint 1h after dipping lacquer It is placed in baking oven, is consolidated by 90 DEG C ± 2 DEG C/1h+120 DEG C ± 2 DEG C/9h+170 DEG C ± 2 DEG C/3h+230 DEG C ± 2 DEG C/6h Change.
Beneficial effect
The present invention provides a kind of polyimide insulative impregnating varnish, and for solid content in (45 ± 1) %, viscosity is 60s~90s (25 ± 1 DEG C, No. 4 agar diffusion methods).Tg (glass transition temperature) is greater than after polyimide insulative impregnating varnish solidification provided by the invention 240℃。
Polyimide insulative impregnating varnish provided by the invention, viscosity is low under construction temperature, and wellability is good, vacuum pressure Dipping time be twice, make insulated paint filled between electrical-coil conducting wire it is full, be evenly distributed, surface of the paint film is smooth, continuous Densification, pin hole are few, and heat resistance, thermal conductivity, mechanical strength and the humidity resistance of motor product can be improved, and extend motor and use the longevity Life.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description Obviously, or practice through the invention is recognized.
Specific embodiment
The embodiment of the present invention is described below in detail, the embodiment is exemplary, it is intended to it is used to explain the present invention, and It is not considered as limiting the invention.
The purpose of the present invention is the requirement to meet the processing of heat resisting motor winding insulation, propose that a kind of high temperature resistant polyamides is sub- Amine insulating impregnating varnish and its preparation method and application improves polyimides dipping under the premise of meeting insulating impregnating varnish heatproof The solid content of paint reduces viscosity, reduces dipping time.The fire resistant polyimide insulating impregnating varnish have it is highly filled, Low viscosity feature is suitable for carrying out insulation processing to 220 class B insulation winding of heatproof using technique of vacuum pressure for dipping electrical.
The fire resistant polyimide insulating impregnating varnish, including four acid diesters of aromatic series, aromatic diamine and solvent, wherein molten Agent uses methanol and N-Methyl pyrrolidone.
The molar ratio of four acid diesters of optimization aromatic and aromatic diamine is (0.95~1.05): 1.
And the preparation method of fire resistant polyimide insulating impregnating varnish, comprising the following steps:
Step 1: aromatic series tetracid dianhydride and anhydrous methanol being heated to reflux 5h~6h in N-Methyl pyrrolidone, obtained Faint yellow four acid diesters solution of aromatic series, by temperature and is down to room temperature;
Step 2: aromatic diamine being dissolved in and is added in N-Methyl pyrrolidone, the aromatic series four of step 1 preparation is added Acid diesters solution, is stirred at room temperature 3h~5h, obtains the fire resistant polyimide insulating impregnating varnish of brown.
Aromatic series tetracid dianhydride described in preferred steps 1 uses 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides.
The molar ratio of aromatic series tetracid dianhydride and anhydrous methanol described in preferred steps 1 is 1:2.5.
The mass ratio of aromatic series tetracid dianhydride and N-Methyl pyrrolidone described in preferred steps 1 is 1:1.
Aromatic diamine described in preferred steps 2 is the one of 4,4 '-diaminodiphenylmethane and 4,4 '-diaminodiphenyl ethers Kind or two kinds of mixtures.
The mass ratio of aromatic diamine described in preferred steps 2 and N-Methyl pyrrolidone is 1:1.
Application method of the fire resistant polyimide insulating impregnating varnish obtained above in machine winding insulation processing, including Following steps:
Step 1: by winding coil in (120 ± 5) DEG C preheating 2 hours, being cooled to 50 DEG C~60 DEG C with baking oven;
Step 2: impregnating vessel being warming up to 30 DEG C~40 DEG C, the winding coil after preheating is transferred to impregnating vessel from baking oven; Impregnating vessel cover is closed, vacuum valve is opened, starts vacuum pump, so that residual compression in tank is lower than 670Pa, keeps the vacuum degree at least 15min;
Step 3: keeping the vacuum in impregnating vessel, open defeated paint valve, paint solution is slowly injected in impregnating vessel, when paint solution liquid level When height is no less than 5mm higher than spare part surface, defeated paint valve is closed, residual compression is lower than dipping lacquer 15min under 670Pa in tank;
Step 4: closing vacuum valve, open intake valve, close intake valve after reaching normal pressure, keep 5min under normal pressure;
Step 5: opening pressurizing valve, be forced into 0.3MPa~0.5MPa, keep pressure 15min;
Step 6: closing pressurizing valve, open back paint valve, paint solution is drained back into storage from impregnating vessel using the overbottom pressure in impregnating vessel In paint can, until paint solution empties, back paint valve is closed, opens relief valve;
Step 7: opening dipping lacquer cover, the winding drop paint 1h after dipping lacquer is placed in baking oven, by 90 DEG C of ± 2 DEG C/1h+ 120 DEG C of ± 2 DEG C/9h+170 DEG C ± 2 DEG C/5h are solidified, and are cooled to 50 DEG C~60 DEG C with baking oven later,
Step 8: repeating step 2~step 6 and carry out secondary dipping lacquer, open dipping lacquer cover, by the winding drop paint 1h after dipping lacquer It is placed in baking oven, is consolidated by 90 DEG C ± 2 DEG C/1h+120 DEG C ± 2 DEG C/9h+170 DEG C ± 2 DEG C/3h+230 DEG C ± 2 DEG C/6h Change.
Specific embodiment is given below:
Embodiment 1:
Blender is being housed, is being added the 3,3 ', 4 of 169.05g in the 1000ml three-necked flask of reflux condensing tube and thermometer, 4 '-benzophenone tetracarboxylic dianhydrides (0.525mol), 40g anhydrous methanol (1.25mol), 169.05gN- methyl pyrrolidone are stirring It is heated to reflux under the conditions of mixing 6 hours, obtains flaxen benzophenone acid dimethyl (BPDE) homogeneous phase solution.
99g4,4 '-diaminodiphenylmethane is added in benzophenone acid dimethyl (BPDE) solution obtained The fire resistant polyimide insulating impregnating varnish for obtaining brown for 3 hours is stirred at room temperature in (0.5mol) and 99gN- methyl pyrrolidone.
Embodiment 2:
Blender is being housed, is being added the 3,3 ', 4 of 169.05g in the 1000ml three-necked flask of reflux condensing tube and thermometer, 4 '-benzophenone tetracarboxylic dianhydrides (0.525mol), 40g anhydrous methanol (1.25mol), 169.05gN- methyl pyrrolidone are stirring It is heated to reflux under the conditions of mixing 6 hours, obtains flaxen benzophenone acid dimethyl (BPDE) homogeneous phase solution.
100g4,4 '-diaminodiphenyl ether is added in benzophenone acid dimethyl (BPDE) solution obtained (0.5mol) and 100gN- methyl pyrrolidone is stirred at room temperature and obtains within 3 hours brown polyimide insulative impregnating varnish.
Polyimide insulative impregnating varnish obtained in both the above embodiment there is into solvent insulating paint according to GB/1981-89 Test method is tested, and solidification temperature condition is volume resistivity, electrical strength, dielectric dissipation factor, bonding force.
Dipping lacquer step are as follows:
Step 1: by winding coil in (120 ± 5) DEG C preheating 2 hours, being cooled to 50 DEG C~60 DEG C with baking oven;
Step 2: impregnating vessel being warming up to 30 DEG C~40 DEG C, the winding coil after preheating is transferred to impregnating vessel from baking oven; Impregnating vessel cover is closed, vacuum valve is opened, starts vacuum pump, so that residual compression in tank is lower than 670Pa, keeps the vacuum degree at least 15min;
Step 3: keeping the vacuum in impregnating vessel, open defeated paint valve, paint solution is slowly injected in impregnating vessel, when paint solution liquid level When height is no less than 5mm higher than spare part surface, defeated paint valve is closed, residual compression is lower than dipping lacquer 15min under 670Pa in tank;
Step 4: closing vacuum valve, open intake valve, close intake valve after reaching normal pressure, keep 5min under normal pressure;
Step 5: opening pressurizing valve, be forced into 0.3MPa~0.5MPa, keep pressure 15min;
Step 6: closing pressurizing valve, open back paint valve, paint solution is drained back into storage from impregnating vessel using the overbottom pressure in impregnating vessel In paint can, until paint solution empties, back paint valve is closed, opens relief valve.
After first pass dipping lacquer, after drop paint 1h, carried out in 90 DEG C ± 2 DEG C/1h+120 DEG C ± 2 DEG C/9h+170 DEG C ± 2 DEG C/5h Solidification;After second time dipping, after drop paint 1h, 90 DEG C ± 2 DEG C/1h+120 DEG C ± 2 DEG C/9h+170 DEG C ± 2 DEG C/3h+230 DEG C ± 2 DEG C/6h solidified.The performance and the performance after solidification of polyimide insulative impregnating varnish are shown in Table 1.
The performance of 1 polyimide insulative impregnating varnish of table
It can be seen that polyimide insulative impregnating varnish provided by the invention, viscosity is low under construction temperature, and wellability is good It is good, vacuum pressure impregnation number be twice, make insulated paint filled between electrical-coil conducting wire it is full, be evenly distributed, paint film table Face is smooth, it is continuous it is fine and close, pin hole is few, and heat resistance, thermal conductivity, mechanical strength and the humidity resistance of motor product can be improved, extend Motor service life.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.

Claims (9)

1. a kind of fire resistant polyimide insulating impregnating varnish, it is characterised in that: including four acid diesters of aromatic series, aromatic diamine and Solvent, the solvent use methanol and N-Methyl pyrrolidone.
2. a kind of fire resistant polyimide insulating impregnating varnish according to claim 1, it is characterised in that: four acid diesters of aromatic series Molar ratio with aromatic diamine is (0.95~1.05): 1.
3. the preparation method of fire resistant polyimide insulating impregnating varnish described in a kind of claim 1, it is characterised in that: including following Step:
Step 1: aromatic series tetracid dianhydride and anhydrous methanol being heated to reflux 5h~6h in N-Methyl pyrrolidone, obtained yellowish Four acid diesters solution of color aromatic series, by temperature and is down to room temperature;
Step 2: aromatic diamine being dissolved in and is added in N-Methyl pyrrolidone, the aromatic series tetracid two of step 1 preparation is added 3h~5h is stirred at room temperature in ester solution, obtains the fire resistant polyimide insulating impregnating varnish of brown.
4. a kind of preparation method of fire resistant polyimide insulating impregnating varnish according to claim 3, it is characterised in that: step Aromatic series tetracid dianhydride described in 1 uses 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides.
5. a kind of preparation method of fire resistant polyimide insulating impregnating varnish according to claim 3, it is characterised in that: step The molar ratio of aromatic series tetracid dianhydride described in 1 and anhydrous methanol is 1:2.5.
6. a kind of preparation method of fire resistant polyimide insulating impregnating varnish according to claim 3, it is characterised in that: step The mass ratio of aromatic series tetracid dianhydride described in 1 and N-Methyl pyrrolidone is 1:1.
7. a kind of preparation method of fire resistant polyimide insulating impregnating varnish according to claim 3, it is characterised in that: step Aromatic diamine described in 2 is one or two kinds of mixtures of 4,4 '-diaminodiphenylmethane and 4,4 '-diaminodiphenyl ethers.
8. a kind of preparation method of fire resistant polyimide insulating impregnating varnish according to claim 3, it is characterised in that: step The mass ratio of aromatic diamine described in 2 and N-Methyl pyrrolidone is 1:1.
9. the application method of fire resistant polyimide insulating impregnating varnish described in a kind of claim 1, it is characterised in that: including following Step:
Step 1: by winding coil in (120 ± 5) DEG C preheating 2 hours, being cooled to 50 DEG C~60 DEG C with baking oven;
Step 2: impregnating vessel being warming up to 30 DEG C~40 DEG C, the winding coil after preheating is transferred to impregnating vessel from baking oven;It closes Impregnating vessel cover opens vacuum valve, starts vacuum pump, so that residual compression in tank is lower than 670Pa, keeps the vacuum degree at least 15min;
Step 3: keeping the vacuum in impregnating vessel, open defeated paint valve, paint solution is slowly injected in impregnating vessel, when paint solution liquid level When being no less than 5mm higher than spare part surface, defeated paint valve is closed, residual compression is lower than dipping lacquer 15min under 670Pa in tank;
Step 4: closing vacuum valve, open intake valve, close intake valve after reaching normal pressure, keep 5min under normal pressure;
Step 5: opening pressurizing valve, be forced into 0.3MPa~0.5MPa, keep pressure 15min;
Step 6: closing pressurizing valve, open back paint valve, paint solution is drained back into storage paint can from impregnating vessel using the overbottom pressure in impregnating vessel In, until paint solution empties, back paint valve is closed, opens relief valve;
Step 7: opening dipping lacquer cover, the winding drop paint 1h after dipping lacquer is placed in baking oven, by 90 DEG C ± 2 DEG C/1h+120 DEG C ± 2 DEG C/9h+170 DEG C ± 2 DEG C/5h are solidified, and are cooled to 50 DEG C~60 DEG C with baking oven later,
Step 8: repeating step 2~step 6 and carry out secondary dipping lacquer, open dipping lacquer cover, by the winding drop paint 1h postposition after dipping lacquer In baking oven, solidified by 90 DEG C ± 2 DEG C/1h+120 DEG C ± 2 DEG C/9h+170 DEG C ± 2 DEG C/3h+230 DEG C ± 2 DEG C/6h.
CN201811210869.3A 2018-10-17 2018-10-17 A kind of fire resistant polyimide insulating impregnating varnish and its preparation method and application Pending CN109337428A (en)

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CN109880519A (en) * 2019-03-13 2019-06-14 四川特聚新材料科技有限公司 A kind of anti-paraffin coating material and preparation method thereof
CN115646789A (en) * 2022-10-27 2023-01-31 佛山市顺德区伊戈尔电力科技有限公司 Environment-friendly reactor and preparation process thereof

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CN102604092A (en) * 2012-02-20 2012-07-25 中国科学院化学研究所 Polyimide resin as well as preparation method and application thereof
CN104485767A (en) * 2014-12-15 2015-04-01 哈尔滨电气动力装备有限公司 High-voltage motor stator coil insulation structure and process for impregnating and curing high-voltage motor stator coil insulation structure
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CN1106843A (en) * 1993-10-18 1995-08-16 巴斯夫漆及染料公司 Solutions of polyimide-forming substances and their use as coating compositions
CN101654518A (en) * 2009-09-23 2010-02-24 中国科学院化学研究所 Thermosetting polyimide resin and preparation method and application thereof
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CN109880519A (en) * 2019-03-13 2019-06-14 四川特聚新材料科技有限公司 A kind of anti-paraffin coating material and preparation method thereof
CN115646789A (en) * 2022-10-27 2023-01-31 佛山市顺德区伊戈尔电力科技有限公司 Environment-friendly reactor and preparation process thereof

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Application publication date: 20190215