CN106519945A - Insulation varnish and preparing method thereof - Google Patents
Insulation varnish and preparing method thereof Download PDFInfo
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- CN106519945A CN106519945A CN201611006389.6A CN201611006389A CN106519945A CN 106519945 A CN106519945 A CN 106519945A CN 201611006389 A CN201611006389 A CN 201611006389A CN 106519945 A CN106519945 A CN 106519945A
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/58—Epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/80—Masked polyisocyanates
- C08G18/8061—Masked polyisocyanates masked with compounds having only one group containing active hydrogen
- C08G18/807—Masked polyisocyanates masked with compounds having only one group containing active hydrogen with nitrogen containing compounds
- C08G18/8074—Lactams
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- 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
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- 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
- H01B3/302—Polyurethanes or polythiourethanes; Polyurea or polythiourea
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention relates to an insulation varnish and a preparing method thereof. The insulation varnish is prepared from, by weight, 100 parts of polyoxazolidone resin, 20-40 parts of bisphenol F epikote, 25-45 parts of acrylate epikote, 15-25 parts of reactive diluent, 2-8 parts of curing agent, 0.5-1 part of initiator and 0.5-1 part of polymerization inhibitor. The viscosity of polyoxazolidone resin is 1000-3000 cps at 25 DEG C. According to the insulation varnish and the preparing method thereof, the insulation varnish adopts polyoxazolidone resin as a main body, and is used in company with acrylate epikote and bisphenol F epikote. Accordingly the insulation varnish has the advantages of being heat resistant, flame retardant, environmentally friendly and the like, and is applicable to insulation processing of high and low voltage motors.
Description
Technical field
The present invention relates to a kind of insulated paint and preparation method thereof.
Background technology
Machine winding can improve the operation safety of winding in motor after insulation impregnating process, improve its insulating properties
With mechanical strength, avoid internal air gap from producing shelf depreciation, strengthen operational reliability, improve the abilities such as moistureproof and salt spray resistance, prolong
Long life.Nowadays domestic electric machine manufacturer is generally using vacuum pressure impregnation (VPI) technology to motors such as motor, transformers
Electrical equipment carries out in insulation processing, therefore market increasingly increasing the demand of VPI solvent-free insulated paints.
In recent years, polyoxazolidone resin shows excellent characteristic at the aspect such as high temperature resistant, resistance to chemical attack, fire-retardant,
It has been applied to multiple fields.In terms of electric insulation, application of result is at aspects such as laminate, copper-clad plates.Using polyazole alkane
Ketone resin makes insulated paint, and its solidfied material has good dimensional stability and heat-resisting resistance to fire resistance.Document report has Ji Cheng
Be prepared for that temperature classification reaches F levels has solvent-borne type oxazolidone impregnated insulating paint.Chinese invention patent application
201210050342.5 a kind of insulation of the solventless impregnating containing polyoxazolidone resin paint formula is disclosed, according to weight proportion
Calculate, its component includes：Solid content is 65%～75% 40～65 parts of unsaturated polyester-imide resin solution, and solid content is
15～35 parts of 75%～85% polyoxazolidone resin solution；10～25 parts of environment-friendly type diluent；3～8 parts of curing agent；Cause
1～3 part of agent；0.01～0.06 part of polymerization inhibitor.
The above-mentioned solventless impregnating insulated paint for having adopted polyoxazolidone resin, polyoxazolidone resin is all as auxiliary
Resin rather than matrix resin are helped, main cause is that polyoxazolidone resin is typically different using excessive general purpose epoxy resin and two
Polyisocyanate reactant forms the compound that epoxy-capped oxazolidone five-membered ring is coexisted with triazine hexatomic ring, and its viscosity is larger.Such as
Fruit prepares solventless impregnating insulated paint as matrix resin, and the viscosity of paint be able to can not be filled at vacuum pressure conditions than larger
There is air gap in the mica tape divided in infiltration machine winding, insulation after solidification, insulation effect receives considerable influence.
The patent of invention of Application No. 201510874470.5 disclose a kind of polyoxazolidone resin, its preparation method and
Application in insulated paint, the composition of raw materials of the insulated paint include the polyoxazolidone resin of 100 weight portions, 30～60 weight portions
Cycloaliphatic epoxy resin, the acrylated epoxy resins of 20～45 weight portions, the reactive diluent of 10～25 weight portions, 2
The curing agent of～8 weight portions, the initiator of 0.5～1 weight portion, the polymerization inhibitor of 0.5～1 weight portion.But the insulated paint is each
Item performance still has much room for improvement.
The content of the invention
The technical problem to be solved is to provide a kind of more excellent insulated paint of properties and its preparation side
Method.
To solve above technical problem, the present invention is adopted the following technical scheme that：
It is an object of the present invention to provide a kind of insulated paint, by weight, its composition of raw materials is：
Wherein, the preparation method of described polyoxazolidone resin is：In the presence of a catalyst, at 150～170 DEG C,
It is disposable in cycloaliphatic epoxy resin to add closing diisocyanate, insulation reaction to prepare for 3～5 hours, wherein, it is described
Closing diisocyanate be to be obtained by the reaction of diisocyanate and sealer, the isocyanic acid of described closing diisocyanate
Root is 1 with the molar ratio of the epoxy radicals of described cycloaliphatic epoxy resin:1.8～2.2, described polyoxazolidone resin
Viscosity at 25 DEG C is 1000～3000cps.
Preferably, described reactive diluent is selected from vinyltoluene, styrene, acrylate, phthalic acid two
One or more combination in allyl ester.
Preferably, described curing agent is selected from chromium acetylacetonate, acetylacetone,2,4-pentanedione zirconium, aluminium acetylacetonate, zinc Isoocatanoate, ring
The combination of one or more in alkanoic acid zinc.
Preferably, described initiator is selected from peroxide type initiators.
Preferably, described polymerization inhibitor be selected from hydroquinones, p methoxy phenol, 1,4-benzoquinone, to tert-butyl o benzene two
The combination of one or more in phenol.
Preferably, the preparation method of described acrylated epoxy resins is：By epoxy resin, polymerization inhibitor, catalyst
It is added in reactor, is warming up to 110～130 DEG C, is then added dropwise acrylic acid in described reactor, insulation reaction 20～
40min, is warming up to 135～145 DEG C, is incubated to acid number test result less than 0.5mg/g, obtains final product described Acrylated Epoxy
Resin, wherein, described epoxy resin, described acrylic acid, described polymerization inhibitor, the mass ratio that feeds intake of described catalyst are
900～1100:90～110:4～6:1.
It is further preferred that described epoxy resin is E44 type epoxy resin.
It is further preferred that described catalyst be Bian amine, tertiary amine, one or more in triphenyl phosphorus of combination.
It is further preferred that described polymerization inhibitor be selected from hydroquinones, p methoxy phenol, 1,4-benzoquinone, to the tert-butyl group
The combination of one or more in catechol.
Preferably, prepare concretely comprising the following steps for described polyoxazolidone resin：Described alicyclic ring is added in reactor
Race's epoxy resin and described catalyst, under conditions of stirring, are warming up to 150～170 DEG C, then it is disposable add it is described
Closing diisocyanate, insulation reaction 3～5 hours prepare described polyoxazolidone resin.
It is further preferred that described cycloaliphatic epoxy resin is selected from 3,4- epoxycyclohexyl-methyls 3,4- epoxy hexamethylenes
Carbamate, 3,4- epoxy -6- methyl-cyclohexyl ylmethyl 3,4- epoxycyclohexyl formic acid esters, double ((3,4- epoxycyclohexyls) first
Base) adipate ester, one or more in adipic acid two (3,4- epoxy -6- methylcyclohexyl methyl esters) of combination.
It is further preferred that described catalyst is one or more in imidazoles, lewis acid or quaternary salt
Combination.
It is further preferable that fluoroform sulphonate of the lewis acid for the fluoroform sulphonate or zirconium chloride of magnesium chloride.
It is further preferable that the imidazoles are 2-ethyl-4-methylimidazole or 2- phenylimidazoles.
It is further preferable that the quaternary salt is tetrabutyl phosphonium bromide phosphine or tetraethylammonium bromide.
It is further preferred that described catalyst and described cycloaliphatic epoxy resin feed intake mass ratio for 0.004～
0.006:1。
It is further preferred that the preparation method of described closing diisocyanate is concretely comprised the following steps：By diisocyanate
With sealer in the presence of a catalyst, at 60～80 DEG C, insulation reaction 3～5 hours prepares described closing two different
Cyanate, wherein, the described isocyano of diisocyanate and the molar ratio of described sealer are 1:1.1～1.3.
It is further preferable that described diisocyanate is selected from toluene di-isocyanate(TDI), two isocyanic acid of methylenediphenyl
The combination of one or more in ester, hexane diisocyanate, IPDI, the support diisocyanate of benzene two.
It is further preferable that described sealer is selected from methyl ethyl ketoxime, acetylacetone,2,4-pentanedione, epsilon-caprolactams, malonic acid diethyl
The combination of one or more in ester, β-thionaphthol.
It is further preferable that described catalyst is one or more in organotin, tertiary amine and carboxylic metallic salt
Combination.
Most preferably, the organotin is stannous octoate or dibutyl tin laurate.
Most preferably, the tertiary amine is triethylamine or triethylenediamine.
Most preferably, the carboxylic metallic salt is zinc naphthenate or zinc octoate.
It is a further object to provide a kind of preparation method of described insulated paint, described polymerization inhibitor is added
In described acrylated epoxy resins, stirring and dissolving, then at 55～65 DEG C, adds described reactive diluent, institute
The polyoxazolidone resin stated, described bisphenol F epoxy resin, described curing agent, stir, are then cooled to 0～40
DEG C, described initiator is added, is stirred, obtain final product described insulated paint.
In the present invention, 3,4- epoxycyclohexyl-methyls 3, the structural formula of 4- epoxycyclohexyl formic acid esters are expressed as follows：
The structural formula of 3,4- epoxy -6- methyl-cyclohexyl ylmethyl 3,4- epoxycyclohexyl formic acid esters is expressed as follows：
The structural formula of double ((3,4- epoxycyclohexyls) methyl) adipate esters is expressed as follows：
The structural formula of adipic acid two (3,4- epoxy -6- methylcyclohexyl methyl esters) is expressed as follows：
Due to the enforcement of above technical scheme, the present invention is had the advantage that compared with prior art：
The present invention is prepared for low viscous polyoxazolidone with closing diisocyanate using cycloaliphatic epoxy resin first
Resin, the polyoxazolidone resin have viscosity low, good manufacturability, the good advantage of thermal stability, and the preparation method is grasped
Make simple, reaction condition is gentle.
The present invention insulated paint based on polyoxazolidone resin, and with acrylated epoxy resins, Bisphenol F epoxy
Resin compounded is used, so that the insulated paint has the advantages such as heat-proof combustion-resistant, environmental protection, goes for height Medium-voltage Motor
Insulation processing.
Description of the drawings
Infrared spectrum of the accompanying drawing 1 for polyoxazolidone resin obtained in embodiment 2.
Specific embodiment
With reference to specific embodiment, the present invention will be further described in detail, but the invention is not restricted to following enforcement
Example.
Embodiment 1
In the reactor, epsilon-caprolactams 87g (0.77mol), dibutyl tin laurate 0.5g is added to start stirring,
70 DEG C are warming up to, 80g methylenediphenyl diisocyanates (isocyano of 0.64mol) are dissolved in into 120mL toluene, are dropped to
In reactor, and 4h is kept at this temperature, terminate reaction, add petroleum ether and stirring after cooling, suction filtration, filter cake is in vacuum drying
65 DEG C of drying in case, obtain epsilon-caprolactams closing diisocyanate (closing MDI).
Embodiment 2
In the reactor, 3,4- epoxycyclohexyl-methyls 3, the 4- epoxycyclohexyl formic acid esters 100g (rings of 0.8mol are added
Epoxide), 2-ethyl-4-methylimidazole 0.5g starts stirring, is warming up to 160 DEG C, disposable to add 1 obtained envelope of 95g embodiments
MDI (isocyano of 0.40mol) is closed, and is incubated 4h at this temperature, terminate reaction, polyoxazolidone resin is obtained, which 25
DEG C when the viscosity that measures be 1250cps, its infrared spectrum referring to Fig. 1, as can be seen from Figure 1：2900cm-1Neighbouring peak is flexible for C-H
Vibration performance peak, 1614cm-1And 1514cm-1For the characteristic peak of phenyl ring skeletal vibration, 1728cm-1It is the carbonyl being connected with alicyclic ring
Stretching vibration peak, 1761cm-1Stretching vibration peak of the neighbouring acromion for carbonyl on oxazolidone ring, 901cm-1For ether epoxy
The symmetrical stretching vibration peak of key C-O-C, 2267cm-1Neighbouring isocyanates stretching vibration peak is wholly absent, and these peaks are illustrated
Polyoxazolidone resin structure synthesizes successfully.
Embodiment 3
In the reactor, 3,4- epoxycyclohexyl-methyls 3, the 4- epoxycyclohexyl formic acid esters 100g (rings of 0.80mol are added
Epoxide), 2-ethyl-4-methylimidazole 0.5g starts stirring, is warming up to 150 DEG C, disposable to add 1 obtained envelope of 95g embodiments
MDI (isocyano of 0.40mol) is closed, and is incubated 4h at this temperature, terminate reaction, polyoxazolidone resin is obtained, which 25
DEG C when the viscosity that measures be 1120cps.
Embodiment 4
In the reactor, 3,4- epoxycyclohexyl-methyls 3, the 4- epoxycyclohexyl formic acid esters 100g (rings of 0.80mol are added
Epoxide), 2-ethyl-4-methylimidazole 0.5g starts stirring, is warming up to 170 DEG C, disposable to add 1 obtained envelope of 95g embodiments
MDI (isocyano of 0.40mol) is closed, and is incubated 4h at this temperature, terminate reaction, polyoxazolidone resin is obtained, which 25
DEG C when the viscosity that measures be 2580cps.
Embodiment 5
In the reactor, 3,4- epoxycyclohexyl-methyls 3, the 4- epoxycyclohexyl formic acid esters 100g (rings of 0.80mol are added
Epoxide), 2-ethyl-4-methylimidazole 0.5g starts stirring, is warming up to 160 DEG C, disposable to add 1 obtained envelope of 95g embodiments
MDI (isocyano of 0.40mol) is closed, and is incubated 6h at this temperature, terminate reaction, polyoxazolidone resin is obtained, which 25
DEG C when the viscosity that measures be 1610cps.
Embodiment 6
In the reactor, 3,4- epoxycyclohexyl-methyls 3, the 4- epoxycyclohexyl formic acid esters 100g (rings of 0.80mol are added
Epoxide), 2-ethyl-4-methylimidazole 0.5g starts stirring, is warming up to 160 DEG C, disposable to add 104.8g embodiments 1 to be obtained
Closing MDI (isocyano of 0.44mol), and be incubated 4h at this temperature, terminate reaction, polyoxazolidone resin is obtained,
The viscosity measured when its 25 DEG C is 2150cps.
Comparative example 1
In the reactor, 3,4- epoxycyclohexyl-methyls 3, the 4- epoxycyclohexyl formic acid esters 100g (rings of 0.80mol are added
Epoxide), 2-ethyl-4-methylimidazole 0.5g starts stirring, is warming up to 160 DEG C, disposable to add obtained in 150g embodiments 1
Closing MDI (isocyano of 0.63mol), and 4h is incubated at this temperature, terminate reaction, polyoxazolidone resin is obtained, its
The viscosity measured when 25 DEG C is 7500cps.
Comparative example 2
In the reactor, 3,4- epoxycyclohexyl-methyls 3, the 4- epoxycyclohexyl formic acid esters 100g (rings of 0.80mol are added
Epoxide), 2-ethyl-4-methylimidazole 0.5g starts stirring, is warming up to 190 DEG C, disposable to add 1 obtained envelope of 95g embodiments
MDI (isocyano of 0.40mol) is closed, and is incubated 4h at this temperature, terminate reaction, polyoxazolidone resin is obtained, which 25
DEG C when the viscosity that measures be 13500cps.
Comparative example 3
In the reactor, 3,4- epoxycyclohexyl-methyls 3,4- epoxycyclohexyl formic acid esters 100g, 2- ethyl -4- first are added
Base imidazoles 0.5g, starts stirring, is warming up to 160 DEG C, and 43.8g methylenediphenyl diisocyanates, and here temperature is dropwise added dropwise
The lower insulation 4h of degree, terminates reaction, and polyoxazolidone resin is obtained, and the viscosity measured when its 25 DEG C is 3270cps.
Comparative example 4
In the reactor, bisphenol A-type glycidol ether (DGEBA) 100g (0.53mol), 2- ethyl -4- methyl miaows are added
Azoles 0.5g, starts stirring, is warming up to 160 DEG C, disposable to add the 1 obtained closing MDI (isocyanic acids of 0.26mol of 62g embodiments
Root), and 4h is incubated at this temperature, terminating reaction, polyoxazolidone resin is obtained, the viscosity measured when its 25 DEG C is
8700cps。
Embodiment 7
This example provides a kind of solvent-free oxazolidone insulated paint, and in parts by weight, its composition of raw materials is as follows：
The preparation method of solvent-free oxazolidone impregnated insulating paint is comprised the following steps：
(1) acrylated epoxy resins are prepared：Epoxy resin E44 100g are added in the reactor with stirring, plus
Enter polymerization inhibitor HQ 0.5g, catalyst Bian amine 0.1g.120 DEG C are warming up to, acrylic acid 10g is added dropwise, insulation reaction 30min is warming up to
140 DEG C, it is incubated to acid number test result less than 0.5mg/g, obtains final product.
(2) by 0.8 part of product added obtained by step (1) of polymerization inhibitor HQ, insulated and stirred is cooled to fully dissolving
60 DEG C, add 20 parts of vinyltoluene, 100 parts of low viscosity polyoxazolidone resin, 30 parts of Bisphenol F epoxy, chromium acetylacetonate 5
Part, it is thoroughly mixed uniformly, gained mixture is cooled to room temperature, adds 0.7 part of initiator DCP, stirring fully to dissolve, obtain
Impregnated insulating paint.
Embodiment 8
This example provides a kind of solvent-free oxazolidone insulated paint, and in parts by weight, its composition of raw materials is as follows：
The preparation method of solvent-free oxazolidone impregnated insulating paint is comprised the following steps：
(1) acrylated epoxy resins are prepared：Epoxy resin E44 100g are added in the reactor with stirring, plus
Enter polymerization inhibitor HQ 0.5g, catalyst Bian amine 0.1g.120 DEG C are warming up to, acrylic acid 10g is added dropwise, insulation reaction 30min is warming up to
140 DEG C, it is incubated to acid number test result less than 0.5mg/g, obtains final product.
(2) by 0.8 part of product added obtained by step (1) of polymerization inhibitor HQ, insulated and stirred is cooled to fully dissolving
60 DEG C, 20 parts of styrene, 100 parts of low viscosity polyoxazolidone resin, 40 parts of Bisphenol F epoxy, 5 parts of acetylacetone,2,4-pentanedione zirconium are added, is filled
Divide and be uniformly mixed, gained mixture is cooled to room temperature, add 0.7 part of initiator DCP, stirring fully to dissolve, must impregnate exhausted
Edge paint.
Comparative example 5
This example provides a kind of solvent-free oxazolidone insulated paint, and in parts by weight, its composition of raw materials is as follows：
The preparation method of solvent-free oxazolidone impregnated insulating paint is comprised the following steps：
(1) acrylated epoxy resins are prepared：Epoxy resin E44 100g are added in the reactor with stirring, plus
Enter polymerization inhibitor HQ 0.5g, catalyst Bian amine 0.1g.120 DEG C are warming up to, acrylic acid 10g is added dropwise, insulation reaction 30min is warming up to
140 DEG C, it is incubated to acid number test result less than 0.5mg/g, obtains final product.
(2) by 0.8 part of product added obtained by step (1) of polymerization inhibitor HQ, insulated and stirred is cooled to fully dissolving
60 DEG C, 20 parts of styrene, 100 parts of low viscosity polyoxazolidone resin, 30 parts of Bisphenol F epoxy, 15 parts of acetylacetone,2,4-pentanedione zirconium are added, is filled
Divide and be uniformly mixed, gained mixture is cooled to room temperature, add 0.7 part of initiator DCP, stirring fully to dissolve, must impregnate exhausted
Edge paint.
Comparative example 6
This example provides a kind of solvent-free oxazolidone insulated paint, and in parts by weight, its composition of raw materials is as follows：
The preparation method of solvent-free oxazolidone impregnated insulating paint is comprised the following steps：
(1) acrylated epoxy resins are prepared：Epoxy resin E44 100g are added in the reactor with stirring, plus
Enter polymerization inhibitor HQ 0.5g, catalyst Bian amine 0.1g.120 DEG C are warming up to, acrylic acid 10g is added dropwise, insulation reaction 30min is warming up to
140 DEG C, it is incubated to acid number test result less than 0.5mg/g, obtains final product.
(2) by 0.8 part of product added obtained by step (1) of polymerization inhibitor HQ, insulated and stirred is cooled to fully dissolving
60 DEG C, 20 parts of vinyltoluene, 100 parts of polyoxazolidone resin, 30 parts of Bisphenol F epoxy, 5 parts of chromium acetylacetonate are added, fully
It is uniformly mixed, gained mixture is cooled to room temperature, adds 0.7 part of initiator DCP, stirring fully to dissolve, obtain varnished insulation
Paint.
Comparative example 7
This example provides a kind of solvent-free oxazolidone insulated paint, and in parts by weight, its composition of raw materials is as follows：
The preparation method of solvent-free oxazolidone impregnated insulating paint is comprised the following steps：
(1) acrylated epoxy resins are prepared：Epoxy resin E44 100g are added in the reactor with stirring, plus
Enter polymerization inhibitor HQ 0.5g, catalyst Bian amine 0.1g.120 DEG C are warming up to, acrylic acid 10g is added dropwise, insulation reaction 30min is warming up to
140 DEG C, it is incubated to acid number test result less than 0.5mg/g, obtains final product.
(2) by 0.8 part of product added obtained by step (1) of polymerization inhibitor HQ, insulated and stirred is cooled to fully dissolving
60 DEG C, 20 parts of vinyltoluene, 100 parts of polyoxazolidone resin, 30 parts of Bisphenol F epoxy, 5 parts of chromium acetylacetonate are added, fully
It is uniformly mixed, gained mixture is cooled to room temperature, adds 0.7 part of initiator DCP, stirring fully to dissolve, obtain varnished insulation
Paint.
Comparative example 8
This example provides a kind of solvent-free oxazolidone insulated paint, and in parts by weight, its composition of raw materials is as follows：
The preparation method of solvent-free oxazolidone impregnated insulating paint is comprised the following steps：
(1) acrylated epoxy resins are prepared：Epoxy resin E44 100g are added in the reactor with stirring, plus
Enter polymerization inhibitor HQ 0.5g, catalyst Bian amine 0.1g.120 DEG C are warming up to, acrylic acid 10g is added dropwise, insulation reaction 30min is warming up to
140 DEG C, it is incubated to acid number test result less than 0.5mg/g, obtains final product.
(2) by 0.8 part of product added obtained by step (1) of polymerization inhibitor HQ, insulated and stirred is cooled to fully dissolving
60 DEG C, 20 parts of vinyltoluene, 100 parts of polyoxazolidone resin, 30 parts of Bisphenol F epoxy, 5 parts of chromium acetylacetonate are added, fully
It is uniformly mixed, gained mixture is cooled to room temperature, adds 0.7 part of initiator DCP, stirring fully to dissolve, obtain varnished insulation
Paint.
By the insulated paint performance of embodiment 7 and 8 and comparative example 5 to 8 according to GB/T 15023-1994《Electric insulation without
Solvent polymerizing resin method of testing》Tested, condition of cure be 140 DEG C 3 hours, 170 DEG C 7 hours, gained performance referring to
Table 1：
Table 1
Above the present invention is described in detail, its object is to allow the personage for being familiar with this art to will appreciate that this
The content of invention is simultaneously carried out, and can not be limited the scope of the invention with this, all Spirit Essence institutes of the invention
The equivalence changes of work or modification, should all cover within the scope of the present invention.
Claims (10)
1. a kind of insulated paint, it is characterised in that：By weight, its composition of raw materials is：
100 parts of polyoxazolidone resin；
20 ~ 40 parts of bisphenol F epoxy resin；
25 ~ 45 parts of acrylated epoxy resins；
15 ~ 25 parts of reactive diluent；
2 ~ 8 parts of curing agent；
0.5 ~ 1 part of initiator；
0.5 ~ 1 part of polymerization inhibitor；
Wherein, the preparation method of described polyoxazolidone resin is：In the presence of a catalyst, at 150 ~ 170 DEG C, to alicyclic ring
It is disposable in race's epoxy resin to add closing diisocyanate, insulation reaction to prepare for 3 ~ 5 hours, wherein, described closing
Diisocyanate is the isocyano of prepared with sealer reaction by diisocyanate, described closing diisocyanate and institute
The molar ratio of the epoxy radicals of the cycloaliphatic epoxy resin stated is 1:1.8 ~ 2.2, described polyoxazolidone resin is at 25 DEG C
When viscosity be 1000 ~ 3000 cps.
2. insulated paint according to claim 1, it is characterised in that：Described reactive diluent be selected from vinyltoluene,
One or more combination in styrene, acrylate, diallyl phthalate；Described curing agent is selected from levulinic
The combination of one or more in ketone chromium, acetylacetone,2,4-pentanedione zirconium, aluminium acetylacetonate, zinc Isoocatanoate, zinc naphthenate；Described initiator
It is selected from peroxide type initiators.
3. insulated paint according to claim 1, it is characterised in that：The preparation side of described acrylated epoxy resins
Method is：Epoxy resin, polymerization inhibitor, catalyst are added in reactor, 110 ~ 130 DEG C are warming up to, then to described reaction
Acrylic acid is added dropwise in device, 20 ~ 40 min of insulation reaction is warming up to 135 ~ 145 DEG C, is incubated to acid number test result and is less than 0.5
Mg/g, obtains final product described acrylated epoxy resins, wherein, described epoxy resin, described acrylic acid, described inhibition
Agent, the mass ratio that feeds intake of described catalyst are 900 ~ 1100:90~110:4~6:1.
4. the insulated paint according to claim 1 or 3, it is characterised in that：Described catalyst is Bian amine, tertiary amine, triphenyl
The combination of one or more in phosphorus；Described polymerization inhibitor be selected from hydroquinones, p methoxy phenol, 1,4-benzoquinone, to tertiary fourth
The combination of one or more in base catechol.
5. insulated paint according to claim 1, it is characterised in that：Prepare the concrete steps of described polyoxazolidone resin
For：Described cycloaliphatic epoxy resin and described catalyst are added in reactor, under conditions of stirring, it is warming up to 150 ~
It is 170 DEG C, then disposable to add described closing diisocyanate, insulation reaction 3 ~ 5 hours to prepare described polyazole
Alkanone resin.
6. insulated paint according to claim 5, it is characterised in that：Described cycloaliphatic epoxy resin is selected from 3,4- epoxies
Cyclohexyl methyl 3,4- epoxycyclohexyl formic acid esters, 3,4- epoxy -6- methyl-cyclohexyl ylmethyl 3,4- epoxycyclohexyl formic acid
It is ester, double（（3,4- epoxycyclohexyls）Methyl）Adipate ester, adipic acid two（3,4- epoxy -6- methylcyclohexyl methyl esters）In one
Plant or various combinations；Described catalyst is the combination of one or more in imidazoles, lewis acid or quaternary salt.
7. insulated paint according to claim 6, it is characterised in that：Fluoroform sulphonate of the lewis acid for magnesium chloride
Or the fluoroform sulphonate of zirconium chloride；The imidazoles are 2-ethyl-4-methylimidazole or 2- phenylimidazoles；The quaternary salt is four
Butyl bromide phosphine or tetraethylammonium bromide.
8. insulated paint according to claim 5, it is characterised in that：The preparation method of described closing diisocyanate
Concretely comprise the following steps：By diisocyanate and sealer in the presence of a catalyst, at 60 ~ 80 DEG C, insulation reaction 3 ~ 5 hours,
Described closing diisocyanate is prepared, wherein, the isocyano and described sealer of described diisocyanate
Molar ratio is 1: 1.1~1.3.
9. insulated paint according to claim 8, it is characterised in that：Described diisocyanate is selected from toluene diisocynate
Ester, methylenediphenyl diisocyanates, hexane diisocyanate, IPDI, the support diisocyanate of benzene two
In one or more of combination；
Described sealer is selected from methyl ethyl ketoxime, acetylacetone,2,4-pentanedione, epsilon-caprolactams, diethyl malonate, β-In thionaphthol
One or more of combination；
Described catalyst is the combination of one or more in organotin, tertiary amine and carboxylic metallic salt.
10. a kind of preparation method of insulated paint as claimed in any one of claims 1-9 wherein, it is characterised in that：By described resistance
During poly- agent adds described acrylated epoxy resins, stirring and dissolving is then at 55 ~ 65 DEG C, active dilute described in addition
Agent, described polyoxazolidone resin, described bisphenol F epoxy resin, described curing agent are released, is stirred, is then lowered the temperature
To 0 ~ 40 DEG C, described initiator is added, is stirred, obtain final product described insulated paint.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722821A (en) * | 2017-10-23 | 2018-02-23 | 重庆大学 | A kind of insulated paint with self-repair function |
| CN108148483A (en) * | 2017-12-18 | 2018-06-12 | 孝感市锐思新材科技有限公司 | A kind of environment-friendly type solvent-free insulated paint and preparation method thereof |
| CN108641550A (en) * | 2018-05-25 | 2018-10-12 | 广州惠利电子材料有限公司 | A kind of curing insulation protection glue and its preparation method and application |
| CN114933845A (en) * | 2022-05-07 | 2022-08-23 | 浙江鑫柔科技有限公司 | Thermosetting weather-proof protective coating material and preparation method and application thereof |
| CN115785800A (en) * | 2022-10-18 | 2023-03-14 | 广州市嵩达新材料科技有限公司 | Photocuring heat-conducting coating and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604384A (en) * | 2012-02-29 | 2012-07-25 | 苏州巨峰电气绝缘系统股份有限公司 | Universal refrigerant resistant solvent-free impregnating resin for high and low voltage motor and preparation method thereof |
| CN105295041A (en) * | 2015-12-03 | 2016-02-03 | 苏州太湖电工新材料股份有限公司 | Polyoxazolidone resin, preparation method of polyoxazolidone resin and application of polyoxazolidone resin in dip varnish |
-
2016
- 2016-11-16 CN CN201611006389.6A patent/CN106519945B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604384A (en) * | 2012-02-29 | 2012-07-25 | 苏州巨峰电气绝缘系统股份有限公司 | Universal refrigerant resistant solvent-free impregnating resin for high and low voltage motor and preparation method thereof |
| CN105295041A (en) * | 2015-12-03 | 2016-02-03 | 苏州太湖电工新材料股份有限公司 | Polyoxazolidone resin, preparation method of polyoxazolidone resin and application of polyoxazolidone resin in dip varnish |
Non-Patent Citations (1)
| Title |
|---|
| 石萌萌: "噁唑烷酮环氧树脂的合成及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722821A (en) * | 2017-10-23 | 2018-02-23 | 重庆大学 | A kind of insulated paint with self-repair function |
| CN108148483A (en) * | 2017-12-18 | 2018-06-12 | 孝感市锐思新材科技有限公司 | A kind of environment-friendly type solvent-free insulated paint and preparation method thereof |
| CN108148483B (en) * | 2017-12-18 | 2021-02-09 | 上海雄润树脂有限公司 | Environment-friendly solvent-free insulating paint and preparation method thereof |
| CN108641550A (en) * | 2018-05-25 | 2018-10-12 | 广州惠利电子材料有限公司 | A kind of curing insulation protection glue and its preparation method and application |
| CN114933845A (en) * | 2022-05-07 | 2022-08-23 | 浙江鑫柔科技有限公司 | Thermosetting weather-proof protective coating material and preparation method and application thereof |
| CN114933845B (en) * | 2022-05-07 | 2023-05-26 | 浙江鑫柔科技有限公司 | Thermosetting weather-proof protective coating material and preparation method and application thereof |
| CN115785800A (en) * | 2022-10-18 | 2023-03-14 | 广州市嵩达新材料科技有限公司 | Photocuring heat-conducting coating and preparation method thereof |
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