CN106752894A - A kind of preparation method of self-lubricating polyamide acid imide enamelled wire paint - Google Patents
A kind of preparation method of self-lubricating polyamide acid imide enamelled wire paint Download PDFInfo
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- CN106752894A CN106752894A CN201611240537.0A CN201611240537A CN106752894A CN 106752894 A CN106752894 A CN 106752894A CN 201611240537 A CN201611240537 A CN 201611240537A CN 106752894 A CN106752894 A CN 106752894A
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- ptfe
- acid imide
- enamelled wire
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- polytetrafluoroethylene
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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
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/14—Polyamide-imides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Paints Or Removers (AREA)
- Insulated Conductors (AREA)
- Organic Insulating Materials (AREA)
Abstract
The present invention relates to a kind of preparation method of self-lubricating polyamide acid imide enamelled wire paint, methods described has excellent high temperature performance and chemical stability using polytetrafluoroethylene (PTFE), good electrical insulating property, non-adhesive, weatherability, not the characteristics of not burning with good lubricity, polyamidoimide is modified, to improve the lubricity of polyamidoimide.Low-viscosity polyamides acid imide (PAI) prepolymer solution is prepared for simultaneously, makes polytetrafluoroethylene (PTFE)（PTFE）Nanometer grade powder is scattered in low-viscosity polyamides acid imide (PAI) prepolymer solution, polytetrafluoroethylene (PTFE) with ball milling, sanding method（PTFE）The dispersiveness of nanometer grade powder is improved, and above-mentioned dispersion liquid is again placed in into reactor heating response after scatter operation terminates, to improve the molecular weight of dispersion liquid.Mix during dispersion liquid containing PTFE powder is added into commercially available or general polyamide-imide enamelled wire varnishes, self-lubricating polyamide acid imide enamelled wire paint is obtained.The enamel-covered wire prepared using self-lubricating polyamide acid imide enamelled wire paint has lubricity more more preferable than common polyamide acid imide enamelled wire, solves the problems, such as scratch of the enamel-covered wire in high-speed winding machine winding process.
Description
Technical field
The present invention relates to wire enamel manufacturing technology, more particularly to both there is resistance to elevated temperatures, there is good self lubricity again
Can be with the preparation method of the wire enamel of submissive performance, the self-lubricating polyamide acid imide enamelled wire paint prepared using the method can
For manufacturing high-performance self-lubricating composite enameled wire, the enamel-covered wire can be widely applied to motor, electrical equipment, transformer particularly magnet ring
Coil makees winding wire.
Background technology
With the development of Power Electronic Technique, all kinds of magnet coils are increasingly strict to the performance requirement of enamel-covered wire, particularly
In fine enameled wire coil high speed winding process, on the one hand require that enamel-covered wire has temperature resistant grade paint film high, on the other hand also
There is good self lubricity and compliance, in existing enamel-covered wire kind, polyamide acid imide enamelled wire has extremely important
Status.Polyamidoimide (PAI) is the transformed lines show developed to improve the machinability shaping of polyimides, it
It is a kind of amorphous fire resistant resin, there is the amide groups of heat-resisting fragrant miscellaneous imine group and flexible lubrication simultaneously in molecule
Group.That is, polyamide acid imide enamelled wire has concurrently, temperature classification is high and the good advantage of greasy property, and heatproof can reach 200
More than DEG C, mechanical performance, coating characteristic of paint liquid of paint film etc. are all more excellent, are the heat stable resins high being used widely
Paint.But, in recent years, the widely used high-speed winding machine of coil-winding technique of electrical equipment, its rotating speed is painted up to thousands of turns per minute
At a high speed by guide wheel, enamel-covered wire can be rubbed and be impacted etc. and be acted on envelope curve during coiling, and the insulating barrier of enamel-covered wire is vulnerable to machinery
Damage, cause decreasing insulating.For the fine enameled wire of small line footpath, in the case of high-speed winding, due to lubrication
It is bad, there is also enamel-covered wire and be attenuated, the phenomenon such as enamel-covered wire line cross-sectional area diminishes causes that coil is scrapped or enamel-covered wire is drawn
Disconnected phenomenon.For reduce coiling when enamelled wire surface coefficient of friction, generally also can on enamel-covered wire coating liquid paraffin or solid
The lubricants such as paraffin, but intermiscibility of the coil of this method coiling when dipping lacquer is processed with impregnating varnish be not good enough, easily produces
The problems such as Poor cohesion.Existing polyamidoimide (PAI) wire enamel is in some purposes, in addition it is also necessary to which further improving should
Plant the self lubricity of wire enamel.In patent CN201410315612.X, a kind of self-lubricating polyamide acid imide insulated paint, with
Nano molybdenum disulfide is main component with metal oxide compounds, prepares the organic dispersions of self-lubricating, is added directly into poly-
In amide imide wire enamel, to reduce the coefficient of friction of enamelled wire surface, enameled wire machining coiling defect is reduced.
In CN201310421069.7 inventions, using fluoro-containing group is introduced in polyamide-imide enamelled wire varnishes, enamel-covered wire is reduced
Coefficient of maximum static friction.In CN201310420489.3 inventions, lubricity is introduced in polyamide acid imide enamelled wire good
Wax liquor, so as to reduce the coefficient of maximum static friction of enamel-covered wire.In CN200910111018.8, the manufacture method of the invention
It is：The lubricant for accounting for that percentage by weight is 1-10% is taken, is added in the dedicated solvent for accounting for percentage by weight 1-10%, heating is simultaneously
Stirring is melted completely to lubricant, obtains lubricant liquid；In 70~80 DEG C of temperature, lubricant liquid is added to common polyamide
In imide enamelled wire varnishes, start agitator and stir 1-1.5 hours.In CN200810040242.8, by directly adding
Plus the mixture of lubricant and organic silicon surfactant, the greasy property of polyamide-imide enamelled wire varnishes film can be improved and rubbed
Wipe coefficient.Above-mentioned various methods there is also some weak points in practice, at present, such as after emollient component is added, to heat-resisting
Property influence, the compatibility of paint liquid and solids stratification phenomenon etc. also have much room for improvement.
The content of the invention
It is an object of the invention to provide a kind of self-lubricating polyamide acid imide enamelled wire paint with excellent self-lubricating property
Preparation method, using the method prepare wire enamel coating manufacture enamel-covered wire be applied to magnet coil, particularly magnet ring
Coil-winding technique uses the operating mode of high-speed winding machine.
The technical scheme is that, the preparation method of the self-lubricating polyamide acid imide enamelled wire paint includes following three
Individual step：
(1) the preparation of low-viscosity polyamides acid imide (PAI) prepolymer solution：
The chemical structure of general formula of polyamidoimide (PAI) resin is as follows：
NCO can be acted on carboxyl, anhydride group under certain condition, and amide groups and imide, polyamides are generated respectively
The direct syntheti c route method of amine acid imide is with TMA（Trimellitic anhydride）PAI is prepared for primary raw material with diisocyanate.I.e.
It is raw material, methyl pyrrolidone with equimolar TMA and diisocyanate（NMP）Be reaction dissolvent, and controlling reaction temperature, when
Between, prepare the PAI of higher degrees of polymerization.In order to increase the flexibility of resin, M-phthalic acid can be suitably added.Diphenyl methane
Diisocyanate, trimellitic anhydride, the mol ratio of M-phthalic acid can be 1:0.8—0.9：0.2—0.1.Its structure is big
Slightly schematically as follows
Direct preparation method has technological process relatively short, advantage simple to operate.In this programme, in order that polyamide acyl is sub-
Amine aqueous solution keeps low viscosity, is more beneficial for polytetrafluoroethylene (PTFE)（PTFE）The dispersion of nanometer grade powder, first synthesizes low-viscosity polyamides
Acid imide (PAI) prepolymer solution, then with the solution dispersion PTFE micro mist and temperature reaction again.Specific synthesis step is as follows：
Methyl diphenylene diisocyanate, trimellitic anhydride are put into equipped with agitating device, the reactor of reflux condensate device,
Its mol ratio of M-phthalic acid is 1:0.8—0.9：0.2-0.1, the quality with above-mentioned three kinds of resin raw materials is 100 parts, is added
Quality is 350 parts of methyl pyrrolidone（NMP）It is reaction dissolvent, 70-80 DEG C is raised to from room temperature, after being incubated 1-2 hours, then
To heat up per hour 15--25 DEG C, reacting balance is carried out, be warming up to 190 DEG C, then be incubated 1-2 hours, system gradually becomes
It is bright, in orange, obtain low-viscosity polyamides acid imide (PAI) prepolymer solution；
(2) polytetrafluoroethylene (PTFE)（PTFE）The preparation of nanometer grade powder dispersion liquid：
By polytetrafluoroethylene (PTFE)（PTFE）Nanometer grade powder is dispersed in the low-viscosity polyamides of the above-mentioned first step with ball milling, sand milling mode
In acid imide (PAI) prepolymer solution, polytetrafluoroethylene (PTFE) has excellent high temperature performance and chemical stability, well electricity
Insulating properties, non-adhesive, weatherability, do not burn and good lubricity.Ball milling, the machinery being sanded are to select nanoscale ball milling
Machine, sand mill are advisable.Its proportioning is 100 parts of low-viscosity polyamides acid imide (PAI) prepolymer solution for taking the first step, is added
20-30 parts of polytetrafluoroethylene (PTFE)（PTFE）Nanometer grade powder, the size distribution of powder should be 95% powder diameter≤200 nanometer,
Ball milling or sanding operation are carried out, 4-5 hours grinding distribution time, polytetrafluoroethylene (PTFE) is obtained（PTFE）The balanced dispersion of nanometer grade powder
In the dispersion liquid of low-viscosity polyamides acid imide (PAI) prepolymer solution.This dispersion liquid is placed in equipped with agitating device, is returned
Heated again in the reactor for flowing condensing unit, be warming up to 190-200 DEG C, insulation is cooled to 70 DEG C, filtering and discharging after 2 hours
Obtain polytetrafluoroethylene (PTFE)（PTFE）Nanometer grade powder dispersion liquid；
(3) the preparation of self-lubricating polyamide acid imide enamelled wire paint：
Take the polytetrafluoroethylene (PTFE) of second step preparation（PTFE）5-15 parts of nanometer grade powder dispersion liquid, general polyamidoimide paint
, be well mixed for the two in the churned mechanically container of band by 100 parts of enamel, and mixing temperature is 50-60 DEG C.Can be prepared by from profit
Sliding polyamide-imide enamelled wire varnishes paint.
The preparation method of this self-lubricating polyamide acid imide enamelled wire paint of the invention mainly has the following advantages：It is prepared for
Low-viscosity polyamides acid imide (PAI) prepolymer solution, solves and directly prepare polyamideimide solution viscosity greatly, polytetrafluoro
Ethene（PTFE）Nanometer grade powder is difficult to scattered problem；Scatter operation terminate after heating response again, improve dispersion liquid point
Son amount.A certain proportion of M-phthalic acid is added in conventional PAI resins synthesis proportioning, the heat resistance of resin and soft has been taken into account
It is pliable；Nanoscale PTFE fine powders are due to smaller with the density contrast of resin liquid, it is easy to which dispersion is suspended in resin liquid.
Specific embodiment
Embodiment 1
The first step：Methyl diphenylene diisocyanate is put into equipped with agitating device, 40 liters of reactors of reflux condensate device
2503 grams, 1537 grams of trimellitic anhydride, 332 grams of M-phthalic acid, its mol ratio is 1:0.8:0.2, add solvent methyl pyrrole
Pyrrolidone（NMP）15302 grams, raw material is 1 with the mass ratio of solvent:3.5.70-80 DEG C are raised to from room temperature, 1-2 hours is incubated
Afterwards, then to heat up per hour 15--25 DEG C, reacting balance is carried out, is warming up to 190 DEG C, then be incubated 1-2 hours, system gradually becomes
For transparent, in orange, low-viscosity polyamides acid imide (PAI) prepolymer solution is obtained；
Second step：Take low-viscosity polyamides acid imide (PAI) prepolymer solution 10kg of the first step, polytetrafluoroethylene (PTFE)（PTFE）Receive
Nanoscale powder 2kg, the grinding distribution in nanoscale ball mill, obtains polytetrafluoroethylene (PTFE) at 4-5 hours grinding distribution time（PTFE）
Nanometer grade powder equilibrium is scattered in the dispersion liquid of low-viscosity polyamides acid imide (PAI) prepolymer solution.By the dispersion liquid, put
Heated again in equipped with agitating device, the reactor of reflux condensate device, be warming up to 190-200 DEG C, insulation is dropped after 2 hours
To 70 DEG C, filtering and discharging is to obtain polytetrafluoroethylene (PTFE) to temperature（PTFE）Nanometer grade powder dispersion liquid；
3rd step：Take the polytetrafluoroethylene (PTFE) of second step preparation（PTFE）The kg of nanometer grade powder dispersion liquid 10, general polyamide acyl
, be well mixed for the two in the churned mechanically container of band by the kg of imide wire coating enamel 200, and mixing temperature is 50-60 DEG C.
Self-lubricating polyamide acid imide enamelled wire paint is obtained.
Embodiment 2
2503 grams of methyl diphenylene diisocyanate is put into equipped with agitating device, 40 liters of reactors of reflux condensate device,
1729 grams of trimellitic anhydride, 166 grams of M-phthalic acid, its mol ratio is 1:0.9:0.1, add solvent methyl pyrrolidones
（NMP）15393 grams, raw material is 1 with the mass ratio of solvent:3.5.Remaining operation is with embodiment 1.
Effect compares：With conventional polyester paint as prime coat, with the self-lubricating polyamide acid imide enamel-cover that embodiment 1,2 is made
Line paint is top coat layer, prepares the self-lubricating composite enameled wire of 0.100mm；With conventional polyester paint as prime coat, common polyamide acyl
Imines is top coat layer, and the common polyamide acid imide enamelled wire for preparing same size is reference substance.Properties are compared,
Result is as follows：
| Test event | Reference examples | Embodiment 1 | Embodiment 2 |
| Conductor diameter/mm | 0.101 | 0.101 | 0.102 |
| Enamel-covered wire external diameter/mm | 0.120 | 0.121 | 0.119 |
| Surface | It is smooth without bright spot | It is smooth without bright spot | It is smooth without bright spot |
| The coefficient of kinetic friction | 0.092042 | 0.043793 | 0.046143 |
| Thermal shock | （280 ± 5 DEG C of test temperature, 30min, diameter of the rod 2D）Test condition Under do not ftracture | （310 ± 5 DEG C, 30min, diameter of the rod 2D）Do not ftractureed under test condition | （310 ± 5 DEG C, 30min, diameter of the rod 2D）Do not opened under test condition Split |
| Softening punctures | （350 ± 5 DEG C of test temperature, test period 2min）Under test condition not Puncture | （370 ± 5 DEG C of test temperature, test period 2min）Under test condition not Puncture | （370 ± 5 DEG C of test temperature, test period 2min）Under test condition Do not puncture |
| Breakdown voltage | 3.5kv | 4.3kv | 4.6kv |
Experiment shows that the present invention can significantly improve the coefficient of kinetic friction, breakdown voltage resistant also to improve a lot.
Claims (3)
1. a kind of preparation method of self-lubricating polyamide acid imide enamelled wire paint, it is characterised in that comprise the steps：
The first step：The preparation of low-viscosity polyamides acid imide (PAI) prepolymer solution：
Methyl diphenylene diisocyanate, trimellitic acid are put into equipped with agitating device, the reactor of reflux condensate device
Acid anhydride, M-phthalic acid adds methyl pyrrolidone（NMP）It is reaction dissolvent, 70-80 DEG C is raised to from room temperature, is incubated 1-2 hours
Afterwards, then to heat up per hour 15--25 DEG C, reacting balance is carried out, is warming up to 190 DEG C, then be incubated 1-2 hours, system gradually becomes
For transparent, in orange, low-viscosity polyamides acid imide (PAI) prepolymer solution is obtained；
Wherein methyl diphenylene diisocyanate, trimellitic anhydride, M-phthalic acid mole ratio is 1:0.8—0.9：
0.2—0.1；Methyl diphenylene diisocyanate, trimellitic anhydride, the quality sum and methyl pyrrolidone of M-phthalic acid
（NMP）The mass ratio of reaction dissolvent is 1:3.5；
Second step：Polytetrafluoroethylene (PTFE)（PTFE）The preparation of nanometer grade powder dispersion liquid：
100 parts of low-viscosity polyamides acid imide (PAI) prepolymer solution of the first step is taken, 20-30 parts of polytetrafluoroethylene (PTFE) are added
（PTFE）Nanometer grade powder, carries out ball milling or sanding operation, 4-5 hours grinding distribution time, obtains polytetrafluoroethylene (PTFE)（PTFE）
Nanometer grade powder equilibrium is scattered in the dispersion liquid of low-viscosity polyamides acid imide (PAI) prepolymer solution, and the dispersion liquid is placed in
Equipped with being heated again in agitating device, the reactor of reflux condensate device, 190-200 DEG C are warming up to, insulation is lowered the temperature after 2 hours
To 70 DEG C, filtering and discharging is to obtain polytetrafluoroethylene (PTFE)（PTFE）Nanometer grade powder dispersion liquid；
3rd step：The preparation of self-lubricating polyamide acid imide enamelled wire paint：
Take the polytetrafluoroethylene (PTFE) of second step preparation（PTFE）5-15 parts of nanometer grade powder dispersion liquid, general polyamidoimide paint
, be well mixed for the two in the churned mechanically container of band by 100 parts of enamel, and mixing temperature is 50-60 DEG C, you can is obtained from profit
Sliding polyamide-imide enamelled wire varnishes.
2. the preparation method of self-lubricating polyamide acid imide enamelled wire paint according to claim 1, it is characterised in that：It is described
Polytetrafluoroethylene (PTFE)（PTFE）The size distribution of nanometer grade powder should be 95% powder diameter≤200 nanometer.
3. the preparation method of self-lubricating polyamide acid imide enamelled wire paint according to claim 1, it is characterised in that：Second
In step, ball milling, be sanded operating process in use ball mill, sand mill be nanoscale ball mill, nanoscale sand mill.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611240537.0A CN106752894A (en) | 2016-12-29 | 2016-12-29 | A kind of preparation method of self-lubricating polyamide acid imide enamelled wire paint |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611240537.0A CN106752894A (en) | 2016-12-29 | 2016-12-29 | A kind of preparation method of self-lubricating polyamide acid imide enamelled wire paint |
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| CN201611240537.0A Pending CN106752894A (en) | 2016-12-29 | 2016-12-29 | A kind of preparation method of self-lubricating polyamide acid imide enamelled wire paint |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114409899A (en) * | 2022-02-10 | 2022-04-29 | 南通百川新材料有限公司 | Novel synthetic method of self-lubricating polyamide-imide insulating resin |
| CN114724744A (en) * | 2022-03-24 | 2022-07-08 | 上海蔚兰动力科技有限公司 | Corona-resistant enameled wire for motor, preparation method of corona-resistant enameled wire and flat wire motor |
-
2016
- 2016-12-29 CN CN201611240537.0A patent/CN106752894A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114409899A (en) * | 2022-02-10 | 2022-04-29 | 南通百川新材料有限公司 | Novel synthetic method of self-lubricating polyamide-imide insulating resin |
| CN114724744A (en) * | 2022-03-24 | 2022-07-08 | 上海蔚兰动力科技有限公司 | Corona-resistant enameled wire for motor, preparation method of corona-resistant enameled wire and flat wire motor |
| CN114724744B (en) * | 2022-03-24 | 2024-01-09 | 上海蔚兰动力科技有限公司 | Corona-resistant enameled wire for motor, preparation method of corona-resistant enameled wire and flat wire motor |
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