CN106497052A - A kind of high temperature resistance polyester imine nanometer ultrathin membrane and preparation method thereof - Google Patents
A kind of high temperature resistance polyester imine nanometer ultrathin membrane and preparation method thereof Download PDFInfo
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Abstract
A kind of high temperature resistance polyester imine nanometer ultrathin membrane and preparation method thereof, the uniform and stable solution system being made up of polyester-imide, CNT, organic solvent, diluent and auxiliary agent is in the presence of mechanical external force, (quartz in clean substrate, glass, metal, monocrystalline silicon, polyfluortetraethylene plate) presentation nanoscale is uniformly sprawled, then polyester-imide nanostructured thin film is generated by chemical imidization or hot imidization.
Description
Technical field
The invention belongs to film preparation and application, more particularly to a kind of high temperature resistance polyester imine nanometer ultrathin membrane and its system
Preparation Method.
Background technology
High temperature resistance polyester imines, is mainly used in enamel-covered wire industry at present.Existing high temperature resistance polyester imines at present, in market
Application commonplace, but exist problem be that mechanical property has much room for improvement, resistance to elevated temperatures needs further to improve；In order to
Meet the demand on market, be badly in need of the new strong self-lubricating of exploitation, high temperature resistance and long life-span polyester-imide.
Content of the invention
The problem to be solved in the present invention is to provide a kind of high temperature resistance polyester imine nanometer ultrathin membrane and preparation method thereof.
A kind of high temperature resistance polyester imine nanometer ultrathin membrane, by parts by weight 100-120 parts polyester-imide and the carbon of 0.1-5 parts
Nano-tube material component；
The polyester-imide is by the polyester imine resin of parts by weight 20-35 parts, the organic solvent of 20-60 parts, 0.1-10
Part diluent, the first auxiliary agent of 0.1-20 parts, the second auxiliary agent of 0.1-20 parts, the 3rd auxiliary agent of 0.1-20 parts composition；
Sun of the carbon nano-tube material by the CNT, the silane coupler of 20-60 parts, 2-5 parts that parts by weight are 100 parts
Ionic surface active agent is constituted.
The CNT using the SWCN of a diameter of 1-100nm, multi-walled carbon nano-tubes, T-shaped CNT,
Any one or more than one of Y type CNTs, N-shaped CNT, p-type CNT are arbitrarily combined.
CNT is comparatively ideal polymer modification agent, hands over good antiacid dissolubility, very low cation
The physicochemical properties such as the amount of changing, preferable fire resistance；CNT have decolourize, heat-insulated, insulation, anticorrosive, radioresistance and thermally-stabilised
Etc. performance.Therefore appropriate CNT is added after insulated paint system, product can be made to have more satisfactory mechanical property and heat
Stability, can form certain wear-resisting point on the surface of material, strengthen its anti-wear performance and greasy property, it is possible to increase its anti-corruption
Corrosion and insulating properties.
The organic solvent be 1-METHYLPYRROLIDONE, chlorobenzene, bromobenzene, dichloro-benzenes, dibromobenzene, ALPHA-tetralone, fenchone,
The combination of any one or more than one arbitrary proportions in phorone, isophorone；
Wherein：1-METHYLPYRROLIDONE can be dissolved each other with materials such as esters, volatility is low, heat endurance and chemical stability are equal
Good, and 1-METHYLPYRROLIDONE effect on environment is little, while low price, be organic solvent in the application most preferably.
Chlorobenzene, bromobenzene, dichloro-benzenes, dibromobenzene belong to benzene class, itself can be used as organic molten, while can be organic molten with other
Agent is dissolved each other, and often independent or mixing in Chemical Manufacture is used as solvent, is particularly used as the solvent of resin.
ALPHA-tetralone, fenchone, phorone, isophorone are ketone, and chemical property is active, is commonly used for such as resin etc.
Solvent.
Above organic solvent can be according to the needs of actual production, to the different requirements of final products performance, in conjunction with each material
The factors such as the complexity that cost, different regions obtain, effect on environment, select a kind of most suitable material therein individually to make
Use for organic solvent, or select the combination of more than one arbitrary substances to be used as organic solvent use, most closed with reaching
Suitable scheme.
For reducing the viscosity of product, the diluent for increasing its mobility addition is ditridecyl phthalate, phthalic acid
Dibutyl ester, diisobutyl phthalate, dioctyl phthalate, diamyl phthalate or phthalic acid diisoamyl
One or more in ester are arbitrarily combined；
For increase polyester imine resin dissolubility add first and second auxiliary agent, the first auxiliary agent be toluene, benzene, ortho-xylene,
One or more in meta-xylene, paraxylene are arbitrarily combined；
Second auxiliary agent is ethylbenzene, second propyl benzene, butyl benzene, isobutyl-benzene, one or more in tert-butyl benzene
Arbitrary combination；
Dissolubility and mobility in order to increase polyester imine resin adds the 3rd auxiliary agent, and the 3rd auxiliary agent is 2- fourths
One or more in ketone, cyclopentanone, cyclohexanone are arbitrarily combined.
For improving the intersolubility of CNT and polyester-imide solution, its mechanical property and insulating properties are further enhanced,
And can make final products that there is long-life and good self-lubricating property to add silane coupler and/or surfactant；
The silane coupler is one or more in KH550, KH560, KH570, KH792, DL602, DL171
Arbitrary combination；
The surfactant is cationic surfactant；The cationic surfactant is quaternary ammonium salt, amine salt, second
Epoxide acid amides, alkyl imidazoline, alkyl imidazoline salt, phosphate, phosphate, sulfonate, quatemay ammonium inner salt, propylamine hydrochlorate, tell
Heating and melting is taken in one or more arbitrary combinations in temperature 60, polyethylene polyamines salt, agent rope Luo Ming A, fatty amine salt
Churned mechanically mode arbitrary proportion mixing；
The quaternary ammonium salt is DTAC, tridecyl trimethyl ammonium chloride, tetradecyltrimethylammonium
Ammonium chloride, pentadecyl trimethyl ammonium chloride, hexadecyltrimethylammonium chloride, heptadecyl trimethyl ammonium chloride, octadecane
Base trimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride, octadecyldimethyl hydroxyethyl ammonium nitrate, octadecyl two
Dimethyl hydroxyethyl ammonium perchlorate, stearic acid trimethyl ammonium chloride, stearic acid dimethyl-penten ammonium chloride；
The amine salt is ethoxy amine salt or ethoxylated fatty amine salt；
The sulfonate is sodium alkyl sulfonate, alkyl diphenyl ether disulphonic acid, alkylbenzenesulfonate, alkylnaphthalene sulfonate, nonyl
Phenoxyl propane sulfonic acid sodium or to nonyl diphenyl ether potassium sulfonate；
The quatemay ammonium inner salt is dodecyl dimethyl quaternary ammonium second inner salt；
The propylamine hydrochlorate is dimethyl ethanol base stearamide propyl ammonium nitrate.
Coupling agent can reduce the viscosity of resin melt, improve decentralization to improve processing characteristics, and then it is good to obtain product
Good surface quality and machinery, heat and electrical property；Surfactant is aligned in the surface energy of solution, and can make surface tension
The material being remarkably decreased；Individually add coupling agent in CNT or individually interpolation surfactant can be to a certain degree
The performance of CNT is improved, but it is preferably add appropriate coupling agent and surfactant simultaneously, two kinds of materials are made jointly
With the surface tension of CNT being down to more preferably level, the tension force on the dispersion surface being beneficial in organic system.
The preparation method of the present invention is as follows：
1) polyester-imide solution is prepared：The polyester imine resin for taking 20-35 parts by weight is dissolved in the organic of 20-60 parts
In solvent, 0.1-10 part diluents, the first auxiliary agent of 0.1-20 parts, the second auxiliary agent of 0.1-20 parts and 0.1-20 part is sequentially added
Three auxiliary agents；
2) take by weight 100 parts nano level CNT, the silane coupler of 20-60 parts, 2-5 parts sun from
Sub- surfactant decentralized processing obtains carbon nano-tube material；
3) carbon nano-tube material for taking 2-5 parts by weight is added in the polyester-imide solution of 100-120 parts and stirs
Uniform polyester-imide solution system；
4) using spin coating method, doctor blade process or substrate the tape casting by step 3) polyester-imide solution system uniformly spread over clean
In net substrate and solvent flashing, pending film is obtained；Then pending film is obtained through imidization method crosslinking curing
High temperature resistance polyester imine nanometer ultrathin membrane.
The step 2) decentralized processing be room temperature at a temperature of 100 DEG C using ultrasonic wave disperse 10-30 minutes.
The step 3) carbon nano-tube material is added with 300-1000 rev/min of mixing speed to 100 DEG C in room temperature
To in polyester-imide solution.
The step 4) by polyester-imide solution system uniformly spread over cleaning suprabasil process be big in vacuum
Carry out in the environment for being equal to 80KPa；The power size that the rotation of sol evenning machine is produced in spin coating method is 0.5-10N, and rotating speed is
120-600r/min, and choice of the substrates has a matrix of 10-70mm effective radiuses, the roughness of clean substrate is less than or equal to
0.5μm；In doctor blade process and substrate the tape casting, the roughness of clean substrate is less than or equal to 0.4 μm.
Described imidization method is chemical imines method, hot imines method and chemical hot imidization method：
Described chemical imidization method：It is that pending film is immersed in 30 DEG C of imidization solution together with substrate, constant temperature
Then pending film is dried 3-4 hours at 50-80 DEG C by 1-2 hours；
Described hot imidization method：It is by pending film constant temperature 0.5-1 hours at 120 DEG C, is then being less than or equal to
150-200 DEG C DEG C of constant temperature 0.5-1 hour is warmed up under the heating rate of 20 DEG C/min；
Described chemical hot imidization method：It is that pending film is immersed 30 DEG C of imidization solution constant temperature 1- together with substrate
2 hours, pending film is dried 3-4 hours at 50-80 DEG C then, then is raised under the heating rate less than 20 DEG C/min
150-200 DEG C of constant temperature 0.5-1 hour.
Specific embodiment
Embodiment 1
The high temperature resistance polyester imine nanometer ultrathin membrane that the present embodiment is provided, which includes that weight is 100～120 parts
The carbon nano-tube material of polyester-imide solution and 0.1～5 part；
Wherein, polyester-imide solution includes the component of following weight：
Polyester imine resin：20-35 parts,
It is used as the organic solvent 1-METHYLPYRROLIDONE of polyester imine resin solvent：20-60 parts,
It is used as the ditridecyl phthalate of diluent：0.1-10 parts
It is used as the toluene of the first auxiliary agent：0.1-20 parts,
It is used as the ethylbenzene of the second auxiliary agent：0.1-20 parts,
It is used as the 2- butanone (i.e. methyl ethyl ketone) of the 3rd auxiliary agent：0.1-20 parts.
Carbon nano-tube material includes the component of following weight：
The CNT of Nano grade：10 parts,
Silane coupling agent KH550：2-6 parts,
DTAC：0.2-0.5 parts.
Wherein, the organic solvent as polyester imine resin solvent, in addition to the 1-METHYLPYRROLIDONE for individually adopting, 2-
Methyl pyrrolidone, chlorobenzene, bromobenzene, dichloro-benzenes, dibromobenzene, ALPHA-tetralone, fenchone, phorone, isophorone be respectively provided with
The very approximate property of 1-METHYLPYRROLIDONE, using them, these very approximate properties can reach dissolved polyester imines tree
The purpose of fat, therefore can arbitrarily select one kind from above-mentioned organic solution；Simultaneously because these organic solvents be respectively provided with excellent
Intersolubility, therefore more than one any combination in above-mentioned organic solvent can be selected, to reach according to the concrete condition of actual production
Arrive most suitable effect.
In the same manner, diluent is in addition to the ditridecyl phthalate for individually adopting, can also using property approximate, can dissolve each other
Dibutyl phthalate, diisobutyl phthalate, dioctyl phthalate, diamyl phthalate or adjacent benzene two
In any one in formic acid diisoamyl ester, or above diluent, more than one arbitrarily combine.
In the same manner, the first auxiliary agent can also adopt, in addition to the toluene for individually adopting, property is approximate, can dissolve each other benzene, adjacent two
In any one in toluene, meta-xylene, paraxylene, or above auxiliary agent, more than one arbitrarily combine.
In the same manner, the second auxiliary agent is in addition to the ethylbenzene for individually adopting, can also, the second propyl benzene that can dissolve each other approximate using property,
In any one in butyl benzene, isobutyl-benzene, tert-butyl benzene, or above auxiliary agent, more than one arbitrarily combine.
In the same manner, the 3rd auxiliary agent is in addition to the 2- butanone (i.e. methyl ethyl ketone) for individually adopting, can also adopt property approximate,
Any one in the cyclopentanone that can dissolve each other, cyclohexanone, or more than one arbitrarily combine in above auxiliary agent.
Coupling agent in carbon nano-tube material, in addition to the Silane coupling agent KH550 for individually adopting, also include KH560,
KH570, KH792, DL602, DL171, can arbitrarily select one kind from above-mentioned organic solution；Simultaneously because these are silane coupled
Agent is respectively provided with excellent intersolubility, therefore can according to the concrete condition of actual production, select in above-mentioned silane coupler a kind of with
Upper any combination, to reach most suitable effect.
In the same manner, the surfactant in carbon nano-tube material includes quaternary ammonium salt (DTAC, tridecane
Base trimethyl ammonium chloride, tetradecyl trimethyl ammonium chloride, pentadecyl trimethyl ammonium chloride, cetyl trimethyl chlorination
Ammonium, heptadecyl trimethyl ammonium chloride, OTAC, dodecyl benzyl dimethyl ammonium chloride, octadecane
Base dimethyl hydroxy ethyl ammonium nitrate, octadecyldimethyl ethoxy ammonium perchlorate, stearic acid trimethyl ammonium chloride, stearic acid two
Methyl amyl ammonium chloride etc.), amine salt (ethoxy amine salt, ethoxylated fatty amine salt etc.), amide ethoxylates, alkyl imidazoline,
Alkyl imidazoline salt, phosphate, phosphate, sulfonate (sodium alkyl sulfonate, alkyl diphenyl ether disulphonic acid, alkylbenzenesulfonate, alkane
Base naphthalene sulfonate, ABPS, to nonyl diphenyl ether potassium sulfonate etc.), quatemay ammonium inner salt (dodecyl dimethyl
Quaternary ammonium second inner salt etc.), propylamine hydrochlorate (dimethyl ethanol base stearamide propyl ammonium nitrate etc.), polysorbate60, polyethylene polyamines
Any one or more than one in salt, agent rope Luo Ming A, fatty amine salt are arbitrarily combined.Above-mentioned for common cationic surface
Activating agent Typical Representative, property are similar to very much, it is also possible to which arbitrary proportion is used in mixed way, and take heating and melting mechanical agitation during mixing
Mode.
Embodiment 2
The preparation method of the polyester-imide insulated paint that the present embodiment is provided, the step of which includes following order：
1) polyester-imide solution is prepared：
Weight is dissolved in 20-60 parts for the polyester imine resin of 20-35 parts and is used as polyester imine resin solvent
In 1-METHYLPYRROLIDONE, stirring be completely dissolved after, sequentially add 0.1-10 parts as diluent ditridecyl phthalate,
0.1-20 parts are used as the ethylbenzene of the toluene of the first auxiliary agent, 0.1-20 parts as the second auxiliary agent, 0.1-20 parts and are used as the 3rd auxiliary agent
2- butanone is until completely dissolved, standby；
2) pretreatment of CNT：
By Nano grade CNT that weight is 5 parts, 4 parts of Silane coupling agent KH550 and 0.5 part 12
Alkyl trimethyl ammonium chloride is well mixed, and then again under room temperature, disperses 10-30 minutes using in ultrasonic cleaner, standby；
3) by step 1) in the polyester-imide solution for preparing, in room temperature within the temperature range of 60 DEG C, with 300-
1000 revs/min of mixing speed, stirs and adds through step 2) carbon nano-tube material that pre-processes.
4) sol evenning machine 0.5N, uniform rotating speed 200r/min are set, vacuum is 80KPa, effective radius is selected for 50mm's
Substrate prepares polyester-imide nanostructured thin film.
5) constant temperature 3 hours under conditions of obtained polyester-imide nanostructured thin film being placed on 120 DEG C, is then slowly risen again
(heating rate be less than 20 DEG C/min) is taken out, you can polyester-imide nano ultrathin membrane is obtained to 200 DEG C of constant temperature 3 hours.
Wherein, the organic solvent as polyester imine resin solvent, in addition to the 1-METHYLPYRROLIDONE for individually adopting, 2-
Methyl pyrrolidone, chlorobenzene, bromobenzene, dichloro-benzenes, dibromobenzene, ALPHA-tetralone, fenchone, phorone, isophorone be respectively provided with
The very approximate property of 1-METHYLPYRROLIDONE, using them, these very approximate properties can reach dissolved polyester imines tree
The purpose of fat, therefore can arbitrarily select one kind from above-mentioned organic solution；Simultaneously because these organic solvents be respectively provided with excellent
Intersolubility, therefore more than one any combination in above-mentioned organic solvent can be selected, to reach according to the concrete condition of actual production
Arrive most suitable effect.
In the same manner, diluent is in addition to the ditridecyl phthalate for individually adopting, can also using property approximate, can dissolve each other
Dibutyl phthalate, diisobutyl phthalate, dioctyl phthalate, diamyl phthalate or adjacent benzene two
In any one in formic acid diisoamyl ester, or above diluent, more than one arbitrarily combine.
In the same manner, the first auxiliary agent can also adopt, in addition to the toluene for individually adopting, property is approximate, can dissolve each other benzene, adjacent two
In any one in toluene, meta-xylene, paraxylene, or above auxiliary agent, more than one arbitrarily combine.
In the same manner, the second auxiliary agent is in addition to the ethylbenzene for individually adopting, can also, the second propyl benzene that can dissolve each other approximate using property,
In any one in butyl benzene, isobutyl-benzene, tert-butyl benzene, or above auxiliary agent, more than one arbitrarily combine.
In the same manner, the 3rd auxiliary agent is in addition to the 2- butanone (i.e. methyl ethyl ketone) for individually adopting, can also adopt property approximate,
Any one in the cyclopentanone that can dissolve each other, cyclohexanone, or more than one arbitrarily combine in above auxiliary agent.
Coupling agent in carbon nano-tube material, in addition to the Silane coupling agent KH550 for individually adopting, also include KH560,
KH570, KH792, DL602, DL171, can arbitrarily select one kind from above-mentioned organic solution；Simultaneously because these are silane coupled
Agent is respectively provided with excellent intersolubility, therefore can according to the concrete condition of actual production, select in above-mentioned silane coupler a kind of with
Upper any combination, to reach most suitable effect.
In the same manner, the surfactant in carbon nano-tube material includes quaternary ammonium salt (DTAC, tridecane
Base trimethyl ammonium chloride, tetradecyl trimethyl ammonium chloride, pentadecyl trimethyl ammonium chloride, cetyl trimethyl chlorination
Ammonium, heptadecyl trimethyl ammonium chloride, OTAC, dodecyl benzyl dimethyl ammonium chloride, octadecane
Base dimethyl hydroxy ethyl ammonium nitrate, octadecyldimethyl ethoxy ammonium perchlorate, stearic acid trimethyl ammonium chloride, stearic acid two
Methyl amyl ammonium chloride etc.), amine salt (ethoxy amine salt, ethoxylated fatty amine salt etc.), amide ethoxylates, alkyl imidazoline,
Alkyl imidazoline salt, phosphate, phosphate, sulfonate (sodium alkyl sulfonate, alkyl diphenyl ether disulphonic acid, alkylbenzenesulfonate, alkane
Base naphthalene sulfonate, ABPS, to nonyl diphenyl ether potassium sulfonate etc.), quatemay ammonium inner salt (dodecyl dimethyl
Quaternary ammonium second inner salt etc.), propylamine hydrochlorate (dimethyl ethanol base stearamide propyl ammonium nitrate etc.), polysorbate60, polyethylene polyamines
Any one or more than one in salt, agent rope Luo Ming A, fatty amine salt are arbitrarily combined.Above-mentioned for common cationic surface
Activating agent Typical Representative, property are similar to very much, it is also possible to which arbitrary proportion is used in mixed way, and take heating and melting mechanical agitation during mixing
Mode.
Claims (8)
1. a kind of high temperature resistance polyester imine nanometer ultrathin membrane, it is characterised in that：By parts by weight 100-120 parts polyester-imide and
0.1～5 part of carbon nano-tube material component；
The polyester-imide is dilute by the polyester imine resin of parts by weight 20-35 parts, the organic solvent of 20-60 parts, 0.1-10 parts
Release agent, the first auxiliary agent of 0.1-20 parts, the second auxiliary agent of 0.1-20 parts, the 3rd auxiliary agent of 0.1-20 parts composition；
Cation of the carbon nano-tube material by the CNT, the silane coupler of 20-60 parts, 2-5 parts that parts by weight are 100 parts
Surfactant is constituted；
The CNT is using the SWCN of a diameter of 1-100nm, multi-walled carbon nano-tubes, T-shaped CNT, Y types
Any one or more than one of CNT, N-shaped CNT, p-type CNT are arbitrarily combined.
2. high temperature resistance polyester imine nanometer ultrathin membrane according to claim 1, it is characterised in that：The organic solvent is N-
Any in methyl pyrrolidone, chlorobenzene, bromobenzene, dichloro-benzenes, dibromobenzene, ALPHA-tetralone, fenchone, phorone, isophorone
The combination of one or more arbitrary proportions；
The diluent is ditridecyl phthalate, dibutyl phthalate, diisobutyl phthalate, phthalic acid
One or more in dioctyl ester, diamyl phthalate or di-iso-amyl phthalate are arbitrarily combined；
First auxiliary agent is that toluene, benzene, ortho-xylene, meta-xylene, one or more in paraxylene are arbitrary
Combination；
Second auxiliary agent is that ethylbenzene, second propyl benzene, butyl benzene, isobutyl-benzene, one or more in tert-butyl benzene are any
Combination；
3rd auxiliary agent is 2- butanone, cyclopentanone, one or more in cyclohexanone are arbitrarily combined.
3. high temperature resistance polyester imine nanometer ultrathin membrane according to claim 1, it is characterised in that：The silane coupler is
One or more in KH550, KH560, KH570, KH792, DL602, DL171 are arbitrarily combined；
The surfactant is cationic surfactant；The cationic surfactant is quaternary ammonium salt, amine salt, ethyoxyl
Change acid amides, alkyl imidazoline, alkyl imidazoline salt, phosphate, phosphate, sulfonate, quatemay ammonium inner salt, propylamine hydrochlorate, polysorbate60,
One or more arbitrary combinations in polyethylene polyamines salt, agent rope Luo Ming A, fatty amine salt take heating and melting machinery to stir
The mode arbitrary proportion mixing that mixes；
The quaternary ammonium salt is DTAC, tridecyl trimethyl ammonium chloride, tetradecyltrimethylammonium chlorination
Ammonium, pentadecyl trimethyl ammonium chloride, hexadecyltrimethylammonium chloride, heptadecyl trimethyl ammonium chloride, octadecyl three
Ammonio methacrylate, dodecyl benzyl dimethyl ammonium chloride, octadecyldimethyl hydroxyethyl ammonium nitrate, octadecyldimethyl
Ethoxy ammonium perchlorate, stearic acid trimethyl ammonium chloride, stearic acid dimethyl-penten ammonium chloride；
The amine salt is ethoxy amine salt or ethoxylated fatty amine salt；
The sulfonate is sodium alkyl sulfonate, alkyl diphenyl ether disulphonic acid, alkylbenzenesulfonate, alkylnaphthalene sulfonate, nonyl benzene
Epoxide propane sulfonic acid sodium or to nonyl diphenyl ether potassium sulfonate；
The quatemay ammonium inner salt is dodecyl dimethyl quaternary ammonium second inner salt；
The propylamine hydrochlorate is dimethyl ethanol base stearamide propyl ammonium nitrate.
4. a kind of preparation method such as any one high temperature resistance polyester imine nanometer ultrathin membrane in claim 1-3, its feature exist
In：
1) polyester-imide solution is prepared：The polyester imine resin for taking 20-35 parts by weight is dissolved in the organic solvent of 20-60 parts
In, sequentially add 0.1-10 part diluents, the first auxiliary agent of 0.1-20 parts, the second auxiliary agent of 0.1-20 parts and 0.1-20 parts the 3rd and help
Agent；
2) take by weight 100 parts nano level CNT, the silane coupler of 20-60 parts, the cation form of 2-5 parts
Face activating agent decentralized processing, obtains carbon nano-tube material；
3) carbon nano-tube material for taking 2-5 parts by weight is added in the polyester-imide solution of 100-120 parts and stirs
Obtain polyester-imide solution system；
4) using spin coating method, doctor blade process or substrate the tape casting by step 3) polyester-imide solution system uniformly spreads over cleaning
In substrate and solvent flashing, pending film is obtained；Then pending film is obtained resistance to height through imidization method crosslinking curing
Warm polyester-imide nanostructured thin film.
5. the preparation method of high temperature resistance polyester imine nanometer ultrathin membrane according to claim 4, it is characterised in that：The step
Rapid decentralized processing 2) is to disperse 10-30 minute using ultrasonic wave in room temperature at a temperature of 100 DEG C.
6. the preparation method of high temperature resistance polyester imine nanometer ultrathin membrane according to claim 4, it is characterised in that：The step
Rapid 3) carbon nano-tube material is added to by polyester-imide solution with 300-1000 rev/min of mixing speed in room temperature to 100 DEG C
In.
7. the preparation method of high temperature resistance polyester imine nanometer ultrathin membrane according to claim 4, it is characterised in that：The step
Rapid 4) by polyester-imide solution system uniformly spread over cleaning suprabasil process be vacuum more than or equal to 80KPa ring
Carry out in border；The power size that the rotation of sol evenning machine is produced in spin coating method is 0.5-10N, and rotating speed is 120-600r/min, and base
Bottom selects the roughness of the matrix with 10-70mm effective radiuses, clean substrate to be less than or equal to 0.5 μm；Doctor blade process and base
In the tape casting of bottom, the roughness of clean substrate is less than or equal to 0.4 μm.
8. the preparation method of high temperature resistance polyester imine nanometer ultrathin membrane according to claim 6, it is characterised in that：Described
Imidization method is chemical imines method, hot imines method and chemical hot imidization method：
Described chemical imidization method：It is that pending film is immersed in 30 DEG C of imidization solution together with substrate, constant temperature 1-2 is little
When, pending film is dried 3-4 hours at 50-80 DEG C then；
Described hot imidization method：Be at 120 DEG C by pending film constant temperature 0.5-1 hours, then less than or equal to 20 DEG C/
150-200 DEG C DEG C of constant temperature 0.5-1 hour is warmed up under the heating rate of min；
Described chemical hot imidization method：It is that pending film is little together with the imidization solution constant temperature 1-2 that substrate immerses 30 DEG C
When, pending film is dried 3-4 hours at 50-80 DEG C then, then is raised under the heating rate less than 20 DEG C/min
150-200 DEG C of constant temperature 0.5-1 hour.
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| CN110853934A (en) * | 2019-11-20 | 2020-02-28 | 陕西科技大学 | Three-dimensional dual-function carbon micron tube/nitrogen-doped reduced graphene oxide composite biomass material and preparation method and application thereof |
| CN111370186A (en) * | 2020-03-25 | 2020-07-03 | 中原工学院 | Preparation method of coating of aluminum wire for electric wire and cable |
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| CN105838071A (en) * | 2016-04-22 | 2016-08-10 | 广东精达里亚特种漆包线有限公司 | Nanometer polyester imide film containing inorganic oxide and preparation method of nanometer polyester imide film |
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| CN1414037A (en) * | 2002-11-15 | 2003-04-30 | 中国科学院兰州化学物理研究所 | Self-lubricating nano composite material and its preparation method |
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| CN110853934A (en) * | 2019-11-20 | 2020-02-28 | 陕西科技大学 | Three-dimensional dual-function carbon micron tube/nitrogen-doped reduced graphene oxide composite biomass material and preparation method and application thereof |
| CN111370186A (en) * | 2020-03-25 | 2020-07-03 | 中原工学院 | Preparation method of coating of aluminum wire for electric wire and cable |
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