CN111825982A - Colorless transparent high-temperature-resistant polyimide film and preparation method thereof - Google Patents
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Abstract
The invention discloses a colorless transparent high-temperature-resistant polyimide film and a preparation method thereof, wherein the preparation method comprises the following steps: dissolving aliphatic diamine and aromatic dianhydride in a polar aprotic solvent to generate a polyamic acid solution, adding a functional auxiliary agent, casting the solution onto a steel belt under a nitrogen atmosphere after defoaming, heating in sections for imidization, and stretching in two directions to obtain the colorless transparent high-temperature-resistant polyimide film. The polyimide film prepared by the invention has high transparency and high heat resistance.
Description
Technical Field
The invention relates to the field of plastic film materials, in particular to a colorless transparent high-temperature-resistant polyimide film and a preparation method thereof.
Background
The polyimide film has high and low temperature resistance, good mechanical property, degradable and recyclable materials and good dielectric property, and is widely applied to the fields of microelectronics, insulating plastics, separation membranes, medical appliances and the like. The common polyimide film has dark yellow color and low light transmittance, and limits the application of the polyimide film in the photoelectric field. Introduction of CF into the system is generally adopted in the prior art3The light transmission performance of the polyimide film is improved by the modes of large steric hindrance side group, twisted non-coplanar structure and the like, but the high temperature resistance of the polyimide film is reduced by the prior art.
Patent CN200710193596.1 uses 4, 4' -triphenyl diether tetracid dianhydride, polymerizing with 2, 2 ' -bis (trifluoromethyl) -4, 4 ' -biphenyldiamine, 3 ' -diaminodiphenyl sulfone and 3, 3 ' -dimethyl-4, 4 ' -diaminodiphenyl methane in a polar solvent to generate polyamic acid, casting the polyamic acid on a clean glass plate, placing the polyamic acid in a film drying oven for 2 hours at the temperature of 80 ℃ until the solvent is volatilized and the film is solidified, the glass plate coated with the polyimide film is moved into an oven, the oven is heated from room temperature to 350 ℃ at the heating rate of 2 ℃/min, and then naturally cooling the temperature to room temperature, taking out the glass plate coated with the polyimide film from the oven, putting the glass plate into water, boiling the glass plate, and peeling the polyimide film from the glass plate to obtain the flexible transparent polyimide film material. The ultraviolet light transmission cutoff wavelength of the polyimide film is 395-430 nm; the glass transition temperature is between 254 and 280 ℃.
Patent CN201210401927.7 discloses a transparent polyimide resin material obtained by polycondensation reaction of 1, 4-bis (3, 4-dicarboxyphenoxy) cyclohexane dianhydride monomer and diamine primary amine monomer. The dianhydride monomer has an alicyclic structure, so that the formation of a charge transfer complex in polyimide molecules and among molecules can be effectively inhibited, and the transparency of the polymer is greatly improved; meanwhile, the phthalic anhydride structures at two ends keep the high reaction activity of dianhydride. The obtained polyimide film has the glass transition temperature of 200-300 ℃, the ultraviolet absorption cutoff wavelength of 340-380 nm and the light transmittance of 70-90% at 450nm, and has good application prospects in the fields of flexible substrate materials of solar cells, flexible transparent conductive film substrate materials, liquid crystal display materials and the like.
Patent CN201910931988.6 discloses a polyimide precursor solution and a transparent polyimide film made from the polyimide precursor solution. The polyimide precursor solution comprises diamine, first dianhydride containing a biphenyl structure, second dianhydride containing a rigid alicyclic structure, third dianhydride containing a non-alicyclic structure and an organic solvent. The polyimide film skeleton structure at least comprises one biphenyl and a rigid alicyclic structure. The transparent polyimide film has the modulus of more than 4.5GPa, the glass transition temperature (Tg) of more than 370 ℃ and the yellowness index of not more than 3.0, and can be used as a substrate to be applied to flexible display fields such as Thin Film Transistors (TFT), Touch Screens (TSP), Organic Light Emitting Diodes (OLED), flexible Liquid Crystal Displays (LCD) and the like or cover plate films in other fields.
The polyimide film is used as a substrate material in the flexible screen, and the polyimide film is required to have the advantages of high temperature resistance, high strength, high transparency and the like, and the glass transition temperature and the heat resistance of the polyimide film are reduced while the transparency of the polyimide film is improved mostly in the patents and the prior art, so that the requirement of the future photoelectric field on the polyimide film cannot be met, and therefore, the polyimide film which is high in transparency and does not lower in high temperature resistance level has great significance in development.
Disclosure of Invention
The invention provides a colorless transparent high-temperature-resistant polyimide film and a preparation method thereof, which solve the problem that the high-temperature resistance of the colorless transparent polyimide film is reduced in the prior art.
According to the preparation method, a functional auxiliary agent is added into a system, so that the polyimide film with high light transmittance and high heat resistance is obtained.
A colorless transparent high temperature resistant polyimide film and a preparation method thereof comprise the following steps:
(1) dissolving 40-60 parts of aromatic diamine in polar aprotic solvent, adding 40-60 parts of alicyclic dianhydride, and controlling the temperature of the reaction solution to be 0-18 DEGoC, stirring and reacting for 4-7h at 200r/min to obtain a polyamic acid solution;
(2) adding 5-15 parts of functional auxiliary agent into polyamic acid, uniformly dispersing, and carrying out vacuum-assisted ultrasonic defoaming on the solution;
(3) and under the protection of nitrogen, casting the defoamed solution onto a steel belt filled with nitrogen, heating in a sectional manner for imidization, wherein the thickness of the cast film is 10-100 mu m, and performing biaxial tension to obtain the colorless transparent high-temperature-resistant polyimide film.
The reaction is as follows:
preferably, the aromatic diamine in step (1) is one or more of p-phenylenediamine, m-phenylenediamine, 4 ' -diaminodiphenylmethane, 4 ' -diaminodiphenyl ether, 4 ' -diaminobenzophenone, 4 ' -diaminodiphenylsulfone, 1, 4-bis (4-aminophenoxy) benzene, 1, 3-bis (4 ' -aminophenoxy) benzene and benzidine.
Preferably, the method according to claim 1, wherein the nonpolar protic solvent in step (1) is one or more of N-methylpyrrolidone, dimethylformamide and dimethylacetamide.
Preferably, the aliphatic dianhydride in step (1) is one or a combination of more of BOCA, CBDA, CPDA, CHDA, TFPPA, DMBD, TCPDA, DAA, DADA, MCA and MMCA.
Preferably, the preparation method of the functional assistant in the step (2) comprises the following steps:
adding 100 parts of hollow glass microspheres, 2.3-6.3 parts of vinyl-dihydroxy-methylsilane and 0.3-1.5 parts of acetic acid into 500 parts of water by mass, controlling the temperature to be 50-70 ℃, stirring for 1-5h, uniformly mixing, filtering, drying to obtain an intermediate product 1,
according to the mass parts, 100 parts of intermediate product 1, 300-500 parts of water, 2.4-4.6 parts of N-acryloxysuccinimide, 0.01-0.1 part of bisphenol A diallyl ether, 2-4 parts of ammonium persulfate and 1-4 parts of hydroxyethyl cellulose are uniformly mixed by controlling the temperature to be 80-95 ℃ and stirring for 2-5h, and then the mixture is filtered, washed and dried in vacuum at 60-80 ℃ for 3-5h to obtain the functional auxiliary agent.
The equation for its partial reaction is schematically:
Preferably, the step (3) comprises the following steps: 100-150oC/10-30min150-200oC/10-30min，200-250oC/10-30min，250-300oC/10-30min，300-350oC/10-30min。
The specification of the hollow glass bead is 800-2500 meshes.
Preferably, the obtained colorless transparent high-temperature resistant polyimide film is mainly used in the photoelectric fields of flexible solar substrates, optical half-wave plates in planar optical waveguide circuits, optical waveguide materials for communication connection, orientation films in liquid crystal displays, multilayer high-speed printed circuit boards, optical fiber communication, liquid crystal display and the like.
Compared with the prior art, the invention has the beneficial effects that: the thickness of the polyimide film obtained by the invention is 50-100 mu m, the cut-off wavelength is 270-360nm, the light transmittance at 450nm is 83-98%, and the vitrification temperature is 330-330 ℃ while the high light transmittance is maintainedoC, initial thermal decomposition temperature of 480-oAnd C, the obtained polyimide film has the heat resistance of aromatic polyimide and the high transparency of alicyclic polyimide, and has good application prospect in the photoelectric field.
Drawings
FIG. 1 is a Fourier infrared spectrum of a colorless, transparent, high temperature resistant polyimide film prepared in example 2:
at 1610/1502/1423/1375cm-1An absorption peak of benzene ring at 1039cm-1An absorption peak of a carbon-nitrogen single bond exists nearby, which indicates that benzidine participates in the reaction; at 1783/1726cm-1The telescopic absorption peak of the carbonyl of the amide exists nearby, which indicates that CBDA participates in the reaction; at 918cm-1An absorption peak of silicate exists nearby, which indicates that the hollow glass beads participate in the reaction; at 1091cm-1An antisymmetric telescopic absorption peak of an ester carbon-oxygen single bond exists nearby, which indicates that N-acryloyloxy succinimide participates in the reaction; at 716cm-1A stretching absorption peak of a silicon-carbon bond exists nearby, and the vinyl-dihydroxy-methylsilane participates in the reaction.
Detailed Description
The raw materials used in the following examples are all commercially available products, the parts are by weight, and the examples are further illustrative of the present invention and do not limit the scope of the present invention;
the performance test methods are as follows:
1. film thickness was measured by SEM;
2. the cut-off wavelength and the light transmittance at 450nm are tested by an ultraviolet-visible spectrophotometer;
3. the glass transition temperature was tested by DMA;
4. the initial thermal decomposition temperature was tested by TGA;
example 1
(1) 40kg of p-phenylenediamine is dissolved in N-methylpyrrolidone, 40kg of BOCA is added, and the temperature of the reaction solution is controlled to be 0oC, stirring and reacting at 200r/min for 7 hours to obtain polyamic acid solution;
(2) adding 5kg of functional additive into polyamic acid, uniformly dispersing, and carrying out vacuum-assisted ultrasonic defoaming on the solution;
(3) casting the defoamed solution on a steel belt filled with nitrogen atmosphere under the protection of nitrogen, wherein the thickness of a casting film is 100 mu m, and then 150oC/30min, 200oC/10min，250oC/30min，300oC/10min，350oAnd C/15min, and obtaining the colorless transparent high-temperature-resistant polyimide film after biaxial stretching.
The preparation method of the functional auxiliary agent comprises the following steps:
adding 100kg of hollow glass beads, 2.3kg of vinyl-dihydroxy-methylsilane and 0.3kg of acetic acid into 300kg of water, controlling the temperature to be 50 ℃, stirring for 1h, uniformly mixing, filtering, drying to obtain an intermediate product 1,
according to the mass kg, 100kg of intermediate product 1, 300kg of water, 5kg of N-acryloxysuccinimide, 0.01kg of bisphenol A diallyl ether, 2kg of ammonium persulfate and 1kg of hydroxyethyl cellulose are stirred for 2 hours at the temperature of 80 ℃ and uniformly mixed, filtered, washed and then dried for 3 hours in vacuum at the temperature of 60 ℃ to obtain the functional additive.
The specification of the hollow glass bead is 800 meshes.
The obtained polyimide film has a cut-off wavelength of 360nm, a light transmittance of 83% and a glass transition temperature of 300oC, initial decomposition temperature of 480oC。
Example 2
(1) 44kg of benzidine was dissolved in dimethylformamide, 44kg of CBDA was added, and the temperature of the reaction solution was controlled to 3.8oC, stirring and reacting for 6 hours at the speed of 200r/min to obtain a polyamic acid solution;
(2) adding 7kg of functional additive into polyamic acid, uniformly dispersing, and carrying out vacuum-assisted ultrasonic defoaming on the solution;
(3) casting the defoamed solution on a steel belt filled with nitrogen atmosphere under the protection of nitrogen, wherein the thickness of a casting film is 80 mu m, and then 100oC/30min，190oC/20min，210oC/10min，290oC/20min，340oAnd C/30min, and obtaining the colorless transparent high-temperature resistant polyimide film after biaxial stretching.
Adding 100kg of hollow glass beads, 3.5kg of vinyl-dihydroxy-methylsilane and 0.5kg of acetic acid into 350kg of water, controlling the temperature to 57 ℃, stirring for 2h, uniformly mixing, filtering, drying to obtain an intermediate product 1,
according to the mass kg, 100kg of intermediate product 1, 380kg of water, 7kg of N-acryloxysuccinimide, 0.03kg of bisphenol A diallyl ether, 2.3kg of ammonium persulfate and 1.5kg of hydroxyethyl cellulose are stirred for 3 hours at the temperature of 87 ℃ and uniformly mixed, filtered, washed and then dried for 3.5 hours in vacuum at the temperature of 65 ℃ to obtain the functional auxiliary agent.
The specification of the hollow glass bead is 1250 meshes.
The obtained polyimideThe cut-off wavelength of the imine film is 342nm, the light transmittance is 85 percent, and the glass transition temperature is 306oC, initial decomposition temperature of 488oC。
Example 3
(1) Dissolving 48kg of 4, 4' -diaminobenzophenone in dimethylacetamide, adding 48kg of CPDA, and controlling the temperature of the reaction solution to be 7 DEGoC, stirring and reacting at 200r/min for 5.8h to obtain a polyamic acid solution;
(2) adding 9kg of functional additive into polyamic acid, uniformly dispersing, and carrying out vacuum-assisted ultrasonic defoaming on the solution;
(3) casting the defoamed solution on a steel belt filled with nitrogen atmosphere under the protection of nitrogen, wherein the thickness of a casting film is 64 mu m, and then 100oC/30min，190oC/20min，210oC/10min，290oC/20min，340oAnd C/30min, and obtaining the colorless transparent high-temperature resistant polyimide film after biaxial stretching.
Adding 100kg of hollow glass beads, 6.3kg of vinyl-dihydroxy-methylsilane and 1.5kg of acetic acid into 500kg of water, controlling the temperature at 70 ℃, stirring for 5 hours, uniformly mixing, filtering, drying to obtain an intermediate product 1,
according to the mass kg, 100kg of intermediate product 1, 500kg of water, 12kg of N-acryloxysuccinimide, 0.1kg of bisphenol A diallyl ether, 4kg of ammonium persulfate and 4kg of hydroxyethyl cellulose are uniformly stirred and mixed at the temperature of 95 ℃ for 5 hours, filtered, washed and then dried in vacuum at the temperature of 80 ℃ for 5 hours to obtain the functional additive.
The specification of the hollow glass bead is 2500 meshes.
The obtained polyimide film had a cut-off wavelength of 324nm, a light transmittance of 89% and a glass transition temperature of 311oC, initial decomposition temperature of 495oC。
Example 4
(1) Dissolving 52kg of 4, 4' -diaminodiphenylsulfone in dimethylformamide, adding 52kg of CHDA, and controlling the temperature of the reaction solution to be 11oC, stirring and reacting for 5 hours at the speed of 200r/min to obtain a polyamic acid solution;
(2) adding 10.8kg of functional auxiliary agent into the polyamic acid, uniformly dispersing, and carrying out vacuum-assisted ultrasonic defoaming on the solution;
(3) casting the defoamed solution on a steel belt filled with nitrogen atmosphere under the protection of nitrogen, wherein the thickness of a casting film is 48 mu m, and then 108oC/28min，182oC/26min，202oC/18min，288oC/25min，346oAnd C/29min, and obtaining the colorless transparent high-temperature resistant polyimide film after biaxial stretching.
Adding 100kg of hollow glass beads, 2.3kg of vinyl-dihydroxy-methylsilane and 1.5kg of acetic acid into 300kg of water, controlling the temperature to be 50 ℃, stirring for 1h, uniformly mixing, filtering, drying to obtain an intermediate product 1,
according to the mass kg, 100kg of intermediate product 1, 500kg of water, 5kg of N-acryloxysuccinimide, 0.1kg of bisphenol A diallyl ether, 2kg of ammonium persulfate and 4kg of hydroxyethyl cellulose are uniformly stirred and mixed at the temperature of 80 ℃ for 5h, filtered, washed and then dried in vacuum at the temperature of 60 ℃ for 5h to obtain the functional additive.
The specification of the hollow glass bead is 800 meshes.
The obtained polyimide film had a cut-off wavelength of 306nm, a light transmittance of 92% and a glass transition temperature of 318oC, initial decomposition temperature of 504oC。
Example 5
(1) 60kg of 4, 4' -diaminodiphenyl ether was dissolved in N-methylpyrrolidone, 60kg of MCA was added, and the temperature of the reaction solution was controlled to 18 deg.CoC, stirring and reacting for 4 hours at 200r/min to obtain polyamic acid solution;
(2) adding 15kg of functional auxiliary agent into the polyamic acid, uniformly dispersing, and carrying out vacuum-assisted ultrasonic defoaming on the solution;
(3) casting the defoamed solution on a steel belt filled with nitrogen atmosphere under the protection of nitrogen, wherein the thickness of a casting film is 10 mu m, and then 123oC/25min，177oC/18min，234oC/20min，276oC/30min，330oAnd C/26min, and obtaining the colorless transparent high-temperature resistant polyimide film after biaxial stretching.
Adding 100kg of hollow glass beads, 6.3kg of vinyl-dihydroxy-methylsilane and 0.3kg of acetic acid into 500kg of water, controlling the temperature to be 50 ℃, stirring for 5 hours, uniformly mixing, filtering, drying to obtain an intermediate product 1,
according to the mass kg, 100kg of intermediate product 1, 300kg of water, 12kg of N-acryloxysuccinimide, 0.01kg of bisphenol A diallyl ether, 4kg of ammonium persulfate and 1kg of hydroxyethyl cellulose are stirred for 2 hours at the temperature of 95 ℃ and uniformly mixed, filtered, washed and then dried for 3 hours in vacuum at the temperature of 80 ℃ to obtain the functional additive.
The specification of the hollow glass bead is 1250 meshes.
The obtained polyimide film has a cut-off wavelength of 270nm, a light transmittance of 98% and a glass transition temperature of 330oC, initial decomposition temperature of 520oC。
Comparative example 1
Comparative example 1 differs from example 5 in that no functional aid was added, and the others were identical.
The obtained polyimide film had a cut-off wavelength of 310nm, a light transmittance of 93% and a glass transition temperature of 280oC, initial decomposition temperature of 450oC。
Comparative example 2
Comparative example 2 differs from example 5 in that the dianhydride added is the aromatic dianhydride BTDA, the others being identical.
The obtained polyimide film has a cut-off wavelength of 440nm, a light transmittance of 75% and a glass transition temperature of 333oC, initial decomposition temperature of 534oC。
Claims (8)
1. A colorless transparent high-temperature resistant polyimide film and a preparation method thereof are characterized by comprising the following steps:
(1) dissolving 40-60 parts of aromatic diamine in polar aprotic solvent, adding 40-60 parts of alicyclic dianhydride, and controlling the temperature of the reaction solution to be 0-18 DEGoC, stirring and reacting for 4-7h at 200r/min to obtain a polyamic acid solution;
(2) adding 5-15 parts of functional auxiliary agent into polyamic acid, uniformly dispersing, and carrying out vacuum-assisted ultrasonic defoaming on the solution;
(3) and under the protection of nitrogen, casting the defoamed solution onto a steel belt filled with nitrogen, heating in a sectional manner for imidization, wherein the thickness of the cast film is 10-100 mu m, and performing biaxial tension to obtain the colorless transparent high-temperature-resistant polyimide film.
2. The colorless transparent high temperature resistant polyimide film and the method for preparing the same as claimed in claim 1, wherein the aromatic diamine in step (1) is one or more selected from the group consisting of p-phenylenediamine, m-phenylenediamine, 4 ' -diaminodiphenylmethane, 4 ' -diaminodiphenyl ether, 4 ' -diaminobenzophenone, 4 ' -diaminodiphenylmethanesulphone, 1, 4-bis (4-aminophenoxy) benzene, 1, 3-bis (4 ' -aminophenoxy) benzene and benzidine.
3. The colorless transparent high temperature resistant polyimide film and the preparation method thereof according to claim 1, wherein the nonpolar protic solvent in step (1) is one or more of N-methyl pyrrolidone, dimethylformamide and dimethylacetamide.
4. The colorless transparent high temperature resistant polyimide film and the preparation method thereof as claimed in claim 1, wherein the aliphatic dianhydride in step (1) is one or more of BOCA, CBDA, CPDA, CHDA, TFPA, DMBD, TCPDA, DAA, DADA, MCA, and MMCA.
5. The colorless transparent high-temperature resistant polyimide film and the preparation method thereof according to claim 1, wherein the preparation method of the functional additive in the step (2) is as follows:
adding 100 parts of hollow glass microspheres, 2.3-6.3 parts of vinyl-dihydroxy-methylsilane and 0.3-1.5 parts of acetic acid into 500 parts of water by mass, controlling the temperature to be 50-70 ℃, stirring for 1-5h, uniformly mixing, filtering, drying to obtain an intermediate product 1,
according to the mass parts, 100 parts of intermediate product 1, 300-500 parts of water, 5-12 parts of N-acryloxysuccinimide, 0.01-0.1 part of bisphenol A diallyl ether, 2-4 parts of ammonium persulfate and 1-4 parts of hydroxyethyl cellulose are uniformly mixed by stirring at the temperature of 80-95 ℃ for 2-5h, filtered, washed and then dried in vacuum at the temperature of 60-80 ℃ for 3-5h, thus obtaining the functional auxiliary agent.
6. The colorless transparent high temperature resistant polyimide film and the preparation method thereof according to claim 1, wherein the step (3) comprises the following steps: 100-150oC/10-30min,150-200oC/10-30min，200-250oC/10-30min，250-300oC/10-30min，300-350oC/10-30min。
7. The colorless transparent high temperature resistant polyimide film and the preparation method thereof according to claim 1, wherein the obtained colorless transparent high temperature resistant polyimide film is mainly used in the photoelectric fields of flexible solar substrates, optical half-wave plates in planar optical waveguide circuits, optical waveguide materials for communication connection, orientation films in liquid crystal displays, multilayer high-speed printed circuit boards, optical fiber communication, liquid crystal display and the like.
8. The colorless transparent high temperature resistant polyimide film as claimed in claim 5, wherein the specification of the hollow glass beads is 800-2500 meshes.
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| CN113667119A (en) * | 2021-04-16 | 2021-11-19 | 江西师范大学 | Polyacetamido imide film and preparation method thereof |
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| CN113667119A (en) * | 2021-04-16 | 2021-11-19 | 江西师范大学 | Polyacetamido imide film and preparation method thereof |
| CN113667119B (en) * | 2021-04-16 | 2023-08-04 | 江西师范大学 | Polyacetamide-imide film and preparation method thereof |
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Application publication date: 20201027 |