CN108424540A - A kind of transparent polyimide film and preparation method thereof - Google Patents

A kind of transparent polyimide film and preparation method thereof Download PDF

Info

Publication number
CN108424540A
CN108424540A CN201810397632.4A CN201810397632A CN108424540A CN 108424540 A CN108424540 A CN 108424540A CN 201810397632 A CN201810397632 A CN 201810397632A CN 108424540 A CN108424540 A CN 108424540A
Authority
CN
China
Prior art keywords
polyimide film
transparent polyimide
preparation
acid anhydrides
transparent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201810397632.4A
Other languages
Chinese (zh)
Other versions
CN108424540B (en
Inventor
路庆华
徐文华
苏远海
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tongji University
Original Assignee
Tongji University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tongji University filed Critical Tongji University
Priority to CN201810397632.4A priority Critical patent/CN108424540B/en
Publication of CN108424540A publication Critical patent/CN108424540A/en
Application granted granted Critical
Publication of CN108424540B publication Critical patent/CN108424540B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003Preparatory processes
    • C08G73/1007Preparatory processes from tetracarboxylic acids or derivatives and diamines
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1039Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1042Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1046Polyimides containing oxygen in the form of ether bonds in the main chain
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1046Polyimides containing oxygen in the form of ether bonds in the main chain
    • C08G73/105Polyimides containing oxygen in the form of ether bonds in the main chain with oxygen only in the diamino moiety
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1075Partially aromatic polyimides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00Characterised by the use of 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 C08J2361/00 - C08J2377/00
    • C08J2379/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors

Abstract

The invention discloses a kind of preparation methods of transparent polyimide film, have steps of:1. fluorinated diamine is added in nitrogen or the polar non-solute of inert gas shielding, at 10 50 DEG C, after stirring makes it completely dissolved, the aliphatic anhydride of copolymerization acid anhydrides and certain molar fraction is added, the molar ratio for controlling diamines and acid anhydrides is 1:1 1.02, it reacts 6 24 hours, obtains transparent polyamic acid solution;2. 1. polyamic acid solution that step is obtained is with predetermined thickness even application on clean substrate, it is subsequently placed in vacuum drying oven and carries out temperature programming to certain temperature removing solvent and carry out hot imidization, after vacuum drying oven temperature is down to environment temperature, take out glass plate, demoulding, it is dry, obtain transparent polyimide film.Transparent polyimide film produced by the present invention has high transparency, superior heat-stability and good mechanical property.

Description

A kind of transparent polyimide film and preparation method thereof
Technical field
The present invention relates to thin polymer film field, a kind of transparent polyimide film and preparation method thereof is specifically disclosed.
Background technology
Polyimides (PI) is navigating because it has remarkable hot property, mechanical property, electrical property and excellent comprehensive performance The industries such as sky, space flight, automobile, machinery are widely applied.However, because its deeper color and poor light transmittance seriously limit Its application in microelectronics and optoelectronic areas is made.Traditional Kapton is in brown color, to visible light (wavelength 400-700nm) light transmittance is relatively low, and to the visible light of 500nm, light transmittance is less than 40%;Wavelength is the visible light quilt of 400nm 100% absorbs, and seriously limits its application in photoelectric field.The color of polyimides is mainly due to aromatic polyimide point Between son and caused by the formation of Intramolecular charge transfer complex, wherein dianhydride is electron acceptor, and diamines is electron donor.
Clear polyimides greatly facilitate its commercialization process in the application potential of flexible optoelectronic part;Optical thin film In Flexible light-emitting diodes, flexible solar battery or photovoltaic cell, flexible thin-film transistor, flexible printed circuit board etc. is in many ways The application in face, to the performance of polyimides, more stringent requirements are proposed;Especially its excellent comprehensive performance is many existing quotient Not available for product material.In order to meet these requirements, organic polymer chemistry and field of chemical engineering have been developed and have been commercialized Many kinds of different types of polyimides, are further improved its performance.
Currently, preparing transparent polyimides common method has:1) introducing fluoro-containing group, 2) introduce the larger substitution of volume Base, 3) dissymmetrical structure introduce fat especially alicyclic structure unit, 4) using the monomer that can make backbone twist, 5) is imported, 6) Reduce conjugated double bond structures etc..Wherein, fluorine atom is introduced into polyimides main chain or branch so that it is negative with high electricity Property, big free volume;The lower polarizability of C-F keys simultaneously, can improve the optical transparence of polyimides, while it is molten to improve its Solution property and reduction dielectric constant.Aliphatic polyimide then has the excellent transparency, mainly drawing due to aliphatic monomer Enter, be based on its low molecule density and low polarity, electric charge transfer interaction can be effectively inhibited.Present invention incorporates fluorine-containing polyamides The comprehensive advantage of imines and aliphatic polyimide provides a kind of transparent polyimide film and preparation method thereof.
Invention content
This is provided a kind of transparent it is an object of the invention to obtain a kind of transparent polyimide film of excellent combination property Kapton and preparation method thereof.
Realizing the technical solution of the object of the invention is:
In the first aspect, the application provides a kind of preparation method of transparent polyimide film, it is characterised in that has Following steps:1. fluorinated diamine is added in nitrogen or the polar non-solute of inert gas shielding, at 10~50 DEG C, stir It mixes after making it completely dissolved, the aliphatic anhydride of copolymerization acid anhydrides and certain molar fraction is added, control mole of diamines and acid anhydrides Than being 1:1~1.02, it reacts 6-24 hours, obtains transparent polyamic acid solution;
2. 1. polyamic acid solution that step is obtained on clean substrate, is subsequently placed in predetermined thickness even application Temperature programming to certain temperature is carried out in vacuum drying oven to remove solvent and carry out hot imidization, waits for that vacuum drying oven temperature is down to environment After temperature, substrate is taken out, is demoulded, it is dry, obtain transparent polyimide film.
In a kind of embodiment of first aspect, step 1. described in fluorinated diamine be:Bis- (the fluoroforms of 2,2'- Base) -4,4'- diamino-phenyl ethers, one or more of 2,2'- bis- (trifluoromethyl) -4,4'- benzidines.
In a kind of embodiment of first aspect, step 1. described in copolymerization acid anhydrides be:The equal benzene tetramethyls of 1,2,4,5- Acid dianhydride, 3,3 ', 4,4 '-benzophenone tetracid dianhydrides, 4,4 '-biphenyl ether dianhydrides, 3,3,4,4- biphenyl dianhydrides, 4,4- hexafluoro isopropyls One or more of base phthalic anhydride.
In a kind of embodiment of first aspect, step 1. described in certain molar fraction be 0%~100%.
In a kind of embodiment of first aspect, step 1. described in aliphatic anhydride be with one kind of lower structure:
In a kind of embodiment of first aspect, step 2. described in certain temperature be:270℃.
In a kind of embodiment of first aspect, the substrate includes glass plate.
In second aspect, it is thin that the application provides a kind of clear polyimides prepared by the method by described in first aspect Film.
Compared with prior art, the present invention gained transparent polyimide film, thickness range at 50 μm or so, 500nm ultraviolet permeabilities are up to 90%, 400nm ultraviolet permeabilities and reach 75% or more, and ultraviolet cut-on wavelength reaches 312nm, lose 5% temperature is weighed at 430 DEG C or more, and excellent in mechanical performance.
Description of the drawings
Fig. 1 is that embodiment prepares the transparent polyamide acid solution of different copolymer acid anhydrides and its corresponding transparent polyimide film Optical photograph figure, wherein being yellow using transparent polyimide film prepared by PMDA;
Fig. 2 is the transparent polyimide film infrared spectrum for the aliphatic anhydride that embodiment prepares different molar fractions;
Fig. 3 is the transparent polyimide film ultraviolet-visible spectrogram that embodiment prepares different copolymer acid anhydrides;
Fig. 4 is the transparent polyimide film UV, visible light that embodiment prepares the aliphatic anhydride with different molar fractions Spectrogram;
Fig. 5 is the transparent polyimide film thermogravimetric curve for the aliphatic anhydride that embodiment prepares different molar fractions Figure.
Number and embodiment correspondence in attached drawing is as follows:PI-6FDA-50 indicates that copolymerization acid anhydrides is 6FDA, aliphatic Acid anhydrides is 50%, is embodiment 1;PI-PMDA-50 indicates that copolymerization acid anhydrides is PMDA, and aliphatic anhydride 50% is embodiment 3; PI-BTDA-50 indicates that copolymerization acid anhydrides is BTDA, and aliphatic anhydride 50% is embodiment 4;PI-BPDA-50 indicates co-polymeric acids Acid anhydride is BPDA, and aliphatic anhydride mass fraction is 50%, is embodiment 5;PI-ODPA-50 indicates that copolymerization acid anhydrides is ODPA, fat Race's acid anhydrides mass fraction is 50%, is embodiment 6;PI-6FDA-70 indicates that copolymerization acid anhydrides is 6FDA, aliphatic anhydride quality point Number is 70%, is embodiment 7;PI-6FDA-90 indicates that copolymerization acid anhydrides is 6FDA, and aliphatic anhydride mass fraction is 90%, is real Apply example 8;PI-6FDA-100 indicates that copolymerization acid anhydrides is 6FDA, and aliphatic anhydride mass fraction is 100%, is embodiment 9;PI- 6FDA-30 indicates that copolymerization acid anhydrides is 6FDA, and aliphatic anhydride mass fraction is 30%, is embodiment 10;PI-6FDA-10 is indicated Copolymerization acid anhydrides is 6FDA, and aliphatic anhydride mass fraction is 10%, is embodiment 11;PI-6FDA-0 indicates that copolymerization acid anhydrides is 6FDA, aliphatic anhydride mass fraction are 0%, are embodiment 12.
Specific implementation mode
Embodiment 1
The preparation of transparent polyimide film is accomplished by the following way in this example:
One, bis- (the trifluoromethyl) -4,4'- diamino-phenyl ethers of 21.62g fluorinated diamines 2,2'- are added to nitrogen or lazy Property gas shield 238.83g polar non-solutes (n,N-dimethylacetamide) in, at 10-30 DEG C, stirring keep its complete After fully dissolved, the molar ratio for controlling diamines and acid anhydrides is 1:Copolymerization acid anhydrides 4,4- hexafluoro isopropyl O-phthalics is added in 1-1.02 The cyclobutanetetracarboxylic dianhydride that acid anhydrides and aliphatic anhydride molar fraction are 50%, reacts 24 hours, obtains transparent polyamide Acid solution.Herein, aliphatic anhydride molar fraction refers to aliphatic molal quantity polyanhydride molal quantity and aliphatic anhydride together The ratio of the sum of molal quantity.
Two, the polyamic acid solution even application for obtaining step 1 is subsequently placed in vacuum baking on clean glass plate Progress temperature programming removes solvents to 270 DEG C and carries out hot imidization and taken after vacuum drying oven temperature is down to environment temperature in case Go out glass plate, demoulds, it is dry, obtain transparent polyimide film.
Embodiment 2
Fluorinated diamine described in step 1 is 2,2'- bis trifluoromethyl -4,4'- benzidines.Other and embodiment 1 It is identical, its role is to:Transparent polyimide film reduction of pliability, mechanical property is more preferably.
Embodiment 3
Copolymerization acid anhydrides described in step 1 is 1,2,4,5- pyromellitic acid anhydrides.It is other same as Example 1, make With being:It is different to be copolymerized acid anhydrides, transparent polyimide film transparency is different.
Embodiment 4
Copolymerization acid anhydrides described in step 1 is 3,3 ', 4,4 '-benzophenone tetracid dianhydrides.It is other same as Example 1, Effect is:It is different to be copolymerized acid anhydrides, transparent polyimide film transparency is different.
Embodiment 5
Copolymerization acid anhydrides described in step 1 is 3,3,4,4- biphenyl dianhydrides.It is other same as Example 1, it acts on In:It is different to be copolymerized acid anhydrides, transparent polyimide film transparency is different.
Embodiment 6
Copolymerization acid anhydrides described in step 1 is 4,4 '-biphenyl ether dianhydrides.It is other same as Example 1, its role is to: It is different to be copolymerized acid anhydrides, transparent polyimide film transparency is different.
Embodiment 7
Aliphatic anhydride molar fraction described in step 1 is 70%.It is other same as Example 1, its role is to: Aliphatic anhydride molar fraction increases, and transparent polyimide film transparency improves.
Embodiment 8
Aliphatic anhydride molar fraction described in step 1 is 90%.It is other same as Example 1, its role is to: Aliphatic anhydride molar fraction increases, and transparent polyimide film transparency improves.
Embodiment 9
Aliphatic anhydride molar fraction described in step 1 is 100%.It is other same as Example 1, its role is to: Aliphatic anhydride molar fraction increases, and transparent polyimide film transparency improves.
Embodiment 10
Aliphatic anhydride molar fraction described in step 1 is 30%.It is other identical as specific real mode, it acts on In:Aliphatic anhydride molar fraction is reduced, and transparent polyimide film transparency reduces.
Embodiment 11
Aliphatic anhydride molar fraction described in step 1 is 10%.It is other same as Example 1, its role is to: Aliphatic anhydride molar fraction is reduced, and transparent polyimide film transparency reduces.
Embodiment 12
Aliphatic anhydride molar fraction described in step 1 is 0%.It is other same as Example 1, its role is to:Fat Fat race acid anhydrides molar fraction is reduced, and transparent polyimide film transparency reduces.
Embodiment 13
Aliphatic anhydride described in step 1 is:
It is other same as Example 1, its role is to:Aliphatic anhydride is that dimethyl replaces cyclobutanetetracarboxylic dianhydride, Transparent polyimide film transparency reduces.
Comparative example 14
Temperature programming described in step 1 is to 300 DEG C.It is other same as Example 1, its role is to:Imidization temperature It increases, transparent polyimide film transparency reduces.
Prepared by this experiment, with different copolymer acid anhydrides transparent polyamide acid solution and transparent polyimide film are made Optical photograph.Polyamic acid solution with different copolymer acid anhydrides almost, when the transparent polyimide film of different copolymer acid anhydrides Copolymerization acid anhydrides be 3,3,4,4- biphenyl dianhydrides and 4, when 4- hexafluoro isopropyl phthalic anhydrides, the optical photograph of film is shown Its is nearly transparent, and the Kapton of other copolymerization acid anhydrides is light yellow.
The transparent polyimide film of prepared by this experiment, with different molar fractions aliphatic anhydrides makees infrared light Spectrum test.As shown in Fig. 2, 1781,1713cm-1It is imide ring C=O stretching vibration peaks, 1373cm-1It is that imide ring C-N is flexible to shake Dynamic peak, 1248cm-1It is C-O stretching vibration peaks, this shows that polyimides is successfully prepared.
Prepared by this experiment, transparent polyimide film with different copolymer acid anhydrides is made ultraviolet-visible spectrogram and is surveyed Examination.As shown in figure 3, as copolymerization acid anhydrides is different, the transparent polyimide film transparency is different;When aliphatic anhydride content is When 50%, PI-PMDA-50 is followed successively by 400nm ultraviolet transmissions<PI-BTDA-50<PI-BPDA-50<PI-ODPA-50< PI-6FDA-50。
Prepared by this experiment, aliphatic anhydrides with different molar fractions transparent polyimide films make it is ultraviolet can See spectrum test.As shown in figure 4, with the continuous improvement of molar fraction, the transparent polyimide film transparency is continuously improved, purple Outer cutoff wavelength is up to 310nm, and 400nm ultraviolet transmissions reach 75% or more, 500nm ultraviolet permeabilities and are up to 90%, transparent It has excellent performance.
The present embodiment transparent polyimide film is made into thermogravimetic analysis (TGA) test.As shown in figure 5, in nitrogen atmosphere, 5% Weightless temperature is at 433-522 DEG C, and 10% weightless temperature is at 460-547 DEG C, and 800 DEG C of Residual carbon is up to 45-50%, and hot property is excellent It is different.
The above-mentioned description to embodiment is that this Shen can be understood and applied for the ease of those skilled in the art Please.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein General Principle is applied in other embodiments without paying performing creative labour.Therefore, the application is not limited to implementation here Example, those skilled in the art make according to herein disclosed content in the case where not departing from the application scope and spirit It improves and changes within all scope of the present application.

Claims (8)

1. a kind of preparation method of transparent polyimide film, it is characterised in that have steps of:
1. fluorinated diamine is added in nitrogen or the polar non-solute of other inert gas shieldings, at 10-50 DEG C, stir It mixes after making it completely dissolved, the aliphatic anhydride of copolymerization acid anhydrides and certain molar fraction is added, control mole of diamines and acid anhydrides Than being 1:1-1.02 reacts 6-24 hours, obtains transparent polyamic acid solution;
2. 1. polyamic acid solution that step is obtained on clean substrate, is subsequently placed in vacuum with predetermined thickness even application Temperature programming to certain temperature is carried out in baking oven to remove solvent and carry out hot imidization, waits for that vacuum drying oven temperature is down to environment temperature Afterwards, substrate is taken out, is demoulded, it is dry, obtain transparent polyimide film.
2. the preparation method of transparent polyimide film according to claim 1, it is characterised in that:Step 1. described in Fluorinated diamine is:2,2'- bis- (trifluoromethyl) -4,4'- diamino-phenyl ethers, 2,2'- bis- (trifluoromethyl) -4,4'- diamino One or more of biphenyl.
3. the preparation method of transparent polyimide film according to claim 1, it is characterised in that:Step 1. described in Being copolymerized acid anhydrides is:1,2,4,5- pyromellitic acid anhydrides, 3,3 ', 4,4 '-benzophenone tetracid dianhydrides, 4,4 '-biphenyl ether dianhydrides, 3, 3,4,4- biphenyl dianhydrides, one or more of 4,4- hexafluoro isopropyl phthalic anhydrides.
4. the preparation method of transparent polyimide film according to claim 1, it is characterised in that:Step 1. described in Certain molar fraction is 0%-100%.
5. the preparation method of transparent polyimide film according to claim 1, it is characterised in that:Step 1. described in Aliphatic anhydride is with one kind of lower structure:
6. the preparation method of transparent polyimide film according to claim 1, it is characterised in that:Step 2. described in Certain temperature is:270℃.
7. the preparation method of transparent polyimide film according to claim 1, which is characterized in that the substrate includes Glass plate.
8. prepared by a kind of preparation method by the transparent polyimide film as described in any one of claim 1-7 Transparent polyimide film.
CN201810397632.4A 2018-04-28 2018-04-28 Colorless transparent polyimide film and preparation method thereof Active CN108424540B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810397632.4A CN108424540B (en) 2018-04-28 2018-04-28 Colorless transparent polyimide film and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810397632.4A CN108424540B (en) 2018-04-28 2018-04-28 Colorless transparent polyimide film and preparation method thereof

Publications (2)

Publication Number Publication Date
CN108424540A true CN108424540A (en) 2018-08-21
CN108424540B CN108424540B (en) 2020-08-04

Family

ID=63162045

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810397632.4A Active CN108424540B (en) 2018-04-28 2018-04-28 Colorless transparent polyimide film and preparation method thereof

Country Status (1)

Country Link
CN (1) CN108424540B (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110951077A (en) * 2019-11-14 2020-04-03 安徽国风塑业股份有限公司 Transparent polyimide precursor and preparation method thereof
CN112062988A (en) * 2020-08-06 2020-12-11 深圳丹邦科技股份有限公司 White polyimide optical film and preparation method thereof
CN112062960A (en) * 2020-09-10 2020-12-11 武汉华星光电半导体显示技术有限公司 Polyimide, polyimide film, preparation method of polyimide film and display device
CN112500803A (en) * 2020-04-21 2021-03-16 中天电子材料有限公司 Polyimide adhesive film and preparation method and application thereof
CN112831182A (en) * 2020-12-31 2021-05-25 宁波长阳科技股份有限公司 Colorless transparent polyimide film, preparation method thereof and LED (light-emitting diode) film pasting screen
CN113260658A (en) * 2018-12-28 2021-08-13 株式会社斗山 Polyamic acid composition and transparent polyimide film using same
CN114573811A (en) * 2021-12-29 2022-06-03 宁波博雅聚力新材料科技有限公司 Imide slurry, synthesis method thereof and composition containing imide slurry

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105646919A (en) * 2008-09-26 2016-06-08 可隆工业株式会社 Polyimide film

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105646919A (en) * 2008-09-26 2016-06-08 可隆工业株式会社 Polyimide film

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PARK J W , KIM Y , LIM H , ET AL.: ""Polyimide as a Plastic Substrate for the Flexible Organic Electroluminescent Device"", 《MRS PROCEEDINGS》 *
Y. H. LU ET AL.: ""Synthesis and Properties of Fluorinated Polyimide Films Based on 1,2,3,4-Cyclobutanetetracarboxylic Dianhydride"", 《ADVANCED MATERIALS RESEARCH》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113260658A (en) * 2018-12-28 2021-08-13 株式会社斗山 Polyamic acid composition and transparent polyimide film using same
CN110951077A (en) * 2019-11-14 2020-04-03 安徽国风塑业股份有限公司 Transparent polyimide precursor and preparation method thereof
CN112500803A (en) * 2020-04-21 2021-03-16 中天电子材料有限公司 Polyimide adhesive film and preparation method and application thereof
CN112062988A (en) * 2020-08-06 2020-12-11 深圳丹邦科技股份有限公司 White polyimide optical film and preparation method thereof
CN112062960A (en) * 2020-09-10 2020-12-11 武汉华星光电半导体显示技术有限公司 Polyimide, polyimide film, preparation method of polyimide film and display device
CN112831182A (en) * 2020-12-31 2021-05-25 宁波长阳科技股份有限公司 Colorless transparent polyimide film, preparation method thereof and LED (light-emitting diode) film pasting screen
CN114573811A (en) * 2021-12-29 2022-06-03 宁波博雅聚力新材料科技有限公司 Imide slurry, synthesis method thereof and composition containing imide slurry
CN114573811B (en) * 2021-12-29 2023-12-22 宁波博雅聚力新材料科技有限公司 Imide slurry, synthesis method thereof and composition containing imide slurry

Also Published As

Publication number Publication date
CN108424540B (en) 2020-08-04

Similar Documents

Publication Publication Date Title
CN108424540A (en) A kind of transparent polyimide film and preparation method thereof
CN107698759B (en) Polyimide, polyamic acid solution, and polyimide film
CN104718239B (en) For manufacturing display, optics or the aromatic polyamide of illumination component
CN105637016A (en) Polyimide-based solution and polyimide-based film prepared by using same
CN106928481A (en) The optimization preparation method of Kapton
CN108822296B (en) Wholly aromatic colorless transparent polyimide film and preparation method thereof
CN103435827B (en) A kind of preparation method of space hyperbranched polyorganosiloxane polyimide transparent hybrid film
JP2014132057A (en) Polyimide porous film and its use
CN108794748B (en) Polyimide film with low dielectric constant and preparation method thereof
CN112175184A (en) Modified high-transparency polyimide flexible film and preparation method thereof
CN106893125A (en) A kind of polyimide film and preparation method thereof
CN109251334A (en) A kind of high light transmission and low dielectric fluorinated graphene/polyimide composite film preparation method
CN111704735A (en) Ultralow-thermal-expansion-coefficient high-strength polyimide optical film material and preparation method thereof
CN111073282B (en) Solvent-resistant colorless transparent cross-linked polyimide film and preparation method thereof
CN104558605A (en) Transparent polyimide film and preparation method thereof
CN115803365A (en) Polyamic acid, polyamic acid solution, polyimide film, laminate, method for producing laminate, and electronic device
CN102675665B (en) Colorless transparent polyimide film preparation method
EP0621888A1 (en) Laminate on the basis of a strengthened polyimide film containing organometallic compounds for improving adhesion
CN109251333A (en) A kind of preparation method of high transparency and low dielectric Kapton
CN110183851A (en) A kind of fluorine-containing alicyclic c-polymer polyimide film material and preparation method thereof
CN110467728B (en) Transparent polyimide film and preparation method and application thereof
CN110372899B (en) High-hydrophobicity colorless transparent heat-resistant polyimide film and preparation method thereof
CN111073283B (en) Cross-linked polyimide film, optical film and preparation method thereof
CN111040156B (en) Solvent-resistant and high-dimensional-stability cross-linked polyimide film
CN109054018B (en) Polyamide acid solution and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant