CN112759775B - Continuous transparent polyimide film manufacturing method for display - Google Patents
Continuous transparent polyimide film manufacturing method for display Download PDFInfo
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- CN112759775B CN112759775B CN201911014187.XA CN201911014187A CN112759775B CN 112759775 B CN112759775 B CN 112759775B CN 201911014187 A CN201911014187 A CN 201911014187A CN 112759775 B CN112759775 B CN 112759775B
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 141
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000004642 Polyimide Substances 0.000 claims abstract description 50
- 239000002243 precursor Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 13
- 230000003287 optical effect Effects 0.000 claims abstract description 7
- 230000009477 glass transition Effects 0.000 claims abstract description 6
- 238000002834 transmittance Methods 0.000 claims abstract description 5
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 10
- 238000010924 continuous production Methods 0.000 claims description 10
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 claims description 8
- -1 4-aminophenoxy Chemical group 0.000 claims description 5
- 150000004985 diamines Chemical class 0.000 claims description 5
- 229920005575 poly(amic acid) Polymers 0.000 claims description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 4
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 2
- 238000004378 air conditioning Methods 0.000 claims description 2
- JGVWEAITTSGNGJ-UHFFFAOYSA-N bicyclo[2.2.1]heptane;n-methylmethanamine Chemical compound CNC.C1CC2CCC1C2 JGVWEAITTSGNGJ-UHFFFAOYSA-N 0.000 claims description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 21
- 239000000203 mixture Substances 0.000 description 18
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 16
- ITQTTZVARXURQS-UHFFFAOYSA-N 3-methylpyridine Chemical compound CC1=CC=CN=C1 ITQTTZVARXURQS-UHFFFAOYSA-N 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 2
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 description 2
- 229940018564 m-phenylenediamine Drugs 0.000 description 2
- HDGLPTVARHLGMV-UHFFFAOYSA-N 2-amino-4-(1,1,1,3,3,3-hexafluoropropan-2-yl)phenol Chemical compound NC1=CC(C(C(F)(F)F)C(F)(F)F)=CC=C1O HDGLPTVARHLGMV-UHFFFAOYSA-N 0.000 description 1
- VIUDTWATMPPKEL-UHFFFAOYSA-N 3-(trifluoromethyl)aniline Chemical compound NC1=CC=CC(C(F)(F)F)=C1 VIUDTWATMPPKEL-UHFFFAOYSA-N 0.000 description 1
- DKKYOQYISDAQER-UHFFFAOYSA-N 3-[3-(3-aminophenoxy)phenoxy]aniline Chemical compound NC1=CC=CC(OC=2C=C(OC=3C=C(N)C=CC=3)C=CC=2)=C1 DKKYOQYISDAQER-UHFFFAOYSA-N 0.000 description 1
- LJMPOXUWPWEILS-UHFFFAOYSA-N 3a,4,4a,7a,8,8a-hexahydrofuro[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1C2C(=O)OC(=O)C2CC2C(=O)OC(=O)C21 LJMPOXUWPWEILS-UHFFFAOYSA-N 0.000 description 1
- XTEBLARUAVEBRF-UHFFFAOYSA-N 4-(1,1,1,3,3,3-hexafluoropropan-2-yl)aniline Chemical compound NC1=CC=C(C(C(F)(F)F)C(F)(F)F)C=C1 XTEBLARUAVEBRF-UHFFFAOYSA-N 0.000 description 1
- JPZRPCNEISCANI-UHFFFAOYSA-N 4-(4-aminophenyl)-3-(trifluoromethyl)aniline Chemical group C1=CC(N)=CC=C1C1=CC=C(N)C=C1C(F)(F)F JPZRPCNEISCANI-UHFFFAOYSA-N 0.000 description 1
- NVKGJHAQGWCWDI-UHFFFAOYSA-N 4-[4-amino-2-(trifluoromethyl)phenyl]-3-(trifluoromethyl)aniline Chemical compound FC(F)(F)C1=CC(N)=CC=C1C1=CC=C(N)C=C1C(F)(F)F NVKGJHAQGWCWDI-UHFFFAOYSA-N 0.000 description 1
- KIFDSGGWDIVQGN-UHFFFAOYSA-N 4-[9-(4-aminophenyl)fluoren-9-yl]aniline Chemical compound C1=CC(N)=CC=C1C1(C=2C=CC(N)=CC=2)C2=CC=CC=C2C2=CC=CC=C21 KIFDSGGWDIVQGN-UHFFFAOYSA-N 0.000 description 1
- CQMIJLIXKMKFQW-UHFFFAOYSA-N 4-phenylbenzene-1,2,3,5-tetracarboxylic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(=O)O)=CC(C(O)=O)=C1C1=CC=CC=C1 CQMIJLIXKMKFQW-UHFFFAOYSA-N 0.000 description 1
- YGYCECQIOXZODZ-UHFFFAOYSA-N 4415-87-6 Chemical compound O=C1OC(=O)C2C1C1C(=O)OC(=O)C12 YGYCECQIOXZODZ-UHFFFAOYSA-N 0.000 description 1
- 239000004262 Ethyl gallate Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- WKDNYTOXBCRNPV-UHFFFAOYSA-N bpda Chemical compound C1=C2C(=O)OC(=O)C2=CC(C=2C=C3C(=O)OC(C3=CC=2)=O)=C1 WKDNYTOXBCRNPV-UHFFFAOYSA-N 0.000 description 1
- MGNZXYYWBUKAII-UHFFFAOYSA-N cyclohexa-1,3-diene Chemical compound C1CC=CC=C1 MGNZXYYWBUKAII-UHFFFAOYSA-N 0.000 description 1
- UKJLNMAFNRKWGR-UHFFFAOYSA-N cyclohexatrienamine Chemical group NC1=CC=C=C[CH]1 UKJLNMAFNRKWGR-UHFFFAOYSA-N 0.000 description 1
- 125000006159 dianhydride group Chemical group 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- OAXARSVKYJPDPA-UHFFFAOYSA-N tert-butyl 4-prop-2-ynylpiperazine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCN(CC#C)CC1 OAXARSVKYJPDPA-UHFFFAOYSA-N 0.000 description 1
- 125000006158 tetracarboxylic acid group Chemical group 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised 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
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention is a method for manufacturing a continuous transparent polyimide film for a display, comprising the steps of providing a roll-to-roll polyimide film; providing a polyimide precursor, and coating the polyimide precursor on the polyimide film; and baking the polyimide precursor, wherein the baking temperature is at least 20 degrees higher than the glass transition temperature of the transparent polyimide film, so that the transparent polyimide film has optical transmittance of more than 85 percent, chromaticity (b) of less than 2, and the standard deviation of the three-axial refractive index of the transparent polyimide film is less than 0.0012, thereby obtaining the transparent polyimide film with low light leakage.
Description
[ field of technology ]
The present invention relates to a method for manufacturing a continuous transparent polyimide film for a display, and more particularly, to a method for manufacturing a continuous transparent polyimide film with a low refractive index standard deviation in a triaxial direction.
[ background Art ]
Polyimide films have excellent heat resistance and mechanical properties, and are therefore often used in flexible circuit board applications with high temperature processes. In addition, since a transparent polyimide film has excellent bending resistance and optical characteristics, in recent years, in the field of displays for electronic display, polyimide films are a few materials that meet the above requirements for optical characteristics and heat resistance.
Referring to fig. 1, a schematic diagram of a conventional transparent polyimide film for a touch pad of a display is shown, wherein the transparent polyimide film 10 is disposed between a polarizer 12 and a light source 14, and the transparent polyimide film 10 is made in a discontinuous manner, and has a small standard deviation of three-axis refractive index, which can achieve low light leakage, but has low manufacturing speed and high cost. However, if the transparent polyimide film is produced in a continuous manner, the difference between the refractive indexes of the film surface in the x-axis direction and the y-axis direction will be too large due to the factors of the biaxial stretching process, and light leakage will be caused when the transparent polyimide film is applied to a touch panel of a display.
[ invention ]
The invention is a continuous transparent polyimide film manufacturing method for a display, which comprises the following steps; providing a polyimide film which is arranged on a continuous process; providing a transparent polyimide precursor, which is coated on the polyimide film; and baking the transparent polyimide precursor at a temperature at least 20 DEG higher than the glass transition temperature of the transparent polyimide film to form a transparent polyimide film having an optical transmittance of more than 85% and a chromaticity (b) of less than 2, and three axial refractive indices (n) x 、n y 、n z ) The standard deviation is less than 0.00120.
Therefore, the technical scheme provided by the invention can improve the production speed of the transparent polyimide film so as to reduce the cost, and the obtained product has small triaxial refractive index standard deviation and lower light leakage.
[ description of the drawings ]
Fig. 1 is a schematic diagram of a conventional transparent polyimide film for a touch pad of a display.
Fig. 2 is a schematic diagram of a method for manufacturing a continuous transparent polyimide film for a display according to the present invention.
FIG. 3 is a transparent polyimide film made in accordance with the present invention.
Fig. 4 is a flowchart of a method of manufacturing a continuous transparent polyimide film for a display according to the present invention.
In fig. 1 to 4, each symbol is described as follows:
polyimide film 20
Transparent polyimide precursor 22
Transparent polyimide film 24
Providing a continuous polyimide film S1
Providing a transparent polyimide precursor S2
S3, coating a transparent polyimide precursor on the continuous polyimide film
Baking the transparent polyimide precursor to form a film, wherein the baking temperature is more than 20 ℃ higher than the glass transition temperature of the transparent polyimide film S4
Removing the polyimide film to obtain a transparent polyimide film S5
[ detailed description ] of the invention
The invention is a method for manufacturing a continuous transparent polyimide film for a display, comprising the steps of;
providing a polyimide film 20 of a continuous process (S1); a transparent polyimide precursor 22 (S2) is provided, which is coated on the polyimide film 20 (S3), and the polyimide precursor 22 may be a polyamic acid solution or a polyimide solution. A kind of electronic device with high-pressure air-conditioning system
The polyimide precursor 22 is baked (S4), the baking temperature is 20 degrees or more higher than the glass transition temperature of the transparent polyimide film 24, the polyimide film 20 is removed (S5) after the transparent polyimide film 24 is formed, so as to obtain the transparent polyimide film 24 with optical transmittance of more than 85% and chromaticity (b) of less than 2, the standard deviation of the three-axial refractive index of the transparent polyimide film 24 is less than 0.00120, and the light leakage performance can be low.
Because the transparent polyimide precursor 22 is coated on the polyimide film 20 and is not affected by biaxial extension when baked into the transparent polyimide 24, the difference of refractive indexes in the x-axis direction and the y-axis direction of the film surface is not excessively large, and when the baking temperature is higher than the glass transition temperature of the transparent polyimide film 14 by more than 20 ℃, polyimide molecular chain segments can be rearranged, and the difference of the refractive index in the z-axis direction and the refractive indexes in the x-axis direction and the y-axis direction of the film surface can be reduced, so that the light leakage performance of the transparent polyimide film is reduced.
The polyimide precursor may be a polyamic acid solution or a polyimide solution.
The polyimide precursor 22 has an intrinsic viscosity (intrinsic viscosity) of more than 1 to ensure a certain degree of mechanical properties of the polyimide film, and is obtained by polymerizing diamine and dianhydride, wherein the diamine may be 4,4 '-Bis (4-aminophenoxy) diphenylsulfone (pBAPS), 4' -Bis (3-aminophenoxy) diphenylsulfone (mBAPS), 1, 3-Bis (3-aminophenoxy) benzene (APB-N) 2, 2-Bis [4- (4-aminophenoxy) phenyl ] -1, 3-Hexafluoropropane (HFBAPP), 4 '-diaminodiphenyl sulfone (44 DDS), 3' -diaminodiphenyl sulfone (33 DDS), 2 '-Bis (trifluoromethyl) diaminobiphenyl (TFMB), a process for preparing the same bicyclo [2.2.1] heptane dimethylamine (NBDA), 2' -Bis (trifluoromethyl) -4,4 '-diaminophenyl ether (6 FODA), 2-Bis (3-amino-4-hydroxyphenyl) hexafluoropropane (6 FAP), 2-Bis (4-aminophenyl) hexafluoropropane (Bis-A-AF), 4' - [1, 4-phenylbis (oxy) ] Bis [3- (trifluoromethyl) aniline ] (FAPB), 5 (6) -amino-1- (4-aminophenyl) -1, 3-Trimethylindan (TMDA), 9, 9-bis (4-aminophenyl) fluorene (BAFL) and m-phenylenediamine (mPDA) are composed of at least one of the diamines described above.
The dianhydride may be 4, 4-hexafluoroisopropyl phthalic anhydride (6 FDA), bisphenol A type diether dianhydride (BPADA), 3',4,4' -biphenyltetracarboxylic dianhydride (BPDA), 3, 4-diphenylsulfone tetracarboxylic dianhydride (DSDA), 4 '-oxydiphthalic anhydride (ODPA), 3',4,4 '-Benzophenone Tetracarboxylic Dianhydride (BTDA), 1,2,3, 4-cyclobutanetetracarboxylic dianhydride (CBDA), 1,2,4, 5-cyclohexanedicarboxylic acid dianhydride (HPMDA), bicyclo [2.2.2] oct-7-ene-2, 3,5, 6-tetracarboxylic dianhydride (BTA), hexahydro-4, 8-ethane-1H, 3H-benzol [1,2-c ]: 4,5-c' ] difuran-1,3,5,7-tetrone (BODA), 2, 3',4' -biphenyltetracarboxylic dianhydride (alpha-BPDA), at least consisting of one of the dianhydrides mentioned above. The thickness of the transparent polyimide film is 5-25 um.
Example 1]
Preparation of polyimide precursor
4.933 kg of mBAPS (0.0114 mole) was added with 30 kg of N, N-dimethylacetamide (DMAc), after all of which 5.067 kg of 6FDA (0.0114 mole) was slowly added, the temperature was controlled to 25℃at the time of addition, and the solution was stirred for a certain period of time to carry out dissolution and reaction, and the temperature of the solution was maintained to 25℃to finally obtain a polyimide precursor having a solid content of 25%.
Production of transparent polyimide film
And adding a proper amount of acetic anhydride and 3-methylpyridine into the polyimide precursor, coating the mixture on a polyimide film, baking the mixture at the highest temperature of 300 ℃ through a continuous process to obtain a composite film of a transparent polyimide film and the polyimide film, and tearing off the transparent polyimide to obtain the transparent polyimide film.
Example 2]
Preparation of polyimide precursor
4.538 kg of mBAPS (0.0105 mole) was added to 30 kg of N, N-dimethylacetamide (DMAc), after all of which was dissolved, 5.434 kg of 6FDA (0.0104 mole) was slowly added thereto, the temperature was controlled to 25℃at the time of addition, and the solution was stirred for a certain period of time to carry out the dissolution and reaction, and the temperature of the solution was maintained to 25℃to finally obtain a polyimide precursor having a solid content of 25%.
Production of transparent polyimide film
And adding a proper amount of acetic anhydride and 3-methylpyridine into the polyimide precursor, coating the mixture on a polyimide film, baking the mixture at a maximum temperature of 260 ℃ through a continuous process to obtain a composite film of a transparent polyimide film and the polyimide film, and tearing off the transparent polyimide to obtain the transparent polyimide film.
Example 3 ]
Preparation of polyimide precursor
2.932 kg of pBAPS (0.0068 mole) was added to 20 kg of N, N-dimethylacetamide (DMAc), and after all had dissolved 1.807 kg of 6FDA (0.0041 mole) was slowly added. 1.046 kg of NBDA and 10 kg of DMAc are uniformly mixed, slowly poured into the mixture of pBAPS and 6FDA, 4.216 kg of 6FDA is slowly added, the mixture is stirred for a certain time to carry out dissolution and reaction, the temperature of the solution is maintained at 25 ℃, and finally, the polyimide precursor with 25% of solid content is obtained.
Production of transparent polyimide film
And adding a proper amount of acetic anhydride and 3-methylpyridine into the polyimide precursor, coating the mixture on a polyimide film, baking the mixture at the highest temperature of 290 ℃ through a continuous process to obtain a composite film of a transparent polyimide film and the polyimide film, and tearing off the transparent polyimide to obtain the transparent polyimide film.
Comparative example 1]
Production of polyamic acid
4.933 kg of mBAPS (0.0114 mole) was added with 30 kg of N, N-dimethylacetamide (DMAc), after all of which 5.067 kg of 6FDA (0.0114 mole) was slowly added, the temperature was controlled to 25℃at the time of addition, and the solution was stirred for a certain period of time to carry out dissolution and reaction, and the temperature of the solution was maintained to 25℃to finally obtain a polyimide precursor having a solid content of 25%.
Production of transparent polyimide film
And adding a proper amount of acetic anhydride and 3-methylpyridine into the polyimide precursor, coating the mixture on a polyimide film, baking the mixture at the highest temperature of 260 ℃ through a continuous process to obtain a composite film of a transparent polyimide film and the polyimide film, and tearing off the transparent polyimide to obtain the transparent polyimide film.
Comparative example 2]
Preparation of polyimide precursor
4.538 kg of mBAPS (0.0105 mole) was added to 30 kg of N, N-dimethylacetamide (DMAc), after all of which was dissolved, 5.434 kg of 6FDA (0.0104 mole) was slowly added thereto, the temperature was controlled to 25℃at the time of addition, and the solution was stirred for a certain period of time to carry out the dissolution and reaction, and the temperature of the solution was maintained to 25℃to finally obtain a polyimide precursor having a solid content of 25%.
Production of transparent polyimide film
And adding a proper amount of acetic anhydride and 3-methylpyridine into the polyimide precursor, coating the mixture on a polyimide film, baking the mixture at the highest temperature of 220 ℃ through a continuous process to obtain a composite film of a transparent polyimide film and the polyimide film, and tearing off the transparent polyimide to obtain the transparent polyimide film.
Comparative example 3 ]
Preparation of polyimide precursor
2.932 kg of pBAPS (0.0068 mole) was added to 20 kg of N, N-dimethylacetamide (DMAc), and after all had dissolved 1.807 kg of 6FDA (0.0041 mole) was slowly added. 1.046 kg of NBDA and 10 kg of DMAc are uniformly mixed, slowly poured into the mixture of pBAPS and 6FDA, 4.216 kg of 6FDA is slowly added, the mixture is stirred for a certain time to carry out dissolution and reaction, the temperature of the solution is maintained at 25 ℃, and finally, the polyimide precursor with 25% of solid content is obtained.
Production of transparent polyimide film
And adding a proper amount of acetic anhydride and 3-methylpyridine into the polyimide precursor, coating the mixture on a polyimide film, baking the mixture at the highest temperature of 270 ℃ through a continuous process to obtain a composite film of a transparent polyimide film and the polyimide film, and tearing off the transparent polyimide to obtain the transparent polyimide film.
Comparative example 4 ]
Production of polyamic acid
24.665 kg of mBAPS (0.057 mole) was added to 150 kg of N, N-dimethylacetamide (DMAc), after all of which 25.335 kg of 6FDA (0.057 mole) was slowly added to the mixture, the temperature was controlled to 25℃at the time of addition, and the mixture was stirred for a certain period of time to perform dissolution and reaction, and the temperature of the solution was maintained to 25℃to finally obtain a polyimide precursor having a solid content of 25%.
Production of transparent polyimide film
And adding proper amount of acetic anhydride and 3-methylpyridine into the polyimide precursor, and baking at the highest temperature of 260 ℃ through a continuous process to obtain the transparent polyimide film.
The optical properties of the transparent polyimide films obtained in the following examples were measured using the following methods:
refractive index was measured using an axome polarization measurement apparatus.
Chromaticity b was measured according to ASTM E313 using an instrument model NE-4000 from Nippon Denshoku Co.
Light transmittance was measured according to ISO 14782 using an instrument model NDH-2000N from Nippon Denshoku Co.
Polymerization method test results of examples and comparative examples
The foregoing description of specific embodiments is provided to illustrate the invention in detail, however, the embodiments are merely illustrative and are not intended to limit the invention. It will be understood by those skilled in the art that various changes and modifications may be made to the present invention without departure from the scope thereof, which is defined by the appended claims.
Claims (4)
1. A method for manufacturing a continuous transparent polyimide film for a display, comprising the steps of;
providing a polyimide film, which is disposed on a continuous process;
providing a transparent polyimide precursor coated on the polyimide film; a kind of electronic device with high-pressure air-conditioning system
Baking the transparent polyimide precursor at a temperature at least 59 ℃ higher than the glass transition temperature of the transparent polyimide film to form a transparent polyimide film having an optical transmittance of more than 85% and a chromaticity (b) of less than 2, and three axial refractive indices (n) x 、n y 、n z ) The standard deviation is less than 0.00114;
wherein the transparent polyimide precursor is obtained by polymerizing diamine and dianhydride, wherein the diamine is selected from one or two of 4,4 '-bis (4-aminophenoxy) diphenyl sulfone (pBAPS), 4' -bis (3-aminophenoxy) diphenyl sulfone (mBAPS) and bicyclo [2.2.1] heptane dimethylamine (NBDA);
the dianhydride is selected from 4, 4-hexafluoroisopropyl phthalic anhydride (6 FDA) or bisphenol A type diether dianhydride (BPADA).
2. The method for manufacturing a continuous transparent polyimide film for a display according to claim 1, wherein the transparent polyimide precursor is selected from a transparent polyamic acid solution or a transparent polyimide solution.
3. The method for manufacturing a continuous transparent polyimide film for a display according to claim 1, wherein the intrinsic viscosity of the transparent polyimide precursor is greater than 1.
4. The method for manufacturing a continuous transparent polyimide film for a display according to claim 1, wherein the thickness of the transparent polyimide film is between 5 and 25 um.
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| CN104582960A (en) * | 2012-09-14 | 2015-04-29 | 三井化学株式会社 | Transparent polyimide laminate and manufacturing method therefor |
| CN109651630A (en) * | 2017-10-11 | 2019-04-19 | 达迈科技股份有限公司 | The manufacturing method of transparent polyimide film |
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| CN104582960A (en) * | 2012-09-14 | 2015-04-29 | 三井化学株式会社 | Transparent polyimide laminate and manufacturing method therefor |
| CN109651630A (en) * | 2017-10-11 | 2019-04-19 | 达迈科技股份有限公司 | The manufacturing method of transparent polyimide film |
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