CN104211963A - Preparation method of polyimide resin and polyimide resin thin film prepared by preparation method - Google Patents
Preparation method of polyimide resin and polyimide resin thin film prepared by preparation method Download PDFInfo
- Publication number
- CN104211963A CN104211963A CN201410478881.8A CN201410478881A CN104211963A CN 104211963 A CN104211963 A CN 104211963A CN 201410478881 A CN201410478881 A CN 201410478881A CN 104211963 A CN104211963 A CN 104211963A
- Authority
- CN
- China
- Prior art keywords
- polyimide resin
- solution
- manufacture method
- mentioned
- chemical formula
- 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
Links
Landscapes
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention relates to a preparation method of a polyimide resin and a polyimide resin thin film prepared by the preparation method. The method can be used for polymerizing plural benzophenonetetracarboxylic dianhydrides which are different from diamine in types, and the thermal stability is excellent and the yellow color index is low. The preparation method of the polyimide resin comprises the following steps: a forming stage of dissolving diamine in a solvent to form a first solvent; a second forming stage of mixing the benzophenonetetracarboxylic dianhydride shown in a chemical formula (1), the benzophenonetetracarboxylic dianhydride shown in a chemical formula (2) and the benzophenonetetracarboxylic dianhydride shown in a chemical formula (3) in the first solution to generate a second solution containing polyamide acid; and a thermal treatment stage of the second solvent. The polyimide resin thin film can be further prepared by using the polyimide resin. The prepared polyimide thin film has excellent commercial applicability. The polyimide resin thin film not only has excellent thermal stability in thermal performance, but also the coefficient of thermal expansion can be further reduced to below existing coefficient. The polyimide resin thin film has excellent dimensional stability.
Description
Technical field
The present invention relates to a kind of manufacture method of polyimide resin and utilize Kapton manufactured by it, more specifically, polymerize with the manufacture method of the resin of the benzophenone tetracarboxylic dianhydride of diamines different sorts plural number and utilize Kapton manufactured by it.
Background technology
Along with the arrival of the informationized society of high speed development in recent years, the liquid crystal orientation film in the optical fiber in optical communication field and optical waveguides, field of display devices, to carry out just in high gear for the exploitation of the optical material such as protective membrane of color filter (color filter).Particularly to substitute and the discussion that is lightweight, the good plastic base (plastic substrate) of suppleness (flexible) of glass substrate in field of display devices, and the research and development of flexible or rollable display screen are subject to extensive concern.Therefore, in this application, the demand of more high performance optical material also constantly increases.General polyimide is coloured to tawny due to the formation of conjugation or charge transfer complex in molecule.
Its solution such as imports fluorine, or give snappiness on main chain, or import large volume side chain, and suppress the formation of charge transfer complex, the method for enhancing the transparency is on the books.
In addition, can use in principle and not produce the half alicyclic or full-cream cycloaliphatic polyimide resin that electric charge moves complex compound, improve method also { No. 2002-348374, the Japanese Laid-Open Patent (patent documentation 1) on the books of the transparency, No. 2005-15629, Japanese Laid-Open Patent (patent documentation 2), No. 2002-161136, Japanese Laid-Open Patent (patent documentation 3) }.As flexible base board, plastic base is relatively suitable for, and is because it is easily processed, low weight and can operate continuously.
But inherently the thermostability of plastic base is lower, also need to improve physicals in order to reality is suitable for, therefore, to have excellent thermotolerance polyimide macromolecular material need day by day increase.
The thermal expansivity of traditional Thermocurable polyimide and water white polyimide is higher, for flexible copper foil base material (FCCL, Flexible Copper Clad Laminate) or the material of flexible base board time, need the film using low thermal coefficient of expansion because dimensional stability is poor.Technical background for the present invention is in No. 10-2003-0009347th, KR published patent (2003.01.29 is open), and Kapton and manufacture method thereof are on the books.
Summary of the invention
The object of the invention is to polymerize the benzophenone tetracarboxylic dianhydride with diamines different sorts plural number, the thermal stability of its excellence, yellowness index is low, thus can provide water white, the manufacture method of polyimide resin and utilize Kapton manufactured by it.
In order to solve the problems of the technologies described above, technical scheme of the present invention is specific as follows:
A manufacture method for polyimide resin, is characterized in that,
Comprise and dissolve diamines in a solvent, form the 1st solution formation stages;
To the benzophenone tetracarboxylic dianhydride of chemical formula (1), the benzophenone tetracarboxylic dianhydride being denoted as chemical formula (2) be denoted as and the benzophenone tetracarboxylic dianhydride that is denoted as chemical formula (3) is mixed in the 1st above-mentioned solution, produce the formation stages of the 2nd solution containing polyamic acid (PAA); And
To the heat treatment stages of above-mentioned 2nd solution;
Above-mentioned diamines can be aromatic diamine, be preferably 2, two (trifluoromethyl)-4 of 2'-, 4'-benzidine (2,2 '-TFDB), 3,3 '-bis-(trifluoromethyl)-4,4 '-benzidine (33 '-TFDB), the one in 4,4'-amine oxidase and Ursol D.
Above-mentioned solvent can be METHYLPYRROLIDONE (NMP) meta-cresol, dimethyl formamide (DMF), dimethyl sulfoxide (DMSO) (DMSO), acetone, at least one in vinyl acetic monomer and N,N-DIMETHYLACETAMIDE (DMAC).After forming above-mentioned 2nd solution, can by the 2nd above-mentioned solution coatings on substrate.Wherein, coating at least use following in one: Spin coating, Doctorblade coating, Slotdie coating.
The heat treatment stages of the 2nd solution described above, comprising above-mentioned 2nd solution is the 1st heat treatment stages carried out between 100 DEG C to 120 DEG C in temperature; And be between 120 DEG C to 450 DEG C, carry out the 2nd heat treatment stages by the 2nd solution through the 1st heat treatment stages in temperature.The 1st described heat treatment stages is enforcement 5 minutes to 20 minutes, by the above-mentioned solvent evaporation in the 2nd solution, obtains the stage of high polyamic acid of purifying.The 2nd described heat treatment stages be enforcement 60 minutes to 90 minutes, by thermopolymerization, above-mentioned polyamic acid is carried out the stage of imidization.
The present invention also provides a kind of Kapton obtained by above-mentioned manufacture method, it is characterized in that, with the benzophenone tetracarboxylic dianhydride being denoted as chemical formula (1) and the benzophenone tetracarboxylic dianhydride being denoted as chemical formula (2) and be denoted as (3) the compounding substances of benzophenone tetracarboxylic dianhydride with the polyimide obtained from aromatic diamine for main component, its yellowness index is lower than 2.0.
The invention has the beneficial effects as follows:
Can polymerize and the dianhydride of diamines different sorts plural number (benzophenone tetracarboxylic dianhydride) according to manufacture method provided by the invention, thermal stability is good, and yellowness index is low.The Kapton produced has fully superior commercial suitability.Particularly not only there is excellent thermostability (thermolysis start temperature high) in thermal characteristics, and thermal expansivity also can be down to below existing coefficient, has excellent dimensional stability.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Fig. 1 is the manufacturing flow chart of polyimide resin of the present invention.
Fig. 2 is the printing opacity analysis chart with the obtained Kapton of UV-vis spectrometer measurement embodiment 1.
Fig. 3 is the thermogravimetric analysis figure measuring the obtained Kapton of embodiment 1 with thermogravimetric analyzer.
Fig. 4 is the thermogravimetric analysis figure measuring the obtained Kapton of embodiment 2 with thermogravimetric analyzer.
Embodiment
Advantage of the present invention and feature, and the method how reaching above-mentioned effect, the detailed description that please refer to drawings and Examples can be more apparent.But, the present invention is not only confined to following embodiment and will embodies various form, embodiment is in order to more complete explanation the present invention, and this category invented more completely is conveyed to these those skilled in the art, is only the category that power claim defines.Whole same reference symbol in specification sheets refers to same integrant.
With reference to figure 1, the manufacture method of polyimide resin of the present invention comprises, diamines is utilized to form the 1st solution phase (closing 110) in a solvent, in the 1st above-mentioned solution mixing be denoted as chemical formula (1) benzophenone tetracarboxylic dianhydride, be denoted as chemical formula (2) benzophenone tetracarboxylic dianhydride and be denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3), form the 2nd solution phase (close 120) containing polyamic acid (PAA); Substrate is coated above-mentioned the 2nd solution phase (closing 130), and by the heat treatment stages (closing 140) of above-mentioned 2nd solution.
At this, above-mentioned diamines can be aromatic diamine, preferably 2,2'-two (trifluoromethyl)-4,4'-benzidine (2,2 '-TFDB), 3,3 '-bis-(trifluoromethyl)-4,4 '-benzidine (33 '-TFDB), one in 4,4'-amine oxidase and Ursol D.
In addition, above-mentioned solvent can be METHYLPYRROLIDONE (NMP) meta-cresol, dimethyl formamide (DMF), dimethyl sulfoxide (DMSO) (DMSO), acetone, at least one in vinyl acetic monomer and N,N-DIMETHYLACETAMIDE (DMAC).
In the manufacturing processed of the polyimide resin of one embodiment of the invention, diamines can be 2, two (trifluoromethyl)-4 of 2'-, 4'-benzidine (2,2 '-TFDB) or 3,3 '-bis-(trifluoromethyl)-4,4 '-benzidine (33 '-TFDB), if more preferably adopt the solvent dissolving diamines to be N,N-DIMETHYLACETAMIDE (DMAC), the water white polyimide resin that yellowness index is lower just can be obtained.
In addition, in the manufacturing processed of the polyimide of one embodiment of the invention, the solvent dissolving diamines is not Ursol D, but METHYLPYRROLIDONE (NMP) meta-cresol, high heat resistance, high heat cured polyimide resin can be obtained.
In the 1st solution, mixing is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (1) and is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2) and is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3), form the 2nd solution phase (closing 120) containing polyamic acid, spontaneous reaction preferably keeps the low temperature of less than about 20 DEG C.If can not maintain above-mentioned low temperature, molecular weight can exceed 100, more than 000, Kapton follow-up under high molecular state is then difficult to be formed, such as, when making flexible copper foil base material (FCCL), there will be tack poor, easily damaged situation occurs.
In the coating of above-mentioned 2nd solution to the stage (close 130) on substrate, coating is at least the one in Spin coating, Doctorblade coating, Slotdie coating.
But the coating process of the 2nd solution is not only limited to this, if the method that can be coated onto on substrate by solution is all applicable.The thermal treatment being coated onto above-mentioned 2nd solution on substrate divides 2 steps to carry out.
The thermal treatment of the 2nd above-mentioned solution can divide following 2 steps, is the 1st heat treatment stages carried out between 100 DEG C to 120 DEG C by above-mentioned 2nd solution in temperature; And be between 120 DEG C to 450 DEG C, carry out the 2nd heat treatment stages by the 2nd solution through the 1st heat treatment stages in temperature.
The 1st above-mentioned heat treatment stages is enforcement 5 minutes to 20 minutes, by the above-mentioned solvent evaporation in the 2nd solution, obtains the stage of high polyamic acid of purifying.
The 2nd above-mentioned heat treatment stages be enforcement 60 minutes to 90 minutes, by thermopolymerization, above-mentioned polyamic acid is carried out the stage of imidization.
Through the manufacture method of the invention described above produce polyimide resin can form 5 μm of Kaptons to 200 μm of thickness.The yellowness index of the polyimide resin that described manufacture method obtains is lower than 2.0, and second-order transition temperature is 300 DEG C to 350 DEG C, and it is 550 DEG C to 600 DEG C that thermolysis starts temperature.The polyimide resin UV-vis spectrometer measurement that described manufacture method obtains, when 550nm, light transmission is 85% to 98%.
Embodiment 1
Prepare the reactor being accompanied with agitator, nitrogen injector, dropping funnel, thermoswitch, condenser.Nitrogen injection in above reactor, puts into the DMAC solvent of 5.97000mol.The temperature of reactor is remained on less than 20 DEG C, dissolves 2,2'-two (trifluoromethyl)-4,4'-benzidine (2,2 '-TFDB) of 0.20000mol.The benzophenone tetracarboxylic dianhydride that 0.15mol is denoted as chemical formula (1) is put in above-mentioned reactor, 0.02299mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2), and 0.04269mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3).Within 24 hours, obtain out viscosity in 1000 ~ 2000cps scope, the water white polyamic acid of solidification 22wt% in reaction later.
Water white polyamic acid solution Spin coating is heat-treated on substrate again.First, by temperature increase to 120 DEG C, after solvent being evaporated 15 minutes, obtain solid, powdery polyamic acid.Be warming up to 450 DEG C more afterwards, through the thermopolymerization of 75 minutes, imidization carried out to polyamic acid, finally get water white polyimide resultant.
Measure the thermal characteristics of resultant polyimide, optical property, mechanical property and electrical property, show the result in table 1, Fig. 2 and Fig. 3.
Embodiment 2
Prepare the reactor being accompanied with agitator, nitrogen injector, dropping funnel, thermoswitch, condenser.Nitrogen injection in above reactor, puts into METHYLPYRROLIDONE (NMP) the meta-cresol solvent of 5.97000mol.The temperature of reactor is remained on less than 20 DEG C, dissolves 3,3 '-bis-(trifluoromethyl)-4, the 4 '-benzidine (33 '-TFDB) of 0.20000mol.The benzophenone tetracarboxylic dianhydride that 0.15000mol is denoted as chemical formula (1) is put in above-mentioned reactor, 0.02299mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2), and 0.04269mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3).Within 24 hours, obtain out viscosity in 1000 ~ 2000cps scope, the water white polyamic acid of solidification 22wt% in reaction later.
Water white polyamic acid solution Doctorblade coating is heat-treated on substrate again.First, by temperature increase to 100 DEG C, after solvent being evaporated 20 minutes, obtain solid, powdery polyamic acid.Be warming up to 450 DEG C more afterwards, through the thermopolymerization of 90 minutes, imidization carried out to polyamic acid, finally get water white polyimide resultant.Measure the thermal characteristics of resultant polyimide, optical property, mechanical property and electrical property, show the result in table 1, Fig. 4.
Reference table 1, Fig. 2 and Fig. 3 are 96.6% with the water white Kapton of the embodiment 1 of UV-vis spectrometer measurement in 550nm visible region.In addition, yellowness index is 1.7, the yellow chromaticity that water white transparency degree is far superior to display screen lower than 3 standard.In addition, visible by the thermogravimetric analysis figure of the Kapton measured with thermogravimetric analyzer, thermolysis starting temperature (DEG C) is 570 DEG C, thermal expansivity (ppm/ DEG C) is 22.5ppm/ DEG C, and thermal expansivity is higher than the Kapton of (the Neopulim L of gas chemical company of Mitsubishi) existing 45 to 60ppm/ DEG C.
In table 1 and Fig. 4, according to embodiment 2, visible in the thermogravimetric analysis figure of the Kapton measured with thermogravimetric analyzer, the beginning temperature of high temperature resistant thermosetting polyimide film is 590 DEG C, thermal expansivity (ppm/ DEG C) is 7.0ppm/ DEG C, and thermal expansivity is higher than the Kapton of (UPILEX-S of UBE Industries Ltd.) existing 12 to 20ppm/ DEG C.
Embodiment 3
Prepare the reactor being accompanied with agitator, nitrogen injector, dropping funnel, thermoswitch, condenser.Nitrogen injection in above reactor, puts into the DMSO solvent of 5.97000mol.The temperature of reactor is remained on less than 20 DEG C, dissolves 4, the 4'-amine oxidases of 0.20000mol.The benzophenone tetracarboxylic dianhydride that 0.15000mol is denoted as chemical formula (1) is put in above-mentioned reactor, 0.02299mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2), and 0.04269mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3).Within 24 hours, obtain out viscosity in 1000 ~ 2000cps scope, the water white polyamic acid of solidification 22wt% in reaction later.
Water white polyamic acid solution Slotdie coating is heat-treated on substrate again.First, by temperature increase to 120 DEG C, after solvent being evaporated 5 minutes, obtain solid, powdery polyamic acid.Be warming up to 450 DEG C more afterwards, through the thermopolymerization of 60 minutes, imidization carried out to polyamic acid, finally get water white polyimide resultant.
Measure the thermal characteristics of resultant polyimide, optical property, mechanical property and electrical property, show the result in table 1.
Embodiment 4
Prepare the reactor being accompanied with agitator, nitrogen injector, dropping funnel, thermoswitch, condenser.Nitrogen injection in above reactor, puts into the DMF solvent of 5.97000mol.The temperature of reactor is remained on less than 20 DEG C, dissolves the Ursol D of 0.20000mol.The benzophenone tetracarboxylic dianhydride that 0.15000mol is denoted as chemical formula (1) is put in above-mentioned reactor, 0.02299mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2), and 0.04269mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3).Within 24 hours, obtain out viscosity in 1000 ~ 2000cps scope, the water white polyamic acid of solidification 22wt% in reaction later.
Water white polyamic acid solution Spin coating is heat-treated on substrate again.First, by temperature increase to 100 DEG C, after solvent being evaporated 15 minutes, obtain solid, powdery polyamic acid.Be warming up to 120 DEG C more afterwards, through the thermopolymerization of 65 minutes, imidization carried out to polyamic acid, finally get water white polyimide resultant.
Measure the thermal characteristics of resultant polyimide, optical property, mechanical property and electrical property, show the result in table 1.
Embodiment 5
Prepare the reactor being accompanied with agitator, nitrogen injector, dropping funnel, thermoswitch, condenser.Nitrogen injection in above reactor, puts into the vinyl acetic monomer solvent of 5.97000mol.The temperature of reactor is remained on less than 20 DEG C, dissolves 2,2'-two (trifluoromethyl)-4,4'-benzidine (2,2 '-TFDB) of 0.20000mol.The benzophenone tetracarboxylic dianhydride that 0.15000mol is denoted as chemical formula (1) is put in above-mentioned reactor, 0.02299mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2), and 0.04269mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3).Within 24 hours, obtain out viscosity in 1000 ~ 2000cps scope, the water white polyamic acid of solidification 22wt% in reaction later.
Water white polyamic acid solution Doctorblade coating is heat-treated on substrate again.First, by temperature increase to 120 DEG C, after solvent being evaporated 10 minutes, obtain solid, powdery polyamic acid.Be warming up to 450 DEG C more afterwards, through the thermopolymerization of 70 minutes, imidization carried out to polyamic acid, finally get water white polyimide resultant.
Measure the thermal characteristics of resultant polyimide, optical property, mechanical property and electrical property, show the result in table 1.
Embodiment 6
Prepare the reactor being accompanied with agitator, nitrogen injector, dropping funnel, thermoswitch, condenser.Nitrogen injection in above reactor, puts into the acetone solvent of 5.97000mol.The temperature of reactor is remained on less than 20 DEG C, dissolves 3,3 '-bis-(trifluoromethyl)-4, the 4 '-benzidine (33 '-TFDB) of 0.20000mol.The benzophenone tetracarboxylic dianhydride that 0.15000mol is denoted as chemical formula (1) is put in above-mentioned reactor, 0.02299mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2), and 0.04269mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3).Within 24 hours, obtain out viscosity in 1000 ~ 2000cps scope, the water white polyamic acid of solidification 22wt% in reaction later.
Water white polyamic acid solution Slotdie coating is heat-treated on substrate again.First, by temperature increase to 100 DEG C, after solvent being evaporated 15 minutes, obtain solid, powdery polyamic acid.Be warming up to 450 DEG C more afterwards, through the thermopolymerization of 80 minutes, imidization carried out to polyamic acid, finally get water white polyimide resultant.
Measure the thermal characteristics of resultant polyimide, optical property, mechanical property and electrical property, show the result in table 1.
[table 1]
As can be seen from above-mentioned result, according to its characteristic of Kapton that the embodiment of the present invention produces, there is fully superior commercial suitability.Particularly not only there is excellent thermostability (thermolysis start temperature high) in thermal characteristics, and thermal expansivity also can be down to below existing coefficient, has excellent dimensional stability.
The thermal expansivity of the Kapton produced according to the embodiment of the present invention is low, and dimensional stability is excellent, is applicable to flexible copper foil base material (FCCL, Flexible Copper Clad Laminate) or the material of flexible base board.In addition, according to the Kapton water white transparency that the embodiment of the present invention produces, optical characteristics is superior, can replace the existing optical thin film for display screen.The present invention can polymerize the benzophenone tetracarboxylic dianhydride with diamines different sorts plural number, the thermal stability of its excellence, and yellowness index is low, the Kapton that thus can provide the manufacture method of water white polyimide resin and utilize it and make.Below mainly around embodiments of the invention, but belonging to the present invention field, the technician with identical knowledge can various change or amendment in addition according to its level.This type of change or amendment, if do not exceeded technical scope provided by the invention, all can be considered category of the present invention.Thereupon, extent of competence of the present invention is determined according to following request scope.
Claims (10)
1. the manufacture method of polyimide resin, is characterized in that,
Comprise and dissolve diamines in a solvent, form the 1st solution formation stages;
To the benzophenone tetracarboxylic dianhydride of chemical formula (1), the benzophenone tetracarboxylic dianhydride being denoted as chemical formula (2) be denoted as and the benzophenone tetracarboxylic dianhydride that is denoted as chemical formula (3) is mixed in the 1st above-mentioned solution, produce the formation stages of the 2nd solution containing polyamic acid (PAA); And
To the heat treatment stages of above-mentioned 2nd solution;
2. the manufacture method of polyimide resin according to claim 1, is characterized in that, described diamines is aromatic diamine.
3. the manufacture method of polyimide resin according to claim 1, it is characterized in that, described diamines be use following in one: 2,2'-two (trifluoromethyl)-4,4'-benzidine (2,2 '-TFDB), 3,3 '-bis-(trifluoromethyl)-4,4 '-benzidine (33 '-TFDB), 4,4'-amine oxidase and Ursol D.
4. the manufacture method of polyimide resin according to claim 1, it is characterized in that, the solvent of described use is at least by the one in following: METHYLPYRROLIDONE (NMP) meta-cresol, dimethyl formamide (DMF), dimethyl sulfoxide (DMSO) (DMSO), acetone, vinyl acetic monomer and N,N-DIMETHYLACETAMIDE (DMAC).
5. the manufacture method of polyimide resin according to claim 1, is characterized in that, comprises after forming above-mentioned 2nd solution, by the 2nd above-mentioned solution coatings to the stage on substrate.
6. the manufacture method of polyimide resin according to claim 5, is characterized in that, in above-mentioned 2nd solution coatings to the stage on substrate, coating at least use following in one: Spin coating, Doctorblade coating, Slotdie coating.
7. the manufacture method of polyimide resin according to claim 1, is characterized in that, the heat treatment stages of described 2nd solution, and comprising above-mentioned 2nd solution is the 1st heat treatment stages carried out between 100 DEG C to 120 DEG C in temperature; And be between 120 DEG C to 450 DEG C, carry out the 2nd heat treatment stages by the 2nd solution through the 1st heat treatment stages in temperature.
8. the manufacture method of polyimide resin according to claim 7, is characterized in that, the 1st described heat treatment stages is enforcement 5 minutes to 20 minutes, by the above-mentioned solvent evaporation in the 2nd solution, obtains the stage of high polyamic acid of purifying.
9. the manufacture method of polyimide resin according to claim 7, is characterized in that, the 2nd described heat treatment stages be enforcement 60 minutes to 90 minutes, by thermopolymerization, above-mentioned polyamic acid is carried out the stage of imidization.
10. the Kapton that obtains of the manufacture method of polyimide resin according to claim 1, it is characterized in that, with the benzophenone tetracarboxylic dianhydride being denoted as chemical formula (1) and the benzophenone tetracarboxylic dianhydride being denoted as chemical formula (2) and be denoted as (3) the compounding substances of benzophenone tetracarboxylic dianhydride with the polyimide obtained from aromatic diamine for main component, its yellowness index is lower than 2.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410478881.8A CN104211963B (en) | 2014-09-18 | 2014-09-18 | The manufacture method of polyimide resin and utilize its manufactured Kapton |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410478881.8A CN104211963B (en) | 2014-09-18 | 2014-09-18 | The manufacture method of polyimide resin and utilize its manufactured Kapton |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104211963A true CN104211963A (en) | 2014-12-17 |
| CN104211963B CN104211963B (en) | 2016-09-28 |
Family
ID=52093892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410478881.8A Active CN104211963B (en) | 2014-09-18 | 2014-09-18 | The manufacture method of polyimide resin and utilize its manufactured Kapton |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104211963B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108424647A (en) * | 2018-03-13 | 2018-08-21 | 苏州柔彩新材料科技有限公司 | It is a kind of for the clear, colorless Kapton of AMOLED, preparation method and AMOLED devices |
| CN110092908A (en) * | 2019-04-03 | 2019-08-06 | 中国科学院化学研究所 | A kind of Kapton and its preparation method and application |
| CN111187414A (en) * | 2020-02-14 | 2020-05-22 | 吉林奥来德光电材料股份有限公司 | High-performance transparent polyimide film and preparation method thereof |
| CN112142999A (en) * | 2019-06-28 | 2020-12-29 | Skc株式会社 | Base film, method of manufacturing the same, and cover window and display device including the same |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002338710A (en) * | 2001-03-16 | 2002-11-27 | Sumitomo Bakelite Co Ltd | Plastic base plate for indication element |
| JP2002363283A (en) * | 2001-06-06 | 2002-12-18 | Nitto Denko Corp | Polyamide acid, polyimide resin obtained from the same and utilization of them for circuit substrate |
| JP2006348259A (en) * | 2005-05-16 | 2006-12-28 | Toyobo Co Ltd | Polyimide film and method for producing the same |
| CN103240936A (en) * | 2012-02-10 | 2013-08-14 | 新日铁住金化学株式会社 | Transparent flexible laminate and laminate roll |
| CN103524767A (en) * | 2013-10-30 | 2014-01-22 | 宏威高新材料有限公司 | Novel electronic-grade polyimide film with low linear expansion coefficient and manufacturing method thereof |
| CN103660458A (en) * | 2012-09-24 | 2014-03-26 | 新日铁住金化学株式会社 | Polyimide laminating body and manufacturing method thereof |
-
2014
- 2014-09-18 CN CN201410478881.8A patent/CN104211963B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002338710A (en) * | 2001-03-16 | 2002-11-27 | Sumitomo Bakelite Co Ltd | Plastic base plate for indication element |
| JP2002363283A (en) * | 2001-06-06 | 2002-12-18 | Nitto Denko Corp | Polyamide acid, polyimide resin obtained from the same and utilization of them for circuit substrate |
| JP2006348259A (en) * | 2005-05-16 | 2006-12-28 | Toyobo Co Ltd | Polyimide film and method for producing the same |
| CN103240936A (en) * | 2012-02-10 | 2013-08-14 | 新日铁住金化学株式会社 | Transparent flexible laminate and laminate roll |
| CN103660458A (en) * | 2012-09-24 | 2014-03-26 | 新日铁住金化学株式会社 | Polyimide laminating body and manufacturing method thereof |
| CN103524767A (en) * | 2013-10-30 | 2014-01-22 | 宏威高新材料有限公司 | Novel electronic-grade polyimide film with low linear expansion coefficient and manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 陈磊等: ""无规嵌段共聚缩聚聚酰亚胺的制备与性能研究"", 《绝缘材料》, vol. 43, no. 6, 25 February 2011 (2011-02-25), pages 1 - 8 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108424647A (en) * | 2018-03-13 | 2018-08-21 | 苏州柔彩新材料科技有限公司 | It is a kind of for the clear, colorless Kapton of AMOLED, preparation method and AMOLED devices |
| CN108424647B (en) * | 2018-03-13 | 2021-05-25 | 苏州柔彩半导体柔性材料科技有限公司 | Transparent colorless polyimide film for AMOLED, preparation method and AMOLED device |
| CN110092908A (en) * | 2019-04-03 | 2019-08-06 | 中国科学院化学研究所 | A kind of Kapton and its preparation method and application |
| WO2020200229A1 (en) * | 2019-04-03 | 2020-10-08 | 中国科学院化学研究所 | Polyimide thin film and preparation method and application thereof |
| CN112142999A (en) * | 2019-06-28 | 2020-12-29 | Skc株式会社 | Base film, method of manufacturing the same, and cover window and display device including the same |
| CN111187414A (en) * | 2020-02-14 | 2020-05-22 | 吉林奥来德光电材料股份有限公司 | High-performance transparent polyimide film and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104211963B (en) | 2016-09-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104379635B (en) | Flexible substrate with thermal stability applied to electronic equipment | |
| EP2744851B1 (en) | Thermally stable, low birefringent copolyimide films | |
| CN108473677A (en) | The polyamic acid composition that bonding force improves and the polyimide film comprising it | |
| CN101831074A (en) | New type fluorine-containing copolyimide and preparation method thereof | |
| WO2016063993A1 (en) | Polyimide film, polyimide precursor, and polyimide | |
| JP7292260B2 (en) | Polyamic acid and its manufacturing method, polyamic acid solution, polyimide, polyimide film, laminate and its manufacturing method, flexible device and its manufacturing method | |
| WO2014007112A1 (en) | Polyamide acid, polyimide, polyamide acid solution, and use of polyimide | |
| KR102500026B1 (en) | Polyamic acid, polyamic acid solution, polyimide, polyimide film, laminate and flexible device, and manufacturing method of polyimide film | |
| CN104211963A (en) | Preparation method of polyimide resin and polyimide resin thin film prepared by preparation method | |
| JP2022008353A (en) | Method for producing electronic device | |
| KR20130003358A (en) | Polyamic acid and polyamic acid solution, polyimide protecive layer, polyimide film | |
| CN105037727A (en) | Polyimide film material capable of serving as conducting film substrate and preparing method of polyimide film material | |
| KR101295653B1 (en) | Polyimide film and method for preparing same | |
| JP6461470B2 (en) | Polyimide precursor composition, polyimide production method, polyimide, polyimide film, and substrate | |
| KR101721555B1 (en) | Process for polyimide resin | |
| KR101749609B1 (en) | Resin composition for display substrates | |
| KR20170007227A (en) | A process for producing a polyimide resin and a polyimide film | |
| CN102675665A (en) | Colorless transparent polyimide film preparation method | |
| KR20140049382A (en) | Polyimide film and method for preparing same | |
| JP6638744B2 (en) | Polyimide precursor composition, method for producing polyimide, polyimide, polyimide film, and substrate | |
| KR102495618B1 (en) | Polyimide film excellent in colorless transparency and flexibility and manufacturing method thereof | |
| KR102704985B1 (en) | Polyimide resin, manufacturing method thereof, and polyimide film and display device comprising the same | |
| CN109337070B (en) | Resin composition | |
| CN116925545A (en) | Colorless polyimide film with high fluorine content, high heat resistance and low expansion, and preparation method and application thereof | |
| CN117043230A (en) | Polyamic acid, polyamic acid solution, polyimide substrate, laminate, and method for producing same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |