CN104211963B - The manufacture method of polyimide resin and utilize its manufactured Kapton - Google Patents
The manufacture method of polyimide resin and utilize its manufactured Kapton Download PDFInfo
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Abstract
The present invention relates to the manufacture method of a kind of polyimide resin and utilize its manufactured Kapton.The method polymerizable goes out and the benzophenone tetracarboxylic dianhydride of diamidogen variety classes plural number, and thermal stability is excellent, and yellow colour index is low.The manufacture method of polyimide resin comprises: dissolves diamidogen in a solvent and forms the 1st solution formation stages；By being denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (1), being denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2) and be denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3) and be mixed in the 1st above-mentioned solution, produced the formation stages of the 2nd solution containing polyamic acid；And the heat treatment stages of above-mentioned 2nd solution；Utilize this polyimide resin also can produce Kapton.The Kapton produced has superior commercial suitability.Particularly not only there is in terms of hot property excellent heat stability, and thermal coefficient of expansion also can be down to below existing coefficient, has excellent dimensional stability.
Description
Technical field
The present invention relates to the manufacture method of a kind of polyimide resin and utilize its manufactured polyimides thin
Film, more specifically, polymerize the manufacturer of the resin of the benzophenone tetracarboxylic dianhydride plural with diamidogen variety classes
Method and utilize its manufactured Kapton.
Background technology
Along with the arrival of the informationized society of high speed development in recent years, the optical fiber in optical communication field and light wave
Lead, liquid crystal orientation film in field of display devices, the optics such as protecting film for colour filter (color filter)
The exploitation of material is carried out the most in high gear.Particularly to the succedaneum of glass substrate in field of display devices i.e.
Lightweight, the discussion of suppleness (flexible) preferably plastic base (plastic substrate), and bendable
The research and development of bent or rollable display screen receive significant attention.Therefore, at this in application, higher performance
The demand of optical material the most constantly increases.General polyimides in intramolecular due to conjugation or charge-transfer complexation
The formation of thing and be coloured to yellowish-brown.
Its solution is, such as, import fluorine, or give pliability on main chain, or import large volume side
Chain, the formation of suppression charge transfer complex, the method enhanced the transparency has been described.
Do not produce electric charge move the half alicyclic or full-cream ring adoption acyl sub-of complex additionally, can use in principle
Polyimide resin, the method improving the transparency also has been described { Japanese Laid-Open Patent 2002-348374 (patent literary composition
Offer 1), Japanese Laid-Open Patent 2005-15629 (patent documentation 2), Japanese Laid-Open Patent 2002-161136
Number (patent documentation 3) }.As flexible base board, plastic base is that comparison is suitable for, and is because it and easily processes,
Low weight and can operating continuously.
But, inherently the heat stability of plastic base is relatively low, also needs to improve physical property in order to reality is suitable for
Can, therefore, to have excellence thermostability polyimides macromolecular material need day by day increase.
The thermal coefficient of expansion of traditional Thermocurable polyimide and water white polyimides is higher, for soft
During the material of property copper foil base material (FCCL, Flexible Copper Clad Laminate) or flexible base board,
Need to use the thin film of low thermal coefficient of expansion owing to dimensional stability is poor.Technical background for the present invention exists
In KR published patent the 10-2003-0009347th (2003.01.29 open), Kapton and
Manufacture method has been described.
Summary of the invention
It is an object of the invention to polymerize and the benzophenone tetracarboxylic dianhydride of diamidogen variety classes plural number, its excellence
Thermal stability, yellow colour index is low, thus can provide water white, the manufacture method of polyimide resin
And utilize its manufactured Kapton.
In order to solve above-mentioned technical problem, technical scheme is specific as follows:
A kind of manufacture method of polyimide resin, it is characterised in that
Comprise and dissolve diamidogen in a solvent, form the 1st solution formation stages；
The benzophenone tetracarboxylic dianhydride of chemical formula (1) will be denoted as, be denoted as the benzophenone four of chemical formula (2)
Acid dianhydride and be denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3) and be mixed in the 1st above-mentioned solution, institute
Produce the formation stages of the 2nd solution containing polyamic acid (PAA)；And
Heat treatment stages to above-mentioned 2nd solution；
Above-mentioned diamidogen can be aromatic diamine, double (trifluoromethyl)-4 of preferably 2,2'-, 4'-benzidine
(2,2 '-TFDB), 3,3 '-bis-(trifluoromethyl)-4,4 '-benzidine (33 '-TFDB), 4,4'-amino oxidases and
One in p-phenylenediamine.
Above-mentioned solvent can be METHYLPYRROLIDONE (NMP) metacresol, dimethylformamide (DMF), two
At least one in methyl sulfoxide (DMSO), acetone, ethyl acetate and dimethyl acetylamide (DMAC).Shape
After becoming above-mentioned 2nd solution, can be by the 2nd above-mentioned solution coatings to substrate.Wherein, coating at least uses
One in following: Spin coating, Doctorblade coating, Slotdie coating.
The heat treatment stages of the 2nd solution described above, comprise by above-mentioned 2nd solution temperature be 100 DEG C extremely
The 1st heat treatment stages carried out between 120 DEG C；And by the 2nd solution through the 1st heat treatment stages in temperature
Degree is to carry out the 2nd heat treatment stages between 120 DEG C to 450 DEG C.The 1st described heat treatment stages is enforcement 5
Minute to 20 minutes, the above-mentioned solvent in the 2nd solution is evaporated, it is thus achieved that the stage of the high polyamic acid purified.
The 2nd described heat treatment stages is for implementing 60 minutes to 90 minutes, by thermal polymerization, by above-mentioned polyamides
Amino acid carries out the stage of imidization.
The present invention also provides for a kind of Kapton obtained by above-mentioned manufacture method, it is characterised in that with
It is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (1) and the benzophenone tetracarboxylic dianhydride being denoted as chemical formula (2)
And it is denoted as the compounding substances of the benzophenone tetracarboxylic dianhydride of (3) and the polyimides obtained from aromatic diamine
For main component, its yellow colour index is less than 2.0.
The invention has the beneficial effects as follows:
The manufacture method provided according to the present invention can polymerize and the dianhydride of diamidogen variety classes plural number
(benzophenone tetracarboxylic dianhydride), thermal stability is good, and yellow colour index is low.The Kapton produced has
The most superior commercial suitability.Particularly not only there is in terms of hot property excellent heat stability (heat point
Solve and start temperature height), and thermal coefficient of expansion also can be down to below existing coefficient, has excellent dimensionally stable
Property.
Accompanying drawing explanation
With detailed description of the invention, the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the manufacturing flow chart of the polyimide resin of the present invention.
Fig. 2 is the printing opacity analysis chart of the Kapton prepared by UV-vis spectrometer measurement embodiment 1.
Fig. 3 is the thermogravimetric analysis figure measuring the Kapton that embodiment 1 prepares with thermogravimetric analyzer.
Fig. 4 is the thermogravimetric analysis figure measuring the Kapton that embodiment 2 prepares with thermogravimetric analyzer.
Detailed description of the invention
Advantages of the present invention and feature, and the method how reaching the effect above, refer to accompanying drawing and enforcement
The detailed description of example can become apparent from.But, the present invention is not only confined to below example and by body
Existing various forms, embodiment is that the category this invented is completeer for the more complete explanation present invention
Convey to these those skilled in the art wholely, be only category defined in power claim.In description
Whole same reference marks refer to same element.
With reference to Fig. 1, the present invention the manufacture method of polyimide resin comprise, utilize diamidogen shape in a solvent
Becoming the 1st solution phase (closing 110), in the 1st above-mentioned solution, mixing is denoted as the hexichol of chemical formula (1)
Ketone tetracarboxylic dianhydride, it is denoted as chemical formula (2) benzophenone tetracarboxylic dianhydride and is denoted as the two of chemical formula (3)
Benzophenone acid dianhydride, forms the 2nd solution phase containing polyamic acid (PAA) (closing 120)；At substrate
On coat above-mentioned the 2nd solution phase (closing 130), and the heat treatment stages of above-mentioned 2nd solution (is closed
140)。
Here, above-mentioned diamidogen can be aromatic diamine, double (trifluoromethyl)-4 of preferably 2,2'-, 4'-diaminourea
Biphenyl (2,2 '-TFDB), 3,3 '-bis-(trifluoromethyl)-4,4 '-benzidine (33 '-TFDB), 4,4'-amine oxidations
One in enzyme and p-phenylenediamine.
Additionally, above-mentioned solvent can be METHYLPYRROLIDONE (NMP) metacresol, dimethylformamide
(DMF), dimethyl sulfoxide (DMSO), acetone, in ethyl acetate and dimethyl acetylamide (DMAC) extremely
Few one.
In the manufacture process of the polyimide resin of one embodiment of the invention, diamidogen can be 2,2'-double (three
Methyl fluoride)-4,4'-benzidine (2,2 '-TFDB) or 3,3 '-bis-(trifluoromethyl)-4,4 '-benzidines
(33 '-TFDB), it may be more desirable to if using the solvent dissolving diamidogen is dimethyl acetylamide (DMAC),
It is achieved with the water white polyimide resin that yellow colour index is lower.
It addition, in the manufacture process of the polyimides of one embodiment of the invention, the solvent dissolving diamidogen is not
P-phenylenediamine, but if METHYLPYRROLIDONE (NMP) metacresol, it is possible to obtain high-fire resistance, height
Heat cured polyimide resin.
In the 1st solution, mixing is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (1) and is denoted as chemical formula
(2) benzophenone tetracarboxylic dianhydride and be denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3), is formed containing poly-
2nd solution phase (closing 120) of amic acid, spontaneous reaction preferably keeps the low temperature of less than about 20 DEG C.As
Fruit can not maintain above-mentioned low temperature, and molecular weight can exceed 100, more than 000, follow-up gathering under producing high-molecular state
Imide membrane is then difficult to be formed, such as when making flexible copper foil base material (FCCL), it may appear that tack is relatively
Difference, the most damaged situation occurs.
In the coating of above-mentioned 2nd solution to the stage (closing 130) on substrate, coating be at least Spin coating,
One in Doctorblade coating, Slotdie coating.
But, the coating process of the 2nd solution is not limited solely to this, if the side that solution can be coated onto on substrate
Method is the most applicable.The heat treatment of above-mentioned 2nd solution being coated onto on substrate divides 2 steps to carry out.
The heat treatment of the 2nd above-mentioned solution can divide following 2 steps, is 100 DEG C by above-mentioned 2nd solution in temperature
The 1st heat treatment stages carried out between 120 DEG C；And will exist through the 2nd solution of the 1st heat treatment stages
Temperature is to carry out the 2nd heat treatment stages between 120 DEG C to 450 DEG C.
The 1st above-mentioned heat treatment stages is for implementing 5 minutes to 20 minutes, by the above-mentioned solvent in the 2nd solution
Evaporation, it is thus achieved that the stage of the high polyamic acid purified.
The 2nd above-mentioned heat treatment stages is for implementing 60 minutes to 90 minutes, by thermal polymerization, by above-mentioned
Polyamic acid carries out the stage of imidization.
What the manufacture method through the invention described above produced polyimide resin can form 5 μm to 200 μm
The Kapton of thickness.The yellow colour index of the polyimide resin that described manufacture method obtains is less than 2.0,
Glass transition temperature is 300 DEG C to 350 DEG C, and it is 550 DEG C to 600 DEG C that thermal decomposition starts temperature.Described system
The polyimide resin UV-vis spectrometer measurement that the method for making obtains, when 550nm, light transmission is 85%
To 98%.
Embodiment 1
Prepare to be accompanied with the reaction of agitator, nitrogen injector, Dropping funnel, thermoregulator, condenser
Device.Nitrogen injection in above reactor, puts into the DMAC solvent of 5.97000mol.By the temperature of reactor
Degree is maintained at less than 20 DEG C, dissolves the 2 of 0.20000mol, double (trifluoromethyl)-4 of 2'-, 4'-benzidine
(2,2′-TFDB).In above-mentioned reactor, put into 0.15mol be denoted as the benzophenone tetracid two of chemical formula (1)
Acid anhydride, 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 1000～2000cps in reaction later
Scope, the water white polyamic acid of solidification 22wt%.
Water white polyamic acid solution Spin coating is carried out heat treatment on substrate again.First, by temperature
Degree is promoted to 120 DEG C, obtains solid, powdery polyamic acid after being evaporated 15 minutes by solvent.It is warming up to the most again
450 DEG C, through the thermal polymerization of 75 minutes, polyamic acid is carried out imidization, finally gets colourless
Transparent polyimides product.
Measure the hot property of product polyimides, optical property, mechanical performance and electrical property, result is shown
In table 1, Fig. 2 and Fig. 3.
Embodiment 2
Prepare to be accompanied with the reaction of agitator, nitrogen injector, Dropping funnel, thermoregulator, condenser
Device.Nitrogen injection in above reactor, puts into the METHYLPYRROLIDONE (NMP) of 5.97000mol
Metacresol solvent.The temperature of reactor is maintained at less than 20 DEG C, dissolves 3,3 '-bis-(the three of 0.20000mol
Methyl fluoride)-4,4 '-benzidine (33 '-TFDB).In above-mentioned reactor, put into 0.15000mol be denoted as
The benzophenone tetracarboxylic dianhydride of chemical formula (1), 0.02299mol is denoted as the benzophenone tetracid of chemical formula (2)
Dianhydride, and 0.04269mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3).Reaction 24 hours
Obtain out viscosity at 1000～2000cps scopes, the water white polyamic acid of solidification 22wt% later.
Water white polyamic acid solution Doctorblade coating is carried out heat treatment on substrate again.First,
Temperature is promoted to 100 DEG C, after being evaporated 20 minutes by solvent, obtains solid, powdery polyamic acid.Rise the most again
Temperature, to 450 DEG C, through the thermal polymerization of 90 minutes, carries out imidization to polyamic acid, finally gets
Water white polyimides product.Measure the hot property of product polyimides, optical property, machinery
Performance and electrical property, show the result in table 1, Fig. 4.
Reference table 1, Fig. 2 and Fig. 3, with the water white polyamides of the embodiment 1 of UV-vis spectrometer measurement
Imines thin film is 96.6% in 550nm visible region.Additionally, yellow colour index is 1.7, water white transparency degree is far away
The yellow chromaticity being better than display screen is less than the standard of 3.It addition, by the polyimides measured with thermogravimetric analyzer
The thermogravimetric analysis figure of thin film is visible, and thermal decomposition initial temperature (DEG C) is 570 DEG C, thermal coefficient of expansion (ppm/ DEG C)
For 22.5ppm/ DEG C, thermal coefficient of expansion is higher than the Neopulim L of chemical company (Rhizoma Sparganii gas) existing 45
To the Kapton of 60ppm/ DEG C.
It is shown in Table 1 and Fig. 4, according to embodiment 2, divides by the thermogravimetric of the Kapton of thermogravimetric analyzer mensuration
Analysing in figure visible, the beginning temperature of high temperature resistant thermosetting polyimide thin film is 590 DEG C, thermal coefficient of expansion
(ppm/ DEG C) is 7.0ppm/ DEG C, and thermal coefficient of expansion is higher than (UPILEX-S of UBE Industries Ltd.)
The Kapton of existing 12 to 20ppm/ DEG C.
Embodiment 3
Prepare to be accompanied with the reaction of agitator, nitrogen injector, Dropping funnel, thermoregulator, condenser
Device.Nitrogen injection in above reactor, puts into the DMSO solvent of 5.97000mol.By the temperature of reactor
Degree is maintained at less than 20 DEG C, dissolves the 4 of 0.20000mol, 4'-amino oxidase.Above-mentioned reactor is put into
0.15000mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (1), and 0.02299mol is denoted as chemical formula (2)
Benzophenone tetracarboxylic dianhydride, and 0.04269mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3).?
Reacting and obtain out viscosity after 24 hours in 1000～2000cps scopes, solidification 22wt%'s is water white
Polyamic acid.
Water white polyamic acid solution Slotdie coating is carried out heat treatment on substrate again.First, will
Temperature is promoted to 120 DEG C, obtains solid, powdery polyamic acid after being evaporated 5 minutes by solvent.It is warming up to the most again
450 DEG C, through the thermal polymerization of 60 minutes, polyamic acid is carried out imidization, finally gets colourless
Transparent polyimides product.
Measure the hot property of product polyimides, optical property, mechanical performance and electrical property, result is shown
In table 1.
Embodiment 4
Prepare to be accompanied with the reaction of agitator, nitrogen injector, Dropping funnel, thermoregulator, condenser
Device.Nitrogen injection in above reactor, puts into the DMF solvent of 5.97000mol.By the temperature of reactor
Degree is maintained at less than 20 DEG C, dissolves the p-phenylenediamine of 0.20000mol.Above-mentioned reactor is put into
0.15000mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (1), and 0.02299mol is denoted as chemical formula (2)
Benzophenone tetracarboxylic dianhydride, and 0.04269mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3).?
Reacting and obtain out viscosity after 24 hours in 1000～2000cps scopes, solidification 22wt%'s is water white
Polyamic acid.
Water white polyamic acid solution Spin coating is carried out heat treatment on substrate again.First, by temperature
Degree is promoted to 100 DEG C, obtains solid, powdery polyamic acid after being evaporated 15 minutes by solvent.It is warming up to the most again
120 DEG C, through the thermal polymerization of 65 minutes, polyamic acid is carried out imidization, finally gets colourless
Transparent polyimides product.
Measure the hot property of product polyimides, optical property, mechanical performance and electrical property, result is shown
In table 1.
Embodiment 5
Prepare to be accompanied with the reaction of agitator, nitrogen injector, Dropping funnel, thermoregulator, condenser
Device.Nitrogen injection in above reactor, puts into the ethyl acetate solvent of 5.97000mol.By reactor
Temperature is maintained at less than 20 DEG C, dissolves the 2 of 0.20000mol, double (trifluoromethyl)-4 of 2'-, 4'-benzidine
(2,2′-TFDB).In above-mentioned reactor, put into 0.15000mol be denoted as the benzophenone tetracid of chemical formula (1)
Dianhydride, 0.02299mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2), and 0.04269mol indicates
Benzophenone tetracarboxylic dianhydride for chemical formula (3).Within 24 hours, obtain out viscosity 1000～2000cps in reaction later
Scope, the water white polyamic acid of solidification 22wt%.
Water white polyamic acid solution Doctorblade coating is carried out heat treatment on substrate again.First,
Temperature is promoted to 120 DEG C, after being evaporated 10 minutes by solvent, obtains solid, powdery polyamic acid.Rise the most again
Temperature, to 450 DEG C, through the thermal polymerization of 70 minutes, carries out imidization to polyamic acid, finally gets
Water white polyimides product.
Measure the hot property of product polyimides, optical property, mechanical performance and electrical property, result is shown
In table 1.
Embodiment 6
Prepare to be accompanied with the reaction of agitator, nitrogen injector, Dropping funnel, thermoregulator, condenser
Device.Nitrogen injection in above reactor, puts into the acetone solvent of 5.97000mol.By the temperature of reactor
It is maintained at less than 20 DEG C, dissolves 3,3 '-bis-(trifluoromethyl)-4 of 0.20000mol, 4 '-benzidine
(33′-TFDB).In above-mentioned reactor, put into 0.15000mol be denoted as the benzophenone tetracid of chemical formula (1)
Dianhydride, 0.02299mol is denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (2), and 0.04269mol indicates
Benzophenone tetracarboxylic dianhydride for chemical formula (3).Within 24 hours, obtain out viscosity 1000～2000cps in reaction later
Scope, the water white polyamic acid of solidification 22wt%.
Water white polyamic acid solution Slotdie coating is carried out heat treatment on substrate again.First, will
Temperature is promoted to 100 DEG C, obtains solid, powdery polyamic acid after being evaporated 15 minutes by solvent.Heat up the most again
To 450 DEG C, through the thermal polymerization of 80 minutes, polyamic acid is carried out imidization, finally gets nothing
The polyimides product that color is transparent.
Measure the hot property of product polyimides, optical property, mechanical performance and electrical property, result is shown
In table 1.
[table 1]
It can be seen from the above results that its characteristic of the Kapton produced according to embodiments of the present invention
There is the most superior commercial suitability.Particularly not only there is in terms of hot property excellent heat stability (heat
Kick off temperature is high), and thermal coefficient of expansion also can be down to below existing coefficient, has excellent size steady
Qualitative.
The thermal coefficient of expansion of the Kapton produced according to embodiments of the present invention is low, dimensional stability
Excellent, it is applicable to flexible copper foil base material (FCCL, Flexible Copper Clad Laminate) or soft
The material of property substrate.Additionally, the Kapton water white transparency produced according to embodiments of the present invention, light
Learn excellent, the existing optical thin film for display screen can be replaced.The present invention can polymerize with diamidogen not
With the benzophenone tetracarboxylic dianhydride of kind plural number, the thermal stability of its excellence, yellow colour index is low, thus can carry
For the manufacture method of water white polyimide resin and utilize it and the Kapton that makes.With
Upper mainly around embodiments of the invention, but at art of the present invention, there is the technology of identical knowledge
Personnel can various change or amendment in addition according to its level.This type of change or amendment are as without departing from this
The technical scope that invention provides, all can be considered scope of the invention.Therewith, the extent of competence of the present invention is root
Depending on following request scope.
Claims (10)
1. the manufacture method of polyimide resin, it is characterised in that
Comprise and dissolve diamidogen in a solvent, form the 1st solution formation stages；
The benzophenone tetracarboxylic dianhydride of chemical formula (1) will be denoted as, be denoted as the benzophenone four of chemical formula (2)
Acid dianhydride and be denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (3) and be mixed in the 1st above-mentioned solution, institute
Produce the formation stages of the 2nd solution containing polyamic acid (PAA)；And
Heat treatment stages to above-mentioned 2nd solution；
Chemical formula (1)
Chemical formula (2)
Chemical formula (3)
The manufacture method of polyimide resin the most according to claim 1, it is characterised in that described
Diamidogen is aromatic diamine.
The manufacture method of polyimide resin the most according to claim 1, it is characterised in that described
Diamidogen be use following in one: 2,2'-double (trifluoromethyl)-4,4'-benzidine (2,2 '-TFDB), 3,3 '-
Double (trifluoromethyl)-4,4 '-benzidine (33 '-TFDB) and p-phenylenediamine.
The manufacture method of polyimide resin the most according to claim 1, it is characterised in that described in make
Solvent at least by the one in following: METHYLPYRROLIDONE (NMP) metacresol, dimethyl formyl
Amine (DMF), dimethyl sulfoxide (DMSO), acetone, ethyl acetate and dimethyl acetylamide (DMAC).
The manufacture method of polyimide resin the most according to claim 1, it is characterised in that comprise shape
After becoming above-mentioned 2nd solution, by the stage in the 2nd above-mentioned solution coatings to substrate.
The manufacture method of polyimide resin the most according to claim 5, it is characterised in that above-mentioned
2nd solution coatings to the stage on substrate, coating at least use following in one: Spin coating,
Doctorblade coating, Slotdie coating.
The manufacture method of polyimide resin the most according to claim 1, it is characterised in that described
The heat treatment stages of 2 solution, comprising above-mentioned 2nd solution in temperature is to carry out between 100 DEG C to 120 DEG C
1st heat treatment stages；And be 120 DEG C to 450 DEG C by the 2nd solution through the 1st heat treatment stages in temperature
Between carry out the 2nd heat treatment stages.
The manufacture method of polyimide resin the most according to claim 7, it is characterised in that described
Above-mentioned solvent in 2nd solution, for implementing 5 minutes to 20 minutes, is evaporated by the 1st heat treatment stages, it is thus achieved that
The stage of the high polyamic acid purified.
The manufacture method of polyimide resin the most according to claim 7, it is characterised in that described
Above-mentioned polyamic acid, for implementing 60 minutes to 90 minutes, by thermal polymerization, is entered by the 2nd heat treatment stages
The stage of row imidization.
The Kapton that the manufacture method of polyimide resin the most according to claim 1 obtains,
It is characterized in that, to be denoted as the benzophenone tetracarboxylic dianhydride of chemical formula (1) and to be denoted as chemical formula (2)
Benzophenone tetracarboxylic dianhydride and be denoted as (3) benzophenone tetracarboxylic dianhydride compounding substances with from aromatic diamine
The polyimides of middle acquisition is main component, and its yellow colour index is less than 2.0.
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| CN110092908B (en) * | 2019-04-03 | 2021-02-05 | 中国科学院化学研究所 | Polyimide film and preparation method and application thereof |
| CN112142999B (en) * | 2019-06-28 | 2023-03-28 | Skc株式会社 | Base film, method of manufacturing the same, and cover window and display device including the same |
| CN111187414B (en) * | 2020-02-14 | 2022-09-06 | 吉林奥来德光电材料股份有限公司 | High-performance transparent polyimide film and preparation method thereof |
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| 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 |
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| CN103524767B (en) * | 2013-10-30 | 2016-07-06 | 宏威高新材料有限公司 | The Novel electronic grade Kapton of a kind of low linear expansion coefficient and manufacture method thereof |
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