CN105001421A - Preparation of polyimide solid powder containing phenolic hydroxyl group and application thereof - Google Patents
Preparation of polyimide solid powder containing phenolic hydroxyl group and application thereof Download PDFInfo
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- CN105001421A CN105001421A CN201510391137.9A CN201510391137A CN105001421A CN 105001421 A CN105001421 A CN 105001421A CN 201510391137 A CN201510391137 A CN 201510391137A CN 105001421 A CN105001421 A CN 105001421A
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Abstract
The invention discloses preparation of a polyimide solid powder containing a phenolic hydroxyl group and an application of the polyimide solid powder. The preparation of the polyimide solid powder containing the phenolic hydroxyl group comprises the following steps: dissolving 2,2'-bis(3-amino-4-hydroxyphenyl)propane in N-methyl-2-pyrrolidone under the protection of inert gas, adding 4,4'-oxydiphthalic anhydride, stirring for 0.5-3 h, adding an azeotropic dehydrating agent and a catalyst, heating up to 180-240 DEG C, conducting refluxing for 3-4 h, cooling to room temperature, pouring a mixed liquid into a precipitant under the high-speed stirring condition so as to separate out a solid product, filtering, washing, and drying to obtain a PI solid powder. The PI solid powder is prepared by a one-step method. The preparation is simple to operate. Yield is high and reaches 95% or above. A thin film is prepared by a conventional two-step method: a dissoluble PI solution is firstly prepared; and then, a solvent is removed by a corresponding measure. Existing PI thin-film production equipment can completely be used in the preparation provided by the invention. The preparation is beneficial to industrialization of the product.
Description
Technical field
The invention belongs to the preparation field of Kapton, be specifically related to a kind of preparation and application thereof of phenolic hydroxy group polyimide solids powder.
Background technology
Polyimide (polyimide, be called for short PI) be macromolecular material molecule main chain containing imide ring structure, it has remarkable dielectric, machinery, radiation hardness, the performance such as heat-resisting within the scope of 200-400 DEG C, is one of best organic polymer material of a class over-all properties.Due to the over-all properties of its excellence, PI has been widely used in the fields such as microelectronics, aviation, nanometer, separatory membrane, liquid crystal, laser, space flight.
1961, it was the PMMI film (PMDA-ODA type, Kapton) of monomer that du pont company takes the lead in producing with pyromellitic dianhydride.1978, company of Ube Industries Ltd. have developed novel poly-biphenyl tetracarboxylic imide, and less than Kapton linear expansivity with its film performance prepared, and otherwise performance is also improved.Along with developing rapidly of the new industry such as be representative with microelectronics, automobile industry, various countries investigator is while ensureing the thermotolerance of the excellence that PI is intrinsic, omnibearing exploration and improvement have also been carried out to the performance of other side, the new variety such as photosensitivity PI, transparent PI, PI used for electronic packaging continue to bring out, accelerate and PI is carried out research and apply as a kind of functional high molecule material, the Application Areas of PI is constantly expanded.
The country that the whole world has the Kapton processing technology of comparative maturity is not a lot, mainly concentrates on the U.S. and Japan.The PI used as thin-film material not only can high-low temperature resistant, dimensional stabilizing, good toughness, and can the use of long-time safety and stability.Wherein excellent with the Apical film performance of the Upilex film of the Kapton film of du pont company, Ube Industries Ltd. and Japanese Zhong Yuan, occupy the market of the overwhelming majority.Start late in China's film aspect, technology is compared down a lot of deficiency, current main exit Korea S, Russia, Taiwan and south east asia.
Usually, functional PI film is prepared by particular monomers on the one hand, then obtains by adding the filler modified traditional PI film of functional nano on the other hand.
About the research work in phenolic hydroxy group or ehter bond polyimide material field has many reports:
It is the polyamic acid of the various structures of monomer and the polyimide resin of correspondence thereof that Donghua University Yu Xin sea etc. has been synthesized with Isosorbide-5-Nitrae-bis-(4-amino-benzene oxygen) benzene and pyromellitic acid anhydride.
Chinese invention patent CN101003716A discloses a kind of preparation method of binder of polyimide of containing phenolic hydroxyl group.
Chinese invention patent CN1927908A discloses a kind of preparation method of phenolic hydroxyl group containing polyimide powder.
Chinese invention patent CN102516541A discloses a kind of polyimide of phenolic hydroxy group.
Chinese invention patent CN102650080A discloses polyimide fiber spinning solution based on 3,3 '-diamino-4,4 '-dihydroxybiphenyl and preparation thereof.
Chinese invention patent CN102660796A discloses polyimide fiber spinning solution based on two (3-amino-4-hydroxylphenyl) HFC-236fa of 2,2-and preparation thereof.
Chinese patent CN102807675A discloses a kind of flexible transparent polyimide film material and preparation method thereof.
Chinese patent CN103524768A discloses a kind of Novel electronic grade Kapton and production method thereof of low coefficient of linear expansion.
Chinese patent CN101484500 discloses thermoplastic polyimide, uses the laminated Kapton of this polyimide and the laminated Kapton of tinsel.
Summary of the invention
For solving the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is the preparation method providing a kind of phenolic hydroxy group polyimide solids powder.
Another object of the present invention is to the phenolic hydroxy group polyimide solids powder providing above-mentioned preparation method to obtain.
Another object of the present invention is to provide above-mentioned phenolic hydroxy group polyimide solids powder preparing the application in phenolic hydroxy group Kapton.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method of phenolic hydroxy group polyimide solids powder, comprise the following steps: under protection of inert gas, by 2, 2 '-bis-(3-amino-4-hydroxylphenyl) propane (BAHPP) is dissolved in METHYLPYRROLIDONE (NMP), then 4 are added, 4 '-Biphenyl Ether dianhydride (OPDA), after stirring for some time, add azeotropy dehydrant and catalyzer, be warmed up to 180 DEG C ~ 240 DEG C, reflux 3 ~ 4 hours, be cooled to room temperature, mixed solution is poured in the precipitating agent under high-speed stirring state, separate out solid product, filter, washing, dry, obtain described phenolic hydroxy group polyimide solids powder (i.e. PI pressed powder).
Described 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane (BAHPP) and 4, the mol ratio of 4 '-Biphenyl Ether dianhydride (OPDA) is 1:1; 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane (BAHPP) and 4, the quality of 4 '-Biphenyl Ether dianhydride (OPDA) accounts for 10% ~ 20% of total reaction system.
Described rare gas element is nitrogen, argon gas or helium.Described churning time can be preferably 0.5h ~ 3h.
Described azeotropy dehydrant is one or more in benzene,toluene,xylene, chlorobenzene and orthodichlorobenzene.
The not special requirement of adding proportion of described azeotropy dehydrant and strong polar non-proton organic solvent METHYLPYRROLIDONE, rule of thumb can be defined as 1:6 by the two volume ratio.
Described catalyzer is γ-valerolactone and pyridine.The addition not special requirement of described catalyzer.
The mixed solution of described precipitating agent to be volume ratio the be first alcohol and water of 1:1.
The phenolic hydroxy group polyimide solids powder that above-mentioned preparation method obtains.
Above-mentioned phenolic hydroxy group polyimide solids powder can be used for preparing phenolic hydroxy group Kapton, concrete steps are: get a certain amount of phenolic hydroxy group polyimide solids powder in strong polar non-proton organic solvent, make certain density solvable PI solution, extracting coats on clean sheet glass (slide glass) in right amount equably, dry 2 ~ 5min at 80 DEG C ~ 95 DEG C, naturally cooling, demoulding, obtains described phenolic hydroxy group Kapton.
Described strong polar non-proton organic solvent is selected from one or more in DMF, N,N-dimethylacetamide, N-ethyl-2-pyrrolidone, METHYLPYRROLIDONE and dimethyl sulfoxide (DMSO).
The massfraction of described solvable PI solution is 10% ~ 20%.
The polyimide used as thin-film material at present and the adhesive property of other materials or consistency mostly bad, the main method improving this deficiency introduces hydroxyl reactive group exactly, the present invention utilizes the diamine monomer containing hydroxyl reactive group---and 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and dianhydride monomer prepare the polyimide of hydroxyl, not only improve consistency or the adhesiveproperties of itself and other materials, ehter bond is introduced in PI molecular chain simultaneously, enhance the snappiness of PI film.In addition, due to the existence of hydroxyl, can be used as the matrix resin of light-sensitive polyimide material, also with various kinds of resin system (as epoxy resin), chemical reaction can occur and obtain the novel material system having various kinds of resin system premium properties concurrently.Chemical equation of the present invention is shown below:
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) containing phenolic hydroxyl group in the polyimide prepared by the present invention, consistency or the adhesiveproperties of itself and other materials can be improved.
(2) containing ehter bond in the polyimide prepared by the present invention, the snappiness of PI film can be improved.
(3) preparation of PI adopts single stage method, simple to operate, and yield is high.
(4) preparation of film adopts conventional two-step approach, namely first makes solvable PI solution, then the removal solvent that takes appropriate measures, and the equipment of existing production PI film can be utilized completely to implement the present invention, be conducive to the industrialization of product.
Accompanying drawing explanation
Fig. 1 is fourier transform infrared spectrometry (FTIR) spectrogram of embodiment 1 gained phenolic hydroxy group polyimide (PI);
Fig. 2 is thermogravimetic analysis (TGA) (TGA) spectrogram of embodiment 1 gained phenolic hydroxy group polyimide (PI);
Fig. 3 is embodiment 1 gained phenolic hydroxy group Kapton transmittance spectrogram at different wavelengths.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Use in the embodiment of the present invention 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane is according to the document (" FeCl such as Long Chunmei etc. " synthesis of 2,2-bis-(4-hydroxyl-3-nitrophenyl) propane " and Zhou Ying
36H
2o/C Compounds with Hydrazine Hydrate Catalyzed reduction preparation 2,2-bis-(4-hydroxyl-3-is amino) phenyl-propane ") disclosed in method prepare, concrete steps are as follows:
22.8g (0.1mol) dihydroxyphenyl propane, 35mL concentrated nitric acid and 95mL water are added in reaction flask, stirring at room temperature 4h; After reaction terminates, filtrations, washing, recrystallization, dry must deep yellow needle-like crystal;
Getting the above-mentioned deep yellow needle-like crystal of 16.9g (0.053mol), 120mL ethanol and 1.5g Pd/C joins in reaction flask, is warmed up to 70 DEG C, under micro-reflux conditions that boils, slowly drips w (H
2nNH
2the hydrazine hydrate (20mL) of)=80%, maintains reaction 6h; Reaction terminates rear filtered while hot, and mother liquor separates out white crystal, and filtration, washing, drying, obtain 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane.
Nitrogen in the embodiment of the present invention also can replace with argon gas or helium.
Embodiment 1
Prepare phenolic hydroxy group Kapton according to the following steps:
(1) phenolic hydroxy group polyimide solids powder is prepared: at N
2under protection, by 2.58g (10mmol) 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 24.34g METHYLPYRROLIDONE add in reaction flask, after stirring and dissolving, add 4,4 '-Biphenyl Ether dianhydride in batches, 3.10g (10mmol) altogether, after stirring reaction 30min, add 4.06g dimethylbenzene and 0.16g pyridine and 0.10g γ-valerolactone, be warmed up to 180 DEG C of backflow azeotropic dehydrations 3.5 hours; After reaction terminates, be cooled to room temperature, with methyl alcohol: the mixing solutions precipitated product of water=1:1 (V/V), filter, washing, vacuum-drying, obtains PI pressed powder;
(2) phenolic hydroxy group Kapton is prepared: get the dried PI pressed powder of 1.00g in 9.00g METHYLPYRROLIDONE, getting after its dissolving is completely coated on clean sheet glass in right amount equably, then carefully sheet glass is put in the air dry oven of modulated good level, 3min is dried at 90 DEG C, naturally cool to room temperature, demoulding can obtain described phenolic hydroxy group Kapton.
Utilize fourier transform infrared spectroscopy to detect gained polyimide solids powder in embodiment 1, find that this pressed powder has obvious imide ring vibration performance absorption peak (1778cm
-1, 1712cm
-1and 1378cm
-1) and obvious OH absorption peak (3432cm
-1), 1106cm
-1place is the absorption peak of ehter bond (-O-) between two phenyl ring, and the charateristic avsorption band 1660cm of polyamic acid
-1, 1559cm
-1undiscovered, as shown in Figure 1.
Thermogravimetic analysis (TGA) is carried out to gained polyimide solids powder in embodiment 1, the temperature of weightlessness more than 5% about 300 DEG C of temperature spots, as shown in Figure 2.
The ultraviolet cut-on wavelength utilizing UV-2550 ultraviolet-visible spectrophotometer to record gained Kapton in embodiment 1 is about 348nm, visible ray maximum transmission more than 80%, as shown in Figure 3.
Embodiment 2
Prepare phenolic hydroxy group Kapton according to the following steps:
(1) phenolic hydroxy group polyimide solids powder is prepared: at N
2under protection, by 2.58g (10mmol) 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 48.69g METHYLPYRROLIDONE add in reaction flask, after stirring and dissolving, add 4,4 '-Biphenyl Ether dianhydride in batches, 3.10g (10mmol) altogether, after stirring reaction 2h, add 8.11g dimethylbenzene and 0.16g pyridine and 0.10g γ-valerolactone, be warmed up to 210 DEG C of backflow azeotropic dehydrations 4 hours; After reaction terminates, be cooled to room temperature, with methyl alcohol: the mixing solutions precipitated product of water=1:1 (V/V), filter, washing, vacuum-drying, obtains PI pressed powder;
(2) phenolic hydroxy group Kapton is prepared: get the dried PI pressed powder of 1.00g in 9.00g N-ethyl-2-pyrrolidone, getting after its dissolving is completely coated on clean sheet glass in right amount equably, then carefully sheet glass is put in the air dry oven of modulated good level, 5min is dried at 80 DEG C, naturally cool to room temperature, demoulding can obtain described phenolic hydroxy group Kapton.
Embodiment 3
Prepare phenolic hydroxy group Kapton according to the following steps:
(1) phenolic hydroxy group polyimide solids powder is prepared: at N
2under protection, by 2.58g (10mmol) 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 32.46g METHYLPYRROLIDONE add in reaction flask, after stirring and dissolving, add 4,4 '-Biphenyl Ether dianhydride in batches, 3.10g (10mmol) altogether, after stirring reaction 30min, add 5.41g dimethylbenzene and 0.16g pyridine and 0.10g γ-valerolactone, be warmed up to 240 DEG C of backflow azeotropic dehydration 3h; After reaction terminates, be cooled to room temperature, with methyl alcohol: the mixing solutions precipitated product of water=1:1 (V/V), filter, washing, vacuum-drying, obtains PI pressed powder;
(2) phenolic hydroxy group Kapton is prepared: get the dried PI pressed powder of 1.00g in 4.00g N, in dinethylformamide, getting after its dissolving is completely coated on clean sheet glass in right amount equably, then carefully sheet glass is put in the air dry oven of modulated good level, 2min is dried at 85 DEG C, naturally cool to room temperature, demoulding can obtain described phenolic hydroxy group Kapton.
Embodiment 4
Prepare phenolic hydroxy group Kapton according to the following steps:
(1) phenolic hydroxy group polyimide solids powder is prepared: at N
2under protection, by 2.58g (10mmol) 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 32.46g METHYLPYRROLIDONE add in reaction flask, after stirring and dissolving, add 4,4 '-Biphenyl Ether dianhydride in batches, 3.10g (10mmol) altogether, after stirring reaction 30min, add 5.41g dimethylbenzene and 0.16g pyridine and 0.10g γ-valerolactone, be warmed up to 180 DEG C of backflow azeotropic dehydration 3h; After reaction terminates, be cooled to room temperature, with methyl alcohol: the mixing solutions precipitated product of water=1:1 (V/V), filter, washing, vacuum-drying, obtains PI pressed powder;
(2) phenolic hydroxy group Kapton is prepared: get the dried PI pressed powder of 1.00g in 5.67g METHYLPYRROLIDONE, getting after its dissolving is completely coated on clean sheet glass in right amount equably, then carefully sheet glass is put in the air dry oven of modulated good level, 3min is dried at 80 DEG C, naturally cool to room temperature, demoulding can obtain described phenolic hydroxy group Kapton.
Embodiment 5
Prepare phenolic hydroxy group Kapton according to the following steps:
(1) phenolic hydroxy group polyimide solids powder is prepared: at N
2under protection, by 2.58g (10mmol) 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 24.34g METHYLPYRROLIDONE add in reaction flask, after stirring and dissolving, add 4,4 '-Biphenyl Ether dianhydride in batches, 3.10g (10mmol) altogether, after stirring reaction 2h, add 4.06g dimethylbenzene and 0.16g pyridine and 0.10g γ-valerolactone, be warmed up to 210 DEG C of backflow azeotropic dehydrations 3.5 hours; After reaction terminates, be cooled to room temperature, with methyl alcohol: the mixing solutions precipitated product of water=1:1 (V/V), filter, washing, vacuum-drying, obtains PI pressed powder;
(2) phenolic hydroxy group Kapton is prepared: get the dried PI pressed powder of 1.00g in 4.00g dimethyl sulfoxide (DMSO), getting after its dissolving is completely coated on clean sheet glass in right amount equably, then carefully sheet glass is put in the air dry oven of modulated good level, 2min is dried at 90 DEG C, naturally cool to room temperature, demoulding can obtain described phenolic hydroxy group Kapton.
Embodiment 6
Prepare phenolic hydroxy group Kapton according to the following steps:
(1) phenolic hydroxy group polyimide solids powder is prepared: at N
2under protection, by 2.58g (10mmol) 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 24.34g METHYLPYRROLIDONE add in reaction flask, after stirring and dissolving, add 4,4 '-Biphenyl Ether dianhydride in batches, 3.10g (10mmol) altogether, after stirring reaction 3h, add 4.06g dimethylbenzene and 0.16g pyridine and 0.10g γ-valerolactone, be warmed up to 180 DEG C of backflow azeotropic dehydration 4h; After reaction terminates, be cooled to room temperature, with methyl alcohol: the mixing solutions precipitated product of water=1:1 (V/V), filter, washing, vacuum-drying, obtains PI pressed powder;
(2) phenolic hydroxy group Kapton is prepared: get the dried PI pressed powder of 1.00g in 5.67g METHYLPYRROLIDONE, getting after its dissolving is completely coated on clean sheet glass in right amount equably, then carefully sheet glass is put in the air dry oven of modulated good level, 3min is dried at 95 DEG C, naturally cool to room temperature, demoulding can obtain described phenolic hydroxy group Kapton.
Embodiment 7
Prepare phenolic hydroxy group Kapton according to the following steps:
(1) phenolic hydroxy group polyimide solids powder is prepared: at N
2under protection, by 2.58g (10mmol) 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 48.69g METHYLPYRROLIDONE add in reaction flask, after stirring and dissolving, add 4,4 '-Biphenyl Ether dianhydride in batches, 3.10g (10mmol) altogether, after stirring reaction 30min, add 8.11g dimethylbenzene and 0.16g pyridine and 0.10g γ-valerolactone, be warmed up to 240 DEG C of backflow azeotropic dehydration 3.5h; After reaction terminates, be cooled to room temperature, with methyl alcohol: the mixing solutions precipitated product of water=1:1 (V/V), filter, washing, vacuum-drying, obtains PI pressed powder;
(2) phenolic hydroxy group Kapton is prepared: get the dried PI pressed powder of 1.00g in 4.00g METHYLPYRROLIDONE, getting after its dissolving is completely coated on clean sheet glass in right amount equably, then carefully sheet glass is put in the air dry oven of modulated good level, 3min is dried at 90 DEG C, naturally cool to room temperature, demoulding can obtain described phenolic hydroxy group Kapton.
Embodiment 8
Prepare phenolic hydroxy group Kapton according to the following steps:
(1) phenolic hydroxy group polyimide solids powder is prepared: at N
2under protection, by 2.58g (10mmol) 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 48.69g METHYLPYRROLIDONE add in reaction flask, after stirring and dissolving, add 4,4 '-Biphenyl Ether dianhydride in batches, 3.10g (10mmol) altogether, after stirring reaction 2h, add 8.11g dimethylbenzene and 0.16g pyridine and 0.10g γ-valerolactone, be warmed up to 180 DEG C of backflow azeotropic dehydration 3.5h; After reaction terminates, be cooled to room temperature, with methyl alcohol: the mixing solutions precipitated product of water=1:1 (V/V), filter, washing, vacuum-drying, obtains PI pressed powder;
(2) phenolic hydroxy group Kapton is prepared: get the dried PI pressed powder of 1.00g in 5.67g N, in N-N,N-DIMETHYLACETAMIDE, getting after its dissolving is completely coated on clean sheet glass in right amount equably, then carefully sheet glass is put in the air dry oven of modulated good level, 5min is dried at 90 DEG C, naturally cool to room temperature, demoulding can obtain described phenolic hydroxy group Kapton.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a phenolic hydroxy group polyimide solids powder, it is characterized in that, comprise the following steps: under protection of inert gas, by 2, 2 '-bis-(3-amino-4-hydroxylphenyl) propane is dissolved in METHYLPYRROLIDONE, then 4 are added, 4 '-Biphenyl Ether dianhydride, after stirring 0.5h ~ 3h, add azeotropy dehydrant and catalyzer, be warmed up to 180 DEG C ~ 240 DEG C, reflux 3 ~ 4 hours, be cooled to room temperature, mixed solution is poured in the precipitating agent under whipped state, separate out solid product, filter, washing, dry, obtain described phenolic hydroxy group polyimide solids powder.
2. the preparation method of a kind of phenolic hydroxy group polyimide solids powder according to claim 1, is characterized in that, described 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 4, and the mol ratio of 4 '-Biphenyl Ether dianhydride is 1:1; Described 2,2 '-bis-(3-amino-4-hydroxylphenyl) propane and 4, the quality of 4 '-Biphenyl Ether dianhydride accounts for 10% ~ 20% of total reaction system.
3. the preparation method of a kind of phenolic hydroxy group polyimide solids powder according to claim 1, it is characterized in that, described rare gas element is nitrogen, argon gas or helium.
4. the preparation method of a kind of phenolic hydroxy group polyimide solids powder according to claim 1, it is characterized in that, described azeotropy dehydrant is one or more in benzene,toluene,xylene, chlorobenzene and orthodichlorobenzene.
5. the preparation method of a kind of phenolic hydroxy group polyimide solids powder according to claim 1, it is characterized in that, described catalyzer is γ-valerolactone and pyridine.
6. the preparation method of a kind of phenolic hydroxy group polyimide solids powder according to claim 1, is characterized in that, the mixed solution of described precipitating agent to be volume ratio the be first alcohol and water of 1:1.
7. the phenolic hydroxy group polyimide solids powder obtained by preparation method described in any one of claim 1 to 6.
8. phenolic hydroxy group polyimide solids powder according to claim 7 is preparing the application in phenolic hydroxy group Kapton, it is characterized in that, the concrete steps of described application are: get a certain amount of phenolic hydroxy group polyimide solids powder in strong polar non-proton organic solvent, make certain density solvable PI solution, extracting coats on clean sheet glass or slide glass in right amount equably, dry 2 ~ 5min at 80 ~ 95 DEG C, naturally cooling, demoulding, obtains described phenolic hydroxy group Kapton.
9. application according to claim 8, it is characterized in that, described strong polar non-proton organic solvent is selected from one or more in DMF, N,N-dimethylacetamide, N-ethyl-2-pyrrolidone, METHYLPYRROLIDONE and dimethyl sulfoxide (DMSO).
10. application according to claim 8, is characterized in that, the massfraction of described solvable PI solution is 10% ~ 20%.
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| CN109694574A (en) * | 2018-12-17 | 2019-04-30 | 无锡创彩光学材料有限公司 | A kind of high adhesiveness Kapton, preparation method and flexible copper-clad plate |
| CN114957660A (en) * | 2021-02-26 | 2022-08-30 | 新应材股份有限公司 | Polyimide resin composition, polyimide resin adhesive layer, laminate, and method for producing electronic component |
| CN115232472A (en) * | 2022-07-20 | 2022-10-25 | 中国航空工业集团公司济南特种结构研究所 | Bismaleimide resin industrial modification prepolymerization method |
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