CN101407588A - Preparation of polyimide film - Google Patents
Preparation of polyimide film Download PDFInfo
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- CN101407588A CN101407588A CNA2008102095316A CN200810209531A CN101407588A CN 101407588 A CN101407588 A CN 101407588A CN A2008102095316 A CNA2008102095316 A CN A2008102095316A CN 200810209531 A CN200810209531 A CN 200810209531A CN 101407588 A CN101407588 A CN 101407588A
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Abstract
The invention discloses a preparation method of a polyimide film, which relates to a preparation method of a high molecular polymer film. The invention aims at providing a synthesis method of a polybenzoxazole imide film containing a single oxazole ring, which solves the problem of poor film forming ability of polybenzoxazole imide containing a dual oxazole ring under a condition without sacrificing the thermal property of a polymer. The method includes the following steps: firstly, 5-amido-2-(phenetidine)benzoxazole and N, N'-dimethylacetamide are mixed and stirred and added with aromatic dianhydride and then a polyamide acid is obtained after reaction is finished; secondly, the polyamide acid prepared in the first step is casted into film and dried; thirdly, heat treatment is carried out; and fourthly, the polyimide film is obtained through water boiling and stripping. The polyimide film prepared by the method is good in thermal property, strong in acid resistance and high in mechanical property. The preparation method is simple and has good film forming performance.
Description
Technical field
The present invention relates to the preparation method of high molecular polymer film.
Background technology
Along with the development of spationautics, Yan Zhi various aircraft are had higher requirement to the resistance to elevated temperatures of material recently.In numerous materials, polyimide becomes the heat subject of scientists study with its excellent high thermal resistance, radiation resistance, lower temperature resistance, mechanics mechanical property and good chemical physical stability etc.In the research of fire resistant polyimide (PI), stable on heating raising mainly is to start with from the molecular structure of design polyimide, and mainly is that the diamines from synthesis of polyimides, the structure of dianhydride monomer are launched research for the design of molecular structure.In recent years, in order to improve the thermotolerance of polyimide, chemist has been introduced in the PI molecule by the synthetic method and has been contained sulphur, nitrogen, the equiatomic heterocycle of oxygen, as benzoxazole, benzoglyoxaline, pyrrole throat, quinoxaline etc.In polymer monomer, introduce double thiazole ring, can improve the thermal characteristics of polyimide.But because polymkeric substance diamine monomer De Shuan oxazole symmetrical structure, make the polymer molecule chain rigidity bigger, crystallinity is stronger, only can generate Kapton with the reaction of the stronger aromatic dianhydride of kindliness, and Kapton is more crisp, and aromatic dianhydride such as pyromellitic acid anhydride, the bibenzene tetracarboxylic dianhydride etc. stronger with rigidity then can not form film.
Summary of the invention
The synthetic method that the purpose of this invention is to provide Han Dan oxazole ring polybenzoxazole imide membrane, this method have solved the problem of Han double thiazole ring polybenzoxazole imide film-forming properties difference under the condition of sacrificial polymer thermal characteristics not.
The preparation method of Kapton realizes according to the following steps among the present invention: one, (p-aminophenyl) benzoxazole is dissolved in the N that handles through vapor enrichment, in N '-N,N-DIMETHYLACETAMIDE, adds pyromellitic acid anhydride again, at N with 5-amino-2-
2Protection under, be to react 3～6 hours under 0～5 ℃ of condition in temperature, obtain polyamic acid; Two, the polyamic acid with step 1 preparation is poured on the sheet glass, casting film-forming, at room temperature dry 3～4 hours, in vacuum drier dry 24～30 hours then; Three, the sheet glass that will handle through step 2 heats up with the temperature rise rate of 10 ℃/min, successively 100 ℃, 150 ℃, 200 ℃ and 300 ℃ of each constant temperature 1 hour, 350 ℃ of constant temperature 0.5 hour; Four, will be cooled to room temperature through the sheet glass that step 3 is handled, the poach demoulding promptly gets Kapton then; Wherein the structural formula of polyimide is
N represents the polymerization degree, 350≤n≤400; Wherein in the step 1 pyromellitic acid anhydride and 5-base-2-(mol ratio of p-aminophenyl) benzoxazole is 1～1.02: 1; The N that every 25ml handles through vapor enrichment in the step 1 is dissolved with 4.44mmol5-amino-2-(p-aminophenyl) benzoxazole in N '-N,N-DIMETHYLACETAMIDE.
The preparation method of another kind of Kapton realizes according to the following steps among the present invention: one, (p-aminophenyl) benzoxazole is dissolved in the N that handles through vapor enrichment with 5-amino-2-, in N '-N,N-DIMETHYLACETAMIDE, add 2 again, 2 ' 3,3 '-bibenzene tetracarboxylic dianhydride is at N
2Protection under, be to react 3～6 hours under 0～5 ℃ of condition in temperature, obtain polyamic acid; Two, the polyamic acid with step 1 preparation is poured on the sheet glass, casting film-forming, at room temperature dry 3～4 hours, in vacuum drier dry 24～30 hours then; Three, the sheet glass that will handle through step 2 heats up with the temperature rise rate of 10 ℃/min, successively 100 ℃, 150 ℃, 200 ℃ and 300 ℃ of each constant temperature 1 hour, 350 ℃ of constant temperature 0.5 hour; Four, will be cooled to room temperature through the sheet glass that step 3 is handled, the poach demoulding promptly gets Kapton then; Wherein the structural formula of polyimide is
N represents the polymerization degree, 350≤n≤400; Wherein in the step 12,2 ' 3, (mol ratio of p-aminophenyl) benzoxazole is 1～1.02: 1 for 3 '-bibenzene tetracarboxylic dianhydride and 5-amino-2-; The N that every 25ml handles through vapor enrichment in the step 1 is dissolved with 4.44mmol5-amino-2-(p-aminophenyl) benzoxazole in N '-N,N-DIMETHYLACETAMIDE.
The preparation method of another kind of Kapton realizes according to the following steps among the present invention: one, (p-aminophenyl) benzoxazole is dissolved in the N that handles through vapor enrichment, adds diaether dianhydride in N '-N,N-DIMETHYLACETAMIDE again, at N with 5-amino-2-
2Protection under, be to react 3～6 hours under 0～5 ℃ of condition in temperature, obtain polyamic acid; Two, the polyamic acid with step 1 preparation is poured on the sheet glass, casting film-forming, at room temperature dry 3～4 hours, in vacuum drier dry 24～30 hours then; Three, the sheet glass that will handle through step 2 heats up with the temperature rise rate of 10 ℃/min, successively 100 ℃, 150 ℃, 200 ℃ and 300 ℃ of each constant temperature 1 hour, 350 ℃ of constant temperature 0.5 hour; Four, will be cooled to room temperature through the sheet glass that step 3 is handled, the poach demoulding promptly gets Kapton then; Wherein the structural formula of polyimide is
N represents the polymerization degree, 350≤n≤400; Wherein in the step 1 diaether dianhydride and 5-amino-2-(mol ratio of p-aminophenyl) benzoxazole is 1～1.02: 1; The N that every 25ml handles through vapor enrichment in the step 1 is dissolved with 4.44mmol5-amino-2-(p-aminophenyl) benzoxazole in N '-N,N-DIMETHYLACETAMIDE.
Adopt the diamine monomer of Dan oxazole unsymmetrical structure and the aromatic dianhydride polybenzoxazole imide that is polymerized among the present invention, can not sacrifice its thermotolerance and form the higher film of mechanical property, compared with prior art, the mechanical property of synthetic polybenzoxazole imide membrane of the present invention has improved 50%; Theoretically, as aromatic dianhydride and 5-amino-2-(when the mol ratio of p-aminophenyl) benzoxazole is 1: 1, the viscosity of the polyamic acid of gained is the highest, the relative molecular mass maximum, but unavoidably there is moisture in reaction system, the aromatic dianhydride hydrolysis is lost activity, therefore a little excessive meeting of aromatic dianhydride makes the viscosity of the polyamic acid that obtains bigger, but the amount of dianhydride increases too many, there are not an amount of diamines and its polymerization, the hydrolysis of dianhydride is more serious, and then viscosity is reduced, the aromatic dianhydride that adopts among the present invention and 5-amino-2-(p-aminophenyl) benzoxazole mol ratio are 1～1.02: 1, and this mole specific energy makes the viscosity of polyamic acid reach maximum value, thereby makes the relative molecular mass maximum of the Kapton that makes; Of the present invention being reflected in the ice-water bath carried out, 0～5 ℃ of controlled temperature because aromatic dianhydride with-(heat release in reaction process of p-aminophenyl) benzoxazole, low temperature helps reaction forward to carry out amino-2-, and then obtains high molecular weight polymers.
The Kapton that the present invention makes can only be dissolved in the vitriol oil, illustrates that the Kapton that the present invention makes has stronger acid resistance.
Description of drawings
Fig. 1 is the infrared spectrogram of Kapton, wherein A is for the pyromellitic acid anhydride being the infrared spectrogram of the Kapton that makes of raw material, B is with 2,2 ' 3,3 '-bibenzene tetracarboxylic dianhydride is the infrared spectrogram of the Kapton that makes of raw material, and C is for the diaether dianhydride being the infrared spectrogram of the Kapton that makes of raw material.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of present embodiment Kapton realizes according to the following steps: one, (p-aminophenyl) benzoxazole is dissolved in the N that handles through vapor enrichment with 5-amino-2-, in N '-N,N-DIMETHYLACETAMIDE, add pyromellitic acid anhydride again, at N
2Protection under, be to react 3～6 hours under 0～5 ℃ of condition in temperature, obtain polyamic acid; Two, the polyamic acid with step 1 preparation is poured on the sheet glass, casting film-forming, at room temperature dry 3～4 hours, in vacuum drier dry 24～30 hours then; Three, the sheet glass that will handle through step 2 heats up with the temperature rise rate of 10 ℃/min, successively 100 ℃, 150 ℃, 200 ℃ and 300 ℃ of each constant temperature 1 hour, 350 ℃ of constant temperature 0.5 hour; Four, will be cooled to room temperature through the sheet glass that step 3 is handled, the poach demoulding promptly gets Kapton then; Wherein the structural formula of polyimide is
N represents the polymerization degree, 350≤n≤400; Wherein in the step 1 pyromellitic acid anhydride and 5-base-2-(mol ratio of p-aminophenyl) benzoxazole is 1～1.02: 1; The N that every 25ml handles through vapor enrichment in the step 1 is dissolved with 4.44mmol5-amino-2-(p-aminophenyl) benzoxazole in N '-N,N-DIMETHYLACETAMIDE.
Curve A from Fig. 1 present embodiment as can be seen generates the polyimide of Han oxazole ring, and imidization is complete; The polyamic acid viscosity that present embodiment makes is 1.20dL/g, and the Kapton that present embodiment makes can only be dissolved in the vitriol oil; The second-order transition temperature of the Kapton that present embodiment makes is 312 ℃, and the temperature during thermal destruction total mass 5% is 553 ℃, and the temperature during thermal destruction total mass 10% is 577 ℃, and the temperature when thermal weight loss speed is maximum is 595 ℃; The breaking tenacity of the Kapton that present embodiment makes is 10.5Mpa.
Embodiment two: what present embodiment and embodiment one were different is that temperature of reaction is 1～4 ℃ in the step 1.Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is that temperature of reaction is 3 ℃ in the step 1.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is that temperature of reaction is 0 ℃ in the step 1.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is that temperature of reaction is 5 ℃ in the step 1.Other is identical with embodiment one.
Embodiment six: present embodiment and embodiment one are different be in the step 1 reaction times be 4～5 hours.Other is identical with embodiment one.
Embodiment seven: present embodiment and embodiment one are different be in the step 1 reaction times be 4.5 hours.Other is identical with embodiment one.
Embodiment eight: present embodiment and embodiment one are different be in the step 1 reaction times be 3 hours.Other is identical with embodiment one.
Embodiment nine: present embodiment and embodiment one are different be in the step 1 reaction times be 6 hours.Other is identical with embodiment one.
Embodiment ten: present embodiment and embodiment one are different be in the step 1 pyromellitic acid anhydride and 5-amino-2-(mol ratio of p-aminophenyl) benzoxazole is 1: 1.Other is identical with embodiment one.
Embodiment 11: present embodiment and embodiment one are different be in the step 1 pyromellitic acid anhydride and 5-amino-2-(mol ratio of p-aminophenyl) benzoxazole is 1.02: 1.Other is identical with embodiment one.
Embodiment 12: the preparation method of present embodiment Kapton realizes according to the following steps: one, (p-aminophenyl) benzoxazole is dissolved in the N that handles through vapor enrichment with 5-amino-2-, in N '-N,N-DIMETHYLACETAMIDE, add 2 again, 2 ' 3,3 '-bibenzene tetracarboxylic dianhydride is at N
2Protection under, be to react 3～6 hours under 0～5 ℃ of condition in temperature, obtain polyamic acid; Two, the polyamic acid with step 1 preparation is poured on the sheet glass, casting film-forming, at room temperature dry 3～4 hours, in vacuum drier dry 24～30 hours then; Three, the sheet glass that will handle through step 2 heats up with the temperature rise rate of 10 ℃/min, successively 100 ℃, 150 ℃, 200 ℃ and 300 ℃ of each constant temperature 1 hour, 350 ℃ of constant temperature 0.5 hour; Four, will be cooled to room temperature through the sheet glass that step 3 is handled, the poach demoulding promptly gets Kapton then; Wherein the structural formula of polyimide is
N represents the polymerization degree, 350≤n≤400; Wherein in the step 12,2 ' 3, (mol ratio of p-aminophenyl) benzoxazole is 1～1.02: 1 for 3 '-bibenzene tetracarboxylic dianhydride and 5-amino-2-; The N that every 25ml handles through vapor enrichment in the step 1, N is dissolved with 4.44mmol5-amino-2-(p-aminophenyl) benzoxazole in the-N,N-DIMETHYLACETAMIDE.
Curve B from Fig. 1 present embodiment as can be seen generates the polyimide of Han oxazole ring, and imidization is complete; The polyamic acid viscosity that present embodiment makes is 1.21dL/g, and the Kapton that present embodiment makes can only be dissolved in the vitriol oil; The second-order transition temperature of the Kapton that present embodiment makes is 314 ℃, and the temperature during thermal destruction total mass 5% is 574 ℃, and the temperature during thermal destruction total mass 10% is 594 ℃, and the temperature when thermal weight loss speed is maximum is 612 ℃; The breaking tenacity of the Kapton that present embodiment makes is 223.2Mpa, and elongation at break is 5.74%, and Young's modulus is 3.91Gpa.
Embodiment 13: what present embodiment and embodiment 12 were different is that temperature of reaction is 1～4 ℃ in the step 1.Other is identical with embodiment 12.
Embodiment 14: what present embodiment and embodiment 12 were different is that temperature of reaction is 3 ℃ in the step 1.Other is identical with embodiment 12.
Embodiment 15: what present embodiment and embodiment 12 were different is that temperature of reaction is 0 ℃ in the step 1.Other is identical with embodiment 12.
Embodiment 16: what present embodiment and embodiment 12 were different is that temperature of reaction is 5 ℃ in the step 1.Other is identical with embodiment 12.
Embodiment 17: present embodiment and embodiment 12 are different be in the step 1 reaction times be 4～5 hours.Other is identical with embodiment 12.
Embodiment 18: present embodiment and embodiment 12 are different be in the step 1 reaction times be 4.5 hours.Other is identical with embodiment 12.
Embodiment 19: present embodiment and embodiment 12 are different be in the step 1 reaction times be 3 hours.Other is identical with embodiment 12.
Embodiment 20: present embodiment and embodiment 12 are different be in the step 1 reaction times be 6 hours.Other is identical with embodiment 12.
Embodiment 21: present embodiment and embodiment 12 are different is in the step 12,2 ' 3, and (mol ratio of p-aminophenyl) benzoxazole is 1: 1 for 3 '-bibenzene tetracarboxylic dianhydride and 5-amino-2-.Other is identical with embodiment 12.
Embodiment 22: present embodiment and embodiment 12 are different is in the step 12,2 ' 3, and (mol ratio of p-aminophenyl) benzoxazole is 1.02: 1 for 3 '-bibenzene tetracarboxylic dianhydride and 5-amino-2-.Other is identical with embodiment 12.
Embodiment 23: the preparation method of present embodiment Kapton realizes according to the following steps: one, (p-aminophenyl) benzoxazole is dissolved in the N that handles through vapor enrichment, adds diaether dianhydride in N '-N,N-DIMETHYLACETAMIDE again, at N with 5-amino-2-
2Protection under, be to react 3～6 hours under 0～5 ℃ of condition in temperature, obtain polyamic acid; Two, the polyamic acid with step 1 preparation is poured on the sheet glass, casting film-forming, at room temperature dry 3～4 hours, in vacuum drier dry 24～30 hours then; Three, the sheet glass that will handle through step 2 heats up with the temperature rise rate of 10 ℃/min, successively 100 ℃, 150 ℃, 200 ℃ and 300 ℃ of each constant temperature 1 hour, 350 ℃ of constant temperature 0.5 hour; Four, will be cooled to room temperature through the sheet glass that step 3 is handled, the poach demoulding promptly gets Kapton then; Wherein the structural formula of polyimide is
N represents the polymerization degree, 350≤n≤400; Wherein in the step 1 diaether dianhydride and 5-amino-2-(mol ratio of p-aminophenyl) benzoxazole is 1～1.02: 1; The N that every 25ml handles through vapor enrichment in the step 1 is dissolved with 4.44mmol5-amino-2-(p-aminophenyl) benzoxazole in N '-N,N-DIMETHYLACETAMIDE.
Curve C from Fig. 1 present embodiment as can be seen generates the polyimide of Han oxazole ring, and imidization is complete; The polyamic acid viscosity that present embodiment makes is 0.98dL/g, and the Kapton that present embodiment makes can only be dissolved in the vitriol oil; The second-order transition temperature of the Kapton that present embodiment makes is 300 ℃, and the temperature during thermal destruction total mass 5% is 532 ℃, and the temperature during thermal destruction total mass 10% is 549 ℃, and the temperature when thermal weight loss speed is maximum is 550 ℃; The breaking tenacity of the Kapton that present embodiment makes is 214.9Mpa, and elongation at break is 7.14%, and Young's modulus is 3.01Gpa.
Embodiment 24: present embodiment and embodiment 23 are different be in the step 1 diaether dianhydride and 5-amino-2-(mol ratio of p-aminophenyl) benzoxazole is 1: 1.Other is identical with embodiment 23.
Embodiment 25: present embodiment and embodiment 23 are different be in the step 1 diaether dianhydride and 5-amino-2-(mol ratio of p-aminophenyl) benzoxazole is 1.02: 1.Other is identical with embodiment 23.
Embodiment 26: what present embodiment and embodiment 23 were different is that temperature of reaction is 1～4 ℃ in the step 1.Other is identical with embodiment 23.
Embodiment 27: what present embodiment and embodiment 23 were different is that temperature of reaction is 3 ℃ in the step 1.Other is identical with embodiment 23.
Embodiment 28: what present embodiment and embodiment 23 were different is that temperature of reaction is 0 ℃ in the step 1.Other is identical with embodiment 23.
Embodiment 29: what present embodiment and embodiment 23 were different is that temperature of reaction is 5 ℃ in the step 1.Other is identical with embodiment 23.
Embodiment 30: present embodiment and embodiment 23 are different be in the step 1 reaction times be 4～5 hours.Other is identical with embodiment 23.
The embodiment hentriaconta-: present embodiment and embodiment 23 are different be in the step 1 reaction times be 4.5 hours.Other is identical with embodiment 23.
Embodiment 32: present embodiment and embodiment 23 are different be in the step 1 reaction times be 3 hours.Other is identical with embodiment 23.
Embodiment 33: present embodiment and embodiment 23 are different be in the step 1 reaction times be 6 hours.Other is identical with embodiment 23.
Claims (9)
1, the preparation method of Kapton, the preparation method who it is characterized in that Kapton realizes according to the following steps: one, (p-aminophenyl) benzoxazole is dissolved in the N that handles through vapor enrichment with 5-amino-2-, in N '-N,N-DIMETHYLACETAMIDE, add pyromellitic acid anhydride again, at N
2Protection under, be to react 3～6 hours under 0～5 ℃ of condition in temperature, obtain polyamic acid; Two, the polyamic acid with step 1 preparation is poured on the sheet glass, casting film-forming, at room temperature dry 3～4 hours, in vacuum drier dry 24～30 hours then; Three, the sheet glass that will handle through step 2 heats up with the temperature rise rate of 10 ℃/min, successively 100 ℃, 150 ℃, 200 ℃ and 300 ℃ of each constant temperature 1 hour, 350 ℃ of constant temperature 0.5 hour; Four, will be cooled to room temperature through the sheet glass that step 3 is handled, the poach demoulding promptly gets Kapton then; Wherein the structural formula of polyimide is
N represents the polymerization degree, 350≤n≤400; Wherein in the step 1 pyromellitic acid anhydride and 5-base-2-(mol ratio of p-aminophenyl) benzoxazole is 1～1.02: 1; The N that every 25ml handles through vapor enrichment in the step 1 is dissolved with 4.44mmol5-amino-2-(p-aminophenyl) benzoxazole in N '-N,N-DIMETHYLACETAMIDE.
2, the preparation method of Kapton according to claim 1 is characterized in that in the step 1 in temperature being to react 4～5 hours under 1～4 ℃ of condition.
3, the preparation method of Kapton according to claim 1 and 2 is characterized in that in the step 1 that (mol ratio of p-aminophenyl) benzoxazole is 1.01: 1 for pyromellitic acid anhydride and 5-amino-2-.
4, the preparation method of Kapton, the preparation method who it is characterized in that Kapton realizes according to the following steps: one, (p-aminophenyl) benzoxazole is dissolved in the N that handles through vapor enrichment with 5-amino-2-, in N '-N,N-DIMETHYLACETAMIDE, add 2 again, 2 ' 3,3 '-bibenzene tetracarboxylic dianhydride is at N
2Protection under, be to react 3～6 hours under 0～5 ℃ of condition in temperature, obtain polyamic acid; Two, the polyamic acid with step 1 preparation is poured on the sheet glass, casting film-forming, at room temperature dry 3～4 hours, in vacuum drier dry 24～30 hours then; Three, the sheet glass that will handle through step 2 heats up with the temperature rise rate of 10 ℃/min, successively 100 ℃, 150 ℃, 200 ℃ and 300 ℃ of each constant temperature 1 hour, 350 ℃ of constant temperature 0.5 hour; Four, will be cooled to room temperature through the sheet glass that step 3 is handled, the poach demoulding promptly gets Kapton then; Wherein the structural formula of polyimide is
N represents the polymerization degree, 350≤n≤400; Wherein in the step 12,2 ' 3, (mol ratio of p-aminophenyl) benzoxazole is 1～1.02: 1 for 3 '-bibenzene tetracarboxylic dianhydride and 5-amino-2-; The N that every 25ml handles through vapor enrichment in the step 1 is dissolved with 4.44mmol5-amino-2-(p-aminophenyl) benzoxazole in N '-N,N-DIMETHYLACETAMIDE.
5, the preparation method of Kapton according to claim 4 is characterized in that in the step 1 in temperature being to react 4～5 hours under 1～4 ℃ of condition.
6, according to the preparation method of claim 4 or 5 described Kaptons, it is characterized in that in the step 12,2 ' 3, (mol ratio of p-aminophenyl) benzoxazole is 1.01: 1 for 3 '-bibenzene tetracarboxylic dianhydride and 5-amino-2-.
7, the preparation method of Kapton, the preparation method who it is characterized in that Kapton realizes according to the following steps: one, (p-aminophenyl) benzoxazole is dissolved in the N that handles through vapor enrichment with 5-amino-2-, add diaether dianhydride in N '-N,N-DIMETHYLACETAMIDE again, at N
2Protection under, be to react 3～6 hours under 0～5 ℃ of condition in temperature, obtain polyamic acid; Two, the polyamic acid with step 1 preparation is poured on the sheet glass, casting film-forming, at room temperature dry 3～4 hours, in vacuum drier dry 24～30 hours then; Three, the sheet glass that will handle through step 2 heats up with the temperature rise rate of 10 ℃/min, successively 100 ℃, 150 ℃, 200 ℃ and 300 ℃ of each constant temperature 1 hour, 350 ℃ of constant temperature 0.5 hour; Four, will be cooled to room temperature through the sheet glass that step 3 is handled, the poach demoulding promptly gets Kapton then; Wherein the structural formula of polyimide is
N represents the polymerization degree, 350≤n≤400; Wherein in the step 1 diaether dianhydride and 5-amino-2-(mol ratio of p-aminophenyl) benzoxazole is 1～1.02: 1; The N that every 25ml handles through vapor enrichment in the step 1 is dissolved with 4.44mmol5-amino-2-(p-aminophenyl) benzoxazole in N '-N,N-DIMETHYLACETAMIDE.
8, the preparation method of Kapton according to claim 7 is characterized in that in the step 1 in temperature being to react 4～5 hours under 1～4 ℃ of condition.
9,, it is characterized in that in the step 1 that (mol ratio of p-aminophenyl) benzoxazole is 1.01: 1 for diaether dianhydride and 5-amino-2-according to the preparation method of claim 7 or 8 described Kaptons.
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2008
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