CN104327291A - Polyimide composite film preparation method - Google Patents
Polyimide composite film preparation method Download PDFInfo
- Publication number
- CN104327291A CN104327291A CN201410488760.1A CN201410488760A CN104327291A CN 104327291 A CN104327291 A CN 104327291A CN 201410488760 A CN201410488760 A CN 201410488760A CN 104327291 A CN104327291 A CN 104327291A
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- CN
- China
- Prior art keywords
- composite film
- solution
- polyimide composite
- quadrol
- oda
- 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.)
- Pending
Links
- 239000004642 Polyimide Substances 0.000 title claims abstract description 26
- 229920001721 polyimide Polymers 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 17
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 20
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 10
- QQGYZOYWNCKGEK-UHFFFAOYSA-N 5-[(1,3-dioxo-2-benzofuran-5-yl)oxy]-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(OC=2C=C3C(=O)OC(C3=CC=2)=O)=C1 QQGYZOYWNCKGEK-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 239000002362 mulch Substances 0.000 claims description 5
- 239000002985 plastic film Substances 0.000 claims description 5
- 229920006255 plastic film Polymers 0.000 claims description 5
- NWSGBTCJMJADLE-UHFFFAOYSA-N 6-o-decyl 1-o-octyl hexanedioate Chemical compound CCCCCCCCCCOC(=O)CCCCC(=O)OCCCCCCCC NWSGBTCJMJADLE-UHFFFAOYSA-N 0.000 abstract 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract 3
- BCJIMAHNJOIWKQ-UHFFFAOYSA-N 4-[(1,3-dioxo-2-benzofuran-4-yl)oxy]-2-benzofuran-1,3-dione Chemical compound O=C1OC(=O)C2=C1C=CC=C2OC1=CC=CC2=C1C(=O)OC2=O BCJIMAHNJOIWKQ-UHFFFAOYSA-N 0.000 abstract 2
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 abstract 1
- 238000005576 amination reaction Methods 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000007790 scraping Methods 0.000 abstract 1
- DMBHHRLKUKUOEG-UHFFFAOYSA-N N-phenyl aniline Natural products C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 8
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 4
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 125000006158 tetracarboxylic acid group Chemical group 0.000 description 4
- 239000000463 material Substances 0.000 description 2
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- Manufacture Of Macromolecular Shaped Articles (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses a polyimide composite film preparation method which comprises the following steps: (1) adding solvents ethylenediamine, ODA (octyl decyl adipate)and PMDA (pyromellitic dianhydride) into a container to generate a polyamic acid solution A; (2) adding solvents ethylenediamine, ODA and ODPA (oxydiphthalicanhydride) into a container to generate a polyamic acid solution B; (3) mixing the A solution and B solution; and (4) coating a glass plate with the solution and scraping to smooth, removing the solvent ethylenediamine in an ordinary oven, and placing in a vacuum oven for complete imide- amination of polyamic acid to obtain a polyimide composite film. The preparation method can improve the polyimide toughness, and enlarges scope of application.
Description
technical field
The present invention relates to a kind of preparation method of polyimide composite film, belong to material processing field.
technical background
In prior art, polyimide effectively insulating sound absorption light material high-low temperature resistant, density is little, nontoxic, smokeless, convenient construction safety, sound absorbing capabilities are good, is the splendid selection of the field thermal insulation and sound-absorbing materials such as boats and ships naval vessels, aerospace, bullet train.But Kapton is under the condition that some is comparatively extreme, as repeatedly bent, winding etc., there is defect that is more crisp, easy fracture in the Kapton of unitary system.
Summary of the invention
The object of this invention is to provide a kind of preparation method of polyimide composite film, the toughness of polyimide can be improved, expand its range of application.
For realizing above object, the preparation method of a kind of polyimide composite film of the present invention, step is: (1) adds solvent quadrol and 4 in container, 4'-dioctyl diphenylamine (ODA), stirring makes it dissolve, dissolving is placed in ice bath, evenly adds pyromellitic acid anhydride (PMDA) while stirring, and reaction 4h generates polyamic acid solution A; The mass ratio of described PMDA and ODA is 1:0.5; (2) in container, solvent quadrol and 4 are added, 4'-dioctyl diphenylamine (ODA), stirs and makes it dissolve, and dissolves and is placed in ice bath, evenly add phenyl ether tetracarboxylic dianhydride (ODPA) while stirring, reaction 4h generates polyamic acid solution B; The mass ratio of ODPA and ODA is 1:1.5; (3) by above-mentioned solution A and B solution mixing, stirred at ambient temperature 4h, obtains the thick liquid of clear, yellowish; (4) above-mentioned solution carried out plastic film mulch on a glass and strike off, except desolventizing quadrol in a conventional oven, then being positioned in vacuum drying oven, making polyamic acid imidization complete, thus the type polyimide composite film that is enhanced.
Further, the solid-liquid ratio of described PMDA and solvent quadrol is 1 g:20-30ml.
Further, the solid-liquid ratio of described ODPA and solvent quadrol is 1 g:20-30ml.
Further, the volume ratio of described solution A and B solution is 1:3-3:1.
Further, described in described step (3), the temperature of vacuum drying oven is 300-400 DEG C, and drying time is 3h.
The beneficial effect that the present invention produces is that the method that the present invention adopts polyamic acid blended, two kinds of polyamic acid solutions have good intermiscibility, effectively improve the elongation at break of laminated film.
Embodiment
Embodiment 1:
Polyimide composite film is prepared by following methods:
(1) in container, 4000ml solvent quadrol and 50g4 is added, 4'-dioctyl diphenylamine (ODA), stirring makes it dissolve, dissolving is placed in ice bath, evenly add 100g pyromellitic acid anhydride (PMDA) while stirring, reaction 4h generates polyamic acid solution A; (2) in container, 4000ml solvent quadrol and 150g 4 is added, 4'-dioctyl diphenylamine (ODA), stirring makes it dissolve, dissolving is placed in ice bath, evenly add 100g phenyl ether tetracarboxylic dianhydride (ODPA) while stirring, reaction 4h generates polyamic acid solution B; (3) be 1:2 mixing by volume by above-mentioned solution A and B solution, stirred at ambient temperature 4h, obtains the thick liquid of clear, yellowish; (4) above-mentioned solution carried out plastic film mulch on a glass and strike off, except desolventizing quadrol in a conventional oven, then being positioned in 300 DEG C of vacuum drying ovens and drying 3h, make polyamic acid imidization complete, thus obtain polyimide composite film.
The Young's modulus of the polyimide composite film prepared is 4.42GPa, tensile strength 382MPa, elongation at break 78%.
Embodiment 2:
Polyimide composite film is prepared by following methods:
(1) in container, 5000ml solvent quadrol and 50g4 is added, 4'-dioctyl diphenylamine (ODA), stirring makes it dissolve, dissolving is placed in ice bath, evenly add 100g pyromellitic acid anhydride (PMDA) while stirring, reaction 4h generates polyamic acid solution A; (2) in container, 5000ml solvent quadrol and 150g 4 is added, 4'-dioctyl diphenylamine (ODA), stirring makes it dissolve, dissolving is placed in ice bath, evenly add 100g phenyl ether tetracarboxylic dianhydride (ODPA) while stirring, reaction 4h generates polyamic acid solution B; (3) be 1:1 mixing by volume by above-mentioned solution A and B solution, stirred at ambient temperature 4h, obtains the thick liquid of clear, yellowish; (4) above-mentioned solution carried out plastic film mulch on a glass and strike off, except desolventizing quadrol in a conventional oven, then being positioned in 350 DEG C of vacuum drying ovens and drying 3h, make polyamic acid imidization complete, thus obtain polyimide composite film.
The Young's modulus of the polyimide composite film prepared is 4.86GPa, tensile strength 395MPa, elongation at break 76%.
Embodiment 3:
Polyimide composite film is prepared by following methods:
(1) in container, 6000ml solvent quadrol and 120g4 is added, 4'-dioctyl diphenylamine (ODA), stirring makes it dissolve, dissolving is placed in ice bath, evenly add 50g pyromellitic acid anhydride (PMDA) while stirring, reaction 4h generates polyamic acid solution A; (2) in container, 6000ml solvent quadrol and 150g 4 is added, 4'-dioctyl diphenylamine (ODA), stirring makes it dissolve, dissolving is placed in ice bath, evenly add 100g phenyl ether tetracarboxylic dianhydride (ODPA) while stirring, reaction 4h generates polyamic acid solution B; (3) be 1:2 mixing by volume by above-mentioned solution A and B solution, stirred at ambient temperature 4h, obtains the thick liquid of clear, yellowish; (4) above-mentioned solution carried out plastic film mulch on a glass and strike off, except desolventizing quadrol in a conventional oven, then being positioned in 400 DEG C of vacuum drying ovens and drying 3h, make polyamic acid imidization complete, thus obtain polyimide composite film.
The Young's modulus of the polyimide composite film prepared is 3.76GPa, tensile strength 399MPa, elongation at break 72%.
Claims (5)
1. a preparation method for polyimide composite film, is characterized in that: step is:
(1) in container, add solvent quadrol and ODA, stir and make it dissolve, dissolve and be placed in ice bath, evenly add PMDA while stirring, reaction 4h generates polyamic acid solution A; The mass ratio of described PMDA and ODA is 1:0.5;
(2) in container, add solvent quadrol and ODA, stir and make it dissolve, dissolve and be placed in ice bath, evenly add ODPA while stirring, reaction 4h generates polyamic acid solution B; The mass ratio of described ODPA and ODA is 1:1.5;
(3) by above-mentioned solution A and B solution mixing, stirred at ambient temperature 4h, obtains the thick liquid of clear, yellowish;
(4) above-mentioned solution carried out plastic film mulch on a glass and strike off, except desolventizing quadrol in a conventional oven, then being positioned in vacuum drying oven, making polyamic acid imidization complete, obtain polyimide composite film.
2. the preparation method of a kind of polyimide composite film according to claim 1, is characterized in that: the solid-liquid ratio of described PMDA and solvent quadrol is 1 g:20-30ml.
3. the preparation method of a kind of polyimide composite film according to claim 1, is characterized in that: the solid-liquid ratio of described ODPA and solvent quadrol is 1 g:20-30ml.
4. the preparation method of a kind of polyimide composite film according to claim 1, is characterized in that: the volume ratio of described solution A and B solution is 1:3-3:1.
5. the preparation method of a kind of polyimide composite film according to claim 1, is characterized in that: described in described step (3), the temperature of vacuum drying oven is 300-400 DEG C, and drying time is 3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410488760.1A CN104327291A (en) | 2014-09-23 | 2014-09-23 | Polyimide composite film preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410488760.1A CN104327291A (en) | 2014-09-23 | 2014-09-23 | Polyimide composite film preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104327291A true CN104327291A (en) | 2015-02-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410488760.1A Pending CN104327291A (en) | 2014-09-23 | 2014-09-23 | Polyimide composite film preparation method |
Country Status (1)
| Country | Link |
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| CN (1) | CN104327291A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109666170A (en) * | 2017-10-17 | 2019-04-23 | 中国石油化工股份有限公司 | The preparation method of uniform high-performance polyimide film |
-
2014
- 2014-09-23 CN CN201410488760.1A patent/CN104327291A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109666170A (en) * | 2017-10-17 | 2019-04-23 | 中国石油化工股份有限公司 | The preparation method of uniform high-performance polyimide film |
| CN109666170B (en) * | 2017-10-17 | 2021-09-03 | 中国石油化工股份有限公司 | Preparation method of uniform high-performance polyimide film |
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Application publication date: 20150204 |