CN104191633B - Cold processing process and polyimide film production line for manufacturing polyimide film - Google Patents
Cold processing process and polyimide film production line for manufacturing polyimide film Download PDFInfo
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- CN104191633B CN104191633B CN201410427617.1A CN201410427617A CN104191633B CN 104191633 B CN104191633 B CN 104191633B CN 201410427617 A CN201410427617 A CN 201410427617A CN 104191633 B CN104191633 B CN 104191633B
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Abstract
The invention discloses a cold processing process and a polyimide film production line for manufacturing a polyimide film. The cold processing process comprises the following step that a polyimide acid self-supporting film obtained after casting is performed enters a drawing process after being subjected to cold processing at -60 DEG C to 25 DEG C for 0.05 to 3 minutes. The cold processing process also comprises the step of carrying out the cold processing at one or more positions after the polyimide acid self-supporting film is longitudinally drawn, transversely drawn and thermally shaped, wherein the cold processing temperature at the positions close to a winding process is gradually decreased according to 10 to 30 percent, and the cold processing time is 0.05 to 3 minutes; the cold processing temperature after the polyimide acid self-supporting film is thermally shaped is -90 to 0 DEG C. According to the polyimide film production line in which the cold processing process is performed, a cold air box is arranged behind a casting machine. Cold air boxes are also arranged behind a longitudinal drawing machine, and/or a transverse drawing machine and/or a thermal shaping drying box. The film is processed for 0.05 to 3 minutes in the cold air box at each position. Through cold processing, the film is prevented from oxidizing and adsorbing moisture before drawing; the electrical performance and the mechanical performance of the film are remarkably improved; the cold processing process and the polyimide film production line are easy to implement.
Description
Technical field
The present invention relates to Kapton manufacturing technology, specially manufacture the cold treatment process of Kapton and adopt
Production Line for Polyimide Film with this kind of technique.
Background technology
Kapton is that have high intensity, high tenacity, the high score of the excellent properties such as wear-resistant, high temperature resistant, corrosion-resistant
Sub- material, is the predominating insulation making various medium-to-high grade electrotechnical, electronic components and parts, is widely used in electrotechnical, electronic industry.
The development trend of and High Reliability Design light, thin, short, little with downstream electronic product, the thin film of the market demand becomes
To in slimming, the performances such as electric, the hot, physics of Kapton are all put forward higher requirement simultaneously.
The conventional method of currently manufactured Kapton is as follows：Led to using dimethyl acetylamide as solvent in reactor
The polyreaction crossing dianhydride with diamidogen produces polyimide precursor polyamic acid solution, and on slobbering machine, sialorrhea obtains afterwards
There is the Polyamic Acid Film of self-supporting, then carry out direction stretching, high temperature imidization in length and breadth, last thermal finalization is processed, winding.
Its electricity of Kapton product of existing process manufacture, the poor-performing such as heat, physics, particularly electrical strength, modulus is relatively low,
Percent thermal shrinkage, water absorption rate, thermal coefficient of expansion, dielectric constant are higher etc..
In order to improve the performances such as electric, the hot, physics of Kapton, in recent years occur in that some about Kapton
In manufacture process, low temperature is cyclized the patent application of handling process, and such as publication date is October 21, Publication No. in 2009
The Chinese invention patent " being manufactured the low temperature method of Kapton by polyamic acid solution " of CN101560304A, is by polyamides
On a substrate, cyclisation under continuous vacuum low pressure and cold service forms Kapton to amino acid solution coating.The method
Coating obtains polyamic acid wet film or dry film, and the cyclisation time is more than 0.5 hour it is impossible to be applied to continuous prodution.
Publication date is on January 5th, 2013, a kind of " enhancing of the Chinese invention patent application of Publication No. CN103059334A
Hydroxypropyl cellulose microporous membrane and preparation method thereof ", it adopts low temperature or freezing simply to realize the solidification of cellulose microporous membrane
Or pore-forming needs, cooling time is more than 1 hour it is impossible to be applied to continuous prodution.
Publication date is Chinese invention patent application " a kind of polyamides of on June 19th, 2013, Publication No. CN103159964A
Amino acid glue low-temperature stabilization storage method and freezing liquid compositionss ", it adopts low temperature or freezing, and simply to realize polyimides thin
Film solidification or stable polyamides acid solution.
Have not yet to see to significantly improve Kapton electricity, the performance such as heat, physics and can be used for serialization manufacture and gather
The new technology of imide membrane.
Content of the invention
The purpose of the present invention is a kind of cold treatment process manufacturing Kapton of design, gained polyamic acid self-supporting
Thin film enters back into stretching process after cold treatment, and the performance such as electric, hot, physics of obtained Kapton significantly improves.
It is another object of the present invention to the polyimides being designed with the cold treatment process manufacturing Kapton are thin
Film production line, introduces packaged air conditioner in the existing Production Line for Polyimide Film, makes the self-supporting that has in manufacture process
Polyamic Acid Film enters back into stretching process after cold treatment, to improve film performance.
The cold treatment process of the manufacture Kapton of present invention design obtains thering is oneself for polyamic acid solution sialorrhea
The Polyamic Acid Film of supportive, then carry out direction stretching in length and breadth, high temperature imidization, wind after thermal finalization；After sialorrhea, gained gathers
Amic acid self-supporting film enters back into stretching process after cold treatment.
After described sialorrhea, gained polyamic acid self-supporting film is -60～25 DEG C through the temperature of cold treatment, preferred range
For -50～-25 DEG C, the cold treatment time of thin film is 0.05～3min.
After the cold treatment process of the manufacture Kapton of present invention design is additionally included in vertical drawing, horizontal draw after and thermal finalization
The cold treatment of at afterwards or many places, indulges the thin film after drawing rear and/or horizontal drawing and/or after thermal finalization and enters back into through cold treatment
Subsequent processing.
After described sialorrhea, vertical draw after, horizontal draw after and thermal finalization after cold treatment temperature, with pressing 10 close to winding process～
30% gradient is successively decreased.Thin film throughout cold treatment time be 0.05～3min.
After thermal finalization, cold treatment temperature is -90～0 DEG C.
For implementing the cold treatment process of the manufacture Kapton of the present invention, the present invention devises Kapton life
Producing line, it includes slobbering machine, stretching-machine, high temperature imidization stove, thermal finalization baking oven and winder, and described stretching-machine is that vertical machine drawing exists
Before, its be followed by transverse stretching machine, or for transverse stretching machine front, it is followed by vertical machine drawing, or is bi-directional synchronization stretching-machine.
Have a packaged air conditioner after slobbering machine, sialorrhea gained have self-supporting Polyamic Acid Film cold after slobbering machine
Pass through in bellows case, enter back into stretching-machine.
The temperature in packaged air conditioner case after slobbering machine is -60～25 DEG C, and the time that thin film is processed in packaged air conditioner is 0.05
～3min.
The preferred temperature in packaged air conditioner case after slobbering machine is -50～-25 DEG C, and the time that thin film is processed in packaged air conditioner is
0.05～3min.
If the stretching-machine of the Production Line for Polyimide Film of the present invention indulge machine drawing front, its be followed by transverse stretching machine, described vertical
There is packaged air conditioner after machine drawing, complete the vertical thin film drawing through packaged air conditioner, enter back into transverse stretching machine；There is packaged air conditioner after transverse stretching machine, complete horizontal stroke
The thin film drawing, through packaged air conditioner, enters back into high temperature imidization stove thereafter；
If transverse stretching machine front, its be followed by vertical machine drawing, have packaged air conditioner after described transverse stretching machine, complete the horizontal thin film drawing through supercool
Bellows, enter back into vertical machine drawing；There is packaged air conditioner after vertical machine drawing, complete the vertical thin film drawing through packaged air conditioner, enter back into high temperature thereafter
Imidization stove；
If bi-directional synchronization stretching-machine, after bi-directional synchronization stretching-machine, there is packaged air conditioner, complete the thin film warp of bi-directional synchronization stretching
Cross packaged air conditioner, enter back into high temperature imidization stove thereafter；
And/or, there is packaged air conditioner after thermal finalization baking oven, the thin film completing thermal finalization enters back into winder through packaged air conditioner.
The temperature in packaged air conditioner case after thermal finalization baking oven is -90～0 DEG C.
Packaged air conditioner after described sialorrhea, vertical draw after packaged air conditioner, horizontal draw after packaged air conditioner and thermal finalization after packaged air conditioner,
With close to winder, the temperature in packaged air conditioner case is successively decreased by 10～30% gradients everywhere, thin film process in each packaged air conditioner when
Between be 0.05～3min.
2～16 transition rollers being parallel to each other are had, the thin film entering packaged air conditioner bypasses each successively in described packaged air conditioner
Transition roller, on the section perpendicular to roller centrage, the traveling process of thin film is S-shaped.
Compared with prior art, the present invention manufactures cold treatment process and the Production Line for Polyimide Film of Kapton
Advantage be：1st, after sialorrhea gained there is the Polyamic Acid Film of self-supporting through cold treatment, can prevent thin film from drawing in entrance
Stretch and produce the side effect such as disproportionation, oxidation, moisture absorption before machine it is ensured that Polyamic Acid Film quality；2nd, adopt this cold treatment process gained
The electrical strength of Kapton product, tensile strength, modulus are substantially greatly improved, and dielectric constant is remarkably decreased, thermal expansion
Coefficient, water absorption rate, shrinkage factor are all greatly reduced；3rd, after cold treatment, gained thin film vertically and horizontally stretches uniformly, and concordance improves, and
Final gained Kapton film roll surfacing, performance improvement；4th, existing Production Line for Polyimide Film only needs to
Packaged air conditioner is set up at corresponding position, you can implement the cold treatment process of the present invention, and transformation of facility is easily achieved, and only need to increase to each
The control of packaged air conditioner, production line routinely runs substantially.
Brief description
Fig. 1 is the schematic diagram of this Production Line for Polyimide Film embodiment.
Fig. 2 is the structural representation of packaged air conditioner in Fig. 1.
Figure internal label is：1st, thin film import, 2, cold wind outlet, 3, transition roller, 4, thin film, 5,
Cold wind import, 6, thin film outlet.
Specific embodiment
This Production Line for Polyimide Film embodiment as shown in figure 1, from left to right each equipment as follows successively：Slobbering machine, cold
Bellows, vertical machine drawing, packaged air conditioner, transverse stretching machine, packaged air conditioner, high temperature imidization stove, thermal finalization baking oven, packaged air conditioner and winder.
This example packaged air conditioner as shown in Fig. 2 there being 7 transition rollers 3 being parallel to each other in case, enter packaged air conditioner thin film 4 according to
Secondary bypass each transition roller 3, on the section perpendicular to roller centrage, the traveling process of thin film 4 is S-shaped, and thin film 4 is each
The time processing in packaged air conditioner is 60 seconds.
This example packaged air conditioner is thermal-insulating body, and in it, setting cold wind import 5 and cold wind outlet 2, blow cold wind into case and maintain
Low temperature in packaged air conditioner, box house may also be employed plenum box structure and directly blows cold wind to thin film upper and lower surface and maintain cold wind
Low temperature in case.Packaged air conditioner two ends have thin film import 1 and thin film outlet 6 respectively.
Each cold wind the temperature inside the box is different.
Temperature in packaged air conditioner after slobbering machine is -50 DEG C.
Temperature in packaged air conditioner after vertical machine drawing is -60 DEG C.
Temperature in packaged air conditioner after transverse stretching machine is -70 DEG C.
Packaged air conditioner the temperature inside the box after thermal finalization baking oven is -80 DEG C.
The cold treatment process of this manufacture Kapton can be implemented on this Production Line for Polyimide Film embodiment.
Sialorrhea in this example Kapton manufacture process, vertical draw, horizontal draw, imidization and thermal finalization be all using existing skill
Art, the Polyamic Acid Film solvent that after sialorrhea, gained has self-supporting is 35%, and longitudinal stretching ratio is 1.15, laterally draws
Stretching ratio is 1.12, and draft temperature is 190 DEG C, and imidization temperature is 420 DEG C, and heat setting temperature is 260 DEG C；Line speed is
6.0m/min.
After polyamic acid solution sialorrhea, gained polyamic acid self-supporting film is -50 DEG C through the temperature of cold treatment, thin film
The time of cold treatment is 60 seconds.
The temperature indulging the Polyamic Acid Film after drawing through cold treatment is -60 DEG C, and the time of thin film cold treatment is 60 seconds.
Horizontal draw after Polyamic Acid Film be -70 DEG C through the temperature of cold treatment, time of thin film cold treatment is 60 seconds.
Kapton after thermal finalization is -80 DEG C through the temperature of cold treatment, and the time of thin film cold treatment is 60 seconds.
Sialorrhea in comparative example Kapton manufacture process, vertical draw, horizontal draw, the technological parameter of imidization and thermal finalization with
The present embodiment is identical, does not simply have cold treatments at different levels.Comparative example and the performance such as table 1 of the present embodiment gained Kapton
Shown：
Table 1 comparative example and the present embodiment gained Kapton Performance comparision table
By the visible cold treatment process gained Kapton of the present invention of table 1 and without cold treatment process gained polyimides
Thin film compares, and electricity, the performance such as heat, physics all obtain larger improvement.Electrical strength lifts more than 60KV/mm, under dielectric constant
Fall 0.5, thermal coefficient of expansion reduces by more than 10%, and shrinkage factor is only the 50% about of comparative example, and water absorption rate then reduces more than one times, draws
Stretch intensity and 60MPa is then significantly increased, modulus improves 0.7GPa.Kapton quality significantly improves.
Above-described embodiment, only the purpose of the present invention, technical scheme and beneficial effect are further described is concrete
Individual example, the present invention is not limited to this.All any modifications made within the scope of disclosure of the invention, equivalent, change
Enter, be all contained within protection scope of the present invention.
Claims (7)
1. manufacture the cold treatment process of Kapton, polyamic acid solution sialorrhea obtains the polyamic acid with self-supporting
Thin film, then carry out direction stretching in length and breadth, high temperature imidization, wind after thermal finalization；It is characterized in that：
After sialorrhea, gained polyamic acid self-supporting film enters back into stretching process after cold treatment；
After described sialorrhea, gained polyamic acid self-supporting film is -50～-25 DEG C through the temperature of cold treatment, the cold treatment of thin film
Time is 0.05～3min.
2. according to claim 1 manufacture Kapton cold treatment process it is characterised in that：
After being additionally included in vertical drawing, horizontal draw after and thermal finalization after one at or many places cold treatment, vertical draw after and/or horizontal draw after,
And/or the thin film after thermal finalization enters back into subsequent processing through cold treatment.
3. according to claim 2 manufacture Kapton cold treatment process it is characterised in that：
After described sialorrhea, vertical draw after, horizontal draw after and thermal finalization after cold treatment temperature, with close to winding process, press 10～30%
Gradient is successively decreased, thin film throughout cold treatment time be 0.05～3min；
After thermal finalization, cold treatment temperature is -90～0 DEG C.
4. adopt the Production Line for Polyimide Film of the cold treatment process of manufacture Kapton described in claim 1, its
Including slobbering machine, stretching-machine, high temperature imidization stove, thermal finalization baking oven and winder, described stretching-machine is vertical machine drawing front, thereafter
Connect transverse stretching machine, or for transverse stretching machine front, it is followed by vertical machine drawing, or is bi-directional synchronization stretching-machine；It is characterized in that：
Have packaged air conditioner after described slobbering machine, sialorrhea gained there is the Polyamic Acid Film of the self-supporting cold wind after slobbering machine
Pass through in case case, enter back into stretching-machine；
The temperature in packaged air conditioner case after described slobbering machine is -50～-25 DEG C, and the time that thin film is processed in packaged air conditioner is 0.05
～3min.
5. Production Line for Polyimide Film according to claim 4 it is characterised in that：
If described stretching-machine indulge machine drawing front, its be followed by transverse stretching machine, have packaged air conditioner after described vertical machine drawing, complete the vertical thin film drawing
Through packaged air conditioner, enter back into transverse stretching machine；There is packaged air conditioner after transverse stretching machine, complete the horizontal thin film drawing through packaged air conditioner, enter back into thereafter
High temperature imidization stove；
If transverse stretching machine front, its be followed by vertical machine drawing, have packaged air conditioner after described transverse stretching machine, complete the horizontal thin film drawing through cold wind
Case, enters back into vertical machine drawing；There is packaged air conditioner after vertical machine drawing, complete the vertical thin film drawing through packaged air conditioner, the high temperature entering back into thereafter is sub-
Amination stove；
If bi-directional synchronization stretching-machine, after bi-directional synchronization stretching-machine, there is packaged air conditioner, the thin film completing bi-directional synchronization stretching is through supercool
Bellows, enter back into high temperature imidization stove thereafter；
And/or, there is packaged air conditioner after thermal finalization baking oven, the thin film completing thermal finalization enters back into winder through packaged air conditioner.
6. Production Line for Polyimide Film according to claim 4 it is characterised in that：
The temperature in packaged air conditioner case after described thermal finalization baking oven is -90～0 DEG C；
Packaged air conditioner after described sialorrhea, vertical draw after packaged air conditioner, horizontal draw after packaged air conditioner and thermal finalization after packaged air conditioner, with
Close to winder, the temperature in packaged air conditioner case is successively decreased by 10～30% gradients everywhere, the time that thin film is processed in each packaged air conditioner
For 0.05～3min.
7. Production Line for Polyimide Film according to claim 5 it is characterised in that：
2～16 transition rollers being parallel to each other are had, the thin film entering packaged air conditioner bypasses each transition successively in described packaged air conditioner
Roller, on the section perpendicular to roller centrage, the traveling process of thin film is S-shaped.
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| CN201410427617.1A CN104191633B (en) | 2014-08-27 | 2014-08-27 | Cold processing process and polyimide film production line for manufacturing polyimide film |
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|---|---|---|---|
| CN201410427617.1A CN104191633B (en) | 2014-08-27 | 2014-08-27 | Cold processing process and polyimide film production line for manufacturing polyimide film |
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| JP2559073B2 (en) * | 1990-04-19 | 1996-11-27 | 富士写真フイルム株式会社 | Method for producing cellulose triacetate film |
| JP4792357B2 (en) * | 2005-09-28 | 2011-10-12 | 富士フイルム株式会社 | Method for producing polymer film |
| CN101096129B (en) * | 2007-06-19 | 2010-05-19 | 广东华业包装材料有限公司 | Method for manufacturing polystyrene torsion film |
| CN102391532B (en) * | 2011-08-26 | 2012-11-14 | 朱宏清 | Biaxially oriented polyimide film for flexible printed circuit board base material and preparation method of biaxially oriented polyimide film |
| CN103232609B (en) * | 2013-04-25 | 2016-04-20 | 安徽朝日电子新能源有限公司 | A kind of preparation method of flyash modified nano aluminium oxide/polyimide composite film |
| CN204036866U (en) * | 2014-08-27 | 2014-12-24 | 桂林电器科学研究院有限公司 | Adopt the Production Line for Polyimide Film of Kapton cold treatment process |
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