CN104497340B - Improve the method and facility of Polyamic Acid Film side imines rate - Google Patents
Improve the method and facility of Polyamic Acid Film side imines rate Download PDFInfo
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- CN104497340B CN104497340B CN201410839912.8A CN201410839912A CN104497340B CN 104497340 B CN104497340 B CN 104497340B CN 201410839912 A CN201410839912 A CN 201410839912A CN 104497340 B CN104497340 B CN 104497340B
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Abstract
The invention discloses a kind of method and facility for improving Polyamic Acid Film side imines rate, this law is the Polyamic Acid Film peeled off from steel band, and avris heating, gradually rises with close to outer rim temperature before stretching.Before the stretching, film side side spray drenches chemical imidization bath foam.Polyamic Acid Film side-flank surfaces temperature is improved during stretching.During imidization, before high-temperature region is entered, Polyamic Acid Film side-flank surfaces temperature, leading imidization, increase intensity are improved.This facility be stretcher before, multiple row heating tube is just installed above and/or under film side parts.Before stretcher, chemical imidization spray equipment is set in film side.In stretcher, the plenum chamber for improving temperature is just set above and/or under side parts.Before imination equipment high-temperature region, auxiliary heating tube is just installed above and/or under film side parts additional.The present invention is easy to implement, improves film avris imidization rate, is allowed to intensity increase, it is to avoid clip broken and pull open, improves thin film yield.
Description
Technical field
It is specially a kind of raising Polyamic Acid Film side imines rate the present invention relates to Kapton manufacturing technology
Method and facility.
Background technology
Kapton is the high score with the excellent properties such as high intensity, high tenacity, abrasion performance, high temperature resistant, corrosion-resistant
Sub- material, is the predominating insulation for making various medium-to-high grade electrotechnical, electronic components, is widely used in electrotechnical, electronic industry.Mesh
The preparation technology of preceding Kapton is that, using polyamic acid resin solution as raw material, salivation obtains self-supporting on slobbering machine
Polyamic Acid Film, then obtain Kapton by heating stretching, high temperature imidization, cooling and shaping processing.
As downstream application product is light, thin, short, small and design requirement of high reliability, the film thickness rule of the market demand
Lattice tend to slimming, and higher requirement is proposed to its technology of preparing, product quality particularly product yield.
In Kapton preparation process, required for the conventional manufacturing process using drawing and setting or tensioning sizing reaches
Thickness and traditional performance.It is required to grip Kapton semi-finished product polyamic acid when drawing and setting or tensioning sizing
Two sides of film, apply horizontal force, i.e., to thin by the clamping device of film both sides to film under the high temperature conditions
Film carries out cross directional stretch.It is also required to grip the side of film two during longitudinal stretching, it is to avoid film is deformed and subtracted to central reduction
Small width.
For example when Kapton is produced, it is typically to be molded polyamic acid resin on slobbering machine by salivating mode
For Polyamic Acid Film, imidization processing is carried out by high temperature furnace afterwards Kapton is made.Will in imidization
The bilateral of semi-finished product film is gripped, and film is carried out cross directional stretch or tensioning processing under clamp position, and keep this shape
State completes high temperature imidization, to improve the traditional performance of film.
The clamping device of existing film line both sides be mainly installed in ring-shaped guide rail chain on chain pincers or
Pin is buckled.Vertically and horizontally stretching is intended to need higher temperature to the imidization that film carries out high-temperature process, particularly Polyamic Acid Film
Processing, maximum processing temperature is up to 500 DEG C.Chain in production line and chain pincers or pin thereon buckle warm in high temperature environments
Degree is also increased, when stretching entry position clamping film easily because high temperature causes film side to clip broken or tear, side
The damaged film in side follow-up stretching, imidization, shape and open in the technical process such as folder easily in chain pincers pincers mouthful position or
Pin, which is buckled thorn button bit and put, to be caused de- pincers or dropout and is pulled open, reduction film stretching quality, or even film can not normally be wound, and be reduced
Film product yield, has a strong impact on film line yield.
Meanwhile, the edge of Polyamic Acid Film upwarps phenomenon due to too thin easy generation, and chain pincers makes film side when clamping
It is folded into double-deck side.High temperature is run into double-deck side clamping process so that chain pincers clip position film is easily torn, and again results in production
Product can not normally be wound, and reduce film product yield.
In actual production line, the pincers of opening of Kapton is closely located to draw wrap-up, and film is drawn when driving pincers
Stretch the comprehensive functions such as stress, drawing tension and winding tension and the rupture of membranes phenomenon such as raw edges, transverse breakage easily occur, thus film without
Method is normally wound, and has a strong impact on thin film yield, reduces film yield.
The problems such as in order to solve edge damage, film breakage in Kapton preparation process, the patent Shen of correlation is occurred in that in recent years
Please, such as Chinese utility model patent " the entering pincers guide device of membrane production equipment ", openly of the notification number for CN202245464U
The Chinese invention patent chain pincers cooling device of machinery " film production ", Publication No. number for CN102441987A
In CN102431161A Chinese invention patent " film line in advance clip opening device ", Publication No. CN102390112A
State's patent of invention " film drawing and setting or the film clamping device of film for being tensioned modular system ", notification number is in CN203236699U
State's utility model patent " one kind solves film stretching rupture of membranes and thickness homogeneous system ", is filled wherein individually disclosing and being guided into pincers
Put, chain pincers cooling device, in advance clip opening device and clamping device etc., although make clamping device cause to clip broken or Tear Film
Some reductions of the problem of side, but fail to that such failure is completely eliminated.And these devices are required to existing production line
Equipment is transformed or replaced, and apparatus structure is complex, also needs higher improvement cost, therefore is difficult to be widely implemented application.
In addition Publication No. CN102416684A Chinese invention patent " adhesive tape processing method in film production of slobbering machine ", public
Chinese invention patent " method for adhesive tape treatment in production of thin film by casting machine " that the number of opening is CN102303388A, notification number are
CN202147343U Chinese utility model patent " polyimide film producing device of automatic erasing releasing agent " etc. is to pass through
Improving manufacturing process processing salivation adhesive tape causes rupture of membranes, film breakage etc. abnormal, and regulation technological parameter is more, and adjustable range is big, especially
Be introduce such as wipe releasing agent can cause film too it is smooth can not normal use in the side effect of downstream product.
The content of the invention
It is an object of the invention to provide a kind of method for improving Polyamic Acid Film side imines rate, to from salivation steel band
The side parts heating of the Polyamic Acid Film one fixed width of upper stripping, gradually rises with close to outer rim temperature, makes film avris
Partial imines rate improves, reduced the polyamide acid content of film side parts, so that Polyamic Acid Film side is strong
Degree increase, be not susceptible to clip broken when clamped or raw edges failure, it is ensured that the quality of film, improve thin film yield.
It is another object of the present invention to design a kind of facility for improving Polyamic Acid Film side imines rate, in polyamide
The above and or below of sour film side parts of one fixed width from rear film traveling process is peeled off on steel band installs heating
Pipe, with close to outer rim, heating tube is gradually reduced with film surface distance, the temperature of film side parts is raised imines rate and carries
It is high.
A kind of method for raising Polyamic Acid Film side imines rate that the present invention is designed, polyamic acid solution is in steel band
Upper salivation is shaped to polyamic acid liquid film, and being dried by hot-air oven turns into the Polyamic Acid Film of self-supporting, then stretched,
Imidization is handled.To the Polyamic Acid Film peeled off from steel band, before being stretched, the wide X of the side parts of film two model
Heating 8 seconds~80 seconds is enclosed, is gradually risen with close to outer rim temperature, outer most edge film surface temperature T=150~200 DEG C, the X
=20~200mm.
It is thin to the polyamic acid peeled off from steel band further to improve the imines rate of Polyamic Acid Film two side
Film, before being stretched, the wide X of film side parts spray chemical imidization bath foam 8 seconds~80 seconds enters to side parts
Row topochemistry imidization, the X=20~200mm.The polyimide content of film side parts further increases, imidization
Rate is improved again, and its intensity is further strengthened.
The chemical imidization bath foam is chemical imidization bath foam known in the industry, contains dehydrating agent and catalyst.
Wherein dehydrating agent be acetic anhydride, propionic andydride, butyric anhydride, benzoyl oxide, lower aliphatic halide, aryl sulfonic acid dihalide,
Any one in the halide of sulfurous acid halogen and phosphorus or any several mixture；Catalyst therein is pyridine and its derivative
Thing, picoline and its derivative, lutidines, quinoline, isoquinolin, porphyrin, imidazoles, triethylamine, triethanolamine, Sanya second
Any one in base diamines and diisopropyl ethyl amine or any several mixture.The proportioning of chemical imidization solution is one
As known match.
The surface temperature of the avris of Polyamic Acid Film two is improved during stretching, the intensity of film avris also can be further improved.
G=150 DEG C of the surface temperature of polyamic acid central film portion~250 DEG C in stretcher, the wide Y=20~200mm models of side parts
It is 1.0~1.5 times of G to enclose internal surface temperature g, is gradually stepped up with close to film outer rim film surface temperature, g is up to 375 DEG C.
During imidization, before high-temperature region is entered, the surface temperature of the avris of Polyamic Acid Film two is improved, makes film avris
It is previously-completed imidization, increases its intensity.H=320 DEG C of the surface temperature of polyamic acid central film portion~450 in imination equipment
DEG C gradually rise, in the range of the wide Y=20~200mm of side parts before high-temperature region is entered, surface temperature h for H 1.0~
1.5 times, gradually stepped up with close to film outer rim film surface temperature, h is up to 650 DEG C.
A kind of facility for raising Polyamic Acid Film side imines rate that the present invention is designed includes mould, carrying stream
Saliva is molded the circulation steel band and baking oven of polyamic acid liquid film, is followed by stretcher and imination equipment, Polyamic Acid Film from
On steel band peel off after, enter stretcher before, in the range of the laterally wide X of its in film traveling process the top of side parts and/
Or heating tube is installed in lower section, the X=20~200mm arranges equidistant in the range of wide X, in film above and or below
2~6 row length directions heating tube parallel with film direct of travel, the length L=u*v of heating tube row, wherein u represents film row
Enter speed, v and represent film treatment time, and 0.5m/min≤u≤20.0m/min, 8 seconds≤v≤80 second.Heating tube and film table
Face vertical range is m, is gradually reduced with close to film outer rim m.In the heating tube and film table of film outer rim above and or below
Identity distance is from minimum M, M=10~30mm, m=(1~8) M.The installation of the side parts above and or below heating tube of film two
Height is symmetrical with the vertical plane on film longitudinal centre line.
When carrying out chemical imidization, on the Polyamic Acid Film transmission stroke peeled off from steel band, entering stretcher
Before, film side sets chemical imidization spray equipment, and spray equipment includes spray head and shower liquid pipe, in laterally wide X models
Film above and or below in enclosing installs spray head, and the X=20~200mm, spray head connects bath foam through shower liquid pipe
Pump, shower liquid pump connection shower liquid storage tank.Spray head is spray face towards film surface, and width is uniform court in X, spray face
To the nozzle of film surface.Spray face is L close to the length of the nozzle file of film edge, is indulged with close to thin film center, nozzle
The length of row is gradually decrease to 0.Side parts film is set gradually to be increased with close to edge by the time sprayed.
Below spray head, there is bath foam collecting tank, the downward projection of spray head falls in bath foam collecting tank.Bath foam is received
Collection groove is connected with shower liquid storage tank.The bath foam of spray is flowed into bath foam collecting tank through film, returns shower liquid storage tank
Interior recycling use.
Air knife is installed in the spray cephalic par close to stretcher and/or the spray head side close to thin film center, leaned on
The air knife length of the spray cephalic par of nearly stretcher is more than X, and the air knife length close to thin film center spray head side is more than L.
Air knife removes the bath foam of film surface, and blocks the central area of bath foam inflow film.
The temperature of side parts film surface during to change stretching, in stretcher, side parts above and or below
The plenum chamber for improving temperature, plenum chamber width Y=20~200mm of side parts, length and the stretching in stretcher are set
Zone length is identical, and the plenum chamber of side parts is connected with improving the heating facility of temperature, and middle part plenum chamber hot blast temperature is
G, the hot blast temperature of side parts plenum chamber is (1.0~1.5 times) G, up to 375 DEG C.
In imination equipment, before high-temperature region is entered, to improve the temperature of side parts film surface, in the wide Z of film
The above and or belows of side parts install auxiliary heating tube additional, the Z=20~200mm, the auxiliary heating tube is arranged as
Equidistant 2~6 row, length direction are parallel with film direct of travel, the front end of auxiliary heating tube row and entering for imination equipment
Mouth end is equal, before the high-temperature region for extending to imination equipment, that is, the length for aiding in heating tube row is imidization zone length
1/2 to 3/4, auxiliary heating tube is k with film surface vertical range, is gradually reduced with close to film outer rim k.In film outer rim
The auxiliary heating tube of side and/or lower section is with film surface apart from minimum K, K=10~30mm, k=(1~5) K.
Compared with prior art, a kind of method for improving Polyamic Acid Film side imines rate of the present invention and facility is excellent
Put and be：1st, the imines rate of the side parts of Polyamic Acid Film two is improved, and is allowed to intensity increase, i.e., in this after-drawing or tensioning
The thin film strength increase of chain pincers or fibula origin of force of clamping device, makes the de- pincers or dropout failure caused by clipping broken, pulling open
It is not susceptible to, from the point of view of testing, edge damage, the situation of film breakage seldom occur, and film product yield is greatly improved；2nd, this method and set
Apply and be easily achieved, need to only adjust time, the vertical range of heating tube and film surface or the independent temperature control of chemical imidization processing
Plenum chamber hot blast temperature, you can control the side parts of Polyamic Acid Film two imines rate, obtain both sides reinforcement polyamides
Amino acid film.
Brief description of the drawings
Fig. 1 for this raising Polyamic Acid Film side imines rate facility embodiment self-supporting Polyamic Acid Film from steel
Take enter after peeling off before stretcher, local heating pipe schematic diagram above film side parts in traveling process.
Fig. 2 is the cross-sectional view of mono- avris of Fig. 1.
Fig. 3 is the facility embodiment of this raising Polyamic Acid Film side imines rate in the self-supporting peeled off from steel band
On Polyamic Acid Film transmission stroke, before stretcher is entered, the chemical imidization facility schematic diagram set in film side.
Fig. 4 for Fig. 3 A-A to sectional view；
Fig. 5 is the static pressure of stretch zones in the facility embodiment transverse stretching machine of this raising Polyamic Acid Film side imines rate
Case cross-sectional view.
Fig. 6 is imidization region avris in the facility embodiment transverse stretching machine of this raising Polyamic Acid Film side imines rate
Auxiliary heating tube top view.
Fig. 7 is the cross-sectional view of a Fig. 6 avris.
In figure marked as：1st, film, 2, heating tube, 3, air knife, 4, bath foam collecting tank, 5, spray head, 6, bath foam storage
Tank, 7, shower liquid pipe, 8, plenum chamber, 9, auxiliary heating tube, 10, imidization heating tube.
Embodiment
Improve the facility embodiment of Polyamic Acid Film side imines rate
The facility embodiment of this raising Polyamic Acid Film side imines rate includes mould, and carrying salivation shaping is poly-
The circulation steel band and baking oven of amic acid liquid film, are followed by transverse stretching machine, and transverse stretching machine is divided into stretch zones and imidization region, are drawn horizontal
Cross directional stretch and imidization are respectively completed in two regions of machine.
After Polyamic Acid Film 1 is peeled off from steel band, before transverse stretching machine is entered, its laterally wide X=in the traveling process of film 1
Heating tube 2 is installed, as shown in figure 1, laterally equidistantly arrangement 4 is arranged in the range of wide 100mm in the range of 100mm above side parts
The length direction heating tube 2 parallel with the direct of travel of film 1, the length L=u*t that heating tube 2 is arranged, wherein u represents that film 1 is advanced
Speed, this example u=6.0m/min, t represents the treatment time of film 1, this example t=45 seconds, this example L=4.5m.As shown in Fig. 2 this
Heating tube 2 of the example above the outer rim of film 1 and the surface vertical range minimum M=20mm of film 1, with leaving the outer rim m of film 1 gradually
Increase, be 60mm with the top heating tube 2 at the outer rim horizontal range 100mm of film 1 and the vertical range on the surface of film 1.
After Polyamic Acid Film 1 is peeled off from steel band, before transverse stretching machine is entered, the side of film 1 sets chemical imidization to spray
Shower device, as shown in figure 3, spray equipment includes spray head 5 and shower liquid pipe 7, this example is in the range of laterally wide X=120mm
Spray head 5 is installed in the top of film 1, and spray head 5 connects shower liquid pump, shower liquid pump connection shower liquid storage tank 6 through shower liquid pipe 7.
As shown in figure 4, spray head 5 is spray face towards the surface of film 1, width is uniform towards the table of film 1 in 120mm, spray face
The nozzle in face.Spray face is 4.5m close to the length of the nozzle file at the edge of film 1, with close to film 1 center, nozzle file
Length is gradually decrease to 0., there is bath foam collecting tank 4 lower section of spray head 5, the downward projection of spray head 5 falls in bath foam collecting tank
In 4.Bath foam collecting tank 4 is connected with shower liquid storage tank 6.The bath foam of spray is flowed into bath foam collecting tank 4 through film 1,
Return recycling use in shower liquid storage tank 6.
This example is mounted on air knife in the end of spray head 5 close to transverse stretching machine and close to the side of spray head 5 of thin film center
3, the length of air knife 3 close to the end of spray head 5 of transverse stretching machine is 200mm, the air knife 3 close to the side of spray head 5 at the center of film 1
Length is 5.0m.
The top of stretch zones side parts of this example in transverse stretching machine sets the plenum chamber 8 of independent temperature control, side parts
The width Y=120mm of plenum chamber 8, as shown in Figure 5.The length of this example plenum chamber and the stretch zones length of transverse stretching machine are all mutually
7.5m.The installation site of the plenum chamber 8 of independent temperature control is with the vertical on the longitudinal centre line of film 1 above 1 liang of side parts of film
Plane is symmetrical.The plenum chamber 8 of side parts is connected with improving the heating facility of temperature, plenum chamber hot blast temperature in the middle part of this example
210 DEG C, the hot blast temperature of side parts plenum chamber 8 is 1.25 times of middle part plenum chamber hot blast temperature, is 262.5 DEG C.
Imidization region of this example in transverse stretching machine, before high-temperature region is entered, in the range of the wide Z=120mm of side parts,
In the equidistant 4 row length direction of the top of the film 1 arrangement auxiliary heating tube 9 parallel with the direct of travel of film 1, heating tube is aided in
9 row length and transverse stretching machine imidization zone length 3/4 be 6.0m, as shown in fig. 6, original imidization heating tube in figure
10 is vertical with the direct of travel of film 1, and the front end that auxiliary heating tube 9 is arranged is equal with the entrance point of imination equipment, extends to imines
Before the high-temperature region for changing equipment.As shown in fig. 7, auxiliary heating tube 9 is k with the surface vertical range of film 1, with close to outside film 1
Edge k is gradually reduced, auxiliary heating tube 9 of this example above the outer rim of film 1 and film 1 surface distance minimum K, K=30mm, with
Top auxiliary heating tube 9 and the vertical range on the surface of film 1 at the outer rim horizontal range 120mm of film 1 are 80mm.1 liang of film
The setting height(from bottom) of auxiliary heating tube 9 is symmetrical with the vertical plane on the longitudinal centre line of film 1 above side parts.
Improve the embodiment of the method for Polyamic Acid Film side imines rate
This example uses the facility embodiment of above-mentioned raising Polyamic Acid Film side imines rate.
The self-supporting Polyamic Acid Film 1 peeled off from steel band is before transverse stretching machine is entered, the avris of film 1 during traveling
The heating tube 2 installed in the range of the X=100mm of part by its top carries out local heat treatment, the heating of the outer fringe surface of this example film 1
Temperature gradually decreases down room temperature up to 180 DEG C from edge to the surface temperature of center position film 1.The side parts local heating time
For 60 seconds.
To the Polyamic Acid Film 1 peeled off from steel band, before transverse stretching machine is entered, the side of the width X=120mm scopes of film 1
Side part spray chemical imidization bath foam 56 seconds, carries out topochemistry imidization.It is dehydrated in this example chemical imidization bath foam
Agent is acetic anhydride and TFAA, and catalyst is quinoline and triethanolamine.The proportioning of chemical imidization bath foam is with parts by weight
Material is remembered：35~45 parts of acetic anhydride, 25~30 parts of TFAA, 45~50 parts of quinoline, 50~60 parts of triethanolamine.
The hot blast temperature of plenum chamber 8 of the side parts independence temperature control of stretch zones is improved in this example transverse stretching machine, polyamic acid
The surface temperature at the middle part of film 1 is 210 DEG C, and the wide Y=120mm boundary inner surfaces temperature of side parts is 265.5 DEG C, is that middle part is thin
1.25 times of the surface temperature of film 1.
Polyamic Acid Film 1 in this example transverse stretching machine imidization region, the side parts Z=before high-temperature region is entered
The auxiliary heating tube 9 installed in the range of 120mm by its top is further heated, the surface temperature H=at the middle part of Polyamic Acid Film 1
320 DEG C~450 DEG C gradually rise, and the surface temperature of film 1 is than the table of middle part film 1 in the range of the wide Z=120mm of the outer rim of this example film 1
Face temperature is high 70 DEG C~and 200 DEG C, gradually decreased down and the surface temperature of middle part film 1 from edge to the surface temperature of center position film 1
Degree is identical, up to 650 DEG C.
Using the uniform film for Q=32% of imines rate as comparative example, in the cross directional stretch and tensioning imines of the same terms
In the process of change, it is compared with the film of the present embodiment processing, as a result as shown in table 1：
The film and comparative example film each operation processing situation comparison sheet of the present embodiment of table 1 processing
| The present embodiment | Comparative example | |
| Into horizontal drawing process front middle part imines rate | 32 | 32 |
| Into the horizontal maximum imines rate of drawing process cephalolateral margin | 64 | 32 |
| Horizontal torn selvedge number (individual/h) | 0.002 | 1.041 |
| It is horizontal to break film number (secondary/h) | 0 | 0.9 |
| Into imidization process front middle part imines rate | 46 | 46 |
| Into the maximum imines rate of imidization process cephalolateral margin | 78 | 46 |
| Imidization edge damage number (individual/h) | 0.001 | 0.896 |
| Imidization film breakage number (secondary/h) | 0 | 0.75 |
| Into high temperature imidization front middle part imines rate | 68 | 68 |
| Into the maximum imines rate of high temperature imidization cephalolateral margin | 86 | 68 |
| High temperature imidization edge damage number (individual/h) | 0.001 | 0.802 |
| High temperature imidization film breakage number (secondary/h) | 0 | 0.72 |
| The edge damage of horizontal drawing and imidization process is total (individual/h) | 0 | 0.851 |
| The film breakage of horizontal drawing and imidization process is total (individual/h) | 0 | 0.73 |
| Thin film yield (%) | 100 | 86 |
| Film yield (%) | 98 | 74 |
The method that Polyamic Acid Film side imines rate is improved using the present invention, makes Polyamic Acid Film side parts
Imines rate is apparently higher than the imines rate of central film portion, and the intensity of film avris improves.It is only in the edge damage number of horizontal drawing process
The 0.2% of traditional films, edge damage number of times is significantly reduced in imidization process, the stretching on Production Line for Polyimide Film and
Total film breakage number of times tends to 0 in tensioning imidization, and product yield tends to 100.0%, and product yield is up to 98.0%.
Above-described embodiment, is only to the specific of the purpose of the present invention, technical scheme and beneficial effect further description
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 (10)
1. a kind of method for improving Polyamic Acid Film side imines rate, polyamic acid solution salivates on steel band and is shaped to gather
Amic acid liquid film, by hot-air oven dry as self-supporting Polyamic Acid Film, then stretched, imidization processing；Its
It is characterised by：
To the Polyamic Acid Film peeled off from steel band, before being stretched, the wide X of the side parts of film two scope heating 8
Second~80 seconds, gradually risen with close to outer rim temperature, outer most edge film surface temperature T=150~200 DEG C, the X=20~
200mm。
2. the method according to claim 1 for improving Polyamic Acid Film side imines rate, it is characterised in that：
To the Polyamic Acid Film peeled off from steel band, before being stretched, the wide X of the film chemical imines of side parts spray
Change bath foam 8 seconds~80 seconds, the carry out topochemistry imidization to side parts, the X=20~200mm；
The chemical imidization bath foam contains dehydrating agent and catalyst, and wherein dehydrating agent is acetic anhydride, propionic andydride, butyric acid
It is any one in acid anhydride, benzoyl oxide, lower aliphatic halide, aryl sulfonic acid dihalide, the halide of sulfurous acid halogen and phosphorus
Plant or any several mixture；Catalyst therein is pyridine and its derivatives, picoline and its derivative, dimethyl pyrazole
It is any in pyridine, quinoline, isoquinolin, porphyrin, imidazoles, triethylamine, triethanolamine, triethylenediamine and diisopropyl ethyl amine
A kind of or any several mixture.
3. the method according to claim 1 for improving Polyamic Acid Film side imines rate, it is characterised in that：
G=150 DEG C of the surface temperature of polyamic acid central film portion~250 DEG C in stretcher, the wide Y=20 of side parts~
200mm boundary inner surface temperature g is 1.0~1.5 times of G, is gradually stepped up with close to film outer rim film surface temperature, g highests
For 375 DEG C.
4. the method according to claim 1 for improving Polyamic Acid Film side imines rate, it is characterised in that：
H=320 DEG C of the surface temperature of polyamic acid central film portion~450 DEG C gradually rise in imination equipment, the wide Y of side parts
In the range of=20~200mm before high-temperature region is entered, surface temperature h is 1.0~1.5 times of H, with close to film outer rim film
Surface temperature is gradually stepped up, and h is up to 650 DEG C.
5. the method design according to any one of claim 1 to 4 for improving Polyamic Acid Film side imines rate
The facility of Polyamic Acid Film side imines rate is improved, the preparation method for the Polyamic Acid Film that side imines rate is improved
Facility includes mould, and the circulation steel band and baking oven of carrying salivation shaping polyamic acid liquid film are followed by stretcher and Asia
Amination equipment, it is characterised in that：
After Polyamic Acid Film (1) is peeled off from steel band, before being stretched, its laterally wide X scope in film (1) traveling process
The above and or below of interior side parts installs heating tube (2), the X=20~200mm, in film (1) in the range of wide X
Above and or below arranges equidistant 2~6 row length direction heating tube (2) parallel with film (1) direct of travel, heating
The length L=u*v of (2) row is managed, wherein u represents that film gait of march, v represent film (1) treatment time, and 0.5m/min≤u
≤ 20.0m/min, 8 seconds≤v≤80 second；Heating tube (2) and film (1) surface vertical range are m, with close to film (1) outer rim m
It is gradually reduced；In the heating tube (2) and film (1) minimum M of surface distance, M=10 of film (1) outer rim above and or below
~30mm, m=(1~8) M.
6. the facility according to claim 5 for improving Polyamic Acid Film side imines rate, it is characterised in that：
On the Polyamic Acid Film transmission stroke peeled off from steel band, before being stretched, chemistry is set in film (1) side
Imidization spray equipment, spray equipment includes spray head (5) and shower liquid pipe (7), upper in the range of film (1) laterally wide X
Side and/or lower section installation spray head (5), the X=20~200mm, spray head (5 connect shower liquid pump through shower liquid pipe (7),
Shower liquid pump connection shower liquid storage tank (6)；Spray head (5) is spray face towards film (1) surface, and width is X, spray face
The upper uniform nozzle towards film (1)；Spray face is L close to the length of the nozzle file at film (1) edge, with close to film
(1) center, the length of nozzle file are gradually decrease to 0.
7. the facility according to claim 6 for improving Polyamic Acid Film side imines rate, it is characterised in that：
Below the spray head (5), there is bath foam collecting tank (4), the downward projection of spray head (5) falls in bath foam collecting tank
(4) in.
8. the facility according to claim 6 for improving Polyamic Acid Film side imines rate, it is characterised in that：
Gas is installed in spray head (5) end close to stretcher and/or close to spray head (5) side at film (1) center
Knife (3), air knife (3) length close to spray head (5) end of stretcher is more than X, the spray head close to film (1) center
(5) air knife (3) length of side is more than L.
9. the facility according to claim 5 for improving Polyamic Acid Film side imines rate, it is characterised in that：
In stretcher, the plenum chamber (8) of side parts above and or below setting raising temperature, the static pressure of side parts
Case (8) width Y=20~200mm, length is identical with the stretch zones length in stretcher, the plenum chamber (8) of side parts
It is connected with the heating facility for improving temperature, middle part plenum chamber hot blast temperature is G, the hot blast temperature of side parts plenum chamber (8)
For (1.0~1.5) times of middle part plenum chamber hot blast temperature, up to 375 DEG C.
10. the facility according to claim 5 for improving Polyamic Acid Film side imines rate, it is characterised in that：
Above and or below in film (1) width Z side parts in imination equipment installs auxiliary heating tube (9) additional, described
Z=20~200mm, the auxiliary heating tube (9) is arranged as equidistant 2~6 row, length direction and film (1) direct of travel
Parallel, the front end of auxiliary heating tube (9) row is equal with the entrance point of imination equipment, extends to the high temperature of imination equipment
Before area, that is, the length for aiding in heating tube (9) row is the 1/2 to 3/4 of imidization zone length, auxiliary heating tube (9) and film
(1) surface vertical range is k, is gradually reduced with close to film (1) outer rim k；In the auxiliary of film (1) outer rim above and or below
Help heating tube (9) and film (1) minimum K of surface distance, K=10~30mm, k=(1~5) K.
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| CN201410839912.8A CN104497340B (en) | 2014-12-30 | 2014-12-30 | Improve the method and facility of Polyamic Acid Film side imines rate |
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| CN104497340B true CN104497340B (en) | 2017-07-14 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104070666A (en) * | 2013-03-26 | 2014-10-01 | 富士胶片株式会社 | Method of producing stretching film and film stretching facility |
| CN104149368A (en) * | 2014-07-28 | 2014-11-19 | 浙江绍兴华东包装有限公司 | Single-point and double-point switching type BOPET thin film processing device and method |
| CN204354377U (en) * | 2014-12-30 | 2015-05-27 | 桂林电器科学研究院有限公司 | Improve the facility of Polyamic Acid Film side imines rate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104070666A (en) * | 2013-03-26 | 2014-10-01 | 富士胶片株式会社 | Method of producing stretching film and film stretching facility |
| CN104149368A (en) * | 2014-07-28 | 2014-11-19 | 浙江绍兴华东包装有限公司 | Single-point and double-point switching type BOPET thin film processing device and method |
| CN204354377U (en) * | 2014-12-30 | 2015-05-27 | 桂林电器科学研究院有限公司 | Improve the facility of Polyamic Acid Film side imines rate |
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