CN104497340A - Method and facility for improving amination rate of side of polyamide acid film - Google Patents

Method and facility for improving amination rate of side of polyamide acid film Download PDF

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Publication number
CN104497340A
CN104497340A CN201410839912.8A CN201410839912A CN104497340A CN 104497340 A CN104497340 A CN 104497340A CN 201410839912 A CN201410839912 A CN 201410839912A CN 104497340 A CN104497340 A CN 104497340A
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film
polyamic acid
temperature
facility
acid film
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CN104497340B (en
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任小龙
姬亚宁
刘业强
周福龙
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Guilin Electrical Equipment Scientific Research Institute Co Ltd
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Guilin Electrical Equipment Scientific Research Institute Co Ltd
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Abstract

The invention discloses a method and facility for improving amination rate of a side of a polyamide acid film. According to the method, the side is heated before the polyamide acid film stripped from a steel band is stretched; the temperature close to an outer edge is gradually increased; the side of the film is sprayed with a chemical amination bath foam before being stretched; the surface temperature of the side of the polyamide acid film is improved during the stretching process; the surface temperature of the side of the polyamide acid film is improved before entering a high-temperature zone in amination; and amination is carried out in advance, so as to increase the strength. By virtue of the facility, a plurality of columns of heating tubes are arranged above and/or below the side part of the film before equipment is stretched; a chemical amination spraying device is arranged on the side of the film before the equipment is stretched; plenum chambers for improving temperature are arranged above and/or below the side part in the stretching equipment; and auxiliary heating tubes are additionally arranged above and/or below the side part of the film. The method and the facility are easy to implement; the amination rate of the side of the film is improved; and the strength is increased; the film is prevented from being broken in gripping and pulling manners; and the yield of the film is improved.

Description

Improve method and the facility of Polyamic Acid Film side imines rate
Technical field
The present invention relates to Kapton manufacturing technology, be specially a kind of method and the facility that improve Polyamic Acid Film side imines rate.
Background technology
Kapton is the macromolecular material with high strength, high tenacity, abrasion performance, the excellent properties such as high temperature resistant, corrosion-resistant, is the predominating insulation making various medium-to-high grade electrotechnical, electronic components and parts, is widely used in electrotechnical, electronic industry.The preparation technology of current Kapton is with polyamic acid resin solution for raw material, and on slobbering machine, salivation obtains the Polyamic Acid Film of self-supporting, then through adding thermal stretch, high temperature imidization, cooling and shaping process obtain Kapton.
The design requirements of and high reliability light, thin, short, little along with downstream application product, the film thickness specification of the market requirement is tending towards slimming, to its technology of preparing, quality product particularly product yield all have higher requirement.
In Kapton preparation process, the conventional manufacturing process of drawing and setting or tensioning sizing that adopts reaches required thickness and traditional performance.All need two sides gripping Kapton work in-process Polyamic Acid Film when drawing and setting or tensioning sizing, rely on the clamping device of film both sides to apply horizontal force to film under the high temperature conditions, namely cross directional stretch is carried out to film.Also need during longitudinal stretching to grip film dual-side, avoid film to reduce width to central reduction distortion.
Such as, when Kapton is produced, normally polyamic acid resin is shaped to Polyamic Acid Film by salivation mode on slobbering machine, carries out imidization process by High Temperature Furnaces Heating Apparatus afterwards and obtain Kapton.The bilateral of work in-process film to be gripped in imidization, make film under clamp position, carry out cross directional stretch or tensioning process, and keep this state to complete high temperature imidization, to improve the traditional performance of film.
The clamping device of existing film line both sides is mainly and is arranged on chain pincers on the chain of ring-shaped guide rail or pin is buckled.The imidization that vertical cross directional stretch all will carry out pyroprocessing, particularly Polyamic Acid Film to film needs the process of higher temperature, and maximum processing temperature can reach 500 DEG C.Chain in production line and on chain pincers or pin buckle temperature in high temperature environments and also increase, when stretching entry position clamping film very easily because high temperature causes film side to clip broken or tear, the film of side breakage in follow-up stretching, imidization, shape and open in the technological processs such as folder and easily buckle thorn button bit in chain pincers pincers mouth position or pin and put and cause de-pincers or dropout and pulled open, reduce film stretching quality, even film cannot normally rolling, reduce film product yield, have a strong impact on film line output.
Meanwhile, the edge of Polyamic Acid Film upwarps phenomenon due to too thin easy generation, makes film side edge break build up double-deck limit during the clamping of chain pincers.Running into high temperature in the clamping process of double-deck limit makes chain pincers clip position film easily tear, and causes product can not normally rolling equally, reduction film product yield.
In actual production line, Kapton open pincers position close to traction wrap-up, when driving pincers, film is subject to the comprehensive actions such as tensile stress, drawing tension and winding tension and easily occurs the rupture of membranes such as raw edges, transverse breakage phenomenon, so that film cannot normally rolling, have a strong impact on thin film yield, reduce film yield.
In order to solve edge damage in Kapton preparation process, the problems such as disconnected film, in recent years there is relevant patent application, as the Chinese utility model patent " the entering pincers guide arrangement of membrane production equipment " that notification number is CN202245464U, publication number is the Chinese invention patent " the chain pincers refrigerating unit of film production machinery " of CN102441987A, publication number is the Chinese invention patent " the opening pincers device in advance of film line " of CN102431161A, publication number is the Chinese invention patent " film clamping device of film of film stretching sizing or tensioning standard equipment " of CN102390112A, notification number is the Chinese utility model patent " a kind of solution film stretching rupture of membranes and thickness homogeneous system " of CN203236699U, wherein individually disclose into pincers guide arrangement, chain pincers refrigerating unit, drive pincers device and clamping device etc. in advance, although clamping device is caused clip broken or Tear Film side problem some reduce, but and fail to eliminate this type of fault completely.And these devices all need to transform existing apparatus for production line or replace, apparatus structure is comparatively complicated, also needs higher improvement cost, therefore is difficult to extensively practice.
In addition publication number is the Chinese invention patent " adhesive tape processing method in film production of slobbering machine " of CN102416684A, publication number is the Chinese invention patent " method for adhesive tape treatment in production of thin film by casting machine " of CN102303388A, notification number is the Chinese utility model patent " polyimide film producing device of automatic erasing releasing agent " etc. of CN202147343U is cause rupture of membranes by improving manufacturing process process salivation adhesive tape, disconnected films etc. are abnormal, adjusting process parameter is more, regulation range is large, particularly introduce as wiping releasing agent can cause film too smooth cannot normal use in the side effect etc. of derived product.
Summary of the invention
The object of this invention is to provide a kind of method improving Polyamic Acid Film side imines rate, the side parts of the Polyamic Acid Film one fixed width peeled off from salivation steel band is heated, raise gradually with close to outer rim temperature, the imines rate of film side parts is made to improve, reduce the polyamide acid content of film side parts, thus the intensity of Polyamic Acid Film side is increased, not easily clipped broken or the fault of raw edges by during clamping, be ensure that the quality of film, improved thin film yield.
Another object of the present invention is a kind of facility improving Polyamic Acid Film side imines rate of design, heating tube is installed in above the side parts peeling off one fixed width in rear film traveling process at Polyamic Acid Film from steel band and/or below, with close to outer rim, heating tube and film surface distance reduce gradually, make the temperature of film side parts raise imines rate and improve.
A kind of method improving Polyamic Acid Film side imines rate of the present invention's design, polyamic acid solution salivate and is shaped to polyamic acid liquid film on steel band, through the dry Polyamic Acid Film becoming self-supporting of hot-air oven, then carry out stretching, imidization process.To the Polyamic Acid Film peeled off from steel band, before stretching, the scope of the wide X of film two side parts is heated 8 seconds ~ 80 seconds, raises gradually, outer most edge film surface temperature T=150 ~ 200 DEG C, described X=20 ~ 200mm with close to outer rim temperature.
For improving the imines rate of Polyamic Acid Film dual-side further, to the Polyamic Acid Film peeled off from steel band, before stretching, the side parts spray chemical imidization bathing agents of the wide X of film 8 seconds ~ 80 seconds, opposite side side part carries out topochemistry imidization, described X=20 ~ 200mm.The polyimide content of film side parts increases further, imines rate is improved again, and its intensity is strengthened further.
Described chemical imidization bathing agents be in the industry known chemical imidization bathing agents, containing dewatering agent and catalyzer.Wherein dewatering agent is any one or the mixture several arbitrarily in the halogenide of diacetyl oxide, propionic anhydride, butyryl oxide, benzoyl oxide, lower aliphatic halogenide, aryl sulfonic acid dihalide, sulfurous acid halogen and phosphorus; Catalyzer is wherein any one or mixtures several arbitrarily in pyridine and its derivatives, picoline and derivative thereof, lutidine, quinoline, isoquinoline 99.9, porphyrin, imidazoles, triethylamine, trolamine, triethylenediamine and diisopropyl ethyl amine.The proportioning of chemical imidization solution is general known proportioning.
Improve the surface temperature of Polyamic Acid Film two avris during stretching, also can improve the intensity of film avris further.Surface temperature G=150 DEG C in stretcher in the middle part of Polyamic Acid Film ~ 250 DEG C, side parts wide Y=20 ~ 200mm boundary inner surface temperature g is 1.0 ~ 1.5 times of G, and improve gradually with close to film outer rim film surface temperature, g is up to 375 DEG C.
During imidization, before entering high-temperature zone, improve the surface temperature of Polyamic Acid Film two avris, make film avris complete imidization in advance, increase its intensity.Surface temperature H=320 DEG C in imination equipment in the middle part of Polyamic Acid Film ~ 450 DEG C raise gradually, before side parts wide Y=20 ~ 200mm scope inherence enters high-temperature zone, surface temperature h is 1.0 ~ 1.5 times of H, improve gradually with close to film outer rim film surface temperature, h is up to 650 DEG C.
A kind of facility improving Polyamic Acid Film side imines rate of the present invention's design comprises forming mould, the circulation steel band of the shaping polyamic acid liquid film of carrying salivation and baking oven, thereafter be stretcher and imination equipment, Polyamic Acid Film is after steel band stripping, before entering stretcher, in film traveling process its laterally within the scope of wide X the top of side parts and/or below heating tube is installed, described X=20 ~ 200mm, within the scope of wide X, above film and/or equally spaced 2 ~ 6 row length directions of the arranged beneath heating tube parallel with film direct of travel, the length L=u*v of heating tube row, wherein u represents film gait of march, v represents the film treatment time, and 0.5m/min≤u≤20.0m/min, 8 seconds≤v≤80 second.Heating tube and film surface vertical range are m, reduce gradually with close to film outer rim m.Above film outer rim and/or the heating tube of below and film surface apart from minimum be M, M=10 ~ 30mm, m=(1 ~ 8) M.Above film two side parts and/or the mounting height of below heating tube with the vertical plane symmetry on film longitudinal cenlerline.
When carrying out chemical imidization, the Polyamic Acid Film peeled off from steel band transmits on stroke, before entering stretcher, film side arranges chemical imidization spray equipment, spray equipment comprises spray header and bathing agents pipe, and spray header is installed, described X=20 ~ 200mm in above the film within the scope of horizontal wide X and/or below, spray header connects shower liquid pump through bathing agents pipe, and shower liquid pump connects bathing agents basin.Spray header is spray face towards film surface, and width is X, the uniform nozzle towards film surface in spray face.Spray face is L near the length of the nozzle file of film edge, is decreased to 0 gradually with the length close to thin film center, nozzle file.The time that side parts film is sprayed increases gradually with close to edge.
Below spray header, have bathing agents receiving tank, the downward projection of spray header drops in bathing agents receiving tank.Bathing agents receiving tank is connected with bathing agents basin.The bathing agents of spray flows in bathing agents receiving tank through film, returns recycling use in bathing agents basin.
Be provided with air knife in the spray header end near stretcher and/or the spray header side near thin film center, the air knife length near the spray header end of stretcher is greater than X, and the air knife length near thin film center spray header side is greater than L.The bathing agents of air knife removing film surface, and block the central zone that bathing agents flows into film.
The temperature of side parts film surface when for a change stretching, in stretcher, above side parts and/or below arrange and improve the plenum chamber of temperature, the plenum chamber width Y=20 ~ 200mm of side parts, length is identical with the stretch zones length in stretcher, the plenum chamber of side parts is connected with the heating facility improving temperature, middle part plenum chamber hot blast temperature is G, and the hot blast temperature of side parts plenum chamber is (1.0 ~ 1.5 times) G, is up to 375 DEG C.
In imination equipment, before entering high-temperature zone, for improving the temperature of side parts film surface, boosting pipe is installed additional in the top of the side parts of the wide Z of film and/or below, described Z=20 ~ 200mm, described boosting pipe is arranged as equally spaced 2 ~ 6 row, length direction is parallel with film direct of travel, the front end of boosting pipe row is equal with the entrance end of imination equipment, before extending to the high-temperature zone of imination equipment, namely the length of boosting pipe row is 1/2 to 3/4 of imidization zone length, boosting pipe and film surface vertical range are k, reduce gradually with close to film outer rim k.Above film outer rim and/or the boosting pipe of below and film surface apart from minimum be K, K=10 ~ 30mm, k=(1 ~ 5) K.
Compared with prior art, the advantage of the present invention a kind of method and facility that improve Polyamic Acid Film side imines rate is: 1, the imines rate of Polyamic Acid Film two side parts improves, make it intensity to increase, namely when this back draft or tensioning, the chain pincers of clamping device or the thin film strength of fibula origin of force increase, make because clipping broken, pulling open the de-pincers that causes or dropout fault not easily occurs, by testing, the situation of edge damage, disconnected film seldom occurs, and film product yield improves greatly; 2, present method and facility are easy to realize, only need regulate the time of chemical imidization process, heating tube and the vertical range of film surface or the plenum chamber hot blast temperature of independent temperature control, the imines rate of Polyamic Acid Film two side parts can be controlled, obtain the Polyamic Acid Film that both sides are strengthened.
Accompanying drawing explanation
Fig. 1 is local heating pipe schematic diagram above the film side parts before the facility embodiment self-supporting Polyamic Acid Film of this raising Polyamic Acid Film side imines rate enters stretcher after steel band stripping, in traveling process.
Fig. 2 is the cross-sectional view of Fig. 1 avris.
Fig. 3 is that the facility embodiment of this raising Polyamic Acid Film side imines rate transmits on stroke at the self-supporting Polyamic Acid Film peeled off from steel band, before entering stretcher, at the chemical imidization facility schematic diagram that film side is arranged.
Fig. 4 is that the A-A of Fig. 3 is to sectional view;
Fig. 5 be this raising Polyamic Acid Film side imines rate facility embodiment transverse stretching machine in the plenum chamber cross sectional representation of stretch zones.
Fig. 6 be this raising Polyamic Acid Film side imines rate facility embodiment transverse stretching machine in the boosting pipe vertical view of imidization region avris.
Fig. 7 is the cross-sectional view of an avris of Fig. 6.
Number in the figure is: 1, film, 2, heating tube, 3, air knife, 4, bathing agents receiving tank, 5, spray header, 6, bathing agents basin, 7, bathing agents pipe, 8, plenum chamber, 9, boosting pipe, 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 comprises forming mould, the circulation steel band of the shaping polyamic acid liquid film of carrying salivation and baking oven, thereafter be transverse stretching machine, transverse stretching machine is divided into stretch zones and imidization region, in two regions of transverse stretching machine, complete cross directional stretch and imidization respectively.
Polyamic Acid Film 1 is after steel band stripping, before entering transverse stretching machine, above side parts, heating tube 2 is installed within the scope of its horizontal wide X=100mm in film 1 traveling process, as shown in Figure 1, the heating tube 2 that laterally equidistantly arrangement 4 row length directions are parallel with film 1 direct of travel within the scope of wide 100mm, the length L=u*t that heating tube 2 arranges, wherein u represents film 1 gait of march, this routine u=6.0m/min, t represent film 1 treatment time, this routine t=45 second, this routine L=4.5m.As shown in Figure 2, the heating tube of this example above film 1 outer rim 2 and the minimum M=20mm of the surperficial vertical range of film 1, strengthening gradually with leaving film 1 outer rim m, is 60mm with the top heating tube 2 at film 1 outer rim horizontal throw 100mm place and the vertical range on film 1 surface.
Polyamic Acid Film 1 is after steel band stripping, before entering transverse stretching machine, film 1 side arranges chemical imidization spray equipment, as shown in Figure 3, spray equipment comprises spray header 5 and bathing agents pipe 7, install spray header 5 above the film 1 of this example within the scope of horizontal wide X=120mm, spray header 5 connects shower liquid pump through bathing agents pipe 7, and shower liquid pump connects bathing agents basin 6.As shown in Figure 4, spray header 5 is spray face towards film 1 surface, and width is 120mm, the uniform nozzle towards film 1 surface in spray face.Spray face is 4.5m near the length of the nozzle file at film 1 edge, is decreased to 0 gradually with the length close to film 1 center, nozzle file.Below spray header 5, have bathing agents receiving tank 4, the downward projection of spray header 5 drops in bathing agents receiving tank 4.Bathing agents receiving tank 4 is connected with bathing agents basin 6.The bathing agents of spray flows in bathing agents receiving tank 4 through film 1, returns recycling use in bathing agents basin 6.
This example is all provided with air knife 3 in spray header 5 end near transverse stretching machine and spray header 5 side near thin film center, and air knife 3 length near spray header 5 end of transverse stretching machine is 200mm, and air knife 3 length near spray header 5 side at film 1 center is 5.0m.
The plenum chamber 8 of independent temperature control is set, the plenum chamber 8 width Y=120mm of side parts, as shown in Figure 5 above the stretch zones side parts of this example in transverse stretching machine.The length of this routine plenum chamber is all 7.5m mutually with the stretch zones length of transverse stretching machine.Above film 1 liang of side parts, the installation site of the plenum chamber 8 of independent temperature control is with the vertical plane symmetry on film 1 longitudinal cenlerline.The plenum chamber 8 of side parts is connected with the heating facility improving temperature, this example middle part plenum chamber hot blast temperature 210 DEG C, side parts plenum chamber 8 hot blast temperature be in the middle part of 1.25 times of plenum chamber hot blast temperature, be 262.5 DEG C.
The imidization region of this example in transverse stretching machine, before entering high-temperature zone, within the scope of the wide Z=120mm of side parts, the boosting pipe 9 that equally spaced 4 row length directions are parallel with film 1 direct of travel is arranged above film 1, the imidization zone length of the length that boosting pipe 9 arranges and transverse stretching machine 3/4 be 6.0m, as shown in Figure 6, in figure, original imidization heating tube 10 is vertical with film 1 direct of travel, the front end that boosting pipe 9 arranges is equal with the entrance end of imination equipment, before extending to the high-temperature zone of imination equipment.As shown in Figure 7, boosting pipe 9 and the surperficial vertical range of film 1 are k, reduce gradually with close to film 1 outer rim k, the boosting pipe 9 of this example above film 1 outer rim is minimum with film 1 surface distance is K, K=30mm is 80mm with the top boosting pipe 9 at film 1 outer rim horizontal throw 120mm place and the vertical range on film 1 surface.Above film 1 liang of side parts, the mounting height of boosting pipe 9 is with the vertical plane symmetry on film 1 longitudinal cenlerline.
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 entering transverse stretching machine, local heat treatment is carried out by the heating tube 2 installed above it within the scope of film 1 side parts X=100mm in traveling process, this routine film 1 outer fringe surface Heating temperature reaches 180 DEG C, drops to room temperature by edge gradually to center position film 1 surface temperature.The side parts local heating time is 60 seconds.
To the Polyamic Acid Film 1 peeled off from steel band, before entering transverse stretching machine, the side parts spray chemical imidization bathing agents of the wide X=120mm scope of film 1 56 seconds, carries out topochemistry imidization.In this routine chemical imidization bathing agents, dewatering agent is diacetyl oxide and trifluoroacetic anhydride, and catalyzer is quinoline and trolamine.The proportioning of chemical imidization bathing agents is remembered with weight part material: diacetyl oxide 35 ~ 45 parts, trifluoroacetic anhydride 25 ~ 30 parts, 45 ~ 50 parts, quinoline, trolamine 50 ~ 60 parts.
In this routine transverse stretching machine, plenum chamber 8 hot blast temperature of the side parts independence temperature control of stretch zones improves, surface temperature in the middle part of Polyamic Acid Film 1 is 210 DEG C, side parts wide Y=120mm boundary inner surface temperature is 265.5 DEG C, is 1.25 times of middle part film 1 surface temperature.
Polyamic Acid Film 1 in this routine transverse stretching machine imidization region, heated further by the boosting pipe 9 installed above it within the scope of side parts Z=120mm before entering high-temperature zone, surface temperature H=320 DEG C in the middle part of Polyamic Acid Film 1 ~ 450 DEG C raise gradually, within the scope of the wide Z=120mm of this routine film 1 outer rim film 1 surface temperature higher than middle part film 1 surface temperature 70 DEG C ~ 200 DEG C, drop to center position film 1 surface temperature identical with middle part film 1 surface temperature gradually by edge, be up to 650 DEG C.
With imines rate evenly for the film of Q=32% is for comparative example, in the cross directional stretch of the same terms and the operation of tensioning imidization, compare with the film of the present embodiment process, result is as shown in table 1:
The film of table 1 the present embodiment process and comparative example film each operation processing situation comparison sheet
The present embodiment Comparative example
Enter and horizontally draw operation front middle part imines rate 32 32
Enter and horizontally draw the maximum imines rate of operation cephalolateral margin 64 32
Horizontal torn selvedge number (individual/h) 0.002 1.041
Horizontally break film number (secondary/h) 0 0.9
Enter imidization operation front middle part imines rate 46 46
Enter the maximum imines rate of imidization operation cephalolateral margin 78 46
Imidization edge damage number (individual/h) 0.001 0.896
Imidization is broken film number (secondary/h) 0 0.75
Enter high temperature imidization front middle part imines rate 68 68
Enter 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 is broken film number (secondary/h) 0 0.72
Horizontally to draw and the edge damage sum of imidization operation (individual/h) 0 0.851
Horizontally draw the disconnected film sum (individual/h) with imidization operation 0 0.73
Thin film yield (%) 100 86
Film yield (%) 98 74
Adopt the present invention to improve the method for Polyamic Acid Film side imines rate, make the imines rate of imines rate apparently higher than central film portion of Polyamic Acid Film side parts, the intensity of film avris improves.0.2% of traditional films is only at the horizontal edge damage number of operation that draws, in imidization operation, edge damage number of times also obviously reduces, in stretching on Production Line for Polyimide Film and tensioning imidization, total disconnected film number of times is tending towards 0, and product yield is tending towards 100.0%, and product yield is up to 98.0%.
Above-described embodiment, be only the specific case further described object of the present invention, technical scheme and beneficial effect, the present invention is not defined in this.All make within scope of disclosure of the present invention any amendment, equivalent replacement, improvement etc., be all included within protection scope of the present invention.

Claims (10)

1. improve a method for Polyamic Acid Film side imines rate, polyamic acid solution salivates and is shaped to polyamic acid liquid film on steel band, becomes the Polyamic Acid Film of self-supporting through hot-air oven drying, then carry out stretching, imidization process; It is characterized in that:
To the Polyamic Acid Film peeled off from steel band, before stretching, the scope of the wide X of film two side parts is heated 8 seconds ~ 80 seconds, raises gradually, outer most edge film surface temperature T=150 ~ 200 DEG C, described X=20 ~ 200mm with close to outer rim temperature.
2. the method for raising Polyamic Acid Film side imines rate according to claim 1, is characterized in that:
To the Polyamic Acid Film peeled off from steel band, before stretching, the side parts of film wide X spray chemical imidization bathing agents 8 seconds ~ 80 seconds, carries out topochemistry imidization, described X=20 ~ 200mm to side parts;
Described chemical imidization bathing agents contains dewatering agent and catalyzer, and wherein dewatering agent is any one or the mixture several arbitrarily in the halogenide of diacetyl oxide, propionic anhydride, butyryl oxide, benzoyl oxide, lower aliphatic halogenide, aryl sulfonic acid dihalide, sulfurous acid halogen and phosphorus; Catalyzer is wherein any one or mixtures several arbitrarily in pyridine and its derivatives, picoline and derivative thereof, lutidine, quinoline, isoquinoline 99.9, porphyrin, imidazoles, triethylamine, trolamine, triethylenediamine and diisopropyl ethyl amine.
3. the preparation method of the Polyamic Acid Film of side imines rate raising according to claim 1, is characterized in that:
Surface temperature G=150 DEG C in stretcher in the middle part of Polyamic Acid Film ~ 250 DEG C, side parts wide Y=20 ~ 200mm boundary inner surface temperature g is 1.0 ~ 1.5 times of G, and improve gradually with close to film outer rim film surface temperature, g is up to 375 DEG C.
4. the preparation method of the Polyamic Acid Film of side imines rate raising according to claim 1, is characterized in that:
Surface temperature H=320 DEG C in imination equipment in the middle part of Polyamic Acid Film ~ 450 DEG C raise gradually, before side parts wide Y=20 ~ 200mm scope inherence enters high-temperature zone, surface temperature h is 1.0 ~ 1.5 times of H, improve gradually with close to film outer rim film surface temperature, h is up to 650 DEG C.
5. the facility of the raising Polyamic Acid Film side imines rate of the method design of the raising Polyamic Acid Film side imines rate according to Claims 1-4, the facility of the preparation method of the Polyamic Acid Film that side imines rate improves comprises forming mould, the circulation steel band of the shaping polyamic acid liquid film of carrying salivation and baking oven, thereafter be stretcher and imination equipment, it is characterized in that:
Polyamic Acid Film (1) is after steel band stripping, before stretching, in film (1) traveling process its laterally within the scope of wide X the top of side parts and/or below heating tube (2) is installed, described X=20 ~ 200mm, at film (1) top and/or equally spaced 2 ~ 6 row length directions of the arranged beneath heating tube (2) parallel with film (1) direct of travel within the scope of wide X, the length L=u*v that heating tube (2) arranges, wherein u represents film gait of march, v represents film (1) treatment time, and 0.5m/min≤u≤20.0m/min, 8 seconds≤v≤80 second, heating tube (2) and film (1) surperficial vertical range are m, reduce gradually with close to film (1) outer rim m, above film (1) outer rim and/or the heating tube (2) of below and film (1) surface distance minimum be M, M=10 ~ 30mm, m=(1 ~ 8) M.
6. the facility of raising Polyamic Acid Film side imines rate according to claim 5, is characterized in that:
The Polyamic Acid Film peeled off from steel band transmits on stroke, before stretching, at film (1) side, chemical imidization spray equipment is set, spray equipment comprises spray header (5) and bathing agents pipe (7), spray header (5) is installed in top within the scope of film (1) laterally wide X and/or below, described X=20 ~ 200mm, (5 connect shower liquid pump through bathing agents pipe (7) to spray header, and shower liquid pump connects bathing agents basin (6); Spray header (5) towards film (1) surface be spray face, width is X, the uniform nozzle towards film (1) in spray face; Spray face is L near the length of the nozzle file at film (1) edge, is decreased to 0 gradually with the length close to film (1) center, nozzle file.
7. the facility of raising Polyamic Acid Film side imines rate according to claim 6, is characterized in that:
Described spray header (5) below, have bathing agents receiving tank (4), the downward projection of spray header (5) drops in bathing agents receiving tank (4).
8. the facility of raising Polyamic Acid Film side imines rate according to claim 6, is characterized in that:
In spray header (5) end near stretcher and/or spray header (5) side near film (1) center, air knife (3) is installed, air knife (3) length near spray header (5) end of stretcher is greater than X, and air knife (3) length near spray header (5) side at film (1) center is greater than L.
9. the facility of raising Polyamic Acid Film side imines rate according to claim 5, is characterized in that:
In stretcher, above side parts and/or below arrange and improve the plenum chamber (8) of temperature, plenum chamber (8) width Y=20 ~ 200mm of side parts, length is identical with the stretch zones length in stretcher, the plenum chamber (8) of side parts is connected with the heating facility improving temperature, middle part plenum chamber hot blast temperature is G, the hot blast temperature of side parts plenum chamber (8) is (1.0 ~ 1.5) G of middle part plenum chamber hot blast temperature, is up to 375 DEG C.
10. the facility of raising Polyamic Acid Film side imines rate according to claim 5, is characterized in that:
Boosting pipe (9) is installed additional in the top of the side parts of film (1) wide Z and/or below in imination equipment, described Z=20 ~ 200mm, described boosting pipe (9) is arranged as equally spaced 2 ~ 6 row, length direction is parallel with film (1) direct of travel, the front end that described boosting pipe (9) arranges is equal with the entrance end of imination equipment, before extending to the high-temperature zone of imination equipment, namely the length that boosting pipe (9) arranges is 1/2 to 3/4 of imidization zone length, boosting pipe (9) and film (1) surperficial vertical range are k, reduce gradually with close to film (1) outer rim k, above film (1) outer rim and/or the boosting pipe (9) of below and film (1) surface distance minimum be K, K=10 ~ 30mm, k=(1 ~ 5) K.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111113754A (en) * 2019-11-22 2020-05-08 桂林电器科学研究院有限公司 Method for improving edge strength of polyamide acid film

Citations (3)

* Cited by examiner, † Cited by third party
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111113754A (en) * 2019-11-22 2020-05-08 桂林电器科学研究院有限公司 Method for improving edge strength of polyamide acid film

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