CN104723581B - The preparation method and apparatus for the method for fluorine-containing layer composite polyimide material - Google Patents
The preparation method and apparatus for the method for fluorine-containing layer composite polyimide material Download PDFInfo
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- CN104723581B CN104723581B CN201510124268.0A CN201510124268A CN104723581B CN 104723581 B CN104723581 B CN 104723581B CN 201510124268 A CN201510124268 A CN 201510124268A CN 104723581 B CN104723581 B CN 104723581B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
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Abstract
The invention discloses a kind of preparation method and apparatus for the method for fluorine-containing layer composite polyimide material.Preparation comprises the following steps：By surface treated Kapton by unreeling the devices such as system, deviation correcting device, sided corona treatment, the extrusion casting system equipped with fluorine material is passed through with 0.5 100 meters of speed, by fluorine Material cladding to Kapton；The Kapton for being compounded with fluorine material enters main formation system further to control fluorine material thickness and fluorine material is sintered in into Kapton surface, and fluorine-containing layer Kapton is made.The present invention realizes MULTILAYER COMPOSITE, mono-/bis-face and is combined, and can prepare the composite of different fluorine thickness degree, and concise in technology, precision are high, efficiency high.
Description
Technical field
The invention belongs to polyimide material field, and in particular to a kind of preparation side of fluorine-containing layer composite polyimide material
Method and apparatus for the method.
Background technology
Fluorine-containing layer composite polyimide material, is contained by Kapton one side or two-sided compound one layer or multilayer
Fluorine material, is molded with by master.This composite combines the advantage of polyimides and fluorine material, with resistance to high/low
Warm, resistance to width penetrates, weather-proof, and can melt self-adhesion at 200-370 DEG C.Its excellent electric property, makes it be widely used in electric wire, electricity
The fields such as cable, petroleum industry, Aero-Space.
The universal fusing point of fluorine material is high, melting range is short；High-melting-point causes fluorine material molten difficult, and short melting range causes fluorine material to flow
Property it is poor, one crosses fusing point, and the viscosity of fluorine material declines rapidly；So the melt-processable of fluorine material is too poor, therefore prior art
In, fluorine-containing layer composite polyimide material is prepared, using dip-coating method, i.e., is coated in the suspension of various fluorine materials poly-
Imide membrane surface, by gravity levelling, then dries or sintering obtains product；But product thickness prepared by the method
Uniformity is poor, and can not avoid such as bubble, the open defect such as particle, gummosis trace, while this method is difficult the ultra-thin fluorine of production
Layer（Less than 0.005mm）And super thick fluorine layer（Higher than 0.15mm）Material.
With the development of science and technology, this fluorine-containing layer composite polyimide material consumption increasingly increases at present, and use environment
It is increasingly harsher, but during cladding process preparation fluorine-containing layer composite polyimide material, by gravity levelling, need to dry large quantity of moisture
It is dry, therefore speed is very slow（Generally 0.8-3m/min）, production efficiency is low；Simultaneously during the suspension regeneration production of fluorine material
The additives such as substantial amounts of emulsifying agent, defoamer are added, this brings very burden when using in machining composite material, later stage,
And a large amount of additives can destroy the immanent structure of fluorine layer material and fluorine layer material and polyimides, have impact on to a certain extent
The performance of fluorine-containing layer composite polyimide material.
At present, the fluorine-containing layer composite polyimide material that prepared by cladding process can not meet the industrial property to such product
It can require, be badly in need of a kind of new technique of research and development efficiently to prepare the fluorine-containing layer composite polyimide material that thickness span is big.
The content of the invention
It is an object of the invention to provide a kind of preparation method of fluorine-containing layer composite polyimide material and for this method
Equipment.Head of the invention on fluorine Material cladding to Kapton, will be realized in the way of fusion-cast MULTILAYER COMPOSITE,
Mono-/bis-face is combined, and can prepare the composite of different fluorine thickness degree, and concise in technology, precision are high, efficiency high, with wide
Prospects for commercial application.
To achieve the above object of the invention, the technical solution adopted by the present invention is：
A kind of preparation method of fluorine-containing layer composite polyimide material, comprises the following steps：
By the Kapton after processing with 0.5-100m/min speed by extrusion casting system, compound fluorine is prepared
The Kapton of material；The Kapton of compound fluorine material obtains fluorine-containing layer polyimides after forming processes and answered
Condensation material；
The extrusion casting system includes accumulator, screw extruder and extrusion die；
The extrusion die is provided with heater；
The step of Kapton of the compound fluorine material of preparation is that fluorine material enters screw extruder by accumulator
In, cast in after extruded die head extrusion on Kapton, obtain the Kapton of compound fluorine material；
The forming processes include cooling treatment；The temperature of the cooling treatment is -15~60 DEG C.
In above-mentioned technical proposal, the processing of the Kapton is surface treatment.It is surface-treated to improve polyamides
The dust greasy dirt on imines adhesion of thin film and removing surface etc., generally sided corona treatment；The condition of sided corona treatment is：Power 0-
6KW, frequency 20-25KHZ, single-side/double-side processing.
It is preferred that technical scheme in, Kapton after deviation correcting device again by extrusion casting system.
In above-mentioned technical proposal, the forming processes also include heat treatment and sintering processes；The temperature of the heat treatment
Spend for less than 50~80 DEG C of fluorine material melting point；The temperature of the sintering processes is higher than 60~120 DEG C of fluorine material melting point.
It is preferred that technical scheme in, the Kapton of compound fluorine material disappears by electrostatic again after forming processes
Remove, obtain fluorine-containing layer composite polyimide material.
It is preferred that technical scheme in, the Kapton after processing is poured with 10-100m/min speed by extrusion
Casting system.The speed of prior art is up to 3m/min, and the present invention reaches as high as 100m/min, and the properties of product prepared
It is good, achieve unexpected effect.
In above-mentioned technical proposal, the fluorine material be polytetrafluoroethylene (PTFE), perfluoroethylene-propylene, soluble poly tetrafluoroethene,
One or more than one kinds of mixing in polytrifluorochloroethylene, ethylene-tetrafluoroethylene copolymer, Kynoar, polyvinyl fluoride
Thing；The Kapton be thermosets, its fusing point not determined, short-period used temperature is more than 400 DEG C.
Prior art thinks that fluorine material melting point height, melting range are short, is not suitable for melt-processed technique, even if reluctantly for it, obtaining
Product appearance it is uncontrollable, defect is more, it is important to which stability is poor, poor adhesive force.The invention extrusion mould
Head setting heater, it is ensured that fluorine material keeps suitable viscosity when being extruded by extrusion die；Further, extrusion die bag
Include die head body and melt flow adjusting lever；The die head body interior is provided with heater and resin flow channel；The die head sheet
Body is provided with the extrusion lip connected with resin flow channel；The resin flow channel is by one section of rack-style runner and one section of narrow-gap annular tube group
Into wherein narrow-gap annular tube is close to extrusion lip.Fluorine material enters the resin of extrusion die after screw extruder melting extrusion
Runner, according to the method for the present invention, fluorine material is introduced into rack-style runner, enters back into narrow-gap annular tube, and creative solves fluorine
The problem of viscosity of material is unstable, thus, fluorine material can be cast to Kapton with suitable viscosity by extrusion lip
Surface.
One side fluorine-containing layer can be prepared according to the preparation method of fluorine-containing layer composite polyimide material disclosed by the invention
Composite polyimide material, then one side fluorine-containing layer composite polyimide material handled according to the method described above can also prepare it is double
Face fluorine-containing layer composite polyimide material, and two sides fluorine-containing layer thickness is adjustable.Further, it can also prepare multilayer fluorine-contained
Layer composite polyimide material.
In above-mentioned technical proposal, fusion-cast method avoids the defect of existing dip-coating method, can accurately control and contain
The thickness and quality of fluorine layer；The fluorine thickness degree of obtained fluorine-containing layer composite polyimide material is above and below 0.001-0.2mm, thickness
Limit is significantly better than the level of prior art, can obtain ultra-thin or super thick fluorine-containing layer composite polyimide material, achieve
Unexpected technique effect.
The invention also discloses a kind of equipment for preparing fluorine-containing layer composite polyimide material, including unwinding device,
Deviation correcting device, corona treatment plant, wrap-up, in addition to extrusion casting system, formation system；The extrusion casting system bag
Include accumulator, screw extruder and extrusion die；The extrusion die is provided with heater；The formation system fills for cooling
Put or the shaping system is made up of cooling device, shaping equipment and sintering equipment.
In above-mentioned technical proposal, unwinding device includes driving motor, variable-frequency governor, tension controller；Wrap-up bag
Include driving motor, variable-frequency governor, tension controller, meter counter.Unwinding device, wrap-up can control Kapton
Hauling speed.
In above-mentioned technical proposal, the extrusion die is made using special corrosion-resisting alloy steel, including die head sheet
Body and melt flow adjusting lever；The die head body interior is provided with heater and resin flow channel；The die head body be provided with
The extrusion lip of resin flow channel connection；The resin flow channel is made up of one section of rack-style runner with one section of narrow-gap annular tube, wherein narrow
Runner is stitched close to extrusion lip.Heater causes extrusion die to keep certain temperature, it is ensured that fluorine material is in resin flow channel
Steady flow；Lip is extruded with die head in resin flow channel connection screw extruder outlet；Melt flow adjusting lever can adjust fluorine material
Expect extrusion capacity, and then adjust fluorine-containing layer thickness in composite polyimide material, it is normally at the oblique upper of extrusion lip.
Fluorine material is entered in screw extruder by accumulator, and the extrusion die through screw extruder mouthful after melting is extruded；So
After cast on Kapton, obtain the Kapton of compound fluorine material.Fluorine material melt does not have solvent, emulsification
The various additives that the prior arts such as agent, defoamer are used, it is to avoid all class additives is to the outer of fluorine-containing layer polyimide material
Sight and the influence of internal performance, it is ensured that the high-quality of final products.
Cooling device mainly includes：The compositions such as two main chill rolls, jockey pulley, freezing unit, temperature controls regulation；Pass through refrigerant
Continuous loop control chilling temperature.The purpose of cooling device is in order that melt extrusion quickly forms cured layer, to be attached to polyamides
Imines surface, in order to avoid there is roll banding phenomenon during by deflector roll below；In order to which higher precision controls composite bed thickness and improves fluorine layer
Adhesive fastness between polyimide film, can increase the polyimides of shaping equipment and sintering equipment to compound fluorine material
Film carries out heat treatment and sintering processes.
The equipment for being used to prepare fluorine-containing layer composite polyimide material according to the present invention, the correction of Kapton process,
After sided corona treatment, by extruding the compound upper fluorine material of casting system, then it is molded through formation system, obtains that thickness is controllable, Gao Pin
The composite polyimide material of the fluorine-containing layer of matter, finally winds；For the ease of the absorption of following process and reduction dust, in winding
Before, the composite polyimide material of fluorine-containing layer is passed through into static eraser.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art:
1. present invention firstly discloses fluorine material is combined to Kapton in the way of fusion-cast, preparation contains
Fluorine layer composite polyimide material, it is to avoid the open defect such as steam bubble, micelle that prior art is present and material property are unstable
The problem of determining, it is ensured that the quality of product.
2. fusion-cast method disclosed by the invention prepares fluorine-containing layer composite polyimide material, without solvent, not only protect
The uniformity of outward appearance, thickness and the performance of product has been demonstrate,proved, more overcome the low defect of existing speed, Kapton is led
100m/min can be reached by drawing speed, exceeded well over existing highest 3m/min, achieved unexpected technique effect.
3. fusion-cast method disclosed by the invention prepares fluorine-containing layer composite polyimide material, equipment precision is high, final production
The thickness of the thickness of product, particularly fluorine-containing layer can be controlled accurately, be 0.001-0.2mm, and thickness bound is significantly better than existing
The level of technology, can obtain ultra-thin or super thick fluorine-containing layer composite polyimide material, and various thickness products lack
Fall into less, Functionality, quality and appealing design, achieve unexpected technique effect.
4. the method disclosed by the invention for preparing fluorine-containing layer composite polyimide material, due to fixed using quick cooling, heat
The techniques such as type, make thickness control more accurate, more efficient；And prior art only has sintering, thickness is controlled by Self-leveling, and
During levelling, it is necessary to leave enough drying times, therefore thickness is difficult accurate control, and speed is slow.
5. think that fluorine material melting point height, melting range are short instant invention overcomes existing, it is difficult to the technology prejudice of melt-processed, wound
Viscosity stability of the fluorine material in each stage is ensure that to the property made, fusion-cast is successfully realized and prepares fluorine-containing layer polyamides Asia
Amine；And fluorine viscosity of material is controllable to be conducive to the production of ultra-thin, super thick and different speed products.
6. the equipment composition disclosed by the invention for being used to prepare fluorine-containing layer composite polyimide material is reasonable, contamination-free row
Put, meet requirement and the direction of contemporary green chemistry；And can be with the thickness of high-precision control product fluorine-containing layer；Prepare
Technique is simple during product, production efficiency is high, and obtained product appearance defect is few, quality is high, suitable for industrial production.
Brief description of the drawings
Fig. 1 be embodiment one in be used for prepare fluorine-containing layer composite polyimide material equipment structural representation；
Fig. 2 is the structural representation of extrusion die in embodiment one；
Wherein, unwinding device 1, deviation correcting device 2, corona treatment plant 3, extrusion casting system 4, accumulator 41, screw rod are squeezed
Go out machine 42, extrusion die 43, die head body 431, melt flow adjusting lever 432, heater 433, extrusion lip 434, clothes hanger
Formula runner 435, narrow-gap annular tube 436, formation system 5, cooling device 51, shaping equipment 52, sintering equipment 53, static eraser
6th, wrap-up 7, Kapton 8, fluorine-containing layer composite polyimide material 9；
Fig. 3 is product and traditional handicraft product adhesive force comparison diagram in embodiment two；
Fig. 4 is product and traditional handicraft product thickness comparison diagram in embodiment three；
Fig. 5 is product appearance figure in embodiment.
Embodiment
Below in conjunction with the accompanying drawings and embodiment the invention will be further described：
The present embodiment uses WDW-500B tensile testing machine test product adhesive force；Tested using TCS-300kg electronic scales
Product weight；Using YKT3-5KVA industrial frequency withstand voltage testing machine test product electric properties；It is thick using Labthink blue streaks CHY-CA
Spend tester test product thickness.
Embodiment one is used for the equipment for preparing fluorine-containing layer composite polyimide material
As shown in figure 1, the equipment of the present invention is by unwinding device 1, deviation correcting device 2, corona treatment plant 3, extrusion casting system
System 4, formation system 5, static eraser 6, wrap-up 7 are constituted.Unwinding device includes driving motor, variable-frequency governor, opened
Force controller；Wrap-up includes driving motor, variable-frequency governor, tension controller, meter counter.Unwinding device, wrap-up
The hauling speed of Kapton can be controlled.Extruding casting system includes accumulator 41, screw extruder 42, extrusion die
43；Formation system includes cooling device 51, shaping equipment 52, sintering equipment 53.In some live-rollers of each position relative set.
Accompanying drawing 2 is the structural representation of above-mentioned extrusion die 43, including die head body 431 and melt flow adjusting lever 432；
The die head body interior is provided with two heaters 433 and resin flow channel；Described die head body one end is provided with and resin flow channel
The extrusion lip 434 of connection；The resin flow channel is made up of one section of rack-style runner 435 with one section of narrow-gap annular tube 436, wherein narrow
Runner is stitched close to extrusion lip.Fluorine material is entered in screw extruder by accumulator, the extrusion through screw extruder mouthful after melting
Die head is extruded；Then cast on Kapton, obtain the Kapton of compound fluorine material.Heater to squeeze
Go out the temperature that die head keeps certain, it is ensured that the steady flow in resin flow channel of fluorine material；Resin flow channel connection screw extruder goes out
Mouth extrudes lip with die head；Melt flow adjusting lever can adjust fluorine material throughput, and then adjust composite polyimide material
Middle fluorine-containing layer thickness.By adjusting melt flow adjusting lever, control die head extrudes the openings of sizes of lip, and then controls extrusion lip
The extrusion capacity in each region of mouth, the final function of realizing adjustment fluorine thickness degree.
Rack-style runner 435 is respectively that existing head uses resin flow channel form, the pipe of narrow-gap annular tube with narrow-gap annular tube 436
Footpath is less than rack-style runner.Both are combined together by the present invention first, and apply in resin with high melting point circulation, are conducive to solution
Certainly melt processable difference fluorine material flowing, viscosity control problem so that its controllable casting takes to Kapton surface
Obtained unexpected effect.
Cooling device mainly includes：Two main chill rolls, jockey pulley, freezing unit, temperature control regulators, it is continuous by refrigerant
The chilling temperature of the main chill roll of loop control；Shaping equipment mainly includes：Two setting rolls, Heat-conduction oil circulation systems, warm up and down
Control system, by two setting roll gaps and setting temperature above and below regulation, heat is carried out to the Kapton for being compounded with fluorine layer
Roll, so that sizing is played, the effect of precise thickness control；Sintering equipment mainly includes：Thermal-insulating body, thin film channel, stainless steel
Heating tube, air exhausting device, pass through sintering, it is possible to reduce the low-molecular material in material, and further fluorine layer and Kapton
Adhesion strength.
Kapton 8 is combined upper fluorine material after unreeling by correction, sided corona treatment, then by extrusion casting system,
Then through cooling, sizing, sintering, obtain that thickness is controllable, high-quality fluorine-containing layer composite polyimide material 9, then by electrostatic
Eliminate, finally wind.
Embodiment two prepares fluorine-containing layer composite polyimide material
Using the equipment of embodiment one
First by the wide 550mm of 60Kg, thick 0.025mm Kapton completes to draw according to specific route；In storage
The perfluoroethylene-propylene particle that 50Kg is dried is added in glassware, it is stand-by；It is 520 mm to adjust extrusion die width；Cooling system temperature
Spend for 50 DEG C, shaping system temperature is 205 DEG C, sintering system temperature is 350 DEG C.
Then Kapton is unreeled by unwinding device, deviation correcting device, sided corona treatment with 40m/min speed,
Progressively the extrusion capacity of adjusting bolt extruder is to 0.65Kg/min, and Kapton is by extruding during casting system, poly- perfluor
Second propylene melt is extruded by extrusion die, is combined to Kapton；
The Kapton for being finally compounded with perfluoroethylene-propylene passes sequentially through cooling, sizing, sintering, obtains fluorine-containing layer
Composite polyimide material；Again through static elimination, winding.
80Kg one side can be made by the winding of 1 hour（0.0125±0.0005）The fluorine-containing layer of mm perfluoroethylene-propylenes
Composite polyimide material.
One side is prepared using existing infusion process（0.0125±0.0005）The fluorine-containing layer polyimides of mm perfluoroethylene-propylenes
Composite, from wide 550mm, thick 0.025mm Kapton.
Product and the product adhesive force comparison diagram of existing infusion process that accompanying drawing 3 is prepared for the present invention, table 1 is adhesive force number
According to, it can be seen that fluorine-containing layer and base material polyimides in the fluorine-containing layer composite polyimide material prepared using the inventive method
Adhesive force between film is much larger than fluorine-containing layer composite polyimide material prepared by existing infusion process；And from maximum, force and most
It is uniform and stable that the data difference of small power can be seen that the product each several part performance of the invention prepared.
Table 2 is the electrical strength data that above-mentioned different process prepares product, it can be seen that prepared using the inventive method
The electrical strength of fluorine-containing layer composite polyimide material is much larger than fluorine-containing layer composite polyimide material prepared by existing infusion process；
And it is uniform and stable from the data difference of maxima and minima to can be seen that the product each several part performance for preparing of the present invention.This master
If fluorine layer prepared by the inventive method is uniform continuous phase, it provides certain electrical strength；And existing infusion process institute
The fluorine layer of formation is discontinuous phase, therefore the electrical strength provided is weaker or can not provide electrical strength.
The different process of table 1 prepares the attachment force data of product
The different process of table 2 prepares the electrical strength data of product
Embodiment three prepares fluorine-containing layer composite polyimide material
Using the equipment of embodiment one
First by the wide 550mm of 60Kg, thick 0.025mm Kapton completes to draw according to specific route；In storage
The polytetrafluoroethylparticle particle that 40Kg is dried is added in glassware, it is stand-by；It is 520 mm to adjust extrusion die width；Cooling system temperature
For 50 DEG C, shaping system temperature is 260 DEG C, and sintering system temperature is 380 DEG C.
Then Kapton is unreeled by unwinding device, deviation correcting device, sided corona treatment with 50m/min speed,
Progressively the extrusion capacity of adjusting bolt extruder is to 0.29Kg/min, and Kapton is by extruding during casting system, polytetrafluoro
Ethene melt is extruded by extrusion die, is combined to Kapton.
The Kapton for being finally compounded with polytetrafluoroethylene (PTFE) passes sequentially through cooling, sizing, sintering, obtains fluorine-containing strata
Acid imide composite；Again through static elimination, winding.
75Kg one side can be made by the winding of 1 hour（0.005±0.0005）The fluorine-containing strata of mm polytetrafluoroethylene (PTFE)
Acid imide composite.
One side is prepared using existing infusion process（0.005±0.0005）The fluorine-containing layer polyimides of mm polytetrafluoroethylene (PTFE) is combined
Material, from wide 550mm, thick 0.025mm Kapton.
Using 500mm*1000mm samples as test object, the thickness of product of the present invention and existing product diverse location is tested,
Product and the product thickness comparison diagram of existing infusion process that accompanying drawing 4 is prepared for the present invention, it can be seen that：Production prepared by existing process
Product thickness fluctuation is larger, and some local thickness are even close to Kapton, and this illustrates that this goes out during being in impregnation
Leak adhesive phenomenon is showed, and product prepared by the present invention, thickness is more uniform, is more not in leak adhesive phenomenon.Thickness fluctuation is larger
When, the serious accumulation of following process tolerance is will result directly in, causes product quality to decline, or even can not be used；Especially leak adhesive
It will also cause air layer to exist, and serious electric weakness occur, and aggravate product disqualification rate.
The different process of table 3 prepares the electrical strength data of product
Table 3 is the electrical strength data that above-mentioned different process prepares product, it can be seen that prepared using the inventive method
The electrical strength of fluorine-containing layer composite polyimide material is much larger than fluorine-containing layer composite polyimide material prepared by existing infusion process；
And it is uniform and stable from the data difference of maxima and minima to can be seen that the product each several part performance for preparing of the present invention.This master
If fluorine layer prepared by the inventive method is uniform continuous phase, it provides certain electrical strength；And existing infusion process institute
The fluorine layer of formation is discontinuous phase, therefore the electrical strength provided is weaker or can not provide electrical strength.
Example IV prepares fluorine-containing layer composite polyimide material
Using the equipment of embodiment one
First by the wide 550mm of 60Kg, thick 0.025mm Kapton completes to draw according to specific route；In storage
The polytetrafluoroethylparticle particle that 40Kg is dried is added in glassware, it is stand-by；It is 520 mm to adjust extrusion die width；Cooling system temperature
For 50 DEG C, shaping system temperature is 260 DEG C, and sintering system temperature is 380 DEG C.
Then Kapton is unreeled by unwinding device, deviation correcting device, sided corona treatment with 60m/min speed,
Progressively the extrusion capacity of adjusting bolt extruder is to 0.35Kg/min, and Kapton is by extruding during casting system, polytetrafluoro
Ethene melt is extruded by extrusion die, is combined to Kapton.
The Kapton for being finally compounded with polytetrafluoroethylene (PTFE) passes sequentially through cooling, sizing, sintering, obtains second containing tetrafluoro
Alkene layer composite polyimide material；Again through static elimination, winding.
Then, cleaning equipment；By above-mentioned containing tetrafluoroethene layer composite polyimide material upset so that be not combined fluorine-containing layer
One side face extrusion die.
The above-mentioned layer composite polyimide material containing tetrafluoroethene is completed to draw according to specific route；Add in accumulator
Enter the perfluoroethylene-propylene particle of 30Kg dryings, it is stand-by；It is 520 mm to adjust extrusion die width；Cooling system temperature is 60
DEG C, shaping system temperature is 205 DEG C, and sintering system temperature is 350 DEG C.
Then Kapton is unreeled by unwinding device, deviation correcting device, sided corona treatment with 70m/min speed,
Progressively the extrusion capacity of adjusting bolt extruder is to 0.18Kg/min, and Kapton is by extruding during casting system, poly- perfluor
Second propylene melt is extruded by extrusion die, is combined to Kapton.
The Kapton for being finally compounded with perfluoroethylene-propylene passes sequentially through cooling, sizing, sintering, obtains fluorine-containing layer
Composite polyimide material；Again through static elimination, winding.
The two-sided of 50Kg can be made by the winding of 1 hour to be combined respectively（0.005±0.0005）Mm polytetrafluoroethylene (PTFE) and
（0.002±0.0005）The fluorine-containing layer composite polyimide material of mm perfluoroethylene-propylenes, product electrical strength average out to 204
KV/mm.Prior art, due to the limitation of technique itself, it is impossible to produce the composite membrane of this fluorine layer.
Embodiment five prepares fluorine-containing layer composite polyimide material
Using the equipment of embodiment one
First by the wide 550mm of 60Kg, thick 0.0125mm Kapton completes to draw according to specific route；In storage
The perfluoroethylene-propylene particle that 20Kg is dried is added in glassware, it is stand-by；It is 520 mm to adjust extrusion die width；Cooling system temperature
Spend for 50 DEG C, shaping system temperature is 205 DEG C, sintering system temperature is 350 DEG C.
Then Kapton is put by unwinding device, deviation correcting device, sided corona treatment with 100m/min speed
Volume, progressively the extrusion capacity of adjusting bolt extruder is poly- full when Kapton is by extrusion casting system to 0.16Kg/min
Fluoro ethyl propene melt is extruded by extrusion die, is combined to Kapton.
The Kapton for being finally compounded with perfluoroethylene-propylene passes sequentially through cooling, sizing, sintering, obtains fluorine-containing layer
Composite polyimide material；Again through static elimination, winding.
70Kg one side can be made by the winding of 1 hour（0.001±0.0005）The fluorine-containing layer of mm perfluoroethylene-propylenes
Composite polyimide material, table 4 is product electrical strength.
The electrical strength data of the product of table 4
Traditional infusion process, due to the limitation of technique itself, it is impossible to produce the composite membrane of this slim fluorine layer, the present invention
It can produce, table 5 is the thickness distribution value of product of the present invention（500mm*1000mm samples）, as shown in Table 5 the present invention prepare
Product thickness is stable, and the thickness deviation of Kapton used in the present invention is ± 5%.
The thickness data of the product of table 5
Embodiment six prepares fluorine-containing layer composite polyimide material
Using the equipment of embodiment one
First by the wide 550mm of 100Kg, thick 0.175mm Kapton completes to draw according to specific route；In storage
The ethylene-tetrafluoroethylene particle that 160Kg is dried is added in glassware, it is stand-by；It is 520 mm to adjust extrusion die width；Cooling system
Temperature is 40 DEG C, and shaping system setting roll gap rises to maximum and do not heated, and sintering system is closed, and retains film access way.
Then Kapton is unreeled with 10m/min speed, progressively adjusted by unwinding device, deviation correcting device, sided corona treatment
The extrusion capacity of screw extruder is to 2.2 Kg/min, and when Kapton is by extrusion casting system, ethylene-tetrafluoroethylene melts
Body is extruded by extrusion die, is combined to Kapton.
The Kapton of ethylene-tetrafluoroethylene is finally compounded with by cooling, fluorine-containing layer polyimides is obtained and is combined
Material；Again through static elimination, winding.
200Kg one side can be made by the winding of 1 hour（0.200±0.002）The fluorine-containing layer of mm ethylene-tetrafluoroethylenes
Composite polyimide material, table 6 is the electrical strength of product.
The electrical strength data of the product of table 6
Traditional infusion process, due to the limitation of technique itself, it is impossible to produce the composite membrane of this thicker fluorine layer, the present invention
It can produce, table 7 is the thickness distribution value of product of the present invention（500*1000mm meters of samples）, as shown in Table 7 the present invention prepare
Product thickness is stable, and the thickness deviation of Kapton used in the present invention is ± 5%.
The thickness data of the product of table 7
Embodiment seven prepares fluorine-containing layer composite polyimide material
Using the equipment of embodiment one
First by the wide 550mm of 8Kg, thick 0.05mm Kapton completes to draw according to specific route；In storing
The perfluoroethylene-propylene particle that 40Kg is dried is added in device, it is stand-by；It is 520 mm to adjust extrusion die width；Cooling system temperature
For 50 DEG C, shaping system temperature is 205 DEG C, and sintering system temperature is 350 DEG C.
Then Kapton is unreeled by unwinding device, deviation correcting device, sided corona treatment with 30m/min speed,
Progressively the extrusion capacity of adjusting bolt extruder is to 0.29Kg/min, and Kapton is by extruding during casting system, poly- perfluor
Second propylene melt is extruded by extrusion die, is combined to Kapton；The polyamides for being finally compounded with perfluoroethylene-propylene is sub-
Amine film passes sequentially through cooling system, shaping system, sintering system, obtains composite polyimide material containing perfluoroethylene-propylene；
Again through static elimination, winding.
Then, cleaning equipment；Above-mentioned composite polyimide material containing perfluoroethylene-propylene is completed according to specific route
Traction so that the one side of compound fluorine-containing layer faces extrusion die；The polytetrafluoroethylparticle particle that 30Kg is dried is added in accumulator,
It is stand-by；It is 520 mm to adjust extrusion die width；Cooling system temperature is 60 DEG C, and shaping system temperature is 260 DEG C, sintering system
Temperature is 380 DEG C.
Then Kapton is unreeled by unwinding device, deviation correcting device, sided corona treatment with 70m/min speed,
Progressively the extrusion capacity of adjusting bolt extruder is to 0.21Kg/min, and Kapton is by extruding during casting system, polytetrafluoro
Ethene melt is extruded by extrusion die, is combined to Kapton；The polyimides for being finally compounded with polytetrafluoroethylene (PTFE) is thin
Film passes sequentially through cooling system, shaping system, sintering system, obtains fluorine-containing layer composite polyimide material；Again through static elimination,
Winding.
The one side that 85Kg can be made by the winding of 1 hour is combined respectively（0.007±0.0005）Mm perfluoroethylene-propylenes
With（0.005±0.0005）The fluorine-containing layer composite polyimide material of mm polytetrafluoroethylene (PTFE), product electrical strength average out to 226
KV/mm.Prior art, due to the limitation of technique itself, it is impossible to produce the composite membrane of this fluorine layer.
Product and the product appearance comparison diagram of existing infusion process that accompanying drawing 5 is prepared for the present invention, it can be seen that：Traditional handicraft
The product of preparation can produce the defects such as more stain, and product prepared by the present invention, substantially without this kind of defect, at the same film surface compared with
Homogeneous and bright.
Table 8 adheres to force data for the product of embodiment three to seven, it can be seen that fluorine-containing layer polyimides prepared by the present invention
Adhesive force in composite between fluorine-containing layer and base material Kapton is high；And from maximum, force and the data difference of minimum force
As can be seen that product each several part performance prepared by the present invention is uniform and stable.
The different process of table 8 prepares the attachment force data of product
Claims (6)
1. a kind of preparation method of fluorine-containing layer composite polyimide material, it is characterised in that comprise the following steps：
By the Kapton after surface treatment with 10-100m/min speed by extrusion casting system, compound fluorine is prepared
The Kapton of material；The Kapton of compound fluorine material obtains fluorine-containing layer polyimides after forming processes and answered
Condensation material；
The extrusion casting system includes accumulator, screw extruder and extrusion die；
The extrusion die is provided with heater；
The extrusion die includes die head body and melt flow adjusting lever；The die head body interior is provided with heater and tree
Fat runner；The die head body is provided with the extrusion lip connected with resin flow channel；The resin flow channel is by one section of rack-style runner
Constituted with one section of narrow-gap annular tube, wherein the close extrusion lip of narrow-gap annular tube,
The step of Kapton of the compound fluorine material of preparation is that fluorine material is entered in screw extruder by accumulator,
Cast in after extruded die head extrusion on Kapton, obtain the Kapton of compound fluorine material；
The forming processes include cooling treatment；The temperature of the cooling treatment is -15~60 DEG C；The forming processes also include
Heat treatment and sintering processes；The temperature of the heat treatment is less than 50~80 DEG C of fluorine material melting point；The sintering processes
Temperature is higher than 60~120 DEG C of fluorine material melting point.
2. the preparation method of fluorine-containing layer composite polyimide material according to claim 1, it is characterised in that：The polyamides is sub-
The surface treatment of amine film is sided corona treatment.
3. the preparation method of fluorine-containing layer composite polyimide material according to claim 1, it is characterised in that：Polyimides is thin
Film is after deviation correcting device again by extrusion casting system.
4. the preparation method of fluorine-containing layer composite polyimide material according to claim 1, it is characterised in that：The polyamides is sub-
Amine film is Thermocurable polyimide film；The fluorine material is polytetrafluoroethylene (PTFE), perfluoroethylene-propylene, soluble polytetrafluoroethyl-ne
It is one or more than one kinds of mixed in alkene, polytrifluorochloroethylene, ethylene-tetrafluoroethylene copolymer, Kynoar, polyvinyl fluoride
Compound.
5. the preparation method of fluorine-containing layer composite polyimide material according to claim 1, it is characterised in that：The fluorine-containing layer
The fluorine thickness degree of composite polyimide material is 0.001-0.2mm.
6. the equipment for preparing fluorine-containing layer composite polyimide material, including unwinding device, deviation correcting device, sided corona treatment dress
Put, wrap-up, it is characterised in that：Also include extrusion casting system, formation system；The extrusion casting system includes storing
Device, screw extruder and extrusion die；The extrusion die is provided with heater；The formation system be cooling device or
The formation system is made up of cooling device, shaping equipment and sintering equipment；The extrusion die includes die head body with melting
Body flow adjusting lever；The die head body interior is provided with heater and resin flow channel；The die head body is provided with and resin stream
The extrusion lip of road connection；The resin flow channel is made up of one section of rack-style runner with one section of narrow-gap annular tube, wherein narrow-gap annular tube
Close to extrusion lip.
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| CN105965815A (en) * | 2016-07-12 | 2016-09-28 | 东营林福商贸有限公司 | Compound technology of polyimide film and fluorine film |
| CN112356415A (en) * | 2020-09-03 | 2021-02-12 | 苏州浅米科技有限公司 | Preparation method of ultrathin PFA (Polytetrafluoroethylene) film for 5G flexible circuit board |
| CN112895641A (en) * | 2021-01-25 | 2021-06-04 | 东营林福商贸有限公司 | Polyimide film-fluorine film and laminating method, laminating device and application thereof |
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