CN104191630B - The vacuum high-temperature debubbling method of polyamic acid resin salivation liquid film and device - Google Patents
The vacuum high-temperature debubbling method of polyamic acid resin salivation liquid film and device Download PDFInfo
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- CN104191630B CN104191630B CN201410427509.4A CN201410427509A CN104191630B CN 104191630 B CN104191630 B CN 104191630B CN 201410427509 A CN201410427509 A CN 201410427509A CN 104191630 B CN104191630 B CN 104191630B
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Abstract
The present invention is the polyamic acid resin salivation vacuum high-temperature debubbling method of liquid film and device, and the polyamic acid resin liquid film that this method is salivation gained first carries out vacuum high-temperature process, then carries out drying and processing and be shaped to the Polyamic Acid Film with self-supporting. The temperature of vacuum high-temperature process is 40��166 DEG C, and negative pressure is-0.1��0MPa, and the time is 0.1��3min. This defoaming device has airtight vacuum high-temperature case between forming mould and salivation baking oven, heating unit is installed in case, casing has vacuum adapter, is connected with blower fan or vacuum pump through pipeline, and steel band entrance and steel band outlet before and after it are in same level with the steel band entrance salivating baking oven. The steel band being loaded with salivation gained liquid film is first through vacuum high-temperature case, then enters salivation baking oven. There is tag vacuum chamber at forming mould rear, and liquid film is smoothly attached to rapidly on steel band. In liquid film of the present invention, micro-bubble is eliminated completely, it is to increase the quality of Kapton, and device simple operations is convenient.
Description
Technical field
The present invention relates to the manufacturing technology of Kapton, it is specially vacuum high-temperature debubbling method and the device of a kind of polyamic acid resin salivation liquid film.
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 widely used in electrotechnical, electronic industry, particularly the primary base material of various high-grade electronic product especially in electron trade.
Along with downstream electronic product is light, thin, short, little and the development trend of high reliability design, the Kapton of the market requirement is tending towards slimming, the Kapton of thickness��12.5 ��m receives favor greatly, to reduce the weight and volume that base material adopts the derived product of Kapton. Arrange line encryption due to derived product and reach micron order, it is desired to dielectric polyimide film can not have micron order, even can not have nano grade air bubbles or impurity, to prevent the faults such as short circuit.
Making the Quality advance that first Kapton that thickness is less than 20 ��m needs polyamide-acid polyimide resin solution, the 2nd to be improved the quality of polyamide-acid polyimide resin salivation liquid film exactly. The even nano level micro-bubble of micron order do not eliminated completely in salivation gained polyamide-acid amine self-supporting film can cause the Kapton product surface of final molding to have flaw defect. These flaw defects not only affect the apparent mass of film, and its position is easily by high electrical breakdown, and failure of insulation cannot use on electric and electronic product.
In traditional polyamide-acid polyimide resin synthesizer, the bubble still that disappears is common tank container, and the polyamide-acid polyimide resin solution completing batching in reactor just simply is pressed in the bubble still that disappears and leaves standstill or vacuum state maintenance a few hours, treats that its nature or negative pressure disappear bubble. Because polyamide-acid polyimide resin soltion viscosity is bigger, traditional bubble still that disappears is difficult to eliminate micron order even nano level micro-bubble within a short period of time with the debubbling method left standstill, not only affect Kapton production efficiency, also it is difficult to solve the defects such as Kapton product surface flaw.
Patent application about resin debubbling method and device has also occurred in recent years, as publication date be on September 7th, 2011 publication number be the Chinese invention patent application " a kind of liquid resin defoaming method for composite vacuum perfusion molding and device " of CN102173061A, defoaming device disclosed in it is the key of its defoaming method, this defoaming device comprises vacuum pump and multi-layer helical laminar flow plate, resin is in multi-layer helical laminar flow plate current mistake, resin solution forms the minimum thin layer of thickness, and under vacuum differential pressure action, the bubble in thin layer is excluded rapidly. This defoaming device structure is more complicated, carries out the resin viscosity of deaeration with it and flow just needs strict limitation. Because having groove on spiral laminar flow plate, it is impossible to form real thin layer, the micro-bubble in liquid resin in a groove cannot thoroughly be eliminated. So this kind of device is little to the micro-bubble effect eliminated in resin.
Not yet there are effective debubbling method and the device of polyamic acid resin salivation liquid film at present.
Summary of the invention
It is an object of the invention to design the vacuum high-temperature debubbling method of a kind of polyamic acid resin salivation liquid film, the polyamic acid resin liquid film of salivation gained first carries out vacuum high-temperature process, then carries out drying and processing, is shaped to the Polyamic Acid Film with self-supporting. Vacuum high-temperature process makes the micro-bubble in the polyamic acid resin liquid film of thin layer effectively eliminate.
It is another object of the present invention to the vacuum high-temperature defoaming device designing a kind of polyamic acid resin salivation liquid film, after polyamic acid resin solution forming mould, for vacuum high-temperature case, the steel band being loaded with salivation gained polyamic acid resin liquid film is introduced into vacuum high-temperature case, then enters salivation baking oven.
The vacuum high-temperature debubbling method of the polyamic acid resin salivation liquid film of inventive design, the polyamic acid resin liquid film of salivation gained first carries out vacuum high-temperature process, polyamic acid resin decrease in viscosity under high temperature, under suction function, micro-bubble in thin electrolyte film moves rapidly to liquid film surface disappearance of breaking, liquid film surface recovers rapidly smooth, local, the surface tiny flaw caused because of bubbles burst can not be caused, effectively eliminate the micro-bubble in thin layer polyamic acid resin liquid film, and make film surface keep smooth. Carry out drying and processing again, it is shaped to the Polyamic Acid Film with self-supporting.
The temperature of described vacuum high-temperature process is 40��166 DEG C, and negative pressure is-0.1��0MPa, and the vacuum high-temperature treatment time is 0.1��3min; Preferred version is temperature is 60��135 DEG C, negative pressure-0.06��-0.03MPa, and the treatment time is 0.5��2min.
The vacuum high-temperature defoaming device of the polyamic acid resin salivation liquid film of inventive design comprises polyamic acid resin solution forming mould, steel band and salivation baking oven, the steel band of annular is advanced around front drum and rear drum circulation, described forming mould is extrusion die or scraper-type salivation mouth, the lip of forming mould is just to the steel band being positioned at front drum highest point, vacuum high-temperature case is also had between forming mould and salivation baking oven, vacuum high-temperature case is containment housing, heating unit is installed in case, casing has vacuum adapter, it is connected with blower fan or vacuum pump through pipeline, before vacuum high-temperature case, end face has steel band entrance, aft end face has steel band to export, the steel band entrance of vacuum high-temperature case and steel band outlet are in same level with the steel band entrance salivating baking oven. it is loaded with the steel band salivating gained polyamic acid resin liquid film through forming mould lip first through vacuum high-temperature case, then enters salivation baking oven.
Temperature in vacuum high-temperature case is 40��166 DEG C, negative pressure is-0.1��0MPa, the time that liquid film is in vacuum high-temperature case is 0.1��3min, preferred version is that in vacuum high-temperature case, temperature is 60��135 DEG C, negative pressure-0.06��-0.03MPa, the time that liquid film is in vacuum high-temperature case is 0.5��2min.
Before described vacuum high-temperature case, the spacing of end face and forming mould lip is 100��300mm.
Before described vacuum high-temperature box back face and salivation baking oven, the spacing of end face is 0��100mm.
Described forming mould rear is provided with tag vacuum chamber, tag vacuum chamber top is connected to valve tube, tag vacuum chamber roof, front and rear wall and left and right wall are tightly connected, bottom opening is blast inlet, tag vacuum chamber antetheca pastes by wall after forming mould, it is less than or equals the distance of forming mould lip and steel strip surface along the distance with steel strip surface, valve tube connecting fan or vacuum pump under tag chamber bottom. Tag vacuum chamber makes to form vacuum below polyamic acid resin liquid film, reduces the air between liquid film and steel band, prevents air to be involved in liquid film and produces bubble, makes liquid film smoothly be attached to rapidly on steel band simultaneously.
Compared with prior art, the vacuum high-temperature debubbling method of polyamic acid resin of the present invention salivation liquid film and the advantage of device are: 1, obtained high-quality polyamic acid self-supporting film, the greatly surface quality of raising Kapton product; 2, effectively eliminating the even nano level micro-bubble of micron order in liquid film through vacuum high-temperature process, salivation liquid film enters the bubble that disappears before salivating baking oven and namely completes, and defoaming effect is good, ensures the continuous operation of follow-up masking production line; 3, defoaming device structure is simple, and de-foaming process is easy to operate; 4, product Kapton thickness evenness improves; 5, preventing the side effect reactions such as polyamic acid resin molecule generation disproportionation, the moisture absorption, product Kapton aberration reduces, and color even is consistent.
Accompanying drawing explanation
Fig. 1 is the vacuum high-temperature defoaming device example structure schematic diagram of this polyamic acid resin salivation liquid film.
In figure, label is: 1, extrusion die, 2, tag vacuum chamber, 3, front drum, 4, steel band, 5, salivation baking oven, 6, high-temperature vacuum case, 7, rouse afterwards.
A, connect polyamic acid resin solution, V, it is connected to vacuum pump.
Embodiment
The vacuum high-temperature defoaming device embodiment of this polyamic acid resin salivation liquid film is as shown in Figure 1, the steel band 4 of annular circulates around front drum 3 and rear drum 7 and advances, the lip of extrusion die 1 is just to the steel band 4 being positioned at front drum 3 highest point, vacuum high-temperature case 6 is also had between extrusion die 1 and salivation baking oven 5, vacuum high-temperature case 6 is containment housing, far-infrared heating tube is installed in case, casing has vacuum adapter, it is connected with vacuum pump through pipeline, before vacuum high-temperature case 6, end face has steel band entrance, aft end face has steel band to export, the steel band entrance of vacuum high-temperature case 6 and steel band outlet are in same level with the steel band entrance salivating baking oven 5. it is loaded with the steel band 4 salivating gained polyamic acid resin liquid film through extrusion die 1 lip first through vacuum high-temperature case 6, then enters salivation baking oven 5.
Before this example vacuum high-temperature case 6, the spacing of end face and extrusion die 1 lip is 100mm. Before vacuum high-temperature case 6 aft end face and salivation baking oven 5, the spacing of end face is 0.
Temperature in this example vacuum high-temperature case 6 is 120 DEG C, negative pressure-0.05Mpa, and the time that liquid film is in vacuum high-temperature case is 1.5min.
Described extrusion die 1 rear is provided with tag vacuum chamber 2, tag vacuum chamber 2 top is connected to valve tube, tag vacuum chamber 2 roof, front and rear wall and left and right wall are tightly connected, bottom opening is blast inlet, tag vacuum chamber 2 antetheca pastes by wall after extrusion die 1, bottom tag vacuum chamber 2, lower edge is less than or equals extrusion die 1 lip and the distance on steel band 4 surface with the distance on steel band 4 surface, valve tube connecting fan or vacuum pump. Tag vacuum chamber 2 forms vacuum environment at extrusion die 1 lip rear, when before salivation, drum 3 rotates, steel band 4 pulls liquid film when moving ahead, the vacuum being between liquid film and steel band 4 gives liquid film and applies to drag the reactive force pulled backward, offset moving ahead of steel band 4 and produce the reactive force of towing, avoid being involved in thus eliminating liquid film open bubble of air between liquid film and steel band 4, also prevent liquid film both sides from shrinking simultaneously, make liquid film be attached at rapidly steel band 4.
Adopt the vacuum high-temperature defoaming device embodiment of above-mentioned polyamic acid resin salivation liquid film, the vacuum high-temperature debubbling method of this polyamic acid resin salivation liquid film can be implemented, polyamic acid resin liquid film on steel band processes in vacuum high-temperature case, the temperature of process is 120 DEG C, negative pressure is-0.05MPa, and the vacuum high-temperature treatment time is 1.5min; Under negative pressure, the bubble of polyamic acid resin liquid film inside moves rapidly to liquid film surface disappearance of breaking, it is in the polyamic acid resin decrease in viscosity of high temperature, after bubbles burst, liquid film surface recovers rapidly smooth, can not cause local, the surface tiny flaw caused because of bubbles burst. Steel band and liquid film contained on it enter salivation baking oven after leaving vacuum high-temperature case immediately, carry out drying and processing, are shaped to the Polyamic Acid Film with self-supporting.
Comparative example is that the salivation gained polyamic acid resin liquid film that is loaded with leaving extrusion die directly enters salivation baking oven.
The quality comparation of the Polyamic Acid Film that comparative example and the present embodiment gained have self-supporting is as shown in table 1:
Table 1 the present embodiment and comparative example debubbling method and defoaming effect compare table
From the results shown in Table 1, this debubbling method embodiment salivation film surface bubble of the defoaming device of the present embodiment is adopted to be only the 0.8% of conventional debubbling method. The thickness deviation of the finished product Kapton reduces greatly, and aberration also reduces greatly, and product appearance is improved greatly.
From the present embodiment, the present invention not only effectively eliminates Polyamic Acid Film surface micro-bubble, improve the surface quality of Kapton product, ensure that Kapton production line continuous operations, and obtain the less high-quality Kapton of thickness deviation, the quality of Kapton product is ensured.
Above-described embodiment, is only the specific case that the object to the present invention, technical scheme and useful effect further describe, and the present invention is not defined in this. All make within the scope of disclosure of the present invention any amendment, equivalent replacement, improvement etc., be all included within protection scope of the present invention.
Claims (6)
1. the vacuum high-temperature defoaming device of polyamic acid resin salivation liquid film, comprise polyamic acid resin solution forming mould (1), steel band (4) and salivation baking oven (5), the steel band (4) of annular is advanced around front drum (3) and rear drum (7) circulation, described forming mould (1) is extrusion die or scraper-type salivation mouth, the lip of forming mould (1) is just to the steel band (4) being positioned at front drum (3) highest point, it is characterised in that:
Vacuum high-temperature case (6) is also had between described forming mould (1) and salivation baking oven (5), vacuum high-temperature case (6) is containment housing, installing heating unit in case, casing has vacuum adapter, is connected with blower fan or vacuum pump through pipeline; Vacuum high-temperature case (6) front end face has steel band entrance, and aft end face has steel band to export, and the steel band entrance of vacuum high-temperature case (6) and steel band outlet are in same level with the steel band entrance salivating baking oven (5); The steel band (4) of polyamic acid resin liquid film being loaded with salivation gained through forming mould (1) lip is first through vacuum high-temperature case (6), then enters salivation baking oven (5).
2. the vacuum high-temperature defoaming device of polyamic acid resin according to claim 1 salivation liquid film, it is characterised in that:
Temperature in described vacuum high-temperature case (6) is 40��166 DEG C, and negative pressure is-0.1��0MPa, and the time that liquid film is in vacuum high-temperature case (6) is 0.1��3min.
3. the vacuum high-temperature defoaming device of polyamic acid resin according to claim 1 salivation liquid film, it is characterised in that:
In described vacuum high-temperature case (6), temperature is 60��135 DEG C, negative pressure-0.06��-0.03MPa, and the time that liquid film is in vacuum high-temperature case (6) is 0.5��2min.
4. the vacuum high-temperature defoaming device of polyamic acid resin according to claim 1 salivation liquid film, it is characterised in that:
The spacing of the front end face of described vacuum high-temperature case (6) and forming mould (1) lip is 100��300mm.
5. the vacuum high-temperature defoaming device of polyamic acid resin according to claim 1 salivation liquid film, it is characterised in that:
Described vacuum high-temperature case (6) aft end face is 0��100mm with the spacing of salivation baking oven (5) front end face.
6. the vacuum high-temperature defoaming device of polyamic acid resin according to claim 1 salivation liquid film, it is characterised in that:
Described forming mould (1) rear is provided with tag vacuum chamber (2), tag vacuum chamber (2) top is connected to valve tube, tag vacuum chamber (2) roof, front and rear wall and left and right wall are tightly connected, bottom opening is blast inlet, tag vacuum chamber (2) antetheca pastes by forming mould (1) wall afterwards, tag vacuum chamber (2) bottom is lower to be less than along the distance with steel band (4) surface or equals forming mould (1) lip and the distance on steel band (4) surface, valve tube connecting fan or vacuum pump.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1624026A (en) * | 2004-10-15 | 2005-06-08 | 浙江大学 | Method for preparing cross-linked polymer film by branching molecule |
| CN102514209B (en) * | 2012-01-10 | 2014-08-06 | 保定华翼风电叶片研究开发有限公司 | Defoaming method and defoaming device |
| CN203994741U (en) * | 2014-08-27 | 2014-12-10 | 桂林电器科学研究院有限公司 | The vacuum high-temperature defoaming device of polyamic acid resin salivation liquid film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6164734A (en) * | 1984-09-07 | 1986-04-03 | Hitachi Ltd | Impartment of antistatic property to plastic |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1624026A (en) * | 2004-10-15 | 2005-06-08 | 浙江大学 | Method for preparing cross-linked polymer film by branching molecule |
| CN102514209B (en) * | 2012-01-10 | 2014-08-06 | 保定华翼风电叶片研究开发有限公司 | Defoaming method and defoaming device |
| CN203994741U (en) * | 2014-08-27 | 2014-12-10 | 桂林电器科学研究院有限公司 | The vacuum high-temperature defoaming device of polyamic acid resin salivation liquid film |
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