CN104107565A - Defoaming kettle and defoaming method for preparing polyamide acid resin - Google Patents
Defoaming kettle and defoaming method for preparing polyamide acid resin Download PDFInfo
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- CN104107565A CN104107565A CN201410356940.4A CN201410356940A CN104107565A CN 104107565 A CN104107565 A CN 104107565A CN 201410356940 A CN201410356940 A CN 201410356940A CN 104107565 A CN104107565 A CN 104107565A
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Abstract
The invention discloses a defoaming kettle and a defoaming method for preparing polyamide acid resin. A thin layer distributor with an arch rotary curve surface is fixedly installed in a defoaming kettle tank body; the distance from the curve surface arch top of the thin layer distributor to the lower end opening of a feeding pipe ranges from 0.01mm to 1/3 of the height of the tank body; the clearance between the lower edge of the curve surface of the thin layer distributor and the inner wall of the tank body is 0.01mm-10mm; the rotary curve surface of the thin layer distributor is a spherical surface; a resin conveying pipeline between a reaction kettle and the defoaming kettle is provided with a metering pump; the tank body is provided with a sandwiched sleeve, and an heat conduction medium inlet and outlet are formed at the top and bottom of the tank body. The defoaming method comprises the step that resin entering the defoaming kettle falls on the arch top of the curve surface of the thin layer distributor, and disperses and flows downward along the curve surface of the thin layer distributor to form a thin layer which results in bubble breakage. The metering pump is used for adjusting the flow rate of resin so as to keep that the thickness of the resin solution layer on the thin layer distributor is less than 5mm. Defoaming is completed immediately when resin is conveyed completely, and then pressurization is carried out for discharging. During defoaming, a heat conduction medium is introduced for warming, and negative pressure is kept in the tank body. According to the invention, defoaming is complete, and the defoaming time is shortened greatly so as to guarantee subsequent continuous film preparation. The defoaming kettle is simple in structure and convenient to operate.
Description
Technical field
The present invention relates to the synthetic technology of polyamic acid resin, be specially and manufacture polyamic acid resin froth breaking still and debubbling method used.
Background technology
Kapton is the macromolecular material with excellent properties such as high strength, high tenacity, abrasion performance, high temperature resistant, anticorrosions, is the main insulating materials of making various medium-to-high grade electrotechnical, electronic components and parts, is widely used in electrotechnical, electronic industry.
At present the production technology of Kapton is to take polyamic acid resin solution as raw material, and on slobbering machine, salivation obtains having the polyamic acid thick film of self-supporting, then processes and obtain Kapton through adding hot-stretch, imidization, cooling and shaping.
Along with downstream application product is light, thin, short, little and High Reliability Design requirement, the film thickness specification of the market demand is tending towards slimming.Make the little film of thickness and just need to improve the quality of polyamide-acid polyimide resin, minute impurities in polyamide-acid polyimide resin and bubble all can cause the flaw defect on salivation form film surface, not only affect the apparent of film, and flaw defective locations place is easily by high electrical breakdown, failure of insulation cannot be used on the electric and electronic product of downstream.
The synthetic conventional method of existing polyamic acid resin is in the reactor in condition of normal pressure, to using dimethylacetylamide to manufacture by the polymerisation of dianhydride and diamines as solvent, in the process of reacting while stirring in reactor, polyamide-acid polyimide resin solution is constantly involved in air and causes resin system to contain a large amount of bubbles.In current polyamide-acid polyimide resin synthesizer, froth breaking still is common tank container, froth breaking does not have special technique yet, the polyamide-acid polyimide resin solution that completes batching in reactor is just pressed into simply standing in froth breaking still or vacuum state and keeps a few hours, treats the standing froth breaking of its nature or negative pressure.Because synthetic polyamide-acid polyimide resin solution viscosity is larger, for current Kapton manufacture, existing defoaming device and standing method are difficult to the small bubble of elimination in the short period, thereby cause serialization to be produced, be difficult to normally carry out, and easily cause film product surface to occur the defects such as bubble flaw.
In recent years also there is the patent application of relevant resin debubbling method and device, as the patent No. Chinese invention patent " a kind of liquid resin defoaming method and device for composite vacuum perfusion molding " that is 201010595145, wherein disclosed defoaming device is the key of its defoaming method, this defoaming device comprises vavuum pump and multi-layer helical laminar flow plate, resin is in multi-layer helical laminar flow plate current mistake, liquid level is the minimum thin layer of thickness, and the bubble under vacuum differential pressure action in thin layer is excluded rapidly.This defoaming device structure is more complicated, spiral laminar flow plate has at least two-layer, and spiral laminar flow plate must be combined closely with the inwall of defoaming device, on each spiral laminar flow plate, has spirality liquid resin flow groove, and its number of turns is all different and different according to liquid resinous flow with the degree of depth.Multi-layer helical laminar flow plate also will arrange flow orifice, so that realize from top to bottom and flowing in the in good time short time of liquid resin, the size in flow orifice aperture is determined by liquid resin viscosity again.This kind of defoaming device, the aperture of flow orifice all cannot be adjusted, just needs strict restriction with resin viscosity and flow that it carries out deaeration because of the number of turns degree of depth of its groove.Because fluted on spiral laminar flow plate, can not form real thin layer, the micro-bubble in the liquid resin in groove cannot thoroughly be eliminated.Moreover, in order to overcome surface tension, guarantee that liquid resin can be from short notice of flow orifice, the aperture of flow orifice is at least Centimeter Level, and the micron order in the drop falling from flow orifice or nano level bubble are also difficult to eliminate.So this device is little to the micro-bubble effect of eliminating in resin.
In addition also has the Chinese utility model patent " resin vacuum defoamation mixer " that the patent No. is 201220275415.6, the patent No. is 201110167565.5 Chinese invention patent application " Quick defoaming device " etc., but existing design can only be shortened foam time, be all difficult to remove micron order or nano level micro-bubble.
Summary of the invention
The object of the invention is to design a kind of polyamic acid resin froth breaking still used of manufacturing, feed pipe below is provided with hemispherical thin layer distributor in its tank body, enters the polyamic acid resin solution straticulation dispersion flows of froth breaking still, the disappearance of breaking of the bubble of solution inside.
Another object of the present invention is a kind of debubbling method of manufacturing polyamic acid resin of design, by polyamic acid resin solution straticulation dispersion flows, reach elimination micro-bubble, shorten foam time, the film quality that gained polyamic acid resin solution makes is improved.
The manufacture polyamic acid resin froth breaking still used of the present invention's design, comprises the froth breaking still that holds polyamic acid resin solution, and there is feed pipe the tank body top of this froth breaking still, and there is discharge nozzle below, and this froth breaking still is sealed shell of tank, has gas interface on tank body.Tank body is provided with pressure-detecting device.
Thin layer distributor is installed in tank body.Thin layer distributor is arch surface of revolution, and the rotating shaft of curved surface overlaps with the central shaft of tank body.The vault of curved surface with stretch into the tank interior height that the distance of the feed pipe lower port in tank is 0.01mm to 1/3, the center line of curved surface overlaps with tank body center line, under curved surface, edge is greater than 1/3 of tank interior height with tank body bottom surface distance, under curved surface, edge is 0.01mm～10mm with the gap of inner tank wall, and the maximum height of curved surface is 1/4 to 1/3 tank interior height.The lower edge of thin layer distributor has a place or many places to be fixedly connected with froth breaking still inner tank wall.
The surface of revolution of described thin layer distributor is sphere, and the height of sphere is spherical diameter 1/3 to 1/2.
The resin solution flowing into from feed pipe lower end, drop on the vault of thin layer distributor curved surface, along the downward dispersion flows of the curved surface of thin layer distributor, form thin layer, then flow in inner tank wall and still keep thin layer through the lower edge of thin layer distributor and the gap of inner tank wall, finally at tank body inner bottom part, assemble.During laminar flows that solution forms, under negative pressure state, its inner micro-bubble migrates to the solution surface disappearance of automatically breaking.
Between reactor and froth breaking still, carry on the pipeline of resin solution measuring pump is installed, by measuring pump rotational speed regulation, enter the flow of the resin solution of froth breaking still, be controlled at the maximum ga(u)ge of the resin solution layer forming on thin layer distributor, be beneficial to froth breaking.
This froth breaking still tank body is provided with chuck, and chuck below has heat-conducting medium entrance, top to have heat-conducting medium outlet, and pipeline connects heat-conducting medium entrance, heat-conducting medium outlet and heat conducting medium heating apparatus, to control the temperature of froth breaking still tank interior.Tank body is provided with temperature-detecting device.
The top of this froth breaking still tank body is also provided with evacuated tube, and described evacuated tube is furnished with electromagnetism and opens and closes valve.
Adopt manufacture polyamic acid resin process of the present invention froth breaking still used, the manufacture polyamic acid resin process of the present invention design debubbling method used is as follows: the synthetic polyamic acid resin solution of reactor is delivered to froth breaking still, feed pipe through tank body top enters the vault that polyamic acid resin in froth breaking still drops on thin layer distributor curved surface, the downward dispersion flows of curved surface along thin layer distributor forms thin layer, through the lower edge of thin layer distributor and the gap of inner tank wall, keep thin layer to continue to dirty along inner tank wall again, finally at tank body inner bottom part, assemble.
Regulate between reactor and froth breaking still and carry the measuring pump rotating speed on resin solution pipeline, the flow that makes to enter resin solution in froth breaking still is 0.5～100kg/min, preferred version is 2.5～12kg/min, the maximum ga(u)ge that is controlled at the resin solution layer forming on thin layer distributor is less than 5mm, can guarantee micro-bubble fast transferring to the surface of resin solution layer and the elimination of breaking rapidly under negative pressure state, resin solution layer is more thin is more conducive to eliminate micro-bubble.
Stop carrying polyamic acid resin solution to froth breaking still, in still after polyamic acid resin liquid level stabilizing standing 10～40 minutes, de-foaming process completed.When the variation in five minutes of the liquid level of resin solution is no more than 1mm, be considered as resin liquid level stable.
During the discharging of froth breaking still, through gas interface, in froth breaking still, pass into carbon dioxide or nitrogen or other inert gas, the gas flow passing in froth breaking still is 0.1～0.8m
3/ min.Regulate the electromagnetic proportional valve in evacuated tube, keeping still internal pressure is 0.3～0.5MPa, and polyamic acid resin force feed to the slobbering machine in froth breaking still is salivated to film forming.
When polyamic acid resin solution enters froth breaking still, regulate heat conducting medium heating apparatus, continue to pass into heat-conducting medium, keeping the temperature of froth breaking still tank interior is 20～100 ℃, to be conducive to froth breaking.After completing, binder stops passing into heat-conducting medium.
When polyamic acid resin solution enters froth breaking still, the gas interface of froth breaking still connects vavuum pump, and keeping in tank body is negative pressure 0.01～0.1MPa.
In the synthetic process of polyamic acid resin, to vacuumizing processing in reactor, keep negative pressure 0.01～0.1MPa in reactor, to synthetic complete.During discharging, in reactor, pass into carbon dioxide or nitrogen or other inert gas, keeping reacting kettle inner pressure is that 0.3～0.5MPa discharging is to froth breaking still.Negative pressure in reactor prevents that in polyamic acid resin building-up process, being involved in air in its system produces bubble.
Compared with prior art, the advantage that the present invention manufactures polyamic acid resin froth breaking still used and debubbling method is: 1, polyamic acid resin solution defoaming is complete, can eliminate the even nano level bubble of micron order, greatly improve the surface quality of subsequent handling gained Kapton; 2, foam time shortens greatly, be reduced to and be less than 1 hour, and defoaming effect is good by a few hours of the standing foam time of tradition, guarantees that follow-up film-forming process works continuously; 3, the thin layer distributor of froth breaking still installation is simple in structure, and de-foaming process is easy to operate; 4, prevent oxidation in the synthetic and froth breaking process of polyamic acid resin, the moisture absorption etc., guarantee to obtain superpolyamide acid resin; 5, prevent the chemical reactions such as polyamic acid resin molecule generation disproportionation, polyamic acid resin color uniformity, the apparent chromatic aberration defect of film product reduces.
Accompanying drawing explanation
The structural representation of the froth breaking still embodiment that this manufacture of Fig. 1 polyamic acid resin is used.
Figure internal label is: 1, feed pipe, 2, evacuated tube, 3, thin layer distributor, 4, temperature-detecting device, 5, heat-conducting medium entrance, 6, discharge nozzle, 7, heat-conducting medium outlet, 8, gas interface, 9, pressure-detecting device.
The specific embodiment
Manufacture polyamic acid resin froth breaking still embodiment used
This manufacture polyamic acid resin froth breaking still embodiment used as shown in Figure 1, comprises that there is feed pipe 1 the froth breaking still tank body top that holds polyamic acid resin liquid, and there is discharge nozzle 6 below, and thin layer distributor 3 is installed in tank body.This routine thin layer distributor 3 is sphere, the center line of sphere overlaps with tank body central shaft, and the vault of sphere is 10mm with the distance that stretches into feed pipe 1 lower port in tank, and under sphere, edge is 1.0mm with the gap of inner tank wall, the height of sphere is 0.4 of spherical diameter, is 1/3 of tank interior height.The lower edge of thin layer distributor has 2 places to be fixedly connected with froth breaking still inner tank wall, and the lower edge of thin layer distributor 3 is in same level height.This routine thin layer distributor 3 is made for transparent material, is convenient to observe resin solution froth breaking situation.
Between reactor and froth breaking still, carry on the pipeline of resin solution measuring pump is installed.
This froth breaking still tank body is provided with chuck, and chuck below has heat-conducting medium entrance 5, top to have heat-conducting medium outlet 7, and pipeline connects heat-conducting medium entrance 5, heat-conducting medium outlet 7 and heat conducting medium heating apparatus.Tank body is provided with temperature-detecting device 4.
This routine froth breaking still is sealed shell of tank, has gas interface 8 on tank body.Tank body is provided with pressure-detecting device 9.
The top of this routine froth breaking still tank body is also provided with evacuated tube 2, and described evacuated tube 2 is furnished with electromagnetism and opens and closes valve.
Manufacture polyamic acid resin process debubbling method embodiment used
Adopt this manufacture polyamic acid resin process of above-mentioned manufacture polyamic acid resin process froth breaking still embodiment used debubbling method embodiment used as follows,
After reinforced in reactor, connect vavuum pump, in reactor, keep negative pressure 0.1MPa, to synthetic complete.Pass into nitrogen, keeping reacting kettle inner pressure is that 0.3～0.5MPa discharging is to froth breaking still again.
The synthetic polyamic acid resin solution of reactor is delivered to froth breaking still, regulate between reactor and froth breaking still and carry the measuring pump rotating speed on resin solution pipeline, the flow that makes to enter the resin solution of froth breaking still is 2.5kg/min, feed pipe 1 through tank body top enters the top that polyamic acid resin in froth breaking still drops on transparent lamina distributor 3 spheres, the downward dispersion flows of sphere along thin layer distributor 3 forms thin layer, through the lower edge of thin layer distributor and the gap of inner tank wall, becoming thin layer again continues to flow downward along inner tank wall, the THICKNESS CONTROL of this routine polyamic acid resin solution is 0.5mm～2.5mm, finally at tank body inner bottom part, assemble.
When polyamic acid resin solution enters froth breaking still, regulate heat conducting medium heating apparatus, and continue to pass into heat-conducting medium, observe temperature-detecting device 4, the temperature of controlling froth breaking still tank interior is 50 ℃.After completing, binder stops passing into heat-conducting medium.
When polyamic acid resin solution enters froth breaking still, the gas interface 8 of froth breaking still connects vavuum pump, observes pressure-detecting device 9, remains negative pressure 0.1MPa in tank body.
Stop carrying polyamic acid resin solution to froth breaking still, after resin liquid level is stable, standing 30 minutes, close vavuum pump.Through gas interface 8, in still, pass into nitrogen, gas flow is 0.5m
3/ min, regulates the electromagnetic proportional valve in evacuated tube 2, and keeping still internal pressure is 0.3～0.5MPa.Polyamic acid resin force feed to slobbering machine in froth breaking still is salivated to film forming.
Comparative example is: the polyamic acid resin solution that identical reactor is manufactured, but do not vacuumize and add negative pressure in building-up process reactor, polyamic acid resin solution is transported in the common froth breaking still without thin layer distributor, keeping in still is negative pressure 0.1MPa, temperature is 30 ℃, and within standing 9 hours, froth breaking completes.
Comparative example and the present embodiment foam time and defoaming effect are more as shown in table 1:
Table 1 the present embodiment and comparative example debubbling method and defoaming effect comparison sheet
From the results shown in Table 1, this debubbling method embodiment of the froth breaking still of use the present embodiment is only with completing froth breaking half an hour, than the foam time of about ten hours that adopts conventional debubbling method to need, significantly shorten, and defoaming effect improves greatly, salivation film blibbing is only 0.6% of conventional debubbling method, and aberration also reduces greatly.
The present invention has not only shortened foam time greatly, improves the production efficiency of polyamic acid resin, has guaranteed Kapton continuous operations, and has obtained high-quality polyamic acid resin solution, and the quality of Kapton in subsequent handling is guaranteed.
Above-described embodiment, is only the specific case that object of the present invention, technical scheme and beneficial effect are further described, and the present invention is not defined in this.All any modifications of making, be equal to replacement, improvement etc., within being all included in protection scope of the present invention within scope of disclosure of the present invention.
Claims (10)
1. manufacture polyamic acid resin froth breaking still used, comprise that there is feed pipe (1) the froth breaking still tank body top that holds polyamic acid resin liquid, there is discharge nozzle (6) below, and froth breaking still is sealed shell of tank, has gas interface (8) on tank body; Tank body is provided with pressure-detecting device (9); It is characterized in that:
Thin layer distributor (3) is installed in described tank body, and this thin layer distributor (3) is arch surface of revolution, and the rotating shaft of curved surface overlaps with the central shaft of tank body; The vault of curved surface with stretch into the tank interior height that the distance of feed pipe (1) lower port in tank is 0.01mm to 1/3, the center line of curved surface overlaps with tank body center line, under curved surface, edge is 0.01mm～10mm with the gap of inner tank wall, and the maximum height of curved surface is 1/4 to 1/3 tank interior height; The lower edge of thin layer distributor (3) has a place or many places to be fixedly connected with froth breaking still inner tank wall, and the lower edge of thin layer distributor (3) is greater than 1/3 of tank interior height with the distance of tank body bottom surface.
2. manufacture polyamic acid resin according to claim 1 froth breaking still used, is characterized in that:
The surface of revolution of described thin layer distributor (3) is sphere, and the height of sphere is spherical diameter 1/3 to 1/2.
3. manufacture polyamic acid resin according to claim 1 and 2 froth breaking still used, is characterized in that:
Between reactor and froth breaking still, carry on the pipeline of resin solution measuring pump is installed.
4. manufacture polyamic acid resin according to claim 3 froth breaking still used, is characterized in that:
Froth breaking still tank body is provided with chuck, and chuck below has heat-conducting medium entrance (5), top to have heat-conducting medium outlet (7), and pipeline connects heat-conducting medium entrance (5), heat-conducting medium outlet (7) and heat conducting medium heating apparatus; Tank body is provided with temperature-detecting device (4).
5. manufacture polyamic acid resin according to claim 4 froth breaking still used, is characterized in that:
The top of froth breaking still tank body is also provided with evacuated tube (2), and described evacuated tube (2) is furnished with electromagnetism and opens and closes valve.
6. the manufacture polyamic acid resin process debubbling method used that manufacture polyamic acid resin according to claim 3 froth breaking still used designs, is characterized in that:
The synthetic polyamic acid resin solution of reactor is delivered to froth breaking still, feed pipe (1) through tank body top enters the vault that polyamic acid resin in froth breaking still drops on thin layer distributor (3) curved surface, the downward dispersion flows of curved surface along thin layer distributor (3) forms thin layer, through the lower edge of thin layer distributor (3) and the gap of inner tank wall, become thin layer along inner tank wall to dirty again, finally at tank body inner bottom part, assemble;
Regulate between reactor and froth breaking still and carry the measuring pump rotating speed on resin solution pipeline, the flow that makes to enter the resin solution of froth breaking still is 0.5～100kg/min, and the maximum ga(u)ge that is controlled at the upper resin solution layer forming of thin layer distributor (3) is less than 5mm;
Stop carrying polyamic acid resin solution to froth breaking still, in still after polyamic acid resin liquid level stabilizing standing 10～40 minutes, de-foaming process completed; When the variation in five minutes of the liquid level of resin solution is no more than 1mm, be considered as resin liquid level stable;
During the discharging of froth breaking still, through gas interface (8), in froth breaking still, pass into carbon dioxide or nitrogen or other inert gas, gas flow is 0.1m
3/ min～0.8m
3/ min, keeping still internal pressure is 0.3～0.5MPa; Polyamic acid resin pressurization in froth breaking still is sent into slobbering machine salivation film forming.
7. manufacture polyamic acid resin according to claim 6 debubbling method used, is characterized in that:
The flow that enters the resin solution of froth breaking still is 2.5～12kg/min.
8. manufacture polyamic acid resin according to claim 6 debubbling method used, is characterized in that:
Froth breaking still tank body is provided with chuck, and chuck below has heat-conducting medium entrance (5), top to have heat-conducting medium outlet (7), and pipeline connects heat-conducting medium entrance (5), heat-conducting medium outlet (7) and heat conducting medium heating apparatus; Tank body is provided with temperature-detecting device (4);
When polyamic acid resin solution enters froth breaking still, regulate heat conducting medium heating apparatus, and continue to pass into heat-conducting medium, observe temperature-detecting device (4), keeping the temperature of resin system in froth breaking still tank body is 20～100 ℃; After completing, binder stops passing into heat-conducting medium.
9. manufacture polyamic acid resin according to claim 6 debubbling method used, is characterized in that:
When polyamic acid resin solution enters froth breaking still, the gas interface of froth breaking still (8) connects vavuum pump, remains negative pressure 0.01～0.1MPa in tank body.
10. manufacture polyamic acid resin according to claim 6 debubbling method used, is characterized in that:
After reinforced in reactor, connect vavuum pump, in reactor, keep negative pressure 0.01～0.1MPa, to synthetic complete; During discharging, in reactor, pass into carbon dioxide or nitrogen or other inert gas, keeping reacting kettle inner pressure is that 0.3～0.5MPa discharging is to froth breaking still.
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| CN107050932A (en) * | 2017-06-06 | 2017-08-18 | 利穗科技(苏州)有限公司 | Double buffering type bubble trap |
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| CN109260769A (en) * | 2018-12-04 | 2019-01-25 | 攀枝花荣鑫油漆有限责任公司 | A kind of paint defoaming device |
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| CN109276916A (en) * | 2018-10-31 | 2019-01-29 | 中国久远高新技术装备公司 | A kind of high viscosity resins liquid evacuation and centrifugal degassing method and device |
| CN109260769A (en) * | 2018-12-04 | 2019-01-25 | 攀枝花荣鑫油漆有限责任公司 | A kind of paint defoaming device |
| CN109537067A (en) * | 2018-12-19 | 2019-03-29 | 四川辉腾科技股份有限公司 | A kind of defoaming method of aramid IIII fiber spinning solution and its application |
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