CN103028274B - Defoaming method in synthesizing process of polyamide resin - Google Patents
Defoaming method in synthesizing process of polyamide resin Download PDFInfo
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- CN103028274B CN103028274B CN201210562145.1A CN201210562145A CN103028274B CN 103028274 B CN103028274 B CN 103028274B CN 201210562145 A CN201210562145 A CN 201210562145A CN 103028274 B CN103028274 B CN 103028274B
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Abstract
The invention discloses a defoaming method in the synthesizing process of polyamide resin. The method comprises the following steps: heating and slowly stirring polyamide resin solution in a kettle at first at the temperature of 35 to 100 DEG C at normal pressure for 0.5 to 1.5h, wherein the stirring speed is less than or equal to 50r/min; then, quickly stirring the polyamide resin solution at a stirring speed of 60 to 100r/min at the same temperature for 2 to 4h; and casting film when the defoaming is completed, wherein CO2, nitrogen or other inert gas can be fed during the casting of the film to prevent the resin from discoloring and deteriorating at a gas flow of 0.1 to 0.8 m<3>/min, and a relative pressure of 0.3 to 0.5MPa is kept in the kettle. According to the method, the foaming is thorough, the surface quality of the film obtained later is improved, the defoaming time is short and the defoaming process is convenient in operation.
Description
Technical field
The present invention relates to the synthetic technology of polyamic acid resin, be specially the debubbling method of polyamic acid resin building-up process.
Background technology
Kapton is the macromolecular material with excellent properties such as high strength, high tenacity, abrasion performance, high temperature resistant, anticorrosions, is widely used in electrotechnical, electronic industry, particularly the main insulating materials of various high-grade electrical equipment especially in electrician trade.
At present the production technology of Kapton is taking polyamic acid resin solution as raw material, salivates moulding and obtains self-supporting polyamic acid thick film, then obtain Kapton through adding hot-stretch, imidization, cooling and shaping processing on slobbering machine.For reducing the weight and volume of downstream application field product, the film thickness specification of the market demand is tending towards slimming.
Making the little film of thickness just needs the quality of polyamide-acid polyimide resin to improve, 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 use on electric and electronic product.
Existing conventional polyamic acid resin is synthetic is the polymerisation manufacture under the effect of solvent dimethylacetylamide by dianhydride and diamines in the reactor in continuing cooling or heating condition.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 in froth breaking still and leaves standstill or vacuum state maintenance a few hours, treats its nature or negative pressure froth breaking.Because polyamide-acid polyimide resin solution viscosity is larger, for current Kapton manufacture, its debubbling method is difficult to eliminate in the short period small bubble, and causes the abnormal and blemish such as producing flaw that manufactures a product of production serialization.
Summary of the invention
The object of the invention is to design a kind of debubbling method of polyamic acid resin building-up process, by heating and stirring the micro-bubble of eliminating in resin solution, the film quality that gained polyamic acid resin solution makes is improved.
The debubbling method of the polyamic acid resin building-up process of the present invention's design comprises the steps:
I, heating low rate mixing
Polyamic acid resin solution after synthetic reaction is pressed into through the charging mouth of pipe of froth breaking still tank body top from reactor, and to the polyamic acid resin solution heating in still, temperature remains on 35～100 DEG C, is preferably 60～80 DEG C, and stir speed (S.S.) is less than or equal to 50r/min; Maintain 0.5～1.5 hour; Within every 5～30 minutes, change a mixing direction, clockwise, counterclockwise replace stirring;
II, heating rapid stirring
Temperature remains unchanged, and speed of agitator is increased to 60～100r/min, and preferred version is 75～85r/min; Within every 5～30 minutes, change a mixing direction; Add thermal agitation and maintain 2～4 hours, froth breaking completes;
III, stream film
Send polyamic acid resin solution to slobbering machine from the discharge nozzle of froth breaking still bottom, until resin salivation is complete in still.
When step I, II are carried out, keeping still internal pressure is normal atmosphere (An), and manometric relative pressure reading is zero.
When step III is carried out, in still, pass into carbon dioxide or nitrogen or other inert gas from the gas access of froth breaking still.The gas flow passing in froth breaking still is 0.1～0.8m
3/ min, is preferably 0.3～0.5m
3/ min.Regulate the aperture of evacuated tube, keeping relative pressure in still is 0.3～0.5MPa.
Compared with prior art, the advantage of the debubbling method of polyamic acid resin building-up process of the present invention is: 1, polyamic acid resin solution resin froth breaking is complete, greatly improves the surface quality of subsequent handling gained Kapton; 2, the foam time that reaches good result shortens to 3～4 hours, ensures film-forming process continuous operations; 3, froth breaking still is simple in structure, and de-foaming process is easy to operate; 4, in froth breaking still, resin temperature homogeneity is good; 5, foam time shortens and reduces polyamic acid resin generation variable color, the reaction such as rotten, polyamic acid resin color uniformity, and the apparent chromatic aberration defect of film product reduces.
Detailed description of the invention
The debubbling method embodiment of this polyamic acid resin building-up process comprises the steps:
I, heating low rate mixing
Polyamic acid resin solution after synthetic reaction is pressed into through the charging mouth of pipe of froth breaking still tank body top from reactor, it is equal with the helical blade peak of stirring that polyamic acid resin is pressed into total amount liquid level under stirring not, or exceed helical blade peak 10mm.In the chuck of froth breaking still, pass into the medium of heating, or also can in the heat-conducting medium pipeline of helical blade hollow, pass into the heat-conducting medium of heating, to the polyamic acid resin solution heating in still, temperature remains on 70 DEG C, and stir speed (S.S.) is 50r/min; Maintain 1 hour; Within every 20 minutes, change a mixing direction, clockwise, counterclockwise replace stirring;
II, heating rapid stirring
Temperature remains unchanged, and speed of agitator is increased to 80r/min; Within every 20 minutes, change a mixing direction; Add thermal agitation and maintain 3 hours, froth breaking completes;
III, stream film
Send polyamic acid resin solution to slobbering machine from the discharge nozzle of froth breaking still bottom, until resin salivation is complete in still.
When step I, II are carried out, keeping relative pressure in still is 0.
When step III is carried out, in still, pass into carbon dioxide from the gas access of froth breaking still, flow is 0.4m
3/ min, the aperture of adjusting evacuated tube, keeping still internal pressure is 0.3MPa.
The debubbling method comparative example of conventional polyamic acid resin building-up process
In reactor, complete routinely synthetic polyamide-acid polyimide resin solution and be pressed in common froth breaking still and keep relative negative pressure-0.1MPa state 9.5 hours, finish froth breaking.
In still, pass into compressed air from the gas access of common froth breaking still, regulate the electromagnetic proportional valve in evacuated tube, keeping still internal pressure is 0.4MPa, until resin salivation is complete in still.
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 foam time and defoaming effect comparison sheet
From the results shown in Table 1, adopt this routine debubbling method only just to complete froth breaking by the half of conventional foam time, and defoaming effect improves greatly, salivation film blibbing is only 2% of conventional debubbling method, the present invention not only improves the production efficiency of polyamic acid resin, ensure Kapton continuous operations, and obtained high-quality polyamic acid resin solution, 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 amendments 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 (5)
1. the debubbling method of polyamic acid resin building-up process, is characterized in that comprising the steps:
I, heating low rate mixing
Polyamic acid resin solution after synthetic reaction is pressed into through the charging mouth of pipe of froth breaking still tank body top from reactor, and to the polyamic acid resin solution heating in still, temperature remains on 35～100 DEG C, and stir speed (S.S.) is less than or equal to 50r/min; Maintain 0.5～1.5 hour; Within every 5～30 minutes, change a mixing direction, clockwise, counterclockwise replace stirring;
II, heating rapid stirring
Temperature remains unchanged, and stir speed (S.S.) is increased to 60～100r/min, adds thermal agitation and maintains 2～4 hours, within when stirring every 5～30 minutes, changes a mixing direction, clockwise, counterclockwise replaces stirring; Froth breaking completes;
III, stream film
Send polyamic acid resin solution to slobbering machine from the discharging mouth of pipe of froth breaking still bottom, until resin salivation is complete in still.
2. the debubbling method of polyamic acid resin building-up process according to claim 1, is characterized in that:
In described step I, temperature remains 60～80 DEG C.
3. the debubbling method of polyamic acid resin building-up process according to claim 1, is characterized in that:
In described step II, stir speed (S.S.) is 75～85r/min.
4. the debubbling method of polyamic acid resin building-up process according to claim 1, is characterized in that:
When described step I, II are carried out, keeping still internal pressure is normal atmosphere (An);
When described step III is carried out, in still, pass into carbon dioxide or nitrogen or other inert gas from the gas access of froth breaking still; The gas flow passing in froth breaking still is 0.1～0.8m
3/ min, keeping relative pressure in still is 0.3～0.5MPa.
5. the debubbling method of polyamic acid resin building-up process according to claim 5, is characterized in that:
When described step III is carried out, the gas flow passing in froth breaking still is 0.3～0.5m
3/ min.
Priority Applications (1)
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| CN201210562145.1A CN103028274B (en) | 2012-12-21 | 2012-12-21 | Defoaming method in synthesizing process of polyamide resin |
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| CN201210562145.1A CN103028274B (en) | 2012-12-21 | 2012-12-21 | Defoaming method in synthesizing process of polyamide resin |
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| CN103028274B true CN103028274B (en) | 2014-09-24 |
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| CN106328829B (en) * | 2016-09-29 | 2018-03-27 | 昆山工研院新型平板显示技术中心有限公司 | The preparation method of flexible base board in a kind of displayer |
| CN107185276A (en) * | 2017-05-25 | 2017-09-22 | 完美（中国）有限公司 | A kind of quick debubbling method of cleaning product |
| CN115212610A (en) * | 2022-06-28 | 2022-10-21 | 北京康宇建医疗器械有限公司 | Method for removing bubbles from polymer film-forming liquid |
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| CH655857A5 (en) * | 1982-07-21 | 1986-05-30 | Micafil Ag | MIXING AND DEGASSING DEVICE FOR POWDERED FLUIDS. |
| EP1757957A3 (en) * | 2005-08-22 | 2007-11-14 | Nippon Shokubai Co., Ltd. | Fluorinated polyamide acid resin composition for optical materials |
| CN100425625C (en) * | 2005-12-16 | 2008-10-15 | 天津科技大学 | Method for eliminating micro-bubble in high-viscosity latex solution |
| CN101062984A (en) * | 2006-04-28 | 2007-10-31 | 宋成根 | Processing technique of super heat-proof polyimide film |
| CN101891891A (en) * | 2010-07-29 | 2010-11-24 | 宜兴市高拓高分子材料有限公司 | Method for preparing low-expansion coefficient polyimide film by nonrandom copolymerization |
| CN102627780A (en) * | 2012-03-30 | 2012-08-08 | 北京化工大学 | Method for preparing submicron polyimide self-supporting film by adopting spin-coating method |
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