CN101081904A - Preparation method of polyimide film used for oscillation film - Google Patents
Preparation method of polyimide film used for oscillation film Download PDFInfo
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- CN101081904A CN101081904A CN 200710041509 CN200710041509A CN101081904A CN 101081904 A CN101081904 A CN 101081904A CN 200710041509 CN200710041509 CN 200710041509 CN 200710041509 A CN200710041509 A CN 200710041509A CN 101081904 A CN101081904 A CN 101081904A
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Abstract
The polyimide film with Tg of 250-350 deg.c is prepared with polyamic acid solution and through flow casting or gumming and filming at 240-400 deg.c. The polyamic acid solution is prepared with 3, 3', 4, 4'-diphenyl ether tetracid dihydride in 20-90 molar weight, other aromatic dihydride in 10-80 molar weight and aromatic diamine in 100 molar weight, and through reaction in polar aprotic solvent at the temperature from room temperature to 100 deg.c. The polyimide film may be shaped into vibrating diaphragm in required shape, and the vibrating diaphragm has modulus of 2.5-3.7 GPa, internal attenuation greater than or equal to 0.03, ultimate elongation not lower than 10.6 %, secondary distortion at frequency higher than 1000 Hz lower than 40 dB, and service life over 5 years.
Description
One, technical field
The present invention relates to the preparation method of polyimide film used for oscillation film, relating to the oxydiphenyl diformic dianhydride or rather is master's the acid anhydrides and the method for aromatic diamine prepared in reaction Kapton.
Two, background technology
Kapton is replaced the device tympanum with what high power acoustics tympanum and electroacoustic and has been obtained very ten-strike, by their thermotolerance height of what, dimensional stability is good, sound propagation velocity is fast, obtains users' favor.Except that large-scale sound equipment, the large-scale loudspeaker of broadcasting and televisor, computer and mobile phone etc. all is extensive use of the polyimide tympanum.
Miniaturization and lightweight along with household electrical appliance, the polyimide tympanum is proposed higher requirement, requirement thermotolerance height, Kapton Tg is in 250～350 ℃ of scopes, use temperature is more than 200 ℃ continuously, the film dimensions good stability, sprayed coating is indeformable under 1.1MPa air pressure, modulus is at 2.5～3.5GPa, the bass resonant frequency is little, and tangent of the dielectric loss angle tan θ is between 0.025～0.4, and frequency causes of sound distortion value when 450Hz, 700Hz, 3000Hz is-40dB, it is 250% that the film elongation is 120%, 300 ℃ for 100 ℃.The consequent is the film of Kapton by a kind of acid anhydrides and a kind of amine polymerization curtain coating or impregnation preparation, transforms to the copolyimide film.
Prior art spy opens flat 2003-289594,10.10.2003 disclosure polyetherimide film modulus is littler than PEN film, it is little that bass resonance relates to rate, but poor dimensional precision, the tympanum roar is big, and tonequality is bad, the film gage distortion, the tonequality of loud speaker has deviation, and production performance is still undesirable.
The special fair 7-101953 of another prior art, disclose November 1 nineteen ninety-five pyromellitic acid anhydride and 4,4 '-Kapton of diaminodiphenyl oxide preparation, 100 ℃ of tension tests of what, thickness is that the film elongation of 50um is 100%, tympanum what with its preparation has the shrinkage strain phenomenon for 200 ℃, and sound propagation velocity 1454m/sec reproduces frequency band upper limit 22000HZ, transient characteristic is moderate, high frequency distortion 80%.But the film fracture takes place when having sheet forming repeatedly, produce the poor performance of good sound equipment with tympanum.
Purpose of the present invention overcomes the polyetherimde films poor dimensional precision exactly, and the tympanum roar is big, 200 ℃ of the little whats of lower tone and heat resisting temperature, and the shortcoming of PMMI film production difference.Good heat resistance is provided, and tonequality is good, and the copolyimide film that dimensional stability is good and productivity is good is for the system used for oscillation.
Three, summary of the invention
The present invention is mainly by 90～20 mole 3,3 ', 4,4 ' one diphenyl ether tetraformic dianhydrides and 10～80 moles of other aromatic dianhydrides become Qie Shi viscosity with 100 moles of aromatic diamines what room temperature～100 ℃ prepared in reaction in polar aprotic solvent N,N-DIMETHYLACETAMIDE (DMAC) be 5～30 minutes polyamic acid solution, via 240～400 ℃ of casting film-formings, the acquisition second-order transition temperature is 250～350 ℃ a Kapton, forms the sounder tympanum of different shapes then at 20～60 ℃ of following plastics sucking mouldings of high what second-order transition temperature.
Its other party family dianhydride here is to choose any one kind of them from the colony that pyromellitic acid anhydride, bibenzene tetracarboxylic dianhydride, benzophenone tetracarboxylic acid dianhydride, dihydroxyphenyl propane diether acid anhydride and trimellitic acid 1,2-anhydride are formed or two kinds mixed anhydride.
Aromatic diamine is from 4,4 ' one diaminodiphenyl oxide, and 4,4 ' one diaminodiphenyl-methane is chosen any one kind of them in the colony that 4,4 ' one diaminodiphenylsulfone(DDS) and dihydroxyphenyl propane diether amine are formed.
Under 20～60 ℃ of high what second-order transition temperatures, the Kapton of the present invention preparation carry out sheet forming system sound equipment with tympanum except that with plastic uptake or the impregnation moulding, method moulding such as also available deep drawing molding, pressurized air air-pressure forming and cotton ginning moulding.
Kapton performance according to the present invention's preparation is as follows:
Outward appearance: the film of golden transparent
Elongation (room temperature) 40～80%
Tensile strength 150～200MPa
Dielectric strength 160～220KV/mm
Thickness 20～125 μ m
250～350 ℃ of second-order transition temperature Tg.
Carry out moulding formation sound equipment tympanums such as plastic uptake with Kapton of the present invention, its performance is as follows:
Modulus 2.5～3.7GPa
Inner decay 〉=0.03
Elongation limit 〉=10.6%
Frequency is more than 1000Hz, and then second-order distortion is＜40dB, deposits under drying conditions, 5 years working lives, still can use after the retest-ok.
Tympanum by the present invention preparation can be made different shape according to customer requirements, shapes such as roof, like garden shape, square, taper, vpg connection does not impose any restrictions, this tympanum can be in 200～250 ℃ of scopes life-time service.
By the Kapton of the present invention's preparation, not only can use what sounder and electroacoustic transducer tympanum, also can be used as the band bonding film of using automatically.
Four, embodiment:
Especially exemplified by example it is described in order to implement the present invention better, but is not limitation of the present invention.
Embodiment 1
To being equipped with agitator, thermometer, drop into 920g (5 moles) 4 in the 10 liter reactors of import and export of nitrogen and charge cavity, 4 '-diaminodiphenyl oxide, the what room temperature is stirring and dissolving in the 4600ml dimethylacetamide solvent, after treating to dissolve fully, add 1085g (3.5 moles) 3,3 ', 4,4 '-diphenyl ether tetraformic dianhydride and 327g (1.5 moles) pyromellitic acid anhydride, reinforced finishing, after 45 ℃ of whats react and are 20 minutes to the Qie Shi viscosity of solution, add N,N-DIMETHYLACETAMIDE and be diluted to 15% solid content, through the stream court of a feudal ruler or impregnation, by 240～350 ℃ of film forming, this film Tg is 275 ℃, is that 275 ℃ of following plastics sucking mouldings make roof, garden shape tympanum 50 ℃ of high what second-order transition temperatures then.
The Kapton of present embodiment preparation is golden yellow transparent face look, elongation (room temperature) 80%, and tensile strength 195MPa, dielectric strength 220KV/mm, thickness 25～90 μ m, thickness tolerance＜4 μ m, Tg275 ℃, can be at 245 ℃ of following life-time service.With the tympanum of its preparation, its modulus is 3.2GPa, inner decay 0.03, and elongation limit 10%, frequency are more than 1000Hz, and then second-order distortion is＜40dB, 5 years working lives.
Embodiment 2
Remove and add 990g (5 moles) 4,4 '-diaminodiphenyl-methane and 1395g (4.5 moles) 3,3 ', 4,4 ', the reaction of-diphenyl ether tetraformic dianhydride and 147g (0.5 mole) bibenzene tetracarboxylic dianhydride, solution Qie Shi viscosity is 10 minutes, solid content is 20%, through curtain coating or impregnation by 240～400 ℃ of film forming, this film Tg is 275 ℃, and 60 ℃ promptly 345 ℃ of high what second-order transition temperatures, it is the same with embodiment 1 with performance index that plastics sucking moulding forms outer other operation of tympanum then.
Embodiment 3
Remove to add 310 (1 moles) 3,3 ', 4,4 ' ,-diphenyl ether tetraformic dianhydride and 2080g (4 moles) dihydroxyphenyl propane dianhydride and 1240g (5 moles) 4,4 ', the reaction of-diaminodiphenylsulfone(DDS), solution Qie Shi viscosity is 25 minutes, and solid content 18% is through curtain coating or impregnation, by 250～400 ℃ of film forming, Tg250 ℃ of this film is that 275 ℃ of following plastics sucking mouldings form outside the tympanum 25 ℃ of high what second-order transition temperatures, and other operation stepss are the same with embodiment 1, film performance is tensile strength 200MPa as a result, elongation 40%, dielectric strength 160KV/mm, film thickness 125 μ m, thickness tolerance 4 μ m, Tg250 ℃, the tympanum modulus is 2.5GPa, and other performances are the same with embodiment 1.
The tympanum of 3 preparations of embodiment 1 to embodiment has higher thermotolerance than the tympanum of polyethylene terephthalate, polyphenylene sulfide, polyetherimide preparation.Relatively has better formability with equal benzene type polyimide.The thin-film acoustic effect spy of the present invention's preparation is good.
Claims (4)
1, the preparation method of polyimide film used for oscillation film, its feature at what mainly by 90～20 mole 3,3 ', 4,4 '-become Qie Shi viscosity with 100 moles of aromatic diamines what room temperature～100 ℃ following prepared in reaction in the polar aprotic solvent N,N-DIMETHYLACETAMIDE be that the polyamic acid solution of 5～30 minutes viscosity is through curtain coating or impregnation for diphenyl ether tetraformic dianhydride and 10～80 moles of other aromatic dianhydrides, by 240～400 ℃ of film forming, the acquisition second-order transition temperature is 250～350 ℃ a Kapton, makes the sounder tympanum of different shape with plastic uptake or compression molding method.
2, the preparation method of polyimide film used for oscillation film according to claim 1, its feature are to choose any one kind of them from pyromellitic acid anhydride, bibenzene tetracarboxylic dianhydride, benzophenone tetracarboxylic acid dianhydride, dihydroxyphenyl propane dianhydride and trimellitic acid 1,2-anhydride or two kinds mixed anhydride at described other aromatic dianhydrides of what.
3, the preparation method of polyimide film used for oscillation film according to claim 1, its feature is from 4 at the described aromatic diamine of what, 4 ' one diaminodiphenyl oxides, 4,4 ' one diaminodiphenyl-methanes, 4,4 ' one diaminodiphenylsulfone(DDS)s are chosen any one kind of them in dihydroxyphenyl propane diether amine and 3,4 ' one diaminodiphenyl oxide.
4, the preparation method of polyimide film used for oscillation film according to claim 1, its feature is 20～60 ℃ of the high what multipolymer of the described plastic uptake film forming of what temperature second-order transition temperatures.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200710041509 CN101081904A (en) | 2007-05-31 | 2007-05-31 | Preparation method of polyimide film used for oscillation film |
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| CN 200710041509 CN101081904A (en) | 2007-05-31 | 2007-05-31 | Preparation method of polyimide film used for oscillation film |
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| CN101081904A true CN101081904A (en) | 2007-12-05 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109366826A (en) * | 2018-10-26 | 2019-02-22 | 镇江龙成绝缘材料有限公司 | A kind of polyimide film curtain coating method production technology |
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2007
- 2007-05-31 CN CN 200710041509 patent/CN101081904A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109366826A (en) * | 2018-10-26 | 2019-02-22 | 镇江龙成绝缘材料有限公司 | A kind of polyimide film curtain coating method production technology |
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Application publication date: 20071205 |