CN104211973B - Polyimide film - Google Patents
Polyimide film Download PDFInfo
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- CN104211973B CN104211973B CN201410129169.7A CN201410129169A CN104211973B CN 104211973 B CN104211973 B CN 104211973B CN 201410129169 A CN201410129169 A CN 201410129169A CN 104211973 B CN104211973 B CN 104211973B
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- polyamic acid
- solution
- film
- kapton
- aromatic diamines
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Abstract
The invention discloses a polyimide film. The polyimide film is obtained by polymerization of aromatic diamine and biphthalicanhydride. A preparation method of the polyimide film mainly comprises raw material treatment, resin synthesis, steel belt curtain-coating and imidization treatment. The polyimide film is prepared directly from a diamine or dianhydride unit having a high rigid structure by a homopolymerization or copolymerization method. Compared with the existing polyimide film, the polyimide film provided by the invention has higher strength, rigidity and size stability.
Description
Technical field
The invention belongs to field of material technology, be specifically related to a kind of insulating polymeric material Kapton.
Background technology
Kapton (PIF) is a kind of novel high temperature resistant organic polymer thin film.It has high-modulus, lower shrinkage, high strength, low water absorption, hydrolysis, radiation hardness, nontoxic, excellent insulativity and resistance to thermo-oxidative stability.Because it is that one of current thin-film material the most expensive is in the world so be called as " gold film ".It is the key insulating material of electric apparatus, is also the key material of micro-electronic manufacturing and encapsulation.
The polymkeric substance that the Kapton of traditional structure is is basic structural unit with pyromellitic acid anhydride (PMDA) and 4 ' 4-diaminodiphenyl oxide (ODA), by the restriction of its chemical structure, there is lower Young's modulus and larger linear expansivity and percent thermal shrinkage.The method of traditional raising Kapton modulus is by adding rigid inorganic nano-filler, adopts the method for in-situ polymerization to prepare Kapton hybrid film, to improve elasticity modulus of materials and dimensional stability.But the Kapton that this method is obtained, intensity is low, poor rigidity, dimensional stability are bad.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing defect, provides a kind of Kapton.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of Kapton of the present invention, it is polymerized primarily of aromatic diamines and biphenyl dianhydride;
Its preparation method is as follows:
(1) Feedstock treating
Aromatic diamines and biphenyl dianhydride carried out grind, pulverize, dry;
(2) resins synthesis
Be that 1:1 ~ 1:1.1 successively joins in dimethylacetamide solution and carries out dissolving and reacting by the aromatic diamines after step (1) process and biphenyl dianhydride according to mass ratio, obtain polyamic acid solution, deaeration is laggard to be entered to salivate operation;
(3) steel band salivation
Carry out steel band salivation through the polyamic acid resin solution of step (2) gained and make polyamic acid solid film;
(4) imidization process
First, when the polyamic acid solid film after salivation being progressively heated to volatilization temperature required for desolventizing and stretching will be close temperature; Afterwards, film is longitudinally elongated; Finally, at 350 ~ 400 DEG C, carry out pyroprocessing, make polyamic acid be converted into polyimide;
(5) film forming
After film after step (4) imidization process is carried out two-way stretch and thermal treatment, obtain Kapton finished product.
Further, in step (1), described aromatic diamines is the one in mphenylenediamine or Ursol D.
Further, in step (1), described biphenyl dianhydride can also be aromatic dianhydride.
Further, in step (1), described aromatic diamines is withering under vacuo, and its vacuum tightness is 80Kpa ~ 100Kpa, and drying temperature is 160 ~ 180 DEG C, 4 ~ 5 hours time of drying.
Further, in step (1), described biphenyl dianhydride is dried in drying room, and its storing temperature is 180 ~ 210 DEG C, baking time 2 ~ 5 hours.
Further, in step (2), the massfraction of described dimethylacetamide solution is 15% ~ 25%.
Further, described dimethylacetamide solution can also be dimethyl formamide solution or N-Methyl pyrrolidone solution.
The beneficial effect that the present invention reaches is:
The present invention, by directly selecting the diamines or dianhydride units with higher rigid structure, adopts Kapton prepared by the method for homopolymerization or copolymerization, and all more existing Kapton of its intensity, rigidity and dimensional stability has had and significantly improves.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Embodiment 1
(1) Feedstock treating
Carried out by mphenylenediamine grinding, pulverizing, then by its drying treatment under vacuo, vacuum tightness is 90Kpa, and temperature is 160 DEG C, 5 hours time of drying;
Carried out by biphenyl dianhydride grinding, pulverizing, then it dried in drying room, storing temperature is 180 DEG C, and baking time is 5 hours, stand-by after being down to room temperature;
(2) resins synthesis
By the mphenylenediamine after step (1) process and biphenyl dianhydride be that 1:1 successively joins in dimethylacetamide solution (its massfraction is 15%) and carries out dissolving and reacting according to mass ratio, obtain polyamic acid solution, deaeration is laggard to be entered to salivate operation;
(3) steel band salivation
Carry out steel band salivation through the polyamic acid resin solution of step (2) gained and make polyamic acid solid film;
(4) imidization process
First, when the polyamic acid solid film after salivation being progressively heated to volatilization temperature required for desolventizing and stretching will be close temperature; Afterwards, film is longitudinally elongated; Finally, at 400 DEG C, carry out pyroprocessing, make polyamic acid be converted into polyimide;
(5) film forming
After film after step (4) imidization process is carried out two-way stretch and thermal treatment, obtain Kapton finished product.
Embodiment 2
(1) Feedstock treating
Carried out by Ursol D grinding, pulverizing, then by its drying treatment under vacuo, vacuum tightness is 80Kpa, and temperature is 180 DEG C, 4 hours time of drying;
Aromatic dianhydride carried out grinding, pulverizing, then it dried in drying room, storing temperature is 210 DEG C, and baking time is 2 hours, stand-by after being down to room temperature;
(2) resins synthesis
By the Ursol D after step (1) process and aromatic dianhydride be that 1:1.1 successively joins in dimethyl formamide solution (its massfraction is 25%) and carries out dissolving and reacting according to mass ratio, obtain polyamic acid solution, deaeration is laggard to be entered to salivate operation;
(3) steel band salivation
Carry out steel band salivation through the polyamic acid resin solution of step (2) gained and make polyamic acid solid film;
(4) imidization process
First, when the polyamic acid solid film after salivation being progressively heated to volatilization temperature required for desolventizing and stretching will be close temperature; Afterwards, film is longitudinally elongated; Finally, at 350 DEG C, carry out pyroprocessing, make polyamic acid be converted into polyimide;
(5) film forming
After film after step (4) imidization process is carried out two-way stretch and thermal treatment, obtain Kapton finished product.
Embodiment 3
(1) Feedstock treating
Carried out by Ursol D grinding, pulverizing, then by its drying treatment under vacuo, vacuum tightness is 100Kpa, and temperature is 170 DEG C, 4.5 hours time of drying;
Carried out by biphenyl dianhydride grinding, pulverizing, then it dried in drying room, storing temperature is 200 DEG C, and baking time is 3 hours, stand-by after being down to room temperature;
(2) resins synthesis
By the Ursol D after step (1) process and biphenyl dianhydride be that 1:1.1 successively joins in N-Methyl pyrrolidone solution (its massfraction is 20%) and carries out dissolving and reacting according to mass ratio, obtain polyamic acid solution, deaeration is laggard to be entered to salivate operation;
(3) steel band salivation
Carry out steel band salivation through the polyamic acid resin solution of step (2) gained and make polyamic acid solid film;
(4) imidization process
First, when the polyamic acid solid film after salivation being progressively heated to volatilization temperature required for desolventizing and stretching will be close temperature; Afterwards, film is longitudinally elongated; Finally, at 350 DEG C, carry out pyroprocessing, make polyamic acid be converted into polyimide;
(5) film forming
After film after step (4) imidization process is carried out two-way stretch and thermal treatment, obtain Kapton finished product.
To according to the obtained Kapton of embodiment 1 to 3 and the finished product property indices selecting Kapton conventional in the market design test as a comparison, result is as follows:
As can be seen from upper table data, the present invention is by directly selecting the diamines or dianhydride units with higher rigid structure, adopt Kapton prepared by the method for homopolymerization or copolymerization, all more existing Kapton of its intensity, rigidity and dimensional stability has had and has significantly improved.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. prepare a method for Kapton, it is characterized in that, it is polymerized primarily of aromatic diamines and biphenyl dianhydride;
Its preparation method is as follows:
(1) Feedstock treating
Aromatic diamines and biphenyl dianhydride carried out grind, pulverize, dry;
(2) resins synthesis
Be that 1:1 ~ 1:1.1 successively joins in dimethylacetamide solution and carries out dissolving and reacting by the aromatic diamines after step (1) process and biphenyl dianhydride according to mass ratio, obtain polyamic acid solution, deaeration is laggard to be entered to salivate operation;
(3) steel band salivation
Carry out steel band salivation through the polyamic acid resin solution of step (2) gained and make polyamic acid solid film;
(4) imidization process
First, when the polyamic acid solid film after salivation being progressively heated to volatilization temperature required for desolventizing and stretching will be close temperature; Afterwards, film is longitudinally elongated; Finally, at 350 ~ 400 DEG C, carry out pyroprocessing, make polyamic acid be converted into polyimide;
(5) film forming
After film after step (4) imidization process is carried out two-way stretch and thermal treatment, obtain Kapton finished product;
In step (1), described aromatic diamines is the one in mphenylenediamine or Ursol D;
In step (1), described aromatic diamines is withering under vacuo, and its vacuum tightness is 80Kpa ~ 100 Kpa, and drying temperature is 160 ~ 180 DEG C, 4 ~ 5 hours time of drying;
In step (1), described biphenyl dianhydride is dried in drying room, and its storing temperature is 180 ~ 210 DEG C, baking time 2 ~ 5 hours;
In step (2), the massfraction of described dimethylacetamide solution is 15% ~ 25%.
2. a kind of method preparing Kapton according to claim 1, is characterized in that, in step (2), described dimethylacetamide solution can also be dimethyl formamide solution or N-Methyl pyrrolidone solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410129169.7A CN104211973B (en) | 2014-04-01 | 2014-04-01 | Polyimide film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410129169.7A CN104211973B (en) | 2014-04-01 | 2014-04-01 | Polyimide film |
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| CN104211973A CN104211973A (en) | 2014-12-17 |
| CN104211973B true CN104211973B (en) | 2015-06-17 |
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| CN201410129169.7A Active CN104211973B (en) | 2014-04-01 | 2014-04-01 | Polyimide film |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104845367A (en) * | 2015-01-14 | 2015-08-19 | 无锡龙舜实业有限公司 | Plastic agricultural film |
| CN104845368A (en) * | 2015-04-01 | 2015-08-19 | 无锡龙舜实业有限公司 | Preparation process of shield plastic film |
| CN106893123A (en) * | 2017-03-01 | 2017-06-27 | 江阴骏友电子股份有限公司 | A kind of preparation method of high-modulus, high-strength novel Kapton |
| CN108284627B (en) * | 2018-01-30 | 2020-05-05 | 中国久远高新技术装备公司 | Preparation method of wet-process casting solidification forming film |
Citations (6)
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|---|---|---|---|---|
| CN1036965A (en) * | 1988-04-13 | 1989-11-08 | 纳幕尔杜邦公司 | Highly soluble aromatic polyimides |
| JP2004068002A (en) * | 2002-06-13 | 2004-03-04 | Du Pont Toray Co Ltd | Method for manufacturing polyimide-mixed film and metal-wiring circuit board using the same as substrate |
| CN101062984A (en) * | 2006-04-28 | 2007-10-31 | 宋成根 | Processing technique of super heat-proof polyimide film |
| CN101168598A (en) * | 2007-10-08 | 2008-04-30 | 江阴市云达电子新材料有限公司 | Method for preparing ultra-thick polyimide film with high heat conductivity and low thermal expansion coefficient |
| CN101321807A (en) * | 2005-12-05 | 2008-12-10 | 可隆株式会社 | Polyimide film |
| CN101798463A (en) * | 2010-03-26 | 2010-08-11 | 上海缘达聚合材料有限公司 | High-performance polyimide film and preparation method thereof |
-
2014
- 2014-04-01 CN CN201410129169.7A patent/CN104211973B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036965A (en) * | 1988-04-13 | 1989-11-08 | 纳幕尔杜邦公司 | Highly soluble aromatic polyimides |
| JP2004068002A (en) * | 2002-06-13 | 2004-03-04 | Du Pont Toray Co Ltd | Method for manufacturing polyimide-mixed film and metal-wiring circuit board using the same as substrate |
| CN101321807A (en) * | 2005-12-05 | 2008-12-10 | 可隆株式会社 | Polyimide film |
| CN101062984A (en) * | 2006-04-28 | 2007-10-31 | 宋成根 | Processing technique of super heat-proof polyimide film |
| CN101168598A (en) * | 2007-10-08 | 2008-04-30 | 江阴市云达电子新材料有限公司 | Method for preparing ultra-thick polyimide film with high heat conductivity and low thermal expansion coefficient |
| CN101798463A (en) * | 2010-03-26 | 2010-08-11 | 上海缘达聚合材料有限公司 | High-performance polyimide film and preparation method thereof |
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| 顾宜、赵炜、刘向阳.酰亚胺化工艺对BTDA-m-PDA型聚酰亚胺聚集态结构的影响.《四川大学学报(工程科学版)》.2005,第37卷(第5期),第88-92页. * |
| 高强度聚酰亚胺的合成与性能表征;黄超伯、张和安、彭信文等;《高分子材料科学与工程》;20070731;第23卷(第4期);第40-43页 * |
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Owner name: HANGZHOU NORMAL UNIVERSITY Effective date: 20150114 |
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Effective date of registration: 20150114 Address after: 214000, Jinshan four branch 11, photoelectric new material science and technology zone, Beitang District, Jiangsu, Wuxi Applicant after: Wuxi Shunxuan New Material Co., Ltd. Applicant after: Hangzhou Normal University Address before: 214000, Jinshan four branch 11, photoelectric new material science and technology zone, Beitang District, Jiangsu, Wuxi Applicant before: Wuxi Shunxuan New Material Co., Ltd. |
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