CN101323672A - Corona-resistant polyimide film and preparing method thereof - Google Patents

Corona-resistant polyimide film and preparing method thereof Download PDF

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Publication number
CN101323672A
CN101323672A CNA2007100243215A CN200710024321A CN101323672A CN 101323672 A CN101323672 A CN 101323672A CN A2007100243215 A CNA2007100243215 A CN A2007100243215A CN 200710024321 A CN200710024321 A CN 200710024321A CN 101323672 A CN101323672 A CN 101323672A
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corona
metal oxide
polyimide film
diamino
resistant polyimide
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CN101323672B (en
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朱艾成
许惠麟
郭振报
聂伟民
朱浩
杨广生
孙志荣
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JIANGSU BINGCHENG ELECTRIC MATERIAL CO Ltd
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JIANGSU BINGCHENG ELECTRIC MATERIAL CO Ltd
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Abstract

The invention relates to a polyimide film with corona resistance, which essentially comprises pyromellitic dianhydride, 4,4' diaminodiphenylether and nanoscale metallic oxide; wherein, the particle size of the nanoscale metallic oxide is less than or equal to 50 nanometers. By adopting the technical proposal, the invention has the advantages as follows: as nanophase materials are adopted by the invention and the nanoscale metallic oxide and N, N' dimethylacetamide are prepared into stable and uniform suspended substance in a high-speed shear disperser, the product adopting the polyimide film with corona resistance produced in the invention has excellent performance of corona resistance, good production technology and high rate of finished products.

Description

A kind of corona-resistant polyimide film and preparation method thereof
Technical field
The present invention relates to a kind of chemical preparations, specifically a kind of corona-resistant polyimide film and preparation method thereof.
Background technology
Domestic research to corona-resistant polyimide film also is in the testing laboratory of colleges and universities or institute and does some exploratory theoretical investigationes, is far from reaching the level of suitability for industrialized production.And the du pont company corona-resistant polyimide film is analyzed, we think that it is good not enough at corona-resistance property.
Summary of the invention
Deficiency at above the invention provides corona-resistant polyimide film and preparation method thereof, has good corona-resistance property, and manufacture craft is good simultaneously, the yield rate height.
In order to reach above purpose, the present invention by the following technical solutions, a kind of corona-resistant polyimide film, it mainly comprises pyromellitic acid anhydride, 4.4 ' diamino-diphenyl ether and nanosize metal oxide, the particle diameter of affiliated nanosize metal oxide≤50 nanometers.
Of the present inventionly further be optimized for: a kind of corona-resistant polyimide film, described metal oxide are one or more in titanium dioxide, aluminium sesquioxide and the silicon-dioxide.
The making method of above-mentioned corona-resistant polyimide film is as follows:
A) the polyimide acid solution is made---and at reactor and solution N, N ' N,N-DIMETHYLACETAMIDE uniform mixing adds the reaction of 4.4 ' diamino-diphenyl ether then and generates the polyimide acid solution with pyromellitic acid anhydride;
B) suspensoid is made---and with nanosize metal oxide (comprise in titanium dioxide, aluminium sesquioxide and the silicon-dioxide one or more) and N, N ' N,N-DIMETHYLACETAMIDE is made the stabilized uniform suspensoid in the high speed shear decollator;
C) stirring---the suspensoid that polyimide acid solution that the A step is made and B step are made joins in the mixing kettle, utilizes ultrasonic drilling machine, stirs;
D) hydrostomia---the uniform mixing liquid that the C step is made joins hydrostomia in the slobbering machine;
E) oven dry---will remove solvent N through the article of D step hydrostomia gained, N ' N,N-DIMETHYLACETAMIDE is dried film forming then in the hot air circulation drying room;
F) imidization is handled---and will carry out the imidization processing through the article that the oven dry of E step makes and make corona-resistant polyimide film.
Because the present invention adopts above technical scheme, the present invention has the following advantages: because the present invention has adopted nano material, simultaneously in the high speed shear decollator with nanosize metal oxide and N, N ' N,N-DIMETHYLACETAMIDE is made the stabilized uniform suspensoid, so product has good corona-resistance property with the corona-resistant polyimide film that the present invention makes, manufacture craft is good simultaneously, the yield rate height.
Embodiment
The invention will be further described below in conjunction with embodiment
Embodiment one
It mainly comprises pyromellitic acid anhydride, 4.4 ' diamino-diphenyl ether and nanosize metal oxide, the particle diameter of affiliated nanosize metal oxide≤50 nanometers.Described metal oxide titanium dioxide (also can be aluminium sesquioxide or silicon-dioxide, also can be two kinds or three kinds mixture among the three).The proportioning of each component is: pyromellitic acid anhydride and 4.4 ' diamino-diphenyl ether 1: 1 in molar ratio are 1 with the weight of pyromellitic acid anhydride and 4.4 ' diamino-diphenyl ether mixture, and nanosize metal oxide then is 4%.
The making method of above-mentioned corona-resistant polyimide film is as follows:
G) the polyimide acid solution is made---and at reactor and solution N, N ' N,N-DIMETHYLACETAMIDE uniform mixing adds the reaction of 4.4 ' diamino-diphenyl ether then and generates the polyimide acid solution with pyromellitic acid anhydride;
H) suspensoid is made---and with nanosize metal oxide (comprise in titanium dioxide, aluminium sesquioxide and the silicon-dioxide one or more) and N, N ' N,N-DIMETHYLACETAMIDE is made stabilized uniform suspensoid (adding tensio-active agent and suspension agent in the making) in the high speed shear decollator;
I) stirring---the suspensoid that polyimide acid solution that the A step is made and B step are made joins in the mixing kettle, utilizes ultrasonic drilling machine, stirs;
J) hydrostomia---the uniform mixing liquid that the C step is made joins hydrostomia in the slobbering machine;
K) oven dry---will remove solvent N through the article of D step hydrostomia gained, N ' N,N-DIMETHYLACETAMIDE is dried in the hot air circulation drying room then, forms film;
L) imidization is handled---and will carry out the imidization processing through the article that the oven dry of E step makes and make corona-resistant polyimide film.
Embodiment two
With a kind of corona-resistant polyimide film of embodiment one, its difference is, is 1 with the weight of pyromellitic acid anhydride and 4.4 ' diamino-diphenyl ether mixture, and nanosize metal oxide then is 8%.
Embodiment three
With a kind of corona-resistant polyimide film of embodiment one, its difference is, is 1 with the weight of pyromellitic acid anhydride and 4.4 ' diamino-diphenyl ether mixture, and nanosize metal oxide then is 12%.
Embodiment four
With a kind of corona-resistant polyimide film of embodiment one, its difference is, is 1 with the weight of pyromellitic acid anhydride and 4.4 ' diamino-diphenyl ether mixture, and nanosize metal oxide then is 16%.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop in the protection domain of requirement of the present invention.

Claims (4)

1, a kind of corona-resistant polyimide film, it mainly comprises pyromellitic acid anhydride, 4.4 ' diamino-diphenyl ether and nanosize metal oxide, the particle diameter of affiliated nanosize metal oxide≤50 nanometers.
2, a kind of corona-resistant polyimide film according to claim 1 is characterized in that: described metal oxide is one or more in titanium dioxide, aluminium sesquioxide and the silicon-dioxide.
3, a kind of corona-resistant polyimide film according to claim 2, it is characterized in that: the proportioning of described pyromellitic acid anhydride, 4.4 ' diamino-diphenyl ether and nanosize metal oxide each component is, pyromellitic acid anhydride and 4.4 ' diamino-diphenyl ether 1: 1 in molar ratio, weight with pyromellitic acid anhydride and 4.4 ' diamino-diphenyl ether mixture is 1, and nanosize metal oxide then is 4-16%.
4, a kind of making method of corona-resistant polyimide film is:
A) the polyimide acid solution is made---and at reactor and solution N, N ' N,N-DIMETHYLACETAMIDE uniform mixing adds the reaction of 4.4 ' diamino-diphenyl ether then and generates the polyimide acid solution with pyromellitic acid anhydride;
B) suspensoid is made---in the high speed shear decollator with nanosize metal oxide and N, N ' N,N-DIMETHYLACETAMIDE is made the stabilized uniform suspensoid, and described nanosize metal oxide comprises one or more in titanium dioxide, aluminium sesquioxide and the silicon-dioxide;
C) stirring---the suspensoid that polyimide acid solution that the A step is made and B step are made joins in the mixing kettle, utilizes ultrasonic drilling machine, stirs;
D) hydrostomia---the uniform mixing liquid that the C step is made joins hydrostomia in the slobbering machine;
E) oven dry---will remove solvent N through the article of D step hydrostomia gained, N ' N,N-DIMETHYLACETAMIDE is dried film forming then in the hot air circulation drying room;
F) imidization is handled---and will carry out the imidization processing through the article that the oven dry of E step makes and make corona-resistant polyimide film.
CN2007100243215A 2007-06-13 2007-06-13 Corona-resistant polyimide film and preparing method thereof Active CN101323672B (en)

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Application Number Priority Date Filing Date Title
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102161828A (en) * 2011-03-01 2011-08-24 天津市天缘电工材料有限责任公司 Corona-resistance polyimide film and manufacturing method thereof
CN102490426A (en) * 2011-11-25 2012-06-13 桂林电器科学研究院 Corona resistance polyimide thin film and preparation method thereof
CN101735716B (en) * 2009-11-24 2013-11-27 丹阳四达化工有限公司 Method for preparing corona-resistant wire enamel
CN107652679A (en) * 2017-09-29 2018-02-02 安徽国风塑业股份有限公司 A kind of Inverter fed motor PI films and preparation method thereof
CN107936249A (en) * 2017-12-07 2018-04-20 黑龙江科技大学 A kind of titanium dioxide nano thread and the dielectric preparation method of polyimides composite Nano
CN110734643A (en) * 2018-10-29 2020-01-31 嘉兴学院 Preparation method of rare earth doped modified polyimide film
CN113943484A (en) * 2021-10-28 2022-01-18 苏州太湖电工新材料股份有限公司 Polyimide composite material, composite film and preparation method thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1197902C (en) * 2003-04-11 2005-04-20 上海市合成树脂研究所 Polyimide material filled with nano zinc oxide
CN1949098A (en) * 2006-09-11 2007-04-18 天津市奥维工贸有限公司 Base pipe prepared by using modified polyimide film as raw material and preparation process thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101735716B (en) * 2009-11-24 2013-11-27 丹阳四达化工有限公司 Method for preparing corona-resistant wire enamel
CN102161828A (en) * 2011-03-01 2011-08-24 天津市天缘电工材料有限责任公司 Corona-resistance polyimide film and manufacturing method thereof
CN102161828B (en) * 2011-03-01 2014-07-09 天津市天缘电工材料有限责任公司 Corona-resistance polyimide film and manufacturing method thereof
CN102490426A (en) * 2011-11-25 2012-06-13 桂林电器科学研究院 Corona resistance polyimide thin film and preparation method thereof
CN107652679A (en) * 2017-09-29 2018-02-02 安徽国风塑业股份有限公司 A kind of Inverter fed motor PI films and preparation method thereof
CN107936249A (en) * 2017-12-07 2018-04-20 黑龙江科技大学 A kind of titanium dioxide nano thread and the dielectric preparation method of polyimides composite Nano
CN110734643A (en) * 2018-10-29 2020-01-31 嘉兴学院 Preparation method of rare earth doped modified polyimide film
CN110734643B (en) * 2018-10-29 2022-03-25 嘉兴学院 Preparation method of rare earth doped modified polyimide film
CN113943484A (en) * 2021-10-28 2022-01-18 苏州太湖电工新材料股份有限公司 Polyimide composite material, composite film and preparation method thereof

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Address after: 225402 Taixing City, Jiangsu province Wang Zhen Yao Wang Road Industrial Zone, Taizhou

Patentee after: Jiangsu Bingcheng Electrical Material Co., Ltd.

Address before: 212323, No. 9, South Main Street, Danyang, Jiangsu

Patentee before: Jiangsu Bingcheng Electrical Material Co., Ltd.