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Preparation method of soluble, colorless, transparent and low-thermal-expansion-coefficient polyamide imide film

A polyamideimide, low thermal expansion coefficient technology, applied in the field of soluble colorless transparent low thermal expansion polyamideimide film preparation, can solve the problem of low glass transition temperature, poor temperature resistance, high heat resistance, etc. problems, to achieve excellent mechanical properties and dimensional stability, reduce intermolecular forces, and increase the effect of free volume

Inactive Publication Date: 2015-11-04
INST OF OPTICS & ELECTRONICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the usual polyimide film is brownish-yellow and insoluble in solvents, while the thermal expansion coefficient of colorless polyimide is extremely high, and the glass transition temperature of most soluble polyimides is very low, and the temperature resistance is poor.
Therefore, although colorless and transparent soluble polyimide has been studied in the past, a polyimide film with certain mechanical properties and a preparation method with extremely low thermal expansion coefficient and high heat resistance are still unknown. have public
The low thermal expansion coefficient and excellent coating solubility described in the published patent document 1 (Fujii Mari, Iwamoto Tomori, Hasegawa Yasutoshi. Polyamide-imide solution and polyamide-imide film. Chinese invention patent, 201280018593.3) Polyamide-imide films are prepared by two methods: the first method is to directly mix fluorine-containing diamine monomers and chlorinated trimellitic anhydride monomers for polycondensation to obtain polyamide-imide solutions and corresponding films. According to the data, the thermal expansion coefficients are all around 15ppm / °C, and the test temperature range is wider and even reaches 20ppm / °C, which does not match the thermal expansion coefficient of inorganic materials, and the optical properties and mechanical properties of the film are not disclosed. Performance data; the second method in Document 1 first obtained the dianhydride monomer containing amide group through complex preparation and purification process, and then obtained the polyamide-imide solution by condensation reaction with the fluorine-containing diamine monomer And film, although public data shows that a lower coefficient of thermal expansion has been obtained, but the preparation process is too cumbersome, and the optical properties and mechanical properties of the film are not disclosed
Publication patent document 2 (Hu Guoyi, Wu Jianhua, Li Yuling. Preparation method of colorless and transparent polyimide film. Chinese invention patent, 201210119407.7) discloses a method for synthesizing polyimide by hydrogenated trimellitic anhydride. The disclosed polyimide Amines have a low coefficient of thermal expansion (about 17ppm / °C) and can be dissolved in aprotic polar solvents; The film does not have high temperature resistance and loses the advantages of aromatic polyimide

Method used

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  • Preparation method of soluble, colorless, transparent and low-thermal-expansion-coefficient polyamide imide film
  • Preparation method of soluble, colorless, transparent and low-thermal-expansion-coefficient polyamide imide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] a) Weigh 2.4g of TFBZ into 7.5ml DMAc, stir and dissolve at room temperature;

[0028]b) Put it in an ice-water bath, after 15 minutes, add 1.89ml of TMSCl, 1.2ml of pyridine and 0.183g of 4-dimethylaminopyridine (DMAP), and stir at room temperature for 15 minutes;

[0029] c) After cooling down in an ice-water bath for 15 minutes, quickly add 1.578 g of TMAC, then add 7.5 ml of DMAC, stir in an ice-water bath at 0°C for 15 minutes, and then stir overnight at room temperature;

[0030] d) After overnight, if the viscosity of the glue is too high, add 7.5ml of DMAc and stir to reduce the viscosity, then add 0.765ml of acetic anhydride and 0.591ml of pyridine mixture, and stir at room temperature for 6h;

[0031] e) After cooling to room temperature, slowly pour the glue solution into 2-propanol to wash and filter for 2 to 4 times;

[0032] f) heat up to 50°C in an oven for 3 hours, and then dissolve it with 60ml of DMAc to obtain a polyamide-imide glue;

[0033] g) Coa...

Embodiment 2

[0036] The implementation method of this example is basically the same as that of Example 1, except that the aprotic polar solvent used is NMP (N-methylpyrrolidone).

[0037] a) Weigh 2.4g of TFBZ into 7.5ml of NMP, stir and dissolve at room temperature;

[0038] b) Put it in an ice-water bath, after 15 minutes, add 1.89ml of TMSCl, 1.2ml of pyridine and 0.183g of 4-dimethylaminopyridine (DMAP), and stir at room temperature for 15 minutes;

[0039] c) After cooling down in an ice-water bath for 15 minutes, quickly add 1.578 g of TMAC, then add 7.5 ml of NMP, stir in an ice-water bath at 0°C for 15 minutes, and then stir overnight at room temperature;

[0040] d) After overnight, if the viscosity of the glue is too high, add 7.5ml of NMP and stir to reduce the viscosity, then add 0.765ml of acetic anhydride and 0.591ml of pyridine mixture, and stir at room temperature for 6 hours;

[0041] e) After cooling to room temperature, slowly pour the glue solution into methanol to was...

Embodiment 3

[0046] The implementation method of this example is basically the same as that of Example 1, except that 1.2 g of TFBZ is firstly added in step a, and then the remaining 1.2 g is added before overnight stirring in step c.

[0047] a) Weigh 1.2g of TFBZ into 7.5ml DMAC, stir and dissolve at room temperature;

[0048] b) Put it in an ice-water bath, after 15 minutes, add 1.89ml of TMSCl, 1.2ml of pyridine and 0.183g of 4-dimethylaminopyridine (DMAP), and stir at room temperature for 15 minutes;

[0049] c) After cooling down in an ice-water bath for 15 minutes, quickly add 1.578g of TMAC, then add 7.5ml of DMAC, stir in an ice-water bath at 0°C for 15 minutes, then add 1.2g of TFBZ, and then stir overnight at room temperature;

[0050] d) After overnight, if the viscosity of the glue is too high, add 7.5ml of DMAC and stir to reduce the viscosity, then add 0.765ml of acetic anhydride and 0.591ml of pyridine mixture, and stir at room temperature for 6 hours;

[0051] e) After co...

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Abstract

The invention discloses a preparation method of a soluble, colorless, transparent and low-thermal-expansion-coefficient polyamide imide film. According to the prepared film, fluorine-containing diamine monomers serve as diamine monomers, trimellitic anhydride acid chloride serves as anhydride monomers, and the polyamide imide film is further prepared through a trimethylchlorosilane activation mechanism under a simple and moderate synthesis condition. The prepared polyamide imide film has high dimensional stability (the CTE is 5-15 ppm / DEG C or so) and good temperature resistance (Tg is 300 DEG C or so), the transmittance of visible light wavebands is 90% or so, the prepared polyamide imide film can be dissolved in an aprotic polar solvent and is convenient to machine and process, and the comprehensive performance of the prepared polyamide imide film meets the material performance requirement of a part of devices in the microelectronics and optoelectronics field.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of a soluble colorless transparent polyamide-imide film with low thermal expansion coefficient. Background technique [0002] More and more organic polymers such as polymethyl methacrylate (PMMA), polystyrene (PS) and polycarbonate (PC) are used as optical devices due to their excellent optical transparency, realizing the realization of optical devices. Thin film, light weight, flexible. However, the temperature resistance and dimensional stability of general-purpose polymer materials have become performance shortcomings, limiting their use in higher temperature and more precise application backgrounds. High temperature-resistant transparent materials refer to transparent materials that can withstand processing above 250°C. They are mainly used for flexible solar cell backplanes, ITO backplanes for liquid crystal displays to replace fra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/14C08L79/08C08J5/18
Inventor 王松刘习奎杨伟吴时彬任戈
Owner INST OF OPTICS & ELECTRONICS - CHINESE ACAD OF SCI
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