Preparation method for colorless transparent high-temperature-resistant polyimide nanometer composite film

A polyimide and nanocomposite technology, which is applied in the field of preparation of colorless, transparent and high temperature resistant polyimide nanocomposite films, can solve the problems of low thermal expansion coefficient, unmentioned film transmittance and glass transition temperature, etc. , to achieve the effect of high light transmittance, good optical performance and high dimensional stability

Active Publication Date: 2016-03-30
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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  • Abstract
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  • Application Information

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Problems solved by technology

The silicon dioxide filling rate of the film reaches 30%, and has good mechanical properties and low thermal expansion coefficient, but the light transmittance and glass transition temperature of the film are not mentioned in the patent

Method used

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  • Preparation method for colorless transparent high-temperature-resistant polyimide nanometer composite film
  • Preparation method for colorless transparent high-temperature-resistant polyimide nanometer composite film
  • Preparation method for colorless transparent high-temperature-resistant polyimide nanometer composite film

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preparation example Construction

[0033] A method for preparing a colorless, transparent, high-temperature-resistant polyimide nanocomposite film, comprising:

[0034] (1) Reaction of 4,4-bicyclohexyl dicarboxylic acid chloride (BCCL) and hexafluoromethylbenzidinediamine (TFDB) in an organic solvent to obtain a semi-aromatic fluorinated diamine precursor ADB (such as figure 1 shown);

[0035] The semi-aromatic fluorinated diamine precursor ADB structural formula is:

[0036]

[0037] (2) The semi-aromatic fluorinated diamine precursor ADB is mixed with hexafluoromethylbenzidine diamine (TFDB), 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA), 3,3, 4,4-biphenyldianhydride (BPDA) monomer copolymerization; or the semi-aromatic fluorinated diamine precursor ADB and hexafluoromethylbenzidinediamine (TFDB), 4,4'-(hexafluoroiso Propylene) diphthalic anhydride (6FDA), hydrogenated 3,3,4,4-biphenyl dianhydride (HBPDA) monomer copolymerization to obtain polyamic acid PAA1 precursor;

[0038] (3) reacting ...

Embodiment 1

[0055] Put 32.0g of hexafluoromethylbenzidinediamine (TFDB), 8.7g of pyridine and 800ml of dimethylacetamide (DMAc) into the reaction flask at room temperature, stir well to make it dissolve completely, then slowly add 14.0g of 4,4-bicyclohexyl dicarboxylic acid chloride, and the mixed solution was maintained under nitrogen protection for 4 hours. After the reaction is finished, pour the mixed solution into 8L of 10% sodium chloride solution, stand at 0°C for 12 hours, wash and filter with water to obtain a white powder, dry the powder at 90°C for 9 hours under the protection of nitrogen to obtain the ADB front body with a yield of about 94%.

[0056] Under the condition of nitrogen protection, 9g of ADB precursor and 100ml of N-methylpyrrolidone were added into the reaction flask, stirred thoroughly at 80°C, and then 6.2g of hexafluoromethylbenzidinediamine (TFDB) was added after the ADB monomer was completely dissolved. Then the reaction temperature was lowered to 20°C, and...

Embodiment 2

[0060] Under the condition of nitrogen protection, 9g of ADB precursor and 100ml of N-methylpyrrolidone were added into the reaction flask, stirred thoroughly at 80°C, and then 6.2g of hexafluoromethylbenzidinediamine (TFDB) was added after the ADB monomer was completely dissolved. Then the reaction temperature was lowered to 20°C, and then 1.5 g of 4,4'-(hexafluoroisopropene) diphthalic anhydride (6FDA) and 9.0 g of hydrogenated 3,3,4,4-biphenyl dianhydride (HBPDA) were added slowly Into the above mixed solution containing ADB and TFDB. The reaction was maintained at 20° C. for 48 hours, and after the reaction was completed, 20 wt % of an anhydride-terminated polyamic acid solution PAA1 precursor was obtained. Subsequently, 1.3ml of silane coupling agent 3, aminotrimethoxysilane (APTMS) was slowly added to the above-mentioned polyamic acid solution precursor and maintained for reaction for 6 hours, and the polyamic acid PAA2 terminated by the silane coupling agent was obtaine...

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Abstract

The invention discloses a preparation method for a colorless transparent high-temperature-resistant polyimide nanometer composite film, which belongs to the field of polymeric materials. The preparation method comprises the following steps: reacting 4,4-biscyclohexyl diformyl chloride (BCCL) with hexafluorobenzidine (TFDB) so as to prepare semi-aromatic fluorodiamine precursor; then subjecting the precursor, TFDB, 4,4'-(hexafluoroisopropenyl)diphthalic acid anhydride (6FDA) and hydrogenated 3,3,4,4-biphenyl dianhydride (HBPDA) to copolymerization so as to prepare polyamide acid precursor; grafting the polyamide acid precursor to a silane coupling agent in situ and carrying out aging and hydrolysis in a mixed solution of tetramethoxysilane (TMOS) and tetraethoxysilane (TEOS) so as to obtain a polyamide acid/silica mixed solution; and subjecting the mixed solution to tape casting and drying so as to obtain a polyimide/SiO2 composite film.

Description

technical field [0001] The invention relates to the technical field of polyimide and its preparation, in particular to a method for preparing a colorless, transparent, high-temperature-resistant polyimide nanocomposite film. Background technique [0002] With the rapid development of optoelectronic technology, the field of optoelectronic devices has shown the development trend of intelligence, light weight, ultra-thin and flexible in recent years. The key to realizing this function is to obtain a transparent film material with light weight, flexibility and superior comprehensive performance. Due to its hard and brittle characteristics, traditional glass substrate materials cannot meet the needs of future flexible packaging technology. Polymer film materials have the characteristics of light weight, flexibility, good transparency, and excellent comprehensive performance, which can well meet the requirements of flexible optoelectronic device substrates, and flexible transpare...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08K3/36C08J5/18C08L79/08
CPCC08G73/1057C08G73/106C08J5/18C08J2379/08C08K3/36C08K2201/011C08L2201/08C08L2201/10C08L2203/16
Inventor 杨木泉张洪峰颜悦厉蕾
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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