Polyamide-imide containing alicyclic group and preparation method of polyamide-imide

A polyamide and imide technology, applied in the field of functional polymer materials, can solve the problems of limiting the application of polyimide, high thermal expansion of polyimide, and high molecular chain strength, and achieve good light transmittance and solubility. , good mechanical properties and heat resistance, simple operation effect

Active Publication Date: 2021-09-03
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the traditional polyimide containing benzene ring, imide ring and other groups, the molecular chain strength is high, the interaction is strong, the degree of conjugation is high, and the molecular chain is densely packed, which makes polyimide insoluble in common Organic solvents, difficult to melt at high temperature, difficult to process, limiting its scope of use
At the same time, due to the existence of the conjugated structure, the electron-withdrawing dianhydride and the electron-donating diamine in the polyimide are easy to form a charge transfer complex in the molecule and between the molecules, which leads to a decrease in the light transmittance of the polyimide. It is brown or brownish yellow, and polyimide has high thermal expansion, which is difficult to meet the packaging requirements, which seriously limits the application of polyimide in the field of flexible optoelectronic devices and solar cells

Method used

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  • Polyamide-imide containing alicyclic group and preparation method of polyamide-imide
  • Polyamide-imide containing alicyclic group and preparation method of polyamide-imide
  • Polyamide-imide containing alicyclic group and preparation method of polyamide-imide

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preparation example Construction

[0039] Further, a preparation method of polyamide-imide containing alicyclic group, the specific operation steps are as follows:

[0040] (2.1), the synthesized NCHABA and TFDB are added into a three-necked flask according to a certain molar ratio, then a solvent is added, nitrogen gas is passed, and magnetic stirring is carried out under an ice bath to obtain a mixed diamine solution;

[0041] (2.2), adding the dianhydride monomer: 6FDA into the obtained mixed diamine solution three times, after the dianhydride monomer is completely dissolved, continue to react for 24 hours at room temperature, thereby obtaining a polyamic acid solution;

[0042] (2.3), then pour the obtained polyamic acid solution into the glass tank, place it in a vacuum oven and carry out temperature programming, thereby obtaining polyamide-imide;

[0043] (2.4), finally stripping the obtained polyamide-imide from the glass tank to finally obtain film-like polyamide-imide containing alicyclic groups.

[0...

Embodiment 1

[0057] In a 500ml three-necked flask equipped with a nitrogen inlet and magnetic stirring, add 29.69g (0.16mol) p-nitrobenzoyl chloride, 42.66g (0.32mol) anhydrous aluminum trichloride and 350ml N,N-dimethylethyl Amide (DMAc) solution, ice bath, after magnetic stirring for half an hour, add 9.13g (0.08mol) trans-1,4-cyclohexanediamine solution dissolved in 50ml DMAc with a syringe, react in ice bath for 5h, then continue to react at room temperature 24h; after the reaction is over, pour the reaction solution into 500ml deionized water for precipitation, filter to obtain a filter cake, wash with deionized water and ethanol, and dry in vacuum for 12h to obtain N,N'-(cyclohexane-1,4- Diyl) bis(4-nitrobenzamide); Weigh 4.12g (0.01mol) of the dinitro compound synthesized above, 35ml DMAc and place it in a 250ml three-neck flask equipped with a condenser tube and nitrogen inlet, add 0.124g (3wt%) Pd / C is used as catalyzer; Under 120 ℃ of magnetic agitation, slowly drip 15ml hydrazin...

Embodiment 2

[0060] In a 500ml three-necked flask equipped with a nitrogen inlet and magnetic stirring, add 29.69g (0.16mol) p-nitrobenzoyl chloride, 42.66g (0.32mol) anhydrous aluminum trichloride and 350ml N,N-dimethylethyl Amide (DMAc) solution, ice bath, after magnetic stirring for half an hour, add 9.13g (0.08mol) trans-1,4-cyclohexanediamine solution dissolved in 50ml DMAc with a syringe, react in ice bath for 5h, then continue to react at room temperature 24h; after the reaction is over, pour the reaction solution into 500ml deionized water for precipitation, filter to obtain a filter cake, wash with deionized water and ethanol, and dry in vacuum for 12h to obtain N,N'-(cyclohexane-1,4- Diyl) bis(4-nitrobenzamide); Weigh 4.12g (0.01mol) of the dinitro compound synthesized above, 35ml DMAc and place it in a 250ml three-neck flask equipped with a condenser tube and nitrogen inlet, add 0.124g (3wt%) Pd / C is used as catalyzer; Under 120 ℃ of magnetic agitation, slowly drip 15ml hydrazin...

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Abstract

The invention discloses polyamide-imide containing an alicyclic group and a preparation method of the polyamide-imide, and belongs to the field of functional polymer materials. According to the invention, a diamine monomer N, N '-(cyclohexane-1, 4-diyl) bis (4-aminobenzamide) (NCHABA) containing an alicyclic group and an amido bond is synthesized, the NCHABA containing the alicyclic group and the amido bond and 2, 2'-bis (trifluoromethyl) diaminobiphenyl (TFDB) containing a trifluoromethyl structure are mixed according to different molar ratios to serve as a diamine monomer, hexafluorodianhydride (6FDA) serves as a dianhydride monomer, and a polyamide-imide film containing the alicyclic group is prepared by a two-step method. The alicyclic group-containing polyamide-imide disclosed by the invention has excellent light transmission, relatively high glass transition temperature and outstanding mechanical properties, and can be used for manufacturing a flexible display substrate.

Description

technical field [0001] The invention belongs to the field of functional polymer materials, and relates to a polyamide-imide containing an alicyclic group, a preparation method thereof, and applications in various fields. Background technique [0002] Due to its good heat resistance, solvent resistance, chemical stability and mechanical properties, polyimide has outstanding comprehensive performance and is widely used in aerospace, nuclear industry, microelectronics and other fields. However, due to the traditional polyimide containing benzene ring, imide ring and other groups, the molecular chain strength is high, the interaction is strong, the degree of conjugation is high, and the molecular chain is densely packed, which makes polyimide insoluble in common Organic solvents are difficult to melt at high temperature and difficult to process, which limits its scope of use. At the same time, due to the existence of the conjugated structure, the electron-withdrawing dianhydrid...

Claims

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Application Information

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IPC IPC(8): C08G73/14C08J5/18C08L79/08
CPCC08G73/14C08J5/18C08J2379/08
Inventor 林保平李志强孙莹张雪勤杨洪
Owner SOUTHEAST UNIV
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