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Modified multi-component copolymerized arylamine and preparation method and application thereof

A multi-component copolyaramide and a technology for copolyaramide, applied in the field of polyaramid, can solve the problems of complex preparation and the like

Active Publication Date: 2018-11-13
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of the polymer must also contain a certain amount of free carboxyl-substituted diamine monomers, and the preparation is relatively complicated

Method used

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  • Modified multi-component copolymerized arylamine and preparation method and application thereof
  • Modified multi-component copolymerized arylamine and preparation method and application thereof
  • Modified multi-component copolymerized arylamine and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0098] Embodiment 1 synthesizes Ar 1-3,10％ T 90％ Ar 2-1,30％ Ar 3-4,70％

[0099] Prepared by low temperature polycondensation method.

[0100] Mix 0.0252g (0.1mmol) of 2,3-naphthaloyl dichloride, 0.183g (0.9mmol) of terephthaloyl chloride with 0.0320g (0.3mmol) of p-phenylenediamine, 0.244g (0.7mmol) of 9,9-bis (4-Aminophenyl)fluorene was mixed in 5 mL of NMP-LiCl (the mass concentration of LiCl was 4%), stirred in an ice bath for 0.5 hours, then the ice bath was removed, and the reaction was continued at 15° C. for 0.5 hours. The reaction solution was poured into 200 mL of methanol, and washed with 200 mL of 100° C. hot water to obtain a white precipitate.

[0101] The polymer was characterized by GPC, and a single peak was obtained, indicating that the polymerization was carried out very efficiently, with a number average molecular weight of 62,000 and a dispersion of 1.87. The polymer has very good solubility properties and can be dissolved in organic solvents such as ...

Embodiment 2

[0102] Example 2 Synthesis of Ar 1-1,50％ T 50％ Ar 3-4,100％

[0103] Prepared by low temperature polycondensation method.

[0104] Mix 0.126 g (0.5 mmol) of 2,6-naphthaloyl dichloride, 0.102 g (0.5 mmol) of terephthaloyl dichloride and 0.349 g (1 mmol) of 9,9-bis(4-aminophenyl)fluorene in 5 mL of NMP - LiCl (the mass concentration of LiCl is 4%), stirred in ice bath for 0.5 hour, then removed the ice bath, and continued to react at 40° C. for 4 hours. The reaction solution was poured into 200 mL of methanol, and washed with 200 mL of 100° C. hot water to obtain a white precipitate.

[0105] The polymer was characterized by GPC, and a single peak was obtained, indicating that the polymerization was carried out very efficiently, with a number average molecular weight of 79,000 and a dispersion of 1.65. The polymer has very good solubility properties and can be dissolved in organic solvents such as NMP, DMSO, DMAc, NMP-LiCl or DMF-LiCl. The thermal properties of the polymer ...

Embodiment 3

[0106] Embodiment 3 synthetic Ar 1-2,10％ T 90％ Ar 2-1,30％ Ar 3-4,70％

[0107] Prepared by low temperature polycondensation method.

[0108] Mix 0.0252g (0.1mmol) 1,4-naphthaloyl dichloride, 0.183g (0.9mmol) terephthaloyl chloride with 0.0320g (0.3mmol) p-phenylenediamine, 0.244g (0.7mmol) 9,9-bis (4-Aminophenyl)fluorene was mixed in 5 mL of NMP-LiCl (the mass concentration of LiCl was 4%), stirred in an ice bath for 0.5 hours, then the ice bath was removed, and the reaction was continued in a 60°C oil bath for 48 hours. The reaction solution was poured into 200 mL of methanol, and washed with 200 mL of 100° C. hot water to obtain a flocculent white precipitate.

[0109] figure 1 Ar for example 3 1-2,10％ T 90％ Ar 2-1,30％ Ar 3-4,70％ The GPC spectrum. It can be seen from the figure that the polymer was characterized by GPC, and a single peak was obtained, indicating that the polymerization was carried out very efficiently, with a number average molecular weight of 81,0...

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Abstract

The invention discloses modified multi-component copolymerized arylamine and a preparation method and application thereof. The polymer is obtained by solution copolymerization of naphthyl-containing aromatic diacid chloride (or aromatic dioctyl phthalate) and aromatic diamine monomer. All monomers can be directly purchased commercially, the preparation method is simple and convenient, and industrialization is facilitated. The prepared polymer can be dissolved in organic solvents such as NMP, DMSO, DMAc, NMP-LiCl or DMF-LiCl and the like, 5% thermal decomposition temperature in air can reach 450 DEG C or above, and a glass-transition temperature can range from 270 DEG C to 320 DEG C. The polymer can be prepared into thin films, fibers, hollow tubes, strip-shaped objects and the like. The tensile strength of the thin films prepared from the polymer can reach 60 MPa or above, the highest tensile modulus can reach 4 GPa, and the maximum breaking elongation can reach 11%. The obtained thinfilm has transparency and fluorescence. The material is expected to be applied to the fields of military, transportation, optics and the like.

Description

technical field [0001] The invention belongs to the technical field of polyarylamide, and in particular relates to a modified multi-component polyarylamide and its preparation method and application. Background technique [0002] Polyamide is a general term for polymers containing amide groups in the repeating unit of the macromolecular main chain. Polyamides can be prepared by ring-opening polymerization of lactams, or by polycondensation of dibasic amines and dibasic acids. Polyamide has good comprehensive properties, including mechanical properties, heat resistance, wear resistance, chemical resistance and self-lubrication, and has a low coefficient of friction, has a certain flame retardancy, is easy to process, and is suitable for glass fiber And other fillers to enhance the modification to improve performance and expand the scope of application. According to the different comonomers, polyamides can be divided into polyarylamides and aliphatic polyamides. Compared wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32C08G69/28C08J5/18D01F6/80B29C55/12C08L77/10B29L7/00
CPCD01F6/805C08G69/28C08G69/32C08J5/18B29C55/12C08J2377/10B29L2007/00
Inventor 周胜张小莉沈志豪赵宁范星河周其凤徐坚
Owner INST OF CHEM CHINESE ACAD OF SCI
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