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Preparation method of hyperbranched polyimide with adjustable branching degree

A technology of polyimide and degree of branching, applied in the field of synthesis of hyperbranched polymers, can solve the problems of difficult synthesis and easy gel generation, so as to avoid the formation of gel, reduce production cost and increase monomer concentration Effect

Inactive Publication Date: 2013-09-11
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But AB 2 type monomer is difficult to synthesize, and A 2 +B 3 Although the polymerization of monomers has the advantages of easy preparation and structure modification, it is necessary to strictly control the molar ratio of the monomers, the order of addition and the rate of addition, otherwise gels are likely to occur, and this method can only obtain two kinds of branches with a certain degree of branching. hyperbranched polyimide

Method used

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  • Preparation method of hyperbranched polyimide with adjustable branching degree
  • Preparation method of hyperbranched polyimide with adjustable branching degree

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add 2.5g of 2,4,6-triaminopyrimidine (TAP) and 50g of N,N-dimethylacetamide (DMAc) into a completely dry 150mL straight four-necked flask equipped with a water separator, At 25°C, with mechanical stirring and N 2 Under protection, 8.88 g of hexafluorodianhydride (6FDA) monomer was added after stirring for 5 minutes, and the bottle wall was washed with 14.5 g of DMAc. The stirring reaction was continued for 48h.

[0023] (2) The temperature of the above solution was raised to 160° C., 20 g of xylene was added, reacted for 6 hours, and the water generated during the imidization process was removed by azeotroping of xylene and water.

[0024] (3) After cooling to room temperature, the above solution was poured into ethanol, washed with ethanol, filtered three times, and vacuum-dried at 150°C for 6 hours to obtain a hyperbranched polyimide with a branching degree of 34%.

Embodiment 2

[0026] (1) Add 2.0833g TAP and 50g DMAc to a completely dry 150mL straight four-neck flask equipped with a water separator, and add 2.0833g TAP and 50g DMAc at 25°C, mechanical stirring and N 2 Under protection, 8.88g of 6FDA monomer was added after stirring for 5 minutes, and the bottle wall was washed with 12.1g of DMAc. The stirring reaction was continued for 48h.

[0027] (2) The temperature of the above solution was raised to 160° C., 20 g of xylene was added, reacted for 6 hours, and the water generated during the imidization process was removed by azeotroping of xylene and water.

[0028] (3) After cooling to room temperature, the above solution was poured into ethanol, washed with ethanol, filtered three times, and vacuum-dried at 150°C for 6 hours to obtain a hyperbranched polyimide with a branching degree of 42%.

Embodiment 3

[0030] (1) Add 1.7857g TAP and 45g DMAc to a completely dry 150mL straight four-neck flask equipped with a water trap, and add 1.7857g TAP and 45g DMAc at 25°C, mechanical stirring and N 2 Under protection, 8.88g of 6FDA monomer was added after stirring for 5 minutes, and the bottle wall was washed with 15.4g of DMAc. The stirring reaction was continued for 48h.

[0031] (2) The temperature of the above solution was raised to 160° C., 20 g of xylene was added, reacted for 6 hours, and the water generated during the imidization process was removed by azeotroping of xylene and water.

[0032] (3) After cooling to room temperature, the above solution was poured into ethanol, washed with ethanol, filtered three times, and vacuum-dried at 150°C for 6 hours to obtain a hyperbranched polyimide with a branching degree of 53%.

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Abstract

The invention relates to a preparation method of hyperbranched polyimide with an adjustable branching degree. The method comprises the following steps of: performing condensation polymerization on a binary anhydride A2-type monomer and a tertiary amine B'B2-type monomer in different mole ratios in a highly-polar aprotic solvent at the room temperature, thereby obtaining a hyperbranched polyamide acid solution; rising the temperature; adding an azeotropic dehydrating agent into the heated hyperbranched polyamide acid solution and aminating with imide; and filtering, washing and drying, thereby obtaining the hyperbranched polyimide with the different branching degrees. In the preparation process of the hyperbranched polyimide, gel is not generated, so that the monomer concentration is improved; the production cost is lowered; and the branching degree and the terminal group of the hyperbranched polyimide are controlled and adjusted. Therefore, the mass production of the hyperbranched polyimide can be realized; and a new application prospect for the hyperbranched polyimide in the newly-developing field is exploited.

Description

technical field [0001] The invention belongs to the synthesis field of hyperbranched polymers, in particular to a method for preparing hyperbranched polyimides with adjustable branching degree. Background technique [0002] In 1952, Flory first proposed the concept of hyperbranched polymers. In 1990, Kim and Webster et al. (Kim Y H, Wester O W.J.Am.Chem.Soc.1990,112,4592-4593.) used bromophenylboronic acid as a monomer The first highly branched polymer was prepared, which set off a wave of research on hyperbranched polymers. This type of polymer has a three-dimensional spherical structure, and there are a large number of terminal functional groups on the periphery of the sphere. The lower chain entanglement and peripheral distribution of functional groups of hyperbranched polymers can make them have extremely high functional activity, good solubility and low melt viscosity, so they have attracted widespread attention from the scientific and industrial circles. . Polyimide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
Inventor 张秋禹陈营雷星锋姚盼张和鹏孙婉露
Owner NORTHWESTERN POLYTECHNICAL UNIV
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