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Process for high-efficiency synthesis of super branched polyester-amine

A high-efficiency technology for hyperbranched polyester, applied in the field of high-efficiency synthesis of hyperbranched polyester-amine, can solve the problems of restricting the research and application of hyperbranched polymers, complicated synthesis steps, low yield, etc., and achieves separation and purification of operation and products. Simple, mature method, high reaction yield effect

Inactive Publication Date: 2004-12-29
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

AB reported in the literature above x Most of the monomers need to be synthesized separately, the synthesis steps are complicated, and the yield is low, which has become a bottleneck restricting the research and application of hyperbranched polymers.

Method used

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  • Process for high-efficiency synthesis of super branched polyester-amine
  • Process for high-efficiency synthesis of super branched polyester-amine

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preparation example Construction

[0009] The invention is a method for efficiently synthesizing hyperbranched polyester-amine. Firstly, the monomer N-(2-acetoxyethyl)-N-(1' , 3'-dicarboxybenzoyl) amine, and the monomer is prepared into hyperbranched polyester-amine by catalyzed and heated polyester reaction. Its synthetic method comprises following three steps:

[0010] 1). Synthesis of N-(2-hydroxyethyl)-N-(1',3'-dicarboxybenzoyl)amine: 1,2,4-trimesic anhydride with a molar ratio of 1:1 to 1.2 and ethanolamine were dissolved in absolute ethanol, respectively. Place the ethanol solution of ethanolamine in a three-necked flask with a stirring device, slowly add the ethanol solution of 1,2,4-trimesic anhydride to the three-necked flask with a constant pressure dropping funnel, and use ice to A water bath controls the temperature of the system to reduce side reactions. After the dropwise addition was completed, the reaction was stirred at room temperature for 1h to 4h. A colorless solution was obtained, and ...

Embodiment 1

[0014] Dissolve 3.3ml (110mmol) of ethanolamine in 30ml of absolute ethanol, and add it into a three-neck flask equipped with stirring. Put it on an ice-water bath, dissolve 9.6g (100mmol) of 1,2,4-benzenetricarboxylic anhydride in 30ml of absolute ethanol, put it in a constant pressure dropping funnel, and slowly drop it into the flask for about 30min. Finish. The ice-water bath was removed, and stirring was continued at room temperature for 2 h. A colorless solution was obtained, and the ethanol was removed by rotary evaporation, and vacuumized in a vacuum oven at 60°C to obtain a white solid crude product, which was washed twice with deionized water and dried to obtain 10.5 g of the monomer product of the first step, and the yield was 90%. The melting point was determined to be 204.3°C by DSC. Proton magnetic spectrum ( 1 H-NMR) result (ppm) is as follows: 8.0~8.5 (ph-H, 3H), 3.6 (-CH 2 -, 4H).

[0015] 10.5 g of the product obtained above was placed in a conical flas...

Embodiment 2

[0018] Except that the vacuuming reaction time in the polymerization reaction was changed to 4 h, other synthesis processes were the same as in Example 1, the yield was 83%, and the Tg of the polymer as determined by DSC was 161° C.

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Abstract

An efficient process for synthesizing the ultrabranched polyester-amine includes aminolysis of acid anhydride, acetylizing hydroxy to obtain nanometer N-(2-acetoxyethyl)-N-(1,3'-dicarboxy benzoyl) amine, putting it along with catalyst in reaction tube, heating reaction in N2 atmosphere, vacuumizing, and cooling. Its advantages are simple process and high yield.

Description

technical field [0001] The invention belongs to the technical scope of polymer material preparation, in particular to a method for efficiently synthesizing hyperbranched polyester-amine through a simple synthesis route. Background technique [0002] At the end of the 1980s, during the research process of using dendritic polymers as rheology modifiers and macromolecular initiators, Kim of DuPont Co., Ltd. considered that the synthesis of dendritic polymers was too difficult and cumbersome. developed by AB 2 A method for synthesizing hyperbranched polymers such as polyphenylene in one step from a type monomer. Surprisingly, these polymers have excellent solubility properties and can be used as rheology modifiers. Since then, hyperbranched polymers have become one of the hot spots in polymer science research in the past ten years. In the following patents: US.5587441, US.5587446, US.5663260, report in SE.92005644, hyperbranched polymer is usually made of AB x Type (x ≥ 2) mo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/685
Inventor 唐黎明付志伟
Owner TSINGHUA UNIV
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