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

A hyperbranched polymerization and high-efficiency technology, which is applied in the field of high-efficiency synthesis of hyperbranched polyester-amines, can solve the problems of complex synthesis steps, low yield, and restrictions on the research and application of hyperbranched polymers, and achieve mature methods and high reaction yields. High, simple operation and product separation and purification

Inactive Publication Date: 2003-03-12
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0009] The present invention is a method for efficiently synthesizing hyperbranched polyester-amine. First, trimellitic anhydride, ethanolamine, and acetic anhydride are synthesized by simple anhydride amidation reaction and hydroxyl acetylation reaction to synthesize monomer N-(2-acetoxyethyl)-N-(1' , 3'-dicarboxybenzoyl) amine, the monomer is prepared into hyperbranched polyester-amine by the polyester reaction method of catalysis and heating. The synthesis method includes the following three steps:

[0010] 1). Synthesis of N-(2-hydroxyethyl)-N-(1',3'-dicarboxybenzoyl)amine: Trimellitic anhydride with a molar ratio of 1:1 to 1.2 Ethanol and ethanolamine were dissolved in an appropriate amount of absolute ethanol. Place the ethanol solution of ethanolamine in a three-necked flask with a stirring device, use a constant pressure dropping funnel to slowly drop the ethanol solution of trimellitic anhydride into the three-necked flask, and use ice during the dropping process. Water b...

Embodiment 1

[0014] Dissolve 3.3ml (110mmol) of ethanolamine in 30ml of absolute ethanol and add it to a stirred three-necked flask. Place on an ice-water bath, dissolve 9.6g (100mmol) trimellitic anhydride in 30ml of absolute ethanol, place it in a constant pressure dropping funnel, and slowly add dropwise to the flask for about 30min. Finish. Remove the ice-water bath, continue to stir and react for 2h at room temperature. Obtain a colorless solution, remove the solvent ethanol by rotary evaporation, vacuum in a vacuum oven at 60°C to obtain a white solid crude product, wash twice with deionized water, and dry to obtain 10.5 g of the monomer product of the first step, with a yield Is 90%. The melting point determined by DSC was 204.3°C. Hydrogen nuclear magnetic spectrum ( 1 H-NMR) results (ppm) are 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 an Erlenmeyer flask. Under a water bath at 80°C, 8.5ml (89mmol) of acetic anhydride wa...

Embodiment 2

[0018] Except that the vacuum reaction time in the polymerization reaction was changed to 4h, the other synthesis process was the same as in Example 1, the yield was 83%, and the Tg of the polymer measured 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, and particularly relates to a method for efficiently synthesizing hyperbranched polyester-amine through a simple and convenient synthesis route. Background technique [0002] In the late 1980s, Kim and others of DuPont were conducting research on dendrimers as rheology modifiers and macroinitiators. They considered that the synthesis of dendrimers was too difficult and cumbersome. Developed by AB 2 A method for synthesizing hyperbranched polymers such as polyphenylene monomer in one step. Surprisingly, these polymers have excellent solubility properties and can be used as rheology modifiers. Since then, hyperbranched polymers have become one of the hotspots of polymer science research in the past decade. It is reported in the following patents: US.5587441, US.5587446, US.5663260, SE.92005644 that hyperbranched polymers are usually made by AB x Type (x≥2) monomer is obtained by one...

Claims

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Application Information

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IPC IPC(8): C08G63/685
Inventor 唐黎明付志伟
Owner TSINGHUA UNIV
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