Green synthesis process of polyamide-dendritic amine polymer

A technology for green synthesis and polyamide, applied in the field of green synthesis technology, can solve the problems of complex treatment of recycled liquid, large environmental pollution, and high energy consumption, and achieve the effects of reducing the original investment of equipment, simplifying the process flow, and reducing reaction by-products.

Inactive Publication Date: 2009-05-27
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This separation method has the problems of complex treatment of recovered liquid, high energy consumption, and great environmental pollution.

Method used

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  • Green synthesis process of polyamide-dendritic amine polymer
  • Green synthesis process of polyamide-dendritic amine polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Synthesis of half-generation 0.5G PAMAM. The ratio of the amount of MA to 0.5G PAMAM terminal group is 5:1, and the sample is synthesized. Add 6.0g (0.1mol) EDA and 64.0g (2.0mol) MeOH to a 500ml round bottom flask, cool to 0°C with ice water, then slowly add 172.2g (2.0mol) MA which was cooled to the round bottom flask. After 24 hours of magnetic stirring at 23±2°C, at 50°C, the excess raw material MA and the solvent MeOH were separated and recovered by rotary evaporation, and the rotary evaporation adopted staged decompression. The recovered liquids under low vacuum and high vacuum were collected, weighed, and analyzed by GC. The condensation temperature of vacuum distillation is -10°C. 197.8 g of recovered liquid was obtained under low vacuum, the recovery rate was 98.0%, and the MA% was 66.3%, about 131.1 g. The yield of 0.5G PAMAM is 98.6%, and the purity is 98.1%. The whole process was carried out under the protection of high-purity nitrogen.

[0023] 197.8 g...

Embodiment 2

[0025] Synthesis of half-generation 0.5G PAMAM. The ratio of the amount of MA to 0.5G PAMAM terminal group is 8:1, and the sample is synthesized. Add 3.0g (0.05mol) EDA and 50.1g (1.6mol) MeOH to a 500ml round-bottomed flask, cool to 0°C with ice water, then slowly add cooled 137.8g (1.6mol) MA into the round-bottomed flask. After magnetically stirring at 23±2°C for 24h, at 50°C, the excess raw material MA and solvent MeOH were separated and recovered by rotary evaporation, and the rotary evaporation adopted staged decompression. The recovered liquids under low vacuum and high vacuum were collected, weighed, and analyzed by GC. The condensation temperature of vacuum distillation is -10°C. 168.0 g of recovered liquid was obtained under low vacuum, the recovery rate was 97.8%, and the MA% was 84.6%, about 116.8 g. The yield of 0.5G PAMAM is 98.3%, and the purity is 98.3%. The whole process was carried out under the protection of high-purity nitrogen.

[0026] 168.0 g of rec...

Embodiment 3

[0028] Synthesis of half-generation 0.5G PAMAM. The ratio of the amount of MA to 0.5G PAMAM terminal group is 6.5:1 and the sample is synthesized. Add 3.0g (0.05mol) EDA and 41.6g (1.30mol) MeOH to a 500ml round bottom flask, cool to 0°C with ice water, then slowly add 111.9g (1.30mol) MA which was cooled to the round bottom flask. After magnetically stirring at 23±2°C for 24h, at 50°C, the excess raw material MA and solvent MeOH were separated and recovered by rotary evaporation, and the rotary evaporation adopted staged decompression. The recovered liquids under low vacuum and high vacuum were collected, weighed, and analyzed by GC. The condensation temperature of vacuum distillation is -10°C. 133.0 g of recovered liquid was obtained under low vacuum, with a recovery rate of 97.6%, wherein MA% was 69.0%, about 91.8 g. The yield of 0.5G PAMAM is 98.6%, and the purity is 98.1%. The whole process was carried out under the protection of high-purity nitrogen.

[0029] 133.0 ...

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Abstract

The green synthesis process of dendritic polyamide-amine (PAMAM) polymer has material methyl acrylate (MA0 and ethylene diamine (EDA) in such amount that the ratio of MA or EDA to PAMAM end group matter is 5-8. The present invention has increased material amount to result in decreased reaction side product, raised purity of destination product, no polymerization in synthesizing high algebraic PAMAM and improved product quality. The present invention has high liquid recovering rate, less pollution, simplified technological process, low synthesis cost, low equipment cost and low power consumption, and reaches the aim of green production.

Description

technical field [0001] The invention relates to a synthesis process of polyamide-amine dendrimer, in particular to a green synthesis process with low energy consumption and low pollution. Background technique [0002] Polyamide-amine (PAMAM) dendritic polymer is a new type of polymer with unique structure and excellent properties, and its research is very active in many fields such as life science, environment, energy, medicine, new materials, analytical chemistry, etc. . At present, when PAMAM is synthesized in the laboratory, the raw material reagents methyl acrylate (MA) and ethylenediamine (EDA) are synthesized in a large excess, wherein the ratio of the amount of MA, EDA to the number of end groups of PAMAM is 4:1 . This synthesis process has many by-products and the problem of low purity of the target product, especially in the synthesis of high algebraic PAMAM, there is a phenomenon of molecular polymerization, which not only seriously affects the quality and perfor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/34
Inventor 曾云龙黄玉芳贺超才
Owner HUNAN UNIV OF SCI & TECH
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