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Preparation method of polyamide-amine dendritic compound

A technology of amine dendrimers and polyamides, which is applied in the field of preparation of polyamide-amine dendrimers, can solve problems such as waste of raw materials, influence on product purity, and incomplete separation of products, and achieve high yield and high purity.

Active Publication Date: 2014-01-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, in the existing preparation process, the molar ratio of MA to PAMAM end groups is greatly excessive (usually greater than 8:1), and the molar ratio of EDA to PAMAM end groups is greatly excessive (usually greater than 24:1), which not only causes waste of raw materials, but also Lead to incomplete separation of later products, affecting product purity

Method used

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  • Preparation method of polyamide-amine dendritic compound
  • Preparation method of polyamide-amine dendritic compound

Examples

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Embodiment 1

[0016] Preparation of semi-algebraic PAMAM G0.5. Take a certain amount of MA methanol solution in a three-necked flask, and a certain amount of EDA methanol solution in a constant pressure dropping funnel. One side of the three-necked flask is connected to a constant pressure dropping funnel, and the other side is connected to a mercury thermometer. Connect a spherical condenser, where the molar ratio of MA to EDA end groups is 3:1. The three-neck flask was placed in a constant temperature water bath, and the EDA solution was added dropwise at a water bath temperature of 20±2°C with stirring. After 24 hours of reaction, the water bath temperature was 40±1°C, the condensation temperature was -8 ~ -15°C, and the vacuum degree was 80KPa. distilled. When the condensate is obviously reduced, the temperature of the distilled water bath is 46±1°C, and the vacuum degree is 98KPa to continue the vacuum distillation to remove the residual methanol and MA. The finally obtained light yel...

Embodiment 2

[0018] Preparation of semi-algebraic PAMAM G0.5. Take a certain amount of MA methanol solution in a three-necked flask, and a certain amount of EDA methanol solution in a constant pressure dropping funnel. One side of the three-necked flask is connected to a constant pressure dropping funnel, and the other side is connected to a mercury thermometer. Connect a spherical condenser, where the molar ratio of MA to EDA end groups is 1.5:1. The three-neck flask was placed in a constant temperature water bath, and the EDA solution was added dropwise at a water bath temperature of 22±2°C with stirring. After 24 hours of reaction, the water bath temperature was 40±1°C, the condensation temperature was -13 to -18°C, and the vacuum degree was 85KPa. distilled. When the condensate is significantly reduced, the temperature of the distilled water bath is 56±1°C, and the vacuum is 100KPa to continue vacuum distillation to remove residual methanol and MA. The final light yellow product is th...

Embodiment 3

[0020] Preparation of Integer Algebraic PAMAM G1.0. Take a certain amount of methanol solution of EDA in a three-necked flask, a certain amount of methanol solution of PAMAM G0.5 in a constant pressure dropping funnel, one side of the three-necked flask is connected to a constant pressure dropping funnel, and the other side is connected to a mercury thermometer , the middle port is connected with a spherical condenser, and the molar ratio of EDA to PAMAM G0.5 end group is 4:1. The three-neck flask was placed in a constant temperature water bath, and PAMAM G0.5 solution was added dropwise at a water bath temperature of 25±2°C with stirring. After 24 hours of reaction, the water bath temperature was 56±1°C, the condensation temperature was -10 to -15°C, and the vacuum degree was 90KPa. Distill under reduced pressure. When the condensate is significantly reduced, the temperature of the distilled water bath is 68±1°C, and the vacuum distillation is continued at 100KPa to remove t...

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Abstract

The invention relates to a preparation method of a polyamide-amine dendritic compound. According to the preparation method, ethanediamine and methyl acrylate are used as initial raw materials, wherein during Michael addition reaction, the mole ratio of methyl acrylate to the base number of to-be-prepared semi-algebraic polyamide-amine ends is (1.5-3):1, and during amidation reaction, the mole ratio of ethanediamine to the base number of to-be-prepared integral-algebraic polyamide-amine ends is (4-6):1. The preparation method disclosed by the invention can be used for optimizing the mole ratios of the base numbers of EDA, MA and PAMAM ends and operating parameters of reduced pressure distillation and simply and conveniently preparing the high-yield and high-purity polyamide-amine dendritic compound, and can be widely applied to the fields of macromolecular materials, gas separation or purification and the like.

Description

technical field [0001] The invention relates to a preparation method of polyamide-amine dendrons, belonging to the fields of polymer materials, gas separation or purification, and the like. Background technique [0002] Dendrimers are a new type of polymers with three-dimensional molecular structure, highly branched and highly ordered, and are a research hotspot in the science of polymer preparation. Since the molecular structure of dendrimers can be precisely controlled by molecular design, there are a large number of terminal functional groups that can be modified or loaded with other substances outside the molecule, and there are hydrophobic cavities that can wrap small molecular compounds inside, and are wrapped under certain conditions. Small molecular compounds can be released again. Therefore, dendrimers have attracted extensive research in nanomaterials, drug release, gene delivery, catalyst supports, etc. Polyamidoamine (PAMAM) is a dendritic compound that has bee...

Claims

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Application Information

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IPC IPC(8): C08G83/00
Inventor 周志斌毛松柏朱道平余勇杨绪甲
Owner CHINA PETROLEUM & CHEM CORP
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