Process for the continuous preparation of polyamidoamines

A polyamide and ethylenediamine technology, applied in the field of functional polymer preparation, can solve the problems of intermittent operation, separation and purification, and low product purity, and achieve the effects of preventing side reactions, easy operation, and high purity

Inactive Publication Date: 2016-01-20
XIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a continuous preparation method of polyamide-amine, which solves the problems of low product purity, separation and purification, and batch operation in the prior art

Method used

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  • Process for the continuous preparation of polyamidoamines
  • Process for the continuous preparation of polyamidoamines
  • Process for the continuous preparation of polyamidoamines

Examples

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preparation example Construction

[0028] The preparation method of the semi-generation polyamide-amine product: dissolve ethylenediamine with methanol, add methyl acrylate under inert gas conditions to obtain it; the reaction temperature is a combination of low and high temperature, that is, react at 0°C for 1-2h, then naturally Raise the temperature to 25°C and react for 13-14 hours; in the early stage of the reaction, the function of the inert gas is to exclude oxygen, and in the late stage of the reaction, the main function is to blow away excessive small molecular substances.

[0029] The specific operation steps are:

[0030] Step 1. Dissolve ethylenediamine in methanol, add a catalyst, place the obtained mixed solution in an ice-water bath, pass through nitrogen and exhaust oxygen, add methyl acrylate dropwise under stirring conditions, raise the temperature to make the reaction complete, and obtain half-generation Polyamide-amine product; the rate of dropping methyl acrylate is 8-16d / min; the molar rati...

Embodiment 1

[0035] A synthetic method for preparing highly purified 1.0 generation polyamide-amine, comprising the following steps:

[0036] Step 1, synthetic 0.5 generation polyamide-amine, its concrete steps are:

[0037] Step 1a, weighing 4.5g (0.075mol) of ethylenediamine and 51.6g (0.6mol) of methyl acrylate, the molar ratio of the two is 1:8;

[0038] Step 1b. Put the ethylenediamine weighed in step 1a into a 250 mL three-necked flask, add 20 mL of methanol and 0.05 g of sodium methoxide catalyst, and stir to completely dissolve it. Then it was placed in a water bath, cooled to 0°C in an ice-water bath, and nitrogen was passed through to exhaust oxygen for 10 min.

[0039] Step 1c, under the conditions of rapid stirring and nitrogen protection, keep the reaction temperature of the system at 0°C, add the methyl acrylate weighed in step 1a dropwise, the dropping speed is 16d / min, and the dropping time is about 1h.

[0040] Step 1d, after the dropwise addition, continue to react at 0...

Embodiment 2

[0050] A synthetic method for preparing highly purified 1.0 generation polyamide-amine, comprising the following steps:

[0051] Step 1, synthetic 0.5 generation polyamide-amine, its concrete steps are:

[0052] Step 1a, weighing 4.5g (0.075mol) of ethylenediamine and 77.4g (0.9mol) of methyl acrylate, the molar ratio of the two is 1:12;

[0053] Step 1b. Put the ethylenediamine weighed in step 1a into a 250 mL three-necked flask, add 25 mL of methanol and 0.2 g of sodium ethoxide catalyst, and stir to completely dissolve it. Then it was placed in a water bath, cooled to 0°C in an ice-water bath, and nitrogen was passed through to exhaust oxygen for 10 min.

[0054] Step 1c, under the conditions of rapid stirring and nitrogen protection, keep the reaction temperature of the system at 0°C, add the methyl acrylate weighed in step 1a dropwise, the dropping speed is 8d / min, and the dropping time is about 2h.

[0055] Step 1d, after the dropwise addition, continue to react at 0°C...

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Abstract

The continuous preparation method of polyamide-amine, dissolving ethylenediamine in methanol, feeding inert gas, adding methyl acrylate under stirring conditions, stirring to make the reaction complete, and obtaining a half-generation polyamide-amine product; dissolving it , Add ethylenediamine under the condition of stirring and inert gas to obtain the whole-generation polyamide-amine product. The present invention adopts a continuous operation mode, and does not need to go through the process of product exporting to the reactor, entering the column chromatography or vacuum distillation device for separation and purification, product weighing calculation, importing into the reactor, etc., which is simple and time-saving; the reaction temperature of the present invention adopts a combination of low and high temperature. It can prevent the occurrence of side reactions, improve the purity of the product, and enable it to fully react, reduce the reaction time, and increase the output. The first-generation polyamide-amine prepared by the method of the invention has high purity, does not need separation and purification, lays a good foundation for subsequent preparation of high-generation dendrimers, and is easy to operate. It solves the problem that high-generation polyamide-amine macromolecules cannot be separated due to similar structures.

Description

technical field [0001] The invention belongs to the technical field of functional polymer preparation, and in particular relates to a continuous preparation method of polyamide-amine. Background technique [0002] Since the first synthesis of polyamidoamines by Tomalia et al. in 1985 [0003] (poly(amido-amine), PAMAM) dendrimers have the characteristics of high geometric symmetry, precise molecular structure, a large number of functional groups, cavities in the molecule and controllable molecular chain growth. , can be used as surfactants, catalysts, membrane materials, nanomaterials, flocculants, and drug carriers, etc., so it has important application prospects in the fields of industry, agriculture, national defense, environmental protection, life sciences, and medicine. One of the hot spots of scientific research. [0004] Polyamide-amine dendrimers are composed of three parts: initiating core, repeating branching units radially connected to the core, and external sur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/10C07C231/02
Inventor 苏洁程文马国营余中马霞王敏
Owner XIAN UNIV OF TECH
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