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A kind of preparation method of branched polyethyleneimine

A technology of branched polyethyleneimine and polyethyleneimine, which is applied in the field of synthesis of cationic polymer compound polyethyleneimine, can solve problems such as unfavorable environmental protection, achieve simple steps, mild reaction conditions, and be conducive to industrial production Effect

Active Publication Date: 2021-12-07
HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aziridine is obtained from ethanolamine through a two- to three-step reaction. In the process of preparing aziridine monomer, a large amount of concentrated sulfuric acid, sodium hydroxide or hydrochloric acid gas, thionyl chloride and other strong acids and alkalis and strong corrosion are required. Sexual substances, not conducive to environmental protection

Method used

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  • A kind of preparation method of branched polyethyleneimine
  • A kind of preparation method of branched polyethyleneimine
  • A kind of preparation method of branched polyethyleneimine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Add 60mL of distilled water and 31.797g (0.3mol) of anhydrous sodium carbonate to a round bottom flask, after fully dissolving, add 18.03g (0.3mol) of ethylenediamine and 29.688g (0.3mol) of 1,2-diamine Ethyl chloride, under the condition of mechanical stirring, the reaction temperature is first raised to 50°C, reacted for 3 hours at 50°C, continued to adjust the reaction temperature to 70°C, reacted for 3 hours at 70°C, continued to increase the reaction temperature, The reaction solution was reacted under reflux for 30 hours. After the reaction, the reaction solution was cooled to room temperature, and the supernatant was filtered out after standing still. The solid in the reaction bottle was fully washed with 200mL of absolute ethanol three times, the washing solution and the supernatant were combined, and the liquid was distilled off under reduced pressure to obtain a yellow viscous liquid.

[0024] The obtained yellow viscous liquid was 19.53g, and the rotatio...

Embodiment 2

[0026] With example 1, reactant mol ratio remains unchanged, in step (1), 1,2-dichloroethane is changed into 12-dibromoethane, gained pale yellow viscous liquid 10.85g, and the reaction time is 72 hours, The rotational viscosity is 910mPa s; the ratio of the three amines in polyethyleneimine is calculated to be 1°(NH 2 ):2°(NH):3°(N)=0.31:0.36:0.33( figure 2 ), wherein the proportion of tertiary amines is 33%, indicating that polyethyleneimine is branched polyethyleneimine.

Embodiment 3

[0028] Same as Example 1, change the amount of ethylenediamine to 14.424g (0.24mol) in step 1, and the resulting light yellow viscous liquid is , with a viscosity of 4150mPa s; calculate the proportions of the three amines in polyethyleneimine according to the carbon spectrum integral is 1°(NH 2 ):2°(NH):3°(N)=0.27:0.40:0.33( image 3 ), wherein the proportion of tertiary amines is 33%, indicating that polyethyleneimine is branched polyethyleneimine.

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Abstract

The invention belongs to the field of polymer synthesis and relates to the synthesis of cationic polymer compound polyethyleneimine. The method uses ethylenediamine and 1,2-dihalogenated ethane as raw materials to synthesize polyethyleneimine in one step through polycondensation reaction in aqueous solution under weak alkaline conditions. The polyethyleneimine synthesized by this method has a viscosity ranging from 900 mPa·s to 15000 mPa·s, and its structure is determined to be branched polyethyleneimine through carbon spectrum characterization. 13 The ratio of primary amine, secondary amine and tertiary amine in PEI was calculated by C NMR integral method. The synthesized branched polyethyleneimine is suitable for gene transfection, water treatment and other fields.

Description

technical field [0001] The invention relates to the synthesis of cationic polymer compound polyethyleneimine, which belongs to the field of polymer synthesis. Background technique [0002] Polyethyleneimine (PEI) is a water-soluble polymer compound whose structural unit is CH 2 CH 2 N, every two carbon atoms has a nitrogen atom that can be protonated, and it is the cationic organic polymer with the highest charge density known so far. The large number of amine groups contained in the polyethyleneimine structure makes it have the characteristics of high cationicity, high adsorption and high reactivity. At present, PEI has been applied in self-assembled membranes, separation, purification and immobilization of biological macromolecules, adsorption and separation of metal ions, construction of pH and biosensors, gene transfection, drug release and other fields. [0003] The synthesis of PEI is the basis for the wide application of PEI in various fields. There are two types o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/02
CPCC08G73/0213
Inventor 曹金丽张彦昌王冬梅赵献增李天仚谢亚雄殷园园
Owner HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI