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Preparation method of dendritic cationic polyion liquid

A polyionic liquid and cationic technology, applied in the field of materials, can solve the problems of cumbersome separation and purification steps, restrictions on the preparation and application of dendrimers, harsh reaction conditions, etc., and achieve simple separation and purification of products, clear and controllable structures, fast response effect

Active Publication Date: 2021-05-11
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the preparation process of these dendritic polymers, there are generally characteristics such as the need for group protection-deprotection, harsh reaction conditions, and cumbersome separation and purification steps, which limit the preparation and application of dendritic polymers.

Method used

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  • Preparation method of dendritic cationic polyion liquid
  • Preparation method of dendritic cationic polyion liquid
  • Preparation method of dendritic cationic polyion liquid

Examples

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Embodiment 1

[0024] The invention discloses a preparation method of a dendritic cationic polyionic liquid, comprising the following steps:

[0025] (1) Prepare the monomer compound of dendritic polyionic liquid:

[0026] (1.1) The precursor bis(dimethylamino)-propanol (2NMeOH) of synthetic monomeric compound, synthetic route is as follows:

[0027]

[0028] The specific experimental steps are as follows: in a 250mL flask, successively add 1,3-dichloropropanol (26g, 0.2mol), a concentration of 40% dimethylamine aqueous solution (112g, 1mol) and 0.2g potassium iodide, at 40°C Heated to reflux for 6 hours. After the reaction, extracted with dichloromethane (100mL×3), dried over anhydrous magnesium sulfate, and removed the solvent dichloromethane to obtain 16.1g of bis(dimethylamino)-propanol (2NMeOH). It is a colorless liquid with a yield of 55.1%.

[0029] (1.2) The precursor bis(dimethylamino)-chloroalkane hydrochloride (2NMeCl) of synthetic monomeric compound, synthetic route is as fo...

Embodiment 2

[0047] The present embodiment provides a kind of preparation method of dendritic cationic polyionic liquid, comprises the following steps:

[0048] (1) Under the action of potassium iodide catalyst, mix 1,3-dibromopropanol with methanol solution of dimethylamine, the molar ratio of 1,3-dibromopropanol to dimethylamine is 1:1, in Reflux at 80°C for 4 hours, extract with dichloromethane, dry over anhydrous magnesium sulfate, and remove the solvent dichloromethane to obtain a colorless liquid of bis(dimethylamino)-propanol; add thionyl chloride dropwise to the In bis(dimethylamino)-propanol, the molar ratio of bis(dimethylamino)-propanol to thionyl chloride is 1:1, react at 50°C for 4 hours to obtain bis(dimethylamino) )-chloroalkane hydrochloride; the bis(dimethylamino)-chloroalkane hydrochloric acid is made into a saline solution with a concentration of 0.05g / mL and mixed with sodium azide, and reacted at 60°C for 30 hours to obtain Prepare the monomer compound of the dendriti...

Embodiment 3

[0052] The present embodiment provides a kind of preparation method of dendritic cationic polyionic liquid, comprises the following steps:

[0053] (1) Under the action of potassium iodide catalyst, mix 1,3-dichloropropanol and dimethylamine at a molar ratio of 1:7, react at 80°C for 4 hours, extract with dichloromethane, and dry over anhydrous magnesium sulfate , after removing solvent dichloromethane, obtain two (dimethylamino)-propanol colorless liquids; Thionyl chloride is added dropwise in the two (dimethylamino)-propanol, described two (dimethylamino) The molar ratio of -propanol to thionyl chloride is 1:4, react at 50°C for 8 hours to obtain bis(dimethylamino)-chloroalkane hydrochloride; the bis(dimethylamino)- Chloroalkane hydrochloric acid is formulated into a saline solution with a concentration of 0.5g / mL and mixed with sodium azide, and reacted at 90°C for 12 hours to obtain a monomer compound for preparing a dendritic polyionic liquid; the potassium iodide catalys...

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Abstract

The invention discloses a preparation method of a dendritic cationic polyion liquid, and belongs to the technical field of high polymer materials, the method comprises the following steps: firstly synthesizing a polyfunctional compound with azide and tertiary amino as a monomer, then respectively carrying out a copper catalyzed azide-alkyne cycloaddition reaction (CuAAC) and a Menshutkin reaction on the monomer and brominated propyne to obtain the dendritic polyion liquid by adopting a gradual growth mode. The preparation method provided by the invention has the advantages of mild reaction conditions and high efficiency, the target product can be obtained only through simple precipitation in the post-reaction treatment method, and the operation is simple. The dendritic polyion liquid has potential application value in the fields of biological medicines, functional materials and the like.

Description

technical field [0001] The invention belongs to the technical field of materials, and relates to a method for preparing a dendritic cationic polyionic liquid, in particular to a method for alternately carrying out a copper-catalyzed azide-alkyne cycloaddition reaction (CuAAC) and a Menshutkin reaction. A method for preparing dendritic cationic polyionic liquids. Background technique [0002] Polyionic liquids are a class of ionic polymers containing anionic and cationic groups in their structure, and have the characteristics of both ionic liquids and polymers. Due to their unique physical and chemical properties, they are becoming a new class of widely used materials. . The synthesis of polyionic liquids can usually be achieved by free radical polymerization of ionic liquid monomers, or the polymer can be ionized first to obtain polyionic liquids, and it can also be functionalized to make polyionic liquids in It is widely used in different fields such as polymer chemistry,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/04
CPCC07D249/04
Inventor 高超高正国赵博
Owner ZHEJIANG UNIV