A kind of preparation method of amino-terminated polymer

An amino-terminated polymer and free radical technology, which can be used in the preparation of organic compounds, the preparation of carboxylic acid amides, chemical instruments and methods, etc. High reactivity, convenient synthesis and purification, and good dispersibility

Inactive Publication Date: 2018-07-24
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Due to the existence of chain transfer and chain termination processes, traditional free radical polymerization has poor control over the molecular weight, polydispersity, and terminal structure of polymers, which limits its wide application.

Method used

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  • A kind of preparation method of amino-terminated polymer
  • A kind of preparation method of amino-terminated polymer
  • A kind of preparation method of amino-terminated polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1, the preparation of ATRP initiator is as follows:

[0023] (1) Dissolve 1g of p-nitroaniline and 2g of triethylamine in 50mL of dichloromethane and place in a 150mL single-necked round bottom flask at room temperature for 1h;

[0024] (2) 2g of 2-bromoisobutyryl bromide was dissolved in 5mL of dichloromethane, added dropwise into the reaction vessel in step (1), and stirred at room temperature for 24h;

[0025] (3) until the reaction is finished, the reaction solution is suction filtered to remove triethylamine hydrochloride, and the filtrate passes through a silica gel column to obtain the initiator, and its structural formula is as follows:

[0026]

[0027] Its NMR spectrum is as figure 1 shown.

[0028] 2. The preparation of the amino-terminated polymer (taking polymethyl methacrylate as an example) is as follows:

[0029] (1) In a schlenk tube, the initiator (0.053g, 1.850×10 -4 mol), methyl methacrylate (0.463g, 4.625×10 -3 mol), 2-2 bipyridine (0.087g, ...

Embodiment 2

[0032] 1, the preparation of ATRP initiator is as follows:

[0033] (1) Dissolve 1.5g of p-nitroaniline and 2.5g of triethylamine in 50mL of dichloromethane and place in a 150mL single-necked round bottom flask at room temperature for 1.5h;

[0034] (2) 3g of 2-bromoisobutyryl bromide was dissolved in 10mL of dichloromethane, added dropwise into the reaction vessel in step (1), and stirred at room temperature for 24h;

[0035] (3) After the reaction is completed, the reaction solution is suction-filtered to remove triethylamine hydrochloride, and the filtrate is passed through a silica gel column to obtain the target product.

[0036] 2. The preparation of the amino-terminated polymer (taking polymethyl methacrylate as an example) is as follows:

[0037] (1) In a schlenk tube, the initiator (0.053g, 1.850×10 -4 mol), methyl methacrylate (3.704g, 3.7×10 -2 mol), 2-2 bipyridine (0.029g, 1.83×10 -4 mol) was dissolved in tetrahydrofuran, and the oxygen was removed through 3 cy...

Embodiment 3

[0040] 1, the preparation of ATRP initiator is as follows:

[0041] (1) Dissolve 2g of p-nitroaniline and 3g of triethylamine in 50mL of dichloromethane and place in a 150mL single-necked round bottom flask and stir at room temperature for 2h;

[0042] (2) 3g of 2-bromoisobutyryl bromide was dissolved in 10mL of dichloromethane, added dropwise into the reaction vessel in step (1), and stirred at room temperature for 24h;

[0043] (3) After the reaction is completed, the reaction solution is suction-filtered to remove triethylamine hydrochloride, and the filtrate is passed through a silica gel column to obtain the target product.

[0044] 2. The preparation of the amino-terminated polymer (taking polyhydroxyethyl methacrylate as an example) is as follows:

[0045] (1) In a schlenk tube, the initiator (0.053g, 1.850×10 -4 mol), hydroxyethyl methacrylate (1.203g, 9.25×10 -3 mol), 2-2 bipyridine (0.087g, 5.49×10 -4 mol) was dissolved in methanol and subjected to three cycles o...

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PUM

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Abstract

A method for preparing an amino-terminated polymer involves radical polymerization. Initiator, free radical polymerizable monomer, ligand and solvent are added to the Schleck tube, oxygen is removed through freezing and thawing cycles, catalyst is added in the frozen state, thawing and freezing cycle is performed again, and then in an inert gas atmosphere After the reaction, the resulting material was diluted with dichloromethane and passed through an alkaline alumina column. The resulting colorless solution was added to n-hexane to obtain a precipitate, and after drying, a nitro-terminated polymer was obtained; the prepared nitro-terminated The base polymer and zinc powder are dissolved in ethanol, and glacial acetic acid is added to react under an inert gas atmosphere. After the reaction, the solution is filtered by suction and passed through a silica gel column to obtain an amino-terminated polymer. The raw materials are simple and easy to obtain, the synthesis and purification are convenient, and the initiation efficiency is high. It can initiate monomers such as polymer hydroxyethyl methacrylate at room temperature, and can better control the polydispersity of the polymer in the configured polymerization system.

Description

technical field [0001] The invention relates to radical polymerization, in particular to a preparation method of an amino-terminated polymer. Background technique [0002] Due to the existence of chain transfer and chain termination processes, traditional free radical polymerization has poor control over the molecular weight, polydispersity, and terminal structure of polymers, which limits its wide application. In 1956, Szwarc (Szwarc M. "Living" polymers [J]. Nature, 1956, 178: 1168-1169) first proposed the concept of living radical polymerization. Living polymerization is a chain-growing polymerization process without chain interruption, including chain transfer and chain termination. Compared with traditional free radical polymerization, it can better control the molecular structure, and is an important means to realize molecular design and synthesize polymers with specific structures and properties. At the same time, its polymerization conditions are mild and have a wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14C08F120/28C08F8/04C07C231/02C07C233/15
Inventor 戴李宗毛杰袁丛辉邵志恒刘诚陈婷许一婷何凯斌
Owner XIAMEN UNIV
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