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A kind of preparation method of high molecular polymer containing azide group

A polymerization method and polymer technology are applied in the fields of chemical synthesis and polymer materials, which can solve the problems of restricting the research and application of azide polymer materials, and achieve the effects of mild reaction conditions, low energy consumption and environmental friendliness.

Active Publication Date: 2020-08-04
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above methods for synthesizing azide polymers all have deficiencies, which limit the research and application of azide polymer materials to a large extent. Therefore, it is very important to carry out research on azide group-containing polymers.

Method used

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  • A kind of preparation method of high molecular polymer containing azide group
  • A kind of preparation method of high molecular polymer containing azide group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Fill a 25ml reaction tube with nitrogen, add 0.05mmol of methacrylic acid aryl azide, 0.005mmol of catalyst ethyl bromophenylacetate, add 0.005mmol of Eosin Y, add rotor, add 0.005mmol of triethylamine , Add 1ml of tetrahydrofuran solution, stir with a magnetic stirrer for 6-10h under the irradiation of blue LED light, and end the reaction. The reaction product was precipitated in methanol, filtered and dried, and the conversion rate was 80% by calculation. The preservation rate of azide was 100%, and the molecular weight distribution was 1.24.

Embodiment 2

[0025] Fill a 25ml reaction tube with nitrogen, add 0.05mmol of hexyl methacrylate azide, 0.005mmol of ethyl bromophenylacetate as catalyst, add 0.005mmol of Eosin Y, add rotor, add 0.005mmol of triethylamine , Add 1ml of tetrahydrofuran solution, stir with a magnetic stirrer for 6-10h under the irradiation of blue LED light, and end the reaction. The reaction product was precipitated in methanol, filtered and dried, and the conversion rate was 65% by calculation. The preservation rate of azide is 100%, and the molecular weight distribution is 1.30.

Embodiment 3

[0027] Fill a 25ml reaction tube with nitrogen, add 0.05mmol of methacrylic acid meta-azide, 0.005mmol of catalyst ethyl bromophenylacetate, add 0.005mmol of Eosin Y, add rotor, add 0.005mmol of triethylamine , Add 1ml of tetrahydrofuran solution, stir with a magnetic stirrer for 6-10h under the irradiation of blue LED light, and end the reaction. The reaction product was precipitated in methanol, filtered and dried. After calculation, the conversion rate was 81%. The preservation rate of azide was 100%, and the molecular weight distribution was 1.22.

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Abstract

The invention discloses a preparation method of an azide group containing high molecular polymer, and belongs to the technical fields of chemical synthesis and high molecular materials. A polymerization method of an azide-group polymer, which is provided by the invention, comprises the following steps of adding a bromophenyl compound as an initiator into a reactor full of nitrogen, adding an azidomonomer, adding eosin Y as a photocatalyst, adding triethylamine as an auxiliary catalyst, adding an organic solvent, at a room temperature, agitating for 6h to 10h under the irradiation of a 7W blueLED (Light Emitting Diode) lamp, pouring product reaction liquid into absolute methanol to separate out a solid, carrying out suction filtration on a methanol solution, so as to obtain a polymer solid, oven-drying the polymer solid, and weighing. The preparation method is used for polymerizing, through the azido monomer under the acceleration of visible light, a high molecular compound under theaction of the catalysts, is mild in reaction condition, low in energy consumption and environmentally friendly, and can be used for obtaining an azido polymer with narrower molecular distribution in ahigh yield manner.

Description

Technical field [0001] The invention relates to a preparation method of an azide group-containing high molecular polymer, which belongs to the technical field of chemical synthesis and high molecular material. Background technique [0002] Azide-based polymers are widely used in the fields of military industry, aerospace and materials. They can not only be used as crosslinking agents and surface performance materials for rocket propellants, but also can be used to manufacture various functional materials. It is a high-tech product with broad application prospects. Molecular materials. Especially since Sharpless put forward the concept of click chemistry in 2004, the preparation of various functional polymer materials through the reaction of azide groups and alkynes has become a current research focus. However, the azide group has high activity and is a typical energetic group. In the traditional thermally promoted polymerization reaction, it is easy to cause explosion hazard due...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/34C08F2/48
CPCC08F2/48C08F120/34
Inventor 钮腾飞王聃轲
Owner JIANGNAN UNIV