Method for preparing polythiourea through multi-component polymerization of isocyanide, sulfur and amine and application of polythiourea

A polythiourea and multi-component technology, applied in the direction of material analysis, material excitation analysis, and material analysis through optical means, to achieve high molecular weight, high yield, and good film-forming properties

Inactive Publication Date: 2017-10-10
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] There are various reactions for the synthesis of sulfur-containing polymers, but t...

Method used

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  • Method for preparing polythiourea through multi-component polymerization of isocyanide, sulfur and amine and application of polythiourea
  • Method for preparing polythiourea through multi-component polymerization of isocyanide, sulfur and amine and application of polythiourea
  • Method for preparing polythiourea through multi-component polymerization of isocyanide, sulfur and amine and application of polythiourea

Examples

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Embodiment 1

[0044] A method for preparing polythiourea by multi-component polymerization of isonitrile, sulfur and amine, the steps are as follows:

[0045] (1) Under the protection of inert gas, add 81.7mg of p-xylylenediamine, 93.7mg of p-phthalonitrile and 76.9mg of sublimed sulfur to 0.4mL of N,N-dimethylformamide and 0.2mL of toluene Dissolve in a solvent, heat up to 100°C, and stir for 1 hour;

[0046] (2) Cool down to room temperature after the reaction, dilute the reaction mother liquor with 5mL of N,N-dimethylformamide solution, and then drop it (dropping speed is 2 drops / second) into 100mL methanol solution for precipitation , collect the precipitate, dry (the drying temperature is 60° C.) to constant weight, and obtain polythiourea. The yield of the product in this example was 88%, the weight average molecular weight was 30000 g / mol, and the PDI was 1.42.

[0047] The terephthalonitrile of this embodiment is disclosed according to the literature (Jerzy Zakrzewski, MariaKrawcz...

Embodiment 2

[0055] A method for preparing polythiourea by multi-component polymerization of isonitrile, sulfur and amine, the steps are as follows:

[0056] (1) Under the protection of inert gas or under air conditions, mix 72μL dimethylpropylenediamine (0.6mmol), 229.5mg1,2-di-p-isocyanophenyl-1,2-diphenylethylene and 76.9mg Add sublimated sulfur into 0.4mL of N,N-dimethylformamide and 0.2mL of toluene mixed solvent to dissolve, raise the temperature to 100°C, and react for 1h under stirring;

[0057] (2) After the reaction is completed, cool to room temperature, dilute the reaction mother liquor with 5mL of N,N-dimethylformamide solution, and then add it dropwise (the dropping speed is 2 drops / second) to 100mL methanol solution for precipitation , collected the precipitate, and dried (the drying temperature was 60° C.) to constant weight to obtain polythiourea P2. The yield of the product in this example was 89%, the weight average molecular weight was 24300 g / mol, and the PDI was 1.39...

Embodiment 3

[0066] A method for preparing polythiourea by multi-component polymerization of isonitrile, sulfur and amine, the steps are as follows:

[0067] (1) Under the protection of inert gas or under air conditions, add 72 μL of dimethylpropylenediamine, 81.6 mg of 1,6-diisonitrile and 76.9 mg of sublimed sulfur to 0.4 mL of N,N-dimethylformaldehyde Dissolve in a mixed solvent of amide and 0.2mL toluene, heat up to 100°C, and react for 1h under stirring;

[0068] (2) After the reaction is completed, cool to room temperature, dilute the reaction mother liquor with 5mL of N,N-dimethylformamide solution, and then add it dropwise (the dropping speed is 2 drops / second) to 100mL methanol solution for precipitation , collected the precipitate, and dried (the drying temperature was 60° C.) to constant weight to obtain polythiourea P3. The yield of this reaction was >99%, with a weight average molecular weight of 122500 g / mol and a PDI of 2.35.

[0069] The reaction equation involved in this...

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Abstract

The invention belongs to the technical field of preparation of sulfur-containing organic polymers and discloses a method for preparing a polythiourea through multi-component polymerization of isocyanide, sulfur and amine and application of the polythiourea. The preparation method comprises, reacting amine monomers, isocyanide monomers and elemental sulfur in solvent, and performing cooling, precipitation and drying processes to obtain the polythiourea, wherein the amine monomers are diamine compounds, and the isocyanide monomers are di-isocyanide compounds. The method for preparing the polythiourea through multi-component polymerization of isocyanide, sulfur and amine can be implemented at room temperature and in air, thereby being simple, high in polymerization reaction yield and atom economy and simple in product separation; the prepared polythiourea is rich in heteroatoms of N and S and obtains special photoelectric properties, thereby obtaining potential unique application value in fields of biological and chemical fluorescence detection and mercury ion detection.

Description

technical field [0001] The invention belongs to the technical field of preparation of sulfur-containing organic polymers, and in particular relates to a method for preparing polythiourea by multi-component polymerization of isonitrile, sulfur and amine and the application of the polythiourea obtained by the method. Background technique [0002] Introducing heteroatoms such as O, N, S, and P into the polymer molecular chain can make the polymer have some special properties. The introduction of sulfur atoms into the molecular chain, on the one hand, can make the polymer have a higher refractive index, on the other hand, the formation of some sulfur-containing functional groups can promote the formation of metal coordination polymers, so that the polymers can detect metal ions and enrich It has potential unique application value in terms of set. At present, sulfur elements in polymers are usually introduced in the form of thioester bonds, thioether bonds, sulfone groups, thiou...

Claims

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Application Information

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IPC IPC(8): C08G75/00C08G73/00G01N21/64
CPCC08G73/00C08G75/00G01N21/643G01N2021/6432
Inventor 唐本忠田甜胡蓉蓉秦安军赵祖金
Owner SOUTH CHINA UNIV OF TECH
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