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Alkyne, sulfur and amine multi-component polymerization method for preparing poly-thioamide

A polythioamide, polymerization method technology, applied in the field of multi-component polymerization of alkynes, sulfur and amines, to achieve the effects of high polymer yield, high molecular weight and high atom economy

Active Publication Date: 2015-10-28
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 there is no report on the synthesis of polythioamides directly using elemental sulfur as a reactant.

Method used

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  • Alkyne, sulfur and amine multi-component polymerization method for preparing poly-thioamide
  • Alkyne, sulfur and amine multi-component polymerization method for preparing poly-thioamide
  • Alkyne, sulfur and amine multi-component polymerization method for preparing poly-thioamide

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Experimental program
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Embodiment 1

[0031] A kind of multi-component polymerization method of alkynes, sulfur and amines for preparing polythioamides in this embodiment, the specific preparation steps are as follows:

[0032] (1) Under the protection of an inert gas, add 68mg of p-xylylenediamine, 94.5mg of 1,4-diethynylbenzene and 64mg of sublimed sulfur into 0.5mL of pyridine to dissolve, raise the temperature to 50-60°C, and react under stirring for 24h ;

[0033] (2) After the reaction is completed, cool to room temperature, dilute the reaction mother liquor with 1mL dimethylformamide solution, add it dropwise to 20mL methanol for precipitation, collect the precipitate, and dry to constant weight to obtain polythioamide.

[0034] The polythioamide of the present embodiment has the structural formula shown in P1:

[0035]

[0036] The reaction equation involved in this embodiment is as follows:

[0037]

[0038] The proton nuclear magnetic spectrum of the polythioamide of the present embodiment in deu...

Embodiment 2

[0043] A kind of multi-component polymerization method of alkynes, sulfur and amines for preparing polythioamides in this embodiment, the specific preparation steps are as follows:

[0044] (1) Under the protection of an inert gas, 68 mg of p-xylylenediamine, 285 mg of diethynyltetraphenylethylene and 64 mg of sublimed sulfur were dissolved in 0.5 mL of pyridine, heated to 100-120 °C, and reacted for 4 hours under stirring;

[0045] (2) After the reaction is completed, cool to room temperature, dilute the reaction mother liquor with 1mL dimethylformamide solution, add it dropwise to 20mL methanol for precipitation, collect the precipitate, and dry to constant weight to obtain polythioamide.

[0046] Diethynyltetraphenylethylene in this example was prepared according to the method disclosed in the literature [Polym.Chem.2012,3,1481].

[0047] The polythioamide of the present embodiment has the structural formula shown in P2:

[0048]

[0049] The reaction equation involved ...

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Abstract

The invention belongs to the technical field of preparing a sulfur-containing organic polymer, and discloses an alkyne, sulfur and amine multi-component polymerization method for preparing poly-thioamide. The method includes the steps that under the condition of inert gas shielding, primary amine monomers containing aromatic groups or aromatic derivatives, terminal diyne monomers containing aromatic groups or aromatic derivatives and elemental sulfur are added into solvent to be dissolved, heated to the temperature of 50 DEG C-120 DEG C so as to react fully, and then cooled to the room temperature, precipitant is added into a reaction mother solution for precipitation, and a precipitate is collected and dried until the weight is constant to obtain the poly-thioamide. The poly-thioamide has a structural general formula shown as the formula (1), wherein n is an integer ranging from two to two hundred, and Ar1 and Ar2 are the same or different aromatic groups or aromatic derivatives. The poly-thioamide has the special photoelectric property and potential application value in biological and chemical fluorescence detection fields.

Description

technical field [0001] The invention belongs to the technical field of preparation of sulfur-containing organic polymers, in particular to a multi-component polymerization method of alkyne, sulfur and amines for preparing polythioamides. Background technique [0002] The introduction of halogen elements (in addition to fluorine), heavy metal ions, benzene rings and condensed rings, sulfur, and phosphorus atoms into polymer molecules can effectively increase the refractive index. The addition of sulfur not only makes the polymer have a higher refractive index, but also It is helpful to reduce the dispersion of the material. In addition, this kind of polymer is easy to prepare and has good environmental stability, so it has attracted widespread attention of scientists. At present, sulfur elements in polymers are usually introduced in the form of thioether bonds, thioester bonds, thiourethanes, sulfone groups, and episulfides. Isothiocyanate and carbon disulfide are expensive ...

Claims

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Application Information

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IPC IPC(8): C08G73/00C09K11/06
Inventor 唐本忠李伟章胡蓉蓉秦安军赵祖金
Owner SOUTH CHINA UNIV OF TECH
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