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A kind of preparation method of the polymer whose terminal is diselenocarbamate

A carbamate and polymer technology, applied in the field of preparation of selenium-containing polymers, can solve problems such as narrow molecular weight distribution, achieve mild reaction conditions, simple and controllable preparation process, and good solubility

Active Publication Date: 2017-02-01
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there are few reports on the synthesis of diselenated carbamate-containing polymers. In order to increase the application of selenium-containing polymers, it is necessary to develop a new method for preparing diselenated carbamate-containing polymers, and it is required The molecular weight of the polymer obtained by this method is controllable and the molecular weight distribution is narrow

Method used

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  • A kind of preparation method of the polymer whose terminal is diselenocarbamate
  • A kind of preparation method of the polymer whose terminal is diselenocarbamate
  • A kind of preparation method of the polymer whose terminal is diselenocarbamate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] molar ratio [styrene] 0 :[Initiator] 0 : [Cuprous bromide] 0 : [Pentamethyldiethyltriamine] 0 =100:1:2:6; By volume, styrene:N,N-dimethylformamide=1:1, catalyst and complexing agent, and initiator diselenocarbamate, The free radical polymerized monomer (styrene) and the solvent were used to prepare the polymerization reaction system in a 5 mL ampoule, freeze-pump-thaw, cycle three times, and seal the tube under an oxygen-free atmosphere. Carry out the polymerization reaction at 120°C for 24 hours. After the reaction, take out the sealed tube, cool it with cold water immediately, open the sealed tube, dissolve it with 2~5mL of tetrahydrofuran, drop it into 250mL of methanol and let it stand overnight, filter it with suction, and dry it to get A diselenocarbamate-terminated polymer. See Table 1 for initiators and corresponding experimental data.

[0033]

Embodiment 2

[0035] molar ratio [styrene] 0 :[CEDSC] 0 : [copper salt] 0 : [Pentamethyldiethyltriamine] 0 = 100:1:1:3. According to the volume ratio, styrene: solvent = 1:1, the catalyst and complexing agent, initiator (CEDSC), monomer (styrene), and solvent are prepared in order. In a 5 mL ampoule, freeze-pump-thaw, cycle three times, and seal the tube under an oxygen-free atmosphere. Carry out the polymerization reaction at 120°C for 24 hours. After the reaction is over, take out the sealed tube, immediately cool it with cold water, open the sealed tube, dissolve it with 2~5mL of tetrahydrofuran, drop it into 250mL of methanol and let it stand overnight, filter it with suction, and dry it to get A diselenocarbamate-terminated polymer. See Table 2 for copper salts, solvents and corresponding experimental data.

[0036]

Embodiment 3

[0038] molar ratio [styrene] 0 :[CEDSC] 0 : [Cuprous bromide] 0 : [nitrogen-containing compounds] 0 = 100:1:1:3. According to the volume ratio, monomer: solvent = 1:1, the catalyst, nitrogen-containing compound, initiator (CEDSC), monomer (styrene), and solvent (toluene) were prepared in sequence in a polymerization reaction system in a 5 mL ampoule , freeze-pump-thaw, cycle three times, and seal the tube under an oxygen-free atmosphere. Carry out the polymerization reaction under heating for 9 hours. After the reaction is over, take out the sealed tube, immediately cool it with cold water, open the sealed tube, dissolve it with 2~5mL of tetrahydrofuran, drop it into 250mL of methanol and place it overnight, filter it with suction, and dry it to get the end. Polymers of diselenated carbamates. See Table 3 for heating temperature, nitrogen-containing compounds and corresponding experimental data.

[0039]

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Abstract

The invention discloses a preparation method for a polymer with bi-seleno-carbamate at the end. The polymer with bi-seleno-carbamate at the end is prepared through atom transfer radical polymerization reaction initiated by the bi-seleno-carbamate. A reaction system comprises a radical polymerizable monomer, an initiator, a complexant and a catalyst. The simple preparation method combines the advantages of atom transfer radical polymerization and uses bi-seleno-carbamate as the initiator to obtain the polymer with a bi-seleno-carbamate structure at the end, which is narrow in molecular weight distribution.

Description

technical field [0001] The invention relates to a preparation method of a selenium-containing polymer, in particular to a preparation method of a polymer whose terminal is a diselenocarbamate. Background technique [0002] In the past few decades, due to the needs of polymer design, polymer materials and functional polymers, living controllable radical polymerization has made great progress, and has already had such as nitroxide stable radical polymerization, atom transfer radical polymerization, Several mature and perfect polymerization methods such as reversible addition-fragmentation chain transfer radical polymerization. [0003] The atom transfer radical polymerization system is mainly composed of free radical polymerization monomers, initiators, ligands and catalysts, among which the initiator is a very important element, which can initiate free radical polymerization; at the same time, the initiator determines the The terminal structure has a great influence on molec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F112/08C08F112/12C08F6/12
Inventor 潘向强高峰朱秀林张正彪朱健程振平张伟周年琛
Owner SUZHOU UNIV