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Method of preparing star polyacrylamide by single-electron-transfer living free radical polymerization

A single-electron transfer and polyacrylamide technology, which is applied in the field of single-electron transfer active radical polymerization to prepare star-shaped polyacrylamide, can solve the problems of poor controllability and achieve environmental friendliness, controllable molecular weight, and solvation strong effect

Active Publication Date: 2018-04-24
NORTHEAST GASOLINEEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] An object of the present invention is to provide a method for preparing star-shaped polyacrylamide by single-electron transfer active radical polymerization, which is used to solve the problem of traditional aqueous solution radical polymerization preparation The problem of poor controllability of polyacrylamide method

Method used

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  • Method of preparing star polyacrylamide by single-electron-transfer living free radical polymerization
  • Method of preparing star polyacrylamide by single-electron-transfer living free radical polymerization
  • Method of preparing star polyacrylamide by single-electron-transfer living free radical polymerization

Examples

Experimental program
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Effect test

Embodiment 1

[0032] At room temperature, with the magneton labeled as In the reaction flask, add deionized H 2 O (2ml) and ligand (Me 6 -TREN, 5.3µl, 0.02mmol) was injected with nitrogen for 10 minutes, then CuBr (0.0043g, 0.03mmol) was added, and nitrogen was continued to disproportionate CuBr for 0.5h under anaerobic conditions. Simultaneously the monomer (AM, 0.3741g, 5.3mmol), the initiator Gly-Br 3 (0.0211g, 0.0111 mmol) and a certain amount of deionized H 2 O A total of 3ml was added and marked as In the reaction flask, and make it mix uniformly, pass nitrogen 10min. After the disproportionation is completed, the reaction bottle The medium solution is injected into the reaction vial with a syringe Continue to pass nitrogen in the medium, and stir on the magnetic stirrer, take it out after a certain period of time, and precipitate the polymer with excess acetone, and then pass through the neutral Al 2 o 3 Column chromatography to remove unreacted Cu 0 Powder and the compl...

Embodiment 2

[0038] The SET-LRP polymerization of AM was carried out with reference to the ratio of Example 1, except that the polymerization reaction was carried out at 0°C.

[0039] The monomer conversion rate was 100% as measured by gravimetric method, and the polymer M was measured by GPC. n GPC =38900, M w / M n =1.19

[0040] Figure 4 Be this polyreaction kinetics curve figure, and embodiment one image 3 In comparison, the polymerization temperature is reduced from room temperature (25 °C) to 0 °C, the chain growth rate constant from 0.1924min -1 increased to 0.2601min -1 ; Molecular weight distribution reduces PDI=1.19 (12min conversion rate can reach 100%, M n GPC =38900). This is because the Cu(0) nanoparticles produced by the disproportionation of CuBr at 0°C are smaller than those at room temperature, which is equivalent to increasing the total surface area of ​​Cu(0) and accelerating the polymerization reaction rate. Another reason is that the reaction is carried ou...

Embodiment 3

[0043] Add deionized H 2 O (2ml) and ligand (Me 6 -TREN, 10.7µl, 0.04mmol) was injected with nitrogen for 10 minutes, then CuBr (0.0057g, 0.04mmol) was added, and nitrogen was continued to disproportionate CuBr for 0.5h under anaerobic conditions. Simultaneously, the monomer (AM, 0.7463g, 10.5mmol; NVP, 0.0333g, 0.3mmol; 2-acrylamido-2-methylpropanesulfonic acid sodium (NaAMPS), 0.15ml, 0.3mmol) and the initiator Gly -Br 3 (0.0211g, 0.0111 mmol) and a certain amount of deionized H 2 A total of 3ml of O was added to the reaction flask marked II, and mixed evenly, and nitrogen gas was introduced for 10 minutes. After the disproportionation is completed, inject the solution in the reaction bottle II into the reaction bottle I with a syringe to continue to pass nitrogen, and stir on a magnetic stirrer, take it out after a certain period of time, and precipitate the polymer with excess acetone, and pass through neutral Al 2 o 3 Column chromatography to remove unreacted Cu 0 P...

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Abstract

The invention relates to a method of preparing star polyacrylamide by single-electron-transfer living free radical polymerization, comprising: preparing water-soluble three-arm initiator Gly-Br3; adding H2O and a ligand in reaction bottle I, stirring for a period of time, adding cuprous bromide CuBr, and disproportioning CuBr; adding a monomer, the initiator Gly-Br3 and water into reaction bottleII, and stirring for mixing well; after disproportioning, injecting a solution in the reaction bottle II into the reaction bottle I, stirring for a period of time, allowing reacting at 0-25 DEG C, taking out material in the reaction bottle I, subjecting the material to column chromatography, precipitating, and drying to obtain star polyacrylamide. The method has the advantages that polymerizationspeed is high, monomer conversion rate is high (up to 95% within 10 min), chain-terminal active chain retention rate is high, molecular weight is controllable, and molecular weight distribution is narrow (lowest to 1.18).

Description

technical field [0001] The invention relates to the field of preparation of acrylamide polymers, in particular to a method for preparing star-shaped polyacrylamide by single electron transfer active radical polymerization. Background technique [0002] In 1948, Flory first proposed the concept of star polymer. Star polymers have a compact three-dimensional core-shell space structure, intramolecular and intermolecular crosslinking is not easy to occur, and the polar functional groups on the multi-arm are highly concentrated and have high modulus, which makes star polymers have some special properties, such as Low crystallinity, diffusion coefficient, melt viscosity, and small hydrodynamic volume have resulted in a series of nanomaterials that can be used in drug delivery, lectin assay, cancer therapy, and photonics. [0003] Polyacrylamide (PAM) is a general term for polymers obtained by homopolymerization of acrylamide monomers or copolymerization with other monomers. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F220/56C08F226/10C08F220/58C08F226/06
CPCC08F283/06C08F220/56
Inventor 王玲丁伟陶冶苑丹丹李振东闫超
Owner NORTHEAST GASOLINEEUM UNIV
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