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Ligand-free Transition Metal Catalytic Activity/Controlled Radical Polymerization Method in Aqueous Phase

A technology of transition metal catalysis and polymerization method, which is applied in the field of transition metal catalyzed radical polymerization without ligands in aqueous phase, and can solve the problems of poor solubility of transition metals and deviation of water solvent from research field of view.

Active Publication Date: 2011-12-28
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Considering that the solubility of transition metals in water is very poor, these make water solvents more and more deviate from people's research field of vision.

Method used

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  • Ligand-free Transition Metal Catalytic Activity/Controlled Radical Polymerization Method in Aqueous Phase
  • Ligand-free Transition Metal Catalytic Activity/Controlled Radical Polymerization Method in Aqueous Phase
  • Ligand-free Transition Metal Catalytic Activity/Controlled Radical Polymerization Method in Aqueous Phase

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Synthesis of P(PEGMA) (sample 1)

[0032] In a 100mL single-necked bottle, add 2.0mL polyethylene glycol monomethyl ether (PEGMA) (Mw=300) and 20mL ultrapure water as monomers, fully dissolve, and after bubbling nitrogen for 30 minutes, add 0.04mmol copper sulfate and 0.06 Mmol ascorbic acid, 20 μL isopropane bromide, continue to pass nitrogen gas for 5 minutes, seal and react at room temperature for 10 minutes. The reaction was quenched with liquid nitrogen, and the product was freeze-dried. Get 20 milligrams of dry matter and dissolve in 2.0 milliliters of tetrahydrofuran, detect its molecular weight and its fraction distribution with GPC as figure 1 shown. It shows that the present invention can successfully polymerize polyethylene glycol monomethyl ether monomer, and obtain a polymer with narrow molecular weight distribution.

Embodiment 2

[0034] Synthesis of P(NIPAM) (sample 2)

[0035] Add 0.3192g of isopropylacrylamide (NIPAM) and 20mL of ultrapure water into a 100mL single-necked bottle, fully dissolve, and after bubbling nitrogen for 30 minutes, add 0.04mmol of copper sulfate and 0.06mmol of ascorbic acid in sequence, 20μL of bromoiso Propane, continue to flow nitrogen for 5 minutes, seal, and react at room temperature for 10 minutes. The reaction was quenched with liquid nitrogen, and the product was freeze-dried. Get 20 mg dry matter and dissolve in 2.0 milliliters of tetrahydrofuran, detect its molecular weight and its molecular weight distribution with GPC as figure 2 shown. It shows that the present invention can successfully polymerize polyisopropylacrylamide monomers and obtain polymers with narrow molecular weight distribution.

Embodiment 3

[0037] Synthesis of HPC-g-P(PEGMA) (sample 3)

[0038] In a 1000mL single-necked bottle, add 4.0g hydroxypropyl cellulose (HPC), 400mL anhydrous tetrahydrofuran (THF) and 5.0mL anhydrous pyridine, stir well to dissolve. The reactor was placed in an ice-water bath, and a mixed solution of 1.0 mL of bromoisobutyryl bromide and 20 mL of anhydrous tetrahydrofuran was slowly dropped into it. After the dropwise addition is completed, seal and place at 30 degrees Celsius for 48 hours of reaction. After standing still, the precipitate was discarded by filtration, and after the excess THF was rotary evaporated, the remaining solution was dialyzed in water for one week, and the water was changed every 8 hours. Freeze-dry the dialyzed solution to obtain hydroxypropyl cellulose macromolecular initiator (HPC-Br). image 3 It is a macromolecular initiator HPC-Br NMR characterization. The NMR characterization shows that the initiator has been successfully prepared, and its Br substitution ...

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Abstract

The invention discloses a novel environmentally-friendly polymerization method. In the method, low-oxidation-state copper catalytic polymerization is used as a basis; and polymerization reaction is initiated in a water-phase system at normal temperature without a ligand. In the reaction, alkyl bromide or various kinds of substances containing the alkyl bromide are used as an initiator; bivalent copper and a reducer are used for producing low-valence copper to serve as a catalyst; and the polymerization of olefin monomer is initiated in aqueous solution at normal temperature. The method has the advantages of high reaction efficiency, environmental friendliness, low cost, low energy consumption and capability of effectively synthesizing an oligomer, a block polymer, a graft polymer, a star polymer and the like.

Description

technical field [0001] The invention relates to a transition metal-catalyzed radical polymerization method without a ligand in water phase Background technique [0002] Free radical polymerization has been greatly developed in recent decades. After several generations of research, free radical polymerization has developed and extended to many fields, the most notable of which is living controllable free radical polymerization. Commonly used living controllable radical polymerization reactions include atom transfer radical polymerization (ATRP), reversible addition chain transfer polymerization (RAFT), etc. This type of reaction can effectively control the concentration of free radicals in the reaction process, so that it is in the Extremely low concentration levels to reduce free radicals caused by collisions between free radicals. Therefore, the mild and controllable reaction of living-controlled radical polymerization can be used to synthesize and design a series of polym...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/00C08F2/10C08F2/22C08F4/40
Inventor 刘瑞刚金鑫黄勇
Owner INST OF CHEM CHINESE ACAD OF SCI
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