Atom transfer radical polymerization method utilizing low temperature eutectic melt effect

A low-temperature eutectic and atom transfer technology, applied in the field of polymer active polymerization, can solve the problems of high toxicity and expensive ligands, and achieve the effects of reducing viscosity, reducing reaction heat, and simplifying post-treatment process.

Active Publication Date: 2017-05-31
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the above defects or improvement needs of the prior art, the object of the present invention is to provide a method for atom transfer radical polymerization utilizing the effect of low-temperature eutectic, wherein the medium environment adopted for the key atom transfer radical polymerization reaction is carried out Improvement, using the low-temperature co-melt as the solvent or ligand of the polymerization system, can further optimize the components of the atom transfer radical polymerization system, and overcome the expensive and toxic ligands used in the atom transfer radical polymerization method in the prior art The biggest disadvantage is that the polymerization method does not need to add any organic compound or polar solvent in the traditional atom transfer radical polymerization as a ligand, which has the advantages of environmental protection; in addition, the present invention can adjust the type of low-temperature eutectic And the amount to adjust the reaction rate, product conversion rate and polymerization control, so as to prepare the desired polymerization product

Method used

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  • Atom transfer radical polymerization method utilizing low temperature eutectic melt effect
  • Atom transfer radical polymerization method utilizing low temperature eutectic melt effect
  • Atom transfer radical polymerization method utilizing low temperature eutectic melt effect

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Experimental program
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Effect test

Embodiment 1

[0041] After the purification of methyl methacrylate monomer and ethyl 2-bromophenylacetate initiator, carry out the preparation of polymerization reaction components, methyl methacrylate, ethyl 2-bromophenylacetate, ferrous bromide (low valence state transition metal catalyst) molar ratio is 100:1:1, methyl methacrylate and low-temperature eutectic (low-temperature eutectic are respectively four groups, namely, acetamide-ammonium thiocyanate low-temperature eutectic, ethyl methacrylate The volume ratio of amide-potassium thiocyanate low-temperature eutectic, urea-ammonium thiocyanate low-temperature eutectic, urea-potassium thiocyanate low-temperature eutectic) is 100:1. The preparation process is as follows: weigh 0.122 grams of ferrous bromide in the glove box and put it into an eggplant-shaped bottle, add 6 ml of methyl methacrylate monomer into the eggplant-shaped bottle, and stir magnetically for 20 minutes to obtain a pre-reaction mixture. liquid.

[0042] Transfer the...

Embodiment 2

[0045] After the purification of methyl methacrylate monomer and ethyl 2-bromophenylacetate initiator, carry out the preparation of polymerization reaction components, methyl methacrylate, ethyl 2-bromophenylacetate, ferrous bromide (low valence state transition metal catalyst) molar ratio is 200:1:1, the volume ratio of methyl methacrylate and low-temperature eutectic is 3:1 (low-temperature eutectic is divided into three kinds, namely caprolactam-acetamide low-temperature eutectic body, acetamide-urea low-temperature eutectic, caprolactam-urea low-temperature eutectic). The preparation process is as follows: weigh 0.061 g of ferrous bromide in the glove box and put it into an eggplant-shaped bottle, add 6 ml of methyl methacrylate monomer into the eggplant-shaped bottle, and stir magnetically for 20 minutes to obtain a pre-reaction mixture liquid.

[0046] The pre-reaction mixture in the eggplant-shaped bottle was transferred to a heating device, and the reaction temperatur...

Embodiment 3

[0048] After purifying the n-butyl methacrylate monomer and ethyl 2-bromophenylacetate initiator, prepare the polymerization reaction components, n-butyl methacrylate, ethyl 2-bromophenylacetate, ferrous bromide (Low-valent transition metal catalyst) The molar ratio is 50:1:1, and the volume ratio of methyl methacrylate and acetamide-potassium thiocyanate low-temperature eutectic is 50:1. The preparation process is as follows: weigh 0.122 grams of ferrous bromide in the glove box and put it into an eggplant-shaped bottle, take 4 ml of n-butyl methacrylate monomer and add it to the eggplant-shaped bottle, and stir magnetically for 20 minutes to obtain a pre-reaction Mixture.

[0049] Transfer the pre-reaction mixture in the eggplant-shaped bottle to a heating device, control the reaction temperature to 60°C, heat and stir for five minutes, then add 30 microliters of acetamide-potassium thiocyanate low-temperature eutectic and 49.5 microliters of 2-bromo Ethyl phenylacetate sta...

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PUM

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Abstract

The invention discloses an atom transfer radical polymerization method utilizing a low temperature eutectic melt effect. The method is characterized in that in a low temperature eutectic melt environment, monomers, an initiator, and a catalyst are mixed to make the monomers carry out atom transfer radical polymerization reactions to generate corresponding polymers, wherein the low temperature eutectic melt is in a liquid state. According to the method, the medium of atom transfer radical polymerization reactions is improved, the low temperature eutectic melt is taken as the solvent or ligand of the polymerization system, and the components of the atom transfer radical polymerization system are further optimized to overcome the shortages of the prior art such as high price of ligands, strong toxicity of ligands, and the like.

Description

technical field [0001] The invention belongs to the field of polymer living polymerization, and more specifically relates to an atom transfer radical polymerization method using low-temperature eutectic melt, which uses the atom transfer reaction of low-temperature eutectic to prepare controllable polymers. Green's Atom Transfer Radical Polymerization Method. Background technique [0002] Atom transfer radical polymerization is widely used because it can solve the problem of poor control in traditional radical polymerization, and then realize the effective design of macromolecular topology and terminal functional groups. However, the ligands used in the usual atom transfer radical polymerization method are mostly volatile organic polar solvents, toxic N, P-containing compounds or ionic liquids, which are not only harmful to the environment but also expensive. Applying more biocompatible and inexpensive ligands to the atom transfer radical polymerization system is an inevita...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F120/18C08F2/06C08F4/80
CPCC08F2/06C08F4/80C08F120/14C08F120/18C08F2438/01
Inventor 薛志刚王计嵘解孝林周兴平韩建宇周俊
Owner HUAZHONG UNIV OF SCI & TECH
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