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Ligand-free atom transfer radical polymerization method under action of alkali

A technology of atom transfer and polymerization method, applied in the field of atom transfer radical polymerization and ligand-free atom transfer radical polymerization, can solve the problems of high toxicity, reduce the degree of environmental damage, reaction cost and high price, and reduce the reaction cost. , reduce the redox potential and accelerate the generation of active free radicals

Active Publication Date: 2017-05-24
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 ligand-free atom transfer radical polymerization method under the action of an alkali, wherein the reaction raw materials used in the key atom transfer radical polymerization reaction are carried out Improvement, the use of bases to participate in the reaction can further optimize the components of the atom transfer radical polymerization system, and overcome the organic compounds or polar solvents used in the atom transfer radical polymerization system in the prior art (such as containing P, N compounds, Organic acids, ionic liquids, and raw materials containing amide groups, etc.) as ligands have disadvantages such as high price, high toxicity and volatility, and reduce the degree of damage to the environment and reaction costs

Method used

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  • Ligand-free atom transfer radical polymerization method under action of alkali
  • Ligand-free atom transfer radical polymerization method under action of alkali
  • Ligand-free atom transfer radical polymerization method under action of alkali

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] After purifying methyl methacrylate monomer, solvent (solvent is respectively toluene, benzene, tetrahydrofuran, anisole, diphenyl ether, ethyl acetate), 2-bromo ethyl isobutyrate initiator and sodium phosphate, carry out Preparation of polymerization reaction components, methyl methacrylate, ethyl 2-bromoisobutyrate, ferrous bromide (low-valence transition metal catalyst) and sodium phosphate molar ratio of 200:1:1:2, methacrylic acid The volume ratio of methyl ester and solvent is 1:1. The preparation process is: take 0.061 gram of ferrous bromide and 0.0928 gram of sodium phosphate in the glove box and put them into the eggplant-shaped bottle, get 6 milliliters of methyl methacrylate monomer and 6 milliliters of solvent into the eggplant-shaped bottle, and magnetically After stirring for 20 minutes, 37.7 microliters of ethyl 2-bromoisobutyrate was added, and stirring was continued for 2 minutes to obtain a pre-reaction mixture.

[0049] Transfer the pre-reaction mix...

Embodiment 2

[0051] After purifying methyl methacrylate monomer, ethyl 2-bromophenylacetate initiator, sodium bicarbonate and stannous octoate, carry out reduction polymerization reaction component preparation (wherein stannous octoate is used as reducing agent), methyl The molar ratio of methyl acrylate, ethyl 2-bromophenylacetate, ferric bromide (or ferric chloride) (high valence transition metal catalyst), sodium carbonate and stannous octoate is 200:1:1:2:3. The preparation process is: take by weighing 0.0459 gram of ferric bromide (or ferric chloride) and 0.0476 gram of sodium bicarbonate in the glove box and put it into an eggplant-shaped bottle, get 6 milliliters of methyl methacrylate monomer and 0.275 milliliters of stannous octoate Add it into an eggplant-shaped flask, stir it magnetically for 20 minutes, then add 49.5 microliters of ethyl 2-bromophenylacetate, and continue stirring for 2 minutes to obtain a pre-reaction mixture.

[0052] Transfer the pre-reaction mixture in the ...

Embodiment 3

[0055] After purifying methyl methacrylate monomer, ethyl 2-bromophenylacetate initiator and sodium carbonate, prepare the polymerization reaction components, methyl methacrylate, ethyl 2-bromophenylacetate, ethylene bromide The molar ratio of iron (low-valence transition metal catalyst) to alkali is 200:1:1:2. The preparation process is: take 0.061 gram of ferrous bromide and a corresponding amount of alkali in the glove box and put it into an eggplant-shaped bottle, get 6 milliliters of methyl methacrylate monomer and add it into the eggplant-shaped bottle, and after magnetic stirring for 20 minutes, Then 49.5 microliters of ethyl 2-bromophenylacetate was added, and stirring was continued for 2 minutes to obtain a pre-reaction mixture.

[0056] Transfer the pre-reaction mixture in the eggplant-shaped bottle to the heating device, and control the reaction temperature to 60°C; after the polymerization reaction reaches the predetermined reaction time interval, take a certain am...

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Abstract

The invention discloses a ligand-free atom transfer radical polymerization method under the action of alkali. The method is characterized by comprising the following step: mixing reaction raw materials comprising a monomer, an initiator and a catalyst without using a ligand under the action of alkali, so that the monomer is subjected to atom transfer radical polymerization reaction to generate a corresponding polymer. The ligand-free atom transfer radical polymerization method improves the reaction raw materials adopted in the key atom transfer radical polymerization reaction, uses alkali to participate in the reaction, can further optimize components of an atom transfer radical polymerization system, overcomes defects that toxic and volatile organic compounds or polar solvents used by the atom transfer radical polymerization system as the ligands are expensive, highly toxic and volatile in the prior art, and reduces the degree of damage to the environment and the reaction cost.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and more specifically relates to a ligand-free atom transfer radical polymerization method under the action of an alkali, which is a new implementation method of the atom transfer radical polymerization method. Background technique [0002] Atom transfer radical polymerization has become one of the most important "living" / controllable polymerization methods due to its excellent controllability, and is widely used to synthesize polymers with controllable molecular weight and narrow distribution, and has good molecular design functions . The traditional atom transfer radical polymerization method needs to add organic compounds (such as P, N-containing compounds, organic acids, ionic liquids, etc.) as ligands to form complexes with catalysts to make the system more active. Expensive and highly toxic, it cannot meet the requirements of green development and widespread use of polymerization methods. ...

Claims

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Application Information

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IPC IPC(8): C08F120/14C08F120/18C08F2/06C08F2/02C08F4/26
CPCC08F2/02C08F2/06C08F4/26C08F120/14C08F120/18C08F2438/01
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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