Toxic ligand free electrochemistry regulated atom transfer radical polymerization method

A technology of atom transfer and polymerization method, which is applied in the field of electrochemically regulated atom transfer radical polymerization of non-toxic ligands, which can solve the problems of difficult storage and handling of low-valence transition metal catalysts, high price, etc., and simplify the post-processing process , reduce the cost of raw materials, optimize the effect of components

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 non-toxic ligand electrochemically regulated atom transfer radical polymerization method, wherein through the reaction raw materials used in the atom transfer radical polymerization reaction, And the reaction conditions are improved, and electrochemical action is app...

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  • Toxic ligand free electrochemistry regulated atom transfer radical polymerization method

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Embodiment 1

[0042] After purification of methyl methacrylate monomer, acetonitrile solvent, and ethyl 2-bromophenylacetate initiator, the polymerization reaction components are prepared, methyl methacrylate, ethyl 2-bromophenylacetate, iron bromide The molar ratio is 200:1:1, and the volume ratio of methyl methacrylate and acetonitrile is 1:1. The preparation process is: weigh 0.0836 grams of ferric bromide and 0.1303 grams of tetraethylammonium tetrafluoroborate in the glove box and put them into a four-necked bottle, take 6 milliliters of methyl methacrylate monomer and 6 milliliters of acetonitrile with a needle tube and add to In the four-neck flask, after 20 minutes of magnetic stirring, 49.5 microliters of ethyl 2-bromophenylacetate was added, and the stirring was continued for 2 minutes to obtain a pre-reaction mixture.

[0043] Transfer the pre-reaction mixture in the four-shaped bottle to the heating device, control the reaction temperature to 60°C; connect the electrode to set t...

Embodiment 2

[0045] After purifying n-butyl methacrylate monomer, acetonitrile and ethyl 2-bromophenylacetate initiator, the polymerization reaction components were prepared, n-butyl methacrylate, ethyl 2-bromophenylacetate, bromide The molar ratio of iron is 200:1:1, and the volume ratio of n-butyl methacrylate and acetonitrile is 1:1. The preparation process is as follows: weigh 0.0836 grams of ferric bromide and 0.1303 grams of tetraethylammonium tetrafluoroborate in the glove box and put them into a four-neck bottle, take 8 milliliters of n-butyl methacrylate monomer and 8 milliliters of acetonitrile and add into a four-neck flask, and after magnetically stirring for 20 minutes, add 49.5 microliters of ethyl 2-bromophenylacetate, and continue stirring for 2 minutes to obtain a pre-reaction mixture.

[0046] Transfer the pre-reaction mixture in the four-shaped bottle to the heating device, control the reaction temperature to 60°C; connect the electrode, set the voltage (voltage is -0.3V...

Embodiment 3

[0048] After purification of methyl acrylate monomer, N-methylpyrrolidone as solvent and ethyl 2-bromophenylacetate initiator, the polymerization reaction components are prepared, methyl acrylate, ethyl 2-bromophenylacetate, bromide The molar ratio of iron is 200:1:1, and the volume ratio of methyl acrylate and N-methylpyrrolidone is 1:1. The preparation process is as follows: weigh 0.0836 grams of ferric bromide and 0.1303 grams of tetraethylammonium tetrafluoroborate into a four-necked bottle in the glove box, and take 6 milliliters of methyl methacrylate monomer and 6 milliliters of N-methyl methacrylate monomer with a needle tube. The base pyrrolidone was added into the four-neck flask, and after magnetic stirring for 20 minutes, 49.5 microliters of ethyl 2-bromophenylacetate was added, and the stirring was continued for 2 minutes to obtain a pre-reaction mixture.

[0049] Transfer the pre-reaction mixture in the four-shaped bottle to the heating device, control the reacti...

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Abstract

The invention discloses a toxic ligand free electrochemistry regulated atom transfer radical polymerization method. According to the method, under an electrochemical effect, no any toxic ligand is used, and five reactions raw materials namely monomers, a catalyst, an initiator, an electrolyte, and a solvent are mixed to make the monomers carry out atom transfer radical polymerization reactions to generate corresponding polymers. The reaction raw materials and reaction conditions of atom transfer radical polymerization reactions are improved; during the process of atom transfer radical polymerization reactions, an electrochemical effect is applied; the problem that a low valent transition metal catalyst is difficult to store and process in an atom transfer radical polymerization system is effectively solved; the shortages such as toxic ligand, pricy reducing agent, strong toxicity, volatility, and the like, are overcome, and the damage to the environment and the reaction cost are both reduced.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and more specifically relates to a non-toxic ligand electrochemically regulated atom transfer radical polymerization method, which is an electrochemically regulated atom transfer radical polymerization method. Background technique [0002] Anionic polymerization is the first living polymerization method discovered, which can keep the end of the polymer chain reactive during the polymerization process, so it can be used to prepare a preset relative molecular mass, low dispersion (narrow relative molecular mass distribution) and polymers with controllable functionality. However, the conditions of anionic polymerization are harsh and difficult to control. Combining the advantages of free radical polymerization, people have discovered a variety of controllable free radical polymerization methods, among which the most widely used method is atom transfer radical polymerization. Its mechanism is to us...

Claims

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Application Information

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IPC IPC(8): C08F2/58C08F120/14C08F120/18C08F120/56C08F112/08C08F120/44C08F120/06
CPCC08F2/58C08F112/08C08F120/06C08F120/14C08F120/18C08F120/44C08F120/56
Inventor 薛志刚田梦颖杜飞鹏王计嵘解孝林周兴平
Owner HUAZHONG UNIV OF SCI & TECH
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