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Atom transfer free radical polymerization method regulated and controlled by inorganic metal salt

An inorganic metal salt and atom transfer technology, which is applied in the field of new and efficient controlled free radical polymerization, can solve the problems of difficult storage and handling, unstable properties of iodohydrocarbons, limiting the scope of application of the polymerization system, etc. The effect of reaction cost

Active Publication Date: 2018-09-18
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this system also successfully realizes the living polymerization of various monomers, the only iodohydrocarbon that can be used as the initiator of this system greatly limits the stability of the polymerization system due to its unstable properties and difficulties in storage and handling. scope of application

Method used

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  • Atom transfer free radical polymerization method regulated and controlled by inorganic metal salt
  • Atom transfer free radical polymerization method regulated and controlled by inorganic metal salt
  • Atom transfer free radical polymerization method regulated and controlled by inorganic metal salt

Examples

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Effect test

Embodiment 1

[0042] After the methyl methacrylate monomer, ethyl 2-bromoisobutyrate initiator and magnesium chloride are purified, the polymerization reaction components are prepared, methyl methacrylate, ethyl 2-bromoisobutyrate, ferrous bromide The molar ratio to magnesium chloride is 200:1:1:2. The preparation process is as follows: in the glove box, 0.061 gram of ferrous bromide and 0.054 gram of magnesium chloride are weighed and put into an eggplant-shaped bottle, and 6 milliliters of methyl methacrylate monomer is added into the eggplant-shaped bottle, and after magnetic stirring for 5 minutes, Then 37.7 microliters of ethyl 2-bromoisobutyrate was added, and stirring was continued for 2 minutes to obtain a pre-reaction mixture.

[0043] Transfer the pre-reaction mixture in the eggplant-shaped bottle to the heating device, and control the reaction temperature to 70°C; after the polymerization reaction reaches the predetermined reaction time interval, take a certain amount of the mixt...

Embodiment 2

[0045] After purification of methyl methacrylate monomer, ethyl 2-bromophenylacetate, halogenated hydrocarbons, and inorganic metal salts, the preparation of polymerization reaction components, methyl methacrylate, ethyl 2-bromophenylacetate, bromine The molar ratio of ferrous chloride and inorganic metal salt is 200:1:1:2. The preparation process is as follows: in the glove box, 0.061 grams of ferrous bromide and the corresponding quality of inorganic metal salts are put into an eggplant-shaped bottle, 6 milliliters of methyl methacrylate monomer is added to the eggplant-shaped bottle, and magnetically stirred for 5 Minutes later, 49.5 microliters of ethyl 2-bromophenylacetate was added, and stirring was continued for 2 minutes to obtain a pre-reaction mixture.

[0046] Transfer the pre-reaction mixture in the eggplant-shaped bottle to the heating device, and control the reaction temperature to 70°C; after the polymerization reaction reaches the predetermined reaction time in...

Embodiment 3

[0049] After purification of methyl methacrylate monomer, ethyl 2-bromophenylacetate halogenated hydrocarbon and calcium chloride, the preparation of polymerization reaction components, methyl methacrylate, ethyl 2-bromophenylacetate, bromine The molar ratio of ferrous chloride and potassium bromide is 200:1:1:4. The preparation process is as follows: weigh 0.061 grams of ferrous bromide and 0.062 grams of calcium chloride in the glove box and put them into an eggplant-shaped bottle, add 6 milliliters of methyl methacrylate monomer into the eggplant-shaped bottle, and stir magnetically for 5 minutes Then, 49.5 microliters of ethyl 2-bromophenylacetate was added, and the stirring was continued for 2 minutes to obtain a pre-reaction mixture.

[0050] Transfer the pre-reaction mixture in the eggplant-shaped bottle to the heating device, and control the reaction temperature to 70°C. After the polymerization reaction reaches the predetermined reaction time interval, take a certain ...

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Abstract

The invention discloses an atom transfer free radical polymerization method regulated and controlled by an inorganic metal salt; according to the method, under a condition without use of other organiccompounds and additives, a polymerization system including vinyl monomers, an initiator, the inorganic metal salt and a transition metal catalyst makes the vinyl monomers undergo an atom transfer free radical polymerization reaction to generate a corresponding polymer under the action of the inorganic metal salt with the catalyst and the initiator. By improvement of the reaction raw materials used in the key atom transfer free radical polymerization reaction, the action of inorganic metal salt cations and the initiator is used, the oxidation-reduction potential of the catalyst is reduced, andthe atom transfer free radical polymerization reaction of the vinyl monomers is more easily catalyzed to generate the polymer with active characteristics. The polymerization method adopts cheap and easily available inorganic metal salt for participating in the reaction, can avoid use of expensive and great-toxicity organic compounds and additives, and reduces the degree of damage to the environmental and reaction costs.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and more specifically relates to an atom transfer radical polymerization method regulated by an inorganic metal salt, which is a novel and efficient controllable radical polymerization method. Background technique [0002] Atom transfer radical polymerization is one of the most commonly used living polymerization methods for designing and synthesizing polymers with controllable molecular weight and structure. Usually, transition metal complexes are used as catalysts to achieve a dynamic balance between active free radicals and dormant species through redox reactions with initiators, endow the polymerization system with a lower free radical concentration, and reduce the occurrence of side reactions such as termination and transfer. So as to achieve the purpose of control. The construction of highly active catalytic systems usually requires the participation of expensive and highly toxic organic l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F120/18C08F265/06C08F220/14C08F2/38
Inventor 薛志刚王计嵘周兴平解孝林
Owner HUAZHONG UNIV OF SCI & TECH
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