Three-arm ATRP (atom transfer radical polymerization) initiator with plane conjugated structure, and preparation and application thereof
A planar conjugation and initiator technology, which is applied in the preparation of organic compounds, carboxylic acid amide preparation, organic chemistry, etc., can solve the problems of complex polymerization reaction system, complex chemical structure design, and difficult synthesis process, and achieve universal reaction system. Good adaptability, ingenious structural design, and simple synthesis steps
Active Publication Date: 2016-06-01
XIAMEN UNIV
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The reason is that the design of the chemical structure of this type of initiator is complicated, the synthesis process is difficult, the raw materials are difficult to obtain, the cost is high, the applicable polymerization reaction system is also extremely complicated, and the post-treatment is difficult.
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[0030] The following embodiments describe the present invention in further detail in conjunction with the accompanying drawings.
[0031] (1) Dissolve 0.5 g of 1,3,5-tris(4-aminophenyl)benzene and 1 ml of bromoisobutyryl bromide in 10 ml of dichloromethane solution, place in an ice bath and stir for 10 min. 2ml of triethylamine solution was slowly added and stirred overnight at room temperature. After the reaction, it was purified by column chromatography, and the eluents were petroleum ether and ethyl acetate. The obtained solid was recrystallized with 10 ml of absolute ethanol to obtain a white solid of the three-armed ATRP initiator.
[0032] (2) Dissolve 0.5 g of three-arm ATRP initiator, 0.3 ml of tris(2-dimethylaminoethyl)amine, 0.1 g of cuprous bromide, and 1 ml of tert-butyl acrylate in DMF solution. Freezing-thawing and degassing were performed three times in succession, and then placed in an oil bath at 90°C for 24 hours after filling with argon for protection. Af...
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The invention provides a three-arm ATRP (atom transfer radical polymerization) initiator with plane conjugated structure, and preparation and application thereof, relating to ATRP initiators. The preparation method comprises the following steps: dissolving 1,3,5-tri(4-aminophenyl)benzene and bromoisobutyryl bromine in a dichloromethane solution, stirring under ice bath conditions, adding a triethylamine solution to react, purifying by column chromatography, and recrystallizing the obtained solid with anhydrous ethanol, thereby obtaining the three-arm ATRP initiator with plane conjugated structure. The three-arm ATRP initiator with plane conjugated structure can be applied to a self-assembly solution of an amphiphilic three-arm white solid polymer, a three-arm amphiphilic block polymer or a three-arm amphiphilic polymer. The preparation method has the advantages of simple synthesis steps and high yield; and the three-arm ATRP initiator has the advantages of high plane conjugation, rich electrons, high initiation activity and high chain transfer efficiency. The three-arm ATRP initiator is applicable to ATRP controllable polymerization of various monomers, and fills up the blank in the plane conjugated rich-electron aromatic ring ATRP initiator.
Description
technical field [0001] The invention relates to an ATRP initiator, in particular to a three-arm ATRP initiator with a planar conjugated structure and its preparation and application. Background technique [0002] Atom transfer radical polymerization (atomtransferradicalpolymerization, ATRP) is the most widely used polymer synthesis method. The polymerization method has the dual characteristics of free radical polymerization and living polymerization at the same time, and has good universality, strong controllability and low cost. The polymer synthesized by this method can not only achieve the expected polymer molecular weight, but also achieve a narrow distribution range of the polymer and a high yield, so it is an effective tool for the design of a new type of macromolecular structure. In recent years, the synthesis of multi-armed and star-shaped polymers by ATRP polymerization is common, and has gradually become a research hotspot in the field of polymer chemistry. At pr...
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Login to View More IPC IPC(8): C08F4/00C08F120/18C08F293/00C08F220/18C08J3/07C07C231/02C07C233/43
CPCC07C231/02C07C233/43C08F4/00C08F120/18C08F220/18C08F220/1804C08F293/005C08F2438/01C08J3/07C08J2353/00C08F293/00
Inventor 戴李宗吴俣哲袁丛辉毛杰李云同许一婷曾碧榕罗伟昂
Owner XIAMEN UNIV