Method for preparing photosensitive graft polymer containing double-azobenzene

A technology of grafting polymer and bisazobenzene is applied in the field of preparation of photosensitive grafting polymer, which can solve the problems of single structure and low molecular weight of polymer, and achieve the effect of convenient design.

Active Publication Date: 2015-07-01
JIANGSU XUETAI PRINTING
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Problems solved by technology

[0003] Living cationic polymerization and AGET ATRP have different advantages and disadvantages: the polymerization process of living cationic polymerization is strictly controlled under anhydrous and anaerobic conditions, and the controllability of the obtained polymer is better than that of general living radical polymerization
[0005] At present, the azobenzene-containing monomers reported at home and abroad are functional polymers synthesized through separate living cationic polymerization and AGET ATRP. The structure is single and the molecular weight of the polymer is not large.

Method used

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  • Method for preparing photosensitive graft polymer containing double-azobenzene
  • Method for preparing photosensitive graft polymer containing double-azobenzene
  • Method for preparing photosensitive graft polymer containing double-azobenzene

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preparation example Construction

[0034] A preparation method of a photosensitive graft polymer containing bisazobenzene, comprising the following steps:

[0035] Step 1) Use p-nitroaniline and phenol as raw materials to synthesize p-nitroazophenol, and carry out sequential chain reaction of phenolic hydroxyl group to alcoholic hydroxyl group; nitro group is reduced to amino group; and phenol azotization to introduce disazo group group; phenolic hydroxyl group and 2-chloroethyl vinyl ether carry out electrophilic substitution reaction to introduce vinyl ether group as monomer for living cationic polymerization; alcoholic hydroxyl group and α -Bromoisobutyryl bromide introduced by esterification α -Bromoisobutyl group as the initiator of AGET ATRP; the final compound obtained is 4-(4-(4-(4-(2-vinyloxy)ethoxy)azophenyl)azophenyl )phenoxy- α- Hexyl bromoisobutyrate (VEBiB);

[0036] Step 2) Using toluene as solvent, the concentration of each component is: monomer (1) 0.76 mol / L, monomer (2) 0.02-0.04 mol / L, Le...

Embodiment 1

[0052] Embodiment one: the synthesis of active cationic monomer AGET ATRP initiator compound VEBiB ( figure 1 )

[0053] Add p-nitroaniline (6.9 g, 50.0 mmol), 30 mL of deionized water and 15 mL of concentrated hydrochloric acid and stir in an ice-water bath to dissolve. o Slowly add sodium nitrite solution (3.9 g, 10 mL) dropwise at ℃, react for 40 min to make diazo component, phenol (8.0 g, 85.0 mmol), NaOH (4.0 g, 100.0 mmol), NaHCO 3 (4.2 g, 50.0 mmol) and 250 mL deionized water were stirred in an ice-water bath to form a coupling solution, and the pH was kept at 8~10, and the temperature was 0~5 o During C, the diazo component was added dropwise to the coupling solution, and the final mixed solution was reacted for 2 h, filtered, dried in vacuo, and purified by recrystallization from absolute ethanol to obtain a dark red compound (1).

[0054] DMF was used as a solvent to dissolve compound (1) (6.1 g, 25.0 mmol) in stirring, then add 6-bromohexanol (5.4 g, 30.0 mmol), K...

Embodiment 2

[0059] Embodiment two: the active cationic copolymerization of IBVE and VEBiB

[0060] In the glove box, take monomer VEBiB (0.02 mol / L, 0.135 g), monomer IBVE (0.76 mol / L, 1 mL), solvent toluene, add alkali ethyl acetate (1 mol / L, 0.98 mL), Lewis acid catalyst Et 1.5 AlCl 1.5 (20 mmol / L, 0.5 mL), cationic initiator IBEA (4 mmol / L, 7 μL) were put into a 30 mL polymerization bottle and placed at 0 o C reacts according to the predetermined time (1~24 h). At the end of the polymerization, a terminator is added, and methanol containing a small amount of ammonia water is used to terminate the reaction. The mixture is taken out from the glove box and precipitated with methanol, filtered, and dried to obtain the polymer PIBVE- co -PVEBiB, GPC and 1 H NMR characterization.

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Abstract

The invention discloses a method for preparing a photosensitive graft polymer containing double-azobenzene. The method comprises the following steps of: firstly, synthetizing compound 4-(4-(4-(4-(2-ethyleneoxy) ethyoxyl) azo phenyl) azo phenyl) phenoxy-alpha-bromo-isobutyl acid ester (VEBiB); then synthetizing a vinyl ether copolymer containing an alpha-bromo-isobutyl group on a branched chain; and finally synthetizing the photosensitive graft polymer containing the double-azobenzene. By adopting the technical scheme disclosed by the invention, the molecular weight can be conveniently designed; and the molecular weight distribution index of the polymer is in the controllable range. Thus, different molecular weights of photosensitive graft polymers containing the double-azobenzene can be controllably designed.

Description

technical field [0001] The invention relates to a preparation method of a photosensitive graft polymer containing bis-azobenzene. Background technique [0002] Both AGET ATRP and living cationic polymerization technology have the characteristics of controllable activity, and they can synthesize high molecular weight polymers with narrow molecular weight distribution index and expected molecular weight. Both can synthesize a variety of structures with different functions (such as light response, pH response, temperature response and solvent response, etc.), different types (such as grafting, block and copolymerization, etc.), and different Regular polymers with terminal functional groups. [0003] Living cationic polymerization and AGET ATRP have different advantages and disadvantages: the polymerization process of living cationic polymerization is strictly controlled under anhydrous and anaerobic conditions, and the controllability of the obtained polymer is better than tha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F261/06C08F220/14C08F216/18C08F216/14
Inventor 程振平陶美霞张丽芬李铭朱秀林
Owner JIANGSU XUETAI PRINTING
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