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Preparation methods of cyclic macromolecular chain transfer agent and cyclic-comb polymers comprising cyclic macromolecular chain transfer agent

A technology of macromolecular chains and transfer agents, which is applied in the field of polymer material synthesis, can solve the difficult problems of ring-comb polymer grafting density controllability, and no ring-comb polymers have been seen, so as to achieve a variety of Effect

Active Publication Date: 2016-04-13
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, "Graftthrough" and "Graftonto" are difficult to achieve the controllability of the graft density of the ring comb polymer, and the "Graftfrom" method is the most potential way to realize the controllability of the ring comb polymer graft density direction; but there is no report on ring comb polymers based on ring macromolecules

Method used

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  • Preparation methods of cyclic macromolecular chain transfer agent and cyclic-comb polymers comprising cyclic macromolecular chain transfer agent
  • Preparation methods of cyclic macromolecular chain transfer agent and cyclic-comb polymers comprising cyclic macromolecular chain transfer agent
  • Preparation methods of cyclic macromolecular chain transfer agent and cyclic-comb polymers comprising cyclic macromolecular chain transfer agent

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Experimental program
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Embodiment 1

[0048] Synthesis of embodiment one cyclic macromolecular chain transfer agent

[0049] Add 5.6g (0.1mol) of propynyl alcohol and 100mL of dichloromethane solvent into a 250mL three-necked flask, then add 12.2g (0.12mol) of triethylamine, cool it down to 0~5°C with an ice-water bath, and then Slowly add 27.6g (0.12mol) 2-bromoisobutyryl bromide into the reaction flask dropwise, stir for 30min after the dropwise addition, remove the ice-water bath and react for 12h, filter with suction, wash the filtrate with water, saturated sodium carbonate solution, and saturated saline Once, dried with anhydrous sodium sulfate for 2 h, concentrated to obtain a crude product, and then distilled under reduced pressure to obtain 10.2 g of the final product PBiB, yield: 50%.

[0050] Add 9.06 g (87.0 mmol) St, 178.4 mg (0.87 mmol) PBiB, 55.8 mg (0.25 mmol) CuBr, 130.0 mg (0.75 mmol) PMDETA, 87.5 mg (0.5 mmol) VC and 10 mL anisole to 25 mL Schlenk In the bottle, react in an oil bath at 90°C for ...

Embodiment 2

[0060] Add St, 2-propargyl bromopropionate, copper iodide, 2,2'-bipyridine, phenol and 10 mL anisole into a 25 mL Schlenk bottle, and react in an oil bath at 110 °C for 5 h. After the reactant was dissolved in THF, the copper salt was removed through a neutral alumina column, then precipitated with methanol and suction filtered, and dried in a vacuum oven for 24 hours to finally obtain a white powdered linear polystyrene ( l -PS); will l -PS, NaN 3 Add DMF and DMF into a 25mL round-bottom flask, react in an oil bath at 25°C for 24h, dissolve the reactant in THF, remove the azide reagent through a neutral alumina column, precipitate with methanol and suction filter, vacuum box After drying for 24 hours, the white powdery azide linear polystyrene ( l -PS-N 3 ); Add toluene into a 1000mL three-necked flask, pass through nitrogen to remove oxygen overnight, add triethylamine, tripropylene glycol methyl ether acetate and cuprous chloride to the 1000mL three-necked flask in seque...

Embodiment 3

[0061] The preparation of embodiment tricyclic comb polymer

[0062] in turn c -PSN (8.39mg, 0.048mmol), St (1.00g, 9.6mmol), AIBN (3.94mg, 0.024mmol) and toluene (1mL) were added to a 5mL ampoule, and the gas was pumped several times at low temperature, Seal the tube under an oxygen-free atmosphere. Place the sealed ampoule in a heating mantle at 90°C, and react according to the predetermined time (1-48 hours). Immediately after the reaction, cool the sealed tube with cold water. After opening the sealed tube, dissolve the polymer with tetrahydrofuran, pour it into 250 mL of methanol and leave it overnight, filter it with suction, and dry it to obtain ring-comb polystyrene with different side chain lengths. c -PSN- g -PS. This process requires strict oxygen removal. During the polymerization process, the molecular weight of the polymer can be controlled by adjusting the reaction time. For details, see Figure 5 and Table 2.

[0063] Table 2 c - Polymerization results o...

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Abstract

The invention discloses preparation methods of a cyclic macromolecular chain transfer agent and cyclic-comb polymers comprising the cyclic macromolecular chain transfer agent. To be specific, the method comprises steps as follows: 1) synthesis of cyclic polystyrene; 2) a benzylic bromination reaction of the cyclic polystyrene; 3) preparation of the cyclic macromolecular chain transfer agent through a nucleophilic substitution reaction; preparation of different cyclic-comb polymers on the basis of the cyclic macromolecular chain transfer agent. The cyclic macromolecular chain is modified, a site capable of triggering RAFT polymerization is constructed, the cyclic macromolecular chain transfer agent is prepared for the first time, polymerization of multiple functional monomers is triggered, a series of cyclic-comb polymers with different main chains and different densities of side chains are prepared, and the grafting density of the cyclic-comb polymers can be regulated by controlling the feed ratio of reaction materials.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and in particular relates to a ring-shaped macromolecular chain transfer agent and a preparation method of a ring-comb polymer. Background technique [0002] As one of the oldest topological structures, cyclic polymers and their derivatives have risen again in the fields of synthetic chemistry and macromolecular structure, and are favored by researchers. Compared with the corresponding linear polymer precursors, cyclic polymers rely on the existence of no end groups to exhibit many excellent properties, such as smaller hydrodynamic size, higher glass transition temperature, larger refractive index, etc. etc., have been well applied in the fields of biomedicine, materials science, supramolecules and self-assembly. For its synthesis method, it can be mainly classified into two categories: ring expansion method and ring closure method. The two methods have their own advantages and disadvan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/08C08F257/02C08F8/48C08F212/08C08F218/08
CPCC08F112/08C08F257/02C08F8/48C08F212/08C08F218/08
Inventor 张伟张双双朱秀林殷露张正彪朱健周年琛
Owner SUZHOU UNIV
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