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Preparation method of ring brush polymer containing polystyrene main chain

A technology of polystyrene and linear polystyrene, which is applied in the field of preparation of ring-brush polymers, can solve difficult problems and achieve the effects of fast reaction rate, high yield and mild reaction conditions

Active Publication Date: 2015-04-29
苏州吉尼尔机械科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to further improve the performance of the polymer, it is possible to consider adjusting the grafting density of the ring-brush polymer, which is a very promising method, but it is obviously difficult to do this for the "Graft through" method

Method used

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  • Preparation method of ring brush polymer containing polystyrene main chain
  • Preparation method of ring brush polymer containing polystyrene main chain
  • Preparation method of ring brush polymer containing polystyrene main chain

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Embodiment 1: Cyclic polystyrene ( c -PS) synthesis (specific synthetic route such as figure 1 shown).

[0078] 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 bottle, 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%.

[0079] 9.06g (87.0mmol) St, 178.4mg (0.87mmol) PBiB, 55.8mg (0.25mmol) CuBr 2 , 130.0mg (0.75mmol) PMDETA, 87.5mg (0.5mmol) VC and 10mL anisole were added to a 25mL Schlenk bottle, and reacted in...

Embodiment 2

[0082] Embodiment 2: the bromination of cyclic polystyrene (reaction scheme is referring to Figure 5 ).

[0083] 300mg (repeating unit 2.88mmol) c -PS, 153.8mg (0.86mmol) NBS, 94.58mg (0.58mmol) AIBN and 50mL CCl 4 Add it into a 100mL round-bottomed flask, stir at room temperature for 30min, and heat to 80°C under reflux to react overnight. Suction filter the reaction solution to remove the floating flocs in the upper layer, wash the filtrate with 0.1M sodium thiosulfate solution and water several times, concentrate the organic phase, precipitate it with methanol and filter it with suction, dissolve it with THF, precipitate it with methanol and filter it with suction. Vacuum drying for 24h gave 238.0 mg of yellow powdered brominated cyclic polystyrene ( c -PS-Br). Use NBS / AIBN / CCl in this process 4 system, the bromine content in the polymer can be adjusted by adjusting the ratio of styrene repeating unit to NBS and AIBN, so as to control the number of side chains of the ...

Embodiment 3

[0085] Embodiment 3: Brominated cyclic polystyrene initiates St polymerization as a macroinitiator (reaction scheme sees Figure 5 ).

[0086]10.31mg (0.087mmol) brominated cyclic polystyrene macromolecular initiator, 12.45mg (0.087mmol) cuprous bromide, 0.9060g (8.7mmol) styrene monomer, 15.08 (0.087mmol) PMDETA ligand Add it into a 5mL ampoule bottle, use anisole as the solvent, and seal the tube under an oxygen-free atmosphere after pumping out the gas several times at low temperature. Place the sealed ampoule in a heating mantle at 90°C, and react according to the predetermined time (1-8 days). Immediately after the reaction, cool the sealed tube with cold water, open the sealed tube and dissolve the contents with tetrahydrofuran, pour it into 250mL of methanol and place it overnight, filter it with suction, and dry it to obtain ring brush-shaped polystyrene with different side chain lengths. This process requires strict oxygen removal. During the polymerization process,...

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Abstract

The invention discloses a preparation method of a ring brush polymer containing a polystyrene main chain. Particularly, the method comprises the following steps: (1) synthesizing linear polystyrene; (2) carrying out azidation of the linear polystyrene; (3) carrying out ring-closure reaction; (4) carrying out benzyl bromination of annular polystyrene; and (5) synthesizing the annular polystyrene. According to the preparation method, the ATRP reaction, CuAAC reaction and Woh1-Ziegler reaction are perfectly combined for the first time; the grafting density of the polymer is controlled by controlling the feeding ratio of reaction materials; the grafting length is controlled by controlling the reaction time; a series of ring brush polymers containing the polystyrene main chain are successfully prepared; and the controllability of the preparation method of the ring brush polymer is fundamentally achieved.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a preparation method of a ring-brush polymer whose main chain contains a polystyrene structure. Background technique [0002] Cyclic polymers are a class of polymers with a special topology. Because they have no end group structure, they exhibit many specific properties compared with linear polymers, such as a larger refractive index and a higher glass transition temperature. , greater density, smaller hydrodynamic size, lower intrinsic viscosity, etc. Due to their special performance advantages, cyclic polymers have been well applied in the fields of materials science, supramolecular and self-assembly, biomedicine, etc., and their synthesis methods have attracted the interest of many researchers. [0003] So far, the synthesis methods of cyclic polymers are mainly divided into two categories: one is the ring expansion method, and the other is the ring clos...

Claims

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Application Information

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IPC IPC(8): C08F257/02C08F212/08C08F8/20C08F8/48C08F8/30
Inventor 张伟张双双朱秀林王蕴姝潘向强周年琛张正彪朱健
Owner 苏州吉尼尔机械科技有限公司
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