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Method of preparing organic porous material through photo-induced electro transfer - reversible addition fragmentation chain transfer polymerization

A technology of chain transfer polymerization and electron transfer, which is applied in the field of polymer materials to achieve the effects of shortening the preparation cycle, regular structure and accelerating mass transfer

Inactive Publication Date: 2018-06-29
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of organic porous materials by photoinduced electron transfer-reversible addition-fragmentation chain transfer polymerization using O / W / O emulsion has not been reported yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Stir and mix 2.653 g of acrylonitrile, 1.13 g of divinylbenzene, 0.095 g of 4-cyanopentanoic acid dithiobenzoic acid, and 0.9 g of polyoxyethylene lauryl ether to obtain an oil phase. The photoredox catalyst TiO 2 1.8 mg and 28.9 g of water were mixed to obtain an aqueous phase. Add the oil phase to the water phase drop by drop under stirring, and then continue to stir, then add 10 ml of toluene, and continue to stir. Add the obtained emulsion into 30 mL of toluene containing 5 g of polyoxyethylene lauryl ether, stir for a while, and pass nitrogen to remove oxygen. At room temperature, the reaction was carried out under light. After the reaction is finished, it is filtered, extracted, and vacuum-dried to obtain a porous oil machine material.

Embodiment 2

[0014] Stir and mix 1.976 g methyl methacrylate, 0.84 g divinylbenzene, 0.083 g 4-cyanovaleric acid dithiobenzoic acid, and 0.85 g polyoxyethylene lauryl ether to obtain an oil phase. 0.05 mg of the photoredox catalyst Eosin Y and 30.3 g of water were mixed to obtain an aqueous phase. Add the oil phase to the water phase drop by drop under stirring, continue to stir after completion, then add 12 ml of cyclohexane, and continue to stir. Add the obtained emulsion into 30 ml of cyclohexane containing 4.6 g of polyoxyethylene lauryl ether, stir for a period of time, and pass nitrogen to remove oxygen. At room temperature, the reaction was carried out under light. After the reaction is finished, it is filtered, extracted, and vacuum-dried to obtain a porous oil machine material.

Embodiment 3

[0016] Stir and mix 1.685 g of styrene, 0.72 g of divinylbenzene, 0.078 g of 4-cyanopentanoic acid dithiobenzoic acid, and 0.92 g of polyoxyethylene lauryl ether to obtain an oil phase. The photoredox catalyst ZnO 1.6 mg and 36.3 g water were mixed to obtain an aqueous phase. Add the oil phase to the water phase drop by drop under stirring, continue stirring after completion, then add 8 ml of n-hexane, and continue stirring. The obtained emulsion was added to 35 ml of n-hexane containing 6.2 g of polyoxyethylene lauryl ether, stirred for a period of time, and nitrogen was removed to remove oxygen. At room temperature, the reaction was carried out under light. After the reaction is finished, it is filtered, extracted, and vacuum-dried to obtain a porous oil machine material.

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PUM

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Abstract

The invention discloses a method of preparing an organic porous material through photo-induced electro transfer - reversible addition fragmentation chain transfer polymerization (RAFT) in an oil / water / oil (O / W / O) double emulsion system. The method includes steps of: under stirring, dropwise adding an oil phase to a water phase, wherein the oil phase includes a polymerizable functional monomer, a crosslinker, a chain transfer reagent and a surfactant and a continuous phase is a water solution of a photo-redox catalyst; dropwise adding an organic solvent to a water phase, continuously stirring the mixture for a certain time to form an oil / water emulsion (O / W); dropwise adding the O / W emulsion to an organic solvent containing a surfactant and further stirring the mixture to prepare the O / W / Oemulsion; feeding nitrogen to displace oxygen, and performing light-irradiation polymerization reaction at room temperature to obtain the organic porous material. The organic porous material has a regular spherical structure, and contains large quantity of pores on surface and in interior.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, in particular to a method for preparing organic porous materials through photoinduced electron transfer-reversible addition-fragmentation chain transfer polymerization. Background technique [0002] Reversible Addition-Fragmentation Chain Transfer (RAFT) Polymerization as an Efficient Method for Preparing Controlled Polymerization Polymers (JohnChiefari, Y. K. (Bill) Chong, Frances Ercole, Julia Krstina, Justine Jeffery, Tam P. T. Le, Roshan T. A. Mayadunne, Gordon F . Meijs, Catherine L. Moad, Graeme Moad, Ezio Rizzardo and San H. Thang Living Free-Radical Polymerization by Reversible Addition−Fragmentation Chain Transfer:  The RAFT Process. Macromolecules, 1998, 31(16): 5559-5562.). RAFT adds a chain transfer agent (CTA) to the system, which can effectively establish the balance between active growth free radicals and dormant species. With the increase of monomer conversion rate, the ...

Claims

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Application Information

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IPC IPC(8): C08F220/44C08F220/14C08F212/08C08F212/36C08F220/56C08F222/14C08F2/30C08F2/38C08F2/48C08J9/28C08L33/26
CPCC08F2/30C08F2/38C08F2/48C08F212/08C08F220/14C08F220/44C08F220/56C08J9/28C08J2325/08C08J2333/12C08J2333/20C08J2333/26C08F212/36C08F222/102
Inventor 王国祥梁恩湘曾乐林
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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