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Method for preparing porous material by reversible addition fragmentation chain transfer polymerization of high internal phase emulsion

A technology of high internal phase emulsion and chain transfer polymerization, which is applied in the field of preparation of porous polymer materials by reversible addition-fragmentation chain transfer polymerization of high internal phase emulsion. Improved performance, mechanical properties, good control effects

Inactive Publication Date: 2012-06-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But at the same time, high porosity also makes the mechanical properties of the material poor. Such a weak support structure greatly limits its application range, which is the biggest problem in high internal phase emulsion polymerization today.

Method used

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  • Method for preparing porous material by reversible addition fragmentation chain transfer polymerization of high internal phase emulsion
  • Method for preparing porous material by reversible addition fragmentation chain transfer polymerization of high internal phase emulsion
  • Method for preparing porous material by reversible addition fragmentation chain transfer polymerization of high internal phase emulsion

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Experimental program
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Effect test

Embodiment 1

[0035] Embodiment 1: traditional method prepares porous polymer material

[0036] The oil phase was prepared by mixing 1.934 parts of styrene, 0.822 parts of divinylbenzene, and 0.908 parts of Span 80. An aqueous phase was obtained by mixing 0.252 parts of anhydrous calcium chloride, 0.046 parts of potassium persulfate and 18.251 parts of water. Stir the oil phase at a speed of 400 rpm, add the water phase to the oil phase drop by drop, stir and mix, and continue stirring for 0.5 hours after the addition is complete. Transfer the emulsion into the reactor and raise the temperature to 60°C to initiate polymerization, stop the reaction after 24 hours of polymerization, slowly cool to room temperature and discharge; extract the product and dry it in vacuum to obtain a porous polymer material sample 1, such as figure 1 (a) and (b) shown.

Embodiment 2

[0038] The oil phase was prepared by mixing 1.934 parts of styrene, 0.822 parts of divinylbenzene, 0.070 parts of chain transfer agent RAFT (1), and 0.908 parts of Span80. An aqueous phase was obtained by mixing 0.252 parts of anhydrous calcium chloride, 0.045 parts of potassium persulfate and 18.251 parts of water. Stir the oil phase at a speed of 400 rpm, add the water phase to the oil phase drop by drop, stir and mix, and continue stirring for 0.5 hours after the addition is complete. Put the emulsion into the reactor and raise the temperature to 60°C to initiate polymerization, stop the reaction after 24 hours of polymerization, slowly cool to room temperature and discharge; extract the product and dry it in vacuum to obtain a porous polymer material sample 2, such as figure 1 (c) and (d) shown.

[0039] from figure 1 It can be seen that the wall surface of sample 2 is smoother than that of sample 1, the pinholes in the pore wall disappear, and the number of connecting c...

Embodiment 3

[0044] The oil phase was prepared by mixing 1.934 parts of styrene, 0.822 parts of divinylbenzene, 0.069 parts of chain transfer reagent RAFT (2), and 0.908 parts of Span80. An aqueous phase was obtained by mixing 0.51 parts of anhydrous calcium chloride, 0.09 parts of potassium persulfate and 36.5 parts of water. Stir the oil phase at a speed of 400 rpm, add the water phase to the oil phase drop by drop, stir and mix, and continue stirring for 0.5 hours after the addition is complete. The emulsion was transferred into a reactor and the temperature was raised to 60°C to initiate polymerization. The reaction was stopped after 24 hours of polymerization, and the material was discharged after being slowly cooled to room temperature. The product was extracted and vacuum-dried to obtain a porous polymer material sample 3. Experiments have proved that the wall surface of the porous polymer material prepared in this embodiment is smoother, pinholes are greatly reduced or even disappe...

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Abstract

The invention discloses a method for preparing a porous material by the reversible addition fragmentation chain transfer polymerization of a high internal phase emulsion. The method comprises the following steps of: mixing a vinyl monomer, a polyvinyl monomer, a surfactant and a chain transfer reagent to form an oil phase; dissolving an electrolyte and a water-soluble initiator in deionized water to form a water phase; dropwise adding the water phase into the oil phase and stirring to form an emulsion system, and continuously stirring and carrying out pre-emulsification to form the high internal phase emulsion; transferring the high internal phase emulsion into a reactor, heating up to the temperature of 60-70 DEG C so as to initiate polymerization, stopping reaction after the polymerization is carried out for 24-48 hours, and cooling to room temperature; and carrying out extraction by adopting deionized water and a good solvent, and putting products into a vacuum baking oven and carrying out vacuum drying to obtain the porous polymeric material. According to the method, the chain transfer reagent and an activated / controllable free radical polymerization method are applied to a high internal phase emulsion template method, the open-cell porous material is successfully prepared, the method is simple and environment-friendly in process, and the mechanical properties of the material are greatly improved.

Description

technical field [0001] The invention relates to a technique for preparing a porous material by using a template method, in particular to a method for preparing a porous polymer material by reversible addition-fragmentation chain transfer polymerization of a high internal phase emulsion. Background technique [0002] High internal phase emulsion (High Internal Phase Emulsion, HIPE), also known as high-concentration emulsion, the volume fraction of its dispersed phase is higher than 74%. The volume fraction of the dispersed phase in the ordinary emulsion system is generally 30%-40%, and the small droplets are dispersed in the continuous phase in the form of unconnected spheres, while in the high internal phase emulsion, with the further increase of the components of the dispersed phase, The droplets squeeze each other to form a polyhedral liquid cell separated by a continuous phase film, like a honeycomb structure. The continuous phase monomer undergoes a polymerization react...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F212/36C08F222/14C08F220/32C08F220/18C08F2/44C08F2/38C08F2/24C08J9/26
Inventor 王安妮高翔罗英武
Owner ZHEJIANG UNIV
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