Rapid generation and control of microporosity, bimodal pore size distribution, and surface area in Davankov-type hyper-cross-linked resins

J.H. Ahn, J.E. Jang, C.G. Oh, S.K. Ihm, J. Cortez, D.C. Sherrington

Research output: Contribution to journalArticle

212 Citations (Scopus)

Abstract

Synthesis of Davankov-type hyper-cross-linked resin beads has been carried out using gel-type and permanently porous poly(divinylbenzene-co-vinylbenzyl chloride) (DVB-VBC) precursor resins without any external electrophile. Of the Lewis acids examined (FeCl3, AlCl3, SnCl4), FeCl3 was by far the most effective catalyst. Rather remarkably in the case of a gel-type 2 mol % DVB-VBC precursor, extensive microporosity was generated within only 15 min of initiating the cross-linking reaction, yielding a surface area (N-2 sorption/BET) of similar to 1200 in which rose steadily to a maximum approaching 2000 m(2) g(-1) in after 18 h. In the case of porous DVB-VBC precursor resins, the presence of discrete pores in the precursor, accompanied by a micropore fraction on hyper-cross-linking, yields resins with a clearly bimodal distribution of pores. Manipulation of the Friedel-Crafts reaction variables and the structure of the precursor resin allows final resin products to be prepared with surface areas in the range similar to 300-2000 m(2) g(-1).
Original languageEnglish
Pages (from-to)627-632
Number of pages5
JournalMacromolecules
Volume39
Issue number2
DOIs
Publication statusPublished - 24 Jan 2006

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Microporosity
Pore size
divinyl benzene
Resins
Chlorides
Gels
Friedel-Crafts reaction
Lewis Acids
Sorption
Catalysts
Acids

Keywords

  • HYPERCROSSLINKED POLYMERIC ADSORBENTS
  • STYRENE-DIVINYLBENZENE COPOLYMERS
  • SOLID-PHASE EXTRACTION
  • PENDANT VINYL GROUPS
  • POLAR COMPOUNDS
  • POLYSTYRENE
  • SORPTION
  • ADSORPTION
  • NETWORKS
  • BEADS

Cite this

Ahn, J.H. ; Jang, J.E. ; Oh, C.G. ; Ihm, S.K. ; Cortez, J. ; Sherrington, D.C. / Rapid generation and control of microporosity, bimodal pore size distribution, and surface area in Davankov-type hyper-cross-linked resins. In: Macromolecules. 2006 ; Vol. 39, No. 2. pp. 627-632.
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Rapid generation and control of microporosity, bimodal pore size distribution, and surface area in Davankov-type hyper-cross-linked resins. / Ahn, J.H.; Jang, J.E.; Oh, C.G.; Ihm, S.K.; Cortez, J.; Sherrington, D.C.

In: Macromolecules, Vol. 39, No. 2, 24.01.2006, p. 627-632.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Rapid generation and control of microporosity, bimodal pore size distribution, and surface area in Davankov-type hyper-cross-linked resins

AU - Ahn, J.H.

AU - Jang, J.E.

AU - Oh, C.G.

AU - Ihm, S.K.

AU - Cortez, J.

AU - Sherrington, D.C.

PY - 2006/1/24

Y1 - 2006/1/24

N2 - Synthesis of Davankov-type hyper-cross-linked resin beads has been carried out using gel-type and permanently porous poly(divinylbenzene-co-vinylbenzyl chloride) (DVB-VBC) precursor resins without any external electrophile. Of the Lewis acids examined (FeCl3, AlCl3, SnCl4), FeCl3 was by far the most effective catalyst. Rather remarkably in the case of a gel-type 2 mol % DVB-VBC precursor, extensive microporosity was generated within only 15 min of initiating the cross-linking reaction, yielding a surface area (N-2 sorption/BET) of similar to 1200 in which rose steadily to a maximum approaching 2000 m(2) g(-1) in after 18 h. In the case of porous DVB-VBC precursor resins, the presence of discrete pores in the precursor, accompanied by a micropore fraction on hyper-cross-linking, yields resins with a clearly bimodal distribution of pores. Manipulation of the Friedel-Crafts reaction variables and the structure of the precursor resin allows final resin products to be prepared with surface areas in the range similar to 300-2000 m(2) g(-1).

AB - Synthesis of Davankov-type hyper-cross-linked resin beads has been carried out using gel-type and permanently porous poly(divinylbenzene-co-vinylbenzyl chloride) (DVB-VBC) precursor resins without any external electrophile. Of the Lewis acids examined (FeCl3, AlCl3, SnCl4), FeCl3 was by far the most effective catalyst. Rather remarkably in the case of a gel-type 2 mol % DVB-VBC precursor, extensive microporosity was generated within only 15 min of initiating the cross-linking reaction, yielding a surface area (N-2 sorption/BET) of similar to 1200 in which rose steadily to a maximum approaching 2000 m(2) g(-1) in after 18 h. In the case of porous DVB-VBC precursor resins, the presence of discrete pores in the precursor, accompanied by a micropore fraction on hyper-cross-linking, yields resins with a clearly bimodal distribution of pores. Manipulation of the Friedel-Crafts reaction variables and the structure of the precursor resin allows final resin products to be prepared with surface areas in the range similar to 300-2000 m(2) g(-1).

KW - HYPERCROSSLINKED POLYMERIC ADSORBENTS

KW - STYRENE-DIVINYLBENZENE COPOLYMERS

KW - SOLID-PHASE EXTRACTION

KW - PENDANT VINYL GROUPS

KW - POLAR COMPOUNDS

KW - POLYSTYRENE

KW - SORPTION

KW - ADSORPTION

KW - NETWORKS

KW - BEADS

UR - http://pubs.acs.org/cgi-bin/article.cgi/mamobx/2006/39/i02/pdf/ma051152n.pdf

UR - http://dx.doi.org/10.1021/ma051152n

U2 - 10.1021/ma051152n

DO - 10.1021/ma051152n

M3 - Article

VL - 39

SP - 627

EP - 632

JO - Macromolecules

JF - Macromolecules

SN - 0024-9297

IS - 2

ER -