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Macromolecules
Volumn 32, Issue 19, 1999, Pages 6377-6379
Control of porous properties and surface chemistry in "molded" porous polymer monoliths prepared by polymerization in the presence of TEMPO
Author keywords

[No Author keywords available]
Indexed keywords

COMPOSITION; FREE RADICAL POLYMERIZATION; ORGANIC POLYMERS; PORE SIZE; POROSITY; REACTION KINETICS; SURFACE CHEMISTRY;
EID: 0342939540     PISSN: 00249297     EISSN: None     Source Type: Journal    
DOI: 10.1021/ma990538t     Document Type: Article
Times cited : (105)
References (26)
  • 4
    • 0642375805 scopus 로고    scopus 로고
    • and references therein
    • Hawker, C. J. Ace. Chem. Res. 1997,30, 373 and references therein,
    • (1997) Ace. Chem. Res. , vol.30 , pp. 373
    • Hawker, C.J.1
  • 16
    • 85037475774 scopus 로고    scopus 로고
    • Benzoyl peroxide (BPO; 0.5 wt % with respect to the monomers) and TEMPO when specified (1.2 molar excess with respect to BPO) were dissolved in a mixture of 20 wt % divinylbenzene (80% grade), 20 wt % styrène, and 60 wt % 1-dodecanol. Equal portions of this mixture (5 g) were weighed into glass ampules and deaerated using three freeze-pump-thaw cycles. The ampules were then sealed under vacuum and submerged in a 130 °C oil bath. The monoliths obtained after different polymerization times were extracted with methanol for 12 h, dried at 60 °C, and weighed to determine the percentage of monomer incorporation.
    • Benzoyl peroxide (BPO; 0.5 wt % with respect to the monomers) and TEMPO when specified (1.2 molar excess with respect to BPO) were dissolved in a mixture of 20 wt % divinylbenzene (80% grade), 20 wt % styrène, and 60 wt % 1-dodecanol. Equal portions of this mixture (5 g) were weighed into glass ampules and deaerated using three freeze-pump-thaw cycles. The ampules were then sealed under vacuum and submerged in a 130 °C oil bath. The monoliths obtained after different polymerization times were extracted with methanol for 12 h, dried at 60 °C, and weighed to determine the percentage of monomer incorporation.
  • 17
    • 85037481836 scopus 로고    scopus 로고
    • The pore size distribution and specific surface area were determined in the dry state by mercury intrusion porosim-etry and nitrogen adsorption/desorption (BET), respectively, using Autopore and ASAP 2010 instruments (Micromeritics, Norcross, GA).
    • The pore size distribution and specific surface area were determined in the dry state by mercury intrusion porosim-etry and nitrogen adsorption/desorption (BET), respectively, using Autopore and ASAP 2010 instruments (Micromeritics, Norcross, GA).
  • 20
    • 85037469704 scopus 로고    scopus 로고
    • The monolithic column for ISEC was prepared by polymerization of a TEMPO-containing mixture at 130 °C for 20 h in a 50 × 8 mm i.d. stainless steel tube fitted with a 10 mm long Teflon tubular extension to eliminate the formation of void volume at the top of the column. After attachment to a Waters HPLC system and washing for 3 h with THF at a flow rate of 0.2 mL/min, solutions of toluene and polystyrene standards in THF were injected at a flow rate of 0.2 mL/min to obtain the calibration curve.
    • The monolithic column for ISEC was prepared by polymerization of a TEMPO-containing mixture at 130 °C for 20 h in a 50 × 8 mm i.d. stainless steel tube fitted with a 10 mm long Teflon tubular extension to eliminate the formation of void volume at the top of the column. After attachment to a Waters HPLC system and washing for 3 h with THF at a flow rate of 0.2 mL/min, solutions of toluene and polystyrene standards in THF were injected at a flow rate of 0.2 mL/min to obtain the calibration curve.
  • 25
    • 85037458748 scopus 로고    scopus 로고
    • The large diameter column experiments were performed as described in ref 13.
    • The large diameter column experiments were performed as described in ref 13.
  • 26
    • 85037486491 scopus 로고    scopus 로고
    • Grafting was carried out in a glass vial at 130 °C for 20 h with a mixture of 0.4 g of crushed monolith prepared in the presence of TEMPO and 4 mL of a 25 vol % solution of the appropriate monomer in cyclohexanol. The product was extracted with methanol for 48 h, dried, and analyzed by FT-IR spectroscopy and elemental analysis.
    • Grafting was carried out in a glass vial at 130 °C for 20 h with a mixture of 0.4 g of crushed monolith prepared in the presence of TEMPO and 4 mL of a 25 vol % solution of the appropriate monomer in cyclohexanol. The product was extracted with methanol for 48 h, dried, and analyzed by FT-IR spectroscopy and elemental analysis.

* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.