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Volumn 12, Issue 4, 2009, Pages 312-315

Synthesis of nanoporous iminodiacetic acid sorbents for binding transition metals

Author keywords

Chelation; Ion chromatography; Ion exchange; Nanoporous; Self assembled monolayer; Sorbent

Indexed keywords


EID: 62649098179     PISSN: 13877003     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.inoche.2009.02.003     Document Type: Article
Times cited : (31)

References (36)
  • 25
    • 62649110455 scopus 로고    scopus 로고
    • Synthesis of IDAA silane. In a 1-L round bottomed flask, 30.5 mL (0.22 mol) of triethylamine was dissolved in 500 mL of dry tetrahydrofuran. The flask was then stoppered with a rubber septum and 24.4 mL (0.104 mol) of 3-aminopropyltriethoxysilane and 23.0 mL (0.208 mol) of ethyl bromoacetate (Caution! Lachrymator, were added sequentially via syringe. The mixture was stirred overnight under N2, then septum was removed and the flask fitted with a reflux condenser and mixture was heated to reflux for 5 h. At the end of this reflux period, it was cooled to room temperature and filtered to separate the precipitated Et3 N-HBr. The solvent was removed by distillation and the crude product subjected to vacuum distillation to afford 35.76 g (87.0 mmol; 84% yield) of a pale yellow liquid (bp 160-170 °C at 0.375 torr, 1H NMR (CDCl3) 4.15 (q, 4H, J, 7.2 Hz, 3.81 (q, 6H, J, 7.2 Hz, 3.55 (s, 4H, 2.71 (pt, 2H, J, 7.5 Hz, 1.59 (quintet, 2H, J, 8.1 Hz, 1.27 t, 6H
    • 3 N-HBr. The solvent was removed by distillation and the crude product subjected to vacuum distillation to afford 35.76 g (87.0 mmol; 84% yield) of a pale yellow liquid (bp 160-170 °C at 0.375 torr). 1H NMR (CDCl3) 4.15 (q, 4H, J = 7.2 Hz), 3.81 (q, 6H, J = 7.2 Hz), 3.55 (s, 4H), 2.71 (pt, 2H, J = 7.5 Hz), 1.59 (quintet, 2H, J = 8.1 Hz), 1.27 (t, 6H, J = 7.2 Hz), 1.22 (t, 9H, J = 7.0 Hz), and 0.61 (m, 2H). 13C NMR (CDCl3) 171.4, 60.4, 58.3, 57.3, 54.9, 21.2, 18.3, 14.2, and 7.6.
  • 26
    • 62649120104 scopus 로고    scopus 로고
    • Deposition into MCM-41. 10.017 g of MCM-41 (920 m2/g, 35 Å pores, 27,28] was suspended in 200 mL of toluene and treated with 3.2 mL of water to hydrate the silica surface [22, This slurry was stirred at room temperature overnight to insure uniform distribution of water throughout the sample. To this slurry, 11.0 g of the IDAA silane was added, and the mixture was heated to reflux for 4 h. After this reflux period, the reflux condenser was replaced with a short path distillation head and the ethanol and water azeotropes were removed via distillation. The product was then collected by vacuum filtration, washed copiously with 2-propanol and air-dried to give 13.752 g of a free-flowing white powder. Given that the original silica sample had a surface area of ∼9215 m2, and we observed a mass increase is 3.735g, if we assume a MW for the hydrolyzed silane of 267.05 g/mol (the HO-Si(O)-R assumption, see Ref, 19, this corresponds to approximatel
    • 2. For this silane, this corresponds to approximately 1.0 mmol/g.
  • 30
    • 62649142003 scopus 로고    scopus 로고
    • note
    • 3 solution to bleach out the color. At this point the sample was once again washed with water, and 2-propanol, then air-dried.
  • 31
    • 62649156944 scopus 로고    scopus 로고
    • note
    • f are the initial and final concentrations in the solution of the target species determined by ICP-MS, V is the solution volume in mL, and M is the mass in gram of the sorbent.
  • 34
    • 85047870218 scopus 로고    scopus 로고
    • For an excellent summary of the structure and properties of activated carbons, see:, Taylor & Francis, New York pp. 1-51
    • For an excellent summary of the structure and properties of activated carbons, see:. Bansal R.C., and Goyal M. Activated Carbon Adsorption (2005), Taylor & Francis, New York pp. 1-51
    • (2005) Activated Carbon Adsorption
    • Bansal, R.C.1    Goyal, M.2
  • 35
    • 62649115125 scopus 로고    scopus 로고
    • .


* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.