Top

Journal of Sol-Gel Science and Technology

Published in:

15-03-2019 | Original Paper: Sol–gel, hybrids and solution chemistries

Synthesis of aluminophosphate xerogels by non-hydrolytic sol–gel condensation of EtAlCl₂ with trialkylphosphates

Authors: Jan Podhorsky, Jan Chyba, Jiri Pinkas, Zdenek Moravec

Published in: Journal of Sol-Gel Science and Technology | Issue 2/2019

Activate our intelligent search to find suitable subject content or patents.

search-config

AI-assisted search

Off

Abstract

We have investigated the preparation of high-surface-area mesoporous aluminophosphates by non-hydrolytic sol–gel method based on reactions of EtAlCl₂ with trialkylesters of phosphoric acid (OP(OR)₃, R = Me, Et, ⁱPr, ⁿBu, in dry organic solvents. The condensations proceed by alkylchloride elimination. Various reaction and calcination conditions were examined. Porosity is obtained after calcination by removal of organic residual groups. This thermal processing at 300 °C of as-synthesized precursor gels leads to amorphous aluminophosphate xerogels with surface areas of 400–500 m² g^–1 provided by small mesopores (2–8 nm). Changes in the coordination environment of aluminium from six- to four-coordinate are evidenced by shift of ²⁷Al MAS NMR resonances.

previous article Amine functionalized mesoporous hybrid materials: influence of KCl and xylene on the textural characteristics and CO2 sorption

next article 2-Triethoxysilylazulene derivatives: Syntheses and optical properties, and hydrolysis—condensation of 2-triethoxysilylazulene

Dont have a licence yet? Then find out more about our products and how to get one now:

Springer Professional "Technik"

Online-Abonnement

Mit Springer Professional "Technik" erhalten Sie Zugriff auf:

über 67.000 Bücher
über 390 Zeitschriften

aus folgenden Fachgebieten:

Automobil + Motoren
Bauwesen + Immobilien
Business IT + Informatik
Elektrotechnik + Elektronik
Energie + Nachhaltigkeit
Maschinenbau + Werkstoffe

Jetzt Wissensvorsprung sichern!

inform now

Springer Professional "Wirtschaft+Technik"

Online-Abonnement

Mit Springer Professional "Wirtschaft+Technik" erhalten Sie Zugriff auf:

über 102.000 Bücher
über 537 Zeitschriften

aus folgenden Fachgebieten:

Automobil + Motoren
Bauwesen + Immobilien
Business IT + Informatik
Elektrotechnik + Elektronik
Energie + Nachhaltigkeit
Finance + Banking
Management + Führung
Marketing + Vertrieb
Maschinenbau + Werkstoffe
Versicherung + Risiko

Jetzt Wissensvorsprung sichern!

inform now

Available only for authorised users

Wilson ST, Lok BM, Messina CA, Cannan TR, Flanigen EM (1982) Aluminophosphate molecular sieves: a new class of microporous crystalline inorganic solids. J Am Chem Soc 104:1146–1147. https://doi.org/10.1021/ja00368a062 CrossRef

Bennett JM, Cohen JM, Artioli G, Pluth JJ, Smith JV (1985) Crystal Structure of AlPO₄-21, a Framework aluminophosphate containing tetrahedral phosphorus and both tetrahedral and trigonal-bipyramidal aluminum in 3-, 4-, 5-, and 8-rings. Inorg Chem 24:188–193. https://doi.org/10.1021/ic00196a014‎ CrossRef

Kirchner RM, Bennett JM (1994) The structure of calcined AlPO₄-41: A new framework topology containing 10-ring pores. Zeolites 14:523–528. https://doi.org/10.1016/0144-2449(94)90185-6CrossRef

Zahendi-Niaki MH, Joshi PN, Kaliaguine J (1996) Synthesis and characterization of AlPO-36, the missing end-member of ATS structure. Chem Commun 1373–1374 https://doi.org/10.1039/CC9960001373

Naydenov V, Tosheva V, Antzutkin AN, Sterte J (2005) Meso/macroporous AlPO-5 spherical macrostructures tailored by resin templating. Micro Mesopor Mat 78:181–188. https://doi.org/10.1016/j.micromeso.2004.10.008 CrossRef

Middelkoop V, Jacques SDM, O´Brien MG, Beale AM, Barnes P (2008) Hydrothermal/autoclave synthesis of AlPO-5: a prototype space/time study of crystallisation gradients. J Mater Sci 43:2222–2228. https://doi.org/10.1007/s10853-007-2038-3CrossRef

Vaughan DEW, Yennawar HP, Perrotta AJ (2006) Synthesis and structure of an aluminophosphate built from 3-rings. Chem Mater 18:3611–3615. https://doi.org/10.1021/cm0521572 CrossRef

Afeworki M, Dorset DL, Kennedy GJ, Strohmaier KG (2006) Synthesis and characterization of a new microporous material. 1. structure of aluminophosphate EMM-3. Chem Mater 18:1697–1704. https://doi.org/10.1021/cm052174r CrossRef

Chen B, Huang Y (2011) Formation of microporous material AlPO₄-18 under dry-gel conversion conditions. Micro Mesopor Mat 143:14–21. https://doi.org/10.1016/j.micromeso.2011.02.002 CrossRef

10.

Kodaira T, Nabata A, Ikeda T (2012) A new aluminophosphate phase, AlPO-NS, with a bellows-like morphology obtained from prolonged hydrothermal process or increased pH value of initial solution for synthesizing AlPO₄-5. Micro Mesopor Mat 162:31–35. https://doi.org/10.1016/j.micromeso.2012.06.003 CrossRef

11.

Flanigen EM, Lok BM, Patton RL, Wilson ST (1986) Aluminophosphate molecular sieves and the periodic table. Pure & Appl Chem 58:1351–1358. https://doi.org/10.1351/pac198658101351 CrossRef

12.

Davis ME, Lobo RF (1992) Zeolite and molecular sieve synthesis. Chem Mater 4:756–768. https://doi.org/10.1021/cm00022a005 CrossRef

13.

Richardson JW, Vogt ETC (1992) Structure determination and rietveld refinement of aluminophosphate molecular sieve AIPO₄-8. Zeolites 12:13–19. https://doi.org/10.1016/0144-2449(92)90003-8CrossRef

14.

Deroche I, Gaberova L, Maurin G, Llewellyn P, Castro M, Wright P (2008) Adsorption of carbon dioxide in SAPO STA-7 and AlPO-18: Grand Canonical Monte Carlo simulations and microcalorimetry measurements. Adsorption 14:207–213. https://doi.org/10.1007/s10450-007-9098-1CrossRef

15.

Carreon ML, Li S, Carreon MA (2012) AlPO-18 membranes for CO₂/CH₄ separation. Chem Commun 48:2310–2312. https://doi.org/10.1039/c2cc17249f CrossRef

16.

Shutilov RA, Grenev IV, Kikhtyanin OV, Gavrilov VY (2012) Adsorption of molecular hydrogen on aluminophosphate zeolites at 77 K. Kinet Catal 53:137–144. https://doi.org/10.1134/S0023158412010119 CrossRef

17.

Arieli D, Vaughan DEW, Strohmaier KG, Thomann H, Bernardo M, Goldfarb D (1999) Studies of Fe(III) incorporated into AlPO₄-20 by X- and W-band EPR spectroscopies. Magn Reson Chem 37:43–54. 0749–1581/99/SI0043–12CrossRef

18.

Frunza L, Pelgrims J, Leeman H, Van Der Voort P, Vansant EF, Schoonheydt RA, Weckhuysen BM (2001) Incorporation of transition metal ions in aluminophosphate molecular sieves with AST structure. J Phys Chem B 105:2677–2686. https://doi.org/10.1021/jp002403r CrossRef

19.

Zhao R, Wang Y, Guo Y, Guo Y, Liu X, Zhang Z, Wang Y, Zhan W, Lu G (2006) A novel Ce/AlPO-5 catalyst for solvent-free liquid phase oxidation of cyclohexane by oxygen. Green Chem 8:459–466. https://doi.org/10.1039/b517656e CrossRef

20.

Franklin IL, Beale AM, Sankar G (2003) On the activity, longevity and recyclability of Mn(II) and Co(II) substituted AlPO-18 catalysts for the conversion of methanol to light olefins. Catal Today 81:623–629. https://doi.org/10.1016/S0920-5861(03)00160-3CrossRef

21.

Zhao X, Sun Z, Zhu Z, Li A, Li G, Wang X (2013) Higher alcohol synthesis over Rh catalysts: conditioning of Rh/N-CNTs by Co and Mn entrapped in the support. Catal Lett 143:657–665. https://doi.org/10.1007/s10562-013-1027-1CrossRef

22.

Raboin L, Yano J, Tilley D (2012) Epoxidation catalysts derived from introduction of titanium centers onto the surface of mesoporous aluminophosphate: Comparisons with analogous catalysts based on mesoporous silica. J Catal 285:168–176. https://doi.org/10.1016/j.jcat.2011.09.023 CrossRef

23.

Danjo Y, Kikuchi I, Ino Y, Ohshima M, Kurokawa H, Miura H (2012) Support effect of Pd/AlPO₄ catalyst in hydrogen storage of organic hydride method in the presence of CO. Reac Kinet Mech. Cat 105:381–389. https://doi.org/10.1007/s11144-011-0395-z

24.

Lertjiamratn K, Praserthdam P, Arai H, Panpranot J (2010) Modification of acid properties and catalytic properties of AlPO₄ by hydrothermal pretreatment for methanol dehydration to dimethyl ether. Appl Catal A 2010 378:119–123. https://doi.org/10.1016/j.apcata.2010.02.013 CrossRef

25.

Yuan H, Liu X, Ren J, Shen L (2013) Surface acidity of aluminum phosphate and its catalytic performance in benzene alkylation with long chain olefin. Chin J Chem Eng 21:627–632. https://doi.org/10.1016/S1004-9541(13)60498-XCrossRef

26.

Fitzgerald JJ, Piedra G, Dec SF, Seger M, Maciel GE (1997) Dehydration studies of a high-surface-area alumina (pseudo-boehmite) using solid-state ¹H and ²⁷Al NMR. J Am Chem Soc 119:7832–7842. https://doi.org/10.1021/ja970788u CrossRef

27.

Pinkas J, Wessel H, Yang Y, Montero ML, Noltemeyer M, Fröba M, Roesky HW (1998) Reactions of phosphoric acid triesters with aluminum and gallium amides. Inorg Chem 1998 37:2450–2457. https://doi.org/10.1021/ic9713036

28.

Mason MR, Matthews RM, Mashuta MS, Richardson JF (1996) Organic-soluble cyclic and cage alkylaluminophosphates: X-ray crystal structure of [(^tBu)₂Al(μ₂-O)₂P(OSiMe₃)₂]₂. Inorg Chem 35:5756–5757. https://doi.org/10.1021/ic960619v CrossRef

29.

Corriu RJP, Leclercq D, Lefévre P, Mutin PH, Vioux A (1992) Preparation of monolithic metal oxide gels by a non-hydrolytic sol–gel process. J Mater Chem 2:673–674. https://doi.org/10.1039/jm9920200673 CrossRef

30.

Andrianainarivelo M, Corriu R, Leclercq D, Mutin PH, Vioux A (1996) Mixed oxides SiO₂–ZrO₂ and SiO₂–TiO₂ by a non-hydrolytic sol–gel route. J Mater Chem 6:1665–1671. https://doi.org/10.1039/JM9960601665 CrossRef

31.

Aboulaich A, Boury B, Mutin PH (2010) Reactive and organosoluble anatase nanoparticles by a surfactant-free nonhydrolytic synthesis. Chem Mater 22:4519–4521. https://doi.org/10.1021/cm101191a CrossRef

32.

Aboulaich A, Boury B, Mutin PH (2011) Reactive and organosoluble SnO₂ nanoparticles by a surfactant‐free non‐hydrolytic sol–gel route. Eur J Inorg Chem 3644–3649. https://doi.org/10.1002/ejic.201100391

33.

Bouchmella K, Mutin PH, Stoyanova M, Poleunis C, Eloy P, Rodemerck U, Gaigneaux EM, Debecker DP (2013) Olefin metathesis with mesoporous rhenium–silicium–aluminum mixed oxides obtained via a one-step non-hydrolytic sol–gel route. J Catal 301:233–241. https://doi.org/10.1016/j.jcat.2013.02.016 CrossRef

34.

Moravec Z, Sluka R, Necas M, Jancik V, Pinkas J (2009) A structurally diverse series of aluminum chloride alkoxides [Cl_xAl(μ-OR)_y]_n (R=ⁿBu, ^cHex, Ph, 2,4-^tBu₂C₆H₃). Inorg Chem 48:8106–8114. https://doi.org/10.1021/ic802251g CrossRef

35.

Loewenstein W (1954) The distribution of aluminum in the tetrahedra of silicates and aluminates. Am Mineral 39:92–96. ISSN 1945-3027

36.

Pinkas J, Chakraborty D, Yang Y, Murugavel R, Noltemeyer M, Roesky HW (1999) Reactions of trialkyl phosphates with trialkyls of aluminum and gallium: New route to alumino- and gallophosphate compounds via dealkylsilylation. Organometallics 18:523–528. https://doi.org/10.1021/om9806702 CrossRef

37.

Daasch LW, Smith DC (1951) Infrared spectra of phosphorus compounds. Anal Chem 23:853–868. https://doi.org/10.1021/ac60054a008 CrossRef

38.

Corbridge DEC (1969) In: Grayson M, Griffith EJ (ed) Phosphorus Compounds, John Wiley, New York

39.

Li HX, Davis ME (1993) Further studies on aluminophosphate molecular sieves. Part 1.—AlPO₄-H2: a hydrated aluminophosphate molecular sieve. J Chem Soc Faraday Trans 89:951–956. https://doi.org/10.1039/FT9938900951 CrossRef

40.

George L, Viswanatham KS, Singh S (1997) Ab initio study of trimethyl phosphate: conformational analysis, dipole moments, vibrational frequencies, and barriers for conformer interconversion. J Phys Chem 101:2459–2464. https://doi.org/10.1021/jp9625570 CrossRef

41.

Jelinek R, Chmelka BF, Wu Y, Grandinetti PJ, Pines A, Barrie PJ, Klinowski J (1991) Study of the aluminophosphates AlPO₄-21 and A1PO₄-25 by ²⁷Al Double-Rotation NMR. J Am Chem Soc 113:4097–4101. 0002–7863/91/1513–4097CrossRef

42.

Blackwell CS, Patton RL (1988) Solid-state NMR of silicoaluminophosphate molecular sieves and aluminophosphate materials. J Phys Chem 92:3969–3970. https://doi.org/10.1021/j100324a055 CrossRef

Title: Synthesis of aluminophosphate xerogels by non-hydrolytic sol–gel condensation of EtAlCl2 with trialkylphosphates
Authors: Jan Podhorsky
Jan Chyba
Jiri Pinkas
Zdenek Moravec
Publication date: 15-03-2019
Publisher: Springer US
Published in: Journal of Sol-Gel Science and Technology / Issue 2/2019
Print ISSN: 0928-0707
Electronic ISSN: 1573-4846
DOI: https://doi.org/10.1007/s10971-019-04953-0

Springer Professional

Abstract

Please log in to get access to your license.

Dont have a licence yet? Then find out more about our products and how to get one now:

Springer Professional "Technik"

Springer Professional "Wirtschaft+Technik"

Other articles of this Issue 2/2019

Correlation between calcination temperature and optical parameter of zinc oxide (ZnO) nanoparticles

Studying the structural, morphological, and optical properties of CuS:Ni nanostructure prepared by a hydrothermal method for biological activity

Nanozeolites: synthesized, properties, applications

ZnO formation through decomposition of zinc bis(ethyl acetoacetate) by steaming treatment

Synthesis and characterization of porous clay-organic heterostructures

Perovskite BiFeO3 nanocatalysts for electrochemical water oxidation

Premium Partners