US 12,290,798 B2
Method for obtaining metal oxides supported on mesoporous silica particles
Maria Colmenares, Berlin (DE); Tomos Harris, Berlin (DE); Julien Sialelli, Berlin (DE); Javier Silva Mora, Berlin (DE); and Arne Thomas, Dallgow-Döberitz (DE)
Assigned to TECHNISCHE UNIVERSITÄT BERLIN, Berlin (DE)
Appl. No. 17/609,339
Filed by TECHNISCHE UNIVERSITÄT BERLIN, Berlin (DE)
PCT Filed May 7, 2020, PCT No. PCT/EP2020/062719
§ 371(c)(1), (2) Date Nov. 5, 2021,
PCT Pub. No. WO2020/225366, PCT Pub. Date Nov. 12, 2020.
Claims priority of application No. 19173277 (EP), filed on May 8, 2019.
Prior Publication US 2022/0161240 A1, May 26, 2022
Int. Cl. B01J 21/08 (2006.01); B01J 29/03 (2006.01); B01J 37/00 (2006.01); B01J 37/04 (2006.01); B01J 37/06 (2006.01); B01J 37/08 (2006.01); B01J 37/10 (2006.01); B01J 37/34 (2006.01); C01B 33/18 (2006.01); C01B 33/193 (2006.01); C01B 39/02 (2006.01); C01B 39/06 (2006.01); C01B 39/08 (2006.01)
CPC B01J 29/0333 (2013.01) [B01J 29/0316 (2013.01); B01J 29/0341 (2013.01); B01J 37/04 (2013.01); B01J 37/082 (2013.01); C01B 39/02 (2013.01); C01B 39/06 (2013.01); C01B 39/08 (2013.01); B01J 2229/18 (2013.01)] 15 Claims
OG exemplary drawing
 
1. A method for preparing metal oxides supported on mesoporous silica particles comprising the steps of:
a) providing a solution of at least one metal salt, wherein the metal is selected from a group consisting of Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ru, Rh, Pd, Ag, Ir, Pt and Au;
b) providing a solution of at least one complex forming agent, wherein the at least one complex forming agent is of the general formulae (I)
Y3Si(CH2)n—X  (I)
wherein:
X is a complexing functional group,
Y is —OH or a hydrolysable moiety selected from the group consisting of halogen, alkoxy, aryloxy, and acyloxy, and
n is ≥1;
c) mixing the metal salt solution of step a) and the complex forming agent solution of step b) to obtain a metal precursor solution with a pH value between 6-12, which functional group/metal ratio is ≥1;
d) adding a buffered solution containing at least one pore structure directing agent (SDA) (or template) adjusted to a pH range between 2 and 8;
e) mixing the metal precursor solution of step c) and the buffered template solution of step d) to obtain a buffered metal precursor-template-mixture;
f) adding at least one alkali silicate solution to the metal precursor-template
mixture of step d) at room temperature to obtain a silica-supported metal complex, at a pH adjusted to a range between 4 and 8; and
g) calcining of the silica-supported metal complex of step f) under air to obtain the supported metal oxide mesoporous silica particles.