Porous monolith containing TiO2 and method for the production thereof

Patent metadata

Field	Value
Publication number	US-11077427-B2
Application number	US-201816608312-A
Country	US
Kind code	B2
Filing date	Apr 23, 2018
Priority date	Apr 28, 2017
Publication date	Aug 3, 2021
Grant date	Aug 3, 2021

Abstract

The invention relates to a porous monolith comprising between 20 wt.-% and 70 wt.-% TiO 2 relative to the total weight of the monolith, and between 30 wt.-% and 80 wt.-% a refractory oxide, selected from silica, alumina or silica-alumina, relative to the total weight of the monolith, characterized in that said porous monolith has a bulk density of less than 0.19 g/mL.

First claim

The invention claimed is:

1. A porous monolith comprising between 20% and 70% by weight of TiO 2 relative to the total weight of the monolith, between 30% and 80% by weight of a refractory oxide, which is silica, alumina or silica-alumina relative to the total weight of the monolith, and wherein said porous monolith has a bulk density of less than 0.19 g/ml.

2. The monolith as claimed in claim 1 , having a bulk density of less than 0.16 g/ml.

3. The monolith as claimed in claim 1 , which comprises a mesoporous volume of from 0.1 to 1 ml/g for a pore diameter between 0.2 and 50 nm.

4. The monolith as claimed in claim 1 , which comprises a type-I macroporous volume, of which the pore diameter is greater than 50 nm and less than or equal to 1000 nm, of between 0.1 and 3 ml/g.

5. The monolith as claimed in claim 1 , which comprises a type-II macroporous volume, of which the pore diameter is greater than 1 μm and less than or equal to 10 μm, of between 0.1 and 8 ml/g.

6. The monolith as claimed in claim 1 , which comprises a mesoporosity and/or a type-I macroporosity and/or a type-II macroporosity.

7. The monolith as claimed in claim 1 , which also comprises a macroporous volume of less than 0.5 ml/g for a pore diameter of greater than 10 μm.

8. The monolith as claimed in claim 1 , which comprises a BET specific surface area of between 150 and 700 m 2 /g.

9. The monolith as claimed in claim 1 , which also comprises at least one element M selected from the group consisting of groups IA, IIA, VIIIB, IB and IIIA elements of the periodic table of elements alone or as a mixture.

10. The monolith as claimed in claim 9 , in which the content of element(s) M is between 0.001% and 20% by weight relative to the total weight of the porous monolith.

11. The monolith as claimed in claim 1 , which also comprises one or more doping elements selected from metal elements, non-metal elements, or a mixture of metal and non-metal elements.

12. The monolith as claimed in claim 11 , in which the content of the doping element is between 0.001% and 5% by weight relative to the total weight of the porous monolith.

13. A process for preparing a porous monolith as claimed in claim 1 , comprising the following steps:
a) mixing a solution containing a surfactant with an acidic aqueous solution to obtain an acidic aqueous solution comprising a surfactant;
b) adding at least one silicon and/or aluminum precursor to the solution obtained in step a);
c) adding at least one liquid organic compound that is immiscible with the solution obtained in step b) to the solution obtained in step b) to form an emulsion;
d) leaving to mature the emulsion obtained in step c) in a wet state to obtain a gel;
e) washing the gel obtained in step d) with an organic solution;
drying the gel obtained in step e) and calcining to obtain a porous monolith;
g) impregnating a solution comprising at least one soluble titanium precursor in the porosity of the porous monolith obtained in step t);
h) optionally, leaving to mature the porous monolith obtained in step g) in a wet state;
i) drying and calcining the porous monolith obtained in step g) or h) to obtain a porous monolith containing TiO 2 .

14. The process as claimed in claim 13 , wherein, in step i), drying is carried out at a temperature of between 5 and 80° C. and calcining is carried out at a temperature of between 300 and 1000° C.

15. The process as claimed in claim 13 , wherein, in step i), calcining is carried out in two consecutive steps: a first temperature stationary phase of between 120 and 250° C. for 1 to 10 hours, then a second temperature stationary phase of between 300 and 950° C. for 2 to 24 hours.

16. The monolith as claimed in claim 1 , which also comprises one or more doping elements selected from metal elements selected from the group consisting of V, Ni, Cr, Mo, Fe, Sn, Mn, Co, Re, Nb, Sb, La, Ce, Ta and Ti, or non-metal elements selected from the group consisting of C, N, S, F or P, or a mixture of said metal and non-metal elements.

Assignees

• Ifp Energies Now

Inventors

• Bernadet Sophie
• Fecant Antoine
• Uzio Denis
• Backov Renal-Vasco
• Ravaine Serge

Classifications

• B01J35/32

  Bulk density · CPC title

• B01J2235/00

  Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties · CPC title

• B01J35/56

  Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional [3D] monoliths · CPC title

• C04B41/009

  characterised by the material treated · CPC title

• B01J21/08 Primary

  Silica · CPC title