# US 11,077,427 B2 · Porous monolith containing TiO2 and method for the production thereof

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- Number: US 11,077,427 B2
- Document ID: US11077427B2
- Status: Granted
- Kind: B2
- Application number: 16/608,312
- Filed: 2018-04-23
- Published: 2021-04-08
- Granted: 2021-08-03
- Earliest claimed: 2017-04-28
- Assignees: Ifp Energies Nouvelles
- Applicants: IFP Energies Nouvelles
- Inventors: Sophie Bernadet; Antoine Fecant; Denis Uzio; Renal-Vasco Backov; Serge Ravaine
- Web page: https://patentgrep.com/patent/US11077427B2

## CPC

- B01J 21/08: Silica
- C04B 41/87: Ceramics
- B01J 21/063: {Titanium; Oxides or hydroxides thereof}
- B01J 35/39: Photocatalytic properties
- B01J 35/60: characterised by their surface properties or porosity
- B01J 35/615: {100-500 m2/g}
- B01J 35/617: {500-1000 m2/g}
- B01J 35/633: {less than 0.5 ml/g}
- B01J 35/635: {0.5-1.0 ml/g}
- B01J 35/638: {more than 1.0 ml/g}
- B01J 35/643: {less than 2 nm}
- B01J 35/647: {2-50 nm}
- B01J 35/653: {500-1000 nm}
- B01J 35/657: {larger than 1000 nm}
- B01J 35/69: bimodal
- B01J 37/0201: {Impregnation}
- B01J 37/0236: {Drying, e.g. preparing a suspension, adding a soluble salt and drying}
- B01J 37/036: {to form a gel or a cogel}
- B01J 37/04: Mixing {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/088: {Decomposition of a metal salt}
- C01B 3/042: Decomposition of water (by electrolysis of water C25B1/04)
- C04B 38/0045: {by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes}
- C04B 38/0051: {characterised by the pore size, pore shape or kind of porosity}
- C04B 38/0058: {open porosity}
- C04B 38/0067: {characterised by the density of the end product}
- C04B 38/007: {characterised by the pore distribution, e.g. inhomogeneous distribution of pores}
- C04B 41/009: {characterised by the material treated}
- C04B 41/5041: {Titanium oxide or titanates}
- B01J 35/32: Bulk density
- B01J 35/56: Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional [3D] monoliths
- B01J 2235/00: Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties
- C04B 2111/00827: {Photocatalysts}
- Y02E 60/36: Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## 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.

## Claims

### Claim 1

A porous monolith comprising between 20% and 70% by weight of TiO2 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.

### Claim 2 (depends on 1)

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

### Claim 3 (depends on 1)

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.

### Claim 4 (depends on 1)

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.

### Claim 5 (depends on 1)

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.

### Claim 6 (depends on 1)

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

### Claim 7 (depends on 1)

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.

### Claim 8 (depends on 1)

The monolith as claimed in claim 1, which comprises a BET specific surface area of between 150 and 700 m2/g.

### Claim 9 (depends on 1)

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.

### Claim 10 (depends on 9)

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.

### Claim 11 (depends on 1)

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.

### Claim 12 (depends on 11)

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.

### Claim 13 (depends on 1)

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 TiO2.

### Claim 14 (depends on 13)

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.

### Claim 15 (depends on 13)

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.

### Claim 16 (depends on 1)

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.