IP Library Granted Patent US 11,577,964
Granted Patent B2
US 11,577,964 · App. 17/011,611 · Granted Feb 14, 2023

Method for producing an alumina gel having a high dispersibility and a specific crystallite size

Inventors: Malika Boualleg (Villeurbanne, FR); Olivier Lafon (Lyons, FR)
Assignee: IFP Energies Nouvelles
C01F7/34B01J13/006B28B3/20B28B11/243C01P2002/04C01P2002/60C01P2002/72C01P2004/64C01P2006/22C01P2006/80
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Quick Facts
Patent No.
US 11,577,964
App. No.
17/011,611
Granted
Feb 14, 2023
Kind
B2
Abstract

Process for preparing alumina gel in a single precipitation step consisting of dissolving an aluminium precursor, aluminium chloride, in water, at a temperature of 10° C. to 90° C. such that the pH of the solution is from 0.5 to 5, for a period of 2 to 60 minutes, then adjusting the pH to 7.5 to 9.5 by adding a basic precursor, sodium hydroxide, to the solution obtained to obtain a suspension, at a temperature of 5° C. to 35° C., and for 5 minutes to 5 hours, followed by a filtration step, said process not comprising any washing steps. Also, novel alumina gel having a high dispersibility index, in particular a dispersibility index of more than 80%, a crystallite dimension of 0.5 to 10 nm, a chlorine content of 0.001% to 2% by weight and a sodium content of 0.001% to 2% by weight, the percentages by weight being expressed with respect to the total weight of the alumina gel.

Claims (16)

1. A process for the preparation of an alumina gel, wherein the alumina gel has a dispersibility index of more than 80%, a crystallite dimension, obtained by the Scherrer X ray diffraction formula along the crystallographic directions [020] and [120], respectively, in the range of 0.5 to 10 nm and in the range of 0.5 to 15 nm, a chlorine content in the range 0.001% to 2% by weight and a sodium content in the range 0.001% to 2% by weight, the percentages by weight being expressed with respect to the total weight of the alumina gel,

the process comprising:

a single precipitation step (a) consisting of dissolving an acidic aluminium precursor, aluminium chloride, AlCl 3 , in water, at a temperature in the range 10° C. to 90° C. and for a period in the range of 2 to 60 minutes, to obtain a solution, in a manner such that the pH of the solution is in the range of 0.5 to 5, then adjusting the pH to a pH in the range of 7.5 to 9.5 by adding a basic precursor, sodium hydroxide, to the solution obtained in order to obtain a suspension, at a temperature in the range 5° C. to 35° C. and for a period in the range of 5 minutes to 5 hours, and

a filtration step b) of the suspension obtained at the end of step a) to obtain a precipitate,

said process not comprising any steps for washing the precipitate obtained at the end of the filtration step b).

2. The process as claimed in claim 1 , in which the acidic aluminium precursor, aluminium chloride, AlCl 3 , is dissolved in water at a temperature in the range 10° C. to 75° C.

3. The process as claimed in claim 1 , in which the pH of the solution of aluminium chloride, AlCl 3 , in water, is in the range 1 to 4.

4. The process as claimed in claim 1 , in which the pH is adjusted at a temperature in the range 10° C. to 30° C.

5. The process as claimed in claim 4 , in which the pH is adjusted at a temperature in the range 10° C. to 25° C.

6. The process as claimed in claim 1 , in which the pH is adjusted to a pH in the range 7.7 to 8.8.

7. The process as claimed in claim 1 , in which the preparation process also comprises a drying step for the filtered suspension obtained at the end of the precipitation step in order to obtain a powder, said drying step being carried out by drying at a temperature of 100° C. or more or by spray drying.

8. The process as claimed in claim 7 , in which the preparation process also comprises a shaping step of the powder obtained in order to obtain a green material.

9. The process as claimed in claim 8 , in which the shaping step is carried out by mixing-extrusion or by oil-drop.

10. The process as claimed in claim 8 , in which the shaped green material then undergoes a heat treatment step at a temperature in the range 500° C. to 1000° C., for a period in the range 2 to 10 h, in the presence or absence of a stream of air containing up to 60% by volume of water.

11. The process as claimed in claim 1 , wherein the alumina gel has a dispersibility index in the range of 85% to 100%.

12. The process as claimed in claim 11 , wherein the alumina gel has a dispersibility index in the range of 88% to 100%.

Priority Claims (1)
FR 1650747 · Jan 29, 2016 · national
Continuity (2)
Division 16072016
Related Publication 20200399138A1 · Dec 24, 2020