Gel with high dispersibility and method for preparing same

Patent metadata

Field	Value
Publication number	US-10858262-B2
Application number	US-201816045118-A
Country	US
Kind code	B2
Filing date	Jul 25, 2018
Priority date	Jun 13, 2014
Publication date	Dec 8, 2020
Grant date	Dec 8, 2020

Abstract

The present invention also discloses the method for preparing said gel comprising at least one step of precipitating at least one aluminium salt, at least one step of heating the suspension obtained and a final heat treatment step for forming the alumina gel.

First claim

The invention claimed is:

1. A preparation method of an alumina gel having a dispersibility index greater than 70%, a crystallite size between 1 and 35 nm, and a sulphur content between 0.001% and 2% by weight, and a sodium content between 0.001% and 2% by weight, the weight percentages being expressed in relation to the total mass of alumina gel, said method comprising at least the following steps:
a) at least one first alumina precipitation step, in an aqueous reaction medium, of at least one basic precursor selected from the group consisting of sodium aluminate, potassium aluminate, ammonia, sodium hydroxide and potassium hydroxide, and at least one acidic precursor selected from the group consisting of aluminum sulphate, aluminum chloride, aluminum nitrate, sulphuric acid, hydrochloric acid, and nitric acid, in which at least one of the basic or acidic precursor comprises aluminum, the relative flow rate of the acidic and basic precursors is chosen so as to obtain a pH of the reaction medium between 8.5 and 10.5, and the flow rate of the acidic and basic precursor or precursors containing aluminum is regulated so as to obtain a rate of progress of said first step between 40 and 100%, the rate of progress being defined as the proportion of alumina formed as Al 2 O 3 equivalent during the first precipitation step with respect to the total amount of alumina formed at the end of the precipitation step or steps, the said first precipitation step being carried out at a temperature between 10 and 50° C. and for a period between 2 minutes and 30 minutes,
b) a heat treatment step of the suspension obtained at the end of step a), at a temperature between 50 and 200° C. for a period between 50 minutes and 5 hours, and
c) a step of the suspension obtained at the end of heat treatment step b), followed by at least one washing step of the obtained gel.

2. The preparation method according to claim 1 , in which in step a) the acidic precursor is aluminum sulphate and the basic precursor is sodium aluminate, wherein the mass ratio of said basic precursor to said acidic precursor is between 1.6 and 2.05.

3. The preparation method according to claim 1 , in which the progression rate of said precipitation step a) is between 45 to 90%.

4. The preparation method according to claim 1 , in which the heat treatment of step b) is at a temperature of 95 to 150° C.

5. A preparation method of an alumina gel having a dispersibility index greater than 70%, a crystallite size between 1 and 35 nm, and a sulphur content between 0.001% and 2% by weight, and a sodium content between 0.001% and 2% by weight, the weight percentages being expressed in relation to the total mass of alumina gel, said method comprising at least the following steps:
a) at least one first alumina precipitation step, in an aqueous reaction medium, of at least one basic precursor selected from the group consisting of sodium aluminate, potassium aluminate, ammonia, sodium hydroxide and potassium hydroxide, and at least one acidic precursor selected from the group consisting of aluminum sulphate, aluminum chloride, aluminum nitrate, sulphuric acid, hydrochloric acid, and nitric acid, in which at least one of the basic or acidic precursor comprises aluminum, the relative flow rate of the acidic and basic precursors is chosen so as to obtain a pH of the reaction medium between 8.5 and 10.5, and the flow rate of the acidic and basic precursor or precursors containing aluminum is regulated so as to obtain a rate of progress of said first step between 45 and 90%, the rate of progress being defined as the proportion of alumina formed as Al 2 O 3 equivalent during the first precipitation step with respect to the total amount of alumina formed at the end of the precipitation step or steps, the said first precipitation step being carried out at a temperature between 20 and 40° C. and for a period between 2 minutes and 30 minutes,
a heating step of the suspension obtained at the end of the step a), carried out between said step a) and a second precipitation step a′), is performed at a temperature between 20 and 90° C. for a period between 7 and 45 minutes,
a′) a second precipitation step of the suspension obtained at the end of the heating step, said second step being carried out by adding to the suspension at least one basic precursor selected from the group consisting of sodium aluminate, potassium aluminate, ammonia, sodium hydroxide and potassium hydroxide and at least one acidic precursor selected from the group consisting of aluminum sulphate, aluminum chloride, aluminum nitrate, sulphuric acid, hydrochloric acid, and nitric acid, in which at least one of the basic or acidic precursors contains aluminum, the relative flow rate of the acidic and basic precursors is chosen so as to obtain a pH of the reaction medium between 8.5 and 10.5 and the flow rate of the acidic and basic precursor or precursors containing aluminum is regulated so as to obtain a rate of progress of the second step between 10 and 55%, the rate of progress being defined as the proportion of alumina formed as Al 2 O 3 equivalent during said second precipitation step with respect to the total amount of alumina formed at the end of the step a′), said step being carried out at a temperature between 40 and 90° C., and for a period between 2 minutes and 50 minutes, a second heating step of the suspension obtained at the end of the said second precipitation step at a temperature between 50 and 95° C.,
b) a heat treatment step of the suspension obtained at the end of step a′), at a temperature between 50 and 200° C. for a period between 50 minutes and 5 hours,
c) a filtration step of the suspension obtained at the end of the heat treatment step b), followed by at least one washing step of the obtained gel,
d) a drying step of the alumina gel obtained at the end of the step c) so as to obtain a powder,
e) a moulding step of the powder obtained at the end of the step d) so as to obtain a crude material, and
f) a heat treatment step of the crude material obtained at the end of the step e) at a temperature between 500 and 1000° C., in the presence or otherwise of a stream of air containing up to 60% by volume of water.

6. The preparation method according to claim 5 , in which the basic precursor in step a) is sodium aluminate.

7. The preparation method according to claim 5 , in which the acidic precursor in step a) is aluminum sulphate.

8. The preparation method according to claim 5 , in which in step a) the mass ratio of said basic precursor to said acidic precursor is between 1.6 and 2.05.

9. The preparation method according to claim 5 , in which the progression rate of said precipitation step a) is between 50 to 85%.

10. The Preparation method according to claim 5 , in which said precipitation step a) takes place at a temperature of 30° C.

11. The preparation method according to claim 5 , in which a step of heating the suspension obtained at the end of precipitation step a) is performed between the two precipitation steps a) and a′), said heating step taking place at a temperature between 40 and 65° C. and for a duration of between 7 and 35 minutes.

12. The preparation method according to claim 5 , in which in step a′) the mass ratio of said basic precursor to said acidic precursor is between 1.6 and 2.05, the basic and acidic precursors being respectively sodium aluminate and aluminium sulphate.

13. The preparation method according to claim 5 , in which the second precipitation step a′) takes place at a temperature between 45 and 70° C.

14. The preparation method according to claim 5 , in which the progression rate of said precipitation step a)

Assignees

• Ifp Energies Now

Inventors

• Boualleg Malika
• Bouvry Celine
• Euzen Patrick

Classifications

• C01F7/441

  by calcination · CPC title

• C01F7/34 Primary

  Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• B01J13/0056

  containing inorganic material and water · CPC title

• C01F7/141 Primary

  from aqueous aluminate solutions by neutralisation with an acidic agent · CPC title