Method for preparing synthetic mineral particles

Patent metadata

Field	Value
Publication number	US-11352264-B2
Application number	US-201615764045-A
Country	US
Kind code	B2
Filing date	Sep 27, 2016
Priority date	Sep 28, 2015
Publication date	Jun 7, 2022
Grant date	Jun 7, 2022

Abstract

The invention relates to a method for preparing synthetic mineral particles with formula (AlyM1-y)2(SixGe1-x)2O5(OH)4, wherein M designates at least one trivalent metal selected from the group made up of gallium and the rare earths, which comprises the following steps: preparing a gel which is a precursor of said synthetic mineral particles by a co-precipitation reaction of at least one salt of metal selected among aluminium and M with at least one silicon source selected from the group made up of potassium metasilicate, sodium metasilicate, potassium metagermanate and sodium metagermanate, the molar ratio of (AlyM1-y) to (SixGe1-x) during the preparation of said precursor gel being equal to 1, at least one base being added during said co-precipitation reaction; and performing a solvothermal treatment of said precursor gel at a temperature of 250° C. to 600° C.

First claim

The invention claimed is:

1. A method for preparing synthetic mineral particles of the following formula (I):
(Al y M 1-y ) 2 (Si x Ge 1-x ) 2 O 5 (OH) 4   (I)

wherein
Al is aluminium,
Si is silicon,
M is at least one trivalent metal selected from the group consisting of gallium, iron, and the rare earth elements,
y is a real number between 0 and 1,
Ge is germanium,
x is a real number between 0 and 1,
O is oxygen, and
H is hydrogen,

said method comprising:
providing a precursor gel of the synthetic mineral particles of formula (I) that is prepared by a co-precipitation reaction between:
at least one salt of a metal selected from the group consisting of aluminium and M,
at least one source of at least one chemical element selected from the group consisting of silicon and germanium, said source of the chemical element selected from the group consisting of silicon and germanium being selected from the group consisting of potassium metasilicate, sodium metasilicate, potassium metagermanate, and sodium metagermanate,
the molar ratio of (Al y M 1-y )/(Si x Ge 1-x ) over the course of the preparation of the precursor gel being equal to 1,
at least one base being added over the course of the co-precipitation reaction; and

subjecting said precursor gel to continuous solvothermal treatment at a temperature between 250 and 600° C. for a period selected so as to allow synthetic mineral particles of formula (I) to be obtained,
wherein said solvothermal treatment is carried out for a period of less than 6 hours
in a continuous piston-flow reactor;
wherein the concentration of the precursor gel is less than or equal to 0.1 mol/L; and
wherein the synthetic mineral particles of formula (I) obtained by the method have an average size of between 20 nm and 600 nm.

2. The method according to claim 1 , wherein said aluminium salt is selected from the group consisting of aluminium chloride and aluminium nitrate.

3. The method according to claim 1 , wherein said solvothermal treatment is carried out using a constant-volume continuous reactor.

4. The method according to claim 1 , wherein said solvothermal treatment is carried out in an aqueous medium.

5. The method according to claim 1 , wherein said solvothermal treatment is carried out at a pressure greater than 1 MPa.

6. The method according to claim 1 , wherein said solvothermal treatment is carried out at a pressure between 22 and 30 MPa.

7. The method according to claim 1 , wherein the duration of said solvothermal treatment is greater than 10 seconds and less than 6 hours.

8. The method according to claim 1 , wherein said precursor gel is washed at least once prior to said solvothermal treatment.

9. The method according to claim 1 , wherein said base is selected from the group consisting of NaOH and KOH.

10. A method for preparing synthetic mineral particles of the following formula (I):
(Al y M 1-y ) 2 (Si x Ge 1-x ) 2 O 5 (OH) 4   (I)

wherein
Al is aluminium,
Si is silicon,
M is at least one trivalent metal selected from the group consisting of gallium, iron, and the rare earth elements,
y is a real number between 0 and 1,
Ge is germanium,
x is a real number between 0 and 1,
O is oxygen, and
H is hydrogen,

said method comprising:
providing a precursor gel of the synthetic mineral particles of formula (I) that is prepared by a co-precipitation reaction between:
at least one salt of a metal selected from the group consisting of aluminium and M,
at least one source of at least one chemical element selected from the group consisting of silicon and germanium, said source of the chemical element selected from the group consisting of silicon and germanium being selected from the group consisting of potassium metasilicate, sodium metasilicate, potassium metagermanate, and sodium metagermanate,
the molar ratio of (Al y M 1-y )/(Si x Ge 1-x ) over the course of the preparation of the precursor gel being equal to 1,
at least one base being added over the course of the co-precipitation reaction; and

subjecting said precursor gel to continuous solvothermal treatment at a temperature between 250 and 600° C. for a period selected so as to allow synthetic mineral particles of formula (I) to be obtained,
wherein said solvothermal treatment is carried out for a period of less than 6 hours in a continuous plug-flow reactor;
wherein the concentration of the precursor gel is of less than or equal to 0.1 mol/L; and
wherein the synthetic mineral particles of formula (I) obtained by the method have an average size of between 20 nm and 600 nm.

Assignees

• Centre Nat Rech Scient
• Univ Toulouse 3 Paul Sabatier

Inventors

• Martin François
• Le Roux Christophe
• Micoud Pierre
• Claverie Marie
• Aymonier Cyril

Classifications

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C04B2235/3427

  Silicates other than clay, e.g. water glass · CPC title

• C01P2002/88

  by thermal analysis data, e.g. TGA, DTA, DSC · CPC title

• C04B2235/3201

  Alkali metal oxides or oxide-forming salts thereof · CPC title

• C09C1/405

  containing combined silica, e.g. mica · CPC title