Synthetic mineral compound, composition including such a compound and method for manufacturing such a compound

Patent metadata

Field	Value
Publication number	US-11174168-B2
Application number	US-201615764018-A
Country	US
Kind code	B2
Filing date	Sep 27, 2016
Priority date	Sep 28, 2015
Publication date	Nov 16, 2021
Grant date	Nov 16, 2021

Abstract

The invention relates to a mineral compound, referred to as synthetic mica, with formula At(Six-Ge1x)4MzO10(OH)2, wherein: A designates at least one monovalent interfoliar cation of a metal element, A having the formula Liw(1)Naw(2)Kw(3)Rbw(4)Cssw(5), each instance of w(i) representing a real number in the interval [0; 1], such that the sum of the instances of w(i) is equal to 1; t is a real number in the interval [0.3; 1]; x is a real number in the interval [0; 1]; M designates at least one divalent metal having the formula Mgy(1)Coy(2)Zny(3)Cuy(4)Mny(5)Fey(6)Niy(7)Cr, each instance of y(i) representing a real number in the interval [0; 1], such as the formula (A); and z is a real number in the interval [2.50; 2.85]. The invention also relates to a composition comprising such a compound and a method for preparing such a compound.∑i=15⁢⁢w⁡(i)=1″∑i=18⁢⁢y⁡(i)=1″

First claim

The invention claimed is:

1. A non-fluorinated synthetic mica compound having the following formula (I):
A t (Si x Ge 1-x ) 4 M z O 10 (OH) 2   (I)

wherein:
A is at least one monovalent interfoliary cation of a metal element having the formula Li w(1) Na w(2) K w(3) Rb w(4) Cs w(5) ; wherein each w(i) represents a real number of the interval [0; 1], such that Σ i=1 5 w(i)=1,
t is a real number of the interval [0.3; 1],
x is a real number of the interval [0; 1],
M is at least one divalent metal having the formula
Mg y(1) Co y(2) Zn y(3) Cu y(4) Mn y(5) Fe y(6) Ni y(7) Cr y(8) ;

wherein each y(i) represents a real number of the interval [0; 1], such that Σ i=1 8 y(i)=1
z is a real number in the range [2.50; 2.85], and
t+2z is a real number of the interval [5.3; 6.0].

2. The non-fluorinated synthetic mica compound according to claim 1 , wherein y(3) is different from 1.

3. The non-fluorinated synthetic mica compound according to claim 1 , wherein in formula (I), A denotes potassium.

4. The non-fluorinated synthetic mica compound according to claim 1 , wherein it has, in X-ray diffraction, at least one diffraction line characteristic of a plane (001) located at a distance of between 9.70 Å and 10.70 Å.

5. The non-fluorinated synthetic mica compound according to claim 1 , wherein said compound is organized according to a solid structure formed of sheets separated from each other by at least one interfoliary space, each cation A being disposed in said interfoliary spaces.

6. A composition comprising at least one non-fluorinated synthetic mica compound according to claim 1 .

7. The composition according to claim 6 , wherein the composition is free of iron.

8. The composition according to claim 6 , wherein the composition is free of aluminum.

9. The composition according to claim 6 , wherein the composition comprises particles of said compound having an average size of between 10 nm and 400 nm, as observed by electron microscopy.

10. A method for preparing a compound of following formula (I):
A t (Si x Ge 1-x ) 4 M z O 10 (OH) 2   (I)

wherein:
A is at least one monovalent interfoliary cation of a metal element having the formula Li w(1) Na w(2) K w(3) Rb w(4) Cs w(5) ; wherein each w(i) represents a real number of the interval [0; 1], such that Σ i=1 5 w(i)=1,
t is a real number of the interval [0.3; 1],
x is a real number of the interval [0; 1],
M is at least one divalent metal having the formula
Mg y(1) Co y(2) Zn y(3) Cu y(4) Mn y(5) Fe y(6) Ni y(7) Cr y(8) ;

wherein each y(i) represents a real number of the interval [0; 1], such that Σ i=1 8 y(i)=1
z is a real number in the range [2.50; 2.85], and
t+2z is a real number of the interval [5.3; 6.0];

said method comprising:
preparing a precursor gel of the compound of formula (I) by a co-precipitation reaction between:
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 and potassium metagermanate,
at least one metal salt of the divalent metal M,
the molar proportion (Si x Ge 1-x )/M during the preparation of the precursor gel being in the range [2/1.425; 1.6]

adding at least one hydroxide of formula AOH to the precursor gel so that the molar proportion of A/M is at least equal to t/z, and
carrying out a solvothermal treatment of the precursor gel at a temperature of between 300° C. and 600° C.

11. The method according to claim 10 , wherein, prior to said solvothermal treatment and following the precipitation of the precursor gel, the precursor gel is washed with a rinsing fluid.

12. The method according to claim 10 , wherein said solvothermal treatment is carried out continuously.

13. The method according to claim 10 , wherein said solvothermal treatment is carried out in aqueous medium.

14. The method according to claim 10 , wherein after said solvothermal treatment, an anhydrous thermal treatment is carried out at a temperature between 500° C. and 600° C.

15. The method according to claim 11 , wherein the rinsing fluid is water.

Assignees

• Centre Nat Rech Scient
• Univ Toulouse 3 Paul Sabatier

Inventors

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

Classifications

• C01B33/425 Primary

  not containing aluminium · CPC title

• C01B33/22

  Magnesium silicates · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• C01P2002/74

  by peak-intensities or a ratio thereof only · CPC title

• C01P2004/20

  extending in two dimensions, e.g. plate-like · CPC title