Process for preparing a composition comprising synthetic mineral particles and composition

Patent metadata

Field	Value
Publication number	US-9884769-B2
Application number	US-201214131076-A
Country	US
Kind code	B2
Filing date	Jul 6, 2012
Priority date	Jul 7, 2011
Publication date	Feb 6, 2018
Grant date	Feb 6, 2018

Abstract

A process for preparing a composition including synthetic mineral particles, in which a hydrogel which is a precursor of the synthetic mineral particles is prepared via a coprecipitation reaction between at least one compound including silicon, and at least one compound including at least one metal element, characterized in that the coprecipitation reaction takes place in the presence of at least one carboxylate salt of formula R 2 —COOM′ in which: —M′ denotes a metal chosen from the group made up of Na and K, and —R 2 is chosen from H and alkyl groups including fewer than 5 carbon atoms. A composition including synthetic mineral particles which is obtained by such a process is also described.

First claim

The invention claimed is:

1. A process for preparing a composition comprising synthetic mineral particles, in which a hydrogel precursor of said synthetic mineral particles is prepared by a coprecipitation reaction between:
at least one compound comprising sodium metasilicate, and
at least one compound comprising at least one metal element,
wherein said coprecipitation reaction takes place in the presence of at least one carboxylate salt of the formula R 2 —COOM′, wherein:
M′ denotes Na or K, and
R 2 is H or an alkyl group having 1 to 4 carbon atoms, and
wherein said carboxylate salt of the formula R 2 —COOM′ is added before the coprecipitation reaction takes place.

2. The process according to claim 1 , wherein said at least one compound comprising at least one metal element is a dicarboxylate salt of the formula M(R 1 —COO) 2 , wherein:
R 1 is H or an alkyl group having 1 to 4 carbon atoms, and
M denotes 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) ; each y(i) representing a real number of the interval [0; 1], such that

∑

i
=
1

8

⁢

y
⁡

(
ⅈ
)

=
1.

3. The process according to claim 1 , wherein after said coprecipitation reaction, said hydrogel precursor is then subjected to a hydrothermal treatment to obtain said synthetic mineral particles.

4. The process according to claim 1 , wherein a coprecipitation medium comprising said hydrogel precursor is subjected directly to a hydrothermal treatment.

5. The process according to claim 2 , wherein R 1 and R 2 are selected from the group consisting of CH 3 —, CH 3 —CH 2 —, and CH 3 —CH 2 —CH 2 —.

6. The process according to claim 1 , wherein the groups R 1 and R 2 are identical.

7. The process according to claim 1 , wherein said synthetic mineral particles are silicate mineral particles.

8. The process according to claim 1 , wherein said synthetic mineral particles are phyllosilicate mineral particles.

9. The process according to claim 1 , wherein said hydrogel precursor of said synthetic mineral particles is a hydrogel of the formula
(Si x Ge 1-x ) 4 M 3 O 11 ,n ′H 2 O,

wherein:
x is a real number of the interval [0; 1], and
n′ is a number of molecule(s) of water associated with said hydrogel precursor.

10. The process according to claim 1 , wherein said at least one carboxylate salt of the formula R 2 —COOM′ is present in an amount so as to give, based on silicon, a molar ratio R 2 —COOM′/Si of from 0.1 to 9.

11. The process according to claim 3 , wherein said hydrothermal treatment is carried out at a temperature of from 150° C. to 400° C.

12. The process according to claim 3 , wherein said hydrothermal treatment is carried out at a pressure of from 5 bar to 200 bar.

13. The process according to claim 2 , wherein after said coprecipitation reaction, said hydrogel precursor is then subjected to a hydrothermal treatment to obtain said synthetic mineral particles.

14. A process for preparing a composition comprising synthetic phyllosilicate mineral particles, the process comprising:
(i) preparing a hydrogel precursor of said synthetic mineral particles by a coprecipitation reaction comprising:
(a) providing a first solution comprising at least one sodium metasilicate and at least one carboxylate salt of the formula R 2 —COOM′, wherein
M′ is Na or K, and
R 2 is H or an alkyl group having 1 to 4 carbon atoms; and

(b) rapidly adding to the first solution a second solution comprising at least one dicarboxylate salt of the formula M(R 1 —COO) 2 , wherein
R 1 is H or an alkyl group having 1 to 4 carbon atoms, and
M denotes 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) , each y(i) representing a real number of the interval [0; 1], such

that

∑

i
=
1

8

⁢

y
⁡

(
ⅈ
)

=
1

;

and
(ii) after said coprecipitation reaction, subjecting said hydrogel precursor to a hydrothermal treatment to obtain said synthetic phyllosilicate mineral particles.

15. The process according to claim 14 , wherein the synthetic phyllosilicate mineral particles have the formula
(Si x Ge 1-x ) 4 M 3 O 10 (OH) 2 ,

wherein
x is a real number of the interval [0; 1], and
M denotes 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) , each y(i) representing a real number of the interval [0; 1], such that

∑

i
=
1

8

⁢

y
⁡

(
i
)

=
1.

16. The process according to claim 14 , wherein
the at least one sodium metasilicate is Na 2 SiO 3 ,
the at least one carboxylate salt of the formula R 2 —COOM′ is CH 3 —COONa,
the at least one dicarboxylate salt of the formula M(R 1 —COO) 2 is Mg(CH 3 —COO) 2 , and
the synthetic phyllosilicate mineral particles have the formula Si 4 Mg 3 O 10 (OH) 2 .

Assignees

• Le Roux Christophe
• Martin Francois
• Micoud Pierre
• Dumas Angela
• Centre Nat Rech Scient
• Univ Toulouse 3 Paul Sabatier

Inventors

• Le Roux Christophe
• Martin Francois
• Micoud Pierre
• Dumas Angela

Classifications

• C01B33/20

  Silicates (persilicates C01B15/14 {; containing aluminium C01B33/26}) · CPC title

• C01B33/22

  Magnesium silicates · CPC title

• C01P2002/82

  by IR- or Raman-data · CPC title

• C01P2002/78

  by stacking-plane distances or stacking sequences · CPC title

• C01P2002/72

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