Method for obtaining oxide catalysts on the base of exfoliated layered aluminosilicates

Patent metadata

Field	Value
Publication number	US-9636661-B2
Application number	US-201314398791-A
Country	US
Kind code	B2
Filing date	May 2, 2013
Priority date	May 9, 2012
Publication date	May 2, 2017
Grant date	May 2, 2017

Abstract

The present invention relates to the method of synthesising large-area oxide catalysts on the base of exfoliated layered aluminosilicates. As layered aluminosilicate are used bentonite, montmorillonite, nontronite and saponite.

First claim

The invention claimed is:

1. The method for obtaining oxide catalysts on the base of exfoliated layered aluminosilicates, comprising: wherein metal cations are introduced into the structure of the aluminosilicates such that at least one basic hydrophilic monomer is introduced to an interlayer space of layered aluminosilicate in the amount of 30% wt. to 90% wt. relative to the weight of aluminosilicate, or with the addition of a hydrophilic crosslinking monomer in the amount of up to 20 wt %. relative to the amount of the remaining basic hydrophilic monomer, and in situ polymerization is carried out in aqueous solution, then a resulting hybrid inorganic-organic layer material is submitted to sorption of at least one metal cation from the aqueous solution of its salt, followed by thermal treatment in the temperature range of 400-700° C., in an oxidizing atmosphere.

2. The method according to claim 1 , wherein bentonite, montmorillonite, nontronite and saponite are used as layered aluminosilicate.

3. The method according to claim 1 , wherein the base monomer is a monomer containing a polar hydrophilic group.

4. The method according to claim 3 , wherein the polar hydrophilic group is a carboxyl, hydroxyl, sulfo, amino, primary or secondary amine group.

5. The method according to claim 1 , wherein the basic monomer is selected from the group containing acrylic acid, methacrylic acid, acrylamide, N-vinylformamide, vinyl alcohol, 2-hydroxyethyl methacrylate.

6. The method according to claim 1 , wherein as a crosslinking monomer a monomer is used which contains in the molecule more than one double bond.

7. The method according to claim 1 , wherein the crosslinking monomer is selected from the group containing N,N′-methylenebisacrylamide, ethylene glycol dimethacrylate, ethylene glycol diacrylate.

8. The method according to claim 1 , wherein the weight ratio of the basic monomer to crosslinking monomer ranges from 1.0 to 4.0.

9. The method according to claim 1 , wherein the polymerization process is carried out at the temperature of 20 to 70° C. in an inert gas atmosphere.

10. The method according to claim 1 , wherein the polymerization process is carried out with the addition of an initiator.

11. The method according to claim 10 , wherein as the initiator ammonium persulfate, dihydrochloride 2,2′-azobis (2-methyl-propionamide) is used.

12. The method according to claim 1 , wherein the metal cation is a transition metal cation.

13. The method according to claim 1 , wherein the metal cation is selected from the group containing Fe, Ni, Co, Cu, Mo, Zn, Cr, Mn.

14. The method according to claim 1 , wherein the metal salt nitrate or chloride salts are used.

15. The method according to claim 1 , wherein the metal salt is selected from the group containing: Fe(NO 3 ) 3 .9H 2 O, FeCl 3 .6H 2 O, Cu(NO 3 ) 2 .3H 2 O, CuCl 2 , Co(NO 3 ) 2 .6H 2 O, CoCl 2 , CoCl 2 .6H 2 O, Ni(NO 3 ) 2 .6H 2 O, NiCl 2 .6H 2 O, NiCl 2 , MoCl 2 , Zn(NO 3 ) 2 .H 2 O, Zn(NO 3 ) 2 , ZnCl 2 , Cr(NO 3 ).9H 2 O, CrCl 3 .6H 2 O, Mn(NO 3 ) 2 .6H 2 O, MnCl 2 .4H 2 O.

16. The method according to claim 1 , wherein sorption stage is carried out in such a way that the hybrid inorganic-organic layer material obtained in the polymerization step a is dried at the temperature of 20 to 90° C., homogenized and milled, then an obtained nanocomposite powder is suspended in a metal salt solution and is stirred in the suspension at the temperature of 20 to 80° C., for 1 to 96 h.

17. The method according to claim 16 , wherein the weight ratio of the nanocomposite to the metal salt in the solution is from 1.0 to 30.0.

18. The method according to claim 1 , wherein the heat treatment is carried out in an air atmosphere for 1 to 24 hours.

19. The method according to claim 1 , wherein the thermal treatment is done by raising temperature at the rate of 0.1 to 50° C./min.

Assignees

• Univ Jagiellonski

Inventors

• Kustrowski Piotr
• Natkanski Piotr
• Bialas Anna
• Janus Paula

Classifications

• B01J23/745 Primary

  Iron · CPC title

• B01J37/0036

  Grinding · CPC title

• B01J37/0201

  Impregnation · CPC title

• B01J37/14

  with gases containing free oxygen · CPC title

• C01B39/026

  After-treatment · CPC title