Polyaluminum salts and their uses in preparation of high-purity colloidal aluminum-silica composite particles and zeolites

Patent metadata

Field	Value
Publication number	US-10654724-B2
Application number	US-201715827396-A
Country	US
Kind code	B2
Filing date	Nov 30, 2017
Priority date	Dec 2, 2016
Publication date	May 19, 2020
Grant date	May 19, 2020

Abstract

Disclosed are novel aqueous aluminum complex compositions and methods of making and using them. The novel compositions comprise very low halide content, even when made from aluminum chlorohydrate. The compositions find use in the production of zeolites, coatings, abrasives, binders, and refractories; and in the treatment of wastewater for example. The methods of making the novel compositions include passing a first aqueous aluminum complex composition through an anion exchange column or otherwise contacting the first composition with the anion exchange resin to provide a second aqueous aluminum complex composition that is different from the first aqueous aluminum complex composition. Also disclosed are methods of making zeolites and aqueous silica-alumina compositions from the novel aqueous aluminum complex compositions.

First claim

What is claimed is:

1. A method comprising:
combining in an aqueous blend a water-soluble aluminum salt and a first acid having a pKa of 3.5 to 9.5 to form a first aqueous aluminum complex composition; and
contacting the first aqueous aluminum complex composition with a water-insoluble anion exchange resin to provide a second aqueous aluminum complex composition.

2. The second aqueous aluminum complex composition of claim 1 .

3. The method of claim 1 , wherein the water-soluble aluminum salt is aluminum chlorohydrate.

4. The method of claim 1 , wherein the method further comprises preconditioning a basic anion exchange resin with a second acid having a pKa of 3.5 to 9.5 to provide the water-insoluble anion exchange resin.

5. The method of claim 4 , wherein each of the first acid and the second acid is individually selected from the group consisting of acetic acid, boric acid, lactic acid, and any combination thereof.

6. The method of claim 4 , wherein the second acid is acetic acid.

7. The method of claim 1 , further comprising, in order:
optionally diluting or concentrating the second aqueous aluminum complex composition; and
combining the second aqueous aluminum complex composition with an aqueous alkali, an aqueous colloidal silica, and optionally a structure directing agent to form an aqueous silica-alumina composition, wherein the structure directing agent is selected from the group consisting of N,N,N-trimethyl-1-adamantylammonium hydroxide, tetramethylammonium hydroxide, tetrapropylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide, tetrahexylammonium hydroxide, tetraoctylammonium hydroxide, methyltributylammonium hydroxide, methyltriethylammonium hydroxide, phenyltrimethylammonium hydroxide, methyltripropylammonium hydroxide, dodecyltrimethylammonium hydroxide, hexadecyltrimethylammonium hydroxide, N-dodecyl N-ethyl N,N-dimethyl ammonium hydroxide, N,N-dimethyl N,N-diethyl ammonium hydroxide, and any combination thereof.

8. The method of claim 7 , wherein silica in the aqueous silica-alumina composition has a particle size of about 3 nm to about 150 nm.

9. The method of claim 7 , wherein the aqueous silica-alumina composition includes the structure directing agent, and the structure directing agent is N,N,N-trimethyl-1-adamantylammonium hydroxide.

10. The method of claim 7 , wherein the aqueous alkali is selected from the group consisting of aqueous sodium hydroxide, aqueous potassium hydroxide, and a combination thereof.

11. The method of claim 7 , the method further comprising heating the aqueous silica-alumina composition under autogenous pressure at a temperature between 100° C. and 250° C. for 12 hours to 24 hours to provide an aqueous zeolite composition comprising an uncalcined zeolite product.

12. The method of claim 11 , the method further comprising separating the uncalcined zeolite product from the aqueous zeolite composition, and washing the uncalcined zeolite product.

13. The method of claim 11 , the method further comprising heating the uncalcined zeolite product for 1 hour to 12 hours at 400° C. to 1000° C. to provide a calcined zeolite.

14. The method of claim 13 , wherein the aqueous silica-alumina composition includes the structure directing agent, the structure directing agent is N,N,N-trimethyl-1-adamantylammonium hydroxide, and the calcined zeolite is a chabazite.

15. The calcined zeolite of claim 13 .

16. A method comprising:
combining in an aqueous blend a water-soluble aluminum salt, a first acid having a pKa of 3.5 to 9.5, and an aqueous colloidal silica to form an aluminum-silica reaction product;
passing the aluminum-silica reaction product through a fixed bed of a water-insoluble anion exchange resin to provide an aluminum-silica effluent;
optionally diluting or concentrating the aluminum-silica effluent; and
combining the aluminum-silica effluent with an aqueous alkali, further aqueous colloidal silica, and optionally a structure directing agent to form an aqueous silica-alumina composition, wherein the structure directing agent is selected from the group consisting of N,N,N-trimethyl-1-adamantylammonium hydroxide, tetramethylammonium hydroxide, tetrapropylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide, tetrahexylammonium hydroxide, tetraoctylammonium hydroxide, methyltributylammonium hydroxide, methyltriethylammonium hydroxide, phenyltrimethylammonium hydroxide, methyltripropylammonium hydroxide, dodecyltrimethylammonium hydroxide, hexadecyltrimethylammonium hydroxide, N-dodecyl N-ethyl N,N-dimethyl ammonium hydroxide, N,N-dimethyl N,N-diethyl ammonium hydroxide, and any combination thereof.

17. The method of claim 16 , wherein silica in the aqueous silica-alumina composition has a particle size of 3 nm to 150 nm.

18. The method of claim 16 , wherein the aqueous silica-alumina composition includes the structure directing agent, and the structure directing agent is N,N,N-trimethyl-1-adamantylammonium hydroxide.

19. The method of claim 16 , the method further comprising heating the aqueous silica-alumina composition under autogenous pressure at a temperature between 100° C. and 250° C. for 12 hours to 24 hours to provide an aqueous zeolite composition comprising an uncalcined zeolite product.

20. The method of claim 19 , the method further comprising heating the uncalcined zeolite product for 1 hour to 12 hours at 400° C. to 1000° C. to provide a calcined zeolite.

Assignees

• Ecolab Usa Inc

Inventors

• Lin Wenyong
• Batllo Francois
• John Shiby
• Romba Michael

Classifications

• C01B33/26

  Aluminium-containing silicates {, i.e. silico-aluminates} · CPC title

• B01J13/0047

  containing a metal oxide · CPC title

• C01B39/48

  using at least one organic template directing agent · CPC title

• B01J20/18

  Synthetic zeolitic molecular sieves · CPC title

• C01F7/46

  Purification of aluminium oxide, aluminium hydroxide or aluminates (C01F7/028 takes precedence) · CPC title