Process for the preparation of double metal oxide powders containing a Group IIIA and a Group IVB element and a novel double metal hydroxyl carboxylate useful in preparing same

• US 5,196,388 A
• Filed: 06/10/1991
• Issued: 03/23/1993
• Est. Priority Date: 06/10/1991
• Status: Expired due to Fees

• Current Assignee: AKZO NV (Nouryon BV)
• Original Assignee: AKZO NV (Nouryon BV)
• Inventors: Shyu, Lieh-Jiun
• Primary Examiner(s): Dixon, Jr., William R.
• Assistant Examiner(s): MARCANTONI, PAUL D
• Application Number:
  US07/713,195
• Time in Patent Office: 652 Days
• Field of Search: 423/593, 423/598, 423/600, 501/126, 501/127, 501/136, 501/139, 501/153, 501/134
• US Class Current: 501/134
• CPC Class Codes: C01B 13/363 Mixtures of oxides or hydroxides by precipitation
• CPC Class Codes: C01G 23/003 Titanates C01G23/001 takes precedence
• CPC Class Codes: C04B 35/478 based on aluminium titanates
• CPC Class Codes: C04B 35/626 Preparing or treating the powders individually or as batches pigments for ceramics C09C1/0009; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B

Abstract

Disclosed is a process for the preparation of double metal oxide ceramic powders which contain at least one metal of Group IIIA, inclusive of aluminum and gallium, and at least one metal of Group IVB, inclusive of titanium and zirconium. The process involves a first step in which an aqueous solution of mixed metal alkoxides or salts is formed and which also contains a chelating agent, preferably a polycarboxylic acid, and a second step in which a base is added in order to cause precipitation of a mixed metal hydroxyl groups-containing precursor that can be calcined or otherwise converted to the final mixed metal oxide. The invention also pertains to novel double metal hydroxyl carboxylates which are useful intermediates in preparing double metal oxides.

Claims

1. A process for the preparation of double metal oxide ceramic powders which contain at least one metal of Group IIIA and at least one metal of Group IVB comprising the steps of:

(a) forming an aqueous solution of mixed metal compounds which respectively contain said Group IIIA and Group IVB metals and which compounds are selected from the group consisting of the metal salts, the metal alkoxides, and the mixtures thereof, the solution also containing a polyfunctional compound capable of chelating the metal compounds;

(b) adding an effective amount of a base to the solution formed under (a) in order to form a homogeneous double metal precipitate; and

,

(c) converting the precipitate formed under (b) into a double metal oxide.

2. A process according to claim 1, wherein the polyfunctional compound capable of chelating said metal compounds is a polycarboxylic compound.

3. A process according to claim 2, wherein the polycarboxylic compound is a polycarboxylic acid.

4. A process according to claim 3, wherein the polycarboxylic acid is a dicarboxylic acid.

5. A process according to claim 4, wherein the dicarboxylic acid is selected from the group consisting of oxalic acid, malonic acid, adipic acid, malic acid, maleic acid, succinic acid, itaconic acid, citraconic acid, glutaric acid, and mixtures thereof.

6. A process according to claim 1, wherein the Group IIIA metal is aluminum and the Group IVB metal is titanium.

7. A process according to claim 6, wherein the polyfunctional compound capable of chelating said metal compounds is oxalic acid.

8. A process according to claim 7, wherein aluminum is used in the form of an inorganic acid salt and titanium is used in the form of an alkoxide.

9. A process according to claim 1, wherein the base is selected from the group consisting of sodium hydroxide, potassium hydroxide, ammonium hydroxide, magnesium hydroxide, calcium hydroxide, and mixtures thereof.

10. A process according to claim 3, wherein the base is selected from the group consisting of sodium hydroxide, potassium hydroxide, ammonium hydroxide, magnesium hydroxide, calcium hydroxide, and mixtures thereof.

11. A process according to claim 8, wherein the base is ammonium hydroxide.

12. A hydroxyl groups-containing double metal compound obtainable by a process involving the steps (a) and (b) as described in claim 1, in accordance with the general molecular formula

15. A double metal compound according to claim 12, wherein the Group IIIA metal is aluminum and the Group IVB metal is titanium.

19. A method of using a double metal compound according to claim 12 to prepare a double metal oxide, comprising the step of subjecting said compound to sufficient heat to effect decomposition.

13. A double metal compound in accordance with the general structural formula ##STR3## in which A represents a Group IIIA metal;

B represents a Group IVB metal;

n represents an integer greater than 1

R represents an organic radical

r is 0 or 1.

14. A double metal compound according to claim 13, wherein the organic radical is of the general formula --(CH₂)_y -- in which y represents an integer of from 0 to 6.

16. Aluminum-titanium-hydroxyl-oxalate.

17. A process for the preparation of a double metal hydroxyl carboxylate containing at least one metal of Group IIIA, inclusive of aluminum and gallium, and at least one metal of Group IVB, inclusive of titanium and zirconium, comprising the steps of

(a) forming a mixed aqueous solution of compounds which contain said metals and which are selected from the group consisting of metal salts, metal alkoxides, and mixtures thereof, the solution also containing a polycarboxylic compound capable of chelating the metal compounds;

and,

(b) adding an effective amount of a base to the solution formed under (a) in order to form a homogeneous double metal precipitate.

18. A method of using a double metal compound obtainable by a process in accordance with claim 17 to prepare a double metal oxide,.comprising the step of subjecting said compound to sufficient heat to effect decomposition.

20. A method of using aluminum-titanium-hydroxyl oxalate to prepare aluminum titanate, comprising the step of heating the hydroxyl oxalate to a temperature of from 1000°

C. to 1500°

C. for a sufficient period of time to effect decomposition.