Process for the manufacture of spherical alumina-containing particles

• US 4,013,587 A
• Filed: 02/03/1976
• Issued: 03/22/1977
• Est. Priority Date: 02/04/1975
• Status: Expired due to Term

• Current Assignee: Kali-Chemie AG (Solvac SA)
• Original Assignee: Kali-Chemie AG (Solvac SA)
• Inventors: Fischer, Hermann, Schindler, Hubert, Weidenbach, Guenter, Kuhrt, Winfried
• Primary Examiner(s): Shine, W. J.
• Application Number:
  US05/654,923
• Time in Patent Office: 413 Days
• Field of Search: 252/448, 252/455 R, 252/463, 252/465, 423/628, 423/630
• US Class Current: 502/8
• CPC Class Codes: B01J 2/08 Gelation of a colloidal solution
• CPC Class Codes: B01J 21/04 Alumina
• CPC Class Codes: B01J 35/51 Spheres
• CPC Class Codes: B01J 37/0018 Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
• CPC Class Codes: B01J 37/0072 Preparation of particles, e.g. dispersion of droplets in an oil bath

Abstract

Disclosed is process for the preparation of alumina-containing particles, comprising the steps of (a) mixing an aluminum oxide hydrosol containing a hydrate of alumina or activated alumina and an additive component selected from a high molecular weight natural organic material which is insoluble in aqueous solution up to a temperature of 50° C. and carbon with a solution of hydrolyzable base to form a mixture; (b) introducing the mixture in dispersed form into a water-immiscible liquid having a temperature of from about 60 to 100° C., whereby gel particles are formed; (c) aging the gel particles in the liquid at the temperature and subsequently in an aqueous ammonia solution; (d) recovering the aged particles; and (e) calcining the recovered particles.

Claims

1. A process for the preparation of alumina-containing particles, comprising the steps of:

a. mixing an aluminum oxide hydrosol containing a hydrate of alumina or activated alumina and an additive component of wood flour, starch, carbon black or carbon powder with a solution of a hydrolyzable base to form a mixture;

b. introducing said mixture in dispersed form into a water-immiscible liquid having a temperature of from about 60°

to 100°

C., whereby gel particles are formed;

c. aging said gel particles in said liquid at said temperature and subsequently in an aqueous ammonia solution;

d. recovering said aged particles; and

e. drying and calcining said recovered particles.

2. The process of claim 1, wherein said recovery step comprises washing said particles with water and drying said washed particles.

3. The process of claim 1, wherein said aluminum oxide hydrosol further contains a low density silica-containing substance.

4. The process of claim 1, wherein said additive component comprises wood flour or starch having a particle size of up to about 100μ

.

5. The process of claim 1, wherein said additive component comprises carbon black having a particle size of up to about 100 m μ

.

6. The process of claim 1, wherein said additive component is present in an amount sufficient to provide from about 3 to 35% by weight based upon the weight of the calcined particles.

7. The process of claim 6, wherein said amount is between about 5 and 25%.

8. The process of claim 1, wherein said particles are dried at a temperature of from about 120°

C. to 200°

C. and are calcined first at a temperature of between about 250°

C. to 400°

C. and then at a temperature of between about 600°

C. and 1000°

C.

9. The process of claim 1, wherein said aluminum oxide in said hydrosol is present in an amount sufficient to provide from about 15 to 35% by weight Al₂ O₃ based upon the mass of the calcined particles.

10. The process of claim 9, wherein said aluminum oxide in said hydrosol provides from about 20 to 30% of said Al₂ O₃.

11. The process of claim 1, wherein the hydrate of alumina or the activated alumina has an average particle diameter of up to about 10 μ

.

12. The process of claim 1, wherein the hydrate of alumina or the activated alumina is present in said hydrosol in an amount sufficient to provide from about 65 to 85% by weight of the calcined particles.

13. The process of claim 12, wherein said amount is from about 70 to 80% by weight.

14. The process of claim 3, wherein said silica-containing substance is present in an amount sufficient to provide a SiO₂ content of from about 10 to 40% by weight of the calcined particles.

15. The process of claim 3, wherein said silica-containing substance comprises a pyrogenic silica.

16. The process of claim 2, wherein said aluminum oxide hydrosol further contains a difficulty-soluble compound of at least one catalytically-active metal.

17. The process of claim 16, wherein said catalytically active metal comprises copper and chromium.

18. The process of claim 17, wherein said compounds of copper and chromium are present in an amount sufficient to provide a content of from about 3 to 15% by weight based upon the calcined particles each of copper-2-oxide and chromium-3-oxide.

19. The process of claim 18, wherein said copper-2-oxide and chromium-3-oxide content are each from about 7 to 10% by weight.