# US 4,392,988 A · Method of producing stable alumina

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- Number: US 4,392,988 A
- Document ID: US4392988A
- Status: Granted
- Kind: A
- Application number: 06/262,230
- Filed: 1981-05-11
- Granted: 1983-07-12
- Earliest claimed: 1981-05-11
- Assignees: GA Technologies Inc.
- Inventors: Jesse C. Dobson; Richard W. Knight, Jr.
- Web page: https://patentgrep.com/patent/US4392988A

## CPC

- B01J 21/12: Silica and alumina
- B01J 20/08: comprising aluminium oxide or hydroxide; comprising bauxite
- B01J 37/08: Heat treatment {(B01J37/0009, B01J37/0018 take precedence)}
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

Microspheres of activated alumina are thermally and chemically stabilized by soaking the spheres in silicone liquid and decomposing the silicone liquid in an inert atmosphere to leave a silica residue infused in the alumina crystal structure resulting in a silica-alumina phase over the internal and external structure of the alumina. The treated microspheres are then heated in the presence of oxygen to burn off residual carbon resulting from the decomposition of the silicone liquid.

## Claims

### Claim 1

A method of treating activated alumina to impart increased chemical stability and heat resistance thereto comprising
soaking activated alumina in silicone liquid to impregnate said activated alumina therewith,
draining excess silicone liquid from said activated alumina, and
heating said silicone liquid impregnated activated alumina in an oxygen-free atmosphere to between about 350.degree. C. and about 1100.degree. C. to leave a silica residue infused in the crystallite structure resulting in a silica-alumina phase over the internal and external structure of said alumina.

### Claim 2 (depends on 1)

A method according to claim 1 in which said activated alumina having said silica residue is further heated in the presence of oxygen to burn off carbon residue at a temperature below the .alpha.-phase conversion temperature of activated alumina.

### Claim 3 (depends on 1)

A method according to claim 1 in which said activated alumina is provided by preparing hydrated alumina gel microspheres and calcining said gel microspheres at temperatures of between about 400.degree. C. and about 1000.degree. C. to drive water from said hydrated gel microspheres and convert the same to activated alumina microspheres.

### Claim 4 (depends on 1)

A method according to claim 1 in which said silicone liquid is polydimethylsiloxane.

### Claim 5 (depends on 1)

A method according to claim 1 wherein said silicone liquid is selected from polysiloxanes and mixtures thereof having the general formula: ##STR2## where R and R' are selected from groups consisting of hydrogen, alkyl, aryl, alkyloxy, and aryloxy.

### Claim 6 (depends on 1)

A method according to claim 1 wherein said silicone liquid has a viscosity at least about 200 cst at 25.degree. C.

### Claim 7 (depends on 3)

A method according to claim 3 wherein said activated alumina microspheres are selected having a maximum diameter of about 1 mm, said silicone liquid is selected having a viscosity of at least about 200 cst at 25.degree. C., and said selected microspheres are soaked for at least about 15 minutes in said silicone liquid heated to between about 150.degree. C. and about 225.degree. C. to reduce its viscosity to below about 20 cst.

### Claim 8 (depends on 1)

A method according to claim 1 wherein said silicone liquid-impregnated alumina is heated to at least about 350.degree. C. to decompose said silicone liquid.

### Claim 9 (depends on 1)

A method according to claim 1 wherein said silicone liquid-impregnated alumina is heated to at least about 600.degree. C. to decompose said silicone liquid.

### Claim 10 (depends on 2)

A method according to claim 2 wherein said activated alumina having said silica residue is heated in an atmosphere having at least about 10% oxygen at a temperature of at least about 600.degree. C.