US3954958A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Preparation of aluminum hydrate
Assignee: Sumitomo Chemical Co Ltd
•
Filing: 1974-12-05
•
Granted: 1976-05-04
•
Expires: 1994-12-05
Abstract
Abstract Powdery alumina hydrate is produced from an alkylaluminum compound by hydrolysis of the alkylaluminum compound by water through the following steps; converting the alkylaluminum compound to an ether complex compound: partially hydrolyzing the ether complex compound in the presence of an non-reactive solvent at a temperature of not higher than about 150 DEG C with stirring so that no alumina hydrate is precipitated until at least 0.8 moles of water reacts with one mole of the alkylaluminum compound, thereby forming polyaluminoxane; completely hydrolyzing the resulting polyaluminoxane at a concentration of not more than about 3.0 grams-atoms as aluminum per liter of non-reactive solvent at a temperature of about 10 DEG to about 150 DEG C with stirring, so that one mole of the feed alkylaluminum compound may be ultimately hydrolyzed completely with 2 to 10 moles of water, thereby precipitating alumina hydrate; and then separating the resulting alumina hydrate from the non-reactive solvent. The alumina hydrate has a good forming ability and also an ability to provide formed shapes having a good mechanical strength.
Inventors
- 👤 Atsuro Matsui
- 👤 Hidekimi Kadokura
- 👤 Tadaaki Yako
- 👤 Hiroshi Umezaki
- 👤 Kazuo Iida
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 06:09
CPC Classifications
C; C01; C01F; C01F7/00; C01F7/02; C01F7/34; C01F7/36
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
254 words
A process for producing a powdery alumina hydrate from an alkylaluminum compound by hydrolysis by water, which comprises reacting an alkylaluminum compound having the general formula: ##EQU6## wherein R 1 represents a hydrogen atom, alkyl group having 1 to 8 carbon atoms or alkoxy group having 1 to 6 carbon atoms, R 2 and R 3 represent alkyl groups having 1 to 8 carbon atoms with an ether to form an ether complex compound, said ether being an ether compound having a boiling point of not more than 175° C and an ability to form a coordination compound with an alkylaluminum compound; partially hydrolyzing the ether complex compound in the presence of a non-reactive solvent selected from the group consisting of ethers having a boiling point of not higher than 175° C as were capable of use in the partial hydrolysis, aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons and mixtures thereof at a temperature of not higher than about 150° C with stirring, while preventing precipitation of alumina hydrate until at least 0.8 moles of water reacts with one mole of the alkylaluminum compound, thereby forming polyaluminoxane; completely hydrolyzing the formed polyaluminoxane at a concentration of not more than about 3.0 gram-atoms as aluminum per liter of said non-reactive solvent at a temperature of from about 10° to about 150° C with stirring, thereby completely hydrolyzing ultimately 1 mole of the feed alkylaluminum compound with 2 to 10 moles of water to precipitate alumina hydrate; and separating the resulting alumina hydrate from said non-reactive solvent.
Claim 2
Dependent Claim
254 words
A process for producing a powdery alumina hydrate from an alkylaluminum compound by hydrolysis by water, which comprises reacting an alkylaluminum compound having the general formula: ##EQU6## wherein R 1 represents a hydrogen atom, alkyl group having 1 to 8 carbon atoms or alkoxy group having 1 to 6 carbon atoms, R 2 and R 3 represent alkyl groups having 1 to 8 carbon atoms with an ether to form an ether complex compound, said ether being an ether compound having a boiling point of not more than 175° C and an ability to form a coordination compound with an alkylaluminum compound; partially hydrolyzing the ether complex compound in the presence of a non-reactive solvent selected from the group consisting of ethers having a boiling point of not higher than 175° C as were capable of use in the partial hydrolysis, aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons and mixtures thereof at a temperature of not higher than about 150° C with stirring, while preventing precipitation of alumina hydrate until at least 0.8 moles of water reacts with one mole of the alkylaluminum compound, thereby forming polyaluminoxane; completely hydrolyzing the formed polyaluminoxane at a concentration of not more than about 3.0 gram-atoms as aluminum per liter of said non-reactive solvent at a temperature of from about 10° to about 150° C with stirring, thereby completely hydrolyzing ultimately 1 mole of the feed alkylaluminum compound with 2 to 10 moles of water to precipitate alumina hydrate; and separating the resulting alumina hydrate from said non-reactive solvent.
Claim 3
Dependent Claim
43 words
A process according to claim 1, wherein the alkylaluminum compound is at least one of trimethylaluminum, triethylaluminum, tri-n-propylaluminum, tri-n-butylaluminum, tri-isobutylaluminum, tripentylaluminum, trihexylaluminum, trioctylaluminum, diethylaluminum hydride, di-n-propylaluminum hydride, di-isobutylaluminum hydride, dipentylaluminum hydride, dihexylaluminum hydride, dioctylaluminum hydride, ethoxydiethylaluminum, isopropoxydiethylaluminum, isopropoxydipropylaluminum, ethoxydibutylaluminum, isopropoxydibutylaluminum, butoxydibutylaluminum and hexoxydioctylaluminum.
Claim 4
Dependent Claim
25 words
A process according to claim 1, wherein the ether is dimethylether, diethylether, diisopropylether, di-n-propylether, diallylether, ethyl-n-propylether, methyl-n-butylether, anisole, phenetole, dioxane, tetrahydrofuran, dihydrofuran, furan, or tetrahydropyran.
Claim 5
Dependent Claim
19 words
A process according to claim 1, wherein the partial hydrolysis is carried out by slowly adding water with stirring.
Claim 6
Dependent Claim
22 words
A process according to claim 1, wherein the partial hydrolysis is carried out by adding ether containing water in a solution state.
Claim 7
Dependent Claim
24 words
A process according to claim 1, wherein the partial hydrolysis is carried out at a temperature of from about 10° to about 110° C.
Claim 8
Dependent Claim
19 words
A process according to claim 1, wherein the polyaluminoxane has a mean molecular weight of not less than 300.
Claim 9
Dependent Claim
21 words
A process according to claim 7, wherein the polyaluminoxane has a mean molecular weight of from about 500 to about 30,000.
Claim 10
Dependent Claim
17 words
A process according to claim 1, wherein the polyaluminoxane is subjected to aging before the complete hydrolysis.
Claim 11
Dependent Claim
28 words
A process according to claim 9, wherein the aging is carried out at a temperature of from 0° to 160° C for about 0.5 to about 10 hours.
Claim 12
Dependent Claim
29 words
A process according to claim 1, wherein the complete hydrolysis is carried out at a concentration of 0.5 to 2.5 gram-atoms as aluminum per liter of the non-reactive solvent.
Claim 13
Dependent Claim
24 words
A process according to claim 1, wherein one mole of the feed alkylaluminum compound is hydrolyzed ultimately with 2.5 to 7 moles of water.
Claim 14
Dependent Claim
24 words
A process according to claim 1, wherein the complete hydrolysis is carried out at a temperature of from about 20° to about 110° C.
Claim 15
Dependent Claim
15 words
A process according to claim 1, wherein the water is supplied in a liquid state.
Claim 16
Dependent Claim
12 words
A process according to claim 14, wherein the water is supplied continuously.
Claim 17
Dependent Claim
12 words
A process according to claim 14, wherein the water is supplied discontinuously.
Claim 18
Dependent Claim
42 words
A process according to claim 1, wherein the non-reactive solvent is dimethylether, diethylether, diisopropylether, di-n-propylether, diallylether, ethyl-n-propylether, methyl-n-butylether, anisole, phenetole, dioxane, tetrahydrofuran, dihydrofuran, furan, tetrahydropyran, pentane, hexane, heptane, octane, cyclopentane, cyclohexane, cyclohexene, benzene, toluene, xylene, petroleum ether, ethylbenzene, cumene, methylcyclohexane or ethylcyclohexane.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-05-04 | 1979-11-03 | 1980-05-04 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-05-04 | 1983-11-03 | 1984-05-04 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-05-04 | 1987-11-03 | 1988-05-04 | $7700.00 | Window Closed / Lapsed |