US4436883A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Polymerization using a support formed by heating silica gel in inert atmosphere
Assignee: Phillips Petroleum Co
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Filing: 1982-09-27
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Granted: 1984-03-13
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Expires: 2002-09-27
Abstract
Abstract A silica hydrogel is contacted with a hydroxy-containing organic compound which is not completely miscible with water but which is sufficiently miscible with water so as to remove water, and thereafter the organic compound is removed by heating in an inert atmosphere prior to activation by heating in air. The heating in the inert atmosphere allows utilizing preferred organic compounds such as C 5 and C 6 alcohols which are desirable from a commercial standpoint because of the easy separation for recycle. In a preferred embodiment, the hydrogel is aged at a pH of 7 to 9 by means of either adding a base or by utilizing a chromium component containing bound nitrogen.
Inventors
- 👤 Donald R. Witt
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 10:41
CPC Classifications
B; B01; B01J; B01J37/00; B01J37/0009; B01J37/0018; B01J21/00; B01J21/06; B01J21/063; B01J23/00; B01J23/16; B01J23/24; B01J23/26; C; C08; C08F; C08F10/00
Claims Analysis
Total Claims: 26
Claim 1
Independent Claim
129 words
A polymerization process comprising: contacting at least one mono-1-olefin having 2 to 8 carbon atoms per molecule in a reaction zone under polymerization conditions with a catalyst produced by a process comprising: (a) forming a silica hydrogel; (b) aging said hydrogel for a time of at least one hour; (c) treating the thus aged hydrogel with a volatile liquid saturated aliphatic alcohol having a solubility in water of less than 6 grams per 100 grams of water to convert said hydrogel to a xerogel; (d) subjecting the thus formed xerogel to a heat treatment in an inert atmosphere at an elevated temperature; (e) activating the thus heat treated xerogel, said xerogel also containing chromium, in an oxygen-containing ambient for a time sufficient to activate same; and recovering a polymer.
Claim 2
Dependent Claim
129 words
A polymerization process comprising: contacting at least one mono-1-olefin having 2 to 8 carbon atoms per molecule in a reaction zone under polymerization conditions with a catalyst produced by a process comprising: (a) forming a silica hydrogel; (b) aging said hydrogel for a time of at least one hour; (c) treating the thus aged hydrogel with a volatile liquid saturated aliphatic alcohol having a solubility in water of less than 6 grams per 100 grams of water to convert said hydrogel to a xerogel; (d) subjecting the thus formed xerogel to a heat treatment in an inert atmosphere at an elevated temperature; (e) activating the thus heat treated xerogel, said xerogel also containing chromium, in an oxygen-containing ambient for a time sufficient to activate same; and recovering a polymer.
Claim 3
Dependent Claim
23 words
A method according to claim 1 wherein said at least one mono-1-olefin is selected from ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 4-methyl-1-pentene, and 1-octene.
Claim 4
Dependent Claim
14 words
A method according to claim 1 wherein said at least one mono-1-olefin comprises ethylene.
Claim 5
Dependent Claim
15 words
A process according to claim 1 wherein said polymerization is carried out under slurry conditions.
Claim 6
Dependent Claim
25 words
A process according to claim 1 wherein said polymer is an ethylene homopolymer or a copolymer having 98 to 99.6 mole percent polymerized ethylene units.
Claim 7
Dependent Claim
14 words
A method according to claim 1 wherein said silica hydrogel is a silica-titania-chromium tergel.
Claim 8
Dependent Claim
19 words
A method according to claim 1 wherein said hydroxy-containing organic compound is a C 5 or C 6 alcohol.
Claim 9
Dependent Claim
19 words
A method according to claim 6 wherein said alcohol is selected from 3-methyl-butanol, 1-pentanol, and 1-hexanol or mixtures thereof.
Claim 10
Dependent Claim
46 words
A method according to claim 1 wherein said inert atmosphere comprises nitrogen and wherein said heat treatment in said nitrogen is carried out for a time within the range of 15 minutes to 1 hour at a temperature within the range of 800° to 1600° F.
Claim 11
Dependent Claim
25 words
A method according to claim 1 wherein said activating is carried out in air at a tempreature within the range of 1200° to 1500° F.
Claim 12
Dependent Claim
94 words
A method according to claim 10 wherein said silica hydrogel is a silica-titania-chromium tergel, said aging is carried out at a temperature of 65° to 200° F. for 1 to 20 hours and said alcohol is a C 5 or C 6 alcohol, said inert atmosphere is nitrogen, said activating is carried out in air and wherein said treatment in said inert atmosphere is carried out at a temperature within the range of 800° to 1600° F. and said activating is carried out at a temperature within the range of 1200° to 1500° F.
Claim 13
Dependent Claim
22 words
A method according to claim 11 wherein said aging is carried out at a pH within the range of 7 to 9.
Claim 14
Dependent Claim
28 words
A method according to claim 12 wherein said pH is maintained within the range of 7 to 9 by means of adding a basic material to said hydrogel.
Claim 15
Dependent Claim
17 words
A method according to claim 13 wherein said basic material is selected from ammonia or ammonium hydroxide.
Claim 16
Dependent Claim
16 words
A method according to claim 12 wherein said basic material is added prior to said aging.
Claim 17
Dependent Claim
29 words
A method according to claim 12 wherein said pH is maintained at said value of 7 to 9 by means of utilizing a coordination chromium compound having nitrogen-containing groups.
Claim 18
Dependent Claim
15 words
A method according to claim 16 wherein said chromium compound is chloropentamine chromium (III) chloride.
Claim 19
Dependent Claim
13 words
A method according to claim 16 wherein said hydrogel is a silica-titania-chromium tergel.
Claim 20
Dependent Claim
22 words
A method according to claim 1 wherein said aging is carried out at a pH within the range of 7 to 9.
Claim 21
Dependent Claim
28 words
A method according to claim 19 wherein said pH is maintained within the range of 7 to 9 by means of adding a basic material to said hydrogel.
Claim 22
Dependent Claim
17 words
A method according to claim 19 wherein said basic material is selected from ammonia or ammonium hydroxide.
Claim 23
Dependent Claim
16 words
A method according to claim 19 wherein said basic material is added prior to said aging.
Claim 24
Dependent Claim
29 words
A method according to claim 19 wherein said pH is maintained at said value of 7 to 9 by means of utilizing a coordination chromium compound having nitrogen-containing groups.
Claim 25
Dependent Claim
15 words
A method according to claim 23 wherein said chromium compound is chloropentamine chromium (III) chloride.
Claim 26
Dependent Claim
13 words
A method according to claim 23 wherein said hydrogel is a silica-titania-chromium tergel.
References Cited (Backward Citations)
US3887494A
Cited
GB1431975A
Cited
GB1530103A
Cited
US4081407A
Cited
GB1575419A
Cited
US4151122A
Cited
US4247421A
Cited
GB2050858B
Cited
GB2074039B
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1987-03-13 | 1987-09-12 | 1988-03-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-03-13 | 1991-09-12 | 1992-03-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-03-13 | 1995-09-12 | 1996-03-13 | $7700.00 | Window Closed / Lapsed |