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US4405501A Expired / Lapsed US ⏱️ 0.0 years remaining

Aging of chromium-containing gel at high pH

Assignee: Phillips Petroleum Co
•
Filing: 1982-01-20
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Granted: 1983-09-20
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Expires: 2002-01-20
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Abstract

Abstract A silica hydrogel containing chromium is aged under conditions such that at least a portion of the aging is carried out at a pH within the range of 7 to 9. The resulting hydrogel is converted to a xerogel by treating with a volatile organic liquid. The desired pH can be obtained either by adding a basic material such as ammonia to the hydrogel prior to or during the aging process or by using a chromium component which inherently gives a higher pH and/or resists the natural tendency for the pH to decrease during aging. An example of such a chromium compound is chloropentammine chromium(III)chloride. The resulting catalyst on activation is particularly suitable for olefin polymerization under conditions where higher melt flow polymer is desire

Inventors

  • 👤 Donald R. Witt

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 22:04
CPC Classifications
C; C08; C08F; C08F10/00

Claims Analysis

Total Claims: 27
Claim 1
Independent Claim 87 words
A process comprising: forming a co-gelled silica-chromium hydrogel; aging said hydrogel for a time of at least one hour; maintaining a pH of said hydrogel during at least a major portion of said aging at a value within the range of 7 to 9; and treating said hydrogel with a volatile liquid organic compound to remove water and thus convert said hydrogel to a xerogel, said chromium being present in an amount to give 0.001 to 10 weight percent chromium based on the weight of said xerogel.
Claim 2
Dependent Claim 87 words
A process comprising: forming a co-gelled silica-chromium hydrogel; aging said hydrogel for a time of at least one hour; maintaining a pH of said hydrogel during at least a major portion of said aging at a value within the range of 7 to 9; and treating said hydrogel with a volatile liquid organic compound to remove water and thus convert said hydrogel to a xerogel, said chromium being present in an amount to give 0.001 to 10 weight percent chromium based on the weight of said xerogel.
Claim 3
Dependent Claim 28 words
A method according to claim 1 wherein said pH is maintained within the range of 7 to 9 by means of adding a basic material to said hydrogel.
Claim 4
Dependent Claim 17 words
A method according to claim 2 wherein said basic material is one of ammonia or ammonium hydroxide.
Claim 5
Dependent Claim 16 words
A method according to claim 2 wherein said basic material is added prior to said aging.
Claim 6
Dependent Claim 15 words
A method according to claim 2 wherein said volatile liquid organic compound is an alcohol.
Claim 7
Dependent Claim 16 words
A method according to claim 5 wherein said alcohol is one of 1-pentanol, 3-methyl-1-butanol, or 1-hexanol.
Claim 8
Dependent Claim 15 words
A method according to claim 1 wherein said volatile liquid organic compound is an alcohol.
Claim 9
Dependent Claim 16 words
A method according to claim 7 wherein said alcohol is one of 1-pentanol, 3-methyl-1-butanol, or 1-hexanol.
Claim 10
Dependent Claim 30 words
A method according to claim 1 wherein said pH is maintained at said value of 7 to 9 by means of utilizing a coordination chromium compound having a nitrogen-containing group.
Claim 11
Dependent Claim 14 words
A method according to claim 9 wherein said chromium compound is chloropentamine chromium(III) chloride.
Claim 12
Dependent Claim 24 words
A method according to claim 1 wherein said hydrogel is formed by adding a solution of sodium silicate into acid containing a chromium compound.
Claim 13
Dependent Claim 40 words
A method according to claim 11 wherein said aging is carried out at a temperature within the range of 65° F. (18° C.) to 200° F. (93° C.) for a time within the range of one hour to 20 hours.
Claim 14
Dependent Claim 36 words
A method according to claim 1 comprising in addition heating said xerogel in an oxygen containing ambient at a temperature within the range of 800° F. (425° C.) to 2000° F. (1095° C.) to activate same.
Claim 15
Dependent Claim 9 words
A catalyst produced by the method of claim 1.
Claim 16
Dependent Claim 51 words
A process comprising: forming a silica, titania, chromium tergel hydrogel, said chromium coming from a coordination chromium compound having a nitrogen-containing group; aging said hydrogel for at least one hour; and treating said hydrogel with a volatile liquid organic compound to remove water and thus convert said hydrogel to a xerogel.
Claim 17
Dependent Claim 51 words
A process comprising: forming a silica, titania, chromium tergel hydrogel, said chromium coming from a coordination chromium compound having a nitrogen-containing group; aging said hydrogel for at least one hour; and treating said hydrogel with a volatile liquid organic compound to remove water and thus convert said hydrogel to a xerogel.
Claim 18
Dependent Claim 14 words
A method according to claim 15 wherein said volatile organic liquid is an alcohol.
Claim 19
Dependent Claim 16 words
A method according to claim 15 wherein said alcohol is one of 1-pentanol, 3-methyl-1-butanol, or 1-hexanol.
Claim 20
Dependent Claim 19 words
A method according to claim 15 wherein said chromium compound is selected from hexamminechromium(III) nitrate and chloropentamine chromium(III) chloride.
Claim 21
Dependent Claim 28 words
A method according to claim 15 wherein said hydrogel is formed by adding a solution of sodium silicate into acid containing a titanium compound and said chromium compound.
Claim 22
Dependent Claim 40 words
A method according to claim 19 wherein said aging is carried out at a temperature within the range of 65° F. (18° C.) to 200° F. (93° C.) for a time within the range of one hour to 20 hours.
Claim 23
Dependent Claim 9 words
A catalyst produced by the method of claim 15.
Claim 24
Dependent Claim 30 words
A method according to claim 1 wherein said chromium is present in an amount within the range of 0.1 to 5 weight percent based on the weight of said xerogel.
Claim 25
Dependent Claim 30 words
A method according to claim 15 wherein said chromium is present in an amount within the range of 0.001 to 10 weight percent based on the weight of said xerogel.
Claim 26
Dependent Claim 30 words
A method according to claim 15 wherein said chromium is present in an amount within the range of 0.1 to 5 weight percent based on the weight of said xerogel.
Claim 27
Dependent Claim 231 words
A method according to claim 15 wherein said chromium compound is selected from (a) compounds of the formula CrX 3 .yNH 3 where X is a halogen ion selected from Cl - , Br - , I 31 and y is an integer ranging from 1 to 6; (b) chromammines containing 6 neutral groups of the formula [CrA 6 ]Z 3 in which A is selected from NH 3 , ethylenediamine and unsymmetrical propylenediamine provided further that a portion of A can be H 2 O and Z is an acid radical selected from Cl - , Br - , I - , NO 3 - , SO 4 -2 and PO 4 -3; (c) chromammine compounds containing 5 neutral groups of the formula: [CrA 5 Y]Z 2 where A and Z are as before and Y is a radical from a monobasic acid selected from Cl - , Br - , I - , NO 2 - , NO 3 - , OH - and CNS - ; and (d) chromammine compounds containing 5 neutral groups of the formula [CrA 5 W]V where A is as before, V is Cl - , Br - , I - , (OH) - , and W is a radical from a dibasic acid selected from SO 3 -2 , SO 4 -2 , CO 3 -2 and C 2 O 4 -2 .

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1986-09-19 1987-03-21 1987-09-20 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1990-09-19 1991-03-21 1991-09-20 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1994-09-19 1995-03-21 1995-09-20 $7700.00 Window Closed / Lapsed

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