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US4169926A Expired / Lapsed US ⏱️ 0.0 years remaining

Inorganic hydrogels and uses thereof

Assignee: Phillips Petroleum Co
•
Filing: 1978-01-16
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Granted: 1979-10-02
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Expires: 1998-01-16
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Abstract

Abstract Inorganic hydrogels, e.g., silica-containing hydrogels, are contacted with contacting agents comprising oxygen-containing organic compounds and then dried to remove the liquid components therefrom. The contacting agent can also be an oxygen-containing organic compound in combination with a liquid hydrocarbon or an oxygen-containing compound in combination with a liquid hydrocarbon and a surfactant. The hydrogel can be treated with a catalytic metal compound prior to or during the contacting with the contacting agents in order to produce a composition after drying and calcining that is catalytically active for olefin polymerization. The treated hydrogel can also, after drying, be treated anhydrously with a catalytic metal compound to produce a composition that is active for 1-olefin polymerization upon calcination.

Inventors

  • 👤 Max P. McDaniel

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-04 21:21
CPC Classifications
C; C08; C08F; C08F10/00

Claims Analysis

Total Claims: 43
Claim 1
Independent Claim 80 words
A method for drying an inorganic hydrogel comprising contacting said hydrogel with a contacting agent which comprises a normally liquid, oxygen-containing, water-miscible organic compound selected from the group consisting of polyhydric alcohols, the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols and mixtures thereof, for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel and then applying sufficient heat to the treated hydrogel to remove the liquid components therefrom.
Claim 2
Independent Claim 80 words
A method for drying an inorganic hydrogel comprising contacting said hydrogel with a contacting agent which comprises a normally liquid, oxygen-containing, water-miscible organic compound selected from the group consisting of polyhydric alcohols, the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols and mixtures thereof, for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel and then applying sufficient heat to the treated hydrogel to remove the liquid components therefrom.
Claim 3
Dependent Claim 14 words
A method according to claim 1 wherein said inorganic hydrogel is a silica-containing hydrogel.
Claim 4
Dependent Claim 23 words
A method according to claim 1 wherein said contacting agent further comprises a normally liquid hydrocarbon in combination with said oxygen-containing organic compound.
Claim 5
Dependent Claim 33 words
A method according to claim 3 wherein said normally liquid hydrocarbon is selected from the group consisting of paraffins, cycloparaffins, aromatic hydrocarbons, and mixtures thereof having boiling points ranging from about 100°-260° C.
Claim 6
Dependent Claim 29 words
A method according to claim 4 wherein said liquid hydrocarbon is a paraffin or mixture thereof constituting a refinery stream having a boiling point range of about 175°-240° C.
Claim 7
Dependent Claim 14 words
A method according to claim 3 wherein said contacting agent further comprises a surfactant.
Claim 8
Independent Claim 85 words
A method for drying an inorganic hydrogel comprising contacting said hydrogel with a contacting agent which comprises a normally liquid, oxygen-containing, water-miscible organic compound selected from the group consisting of the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols in combination with a normally liquid hydrocarbon for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel and then drying said treated hydrogel by the application of sufficient heat to remove the liquid components therefrom.
Claim 9
Independent Claim 85 words
A method for drying an inorganic hydrogel comprising contacting said hydrogel with a contacting agent which comprises a normally liquid, oxygen-containing, water-miscible organic compound selected from the group consisting of the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols in combination with a normally liquid hydrocarbon for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel and then drying said treated hydrogel by the application of sufficient heat to remove the liquid components therefrom.
Claim 10
Dependent Claim 14 words
A method according to claim 7 wherein said contacting agent further comprises a surfactant.
Claim 11
Dependent Claim 26 words
A method according to claim 1 wherein the weight ratio of the contacting agent to hydrogel is in the range from about 100:1 to about 0.5:1.
Claim 12
Dependent Claim 28 words
A method according to claim 3 wherein the weight ratio of the hydrocarbon to the oxygen-containing organic compound is in the range from about 20:1 to about 0.5:1.
Claim 13
Dependent Claim 32 words
A method according to claim 6 wherein the weight percent of said surfactant, based on the weight of the contacting agent, is in the range of about 0.1 to 5 weight percent.
Claim 14
Dependent Claim 16 words
A method according to claim 1 wherein said treated hydrogel is dried in a vacuum oven.
Claim 15
Independent Claim 109 words
A method of preparing a silica-containing composition catalytically active for olefin polymerization comprising: (a) contacting a silica-containing hydrogel with a contacting agent comprising a normally liquid, water-miscible organic compound selected from the group consisting of polyhydric alcohols, the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols and mixtures thereof for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel; (b) drying the treated hydrogel sufficiently to remove the liquid components therefrom; (c) incorporating anhydrously a catalytic metal compound into the dried gel; and (d) calcining the gel in air to produce a composition catalytically active for olefin polymerization.
Claim 16
Independent Claim 109 words
A method of preparing a silica-containing composition catalytically active for olefin polymerization comprising: (a) contacting a silica-containing hydrogel with a contacting agent comprising a normally liquid, water-miscible organic compound selected from the group consisting of polyhydric alcohols, the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols and mixtures thereof for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel; (b) drying the treated hydrogel sufficiently to remove the liquid components therefrom; (c) incorporating anhydrously a catalytic metal compound into the dried gel; and (d) calcining the gel in air to produce a composition catalytically active for olefin polymerization.
Claim 17
Dependent Claim 23 words
A method according to claim 13 wherein said contacting agent further comprises a normally liquid hydrocarbon in combination with said oxygen-containing organic compound.
Claim 18
Dependent Claim 33 words
A method according to claim 14 wherein said normally liquid hydrocarbon is selected from the group consisting of paraffins, cycloparaffins, aromatic hydrocarbons, and mixtures thereof having boiling points ranging from about 100°-260° C.
Claim 19
Dependent Claim 29 words
A method according to claim 15 wherein said liquid hydrocarbon is a paraffin or mixture thereof constituting a refinery stream having a boiling point range of about 175°-240° C.
Claim 20
Dependent Claim 14 words
A method according to claim 14 wherein said contacting agent further comprises a surfactant.
Claim 21
Dependent Claim 26 words
A method according to claim 13 wherein the weight ratio of the contacting agent to hydrogel is in the range from about 100:1 to about 0.5:1.
Claim 22
Dependent Claim 28 words
A method according to claim 14 wherein the weight ratio of the hydrocarbon to the oxygen-containing organic compound is in the range from about 20:1 to about 0.5:1.
Claim 23
Dependent Claim 32 words
A method according to claim 17 wherein the weight percent of said surfactant, based on the weight of the contacting agent, is in the range of about 0.1 to 5 weight percent.
Claim 24
Dependent Claim 16 words
A method according to claim 13 wherein said treated hydrogel is dried in a vacuum oven.
Claim 25
Independent Claim 116 words
A method of preparing a silica-containing composition catalytically active for olefin polymerization comprising: (a) contacting a silica-containing hydrogel with a contacting agent comprising a normally liquid, water-miscible organic compound selected from the group consisting of the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols in combination with a normally liquid hydrocarbon for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel; (b) drying the treated hydrogel by the application of sufficient heat to remove the liquid components therefrom; (c) incorporating anhydrously a catalytic metal compound into the dried gel; and (d) calcining the gel in air to produce a composition catalytically active for olefin polymerization.
Claim 26
Independent Claim 116 words
A method of preparing a silica-containing composition catalytically active for olefin polymerization comprising: (a) contacting a silica-containing hydrogel with a contacting agent comprising a normally liquid, water-miscible organic compound selected from the group consisting of the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols in combination with a normally liquid hydrocarbon for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel; (b) drying the treated hydrogel by the application of sufficient heat to remove the liquid components therefrom; (c) incorporating anhydrously a catalytic metal compound into the dried gel; and (d) calcining the gel in air to produce a composition catalytically active for olefin polymerization.
Claim 27
Dependent Claim 17 words
A method according to claim 22 wherein said contacting agent of step (a) further comprises a surfactant.
Claim 28
Dependent Claim 18 words
A method according to claim 13 wherein said catalytic metal compound of step (c) is a chromium compound.
Claim 29
Independent Claim 113 words
A method of preparing a silica-containing composition catalytically active for olefin polymerization comprising: (a) contacting a silica-containing hydrogel, in which a catalytic metal compound has been incorporated, with a contacting agent comprising a normally liquid, water-miscible organic compound selected from the group consisting of polyhydric alcohols, the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols and mixtures thereof for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel; (b) drying the treated hydrogel by the application of sufficient heat to remove the liquid components therefrom; and (c) calcining the impregnated gel in air to produce a composition catalytically active for olefin polymerization.
Claim 30
Independent Claim 113 words
A method of preparing a silica-containing composition catalytically active for olefin polymerization comprising: (a) contacting a silica-containing hydrogel, in which a catalytic metal compound has been incorporated, with a contacting agent comprising a normally liquid, water-miscible organic compound selected from the group consisting of polyhydric alcohols, the mono- and dialkyl ethers of alkylene glycols and poly(alkylene) glycols and mixtures thereof for a length of time sufficient to obtain penetration of the contacting agent into the pores of the hydrogel; (b) drying the treated hydrogel by the application of sufficient heat to remove the liquid components therefrom; and (c) calcining the impregnated gel in air to produce a composition catalytically active for olefin polymerization.
Claim 31
Dependent Claim 23 words
A method according to claim 25 wherein said contacting agent further comprises a normally liquid hydrocarbon in combination with said oxygen-containing organic compound.
Claim 32
Dependent Claim 33 words
A method according to claim 26 wherein said normally liquid hydrocarbon is selected from the group consisting of paraffins, cycloparaffins, aromatic hydrocarbons, and mixtures thereof having boiling points ranging from about 100°-260° C.
Claim 33
Dependent Claim 29 words
A method according to claim 27 wherein said liquid hydrocarbon is a paraffin or mixture thereof constituting a refinery stream having a boiling point range of about 175°-240° C.
Claim 34
Dependent Claim 14 words
A method according to claim 26 wherein said contacting agent further comprises a surfactant.
Claim 35
Dependent Claim 66 words
A method according to claim 25 wherein: said silica-containing hydrogel is a silica-titania cogel hydrogel; said catalytic metal compound is chromium acetate; and said contacting agent is selected from the group consisting of monoethyl ether of ethylene glycol, mono-n-butyl ether of ethylene glycol, mono-n-butyl ether of diethylene glycol, diethyl ether of diethylene glycol, dimethyl ether of diethylene glycol, dimethyl ether of triethylene glycol, 1,2-propanediol, and 1,3-butanediol.
Claim 36
Dependent Claim 76 words
A method according to claim 26 wherein: said silica-containing hydrogel is a silica-titania cogel hydrogel; said catalytic metal compound is chromium acetate; and said contacting agent is selected from the group consisting of a refinery product hydrocarbon mixture having a boiling range of about 218°-238° C. in combination with mono-n-butyl ether of diethylene glycol and a refinery product hydrocarbon mixture having a boiling range of about 176°-207° C. in combination with mono-n-butyl ether of diethylene glycol.
Claim 37
Dependent Claim 51 words
A method according to claim 29 wherein: said silica-containing hydrogel is a silica-titania cogel hydrogel, said catalytic metal compound is chromium acetate, and said contacting agent is a refinery product hydrocarbon mixture having a boiling range of about 218°-238° C. in combination with mono-n-butyl ether of diethylene glycol and sorbitan monolaurate.
Claim 38
Dependent Claim 23 words
A method of polymerizing olefins in the presence of a catalyst wherein said catalyst is the product of the method in claim 25.
Claim 39
Dependent Claim 23 words
A method of polymerizing olefins in the presence of a catalyst wherein said catalyst is the product of the method in claim 13.
Claim 40
Dependent Claim 12 words
A method according to claim 33 in which said olefin is ethylene.
Claim 41
Dependent Claim 12 words
A method according to claim 34 in which said olefin is ethylene.
Claim 42
Dependent Claim 11 words
An olefin polymerization catalyst produced by the method of claim 13.
Claim 43
Dependent Claim 11 words
An olefin polymerization catalyst produced by the method of claim 25.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1982-10-01 1983-04-02 1983-10-02 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1986-10-01 1987-04-02 1987-10-02 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1990-10-01 1991-04-02 1991-10-02 $7700.00 Window Closed / Lapsed

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