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US4659684A Expired / Lapsed US ⏱️ 0.0 years remaining

Removal of arsenic, vanadium and/or nickel compounds from spent catecholated polymer

Assignee: United States Department of Energy
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Filing: 1986-03-21
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Granted: 1987-04-21
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Expires: 2006-03-21
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Abstract

Abstract Described is a process for removing arsenic, vanadium, and/or nickel from petroliferous derived liquids by contacting said liquid at an elevated temperature with a divinylbenzene-crosslinked polystyrene having catechol ligands anchored thereon. For vanadium and nickel removal an amine, preferably a diamine is included. Also, described is a process for regenerating spent catecholated polystyrene by removal of the arsenic, vanadium, and/or nickel bound to it from contacting petroliferous liquid as described above and involves: treating the spent polymer containing any vanadium and/or nickel with an aqueous acid to achieve an acid pH; and, separating the solids from the liquid; and then treating said spent catecholated polystyrene, at a temperature in the range of about 20 DEG to 100 DEG C. with an aqueous solution of at least one carbonate and/or bicarbonate of ammonium, alkali and alkaline earth metals, said solution having a pH between about 8 and 10; and, separating the solids and liquids from each other. Preferably the regeneration treatment of arsenic containing catecholated polymer is in two steps wherein the first step is carried out with an aqueous alcoholic carbonate solution containing lower alkyl alcohol, and, the steps are repeated using a bicarbonate.

Inventors

  • 👤 Richard H. Fish

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 17:58
CPC Classifications
C; C10; C10G; C10G25/00; C10G25/003; Y; Y10; Y10S; Y10S502/00; Y10S502/515; Y10S502/516

Claims Analysis

Total Claims: 11
Claim 1
Independent Claim 109 words
Process of removal of compounds containing at least one of vanadium and nickel from spent catecholated polymer comprising: (a) acidifying a spent catecholated polystyrene-divinylbenzene polymer containing at least one of vanadium and nickel, which has been removed from a petroliferous liquid in the presence of an amine stabilizer by contact with said cathecholated polymer, with sufficient of an acidifying agent to hydrolyze the catechol moieties of the polymer and thereby to release the at least one of vanadium and nickel complexed therewith, the hydrolysis and release providing a regenerated catecholated polystyrene-divinylbenzene polymer; and, (b) separating said regenerated catecholated polystyrene-divinylbenzene polymer from said at least one of vanadium and nickel.
Claim 2
Dependent Claim 109 words
Process of removal of compounds containing at least one of vanadium and nickel from spent catecholated polymer comprising: (a) acidifying a spent catecholated polystyrene-divinylbenzene polymer containing at least one of vanadium and nickel, which has been removed from a petroliferous liquid in the presence of an amine stabilizer by contact with said cathecholated polymer, with sufficient of an acidifying agent to hydrolyze the catechol moieties of the polymer and thereby to release the at least one of vanadium and nickel complexed therewith, the hydrolysis and release providing a regenerated catecholated polystyrene-divinylbenzene polymer; and, (b) separating said regenerated catecholated polystyrene-divinylbenzene polymer from said at least one of vanadium and nickel.
Claim 3
Dependent Claim 24 words
Process according to claim 1 wherein said acidifying operation is carried out to obtain a pH in the range of about 1 to 5.
Claim 4
Dependent Claim 24 words
Process according to claim 1 wherein said acidifying operation is carried out to obtain a pH in the range of about 2 to 4.
Claim 5
Dependent Claim 34 words
Process according to claim 1 wherein said acidifying operation is carried out in the presence of an amine stabilizer and said separating operation includes separating said regenerated catecholated polystyrene-divinylbenzene polymer from said amine stabilizer.
Claim 6
Dependent Claim 15 words
Process according to claim 1 wherein said acidifying operation is carried out with hydrochloric acid.
Claim 7
Dependent Claim 15 words
Process according to claim 1 wherein said acidifying operation is carried out with acetic acid.
Claim 8
Dependent Claim 15 words
Process according to claim 1 wherein said acidifying operation is carried out with nitric acid.
Claim 9
Dependent Claim 181 words
Process of removal of compounds containing arsenic and at least one of vanadium and nickel from mixed spent catecholated polymer comprising: (a) acidifying a spent catecholated polymer having arsenic and at least one of vanadium and nickel complexed with catechol moieties of said polymer with sufficient of an acidifying acid to hydrolyze and release at least some of the at least one of vandium and nickel and to form a solid phase including catecholated polymer and a liquid phase including the released vanadium and/or nickel; (b) separating said solid phase from the liquid phase, (c) treating said catecholated polymer of the solid phase with an aqueous solution of at least one carbonate or bicarbonate selected from the group consisting of ammonium, alkali and alkaline earth metal carbonates and bicarbonates at a temperature in the range of about 20° to 100° C., at substantially atmospheric pressure and at a basic pH not greater than about 10, the treating being sufficient to release at least some of the arsenic from the catecholated polymer; and, (d) isolating the catecholated polymer from the released arsenic.
Claim 10
Dependent Claim 181 words
Process of removal of compounds containing arsenic and at least one of vanadium and nickel from mixed spent catecholated polymer comprising: (a) acidifying a spent catecholated polymer having arsenic and at least one of vanadium and nickel complexed with catechol moieties of said polymer with sufficient of an acidifying acid to hydrolyze and release at least some of the at least one of vandium and nickel and to form a solid phase including catecholated polymer and a liquid phase including the released vanadium and/or nickel; (b) separating said solid phase from the liquid phase, (c) treating said catecholated polymer of the solid phase with an aqueous solution of at least one carbonate or bicarbonate selected from the group consisting of ammonium, alkali and alkaline earth metal carbonates and bicarbonates at a temperature in the range of about 20° to 100° C., at substantially atmospheric pressure and at a basic pH not greater than about 10, the treating being sufficient to release at least some of the arsenic from the catecholated polymer; and, (d) isolating the catecholated polymer from the released arsenic.
Claim 11
Dependent Claim 44 words
Process according to claim 8 wherein said acidifying operation is carried out to obtain a pH in the range of about 2 to 4 and said arsenic treating operation is carried out at a pH in step (c) in the range of about 8-10.

References Cited (Backward Citations)

US4383104A Cited
US4532044A Cited
US4530963A Cited
US4552854A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1990-04-20 1990-10-20 1991-04-21 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1994-04-20 1994-10-20 1995-04-21 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1998-04-20 1998-10-20 1999-04-21 $7700.00 Window Closed / Lapsed

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