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US4224142A Expired / Lapsed US ⏱️ 0.0 years remaining

Treatment of recycled ammonium sulfate-bisulfate solution

Assignee: Phillips Petroleum Co
•
Filing: 1979-06-29
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Granted: 1980-09-23
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Expires: 1999-06-29
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Abstract

Abstract Ammonium sulfate-bisulfate solution contaminated with metal and other ash producing contaminants is treated by adjusting the pH of the solution to the range that produces a precipitate of the contaminant by the addition of ammonia or ammonium hydroxide; cooled to at least the temperature at which a precipitate is produced; removing the precipitate from the solution; the pH of the solution from which the precipitate has been removed is adjusted to the range at which precipitation is substantially completed by the addition of sulfuric acid; and the SO 4 = ion concentration and the NH 4 + ion concentration of the solution are adjusted to the range of the solution before initial circulation to produce a solution in which the metal concentration has been sufficiently reduced to permit recycle for use in reclaiming used motor oils.

Inventors

  • 👤 Bruce C. Benedict

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-01 21:18
CPC Classifications
C; C01; C01C; C01C1/00; C01C1/24; C01C1/242; C10; C10M; C10M175/00; C10M175/0016

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 125 words
A method for regenerating an aqueous ammonium sulfate-bisulfate treating solution containing metal and other contaminants which form ash, said method comprising: (a) adjusting the pH of said solution to the range that produces a precipitate of said contaminant by addition of NH 3 or NH 4 OH; (b) cooling the pH adjusted solution to a temperature that substantially completes the precipitation; (c) removing the precipitate from the solution; (d) adjusting the pH of the solution after precipitate removal to the range of the treating solution before initial circulation by addition of H 2 SO 4 ; and (e) adjusting the SO 4 = ion concentration of the solution and the NH 4 + ion concentration to the range of the treating solution before initial circulation.
Claim 2
Independent Claim 125 words
A method for regenerating an aqueous ammonium sulfate-bisulfate treating solution containing metal and other contaminants which form ash, said method comprising: (a) adjusting the pH of said solution to the range that produces a precipitate of said contaminant by addition of NH 3 or NH 4 OH; (b) cooling the pH adjusted solution to a temperature that substantially completes the precipitation; (c) removing the precipitate from the solution; (d) adjusting the pH of the solution after precipitate removal to the range of the treating solution before initial circulation by addition of H 2 SO 4 ; and (e) adjusting the SO 4 = ion concentration of the solution and the NH 4 + ion concentration to the range of the treating solution before initial circulation.
Claim 3
Dependent Claim 19 words
A method of claim 1 wherein precipitate in said solution to be treated is removed prior to step (a).
Claim 4
Dependent Claim 14 words
A method of claim 1 wherein precipitate is removed by settling, filtration, or centrifugation.
Claim 5
Dependent Claim 14 words
A method of claim 2 wherein precipitate is removed by settling, filtration, or centrifugation.
Claim 6
Dependent Claim 20 words
A method of claim 1 wherein the temperature in step )b) is reduced to at least 100° F. (38° C.).
Claim 7
Dependent Claim 22 words
A method of claim 1 wherein the pH in step (d) is adjusted to the range of about 0.4 to about 1.3.
Claim 8
Dependent Claim 32 words
A method of claim 1 wherein the solution of step (e) is (f) heated to a temperature sufficient for reaction with used oil, and (g) contacted with used oil in a reactor.
Claim 9
Independent Claim 127 words
A method for regenerating an aqueous ammonium sulfate-bisulfate treating solution containing metal and other contaminants which form ash, said method comprising: (a) removing contained precipitate from said solution; (b) adjusting the pH of said solution to the range that produces a precipitate by addition of NH 3 or NH 4 OH; (c) cooling the pH adjusted solution to a temperature that substantially completes precipitation; (d) removing the precipitate from the solution; (e) adjusting the pH of the solution after precipitate removal to the range of the treating solution before initial circulation by addition of H 2 SO 4 ; (f) adjusting the SO 4 = ion concentration of the solution and the NH 4 + ion concentration to the range of the treating solution before initial circulation.
Claim 10
Independent Claim 127 words
A method for regenerating an aqueous ammonium sulfate-bisulfate treating solution containing metal and other contaminants which form ash, said method comprising: (a) removing contained precipitate from said solution; (b) adjusting the pH of said solution to the range that produces a precipitate by addition of NH 3 or NH 4 OH; (c) cooling the pH adjusted solution to a temperature that substantially completes precipitation; (d) removing the precipitate from the solution; (e) adjusting the pH of the solution after precipitate removal to the range of the treating solution before initial circulation by addition of H 2 SO 4 ; (f) adjusting the SO 4 = ion concentration of the solution and the NH 4 + ion concentration to the range of the treating solution before initial circulation.
Claim 11
Dependent Claim 102 words
A method for reducing ash content of used lubricating oil comprising: (a) contacting used lubricating oil with an aqueous solution of ammonium sulfate and/or ammonium bisulfate under conditions of temperature and pressure sufficient to react said ammonium sulfate and/or ammonium bisulfate with metal-containing components present in the used lubricating oil and form metal-containing solids; (b) allowing the reaction mass of (a) to separate into an oil phase and an aqueous phase containing said solids; (c) removing said oil phase; (d) recovering said aqueous phase; (e) treating said aqueous phase according to claim 1; and (f) recycling treated aqueous phase to step (a).
Claim 12
Dependent Claim 102 words
A method for reducing ash content of used lubricating oil comprising: (a) contacting used lubricating oil with an aqueous solution of ammonium sulfate and/or ammonium bisulfate under conditions of temperature and pressure sufficient to react said ammonium sulfate and/or ammonium bisulfate with metal-containing components present in the used lubricating oil and form metal-containing solids; (b) allowing the reaction mass of (a) to separate into an oil phase and an aqueous phase containing said solids; (c) removing said oil phase; (d) recovering said aqueous phase; (e) treating said aqueous phase according to claim 8; and (f) recycling treated aqueous phase to step (a).

References Cited (Backward Citations)

US3169917A Cited
US3294678A Cited
US3791965A Cited
US3879282A Cited
US3930988A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1983-09-23 1984-03-24 1984-09-23 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1987-09-23 1988-03-24 1988-09-23 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1991-09-23 1992-03-24 1992-09-23 $7700.00 Window Closed / Lapsed

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