US4457812A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Critical solvent separations in inorganic systems
Assignee: Kerr McGee Corp
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Filing: 1983-07-18
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Granted: 1984-07-03
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Expires: 2003-07-18
Abstract
Abstract A process for separating inorganic substances involving their abstraction from a mixture with near-supercritical inorganic fluids. One or more inorganic substances are abstracted and then separatively recovered by retrograde condensations. The process particularly is applicable with mixtures obtained from the chlorination of metalliferous ores and may be conjoined to many ancillary metal abstraction processes such as volatilizations, distillations or electrolyses.
Inventors
- 👤 Theodore A. Rado
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 20:12
CPC Classifications
C; C01; C01G; C01G49/00; C01G49/10; B; B01; B01D; B01D11/00; B01D11/04; B01D11/0403; B01D11/0407; C01B; C01B9/00; C01F; C01F7/00; C01F7/48; C01F7/56; C01G1/00; C01G1/06; C01G21/00; C01G21/16; C01G9/00; C01G9/04; C22; C22B; C22B9/00; C22B9/02; C25; C25C; C25C1/00; C25C1/16; C25C1/18; Y; Y02; Y02P; Y02P10/00; Y02P10/20; Y02P20/00; Y02P20/50; Y02P20/54; Y10; Y10S; Y10S210/00; Y10S210/902; Y10S210/911; Y10S210/912
Claims Analysis
Total Claims: 36
Claim 1
Independent Claim
136 words
A process for separating metallic halides from a mixture comprising metallic halides, the process comprising: contacting said mixture with a near-supercritical inorganic fluid having a critical temperature between about 100 degrees centigrade and about 500 degrees centigrade and comprising the same halide as the metallic halides to be separated from the mixture and preferentially taking up at least one metallic halide at the contacting conditions of near-supercritical temperature and pressure such that the near-supercritical inorganic fluid takes up at least a portion of at least one metallic halide forming a near-supercritical fluid phase; segregating the near-supercritical fluid phase from any of the mixture not taken up by the near-supercritical fluid while still maintaining aforesaid near-supercritical conditions; and separating at least a portion of at least one of said taken-up metallic halides from the near-supercritical fluid phase.
Claim 2
Dependent Claim
136 words
A process for separating metallic halides from a mixture comprising metallic halides, the process comprising: contacting said mixture with a near-supercritical inorganic fluid having a critical temperature between about 100 degrees centigrade and about 500 degrees centigrade and comprising the same halide as the metallic halides to be separated from the mixture and preferentially taking up at least one metallic halide at the contacting conditions of near-supercritical temperature and pressure such that the near-supercritical inorganic fluid takes up at least a portion of at least one metallic halide forming a near-supercritical fluid phase; segregating the near-supercritical fluid phase from any of the mixture not taken up by the near-supercritical fluid while still maintaining aforesaid near-supercritical conditions; and separating at least a portion of at least one of said taken-up metallic halides from the near-supercritical fluid phase.
Claim 3
Dependent Claim
17 words
The process of claim 1 wherein the inorganic near-supercritical fluid is defined further as being titanium tetrachloride.
Claim 4
Dependent Claim
17 words
The process of claim 1 wherein the inorganic near-supercritical fluid is defined further as being silicon tetrachloride.
Claim 5
Dependent Claim
24 words
The process of claim 1 wherein the inorganic near-supercritical fluid is defined further as being boron trichloride, tin tetrachloride, phosphorous trichloride or sulfur monochloride.
Claim 6
Dependent Claim
17 words
The process of claim 1 wherein the inorganic near-supercritical fluid is defined further as being carbon tetrachloride.
Claim 7
Dependent Claim
32 words
The process of claim 1 wherein the mixture is defined further as containing a plurality of metallic halides and a plurality of said metallic halides are taken up by the near-supercritical fluid.
Claim 8
Dependent Claim
36 words
The process of claim 6 wherein the separating step is defined further as subjecting the near-supercritical fluid phase containing a plurality of metallic halides to stepwise recovery and the products of these steps are recovered separately.
Claim 9
Dependent Claim
40 words
The process of claim 1 wherein said separating is caused by raising the temperature, reducing the pressure or raising the temperature and reducing the pressure of the near-supercritical fluid phase, to thereby induce the retrograde condensation of taken-up metallic halides.
Claim 10
Dependent Claim
32 words
The process of claim 1 wherein the temperature of the near-supercritical fluid during said contacting is defined further as being within a reduced temperature (T R ) range of 0.8 to 1.5.
Claim 11
Dependent Claim
20 words
The process of claim 1 wherein the metallic halides are defined further as being metallic fluorides, bromides, chlorides or iodides.
Claim 12
Dependent Claim
16 words
The process of claim 10 wherein the metallic halides are defined further as comprising aluminum trichloride.
Claim 13
Dependent Claim
19 words
The process of claim 10 wherein the metallic halides are defined further as comprising aluminum trichloride and iron chlorides.
Claim 14
Dependent Claim
19 words
The process of claim 10 wherein the metallic halides are defined further as comprising zinc chloride and lead chloride.
Claim 15
Dependent Claim
21 words
The process of claim 10 wherein the metallic halides are defined further as being produced by halogenation of a metalliferous ore.
Claim 16
Dependent Claim
26 words
The process of claim 14 wherein the metallic halides are defined further as comprising aluminum trichloride and iron chlorides produced by the chlorination of aluminiferous ore.
Claim 17
Dependent Claim
30 words
The process of claim 14 wherein the metallic halides are defined further as comprising zinc chloride and lead chloride produced by the chlorination of an ore comprising zinc and lead.
Claim 18
Dependent Claim
22 words
The process of claim 1 wherein the inorganic near-supercritical fluid is chemically inert with respect to the mixture under the process conditions.
Claim 19
Dependent Claim
107 words
The process of claim 15 wherein the aluminiferous ore is defined further as being bauxite and the chlorination is defined further as comprising: providing a source of bauxite; introducing the bauxite into a first chlorination zone; providing a source of carbonaceous reductant; introducing the carbonaceous reductant into the first chlorination zone to form a first loaded chlorination zone; maintaining the first loaded chlorination zone at a temperature ranging from about 900 degrees centigrade and about 1000 degrees centigrade; providing a source of chlorine gas; and passing the chlorine gas into the first loaded chlorination zone to produce a first product stream comprising aluminum trichloride and iron chlorides.
Claim 20
Dependent Claim
49 words
The process of claim 18 wherein the mixture is defined further as being produced by passing the first product stream into a first condensation zone having a temperature between about 20 degrees centigrade and about 70 degrees centigrade to produce a condensate comprising solid chlorides of aluminum and iron.
Claim 21
Dependent Claim
36 words
The process of claim 19 wherein the first condensation zone is defined further as comprising a recycle solvent of titanium tetrachloride or silicon tetrachloride to produce a first slurry comprising about 66 weight percent recycle solvent.
Claim 22
Dependent Claim
90 words
The process of claim 20 wherein the contacting step is defined further as comprising: passing at least a portion of the first slurry to a first settling zone; maintaining the first slurry in the first settling zone within a reduced temperature (T R ) range of 0.8 to 1.5 of the recycle solvent and at about the supercritical pressure of this recycle solvent to produce a near-supercritical phase characterized as a first near-supercritical fluid phase comprising recycle solvent and taken-up aluminum trichloride and a first solid phase comprising iron chlorides.
Claim 23
Dependent Claim
66 words
The process of claim 21 wherein the segregating step is defined further as permitting the first solid phase to settle in the first settling zone to produce a settled first solid phase and a clarified first near-supercritical fluid phase and steps are added comprising: withdrawing the settled first solid phase from the first settling zone; and recovering at least a portion of the first solid phase.
Claim 24
Dependent Claim
128 words
The process of claim 22 wherein the separating step is defined further as including the steps of: passing the clarified first near-supercritical fluid phase from the first settling zone to a second settling zone; maintaining the clarified first near-supercritical fluid phase in the second settling zone at an increased temperature to produce a second near-supercritical fluid phase and a second solid phase comprising aluminum trichloride; permitting the second solid phase to settle in the second settling zone to produce a settled second solid phase and a clarified second near-supercritical fluid phase; withdrawing the settled second solid phase from the second settling zone; recycling the clarified second near-supercritical fluid phase as recycle solvent to the first condensation zone; and recovering the aluminum trichloride from the settled second solid phase.
Claim 25
Dependent Claim
113 words
The process of claim 16 wherein the ore comprising zinc and lead is defined further as being oxidized ore and the chlorination is defined further as comprising: providing a source of oxidized ore; introducing the oxidized ore into a second chlorination zone; providing a source of carbonaceous reductant; introducing the carbonaceous reductant into the second chlorination zone to produce a second loaded chlorination zone; maintaining the second loaded chlorination zone at a temperature ranging from about 600 degrees centigrade to about 1000 degrees centigrade; providing a source of chlorine gas; and passing the chlorine gas into the second loaded chlorination zone to produce a second product stream comprising lead chloride and zinc chloride.
Claim 26
Dependent Claim
48 words
The process of claim 24 wherein the mixture is defined further as being produced by passing the second product stream into a second condensation zone having a temperature between about 20 degrees centigrade and about 70 degrees centigrade to produce a condensate comprising lead chloride and zinc chloride.
Claim 27
Dependent Claim
36 words
The process of claim 25 wherein the second condensation zone is defined further as comprising a recycle solvent of titanium tetrachloride or silicon tetrachloride to produce a second slurry comprising about 66 weight percent recycle solvent.
Claim 28
Dependent Claim
105 words
The process of claim 26 wherein the contacting step is defined further as comprising: passing at least a portion of the second slurry to a third settling zone; maintaining the second slurry in the third settling zone at a temperature within a reduced temperature (T R ) range of 0.8 to 1.5 of the recycle solvent and at about the supercritical pressure of this recycle solvent to produce a third near-supercritical fluid phase comprising recycle solvent, taken-up lead chloride and taken-up zinc chloride and a third solid phase comprising copper chlorides and gangue; and segregating the third solid phase from the third near-supercritical fluid phase.
Claim 29
Dependent Claim
56 words
The process of claim 27 wherein the segregating step is defined further as permitting the third solid phase to settle in the third settling zone to produce a settled third solid phase and a clarified third near-supercritical fluid phase and a step is added comprising: withdrawing the settled third solid phase from the third settling zone.
Claim 30
Dependent Claim
77 words
The process of claim 28 wherein the segregating step is defined further as including the steps of: passing the clarified third near-supercritical fluid phase into a fourth settling zone; and maintaining the clarified third near-supercritical fluid phase in the fourth settling zone at a temperature increased above that of the third settling zone to produce a fourth near-supercritical fluid phase comprising taken-up zinc chloride and recycle solvent and a fourth solid phase comprising particles of lead chloride.
Claim 31
Dependent Claim
52 words
The process of claim 29 wherein the separating step is defined further as including the steps of: permitting the fourth solid phase to settle in the fourth settling zone to produce a settled fourth solid phase and a clarified fourth near-supercritical fluid phase; and recovering lead from the settled fourth solid phase.
Claim 32
Dependent Claim
43 words
The process of claim 30 wherein the recovery of lead is defined further as including the steps of: separating the fourth solid phase from the clarified fourth near-supercritical phase; and subjecting the settled fourth solid phase to electrolysis in a first electrolytic zone.
Claim 33
Dependent Claim
83 words
The process of claim 30 wherein the segregating step is defined further as being stepwise and as including the steps of: separating the clarified fourth near-supercritical fluid phase; passing the clarified fourth near-supercritical fluid phase into a fifth settling zone; maintaining the clarified fourth near-supercritical fluid phase in the fifth settling zone at a temperature increased above that of the fourth settling zone to produce a fifth near-supercritical fluid phase comprising recycle solvent and a fifth solid phase comprising particles of zinc chloride.
Claim 34
Dependent Claim
54 words
The process of claim 32 wherein the separating step is defined further as being stepwise and including the steps of: permitting the fifth solid phase to settle in the fifth settling zone to produce a clarified fifth near-supercritical phase and a settled fifth solid phase; and recovering zinc from the settled fifth solid phase.
Claim 35
Dependent Claim
45 words
The process of claim 33 wherein the recovery of zinc is defined further as including the steps of: separating the settled fifth solid phase from the clarified fifth near-supercritical fluid phase; and subjecting the settled fifth solid phase to electrolysis in a second electrolytic zone.
Claim 36
Dependent Claim
40 words
The process of claim 33 wherein the segregating step is defined further as including the steps of: separating the clarified fifth near-supercritical fluid phase; and recycling the clarified fifth near-supercritical fluid phase as recycle solvent to the second condensation zone.
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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) | 1987-07-03 | 1988-01-02 | 1988-07-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-07-03 | 1992-01-02 | 1992-07-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-07-03 | 1996-01-02 | 1996-07-03 | $7700.00 | Window Closed / Lapsed |