US4051223A
Expired / Lapsed
US
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Process for the recovery of magnesium
Assignee: General Mills Chemicals Inc
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Filing: 1975-11-10
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Granted: 1977-09-27
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Expires: 1995-11-10
Abstract
Abstract Magnesium values are selectively extracted from aqueous solutions thereof also containing calcium using quaternary ammonium salts of selected hydrogen ion exchange reagents. Magnesium is stripped from the resulting organic phase with acids.
Inventors
- 👤 Kenneth D. MacKay
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 10:48
CPC Classifications
C; C22; C22B; C22B26/00; C22B26/20; C22B26/22; C22B3/00; C22B3/20; C22B3/26; C22B3/28; C22B3/288; C22B3/306; C22B3/36; C22B3/362; C22B3/364; Y; Y02; Y02P; Y02P10/00; Y02P10/20
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
333 words
The process of selectively recovering magnesium from an aqueous solution thereof which also contains calcium ions which comprises contacting said solution with a solution of a quaternary ammonium salt of a hydrogen ion exchange reagent in an essentially water-immiscible organic solvent to extract at least a portion of but less than 100% of the magnesium values into the organic phase, separating the magnesium loaded organic phase from the aqueous phase and stripping magnesium from the organic phase, said hydrogen ion exchange reagent being selected from the group consisting of: A. β-diketones having the formula ##STR26## where R is phenyl or alkyl substituted phenyl, R' is alkyl, alkyl substituted phenyl or chloro substituted phenyl and R" is H or --CN with the provisos that (1) when R is phenyl, R' is a branched chain alkyl group of at least seven carbon atoms and (2) when R is alkyl substituted phenyl, the number of carbon atoms in the alkyl substituent or substituents is at least 7 and at least one such alkyl substituent is branched chain; B. fluorinated β-diketones having the formula ##STR27## where n is a whole integer of 1 to 4, m is 0, 1 or 2 and R is an alkyl group of 1-25 carbon atoms; C. benzoxazoles having the formula ##STR28## where R is hydrogen or an alkyl group having from 1 to 20 carbon atoms, R' is hydrogen, chlorine or an alkyl group containing from 1 to 20 carbon atoms, X is H or chlorine and the total number of carbon atoms in R and R' is 6 to 40 with the proviso that one of R and R' must be an alkyl group of at least 6 carbon atoms; and D. 8-hydroxyquinolines of the formula ##STR29## where R is a branched chain alkyl or alkenyl radical containing about 8 to 20 carbon atoms, R 1 , R 2 and R 3 are hydrogen or alkyl groups of 1 to 4 carbon atoms and X is H, chlorine or bromine.
Claim 2
Dependent Claim
333 words
The process of selectively recovering magnesium from an aqueous solution thereof which also contains calcium ions which comprises contacting said solution with a solution of a quaternary ammonium salt of a hydrogen ion exchange reagent in an essentially water-immiscible organic solvent to extract at least a portion of but less than 100% of the magnesium values into the organic phase, separating the magnesium loaded organic phase from the aqueous phase and stripping magnesium from the organic phase, said hydrogen ion exchange reagent being selected from the group consisting of: A. β-diketones having the formula ##STR26## where R is phenyl or alkyl substituted phenyl, R' is alkyl, alkyl substituted phenyl or chloro substituted phenyl and R" is H or --CN with the provisos that (1) when R is phenyl, R' is a branched chain alkyl group of at least seven carbon atoms and (2) when R is alkyl substituted phenyl, the number of carbon atoms in the alkyl substituent or substituents is at least 7 and at least one such alkyl substituent is branched chain; B. fluorinated β-diketones having the formula ##STR27## where n is a whole integer of 1 to 4, m is 0, 1 or 2 and R is an alkyl group of 1-25 carbon atoms; C. benzoxazoles having the formula ##STR28## where R is hydrogen or an alkyl group having from 1 to 20 carbon atoms, R' is hydrogen, chlorine or an alkyl group containing from 1 to 20 carbon atoms, X is H or chlorine and the total number of carbon atoms in R and R' is 6 to 40 with the proviso that one of R and R' must be an alkyl group of at least 6 carbon atoms; and D. 8-hydroxyquinolines of the formula ##STR29## where R is a branched chain alkyl or alkenyl radical containing about 8 to 20 carbon atoms, R 1 , R 2 and R 3 are hydrogen or alkyl groups of 1 to 4 carbon atoms and X is H, chlorine or bromine.
Claim 3
Dependent Claim
16 words
The process of claim 1 wherein the hydrogen ion exchange reagent is a fluorinated β-diketone (B).
Claim 4
Dependent Claim
12 words
The process of claim 2 wherein the fluorinated β-diketone (B) is 1-dodecylphenyl-3-trifluoromethyl-1,3-propanedione.
Claim 5
Dependent Claim
15 words
The process of claim 1 wherein the magnesium is stripped using an acid stripping medium.
Claim 6
Dependent Claim
23 words
The process of claim 4 wherein the acid stripping medium is an aqueous solution of an acid selected from sulfuric and hydrochloric acid.
Claim 7
Dependent Claim
22 words
The process of claim 1 wherein the magnesium and calcium containing aqueous solution has a pH of from about 4 to 12.
Claim 8
Dependent Claim
17 words
The process of claim 6 wherein the solution has a pH of from about 6 to 9.
Claim 9
Dependent Claim
34 words
The proces of claim 1 wherein the quaternary ammonium salt of the hydrogen ion exchange reagent is present in the essentially water-immiscible organic solvent in an amount of about 2 to 15% by weight.
Claim 10
Dependent Claim
15 words
The process of claim 1 wherein the essentially water-immiscible organic solvent is a liquid hydrocarbon.
Claim 11
Dependent Claim
53 words
The process of claim 1 wherein quaternary ammonium cation of the salt of the hydrogen ion exchange reagent has the formula: ##STR30## where R 1 is a hydrocarbon radical of 6 to 24 carbon atoms and R 2 , R 3 and R 4 are hydrocarbon radicals of 1 to 24 carbon atoms.
Claim 12
Dependent Claim
40 words
The process of claim 1 wherein the salt is prepared by the neutralization of the hydrogen ion exchange reagent with the starting quaternary ammonium compound in a mole ratio of the latter to the former of about 3:5 to 7:5.
Claim 13
Dependent Claim
44 words
The process of claim 1 wherein the stripped organic phase is separated from the acid stripping medium, neutralized to reform the quaternary ammonium salt of the hydrogen ion exchange reagent and recycled for contacting further quantities of the magnesium and calcium containing aqueous solution.
Claim 14
Dependent Claim
49 words
The process of claim 1 wherein the hydrogen ion exchange reagent is a fluorinated β-diketone (B), the essentially water-immiscible organic solvent is a liquid hydrocarbon, the pH of the magnesium and calcium containing aqueous solution is from about 6 to 9 and the stripping medium is aqueous sulfuric acid.
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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) | 1980-09-26 | 1981-03-28 | 1981-09-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-09-26 | 1985-03-28 | 1985-09-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-09-26 | 1989-03-28 | 1989-09-27 | $7700.00 | Window Closed / Lapsed |