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US4181672A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for preparing metal chelates

Assignee: WR Grace and Co
•
Filing: 1977-09-27
•
Granted: 1980-01-01
•
Expires: 1997-09-27
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Abstract

Abstract An aqueous solution of a chelate of: (a) at least one metal selected from a first group consisting of: (i) magnesium; (ii) calcium; (iii) zinc; and (iv) manganese (II); and (b) at least one chelating agent selected from a second group consisting of moieties of: (i) ethylenediaminetetraacetic acid; (ii) nitrilotriacetic acid; (iii) diethylenetriaminepentaacetic acid; and (iv) hydroxyethylethylenediaminetriacetic acid is prepared by a process comprising forming a first admixture by admixing in an aqueous system an oxide or hydroxide of at least one member of the first group and at least one member selected from a third group consisting of a tetraalkali metal salt of ethylenediaminetetraacetic acid, a trialkali metal salt of nitrilotriacetic acid, a pentaalkali metal salt of diethylenetriaminepentaacetic acid, and a trialkali metal salt of hydroxyethylethylenediaminetriacetic acid; forming a second admixture by admixing the first admixture and a nitrile selected from a fourth group consisting of ethylenediaminetetraacetonitrile, nitrilotriacetonitrile, and diethylenetriaminepentaacetonitrile, and heating the second admixture to form the chelate and evaporate by-product ammonia therefrom, the pH of the resulting substantially ammonia-free product can then be adjusted to about 5-9.5 or preferably 6-9 if it is not already within this pH range.

Inventors

  • 👤 Felix B. Popper
  • 👤 Jeremiah B. McCarthy
  • 👤 James R. Hart

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-29 02:59
CPC Classifications
C; C07; C07F; C07F13/00; C07F13/005; C07F3/00; C07F3/003

Claims Analysis

Total Claims: 19
Claim 1
Independent Claim 235 words
A process for preparing an aqueous solution of a chelate of: (a) at least one metal selected from a first group consisting of: (i) magnesium; (ii) calcium; (iii) zinc; and (iv) manganese(II); and (b) at least one chelating agent selected from a second group consisting of moieties of: (i) ethylenediaminetetraacetic acid; (ii) nitrilotriacetic acid; (iii) diethylenetriaminepentaacetic acid; and (iv) hydroxyethylethylenediaminetriacetic acid; said process comprising: (A) forming a first admixture by admixing in an aqueous system an oxide or hydroxide of at least one member of the first group and at least one member selected from a third group consisting of: (I) a tetraalkali metal salt of ethylenediaminetetraacetic acid; (II) a trialkali metal salt of nitrilotriacetic acid; (III) a pentaalkali metal salt of diethylenetriaminepentaacetic acid; and (IV) a trialkali metal salt of hydroxyethylethylenediaminetriacetic acid; (B) admixing the first admixture and a member selected from a fourth group consisting of: (i) ethylenediaminetetraacetonitrile; (II) nitrilotriacetonitrile; and (III) diethylenetriaminepentacetonitrile to form a second admixture; (C) heating the second admixture to a temperature effective for hydrolyzing the nitrile and evaporating by-product ammonia from the second admixture, and maintaining the second admixture at this temperature for a time effective for hydrolyzing the nitrile and evaporating the by-product ammonia to form a substantially ammonia-free aqueous solution of the chelate; and (D) adjusting the pH of the resulting substantially ammonia-free aqueous solution of the chelate to about 5-9.5 and recovering the resulting product.
Claim 2
Dependent Claim 235 words
A process for preparing an aqueous solution of a chelate of: (a) at least one metal selected from a first group consisting of: (i) magnesium; (ii) calcium; (iii) zinc; and (iv) manganese(II); and (b) at least one chelating agent selected from a second group consisting of moieties of: (i) ethylenediaminetetraacetic acid; (ii) nitrilotriacetic acid; (iii) diethylenetriaminepentaacetic acid; and (iv) hydroxyethylethylenediaminetriacetic acid; said process comprising: (A) forming a first admixture by admixing in an aqueous system an oxide or hydroxide of at least one member of the first group and at least one member selected from a third group consisting of: (I) a tetraalkali metal salt of ethylenediaminetetraacetic acid; (II) a trialkali metal salt of nitrilotriacetic acid; (III) a pentaalkali metal salt of diethylenetriaminepentaacetic acid; and (IV) a trialkali metal salt of hydroxyethylethylenediaminetriacetic acid; (B) admixing the first admixture and a member selected from a fourth group consisting of: (i) ethylenediaminetetraacetonitrile; (II) nitrilotriacetonitrile; and (III) diethylenetriaminepentacetonitrile to form a second admixture; (C) heating the second admixture to a temperature effective for hydrolyzing the nitrile and evaporating by-product ammonia from the second admixture, and maintaining the second admixture at this temperature for a time effective for hydrolyzing the nitrile and evaporating the by-product ammonia to form a substantially ammonia-free aqueous solution of the chelate; and (D) adjusting the pH of the resulting substantially ammonia-free aqueous solution of the chelate to about 5-9.5 and recovering the resulting product.
Claim 3
Dependent Claim 14 words
The process of claim 1 in which the chelate is a chelate of zinc.
Claim 4
Dependent Claim 14 words
The process of claim 1 in which the chelate is a chelate of manganese(II).
Claim 5
Dependent Claim 14 words
The process of claim 1 in which the chelate is a chelate of magnesium.
Claim 6
Dependent Claim 14 words
The process of claim 1 in which the chelate is a chelate of calcium.
Claim 7
Dependent Claim 19 words
The process of claim 1 in which the third group member is a tetraalkali metal salt of ethylenediaminetetraacetic acid.
Claim 8
Dependent Claim 18 words
The process of claim 1 in which the third group member is pentaalkali metal salt of diethylenetriaminepentaacetic acid.
Claim 9
Dependent Claim 19 words
The process of claim 1 in which the third group member is a trialkali metal salt of nitrilotriacetic acid.
Claim 10
Dependent Claim 19 words
The process of claim 1 in which the third group member is a trialkali metal salt of hydroxyethylethylenediaminetriacetic acid.
Claim 11
Dependent Claim 23 words
The process of claim 1 in which the second admixture is maintained at 65°-110° C. for 1-4 hours to vaporize by-product ammonia therefrom.
Claim 12
Dependent Claim 11 words
The process of claim 1 in which the second admixture boiled.
Claim 13
Dependent Claim 20 words
The process of claim 11 in which the second admixture is boiled for about 1-2.5 hours to evaporate ammonia therefrom.
Claim 14
Dependent Claim 22 words
The process of claim 1 in which the pH of the substantially ammonia-free aqueous solution of the chelate is adjusted to 6-9.
Claim 15
Dependent Claim 13 words
The process of claim 1 in which the fourth group member is ethylenediaminetetraacetonitrile.
Claim 16
Dependent Claim 13 words
The process of claim 1 in which the fourth group member is nitrilotriacetonitrile.
Claim 17
Dependent Claim 13 words
The process of claim 1 in which the fourth group member is diethylenetriaminepentaacetonitrile.
Claim 18
Dependent Claim 271 words
A process for preparing an aqueous solution of a chelate of: (a) at least one metal selected from a first group consisting of: (i) magnesium; (ii) calcium; (iii) zinc; and (iv) manganese(II); and (b) at least one chelating agent selected from a second group consisting of moieties of: (i) ethylenediaminetetraacetic acid; (ii) nitrilotriacetic acid; (iii) diethylenetriaminepentaacetic acid; and (iv) hydroxyethylenediaminetriacetic acid; said process comprising: (A) forming a first admixture by admixing in an aqueous system an oxide or hydroxide of at least one member of the first group and at least one member selected from a third group consisting of: (I) a tetraalkali metal salt of ethylenediaminetetraacetic acid; (II) a trialkali metal salt of nitrilotriacetic acid; (III) a pentaalkali metal salt of diethylenetriaminepentaacetic acid; and (IV) a trialkali metal salt of hydroxyethylethylenediaminetriacetic acid; (B) heating the first admixture to a temperature effective for: (1) hydrolyzing, in a later recited step, a nitrile selected from a fourth group consisting of: (I) ethylenediaminetetraacetonitrile; (II) nitriolotriacetonitrile; and (III) diethylenetriaminepentaacetonitrile; and (2) evaporating by-product ammonia therefrom in the later recited step; (C) admixing the heated first admixture and the fourth group member while maintaining the first admixture and the resulting second admixture at the temperature effective for: (I) hydrolyzing the nitrile; and (II) evaporating by-product ammonia from the second admixture, and maintaining the second admixture at this temperature for a time effective for hydrolyzing the fourth group member and evaporating by-product ammonia therefrom to form a substantially ammonia-free solution of the chelate; and (D) adjusting the pH of the resulting substantially ammonia-free aqueous solution of the chelate to about 5-9.5 and recovering the resulting product.
Claim 19
Dependent Claim 271 words
A process for preparing an aqueous solution of a chelate of: (a) at least one metal selected from a first group consisting of: (i) magnesium; (ii) calcium; (iii) zinc; and (iv) manganese(II); and (b) at least one chelating agent selected from a second group consisting of moieties of: (i) ethylenediaminetetraacetic acid; (ii) nitrilotriacetic acid; (iii) diethylenetriaminepentaacetic acid; and (iv) hydroxyethylenediaminetriacetic acid; said process comprising: (A) forming a first admixture by admixing in an aqueous system an oxide or hydroxide of at least one member of the first group and at least one member selected from a third group consisting of: (I) a tetraalkali metal salt of ethylenediaminetetraacetic acid; (II) a trialkali metal salt of nitrilotriacetic acid; (III) a pentaalkali metal salt of diethylenetriaminepentaacetic acid; and (IV) a trialkali metal salt of hydroxyethylethylenediaminetriacetic acid; (B) heating the first admixture to a temperature effective for: (1) hydrolyzing, in a later recited step, a nitrile selected from a fourth group consisting of: (I) ethylenediaminetetraacetonitrile; (II) nitriolotriacetonitrile; and (III) diethylenetriaminepentaacetonitrile; and (2) evaporating by-product ammonia therefrom in the later recited step; (C) admixing the heated first admixture and the fourth group member while maintaining the first admixture and the resulting second admixture at the temperature effective for: (I) hydrolyzing the nitrile; and (II) evaporating by-product ammonia from the second admixture, and maintaining the second admixture at this temperature for a time effective for hydrolyzing the fourth group member and evaporating by-product ammonia therefrom to form a substantially ammonia-free solution of the chelate; and (D) adjusting the pH of the resulting substantially ammonia-free aqueous solution of the chelate to about 5-9.5 and recovering the resulting product.

References Cited (Backward Citations)

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US3966803A Cited
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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) 1982-12-31 1983-07-02 1984-01-01 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1986-12-31 1987-07-02 1988-01-01 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1990-12-31 1991-07-02 1992-01-01 $7700.00 Window Closed / Lapsed

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