US3715393A
Expired / Lapsed
US
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Method of preparing sodium nitrilotriacetate
Assignee: Montedison SpA
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Filing: 1970-05-15
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Granted: 1973-02-06
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Expires: 1990-05-15
Abstract
Abstract Preparation of N(CH2COONa)3 in crystalline form by hydrolyzing N(CH2CN)3 in the presence of NaOH. Involves suspending N(CH2CN)3 in recycled mother liquor, adding aqueous NaOH to the suspension, partially hydrolyzing at about 65* to 75*C., further hydrolyzing at about 70* to 90*C. to form N(CH2COONa)3, separating N(CH2COONa)3 from the mother liquor, and recycling the mother liquor.
Inventors
- 👤 G Ribaldone
- 👤 S Gafa
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 18:09
CPC Classifications
C; C11; C11D; C11D3/00; C11D3/16; C11D3/26; C11D3/33
Claims Analysis
Total Claims: 3
Claim 1
Independent Claim
192 words
In a continuous method of making sodium nitrilotriacetate in crystalline form by hydrolyzing nitrilotriacetonitrile in the presence of sodium hydroxide, the improvement comprising a. suspending nitrilotriacetonitrile in recycled mother liquor, said mother liquor containing sodium nitrilotriacetate and sodium hydroxide, the amount of sodium hydroxide contained in said mother liquor being from about 20 to 30 percent of the stoichiometric amount required to effect hydrolysis of said nitrilotriacetonitrile, the temperature of said suspension being maintained at from about 20* to 60*C, b. adding to said suspension an aqueous solution of sodium hydroxide in an amount of 3 moles of NaOH per mole of nitrilotriacetonitrile whereby the total amount of NaOH in the reaction mixture is about 3.6 to 3.9 moles per mole of nitrilotriacetonitrile, c. partially hydrolyzing said nitrilotriacetonitrile at a temperature of from about 65* to 75*C to form a mixture comprising sodium nitrilotriacetate and sodium-N-(2-acetamido)-iminodiacetate, d. completing the hydrolysis at a temperature which is higher than the temperature in step (c) and which is from about 70* to 90*C to form sodium nitrilotriacetate, e. separating and recovering sodium nitrilotriacetate crystals from said mother liquor, and f. thereafter recycling said mother liquor.
Claim 2
Dependent Claim
192 words
In a continuous method of making sodium nitrilotriacetate in crystalline form by hydrolyzing nitrilotriacetonitrile in the presence of sodium hydroxide, the improvement comprising a. suspending nitrilotriacetonitrile in recycled mother liquor, said mother liquor containing sodium nitrilotriacetate and sodium hydroxide, the amount of sodium hydroxide contained in said mother liquor being from about 20 to 30 percent of the stoichiometric amount required to effect hydrolysis of said nitrilotriacetonitrile, the temperature of said suspension being maintained at from about 20* to 60*C, b. adding to said suspension an aqueous solution of sodium hydroxide in an amount of 3 moles of NaOH per mole of nitrilotriacetonitrile whereby the total amount of NaOH in the reaction mixture is about 3.6 to 3.9 moles per mole of nitrilotriacetonitrile, c. partially hydrolyzing said nitrilotriacetonitrile at a temperature of from about 65* to 75*C to form a mixture comprising sodium nitrilotriacetate and sodium-N-(2-acetamido)-iminodiacetate, d. completing the hydrolysis at a temperature which is higher than the temperature in step (c) and which is from about 70* to 90*C to form sodium nitrilotriacetate, e. separating and recovering sodium nitrilotriacetate crystals from said mother liquor, and f. thereafter recycling said mother liquor.
Claim 3
Dependent Claim
37 words
The method of claim 1, wherein said crystals of sodium nitrilotriacetate separated from the mother liquor are washed with water, the wash water is then added to the mother liquor, and the mother liquor-water is then recycled.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1976-02-06 | 1976-08-07 | 1977-02-06 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1980-02-06 | 1980-08-07 | 1981-02-06 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1984-02-06 | 1984-08-07 | 1985-02-06 | $7700.00 | Window Closed / Lapsed |