Patent US4146575A successfully refreshed from Google Patents.
US4146575A
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Preparation of sodium tripolyphosphate
Assignee: Euteco SpA
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Filing: 1977-11-03
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Granted: 1979-03-27
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Expires: 1997-11-03
Abstract
Abstract The purity grade of sodium tripolyphosphate obtained by neutralization with sodium hydroxide of aqueous phosphoric acid obtained by the wet method, removal of the precipitate formed, evaporation to dryness of the resulting solution and calcination of the evaporation residue, is improved by carrying out the neutralization at a temperature not exceeding 85° C., maturing the neutralization product at 70°-85° C. for at least one hour before separating the precipitate, concentrating the sodium phosphate solution, if necessary, to a sodium phosphate content of at least 40 wt.%, and heat treating the solution at 100°-200° C. and at boiling point or under to precipitate the magnesium compounds, prior to the evaporation step.
Inventors
- 👤 Onorio Gallistru
- 👤 Artemio Gellera
- 👤 Luciano Cavalli
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 16:19
CPC Classifications
C; C01; C01B; C01B25/00; C01B25/16; C01B25/26; C01B25/30; C01B25/301; C01B25/303; C01B25/38; C01B25/40; C01B25/41; C01B25/412; C01B25/416
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
188 words
In a process for the preparation of sodium tripolyphosphate wherein an aqueous solution of phosphoric acid obtained by the wet method which contains magnesium compounds dissolved therein is neutralized by addition of an aqueous solution of sodium hydroxide, the precipitated impurities are separated from the sodium phosphate solution thus obtained, the sodium phosphate solution is evaporated to dryness and the evaporation residue is calcined, the improvement which comprises neutralizing said aqueous solution of phosphoric acid at a temperature not exceeding 85° C., maturing the neutralization product at a temperature of from 70° to 85° C. for a period of at least one hour before separating said precipitated impurities, submitting the sodium phosphate solution, having a sodium phosphate content of at least 40% by weight, prior to the evaporation to dryness, to a heat treatment at a temperature of from 100° to 200° C., at boiling point or under, and at atmospheric or superatmospheric pressure, for a period such as to induce substantially complete precipitation of the magnesium compounds dissolved in said sodium phosphate solution, the precipitate resulting from this heat treatment being separated from the heat treated solution.
Claim 2
Dependent Claim
188 words
In a process for the preparation of sodium tripolyphosphate wherein an aqueous solution of phosphoric acid obtained by the wet method which contains magnesium compounds dissolved therein is neutralized by addition of an aqueous solution of sodium hydroxide, the precipitated impurities are separated from the sodium phosphate solution thus obtained, the sodium phosphate solution is evaporated to dryness and the evaporation residue is calcined, the improvement which comprises neutralizing said aqueous solution of phosphoric acid at a temperature not exceeding 85° C., maturing the neutralization product at a temperature of from 70° to 85° C. for a period of at least one hour before separating said precipitated impurities, submitting the sodium phosphate solution, having a sodium phosphate content of at least 40% by weight, prior to the evaporation to dryness, to a heat treatment at a temperature of from 100° to 200° C., at boiling point or under, and at atmospheric or superatmospheric pressure, for a period such as to induce substantially complete precipitation of the magnesium compounds dissolved in said sodium phosphate solution, the precipitate resulting from this heat treatment being separated from the heat treated solution.
Claim 3
Dependent Claim
23 words
The process of claim 1, in which the solution of phosphoric acid is neutralized at a temperature of from 70° to 85° C.
Claim 4
Dependent Claim
23 words
The process of claim 1, in which said neutralisation product is left to mature for a period of from 2 to 3 hours.
Claim 5
Dependent Claim
86 words
The process of claim 1, in which the solution of phosphoric acid is neutralized in two stages, sodium hydroxide being added in the first stage in an amount necessary for the formation of monosodium phosphate, and in the second stage in an amount necessary for the formation of 2 moles of disodium phosphate for each mole of monosodium phosphate, the product obtained after each stage being left to mature at a temperature of from 70° to 85° C. for a period of at least one hour.
Claim 6
Dependent Claim
24 words
The process of claim 1, in which the sodium phosphate solution is concentrated at a temperature less than 80° C. and at subatmospheric pressure.
Claim 7
Dependent Claim
28 words
The process of claim 1, in which the sodium phosphate solution submitted to said heat treatment has a sodium phosphate content of from 40 to 50% by weight.
Claim 8
Dependent Claim
44 words
The process of claim 1, in which said heat treatment is carried out for a period such as to obtain in the sodium phosphate solution a magnesium content not exceeding 250 ppm, with respect to the P 2 O 5 content of said solution.
Claim 9
Dependent Claim
15 words
The process of claim 7, wherein said magnesium content is from 100 to 250 ppm.
Claim 10
Dependent Claim
55 words
The process of claim 1, wherein prior to submitting the sodium phosphate solution to said heat treatment at a temperature of from 100 to 200° C. said sodium phosphate solution is concentrated to a sodium phosphate content of at least 40% by weight, with separation of precipitated impurities thus obtained from the resulting concentrated solution.
Claim 11
Dependent Claim
37 words
The process of claim 7, wherein said magnesium compounds are initially present in an amount of about 1500-3000 ppm, as metal, with respect to the P 2 O 5 content of the aqueous solution of phosphoric acid.
Claim 12
Dependent Claim
78 words
The process of claim 4, wherein in the first stage of said neutralizing the pH is brought to a value on the order of 3.8-4, and during the second stage the pH is brought to a value on the order of 6.7-6.8, divalent iron and aluminum in the form of phosphates precipitating during said first stage and precipitation of calcium present and a part of the magnesium present in the form of phosphates occuring during said second stage.
Claim 13
Dependent Claim
25 words
The process of claim 1, wherein further impurities initially present include calcium, iron, aluminum, nickel and chromium, the contents thereof being reduced during said process.
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) | 1982-03-26 | 1982-09-25 | 1983-03-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-03-26 | 1986-09-25 | 1987-03-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-03-26 | 1990-09-25 | 1991-03-27 | $7700.00 | Window Closed / Lapsed |