US4011300A
Expired / Lapsed
US
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Method of producing ammonium polyphosphate
Assignee: Union Oil Company of California
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Filing: 1975-06-27
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Granted: 1977-03-08
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Expires: 1995-06-27
Abstract
Abstract Phosphoric acids having H 2 0/P 2 O 5 mole ratios of about 4.5 or less are converted to aqueous solutions of ammonium polyphosphates of which at least about 40 percent of the P 2 O 5 is present as acyclic polyphosphates. The reaction is conducted at 500° to about 750° F. sufficient to increase the polymeric P 2 O 5 content at least 10 percent by reacting a highly dispersed, unconfined acid spray with substantially anhydrous ammonia. High conversions to polymeric species are obtained while minimizing both reactor fouling when using impure wet-process acids, and corrosion occurring with either wet-process or "white" acids.
Inventors
- 👤 Bruce A. Harbolt
- 👤 Donald C. Young
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 17:06
CPC Classifications
C; C05; C05B; C05B13/00; C05B13/06; C01; C01B; C01B25/00; C01B25/16; C01B25/26; C01B25/28; C01B25/38; C01B25/40; C01B25/405
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
362 words
The method of producing aqueous solutions of mixed ammonium phosphates, of which at least 40 percent of the equivalent P 2 O 5 is present as polyphosphates, from a phosphoric acid feed of which less than 40 percent of the total P 2 O 5 is in the form of a member selected from the group consisting of polymerized phosphoric acid, ammonium polyphosphates and combinations thereof, which feed has an H 2 O/P 2 O 5 mole ratio of about 4.5 or less, by spraying said acid from an acid spray means downwardly through an unconfined reaction zone having a minimum internal diameter of about at least 2 feet and a height of at least about 2 feet determined as the distance between said acid spray means and the upper surface of said aqueous quench and into a liquid phase, aqueous quench under conditions sufficient to produce a dispersed liquid acid spray, jetting ammonia radially inwardly into said acid spray in said unconfined reaction zone around the full periphery of said acid spray in a direction and at a velocity having an inward radial vector of at least about 200 feet per second and a mass flow rate of at least about 0.12 weight parts ammonia per weight part acid determined as P 2 O 5 and further dispersing said acid phase into discontinuous small liquid droplets, surrounding said acid droplets with said ammonia, and reacting said ammonia with said acid to adiabatically heat the unconfined acid droplets to a temperature within the range of about 500° to about 750° F. by the autogenous heat of reaction, increase the polymeric P 2 O 5 content by an amount corresponding to at least about 10 percent of the total P 2 O 5 present, and convert said acid to an ammoniated, polymerized melt, of which at least about 40 percent of the phosphate determined as P 2 O 5 is present as ammonium polyphosphates, within less than about 5 feet of said acid spray means and before said acid spray contents said aqueous quench, and quenching said melt to a temperature of less than about 200° F. by immersion in said aqueous quench.
Claim 2
Independent Claim
362 words
The method of producing aqueous solutions of mixed ammonium phosphates, of which at least 40 percent of the equivalent P 2 O 5 is present as polyphosphates, from a phosphoric acid feed of which less than 40 percent of the total P 2 O 5 is in the form of a member selected from the group consisting of polymerized phosphoric acid, ammonium polyphosphates and combinations thereof, which feed has an H 2 O/P 2 O 5 mole ratio of about 4.5 or less, by spraying said acid from an acid spray means downwardly through an unconfined reaction zone having a minimum internal diameter of about at least 2 feet and a height of at least about 2 feet determined as the distance between said acid spray means and the upper surface of said aqueous quench and into a liquid phase, aqueous quench under conditions sufficient to produce a dispersed liquid acid spray, jetting ammonia radially inwardly into said acid spray in said unconfined reaction zone around the full periphery of said acid spray in a direction and at a velocity having an inward radial vector of at least about 200 feet per second and a mass flow rate of at least about 0.12 weight parts ammonia per weight part acid determined as P 2 O 5 and further dispersing said acid phase into discontinuous small liquid droplets, surrounding said acid droplets with said ammonia, and reacting said ammonia with said acid to adiabatically heat the unconfined acid droplets to a temperature within the range of about 500° to about 750° F. by the autogenous heat of reaction, increase the polymeric P 2 O 5 content by an amount corresponding to at least about 10 percent of the total P 2 O 5 present, and convert said acid to an ammoniated, polymerized melt, of which at least about 40 percent of the phosphate determined as P 2 O 5 is present as ammonium polyphosphates, within less than about 5 feet of said acid spray means and before said acid spray contents said aqueous quench, and quenching said melt to a temperature of less than about 200° F. by immersion in said aqueous quench.
Claim 3
Dependent Claim
58 words
The method of claim 1 wherein said H 2 O/P 2 O 5 mole ratio of said acid feed is about 3.3 or less, and said reaction temperature is at least about 600° F. sufficient to produce a reaction melt product of which at least 55 percent of the P 2 O 5 is present as polymeric species.
Claim 4
Dependent Claim
76 words
The method of claim 1 wherein said acid feed is a wet process acid having and H 2 O/P 2 O 5 molar ratioa of about 3.3 or less, a viscosity of at least about 4000 cp at 80° F. and containing about 2 to about 20 weight percent cogeneric impurities, and said acid is ejected from said spray means at a temperature of about 250° to about 500° F. sufficient to substantially reduce said viscosity.
Claim 5
Dependent Claim
63 words
The method of claim 3 wherein said acid feed is heated to said temperature between about 250° and about 500° F. prior to passage to said spray means at least in part by reaction of said feed with ammonia in an amount corresponding to about 0.04 to about 0.1 weight parts ammonia per weight part acid determined as P 2 O 5 .
Claim 6
Dependent Claim
84 words
The method of claim 1 wherein said unconfined reaction zone is defined by a substantially gas tight enclosure having an internal diameter of at least about two feet, the upper portion thereof containing said spray means and ammonia jet and the lower portion thereof containing said aqueous quench, the vertical distance between said spray means and the upper surface of said quench being at least about two feet and the ratio of said vertical distance to said internal diameter being less than about 4.
Claim 7
Dependent Claim
47 words
The method of claim 5 wherein said ammonia and feed acid are reacted in the substantial absence of air and all of said feed acid and ammonia fed to said unconfined reaction zone, and the reaction products obtained in said zone are absorbed in said aqueous quench.
Claim 8
Dependent Claim
41 words
The method of claim 1 wherein said aqueous quench is maintained at a temperature of about 150° F. or less, a pH between about 5.5 and 8.5, and a P 2 O 5 concentration of less than about 50 weight percent.
Claim 9
Dependent Claim
56 words
The method of claim 1 wherein said ammonia jet and said acid spray means are surrounded by a gas directing shroud having a substantially vertical longitudinal axis, being open at its lower end and having a length of about 4 feet or less and a length to minimum internal diameter ratio of about 10 or less.
Claim 10
Dependent Claim
33 words
The method of claim 1 wherein said acid feed comprises wet-process acid containing at least 1 weight percent incident metallic impurities comprising compounds of iron, magnesium and aluminum determined as the corresponding oxides.
Claim 11
Dependent Claim
24 words
The method of claim 1 wherein said feed acid contains less than 1 weight percent of metallic impurity compounds determined as the corresponding oxides.
Claim 12
Dependent Claim
15 words
The method of claim 10 wherein said feed acid consists essentially of white phosphoric acid.
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) | 1980-03-07 | 1980-09-06 | 1981-03-08 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-03-07 | 1984-09-06 | 1985-03-08 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-03-07 | 1988-09-06 | 1989-03-08 | $7700.00 | Window Closed / Lapsed |