US3950495A
Expired / Lapsed
US
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Method for the continuous preparation of stable aqueous ammonium polyphosphate compositions
Assignee: Platte Chemical Co
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Filing: 1973-12-21
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Granted: 1976-04-13
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Expires: 1993-12-21
Abstract
Abstract An improved method for the continuous production of stable aqueous ammonium polyphosphate compositions which are useful as fertilizers and fire retardants. Wet-process superphosphoric acid which is primarily in the orthophosphate form and anhydrous ammonia vapor are combined in a pipe reactor wherein the exothermic ammoniation of the acid and the conversion of a portion of the orthophosphate to polyphosphate caused by the heat liberated in the exothermic ammoniation reaction occur. A stream of the acid is introduced into the interior of a stream of ammonia vapor in the pipe reactor in order to avoid corrosion of the pipe reactor.
Inventors
- 👤 Alvin William Ries
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 15:30
CPC Classifications
C; C05; C05B; C05B1/00; C05B1/06; C01; C01B; C01B25/00; C01B25/16; C01B25/26; C01B25/28; C01B25/38; C01B25/40; C01B25/405
Claims Analysis
Total Claims: 7
Claim 1
Independent Claim
478 words
An improved method for the continuous production of a stable aqueous ammonium polyphosphate composition comprising A. reacting in a pipe reactor wet-process superphosphoric acid, said acid being primarily in the orthophosphate form, and anhydrous ammonia vapor in an exothermic ammoniation to thereby ammoniate a portion of the acid and to dehydrate and convert a portion of the orthophosphate to polyphosphate in the pipe reactor by means of the heat generated by the exothermic ammoniation reaction by I. introducing the ammonia in the form of a single stream and exclusively into the pipe reactor and introducing the acid in the form of a single stream and exclusively into the pipe reactor along the axis of the pipe reactor and into the center of the stream of ammonia in the pipe reactor to thereby form the reaction mixture and to prevent corrosion of the pipe reactor by minimizing contact of the pipe reactor walls with the acid heated by the heat evolved in the ammoniation reaction, said streams containing the exact stoichiometric amounts of the acid and the ammonia that are required in the analysis desired for the final stable aqueous ammonium polyphosphate composition and said acid stream being introduced into said ammonia stream at a point downstream from where said ammonia stream is introduced into the pipe reactor; Ii. reducing the linear velocity of the combined ammonia and acid streams in the pipe reactor as they are being combined to form the reaction mixture in order to achieve efficient mixing of the combined streams within the pipe reactor; and Iii. allowing the temperature of the reaction mixture in the pipe reactor to increase in response to the heat liberated by the ammoniation reaction and without the addition or removal of heat by external means and thereby effecting the partial conversion of orthophosphate to polyphosphate in the pipe reactor; B. quenching the conversion reaction by removing the hot reaction mixture stream from the pipe reactor and adding to it a cooler stream consisting essentially of water, said water being at such a temperature as to lower the temperature of the reaction mixture enough to quench the conversion reaction and said water being added in the exact stoichiometric amount that is required in the analysis desired for the final stable aqueous ammonium polyphosphate composition; and C. completing rapidly the ammoniation reaction and the conversion of the reaction mixture stream to a reaction product stream in a reaction medium formed by next introducing the reaction mixture stream into a cooler stream of the desired final stable aqueous ammonium polyphosphate, said cooler stream being at such temperature as to lower the temperature of the reaction mixture below that at which loss of polyphosphate due to hydrolysis is significant; wherein steps A, B, and C are performed in a completely closed system, thereby eliminating additional separation steps and losses of volatile components by volatilization.
Claim 2
Dependent Claim
478 words
An improved method for the continuous production of a stable aqueous ammonium polyphosphate composition comprising A. reacting in a pipe reactor wet-process superphosphoric acid, said acid being primarily in the orthophosphate form, and anhydrous ammonia vapor in an exothermic ammoniation to thereby ammoniate a portion of the acid and to dehydrate and convert a portion of the orthophosphate to polyphosphate in the pipe reactor by means of the heat generated by the exothermic ammoniation reaction by I. introducing the ammonia in the form of a single stream and exclusively into the pipe reactor and introducing the acid in the form of a single stream and exclusively into the pipe reactor along the axis of the pipe reactor and into the center of the stream of ammonia in the pipe reactor to thereby form the reaction mixture and to prevent corrosion of the pipe reactor by minimizing contact of the pipe reactor walls with the acid heated by the heat evolved in the ammoniation reaction, said streams containing the exact stoichiometric amounts of the acid and the ammonia that are required in the analysis desired for the final stable aqueous ammonium polyphosphate composition and said acid stream being introduced into said ammonia stream at a point downstream from where said ammonia stream is introduced into the pipe reactor; Ii. reducing the linear velocity of the combined ammonia and acid streams in the pipe reactor as they are being combined to form the reaction mixture in order to achieve efficient mixing of the combined streams within the pipe reactor; and Iii. allowing the temperature of the reaction mixture in the pipe reactor to increase in response to the heat liberated by the ammoniation reaction and without the addition or removal of heat by external means and thereby effecting the partial conversion of orthophosphate to polyphosphate in the pipe reactor; B. quenching the conversion reaction by removing the hot reaction mixture stream from the pipe reactor and adding to it a cooler stream consisting essentially of water, said water being at such a temperature as to lower the temperature of the reaction mixture enough to quench the conversion reaction and said water being added in the exact stoichiometric amount that is required in the analysis desired for the final stable aqueous ammonium polyphosphate composition; and C. completing rapidly the ammoniation reaction and the conversion of the reaction mixture stream to a reaction product stream in a reaction medium formed by next introducing the reaction mixture stream into a cooler stream of the desired final stable aqueous ammonium polyphosphate, said cooler stream being at such temperature as to lower the temperature of the reaction mixture below that at which loss of polyphosphate due to hydrolysis is significant; wherein steps A, B, and C are performed in a completely closed system, thereby eliminating additional separation steps and losses of volatile components by volatilization.
Claim 3
Dependent Claim
84 words
The method of claim 1 wherein the step of reacting the acid and ammonia in the pipe reactor comprises additionally introducing the stream of acid into the pipe reactor at a constant flow rate; introducing the stream of ammonia into the pipe reactor at an adjustable flow rate; measuring the pH of the reaction product stream; and adjusting the flow rate of the stream of ammonia in a predetermined relation to the pH of the reaction product stream and the desired final composition requirements.
Claim 4
Dependent Claim
63 words
The method of claim 1 wherein the step of quenching the conversion reaction comprises additionally introducing the stream of water at an adjustable flow rate; measuring the specific gravity of the reaction product stream; and adjusting the flow rate of the stream of water in a predetermined relation to the specific gravity of the reaction product stream and the desired final composition requirements.
Claim 5
Dependent Claim
67 words
The method of claim 1 wherein the wet-process superphosphoric acid introduced into the pipe reactor contains from about 60 percent up to about 72 percent P 2 O 5 by weight and sufficient orthophosphate is converted into polyphosphate in the pipe reactor so that at least 50 percent of the P 2 O 5 content of the final aqueous ammonium polyphosphate composition is in the polyphosphate form.
Claim 6
Dependent Claim
90 words
The method of claim 1 comprising additionally cooling the reaction product stream; transferring a portion of the reaction product stream to storage, said portion corresponding in flow rate to that of the quenched reaction mixture stream which is continuously being combined with the cooler stream of the desired final stable aqueous ammonium polyphosphate; and transferring the remainder of the reaction product stream to a recycle stream and using it as the cooler stream of the desired final stable aqueous ammonium polyphosphate which is combined with the quenched reaction mixture stream.
Claim 7
Dependent Claim
206 words
The method of claim 5 wherein the step of reacting the acid and ammonia in the pipe reactor comprises additionally introducing the stream of acid into the pipe reactor at a constant flow rate; introducing the stream of ammonia into the pipe reactor at an adjustable flow rate; measuring the pH of the reaction product stream; and adjusting the flow rate of the stream of ammonia in a predetermined relation to the pH of the reaction product stream and the desired final composition requirements; and wherein the step of quenching the conversion reaction comprises additionally introducing the stream of water at an adjustable flow rate; measuring the specific gravity of the reaction product stream; and adjusting the flow rate of the stream of water in a predetermined relation to the specific gravity of the reaction product stream and the desired final composition requirements; and wherein the wet-process superphosphoric acid introduced into the pipe reactor contains from about 60 percent up to about 72 percent P 2 O 5 by weight and sufficient orthophosphate is converted into polyphosphate in the pipe reactor so that at least 50 percent of the P 2 O 5 content of the final aqueous ammonium polyphosphate composition is in the polyphosphate form.
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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) | 1979-04-13 | 1979-10-13 | 1980-04-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-04-13 | 1983-10-13 | 1984-04-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-04-13 | 1987-10-13 | 1988-04-13 | $7700.00 | Window Closed / Lapsed |