And Ammonia Patents (Class 423/310)
  • Patent number: 10947164
    Abstract: The invention relates to a method for manufacturing an ammonium phosphate fertilizer from a phosphoric acid aqueous solution that has less than 50% P2O5 concentration and is obtained by wet phosphate ore treatment, said phosphoric acid containing traces of cadmium, comprising the following steps: (a) neutralizing said phosphoric acid solution (1) with ammonia (3) up to a molar ratio N/P of between 0.1 and 0.8, (b) reacting said partially neutralized solution (4) with a sulfide source (6) so as to form a cadmium sulfide precipitate (9), (c) separating said precipitate (9) so as to obtain a refined ammoniated phosphoric acid solution (10), (d) ammoniating and granulating said refined solution (10) so as to form said fertilizer (12).
    Type: Grant
    Filed: August 3, 2016
    Date of Patent: March 16, 2021
    Inventors: Mehdi Khouloud, Abdelaali Kossir, Kamal Samrane
  • Patent number: 8821163
    Abstract: Colorless dental compositions for restoring the enamel layer of a tooth are disclosed. The colorless enamel compositions are combined with pigmented dentin compositions to provide a true color match and natural esthetics. Methods that utilize the compositions in placement/build-up techniques in direct restorations are also disclosed.
    Type: Grant
    Filed: August 3, 2010
    Date of Patent: September 2, 2014
    Assignee: Ivoclar Vivadent, Inc.
    Inventor: Terry Lee Culp
  • Patent number: 8658117
    Abstract: A method for production of ammonium phosphates includes providing (210) of a phosphorus-loaded water immiscible liquid phase, adding (212) of anhydrous ammonia to the water immiscible liquid phase, precipitating (214) of mono-ammonium phosphate and/or di-ammonium phosphate from the water immiscible liquid phase and extracting (218) of the precipitated mono-ammonium phosphate and/or di-ammonium phosphate from the water immiscible liquid phase. The method further includes controlling (216) of a temperature of the water immiscible liquid phase during the adding (212) and precipitating (214) to a predetermined temperature interval.
    Type: Grant
    Filed: September 18, 2009
    Date of Patent: February 25, 2014
    Assignee: EasyMining Sweden AB
    Inventor: Yariv Cohen
  • Patent number: 8608821
    Abstract: The invention provides a method for the combined production of (i) a fertilizer selected from the group consisting of ammonium nitrate, ammonium phosphates or a combination thereof, (ii) a concentrated stream of CO2 through an indirect neutralization of ammonia with an acid selected from the group consisting of nitric acid, phosphoric acid, a salt thereof and a combination thereof; said method comprising: (I) reacting a carbonate product with a reagent selected from the group consisting of nitric acid, phosphoric acid, a salt thereof, and a mixture thereof to form CO2, and a fertilizer containing an ammonia component; and (II) separating at least a portion of said carbon dioxide from said fertilizer in a condensed and relatively concentrated stream.
    Type: Grant
    Filed: July 31, 2006
    Date of Patent: December 17, 2013
    Assignee: Clue AS
    Inventor: Riki Canari
  • Patent number: 8172939
    Abstract: A material for cement which comprises a calcium salt powder with an inositol phosphate and/or a salt thereof as adsorbed on the surface thereof, the powder having a specific surface area of 60-120 m2/g. A method of producing a material for cement comprises the step of mixing a calcium ion-containing solution adjusted to alkalinity with a phosphate ion-containing solution to produce a precipitate, the step of maturing the precipitate-containing system while maintaining the alkalinity to obtain a calcium salt powder, the step of recovering the calcium salt powder and drying the same, and the step of immersing the dried calcium salt powder in a solution containing an inositol phosphate and/or a salt thereof to cause the inositol phosphate and/or salt thereof to be adsorbed on the surface of the calcium salt powder.
    Type: Grant
    Filed: September 18, 2007
    Date of Patent: May 8, 2012
    Assignee: Meiji University
    Inventors: Mamoru Aizawa, Yukiko Horiguchi
  • Patent number: 8152891
    Abstract: The invention provides a method for the combined production of (I) a sulfur oxide containing product and (II) a fertilizer selected from a group consisting of ammonium nitrate, ammonium phosphates and a combination thereof, through an indirect neutralization of ammonia with an acid selected from the group consisting of nitric acid, phosphoric acid and a combination thereof, the method comprising: a. contacting a precipitate containing calcium sulfite with a solution of nitric acid and a solution of ammonia in two separate steps, to form the fertilizer, the sulfur oxide containing product and a precipitate containing calcium hydroxide; and b. separating at least portion of the fertilizer, the sulfur oxide and the calcium hydroxide into three separated streams.
    Type: Grant
    Filed: November 28, 2006
    Date of Patent: April 10, 2012
    Assignee: Clue AS
    Inventor: Riki Canari
  • Publication number: 20090025376
    Abstract: A catalytic converter has a housing. The housing defines a conduit and has a support wall defining an opening in the conduit. A removable catalyst element covers the opening for treating an exhaust gas passing through the conduit. A removable bar abuts the catalyst element. A first end of the bar is anchored to the wall and a second end of the bar is bolted to the wall thus clamping the catalyst element between the wall and the bar.
    Type: Application
    Filed: July 27, 2007
    Publication date: January 29, 2009
    Inventor: Mehmood Ahmed
  • Patent number: 7258848
    Abstract: The present invention provides a process for removing ammonia as an aqueous salt solution from an acid gas comprising ammonia and hydrogen sulfide. A strong acid, such as sulfuric acid, is used as a scrubbing agent to convert ammonia to an ammonium salt. Control of pH and stripping in combination with reboiler or evaporators reduces hydrogen sulfide concentration. The ammonium salt is produced as an aqueous solution, which may crystallized to form a solid product. The ammonium salt solution or solid may be used as a fertilizer.
    Type: Grant
    Filed: July 31, 2006
    Date of Patent: August 21, 2007
    Assignee: E. I. du Pont de Nemours and Company
    Inventors: Benny E. Blackwell, Luis Alberto Chu, Monroe Davis, Wayne B. Ely, Robert Joseph Flowers, Steven Lamar Grise, Zeru Berhane Tekie
  • Patent number: 7128880
    Abstract: The invention is directed to a process for enhancing the plant nutrient value of relatively low analysis organic waste material (e.g. sewage sludge) involves treating the waste material with an acid and base in a pipe-cross reactor or tubular to form a melt; spraying the melt onto a recycling bed of fines in a granulator and flashing off the water contained in the melt as steam; rolling the melt onto recycled fine particles in a granulator to form granulated particles; and drying these granulated particles to form an enhanced plant nutrient value composition (e.g. a fertilizer or soil conditioner having a greater NPK value than the original relatively low analysis organic waste material). The process further includes drawing off the fumes from the granulator, passing them through a dryer with the granulated particles, and subsequently oxidizing the fumes to eliminate volatile organic compounds and/or gaseous hydrocarbon pollutants be converting such into carbon dioxide and water vapor.
    Type: Grant
    Filed: December 19, 2002
    Date of Patent: October 31, 2006
    Assignee: Environmental Technologies Capital Partners LLC
    Inventors: Gary L. Dahms, Gary D. Greer
  • Patent number: 6949236
    Abstract: Addition of an aminosulfonate product to an inorganic nitrogen-containing salt provides a composition of matter with improved properties. In particular, 2-acrylamido-2-methylpropanesulfonic acid and its derivatives can be added to ammonium nitrate to provide improved prills.
    Type: Grant
    Filed: November 6, 2001
    Date of Patent: September 27, 2005
    Assignee: The Lubrizol Corporation
    Inventors: Kastrui Lal, Alvin E. Haas, Ricardo M. Collins, Jeffrey M. Carey
  • Publication number: 20020155144
    Abstract: This invention relates to novel room-temperature process for obtaining calcium phosphate, in particular hydroxyapatite, coatings and microspheres that encapsulate drugs, proteins, genes, DNA for therapeutical use. The coatings and microspheres are designed to perform a defined biological function related to drug delivery, such as gene therapy through gene delivery. A novel method for encapsulation, and subsequent controlled release of therapeutically active agents from such biofunctional coatings and microspheres is disclosed. Such coatings and microspheres are useful for side-effects free, long-term, targeted, controlled release and delivery of drugs, proteins, DNA, and other therapeutic agents.
    Type: Application
    Filed: April 20, 2001
    Publication date: October 24, 2002
    Inventors: Tomasz Troczynski, Dean-Mo Liu, Quanzu Yang
  • Publication number: 20020127260
    Abstract: A stable, phase-pure magnesium-substituted crystalline hydroxyapatite containing from about 2.0 to about 29 wt % magnesium, wherein at least 75 wt % of the magnesium content is substituted for calcium ions in the hydroxyapatite lattice structure.
    Type: Application
    Filed: March 6, 2001
    Publication date: September 12, 2002
    Inventors: Richard E. Riman, Wojciech Suchanek, Pavel Shuk, Kevor S. TenHuisen
  • Patent number: 6280494
    Abstract: A process of forming a mixture of diammonium phosphate and triammonium phosphate by the reaction of phosphoric acid with gaseous ammonia in a spray column. In the process, the reaction occurs under pressure. With the appropriate selection of the ammonia pressure and the phosphoric acid feed rate sprayed into the spray column, the amount of each of the diammonium phosphate and triammonium phosphate formed can be controlled.
    Type: Grant
    Filed: July 21, 1999
    Date of Patent: August 28, 2001
    Assignee: IMC-Agrico Co.
    Inventor: Kenneth J. Jardine
  • Patent number: 6241796
    Abstract: A process for the preparation of granular fertilizer grade DAP (a product composed of ammonium phosphates, principally diammonium phosphate, resulting from the ammoniation of phosphoric acid, as defined in Official Publication No. 52 of the Association of American Plant Food Officials, dated 1999) comprising partially preneutralizing orthophosphoric acid with ammonia, completing the ammoniation of the orthophosphoric acid with ammonia in a rotary ammoniator-granulator to provide granular DAP, sizing the granular DAP to provide the granular DAP product, reducing the particle size of the oversized granular DAP, and recycling the undersized granular DAP and the sized-reduced oversized granular DAP to the ammoniator-granulator.
    Type: Grant
    Filed: July 21, 1999
    Date of Patent: June 5, 2001
    Assignee: IMC-Agrico Company
    Inventors: Kenneth J. Jardine, Vaughn V. Astley
  • Patent number: 6117406
    Abstract: A process for manufacturing ammonium salts using a reactor which includes a first tubular reaction chamber having at least one acid feed and at least on ammonia feed which are arranged in a first up-stream part of the reactor. At least one second ammonia feed is introduced into a second part of the reactor which is arranged as an extension of the first and which includes, in a flow direction, a convergent segment, a cylindrical tube and a divergent segment. The second ammonia feed communicates with the second part in the vicinity of the convergent segment and the processes is controlled to obtain basic vapors at an outlet of the reactor.
    Type: Grant
    Filed: February 12, 1999
    Date of Patent: September 12, 2000
    Assignee: Kaltenbach-Thuring S.A.
    Inventors: Edmond Vogel, Jacques Monsterleet
  • Patent number: 5578107
    Abstract: There is disclosed a caking inhibitor for mono-and diammonium phosphates which is water soluble and effective at small concentrations rendering the phosphates acceptable in most utilities without separation of the inhibitor. The inhibitor is sodium sulfate. Effective amounts of this salt range from about 0.5 percent to about 1 percent by weight in the ammonium phosphates. It is particularly advantageous that this salt is useful in both types of ammonium phosphates.
    Type: Grant
    Filed: June 6, 1995
    Date of Patent: November 26, 1996
    Assignee: Monsanto Company
    Inventors: Robert V. Brill, Louis A. Highfill
  • Patent number: 5244645
    Abstract: This invention is a process for removing NH.sub.3 from a NH.sub.3 -containing liquid stream. The process contains the following steps: (a) passing a NH.sub.
    Type: Grant
    Filed: October 1, 1991
    Date of Patent: September 14, 1993
    Assignee: Shell Oil Company
    Inventor: Humbert H. Chu
  • Patent number: 5022913
    Abstract: An improved batch process for the production, in equipment readily available at the fertilizer dealer level, of high-analysis stable ammonium orthophosphate suspension fertilizers effected by the ammoniation of solid intermediates derived from wet-process orthophosphoric acids or combinations of the solid intermediates with such wet-process type acid or other impure phosphoric acids. Fluorosilicic acid, a by-product of the phosphate industry which is readily available and relatively inexpensive, is utilized as a source of fluoride. The fluorosilicic acid is added to the batch formulation prior to the ammoniation step thereby allowing the fluorosilicic acid to be converted to ammonium fluoride. Subsequently, the metallic impurities are allowed to precipitate as fluoride compounds instead of the usual troublesome impurity-phosphate-water gels which have been identified as causing complete destruction of suspension fluidity during storage.
    Type: Grant
    Filed: August 28, 1989
    Date of Patent: June 11, 1991
    Assignee: Tennessee Valley Authority
    Inventors: Ewell F. Dillard, James R. Burnell
  • Patent number: 4919906
    Abstract: New processes and equipment are disclosed for producing elemental phosphorus and thermal phosphoric acid. Benefits are listed below.1. Phosphorus-containing solids are recycled to smelting furnaces thus eliminating hazardous waste generation.2. Phosphorus furnace feedstock is upgraded and this permits unbeneficiated phosphate ore to be smelted.3. Energy is conserved during manufacture of elemental phosphorus and phosphoric acid.4. Electric energy is produced by cogeneration.5. Fluorine in phosphate ore is recovered as ammonium fluoride.6. Phosphorus-containing liquids are used as feedstock for production of suspension fertilizers.Benefits are achieved by agglomerating phosphate ore with monocalcium phosphate binder by a method which upgrades the ore. Phosphorus-containing solids are fluidized and burned to form an impure phosphoric acid mixture which is reacted with small sized phosphate ore to form monocalcium phosphate binder.
    Type: Grant
    Filed: June 3, 1988
    Date of Patent: April 24, 1990
    Assignee: James C. Barber and Associates, Inc.
    Inventor: James C. Barber
  • Patent number: 4781905
    Abstract: A process is developed for producing phosphoric acid and phosphates from wet-process phosphoric acid. The crude acid is extracted with a waterimmiscible solvent mixture consisting of mixed trialkyl phosphine oxide and a diluent, wherein about 2/3 P.sub.2 O.sub.5 in the crude acid is extracted into solvent mixture and the balance remains in the raffinate. Pure phosphoric acid or phosphates are produced by stripping the loaded solvent with appropriate aqueous phase and secondary calcium phosphate fertilizer is obtained by neutralizing the raffinate with calcium carbonate.
    Type: Grant
    Filed: May 30, 1986
    Date of Patent: November 1, 1988
    Inventors: Jiang Yu-Ming, Su Yuan-Fu
  • Patent number: 4744965
    Abstract: A process is disclosed for the manufacture of granular diammonium phosphate (DAP) by reacting anhydrous ammonia with phosphoric acid in a reactor to form reaction product consisting of a partially reacted slurry of monoammonium phosphate and diammonium phosphate. The slurry is pumped to a rotary granulator-reactor where it is further reacted with anhydrous ammonia to form a solid granular diammonium phosphate mixture having a range of particle sizes consisting of undersize, oversize and product. After drying the diammonium phosphate mixture, a portion of the dried granular diammonium phosphate mixture is diverted back to the granulator-reactor prior to delivery to a classifying means. The portion of dried granular diammonium phosphate mixture not diverted to the granulator-reactor, is introduced to a classifying means set to a narrow separation to separate undersize and oversize granular particles from the desired product granular particles.
    Type: Grant
    Filed: August 28, 1986
    Date of Patent: May 17, 1988
    Assignee: Conserv, Inc.
    Inventor: William D. Fairchild
  • Patent number: 4704262
    Abstract: A process for the production of dialkali metal phosphates by ion exchange is disclosed. The process is carried out by first ammoniating a water-soluble phosphate source such as phosphoric acid or monocalcium phosphate. The resulting ammoniated phosphate solution is then contacted with a weak cation exchange resin in the alkali metal form to produce the dialkali metal phosphate as well as an ammonium-loaded weak cation exchange resin. The cation exchange resin is regenerated by contacting it with an alkali metal salt solution which effects an exchange of alkali metal from ammonium to produce a rgenerated weak cation exchange resin in the alkali metal form as well as a water-soluble ammonium salt corresponding to the initial alkali metal salt.
    Type: Grant
    Filed: January 14, 1986
    Date of Patent: November 3, 1987
    Assignee: Advanced Separation Technologies Incorporated
    Inventor: W. Wes Berry
  • Patent number: 4678650
    Abstract: An aqueous alkali phosphate solution is made. An organic phase is countercurrently mixed with an aqueous phase, the two phases being used in a volume ratio larger than 1:1 and formed aqueous alkali phosphate solution is separated from the remaining organic phase. The two phases are mixed and reacted in a reaction zone comprised of a mixing and separating zone. The organic phase is continuously dispersed in the aqueous phase. A volume excess of aqueous phase is maintained in the mixing zone and the two phases are used in an overall quantity sufficient to provide a volume ratio of organic to aqueous phase of 4:6 to 2:8.
    Type: Grant
    Filed: March 22, 1985
    Date of Patent: July 7, 1987
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Reinhard Gradl, Gero Heymer
  • Patent number: 4662929
    Abstract: The invention relates to a method of recovering nutrients from the flue gases of a fertilizer plant by exposing hot, almost water-saturated reaction gases (4) obtained from the fertilizer production process to a countercurrent scrubbing (5, 6) and by scrubbing the hot gases (19) obtained from the drying (16) of the fertilizer, in order to recover the gaseous impurities present in the gases. According to the invention, the hot gases (19) obtained from the drying of the fertilizer are scrubbed (21) with the scrubbing solution (7) coming from the countercurrent scrubbing (5, 6) of the hot, almost water-saturated reaction gases (4), in order to concentrate this scrubbing solution (7) before it is returned to the fertilizer production process (1-3).
    Type: Grant
    Filed: June 12, 1985
    Date of Patent: May 5, 1987
    Assignee: Kemira Oy
    Inventor: Pekka T. Lammi
  • Patent number: 4652295
    Abstract: An improved continuous process for the production of fertilizers, wherein the reactions, mixing, sizing, and moisture removal required to produce a resultant product are carried out on a simple, flat surface that moves horizontally, and wherein, in the reactor-mixing zone of said surface, the surface movement, the shearing action of moving blades, the moving spargers for distributing reactants and reaction products, the unusually wide dispersion of the reactants and reaction products, and the unusually long retention time and extensive aeration of the final reaction products and reacted product have the useful benefits of low consumption of energy, close product size control, elimination of the need for recycling produced materials as a means of wetness control in the reactor-mixing zone, and of achieving relatively simple, low cost processing.
    Type: Grant
    Filed: October 14, 1981
    Date of Patent: March 24, 1987
    Inventor: Norval K. Alfrey
  • Patent number: 4637921
    Abstract: An improved process of concentrating wet process phosphoric acid by continuously contacting an acid feed containing at least about 56 weight percent of P.sub.2 O.sub.5 based on the total weight of the feed with heated gases consisting of air and gaseous fuel combustion products thereby forming a mixture of said gases containing entrained superphosphoric acid particles, continuously coalescing said mixture in a coalescence zone forming coalesced superphosphoric acid and continuously removing the coalesced superphosphoric acid from said coalescence zone.
    Type: Grant
    Filed: April 19, 1985
    Date of Patent: January 20, 1987
    Inventors: James E. Sansing, Byron M. McCarver
  • Patent number: 4632813
    Abstract: A process is disclosed for the production of water soluble ammonium phosphates, comprising the following steps:(a) to react in a reaction step ammonia and untreated phosphoric acid with P.sub.2 O.sub.5 concentration comprised within the range of from 30 to 54%, outcoming from wet processes;(b) to filter under high temperature conditions the reaction suspension, separating the impurity-containing sludges from an aqueous solution of ammonium phosphate;(c) to cool and crystallize the aqueous solution of ammonium phosphate;(d) to separate the formed ammonium phosphate crystals from the mother liquors.
    Type: Grant
    Filed: April 11, 1985
    Date of Patent: December 30, 1986
    Assignee: Enichem Agricolutra
    Inventors: Filippo Anastasi, Guido Anania, Vito Cultrera, Giuseppe Carfi'
  • Patent number: 4610862
    Abstract: A process for producing purified diammonium phosphate (abbreviated to DAP) directly from wet process phosphoric acid with a high yield is provided, which process comprises reacting wet process phosphoric acid with NH.sub.3 at 50.degree..about.80.degree. C. while keeping the molar ratio of NH.sub.3 /H.sub.3 PO.sub.4 at 1.65-1.90; separating the resulting slurry containing DAP crystals and an insoluble sludge into a slurry containing the former and a slurry containing the latter; treating the former slurry in a conventional manner to recover DAP; while treating the latter slurry by heating it to 60.degree..about.95.degree. C. to dissolve DAP contained therein, removing the sludge by centrifugal separation and concentrating the filtrate to recover DAP; and combining the two portions of DAP.
    Type: Grant
    Filed: March 11, 1985
    Date of Patent: September 9, 1986
    Assignee: Chisso Corporation
    Inventors: Taizo Kajitani, Shigeo Fujii, Tadao Sato, Ikuo Yonehara, Chikashi Fukumura, Kenji Harita
  • Patent number: 4610853
    Abstract: A process for producing purified monoammonium phosphate (abbreviated to MAP) directly from wet process phosphoric acid with a high yield is provided, which process comprises reacting wet process phosphoric acid with NH.sub.3 at 50.degree..about.80.degree. C. while keeping the molar ratio of NH.sub.3 /H.sub.3 PO.sub.4 at 0.9.about.1.35; separating the resulting slurry containing MAP crystals and an insoluble sludge into a slurry containing the former and a slurry containing the latter; treating the former slurry in a conventional manner to recover MAP; while treating the latter slurry by heating it to 60.degree..about.95.degree. C. to dissolve MAP contained therein, removing the sludge by centrifugal separation and concentrating the filtrate to recover MAP; and combining the two portions of MAP.
    Type: Grant
    Filed: March 8, 1985
    Date of Patent: September 9, 1986
    Assignee: Chisso Corporation
    Inventors: Taizo Kajitani, Shigeo Fujii, Tadao Sato, Ikuo Yonehara, Chikashi Fukumura, Kenji Harita
  • Patent number: 4592771
    Abstract: A novel method is provided to produce di-ammonium phosphate fertilizer by operating a DAP reactor and granulator in such a manner that part of the hot exhaust gases from the DAP reactor are diverted into a vaporizer where liquid ammonia is vaporized for use in the DAP reactor and the granulator. Considerable savings in energy and other advantages are achieved through such operation.
    Type: Grant
    Filed: August 29, 1984
    Date of Patent: June 3, 1986
    Assignee: Brunswick Mining and Smelting Corporation Ltd.
    Inventors: Loftus A. Benjamin, Donald T. Aikens, Thomas B. Gravestock, Herman Soehodho
  • Patent number: 4565680
    Abstract: In the process of the invention spent phosphoric acid is concentrated and stripped with air to a greater than 50% P.sub.2 O.sub.5 concentration to remove nitric acid. As a result of concentrating the spent acid a portion of the aluminum precipitates as monoaluminum phosphate, which is recovered by filtration. The filtrate is then ammoniated to produce a monoammonium phosphate solution. The solids precipitated during ammoniation and comprising aluminum ammonium phosphate which contains other metal phosphates are washed and reacted with aqueous ammonia to form diammonium phosphate.
    Type: Grant
    Filed: January 14, 1985
    Date of Patent: January 21, 1986
    Assignee: Stauffer Chemical Company
    Inventors: Lanny E. Todd, Philip E. Burke, Danny L. Smith, Carla T. Gleason
  • Patent number: 4536378
    Abstract: Processes for the preparation of phosphoric acid, such as merchant phosphoric acid, and for the provision of phosphoric acid suitable for the preparation of ammonium phosphates, are disclosed. Such processes comprise providing a source stream of phosphoric acid comprising more than about 30% P.sub.2 O.sub.5, said source stream having impurities, and removing from the source stream a minor proportion, 20% or less, to form a treatment stream. The level of impurities in the treatment stream is reduced employing any of the means known to those skilled in the art, especially solvent extraction. At least a portion of the treated treatment stream is combined with the balance of the source stream to form a product stream. The treated treatment stream and source stream are proportioned so as to render the product stream less susceptible to post-precipitation than the source stream.
    Type: Grant
    Filed: October 13, 1983
    Date of Patent: August 20, 1985
    Inventor: Edward A. White
  • Patent number: 4505733
    Abstract: The process for producing liquid combined fertilizers according to the present invention comprises neutralization of extraction-type phosphoric acid with an excess of gaseous ammonia taken in an amount of 1-1.2 parts by weight relative to the content thereof in the final product at a temperature of the reagents of from 60.degree. to 250.degree. C., mixing of the resulting neutralization products with a liquid phase consisting of water or ammonia water and a portion of the final product recycled to the process; said mixing is conducted under a pressure of 0.05-0.7 atm and at an excess of water in the liquid phase of 1.05-2.0 parts by weight relative to the content thereof in the final product; the process is carried out at a ratio of circulation of the final product of 2 to 40 and at a pressure differential at the stages of neutralization and mixing of from 0.1 to 6 atm.The process according to the present invention may be useful in the agriculture.
    Type: Grant
    Filed: February 2, 1984
    Date of Patent: March 19, 1985
    Inventors: Mikhail V. Lykov, Vladimir M. Lembrikov, Svetlana I. Golovkina, Nadezhda N. Malakhova, Vladimir N. Sterlin, Viktor N. Kochetkov, Gennady M. Markovin
  • Patent number: 4500502
    Abstract: A method of preparing a purified ammoniated phosphoric acid composition, comprising, reacting an aqueous wet process phosphoric acid with an ammonium ion source at a N/P.sub.2 O.sub.5 weight ratio ranging from about 0.06 to about 0.15 in the presence of solid phase metal ion containing impurities for a time sufficient to precipitate the majority of the impurities in the acid, the impurity precipitation comprising at least several complex metal salts at least one of which contains magnesium, aluminum and fluorine, and obtaining the purified ammoniated phosphoric acid by separating the precipitated impurities therefrom.
    Type: Grant
    Filed: June 28, 1983
    Date of Patent: February 19, 1985
    Assignee: Mississippi Chemical Corporation
    Inventors: Daniel P. McDonald, James C. Wade
  • Patent number: 4493820
    Abstract: A process for the partial removal of impurities present in a wet process phosphoric acid used in the production of granulated mono- or di-ammonium phosphate fertilizers in order to control the grade of the final product. All or a portion of the liquid from the primary scrubbers is clarified to remove the precipitated impurities and the clarified flow is then fed into the reactor along with any unclarified portions of the primary scrubber liquid.
    Type: Grant
    Filed: October 1, 1982
    Date of Patent: January 15, 1985
    Assignee: Gardinier, Inc.
    Inventor: Herbert J. Clausen
  • Patent number: 4451277
    Abstract: Processes and compositions of matter are disclosed for the production of liquid fertilizers wherein wastewater from a phosphorus smelting furnace is incorporated in lqiuid fertilizer processes. The wastewater replaces water evaporated and the wastewater dissolves fertilizer salts. A serious water pollution problem is avoided when wastewater is incorporated in liquid fertilizers. The invention discloses a process for making orthophosphate suspension fertilizer wherein impure phosphoric acid is neutralized in the condensing system, water from the condensing system is bled off, and a suspending clay is added to produce orthophosphate suspension fertilizer. In this process, phosphorus sludge made at phosphorus furnaces is used to produce suspension fertilizer, and wastewater from phosphate smelting furnaces is recovered. New compositions of matter are disclosed.
    Type: Grant
    Filed: September 30, 1982
    Date of Patent: May 29, 1984
    Assignee: James C. Barber and Associates, Inc.
    Inventor: James C. Barber
  • Patent number: 4442081
    Abstract: A wet process phosphoric acid which has been treated with aluminosilicate after the first stage of clarification can be further stabilized against precipitation of solids during storage and transport and the solids from the crystallizer more economically used to make diammonium and triple superphosphate fertilizers by introducing a second stage of clarification of the acid at a P.sub.2 O.sub.5 concentration of 38 to 42 weight percent.
    Type: Grant
    Filed: December 2, 1982
    Date of Patent: April 10, 1984
    Assignee: W. R. Grace & Co.
    Inventors: Roberto I. Morrell, Charles F. Peters
  • Patent number: 4420321
    Abstract: Black carbonaceous floc in wet-process phosphoric acid is removed by contact with an oxidizing agent during the neutralization step with ammonia. In an embodiment the black floc is removed in liquid fertilizers derived from wet-process phosphoric acid by reaction with an oxidizing agent at high temperatures.The oxidizing agent is preferably nitric acid.
    Type: Grant
    Filed: September 30, 1982
    Date of Patent: December 13, 1983
    Assignee: Phillips Petroleum Company
    Inventor: Joseph F. Wilson
  • Patent number: 4390509
    Abstract: A process for the manufacture of phosphoric acid from phosphate rock is provided. The phosphate rock is digested or acidulated with an acid solution containing oxalic acid to produce phosphoric acid and calcium oxalate. Useful by-products are also formed and include calcium carbonate and ammonium oxalate. More specifically, the process provides for the production of phosphoric acid, ammonium phosphate and useful by-products utilizing synthesis gas and air to produce oxalic acid and ammonia. The synthesized oxalic acid is utilized for phosphate rock digestion to produce phosphoric acid, which can be reacted with ammonia to produce ammonium phosphate. Calcium oxalate from phosphate rock digestion is utilized to produce calcium carbonate, ammonium oxalate and oxamide.
    Type: Grant
    Filed: April 16, 1981
    Date of Patent: June 28, 1983
    Assignee: Agrico Chemical Company
    Inventors: Charles W. Weston, Padraic S. O'Neill
  • Patent number: 4383847
    Abstract: A process and product of waste recovery at phosphorus furnaces is disclosed wherein small sized discrete particles of carbonaceous material or beneficiated phosphate ore are mixed with a mineral axis, an alkaline fluid and water, and the reacted mixture is tumbled in a horizontal cylinder at a temperature below that at which the carbonaceous material oxidizes to form agglomerates which are then indurated to discrete particulate size as desired for a charge component; the agglomerates are fed to a phosphorus smelting furnace together with other materials needed to make elemental phosphorus, furnace gases are cooled with recirculating water, a side stream of the water is taken off, treated, and used as feedstock in fluid fertilizers. The side stream of water contains elemental phosphorus, and the side stream is used as make-up water in fertilizer processes. Apparatus is disclosed for agglomerating coke and phosphate and, further, for measuring the abrasion and shatter resistance of agglomerates.
    Type: Grant
    Filed: September 11, 1981
    Date of Patent: May 17, 1983
    Assignee: James C. Barber and Associates, Inc.
    Inventor: James C. Barber
  • Patent number: 4377406
    Abstract: A process for the production of fluid fertilizers (suspensions and/or solution type) made from merchant-grade phosphoric acid (50-58 percent P.sub.2 O.sub.5), sulfuric acid, liquid anhydrous ammonia, and water, wherein liquid ammonia is heated in heat exchange means juxtaposed hot fertilizer product to form gaseous ammonia, which gaseous ammonia, along with phosphoric acid and sulfuric acid, is fed to a pipe-cross reactor wherein a melt of ammonium polyphosphate sulfate is formed, which melt is subsequently mixed with cooled recycled product to produce a fluid fertilizer with N:P.sub.2 O.sub.5 weight ratios ranging from about 0.3 to 1, which contains from about 10 to 60 percent of its P.sub.2 O.sub.5 values in the form of polyphosphates and 3 to 8 percent by weight sulfur. About 45 percent of the P.sub.2 O.sub.5 as polyphosphate is easily attainable in the product with ambient acid feed temperatures, i.e., about 50.degree. F. to 100.degree. F.
    Type: Grant
    Filed: January 4, 1982
    Date of Patent: March 22, 1983
    Assignee: Tennessee Valley Authority
    Inventors: Frank P. Achorn, Kenneth E. McGill
  • Patent number: 4375980
    Abstract: An improved process for the production of concentrated, high-grade, nitrogen-phosphate (N--P.sub.2 O.sub.5) base suspension fertilizer from wet-process or other phosphoric acids and ammonia. The process involves addition of small proportions of fluosilicic acid during preparation of the suspension to cause modification of monoammonium phosphate crystals to shapes and sizes that do not settle during vibration such as occurs during shipment.
    Type: Grant
    Filed: March 19, 1979
    Date of Patent: March 8, 1983
    Assignee: Tennessee Valley Authority
    Inventors: Thomas M. Jones, John M. Stinson
  • Patent number: 4370304
    Abstract: Ammonium orthophosphate products are prepared by reacting ammonia and phosphoric acid together at high speed under vigorous mixing conditions by spraying the reactants through a two-phase, dual coaxial mixer/sprayer and separately controlling the supply and axial outflow rate of the phosphoric acid at 1 to 10 m/sec. and the outflow rate of ammonia at 200 to 1000 m/sec. (N.T.P.). Thorough mixing and a homogeneous product is obtained by directing the outflow spray into a coaxial cylindrical reaction chamber of a specified size with respect to the diameter of the outermost duct of the sprayer/mixer. The product may be granulated on a moving bed of granules and adjusted in respect of the NH.sub.3 to H.sub.3 PO.sub.4 content by changing the concentration of the phosphoric acid and/or supplying additional ammonia to the granulation bed.
    Type: Grant
    Filed: August 21, 1981
    Date of Patent: January 25, 1983
    Assignee: Unie van Kunstmestfabrieken, B.V.
    Inventors: Petrus F. A. M. Hendriks, Arie Jansen, Willem B. van den Berg, Cornelis Hoek
  • Patent number: 4337079
    Abstract: An energy efficient process and apparatus is described that allows production of concentrated polyphosphate containing ammonium phosphate suspension fertilizers that can be stored and handled at temperatures well below 0.degree. F. Ammoniation of the merchant-grade wet-process phosphoric acid provides all of the heat required by the process. Use of a unique enlarged dual pipe-type reactor system allows operation for extended periods without clogging. To obtain the high concentration and excellent low temperature storage and handling properties, the ammonium phosphate must be produced within closely specified and previously undisclosed N:P.sub.2 O.sub.5 and solution concentration ranges. Operation outside the specified composition range will reduce the maximum plant food concentration and may cause some of the ammonium phosphate salts to crystallize and foul the heat-transfer surfaces.
    Type: Grant
    Filed: May 18, 1981
    Date of Patent: June 29, 1982
    Assignee: Tennessee Valley Authority
    Inventors: Horace C. Mann, Jr., Robert S. Meline
  • Patent number: 4336053
    Abstract: A stable liquid fertilizer solution containing nitrogen, phosphorus, iron and optionally sulfur is prepared by mixing a water-soluble iron compound with ammonium polyphosphate and water to produce an iron phosphate slurry having a molar ratio of polyphosphate phosphorus to iron of at least about 2:1, adding ammonia to the iron phosphate slurry to produce a solubilized iron complex; and adding an inorganic acid to the iron complex solution. The amount of acid added is generally that which brings the pH of the fertilizer solution to within the range of about 5.5 to 7.0.
    Type: Grant
    Filed: June 10, 1980
    Date of Patent: June 22, 1982
    Assignee: Phillips Petroleum Company
    Inventor: Joseph R. Kenton
  • Patent number: 4329326
    Abstract: A process for preparing crystalline ammonium dihydrogen phosphate, comprises the steps of (a) adding a sequestering agent into ammonium hydrogen phosphate aqueous solution, the sequestering agent reacting with metallic ions contained in the aqueous solution to form water solouble compounds, (b) heat-treating the aqueous solution at a temperature of 70.degree. C. or more after addition of the sequestering agent, and (c) crystallizing ammonium dihydrogen phosphate out of the aqueous solution after the heat-treating, so that crystalline ammonium dihydrogen phosphate can be obtained in high whiteness and in the form of columnar crystals.
    Type: Grant
    Filed: October 29, 1980
    Date of Patent: May 11, 1982
    Assignee: Central Glass Company, Limited
    Inventors: Soichi Asagao, Masaru Nakatani, Shinsuke Nakagawa, Yoshiyuki Takahara, Naoki Okada
  • Patent number: 4325927
    Abstract: A method of producing purified monoammonium phosphate from wet process phosphoric acid and ammonia is provided. The ammoniation takes place in two stages, the acid being ammoniated in the first stage to a pH between about 1.5 and 2.5. This mixture is allowed to age after which the mixture is ammoniated to a pH between about 4 and 5. An impurity-containing precipitate is formed in the first and second stages of ammoniation that is easily filterable from the monoammonium phosphate solution derived from the second ammoniation stage.
    Type: Grant
    Filed: December 10, 1980
    Date of Patent: April 20, 1982
    Assignee: Agrico Chemical Company
    Inventors: Charles W. Weston, John W. Wen
  • Patent number: 4313918
    Abstract: Ammonium orthophosphate products are prepared by reacting ammonia and phosphoric acid together at high speed under vigorous mixing conditions by spraying the reactants through a two-phase, dual coaxial mixer/sprayer and separately controlling the supply and axial outflow rate of the phosphoric acid at 1 to 10 m/sec. and the outflow rate of ammonia at 200 to 1000 m/sec. (N.T.P.). Thorough mixing and a homogeneous product is obtained by directing the outflow spray into a coaxial cylindrical reaction chamber of a specified size with respect to the diameter of the outermost duct of the sprayer/mixer. The product may be granulated on a moving bed of granules and adjusted in respect of the NH.sub.3 to H.sub.3 PO.sub.4 content by changing the concentration of the phosphoric acid and/or supplying additional ammonia to the granulation bed.
    Type: Grant
    Filed: May 29, 1979
    Date of Patent: February 2, 1982
    Assignee: Unie Van Kunstmestfabrieken, B.V.
    Inventors: Petrus F. A. M. Hendriks, Arie Jansen, Willem B. van den Berg, Cornelis Hoek
  • Patent number: 4308049
    Abstract: A process is disclosed for the absorption of gaseous or liquid ammonia in acid solutions or slurries, including an ammonia absorption zone separated from a water vapor generation zone disposed at a higher level. A pressure difference is created between the two zones, so that the ammonia absorption takes place completely in the neighborhood of the point of inflow of the ammonia, with a temperature increase localized only near to said inflow point, and thus without giving rise to the generation of water vapor which therefore takes place in a liquid-vapor separation zone located at a higher level with respect to the ammonia absorption zone. The acid solutions or slurries to be neutralized may consist essentially of solutions of phosphoric acid, sulphuric acid, nitric acid, solutions resulting from the nitric acid attack on phosphorites, acid slurries resulting from nitric acid attack or sulphonitric acid attack on phosphorites, or mixtures thereof.
    Type: Grant
    Filed: November 28, 1978
    Date of Patent: December 29, 1981
    Assignee: Montedison, S.p.A.
    Inventor: Iti Mini
  • Patent number: T102601
    Abstract: Method for production of granular ammonium polyphosphate fertilizer in which ammonium polyphosphate melt is prepared in a simple inline reactor and distributed onto a bed of solids in a drum granulator to bind smaller fertilizer particles into granules. The desired polyphosphate content can be obtained in the granular product by adjusting the total heat input of the feed reactants to the reactor by means of energy conservation modifications to the system. Energy losses from the reaction system are controlled by use of a predetermined quantity of insulation so that varying amounts of the maximum theoretical heat input can be utilized to produce products of polyphosphate contents as desired.
    Type: Grant
    Filed: March 15, 1982
    Date of Patent: January 4, 1983
    Inventors: Byron R. Parker, Thomas R. Stumpe