CS214520B1 - A method of producing urea or ammonium phosphate feed phosphate - Google Patents

A method of producing urea or ammonium phosphate feed phosphate Download PDF

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CS214520B1
CS214520B1 CS795477A CS547779A CS214520B1 CS 214520 B1 CS214520 B1 CS 214520B1 CS 795477 A CS795477 A CS 795477A CS 547779 A CS547779 A CS 547779A CS 214520 B1 CS214520 B1 CS 214520B1
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phosphate
urea
ammonium phosphate
ammonium
solution
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CS795477A
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Czech (cs)
Slovak (sk)
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Jozef Papp
Walter Waradzin
Richard Bartik
Vladimir Bartos
Eduard Oravec
Jan Buransky
Jan Palka
Rudolf Knopp
Jozef Kollar
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Jozef Papp
Walter Waradzin
Richard Bartik
Vladimir Bartos
Eduard Oravec
Jan Buransky
Jan Palka
Rudolf Knopp
Jozef Kollar
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Priority to CS795477A priority Critical patent/CS214520B1/en
Publication of CS214520B1 publication Critical patent/CS214520B1/en

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Abstract

SpSsob výroby krmného fosforečnanu močoviny alebo fosforečnanu amonného z nečištej (extrakonej) kyseliny fosforečnéj je založený na odvodnění reakčného roztoku a extrakcie rozpustných nečistot z povrchu a jadra častíc nasýteným vodným roztokom fosforečnanu močoviny alebo fosforečnanu amonného. Vyčištěný produkt sa potom dosuší a expeduje. Extrahovadlo sa potom spracováva na NP alebo NEK hnojivo.The method of producing feed urea phosphate or ammonium phosphate from impure (extracted) phosphoric acid is based on dewatering the reaction solution and extracting soluble impurities from the surface and core of the particles with a saturated aqueous solution of urea phosphate or ammonium phosphate. The purified product is then dried and shipped. The extractant is then processed into NP or NEK fertilizer.

Description

Vynález sa týká spSsobu výroby krmného fosforečnanu močoviny, alebo fosforečnanu amonného připraveného z nečistaj (extrakčnej) kyseliny fosforečnéj.The invention relates to a process for the production of feed urea phosphate or ammonium phosphate prepared from impure (extractive) phosphoric acid.

Sposob přípravy fosforečnanu močoviny alebo fosforečnanu amonného z extrakčnej kyseliny. fosforečnéj priamym sušením vodných roztokov výchto solí a následnou extrakoiou s nasýtsnými roztokmi týohto solí, ako je vo vynáleze riešené, sa v literatuře nepopisuje. Popisujú sa technologie čistenia fosforečnanu močoviny n^pr.: dvojstupňovou kryštalizáoiou fosforečnanu močoviny podlfe postupu TVA, ktorý využívá reoyklu matečných lúhov dávkovaných po separácii krystalickéj fázy odstředivkou do prvého kryštalizátoru, kam sa dávkuje extrakčná kyselina fosforečná (54 % ^2^5^ a Pevn® močovina (viďTVA 12^ Demonstration Ootober 18-19, 1978 - New Development in Fertilizer Technology, TVAMuscle Schoals, Alabama USA). (Η. T. Lewis, T. M. Jones, G. T, Getsinger, Urea Phosphate From Wet Proces Acid and Urea, Paper presentd at ACS Meeting 1975).Process for preparing urea or ammonium phosphate from extraction acid. Phosphoric direct drying of aqueous solutions of these salts and subsequent extraction with saturated solutions of these salts, as described herein, is not described in the literature. Urea phosphate purification technologies are described for example: two-stage crystallization of urea phosphate according to the TVA procedure, which utilizes the reoyl of the mother liquors dosed after separation of the crystalline phase by centrifugation into the first crystallizer where the phosphoric acid extraction extract (54% ^ 2 ^ 5 ^ and P) evn ® urea (see TVA 12 ^ Demonstration Ootober 18-19, 1978 - New Development in Fertilizer Technology, TVAMuscle Schoals, Alabama USA). and Urea, Paper Present at ACS Meeting 1975).

Fosforečnan močoviny alebo fosforečnan amonný sa připraví reakciou kyseliny fosforečnej extrakčnej s močovinou alebo s čpavkom vo vodnom roztoku. Získaný roztok fosforečnanu močoviny, alebo fosforečnanu amonného sa vysuší buď rozprášením do rozprašovačej susiarne, alebo v bubnovéj sušiarni sa neohá odvodnit· za súčasnej kryštalizáoie produktu. Pri obooh sposobooh přípravy sa na povrohu kryštálov lokalizujú nečistoty z extrakčnej kyseliny fosforečné j, ktoré boli'rozpuštěné v kyselině fosforečnéj, resp. po reakcii s močovinou stali sa rozpustné. Takto získaný fosforečnan močoviny alebo fosforečnan amonný sa extrahuje v jednom stupni alebo viaostupňovo, protiprúdovo nasýteným vodným roztokom týohto fosforečnanov. Pri prvom kontaktnom stupni sa použije parný kondenzát alebo čistá voda, ktoré z povrohu častíc rozpúštajú jemné částice fosforeonanovýoh a iných rozpustných nečistit ako i jemné častioe fosforečnanu močoviny alebo fosforečnanu amonného a tým sa nasycuje extrakčný ťbztok, ktorý je s produktom v pomere 1 : 1 až 1 5. V dalších stupňoch extrakcie sa extrahovadlo (nasýtený vodný roztok fosforečnanu močoviny alebo fosforečnanu amonného) sýti nečistotami, ako močovinové komplexy želežitých solí, taktiež fosforečnými, fluoridovými solfemi a arzénovými sol’ami, V poslednom stupni (pri kontakte horúcioh alebo vychladenýoh kryštálov s extrahovadlom) doohádza v prvom řade k žvlhoovaniu kryštálov.Urea phosphate or ammonium phosphate is prepared by reacting phosphoric acid extractive with urea or ammonia in an aqueous solution. The resulting urea phosphate or ammonium phosphate solution is either spray dried to a spray dryer or is not dewatered in a tumble dryer while crystallizing the product. In both processes, impurities from the phosphoric acid extract, which were dissolved in the phosphoric acid and the phosphoric acid, are located on the surface of the crystals. after reaction with urea they became soluble. The urea phosphate or ammonium phosphate thus obtained is extracted in one step or in a multi-stage, countercurrent saturated aqueous solution of these phosphates. In the first contacting step, steam condensate or pure water is used, which dissolves fine particles of phosphoronate and other soluble impurities as well as fine particles of urea or ammonium phosphate from the surface of the particles, thereby saturating the extraction solution, which is 1: 1 to 1 5. In the next extraction steps, the extractant (saturated aqueous urea or ammonium phosphate solution) is saturated with impurities, such as urea complexes of iron salts, also with phosphorus, fluoride and arsenic salts, in the last step (in contact with hot or cold crystals) with an extractor), the crystals are firstly humidified.

V případe, ak sú přítomné organioké zbytky v kyselino fosforečnéj sa tieto ešte před vlastnou extrakoiou samostatné extrahujú organickým extrahovadlom, ktoré nerozpúšťa fosforečnan močoviny alebo fosforečnan amonný, ale len organioké nečistoty a je ltthko prohavý. Nasýtený roztok, ktorý slúžil ako extrahovadlo po oddělení od kryštálov, resp. čiastočiek v poslednom stupni extrakcie, sa čBalej može spraoovávať cez kysličník křemičitý, připadne jeho iné zlúceniny, čím fluor sa prevedie na fluorokremičitany, upraví sa ekvimolárny poměr kyseliny fosforečnéj a močoviny, alebo čpavku a znova sa vysuší. Vysušené kryštály sa mSžu upravovat’na NP alebo NKP hnojivo, alebo rozpuštěním fosforečnanu močoviny alebo amonného vo vodě sa vráti roztok na extrakciu. Nerozpustné fluorozlúčeniny sa oddelia ako sediment alebo filtračný koláč a dá sa na dtalšie spraoovanie.If there are organic phosphoric acid residues present, they are separately extracted prior to the actual extraction with an organic extract, which does not dissolve urea or ammonium phosphate, but only organic impurities and is very volatile. A saturated solution which served as an extractant after separation from the crystals, respectively. The particles in the final extraction step can be further processed through silica or other compounds thereof, whereupon the fluorine is converted to fluorosilicates, the equimolar ratio of phosphoric acid to urea or ammonia is adjusted and dried again. The dried crystals may be treated to NP or NKP fertilizer, or by dissolving urea or ammonium phosphate in water to return the extraction solution. The insoluble fluoro compounds are separated as a sediment or filter cake and subjected to further treatment.

V prvom stuphi extrakcie sa oddělí produkt, ktorý kvalitou zodpovedá krmnému fosforečnanu močoviny alebo fosforečnanu amonnému. Tento sa po vysušení pod 0,5 hm vody balí a expeduje.In the first extraction step, a product is obtained which is of a quality corresponding to feed urea phosphate or ammonium phosphate. This is packed and shipped after drying under 0.5 wt.

Předložený vynález umožňuje využit kyselinu fosforečná extrakČnú na přípravu krmného fosforečnanu močoviny alebo fosforečnanu amonného s vysokým stupňom účinnosti na využitie fosforečnej zložky. Takéto spraoovanie kyseliny fosforečnej na fosforečnan močoviny je po technologiokej stránke jednoduché, ekonomické a umožňuje v jednom prúde připravit, s vysokou účinnositou na využitie surovin, hotový produkt.The present invention makes it possible to use phosphoric acid extracted for the preparation of feed urea phosphate or ammonium phosphate with a high degree of efficiency for utilizing the phosphorus component. Such processing of phosphoric acid to urea phosphate is technologically simple, economical, and allows the preparation of a finished product in one stream, with high raw material efficiency.

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Příklady provedenia:Examples:

Příklad 1 „Example 1 "

Extrakčná kyselina fosforečná v množstve 14,7 kg/h a obsahom 50 % hm PgO^, 3 % hm kyslioníkov trojmooného Pe a AI, 0,5 hm P a 0,0017 % hm As sa nechá reagovat’s 10,9 kg/h ' 55 % hm.vodného roztoku močoviny. Získáný roztok fosforečnanu močoviny sa vysuší pri teplota 120 °C v rozprešovacej sušiarni na obsah vody 0,5 % hm. Získá sa 16,5 kg/h produktu. Teplý produkt sa v osemstupňovom extraktore protiprúdne extrahuje nasýteným roztokom (vodným roztokom) fosforečnanu močoviny, ktorý vznikol tak, že.sa 1 váhový diel vody zmieša v prvom stupni extraktora s 3 váhovými dielmi tuhého produktu pri teplote 20 °C. Nasýtený roztok (extrahovadld) obsahuje 50 % hm fosforečnanu močoviny a zostáva vyčištěný krystalický fosforečnan močoviny bez oxidov Pe a AI. Obsah P“ poklesol na hodnotu 0,001 % hm a As poklesol na hodnotu 0,0008 % hm. Z prvého stupňa extraktora, po oddělení nasýteného roztoku, sa získá 11,0 kg/h krmného fosforečnanu močoviny s obsahom okolo 3 % hm vody. Po vysušení sa získá 10,6 kg/h produktu s obsahom min.* 17 % hmot. N a 44 % hmot. PgO^, 8o představuje 66 %-účinnosf na výohodziu surovinu. Produkt je krystalický, bielej farby, bez zápachu a tepeltoe stabilný do 60 °C. Extrahovadlo po poslednom stupni extrakcie sa doneutralizuje a vysuší a získá sa cca 6 kg/h NP hnojivá.Extractive phosphoric acid in an amount of 14.7 kg / ha containing 50% by weight of PgO4, 3% by weight of tri-monobasic acid Pe and Al, 0.5% by weight of P and 0.0017% by weight of As is reacted with 10.9 kg / h '55 % by weight aqueous urea solution. The resulting urea phosphate solution is dried at 120 ° C in a spray drier to a water content of 0.5% by weight. 16.5 kg / h of product are obtained. The warm product in the eight-stage extractor is countercurrently extracted with a saturated (aqueous) solution of urea phosphate, which is formed by mixing 1 part by weight of water in the first stage of the extractor with 3 parts by weight of solid product at 20 ° C. The saturated solution (extra-solvent) contains 50 wt% urea phosphate and the purified crystalline urea phosphate is free of Pe and Al oxides. The P 'content decreased to 0.001 wt% and the As decreased to 0.0008 wt%. From the first stage of the extractor, after separation of the saturated solution, 11.0 kg / h of feed urea phosphate containing about 3% by weight of water are obtained. After drying, 10.6 kg / h of product with a minimum content of 17% by weight are obtained. % N and 44 wt. Pg0.880 represents 66% efficacy on raw material convenience. The product is crystalline, white, odorless and thermo-stable up to 60 ° C. The extender after the last extraction stage is neutralized and dried, yielding about 6 kg / h of NP fertilizer.

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Příklad 2 : Extrakčná kyselina fosforečná v množstve 0,147 kg a obsahom 50 % hm Ρ20^, 3 % hm kysličníkov trojmocných kovov, 0,5 % hm P” a 0,0017 % Aš, s prídavkom 0,028 kg vody sa nechá reagovat’ s čpavkom v množstve 0,013 kg. Získá sa roztok s 45,5 %-ným obsahom vody. Po vysušení sa získá 0,089 kg produktu, ktorý sa extrahuje nasýteným vodným roztokom fosforečnanu amonného vo váhovom pomere roztok ! produkt - 1 : 5. Po oddělení roztoku sa získá 0,0885 kg vlhkého produktu s obsahom cca 3 % hm vody. Z tohoto podielu sa 0,02 kg rozpustí na nasýtený roztok a použije sa znova ako extrahovadlo. Vlhký produkt sa potom suší a získá sa 0,0665 kg vyčištěného fosforečnanu amonného s obsahom 12,2 % hmot. N a 61,2 % hmot. P20,j bez P“ a oxidov a obsah As poklesol na 0,0008 % hm. Produkt je krystalický, bielej farby a bez zápachu. Extrahovadlo sa po procese vysuší, doneutralizuje a přidá do NPK hnojív.Example 2: Extraction phosphoric acid in an amount of 0.147 kg and a 50% w Ρ ^ 2 0, 3% by weight of trivalent metal oxides, 0.5% by weight P "and 0.0017%, and, with the addition of 0.028 kg of water is treated with ammonia in an amount of 0,013 kg. A solution is obtained with a water content of 45.5%. After drying, 0.089 kg of product is obtained, which is extracted with a saturated aqueous solution of ammonium phosphate in a solution by weight ratio. product - 1: 5. After separation of the solution, 0.0885 kg of wet product containing about 3% by weight of water is obtained. 0.02 kg of this is dissolved in a saturated solution and reused as an extract. The wet product is then dried to give 0.0665 kg of purified ammonium phosphate containing 12.2 wt. N and 61.2 wt. P 2 O, without P "and oxides, and the As content dropped to 0.0008 wt%. The product is crystalline, white and odorless. The extender is dried after the process, made neutralized and added to the NPK fertilizer.

Claims (1)

SpSsob výroby krmného fosforečnanu močoviny alebo fosforečnanu amonného reakciou extrakčnej kyseliny fosforečnéj s močovinou alebozčpavkom, čistěním a následným sušením pre prmné účely, vyznačujúci sa tým, že vysušený fosforečnan močoviny alebo fosforečnan amonný sa extrahuje nasýteným roztokom uvedenýoh fosforeonanov vo vzájomnom váhovom pomere roztok : produkt - 1 í 3 a pri teplote do 20 6C, pričom matečný lúh sa spraciuje na NP resp, NPK hnojivo a čistý fosforečnan močoviny alebo amonný sa znova suší pri teplote do 140 °C a upravuje sa.The means by the production of feed phosphate, urea or ammonium phosphate by treatment of the extraction of phosphoric acid with urea or ammonia, washing and then drying the prmné purposes, characterized in that the dried urea phosphate, or ammonium phosphate was extracted with saturated uvedenýoh fosforeonanov in a mutual weight ratio of solution: product - 1 s 3 and at 6 to 20 C, the mother liquor was spraciuje the BS respectively, NPK fertilizers and pure urea phosphate and ammonium was again dried at 140 ° C and is adjusted.
CS795477A 1979-08-10 1979-08-10 A method of producing urea or ammonium phosphate feed phosphate CS214520B1 (en)

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