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WO2001051429A2 - Procede de production d'une substance fertilisante a base de sulfate d'ammonium et d'uree - Google Patents

Procede de production d'une substance fertilisante a base de sulfate d'ammonium et d'uree Download PDF

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Publication number
WO2001051429A2
WO2001051429A2 PCT/EP2001/000350 EP0100350W WO0151429A2 WO 2001051429 A2 WO2001051429 A2 WO 2001051429A2 EP 0100350 W EP0100350 W EP 0100350W WO 0151429 A2 WO0151429 A2 WO 0151429A2
Authority
WO
WIPO (PCT)
Prior art keywords
urea
ammonium sulfate
ammonia
solution
ammonium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2001/000350
Other languages
German (de)
English (en)
Other versions
WO2001051429A3 (fr
Inventor
Horst Bendix
Wolfgang Kristof
Heinz Lange
Hans-Joachim Wachsmuth
Hans-Dieter Wendt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SKW Stickstoffwerke Piesteritz GmbH
Original Assignee
SKW Stickstoffwerke Piesteritz GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SKW Stickstoffwerke Piesteritz GmbH filed Critical SKW Stickstoffwerke Piesteritz GmbH
Priority to EP01909619A priority Critical patent/EP1248752A2/fr
Priority to AU2001237297A priority patent/AU2001237297A1/en
Publication of WO2001051429A2 publication Critical patent/WO2001051429A2/fr
Publication of WO2001051429A3 publication Critical patent/WO2001051429A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C1/00—Ammonium nitrate fertilisers
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor

Definitions

  • the present invention relates to a method for producing a fertilizer containing ammonium sulfate and urea, by means of which it is possible to produce high-quality nitrogen fertilizers with sulfur contents as required by combining a urea synthesis part with the process-integrated conversion of ammonia and sulfuric acid to ammonium sulfate.
  • Ammonia process produced carbon dioxide (CO2), but has considerable disadvantages.
  • the nitrogen content is extremely low at 17.7%, so that considerable expenses have to be accepted for storage, transport and application. In addition, he already leans
  • urea is characterized by its high nitrogen content, which at 46% is far higher than that of all other bulk fertilizers.
  • the fact that the nitrogen bound in the amide form is hydrolyzed to ammonia and CO2 after its application in the presence of the soil moisture must be regarded as particularly disadvantageous in the case of urea.
  • the crude urea solution is usually stripped at synthesis pressure using ammonia or CO2, which takes about 1.5 to 2 GJ / t of urea to dissolve the ammonium carbamate, desorb the ammonia, evaporate water according to partial pressure and heat for one to apply certain inevitable urea hydrolysis. Basically, about 5 to 10% of the ammonium carbamate remains in the urea solution after this process step, which must be expelled thermally by means of further heat expenditure at lower pressures.
  • the heat recovery from the respective recondensation of the ammonium carbamate is only successful in an exergetically disadvantageous way in the form of low pressure steam or as a loss of cooling water.
  • Ammonia and CO2 are absorbed from the gaseous stream leaving the reactor under high pressure conditions.
  • this process is limited by the enrichment of inert substances up to the explosion area.
  • Even if one tries to counter this by complex measures (reduction of the use of oxygen for the corrosion inhibition of the stripper described above, catalytic separation of the residual hydrogen from the CC> 2 gas of the upstream ammonia system, overstoichiometric use of CO2, explosion-proof design of this absorber) remains in everyone In the case of an ammonia-containing residual gas that has to be cleaned in the low-pressure range to such an extent that no environmental damage occurs when it is emitted.
  • Elemental sulfur is offered both on its own and in combination with a wide variety of mass fertilizers, although it requires a relatively high level of effort to produce the sulfur so finely divided that as is necessary in order to convert it bacterially into the plant physiologically accessible sulfate form in a sufficiently short time after its application.
  • a well-known fertilizer of this kind is the "golden urea" with 40% nitrogen and 10% sulfur.
  • thiosulfates usually ammonium thiosulfate, more rarely potassium thiosulfate, can only be used with liquid fertilization alone or together with other fertilizers such as ammonium nitrate-urea solution (AHL) and are also comparatively expensive even when they are obtained from SO2-containing exhaust gases.
  • AHL ammonium nitrate-urea solution
  • Potassium sulfate with 17 to 18% sulfur as a chlorine-free potash fertilizer will, due to its high price, only be used in the future for special chlorine-sensitive crops and therefore will hardly experience any large increases in volume.
  • Calcium sulphate as gypsum or anhydrite which is obtained in large quantities from the flue gas cleaning of combustion plants or is available from natural sources, has very different opinions about its application properties and the forms of its application. It can therefore be assumed with a high degree of probability that the amount of ammonium sulfate has to be increased considerably in order to cover the sulfur requirement in the future.
  • the sulfur required for this can be covered as a result of increasingly stringent environmental laws and increasing consumption of fossil raw materials from the desulfurization of natural gas, petroleum, petroleum, tar sands and coal, from sulfide processing in metallurgy and, if necessary, from natural sulfur deposits.
  • Ammonium sulfate is also a by-product of caprolactam production and, to a lesser extent, of acrylonitrile production.
  • caprolactam capacities worldwide, the ammonium sulfate volume from this source will decrease steadily in the coming years. Modern processes have already reduced the amount of this by-product by over 50%, and there is already a caprolactam process that works completely without ammonium sulfate. It can therefore be assumed with a high probability that while the sulfur requirement increases and the ammonium sulfate volume decreases as a by-product, the synthetic production of this fertilizer will gain increasing importance as it did decades ago. Then there are no more cost-cutting synergies with his
  • the Austrian patent AT 204 054 claims a process for the production of a fertilizer containing urea and ammonium sulfate, wherein ammonium sulfate is formed in the urea solution in situ by simultaneously forming the formation components for the ammonium sulfate (ammonia and sulfuric acid) in a urea solution at temperatures below 140 ° C or introduces one after the other and drives off the main part of the water contained in the reaction mixture by the heat of neutralization.
  • the resulting, almost solid product can be with a screw conveyor or the like. removed from the reaction vessel and dried if necessary.
  • a disadvantage of this process is that very large amounts of these reactants are required to drive off the bulk of the water from a urea solution by the heat of neutralization of the reaction of sulfuric acid with ammonia, so that the product obtained by the process of AT 204 054 has very high ammonium sulfate contents. These high levels of ammonium sulfate are often unfavorable or undesirable for agricultural use; in particular, only relatively small nitrogen / sulfur nutrient ratios can be set, which is not useful for all soils.
  • the suspension is then processed into solid or liquid fertilizers.
  • the invention further relates to the products obtainable or obtained by such processes.
  • the present invention relates in particular to urea ammonium sulfate granules or prills, wherein at least 85% of the ammonium sulfate crystals contained therein have a size (diameter) of less than 100 ⁇ m, preferably less than 50 ⁇ m, particularly preferably less than 32 ⁇ m.
  • the size of the ammonium sulfate crystals can be determined using well known methods such as fractional sieving using sieves with appropriate meshes, scanning electron microscopic analysis of a representative sample section and analysis of the width and shape of X-ray diffraction reflections.
  • fractional sieving using sieves with appropriate meshes
  • scanning electron microscopic analysis of a representative sample section and analysis of the width and shape of X-ray diffraction reflections.
  • Urea ammonium sulfate granules or prills with the above. Properties can be obtained with the process according to the invention by producing a melt suspension (for example in a conventional evaporator melter) from the urea ammonium sulfate solution or suspension according to the prior art (for example WO 99/65 845) and this is then converted into granules or prills using customary methods.
  • a melt suspension for example in a conventional evaporator melter
  • the urea ammonium sulfate solution or suspension according to the prior art (for example WO 99/65 845) and this is then converted into granules or prills using customary methods.
  • Comminution procedures can be fed to a shaping part (e.g. a device for granulating or for producing prills).
  • a shaping part e.g. a device for granulating or for producing prills.
  • the urea and the ammonium sulfate are extremely finely divided and, moreover, are particularly homogeneously distributed.
  • Such urea ammonium sulfate fertilizers with a freely selectable nitrogen / sulfur nutrient ratio can be produced using conventional industrial processes in which a pure urea solution or melt and solid ammonium sulfate are used
  • the homogeneous distribution and fine particle size of the urea and ammonium sulfate in the solid fertilizers according to the invention is particularly advantageous for nutrient uptake by plants.
  • an aqueous urea ammonium sulfate solution or suspension is first produced by mixing an aqueous Urea solution which, based on the total weight of the solution, contains 0.1 to 50% by weight of free and / or ammonia bound in the form of ammonium carbamate, is reacted with sulfuric acid.
  • the weight ratio ammonium sulfate to urea can be varied within wide limits by the proportions of the starting components.
  • the weight ratio of ammonium sulfate to urea is preferably set to 10:90 to 65:35, in particular 40:60 to 60:40 and particularly preferably 45:55 to 55:45.
  • the concentration of the sulfuric acid used is also not critical, i. H. this can be, for example
  • an aqueous urea solution is used for the ammonium sulfate synthesis which, based on the total weight of the solution, contains 0.1 to 50% by weight of free and / or ammonia carbamate-bound ammonia.
  • the urea content of the aqueous solution is preferably 1 to 60% by weight.
  • Product stream is obtained and which has the corresponding contents of ammonia or ammonium carbamate.
  • the method according to the invention can be easily combined with an existing urea plant, and the previously required and very expensive fine cleaning of the raw urea solution can be dispensed with in the urea process. Due to the savings in investment LO OJ tt HP * o L ⁇ oo
  • FIG. 2 shows a process diagram of a urea plant which has previously only produced urea and is now set up to carry out the method according to the invention. The process is described in more detail in exemplary embodiment 2 below.
  • a urea plant which until now has only produced 1200 t / d of urea, is converted according to FIG. 2 to the production of 2400 t / d of urea ammonium sulfate fertilizer in a weight ratio of 50/50.
  • the urea reactor 28 working at 150 bar and 188 ° C. leaves via line 42 a 65% converted crude urea solution which contains 52100 kg / h urea 38607 kg / h ammonia and 20573 kg / h CO 2 .
  • large parts of the ammonium carbamate and ammonia are freed from the existing stripper 31, which is heated with 22 bar steam and to which 19300 Nm 3 / h CO2 are also fed via line 41, so that a

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

L'invention concerne un procédé permettant de produire une substance fertilisante à base de sulfate d'ammonium et d'urée. Une solution d'urée aqueuse qui contient, par rapport au poids total de la solution, entre 0,1 et 50 % en poids d'ammoniac lié libre et/ou sous forme de carbamate d'ammonium, est mise à réagir avec de l'acide sulfurique et éventuellement de l'ammoniac, dans une plage de températures comprise entre 25 et 250 DEG C et dans une plage de pression de l'ordre de 0,1 à 250 bar, pour donner lieu à une solution ou à une suspension urée-sulfate d'ammonium, dans des quantités permettant de parvenir à un rapport en poids du sulfate d'ammonium à l'urée dans cette solution ou suspension urée-sulfate d'ammonium, de l'ordre de 10 : 90 à 65 : 35. Le CO2 et l'ammoniac expulsés dans ces conditions sont renvoyés dans la synthèse d'urée. Cette solution ou suspension urée-sulfate d'ammonium subit ensuite un traitement ultérieur pour former des substances fertilisantes solides ou liquides. Selon un second aspect, l'invention concerne des granulés d'urée et de sulfate d'ammonium ou des sphérules pouvant être obtenus au moyen dudit procédé et présentant des propriétés d'application technique remarquables.
PCT/EP2001/000350 2000-01-13 2001-01-12 Procede de production d'une substance fertilisante a base de sulfate d'ammonium et d'uree Ceased WO2001051429A2 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP01909619A EP1248752A2 (fr) 2000-01-13 2001-01-12 Procede de production d'une substance fertilisante a base de sulfate d'ammonium et d'uree
AU2001237297A AU2001237297A1 (en) 2000-01-13 2001-01-12 Method for producing a fertilizer containing ammonium sulfate and urea

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10001082.2 2000-01-13
DE2000101082 DE10001082B4 (de) 2000-01-13 2000-01-13 Verfahren zur Herstellung eines Ammoniumsulfat und Harnstoff enthaltenden Düngemittels

Publications (2)

Publication Number Publication Date
WO2001051429A2 true WO2001051429A2 (fr) 2001-07-19
WO2001051429A3 WO2001051429A3 (fr) 2001-12-20

Family

ID=7627345

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2001/000350 Ceased WO2001051429A2 (fr) 2000-01-13 2001-01-12 Procede de production d'une substance fertilisante a base de sulfate d'ammonium et d'uree

Country Status (4)

Country Link
EP (1) EP1248752A2 (fr)
AU (1) AU2001237297A1 (fr)
DE (1) DE10001082B4 (fr)
WO (1) WO2001051429A2 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2373148C2 (ru) * 2005-03-02 2009-11-20 Яра Интернейшнл Аса Трубчатый реактор и установка для производства композиции мочевины и сульфата аммония
US7837758B2 (en) 2004-07-01 2010-11-23 Yara International Asa Method for producing a fertilizer containing urea and ammonium sulphate
WO2011032786A1 (fr) * 2009-09-16 2011-03-24 Dsm Ip Assets B.V. Élimination d'urée et d'ammoniac de gaz d'échappement
US8524165B2 (en) 2005-03-02 2013-09-03 Yara International Asa Pipe reactor and plant for manufacturing of especially urea ammonium sulphate
ITMI20130847A1 (it) * 2013-05-24 2014-11-25 Saipem Spa Metodo e sistema per il recupero di solfato di ammonio da un flusso gassoso di un impianto urea
US9346016B2 (en) 2005-03-09 2016-05-24 Stamicarbon B.V. Process for the preparation of a urea-comprising aqueous stream
WO2019164389A1 (fr) * 2018-02-21 2019-08-29 Newbauer S.A. De C.V. Procédé de création d'un engrais liquide ayant une teneur élevée en azote et conditionné avec du soufre
CN111936233A (zh) * 2018-03-20 2020-11-13 雅苒国际集团 用于生产尿素硫酸铵的方法和反应器

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT204054B (de) 1956-08-03 1959-06-25 Bergwerksgesellschaft Hibernia Verfahren zur Herstellung eines Harnstoff und Ammonsulfat enthaltenden Düngemittels
US3785796A (en) 1972-01-27 1974-01-15 Tennessee Valley Autority Production of urea-ammonium sulfate
EP0289074A1 (fr) 1987-04-16 1988-11-02 Hydro Agri Sluiskil B.V. Procédé de fabrication d'engrais granulés
US4943308A (en) 1985-10-17 1990-07-24 Hydro Agri Sluiskil B.V. Method of producing fertilizer granules containing urea and ammonium sulphate
WO1999065845A1 (fr) 1998-06-15 1999-12-23 Skw Stickstoffwerke Piesteritz Gmbh Procede de preparation d'engrais sous forme de granules contenant de l'uree et du sulfate d'ammonium

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3928015A (en) * 1974-10-29 1975-12-23 Tennessee Valley Authority Manufacture of urea-ammonium sulate from sulfuric acid, ammonia, and urea
US4116664A (en) * 1976-11-04 1978-09-26 Jones Leon R Fertilizer composition and method of making same
US4388101A (en) * 1979-03-14 1983-06-14 Occidental Chemical Agricultural Products, Inc. Non-pressure nitrogen carrier fertilizer solutions and dispersions and process of manufacture
US4310343A (en) * 1979-11-27 1982-01-12 Verdegaal Bros. Fertilizer Process for making liquid fertilizer
US4531962A (en) * 1984-03-12 1985-07-30 Tennessee Valley Authority Production of acid-type fertilizer solutions

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT204054B (de) 1956-08-03 1959-06-25 Bergwerksgesellschaft Hibernia Verfahren zur Herstellung eines Harnstoff und Ammonsulfat enthaltenden Düngemittels
US3785796A (en) 1972-01-27 1974-01-15 Tennessee Valley Autority Production of urea-ammonium sulfate
US4943308A (en) 1985-10-17 1990-07-24 Hydro Agri Sluiskil B.V. Method of producing fertilizer granules containing urea and ammonium sulphate
EP0289074A1 (fr) 1987-04-16 1988-11-02 Hydro Agri Sluiskil B.V. Procédé de fabrication d'engrais granulés
WO1999065845A1 (fr) 1998-06-15 1999-12-23 Skw Stickstoffwerke Piesteritz Gmbh Procede de preparation d'engrais sous forme de granules contenant de l'uree et du sulfate d'ammonium

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7837758B2 (en) 2004-07-01 2010-11-23 Yara International Asa Method for producing a fertilizer containing urea and ammonium sulphate
US8524165B2 (en) 2005-03-02 2013-09-03 Yara International Asa Pipe reactor and plant for manufacturing of especially urea ammonium sulphate
RU2373148C2 (ru) * 2005-03-02 2009-11-20 Яра Интернейшнл Аса Трубчатый реактор и установка для производства композиции мочевины и сульфата аммония
US9346016B2 (en) 2005-03-09 2016-05-24 Stamicarbon B.V. Process for the preparation of a urea-comprising aqueous stream
EA021089B1 (ru) * 2009-09-16 2015-04-30 Стамикарбон Б.В. Удаление мочевины и аммиака из отработанных газов
US9464009B2 (en) 2009-09-16 2016-10-11 Stamicarbon B.V. Removal of urea and ammonia from exhaust gases
EP2477961B2 (fr) † 2009-09-16 2023-12-06 Stamicarbon B.V. Élimination de l'urée et de l'ammoniac de gaz d'échappement
US10640428B2 (en) 2009-09-16 2020-05-05 Stamicarbon B.V. Removal of urea and ammonia from exhaust gases
EP2301917A1 (fr) * 2009-09-16 2011-03-30 Stamicarbon B.V. Élimination de l'urée et de l'ammoniac de gaz d'échappement
EP2477961B1 (fr) 2009-09-16 2016-04-20 Stamicarbon B.V. Élimination de l'urée et de l'ammoniac de gaz d'échappement
WO2011032786A1 (fr) * 2009-09-16 2011-03-24 Dsm Ip Assets B.V. Élimination d'urée et d'ammoniac de gaz d'échappement
CN102596901A (zh) * 2009-09-16 2012-07-18 斯塔米卡邦有限公司 从废气中去除尿素和氨的方法
US9556077B2 (en) 2009-09-16 2017-01-31 Stamicarbon B.V. Removal of urea and ammonia from exhaust gases
WO2014188371A1 (fr) * 2013-05-24 2014-11-27 Saipem S.P.A. Procédé et système de récupération de sulfate d'ammonium dans un flux gazeux d'usine d'urée
ITMI20130847A1 (it) * 2013-05-24 2014-11-25 Saipem Spa Metodo e sistema per il recupero di solfato di ammonio da un flusso gassoso di un impianto urea
WO2019164389A1 (fr) * 2018-02-21 2019-08-29 Newbauer S.A. De C.V. Procédé de création d'un engrais liquide ayant une teneur élevée en azote et conditionné avec du soufre
CN111936233A (zh) * 2018-03-20 2020-11-13 雅苒国际集团 用于生产尿素硫酸铵的方法和反应器
CN111936233B (zh) * 2018-03-20 2023-09-01 雅苒国际集团 用于生产尿素硫酸铵的方法和反应器
US11993557B2 (en) 2018-03-20 2024-05-28 Yara International Asa Method and reactor for producing urea ammonium sulphate

Also Published As

Publication number Publication date
DE10001082A1 (de) 2001-08-02
EP1248752A2 (fr) 2002-10-16
AU2001237297A1 (en) 2001-07-24
DE10001082B4 (de) 2004-11-18
WO2001051429A3 (fr) 2001-12-20

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