EP1094997A1 - Procede de preparation d'engrais sous forme de granules contenant de l'uree et du sulfate d'ammonium - Google Patents

Procede de preparation d'engrais sous forme de granules contenant de l'uree et du sulfate d'ammonium

Info

Publication number
EP1094997A1
EP1094997A1 EP99931067A EP99931067A EP1094997A1 EP 1094997 A1 EP1094997 A1 EP 1094997A1 EP 99931067 A EP99931067 A EP 99931067A EP 99931067 A EP99931067 A EP 99931067A EP 1094997 A1 EP1094997 A1 EP 1094997A1
Authority
EP
European Patent Office
Prior art keywords
ammonium sulfate
urea
fluidized bed
melt
grain
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.)
Withdrawn
Application number
EP99931067A
Other languages
German (de)
English (en)
Inventor
Horst Bendix
Heinz Lange
Klaus SCHÜBEL
Hans-Joachim Wachsmuth
Tetsuzo Honda
Eiji Sakata
Genshi Nishikawa
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
Publication of EP1094997A1 publication Critical patent/EP1094997A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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

  • ammonium sulfate melts at over 500 ° C, so that granulation from a mixture melt with high ammonium sulfate contents is excluded. Only up to about 20% by weight of ammonium sulfate is soluble in a urea melt at conventional melt temperatures and can therefore be granulated homogeneously.
  • US Pat. No. 3,785,796 discloses a process for producing ammonium sulfate-urea granules, with which it is in principle possible to produce granules with an ammonium sulfate content of 30 to 70% by weight.
  • Commercially available, unmilled ammonium sulfate is mixed with a urea melt and granulated in an "oil" or "plate” granulator, the corresponding slurry being dripped on. Both types of granulator have the advantage that they work virtually dust-free, so that dust recycling can be omitted.
  • a disadvantage of this process is the fact that the granules are of poor quality due to their inhomogeneous structure due to the granulation process.
  • the ammonium sulfate particles must therefore be ground very finely so that they are sufficiently wetted with liquid and non-solid ammonium sulfate particles due to the difference in density to the urea solution from the drop to solve.
  • the present invention was therefore based on the object of producing a process for producing fertilizer granules containing urea and ammonium sulfate with an ammonium sulfate content of von 60% by weight, which does not have the disadvantages mentioned according to the prior art, but enables the production of homogeneous urea-ammonium sulfate granules with a relatively high proportion of ammonium sulfate, which has good application properties and at the same time can be produced with little technical effort and inexpensively.
  • melt suspension comprising ammonium sulfate with an average particle size of 30 to 300 microns and urea in one
  • melt suspension formed in stage a) is sprayed onto f one-piece ammonium sulfate-urea particles from below in a fluidized bed granulator with the aid of at least one nozzle, the
  • Fluid bed is loosened by a gas, in particular a bubbling air stream in the area of the injection point and then c) the fertilizer granulate formed in the fluid bed is separated off and possibly worked up.
  • the process according to the present invention thus comprises at least three reaction stages.
  • a melt suspension comprising ammonium sulfate and urea is produced in a temperature range from 120 to 15 ° C., the ammonium sulfate having an average particle size of 30 to 300 ⁇ m.
  • the mean particle size is the mean particle size determined with the aid of the sieve analysis.
  • the concentration range in which ammonium sulfate can be added to the urea melt depends on the ammonium sulfate particle size and decreases with decreasing particle size due to increases in viscosity.
  • ammonium sulfate and urea-containing melt suspension are unproblematic and can be done in various ways.
  • preheated ammonium sulfate can be introduced into a urea melt at a preferred temperature of 100 to 150 ° C. and then dispersed.
  • the ammonium sulfate has a preferred average particle size of 60 to 150 ⁇ m and the urea melt, in particular a concentration of> 98% by weight.
  • ammonium sulfate and urea-containing melt suspension consists in introducing coarse-grained and preheated ammonium sulfate with a preferred temperature of 100 to 150 ° C into the corresponding urea melt, the resulting melt suspension using a wet mill to the average particle size of 30 to 300 ⁇ m, preferably 60 to 1 50 ⁇ m, milled and then dispersed.
  • the coarse-grained ammonium sulfate preferably has an average particle size of 0.1 to 2.0 mm.
  • the ammonium sulfate in stage a) is introduced into the urea melt by a highly turbulent dispersion. Due to this highly turbulent dispersion, Introducing kinetic energy with the aid of the usual dispersants, the viscosity of the ammonium sulfate-urea melt suspension can be reduced to ⁇ 1 50 cP and, even at high solids contents, kept sufficiently low until atomization. In general, a ratio of ammonium sulfate / urea in the melt suspension according to a) from 45/55 to 55/45 is preferred.
  • the melt suspension formed in stage a) is then injected with the aid of a nozzle from below into a fluidized bed granulator onto f-piece ammonium sulfate-urea particles, which preferably have an average particle size of 1.0 to 3.0 mm exhibit.
  • Such finely divided ammonium sulfate-urea particles are preferably composed of the return of undersize and comminuted oversize of the granulator product which is customary in granulation.
  • the maximum moistening, at which no agglomerates are formed, depends not only on the material properties of the melt suspension, but also on the type of nozzle, its spray pattern and the design of the fluidized bed. Therefore, full cone nozzles with a spray angle of 45 to 90 °, preferably 60, are preferred up to 80 °.
  • the nozzles, in particular single-substance nozzles, are preferably charged with 100 to 1,000 kg / h of the melt suspension.
  • the height of the fluidized bed in the fluidized bed granulator can be varied within wide limits, but it has proven to be particularly advantageous to set fluidized bed heights of 300 to 600 mm. Fluid bed heights of ⁇ 300 mm reduce the agglomeration rate, but there is a risk of drops blowing through the fluid bed, which leads to a higher dust accumulation in the granulator. With fluidized bed heights> 600 mm there is a risk that the upper layers will no longer be sprayed on and thus only unnecessarily energy will be used to compress the fluidized air.
  • the fluidized bed is loosened by a gas stream, in particular a bubbling air stream, in the region of the injection point without atomizing the melt suspension drops.
  • a gas stream in particular a bubbling air stream
  • This loosening effect is preferably achieved in that the melt nozzles are enveloped by the gas stream, in particular the bubbling air stream, which is preferably 0.75 to 1.5 times
  • Nm 3 denotes a normal cubic meter, i.e. a cubic meter under normal conditions.
  • the fertilizer granules formed in the fluidized bed are separated off and possibly worked up.
  • the fertilizer granulate is separated into three grain fractions with the usual devices, namely into the fine grain with a particle size ⁇ 1.0 mm, in particular ⁇ 1.6 mm, the good grain with a particle size of 1.0 to 5.0 mm, especially 1.6 up to 5.0 mm as well as the coarse grain with a particle size> 5 mm.
  • the fine grain is recycled into the fluidized bed reactor in step b), this fine grain preferably being returned to the fluidized bed reactor below the upper edge of the fluidized bed.
  • the coarse grain can optionally be ground with a part of the good grain to a preferred average particle size of 1.0 to 3.0 mm and, like the fine grain, can be returned to the fluidized bed granulator.
  • the good grain in particular with the preferred particle size of 1.6 to 5.0 mm, can be subjected to a final hydrophobic treatment by customary methods and can be marketed as a salable product in this form. Such hydrophobization can be carried out, for example, with oil / paraffin.
  • this problem can be solved by separating the dust formed in granulation stage b) by dry separation, for example with the aid of cyclones or conventional dust filters, into a fine-grain ammonium sulfate-poor and coarse-grain ammonium sulfate-rich fraction.
  • the low-ammonium sulfate fraction with an ammonium sulfate content of preferably ⁇ 60% by weight and a preferred grain size of ⁇ 50 ⁇ m is preferably separated with the aid of wet washing and discharged from the process.
  • the ammonium sulfate-rich coarse-grained dust fraction with an ammonium sulfate content of preferably> 60% by weight and a particle size of> 50 ⁇ m is either returned directly to the fluidized bed of the granulator and / or after wet grinding of the coarse-grained ammonium sulfate particles to an average particle size of preferably 30 to 300 ⁇ m, in particular 60 to 1 50 / m, combined with the urea-ammonium sulfate melt suspension before the granulation stage b).
  • the ammonium sulfate-rich, ground dust fraction is mixed into the urea-ammonium sulfate melt suspension in the storage container for the atomization.
  • the process according to the invention proves to be particularly advantageous if part of the ammonium sulfate-rich dust fraction is returned to the fluidized bed granulator and at the same time the other part of this dust fraction is ground and dispersed together with the melt suspension. In this way, the grain size of the granulate can be optimally controlled without the need to comminute good grain. It also significantly reduces the proportion of dust that has to be returned, so that the ammonium sulfate concentration in the melt suspension does not increase by more than 3% by weight compared to the ammonium sulfate concentration in the product.
  • homogeneous urea ammonium sulfate granules with a particle size of 1.0 to 5.0 mm, preferably 1.6 to 5.0 mm and an ammonium sulfate content of up to can be obtained in a technically simple and therefore inexpensive manner 60% by weight, preferably up to 55% by weight and at least 30% by weight, preferably at least 4 5% by weight. -%, s o w i e g u t e n L a g e r - and production characteristics. Since it also works in an environmentally friendly manner due to a possible dust recirculation, it is particularly suitable for implementation on a technical scale.
  • homogeneous urea-ammonium sulfate granules with an ammonium sulfate content of 30 to 60% by weight can be produced without problems, the grain size of the granules being able to be adjusted in a targeted manner and the dust emissions during granulation being reduced to a minimum.
  • This ammonium sulfate-urea melt suspension is fed via line 5 directly into the pump reservoir 6 and from there by means of a pump 8 via the pipeline 9 to the nozzle 10.
  • a pressure of 3.5 bar is set by means of the pressure control valve 7.
  • a single-component nozzle 10 sprays 875 kg / h of the melt suspension into the fluidized bed of the granulator 11.
  • the full cone nozzle 1 0 produces an average drop diameter of 370 ⁇ m at a spray angle of 61 °.
  • the nozzle is located at the level of the sieve base on which the fluidized bed is built and sprays from below into the bed, which has a height of 350 mm, at a speed of 29 m / s.
  • the fluidized bed is generated by an empty pipe speed of 1.8 m / s.
  • the nozzle 10 is located in a bubble air tube 1 3, where 900 Nm 3 / h bubble air are blown in via line 14 at a speed of 20 m / s in order to loosen up the fluidized bed at the injection point.
  • the granules with an average diameter of 3.2 mm are drawn off via chute 15 and fed to the sieve 16, where the product is separated into three fractions. 350 kg / h of fine product ⁇ 2.5 mm are recycled into the granulator 11 via the conveying path 17 as below the upper edge of the fluidized bed and form the fluidized bed.
  • the waste air obtained in the granulator 11 comes via channel 22 into the cyclone 23, where 60 kg / h of dust with a concentration of 82% by weight of ammonium sulfate are separated off. From the cyclone exhaust air 5 kg / h of dust with an ammonium sulfate concentration of 60% by weight and a grain size ⁇ 60 ⁇ m pass through line 24 into a wet scrubber (not shown).
  • the dust separated in the cyclone is fed via the conveyor section 25 into the wet mill 26, where the ammonium sulfate particles in the ammonium sulfate-urea melt suspension circulated via line 27 are ground in a highly turbulent manner to an average diameter of 100 ⁇ m.
  • the highly concentrated ammonium sulfate-urea melt suspension reaches the storage container 6 via pipeline 28.
  • Example 2 proceeds as described in Example 1, except that part of the highly concentrated ammonium sulfate dust deposited in the cyclone 23 is 250 mm below the upper edge of the fluidized bed is introduced. Of the 60 kg / h of ammonium sulfate-rich dust separated in the cyclone 23, 20 kg / h are introduced directly into the granulator 11. As a result, the average particle size of the granules produced drops from 3.8 to 3.4 mm and the supply of 20 kg / h of good grain from the crusher 20 is eliminated. The amount of dust fed to the wet mill 26 is reduced to 40 kg / h, so that only 855 kg / h of melt suspension have to be atomized. The ammonium sulfate content of the melt suspension which is conveyed to the nozzles is reduced from 52.8% to 52.2% by weight.
  • ammonium sulfate crystals 507 kg / h of commercially available ammonium sulfate crystals (particle size 0.1 to 1.0 mm) are fed via line 1 to pin mill 2 and ground there to an average particle size of 95 ⁇ m.
  • the ammonium sulfate particles reach the heating screw 4 via line 3, where they are heated to 1,35 ° C. by means of steam from line 5.
  • the ammonium sulfate particles reaching the mixer 8 via the pipeline 6 are mixed with 504 kg / h urea prills, which are fed in via the line 7.
  • the solid urea melts in the presence of ammonium sulfate by supplying heat to the mixer.
  • the melt suspension with a temperature of 1 30 ° C is withdrawn via pipe 9 from the pump 10 and conveyed via line 1 1 to the disperser 1 2, where the viscosity is reduced to 100 cP by introducing shear forces between stationary and rotating pins, so that the melt suspension becomes fluid.
  • the melt suspension passes through the pipes 1 5a and 1 5b to two full cone nozzles 1 7 and 1 8, each with a capacity of 505.5 kg / h.
  • pressure control valve 1 3 in line 14 By means of pressure control valve 1 3 in line 14, a pre-pressure of 3 bar set.
  • the nozzles 1 7 and 1 8 spray the melt suspension with a spray angle of 70 ° into the fluidized bed of the granulator 1 9 at a speed of 29 m / s (measured at a distance of 1 0 cm from the nozzle outlet opening), droplets having an average diameter of 41 0 ⁇ m arise.
  • the drops are injected from below into a fluidized bed, which is 450 mm above the nozzles.
  • the fluidized bed is generated at an empty pipe speed of 1.9 m / s.
  • the nozzles 1 7 and 1 8 are located in bubbling air pipes 21 and 22, where 550 Nm 3 / h of bubbling air are blown in via the pipe 1 6 at an empty pipe speed of 28 m / s, around the nozzles, at the points where there are nozzles to loosen the fluidized bed.
  • the finished granulate is discharged via the centrally arranged discharge line 23. Air is blown into this discharge line via line 24 and discharged with an air quantity of 560 Nm 3 / h of granules with an average particle size of 3.0 mm.
  • the granulate passes through the rotary valve 25 and the chute 26 to the sieve 27, where the product is separated into three fractions.
  • 80 kg / h of fine product ⁇ 1 mm returns to the granulator 19 via the conveying path 28.
  • 40 kg / h of coarse grain> 5 mm is fed via line 29 to the roller crusher 30 and broken there to an average diameter of 2 mm. The broken product returns to the granulator 19 via lines 31 and 28 and forms the fluidized bed here.
  • the finished product (1 001 kg / h) arrives via pipe 32 from the plant with an ammonium sulfate content of 50% by weight and is stored with an oil / paraffin mixture after it has been made hydrophobic.
  • the exhaust air obtained in the granulator 1 9 reaches the bag filter 34 via pipe 33, where dust particles> 50 ⁇ m are separated.
  • 1,50 kg / h of dust with a concentration of 85% by weight of ammonium sulfate are piped in 35 250 mm below the upper edge of the fluidized bed returned the granulator 19.
  • 10 kg / h of dust ⁇ 50 microns with a concentration of 60 wt .-% ammonium sulfate emits from the bag filter 34 via line 36 or is led to the wet wash, not shown.

Landscapes

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

Abstract

L'invention concerne un procédé permettant de préparer des engrais sous forme de granulés contenant de l'urée et du sulfate d'ammonium, à une concentration en sulfate d'ammonium </=60 % en poids. Selon ce procédé, a) on prépare une suspension de matière fondue à base de sulfate d'ammonium de grandeur particulaire moyenne comprise entre 30 et 300 mu m et d'urée, à une température comprise entre 120 et 155 DEG C; b) la suspension de matière fondue obtenue à l'étape a) est ensuite diffusée depuis le bas à l'aide d'au moins une buse, dans un granulateur à lit fluidisé sur des particules de sulfate d'ammonium et d'urée, le lit fluidisé est ramolli par un flux d'air tourbillonnant dans la zone du point d'injection; puis c) les engrais sous forme de granulés formés dans le lit fluidisé sont séparés et éventuellement traités. Ce procédé permet de préparer aisément des engrais sous forme de granulés homogènes, à base d'urée et de sulfate d'ammonium, avec une teneur en sulfate d'ammonium comprise entre 30 et 60 % en poids. La grosseur granulaire des granulés peut être ajustée de manière ciblée et les émissions de poussières intervenant au cours de la granulation peuvent être réduites à un minimum.
EP99931067A 1998-06-15 1999-06-14 Procede de preparation d'engrais sous forme de granules contenant de l'uree et du sulfate d'ammonium Withdrawn EP1094997A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19826570A DE19826570C2 (de) 1998-06-15 1998-06-15 Verfahren zur Herstellung von Harnstoff und Ammonsulfat enthaltenden Düngemittel-Granulaten
DE19826570 1998-06-15
PCT/EP1999/004094 WO1999065845A1 (fr) 1998-06-15 1999-06-14 Procede de preparation d'engrais sous forme de granules contenant de l'uree et du sulfate d'ammonium

Publications (1)

Publication Number Publication Date
EP1094997A1 true EP1094997A1 (fr) 2001-05-02

Family

ID=7870912

Family Applications (1)

Application Number Title Priority Date Filing Date
EP99931067A Withdrawn EP1094997A1 (fr) 1998-06-15 1999-06-14 Procede de preparation d'engrais sous forme de granules contenant de l'uree et du sulfate d'ammonium

Country Status (10)

Country Link
US (1) US6179893B1 (fr)
EP (1) EP1094997A1 (fr)
JP (1) JP4459326B2 (fr)
BG (1) BG105040A (fr)
CZ (1) CZ20004733A3 (fr)
DE (1) DE19826570C2 (fr)
EE (1) EE200000753A (fr)
NO (1) NO20006283L (fr)
PL (1) PL344857A1 (fr)
WO (1) WO1999065845A1 (fr)

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JP2002306944A (ja) * 2001-04-12 2002-10-22 Okawara Mfg Co Ltd 造粒乾燥方法並びに流動層造粒乾燥装置
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NL1025954C2 (nl) * 2004-04-15 2005-10-18 Dsm Ip Assets Bv Werkwijze voor het optimaliseren van een fluïdbed granulator.
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EP1868963B1 (fr) * 2005-04-18 2017-05-10 Stamicarbon B.V. Procede de production de particules comprenant de l'uree
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EP2253374A1 (fr) 2009-05-20 2010-11-24 Stamicarbon B.V. Procédé de production de granulés
JP5399276B2 (ja) * 2010-01-19 2014-01-29 日本電信電話株式会社 コンテンツ配信システムと方法およびプログラム
EP2431346A1 (fr) * 2010-09-15 2012-03-21 Uhde Fertilizer Technology B.V. Procédé de production d'engrais d'urée avec des faibles tendances d'absorption d'humidité
AU2012290064B2 (en) 2011-08-04 2017-08-17 Mos Holdings Inc. Compacted muriate of potash fertilizers containing micronutrients and methods of making same
CN102887777A (zh) * 2012-10-25 2013-01-23 新疆禾稼欢肥业科技有限责任公司 多肽氮肥
CN105102401B (zh) * 2013-03-14 2021-09-28 美盛农资（北京）有限公司 肥料组合物及其制备方法
US9174885B2 (en) 2013-03-15 2015-11-03 University Of Kentucky Research Foundation Nitrogen fertilizer composition and method to improve detection and lessen the explosive potential of nitrogen-based fertilizers
CN104072260B (zh) * 2014-05-29 2016-06-22 苏州上研化肥科技发展有限公司 一种生产复合肥料的生产系统
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US10330654B2 (en) * 2014-07-20 2019-06-25 Sabic Global Technologies B.V. Methods for determining low sulfate concentrations in synthetic urea samples, produced in a manufacturing process and containing high levels of impurities
GEP20207124B (en) * 2015-07-06 2020-06-25 Stamicarbon Granulation of urea products
MA42900A (fr) * 2015-07-07 2018-05-16 Yara Int Asa Procédé de fabrication de matériau particulaire à base d'urée contenant du soufre élémentaire
ES2822576T3 (es) 2015-09-08 2021-05-04 Yara Int Asa Composición mejorada a base de sulfato de amonio y urea y método para su fabricación
JOP20190228A1 (ar) 2017-03-31 2019-09-30 Mosaic Co أسمدة تحتوي على مصادر سريعة و بطيئة لاطلاق البورون
EP3461803A1 (fr) * 2017-10-02 2019-04-03 Evonik Degussa GmbH Procédé de fabrication pour granules contenant du dipeptide
EP3542899A1 (fr) * 2018-03-20 2019-09-25 Yara International ASA Procédé et réacteur pour produire du sulfate d'ammonium d'urée
EP3768416B1 (fr) * 2018-03-23 2022-11-09 thyssenkrupp Fertilizer Technology GmbH Systeme de granulation a lit fluidise avec matériau de revêtement pour empêcher l'accumulation de poussière dans des systèmes pneumatiques d'installations de granulation d'urée
EP3567018A1 (fr) 2018-05-07 2019-11-13 Yara International ASA Composition améliorée à base de sulfate d'ammonium d'urée et son procédé de fabrication
EP3567019A1 (fr) 2018-05-09 2019-11-13 Yara International ASA Composition de mélange améliorée à base d'urée et son procédé de fabrication
EP3567020A1 (fr) 2018-05-11 2019-11-13 Yara International ASA Composition améliorée à base d'urée comprenant du soufre élémentaire et son procédé de fabrication
EP3593898B1 (fr) * 2018-07-13 2021-09-01 thyssenkrupp Fertilizer Technology GmbH Production de granulés de fertilisant ayant une distribution de taille définie
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EP3907208A1 (fr) 2020-05-08 2021-11-10 Yara International ASA Composition à base de sulfate d'ammonium et d'urée
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Also Published As

Publication number Publication date
NO20006283L (no) 2001-02-12
PL344857A1 (en) 2001-11-19
DE19826570A1 (de) 1999-12-23
CZ20004733A3 (cs) 2002-01-16
WO1999065845A1 (fr) 1999-12-23
EE200000753A (et) 2002-04-15
BG105040A (bg) 2001-07-31
US6179893B1 (en) 2001-01-30
JP4459326B2 (ja) 2010-04-28
DE19826570C2 (de) 2002-10-31
JP2000044371A (ja) 2000-02-15
NO20006283D0 (no) 2000-12-11

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