EP3529225A1 - Granulés contenant du sulfate d'ammonium, procédé et installation pour leur production - Google Patents

Granulés contenant du sulfate d'ammonium, procédé et installation pour leur production

Info

Publication number
EP3529225A1
EP3529225A1 EP17784623.5A EP17784623A EP3529225A1 EP 3529225 A1 EP3529225 A1 EP 3529225A1 EP 17784623 A EP17784623 A EP 17784623A EP 3529225 A1 EP3529225 A1 EP 3529225A1
Authority
EP
European Patent Office
Prior art keywords
sulfate
granulation
ammonium sulfate
fluidized bed
fertilizer granules
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Withdrawn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
EP17784623.5A
Other languages
German (de)
English (en)
Inventor
Peter Banik
Dennis BOROWEC
Jens Mathiak
Daniel MIKAUTSCH
Christian RENK
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.)
ThyssenKrupp AG
ThyssenKrupp Industrial Solutions AG
Original Assignee
ThyssenKrupp AG
ThyssenKrupp Industrial Solutions AG
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 ThyssenKrupp AG, ThyssenKrupp Industrial Solutions AG filed Critical ThyssenKrupp AG
Publication of EP3529225A1 publication Critical patent/EP3529225A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C7/00—Fertilisers containing calcium or other cyanamides
    • C05C7/02—Granulation; Pelletisation; Degassing; Hydrating; Hardening; Stabilisation; Oiling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/16—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by suspending the powder material in a gas, e.g. in fluidised beds or as a falling curtain
    • 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
    • C05C3/005—Post-treatment
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G5/00—Fertilisers characterised by their form
    • C05G5/10—Solid or semi-solid fertilisers, e.g. powders
    • C05G5/12—Granules or flakes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D9/00—Chemical paint or ink removers
    • C09D9/02—Chemical paint or ink removers with abrasives
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D9/00—Other inorganic fertilisers
    • C05D9/02—Other inorganic fertilisers containing trace elements

Definitions

  • the present invention relates to an ammonium sulfate-containing fertilizer comprising one or more trace elements in the form of metal salts and at least one further metal salt as granulation aids and to a method for producing a fertilizer granules.
  • Ammonium sulfate finds a variety of uses. For example, ammonium sulfate is used as fertilizer or fertilizer additive. Ammonium sulfate is a source of both nitrogen and sulfur, which are important plant nutrients. There is a lack of sulfur worldwide in many soils, which can be at least partially compensated by the targeted addition of ammonium sulfate.
  • trace elements Plant growth and human health as consumers requires a multitude of trace elements in the form of metal cations. These trace elements can be introduced in a defined concentration in a fertilizer in the form of ammonium sulfate granules and thus made available to the soil, the plants and at the end of the food chain man.
  • Granulation additives this includes all components that make up a small amount, generally ⁇ 5% of the dry matter of the granules, are housed in the fertilizer and have different functions.
  • Granulation aids are understood to mean granulation additives whose function is mainly to improve the granulation capacity of the fertilizer, to reduce the amount of dust and to improve the granule properties (for example pressure resistance, granule structure, surface procurement).
  • ammonium sulfate can be done in various ways.
  • ammonium sulfate can be formed by reaction of ammonia with sulfuric acid.
  • Industrial ammonium sulfate is often crystallized from solutions which are obtained as a by-product, for example, in coal stoves or plants for the production of caprolactam.
  • the crystallization of ammonium sulfate usually produces angular crystals, which usually have a diameter of 1 to 2 mm.
  • Ammonium sulfate is usually not the only component of a fertilizer; rather, fertilizers include combinations of various plant nutrients (such as nitrogen, phosphorus, potassium or sulfur). Ammonium sulfate is therefore often mixed in use with granulated fertilizers to produce a balanced fertilizer mixture.
  • crystalline ammonium sulfate has some disadvantages that make it difficult to incorporate into granulated fertilizer mixtures.
  • the particles of ammonium sulfate formed in the crystallization are relatively small, on the other hand, the particles often vary greatly in size due to abrasion and dust formation. These properties make it difficult to prepare physically homogeneous fertilizer mixtures with ammonium sulfate.
  • a uniform mixing and particle size distribution of the individual components is essential. Too large a width of the particle size distribution can also lead to mechanical problems in the uniform discharge of the fertilizer mixture.
  • Granulated ammonium sulfate is ideally spherical and the individual particles of the granules have, for example, a diameter of 2 to 4 mm. This size is based on the urea granules, which is the world's most widely used fertilizer.
  • US 4 589 904 describes the granulation of ammonium sulfate in a drum granulation with a downstream dryer, wherein the solution preparation is carried out in a Vorneutralisierer.
  • US 2012/0231277 relates to the production of build-up granules by fluidized bed or jet bed granulation. For this granulation (Nuclei), which were previously prepared separately, sprayed with an ammonium sulfate-containing solution and then dried.
  • a problem with the granulation of ammonium sulfate is the formation of dust, which is understood to mean particles with a diameter of less than 0.5 mm. The formation of dust is mainly due to three sources.
  • the nozzles that spray the material to be granulated each produce droplets having a certain distribution of diameters, with some of the finest droplets solidifying before they strike the ammonium sulfate particles, so that the dust so formed leaves the pelletizer with the exhaust air again.
  • the abrasion of the granules due to movements and collisions of the particles is to be mentioned as a dust source, for example in a fluidized bed, wherein the amount of the resulting dust depends significantly on the mechanical properties of the granules.
  • the dust resulting from the mechanical comminution to large granular particles should be mentioned, which is usually transferred directly back into the granulator in the methods and systems according to the prior art.
  • granulation additives are frequently used as granulation aids, which are intended to reduce this dust formation.
  • the addition of these additives causes the granules particles and in particular their surface remain plastic, so that due to their rolling motions and collisions predominantly round particles with a smooth surface and a good mechanical stability are obtained. Therefore, the granules thus obtained has a high pressure and impact resistance, a low tendency to dust formation by abrasion and beyond even a prolonged storage only a slight tendency to clumping.
  • Corresponding granulation additives find their application not only in fluid bed granulation, but also in other processes, such as, for example, prilling or drum granulation. To avoid or reduce the formation of dust, different methods have been described in the prior art.
  • WO 89/04291 A1 describes a process for producing a granulate in which ammonium sulfate is first prepared from ammonia and sulfuric acid in a tubular reactor and a slurry of this ammonium sulfate is applied to a bed of fine-grained recycled ammonium sulfate. It is then granulated in the presence of a granulation aid and the resulting product is dried, sieved and cooled.
  • Conventional rotary granulators can be used for granule production. Aluminum granules may be used as granulation aids.
  • the object of the present invention is to provide an improved ammonium sulfate containing granules available.
  • the solution of this problem provides an inventive granules of the type mentioned above with the features of claim 1.
  • the inventive solution is based on the idea that it is useful due to the potentially harmful effect of aluminum sulfate to reduce the aluminum content in the fertilizer granules by alternative granulation aids are used, while at the same time enriching the fertilizer with additional trace elements that promote plant growth.
  • the granulation additive used is a sulfate of a metal selected from the group comprising Cu, Co and Mo.
  • Containing fertilizer granules according to the invention a copper sulfate as a granulation additive, then this can be used 5 H 2 0, for example, in the form of CuS0 4 ⁇ .
  • a preferred embodiment of the invention provides that the fertilizer granules further contain elemental sulfur and / or a calcium salt.
  • the elemental sulfur and / or the calcium salt are preferably contained as finely ground solid.
  • the fertilizer granules of the invention further contains at least one metal sulfate selected from the group consisting of zinc sulfate, magnesium sulfate, manganese sulfate, iron sulfate or aluminum sulfate, said metal sulfate can also be used in the function as Granulationsangesmittel and wherein it is particularly advantageous that the cation of this Metal sulfate is also suitable as a trace element to promote plant growth and is also important for human nutrition.
  • the granulation additive according to the invention in an amount of 0.5 to 2.5 wt .-% based on the total mass of the dry, granulated product in the granules.
  • At least one metal sulfate selected from the group comprising zinc sulfate, magnesium sulfate, manganese sulfate, iron sulfate or aluminum sulfate in an amount of 0.5 to 2.5 wt .-% based on the total mass of the dry, granulated product in the granules.
  • the total amount of all the aforementioned substances (metal sulfates) used as granulation additives is from 0.5 to 2.5% by weight, based on the total mass of the dry, granulated product in the granules.
  • the present invention further provides a process for producing a fertilizer granulate, in particular of the aforementioned type, by granulation in a fluidized bed granulator, wherein an aqueous composition containing at least the ammonium sulfate and at least one granulation additive and / or granulation aid and / or trace element on a fluidized bed fluidized ammonium sulfate-containing germs is sprayed.
  • a sulfate of a metal selected from the group consisting of Cu, Co, and Mo may be used as a granulation additive in the process of the present invention.
  • at least one metal sulfate selected from the group comprising zinc sulfate, magnesium sulfate, manganese sulfate, iron sulfate or aluminum sulfate may also be used as granulation aids.
  • Granulation aids have proved to be advantageous in experiments in connection with the present invention, in which the aluminum sulphate, which is of concern for the health effects, is partly replaced by iron sulphate.
  • the aluminum sulphate which is of concern for the health effects, is partly replaced by iron sulphate.
  • a considerable proportion of the aluminum sulfate can be replaced by iron sulfate, wherein the advantageous properties of the aluminum sulfate are retained as Granulationsangesmittel, in particular the low tendency to Dust formation, the relatively high granule hardness and high bulk density.
  • Mixtures of iron sulfate and aluminum sulfate proved to be particularly suitable as granulation aids with a proportion of 50% by weight or less of iron sulfate and a proportion of 50% by weight or more of aluminum sulfate.
  • first a first composition comprising at least one granulation additive in aqueous solution and a second composition containing ammonium sulfate in aqueous solution are prepared separately, these two solutions are then mixed together and the solution mixture is sprayed in the fluidized bed granulator.
  • water may for example be supplied to a mixing device to which the aforementioned first composition and / or the aforementioned second composition can be supplied via a separate line.
  • ammonium sulfate as solid to the solution mixture before spraying in order to set a defined concentration and a defined mixing ratio.
  • This solid ammonium sulfate may, for example, be supplied to a mixing device to which the aforementioned first composition and / or the aforementioned second composition can be supplied via a separate conduit.
  • each metal sulfate and the ammonium sulfate separate aqueous solutions, and then combine them to achieve a defined mixing ratio, so that in this
  • three or more aqueous solutions prepared separately and then from these a solution mixture can be prepared, which is sprayed into the fluidized bed granulator.
  • a preferred development of the method according to the invention provides that the aqueous composition is sprayed from below into the fluid bed granulator and / or into the fluidized bed.
  • the aqueous composition is sprayed through nozzles having a spray rate of at least about 150 ml / min per nozzle.
  • Granules preferably comprise particles which are uniformly shaped and of homogeneous composition, their nature and their physical behavior being known to the person skilled in the art.
  • the granules of a granulate can assume different sizes, wherein the width of the particle size distribution is a criterion for the quality of a granulate.
  • the granules according to the invention preferably have a narrow particle size distribution, wherein the largest and smallest particle diameters preferably deviate from one another by at most 10 mm, more preferably at most 8 mm, at most 6 mm, at most 4 mm, at most 3 mm or at most 2 mm.
  • the granules of the invention have a size in the range of 2 to 5 mm, more preferably in the range of 2 to 4.5 mm, even more preferably in the range of 2 to 4 mm and most preferably in the range of 2.5 to 4 mm.
  • a composition comprising the granulation additives and ammonium sulfate is prepared.
  • the composition further comprises water.
  • ammonium sulfate, granulation additives and water are mixed together in a mixing device. Particular preference is given to using a first composition of ammonium sulfate and water and a second composition of granulation additives and water, which are mixed in a corresponding ratio in liquid form.
  • the content of ammonium sulfate in the composition is in the range of 30% by weight to at most the saturated solution about 50% by weight, more preferably in the range of 31 to 49% by weight, in the range of 32 to 48 wt .-%, in the range of 33 to 47 wt .-%, in the range of 34 to 46 wt .-% or in the range of 35 to 45 wt .-%, each based on the total mass of the composition, always below the temperature-dependent crystallization limit.
  • the content of pure granulation additive in the solids fractions of the composition is in the range of 0.5 to 2.5 wt%, more preferably in the range of 0.55 to 2.3 wt%, in the range of 0 , 6 to 2, 1 wt .-%, in the range of 0.65 to 1.9 wt .-%, in the range of 0.7 to 1, 7 wt .-%, in the range of 0.75 to 1, 5 wt .-%, in the range of 0.8 to 1.3 wt .-%, in the range of 0.85 to 1, 2 wt .-% or in the range of 0.9 to 1, 1 wt .-% , in each case based on the total mass of the dry, granulated product.
  • the content of pure granulation additive in the composition is at most 2.5 wt%, more preferably at most 2.3 wt%, at most 2, 1 wt%, at most 1.9 wt% , at most 1.7% by weight, at most 1.5% by weight, at most 1.3% by weight, at most 1.2% by weight, at most 1.1% by weight or at most 1.0 Wt .-%, each based on the total mass of the dry, granulated product.
  • the composition is preferably in the form of a mixture, wherein the mixture may be in the form of a solution, for example.
  • the granulation of the composition can be carried out by customary methods known to the person skilled in the art, for example by means of prilling, drum granulation, crystallization or fluid bed granulation.
  • granulation of the composition in the present invention is by fluid bed granulation.
  • the production of the germs is preferably carried out by drying the solidifying droplets of the composition, but can also be done by abrasion of already existing, already solidified granules. By wetting such granular particles with other droplets, the particles grow and preferably form a homogeneous granules.
  • the granulation is carried out by means of fluid bed granulation, comprising the steps:
  • ammonium sulfate-containing microorganisms are provided.
  • the germs are preferably produced by sieving and / or crushing granulated ammonium sulfate as oversize particles.
  • the germs according to the invention preferably have a narrow size distribution, wherein the largest and the smallest germ diameter preferably differ from each other by more than 4 mm, more preferably at most 2 mm, at most 1 mm or at most 0.5 mm. Methods for determining a germ diameter are known to a person skilled in the art.
  • the diameter of the ammonium sulfate-containing nuclei is in the range of 0.1 to 4.0 mm, more preferably in the range of 0.1 to 2.0 mm and most preferably in the range of 0.5 to 2.0 mm ,
  • the ammonium sulfate-containing seeds are preferably fluidized in a fluidized bed.
  • a fluidized bed is suitable for a large number of process engineering processes for the treatment of solids and liquids, and its structure is known to the person skilled in the art.
  • the fluidized bed according to the invention is preferably formed by the ammonium sulfate-containing nuclei.
  • the fluidized bed is traversed by a fluid.
  • the ammonium sulfate-containing nuclei are preferably caused by an upward flow of the fluid in a fluidized state. This creates a liquid-like state of the germs, which is also known as 'fluidized bed!'
  • the fluid comprises air.
  • the so-called empty tube velocity of the fluid which is used for fluidizing the ammonium sulphate-containing nuclei is preferably in the range of 1-5 m / s, more preferably in the range of 1.5-4.5 m / s, in the range of 2. 4 m / s or in the range of 2.5 - 3.5 m / s.
  • the temperature of the fluidized bed is in the range of 50 ° C to about 120 ° C, more preferably in the range of 60 ° C to 90 ° C, or in the range of 70 ° C to 80 ° C.
  • the fluid is preheated accordingly to adjust the fluidized bed temperature.
  • the composition previously provided as an aqueous solution in the desired mixing ratio is preferably sprayed onto the ammonium sulfate-containing nuclei.
  • the droplets formed during the spraying of the composition preferably pass into the fluidized bed of fluidized, ammonium sulphate-containing germs.
  • the droplets Upon reaching the fluidized bed, the droplets are preferably flowed around from the fluid, preferably from the air, from the bottom up, whereby the fluid causes the droplets to dry and predominantly solidify on the germs, thereby contributing to the growth of the germs.
  • the spraying of the composition is preferably carried out within the fluidized bed, so that the droplets formed during spraying are sprayed from bottom to top in the fluidized bed, whereby the sprayed composition is transferred to the particles in the fluidized bed and dried.
  • spraying of the composition provided as an aqueous solution is effected via nozzles, wherein at least 150 ml of the composition are sprayed via each nozzle per minute, more preferably at least 250 ml per minute, at least 500 ml per minute, at least 1000 ml per minute, at least 1500 ml per minute or at least 2000 ml per minute.
  • air is used to spray the composition.
  • a slight negative pressure prevails in the granulator above the fluidized bed.
  • the reduced pressure is preferably at most 10 mbar, more preferably at most 5 mbar or at most 2 mbar.
  • the flow rate of air used to spray the composition across each nozzle is in the range of 10 to 200m 3 per hour, more preferably in the range of 20 to 180m 3 per hour, in the range of 40 to 160m 3 per hour, in Range of 60 to 140m 3 per hour or in the range of 80 to 120m 3 per hour.
  • the droplets preferably wet the ammonium sulphate-containing nuclei or the already present, already solidified granulate particles, so that they grow uniformly and form a homogeneous granulate.
  • the granules leave the fluidized bed and are preferably transferred to a sorter.
  • Suitable measures for transferring granulate particles from a fluidized bed to another device are known to a person skilled in the art. For example, by using specially designed distribution plates, the granular particles can be added in the fluidized state not only in vertical movement, but also in horizontal movement and thus gradually leave the fluidized bed.
  • At least a portion of the air used for fluidizing is cleaned as exhaust air in a purification step.
  • the air is discharged and fed to the purification stage.
  • the air is purified in the purification step, i. E. especially freed from solid particles and droplets.
  • the cleaning step is a wet scrubber.
  • the granules are divided after their preparation into at least three fractions, wherein
  • fraction (F 2 ) contains particles of a size above the desired target size
  • a fraction (F 3 ) contains particles of a size below the desired target size.
  • fraction (Fi) containing particles having the desired target size is further processed after leaving the fluidized bed or packed as a product.
  • the fraction (F 2 ) containing particles having a size above the desired target size is fed to a comminution device, which is preferably configured to comminute granule particles.
  • a comminution device which is preferably configured to comminute granule particles.
  • the particles of the fraction (F 2 ) are comminuted in the comminution device and the comminuted particles are preferably fed again to the fluidized bed.
  • the fraction (F 3 ) containing particles below the desired target size is returned to the fluidized bed as nuclei for further growth.
  • the finished granules comprise at least 95% by weight of the sprayed amount of ammonium sulfate and granulation aid, more preferably at least 95.5% by weight, at least 96% by weight, more preferably at least 96.5% by weight, at least 97 wt .-%, at least 97.5 wt .-% or at least 98 wt .-%.
  • the amount of ammonium sulfate and granulation aids which do not contribute to the mass of the finished granules and form, for example, dust is at most 10% by weight, more preferably at most 9% by weight, at most 8% by weight, at most 7% by weight .-%, at most 6 wt .-%, at most 5 wt .-%, at most 4 wt .-%, at most 3 wt .-%, at most 2 wt .-% or at most 1 wt .-%, each based on the dry total mass of sprayed ammonium sulfate and granulation additives.
  • Another aspect of the invention relates to a granulate comprising ammonium sulfate and at least one granulation aid and / or trace element, wherein all particles of the granules have a comparable composition and wherein the content of pure granulation aids and / or trace elements in the granules in the range of 0.5 to 2.5 wt .-% is.
  • Comparable composition in the sense of the invention means that the molar amounts of the individual components of the granules according to the invention in the individual granules differ by more than 2% from the average of the molar amounts of the respective component in the total granules, more preferably at most 1, 5% or at most 1%.
  • Methods for determining the molar amounts of a granulate are known to a person skilled in the art.
  • the content of ammonium sulfate in the granules is at least 97.5 wt .-%, more preferably at least 98 wt .-%, at least 98.5 wt .-%, or at least 99 wt .-%, each based on the total mass of the granules.
  • the content of pure granulation additives in the granules is in the range from 0.5 to 2.5% by weight, more preferably in the range from 0.6 to 2% by weight, in the range from 0.7 to 1 , 5 wt .-%, or in the range of 0.8 to 1.0 wt .-%, each based on the total mass of the granules.
  • the granules may optionally comprise further constituents.
  • the particulate composition comprises water as residual moisture.
  • the content of water in the granules is at most 1, 0 wt .-%, more preferably at most 0.8 wt .-%, at most 0.6 wt .-%, at most 0.4 wt .-%, or at most 0.2 Wt .-%, each based on the total mass of the granules.
  • Residual moisture is understood to mean the water content (without water of crystallization, only free moisture) of the granulated fertilizer which remains in the porous structure of the granulate particles even after drying.
  • the residual moisture has an influence on the shelf life of the product and on the formation of possible clumps.
  • a further aspect of the invention relates to a device for producing granules comprising ammonium sulfate, wherein the device comprises the components which are at least temporarily in active connection with one another:
  • (C) a fluid bed granulator configured to produce the granules.
  • the components of the device according to the invention are in operative connection with each other, ie. are connected to each other by suitable piping etc. in a manner which ensures the general functioning of the device.
  • the necessary measures are known to a person skilled in the art.
  • the mixing device according to the invention is preferably configured to produce a composition comprising ammonium sulfate and at least one granulation additive.
  • the structure and operation of such a mixing device are known to a person skilled in the art.
  • the composition which is produced in the mixing device according to the invention is preferably sprayed.
  • the atomization device is disposed within the fluidized bed and sprays the composition from bottom to top of the fluidized bed.
  • the spraying device is configured such that the droplets formed during spraying have a narrow size distribution and are evenly distributed.
  • the fluidized bed is preferably configured to fluidize the ammonium sulfate nuclei and the resulting granule particles.
  • the device comprises the components additionally in operative connection with the device:
  • the partitioning device is preferably arranged downstream of the fluidized bed and configured to divide the granules into fractions of different particle size.
  • those particles which have the desired target size are preferably further processed or packaged after leaving the fluidized bed.
  • Particles with a size above the desired target size, possibly also a small part of the product stream, are preferably fed to a comminuting device and comminuted there.
  • the comminuted particles are again fed to the fluidized bed as nuclei.
  • Particles having a size below the desired target size are again fed to the fluidized bed as nuclei.
  • the purification step is preferably configured to purify the air that has passed through the fluidized bed, i. E. in particular free of solid particles and droplets.
  • the cleaning step is a wet scrubber.
  • the present invention further relates to a plant for producing a fertilizer granules based on ammonium sulfate, in particular according to a method of the aforementioned type comprising a fluidized bed granulator to which process air is supplied via a line and the preferably via a pump, a solution containing ammonium sulfate and granulation additives which is injected via a spray nozzle in the fluidized bed granulator, wherein the system comprises at least two separate containers, wherein a first container receives a first solution containing granulation additives in water and a second container receives a solution containing ammonium sulfate in water, both containers via a line are connected to each other or to another container and at least one of Container or the other container via a line directly or indirectly is in operative connection with the fluidized bed granulator.
  • Figure 1 is a flow diagram of an exemplary granulation plant, which was used to prepare a fertilizer granules of the invention.
  • FIG. 1 shows a flow chart of an exemplary granulation plant, which was used for the production of fertilizer granules according to the invention. It is a so-called fluidized bed granulator 17.
  • the air used for fluidization is sucked from the environment, which then flows via line 18 and via a distributor plate 2 into the process chamber 1. Before entering the process chamber, the air passes through an electric air heater 10.
  • a spray nozzle 3 (external mixing two-fluid nozzle, with a cleaning needle) which is installed in "bottom spray” configuration and the solution in cocurrent to the fluidization air sprayed vertically upward
  • the spray nozzle 3 is supplied via line 20 with compressed air.
  • the spray solution is prepared batchwise in containers 8.
  • Granulation additives are dissolved in a first container 8 a.
  • This first container 8 a the granulation additives are supplied via a line 11.
  • This first container 8 a 12 water is supplied via another line.
  • the ammonium sulfate solution is prepared in a second container 8 b.
  • This second container 8 b is supplied to a connected via a line 12 branch line 13 water and the ammonium sulfate (AS) is added via a further line 14 into the second container 8 a.
  • AS ammonium sulfate
  • the appropriate amount of additive solution from the first container 8 a is metered into the second container 8 b with the AS solution.
  • the solution is homogenized by a stirrer and preheated to the process temperature.
  • the solution is then conveyed via a pump 5 via the line 19 into the fluidized-bed granulator 17.
  • the exhaust air enters an external purification stage 6 and is freed there from discharged particles.
  • After the cleaning stage is a fan 7, so that the entire system in the suction mode (vacuum) is operated.
  • the removed granules are classified by means of a sieving tower 9 into the three fractions oversize (> 4 mm), product (2-4 mm) and undersize ( ⁇ 2 mm).
  • the screened undersize (fine grain) is recycled via lines 15, 16 and added to the granulator together with additional seed material.
  • the entire process is operated and monitored via a programmable logic controller (PLC). All relevant data is displayed in a real-time flowchart on a PC and stored in defined clocking.
  • the regulation of the fluidizing air flow and the air heater power takes place automatically, wherein the desired volume flow and the supply air temperature are specified.
  • the sprayed mass flow is controlled by the pump 5.
  • Granule hardness The hardness of the resulting granules was measured using a Texture Analyzer from Stable Micro Systems Ltd. measured. To determine the granule hardness, granules with a particle size of between 2.5 and 2.8 mm were always used, which were separated from the remaining sample by sieving. From the recorded force-displacement curve, the granule hardness was determined by means of a prescribed macro. The granule hardness is defined as the maximum force [N] that a particle can absorb before it breaks. To increase the statistical reliability, at least 30 particles were measured for each sample selected to measure the granule hardness. From the at least 30 values determined then the mean value, standard deviation and the maximum and minimum values were determined.
  • Particle size distribution To measure the particle size distribution, a so-called "CAMSIZER XT® from Retsch Technology was used, which is based on an optical method. Via a channel, the granules are conveyed to a freefall device. The dispersed particles fall through the measurement plane, where they pass two LED strobe light sources. The shadow projections of the granules are recorded by two digital cameras. The cameras differ in terms of their resolution, so that one camera captures the smaller particles and the other captures the larger particles. The raw data is automatically evaluated by software and the distribution curves are calculated in real time.
  • Residual moisture determination The residual moisture content of all samples was determined. For this purpose, a weighed sample was stored on a small bowl overnight at 100 ° C in a drying oven and the weight of the sample was measured again after drying. Using the following formula, the percentage of residual moisture content (RF), based on the wet sample, can be calculated from the measured values. A duplicate determination was always carried out for each sample.
  • RF residual moisture content
  • trace elements were examined as granulation additives from only one substance, namely copper sulfate pentahydrate, zinc sulfate heptahydrate and iron (II) sulfate Heptahyd rat and also combinations of iron sulfate and aluminum sulfate, in which the aluminum sulfate in different proportions partially was replaced by iron sulfate.
  • the proportions of the additives were always based on sulphate-free sulphates.
  • the hardnesses were within an acceptable range.
  • Residual moisture levels were below 0.5% in most cases.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Fertilizers (AREA)

Abstract

L'invention concerne des granulés d'engrais contenant du sulfate d'ammonium comprenant au moins un sel métallique en tant qu'additif de granulation servant d'oligo-élément et/ou d'auxiliaire de granulation. L'additif de granulation contient un sulfate d'un métal choisi dans le groupe comprenant Cu, Co et Mo. En outre, l'invention concerne un procédé pour produire des granulés d'engrais dans lequel ces granulés d'engrais sont produits par granulation dans un granulateur à lit fluidisé dans lequel une composition aqueuse contenant au moins le sulfate d'ammonium et au moins un additif de granulation est pulvérisée sur un lit fluidisé constitué de germes fluidisés contenant du sulfate d'ammonium. L'auxiliaire de granulation selon l'invention peut en outre contenir au moins un sulfate métallique choisi dans le groupe comprenant le sulfate de zinc, le sulfate de magnésium, le sulfate de manganèse, le sulfate de fer ou le sulfate d'aluminium. Comme on suppose depuis récemment que le sulfate d'aluminium peut-être préjudiciable à la santé, la présente invention tient à ce que le sulfate d'aluminium soit remplacé, au moins partiellement voire totalement, par au minimum un autre auxiliaire de granulation. L'invention concerne donc, pour ce qui est de l'auxiliaire de granulation utilisé, de préférence un sel favorisant la croissance des végétaux et dont le cation est en même temps adapté en tant qu'oligo-élément.
EP17784623.5A 2016-10-20 2017-10-12 Granulés contenant du sulfate d'ammonium, procédé et installation pour leur production Withdrawn EP3529225A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102016220648.6A DE102016220648A1 (de) 2016-10-20 2016-10-20 Ammoniumsulfat enthaltendes Granulat
PCT/EP2017/075998 WO2018073085A1 (fr) 2016-10-20 2017-10-12 Granulés contenant du sulfate d'ammonium, procédé et installation pour leur production

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EP3529225A1 true EP3529225A1 (fr) 2019-08-28

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EP17784623.5A Withdrawn EP3529225A1 (fr) 2016-10-20 2017-10-12 Granulés contenant du sulfate d'ammonium, procédé et installation pour leur production

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US (1) US20190241478A1 (fr)
EP (1) EP3529225A1 (fr)
KR (1) KR20190071762A (fr)
CN (1) CN109890780A (fr)
DE (1) DE102016220648A1 (fr)
TW (1) TW201829333A (fr)
WO (1) WO2018073085A1 (fr)

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US11957126B2 (en) * 2018-08-08 2024-04-16 Kop-Coat, Inc. Granulated agricultural adjuvant and method of making and using same
DE102019112681A1 (de) 2019-05-15 2020-11-19 Taprogge Gmbh Ammoniumsulfat enthaltendes Düngemittel-Granulat sowie Vorrichtung, Verfahren und Stoffgemisch zur dessen Herstellung
IL288660B2 (en) * 2019-09-24 2024-02-01 ICL Europe Cooperatief UA Granules of polyhalite and urea
DE102020130094B3 (de) 2020-11-13 2021-09-02 Taprogge Gesellschaft Mbh Verfahren und Vorrichtung zur Herstellung eines Ammoniumsulfat enthaltenden Düngemittel-Granulats

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TW201829333A (zh) 2018-08-16
CN109890780A (zh) 2019-06-14
WO2018073085A1 (fr) 2018-04-26
DE102016220648A1 (de) 2018-04-26
KR20190071762A (ko) 2019-06-24
US20190241478A1 (en) 2019-08-08

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