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WO2025007163A1 - Procédé de production d'engrais à base de carbamide-soufre - Google Patents

Procédé de production d'engrais à base de carbamide-soufre Download PDF

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Publication number
WO2025007163A1
WO2025007163A1 PCT/UZ2024/050002 UZ2024050002W WO2025007163A1 WO 2025007163 A1 WO2025007163 A1 WO 2025007163A1 UZ 2024050002 W UZ2024050002 W UZ 2024050002W WO 2025007163 A1 WO2025007163 A1 WO 2025007163A1
Authority
WO
WIPO (PCT)
Prior art keywords
sulfur
urea
drum
granules
curtain
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.)
Pending
Application number
PCT/UZ2024/050002
Other languages
English (en)
Russian (ru)
Inventor
Альфит Рафитович БАКИРОВ
Кирилл Викторович ФОМЕНКОВ
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.)
"sulphotech" LLC
Original Assignee
"sulphotech" LLC
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 "sulphotech" LLC filed Critical "sulphotech" LLC
Publication of WO2025007163A1 publication Critical patent/WO2025007163A1/fr
Anticipated expiration legal-status Critical
Pending legal-status Critical Current

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Classifications

    • 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
    • B01J2/12—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in rotating drums
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C9/00—Fertilisers containing urea or urea compounds
    • 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
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/50—Surfactants; Emulsifiers
    • 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

Definitions

  • This utility model relates to agriculture, namely to a method for producing granulated fertilizer containing urea and sulfur.
  • urea is commonly used as a fertilizer to supply plants with nitrogen.
  • fertilizers containing sulfur in the form of a coating on the surface of urea granules are of special interest, since such a structure of fertilizer particles ensures reduced adhesion of granules, slow dissolution of urea in the soil and, accordingly, a reduction in its losses due to leaching from the soil.
  • a method for producing granulated fertilizer containing urea and elemental sulfur in which molten urea is mixed with molten sulfur in the presence of special additives (C6-C30 temperature-resistant fatty acids and their esters). Solid granules are then obtained from the resulting homogeneous phases. The resulting fertilizer granules contain sulfur distributed throughout the granule in a finely dispersed state. The size of sulfur particles is approximately 10-150 ⁇ m and depends on the concentration of additives [RU 2 296 730, C05C 9/00].
  • the urea melt and the sulfur melt are passed through one or more devices for high-intensity mixing at a temperature above the melting temperatures.
  • the pressure drop across said mixing device is at least 200 kPa.
  • the result is fertilizer granules in which the sulfur is distributed throughout the granule volume in a finely dispersed state.
  • the size of the sulfur particles is less than approximately 100 ⁇ m [US 4 330 319, C05C 9/00].
  • a method for producing a granulated fertilizer that contains urea and elemental sulfur by spraying urea and sulfur in a liquid state onto a curtain of bulk material in the volume of a rotating drum, wherein the spraying is carried out in a drum with blades mounted on its inner surface, the sulfur melt and the urea melt or solution are sprayed simultaneously by two separate non-intersecting torches of circular cross-section with diameters approximately equal to half the diameter of the circle formed by the free ends of the drum blades, wherein the spraying of the sulfur melt and the urea melt or solution is carried out along the axis of rotation of the drum in one direction.
  • the invention makes it possible to ensure the distribution of sulfur in the volume of the fertilizer granule in a finely dispersed state without preliminary mixing of the components [RU 2 484 072 Cl, C05C 9/00].
  • the closest technical solution is a method for producing granulated urea coated with sulfur, which involves introducing urea granules into a rotating drum and simultaneously splashing molten sulfur onto the surface of the urea granules in the rotating drum.
  • the temperature of the urea granules introduced into the drum is 20-60°C.
  • the rotating drum is a drum with blades mounted on its inner surface.
  • the rotation speed of the drum is 81-99% of the critical rotation speed. Splashing of molten sulfur is carried out in the direction of the axis of rotation of the drum [RU 2 436 754, C05C 9/00, B05D 1/02, B05D 7/00].
  • the main disadvantage of the prototype is the superficial nature of the coating of the resulting granules, which excludes the possibility of creating composite granules with a structure of embedded fragments in the volume of the granule.
  • Homogenized melt of urea and sulfur is a very unstable system.
  • a stable emulsion of sulfur in urea cannot be obtained by conventional mixing of the melts, since these two melts differ significantly in surface tension and density and thus tend to immediately separate into two separate phases.
  • the claimed method uses an emulsification stage with the introduction of a special additive, such as a surfactant (SAS), which affects the surface tension between the phases of urea and sulfur, which promotes the formation of a homogeneous mixed phase and prevents the resulting emulsion from separating during mixing of the two liquids.
  • SAS surfactant
  • high-intensity ultrasound is used, which supplies a power of 500 W, necessary for liquid dispersion.
  • exploding cavitation bubbles cause the formation of intensely colliding waves in the surrounding liquid and lead to the formation of liquid jets with high speed.
  • SAS surface-active substance
  • Lignosulfonate actually improves droplet destruction at constant energy density.
  • lignosulfonate has a noticeable biostimulating effect, so research is constantly ongoing to develop organic-mineral fertilizers based on it.
  • lignosulfonate in high concentrations is a powerful inhibitor.
  • the molecular structure of lignosulfonate contains a mixture of humic compounds and an admixture of basic binders for their transformation into humic-like molecules.
  • the problem solved by the declared utility model is to improve the technology and expand the range of produced granulated compositions for obtaining fertilizer containing sulfur and urea.
  • the set task is achieved by the fact that in the method for producing carbamide-sulfur compositions in a rotating drum, the carbamide and sulfur melts are preliminarily subjected to emulsification in the ultrasonic treatment mode with subsequent splashing of the emulsified melt onto a movable curtain formed by a packing system of the inner generatrix of the drum at a counter air flow speed within 0.5-5 m/sec.
  • the packing system is made in the form of blades along the inner generatrix of the drum and has a reverse angle of inclination relative to the drum axis.
  • Emulsification is carried out in the presence of surfactants, namely lignosulfonate, at a consumption of 0.4-0.5 mass parts relative to sulfur at the emulsification stage in an ultrasonic disperser.
  • the method can be implemented on any device similar to a drum granulator. More details about the granulator device and the implementation of the technical solution, with a technological scheme for obtaining granules are shown in Fig. 1 and 2.
  • Fig. 1 drum granulator and longitudinal sectional view of the granulator.
  • Fig. 2 flow chart for producing granulated fertilizer.
  • Prilled urea fed through pipe 5, secured in fixed loading chamber 3, enters drum 1, equipped with transport nozzle 2.
  • the blades of nozzle 2 lift and throw out product particles along a parabolic trajectory in the cross-section of the drum with the formation of a dense and uniform curtain of falling product particles.
  • molten sulfur and molten or urea solution are sprayed into the front part of drum 1 onto the formed curtain of falling particles by means of nozzles 7 and 8 along the drum axis in the direction of the unloading chamber with two non-intersecting torches of circular cross-section with diameters approximately equal to half the diameter of the circle formed by the free ends of the blades.
  • drops of molten sulfur and molten or urea solution enter and solidify on the granules.
  • the granules gradually move to the opposite end of the drum 1, from where they enter the unloading chamber 4 and are removed from the apparatus as a finished product through the nozzle 10.
  • Cooling air is supplied through the nozzle 9, which passes through the drum 1 countercurrent to the direction of movement of the hot granules and then through the loading chamber 3 and nozzle 6 goes for cleaning.
  • the granules After moving to the opposite end of the drum 1, the granules enter the classifier 13. Granules of the required size, having reached the end of the classifier, enter the unloading chamber 4 and are removed from the apparatus as a finished product through the nozzle 10.
  • the fine fraction of the product passes through the classifier 13 into the space between the inner 1 and outer 11 drums and is transported by means of the screw 12 to the front part of the outer drum 11 to the receiving windows 14, through which the product enters the inner drum 1 for further build-up in the falling curtain. Due to the rolling in the lower part of the drum 1, the granules acquire a smooth (without pimples) surface.
  • cooling water with a temperature of 22 ⁇ -28°C is supplied to the nozzle 17 of the casing 15 (if necessary).
  • Prilled (granulated) urea is one of the most effective nitrogen fertilizers, contains 46.2% nitrogen in amide form, which makes its use most profitable in agriculture as a fertilizer. Prilled urea granules have a size of 1-4 mm, which distinguishes it from other granulated types of urea with a free ammonia content of 0.03% (GOST 2081-2010. Urea. Technical conditions).
  • Lump sulfur is an allotropic crystalline substance of a light yellow hue. Density is 2.07 g/cm3, melting point is 113°C. It is practically insoluble in water, and when heated, it easily interacts with many substances, with the exception of nitrogen, iodine, gold, platinum, and inert gases. In a finely dispersed state, sulfur is oxidized by atmospheric oxygen to sulfurous and sulfuric acids (GOST 127-1-93. Technical sulfur. Specifications).
  • Bulk material used in the technology of obtaining fertilizer with sulfur and urea may be any known and widely used in agriculture solid bulk fertilizers that require additional saturation with sulfur and urea. At the same time, the applicant does not claim protection of objects included in the scope of the specified feature "bulk material".
  • Emulsification was performed using melts of urea and sulfur in a weight ratio of 15:1.
  • Lump sulfur is fed into sulfur melter 1 (description in Fig. 2 - process flow chart for obtaining granulated fertilizer).
  • the heating and melting of the lump sulfur occurs at a temperature of 120°C.
  • melter 2 with prilled urea at a temperature of 140°C.
  • the sulfur and urea melts obtained in melters 1 and 2 are fed by appropriate pumps 3 into the ultrasonic disperser UZD1-1.6/22 4 with an operating sound frequency of 22 kHz, a power of 500 W at a temperature of 150°C.
  • the disperser produces an emulsion of sulfur in urea.
  • the resulting emulsion is fed into a buffer tank, from where it is fed by a pump for spraying into the nozzle of the drum granulator 5.
  • the emulsion of sulfur in urea is sprayed onto the a curtain of bulk material, which is formed by means of lifting and pouring blades installed inside the drum.
  • the resulting emulsified melt is sprayed onto a moving curtain of material at a counter air flow speed of 0.5 m/sec.
  • the fraction of granules 2-5 mm is a finished product (mixed fertilizer), which is sent for cooling to the fluidized bed cooler.
  • the cooling of granules occurs due to direct contact of materials and atmospheric air supplied to the refrigerator by a fan.
  • the sulfur content in the finished product is 7.6%.
  • the process is carried out similarly to example 1, with the difference that the emulsification was carried out using melts of urea and sulfur in a mass ratio of 10:1, and the resulting emulsified melt was sprayed onto a moving curtain of material at a counter-air flow speed of 0.5 m/sec.
  • the process is carried out similarly to example 1, with the difference that the emulsification was carried out using melts of urea and sulfur in a mass ratio of 6:1, and the resulting emulsified melt was sprayed onto a moving curtain of material at a counter-air flow speed of 0.5 m/sec.
  • Granules with uniform distribution of urea in the granule volume were obtained.
  • the sulfur content in the finished product is 10.2%.
  • Example 4 The process is carried out similarly to example 1, with the difference that lignosulfonate is additionally added to the disperser and melts of urea, sulfur and lignosulfonate are emulsified in mass ratios of 5: 1: 0.4, and the resulting emulsified melt is sprayed onto a moving curtain of material at a counter air flow speed of 0.5 m/sec.
  • the method produced granules with a uniform distribution of components in a narrower range of granulometric composition.
  • the sulfur content in the finished product is 20.7%.
  • the method produced granules with a uniform distribution of components in a narrower range of granulometric composition.
  • the sulfur content in the finished product is 23.1%.
  • the process is carried out similarly to example 1, with the difference that the emulsification was carried out using melts of urea and sulfur and lignosulfonate in mass ratios of 5:1:0.5, and the resulting emulsified melt was sprayed onto a moving curtain of material at a counter-air flow speed of 0.5 m/sec.
  • the method produced granules with a uniform distribution of components in a narrower range of granulometric composition.
  • the sulfur content in the finished product is 24.8%.
  • the method produced granules with a uniform distribution of components in a narrower range of granulometric composition.
  • the sulfur content in the finished product is 25.7%.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Fertilizers (AREA)

Abstract

L'invention se rapporte au domaine de l'agriculture. Le but de l'invention est d'élargir la gamme des composition granulées éjectables. L'invention concerne essentiellement un procédé de production d'engrais granulé contenant du carbamide et du soufre élémentaire, consistant à pulvériser du carbamide et du soufre à l'état liquide sur un rideau de matériau pulvérulent dans le volume d'un tambour rotatif avec des pales disposées sur sa surface interne le long de l'axe du tambour dans une direction; avant la pulvérisation, le soufre et le carbamide fondus sont soumis à une émulsion dans un champ d'ultrasons à une puissance sonore de 500 W et une température de 150°C en présence d'une substance tensio-active consistant en du sulfonate de lignine dans une quantité de 0,4-0,5% de la masse de soufre, et le bain de fusion émulsionné obtenu est pulvérisé sur un rideau mobile du matériau à une vitesse d'un flux d'air à contresens dans les limites de 0,5-5 m/sec.
PCT/UZ2024/050002 2023-06-26 2024-05-18 Procédé de production d'engrais à base de carbamide-soufre Pending WO2025007163A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
UZFA20230231 2023-06-26
UZFAP20230231 2023-06-26

Publications (1)

Publication Number Publication Date
WO2025007163A1 true WO2025007163A1 (fr) 2025-01-02

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ID=93939999

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/UZ2024/050002 Pending WO2025007163A1 (fr) 2023-06-26 2024-05-18 Procédé de production d'engrais à base de carbamide-soufre

Country Status (1)

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WO (1) WO2025007163A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EA201070693A1 (ru) * 2007-12-11 2010-12-30 Сэндвик Материалз Текнолоджи Дойчланд Гмбх Способ и устройство для формирования капель для изготовления таблеток и способ получения серного удобрения
RU2484072C1 (ru) * 2012-01-17 2013-06-10 Открытое Акционерное Общество "Научно-Исследовательский И Проектный Институт Карбамида И Продуктов Органического Синтеза" (Оао Ниик) Способ получения гранулированного удобрения
CN106045687A (zh) * 2016-05-31 2016-10-26 湖北富邦科技股份有限公司 一种新型防结块颗粒肥料的制备方法
WO2017005695A1 (fr) * 2015-07-07 2017-01-12 Yara International Asa Procédé de fabrication de matériau particulaire à base d'urée contenant du soufre élémentaire
RU2757337C1 (ru) * 2018-06-12 2021-10-13 Тиссенкрупп Фертилайзер Текнолоджи Гмбх Форсунка для производства карбамидно-серного удобрения

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EA201070693A1 (ru) * 2007-12-11 2010-12-30 Сэндвик Материалз Текнолоджи Дойчланд Гмбх Способ и устройство для формирования капель для изготовления таблеток и способ получения серного удобрения
RU2484072C1 (ru) * 2012-01-17 2013-06-10 Открытое Акционерное Общество "Научно-Исследовательский И Проектный Институт Карбамида И Продуктов Органического Синтеза" (Оао Ниик) Способ получения гранулированного удобрения
WO2017005695A1 (fr) * 2015-07-07 2017-01-12 Yara International Asa Procédé de fabrication de matériau particulaire à base d'urée contenant du soufre élémentaire
CN106045687A (zh) * 2016-05-31 2016-10-26 湖北富邦科技股份有限公司 一种新型防结块颗粒肥料的制备方法
RU2757337C1 (ru) * 2018-06-12 2021-10-13 Тиссенкрупп Фертилайзер Текнолоджи Гмбх Форсунка для производства карбамидно-серного удобрения

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