• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
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  • 优先权
    • 专利摘要:
    A METHOD FOR THE PRODUCTION OF UREA GRANULES WITH LOW MOISTURE ABSORPTION CAPACITY AND UREA GRANULES. A method for the production of urea granules with low unit absorption capacity, with a urea granulator, which has an inlet side of the flow of granules and opposite an outflow side of the flow of granules, which forms an axis to the over which the urea granules are formed from a urea solution and a urea / ammonium salt stream, in which the urea solution and the urea / ammonium salt stream are sprayed as a mixture or separately, via a feed system unit by means of several nozzles, in the urea granulator on a source material. In this process, the largest amount of the urea / ammonium salt stream is sprayed into the urea granulator at the inlet side of the granule stream, and the amount of the urea / ammonium salt stream is reduced along the granulator axis. of urea from the inlet side of the granule flow to the outlet side (...).
    公开号:BR112013005875B1
    申请号:R112013005875-7
    申请日:2011-08-31
    公开日:2020-10-13
    发明作者:Paul Niehues；Harald Franzrahe；Matthias Potthoff；Luc Albert Vanmarcke
    申请人:Uhde Fertilizer Technology B.V.；
    IPC主号:
    专利说明:

    [001] The invention relates to a urea granulation process and to the urea granule produced by the process. The invention integrates a method for recycling ammonia salts that are currently sent to other processes, for example, to the UAN or NPK processes, or to a conventional urea production process. The ammonia salts are homogeneously mixed in the urea granulator in the present invention, so that the urea fertilizer shows tendencies towards low moisture absorption.
    [002] In a urea equipment, the air used that leaves a urea granulator equipped with a fluidized bed, contains, in addition to the urea powder, also ammonia. This ammonia contamination must be eliminated before the flow of gaseous effluents can be vented into the atmosphere.
    [003] The removal of ammonia from a stream of gaseous effluents is a well-known technology, as described in EP1695755A1, for example. Normally, the flow of gaseous effluents is treated with an acidic washing solution. Such a washing solution can be easily manufactured by adding an acid, such as nitric acid or sulfuric acid in water. The ammonia is removed from the gas stream by chemical absorption and is converted to the corresponding ammonium salt. The use of nitric acid produces ammonium nitrate (NA), and the use of sulfuric acid produces ammonium sulfate (SA), respectively.
    [004] In such processes a purge solution is produced, which contains a low concentration of ammonium salt and a high concentration of urea. These solutions can either be discharged from the equipment or, being more favorable, added to the urea melted by the synthesis and granulated in a typical urea granulation equipment. Product specification and quality are not influenced to a large extent by the addition of these small amounts of ammonium salts. The N content of the urea product is still above 46% N, so the product is still a typical urea-based fertilizer.
    [005] However, there is a significant disadvantage when mixing urea and an ammonium salt which is the significant reduction in the critical relative humidity of the resulting product.
    [006] The critical relative humidity (HCR) of a salt is defined as the relative humidity of the ambient atmosphere at which
    [007] the material starts absorbing moisture from the atmosphere.
    [008] When the humidity in the atmosphere is equal (or higher) to the critical relative humidity of a salt sample, the sample will absorb water until all of the salt is dissolved to give a saturated solution.
    [009] A product with reduced critical humidity is difficult to store, transport and apply, as it tends to agglomerate and form lumps. With a high humidity in the air, as found in marine or tropical environments, such fertilizer can even be destroyed.
    [010] This is a phenomenon exhibited by all ammonium salt fertilizers, and many coating systems and coating substances have been developed to prevent deterioration of the product. However, since urea typically has a relatively high critical humidity of more than 70%, most urea producing equipment does not need, or do not have, a facility to treat the product prior to storage. This would prevent the use of the proposed integrated ammonia recovery systems without additional investment and would incur operating costs for the coating.
    [011] When urea is mixed with ammonium salts, however, the critical moisture in the final product drops significantly. A mixture of urea and ammonium nitrate has a critical humidity of about 20%, a mixture of urea and ammonium sulfate of only 60%. These values would cause serious problems in handling the product. Therefore, it is expected that such products should be treated before leaving the equipment. Alternatively, a way to avoid moisture uptake by the urea granules / ammonium salt should be developed.
    [012] The feed system for a urea granulator
    [013] 3, as shown in Fig. 1 a), consists of a feeding system 5, from which the urea solution 4 is distributed to spray nozzles 6 inside the urea granulator 3. In the system of the urea state of the art, as shown here, only the urea solution is introduced into the urea granulator 3. Alternatively, as shown in Fig.
    [014] 1 b), the urea solution 4 and a stream of urea / ammonium salt 8, containing urea and ammonium salt, are introduced into the urea granulator 3, either separately or as a mixture, on the side of the flow inlet of granules 1 of the urea granulator only, and this mixture flows in countercurrent to the granules to be formed in the urea granulator 3. Therefore, in both examples, a product 7 is generated by passing through the side inlet of the granule stream 1 to the outlet side of the granule stream 2, which consists of a homogeneous distribution of ammonium salt and urea. Therefore, the granules produced in this way have a low critical humidity. The gaseous effluents 14 from the urea granulator are subjected to common washing systems of the prior art and are released into the atmosphere.
    [015] It is a state of the art technology to provide coatings of different types in hygroscopic fertilizers, soluble in water to improve the physical or agronomic properties of the product. US3205061 describes the coverage of the fertilizer with molten wax. The use of urethane resin to coat soluble fertilizers is disclosed in US3372019. Hygroscopic fertilizers are usually coated with water-resistant sealants, such as oils, waxes, and other organic materials, to reduce moisture absorption and subsequent agglomeration of individual particles.
    [016] The various coated products have several drawbacks, including low production rates, high operating costs, as well as the requirements for large amounts of coating material that has to be used.
    [017] EP0289074 describes a process for the production of fertilizer granules containing urea and ammonium sulfate by granulation in a fluidized bed of particles. In this process, ammonium sulphate particles prepared separately are introduced, which serve as nuclei. These ammonium sulphate cores are applied with urea by spraying an aqueous liquid containing urea with a urea concentration of 70-99.9% by weight for the cores. The final product is a granulate having an urea-coated ammonium sulphate core.
    [018] In US3725029, ammonium sulfate is granulated through a specific binder. These particles are coated with molten urea and the coated particles are contacted with a dry powder as an anti-caking agent.
    [019] Both processes described in EP0289074 and US3725029 use granulated ammonium sulfate as nuclei to generate the final granulate. Therefore, both methods include the drawback that granulators specific for granulation of ammonium sulphate are necessary, leading to increased production costs.
    [020] The object of the present invention is, therefore, to provide an alternative process that avoids the above mentioned problems caused by the critical moisture of a mixture of urea and ammonium salt. The disadvantage and deficiencies of fertilizers coated with a coating material must also be eliminated by means of the present invention.
    [021] This is achieved through a method for the production of urea granules that have a low moisture absorption capacity, with a urea granulator, which has an inlet side of the flow of granules and opposite an outflow side of granules, which forms an axis along which urea granules are formed from a urea solution and a stream of urea / ammonium salt, whereby the urea solution and the urea / salt stream of ammonium are sprayed, in the form of a mixture or separately, by means of a feeding system unit, through several nozzles, into the urea granulator on a source material. In this process, the higher amount of the urea / ammonium salt stream is sprayed into the urea granulator on the inlet side of the granule stream and the amount of the urea / ammonium salt stream is reduced along the axis of the granulator. of urea, from the inlet side of the granule stream to the outlet side of the urea granule stream, so the urea / ammonium salt stream comprises a urea: ammonium salt ratio, between 4 and 20, a water content of 0-10% by weight, and optionally up to 1-5% by weight of additives, the largest amount of urea solution being sprayed into the urea granulator on the outlet side of the granule flow, and the amount of urea solution is reduced along the axis of the urea granulator, from the outlet side of the granule stream to the inlet side of the granule stream.
    [022] Other embodiments of the present invention are related to the composition of the streams introduced into the urea granulator. Preferably, the current introduced into the flow inlet side of the urea granulator consists exclusively of the urea / ammonium salt stream, and the flow introduced into the flow outflow side of the urea granulator consists exclusively of the urea solution without mix both streams.
    [023] The urea / ammonium salt stream preferably comprises a urea: ammonium salt ratio between 7 and 16. The water content of this stream is preferably 0-5% by weight. Optionally, it comprises between 0.4 to 0.8% by weight of additives. The additives for the urea / ammonium salt stream are thus selected from the group comprising formaldehyde, aluminum sulphate, magnesium sulphate, micronutrients and other carbohydrate granulation additives or mixtures thereof. As a preferred additive, formaldehyde is used.
    [024] The urea solution introduced into the outlet side of the granule flow of the urea granulator comprises a water content of 0-10% by weight, preferably a water content of 0-5% by weight and, optionally , up to 1.5% by weight of additives, preferably between 0.4 to 0.8% by weight of additives, where the additives by weight are selected from the group comprising formaldehyde, aluminum sulphate, magnesium sulphate, micronutrients and other carbohydrate granulation additives or mixtures thereof. As a preferred additive, formaldehyde is used. It is also possible that the urea solution has a lower impurity content, such as biuret.
    [025] Additives for the urea / ammonium salt stream, as well as for the urea solution, are selected from the group comprising formaldehyde, aluminum sulphate, magnesium sulphate, micronutrients and other carbohydrate granulation additives. or their mixtures. As a preferred additive, formaldehyde is used.
    [026] Advantageously, the source material is chemically compatible with the produced urea granules. This means that the composition of the source material can be of any natural or synthetic composition. Materials that are environmentally friendly, degradable and not harmful to the soil and plants to be fertilized are preferred. To give some examples, they can be earth, sand or biodegradable plastics. Other fertilizers are also possible. Most preferred are the large urea granules or small crushed urea granules, which are produced by the process of the present invention. This source material must be less than the desired end product. The source material is ideally sized if it is 20-80% smaller than the desired final product, and preferably if it is 40-80% smaller than the final product, and more preferably if it is 60-80% smaller than the final product. To result in urea granules with a low moisture absorption capacity, it is important to choose the size of the starting material as small as possible, in order to ensure a source material fully covered with the urea solution.
    [027] Optionally, the highest amount of the urea / ammonium salt stream is sprayed into the urea granulator at the inlet side of the granule stream, and the amount of the urea / ammonium salt stream sprayed in the urea granulator. is reduced to zero in the first half of the axis from the granule flow inlet side to the granule flow out side, and is preferably reduced to zero in the first fifth of the axis from the granule flow inlet side to the side outflow of granule flow.
    [028] It is advantageous for the urea / ammonium salt stream to be released from a washing system to remove ammonia from the gaseous effluents in a urea granulator.
    [029] It is known to the person skilled in the art that the temperature of the urea / ammonium salt stream and of the urea solution entering the urea granulator is above the melting temperature of these streams. It is also known that the melting temperature depends on the composition of the currents. Therefore, a person skilled in the art would automatically choose a suitable temperature for both streams. Advantageously, the temperature of both streams is in the same range.
    [030] In another embodiment of the present invention, the pressure of the urea stream / ammonium salt entering the supply system unit on the inlet side of the granule flow of the urea granulator is higher than the pressure of the urea entering the supply system unit on the outlet side of the granule flow from the urea granulator. This serves to regulate the amount of the urea / ammonium salt stream and the amount of urea solution that enters the supply system unit. In this way, the composition of urea granules produced is regulated. Preferably, the pressure of the urea stream / ammonium salt entering the supply system unit, on the inlet side of the granule flow of the urea granulator, is 0.1 - 1 bar higher than the pressure of the urea solution that enters the feed system unit at the granule flow outlet side of the urea granulator.
    [031] The method described for the production of urea granules with a low moisture absorption capacity is to work in a fluidized bed urea granulation apparatus comprising a urea granulator, which has an inlet side of the flow of granules and opposite an outlet side of the granule stream, which forms an axis along which urea granules are formed, which comprise a feeding system unit for the transport of a urea solution and a urea / salt stream. ammonium, in the form of a mixture or separately, through several spray nozzles into the urea granulator whereby the feed system unit is equipped with means for transporting the urea / ammonium salt stream to the inlet side of the granule flow from the urea granulator and with means for transporting the urea solution to the outlet side of the granule flow from the urea granulator.
    [032] An additional option of the device is that the supply system unit is equipped with one or more collectors with openings with equal or different sizes, which transport different amounts of urea solution or urea stream / ammonium salt to nozzles. to be connected to the urea granulator. In addition, the one or more collectors optionally have means to adjust the flow to the nozzles to be connected to the urea granulator.
    [033] Another embodiment is that the fluidized bed urea granulation apparatus comprises a washing system, releasing the urea / ammonium salt stream and a means for conveying the urea / ammonium salt stream to the urea granulator. .
    [034] Optionally, the fluidized bed urea granulation apparatus comprises means for pressurizing the urea / ammonium salt stream and for the urea solution.
    [035] This pressurization step is optionally carried out by self-regulating the amount of urea / ammonium salt stream and urea solution entering the supply system unit. This is, for example, a measurement of the ammonium salt content in the urea / ammonium salt stream connected with the pressurization of the respective streams. Therefore, a constant product composition is ensured, regardless of slight changes in the ammonium salt content in the urea / ammonium salt stream.
    [036] Also claimed is the urea granule which is produced by the process for the production of urea granules with low moisture absorption capacity, with a urea granulator, which has an inlet side of the flow of granules and an opposite side outflow of the granule stream, which forms an axis along which urea granules are formed from a urea solution and a stream of urea / ammonium salt, so the urea solution and the urea stream / ammonium salt is sprayed, in the form of a mixture or separately, through a feed system unit through several nozzles, to the urea granulator on a source material. Thus, the higher amount of the urea / ammonium salt stream is sprayed into the urea granulator on the inlet side of the granule stream and the amount of the urea / ammonium salt stream is reduced along the axis of the granulator. urea from the inlet side of the granule stream to the outlet side of the granule stream, and the highest amount of the urea solution is sprayed into the urea granulator on the outlet side of the granule stream and the amount of the urea solution is reduced along the axis of the urea granulator from the outlet side of the granule stream to the inlet side of the granule stream.
    [037] Optionally, the total concentration of ammonium salts in the urea granules is up to 5% by weight of ammonium salts, preferably 0.5 to 1.5% by weight, with a nitrogen content of at least 46% by weight. This ensures that a nitrogen content of at least 46% by weight is achieved in the urea granule and is therefore, by definition, still a urea fertilizer grade product.
    [038] The granules thus consist of a center of a source material, as described above. This source material is surrounded by subsequent layers composed of a mixture of ammonium salt and urea, in which the concentration of urea increases from the center to the outer layer of the granule, where the outer layer of the granule contains up to 80 a
    [039] 100% urea. More preferably, the outer layer of the granule contains 100% urea.
    [040] The advantage obtained with this arrangement is that the layers composed of a mixture of ammonium salt and urea, with their reduced critical humidity, are totally surrounded by urea and, therefore, are protected against the humidity of the ambient air. As a consequence, the final product, which leaves the urea granulator, has the same resistance to the capture of moisture from the ambient air, as the urea granules composed of pure urea. This offers an opportunity to integrate ammonium salt streams, which are currently emitted by a conventional urea production process, into the urea granulator so that the urea fertilizer shows low moisture absorption trends. If a stream comprising ammonium salts were introduced in a state of the art urea granulation process, the final product produced would show trends in high moisture absorption and a second coating step would be necessary, for example, with the urea. In using the present invention, the need for additional coating systems for the final product produced is eliminated. In addition, the recovered ammonia is included in the product; therefore, urea production is increased, leading to significant economic benefit.
    [041] In the following, the invention is described in more detail by way of example. Fig. 2 shows a schematic block diagram of a urea granulator with a fluidized bed 3. A stream of urea / ammonium salt 8 is introduced into the urea granulator 3 on the inlet side of the granule stream 1 through a supply system 5. As a result of the urea solution 4 being introduced into the urea granulator 3, on the outlet side of the granule flow 2 through the supply system 5. Thus, the supply system 5 consists of one or more collectors, which are equipped with several spray nozzles 6 to introduce the urea / ammonium salt stream 8 and the urea solution 4 into the urea granulator. In addition, the feed system 5 is equipped with means for adjusting the flow to the nozzles 6 to control and adjust the amount of urea stream / ammonium salt 8 and / or urea solution 4 introduced in the urea granulator 3. Therefore the urea / ammonium salt stream is sprayed onto the parent material 11 generally present in a urea granulator.
    [042] The amount of urea / ammonium salt stream 8 fed into the urea granulator drops from the inlet side of the granule stream 1 to the outflow side of the granule stream 2, so it is about 100% in the inlet side of the granule flow 1. The amount of the urea solution is higher and preferably 100% on the outflow side of the granule flow 2 of the urea granulator 3.
    [043] When feeding the urea / ammonium salt stream 8 in this way into the urea granulator 3, the concentration of the ammonium salt is reduced to almost zero on the outlet side of the granule flow 2 from the urea granulator 3. For better results, the amount of the urea / ammonium salt stream 8 fed into the urea granulator 3 is adjusted to zero within the first fifth along the axis from the inlet side of the granule stream 1 to the outlet side of the granule stream 2. This is shown exemplarily in graph 10. Graph 10 demonstrates the ideal amount of urea / ammonium salt stream 8 present in the respective location in the urea granulator 3. In the final section of the granulator, only urea solution 4 is sprayed on the growing urea granules 13.
    [044] The urea granules are therefore constructed in such a way that the ammonium salt contained in the urea / ammonium salt stream 8 is at the center of the urea granules 12 around the parent material 11, while the subsequent layers of the growing urea granules 13 around that center of the urea granules 12 contain an increasing amount of urea and the final layer of the resulting product of the invention 9 consists only of urea.
    [045] By this means, the urea / ammonium salt stream 8 is released from a washing system to remove ammonia from the gaseous effluents 14 of the urea granulator 3 or, alternatively, it can be introduced separately into the feeding system 5.
    [046] The advantages of the proposed invention are: • the urea involvement of the ammonium salt, with its critical humidity reduced, and therefore the protection against the humidity of the ambient air in a one-step process, so that no step additional coating is required • the final product has the same resistance to trapping moisture from ambient air as the urea granules composed of pure urea. • there is no need for coating systems • simple and economical method • integration with existing urea granulation devices is possible • a simple way to process the ammonium salts in existing urea granulation equipment is used without negatively influencing the quality of the product • a typical product with a urea fertilizer grade is produced. The product has a nitrogen content of at least 46% by weight and, therefore, is still a product with a urea fertilizer grade.
    [047] Key for referenced items 1 granule flow inlet side 2 granule flow outflow side 3 urea granulator 4 urea solution 5 supply system 6 spray nozzles 7 product 8 urea stream / ammonium salt 9 resulting inventive product 10 graph showing the amount of urea / ammonium salt current present in the respective location of the urea granulator 11 source material 12 center of the urea granule 13 urea granules growing gaseous effluents
    权利要求:
    Claims (8)
    [0001]
    1. METHOD FOR THE PRODUCTION OF UREAN GRANULES WITH LOW MOISTURE ABSORPTION CAPACITY, with a urea granulator, which has an inlet side of the flow of granules and opposite an exit side of the flow of granules, which forms an axis to the over which the urea granules are formed from a urea solution and a stream of urea / ammonium salt, in which • the urea solution and the stream of urea / ammonium salt are sprayed, in the form of a mixing or separately, through a feed system unit through several nozzles, in the urea granulator on a source material; characterized in that • the largest amount of the urea / ammonium salt stream is sprayed into the urea granulator on the inlet side of the granule stream, and the amount of the urea / ammonium salt stream is reduced along the granulator axis of urea from the inlet side of the granule flow to the outlet side of the granule flow, whereby the urea / ammonium salt stream comprises a urea: ammonium salt ratio between 4 and 20, a water content from 0-10% by weight, and optionally up to 1-5% by weight of additives, and • the largest amount of urea solution is sprayed into the urea granulator on the outlet side of the granule flow and the amount of solution of urea is decreased along the axis of the urea granulator from the outlet side of the granule stream to the inlet side of the granule stream.
    [0002]
    METHOD according to claim 1, characterized in that the urea / ammonium salt stream introduced at the inlet side of the granule flow of the urea granulator comprises a urea ratio: ammonium salt between 7 and 16, a water content 0-5% by weight and, optionally, between 0.4 to 0.8% by weight of additives.
    [0003]
    METHOD, according to claim 2, characterized in that the additives are selected from the group comprising formaldehyde, aluminum sulfate, magnesium sulfate, micronutrients and other carbohydrate granulation additives or mixtures thereof.
    [0004]
    METHOD according to either of claims 1 or 2, characterized in that the urea solution introduced into the outlet side of the granule flow of the urea granulator comprises a water content of 0-10%, by weight, preferably a water content of 0-5% by weight and, optionally, up to 1.5% by weight of additives, preferably between 0.4 to 0.8% by weight of additives, where additives by weight are selected from from the group comprising formaldehyde, aluminum sulphate, magnesium sulphate, micronutrients and other carbohydrate granulation additives or mixtures thereof.
    [0005]
    METHOD according to any one of claims 1 to 4, characterized in that the largest amount of the urea / ammonium salt stream is sprayed into the urea granulator on the inlet side of the granule stream and the amount of the stream of urea / ammonium salt sprayed into the urea granulator is reduced to zero in the first half of the axis from the granule flow inlet side to the granule flow outflow side, and preferably be reduced to zero in the first fifth of the axis from the inlet side of the granule stream to the outlet side of the granule stream.
    [0006]
    Method according to any one of claims 1 to 5, characterized in that the urea / ammonium salt stream is released from a washing system to remove ammonia from the gaseous effluents of a urea granulator.
    [0007]
    METHOD according to any one of claims 1 to 6, characterized in that the pressure of the urea / ammonium salt stream entering the feed system unit on the inlet side of the granule flow of the urea granulator is higher to the pressure of the urea solution entering the supply system unit on the outlet side of the granule flow from the urea granulator.
    [0008]
    8. UREA GRANULES, comprising a center of a source material, obtained according to the method defined in claim 1, characterized in that the source material is surrounded by subsequent layers composed of a mixture of ammonium salt and urea, in which the concentration of urea increases from the center to the outer layer of the granule, where the outer layer of the granule contains up to 80 to 100% by weight of urea.
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    法律状态:
    2018-07-10| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2019-05-07| B06T| Formal requirements before examination [chapter 6.20 patent gazette]|
    2019-12-24| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application [chapter 6.1 patent gazette]|
    2020-04-22| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-10-13| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 31/08/2011, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    EP10009615.5|2010-09-15|
    EP10009615A|EP2431346A1|2010-09-15|2010-09-15|Method for producing urea fertilizer with low moisture absorption tendencies|
    PCT/EP2011/004398|WO2012034650A1|2010-09-15|2011-08-31|Method for producing urea fertilizer with low moisture absorption tendencies|
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