WO2023156360A1 - Préparation de condensat de traitement optimisée - Google Patents

Préparation de condensat de traitement optimisée Download PDF

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Publication number
WO2023156360A1
WO2023156360A1 PCT/EP2023/053567 EP2023053567W WO2023156360A1 WO 2023156360 A1 WO2023156360 A1 WO 2023156360A1 EP 2023053567 W EP2023053567 W EP 2023053567W WO 2023156360 A1 WO2023156360 A1 WO 2023156360A1
Authority
WO
WIPO (PCT)
Prior art keywords
process condensate
purification device
coarse
urea
condensate purification
Prior art date
Application number
PCT/EP2023/053567
Other languages
German (de)
English (en)
Inventor
Ivo Müller
Original Assignee
Thyssenkrupp Industrial Solutions Ag
Thyssenkrupp 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
Priority claimed from DE102022201727.7A external-priority patent/DE102022201727A1/de
Priority claimed from LU102914A external-priority patent/LU102914B1/de
Application filed by Thyssenkrupp Industrial Solutions Ag, Thyssenkrupp Ag filed Critical Thyssenkrupp Industrial Solutions Ag
Publication of WO2023156360A1 publication Critical patent/WO2023156360A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/38—Steam distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B01D53/58—Ammonia
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/10—Treatment of water, waste water, or sewage by heating by distillation or evaporation by direct contact with a particulate solid or with a fluid, as a heat transfer medium
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
    • C07C273/04—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds from carbon dioxide and ammonia
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
    • C07C273/14—Separation; Purification; Stabilisation; Use of additives
    • C07C273/16—Separation; Purification
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/16—Nitrogen compounds, e.g. ammonia
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions

Definitions

  • the invention relates to the processing of the process condensate obtained in the urea synthesis.
  • the process condensate occurring in the urea synthesis contains both ammonia and urea as impurities. It is therefore cleaned in a three-stage process before it is used again.
  • ammonia is often removed at temperatures of around 115 to 140 °C.
  • a hydrolysis is then carried out at temperatures of around 190 to 200° C. and usually more than 15 bar and for a time of 60 to 120 minutes, in which urea decomposes into ammonia and carbon dioxide.
  • the resulting ammonia and carbon dioxide are then removed in a third step.
  • the separation processes in the first and third step are identical, so these two steps are usually carried out in a column that is only split down the middle to interpose the second step.
  • This three-step process makes the entire process condensate stream very clean, specifically less than 3 ppm ammonia and less than 3 ppm urea. This is correspondingly complex and requires a lot of energy. There are also applications with less high purity requirements, especially with the exhaust gas scrubbing required for urea formation, in particular urea granulation or urea prilling, especially since urea is introduced there as an impurity from the exhaust gas.
  • US 2019 / 0177180 A1 proposes separating a partial flow after the first stage and feeding it to the exhaust gas scrubber. However, this means that the streams in the first stage and the third stage, which are in a common column, have very different amounts, which can have a disadvantageous effect on the design and operation.
  • US Pat. No. 4,652,678 A discloses a method for recovering valuable components from a waste gas stream from urea synthesis. i A method for removing urea, ammonia and carbon dioxide from a dilute aqueous solution is known from US Pat. No. 4,410,503 A.
  • the object of the invention is to provide a process condensate treatment which, on the one hand, has the high purity for the usual uses and, on the other hand, has a lower purity for the waste gas scrubbing, and at the same time enables optimal process management with minimal energy consumption.
  • the system network serves to produce a urea molding material, in particular urea granules or urea prills.
  • granulate or prill are usually used; they are particulate, agglomerated material which has a particle size suitable for application as a fertilizer and is usually produced in a shaping step following the synthesis, ie granulation or prilling.
  • the plant network has at least one urea synthesis device and one urea forming device.
  • the plant network usually also has a device for synthesizing ammonia and, in many cases, a reformer for producing the hydrogen. Ammonia is produced from hydrogen and nitrogen in the device for the synthesis of ammonia.
  • urea is produced with carbon dioxide in the urea synthesis device and partly processed with other components, for example ammonium nitrate, sulfur compounds, lime and the like, in the urea forming device to form granules which are widely used in particular as fertilizers.
  • the plant network can optionally also have a nitric acid synthesis device and optionally also an ammonium nitrate synthesis device.
  • ammonium nitrate for example, can be mixed with the urea as a further component and shaped together, in particular granulated.
  • the plant network has a process condensate purification device, wherein the process condensate purification device for separating ammonia and Urea is formed from the process condensate of the urea synthesis device. This enables further use of the water inside or outside of the system network or its disposal.
  • the process condensate purification device has a purification flow up to the process condensate outlet.
  • the purification stream usually leads the process condensate through three stages in order to achieve a high degree of purity of the process condensate. This means that the purified process condensate can be used in a variety of ways.
  • the plant network has a shaping exhaust air washing device, which is connected to the urea shaping device and is used to clean the exhaust gases of this device.
  • the molding exhaust air washing device serves to remove the urea that has gotten into the exhaust air by washing it out with water, thus reducing the emission of nitrogen.
  • the forming effluent scrubber includes a second stage in which a scrub with an acidic medium removes ammonia.
  • the plant network has a coarse process condensate purification device in addition to the process condensate purification device.
  • the coarse process condensate purification device has a coarse purification stream. In the coarse purification flow, a simpler purification took place compared to the process condensate purification device, so that the roughly purified process condensate has a lower purity, but the effort required for the coarse purification is correspondingly reduced.
  • the coarse purification stream is separate and distinct from the purification stream.
  • the coarse process condensate purification device and the process condensate purification device are thus two separate devices and the coarse process condensate purification device is not just, for example, the first stage of the process condensate purification device.
  • the urea synthesis device is connected to the process condensate purification device and the coarse process condensate purification device for transferring process condensate.
  • the coarse process condensate purification device is equipped with the
  • the flow of the process condensate of the urea synthesis device is divided into two partial flows.
  • a first partial flow goes into the prior art process condensate purification device. Since this stream is completely purified, the first stage and the third Stage designed for the same volume flow and are also operated in this way.
  • the new coarse process condensate purification device, into which a second partial flow is fed, is arranged parallel to the conventional process condensate purification device.
  • the need for the first partial flow and the second partial flow can be approximately the same, for example.
  • the water flow required for the forming exhaust air washing device is cleaned sufficiently in the coarse process condensate cleaning device only for this application and is therefore much more energy-efficient.
  • a removal of the urea from the process condensate is not necessary for its use in the exhaust air scrubber.
  • the coarse process condensate purification device has only one stage and therefore, above all, no hydrolysis in a second step.
  • the amount of ammonia in the process condensate can be specifically adjusted by the separate coarse process condensate purification device.
  • the ammonia released from the exhaust air during the forming process, in particular during the granulation or prilling process is preferably removed by acidic scrubbing, for example with nitric acid or sulfuric acid.
  • the associated ammonia salt is formed, which can also be used as a fertilizer or as a feedstock for other processes, for example for the production of urea ammonium nitrate (UAN).
  • UAN urea ammonium nitrate
  • the amount of heat required for the process condensate purification device is provided in the form of steam, which is predominantly fed directly into the process and is thus itself the process condensate. If the process condensate cleaning takes place more energy-efficiently, this amount of steam fed in can be reduced. This leads to a reduction in the amount of process condensate that occurs, since the saved steam means that no additional water is introduced, which would increase the amount of process condensate.
  • the strict separation of the process condensate purification device and the purification flow from the coarse process condensate purification device and the coarse purification flow results in two fundamental advantages.
  • the first benefit is that in particular the process condensate purification device is designed for a constant continuous purification stream. All stages are therefore designed for an identical volume flow, which is advantageous.
  • the second advantage is that retrofitting as part of a capacity expansion is easily possible.
  • an existing process condensate purification device can continue to be operated and a new, additional and separate coarse process condensate purification device is installed, which cleans the process condensate flow added by the capacity expansion in a simple and reduced manner and for corresponding Applications, in particular the forming exhaust air scrubber provides.
  • a capacity expansion of the process condensate purification device can thus advantageously be dispensed with.
  • the coarse process condensate purification device is designed in one stage for the removal of ammonia.
  • the coarse process condensate purification device is designed in the form of a column, in particular a tray column or a packed column.
  • a second stage for the hydrolysis of urea to form ammonia and CO2 is therefore preferably not part of the coarse process condensate purification device.
  • the coarse process condensate purification device has a first heat exchanger.
  • the first heat exchanger is designed to preheat the process condensate stream coming from the urea synthesis device. This takes place in that the heat exchanger is designed to cool the coarsely cleaned process condensate flow emerging from the coarse process condensate purification device. The process heat can thus be kept in the coarse process condensate purification device.
  • the coarse process condensate purification device has a second heat exchanger.
  • the second heat exchanger is designed to condense the gas stream exiting the coarse process condensate purification device.
  • the gas mixture can which contains in particular water, ammonia and carbon dioxide, are condensed.
  • This process condensate can also be referred to as a carbamate solution, since the ammonia and carbon dioxide contained there partially react with one another in an aqueous solution, to form carbamate, among other things.
  • the second heat exchanger and the coarse process condensate purification device are preferably connected to a carbamate return line. As a result, a partial flow of the carbamate solution can be fed back into the coarse process condensate purification device.
  • the proportion of water in the carbamate solution can be reduced if necessary in order to increase the concentration of ammonia and carbon dioxide. This is advantageous since this carbamate solution is fed to the urea synthesis device, where a low water input is advantageous for the reaction process.
  • the coarse process condensate purification device has a third heat exchanger.
  • the coarse process condensate purification device also has a recirculation line for a partial flow of the coarsely cleaned process condensate flow.
  • the third heat exchanger is arranged in the recirculation line and is designed to heat the recirculated partial flow.
  • this direct steam feed increases the amount of water in the coarsely cleaned process condensate stream.
  • the indirect heat input through a heat exchanger leaves the total quantity unchanged.
  • the partial flow can in particular also be evaporated.
  • the system network has a process condensate reservoir.
  • the process condensate reservoir is arranged after the urea synthesis device and before the process condensate purification device and the coarse process condensate purification device.
  • the coarse process condensate purification device and the urea synthesis device are connected via a first line for returning the in the coarse process condensate purification device resulting carbamate solution connected.
  • the process condensate purification device and the urea synthesis device are connected via a second output for recycling the carbamate solution emerging from the process condensate purification device.
  • the first line and the second line are connected to each other. In particular, these can flow into one another and be routed as a common line into the urea synthesis device.
  • the urea forming device has one or more fine waste air washing devices, for example droplet separation using a demister. Since this is the last cleaning step before the exhaust air is released into the environment, special cleanliness requirements are placed on the cleaning solution used. If this requirement is not met by the coarsely cleaned process condensate from the coarse process condensate cleaning device, a different source for the washing solution must be selected for this final cleaning step. Then, as before, the clean process condensate from the process condensate purification device is usually used. The amount of water in the fine exhaust air washing device is usually small compared to the total water requirement of the laundry. Therefore, the stated positive effects of the coarse process condensate purification device are also retained in this embodiment.
  • fine waste air washing devices for example droplet separation using a demister. Since this is the last cleaning step before the exhaust air is released into the environment, special cleanliness requirements are placed on the cleaning solution used. If this requirement is not met by the coarsely cleaned process condensate from the coarse process condensate cleaning device, a different source for
  • FIG. 1 shows a section of a system network. Ammonia and carbon dioxide are fed to the urea synthesis device 1 at the reactant inlet 30 and converted there to urea. The urea is then transferred to the urea forming device 2 . The exhaust air from the urea molding device 2 is transferred to the molding exhaust air washing device 4 .
  • the process condensate which is produced during the synthesis of urea from ammonia and carbon dioxide, is transferred from the urea synthesis device 1 to a process condensate store 3 .
  • the process condensate stream is divided according to the invention.
  • a partial flow for example 50%, is transferred to the process condensate purification device 10, as is known and customary from the prior art for such a plant network.
  • the process condensate is first fed through the fourth heat exchanger 14 into the first stage 11 and separated there at, for example, 140° C. and 3 bar of ammonia. After passing through the first stage 11, the process condensate reaches the second stage 12 through the fifth heat exchanger 15, for example for 60 minutes at 200° C. and 16 bar.
  • the urea is converted with water into ammonia and carbon dioxide.
  • the process condensate passes through the fifth heat exchanger 15 into the third stage 13, where ammonia is separated off under the same conditions as in the first stage 11 (in a common column). This then returns via a second line 41 to the urea synthesis device 1.
  • the cleaned process condensate passes from the third stage 13 through the fourth heat exchanger 14 to the process condensate outlet 32 and can be transferred to other processes.
  • Another partial flow, for example 50%, of the process condensate is transferred from the process condensate storage 3 into the coarse process condensate purification device 20 .
  • the process condensate first reaches the first heat exchanger 22 and is preheated there and transferred to the column 21, for example a packed column.
  • the gas stream emerging at the upper end of the column 21 is passed through the second heat exchanger 23 and condensed.
  • a partial flow thereof is fed back into the column 21 , and the remaining partial flow is fed through the first line 40 into the urea synthesis device 1 .
  • the coarsely cleaned process condensate exiting at the lower end of the column is divided and a partial flow is heated through the process condensate return line and the third heat exchanger 24 , at least partially evaporated, and fed back to the column 21 .
  • the rest Partial flow of the coarsely cleaned process condensate is routed via the first heat exchanger 22 to recover the heat and then routed into the forming exhaust air washing device 4 in order to take up more urea from the exhaust air there.

Abstract

L'invention concerne un système combiné de production d'un matériau de formation d'urée. Le système combiné comprend au moins un dispositif de synthèse d'urée (1) et un dispositif de formation d'urée (2), et le système combiné comprend un dispositif de nettoyage de condensat de traitement (10), le dispositif de nettoyage de condensat de traitement (10) étant conçu pour séparer l'ammoniac et l'urée du condensat de traitement du dispositif de synthèse d'urée (1), et le système combiné comprend un dispositif de lavage de l'air d'échappement de formation (4). L'invention est caractérisée en ce que le système combiné comprend en outre un dispositif de nettoyage de condensat de traitement grossier (20) en plus du dispositif de nettoyage de condensat de traitement (10). Le dispositif de synthèse d'urée (1) est relié au dispositif de nettoyage de condensat de traitement (10) et au dispositif de nettoyage de condensat de traitement grossier (20) afin de transférer le condensat de traitement, et le dispositif de nettoyage de condensat de traitement grossier (20) est relié au dispositif de lavage d'air d'échappement de formation (4).
PCT/EP2023/053567 2022-02-18 2023-02-14 Préparation de condensat de traitement optimisée WO2023156360A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
LULU102914 2022-02-18
DE102022201727.7A DE102022201727A1 (de) 2022-02-18 2022-02-18 Optimierte Prozesskondensataufbereitung
LU102914A LU102914B1 (de) 2022-02-18 2022-02-18 Optimierte Prozesskondensataufbereitung
DE102022201727.7 2022-02-18

Publications (1)

Publication Number Publication Date
WO2023156360A1 true WO2023156360A1 (fr) 2023-08-24

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1528051A (en) * 1974-09-30 1978-10-11 Foster Wheeler Energy Corp Pollution control process for fertilizer plant
DE3002460A1 (de) * 1979-01-30 1980-08-21 Cf Ind Verfahren und vorrichtung zur nachbehandlung, insbesondere fuer harnstoff- und ammonnitratanlagen
US4410503A (en) 1981-02-28 1983-10-18 Unie Van Kunst-Mestfabrieken Process for the removal of urea, ammonia, and carbon dioxide from dilute aqueous solutions
US4652678A (en) 1981-05-15 1987-03-24 Stamicarbon B.V. Process for the recovery of valuable components from the waste streams obtained in the preparation of urea
WO2013165245A1 (fr) * 2012-05-03 2013-11-07 Stamicarbon B.V. Usine de production d'urée
US20170341951A1 (en) * 2016-05-24 2017-11-30 Toyo Engineering Corporation Method and apparatus for treating urea aqueous solution
US20190177180A1 (en) 2017-12-08 2019-06-13 Toyo Engineering Corporation Treatment method of an aqueous solution containing urea, ammonia and carbon dioxide and treatment equipment therefor
EP3782979A1 (fr) * 2019-08-20 2021-02-24 Yara International ASA Préparation de solution d'urée et installation associée
WO2021137701A1 (fr) * 2019-12-30 2021-07-08 Stamicarbon B.V. Production d'urée avec de multiples évaporateurs
WO2021137700A1 (fr) * 2019-12-30 2021-07-08 Stamicarbon B.V. Élimination d'ammoniac au stade final de la production d'urée

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1528051A (en) * 1974-09-30 1978-10-11 Foster Wheeler Energy Corp Pollution control process for fertilizer plant
DE3002460A1 (de) * 1979-01-30 1980-08-21 Cf Ind Verfahren und vorrichtung zur nachbehandlung, insbesondere fuer harnstoff- und ammonnitratanlagen
US4410503A (en) 1981-02-28 1983-10-18 Unie Van Kunst-Mestfabrieken Process for the removal of urea, ammonia, and carbon dioxide from dilute aqueous solutions
US4652678A (en) 1981-05-15 1987-03-24 Stamicarbon B.V. Process for the recovery of valuable components from the waste streams obtained in the preparation of urea
WO2013165245A1 (fr) * 2012-05-03 2013-11-07 Stamicarbon B.V. Usine de production d'urée
US20170341951A1 (en) * 2016-05-24 2017-11-30 Toyo Engineering Corporation Method and apparatus for treating urea aqueous solution
US20190177180A1 (en) 2017-12-08 2019-06-13 Toyo Engineering Corporation Treatment method of an aqueous solution containing urea, ammonia and carbon dioxide and treatment equipment therefor
EP3782979A1 (fr) * 2019-08-20 2021-02-24 Yara International ASA Préparation de solution d'urée et installation associée
WO2021137701A1 (fr) * 2019-12-30 2021-07-08 Stamicarbon B.V. Production d'urée avec de multiples évaporateurs
WO2021137700A1 (fr) * 2019-12-30 2021-07-08 Stamicarbon B.V. Élimination d'ammoniac au stade final de la production d'urée

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