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  • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
  • C01B3/025—Preparation or purification of gas mixtures for ammonia synthesis
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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  • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J19/24—Stationary reactors without moving elements inside
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  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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  • C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
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  • C01—INORGANIC CHEMISTRY
  • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
  • C01C1/00—Ammonia; Compounds thereof
  • C01C1/02—Preparation, purification or separation of ammonia
  • C01C1/04—Preparation of ammonia by synthesis in the gas phase
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  • C01C1/00—Ammonia; Compounds thereof
  • C01C1/02—Preparation, purification or separation of ammonia
  • C01C1/04—Preparation of ammonia by synthesis in the gas phase
  • C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
  • C01C1/00—Ammonia; Compounds thereof
  • C01C1/02—Preparation, purification or separation of ammonia
  • C01C1/04—Preparation of ammonia by synthesis in the gas phase
  • C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
  • C01C1/0488—Processes integrated with preparations of other compounds, e.g. methanol, urea or with processes for power generation
• • 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
  • C07C273/10—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 combined with the synthesis of ammonia
• • 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
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/02—Processes for making hydrogen or synthesis gas
  • C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
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  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/02—Processes for making hydrogen or synthesis gas
  • C01B2203/0283—Processes for making hydrogen or synthesis gas containing a CO-shift step, i.e. a water gas shift step
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  • C01B2203/042—Purification by adsorption on solids
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  • C01B2203/042—Purification by adsorption on solids
  • C01B2203/043—Regenerative adsorption process in two or more beds, one for adsorption, the other for regeneration
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  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
  • C01B2203/0465—Composition of the impurity
• • C—CHEMISTRY; METALLURGY
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  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
  • C01B2203/0465—Composition of the impurity
  • C01B2203/0475—Composition of the impurity the impurity being carbon dioxide
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  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
  • C01B2203/0465—Composition of the impurity
  • C01B2203/048—Composition of the impurity the impurity being an organic compound
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  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
  • C01B2203/0465—Composition of the impurity
  • C01B2203/0495—Composition of the impurity the impurity being water
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  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/06—Integration with other chemical processes
  • C01B2203/068—Ammonia synthesis
• • C—CHEMISTRY; METALLURGY
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  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/08—Methods of heating or cooling
  • C01B2203/0872—Methods of cooling
• • C—CHEMISTRY; METALLURGY
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  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/12—Feeding the process for making hydrogen or synthesis gas
  • C01B2203/1205—Composition of the feed
  • C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
  • C01B2203/1235—Hydrocarbons
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  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/14—Details of the flowsheet
  • C01B2203/146—At least two purification steps in series
  • C01B2203/147—Three or more purification steps in series
• • C—CHEMISTRY; METALLURGY
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  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/14—Details of the flowsheet
  • C01B2203/148—Details of the flowsheet involving a recycle stream to the feed of the process for making hydrogen or synthesis gas
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
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  • C01B2210/00—Purification or separation of specific gases
  • C01B2210/0001—Separation or purification processing
  • C01B2210/0009—Physical processing
  • C01B2210/0014—Physical processing by adsorption in solids
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
  • Y02P20/00—Technologies relating to chemical industry
  • Y02P20/50—Improvements relating to the production of bulk chemicals
  • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Definitions

• the present invention relates to a method and installation for the combined production of synthesis gas of ammonia and carbon dioxide from a hydrocarbon source. More particularly, the present invention relates to a process for the combined production of synthesis gas of ammonia and carbon dioxide from a synthesis gas obtained by reforming hydrocarbons, and in particular natural gas.
• the invention also relates to a method and an integrated production plant for ammonia and carbon dioxide and a method and a plant for producing urea.
• step 4 When it is desired to recover the CO2 extracted in step 4 (for example to facilitate the extraction of oil or for a chemical production such as urea, etc.) or if it is desired to sequester it to reduce emissions of greenhouse gases, it is necessary to add a step of compression and drying of the CO2 extracted in step 4.
• the proposed invention aims to significantly reduce the cost of production of NH 3 when the CO2 must be compressed to be valued as mentioned above.
• a process for the combined production of synthesis gas of ammonia and carbon dioxide from a mixture of hydrocarbons comprising at least:
• PSA waste containing carbon dioxide, nitrogen, methane and carbon monoxide, at a pressure of the order of 1 to 3 bar abs
• a step of treating said PSA waste to obtain a fluid enriched in carbon dioxide comprising at least:
• each of the steps includes itself: a condensation step of all or part of the CO2 contained in the gas from the previous step, followed by
• step or steps are carried out at temperatures between room temperature and -56 ° C,
• the depleted flow rate of CO2 is sent to methanation at a pressure of at least 35 bar.
• CO2 is sent to the adsorption unit by pressure modulation.
• the process comprises a reverse conversion step to the synthesis gas vapor to oxidize most of the carbon monoxide it contains to carbon dioxide, with corresponding production of hydrogen
• the process comprises a step of reforming the hydrocarbon mixture to obtain synthesis gas containing at least carbon dioxide, hydrogen, carbon monoxide, methane, and water vapor;
• the gas containing methane and nitrogen is returned to the reforming step.
• all the nitrogen sent to the treatment unit is contained in the at least a portion of the hydrogen enriched stream and the at least a portion of the nitrogen and methane containing gas mixed to form a synthesis gas; 'ammonia.
• Ammonia is reacted with carbon dioxide to produce urea.
• an apparatus for the combined production of synthesis gas of ammonia and carbon dioxide from a mixture of hydrocarbons comprising at least:
• PSA waste a waste gas containing carbon dioxide, nitrogen, methane and carbon monoxide
• a processing unit of said PSA waste to obtain a fluid enriched in carbon dioxide comprising at least:
• a PSA waste drying unit compressed by removing the water contained to obtain a dry gas
• step or steps are carried out at temperatures between room temperature and -56 ° C,
• a CO2 depletion unit of a gaseous phase resulting from at least one separation step, for example by permeation, to produce a depleted flow rate of CO2 and a flow enriched with CO2
• the apparatus may include means for sending the CO2 enriched flow from the CO2 depletion step to the pressure modulation adsorption unit.
• an apparatus for producing ammonia and carbon dioxide as described above comprising a processing unit for treating ammonia synthesis gas to produce a flow rate of ammonia and a gas containing methane and nitrogen.
• the apparatus may include means for returning the gas containing methane and nitrogen to the reforming step.
• the apparatus may include a synthesis gas reverse conversion unit for oxidizing most of the carbon monoxide it contains to carbon dioxide, with corresponding hydrogen production.
• the apparatus may comprise a reforming unit of the hydrocarbon mixture for obtaining synthesis gas containing at least carbon dioxide, hydrogen, carbon monoxide, methane and water vapor.
• the apparatus may include a unit in which the ammonia is reacted with the carbon dioxide to produce urea.
• the solution according to the invention consists in using the incondensable gases of a process for producing carbon dioxide by separation at low temperature to supply an ammonia synthesis production unit.
• the PSA residue contains a quantity of CO2 of about 45% from reforming and reverse conversion (the exact content of CO2 is naturally a function of the composition of the mixture initial hydrocarbons).
• the process then makes it possible, starting from the residual gas of the PSA, whose pressure is typically less than 2 bar, to dispose, thanks to the compression of a gas, at a total pressure of between 40 and 80 bar, corresponding to a partial pressure of CO2. between 15 and 40 bar, compatible with cryogenic purification. These pressures will make it possible to use the fluids in the rest of the process without having to resort to additional compressions.
• the PSA waste is purified by partial condensation and optionally by permeation to produce a liquid flow rich in CO2.
• This liquid can, thanks to appropriate complementary treatments, be used or sequestered on site or nearby in gaseous form; it can be exported for use or sequestered in gaseous or liquid form. It can particularly and particularly advantageously be used in the food industry, through a suitable purification.
• all or part of the liquid is vaporized after expansion, with recovery of cold, to produce CO2 in gaseous form under pressure between 10 and 35 bar.
• the recovered cold is advantageously used for the cooling of process fluids in addition to the refrigerating apparatus.
• the CO2 can then be compressed to be transported by pipeline to a site of use and / or sequestration.
• the process is particularly advantageous when it is used to optimize the production of ammonia synthesis gas and jointly produce carbon dioxide.
• FIG. 1 represents a functional diagram illustrating an embodiment of the invention for the production of synthesis gas of ammonia and, respectively, of carbon dioxide, for example carbon dioxide to be sequestered.
• the feedstock to the process consists of a mixture of hydrocarbons - here natural gas (NG) - the hydrocarbon stream 1 feeds a plant 3 comprising a desulfurization unit, a pre-reformer to produce a pre-reformed mixture, mixture consisting essentially of methane, hydrogen, carbon monoxide, carbon dioxide and water, a reforming module fed by the pre-reformed mixture which produces a synthesis gas substantially containing hydrogen, monoxide of carbon, carbon dioxide, methane and water vapor and a reverse conversion module.
• NG natural gas
• the synthesis gas is cooled and then the cooled gas is treated in this inverse conversion module, where the CO is converted to H 2 and CO2.
• the gaseous mixture 5 leaving the plant 3 is cooled and then treated in a hydrogen purification unit 7 of pressure swing adsorption or PSA type, to obtain a gaseous stream enriched with hydrogen 9 at a purity at least equal to 98% and a residue gas 1 1 - waste PSA- containing carbon dioxide, methane, nitrogen, argon, hydrogen and carbon monoxide.
• This residual PSA 1 1 is available at a pressure of the order of 1 to 3 bar abs, it contains substantially all the CO2 co-produced during the reforming and reverse conversion steps.
• the average composition of the PSA 1 1 waste is close to: CO 2 : 45% - CO: 12% - H2: 23% - CH 4 : 17% - H 2 O: 1% - N 2 : 2%.
• CO2 content is between 42 and 48%, the content of H 2 varies between 20 and 26%, the contents of other constituents remaining approximately constant.
• the PSA residue 1 1 is then purified in a purification unit 13.
• the PSA 11 1 waste is first compressed in a compression module of the purification unit, to obtain a residual PSA compressed . It is compressed to about 60 bar, which ensures a partial pressure of CO2 of the order of 27 bar. Then it is freed from its heavy impurities in an adsorption module of the purification unit, by a succession of regenerable adsorptions for example, one thus obtains a purified compressed waste which is then dried in a drying module of the purification unit for obtaining a compressed waste, freed from heavy impurities and dried.
• This waste is then cooled to be separated by liquefaction in a separation module forming part of the purification unit, which makes it possible to obtain a liquid containing essentially liquid CO2 and a gaseous mixture containing an uncondensed fraction of CO2. than lighter compounds called incondensable.
• the cooling of the waste 1 1 is carried out by countercurrent circulation of the cold fluids resulting from the cryogenic purification and / or by heat exchange with an associated external refrigerating unit.
• the liquid contains essentially CO2, however, in order to obtain pure CO2, the liquid results from a distillation in order to rid it of the light impurities entrained in the liquid phase. For this, the waste can be expanded to 23 bar before feeding the distillation column.
• the gas phase 17 obtained at the end of the separation contains the light impurities of the charge 1 and is at least 40 bar abs; warmed to room temperature in the heat exchangers, it is the purge of incondensables, available at a pressure of 58 bar.
• the composition of the purge is of the order of: CO 2 : 21% - CO: 18% - H 2: 36% - CH 4 : 24% - N 2 : 1%.
• the purge of incondensables 17 is then treated in the adsorption or permeation module of a CO2 depletion unit 19 for reduce its carbon dioxide content.
• a product gas 21 has a reduced content of carbon dioxide.
• the other product gas 20, enriched in CO2 and rich in hydrogen, is sent to the unit PSA 7 to improve its performance, without being mixed upstream with the flow 5.
• the efficiency of the PSA unit 7 is very low because of the strong hold in N 2, one way of improving it is to introduce the gas (possibly being a permeate), which is certainly richer in H2 that the PSA feed, at the right time of the cycle, to improve the performance of PSA.
• the PSA unit differs from the usual H 2 PSA that must stop CO / CO 2 and N 2 .
• the unit 7 stops the CO and the CO2, but can let the nitrogen pass, which makes it possible not to have to penalize itself on the yield H 2 of the unit PSA 7.
• the gas 21 is then treated by methanation in a methanation unit 23 to convert the carbon dioxide and carbon monoxide residues into methane, forming a gas.
• the gas is mixed with the pure hydrogen 9 to form an ammonia synthesis gas 27.
• the ammonia synthesis gas 27 is sent to an ammonia synthesis unit 29 to produce ammonia 31.
• the ammonia synthesis unit also produces a gas 33 containing methane, nitrogen, argon, and hydrogen which is returned to unit 3.
• ammonia 31 and carbon dioxide 15 can feed a urea production unit 35.

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• 2012
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