WO2018091146A1 - Verfahren und vorrichtung zur synthesegaszerlegung mittels sauergaswäsche und kryogenem trennprozess - Google Patents
Verfahren und vorrichtung zur synthesegaszerlegung mittels sauergaswäsche und kryogenem trennprozess Download PDFInfo
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- WO2018091146A1 WO2018091146A1 PCT/EP2017/025324 EP2017025324W WO2018091146A1 WO 2018091146 A1 WO2018091146 A1 WO 2018091146A1 EP 2017025324 W EP2017025324 W EP 2017025324W WO 2018091146 A1 WO2018091146 A1 WO 2018091146A1
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- gas
- cryogenic
- pressure level
- carbon monoxide
- nitrogen
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/506—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification at low temperatures
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- 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
- B01D53/14—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 by absorption
- B01D53/1456—Removing acid components
- B01D53/1462—Removing mixtures of hydrogen sulfide and carbon dioxide
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- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/52—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with liquids; Regeneration of used liquids
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- F25J3/04539—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the H2/CO synthesis by partial oxidation or oxygen consuming reforming processes of fuels
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- 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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- 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
- C01B2203/0485—Composition of the impurity the impurity being a sulfur compound
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
Definitions
- the invention relates to a process for the decomposition of a syngas, from which carbon dioxide and sulfur components are separated in an acid gas scrubbing to obtain a largely consisting of hydrogen and carbon monoxide, methane-containing synthesis gas from which subsequently in a cryogenic separation process, a carbon monoxide product is obtained in the sour gas scrubbing a stripping gas is used at a first pressure level provided by a nitrogen source at a second pressure level above the first level.
- the invention relates to a device for carrying out the
- pressure level and "temperature level” are used to characterize pressures and temperatures, which is intended to express that parameters for carrying out the method according to the invention need not have an exact value. Rather, they move around an average. Corresponding levels are in disjoint areas.
- Sour gas scrubber supplied in which the acid gases are separated using a methanol detergent, wherein a largely of hydrogen and
- Carbon monoxide existing methane-containing synthesis gas and a loaded with the separated acid gases detergent can be obtained.
- the loaded detergent regenerated, wherein acid gases are usually expelled at a pressure between 1, 5 and 3bar (a) by nitrogen used as stripping gas.
- Carbon monoxide product and hydrogen is decomposed.
- the raw hydrogen is normally used for regeneration of the temperature change adsorber before it is purified by pressure swing adsorption to a hydrogen product and then reacted together with the carbon monoxide product to monoethylene glycol.
- the oxygen required for the coal gasification is provided by a cryogenic
- Air Separator delivered which also uses nitrogen as the stripping gas for the
- Sour gas washing provides. Typically, the nitrogen falls in the
- the stated object is achieved in that the gas provided by the nitrogen source is used as the refrigerant in the cryogenic separation process and is thereby expanded to the first pressure level in order subsequently to be supplied to the sour gas scrubbing as stripping gas.
- the method according to the invention it is possible to use as stripping gas
- the chemical Composition of the gas supplied from the nitrogen source is not changed, so that it requires no further treatment in order to be used as a stripping gas in the sour gas scrubbing.
- the pressure level of the carbon monoxide product determines the minimum level of the
- the amount of gas supplied as a refrigerant from the nitrogen source used in the cryogenic separation process is preferably equal to the amount of stripping gas required in the acid gas scrubbing and is completely supplied to the sour gas scrubbing after the expansion to the first pressure level.
- gas from the nitrogen source in an amount in the cryogenic separation process as the refrigerant, which is larger or smaller than the required Strippgasmenge.
- the missing part is expediently fed directly from the nitrogen source, wherein the relaxation of the nitrogen from the second to the first pressure level via a throttle body. If the cold that can be generated via the gas supplied from the nitrogen source as the refrigerant for the operation of the cryogenic separation process is insufficient, liquid nitrogen can additionally be used as the refrigerant.
- the method according to the invention is used when the cryogenic separation process is a condensation process.
- the condensation process has been state of the art and known to experts for many years. It is preferably used for the decomposition of synthesis gases obtained by partial oxidation and therefore having a high carbon monoxide and a low methane content.
- the synthesis gas is here by
- Both refrigeration circuits are driven by multi-stage compressors. While a two-stage, relatively low-cost compressor can be used in a nitrogen cycle, a carbon monoxide compressor incurs significantly higher costs. The reason for this is firstly that a carbon monoxide compressor must be designed with at least three compressor stages to a thermal To avoid decomposition of carbon monoxide and resulting soot deposits. On the other hand, it must be explosion-proof and be operated in a particularly secure area in order to prevent leaks
- the costs for the compressor of a carbon monoxide cycle are therefore up to 50% higher than those for a compressor which is suitable for driving a corresponding nitrogen cycle.
- the inventive method allows the refrigeration cycle of the
- Nitrogen source gas supplied to the design of the compressor is influenced by the height of the third pressure level, which depends significantly on the process management within the condensation process.
- a condensation process of the type indicated above was identified, in which the CO / CH 4 separation column is heated by nitrogen used as a refrigerant and at least a portion of the synthesis gas to be separated, the second
- Liquid phase is divided into a first, a second and a third partial stream, of which the first against the condensed nitrogen cooled in the heating of the CO / CH 4 separation column and the second against partial
- condensing synthesis gas evaporates and the vapor phases thereby formed are fed to the CO / CH 4 separation column as intermediate heating, while the third substream of the CO / CH 4 separation column is introduced as an intermediate reflux.
- the carbon monoxide yield of the condensation process depends essentially on the achievable temperature level of the peak cold, which is due to the first
- Pressure level is determined. Since nitrogen is used as the refrigerant, a first pressure level of between 2 and 3 bar (a) is sufficient to achieve a comparable yield to a much more costly carbon monoxide refrigeration cycle. In such a condensation process is used as a refrigerant
- Nitrogen is preferably depressurized by less than 13 bar, and more preferably by less than 10 bar, to reach the first pressure level.
- the invention relates to a device for decomposing a
- Synthesis raw gas with an acid gas scrubbing to obtain a largely consisting of hydrogen and carbon monoxide, methane-containing synthesis gas by separating carbon dioxide and sulfur components from the
- Carbon monoxide product can be obtained, and a nitrogen source, from the
- Stripping gas on a second, above the first lying pressure levels can be removed.
- cryogenic gas separator is connected to the sour gas scrubber and the nitrogen source in such a way that it can be supplied with gas from the nitrogen source in order to use it as refrigerant and subsequently to the first pressure level in the sour gas scrubber to be able to deliver as stripping gas.
- the device according to the invention comprises a compressor connected to the nitrogen source and the cryogenic gas separator, via which gas taken from the nitrogen source as refrigerant is compressed to a third pressure level before being introduced into the cryogenic gas separator.
- cryogenic gas separator for performing a
- a second liquid phase can be generated, and a CO / CH 4 separation column, which is connected to a reboiler, which is part of a refrigeration cycle and heat extracted via the guided in the cooling circuit nitrogen and a portion of the synthesis gas to be separated heat the CO / CH 4 - separation column can be supplied to the heating to from the second
- Liquid phase a carbon monoxide-rich gas phase with a purity that allows their release as a carbon monoxide product, and a largely of methane and Carbon monoxide existing bottoms product, the second
- Liquid phase can be divided into a first, a second and a third partial stream, of which the first against the cooled during the heating of the CO / CH 4 - separating column, condensing nitrogen and the second vaporizable against partially condensing synthesis gas and the vapor phases of CO formed thereby / CH 4 separation column can be fed as an intermediate heating, while the third part of the current CO / CH 4 separation column can be given as an intermediate reflux.
- the nitrogen source is a cryogenic
- Air Separator which can provide nitrogen gas with a pressure between 4 and 6bar (a).
- the acid gas scrubbing is preferably carried out as methanol scrubbing, in which nitrogen can be used at a pressure level between 1.5 and 3 bar (a) as stripping gas in the detergent regeneration.
- FIG. 1 shows the production of monoethylene glycol, in which a synthesis crude is decomposed in the manner according to the invention.
- FIG. 2 shows a cryogenic, operated after the condensation process
- a carbonaceous feed such as coal or heavy oil is fed via line 1 to the reactor R and there reacted with oxygen 2 from the cryogenic air separation L by partial oxidation to a synthesis gas, the after Separation of soot via line 3 in the synthesis gas cooler K passes. Cooled and dried, the synthesis crude gas 4 is supplied to the sour gas scrubber M, in which carbon dioxide and other acid gases are separated with the aid of a methanol detergent, wherein a largely consisting of hydrogen and carbon monoxide, methane-containing synthesis gas 5 and a laden with the separated acid gases detergent are obtained ,
- a largely consisting of hydrogen and carbon monoxide, methane-containing synthesis gas 5 and a laden with the separated acid gases detergent are obtained .
- Carbon Monoxide Product 9 in the synthesis G is converted to monoethylene glycol 10.
- the oxygen required for the partial oxidation 2 provides the cryogenic air separation L liquid nitrogen 1 1 to cover the refrigeration demand of the cryogenic separation device T and gaseous nitrogen 12 at a pressure level between 4 and 6bar (a), as stripping gas in the regeneration of the loaded cryogenic separation device T and gaseous nitrogen 12 at a pressure level between 4 and 6bar (a), as stripping gas in the regeneration of the loaded
- the pressure of the gaseous nitrogen 12 is raised to a value between 12 and 16 bar (a) by means of the preferably single-stage compressor P and introduced into the cooling circuit of the cryogenic separator T as refrigerant 13, where it is depressurized, to provide much of the required cooling capacity.
- the expanded nitrogen 14 leaves the cryogenic separator T and is forwarded to the sour gas scrub M. If in the cryogenic separator T less nitrogen than
- Refrigerant can be used as is needed in the acid gas M as stripping gas, a portion 15 of the gaseous nitrogen 12 is diverted from the cryogenic air separator L upstream of the compressor P and relaxed via the throttle body a, before he is also fed as stripping the sour gas scrubbing M ,
- cryogenic separator T shown in Figure 2 is in the
- Temperatur Railadsorber A purified synthesis gas 6 with a pressure between 30 and 60bar (a) in a first heat exchanger E1 to be heated Process streams without condensing cooled and then divided into a first 22 and a second partial stream 23, of which the first 22 for heating the CO / CH 4 separation column T2 in the reboiler R heat is withdrawn, wherein a further cooled, fully gaseous first partial stream 24th arises, with the second, guided in the bypass to the reboiler R partial stream 23 is combined to the synthesis gas stream 25.
- the quantitative ratio of the two partial streams 22 and 23 can be varied.
- the synthesis gas stream 25 is cooled to such an extent that the condensation of components results in a two-phase mixture 26 which is separated in the separator B into a hydrogen-containing liquid phase and a hydrogen-rich gas phase consisting largely of carbon monoxide and methane.
- the gas phase is withdrawn via line 27 from the separator B and after heating in the heat exchangers E2 and E1 as raw hydrogen 7 for
- Pressure swing adsorber D is forwarded.
- the liquid phase 29 is fed to the H 2 separation column T1.
- it is split into two partial streams, of which the first 30 is expanded as reflux to the top of the H 2 separation column T1, while the second partial stream 31 after relaxation and subsequent
- the H 2 separation column T1 which is operated at a pressure which is between one fifth and one third of the pressure of the synthesis gas 6, serves to remove the hydrogen dissolved in the liquid phase 29. It is heated by a circulating heater 32, which is integrated in the heat exchanger E2.
- the hydrogen-rich overhead fraction 33 from the H 2 separation column T1 is after
- Carbon monoxide and methane existing bottom fraction 35 is split into three substreams 36, 37 and 38 and in the at a pressure between 5 and 10bar (a) operated CO / CH 4 separation column T2 is expanded.
- the CO / CH 4 separation column T2 is heated via the reboiler R, in which the reboiler flow 39 is at least partially vaporized.
- the peak cooling required for the cryogenic separation process is obtained via a refrigeration cycle driven by the compressor P, in which the nitrogen 12 gaseously provided by the cryogenic gas separator L circulates as refrigerant.
- the nitrogen 13 leaves the preferably single-stage compressor P with a pressure which is not more than 13 bar above the pressure of the stripping gas required in the acid gas M, is subsequently cooled in the heat exchanger E1 and R in the reboiler together with the first partial stream 22 of the synthesis gas 6 further cooled against the reboiler 39 from the CO / CH 4 separation column T2, without condense.
- the heat exchanger E3 the cooled in the reboiler R nitrogen 40 against the partial stream 36, which is typically more than 45% of the amount of
- a part 45 of the nitrogen 41 condensed in the heat exchanger E3 is depressurized to the top of the CO / CH 4 separation column T2, where a condenser C is arranged which, cooled by liquid nitrogen, provides a temperature difference for driving an internal column carbon monoxide return 46.
- the second part 47 of the condensed nitrogen 41 and gaseous nitrogen 48 from the top of the CO / CH 4 separation column T2 are each cooled to the pressure level of the stripping gas required in the acid gas scrubbing relaxed and merged to the two-phase nitrogen flow 49, the peak cold for the cold End of the heat exchanger E2 supplies.
- Heat exchangers E2 and E1 the nitrogen 49 as the stripping gas 14 of the
- Carbon Monoxide Product 9 Forwarded to Monoethylene Glycol Synthesis G. Additional cooling is supplied to the separation process via the liquid 11 obtained from the cryogenic air separation L 1, which is discharged after evaporation and heating in the heat exchangers E2 and E1 via line 51 in gaseous form into the atmosphere or a flare system.
- a methane-rich, carbon monoxide-containing liquid phase 52 collects, which is also vaporized and warmed in the heat exchangers E2 and E1 before it can be discharged as fuel gas 53.
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FR3097951B1 (fr) * | 2019-06-26 | 2022-05-13 | Air Liquide | Procede et appareil de separation cryogenique d’un gaz de synthese pour la production de ch4 |
EP3851179A1 (en) * | 2020-01-14 | 2021-07-21 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and apparatus for separating a synthesis gas by cryogenic distillation |
Citations (5)
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EP0677483A1 (fr) * | 1994-04-13 | 1995-10-18 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Procédé et installation de séparation d'un mélange gazeux |
WO2000069774A1 (en) * | 1999-05-14 | 2000-11-23 | Texaco Development Corporation | Hydrogen recycle and acid gas removal using a membrane |
EP1724542A1 (de) * | 2005-05-10 | 2006-11-22 | Linde Aktiengesellschaft | Verfahren und Vorrichtung zur Gewinnung von Produkten aus Synthesegase |
DE102005025651A1 (de) * | 2005-06-03 | 2006-12-07 | Linde Ag | Verfahren und Vorrichtung zur Gewinnung von Produkten aus Synthesegas |
EP2311544A1 (en) * | 2009-10-05 | 2011-04-20 | L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Process and apparatus for the treatment of a synthesis gas |
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FR2775276B1 (fr) * | 1998-02-20 | 2002-05-24 | Air Liquide | Procede et installation de production de monoxyde de carbone et d'hydrogene |
WO2012097497A1 (en) * | 2011-01-17 | 2012-07-26 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Process and apparatus for production of ammonia synthesis gas and pure methane by cryogenic separation |
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Patent Citations (5)
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EP0677483A1 (fr) * | 1994-04-13 | 1995-10-18 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Procédé et installation de séparation d'un mélange gazeux |
WO2000069774A1 (en) * | 1999-05-14 | 2000-11-23 | Texaco Development Corporation | Hydrogen recycle and acid gas removal using a membrane |
EP1724542A1 (de) * | 2005-05-10 | 2006-11-22 | Linde Aktiengesellschaft | Verfahren und Vorrichtung zur Gewinnung von Produkten aus Synthesegase |
DE102005025651A1 (de) * | 2005-06-03 | 2006-12-07 | Linde Ag | Verfahren und Vorrichtung zur Gewinnung von Produkten aus Synthesegas |
EP2311544A1 (en) * | 2009-10-05 | 2011-04-20 | L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Process and apparatus for the treatment of a synthesis gas |
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