WO2017186526A1 - Procédé de production d'un gaz riche en hydrogène - Google Patents

Procédé de production d'un gaz riche en hydrogène Download PDF

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Publication number
WO2017186526A1
WO2017186526A1 PCT/EP2017/059098 EP2017059098W WO2017186526A1 WO 2017186526 A1 WO2017186526 A1 WO 2017186526A1 EP 2017059098 W EP2017059098 W EP 2017059098W WO 2017186526 A1 WO2017186526 A1 WO 2017186526A1
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WO
WIPO (PCT)
Prior art keywords
gas
reactor
steam
stream
inlet
Prior art date
Application number
PCT/EP2017/059098
Other languages
English (en)
Inventor
Christian Wix
Rasmus TRANE-RESTRUP
Original Assignee
Haldor Topsøe A/S
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Haldor Topsøe A/S filed Critical Haldor Topsøe A/S
Priority to CN201780023672.6A priority Critical patent/CN109071215A/zh
Publication of WO2017186526A1 publication Critical patent/WO2017186526A1/fr
Priority to ZA2018/05928A priority patent/ZA201805928B/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
    • C01B3/12—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents by reaction of water vapour with carbon monoxide
    • C01B3/16—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents by reaction of water vapour with carbon monoxide using catalysts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • 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

Definitions

  • the present invention relates to a method for production of a hydrogen enriched gas from a synthesis gas.
  • Said method comprises the combined steps of adding steam and recycling product gas, especially during startup and at reduced load, in order to control the process gas reactivity especially while the catalyst is fresh and highly active.
  • steam is added as a reactant to a synthesis gas comprising CO, which reacts with 3 ⁇ 40 to form 3 ⁇ 4 and CO 2 according to the water gas shift reaction.
  • a side reaction - especially at elevated tempera- tures - is methanation.
  • excess steam may be added such that the reactor feed gas has a high steam to carbon monoxide ( S : CO) -ratio (i.e. above 2).
  • the present disclosure proposes, at least during a part of the catalyst life cycle, to operate a reactor for sour or sweet water gas shift reaction with a combination of recycle and steam addition for moderation of the reactivity.
  • the moderation by recycle may be reduced or omitted.
  • the recycle gas may be driven by an ejector, having steam as motive gas, to avoid an increase in operational cost and capital investment .
  • water gas shift process (or the shift process) shall be used for a chemical process in which CO and 3 ⁇ 40 reacts to form 3 ⁇ 4 and CO 2 .
  • sour shift shall be used for a water gas shift process taking place in the presence of sulfur compounds employing a catalytically active material which is not deactivated by sulfur compounds, such as co ⁇ balt/molybdenum sulfides on a support.
  • sweet shift process shall be used for a water gas shift process taking place in the absence of sulfur compounds employing a catalytically active mate ⁇ rial which is sensitive to sulfur deactivation, such as copper/zinc/aluminum on a support.
  • methanation process or formation of methane shall be used for a chemical process in which CO or CO 2 and 3 ⁇ 4 reacts to form CH 4 and 3 ⁇ 40.
  • synthesis gas or syngas shall be used for a gas comprising CO and 3 ⁇ 4 in which the combined concentration of CO and 3 ⁇ 4 is at least 15%.
  • such a stage may be implemented in one or more reac ⁇ tors or reactor beds .
  • a broad aspect of the present invention relates to a pro ⁇ cess for production of a hydrogen rich gas, comprising the steps of (a) providing a reactor feed gas, comprising at least 25%, 40% or 70% on dry basis of CO and 3 ⁇ 4 in combi ⁇ nation, as well as steam,
  • the change between said first peri ⁇ od of high recycle operation and said second period of low recycle operation is made upon the evaluation of a tempera ⁇ ture of the material catalytically active in water gas shift reaction
  • This temperature may be monitored in one or more positions in the reactor or proximate to the reactor.
  • the change between said first peri ⁇ od of high recycle operation and said second period of low recycle operation is made upon an indirect evaluation of the temperature of the material catalytically active in wa- ter gas shift reaction, such as a parameter obtained indi ⁇ rectly from process data correlated to the temperature.
  • the change between said first peri ⁇ od of high recycle operation and said second period of low recycle operation is made upon an evaluation of the compo ⁇ sition of the product gas with the associated benefit that the composition of the product gas reflects the actual op ⁇ eration of the process, especially the amount of CO not re ⁇ acted in the process gas.
  • said synthesis gas comprises at least 20% CO on dry basis and at most 70% CO on dry basis, with the associated benefit of such a syngas being indus ⁇ trially relevant for conversion by the water gas shift pro- cess.
  • said synthesis gas comprises at least 200 ppm sulfur, with the associated benefit of such a gas not having undergone expensive desulfurization .
  • said amount of product gas is driv ⁇ en by an ejector, having steam as motive gas, with the associated benefit of an ejector being a simple piece of equipment, have low capital and operational cost.
  • a further aspect of the present disclosure relates to a process plant for production of a hydrogen rich gas, comprising a reactor having an inlet and an outlet,
  • said process plant being configured for receiving by sepa ⁇ rate lines
  • said recycle line further comprises an ejector having a mo- tive gas inlet, a suction gas inlet and a discharge outlet, in which the motive gas inlet is in fluid communication with said stream of steam, the suction gas inlet is in fluid communication with said reactor outlet and the discharge outlet is in fluid communication with the inlet of the re- actor and wherein said process plant comprises a means for controlling the amount of gas drawn through said suction gas inlet,
  • the process plant further comprises a steam control valve having an inlet and an outlet config ⁇ ured such that the steam control valve inlet is in fluid communication with said stream of steam and the steam con- trol valve outlet is in fluid communication with said reac ⁇ tor inlet, with the associated benefit of said steam valve controlling the amount of steam directed as motive gas to the ejector and thus the amount of recycle.
  • Hy- drogen may either be required as pure hydrogen, e.g. for ammonia production or for hydroprocessing in refineries or it may be required in combination with carbon monoxide, e.g. for synthesis of methanol or synthetic natural gas or for feed to the Fischer-Tropsch process.
  • Hydrogen is, as part of a synthesis gas, provided from gasification in the presence of water of a carbonaceous material or a hydrocar ⁇ bon. Often the amount of carbon monoxide in the synthesis gas is higher than desired in the subsequent processes.
  • the well-known water gas shift reaction is used to partially or fully “shift" the carbon monoxide in the gas to hydrogen, in the presence of an appropriate catalyst by reaction of the carbon monoxide with water.
  • the product of the reaction comprises CO 2 , which conveniently is simple to separate from the synthesis gas.
  • the present disclosure will typically find use in the process known as sour shift, which typically employ catalysts comprising cobalt and ei ⁇ ther molybdenum or tungsten, and which have the benefit of operating at moderate temperatures, and without requiring sulfur removal from the synthesis gas, but which also have a tendency to catalyze formation of methane from CO and 3 ⁇ 4 instead of hydrogen at elevated temperatures, as a side re ⁇ action.
  • Temperature control of water gas shift reaction by processes according to the present disclosure may however also be relevant for other water gas shift catalysts like catalysts for sweet shift.
  • the composition of the synthesis gas is dependent on a num ⁇ ber of aspects, including the gasifier design. Some examples of the composition are given in Higman, C. and van der
  • the synthesis gas in oxygen fired gasifiers comprises 25-50% 3 ⁇ 4 and 15-75% CO and CO 2 in combination, but other gases
  • constituents e.g. up to 10% CH 4 may also be present. If the gasifier operates on atmospheric air, the composition will naturally be dominated by N 2 , such that other
  • synthesis gas may also be provided from other processes, such that the composition may vary from the above, but the combined concentration of CO and H 2 will be above 25
  • methane formation is a side reaction of the water gas shift reaction especially over so-called sour shift catalysts since sour shift catalysts typically oper ⁇ ate at moderate stoichiometric excess of steam.
  • Methane formation is undesired, the process is exothermal and has a high activation temperature, and various methods have been used to minimize methane formation.
  • the most common measure is addition of excess steam to reduce the reactivity to ⁇ wards methane formation in order to reduce the reactor out- let temperature, and thus protect the catalyst against sin ⁇ tering and moderate the methanation reaction.
  • the process is often designed to operate under less active conditions for methanation e.g.
  • the process is dynamically configured in ac- cordance with process parameters, such as the temperature of the catalytically active material, the processed volume of synthesis gas or the catalyst activity.
  • the means for pressurizing the recycle stream is an ejector with the added steam as motive gas, which avoids the otherwise significant operational and investment cost of a compressor.
  • the extent of recycle may in this respect be controlled by controlling the amount of steam sent as motive gas for the ejector, e.g. by a line by-passing the ejector and directing the steam directly to the inlet of the reactor.
  • Figure 1-4 shows a reactor in a water gas shift process configuration according to the present disclosure, with variable recycle driven different types ejectors and modes of controlling the recycle and steam addition.
  • Figure 5 shows the reactor in a traditional water gas shift process configuration according to the prior art.
  • FIG. 1 shows a reactor in a water gas shift process con ⁇ figuration according to the present disclosure, with recy ⁇ cle around the reactor driven by a variable ejector.
  • a feed syngas 102 is first split into a main stream 106 and an op ⁇ tional feed bypass stream for adjustment 110.
  • the main stream 106 may optionally be heated in a heat exchanger be ⁇ fore being combined with a recycle stream 128.
  • the combined feed stream 114 is directed to the water gas shift reactor 150 followed by cooling of the product stream 124 e.g. in a waste heat boiler 152 with steam production, but the released heat may also be used for other purposes.
  • An amount of the cooled product stream may be recycled 126 around the reactor depending on the setting of the variable ejector 154.
  • the recycle stream 126 is drawn by ejector 154 using steam 120 as motive stream. It is desired to keep the molar flow ratio be ⁇ tween 106 and 120 constant to ensure a constant conversion of CO to H2 in the shift unit. In practice 102 and thus 106 are given by the desired plant load and the steam addition 120 is then adjusted accordingly by the internal needle valve in variable ejector 154 in combination with the bypass control valve 162. The recycle flow 126 then deter ⁇ mines the reactor outlet temperature 124. The recycle flow is controlled by the internal needle in the ejector. The amount of recycle may be controlled in dependence of a tem ⁇ perature measured in the reactor or in the outlet stream from the reactor.
  • the remaining product stream forms the product gas stream 130 which may be directed to a second water gas shift reactor (not shown) .
  • the product gas stream 130 may optionally be cooled and combined with the feed by- pass stream for adjustment 110 to form the shifted and ad ⁇ justed product stream 134.
  • the combination of the product gas stream 130 with the feed bypass stream for adjustment 110 is optional and may be omitted e.g. if a high module (i.e. a high amount of 3 ⁇ 4 relative to CO) product gas is required, especially if pure hydrogen is produced.
  • a high module i.e. a high amount of 3 ⁇ 4 relative to CO
  • an optional guard reactor may be positioned upstream the il- lustrated reactor, and that the feed temperature may be controlled by quenching with water. Quenching will have the effect of moderating the reaction in a manner similar to steam.
  • a further embodiment of the process will be to provide ma ⁇ terial catalytically active in two or more shift reactors and quenching an intermediate product gas with water, while recycling the product gas from the second shift reactor.
  • Figure 2 shows a further embodiment according to the pre ⁇ sent disclosure, with a reactor in a water gas shift pro ⁇ cess configuration, with recycle around the reactor driven by an ejector.
  • FIG. 1 This embodiment is equivalent to that of Figure 1, but an external valve 264 and a traditional ejec ⁇ tor 254 is used.
  • a variable ejector according to figure 1 is preferred due its increased flexibility in terms of turndown ratio, but a configuration with separate ejector and valve according to figure 2 is more simple con ⁇ figuration for controlling recycle.
  • a feed syngas 202 is combined with a recycle stream 228.
  • the combined feed stream 214 is directed to the water gas shift reactor 250 followed by cooling of the product stream 224 in waste heat boiler 252 e.g. with steam production, but the released heat may also be used for other purposes.
  • An amount of the cooled product stream 226 may be recycled around the reac ⁇ tor by ejector 254 using steam 222 as motive stream, to re- prise the reactor outlet temperature. It is desired to keep the molar steam to CO ratio (i.e. the flow ratio between 206 and 220) constant to ensure a constant conversion of CO to H2 in the shift unit.
  • molar steam to CO ratio i.e. the flow ratio between 206 and 220
  • the recycle flow 226 determines the reactor outlet temperature 224.
  • the recycle flow is controlled by a valve 262 which bypasses steam around the ejector 254.
  • the amount of recycle may be controlled in dependence of a temperature measured in the reactor or in the outlet stream from the reactor.
  • the remaining product stream forms the product gas stream 230 which may be di ⁇ rected to a second water gas shift reactor (not shown) .
  • Figure 3 shows a further embodiment according to the pre ⁇ sent disclosure, with a reactor in a water gas shift pro ⁇ cess configuration, with recycle around the reactor driven by an ejector.
  • the amount of recycle is controlled by a valve in the recycle line, which has a higher flexibility than a configuration where steam by-passes the ejector as in Figure 1 and Figure 2 since steam addition and recycle flow can be adjusted independently.
  • a feed syngas 302 is combined with a recycle stream 328.
  • the combined feed stream 314 is directed to the water gas shift reactor 350 followed by cooling of the product stream 324 in waste heat boiler 352 e.g. with steam production, but the released heat may also be used for other purposes.
  • An amount of the cooled product stream may be recycled 326 around the reac ⁇ tor by ejector 354 using steam 322 as motive stream.
  • the overall steam to CO ratio is controlled by valve 364 and the reactor outlet temperature controlled by the amount of recycle, i.e. by adjustment of valve 360.
  • the amount of re ⁇ cycle may be controlled in dependence of a temperature measured in the reactor or in the outlet stream from the reactor.
  • the remaining product stream forms the product gas stream 330 which may be directed to a second water gas shift reactor (not shown) .
  • Figure 4 shows a further embodiment according to the pre ⁇ sent disclosure, with a reactor in a water gas shift pro ⁇ cess configuration, with recycle around the reactor driven by an ejector.
  • a feed syngas 402 is combined with a recycle stream 428.
  • the combined feed stream 414 is directed to the water gas shift reactor 450 followed by cooling of the product stream 424 in waste heat boiler 452 e.g. with steam production, but the released heat may also be used for oth- er purposes.
  • An amount of the cooled product stream 426 may be recycled around the reactor by variable ejector 454, controlled by an internal needle valve, using steam 420 as motive stream, with the ejector recycle efficiency being defined by ad- justing the internal valve of ejector 454, yielding a recycle stream 428.
  • the amount recycled is controlled by valve 460in accordance with the desired process temperature, and the needle valve of the variable ejector 454 will define the amount of steam drawn from 420.
  • the amount of recycle may be controlled in dependence of a temperature measured in the reactor or in the outlet stream from the reactor.
  • the remaining product stream forms the product gas stream 430 which may be directed to a second water gas shift reac ⁇ tor (not shown) .
  • FIG. 5 shows a reactor in a water gas shift process lay ⁇ out according to the prior art.
  • a feed syngas 502 is op ⁇ tionally split into a main stream 506 and a feed bypass stream 510.
  • the main stream 506 may optionally be heated in a heat exchanger before it is combined with a stream of steam 520.
  • the combined feed stream 514 is directed to the water gas shift reactor 550 followed by cooling of the in ⁇ termediate product stream 524 in waste heat boiler 552 with steam production.
  • This cooled intermediate product stream may be directed to a second water gas shift reactor (not shown) .
  • the product gas stream 530 may also be cooled in a heat exchanger and optionally be combined with the feed by ⁇ pass stream for adjustment 510 to form the final shifted and adjusted product stream 536. Examples
  • a feed synthesis gas is characterized, corre ⁇ sponding to a synthesis gas from a single stage dry feed gasifier operated at 1500 °C and 30 bar.
  • the feed flow rate is assumed to be 200.000 Nm 3 /h.
  • Example 1 correspond to a de ⁇ activated (end of run) catalyst. 77 m 3 catalytically active material is required in the example, and the resulting out ⁇ let temperature is 470°C. Steam consumption is 155 t/h.
  • Example 2 correspond to start up conditions, as stated above, which was designed based on the end of run requirement of Example 1. The resulting out ⁇ let temperature is 500°C, which is above the desired range.
  • Example 3 correspond to a start up condition as in Example 2, but with temperature moderation by steam addition, such that the temperature becomes 470°C.
  • An additional 14 t/h of steam is, during half load start up, required compared to Example 2, and in full load operation this would become 28 t/h.
  • the amount of ex ⁇ cessive steam may be reduced continuously over the lifetime of the catalyst.
  • Example 4 considers start up conditions according to an em ⁇ bodiment of the present disclosure, which shows that the combination of recycle and steam addition provided the pos ⁇ sibility of maintaining the desired module in product gas at 470°C, i.e. a temperature below that obtained with steam addition alone. Furthermore, the steam addition is reduced by 30 % compared with example 3.
  • Example 5 shows the effect of increasing the production from 50% load to full load. In this example the space ve ⁇ locity decreases, and thus the required amount of recycle is slightly reduced. The steam addition is reduced by 20 % compared with example 1.
  • Example 6 and 7 refer to catalyst with reduced activity, and they show that even as the catalyst activity decreases with time, the combined steam addition and recycle is bene ⁇ ficial. By combining the two activity moderators the amount of steam added will be 127 t/h, compared to 155 t/h of Ex ⁇ ample 1.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Abstract

La présente invention concerne un procédé et une installation de traitement associée pour la production d'un gaz riche en hydrogène, comprenant les étapes consistant à : (a) prendre un gaz d'alimentation de réacteur, comprenant au moins 25 %, 40 % ou 70 %, sur base sèche, de CO et de H2 en combinaison, ainsi que de la vapeur, (b) diriger ledit gaz d'alimentation de réacteur pour qu'il entre en contact avec un matériau catalytiquement actif dans une réaction de conversion de gaz à l'eau, ce qui produit un gaz produit, caractérisé en ce que, pendant une première période de fonctionnement de recyclage élevé, une première quantité dudit gaz produit est recyclée pour entrer en contact avec ledit matériau catalytiquement actif conjointement avec ledit gaz d'alimentation de réacteur et, pendant une deuxième période de fonctionnement de recyclage faible, ledit gaz produit n'est pas recyclé ou une deuxième quantité inférieure à ladite première quantité dudit gaz produit est recyclée pour entrer en contact avec ledit matériau catalytiquement actif conjointement avec ledit gaz d'alimentation de réacteur. L'avantage associé d'un tel traitement réside en ce que le changement entre les modes de fonctionnement peut être effectué selon des critères de traitement appropriés, de telle sorte que les conditions de traitement optimales sont toujours appliquées, tout en réduisant les coûts de fonctionnement, y compris la consommation de vapeur.
PCT/EP2017/059098 2016-04-25 2017-04-18 Procédé de production d'un gaz riche en hydrogène WO2017186526A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201780023672.6A CN109071215A (zh) 2016-04-25 2017-04-18 生产富氢气体的方法
ZA2018/05928A ZA201805928B (en) 2016-04-25 2018-09-04 Method for production of a hydrogen rich gas

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DKPA201600239 2016-04-25
DKPA201600239 2016-04-25

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WO2017186526A1 true WO2017186526A1 (fr) 2017-11-02

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022013239A1 (fr) 2020-07-14 2022-01-20 Engie Dispositif et procédé de production hybride de dihydrogène de synthèse et/ou de méthane de synthèse

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203768006U (zh) * 2014-03-24 2014-08-13 中石化宁波工程有限公司 一种节能型循环co变化装置
US20140225037A1 (en) * 2009-11-05 2014-08-14 Johnson Matthey Plc Water gas shift reaction process
WO2015062986A1 (fr) * 2013-10-28 2015-05-07 Haldor Topsøe A/S Procédé et réacteur pour réaction exothermique
US20150144842A1 (en) * 2013-11-25 2015-05-28 Siemens Aktiengesellschaft Treatment of synthesis gases from a gasification facility

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203768005U (zh) * 2014-03-24 2014-08-13 中石化宁波工程有限公司 一种防超温循环co变换装置

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140225037A1 (en) * 2009-11-05 2014-08-14 Johnson Matthey Plc Water gas shift reaction process
WO2015062986A1 (fr) * 2013-10-28 2015-05-07 Haldor Topsøe A/S Procédé et réacteur pour réaction exothermique
US20150144842A1 (en) * 2013-11-25 2015-05-28 Siemens Aktiengesellschaft Treatment of synthesis gases from a gasification facility
CN203768006U (zh) * 2014-03-24 2014-08-13 中石化宁波工程有限公司 一种节能型循环co变化装置

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022013239A1 (fr) 2020-07-14 2022-01-20 Engie Dispositif et procédé de production hybride de dihydrogène de synthèse et/ou de méthane de synthèse

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CN109071215A (zh) 2018-12-21
ZA201805928B (en) 2024-01-31

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