WO2020178330A1 - Procédé pour la préparation de méthanol ou de méthane - Google Patents

Procédé pour la préparation de méthanol ou de méthane Download PDF

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Publication number
WO2020178330A1
WO2020178330A1 PCT/EP2020/055679 EP2020055679W WO2020178330A1 WO 2020178330 A1 WO2020178330 A1 WO 2020178330A1 EP 2020055679 W EP2020055679 W EP 2020055679W WO 2020178330 A1 WO2020178330 A1 WO 2020178330A1
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Prior art keywords
plant
exhaust gas
methanol
gas stream
methane
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PCT/EP2020/055679
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German (de)
English (en)
Inventor
Alexander Schulz
Original Assignee
Thyssenkrupp Industrial Solutions Ag
Thyssenkrupp Ag
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Publication of WO2020178330A1 publication Critical patent/WO2020178330A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
    • C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
    • C07C1/12—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon dioxide with hydrogen
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
    • C07C29/151—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases
    • C07C29/1516—Multisteps

Definitions

  • the present invention relates to a process for the production of methanol or methane by reacting hydrogen with carbon dioxide, at least one exhaust gas flow occurring in the plant for the production of methanol or methane being branched off from this plant.
  • Methane or synthetic natural gas which mainly consists of methane, can be produced by a so-called methanation reaction (also known as the Sabatier reaction), in which carbon dioxide and hydrogen are converted according to the reaction equation (2) given below:
  • EP 0 128 404 B1 a combination of i.a. a power plant and a plant for generating an energy source such.
  • a gas turbine power plant is coupled with a methanol synthesis plant. The residual flow of the
  • the methanol plant is fed into the combustion chamber of the power plant via a pipe. It is mentioned that this means that there is no need for a recycle stream in the methanol plant, which reduces the effort for the methanol plant. In times of low load, when little electrical energy is taken from the power plant, you can get through
  • WO 2018/019875 A1 describes a method for producing methanol by reacting carbon dioxide with hydrogen, in which a product stream obtained in the methanol synthesis reaction is fed, among other things, to a high-pressure separator in which a gas stream is separated off from a methanol-containing product stream.
  • This process provides for volatile components, which are only produced in small quantities, either to be discharged from the system via a pipe or to be burned via a flare.
  • a catalytic exhaust gas purification for example, is provided in this known method, the purified exhaust gas flow then then complying with possible existing emission limit values and thus being able to be released into the environment.
  • the object of the present invention is to provide a process for the production of methanol or methane with the features of the type mentioned at the outset, in which the exhaust gas streams incurred can be put to a meaningful use and the emission regulations can be complied with.
  • the branched off exhaust gas stream is fed to a second system which is connected to the system for the production of methanol or methane in the network, the exhaust gas stream being burned in this second system, this exhaust gas stream having a proportion of at least 20 wt. Contains% carbon dioxide and contains less than 20% by weight of carbon monoxide.
  • an exhaust gas stream is burned in the second system which contains more carbon dioxide than carbon monoxide, i.e. which contains carbon dioxide as the main component, which in its pure form is not combustible in the present case.
  • carbon monoxide is flammable and burns with oxygen in a blue, transparent flame to form carbon dioxide.
  • the fact that carbon dioxide is not flammable stands a combustion of the exhaust gas flow according to the invention in a second system does not preclude, on the one hand, a carbon dioxide-containing exhaust gas flow from the methanol or methane production can be mixed with another gas flow in the second system which contains combustible gases.
  • the proportion of the admixed carbon dioxide-containing gas can be comparatively small in relation to the volume of the other gas flow to which it is admixed, so that the combustion can take place without further ado.
  • the carbon dioxide-containing exhaust gas stream from the first system can also contain, for example, a proportion of hydrogen, so that it is combustible overall.
  • the carbon dioxide-containing exhaust gas stream according to the invention from the plant for the production of methanol or methane can have a composition such that it is itself combustible or else is non-combustible, but this gas stream in any case has a comparatively high proportion of non-combustible carbon dioxide of at least 20% by weight.
  • solution principle according to the invention can also be used analogously in processes for producing higher alcohols instead of methanol and for producing higher hydrocarbons instead of methane.
  • the exhaust gas stream contains a proportion of at least 30% by weight of carbon dioxide.
  • a gas stream with this carbon dioxide content can also be burned without further ado if, for example, it is mixed in a smaller amount with a second gas stream which, according to its composition, is present as a combustible gas stream.
  • a second gas stream which, according to its composition, is present as a combustible gas stream.
  • the measure according to the invention has the advantage that an optionally non-combustible exhaust gas stream from the methanol or methane production can also be burned in order to comply with any emission limit values. If the exhaust gas stream from the methanol or methane production mentioned contains other flammable components such as carbon monoxide or hydrogen in addition to carbon dioxide, thermal energy can also be obtained when such an exhaust gas stream is burned in the second system, which is useful, for example, in the second system or in the methanol system be used.
  • the exhaust gas stream that occurs in the plant for producing methanol or methane contains less than 15% Wt .-%, preferably less than 10 wt .-% of carbon monoxide.
  • the proportion of carbon monoxide in the exhaust gas stream is thus preferably not only less but also considerably less than the proportion of carbon dioxide in the exhaust gas stream.
  • the ratio of the gases carbon dioxide and carbon monoxide in the exhaust gas flow based on their respective proportions in% by weight can be, for example, at least 2: 1, preferably at least 3: 1, particularly preferably at least 4: 1.
  • the exhaust gas stream preferably contains a proportion of at least 40% by weight of carbon dioxide.
  • the proportion of carbon dioxide can be, for example, at least 45% by weight or, for example, at least 50% by weight, so that in the last-mentioned case there is an exhaust gas stream which consists predominantly of carbon dioxide.
  • the exhaust gas stream according to the invention can contain further components, in particular further combustible components, for example a proportion of hydrogen.
  • a proportion of hydrogen in the exhaust gas flow can possibly only be small, but hydrogen can certainly also be contained in an appreciable proportion, whereby the combustibility of the exhaust gas flow is naturally increased.
  • a waste gas stream from a plant for the production of methanol in which the conversion of carbon dioxide with hydrogen takes place according to the reaction equations mentioned at the beginning, contains hydrogen in an amount of at least 20% by weight, preferably at least 25% by weight, in particular preferably at least 30% by weight.
  • the proportion of carbon monoxide contained in the exhaust gas stream can not only be less than the proportion of carbon dioxide contained in the exhaust gas stream, but also, for example, less than the proportion of hydrogen contained in the exhaust gas stream, which is due to the water gas shift reaction (3) in the exhaust gas stream is included.
  • the exhaust gas stream can contain one or more further components, in particular at least one further component from the group comprising methanol, methane and dimethyl ether.
  • further components such as nitrogen or water vapor, for example, which are usually only present in relatively small proportions by weight, may optionally be present.
  • the exhaust gas stream according to the invention from a plant for the production of methanol contains, for example
  • the nitrogen content depends primarily on the C0 2 purity of the feed stream.
  • the exhaust gas flow in a typical plant according to the invention for the production of methane looks, for example, as follows: about 80 to 85% by weight of carbon dioxide less than 1% by weight of carbon monoxide less than 1% by weight of hydrogen less than 1 Wt .-% water vapor about 12 to 18 wt .-%, in particular about 14 to 16 wt .-% methane.
  • the hydrogen reacted with carbon dioxide in the production of methanol or methane is generated electrolytically beforehand.
  • the electrolytic generation of hydrogen by electrolysis of water is particularly advantageous if the electricity for the electrolysis can be obtained from renewable energies. For example, with wind power or solar systems, energy peaks can occur at times when more energy is being produced than can be taken from the system by feeding it into the power grid. This excess regeneratively obtained electrical energy can be used for the electrolysis of hydrogen, which in turn can be converted to methanol or methane according to the process according to the invention, whereby these are products that are good in liquid or gaseous form in containers or tanks save.
  • Methane or synthetically produced natural gas can be fed into the natural gas network.
  • the plant according to the invention for the production of methanol or methane is particularly preferably a comparatively small plant in which it is not worthwhile to purify an accumulating exhaust gas in a complex form so that it can then be released into the environment if necessary.
  • a relatively small plant is used if it is a plant with a low daily capacity, for example a plant with a capacity of less than 300 t / day and / or if the exhaust gas flow occurring in this plant is less than 50 kg / hour.
  • said exhaust gas flow can occur at different points in the system.
  • the exhaust gas stream preferably occurs in a high-pressure separator arranged downstream of a methanol synthesis unit, in which a gas stream is separated from a previously produced crude methanol.
  • an exhaust gas stream can arise, for example, in a distillation device arranged downstream of a methanol synthesis unit, in which water and / or gaseous or volatile substances are separated from the previously generated methanol, the exhaust gas stream then being fed to the second plant, which is connected to the plant for the production of Methanol is connected in the network.
  • a liquid stream separated in the high-pressure separator can first be fed to a distillation device in which water and / or gaseous or volatile substances are separated from the methanol previously generated, with an in this distillation device separated waste gas stream is then fed to the second plant.
  • the second system can be systems of the most varied types which are set up in such a way that an exhaust gas flow can also be supplied and burned, even if the exhaust gas flow itself consists at least partially of non-combustible components such as carbon dioxide.
  • such systems are suitable as the second system in which a device for the combustion of a gas flow is already present.
  • This can be, for example, a power plant, a steelworks, a waste incineration plant, a device for generating steam or electricity or a cement factory, to name just a few examples.
  • the second plant is usually a plant that has at least one combustion chamber, which then feeds the exhaust gas flow generated in the plant for the production of methanol or methane, usually via a suitable line system, can be fed.
  • the plant for the production of methanol or methane is connected in the network with the second plant to which the exhaust gas flow is fed, whereby it is generally the case that the two plants are spatially not too far apart are.
  • Connected in a network means that both plants are in some form in operative connection with each other, whereby it is usually the case that one or more lines in which one or more exhaust gas flows are conveyed from the plant for the production of methanol or methane lead to the second plant.
  • the second system can also be operated without interference without the exhaust gas flow.
  • second system used in the application is not to be understood as restrictive in the sense that the system network only comprises a total of two systems. Rather, it can of course also be a system network consisting of a system for the production of methanol or methane and one, two, three or more other systems, with the exhaust gas stream that is generated in the system for the production of methanol or methane also being divided up in principle and, for example, partially fed to a second and partially to a third system connected in conjunction with the exhaust-gas generating system and can be burned there.
  • a nitrogen-containing purge gas stream which is used to purge at least a portion of the plant for the production of methanol or methane, or which arises in a water electrolysis for the production of hydrogen, the composition of this purge gas flow possibly being different from that in the production of methanol or methane accumulating exhaust gas flow is different, are also fed to the second plant for the purpose of combustion in this.
  • the aforementioned purge gas stream has, in particular, a composition which can be different from that of the exhaust gas stream. Furthermore, it may be the case that the amount of Purge gas that occurs in the plant for the production of methanol or methane, can be greater than the amount of exhaust gas generated in this plant.
  • the composition of such a purge gas flow is often not constant, but rather variable. It can also be the case that the purge gas flow does not occur continuously, but only temporarily.
  • the purge gas stream contains at least nitrogen in addition to other components. Alternatively, you can flush with hydrogen instead of nitrogen. This may be advantageous for the catalyst, so that it is then also possible to purge only the reactor with hydrogen.
  • a possible optional variant of the method according to the invention provides that in the plant for the production of methanol or methane upstream of the methanol or methane synthesis reactor, a further gas stream is added to the feed gas stream, which in particular contains hydrogen and / or carbon monoxide and / or carbon dioxide.
  • the further gas stream mentioned can in principle contain the three components hydrogen, carbon monoxide and carbon dioxide in any desired composition.
  • a possible alternative variant of the method according to the invention provides that the first plant is not a plant for the production of methanol, but a plant for the production of methane or synthetic natural gas (SNG), and that a gas flow occurring there is discontinuous or continuously accumulates, this gas flow being an exhaust gas flow or flushing gas flow or a gas flow which does not correspond to a desired specification with regard to the gas composition (off spec gas flow) and that this gas flow is fed to the second plant.
  • Synthetic natural gas (SNG) usually contains the vast majority of methane.
  • the synthetic natural gas contains at least 95% methane and also smaller amounts of carbon monoxide, hydrogen, nitrogen, noble gases and carbon dioxide.
  • the composition varies depending on the details of the manufacturing process.
  • FIG. 1 shows a schematically simplified representation of the essential components of a plant according to the invention for the production of methanol
  • FIG. 2 shows a schematically simplified representation of a similar plant for the production of methanol according to an exemplary alternative embodiment of the present invention
  • FIG. 3 shows a schematically simplified representation of a further plant for the production of methanol according to an exemplary alternative embodiment of the present invention
  • FIG. 4 shows a schematically simplified representation of an alternative embodiment variant of the invention in which a plant for the production of methane (SNG) is used.
  • SNG methane
  • FIG. 1 is a so-called “small-scale” system, ie a small system with a capacity of the order of magnitude, for example, less than about 300 t / day.
  • An external source of carbon dioxide is provided, which can be present in cryogenic form, for example, and is fed to an evaporator, from where the CO 2 passes in gaseous form via a line 11 into a compressor 12.
  • the second starting material for the production of methanol is hydrogen, which is obtained, for example, electrolytically from water.
  • electricity 13 obtained from regenerative energies is preferably used in order to operate the electrolysis device 14.
  • the starting material for the electrolysis is water, which is initially passed via a line 15, if necessary, into a treatment device 16 in which, for example, reverse osmosis and / or ion exchange is provided. From there, the treated water reaches the electrolysis device 14 as an educt via the line 17.
  • the waste water from the treatment device 16 can be discharged from the system via the sewage line 10, for example.
  • oxygen is also produced, which is derived from the electrolysis device 14 via a line 18 and a suitable one
  • Purpose of use can be fed outside the system.
  • the one in electrolysis The hydrogen produced is fed via line 20 to the compressor 12, to which the C0 2 is also fed via line 11. From the compressor 12, the combined starting material mixture of CO 2 and H 2 is then fed as a feed gas stream via line 21 into the methanol synthesis reactor 22.
  • the methanol synthesis takes place in the methanol synthesis reactor 22 and the product stream leaving this reactor is fed to a high pressure separator 24 via the line 23. From this, a return line 25 can be provided to a compressor 19, in which a gas mixture still containing educt, which was separated from the product flow in the high pressure separator 24, is compressed and, after compression, is returned and via the line 21 into which the return line from the compressor 19 opens, is fed back to the methanol synthesis reactor 22.
  • this methanol synthesis reactor 22 operates at an elevated temperature, for example in the order of 200 ° C. to 300 ° C. and at an elevated pressure which can be, for example, in a range from approximately 30 bar to 100 bar.
  • a catalyst is usually used for the methanol synthesis.
  • the methanol-containing product stream that leaves the methanol synthesis reactor 22 is fed to the high-pressure separator 24, leaves it via line 27, and is then optionally fed to a low-pressure separator 28, in which a further separation of gases from the methanol-containing product stream takes place.
  • This raw methanol is further purified in a distillation device 30 connected to the low-pressure separator 28 via a line, in which, on the one hand, volatile components are separated off, which can be diverted from the top of the distillation device 30 via a line 34 and returned to an area upstream the compressor 12.
  • volatile components are separated off, which can be diverted from the top of the distillation device 30 via a line 34 and returned to an area upstream the compressor 12.
  • water can be separated from the methanol via the sump in the distillation device 30 and the process water in this system can be discharged from the system via the line 41.
  • the methanol is then discharged from the system in a high degree of purity via line 32 via a side draw and can be stored in tanks, for example.
  • the exhaust gas flow is fed as a proportionately smaller inflow to a combustion chamber in which a proportionately larger gas flow is burned.
  • the fluid flow of the volatile components separated in the distillation device 30 is returned as a recycle flow via the return line 34 to an area which is upstream of the first compressor or a first compressor stage 12 and upstream of the methanol synthesis reactor 22.
  • the process gas compressor (the compressor stage) 12 is supplied on the one hand with the hydrogen from the electrolysis 14 and also this recycling flow from the return line 34.
  • the mixture leaving the first compressor 12, consisting of the feed stream and the cycle gas from the line 34, is then Before it reaches the methanol synthesis reactor 22, the circulating gas returned from the high pressure separator 24 via the return line 25 is additionally supplied after it has been compressed in the compressor 19, and this combined gas mixture then passes via the line 21 into the methanol synthesis 22.
  • the water that accumulates in the sump during the distillation 30 cannot be discharged from the system, but instead can be circulated back into the water electrolysis 14 via the return line 41 as process water. If necessary, this water separated off in the distillation can also be treated first, for example to remove methanol by a suitable process.
  • An exhaust gas stream which, in the embodiment according to FIG. 1, is discharged from the system via the exhaust gas line 40 after separation in the high-pressure separator 24, can, for example, have the following composition, which is typical for such an exhaust gas stream from a methanol system:
  • FIG. 2 shows an alternative embodiment variant of a plant according to the invention for the production of methanol, in which the structure is largely similar to that of the embodiment variant described above with reference to FIG.
  • the same parts of the plant are therefore denoted by the same reference numerals as in FIG. 1 and are only briefly explained below, with additional reference being made to the above statements relating to FIG.
  • These are in particular the inlet line 11 for the carbon dioxide, the line 13 for the power supply, the inlet line 15 for water, which is treated in the device 16, the electrolysis device 14, the feed stream compressor 12, the methanol synthesis reactor 22, the high pressure separator 24, the return line 25 from the high pressure separator 24, the further compressor 19, the low pressure separator 28 and the distillation device 30.
  • the main difference to the embodiment variant described above lies in the variant according to FIG. 2 that the circulating gas flow via the return line 34 from the top of the distillation device 30 back to the area in front of the compressor 12 is omitted and instead an additional exhaust gas flow via the line 33 at the top of the distillation device 30 is discharged from the plant for the production of methanol.
  • This exhaust gas stream thus contains the more volatile components separated from the methanol product stream 32 in the distillation device 30.
  • This exhaust gas flow can be fed via the line 33 together with the exhaust gas flow via the line 40 to a second system, not shown here, which is present in the system for the production of methanol shown in FIG. 2 and is fed to a combustion there, so that in this Variant of the interconnection of the system, the circulating gas flow via line 34 can be omitted.
  • the amount of exhaust gas for this stream is about 20 kg / h for a capacity of 12 tpd (tons per day) of methanol.
  • FIG. 3 shows a further alternative embodiment of the method according to the invention, this being a simplified concept of a smaller (small-scale) plant for the production of methanol.
  • the same parts of the system are again provided with the same reference numerals as in the exemplary embodiments described above.
  • the supply line 11 for carbon dioxide, the electrolysis device 14, the compressor 12 for the feed gas flow, the processing device 16 for the supplied water, the methanol synthesis reactor 22, the high pressure separator 24, the low pressure separator 28 and the Distillation device 30 In contrast to the variant of FIG. 1, the return line 34 for circulating gas from the distillation device 30 is also omitted here.
  • the gas phase from the low-pressure separator 28 is introduced directly into the distillation device (distillation column) 30 via a further line 45.
  • the return line 25 emanating from the high pressure separator 24 is missing here.
  • the flow of the more volatile components separated in the high pressure separator 24 is discharged via a line 44, which opens into the further line 45 downstream of the low pressure separator 28 or directly into the distillation device 30 (not shown in the figures). The combined flow of the more volatile components from the high pressure separator 24 and the low pressure separator 28 is then introduced into the distillation device 30 via this line 45.
  • FIG. 3 shows a greatly simplified concept without a recycle stream.
  • the concept shown there has the disadvantage that the efficiency of such a system is lower and only a little C0 2 is bound.
  • the exhaust gas flow would be considerably greater than in the variants according to FIGS. 1 and 2 and the composition would be considerably different from exhaust gas flow 40.
  • HP high pressure range
  • FIG. 4 shows an alternative variant of the invention in which methane (SNG) is synthesized instead of methanol and consequently the reactor units 22 and 46 are each a methane synthesis reactor.
  • the methanation can also be carried out in one stage.
  • the feed gas mixture arrives first in a methanation reactor 22, which forms a first stage of methanation, is then fed via line 23 to a high pressure separator 24 and then reaches a second methanation stage 46, which is followed by a second high pressure separator 47.
  • the more volatile components separated there contain the product gas methane and are fed via a line 48 to a high-pressure absorber 49, from which the methane can be discharged as a product stream via the line 50.
  • the water occurring in the high-pressure separators 24 and 47 is fed to a low-pressure separator 28, in which the dissolved components are separated from the process water, which can be returned to the water electrolysis 14 via the return line 51.
  • a low-pressure separator 28 in which the dissolved components are separated from the process water, which can be returned to the water electrolysis 14 via the return line 51.
  • an exhaust gas flow 52 occurs in the low-pressure separator 28, which can then be fed to a second system, not shown here, as described above.
  • SNG synthetic natural gas
  • the amount of exhaust gas is less than 0.5 kg / h with a plant capacity of approximately 900 kg / d (kg per day) methane.
  • HP high pressure range: greater than 10 bar (for example 16 bara)

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention concerne un procédé pour la préparation de méthanol ou de méthane par transformation d'hydrogène avec du dioxyde de carbone, au moins un flux de gaz d'échappement (40, 52) produit dans l'installation pour la préparation de méthanol ou de méthane étant dévié de cette installation et ce flux de gaz d'échappement dévié étant fourni à une deuxième installation, qui est connectée en réseau avec l'installation pour la préparation de méthanol ou de méthane, le flux de gaz échappement étant brûlé dans cette deuxième installation. Ce flux de gaz échappement (40, 52), qui est fourni à la deuxième installation, contient une proportion d'au moins 20 % en poids de dioxyde de carbone et une proportion inférieure à 20 % en poids de monoxyde de carbone ainsi qu'également éventuellement de l'hydrogène. Ce flux de gaz échappement (40, 52) peut en être un qui est majoritairement constitué de gaz non combustibles comme le dioxyde de carbone. Du fait de la solution selon l'invention, une purification catalytique de gaz d'échappement est par exemple supprimée ou une torche, qui est sinon habituellement nécessaire, lorsque le flux de gaz d'échappement, conformément aux exigences en matière d'émissions, doit être relâché dans l'environnement, est supprimée et le flux de gaz d'échappement peut être éliminé sans grand effort dans la deuxième installation, éventuellement avec l'utilisation de l'énergie résiduelle contenue dans le flux de gaz échappement.
PCT/EP2020/055679 2019-03-06 2020-03-04 Procédé pour la préparation de méthanol ou de méthane WO2020178330A1 (fr)

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DE102019203065.3A DE102019203065A1 (de) 2019-03-06 2019-03-06 Verfahren zur Herstellung von Methanol oder Methan
DE102019203065.3 2019-03-06

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