WO2017141138A1 - Conversion of adjusted methane steam reforming gas composition with co2 for the production of syngas composition for oxo-synthesis - Google Patents
Conversion of adjusted methane steam reforming gas composition with co2 for the production of syngas composition for oxo-synthesis Download PDFInfo
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- WO2017141138A1 WO2017141138A1 PCT/IB2017/050681 IB2017050681W WO2017141138A1 WO 2017141138 A1 WO2017141138 A1 WO 2017141138A1 IB 2017050681 W IB2017050681 W IB 2017050681W WO 2017141138 A1 WO2017141138 A1 WO 2017141138A1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/49—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide
- C07C45/50—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide by oxo-reactions
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- 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
- C01B3/32—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
- C01B3/34—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 by reaction of hydrocarbons with gasifying agents
- C01B3/38—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 by reaction of hydrocarbons with gasifying agents using catalysts
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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
- C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
- C01B2203/0233—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being a steam reforming step
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- 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
- C01B2203/06—Integration with other chemical processes
- C01B2203/063—Refinery processes
- C01B2203/065—Refinery processes using hydrotreating, e.g. hydrogenation, hydrodesulfurisation
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Abstract
Methods of preparing syngas are provided. Blend gas obtained from methane steam reforming can be reacted with CO2 in the presence of a catalyst to provide syngas with a composition ideal for oxo-synthesis.
Description
CONVERSION OF ADJUSTED METHANE STEAM REFORMING GAS COMPOSITION WITH C02 FOR THE PRODUCTION OF SYNGAS
COMPOSITION FOR OXO-SYNTHESIS
CROSS-REFERENCE TO RELATED APPLICATIONS [0001] This application claims the benefit of priority of U.S. Provisional Patent Application No. 62/295,579, filed February 16, 2016, which is hereby incorporated by reference in its entirety.
FIELD
[0002] The presently disclosed subject matter relates to methods for production of synthesis gas with a composition ideal for oxo-synthesis.
BACKGROUND
[0003] Synthesis gas (also known as syngas) is a mixture of carbon monoxide (CO) and hydrogen (H2). Syngas can be prepared in a number of different ways including through a reverse water gas shift (RWGS) reaction or methane steam reforming. The steam reforming reaction can be described by the following equation:
CH4 + H20≠CO + 3H2 (1) and occurs in the presence of a metal catalyst at high temperatures. The reaction can produce some amounts of C02, through the water shift reaction, thereby creating an overall product blend gas composition that includes C02, H2, and CO. The water shift reaction can be described by the following equation:
CO+ H2O^C02+ H20 (2)
[0004] Syngas is a versatile mixture that can be used to prepare light olefins, methanol, acetic acid, aldehydes, and many other important industrial chemicals. However, the efficiency of the preparation of different chemicals, for example, aldehydes and methanol, from syngas can depend on the composition of the syngas. Syngas containing H2 and CO in a molar ratio (H2:CO) of about 1 : 1 can be useful for producing aldehydes and alcohols, e.g.,
oxo-synthesis, whereas a molar ratio of more than 4.5 : 1 can be useful for methanol synthesis. Syngas produced by methane steam reforming is typically suitable only for methanol synthesis. In order to use syngas produced by methane steam reforming for applications such as oxo-synthesis, the molar ratio of H2 and CO must be adjusted to closer to stoichiometric.
[0005] Thus, there remains a need in the art for new methods for producing syngas with ideal molar ratios of H2:CO for different synthesis applications.
SUMMARY OF THE DISCLOSED SUBJECT MATTER
[0006] The presently disclosed subject matter provides for processes for C02 hydrogenation, which can include feeding blend gas and C02 into a reactor. The blend gas can include CO, C02 and H2. The processes can further include forming hydrogenation reaction products with a catalyst at from about 580°C to about 630°C. The catalyst can include a fresh chromia-alumina catalyst. The processes can also include recovering hydrogenation reaction products H2 and CO in a ratio of from about 2: 1 to about 1 :2.
[0007] In certain embodiments, the blend gas comprises from about 10% to about 20% CO, from about 5% to about 20% C02 and from about 60% to about 80% H2.
[0008] In certain embodiments, the blend gas comprises about 14.2% CO, about 8.1% C02 and about 78.2% H2 or 21.7%CO , about 18.1%C02, and about 59.8%H2.
[0009] In certain embodiments, the reaction temperature is about 630 °C. In certain embodiments, the reaction temperature is about 600 °C. In certain embodiments, the reaction temperature is about 580 °C.
[0010] In certain embodiments, the product mixture can include H2 and CO in a molar ratio (H2:CO) of about 1 : 1 or about less than 1 : 1.
[0011] In certain embodiments, the product mixture can further include C02 and H20.
[0012] In certain embodiments, the reactor is a quartz or metal reactor.
[0013] In certain embodiments, C02 is present in a flow rate amount of from about 5 to
about 3000 cc/min. In certain embodiments, C02 is present in a flow rate amount of about 192 cc/min or about 217 cc/min.
[0014] In certain embodiments, the blend gas is present in a flow rate amount of from about 5 cc/min to about 3000 cc/min. In certain embodiments, the blend gas is present in a flow rate from about 150 cc/min to about 2500 cc/min.
[0015] In certain embodiments, C02 and blend gas is present in a ratio of about 1 : 1. In certain embodiments, the forming step further comprises an alkaline promoter.
[0016] The presently disclosed subject matter also provides for processes for C02 hydrogenation, which can include feeding blend gas and C02 into a reactor. The blend gas can include CO, C02 and H2. The processes can further include forming hydrogenation reaction products with a catalyst at from about 580°C to about 630°C. The catalyst can include a fresh chromia-alumina catalyst. The processes can also include recovering hydrogenation reaction products H2 and CO in a ratio of about 1 : 1. The processes can also include contacting the H2 and CO with a second catalyst and an olefin stream to form oxo- synthesis products.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] FIG. 1 is a schematic diagram presenting an exemplary process for preparation of syngas.
DETAILED DESCRIPTION
[0018] There remains a need in the art for new methods of preparing syngas with different ratios of H2:CO, e.g., ratios close to 1 : 1. The presently disclosed subject matter provides novel methods and catalysts for converting C02 and a blend gas mixture into syngas with H2:CO ratios close to 1 : 1. The presently disclosed subject matter includes the surprising discovery that syngas obtained from methane steam reforming processes can be reacted with C02 in the presence of a fresh chromia-alumina catalyst to achieve a ratio of H2:CO close to
1 : 1 in a product mixture.
[0019] As used herein, the term "about" or "approximately" means within an acceptable error range for the particular value as determined by one of ordinary skill in the art, which will depend in part on how the value is measured or determined, i.e., the limitations of the measurement system. For example, "about" can mean a range of up to 20%, up to 10%, up to 5%), and or up to 1% of a given value.
Reactors and Reaction Chambers
[0020] The methods of the present disclosure can involve fixed bed isothermal reactors suitable for reactions of gaseous reactants and reagents catalyzed by solid catalysts. The reactor can be constructed of any suitable materials capable of holding temperatures, for example from about 500°C to about 700°C. Non-limiting examples of such materials can include quartz, metals, alloys (including steel), glasses, ceramics or glass lined metals, and coated metals.
[0021] The dimensions of the reaction vessel and reaction chamber are variable and can depend on the production capacity, feed volume, and catalyst. The geometries of the reactor can be adjustable in various ways known to one of ordinary skill in the art.
[0022] In certain embodiments, reaction conditions within the reaction chamber can be isothermal. That is, hydrogenation of C02 can be conducted under isothermal conditions.
[0023] The pressure within the reaction chamber can be varied, as is known in the art. In certain embodiments, the pressure within the reaction chamber can be atmospheric pressure, i.e., about 1 bar. In certain embodiments, the pressure can be from about 1 bar to about 26 bar.
Catalysts
[0024] Catalysts suitable for use in conjunction with the presently disclosed matter can be catalysts capable of catalyzing hydrogenation of C02. More specifically, a suitable catalyst
shows high reaction rates, high olefin selectivity and has a longer stability.
[0025] In certain embodiments, the catalyst can be a metal oxide or mixed metal oxide. In specific embodiments, the catalyst can include one or more transition metals. More specifically, the catalyst can include chromium (Cr).
[0026] In certain embodiments, the catalyst can be a solid catalyst, e.g., a solid-supported catalyst. In certain embodiments, the catalyst can be located in a fixed packed bed, i.e., a catalyst fixed bed. In certain embodiments, the catalyst can include solid pellets, granules, plates, tablets, or rings.
[0027] In certain embodiments, the solid support can include zirconia (zirconium oxide), alumina (aluminum oxide), magnesia (magnesium oxide), SAPO-34 (silicoaluminophosphate) compositions, zeolites, and combinations thereof. The amount of the solid support present in the catalyst can be between about 15% and about 95%, by weight, relative to the total weight of the catalyst. By way of non-limiting example, the solid support can constitute about 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, or 95% of the total weight of the catalyst.
[0028] In certain embodiments, the catalyst can include about 1% to about 25% Cr, by weight. For example, the catalyst can include about 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 20%, 22%, or 25% Cr by weight. The remainder of the catalyst can be solid support (e.g., AI2O3).
[0029] In specific embodiments, the catalyst is a fresh Catofin® catalyst (Clariant). As used herein, a Catofin® catalyst is a chromia-alumina catalyst (CrOx/Al203) with an alkaline promotor. A promotor can be selected from the group consisting of alkaline earth metals, lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium, strontium, barium, tin, platinum-tin, zinc, copper, molybdenum, ruthenium, lanthanum and a combination thereof.
[0030] Other catalysts suitable for dehydrogenation of light alkanes to light olefins are also contemplated by the presently disclosed subject matter. Dehydration catalysts include chromium oxide support catalysts with promotors as discussed, platinum supported catalysts with one or more promotors and one or more Group VIII metals (i.e., iron (Fe), ruthenium (Ru), osmium (Os) and hassium (Hs)), vanadium oxide catalysts, molybdenum oxide catalysts, gallium supported catalysts, and carbon-based catalysts (e.g., carbon nanotubes and nanofibers).
Reaction Mixtures
[0031] The presently disclosed subject matter provides methods of converting H2 within a blend gas mixture and C02 into syngas. Blend gas can include a mixture of CO, C02, and H2. A mixture of blend gas and C02 can be termed a "reaction mixture." The mixture of blend gas and C02 can alternatively be termed a "feed mixture" or "feed gas."
[0032] The C02 in the reaction mixture can be derived from various sources. In certain embodiments, the C02 can be a waste product from an industrial process. In certain embodiments, C02 that remains unreacted can be recovered and recycled back into the reaction.
[0033] Reaction mixtures suitable for use with the presently disclosed methods can include various proportions of blend gas. In certain embodiments, the blend gas is obtained from a methane steam reforming process. In other embodiments, the blend gas is obtained from a C02 injected methane steam reforming process. In certain embodiments, the blend gas can include from about 5% to about 25% CO. In other embodiments, the blend gas can include from about 5% to about 25% C02. In additional embodiments, the blend gas can include from about 50% to 90% H2. In certain embodiments, the reaction mixture can include a blend gas comprising 14.2%CO + 8.1%C02+ 78.2%H2 or 21.7%CO + 18.1%C02+ 59.8%H2.
Methods of Preparing Syngas
[0034] The methods of the presently disclosed subject matter include methods of preparing syngas. In one embodiment, and with reference to FIG. 1, an exemplary method 100 can include providing a reaction chamber, as described above. The reaction chamber can include a solid-supported catalyst, e.g. a fresh Cr/Al203 catalyst as described above. The method can further include feeding blend gas and C02 into a reactor, wherein the blend gas includes CO, C02 and H2 101. The method can additionally include forming hydrogenation reaction products with the catalyst at from about 580°C to about 630°C 102. The method can also include recovering hydrogenation reaction products H2 and CO in a ratio of from about 2: 1 to about 1 :2 103. In further embodiments, the hydrogenation reaction products can undergo oxo-synthesis in the presence of a second catalyst and an olefin stream to produce alcohols and/or aldehydes.
[0035] The reaction mixture can be fed into the reaction chamber at various flow rates. The flow rate can be varied for each component of the reaction mixture, e.g., blend gas and C02, as is known in the art. In certain embodiments, the flow rate of the blend mixture can be from about 5 cc/min to about 3000 cc/min. In certain embodiments, the flow rate can be from about 150 cc/min to about 2500 cc/min. In certain embodiments, the flow rate can be about 192 or 217 cc/min. In certain embodiments, the flow rate of the C02 can be from about 5 cc/min to about 3000 cc/min. In certain embodiments, the flow rate can be from about 150 cc/min to about 500 cc/min. In certain embodiments, the flow rate of reaction components can be about 192 or 217 cc/min.
[0036] In certain embodiments, the ratio of C02:blend gas in the reaction mixture is from about 3 : 1 to about 1 :3. In other embodiments, the ratio of C02:blend gas in the reaction mixture is about 1 : 1, about 1.5: 1, or about 0.8: 1.
[0037] The flow rate of the components of the reaction and total gas mixture can be
selected to provide gas hour space velocity (GHSV) from about 280 to about 2400 h-1.
[0038] In certain embodiments, the catalyst is present in an amount of from about 1 to about 1000 mL. In certain embodiments, the catalyst is present in an amount of from about 2 to about 20 mL. In certain embodiments, the catalyst is present in an amount of about 9 ml or about 15 ml.
[0039] The reaction temperature can be understood to be the temperature within the reaction chamber. The reaction temperature can influence the hydrogenation reaction, including conversion of C02 and H2, the ratio of H2:CO in the product mixture, and the overall yield. In certain embodiments, the reaction temperature can be greater than 560 °C, e.g., greater than about 570 °C, 580 °C, 590 °C, 600 °C. In certain embodiments, the reaction temperature can be between about 500 °C and about 900 °C. In certain embodiments, the reaction temperature can be about 630 °C. In certain embodiments, the reaction temperature can be about 600 °C. In certain embodiments, the reaction temperature can be about 580 °C.
[0040] In certain embodiments, the product mixture can include H2 and CO in a molar ratio (H2:CO) of about 0.1 :3 to about 3 :0.1. In certain embodiments, the product mixture can include H2 and CO in a molar ratio (H2:CO) of from about 0.5:2 to about 2:0.5, e.g., about 0.5:2, 0.6:2, 0.7:2, 0.8:2, 0.9:2, 1 :2, 1.1 :2, 1.2:2, 1.3 :2, 1.4:2, 1.5:2, 1.6:2, 1.7:2, 1.8:2, or 1.9:2. In certain embodiments, the product mixture can include H2 and CO in a molar ratio (H2:CO) of about 1 : 1.
[0041] The methods of the presently disclosed subject matter can have advantages over other techniques for preparation of syngas from methane steam reforming gas. The presently disclosed subject matter includes the surprising discovery that the syngas composition can be varied by conversion with C02 in the presence of a fresh chromia-alumina catalyst. Smaller amounts of catalyst are required. Use of a fresh chromia-alumina catalyst can result in H2:CO ratios of about 1 : 1, ideal for use in oxo-synthesis.
EXAMPLES
[0042] The following examples are merely illustrative of the presently disclosed subject matter and should not be considered as limiting in any way.
EXAMPLE 1 - Hydrogenation of CO? with blend gas
[0043] A quartz reactor was charged with 9 ml of a fresh Catofin® catalyst (Clariant; fixed bed Cr/alumina catalyst). The reactor temperature was 600 °C. The catalyst particle size was 3x7 mm. A reaction mixture containing 21.7%CO + 18.1%C02+ 59.8%H2 at a flow rate of 192 cc/min and a stream of C02 at a flow rate of 192 cc/min was fed into the reactor, thereby contacting the reaction mixture with the catalyst and inducing a hydrogenation reaction. A product mixture containing H2, C02, and CO was removed from the reactor. The composition of the dry gas mixture after the reaction is presented in Table 1.
Table 1. Composition of dry gas
EXAMPLE 2 - Hydrogenation of CO? at 580 °C
[0044] The process of Example 1 was repeated with a change in flow rate and temperature. The blend gas was fed into the reactor at 192 cc/min and C02 at 192 cc/min. The reaction temperature was 580 °C. The composition of the dry gas mixture after the reaction is presented in Table 2.
Table 2. Composition of dry gas
EXAMPLE 3 - Hydrogenation of CO? at 630 °C
[0045] The process of Example 1 was repeated with a change in flow rate and temperature. The blend gas was fed into the reactor at 217 cc/min and C02 at 217 cc/min. The reaction temperature was 630 °C. The composition of the dry gas mixture after the reaction is presented in Table 3.
Table 3. Composition of dry gas
* * *
[0046] Although the presently disclosed subject matter and its advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the disclosed subject matter as defined by the appended claims. Moreover, the scope of the disclosed subject matter is not intended to be limited to the particular embodiments described in the specification. Accordingly, the appended claims are intended to include within their scope such alternatives.
Claims
1. A process for C02 hydrogenation, the process comprising:
a. feeding blend gas and C02 into a reactor, wherein the blend gas comprises CO, C02 and H2; and
b. contacting the blend gas and C02 with a fresh chromia-alumina catalyst at from about 580°C to about 630°C to form a product mixture comprising H2 and CO in a ratio of from about 2: 1 to about 1 :2.
2. The process of claim 1, wherein the blend gas comprises from about 10% to about 20% CO, from about 5% to about 20% C02 and from about 60% to about 80% H2.
3. The process of claim 2, wherein the blend gas comprises about 14.2% CO, about 8.1% C02 and about 78.2% H2.
4. The process of claim 2, wherein the blend gas comprises about 21.7%CO, about
18.1%C02, and about 59.8%H2.
5. The process of claim 1, wherein the reaction temperature is about 630 °C.
6. The process of claim 1, wherein the reaction temperature is about 600 °C.
7. The process of claim 1, wherein the reaction temperature is about 580 °C.
8. The process of claim 1, wherein the product mixture comprises H2 and CO in a molar ratio (H2:CO) of about 1 : 1.
9. The process of claim 1, wherein the product mixture comprises H2 and CO in a molar ratio (H2:CO) of about less than 1 : 1.
10. The process of claim 1, wherein the product mixture further comprises C02 and H20.
1 1. The process of claim 1, wherein the reactor is a quartz or metal reactor.
12. The process of claim 1, wherein C02 is present in a flow rate amount of from about 5 to about 3000 cc/min.
13. The process of claim 12, wherein C02 is present in a flow rate amount of about 192 cc/min.
14. The process of claim 12, wherein C02 is present in a flow rate amount of about 217 cc/min.
15. The process of claim 1, wherein the blend gas is present in a flow rate amount of from about 5 cc/min to about 3000 cc/min.
16. The process of claim 15, wherein the blend gas is present in a flow rate from about 150 cc/min to about 2500 cc/min.
17. The process of claim 1, wherein C02 and blend gas is present in a ratio of about 1 : 1 in step a).
18. The process of claim 1, wherein the forming step further comprises an alkaline
promoter.
19. The process of claim 1, wherein the blend gas is obtained from a methane steam
reforming reaction.
20. A process for C02 hydrogenation, the process comprising:
a. feeding blend gas and C02 into a reactor, wherein the blend gas comprises CO, C02 and H2;
b. contacting the blend gas and C02 with a fresh chromia-alumina catalyst at from about 580°C to about 630°C to form a product mixture comprising H2 and CO in a ratio of about 1 : 1; and
c. contacting the product mixture with a second catalyst and an olefin stream to form oxo-synthesis products.
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| US201662295579P | 2016-02-16 | 2016-02-16 | |
| US62/295,579 | 2016-02-16 |
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| US20040013605A1 (en) * | 2002-07-16 | 2004-01-22 | Conoco Inc. | Controlling syngas H2:CO ratio by controlling feed hydrocarbon composition |
| US20080031809A1 (en) * | 2006-07-18 | 2008-02-07 | Norbeck Joseph M | Controlling the synthesis gas composition of a steam methane reformer |
| US20100105962A1 (en) * | 2007-06-25 | 2010-04-29 | Saudi Basic Industries Corporation | Catalytic hydrogenation of carbon dioxide into syngas mixture |
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| US20130005838A1 (en) * | 2011-06-30 | 2013-01-03 | Neste Oil Oyj | Method for adjusting hydrogen to carbon monoxide ratio in synthesis gas |
| US8551434B1 (en) * | 2012-06-29 | 2013-10-08 | Saudi Basic Industries Corporation | Method of forming a syngas mixture |
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| US3271458A (en) * | 1962-11-23 | 1966-09-06 | Exxon Research Engineering Co | Cooling and catalyst recycle in oxo synthesis |
| US20040013605A1 (en) * | 2002-07-16 | 2004-01-22 | Conoco Inc. | Controlling syngas H2:CO ratio by controlling feed hydrocarbon composition |
| US20080031809A1 (en) * | 2006-07-18 | 2008-02-07 | Norbeck Joseph M | Controlling the synthesis gas composition of a steam methane reformer |
| US20100105962A1 (en) * | 2007-06-25 | 2010-04-29 | Saudi Basic Industries Corporation | Catalytic hydrogenation of carbon dioxide into syngas mixture |
| US20110301386A1 (en) * | 2008-12-17 | 2011-12-08 | Saudi Basic Industries Corporation | Process for Increasing the Carbon Monoxide Content of a Syngas Mixture |
| US20130005838A1 (en) * | 2011-06-30 | 2013-01-03 | Neste Oil Oyj | Method for adjusting hydrogen to carbon monoxide ratio in synthesis gas |
| US8551434B1 (en) * | 2012-06-29 | 2013-10-08 | Saudi Basic Industries Corporation | Method of forming a syngas mixture |
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