CN113120860A - Method for preparing high-purity hydrogen by methanol two-phase reforming - Google Patents
Method for preparing high-purity hydrogen by methanol two-phase reforming Download PDFInfo
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- CN113120860A CN113120860A CN202110305795.7A CN202110305795A CN113120860A CN 113120860 A CN113120860 A CN 113120860A CN 202110305795 A CN202110305795 A CN 202110305795A CN 113120860 A CN113120860 A CN 113120860A
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 38
- 239000001257 hydrogen Substances 0.000 title claims abstract description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000002407 reforming Methods 0.000 title description 12
- 239000012071 phase Substances 0.000 claims abstract description 19
- 239000007791 liquid phase Substances 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims description 35
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 11
- 239000011029 spinel Substances 0.000 claims description 9
- 229910052596 spinel Inorganic materials 0.000 claims description 9
- -1 magnesium aluminate Chemical class 0.000 claims description 8
- 229910000510 noble metal Inorganic materials 0.000 claims description 6
- 238000011068 loading method Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 239000011865 Pt-based catalyst Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000007868 Raney catalyst Substances 0.000 claims description 2
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 2
- 229910007470 ZnO—Al2O3 Inorganic materials 0.000 claims description 2
- 229910007676 ZnO—SiO2 Inorganic materials 0.000 claims description 2
- 229910000808 amorphous metal alloy Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000001833 catalytic reforming Methods 0.000 claims description 2
- 238000000975 co-precipitation Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims description 2
- DOARWPHSJVUWFT-UHFFFAOYSA-N lanthanum nickel Chemical compound [Ni].[La] DOARWPHSJVUWFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical group 0.000 claims description 2
- 238000006057 reforming reaction Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 27
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 238000000508 aqueous-phase reforming Methods 0.000 abstract description 8
- 239000007864 aqueous solution Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000446 fuel Substances 0.000 description 6
- 238000001651 catalytic steam reforming of methanol Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 239000002803 fossil fuel Substances 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000000629 steam reforming Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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
- C01B3/32—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
- C01B3/323—Catalytic reaction of gaseous or liquid organic compounds other than hydrocarbons with gasifying agents
-
- 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
- C01B2203/02—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
-
- 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
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal 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
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
- C01B2203/1052—Nickel or cobalt catalysts
- C01B2203/1058—Nickel 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
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
- C01B2203/1064—Platinum group metal catalysts
- C01B2203/107—Platinum 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
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1076—Copper or zinc-based 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
- C01B2203/12—Feeding the process for making hydrogen or synthesis gas
- C01B2203/1205—Composition of the feed
- C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
- C01B2203/1217—Alcohols
- C01B2203/1223—Methanol
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Hydrogen, Water And Hydrids (AREA)
Abstract
The invention discloses a method for efficiently producing hydrogen from methanol, and belongs to the technical field of hydrogen preparation. The method controls the existence phase state of the methanol aqueous solution in the reaction system to enable the methanol aqueous solution to simultaneously exist a gas phase and a liquid phase, and controls the proportion of the gas phase and the liquid phase to realize the high-efficiency hydrogen production of the methanol, and the CO content in the product is extremely low. Compared with the traditional gas phase hydrogen production, the method can effectively reduce the content of CO in the product. Compared with aqueous phase reforming, the technology can greatly improve the conversion rate of methanol.
Description
Technical Field
The invention relates to a novel method for preparing hydrogen by reforming methanol, belonging to the technical field of hydrogen preparation.
Background
The development and utilization of new energy sources are the urgent necessity for the development of the current human society. Hydrogen energy is the cleanest and most efficient energy source of secondary energy sources. In view of the many advantages and important roles of hydrogen energy in future markets, many countries tighten the deployment and implementation of hydrogen energy strategies. However, hydrogen energy is the same as electric energy, has no direct resource storage on the earth, and is obtained by conversion from other primary energy sources, so that the hydrogen energy belongs to secondary energy sources.
Hydrogen is a promising renewable energy source, and the use of fuel cell vehicles in particular further expands the use of hydrogen. But because hydrogen is a very light gas, it contains much less energy per unit volume than conventional liquid fuels at the same pressure. Thus, the use of storage materials to release the required hydrogen in situ is a very promising route. At present, the hydrogen production technology in the world mainly comprises hydrogen production by fossil fuel, hydrogen production by hydrolysis and hydrogen production by biomass. Wherein, the hydrogen production by fossil fuel and the hydrogen production by biomass can be realized by a methanol platform. Both fossil fuels and biomass can be converted to syngas, which can then be used to synthesize methanol. The methanol hydrogen production has important application in small-sized oil refining hydrogenation devices and mobile source hydrogenation devices, and especially has very important potential value in the aspect of in-situ hydrogen production of hydrogen energy fuel cells for vehicles.
The methanol and the water which are cheap, easy to store and transport and high in hydrogen content are used for reforming to generate the hydrogen in situ, so that the hydrogen becomes an important component of a future fuel cell automobile. Research today on the production of hydrogen by reforming methanol and water includes steam reforming and aqueous phase reforming. The CO selectivity of methanol steam reforming is very high, which cannot meet the use of fuel cells, methanol steam reforming, namely gas phase reforming, is mainly adopted for hydrogen production by methanol reforming, and the reaction of methanol and water after vaporization is commercialized, and the used catalyst is a copper-zinc-aluminum catalyst. But the Cu catalyst is easily oxidized by water at the reaction temperature of 250 ℃ and 300 ℃. Noble metal catalysts, other than Cu-based catalysts, are generally supported on oxides, but on oxide-supported noble metal catalysts, methanol is more susceptible to decomposition reactions, resulting in very high CO content, which far exceeds the tolerance of fuel cells.
In addition to methanol steam reforming, the prior art also includes methanol aqueous phase reforming, i.e., pressurizing the reaction system to keep both methanol and water in liquid phase in the system. The methanol aqueous phase reforming CO selectivity is very low. This may be due to the different activities of the coal-water vapor shift reaction under the two conditions. However, in the aqueous phase reforming technology, the methanol conversion rate still needs to be improved under the condition of higher space velocity. For example, we report a space velocity of 1.47h under continuous flow aqueous phase reforming conditions-1When the catalyst is used, the conversion rate of the methanol can reach 100 percent, but the space velocity is increased to 5.88h-1When the conversion rate is reduced to about 40% (ACS Catalysis,2019, 9, 9671-9682).
In summary, it can be seen that hydrogen produced by steam reforming of methanol in the prior art has a high CO content, while aqueous phase reforming can effectively reduce the CO content, but the methanol conversion rate is severely reduced at high space velocity.
Disclosure of Invention
The invention aims to overcome the defects of high CO content in methanol steam reforming and low conversion rate of aqueous phase reforming when the space velocity is increased in the prior art, provide a novel method for preparing hydrogen by methanol reforming, and simultaneously give consideration to low CO content and relatively high conversion rate under high space velocity.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for preparing hydrogen by methanol gas-liquid phase catalytic reforming, which comprises the step of carrying out reforming reaction on methanol and water under the condition of a certain gas-liquid phase ratio and the existence of a catalyst, and is characterized in that the methanol and the water must exist in a gas phase and a liquid phase simultaneously, and the gas-liquid phase ratio meets a strict numerical range at a specific temperature.
Further, the gas-liquid phase ratio of methanol to water is such that the gas-liquid phase ratio of the total feed is in the range of 0.25 to 9, preferably 0.43 to 4.
Further, in order to realize the reforming process, the catalyst is one or more of a noble metal Pt-based catalyst, a non-noble metal Ni-based catalyst, a Fe-based catalyst and a Cu-based catalyst.
Alternatively, the Pt-based catalyst is a supported catalyst and the support is a metal oxide alumina, a spinel such as magnesium aluminate spinel, nickel aluminate spinel, a perovskite such as lanthanum nickel perovskite, carbon, and the like. Preferably nickel aluminate spinel.
Alternatively, the loading of Pt is 0.1% to 5%, preferably 0.2% to 1.2%. The supporting method is impregnation or coprecipitation.
Alternatively, the Ni-based catalyst is supported or skeletal. The supported carrier according to claim 5, wherein the Ni content is 1 to 50%, preferably 3 to 20%. The skeleton type Ni catalyst may be one or several of Raney nickel, NiB and NiP amorphous alloy.
Alternatively, the Fe-based catalyst is a composite oxide catalyst including, but not limited to FeCrOx, FeAlOx, and the like.
Alternatively, the Cu-based catalyst is CuO-ZnO-Al2O3、CuO-ZnO-SiO2One or more of them.
Further, the molar ratio of methanol to water is 0.01 to 1.0, preferably 0.05 to 0.8.
Further, the space velocity of the raw materials including methanol and water is 0.1-15 h-1Preferably 1-5 h-1。
The invention has the following beneficial effects:
(1) under the same reaction temperature, the conversion rate of gas-liquid two-phase reformed methanol is high; (2) the CO concentration of the prepared hydrogen is low, generally lower than 100ppm and can reach 10ppm at least.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1:
the gas-liquid two-phase reforming of methanol was carried out in a fixed bed reactor with an internal diameter of 6 mm. The catalyst is a nickel aluminate spinel catalyst loaded with 1wt% of Pt, the loading amount is 1mL, and the space velocity is 5.88h-1. By adjusting the pressure and temperature of the reaction system, the aqueous methanol solution with the concentration of 10wt% exists in a gas-liquid two-phase manner in the reaction system, and the ratio is 0.67. And reacting for 20h, and sampling and analyzing the concentrations of products such as hydrogen, CO and the like when the system is balanced.
Example 2:
the conditions were the same as in example 1 except that the gas-liquid two-phase ratio was adjusted to 1.5.
Example 3:
the conditions were the same as in example 1 except that the gas-liquid two-phase ratio was adjusted to 4.
Comparative example 1:
the conditions were the same as in example 1 except that the methanol aqueous solution was entirely present in the reaction system in the form of a gas phase.
Comparative example 2:
the conditions were the same as in example 1 except that the aqueous methanol solution was entirely present in the reaction system in the liquid phase.
Example 4:
the conditions were as in example 1 except that the catalyst was changed to Pt/Al2O3。
Comparative example 3:
the conditions were the same as in example 4 except that the methanol aqueous solution was entirely present in the reaction system in the form of a gas phase.
Comparative example 4:
the conditions were the same as in example 4 except that the aqueous methanol solution was entirely present in the reaction system in the liquid phase.
Example 5:
the conditions were as in example 1 except that the catalyst was changed to Pt/SiO2。
Comparative example 5:
the conditions were the same as in example 5 except that the methanol aqueous solution was entirely present in the reaction system in the form of a gas phase.
Comparative example 6:
the conditions were the same as in example 5 except that the aqueous methanol solution was entirely present in the reaction system in the liquid phase.
The results of the examples and comparative examples are shown in Table 1.
Table 1 comparison of the activity of the methanol reforming hydrogen production reaction.
It can be seen from table 1 that the gas-liquid two-phase reforming technique of the present invention performed on the same catalyst was excellent in both increasing the methanol conversion and reducing the CO concentration in the product.
Description of the drawings: the gas-liquid two-phase ratio in the embodiment of the invention is obtained by calculation through thermodynamic data (AspenPlus software is used for calculation in the invention), and the reaction temperature is 210oAnd C, controlling the gas-liquid two-phase ratio by controlling the reaction pressure of the system.
Claims (10)
1. A method for preparing hydrogen by methanol gas-liquid phase catalytic reforming, which comprises the step of carrying out reforming reaction on methanol and water under the condition of a certain gas-liquid phase ratio and the existence of a catalyst, and is characterized in that the methanol and the water must exist in a gas phase and a liquid phase simultaneously, and the gas-liquid phase ratio meets a strict numerical range at a specific temperature.
2. According to claim 1, the gas-liquid ratio of methanol to water is such that the gas-liquid ratio of the total feed is between 0.25 and 9, preferably between 0.43 and 4.
3. The catalyst according to claim 2, wherein the catalyst is one or more of a noble metal Pt-based catalyst, a non-noble metal Ni-based catalyst, a Fe-based catalyst and a Cu-based catalyst.
4. According to claim 3, the Pt-based catalyst is a supported catalyst, the support is a metal oxide alumina, a spinel such as magnesium aluminate spinel, nickel aluminate spinel, a perovskite such as lanthanum nickel perovskite, carbon, etc., preferably nickel aluminate spinel.
5. According to claim 4, the Pt loading is 0.1-5%, preferably 0.3-1.2%, and the loading method is impregnation or coprecipitation.
6. According to claim 3, the Ni-based catalyst is supported or skeleton type, the supported carrier is the same as the supported carrier in claim 5, the Ni loading is 1-50%, preferably 3-20%, and the skeleton type Ni catalyst can be one or more of Raney nickel, NiB and NiP amorphous alloy.
7. According to claim 3, the Fe-based catalyst is a composite oxide catalyst including but not limited to FeCrOx, FeAlOx, and the like.
8. According to claim 3, the Cu-based catalyst is CuO-ZnO-Al2O3、CuO-ZnO-SiO2One or more of them.
9. According to claims 1-8, the molar ratio of methanol to water is 0.01-1.0, preferably 0.05-0.8.
10. The process of claims 1 to 9, wherein the space velocity of the feedstock comprising methanol and water is between 0.1 and 15 h-1Preferably 1-5 h-1。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110305795.7A CN113120860A (en) | 2021-03-23 | 2021-03-23 | Method for preparing high-purity hydrogen by methanol two-phase reforming |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110305795.7A CN113120860A (en) | 2021-03-23 | 2021-03-23 | Method for preparing high-purity hydrogen by methanol two-phase reforming |
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| Publication Number | Publication Date |
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| CN113120860A true CN113120860A (en) | 2021-07-16 |
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|---|---|---|---|
| CN202110305795.7A Pending CN113120860A (en) | 2021-03-23 | 2021-03-23 | Method for preparing high-purity hydrogen by methanol two-phase reforming |
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| CN (1) | CN113120860A (en) |
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- 2021-03-23 CN CN202110305795.7A patent/CN113120860A/en active Pending
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