WO2004037716A1 - Procede et appareil de formation d'hydrogene au moyen d'alcool - Google Patents

Procede et appareil de formation d'hydrogene au moyen d'alcool Download PDF

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Publication number
WO2004037716A1
WO2004037716A1 PCT/JP2002/011138 JP0211138W WO2004037716A1 WO 2004037716 A1 WO2004037716 A1 WO 2004037716A1 JP 0211138 W JP0211138 W JP 0211138W WO 2004037716 A1 WO2004037716 A1 WO 2004037716A1
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Prior art keywords
hydrogen
alcohol
reactor
reaction
electrode
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PCT/JP2002/011138
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English (en)
Japanese (ja)
Inventor
Yasushi Sekine
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Yasushi Sekine
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Filing date
Publication date
Application filed by Yasushi Sekine filed Critical Yasushi Sekine
Priority to AU2002344021A priority Critical patent/AU2002344021A1/en
Priority to PCT/JP2002/011138 priority patent/WO2004037716A1/fr
Publication of WO2004037716A1 publication Critical patent/WO2004037716A1/fr

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    • 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
    • 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
    • C01B2203/0211—Processes for making hydrogen or synthesis gas containing a reforming step containing a non-catalytic reforming step
    • C01B2203/0216—Processes for making hydrogen or synthesis gas containing a reforming step containing a non-catalytic reforming step containing a non-catalytic 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
    • C01B2203/08—Methods of heating or cooling
    • C01B2203/0805—Methods of heating the process for making hydrogen or synthesis gas
    • C01B2203/0861—Methods of heating the process for making hydrogen or synthesis gas by plasma
    • 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

Definitions

  • the present invention relates to a method and an apparatus for producing hydrogen. Background art
  • Hydrogen is an important industrial gas, and has been widely used in the synthesis of ammonia and methanol, hydrodesulfurization, hydrocracking, hydrogenation of oils and fats, welding, and semiconductor manufacturing. Recently, new fields of use, such as reactants in fuel cells and fuels for automobiles, aircraft, power generation, and kitchens, are attracting attention.
  • steam reforming As a method for producing hydrogen, a method of reacting alcohol with water vapor (steam reforming) is conventionally known. Steam reforming is also called steam reforming, and is specifically represented by the following chemical reaction formula (1) or (2).
  • the present inventor has conducted intensive studies in view of the above-mentioned conventional situation, and as a result, the present invention can be carried out at a lower temperature and normal pressure than the conventional method, and can be carried out without using a catalyst.
  • New steam riff with high conversion rate and no miscellaneous side reactions We have found a forming method and have already filed a patent application (Japanese Patent Application No. 2000-15032).
  • a direct-current pulse discharge is performed in a mixed gas containing gaseous chain hydrocarbons and water vapor to react the chain hydrocarbons and water vapor to generate hydrogen and carbon monoxide. It can be implemented with a low-cost, small-sized, portable reactor.For example, natural gas is converted into gasoline, transported to consuming areas, supplied to automobiles, etc., reformed, and converted to fuel cells. It is expected to be used for hydrogen supply.
  • the method according to the above-mentioned application uses gasoline or the like as a raw material, and has a problem that by-products are slightly generated.
  • the present invention is a production method that can be carried out at a lower temperature and normal pressure and at lower cost than in the past, and can efficiently obtain hydrogen with a high yield. Therefore, it is an object of the present invention to provide a novel production method and an apparatus that do not deposit carbon or generate by-products such as acetylene. Disclosure of the invention
  • the method of the present invention comprises: performing a pulse discharge in a raw material gas containing a gaseous alcohol and water vapor to induce a reaction between the alcohol and the water vapor to generate hydrogen. It is characterized by making it. Further, in a source gas containing a gaseous alcohol, a pulse discharge is performed to induce a reaction of the alcohol to generate hydrogen.
  • FIG. 1 is a diagram showing an embodiment of the hydrogen generator of the present invention. BEST MODE FOR CARRYING OUT THE INVENTION
  • the present invention is characterized in that a pulse discharge is performed in a raw material gas containing a gaseous alcohol and water vapor to induce a reaction between the alcohol and the water vapor to generate hydrogen.
  • a reforming reaction between alcohol and water vapor occurs due to the pulse discharge, and as a result, the target hydrogen is efficiently produced in a high yield as in the above-described case. Is done.
  • alcohol may be involved in the reaction as a result, and thus includes a case where ether is used as a raw material, and the ether is hydrolyzed to alcohol, and the alcohol reacts.
  • the present invention is characterized in that a pulse discharge is performed in a raw material gas containing a gaseous alcohol to induce a reaction of the alcohol to generate hydrogen.
  • the decomposition reaction of the alcohol is caused by the pulse discharge, and as a result, the target hydrogen is efficiently produced at a high yield.
  • This reaction can be performed, for example, at a low temperature of 80 to 120 ° C. and at normal pressure, depending on the type of alcohol.
  • the present invention is characterized in that the above production method is performed in the absence of a catalyst.
  • the present invention is characterized in that the above generation method is performed by a continuous method of continuously supplying a source gas.
  • the present invention is an apparatus for performing the above-mentioned generation method, comprising: a reactor; an electrode housed in the reactor; and a DC power supply for applying a DC voltage to the electrode. And an outlet for discharging hydrogen.
  • an apparatus for producing hydrogen is provided.
  • This equipment In the reactor, the raw material gas is charged into the reactor. Then, a pulse discharge is performed between the electrodes, and the generated hydrogen is discharged from the outlet and used effectively.
  • the present invention provides an apparatus for performing the above-described method for generating a source gas continuously, comprising: a reactor; an electrode housed in the reactor; It is characterized by including a DC power supply for applying a DC voltage, a supply port for continuously supplying a source gas, and a discharge port for discharging generated hydrogen.
  • the raw material gas is continuously replenished from the supply port into the reactor, and hydrogen is efficiently produced.
  • a pulse discharge is performed in a raw material gas containing a gaseous alcohol and, if necessary, water vapor to induce a reaction between the alcohol or the alcohol and the water vapor. And a method for generating hydrogen.
  • the alcohol is not particularly limited, and can be appropriately selected from various alcohols. Examples thereof include methanol, ethanol, n-propanol, 2-propanol, 1-butanol, ethylene glycol, and the like, and a mixture thereof. Furthermore, since alcohol may be reacted as a result, ether is used as a raw material, and the ether is hydrolyzed with steam to produce various alcohols as described above, and the alcohol reacts. Specific examples of the ether include dimethinole ether, methyl ethyl ether, and getyl ether.
  • pulse discharge is performed in a source gas containing the alcohol and, if necessary, water vapor.
  • pulse discharge means passing a pulse current between the electrodes.For example, electron irradiation is repeated within a very short time of 1 ⁇ s or less, so the temperature of the gas phase does not rise and the reaction occurs at a very low temperature. Can be done.
  • the pulse discharge is usually performed at regular intervals, but may be intermittent. In performing the discharge, a pulse power supply can be used. However, a DC self-excited pulse discharge in which a constant voltage is applied between the electrodes and the pulse discharge is performed in a self-excited manner is preferably employed.
  • the number of pulse discharges per second (hereinafter, sometimes referred to as “pulse generation frequency”) is suitably about 5 to 100 times, and especially about 50 to 100 times. preferable.
  • the pulse generation frequency increases as the current increases under a constant voltage, and decreases as the distance between the electrodes increases. Therefore, the preferable voltage, current, and interelectrode distance are naturally set by adjusting the voltage, current, and interelectrode distance so that the above-described pulse generation frequency is achieved.
  • the applied voltage is about 1 kV to 2 kV
  • the current is about 1 to 20 mA
  • the electrode is The distance is preferably about 2 mm to 10 mm.
  • the applied voltage, current, and distance between the electrodes are not limited to the above ranges.
  • the distance between the electrodes is increased and the above-described pulse is applied. It can be implemented by increasing the applied voltage and current accordingly to achieve the frequency of occurrence.
  • a radical is generated by irradiating the discharge current, that is, the electron beam from the electrode, and this radical causes a reaction. Therefore, as the discharge current is increased and the distance between the electrodes is increased, the number of molecules that collide with the electron beam increases, so that the reaction rate increases and the conversion rate per unit time tends to increase. There is.
  • the reaction temperature is not particularly limited, but the lower the temperature, the lower the energy cost. Therefore, it is preferable to select a temperature within a temperature range higher than the boiling points of both the alcohol used as a raw material and, if necessary, the steam used, and as low as possible.
  • the reaction temperature is about 101 ° C to 130 ° C (normal pressure conditions) because water has a higher boiling point. Below) is preferable.
  • the reaction temperature should be 100 ° C to 150 ° C. It is preferable to be about C. Since water vapor tends to be concentrated, when the boiling point of alcohol is lower than that of water, the raw material gas containing alcohol and water vapor is subjected to a reaction temperature of about 130 to 15 oC in advance. It is preferred to feed the reactor after preheating at a higher temperature. When only methanol is used as a raw material, the temperature is preferably about 80 to 120 ° C.
  • the total pressure of the source gas is not particularly limited, and may be, for example, about 0.1 to 10 atmospheres. However, since the reaction proceeds sufficiently at normal pressure and a robust reactor is not required at that time, it can be said that the reaction at normal pressure is particularly preferable in industry.
  • the mixing ratio of alcohol and water vapor may be a stoichiometric amount, but if desired, one of the substances may be increased or decreased to about 1 Z 2 to 2 times the stoichiometric amount. However, if the partial pressure of steam is higher than the stoichiometric amount, the conversion of the raw material may decrease slightly. This is thought to be due to the fact that electrons generated by the discharge are captured by water molecules.
  • various alcohols can be used as described above.
  • methanol, ethanol, and propanol are used as the alcohol.
  • ethanol undergoes a reforming (reforming) reaction as shown in the following formula (3) with water vapor to produce target hydrogen without generating acetylene or the like.
  • a reforming reaction between methanol and water vapor is unlikely to occur, and usually, a decomposition reaction of methanol itself as shown in the following formula (4) proceeds. Whether the reforming reaction or the decomposition reaction is dominant depends on the structure and reactivity of the raw materials.
  • methanol is particularly preferably employed as the alcohol.
  • Methanol causes a decomposition reaction as shown in the following formula (4) by pulse discharge to generate hydrogen, but does not generate by-products such as acetylene.
  • the production method of the present invention is excellent as a method for producing hydrogen.
  • the generated hydrogen can be effectively used for, for example, synthesis of ammonia and methanol, hydrodesulfurization, hydrocracking, hydrogenation of fats and oils, welding, and semiconductor production.
  • turbine fuel there is an advantage that burning calories converted to hydrogen and carbon monoxide has a larger calorific value than burning alcohol as it is.
  • the production method of the present invention can proceed sufficiently in the absence of a catalyst. Since no catalyst is used, the cost can be reduced, and there is no problem of a decrease in the reaction rate due to a decrease in the activity of the catalyst.
  • FIG. 1 shows an example of the generation device of the present invention.
  • the generator 1 of FIG. 1 includes a reactor 10 made of quartz or other glass, ceramic, or the like.
  • a pair of electrodes 11 and 12 are provided in the reactor 10 so as to face each other, and a discharge region 13 is formed between the electrodes 11 and 12.
  • the electrode material use common materials such as SUS, nickel, copper, aluminum, iron, carbon, etc.
  • the shape of the electrode is not particularly limited, and may be various shapes such as a needle shape and a flat shape.
  • Each of the electrodes 11 and 12 extends out of the reactor 10, and a DC power supply 14 for applying a negative high voltage is connected to the electrode 11, and the DC power supply 14 is connected to the electrode 11.
  • a digital oscilloscope 15 is connected between the electrodes 11.
  • the electrode 12 is grounded outside the reactor 10.
  • a three-way port 16 is connected to the inlet side of the reactor 10, and an electrode 11 extending from the reactor 10 to the other side penetrates one port of the three-way port 16, and the other port has A supply port 17 for supplying a raw material gas to the reactor 10 is provided.
  • a tube 19 filled with quartz wool 18 is connected to the supply port 17, and a preheater 20 is provided so as to surround an area of the tube 19 filled with quartz wool 18.
  • a water vapor supply pipe 21 configured to supply water vapor W is provided with one end opened in the quartz wool 18 and the other end opened outside the pipe 19.
  • a thermocouple 22 is provided with one end inserted into quartz wool 18, and an alcohol supply pipe 24 is connected to pipe 19 via a three-way port 23.
  • a three-way port 25 is connected to the inlet side of the alcohol supply pipe 24, and a conductor 26 connected to the thermocouple 22 penetrates one port of the three-way port 25, and the other port is connected to the other port. It is configured so that gaseous alcohol A can be supplied.
  • a three-way port 27 is connected to the outlet side of the reactor 10, and an electrode 12 extending from the reactor 10 to the outside penetrates one of the three-way ports 27, and is connected to the other side. mouth has a discharge port 2 8 for discharging the hydrogen H 2 generated by pulse discharge. Note that the distance between the electrodes 11 and 12 can be arbitrarily adjusted.
  • water vapor W is supplied from the steam supply pipe 21 and gaseous alcohol A is supplied from the alcohol supply pipe 24.
  • the mixture is appropriately heated at 0 and supplied into the reactor 10 from the supply port 17.
  • a negative voltage is applied to the electrode 11 by the DC power supply 14, self-excited pulse discharge occurs between the electrodes 11 and 12, and the reaction occurs. Induced, producing hydrogen H 2.
  • the generated hydrogen H 2 is discharged from the outlet 28 and used for various purposes.
  • the generator 1 shown in FIG. 1 is configured to be able to continuously supply the raw material gas into the reactor 10, so that it is efficient and industrially excellent.
  • the feed rate of the raw material gas is adjusted to a value such that the conversion rate of the raw material gas becomes a certain value or more, for example, 60% or more, by analyzing the hydrogen H 2 discharged from the outlet 28. It is preferable to set appropriately.
  • the distance between the electrodes is about lmm to 10 mm, and the applied voltage is about 1 to 5 kV, alcohol and water vapor are contained.
  • the supply flow rate of the raw material gas is suitably about 10 to 100 Om1Z, especially about 50 to 100 Om1 minute. It should be noted that it is also possible to perform the measurement in a batch system instead of the continuous system as shown in FIG.
  • a DC power supply 14 is used as a power supply connected to the electrode 11.
  • any other power supply that can perform pulse discharge can be applied.
  • a power supply or the like configured to supply a half-wave or full-wave current by combining a rectifier with the power supply can be appropriately used.
  • the number of electrodes accommodated in the reactor 10 is not limited to one pair, and a plurality of electrodes can be used as needed.
  • the production device of the present invention can be used as a small and portable hydrogen production device.
  • hydrogen gas is obtained immediately after the start of the reaction, the response is fast, and the hydrogen gas can be continuously produced at low temperature and normal pressure. It can be used as a hydrogen supply device.
  • the device shown in Fig. 1 was produced as a generator.
  • a quartz tube having an outer diameter of 6 mm, an inner diameter of 5 mm, and a length of 300 mm was used as a reactor, and SUS316 was used as a pair of electrodes facing each other.
  • the distance between the electrodes was set to 1 to 1 Omm, and ethanol and water vapor were supplied.
  • the supply ratio of ethanol and steam was set to 1: 1 (partial pressure ratio).
  • the mixed gas of ethanol and water vapor was heated to 120 ° C by a preheater in advance and then supplied to the quartz tube.
  • the supply speed of the mixed gas is 30 ml
  • the molar ratio of carbon oxide was almost 2, suggesting that a reforming reaction had occurred.
  • the frequency of pulse generation during discharge was about 50 times Z seconds.
  • composition and amount of generated gas were measured in the same manner as in Example 1 except that the partial pressure ratio between ethanol and steam was set to 2: 1 and the supply rate of the mixed gas was set to 30 m1 minute. did.
  • the measurement results are shown in (Table 2).
  • Table 2 Current / mA conversion 1% CO selectivity 1% CO ⁇ ⁇ mol H 2 / CO
  • Ethanol alone was used as the raw material gas, and was supplied into the English pipe at a supply rate of 30 mlZ. At this time, the temperature (reaction temperature) in the quartz tube was normal temperature, and the pressure was normal pressure. In other configurations, the composition of the generated gas and the generated amount were measured in the same manner as in Example 1 above. The measurement results are shown in (Table 3)

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  • 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)
  • Hydrogen, Water And Hydrids (AREA)

Abstract

La présente invention concerne un nouveau procédé de formation d'hydrogène qui consiste à effectuer une décharge par impulsion dans une matière brute gazeuse contenant un alcool gazeux et de la vapeur de façon à induire une réaction de cet alcool et ce cette vapeur formant de l'hydrogène. On peut utiliser du méthanol, de l'éthanol, du propanol et d'autres composés similaires comme alcool. Dans ce procédé, une réaction de reformage entre l'alcool et la vapeur peut être obtenue par une décharge par impulsion et, l'hydrogène peut ainsi être formé efficacement à haut rendement. Ce procédé peut être utilisé pour produire de l'hydrogène à température plus basse, sous une pression normale, à haut rendement, avec une meilleure efficacité et, de plus, ce procédé est exempt de dépôt de carbone et de la formation d'un sous produit tel que l'acétylène.
PCT/JP2002/011138 2002-10-28 2002-10-28 Procede et appareil de formation d'hydrogene au moyen d'alcool WO2004037716A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU2002344021A AU2002344021A1 (en) 2002-10-28 2002-10-28 Method and apparatus for forming hydrogen by the use of alcohol
PCT/JP2002/011138 WO2004037716A1 (fr) 2002-10-28 2002-10-28 Procede et appareil de formation d'hydrogene au moyen d'alcool

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2002/011138 WO2004037716A1 (fr) 2002-10-28 2002-10-28 Procede et appareil de formation d'hydrogene au moyen d'alcool

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998028223A1 (fr) * 1996-12-24 1998-07-02 H2-Tech S.A.R.L. Procede et appareils de production d'hydrogene par reformage a plasma
JP2001167784A (ja) * 1999-12-10 2001-06-22 Mitsubishi Motors Corp 燃料電池システム
WO2001089988A1 (fr) * 2000-05-24 2001-11-29 Yasushi Sekine Procede et appareil destine au reformage a la vapeur d'une chaine d'hydrocarbure
WO2002092499A1 (fr) * 2001-05-15 2002-11-21 Yasushi Sekine Procede et appareil de reformage en phase liquide d'un hydrocarbure ou d'un compose contenant de l'oxygene

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998028223A1 (fr) * 1996-12-24 1998-07-02 H2-Tech S.A.R.L. Procede et appareils de production d'hydrogene par reformage a plasma
JP2001167784A (ja) * 1999-12-10 2001-06-22 Mitsubishi Motors Corp 燃料電池システム
WO2001089988A1 (fr) * 2000-05-24 2001-11-29 Yasushi Sekine Procede et appareil destine au reformage a la vapeur d'une chaine d'hydrocarbure
WO2002092499A1 (fr) * 2001-05-15 2002-11-21 Yasushi Sekine Procede et appareil de reformage en phase liquide d'un hydrocarbure ou d'un compose contenant de l'oxygene

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