JP2006220173A - Hydrogen adsorbing material activating method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a hydrogen adsorbing material activating method for avoiding the deterioration of a container without increasing the weight of a fuel cell vehicle and degrading a degree of freedom in equipment arrangement. <P>SOLUTION: A metal-organic framework structure MOF as a hydrogen adsorbing material is stored in the container 10. Into the container 10, inactive gas is introduced from an inactive gas cylinder 35 through a refining tool 38 and a heater 40. The inactive gas desorbs gas adsorbed onto the metal-organic framework structure MOF. The gas is exhausted from the container 10 while accompanying the inactive gas. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a method for activating a hydrogen adsorbent that improves the hydrogen gas adsorption capacity of a hydrogen adsorbent contained in a hydrogen gas storage tank.

  In recent years, a fuel cell vehicle equipped with a fuel cell has attracted attention due to a growing interest in environmental protection. This is because the fuel cell vehicle uses the fuel cell as a travel drive source, so there is no need to burn gasoline or light oil, and therefore no hydrocarbon gas, NOx, SOx, or the like is discharged.

  It is necessary to supply a fuel gas containing hydrogen and an oxidant gas containing oxygen to the fuel cell. As the oxidant gas, for example, air can be used. However, the fuel gas must be supplied from a fuel gas supply source such as a hydrogen gas storage tank. For this reason, the fuel cell vehicle is equipped with a fuel gas supply source in addition to the fuel cell.

  Thus, when a hydrogen gas storage tank is used as a fuel gas supply source, it has been studied that a hydrogen adsorbent is accommodated therein. In this case, since the hydrogen adsorbent adsorbs and holds hydrogen, more hydrogen can be stored as compared with the case where the hydrogen adsorbent is not accommodated.

  By the way, when a gas other than hydrogen gas is adsorbed on the hydrogen adsorbent, the hydrogen gas adsorption amount of the hydrogen adsorbent is inevitably lowered. For this reason, a process for releasing the adsorbed hydrogen gas is required. As one type of such a processing method, for example, as described in Non-Patent Document 1, evacuation of carbon nanotubes at 350 ° C. for 3 hours can be mentioned.

  Patent Document 1 discloses that the adsorbent is accommodated while introducing nitrogen gas or the like into the adsorbent accommodating portion of the adsorption device.

2001 NEDO result report “NEDO-WE-NET0011” for publication 51101633-3-1, Hydrogen Utilization International Clean Energy System Technology (WE-NET) Phase II R & D Task 11, “Development of Hydrogen Storage Materials” p355 -357 JP-A-5-76716

  In the method described in Non-Patent Document 1, vacuum evacuation is performed at 350 ° C. for 3 hours after the carbon nanotube is filled in the container. In this case, since the container is heated, there is a concern that the container is deteriorated due to thermal strain or the like.

  Further, in the method described in Patent Document 1, it is necessary to attach a supply system of nitrogen gas or the like. When such a supply system is mounted on a fuel cell vehicle, the weight of the fuel cell vehicle increases, and a space for mounting the supply system is required, leading to a problem that the degree of freedom in equipment arrangement is reduced.

  The present invention has been made to solve the above-described problems, and does not deteriorate the container, and does not increase the weight of the fuel cell vehicle, and does not reduce the degree of freedom of equipment arrangement. It aims at providing the activation method of material.

In order to achieve the above object, the present invention provides a hydrogen adsorbent for removing gas other than hydrogen gas adsorbed on the surface of the hydrogen adsorbent accommodated in the container before filling the container with hydrogen gas. An activation method comprising:
Storing a hydrogen adsorbent in a container having a supply port and a discharge port;
Introducing an inert gas that is not adsorbed by the hydrogen adsorbent from the supply port, and discharging the inert gas accompanied by the gas adsorbed on the surface of the hydrogen adsorbent from the discharge port;
It is characterized by having. The “inert gas” in the present invention refers to a gas that is not adsorbed by the hydrogen adsorbent.

  For example, a gas other than hydrogen gas such as water vapor is adsorbed to a hydrogen adsorbent exposed to the atmosphere when stored in a container. In the present invention, an inert gas is circulated in the container so that the gas is absorbed by the inert gas, so that the gas is separated from the hydrogen adsorbent. For this reason, the site | part which can adsorb | suck hydrogen gas in a hydrogen adsorbent increases, Therefore, hydrogen gas adsorption capacity improves. In other words, the hydrogen adsorbent is activated.

  In the container, since the inert gas contacts the hydrogen adsorbent evenly, it is possible to avoid occurrence of a portion where the gas is not removed in the hydrogen adsorbent. Further, it is not particularly necessary to heat the container itself, and in this case, thermal distortion does not occur in the container.

  Moreover, for example, since the hydrogen adsorbent in the container can be activated before being mounted on the fuel cell vehicle, it is not necessary to mount an activation system on the fuel cell vehicle. Therefore, the weight of the fuel cell vehicle is not increased, and the degree of freedom in device arrangement is not reduced.

  In the present invention, the inert gas may be heated and introduced into the container. In this case, since heat energy is also given to the gas adsorbed on the hydrogen adsorbent, the gas can be separated more efficiently.

In addition, since H ₂ O, CO ₂ , CO, and O ₂ in the inert gas are adsorbed by the hydrogen adsorbent, the number of sites where hydrogen gas can be adsorbed is reduced. In order to avoid this, it is preferable to reduce the concentration of at least H ₂ O, CO ₂ , CO, O ₂ by purifying the inert gas and introduce it into the container.

  The inert gas discharged from the discharge port may be reintroduced into the container from the supply port. In this case, the inert gas consumption for activating the hydrogen adsorbent is significantly reduced, which is advantageous in terms of cost.

  Moreover, it is preferable to exhaust the inside of the container before introducing the inert gas. Thereby, it becomes easy to make an inert gas reach the inside of a container.

  In any case, a preferred example of the hydrogen adsorbent includes a metal-organic skeleton structure.

  According to the present invention, the hydrogen adsorbent previously accommodated in the container is activated by circulating an inert gas in the container. For this reason, thermal distortion does not occur in the container. In addition, since the hydrogen adsorbent in the container can be activated before actual use such as mounting the container on a fuel cell vehicle, there is no need to provide an activation system.

  Moreover, in the present invention, the hydrogen gas adsorbing ability of the hydrogen adsorbent can be easily improved by performing an extremely simple operation of circulating an inert gas in the container.

  Hereinafter, preferred embodiments of the method for activating the hydrogen adsorbent according to the present invention will be described in detail with reference to the accompanying drawings. In the present embodiment, a metal-organic skeleton structure which is a kind of complex will be described as an example of the hydrogen adsorbent.

  The metal-organic framework structure is a structure in which metal atoms or metal ions are coordinated and bound so that the organic molecules or organic ions surround them, and maintains a stable porous framework structure even in the absence of guest molecules. To do. Note that hydrogen gas is adsorbed in the porous skeleton structure.

Specific examples of the metal-organic skeleton structure include [M ₂ (4,4′-bipyridine) ₃ (NO ₃ ) ₄ ] (where M is any one of Co, Ni, and Zn), [M ₂ (1 , 4-benzenedicarboxylate anion) ₂ ] (wherein M is either Cu or Zn), [Fe ₂ (trans-4,4′-azopyridine) ₄ (NCS) ₄ ] and the like.

As another specific example of the metal-organic framework, as described in US Patent Application Publication No. 2003/0004364, the general formula is represented by M ₄ O (aromatic dicarboxylate anion) ₃ . What is done. Suitable examples of M include Zn, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Al, Ru, Rh, Pd, Ag, and Pt. Moreover, it may be composed of an aromatic dicarboxylate anion derivative instead of the aromatic dicarboxylate anion.

  Preferable examples of the aromatic dicarboxylate anion or a derivative thereof include 1,4-benzenedicarboxylate anion, 2-bromo-1,4-benzenedicarboxylate anion, 2-amino-1,4-benzenedi Carboxylate anion, 2,5-propyl-1,4-benzenedicarboxylate anion, 2,5-pentyl-1,4-benzenedicarboxylate anion, cyclobutene-1,4-benzenedicarboxylate anion, 1, 4-naphthalenedicarboxylate anion, 2,6-naphthalenedicarboxylate anion, 4,4′-biphenyldicarboxylate anion, 4,5,9,10-tetrahydropyrene-2,7-dicarboxylate anion, pyrene -2,7-dicarboxylate anion, 4, "-. Terphenyl dicarboxylate anion, etc. Each structural formula is as follows.

  Hereinafter, the activation method according to the present embodiment will be described.

FIG. 1 schematically shows an activation system 16a schematically showing a state where an inert gas supply line 12 and an exhaust line 14 are connected to a container 10 in which a metal-organic framework MOF as a hydrogen adsorbent is accommodated. It is a block diagram. In this case, the container 10 is made of SUS304, which is a kind of stainless steel, and has a pressure resistance of 20 MPa and a volume of 100 cm ³ . The metal-organic skeleton structure MOF may be an unused one filled in the container 10, or a hydrogen gas adsorbing ability may be reduced due to repeated adsorption / release of hydrogen gas. Good.

  A first cylindrical projecting portion 20 and a second cylindrical projecting portion 22 are respectively provided on the lower end surface and the upper end surface of the container 10, and the first cylindrical projecting portion 20 and the second cylindrical projecting portion 22 are provided. Valves 24 and 26 and connectors 28 and 30 are connected to each. In addition, filters 32 and 34 are held in the respective openings reaching the first cylindrical protrusion 20 or the second cylindrical protrusion 22.

  In the inert gas supply line 12 connected via the connector 28, a valve 36, a purifier 38, and a heater 40 are disposed from the inert gas cylinder 35 to the connector 28. On the other hand, a gas sampling pipe 46 and a vent pipe 48 are branched from the exhaust line 14 connected via the connector 30 to the valve 44 disposed on the upstream side of the vacuum pump 42. A valve 50 is interposed in the vent pipe 48, and a pressure gauge 52 is installed in the vicinity of the vent pipe 48.

  The valves 24, 26, 36, 44, and 50 are fully closed, the vacuum pump 42 is energized, and the valves 26 and 44 are opened. Thereby, exhaust in the container 10 is made. By this exhaust, replacement in the container 10 with an inert gas, which will be described later, can be completed in a short time. In other words, the inside of the container 10 can be efficiently replaced with an inert gas by exhausting.

When it is confirmed by the instruction of the pressure gauge 52 that the inside of the container 10 is about 10 ⁻¹ Torr, the valve 44 is closed. Next, the valves 36, 26 and 24 are opened, and an inert gas is introduced from the inert gas cylinder 35.

Here, the inert gas refers to a gas that is not adsorbed by the metal-organic framework MOF that is a hydrogen adsorbent. Preferable examples of such a gas include N ₂ , Ar, Ne, He, Xe, Kr and the like.

The inert gas is first introduced into the purifier 38. For example, a column filled with molecular sieve is accommodated in the purifier 38, and H ₂ O, CO ₂ , CO, and O ₂ are removed from the inert gas that has passed through the column.

  The purified inert gas is heated to about 100 to 130 ° C. by the heater 40 and then introduced into the container 10. The gas adsorbed on the metal-organic framework structure MOF is absorbed by the introduced inert gas, and then desorbs from the metal-organic framework structure MOF. Further, since the inert gas is heated, the gas adsorbed on the metal-organic skeleton structure MOF is also activated by the transfer of thermal energy from the inert gas. Therefore, the gas can be separated from the metal-organic framework structure MOF more efficiently.

  When it is confirmed from the instruction of the pressure gauge 52 that the inside of the container 10 has become about 1 atm, the valve 50 is opened. Along with this, the inert gas is discharged from the vent pipe 48, and as a result, the inert gas flows through the container 10.

  As described above, the gas adsorbed on the metal-organic skeleton structure MOF is released by being absorbed in the inert gas and supplying thermal energy from the inert gas. The detached gas is discharged from the vent pipe 48 along with the inert gas flowing through the container 10.

  During this flow, the exhaust gas is sampled with a microsyringe through the gas sampling tube 46. The sampled exhaust gas is analyzed with a quadrupole mass spectrometer or gas chromatography, and when the peak based on components other than the inert gas no longer appears, the gas detaches from the metal-organic framework MOF, in other words, For example, it is determined that the activation of the metal-organic framework MOF is completed.

  Alternatively, as shown in FIG. 2, a branch line 54 branched from the downstream side of the purifier 38 and bridged by the vent pipe 48 may be provided. In this case, the branch line 54 and the vent pipe 48 may be connected via the thermal conductivity detector 56.

  In the activation system 16b shown in FIG. 2, the thermal conductivity detector 56 discharges the inert gas introduced into the container 10 and the gas separated from the metal-organic framework structure MOF together with the inert gas. The difference in thermal conductivity with the exhaust gas is detected. If there is a difference between both thermal conductivities, it means that the exhaust gas contains a gas other than inert gas, and if both thermal conductivities are equal, the components of the inert gas and exhaust gas are equivalent. Means that That is, when the difference in thermal conductivity becomes equal, it is determined that the gas detachment from the metal-organic framework structure MOF, that is, the activation of the metal-organic framework structure MOF is completed.

  Further, in place of the vent pipe 48, as shown in FIG. 3, a circulation line 58 bridged from the upstream side of the purifier 38 to the upstream side of the valve 44 may be provided. In this case, a check valve 59, a circulation pump 60, and a valve 50 are interposed in the circulation line 58.

  In the activation system 16c shown in FIG. 3, after introducing an inert gas into the container 10 in accordance with the activation system 16a shown in FIG. 1, the valve 36 is closed, and then the circulation pump 60 is energized. The valve 50 is opened. As a result, the inert gas is reintroduced into the container 10 via the check valve 59, the purifier 38, and the heater 40. That is, the inert gas is circulated. Note that the gas accompanying the inert gas is separated by the purifier 38.

  By circulating the inert gas in this way, the consumption of the inert gas for activating the metal-organic framework structure MOF is remarkably reduced. That is, it is advantageous in terms of cost.

  In the activation system 16c shown in FIG. 3 as well, the activation of the metal-organic framework structure MOF is performed by using the quadrupole mass of the gas sampled through the gas sampling tube 46 as in the activation system 16a shown in FIG. What is necessary is just to judge that it complete | finished when the peak based on components other than an inert gas no longer appears by analyzing with an analyzer or gas chromatography.

  When detecting the difference in thermal conductivity as in the activation system 16b shown in FIG. 2, as shown in FIG. 4, the inert gas that has passed through the purifier 38 and the exhaust gas that has passed through the circulation pump 60 are used. The activation system 16d may be constructed by providing the thermal conductivity detector 56 so as to detect the difference in thermal conductivity between the activation system 16d and the activation system 16d.

  By circulating the inert gas in the container 10 in this manner, the gas adsorbed on the metal-organic skeleton structure MOF (hydrogen adsorbent) can be efficiently removed. In the metal-organic framework MOF from which the gas has been removed, there are many sites where hydrogen gas can be adsorbed. For this reason, a large amount of hydrogen gas can be adsorbed. In other words, the metal-organic framework structure MOF is activated by flowing an inert gas.

  In such an activation process, since the inert gas itself is heated, the heated inert gas is introduced into the container 10. Therefore, since the heated inert gas uniformly contacts the metal-organic framework structure MOF accommodated in the container 10, a portion where the gas is not removed is generated in the metal-organic framework structure MOF. Is avoided. Further, thermal distortion does not occur in the container 10.

  Moreover, since the metal-organic framework MOF in the container 10 can be activated before the container 10 is mounted on the fuel cell vehicle, it is necessary to provide an activation system for activation in the fuel cell vehicle. Nor. For this reason, the weight of the fuel cell vehicle is not increased, and the degree of freedom in device arrangement is not reduced.

  After the activation of the metal-organic framework MOF, the valves 24 and 50 are closed and the valve 44 is opened. Thereby, the inside of the container 10 is exhausted by the vacuum pump 42.

When the pressure in the container 10 reaches about 10 ⁻¹ Torr, the valve 26 is closed and the inert gas supply line 12 and the exhaust line 14 are disconnected from the connectors 28 and 30. Thereafter, the container 10 may be connected to a hydrogen gas supply system and charged with hydrogen gas.

  In the above-described embodiment, the metal-organic skeleton structure MOF has been described as an example of the hydrogen adsorbent, but it goes without saying that the hydrogen adsorbent is not particularly limited to this.

  Further, it is not particularly necessary to heat the inert gas before introducing it into the container 10, and therefore it is not particularly necessary to provide the heater 40 in the inert gas supply line 12.

Further, in order to purify the inert gas, a column other than a column packed with molecular sieves may be used. For example, when H ₂ O is removed from the inert gas, silica gel or diphosphorus pentoxide (P ₂ O _{5) is used.} ) May be used.

  Furthermore, when the inert gas is introduced after the inside of the container 10 is evacuated, it is not particularly necessary to close the valve 26, and the inert gas is supplied while the valve 44 is closed while the valves 26 and 50 are opened. You may make it introduce.

1.2 g 2,6-naphthalenedicarboxylic acid and 11 g Zn (NO ₃ ) ₂ .4H ₂ O were dissolved in 1000 ml diethylformamide (DEF) in a closed vessel.

This solution was stored in a sealed container and heated at 95 ° C. for 20 hours while keeping the sealed container sealed, and Zn ₄ O (2,6-naphthalene) in which DEF molecules were physically adsorbed on the porous skeleton structure. Carboxylate anion) ₃ · (DEF) ₆ was obtained. The reaction product was filtered to separate it from the solvent DEF, and the filter residue Zn ₄ O (2,6-naphthalenedicarboxylate anion) _3. (DEF) ₆ was immersed in chloroform at room temperature for 24 hours. The DEF molecules physically adsorbed on the porous skeleton structure were replaced with CHCl ₃ molecules. This was separated from the solvent by filtration or the like, and then left standing in a vacuum evacuator and evacuated to desorb CHCl ₃ molecules from the porous skeleton structure, and Zn ₄ O (2,6-naphthalene). Carboxylate anion) ₃ .

This operation was repeated to obtain 210 g of powdery Zn ₄ O (2,6-naphthalenedicarboxylate anion) ₃ .

Next, 50 g of the obtained Zn ₄ O (2,6-naphthalenedicarboxylate anion) ₃ is accommodated in the container 10 at an atmospheric pressure of 20 ° C., and an inert gas is supplied as shown in FIG. The line 12 and the exhaust line 14 were connected, and the valves 24, 26, 36, 44, and 50 were fully closed. In this state, the vacuum pump 42 was energized. The valves 26 and 44 were opened to evacuate the container 10, and the valve 44 was closed when the pressure in the container 10 reached 10-1 Torr.

Further, the valves 36, 26 and 24 were opened, and N ₂ gas was supplied from the inert gas cylinder 35. N ₂ gas was purified to 99.999% by the purifier 38 and then heated to 110 ° C. by the heater 40.

When the N ₂ gas pressure in the container 10 reached 1 atm or higher, the valve 50 was opened and 110 ° C. N ₂ gas was circulated. After 30 minutes, the exhaust gas was sampled from the gas sampling tube 46 and analyzed by gas chromatography. As a result, no peak based on components other than N ₂ gas appeared. From this, it is determined that the desorption of the gas from Zn ₄ O (2,6-naphthalenedicarboxylate anion) ₃ is completed, and the valves 36, 24, 50 are closed, while the valve 44 is opened to close the container. The inside of 10 was evacuated to 10 ⁻¹ Torr. Thereafter, the valve 26 was closed, and the container 10 was removed from the connectors 28 and 30.

  Next, the container 10 was incorporated into the hydrogen gas adsorption amount measuring system 70 shown in FIG. 5 and the adsorbed hydrogen gas amount was measured.

  In this hydrogen gas adsorption amount measuring system 70, a supply line 72 for supplying hydrogen gas to the container 10 and a discharge line 74 for releasing hydrogen gas from the container 10 are provided to branch from the connector 28.

  The supply line 72 is bridged from the hydrogen gas cylinder 76 to the container 10. A regulator 78 and a manual valve 80 are interposed in the supply line 72 from the hydrogen gas cylinder 76 side.

  On the other hand, a vacuum pump 82 is interposed in the discharge line 74, and until reaching the vacuum pump 82, a manual valve 84, a regulator 86, a needle valve 88, a mass flow meter 90, and an automatic valve 92 are arranged from the container 10 side. In FIG. 5, reference numerals 94 and 96 both indicate pressure gauges.

In order to remove the gas in the supply line 72 and the discharge line 74, the vacuum pump 82 is energized, both the valve 24 and the manual valves 80 and 84 are opened, and the automatic valve 92 is opened, so that the pressure is 10 ^−3. Vacuuming is continued until Torr is reached. Thereafter, the manual valves 80 and 84 and the automatic valve 92 are closed.

  Next, the regulator 78 is set to 10 MPa, the manual valve 80 is opened, and 10 MPa hydrogen gas is introduced into the container 10.

  Thereafter, the manual valve 80 is closed, the vacuum pump 82 is energized, and the automatic valve 92 is opened. Further, if the manual valve 84 is opened, the hydrogen gas in the container 10 is released under the action of the vacuum pump 82.

  The released hydrogen gas is reduced in pressure to 0.1 MPa by the regulator 86 and the needle valve 88 and reaches the mass flow meter 90. The integrated flow rate of hydrogen gas that has passed through the mass flow meter 90 is obtained. When the increase in the integrated flow rate is no longer recognized, it is determined that all the hydrogen gas has been released, the manual valve 84 and the automatic valve 92 are closed, and the vacuum pump 82 is stopped.

  The number of moles of released hydrogen gas determined as described above was 0.70 mol.

For comparison, the amount of released hydrogen gas of Zn ₄ O (2,6-naphthalenedicarboxylate anion) ₃ was measured in the same manner as above except that N ₂ gas was not circulated. The number of moles of gas was 0.66 mol. From this result, it is clear that after the metal-organic skeleton structure MOF is accommodated in the container, an inert gas is circulated in the container, so that a hydrogen adsorbing material having excellent hydrogen gas adsorption ability is obtained.

After storing 50 g of Zn ₄ O (2,6-naphthalenedicarboxylate anion) ₃ in the container 10, the activation system 16 a shown in FIG. 1 was constructed. After activation by the flow of N ₂ gas in accordance with Example 1, the container 10 was incorporated into the hydrogen gas adsorption amount measurement system 70 shown in FIG. 5 and the hydrogen gas adsorption / release operation was repeated 500 times.

Thereafter, the container 10 was disconnected from the hydrogen gas adsorption amount measurement system 70, and the activation system 16a shown in FIG. 1 was constructed again, and activation was performed by flowing N ₂ gas. Then, when the container 10 was incorporated again in the hydrogen gas adsorption amount measuring system 70 shown in FIG.

For comparison, the adsorption / release operation of hydrogen gas was repeated 500 times without activation of Zn ₄ O (2,6-naphthalenedicarboxylate anion) ₃ , and the hydrogen gas was regenerated without reactivation. Adsorption / release operation was performed. At this time, the number of moles of released hydrogen gas was 0.61 mol. That is, it was confirmed that the number of moles of released hydrogen gas decreased by repeating the adsorption / release operation of hydrogen gas.

Further, from this result, even Zn ₄ O (2,6-naphthalenedicarboxylate anion) ₃ that repeatedly performed adsorption and release of hydrogen gas can be reactivated by circulating N ₂ gas. Obviously you can.

It is a schematic block diagram of the activation system for activating the hydrogen adsorbent accommodated in the container. It is a schematic block diagram of the activation system of a form different from FIG. It is a schematic block diagram of the activation system of a form different from FIG. 1, FIG. It is a schematic block diagram of the activation system of a form different from FIGS. 1-3. It is a system schematic block diagram which shows the hydrogen gas adsorption amount measuring system for measuring the hydrogen gas discharge | release amount of a hydrogen adsorbent.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 ... Container 12 ... Inert gas supply line 14 ... Exhaust line 16a-16d ... Activation system 38 ... Purifier 40 ... Heater 42, 82 ... Vacuum pump 48 ... Vent pipe 54 ... Branch line 56 ... Thermal conductivity detector 58 ... circulation line 60 ... circulation pump 70 ... hydrogen gas adsorption amount measuring system 72 ... supply line 74 ... discharge line 76 ... hydrogen gas cylinder 90 ... mass flow meter MOF ... metal-organic framework

Claims (6)

A method of activating a hydrogen adsorbent that removes gas other than hydrogen gas adsorbed on the surface of the hydrogen adsorbent contained in the container before filling the container with hydrogen gas,
Storing a hydrogen adsorbent in a container having a supply port and a discharge port;
Introducing an inert gas that is not adsorbed by the hydrogen adsorbent from the supply port, and discharging the inert gas accompanied by the gas adsorbed on the surface of the hydrogen adsorbent from the discharge port;
A method for activating a hydrogen adsorbent characterized by comprising:   The activation method according to claim 1, wherein the inert gas is heated and introduced into the container. 3. The activation method according to claim 1, wherein the inert gas is purified to reduce the concentration of at least H ₂ O, CO ₂ , CO, O ₂ and introduce the reduced gas into the container. Activation method of hydrogen adsorbent.   The activation method according to claim 1, wherein the inert gas discharged from the discharge port is reintroduced into the container from the supply port. Method.   5. The activation method according to claim 1, wherein the inside of the container is evacuated before the inert gas is introduced.   6. The activation method according to claim 1, wherein the metal-organic skeleton structure as the hydrogen adsorbing material is housed in the container.

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