# US 10,501,319 B2 · Operation method for hydrogen production apparatus, and hydrogen production apparatus

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- Number: US 10,501,319 B2
- Document ID: US10501319B2
- Status: Granted
- Kind: B2
- Application number: 15/541,398
- Filed: 2015-12-24
- Published: 2018-01-25
- Granted: 2019-12-10
- Earliest claimed: 2015-01-05
- Assignees: Osaka Gas Co., Ltd.
- Applicants: Osaka Gas Co., Ltd.
- Inventors: Kazuhiko Murata; Tsubasa Shimizu; Satoshi Takagi
- Web page: https://patentgrep.com/patent/US10501319B2

## CPC

- C01B 3/48: followed by reaction of water vapour with carbon monoxide
- B01D 53/053: with storage or buffer vessel
- B01J 8/0492: {Feeding reactive fluids (for solid material, see B01J8/0015)}
- B01J 8/0496: {Heating or cooling the reactor}
- C01B 3/38: using catalysts
- C01B 3/384: with external heating of the catalyst
- C01B 3/56: by contacting with solids; Regeneration of used solids
- H01M 8/04231: {Purging of the reactants}
- H01M 8/0612: from carbon-containing material
- H01M 8/0675: {Removal of sulfur}
- B01D 2253/102: Carbon
- B01D 2253/106: Silica or silicates
- B01D 2253/108: Zeolites
- B01D 2256/16: Hydrogen
- B01D 2259/403: using three beds
- C01B 2203/0233: the reforming step being a steam reforming step
- C01B 2203/0283: containing a CO-shift step, i.e. a water gas shift step
- C01B 2203/042: Purification by adsorption on solids
- C01B 2203/043: Regenerative adsorption process in two or more beds, one for adsorption, the other for regeneration
- C01B 2203/0805: Methods of heating the process for making hydrogen or synthesis gas
- C01B 2203/0816: Heating by flames
- C01B 2203/1058: Nickel catalysts
- C01B 2203/1241: Natural gas or methane
- C01B 2203/127: Catalytic desulfurisation
- C01B 2203/1276: Mixing of different feed components
- C01B 2203/1604: Starting up the process
- C01B 2203/1609: Shutting down the process
- Y02E 60/50: Fuel cells
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A hydrogen production apparatus including a desulfurizer, a reformer, a CO transformer a gas flow path, and a purge gas supply path which is provided where a purge gas is supplied to an upstream side of a pressure feeding apparatus in the gas flow path, prior to a stopping operation, a purging step of replacing gas within the gas flow path with the purge gas and filling the purge gas into the gas flow path is performed, and in a start-up operation in which a heating means is operated to increase the temperature of the gas within the gas flow path, which is performed prior to a hydrogen purification operation, a pressure increasing step of supplying the purge gas from the purge gas supply path to the closed circulation circuit and increasing the pressure within the closed circulation circuit is performed.

## Claims

### Claim 1

An operation method for a hydrogen production apparatus, the hydrogen production apparatus comprising a desulfurizer that desulfurizes a source gas, a reformer that heats the desulfurized source gas in a state mixed with steam with a heater and obtains a reformed gas, a CO transformer that causes carbon monoxide in the reformed gas to react with steam and obtains a transformed gas, and a hydrogen purification unit that separates impurities other than hydrogen from the transformed gas after processing by the CO transformer to purify hydrogen gas, the operation method comprising:
providing a gas flow path that allows gas comprising at least one of the source gas, the desulfurized source gas, the reformed gas, the transformed gas, and/or the hydrogen gas to flow to the desulfurizer, the reformer, the CO transformer, and/or the hydrogen purification unit, and providing a pressure feed configured to cause the gas to flow in the gas flow path,
providing a hydrogen purification operation for operating the heater and the pressure feed to supply the gas to the gas flow path, and a stopping operation configured to stop operation of the heater and the pressure feed, being performed in order,
providing in the gas flow path a closed circulation circuit that returns and circulates the gas by the pressure feed in an order of the desulfurizer, the reformer, and then the CO transformer while bypassing the hydrogen purification unit, and providing a purge gas supply path where a purge gas is supplied to an upstream side of the pressure feed in the gas flow path,
providing a throttle unit in a return path that returns and circulates the gas while bypassing the hydrogen purification unit in the closed circulation circuit, the throttle unit switching between a throttled state in which a large flow path resistance is set and a throttle released state in which a small flow path resistance is set,
prior to the stopping operation, performing a purging step of replacing the gas within the gas flow path with the purge gas and filling the purge gas into the gas flow path, and
in a start-up operation in which the heater is operated to increase the temperature of the gas within the gas flow path, which is performed prior to the hydrogen purification operation, performing a pressure increasing step for supplying the purge gas from the purge gas supply path to the closed circulation circuit and increasing the pressure within the closed circulation circuit while operating the pressure feed, and subsequently performing a temperature increasing step for operating the pressure feed and the heater and increasing the temperature,
wherein the pressure increasing step is performed with the throttle unit switched to the throttled state, and the temperature increasing step is performed with the throttle unit switched to the throttle released state.

### Claim 2 (depends on 1)

The operation method for the hydrogen production apparatus according to claim 1, comprising providing a pressure detection unit that detects an internal pressure within the closed circulation circuit, and when performing the start-up operation, in a case where the pressure detected by the pressure detection unit is lower than a predetermined pressure, supplying the purge gas into the closed circulation circuit from the purge gas supply path.

### Claim 3 (depends on 2)

The operation method for the hydrogen production apparatus according to claim 2, wherein the purge gas is hydrogen gas that has been purified by the hydrogen purification unit, and stored in a product tank.

### Claim 4 (depends on 1)

The operation method for the hydrogen production apparatus according to claim 1, wherein the purge gas is hydrogen gas that has been purified by the hydrogen purification unit, and stored in a product tank.

### Claim 5 (depends on 1)

The operation method for the hydrogen production apparatus according to claim 1, wherein:
the return path includes a first return path having a small flow path cross-sectional area that sets a large flow path resistance, and a second return path having a large flow path cross-sectional area that sets a small flow path resistance, the first and second return paths being arranged in parallel, and
the throttle unit switches between the throttled state in which a large flow path resistance of the return path is set by opening a first on/off valve provided in the first return path and closing a second on/off valve provided in the second return path, and the throttle released state in which a small flow path resistance of the return path is set by opening at least a second on/off valve provided in the second return path.