Gas supply device and gas process system
The on-site generation of hydrogen gas for filter regeneration in gas purification systems addresses filter saturation issues, enhancing safety and reducing costs by eliminating the need for pressurized cylinders and ensuring consistent global safety standards.
Patent Information
- Application Number
- DE102024134148
- Authority / Receiving Office
- DE · DE
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2024-11-20
- Publication Date
- 2026-05-21
AI Technical Summary
Existing gas purification systems face challenges with filter saturation, requiring costly and complex filter regeneration using pressurized gas cylinders, which pose safety risks and are not globally consistent, and rely on unreliable external gas sources.
A gas supply device generates hydrogen gas on-site for filter regeneration, eliminating the need for pressure vessels and integrating safety features to ensure cost-effective and safe operation.
This approach reduces the reliance on external gas sources, enhances safety, and simplifies operations by generating regeneration gas locally, thereby reducing costs and personnel requirements while maintaining high purity standards.
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Abstract
Description
[0001] Various embodiments relate to a gas supply device and a gas processing system.
[0002] For various applications, such as glove boxes, highly purified inert gas is used, which undergoes complex filtration (also known as gas purification) to meet the required purity standards. This process removes impurities, such as oxygen and / or moisture, from the inert gas to increase its purity. During gas purification, the filter becomes saturated, reducing its ability to separate impurities from the inert gas. The saturated filter is then either replaced or regenerated, typically using a regeneration gas from a pressurized gas cylinder or other pressure vessel.
[0003] Various designs have demonstrated that filter regeneration can be simplified. The use of pressure vessels (e.g., for assembly and disassembly) necessitates elaborate safety precautions and trained personnel to mitigate the risks posed by the regeneration gas, which is costly. Furthermore, the availability of regeneration gas from pressure vessels is not always reliable, making procurement expensive. Additionally, safety precautions vary considerably worldwide and do not always meet requirements, complicating global customer support.
[0004] Various embodiments demonstrate how the regeneration gas can be generated directly at the filter location, thus eliminating the need for pressure vessels, increasing safety, and reducing dependence on external regeneration gas producers. This is achieved by generating hydrogen gas, which is then used to produce the regeneration gas, for example, by mixing the hydrogen gas with the inert gas already on hand for the application. Because of the local generation, the hydrogen gas and the regeneration gas are consumed directly, significantly reducing the total amount of hydrogen gas required on-site compared to the capacity of a pressure vessel.
[0005] Various designs of the gas supply device used to mix the regeneration gas feature, among other things, a simple and cost-effective construction without compromising on meeting high safety requirements. This also allows for cost-effective and safe retrofitting of existing systems. Alternatively or additionally, the gas supply device can be configured to mix the regeneration gas automatically, reducing the risk of operator error and the formation of flammable regeneration gas. This, in turn, simplifies operation and reduces personnel requirements.
[0006] The following are various examples that relate to what is described herein and depicted in the figures.
[0007] Example 1 (e.g., a gas supply device) is configured according to one of the appended claims and / or comprises: an inert gas inlet for receiving inert gas; a feed material inlet for receiving a feed material; a hydrogen generator for releasing hydrogen gas from the feed material; and a regeneration gas outlet (e.g., connection) for providing regeneration gas to a filter device (e.g., for regenerating the filter device); optionally, a piping network (e.g., internal piping network). The feed material inlet can, for example, be arranged inside the gas supply device (e.g., a chamber housing thereof), e.g., for connecting an integrated storage container (e.g., water tank).
[0008] Example 2 is a method (e.g., for operating the gas supply device according to Example 1) comprising: releasing hydrogen gas from the starting material, e.g., by means of the hydrogen generator; regenerating a filter device using the hydrogen gas, e.g., by means of a regeneration gas containing the hydrogen gas.
[0009] Example 3 is the use of a hydrogen generator (e.g., of Example 1 or 2) to produce hydrogen gas (e.g., by electrolysis and / or by releasing the hydrogen gas from the starting material), whereby a filter device is regenerated using the hydrogen gas (e.g., using a regeneration gas containing the hydrogen gas).
[0010] Example 4 is set up according to one of Examples 1 to 3, wherein the starting material is a fluid, e.g., a liquid, and / or contains water (e.g., consists of it); and / or wherein the regeneration gas contains hydrogen gas. This reduces the effort and increases safety.
[0011] Example 5 is set up according to one of Examples 1 to 4, wherein the hydrogen generator is configured to decompose the starting material, e.g. by means of an electric current and / or a redox reaction, which is optionally stimulated by the electric current. This is particularly cost-effective to operate.
[0012] Example 6 is set up according to one of Examples 1 to 5, wherein the hydrogen generator includes or is formed from an electrolyzer, pyrolyzer and / or a plasma lyser. The electrolyzer is particularly cost-effective to operate.
[0013] Example 7 is set up according to one of Examples 1 to 6, wherein the hydrogen generator has multiple electrodes and / or an electrical connection. This simplifies assembly.
[0014] Example 8 is set up according to one of Examples 1 to 7, wherein the input material inlet has a thread and / or a water connection for supplying the gas supply device with water as the input material. This is particularly cost-effective in operation.
[0015] Example 9 is set up according to one of Examples 1 to 8, wherein the gas supply device is set up to produce the regeneration gas by mixing the hydrogen gas (e.g. from the hydrogen generator) with the inert gas, e.g. with a process gas (also referred to as operating gas) which contains the inert gas.
[0016] Example 10 (e.g., a gas processing system) includes: a filter device and / or a working device (e.g., working chamber); a gas supply device, e.g., a gas supply device according to one of Examples 1 to 9; and optionally a piping network (e.g., external piping network).
[0017] Example 11 is set up according to Example 10, further comprising: the inert gas inlet or an additional inert gas inlet of the filter device for receiving an inert gas, e.g. a process gas.
[0018] Example 12 is set up according to Example 10 or 11, wherein the filter device is set up to filter a process gas and / or wherein the filtering is carried out by means of (e.g. chemical) binding of at least one impurity (e.g. oxygen) carried along with (e.g. mixed with) an inert gas.
[0019] Example 13 is set up according to one of Examples 10 to 12, wherein the filter device is set up for gas purification by (e.g. chemical) binding of at least one impurity.
[0020] Example 14 is set up according to one of Examples 10 to 13, the external piping network is set up to supply the filter device in a regeneration mode with a larger volume flow of hydrogen gas (e.g. by means of the regeneration gas) than in the separation mode.
[0021] Example 15 is set up according to one of Examples 10 to 14, wherein the filtering (e.g. binding) is carried out by means of a chemical reaction (then the filter device is also referred to as a reactor) and / or at least one binding agent of the filter device which is exposed to the inert gas and / or the contaminant.
[0022] Example 16 is set up according to one of Examples 10 to 15, wherein the impurity (e.g. molecular) contains oxygen and / or moisture (e.g. water vapor).
[0023] Example 17 is set up according to one of Examples 10 to 16, wherein the process gas: is supplied to the working device in a state (also referred to as a purified state) provided by the filter device; and / or is supplied to the filter device in a state provided by the working device.
[0024] Example 18 is set up according to one of Examples 10 to 17, wherein the process gas in a state leaving the filter device has a lower proportion of impurities than in a state being fed into the filter device.
[0025] Example 19 is set up according to one of Examples 10 to 18, wherein the filter device has a regeneration gas inlet (e.g. a regeneration gas connection) for receiving a regeneration gas (into the filter device) for regenerating the filter device.
[0026] Example 20 is set up according to one of Examples 10 to 19, wherein the filter device has a first filter stage configured to bind oxygen (e.g., as a contaminant), wherein the first filter stage optionally includes a sorbent and is configured to bind oxygen by means of the sorbent. It can be understood that the first filter stage may, for example, be a combined filter stage (then also referred to as a combination filter stage) configured to bind several (e.g., chemically) different contaminants, e.g., oxygen and moisture.
[0027] Example 21 is set up according to one of Examples 10 to 20, wherein the working device has a (e.g. gas-tight sealed) working area (e.g. a chamber interior).
[0028] Example 22 is set up according to one of Examples 10 to 21, wherein the working device is set up to provide an atmosphere of (e.g. filtered) process gas in the working area.
[0029] Example 23 is set up according to one of Examples 10 to 22, wherein the filter device is set up to filter the process gas of the working device, which flows along a closed circuit which couples the filter device and the working device together.
[0030] Example 24 is configured according to one of Examples 1 to 23, further comprising at least one actuator configured (e.g. to be actuated and / or controlled in response to it) to bring the gas supply device and / or the piping network into a separation mode or a regeneration mode and / or to influence (e.g. to interrupt) a fluid piping path (e.g. of the piping network) that leads into the filter device and / or into the hydrogen generator.
[0031] Example 25 is set up according to Example 24, which has at least one actuator: one or more than one first actuator (e.g. valve) that is set up to influence a connection of the piping network, optionally when a change between the separation mode and the regeneration mode takes place.
[0032] Example 26 is configured according to Example 24 or 25, comprising at least one actuator: one or more than one second actuator (e.g., an electrical switch) configured to influence the supply of electrical power (also referred to as power supply) to the hydrogen generator, optionally when switching between the disconnect mode and the regeneration mode, optionally such that: in the regeneration mode, the hydrogen generator is supplied with electrical power; and in the disconnect mode and / or in a fault mode, the hydrogen generator is supplied with electrical power.
[0033] Example 27 is set up according to one of Examples 1 to 26, wherein the piping network provides one or more fluid paths (e.g., gas paths), of which: a first fluid path (e.g., inert gas path) leads from the inert gas inlet to the regeneration gas outlet (e.g., of the associated filter device, if present), which is optionally interrupted in the separation mode; and / or a second fluid path leads from the hydrogen generator to the regeneration gas outlet (e.g., of the associated filter device, if present); and an optional third fluid path leads from a gas mixing element, if present, to the regeneration gas outlet, which is optionally interrupted or vented in the separation mode. The inert gas path, for example, passes through the gas mixing element, if present.
[0034] Example 28 is configured according to one of Examples 1 to 27, further comprising a control device which (e.g., partially integrated in the filter device and) is configured to initiate a change between the separation mode and the regeneration mode, preferably by controlling the at least one actuator of the gas process system and / or by means of a regeneration signal.
[0035] Example 29 is set up according to Example 28, wherein the control device is set up to initiate the change from the separation mode to the regeneration mode (e.g. by actuating at least one actuator), optionally according to a change sequence and / or when a criterion (then also referred to as the regeneration criterion) is met.
[0036] Example 30 is set up according to Example 29, where the criterion is implemented by the control device (e.g., stored) and / or represents a regeneration requirement of the filter device.
[0037] Example 31 is set up according to Example 29 or 30, wherein the criterion is met if: a (e.g., sensor-detected) state of the filter device meets the criterion; a quantity of the sorbent of the filter device and / or of a resulting sorbate of the filter device meets the criterion; a time period for which the separation mode lasts meets the criterion; and / or if the control device receives a regeneration signal.
[0038] Example 32 is set up according to one of Examples 29 to 31, wherein the switching sequence is conditioned by a comparison of an actual state (e.g., of the gas process system or the gas supply device) with a target state (e.g., of the gas process system or the gas supply device) and / or includes: a first phase (also referred to as the first supply phase) in which the supply of water to the hydrogen generator is started; and / or in which a fluid line path of the piping network, which leads from the hydrogen generator to the filter device and / or passes through a gas mixing element, is at least partially purged with the inert gas; a second phase (also referred to as the second supply phase) in which the supply of electrical power to the hydrogen generator is started.
[0039] Example 33 is set up according to Example 32, wherein the second phase is started with a time delay, e.g. by several (e.g. 10 or more, e.g. 20 or more) seconds, compared to the first phase, e.g. after the hydrogen generator has been supplied with water; and / or wherein the first phase is started based on a result of a comparison.
[0040] Example 34 is configured according to one of Examples 1 to 33, further comprising: a gas mixing element for generating the regeneration gas, wherein the gas mixing element is optionally coupled to a piping network and / or is optionally configured to generate the regeneration gas, which comprises the hydrogen gas generated by the hydrogen generator.
[0041] Example 35 is set up according to Example 34, wherein the piping network in which regeneration mode is set up supplies the gas mixing element with the inert gas received via the inert gas inlet and the hydrogen gas produced by the hydrogen generator, and supplies the regeneration gas formed thereon by means of the gas mixing element to the filter device.
[0042] Example 36 is set up according to Example 34 or 35, wherein the gas mixing element is provided by means of a container (then also referred to as a gas mixing container) and / or provides a condensate separator which is set up to separate condensate (then also referred to as wastewater) that is carried along with the hydrogen gas produced by the hydrogen generator. The condensate separator promotes a dry regeneration gas.
[0043] Example 37 is set up according to one of Examples 1 or 36, wherein the regeneration gas has a hydrogen gas volume fraction of less than 10% (e.g., 5% or less, e.g., 4% or less) and / or an inert gas volume fraction of more than 90% (e.g., 95% or more). This meets the highest purity requirements.
[0044] Example 38 is configured according to one of Examples 1 to 37, further comprising: an exhaust gas outlet (e.g., exhaust gas connection) and a service gas outlet (e.g., service gas connection) which are coupled to the filter device by means of the piping network, wherein optionally, when configured in separation mode, the piping network is fluidly coupled to the service gas outlet on the outlet side and, when configured in regeneration mode, the filter device is fluidly coupled to the exhaust gas outlet on the outlet side. The service gas outlet can be used to connect the working device.
[0045] Example 39 is set up according to one of Examples 1 to 38, wherein the hydrogen generator releases less hydrogen gas in the separation mode than in the regeneration mode; and / or wherein the filter device is exposed to less hydrogen gas in the separation mode than in the regeneration mode.
[0046] Example 40 is set up according to one of Examples 1 to 39, wherein the process gas is an inert gas, e.g. nitrogen or a noble gas, optionally consisting substantially (e.g. more than 99%) of it.
[0047] Example 41 is set up according to Example 1 or 40, further comprising a storage container (e.g. water tank) which is coupled to the hydrogen generator (e.g. input side) by means of the input material inlet, for holding the input material, wherein the storage container is optionally coupled to the hydrogen generator by means of a pump (e.g. diaphragm pump).
[0048] Example 42 is set up according to Example 41, wherein the storage container has a pressure equalization opening which is set up to release gas (e.g. oxygen) from the storage container to its surroundings (e.g. into the safety container).
[0049] Example 43 is configured according to one of Examples 1 to 42, and further comprises a safety device configured (e.g., in regeneration mode) to interrupt the release of hydrogen gas (e.g., by interrupting the electrical supply to the hydrogen generator) when a criterion (then also referred to as a fault criterion) is met (which is determined as, for example, a fault condition). The fault criterion is optionally met if at least one operating parameter (e.g., of the gas process system or at least of the gas supply device) meets the fault criterion. This increases safety.
[0050] Example 44 is set up according to Example 43 and further comprises a sensor arrangement configured to detect at least one operating parameter. This increases safety.
[0051] Example 45 is set up according to Example 43 or 44, wherein at least one operating parameter relates to supplying the hydrogen generator with water, and / or represents one or more than one of the following: a temperature of the water; an electrical conductivity of the water; and / or a supply of water, e.g., a water level; a flow rate at which the water is supplied to the hydrogen generator. This prevents dry running.
[0052] Example 46 is set up according to one of Examples 43 to 45, wherein the at least one operating parameter represents a pressure (e.g., an overpressure) which is optionally: the gas pressure of a safety atmosphere in which the hydrogen generator and / or at least one component of the piping network and / or the gas mixing element are located; a gas pressure of the hydrogen gas (e.g., to which the hydrogen generator is exposed); or a gas pressure of the regeneration gas (e.g., to which the hydrogen generator and / or the regeneration gas connection is exposed). This inhibits hydrogen gas enrichment.
[0053] Example 47 is set up according to one of Examples 43 to 46, wherein the at least one operating parameter represents a pressure (or a flow rate) of the regeneration gas (or the hydrogen gas) with which the hydrogen gas and / or the regeneration gas is supplied to the filter device; and / or wherein the at least one operating parameter represents a flow rate and / or a pressure of the inert gas. This inhibits an enrichment of hydrogen gas.
[0054] Example 48 is set up according to one of Examples 43 to 47, wherein the at least one operating parameter represents a state of a chamber housing in which the hydrogen generator and / or at least one component of the piping network and / or the gas mixing element are arranged, wherein the state optionally indicates whether the chamber housing (e.g., its door) is in a closed (e.g., gas-tight) state or not, and / or whether the chamber housing is permeated by a gas flow (e.g., an air flow or a nitrogen gas flow). This inhibits hydrogen gas enrichment.
[0055] Example 49 is set up according to one of Examples 43 to 48, wherein at least one operating parameter represents a state (e.g., pressure and / or chemical composition) of a safety atmosphere in which the hydrogen generator and / or at least one component of the piping network and / or the gas mixing element are located. This inhibits an enrichment of hydrogen gas.
[0056] Example 50 is set up according to one of Examples 43 to 49, wherein the safety device is implemented by means of the control device and / or by means of an electric generator configured to supply the hydrogen generator with electrical power. This facilitates a cost-effective implementation.
[0057] Example 51 is configured according to Example 1 or 50, further comprising a chamber housing (also referred to as a safety housing), e.g., a cabinet (e.g., a control cabinet), in which the hydrogen generator and / or the gas mixing element are arranged, wherein the chamber housing optionally has a chamber cover which, when the chamber housing is closed, is configured to seal a maintenance opening of the chamber housing gas-tight. This increases safety. The chamber cover can, for example, be configured as a door.
[0058] Example 52 is configured according to one of Examples 1 to 51, further comprising a gas supply device (e.g. a blower, e.g. having a fan) which is configured to flush the hydrogen generator with a (e.g. non-flammable) gas stream (e.g. air, e.g. ambient air) and / or to supply the gas stream to the chamber housing, by means of which a safety atmosphere and / or an overpressure is optionally formed (e.g. in the chamber housing), wherein the hydrogen generator and / or at least one component of the piping network and / or the gas mixing element are arranged.
[0059] Example 53 is set up according to Example 52, wherein the chamber housing has a gas outlet restrictor (e.g., an orifice plate) which is either fixed or adjustable, e.g., can be selectively set to a first state or a second state, which differ from each other in a resistance that opposes the gas flow out of the chamber housing. This facilitates the adjustment of the safety atmosphere.
[0060] Example 54 is set up according to Example 53, wherein the first state or the second state of the gas outlet throttle and the gas delivery device are configured relative to each other such that: the pressure of the safety atmosphere in the chamber housing is greater than the hydrostatic pressure (then also referred to as ambient pressure) of the Earth's atmosphere (also referred to as air) at the location of the gas process system, optionally by at least 1 millibar (e.g., 5 millibar, e.g., 10 millibar, e.g., 20 millibar, e.g., 50 millibar) and / or by a maximum of 500 millibar above ambient pressure; and / or the gas flow has a larger volume flow (e.g., at least ten times or at least one hundred times) than the hydrogen gas released by the hydrogen generator. This inhibits the enrichment of hydrogen gas.
[0061] Example 55 is set up according to one of Examples 1 to 54, wherein the filter apparatus includes a sorbent (e.g. as a first separation stage) configured to bind oxygen or to produce sorbate therefrom, wherein the sorbent is optionally a chemical absorbent.
[0062] Example 56 is set up according to Example 55, wherein the sorbent comprises a metal, optionally copper; and / or wherein the sorbent is in a solid state of matter, optionally granular.
[0063] Example 57 is set up according to one of Examples 1 to 56, wherein the filter device includes an additional sorbent (e.g., as a second separation stage or implemented by means of the first filter stage) configured to bind moisture. For the sake of clarity, reference is made here to multiple filter stages for the purposes of understanding the functions of the filter device, although it should be understood that these need not necessarily be separate filter stages. The description provided here can therefore apply analogously to a filter device that includes (e.g., only) the combined filter stage, which integrates the properties of both the first and second filter stages.
[0064] Example 58 is set up according to Example 57, wherein the additional sorbent includes a desiccant, e.g., silicate (e.g., zeolite), carbonate, and / or silica gel. Alternatively or additionally to the desiccant, a cold trap can be used, for example, to bind water. Zeolite is particularly cost-effective and requires little maintenance.
[0065] Example 59 is configured according to one of Examples 1 to 58, further comprising a heating device which is configured to supply thermal power to the filter device (e.g., the sorbent and / or additional sorbent), e.g., in the regeneration mode and / or more than in the separation mode. This promotes (e.g., accelerates) the regeneration of the filter device.
[0066] Example 60 is set up according to one of Examples 1 to 59, wherein the hydrogen generator has at least one electrolysis cell (e.g., one or more electrolysis cells), which optionally includes a proton-permeable polymer membrane (PEM) (then also referred to as a PEM cell). The PEM cell is easy to operate and requires a low operating voltage, which improves safety.
[0067] Example 61 is set up according to Example 60, wherein the hydrogen generator has several electrolysis cells which are optionally connected electrically in series, and wherein the several electrolysis cells are optionally several PEM cells. The series connection reduces the electrical current, which improves safety.
[0068] Example 62 is set up according to one of Examples 1 to 61, further comprising several modules, of which: a first module (e.g. gas supply module) comprises the hydrogen generator and a first connection coupling (e.g. of the piping network), a second module (e.g. filter module) comprises the filter device and a second connection coupling (e.g. of the piping network), wherein the first connection coupling and the second connection coupling are configured to be fluidly joined together.
[0069] Example 63 is set up according to Example 62, wherein the first coupling and the second coupling are joined together to provide several separate fluid routing paths.
[0070] Example 64 is set up according to Example 62 or 63, wherein the pipeline network has two gas lines which are parallel to each other (spatially and / or in terms of circuitry) and each gas line terminates in the first coupling and in the gas mixing element.
[0071] Example 65 is configured according to one of Examples 62 to 64, wherein the first module comprises a first control unit of the control device and / or wherein the second module comprises a second control unit of the control device, the second control unit being configured to generate the regeneration signal when the regeneration criterion is met, which is optionally implemented (e.g., stored) by the second control unit and / or represents a regeneration requirement of the filter device. The regeneration signal can, for example, be transmitted from the second control unit to the first control unit, which is configured to initiate the changeover sequence or at least to initiate the start of the generation of the regeneration gas.
[0072] Example 66 is set up according to one of Examples 1 to 65, furthermore comprising a gas source which contains the inert gas (e.g. as a component of the process gas) and / or is coupled to the inert gas inlet.
[0073] Example 67 is set up according to one of Examples 1 to 66, wherein the filter device has two first separation stages (e.g. each having the sorbent) and an actuator, wherein the actuator is set up to alternately connect the two first separation stages to the gas supply device and / or the working device in a gas-conducting manner.
[0074] Example 68 (e.g., a process arrangement) is set up according to one of Examples 1 to 67, which includes the working device, wherein the working device is, for example, coupled to the process gas outlet and / or set up to provide a working process using the inert gas supplied by the filter device.
[0075] Example 69 is set up according to Example 68, wherein the working device comprises one of the following: a working chamber (e.g., glove box) configured to hold the inert gas and / or an object; and / or a process device (e.g., welding device) configured to process an object using the inert gas provided by the gas process system. The process device may, for example, be a joining device. For example, welding may be performed using argon as the inert gas.
[0076] Example 70 (e.g., a method for operating the configuration according to any of Examples 1 to 69) includes: supplying a working device with inert gas provided (e.g., filtered) by the filter device in the separation mode; regenerating the filter device (e.g., its sorbates) by means of hydrogen gas provided by the hydrogen generator in the regeneration mode.
[0077] Example 71 is set up according to one of Examples 1 to 70, wherein oxygen gas carried along with the inert gas taken in by the inert gas inlet is bound in the separation mode by means of the filter device (e.g. its sorbents) and the resulting product is supplied to the working device.
[0078] Example 72 is set up according to one of Examples 1 to 71, wherein the regeneration gas comprises the generated hydrogen gas and / or wherein regeneration gas is produced by mixing the generated hydrogen gas with the inert gas (e.g. process gas).
[0079] Example 73 is set up according to one of Examples 1 to 72, wherein the process gas provided (filtered) by the filter device has a mass fraction of inert gas (e.g. argon and / or nitrogen gas) of more than 99%, e.g. more than 99.9% (corresponding to a purity of 1N), e.g. more than approximately 99.99% (corresponding to a purity of 2N), e.g. more than approximately 99.999% (corresponding to a purity of 3N), e.g. more than approximately 99.9999% (corresponding to a purity of 4N), e.g. more than approximately 99.99999% (corresponding to a purity of 5N), e.g. more than approximately 99.99999% (corresponding to a purity of 6N).
[0080] Example 74 is set up according to one of Examples 1 to 73, wherein the process gas: has a larger proportion of inert gas than the regeneration gas; and / or wherein the regeneration gas has a larger proportion of hydrogen gas than the process gas.
[0081] Example 75 is set up according to one of Examples 1 to 74, wherein the starting material (e.g. water) is deionized.
[0082] Example 76 is set up according to one of Examples 1 to 75, wherein the impurity is gaseous and / or contains oxygen.
[0083] Example 77 is set up according to one of Examples 1 to 76, wherein the process gas is the inert gas and includes (e.g., is mixed with) an impurity (e.g., consists of).
[0084] Example 78 is set up according to one of Examples 1 to 77, wherein the regeneration gas outlet, the inert gas inlet, the feedstock inlet and / or the regeneration gas inlet have: a connection (e.g. consisting of) and / or a fluid line which, for example, leads into the connection.
[0085] Example 79 is set up according to one of Examples 1 to 78, wherein the gas supply device includes a hydrogen generator for producing the hydrogen gas by electrolysis of water (also known as water electrolysis). This is cost-effective and user-friendly.
[0086] Example 80 is set up according to one of Examples 1 to 79, further comprising: the (e.g. external) piping network, which is set up: in a separation mode, to supply the filter device (only) the process gas taken in by means of the inert gas inlet (or the additional inert gas inlet), and / or in a regeneration mode, to supply the filter device with the hydrogen gas produced by means of the hydrogen generator (e.g. by means of the regeneration gas).
[0087] Example 81 is set up according to one of Examples 1 to 80, further comprising: the (e.g. internal) piping network which is set up: in a regeneration mode to supply the inert gas taken in at the inert gas inlet to the generation of the regeneration gas; and / or is set up in a separation mode to displace the regeneration gas from the filter device and / or the gas supply device by means of the inert gas taken in at the inert gas inlet (e.g. at least sectionally) and / or to shut off the inert gas inlet from the regeneration gas outlet.
[0088] They show Fig. 1A a gas supply device according to various embodiments in a schematic assembly diagram; Fig. 1B a gas process system according to various embodiments in a schematic diagram; Fig. 2 a gas supply device according to various embodiments in a schematic diagram; Fig. 3A a gas supply module according to various embodiments in a schematic perspective view; Fig. 3B a method according to different embodiments in a schematic flowchart; Fig. 4A and Fig. 4B each a gas process system according to different embodiments in a schematic circuit diagram; Fig. 5A a gas process system according to various embodiments in a schematic diagram; and Fig. 5B the phases of a switching sequence according to different embodiments in a schematic flowchart.
[0089] The following detailed description refers to the accompanying drawings, which form part thereof and illustrate specific embodiments in which the invention can be implemented. In this context, directional terminology such as "top," "bottom," "front," "back," "anterior," "rear," etc., is used with reference to the orientation of the described figure(s). Since components of embodiments can be positioned in a number of different orientations, the directional terminology serves only for illustration and is in no way limiting. It is understood that other embodiments may be used and structural or logical modifications may be made without deviating from the scope of protection of the present invention.It is understood that the features of the various exemplary embodiments described herein can be combined with one another, unless specifically stated otherwise. The following detailed description is therefore not to be interpreted in a limiting sense, and the scope of protection of the present invention is defined by the appended claims.
[0090] Within the scope of this description, the terms "connected," "connected," and "coupled" are used to describe both direct and indirect connections (e.g., resistive and / or electrically conductive, such as an electrically conductive connection), direct or indirect connections, and direct or indirect couplings. In the figures, identical or similar elements are designated with identical reference numerals where appropriate.
[0091] The term "gas mixing element" (also referred to as a gas mixing device) refers to a device designed to form a gas mixture. The gas mixing element can have: several inlets (e.g., fluid lines) through which several gases can be supplied separately, and a cavity (also referred to as a mixing chamber) into which the inlets open to combine the gases so that they mix and form the mixture. The mixing chamber is provided, for example, by a gas mixing vessel, but can also be provided by a pipe branching system.
[0092] The term "gas" here refers to a gaseous material, e.g., a pure gas or a gas mixture. For some pure substances, their gaseous (e.g., molecular) state is expressed by the suffix "-gas," such as "hydrogen gas" for pure hydrogen. The term "hydrogen gas" refers to molecular hydrogen. The term "oxygen gas" refers to molecular oxygen. The term "nitrogen gas" refers to molecular nitrogen.
[0093] The term "inert gas" refers to a gas (e.g., a pure gaseous substance) that is unreactive under normal conditions and hardly (e.g., not at all) participates in chemical reactions. The inert gas is, for example, inert to the filter device or at least its separation stages, such as the sorbent (also called a sorbent). Examples of inert gases include noble gases (e.g., argon) and nitrogen gas. If the inert gas contains at least one (e.g., gaseous) impurity, the resulting mixture is called "process gas," which consists essentially of the inert gas, e.g., with a purity greater than 1N, e.g., 2N, 3N, 4N, or 5N. For the sake of simplicity, the term "inert gas" is used here to refer to the process gas, which can be provided, for example, by means of the process gas, which may contain at least one impurity.Examples of contamination include: oxygen gas and / or moisture (i.e., gaseous water vapor).
[0094] The term "filtration" generally refers to a separation process (also called separation for short) by which two components of a mixture (e.g., a gas mixture) are separated, for example, by sorption (e.g., adsorption and / or absorption). Examples of separation processes include chemical separation (e.g., by absorption) and physical separation (e.g., by adsorption). Sorption is a binding process (also called binding) that leads to the accumulation of an impurity within a chemical phase (then also called absorption) or at an interface between two chemical phases (then also called adsorption). In sorption, the sorbent (also called sorbent) is converted into a sorbate containing the bound impurity by binding the impurity (then also called sorbent).During regeneration, the process reversed to sorption is stimulated, in which the sorbate is transferred back into the sorbent, releasing the impurity.
[0095] The term "electrolysis" refers to a chemical process that is initiated (e.g., forced) by the application of electrical power. This electrical power supplies chemical energy to a starting material, causing it to release several reaction products into which it is, for example, broken down. One example is the electrolysis of water (also called water electrolysis), which releases hydrogen gas and oxygen gas as reaction products. The electrical power can be supplied by a direct current source and delivered to the electrolyzer, where the electrolysis takes place.
[0096] The term "control device" can be understood as any type of logic-implementing entity that may, for example, have circuitry, instructions, and / or a processor capable of executing software stored in a memory medium, firmware, or a combination thereof, and outputting instructions based on that software. The control device may, for example, be configured using code segments (e.g., software) to provide various functions implemented by those code segments.
[0097] The term "actuator" (e.g., comprising an actuator) can be understood as a transducer designed to influence a given state, for example, in response to the actuator being activated or the actuator being controlled by a control signal. An actuator can be used to influence, for example, a physical quantity (such as pressure or temperature), a process (e.g., gas flow), or a device. Examples of actuator components include: a shut-off device (e.g., a shut-off valve or butterfly valve), a throttling device (e.g., a gas flow regulator, pressure valve, or needle valve), a directional control valve, a drive device as an actuator (e.g., an electric motor, solenoid, or piston), an electrical switch, or similar devices. The control signal can be generated, for example, by a control device and / or transmitted via an electrical line.An actuator can be part of a control chain, which includes a corresponding infrastructure (e.g., a processor, storage medium, and / or bus system, or similar components) to control the actuator based on a target state as input and to generate a corresponding electrical control signal representing the controlled variable. The control chain can be implemented, for example, by means of a control device.
[0098] The term "sensor" (also referred to as detector) can be understood as a transducer designed to qualitatively or quantitatively detect a property of its environment corresponding to the sensor type, such as a physical or chemical property and / or a material composition. The measured quantity is the physical quantity to which the sensor applies. A sensor can be part of a measurement chain, which includes a corresponding infrastructure (e.g., a processor, storage medium, and / or bus system, or similar components) to control the sensor, process its detected measured quantity as an input, and, based on this, provide an electrical signal as an output representing the input quantity. The measurement chain can be implemented, for example, by means of a control device.
[0099] The term "gas-tight" when referring to a hollow body (e.g., a chamber or other container, a pipe) or its cavity (e.g., a section) expresses that several adjacent parts (e.g., walls) of the hollow body can be sealed or connected to another hollow body by means of a seal. Examples of hollow bodies include: a pressure chamber, a vacuum chamber, an atmospheric pressure chamber, etc.
[0100] The term "desiccant" here refers to a water-binding (e.g., hygroscopic) material designed to bind water physically or chemically. Zeolite as a desiccant is particularly low-maintenance because it is durable and readily regenerable, non-toxic, and therefore safe and cost-effective.
[0101] Quantity specifications relating to a gas, e.g., its proportion in a gas mixture or in relation to another gas, refer here to its volume, for example, expressed as a volume percent (Vol%), which is also referred to as volume fraction. These specifications are based on the same reference conditions, e.g., standard conditions.
[0102] The term "monitoring" in connection with an operating parameter (or, by analogy, a state represented by it) can be understood as a process in which the operating parameter is recorded as its actual state (e.g., the current value of the operating parameter) and compared with a target (e.g., a desired state and / or criterion). Optionally, a signal can be generated based on this comparison. For example, if the deviation of the actual state from the desired state meets the criterion that represents a fault condition (then also referred to as the fault criterion), the signal representing the fault condition can be generated. Examples of such a signal include: an electrical signal, an acoustic signal, and an optical signal. For example, the signal could trigger the shutdown of the hydrogen generator, e.g., by interrupting the supply of electrical power to the hydrogen generator.
[0103] For clarity, a material interface is referred to here as an "inlet" or "outlet," such as a regeneration gas outlet, inert gas inlet, or output material inlet. The material interface is conductive (e.g., fluid-conductive) and therefore has a cavity through which the material is guided, transported, or can flow. Examples of interface components include: fluid lines, connections, and couplings. Examples of connections include: quick couplings (e.g., gas quick couplings), flanges, push-in fittings, sockets, etc. Examples of fluid lines include: pipes (e.g., supply pipes) and hoses. The material interface may, for example, have an integrated coupling, such as a bayonet coupling, snap-in coupling, screw coupling, etc.
[0104] For the sake of simplicity, this section refers to an example configuration (see Example 6) of the hydrogen generator, which is set up as an electrolyzer. During operation, this electrolysis process produces water to generate hydrogen and oxygen gas. The description provided here can be applied analogously to any other process by which hydrogen can be produced, such as steam reforming or pyrolysis, as well as to any other type of feedstock.
[0105] This section explains aspects based on various components (e.g., gas supply device, filter device, working device) and a gas process system formed from them, whereby it can be understood that these components can also be provided individually, e.g., not necessarily as part of the gas process system.
[0106] Fig. Figure 1A illustrates a gas supply device according to various embodiments 100a in a schematic diagram, optionally configured according to Example 1. For ease of understanding, the existing fluid lines 110a, 110b, 110c are shown, some of which can be controlled (e.g., interrupted or connected) by means of an actuator (if present). For each of the existing connections, for example, the feed material inlet 104, the regeneration gas outlet 106, and the inert gas inlet 108 (see Example 78), there is a fluid line 110a, 110b, 110c, which terminates in the connection. It can be understood that a fluid line 110a, 110b, 110c can be provided by means of at least one fluid line, but this is not necessarily required if the connection is directly mounted.For example, the input material inlet 104 (also referred to as input material inlet) can be mounted on the electrolyzer 102 and provide its input port, or it can be connected to the input port of the hydrogen generator 102 by means of a fluid line 104a.
[0107] Additionally, the fluid lines can branch, but this is not mandatory. For the sake of simplicity, reference is made to a pipe network 110 (see Example 25) which is formed by the fluid lines and (if present) the actuators and provides the fluid line paths 110a, 110b, 110c.
[0108] An example configuration of water electrolysis is started in phases, for example, when the regeneration mode is initiated. In a first supply phase, the electrolyzer 102 is supplied with water as the feedstock. This is done, for example, by opening a valve and / or starting a pump 168. The water is located in a storage tank 166 (see Example 41), which can be refilled as needed. In a second supply phase, electrical power is supplied to the electrolyzer 102, which is converted by the water electrolysis. The hydrogen produced is fed to the regeneration gas outlet 106, for example, before or after it is mixed with inert gas, which is taken in via the inert gas inlet 108.
[0109] Fig. Figure 1B illustrates a gas process system according to various embodiments 100b in a schematic diagram, for example set up according to Example 10 and / or comprising a gas supply device 156 according to embodiments 100a.
[0110] An example configuration of the filter device 152 (also referred to as the separation device) has several cascaded filter stages 152a, 152b (also referred to as separation stages), each filter stage being configured to bind an impurity carried by the inert gas passing through the filter stage. The filter stages 152a, 152b have a first filter stage (optional according to Example 56) configured to bind oxygen using copper as a sorbent (then also referred to as the copper filter stage 152a). The filter stages 152a, 152b further have a second filter stage (optional according to Example 58) configured to bind moisture using a zeolite as a sorbent. It can be understood that any other sorbent capable of binding the existing impurity (e.g., a metal other than copper) can be used.
[0111] In regeneration mode, the copper and / or zeolite (if present) are exposed to the process gas flowing through the filter device. The oxygen in the process gas is bound by the copper via a chemical reaction to form copper oxide as a sorbate. The moisture in the process gas is adsorbed by the zeolite. The process gas output by the filter device in separation mode (then also referred to as filtered process gas) can, for example, have an inert gas purity of more than 1N, e.g., 2N, 3N, 4N, or 5N.
[0112] An example configuration of the working device 152 (optionally according to Example 10 and / or Example 65) has a gas-tight working chamber (also referred to as an enclosure) in which a cavity 154 is formed as a working area. The working device 152 is configured to create an atmosphere in the cavity 154 of the filtered process gas (then also referred to as the process gas atmosphere), which flows from the filter device 152 to the working device 152. For this purpose, a self-contained fluid path 160 (then also referred to as the working path) can be provided, which connects the filter device 152 and the working device 152. If the working device 152 is configured as a glove box (then also referred to as a glove box) (see Example 65), it can further include one or more gloves adjacent to the cavity 154.
[0113] The filter device 152 can couple two control valves 164, 162, e.g., directional control valves, as actuators (or components thereof) by means of which the working path 160 can be interrupted, e.g., in regeneration mode. By means of the control valves 164, 162, a fluid path (then also referred to as the regeneration path) is provided in regeneration mode from the regeneration gas outlet 106 through the filter device 152 to an outlet 114 (e.g., a disposal outlet), and in separation mode through the filter device 152 to the process gas outlet 124.
[0114] In regeneration mode, the copper oxide (or copper, if present) and / or the zeolite (if present) can be exposed to the regeneration gas flowing through the filter device. The hydrogen gas in the regeneration gas reacts chemically with the copper oxide to form copper, releasing moisture, which is carried along with the remaining regeneration gas to outlet 114. The water adsorbed by the zeolite is released into the regeneration gas and carried along by it to outlet 114. Furthermore, a heating device (see Example 59) is provided, which, in regeneration mode, supplies thermal energy to the filter device so that the copper oxide and / or the zeolite are heated, thus promoting regeneration.
[0115] Other examples of the work device 152 or components thereof (see example 69) exhibit: - a joining device (e.g. welding device) as a process device, which is set up to join (e.g. welding) using the process gas, e.g. to weld titanium, to carry out a 3D print using titanium, and / or to machine an aircraft engine; - a work chamber in which sensitive objects are to be stored or processed, e.g. objects sensitive to moisture or oxygen; - a working chamber (e.g. vacuum chamber) in which a sensitive process (e.g. research process) is carried out; - a work chamber of a manufacturing plant.
[0116] Examples of such sensitive objects include: - Semiconductor electronics, such as displays, or their components, for example OLED displays or OLEDs (organic light-emitting diodes), - Raw materials, e.g. organic materials and / or dyes; - Batteries and their components, such as electrodes, lithium-containing components, etc. - Electronics of a different type.
[0117] An example configuration of the process gas atmosphere is inert and / or has a mass fraction of inert gas (e.g., argon and / or nitrogen gas) of more than 99%, e.g., more than 99.9% (corresponding to a purity of 1N), e.g., more than approximately 99.99% (corresponding to a purity of 2N), e.g., more than approximately 99.999% (corresponding to a purity of 3N), e.g., more than approximately 99.9999% (corresponding to a purity of 4N), e.g., more than approximately 99.99999% (corresponding to a purity of 5N), e.g., more than approximately 99.99999% (corresponding to a purity of 6N).
[0118] A particularly compact example configuration of the gas process system has exactly one inert gas source 120. The inert gas source 120 is connected to the inert gas inlet 108 of the gas supply device to supply the gas supply device with inert gas in regeneration mode, which is then mixed with the hydrogen gas to form the regeneration gas. Furthermore, the inert gas source 120 is connected to the working path 160, for example, by means of a branch inert gas inlet 118 (if present) or by means of the filter device 108. This allows the filter device to be supplied with a quantity of inert gas in separation mode that replaces inert gas escaping from the working device 154.The description for the compact implementation can apply analogously to multiple inert gas sources, of which a first inert gas source is connected to the inert gas inlet 108 of the gas supply device and a second inert gas source is connected to the inert gas inlet 118 branching off from the working path 160. Examples of inert gas sources include: a gas cylinder or a building gas line in which the inert gas is located.
[0119] An example configuration of the gas process system (optional according to Example 62), which facilitates the retrofitting of an existing filter device with the gas supply device 156, has a modular design. Here, the gas supply device 156 is provided as a first module (then also referred to as the gas supply module), and the filter device is provided as a second module (then also referred to as the filter module). The filter module and the gas supply module each have complementary connection couplings by means of which they can be coupled to each other. For example, the connection coupling of the gas supply module can provide the regeneration gas outlet 106, optionally the inert gas inlet 108, and optionally an electrical connection (then also referred to as the signal connection).Correspondingly, the connection coupling of the filter device 152 can be configured to receive the regeneration gas from the regeneration gas outlet 106, optionally to supply the inert gas inlet 108 with inert gas, and / or optionally to couple a regeneration signal into the signal port. In simple terms, the regeneration signal indicates that regeneration of the filter device 152 is to take place. For example, the two control valves 164 and 162 can be switched using the regeneration signal.
[0120] The regeneration signal can be provided, for example, by means of a DC voltage applied to the signal terminal while the regeneration phase is active. The regeneration signal 168 can, of course, also be more complex or generated according to a communication protocol (e.g., a fieldbus communication protocol) if instructions and / or more information need to be transmitted.
[0121] An example configuration of the regeneration signal (see Example 31) is generated by a control unit of the filter module as soon as the separation mode has been active for a set period of time. Alternatively or additionally, the electrical conductivity of the copper can be monitored by sensors as a representative of the saturation of the copper filter stage. Correspondingly, the gas supply module has a control unit that starts the water electrolysis, e.g., in phases, in response to receiving the regeneration signal from the filter device.
[0122] Fig. Figure 2 illustrates a gas supply device according to various embodiments 200 in a schematic diagram, which may optionally be configured according to one of the embodiments 100a or 100b.
[0123] An example configuration of the safety enclosure 230 (see Example 51) houses the electrolyzer 102, the gas mixing element 240, and the water tank 166. Cost savings are achieved by providing the safety enclosure in the form of a control cabinet, which has a maintenance opening and a door 262 (also referred to as a chamber door) that closes the maintenance opening. The door 262 is equipped with a seal to create a gas-tight closure for the maintenance opening. The seal can be mounted, for example, on the door 262 or on a frame of the safety enclosure 230 in which the maintenance opening is formed, and can be configured to seal any gap between the frame and the door 262.
[0124] To increase safety, the safety enclosure 230 can be actively ventilated by means of a fan 216 as a gas supply device (see Example 52). The fan 216 is configured to draw in ambient air (e.g., from the Earth's atmosphere) and transport it as a gas flow into the safety enclosure (then also referred to as the safety atmosphere). This promotes a pressure increase within the safety enclosure. The safety atmosphere exits the safety enclosure 230 through a gas outlet throttle 318 (e.g., configured as an actuator) (see Example 53). The gas outlet throttle 318 can optionally be manually adjustable, which facilitates the adjustment of the pressure in the safety enclosure and / or the gas flow. To reduce costs, the gas outlet throttle 318 has several orifices of different diameters, which can be interchanged.However, a fixed gas outlet throttle 318 can also be used, for example if the adjustment is only to be carried out once during assembly.
[0125] The gas supply device has (optionally according to Example 24, e.g., Example 26) several actuators by means of which the gas flow in the gas supply device can be influenced and which are represented here by way of example as valves. In this regard, it can be understood that what is described here can apply analogously to differently implemented actuators, e.g., a mass flow controller, a throttle valve, or similar. Likewise, it can be understood that the functions for influencing the gas flow, which are explained using separate actuators, can also be implemented together in one actuator and vice versa. Furthermore, some actuators have an electrical signal input 250 by means of which they can be electrically controlled by a control signal that is generated by the control device (not shown) and supplied to the signal input 250.
[0126] The piping network (optionally as shown in Example 27) provides an inert gas path 110c as a fluid path, which leads from the inert gas inlet 108 through the gas mixing element 240 to the regeneration gas outlet 106. The piping network also provides a hydrogen path as a fluid path 110b, which leads from a hydrogen port A2 of the electrolyzer 102 through the gas mixing element 240 to the regeneration gas outlet 106. The piping network further provides a regeneration gas path 110d as a fluid path, which leads from the gas mixing element 240 to the regeneration gas port 106 and from which a vent path 110e branches off as a fluid path. The vent path 110e terminates in a venting actuator 230 and / or a safety valve 232.
[0127] The inert gas flow received and supplied to the regeneration gas outlet 106 along the inert gas path 110c is controlled by a blocking actuator 228 (e.g., a shut-off valve) and / or an adjustment actuator 220 (e.g., a needle valve and / or a gas flow regulator). The blocking actuator 228 is controlled by a control signal generated according to the current mode, which can be, for example, the regeneration mode or the separation mode. If the current mode is the separation mode, the inert gas path 110c is interrupted (i.e., shut off) by the blocking actuator 228. If the current mode is the regeneration mode, the blocking actuator 228 releases the inert gas path 110c (i.e., the inert gas flow is released). The adjustment actuator 220 is designed to be operated manually in order to manually increase or decrease the inert gas flow 202i (also referred to as adjustment).Once set, the adjustment actuator 220 can remain unchanged for several cycles of separation mode and regeneration mode, for example.
[0128] An example configuration of the gas mixing element 240 (optional according to Example 34) includes a gas mixing vessel (then also referred to as a mixing vessel). A condensate separator 240a is arranged in the gas mixing vessel, through which the hydrogen path 110b passes and which is designed to release moisture carried along with the hydrogen gas into the gas mixing vessel. The condensate separator 240a is provided, for example, by means of a fluid line opening freely into the gas mixing vessel, from which condensed moisture (then also referred to as water condensate) can drip off. The water condensate is collected in the gas mixing vessel and disposed of, since small amounts of hydrogen gas are dissolved in the water condensate. This increases safety.
[0129] The venting actuator 230 is controlled by a control signal generated according to the current mode, which can be, for example, regeneration mode or isolation mode. If the current mode is isolation mode, the regeneration gas path 110e is vented by means of the venting actuator 230, e.g., into the safety housing 230. If the current mode is regeneration mode, the venting actuator 230 is closed. The safety valve 232 is designed to be manually operated to manually increase or decrease the pressure of the regeneration flow 202r to which the regeneration gas outlet 106 is exposed (also referred to as adjustment). Once set, the safety valve 232 can remain unchanged, e.g., for several cycles of isolation and regeneration modes. The safety valve serves, e.g., as overpressure protection and is, e.g., preset and unchangeable, or at least not manually adjustable (e.g., without tools).
[0130] In the illustrated exemplary configuration, the water (then also referred to as supply water), driven by a pump 168, circulates through the electrolyzer 102 in a closed circuit (then also referred to as supply circuit). The supply circuit has the fluid line path 110a (also referred to as water inlet), which leads from the water tank 166 to an inlet port A1 of the electrolyzer 102. The water tank 166 can, for example, be connected to the output material inlet 104, e.g., by screwing it in. The supply circuit has an additional fluid line path 252r (also referred to as water return), which leads from a return port A3 of the electrolyzer 102 to the water tank 166. Furthermore, the water tank 166 has a venting device (e.g., a pipe or opening) by means of which the water tank 166 can be vented, e.g., into the safety housing 230.This facilitates the removal of oxygen gas 202o, which is carried along with the supply water (e.g. dissolved in it) and released in the water tank 166, from the supply circuit.
[0131] Furthermore, various sensors may be present to monitor the current state of the gas supply device, e.g., one or more of its operating parameters. Examples of such sensors include: - a first motor sensor 210, which is set up to record the speed of the pump 168 (e.g. of one motor M thereof) as an actual operating parameter; - a second motor sensor 212, which is configured to record the speed of the fan 216 (e.g. of one motor M thereof) as an actual operating parameter; - a water flow sensor 222, which is set up to record a flow rate 202w of the supply water through the electrolyzer 102 as an actual operating parameter; - several sensors as the first measuring element 208, which are configured to record the current state of the supply water (see example 45) as an actual operating parameter, e.g. a temperature of the supply water as an actual operating parameter, an electrical conductivity of the supply water as an actual operating parameter; and / or a fill level of the supply water in the water tank 166 as an actual operating parameter; - several sensors as a second measuring element 218, which are configured to record the actual state of the inert gas flow 202i as an actual operating parameter, e.g. the supply pressure of the inert gas to which the inert gas inlet 108 is exposed, and / or the mixing pressure of the inert gas to which the gas mixing element 240 is exposed; - a pressure sensor 206, which is set up to record the pressure in the safety housing 230 as an actual operating parameter.
[0132] For safety reasons, the gas supply device may include a safety device (not shown) which is coupled to one or more of the sensors via a signal line 204, 214 in order to read the sensor data. The safety device may be configured to implement one or more safety mechanisms using the sensors. A first safety mechanism is configured to interrupt the electrical power supplied to the electrolyzer 102 when a fault condition is detected, in order to interrupt the water electrolysis (also referred to as fault mode). An optional second safety mechanism is configured to emit an alarm signal (e.g., an audible one) when the fault condition is detected.
[0133] Examples where the error state is determined include: - if the speed of the pump 168 (e.g. of one motor M thereof) and / or that of the fan 216 falls below a threshold value; - if the flow rate 202w of the supply water through the electrolyzer 102 falls below a threshold value; - if the temperature of the supply water exceeds a threshold value; - if the electrical conductivity of the supply water and / or the fill level of the supply water falls below a threshold value; - if the supply pressure of the inert gas, the mixed pressure of the inert gas, or a difference thereof leaves a range between two threshold values; - the pressure in safety chamber 230 falls below a threshold value.
[0134] The threshold values clearly define the range for each operating parameter within which the operation of the gas supply device meets the safety requirements. For example, if fan 216 fails, there is a risk that a flammable gas mixture will accumulate in safety chamber 230. If pump 210 fails, there is a risk that electrolyzer 102 will overheat or at least run dry. If the pressure of the inert gas is too high or too low, there is a risk that the resulting regeneration gas will become flammable.
[0135] Fig. Figure 3A illustrates a gas supply module according to various embodiments 300a in a schematic perspective view, which are optionally configured according to one of the embodiments 100a to 200. An example configuration of the connection coupling 302 (see Example 62) of the gas supply module has the inert gas inlet 108, by means of which the gas supply module can draw the inert gas from the filter device. The connection coupling 302 of the gas supply module also has the regeneration gas outlet 10, by means of which the gas supply module can supply the regeneration gas to the filter device.
[0136] An example configuration of the maintenance opening 304 (see example 51) is set up such that, when the chamber cover is removed from the safety housing 302, it allows access to the electrolyzer 102, the gas mixing element 240 and the water tank 166.
[0137] An example configuration of the water tank 166 and the gas mixing element 240 (e.g., their containers) are identically designed and / or have a thread by means of which they can be positively connected to the respective connections. This reduces maintenance effort.
[0138] Fig. 3B illustrates a method according to various embodiments 300b in a schematic flowchart, optionally set up according to Example 2.
[0139] An example configuration for releasing hydrogen gas is described in 351 by means of water electrolysis and / or in the regeneration mode. An example configuration for regenerating the filter device is described in 353 by chemically reducing the copper oxide of the filter device to copper, to which thermal energy is supplied by means of the heating device. For example, the copper oxide can be heated to more than 100°C (e.g., to a thermal decomposition temperature or at least above 500°C), but not above its melting point.
[0140] The copper oxide is formed during a separation process that includes gas purification. This process involves exposing the copper to an inert gas containing oxygen. The copper then reacts chemically with the oxygen to form copper oxide, thus reducing the amount of oxygen carried along with the inert gas.
[0141] Fig. 4A and Fig. Figure 4B illustrates a gas process system according to different embodiments, when the actual mode is regeneration mode 400a and when the actual mode is separation mode 400b, in a schematic connection diagram, which are optionally configured according to one of the embodiments 100a to 300b. Solid arrows in the connection diagram represent enabled fluid paths. Dashed arrows in the connection diagram represent interrupted (e.g., blocked) fluid paths.
[0142] Fig. Figure 5A illustrates a gas processing system according to various embodiments 500a in a schematic diagram, which are optionally configured according to one of the embodiments 100a to 400b. The gas processing system comprises a system of several filter devices 152, 552 (hereinafter also referred to as the filter system), each filter device having two filter stages 152a, 152b. The first filter device 152 of the filter system 152, 552 is alternately switched to separation mode and regeneration mode. Complementarily, a second filter device 552 of the filter system 152, 552 is switched to regeneration mode when the first filter device 152 is in separation mode, and to separation mode when the first filter device 152 is in regeneration mode. This promotes a high and uninterrupted throughput of the filter process.The gas supply device can also generate the regeneration gas when one of the filter devices 152, 552 is in separation mode, but this does not necessarily have to be continuous.
[0143] The two filter devices 152, 552 can be coupled to each other by means of a 4-2-way valve as a control valve 164, which is configured to connect the one of the two filter devices 152, 552 which is in the separation mode to the working device 154 in a fluid-conducting manner, and the other of the two filter devices 152, 552 which is in the regeneration mode to the gas supply device 156 in a fluid-conducting manner.
[0144] Fig. 5B illustrates the phases of a change sequence according to different embodiments 500b in a schematic flow diagram (see Example 32), according to which the transition from the separation phase to the regeneration phase takes place.
[0145] The following describes various work examples that relate to what is described herein and depicted in the figures, and are aimed at concrete implementations thereof.
[0146] According to working example 1, the flow rate of the supply water through the electrolyzer is 1 liter per minute (l / min). Correspondingly, the flow rate of hydrogen gas produced by the electrolyzer is 1 liter per minute. Furthermore, the proportion of hydrogen gas in the regeneration gas is 10% or less. This inhibits the flammability of the hydrogen gas. The regeneration gas supplied to the filter device, for example, has a hydrogen gas content of a maximum of 5 vol%. The flow rate of the regeneration gas supplied to the filter device is then 20 l / min.
[0147] According to working example 2, the process gas, which consists essentially of the inert gas and contains oxygen and / or moisture as impurities, circulates through a glovebox and the filter device. The flow rate of the process gas through the glovebox can, for example, be greater than F S This facilitates cost-effective gas purification. The value F S The flow rate of the process gas through the glovebox can be a function of the internal volume V of the glovebox, for example, such that several (e.g., at least 10) volume changes occur per hour. For a glovebox with an internal volume of V = 1 m³ 3 The value is, for example, F S = 60 m 3 / h or more. This promotes efficient mixing and the removal of impurities.
[0148] According to working example 3, two filter stages (e.g., copper filter stages) are used to bind oxygen gas, one of which is always in separation mode. This allows for continuous operation. Once the filter stage in separation mode is saturated, it is switched to regeneration mode, and the other filter stage is switched to separation mode. Similarly, more than two filter stages can be used, which are switched to separation mode sequentially.
[0149] According to working example 4, the hydrogen generator during operation (when it generates hydrogen gas) is surrounded by a volume flow of the safety atmosphere (e.g. atmospheric air) which has a pressure of at least 10 mbar above atmospheric pressure.
[0150] According to working example 5, each filter device has a heating device which supplies thermal energy to the filter stage(s) of the filter device when it is in regeneration mode.
[0151] According to working example 6, the supply water is deionized and monitored, e.g., its electrical conductivity to ensure water quality and the degree of deionization. Furthermore, the water level and temperature are monitored to prevent overheating of the hydrogen generator. The supply water is monitored using a combination probe, which incorporates multiple sensors and is located in the water tank. Poor water quality (e.g., contamination) can damage the electrolyzer. Monitoring the water level protects the pump and electrolyzer from running dry and ensures that sufficient water is available for pumping.
[0152] According to working example 7, oxygen gas produced during water electrolysis is drawn into the safety enclosure, through which the safety atmosphere, supplied by ambient air, flows. This prevents a potentially dangerous accumulation of oxygen gas near the hydrogen generator. Alternatively or additionally, water extracted from the water electrolysis (then also referred to as wastewater), which is carried along with the hydrogen gas, is separated from the hydrogen gas and collected in the gas mixing vessel. This facilitates a cost-effective and safe design.
[0153] According to working example 8, the pressure of the hydrogen gas and / or the regeneration gas is low pressure and / or at least less than 2 bar (e.g., 1.5 bar absolute pressure or less). This reduces the requirements for the components and the tightness, which facilitates regulatory approval, simplifies operation, and saves costs.
[0154] According to working example 9, the electrolyzer has several (e.g., three or more) electrolysis cells connected in series (see example 61). This series connection reduces the electrical current required for a given electrical power output by the electrolyzer. This also reduces the requirements for the electrical supply infrastructure of the electrolyzer (e.g., electrical cables and generator), saving costs and simplifying operation.
[0155] According to working example 10, the electrolyzer has at least one proton-permeable polymer membrane (PEM) per electrolysis cell, by means of which the electrolysis cell is provided (then also referred to as a PEM cell). The PEM cell is inexpensive, requires little maintenance, and is easy to operate. For example, the PEM cell does not require pressure build-up and is therefore immediately ready for use, requires no run-up time, no venting, and can be started at room temperature.
[0156] According to working example 11, the wastewater is not returned to the water electrolysis process but is disposed of. For this purpose, an open end to the water circuit is provided at the outlet of the electrolyzer. This inhibits the mixing of oxygen and hydrogen gas and is more cost-effective to implement than a closed water circuit, which would return the condensate water to the supply water and therefore require additional safety precautions.
[0157] According to working example 12, the safety enclosure is a pressurized chamber in which overpressure is created by introducing air into the enclosure using a fan (also referred to as a blower). The volume of air introduced into the safety enclosure is greater than the volume of hydrogen gas produced by the hydrogen generator (e.g., tenfold, one hundredfold, or more). This ensures sufficient dilution, even if all the hydrogen gas escapes due to a leak. If the door of the safety enclosure is open or the leak is detected by a sensor, the hydrogen generator is automatically deactivated, e.g., by interrupting the electrical power supply. The overpressure can be, for example, 10 millibars above the hydrostatic pressure of the Earth's atmosphere (also referred to as atmospheric pressure) at the location of the hydrogen generator.Alternatively or additionally, the overpressure is manually set once using a mechanical gas outlet throttle, allowing the use of an unregulated blower and thus saving costs. The blower and the gas outlet throttle are protected by a grille, increasing operational safety. Alternatively or additionally, the blower can be equipped with a dust filter, which further enhances operational safety.
[0158] According to working example 13, the regeneration gas and the process gas are identical in the inert gas. This eliminates the need to purge the filter device during gas changes, saving gas, time, and therefore costs. For example, argon can be used as the inert gas in both the regeneration gas and the process gas. Even small amounts of nitrogen gas can be problematic in an argon-based application. Optionally, the process gas supplied to the filter device in separation mode is used in regeneration mode to be mixed with hydrogen gas to form the regeneration gas. This further simplifies the setup and / or prevents the filter device from being subjected to pressure fluctuations. For example, the process gas, which has a pressure between 5 and 6 bar, is supplied to the filter device and / or the gas supply device. Optionally, the regeneration gas exiting the filter device is disposed of, for example, via a discharge outlet.
[0159] According to working example 14, the regeneration signal (e.g., 24 volts), which controls the control valves, is tapped from one of the control valves and fed to the gas supply device. This simplifies the design and thus reduces costs. As soon as the control valve receives the regeneration signal, the hydrogen generator is started, e.g., according to the switching sequence. When the regeneration signal is switched off, the hydrogen generator is stopped, e.g., according to a reversed switching sequence.
[0160] According to working example 15, the following occurs sequentially when starting the hydrogen generator (e.g. according to the switching sequence): - Checking the stored water (e.g. its fill level, conductivity and / or temperature); - Starting the pump to supply the stored water to the hydrogen generator and thus flush it (e.g. its electrolysis cells); - Injecting the inert gas into the gas mixing vessel to purge it, which reduces the risk of air entering the filter device: - After 10-20 seconds, electrical power is coupled into the hydrogen generator to start the water electrolysis, which produces hydrogen gas and feeds it into the gas mixing container.
[0161] According to working example 16, the following occurs sequentially when the hydrogen generator is stopped (e.g. according to the reversed change sequence): - Interruption of the electrical power, so that the water electrolysis ends; - After 10-20 seconds, the injection of the inert gas into the gas mixing container is interrupted, so that the gas mixing container is purged again for this time; - Stopping the pump so that no more water is supplied to the hydrogen generator. If the changeover sequence runs in reverse, checking the water level can be omitted.
[0162] According to working example 17, the storage container and / or the gas mixing element are supplied by means of a screw-in cylinder (also referred to as a screw-in cylinder). This is cost-effective and can be scaled with little effort. For example, a 1-liter screw-in cylinder can be exchanged for a screw-in cylinder with a larger or smaller capacity without having to change the design of the gas supply system.
[0163] According to working example 18, the safety of the gas supply device is increased cost-effectively by means of: - a splash-proof electric generator; - a protective device for manually adjustable valves that are designed to influence the chemical composition of the regeneration gas (e.g. safety valve and / or adjustment actuator); - a measuring chain by means of which safety-relevant operating parameters are monitored by sensors, e.g. the water pressure in the electrolyzer, the pressure of the hydrogen gas at the outlet of the electrolyzer and / or in the gas mixing vessel, the pressure of the safety atmosphere; and - a control unit which triggers an interruption of the electrical power supplied to the electrolyzer when the measuring chain determines that the actual state of at least one of the monitored operating parameters exceeds or falls below a threshold value.
[0164] For example, a leak or incorrectly installed container (e.g., gas mixing container) can be detected by a deviation in the pressure of the regeneration gas and / or the hydrogen gas.
[0165] According to working example 19, each of the following applications provided by means of the working device which has an enclosure is particularly suitable to be supplied by means of the inert gas from the filter device: - a glovebox, which is provided, for example, by means of the enclosure; - Welding under argon, e.g. in an enclosure; - an OLED manufacturing process, e.g. in an enclosure, - Examination, manufacturing or storage of dyes, e.g. in the enclosure; - Examination, manufacturing or storage of Li-ion batteries or components thereof, e.g. in the enclosure.
[0166] These applications reflect only a fraction of the possible applications of the device, where processes are carried out that are sensitive to the influence of humidity and oxygen gas.
[0167] According to Working Example 20, a hydrogen-inert gas mixture is used as a regeneration gas for the regeneration of several reactors, which are used for gas purification. In contrast, commercially available hydrogen-inert gas mixtures are usually supplied in pressurized gas cylinders, which increases costs and, more importantly, limits availability. Furthermore, the required hydrogen gas flow rate is generated directly using a PEM electrolysis cell (also referred to as a PEM cell) and immediately mixed (i.e., diluted) with an inert gas (e.g., nitrogen or argon), so that a potentially dangerous accumulation of hydrogen gas can never occur. The gas supply device is housed in a forced-ventilation safety enclosure, the internal pressure of which is monitored to detect and prevent the formation of potentially dangerous hydrogen gas concentrations (e.g., in the event of a leak).The PEM cell is supplied with water via a system consisting of a reservoir (also called a storage tank) and a water separator, which are supplied by laboratory gas cylinders. This simplifies the setup and reduces costs. Monitoring of the water supply (e.g., fill level, temperature, and / or conductivity of the supply water) is performed using a flexible combination probe inserted into the reservoir from above. The gas mixing takes place directly in the water separator, minimizing the water content of the regeneration gas. An advantage of this working example compared to a conventional configuration is its application-specific, simple design with a significantly reduced need for safety technology and thus considerably lower costs compared to a universal configuration.
[0168] According to working example 21, one or more reactors are regenerated using a regeneration gas containing hydrogen. The standard volumetric flow rate of the regeneration gas is 20 l / min. The regeneration gas mixture meets at least the requirements for regenerating systems with a volume of up to 60 m³. 3 Volume flow capacity per hour. The regeneration gas contains a maximum of 5% hydrogen gas by volume. This inhibits its flammability. As a result, the maximum volume flow rate of hydrogen gas generated by the electrolyzer is 1 l / min.
[0169] According to working example 22, hydrogen gas is produced using an electrolyzer (e.g., comprising one or more PEM electrolysis cells). The electrolyzer is supplied with water by a DC diaphragm pump, which delivers a water flow rate of approximately 1 l / min. The pump draws the water from the reservoir and feeds it into a dedicated inlet port (then also referred to as the H₂O inlet) of the electrolyzer. The water, along with the oxygen gas produced during water electrolysis, exits the electrolyzer at the reflux port (then also referred to as the O₂ outlet) and is returned to the reservoir. The proportion of water that is electrolyzed is 0.8 ml / min (milliliters per minute). The remaining water can be used to cool the electrolyzer.
[0170] According to working example 23, a laboratory glass bottle (e.g., with a capacity of 1 liter) is used as a storage container. The laboratory glass bottle is removed from the input material inlet (e.g., its screw cap) for filling and emptying. A flexible combination probe extends from the top into the laboratory glass bottle to measure the conductivity, temperature, and fill level of the storage water. The hydrogen connection (then also referred to as the H₂ outlet) of the electrolyzer is fluid-conductingly coupled to an additional laboratory glass bottle (e.g., with a capacity of 1 liter) that serves as the container for the gas mixing element, in which water droplets are separated. This additional laboratory glass bottle is also mounted in a removable manner, allowing the operator to empty it after regeneration. In this additional laboratory glass bottle, the hydrogen gas is mixed with an inert gas (e.g., nitrogen gas) to form the regeneration gas.The flow of inert gas into the additional laboratory glass bottle can be controlled by a needle valve, which, once adjusted, typically only needs readjusting in the event of a malfunction or during maintenance. The needle valve connects the additional laboratory glass bottle to the inert gas inlet, to which, for example, the inert gas source connected to the filter unit is attached. The pressure supplied by the inert gas source (e.g., approximately 6 bar above atmospheric pressure) is reduced to approximately 0.5 bar above atmospheric pressure, which is then the pressure of the regeneration gas. This ensures that the flow of the regeneration gas through the filter unit is sufficiently stable despite fluctuations in the back pressure within the filter unit, thus eliminating the need for an additional pressure or flow regulator and saving costs.
[0171] According to working example 24, deviations between the actual chemical composition of the regeneration gas and the target chemical composition (e.g., specified as the ratio of hydrogen gas to inert gas) are minimized. For this purpose, the pressure of the inert gas to which the gas mixing element and / or the inert gas inlet 108 are exposed is monitored by means of the second measuring element. This second measuring element has two pressure switches exposed to the inert gas flowing from the inert gas inlet to the gas mixing element. The two pressure switches monitor whether the inert gas pressure is within a specified range between a minimum and maximum pressure. The switches are triggered, for example, by a blocked regeneration gas connection or similar faults.
[0172] According to working example 25, the electrolyzer (e.g., its PEM cell) is supplied with electrical power by a constant DC current source, which provides, for example, an electrical voltage in the range of 3 volts (V) (e.g., 10 V) and 20 V and / or an electrical current in the range of 10 amperes (A) and 100 A. The power supply is interrupted in response to the detection of a fault condition (also referred to as a disturbance). The fault condition is detected when at least one safety-relevant operating parameter meets the fault criterion. For example, the electrolyzer can consume an electrical power in the range of 100 watts to 500 watts during operation, e.g., approximately 220 watts.
[0173] According to working example 26, the fault criterion is met if the inert gas pressure, as a safety-relevant operating parameter, is lower than a specified value, e.g., the minimum pressure, and / or higher than a specified value, e.g., the maximum pressure. Alternatively or additionally, the fault criterion is met if it is determined that the gas supply device has failed or is impaired (e.g., by means of the second motor sensor).
[0174] According to working example 27, the safety device is implemented as a switching circuit using a relay network. This switching circuit monitors the operating parameters of the gas supply device. This allows for a cost-effective implementation, as no programmable logic controller (PLC) is required as a safety device. Alternatively or additionally, visualization and / or control of the gas supply device's operating parameters, which are not safety-relevant, is achieved using a system that includes a miniature PLC and a display for showing the most important operating parameters.
[0175] According to working example 28, the regeneration phase, in which the regeneration gas is produced, is initiated by means of the regeneration signal generated by the filter device, e.g., by its control unit. The regeneration signal is a 24 V signal, which is used to control the control valves (e.g., in the valve block).
[0176] According to working example 29, the safety device, the hydrogen generator, the gas mixing element, and the storage tank are arranged in a gas-tight safety enclosure. A blower continuously supplies the safety enclosure with sufficient ambient air, which exits (e.g., throttled) through exactly one air outlet. This ensures that the safety pressure within the enclosure is an overpressure, for example, a maximum of approximately 50 mbar (millibar) above atmospheric pressure. This safety pressure is monitored by a pressure switch, which facilitates the detection of blower failure. The volume flow of ambient air through the safety enclosure is designed such that even if the maximum possible quantity of generated hydrogen gas escapes directly into the enclosure, a safety-relevant accumulation of hydrogen gas is prevented.For this purpose, the volume flow of ambient air through the safety housing can be at least approximately 50 l / min (which corresponds to approximately 3 cubic meters per hour).
Claims
[1] comprising a gas supply device (156): • an inert gas inlet (106) for receiving inert gas; • an input material inlet (104) for receiving an input material; • a hydrogen generator (102) for releasing hydrogen gas from the starting material; and • a regeneration gas outlet (108) for providing a regeneration gas to a filter device; • wherein the gas supply device (156) is configured to produce the regeneration gas by mixing the generated hydrogen gas with the inert gas. [2] Gas supply device (156) according to claim 1, further comprising a gas mixing element (240) for generating the regeneration gas, wherein the gas mixing element (240) has a condensate separator which is configured to separate water which is carried along with the hydrogen gas generated by the hydrogen generator (102). [3] Gas supply device (156) according to one of claims 1 to 2, wherein the hydrogen generator (102) comprises an electrolyzer. [4] Gas supply device (156) according to one of claims 1 to 3, wherein the inert gas is provided by means of a process gas which has an impurity and has a larger proportion of the inert gas than the regeneration gas. [5] Gas supply device (156) according to any one of claims 1 to 4, further comprising a safety device which is configured to interrupt the release of hydrogen gas when an operating parameter of the gas supply device (156) meets a criterion, wherein the operating parameter: • refers to supplying the hydrogen generator (102) with water; • represents the pressure of a safety atmosphere in which the hydrogen generator (102) is located; • represents a pressure of the regeneration gas; and / or • represents a pressure of the inert gas. [6] Gas supply device (156) according to one of claims 1 to 5, further comprising a pipeline network which is set up: • in a regeneration mode, to supply the inert gas taken in by means of the inert gas inlet (108) to the generation of the regeneration gas; • and is set up in a separation mode to displace the regeneration gas from the gas supply device (156) by means of the inert gas taken in at the inert gas inlet (108). [7] Gas process system, comprising: • the gas supply device (156) according to any one of claims 1 to 6, • and the filter device (152), which is designed to filter a process gas. [8] Gas process system, comprising: • a working device comprising a working area, wherein the working device (154) is configured to provide an atmosphere of a process gas in the working area; • a filter device (152) for filtering the process gas of the working device, wherein the filter device (152) has a regeneration gas inlet for receiving a regeneration gas for regenerating the filter device (152); • a gas supply device (156) which is set up to produce the regeneration gas by mixing hydrogen with the process gas. [9] Gas process system according to one of claims 7 to 8, wherein the filter device (152) is configured to chemically bind oxygen gas as an impurity of the process gas, preferably by means of a metal. [10] Gas processing system according to any one of claims 7 to 9, further comprising: • a chamber housing in which the hydrogen generator (102) and preferably the feedstock inlet are arranged, the chamber housing having a chamber cover which is configured to close a maintenance opening of the chamber housing gas-tight in a closed state of the chamber housing; and • a blower which is set up to supply ambient air to the chamber housing, by means of which an overpressure is created in the chamber housing.
Citation Information
Patent Citations
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