Transient operation method for separation device
The transient operation method for separation devices with controlled humidity and temperature management addresses damage during startup and shutdown, stabilizing the separation membrane and enhancing device longevity.
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- NGK CORP
- Filing Date
- 2024-01-31
- Publication Date
- 2026-07-03
AI Technical Summary
Existing separation devices with separation membranes face damage during startup due to thermal shock, boiling, and rapid expansion of water, which can be exacerbated by humidity differences.
A transient operation method involving controlled humidity and temperature management in separate flow paths to prevent damage, using a separation membrane complex with distinct humidity levels in each path to stabilize the membrane during startup and shutdown.
Prevents damage to the separation membrane and device by stabilizing the membrane during transient operations, ensuring consistent performance and extending the device's lifespan.
Smart Images
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Abstract
Description
Technical Field
[0001] The present invention relates to a method for transient operation of a separation device.
Background Art
[0002] A membrane separation method for separating a specific substance from a mixture using a separation membrane is known. As such a membrane separation method, for example, a separation method using a zeolite membrane has been proposed (see Non-Patent Document 1). In a separation device provided with a separation membrane, heating of the separation membrane may be required at the time of device startup in order for the separation membrane to exhibit a predetermined function.
Prior Art Documents
Non-Patent Documents
[0003]
Non-Patent Document 1
Summary of the Invention
Problems to be Solved by the Invention
[0004] A main object of the present invention is to provide a method for transient operation of a separation device provided with a separation membrane composite, which can prevent damage to the separation device and the separation membrane composite.
Means for Solving the Problems
[0005] [1] A transient operation method for a separation apparatus according to an embodiment of the present invention is a transient operation method for a separation apparatus comprising a separation membrane complex having a separation membrane and a substrate disposed on one side of the separation membrane, wherein the separation apparatus has a first flow path and a second flow path, the first flow path being located on the separation membrane side of the separation membrane complex and the second flow path being located on the substrate side of the separation membrane complex, and the method includes supplying gas to the first flow path and the second flow path, and heating the separation membrane complex, wherein the average relative humidity of gas A supplied to the first flow path is higher than the average relative humidity of gas B supplied to the second flow path. [2] In the transient operation method of the separation apparatus described in [1] above, the average relative humidity of gas B may be 10% or less. [3] In the transient operation method of the separation apparatus described in [1] or [2] above, the separation membrane may be a zeolite membrane. [4] In the transient operation method of the separation apparatus described in any of [1] to [3] above, the zeolite membrane may be composed of LTA type zeolite. [5] A transient operation method for a separation apparatus according to another embodiment of the present invention is a transient operation method for a separation apparatus comprising a separation membrane complex having a separation membrane and a substrate disposed on one side of the separation membrane, wherein the separation apparatus has a first flow path and a second flow path, the first flow path being located on the separation membrane side of the separation membrane complex and the second flow path being located on the substrate side of the separation membrane complex, and the method includes supplying gas to the first flow path and the second flow path, and heating the separation membrane complex, wherein the relative humidity of gas A supplied to the first flow path is higher than the relative humidity of gas B supplied to the second flow path. [6] The transient operation method described in any of the above "1" to [5] may also be a startup method. [7] The transient operation method described in any of the above "1" to [5] may also be a stopping method. [Effects of the Invention]
[0006] According to embodiments of the present invention, a transient operation method for a separation apparatus comprising a separation membrane complex can be provided, which can prevent damage to the separation apparatus and the separation membrane complex. [Brief explanation of the drawing]
[0007] [Figure 1] Figure 1 is a schematic diagram of a separation membrane complex used in a transient operation method for a separation apparatus according to one embodiment of the present invention. [Figure 2] Figure 2 is a schematic diagram of the separation membrane and substrate shown in Figure 1. [Figure 3] Figure 3 is a schematic diagram of one modified example of the separation membrane complex. [Figure 4] Figure 4 is a schematic cross-sectional view of the separation membrane composite shown in Figure 3. [Figure 5] Figure 5 is a schematic diagram of another modified example of the separation membrane complex. [Figure 6] Figure 6 is a schematic diagram illustrating the operation method of a separation device according to one embodiment of the present invention. [Modes for carrying out the invention]
[0008] Embodiments of the present invention will be described below with reference to the drawings, but the present invention is not limited to these embodiments. Furthermore, in order to clarify the explanation, the drawings may schematically represent the width, thickness, shape, etc., of each part compared to the embodiments; however, these are merely examples and do not limit the interpretation of the present invention.
[0009] A. Transient operation method of the separation device Figure 1 is a schematic diagram of a separation membrane composite used in a transient operation method of a separation apparatus according to one embodiment of the present invention; Figure 2 is a schematic diagram of the separation membrane and substrate of Figure 1.
[0010] A transient operation method for a separation apparatus according to one embodiment of the present invention is a transient operation method for a separation apparatus 1 comprising a separation membrane complex 10 having a separation membrane 2 and a substrate 3 disposed on one side of the separation membrane 2. The separation apparatus 1 has a first flow path 21 and a second flow path 22. The first flow path 21 is located on the separation membrane 2 side of the separation membrane complex 10. More specifically, the first flow path 21 may be located on the separation membrane 2 side of the separation membrane complex 10 than the substrate 3, and other elements (not shown) may or may not be present between the separation membrane 2 and the first flow path 21. The second flow path 22 is located on the substrate 3 side of the separation membrane complex 10. More specifically, the second flow path 22 may be located on the substrate 3 side of the separation membrane complex 10 than the separation membrane 2, and other elements (not shown) may or may not be present between the substrate 3 and the second flow path 22. Although not shown, the separation membrane complex 10 may include any other suitable elements as long as the effects of the present invention are obtained. For example, the separation membrane 2 may be provided with a layer or powder that protects all or part of it, elements having a separation function such as another separation membrane, or another substrate (for example, a layer thinner than the substrate 3 and with the same composition as the substrate 3) located on the opposite side of the substrate 2 from the substrate 3. Also, part of the substrate 3 may be exposed.
[0011] The transient operation method of the above-described separation apparatus includes supplying gas to the first channel 21 and the second channel 22, and changing the temperature of the separation membrane complex 10 (i.e., heating or cooling it). Hereinafter, an embodiment of heating the separation membrane complex 10 will be described as a representative example. In one embodiment, the separation membrane complex 10 is heated by supplying gas to the first channel 21 and the second channel 22. Alternatively, the separation membrane complex 10 may be heated from an external source (for example, by heating using any suitable heating device). In one embodiment, in the above-described transient operation method, the average relative humidity of gas A supplied to the first channel 21 is higher than the average relative humidity of gas B supplied to the second channel 22. In this specification, average relative humidity is the average value of the relative humidity at the upstream end and the relative humidity at the downstream end for each channel. More specifically, when the relative humidity at the inlet of each channel is calculated from the temperature and water vapor partial pressure at the inlet and denoted as RH1, and the relative humidity at the outlet is calculated from the temperature and water vapor partial pressure at the outlet and denoted as RH2, the average relative humidity can be calculated using the formula (RH1 + RH2) / 2. Relative humidity is the ratio of the measured water vapor partial pressure to the saturated water vapor pressure at a given temperature. In this specification, relative humidity is measured using a dew point meter (capacitive type). Relative humidity measured by other methods may also be close to the relative humidity measured by the above method. For example, relative humidity measured by sampling gas from a predetermined measurement position, measuring the proportion of condensed components by cooling, and analyzing the proportion of water contained in the condensed components by liquid chromatography may also be close. Furthermore, the relative humidity at the downstream end of each channel may also show a similar trend to the average relative humidity described above. In one embodiment, gas is supplied to the first channel under conditions where condensation does not occur on the separation membrane complex. In another embodiment, gas is supplied to the second channel under conditions where condensation does not occur on the separation membrane complex.
[0012] In one embodiment, the relative humidity (hereinafter also referred to as relative humidity (AU)) at the downstream end of the first flow path 21 of gas A supplied to the first flow path 21 is higher than the relative humidity (hereinafter also referred to as relative humidity (BU)) at the downstream end of the second flow path 22 of gas B supplied to the second flow path 22.
[0013] In one embodiment, after starting the separation apparatus 1 using the transient operation method described above, heating is continued until the separation membrane reaches a predetermined temperature, and the separation apparatus transitions to steady-state operation. During steady-state operation, a fluid that permeates the separation membrane 2 (for example, a mixture containing water as a permeable substance and organic compounds that are impermeable) is supplied to the first channel 21. The substance that has permeated the separation membrane 2 flows through the second channel 22. By heating the separation membrane complex 10 using the transient operation method described above, the separation membrane 2 exhibits a predetermined separation capacity during steady-state operation.
[0014] In embodiments of the present invention, by lowering the average relative humidity of gas B supplied to the second channel 22, that is, the relative humidity of gas B supplied to the substrate 3 side, or the relative humidity at the downstream end of the channel, it is possible to suppress boiling, rapid expansion, thermal shock, etc., of water within the substrate 3, and prevent damage to the separation membrane complex 10 and / or separation device 1. In one embodiment, the amount of moisture (relative humidity) of gas A supplied to the first channel is set to a certain amount or more. By supplying a gas containing moisture at startup, damage to the separation membrane can be prevented. Furthermore, in the present invention, by lowering the average relative humidity of gas B or the relative humidity at the downstream end of the channel, problems caused by water content (damage to the separation membrane due to boiling, rapid expansion, thermal shock, etc. of water) can be solved.
[0015] The difference between the average relative humidity of the above gas B and the average relative humidity of the above gas A (average relative humidity of gas B (%) - average relative humidity of gas A (%)) is preferably greater than 2% (points) and not more than 95% (points), more preferably 2% (points) to 50% (points), and even more preferably 2% (points) to 15% (points). If it is within such a range, the above effects will be remarkable. Also, it is possible to prevent the separation membrane 2 from being damaged during heating. For example, when the average relative humidity of gas B is 70% and the average relative humidity of gas A is 50%, the difference between the average relative humidity of gas B and the average relative humidity of the above gas A (average relative humidity of gas B (%) - average relative humidity of gas A (%)) is 20%.
[0016] The difference between the relative humidity (BU) of the above gas B and the relative humidity (AU) of the above gas A (relative humidity (BU) (%) - relative humidity of gas A (AU) (%)) is preferably greater than 2% (points) and not more than 95% (points), more preferably 2% (points) to 50% (points), and even more preferably 2% (points) to 15% (points). If it is within such a range, the above effects will be remarkable. Also, it is possible to prevent the separation membrane 2 from being damaged during heating.
[0017] The average relative humidity of the above gas A is preferably 0.1% or more, more preferably 0.5% or more, and even more preferably 5% or more. If it is within such a range, it is possible to prevent the separation membrane 2 from being damaged during heating. Also, it is possible to simplify the measuring instrument. Also, general-purpose products can be used for the measuring instrument, and cost reduction can be achieved. Also, the upper limit of the average relative humidity of the above gas A is, for example, 100%, and more preferably 95%. If it is within such a range, it is possible to prevent the separation membrane 2 from being damaged during heating. Also, by setting the average relative humidity of gas A to 95% or less, the effects of the present invention can be stably obtained.
[0018] The relative humidity (AU) of the above gas A is preferably 0.1% or more, more preferably 0.5% or more, and still more preferably 5% or more. If it is within such a range, breakage of the separation membrane 2 during heating can be prevented. Also, simplification of the measuring equipment becomes possible. Further, general-purpose products can be used for the measuring equipment, and cost reduction can be achieved. Also, the upper limit of the relative humidity (AU) of the above gas A is, for example, 100%, more preferably 95%. If it is within such a range, breakage of the separation membrane 2 during heating can be prevented. Also, by setting the relative humidity (AU) of gas A to 95% or less, the effects of the present invention can be obtained stably.
[0019] The average relative humidity of the above gas B is preferably 10% or less, more preferably 5% or less. If it is within such a range, boiling over, rapid expansion, thermal shock, etc. of water can be suppressed, and the effect of preventing breakage of the separation membrane composite 10 and / or the separation device 1 becomes remarkable. The lower limit of the average relative humidity of the above gas B is not particularly limited, but is, for example, 0.01%, more preferably 0.05%. If it is within such a range, the dryer performance in the compressor can be simplified.
[0020] The relative humidity (BU) of the above gas B is preferably 10% or less, more preferably 5% or less. If it is within such a range, boiling over, rapid expansion, thermal shock, etc. of water can be suppressed, and the effect of preventing breakage of the separation membrane composite 10 and / or the separation device 1 becomes remarkable. The lower limit of the relative humidity (BU) of the above gas B is not particularly limited, but is, for example, 0.01%, more preferably 0.05%. If it is within such a range, the dryer performance in the compressor can be simplified.
[0021] In one embodiment, the pressure in the first channel 21 and / or the second channel 22 is adjusted according to the ambient temperature in which the separation membrane complex 10 (substantially the separation membrane 2) is located. In the transient operation method of the separation apparatus, the initial temperature of the separation membrane 2 is, for example, 0°C to 35°C, and the initial pressure in the first channel 21 is, for example, 0.1 MPaG to 20 MPaG. Furthermore, at the completion of startup of the separation apparatus, the temperature of the separation membrane 2 is, for example, 100°C to 350°C, and the pressure in the first channel 21 is, for example, 0.1 MPaG to 20 MPaG.
[0022] In this specification, "transient operation method" is a concept that includes a start-up method and a stop-down method. Therefore, in the description of the embodiments above, "transient operation method" may be "start-up method" (i.e., "transient operation method" may be read as "start-up method") or "stop-down method". In this specification, "start-up method" is a method that includes heating the separation membrane. Also, "stop-down method" is a method that includes cooling the separation membrane.
[0023] B. Separation device B-1. Separation membrane complex As shown in Figure 1, the separation device 1 typically comprises a separation membrane complex 10 including a substrate 3 and a separation membrane 2. Although not shown, the separation membrane complex 10 is used in any suitable case. Typically, the separation membrane complex 10 extends in the same direction as the first flow path 21. The length of the separation membrane complex 10 can be arbitrarily and appropriately adjusted.
[0024] B-1-1. Base material The substrate 3 supports the separation membrane 2. In one embodiment, the substrate 3 is a porous substrate. The porous substrate has, for example, a so-called monolithic structure, comprising a three-dimensional network-like continuous skeleton and communicating pores defined by the skeleton. The substrate 3 may contain components that constitute the separation membrane 2.
[0025] The porous substrate can be composed of any suitable material. Typical materials for the porous substrate include ceramic sintered bodies. Examples of ceramic sintered bodies include alumina, silica, mullite, zirconia, titania, yttria, silicon nitride, silicon carbide, and cordierite. Ceramic sintered bodies can be used alone or in combination. Among ceramic sintered bodies, alumina is preferred.
[0026] The porous substrate may contain an inorganic binder. Examples of inorganic binders include titania, mullite, easily sintered alumina, silica, glass frit, clay minerals, and easily sintered cordierite. The inorganic binders can be used alone or in combination.
[0027] The porous substrate may consist of a single layer or have a multilayer structure in which multiple layers are stacked. In one embodiment, the porous substrate has a multilayer structure having multiple layers with different pore sizes, as shown in Figure 2. In this case, it is preferable that the pore size is smaller closer to the separation membrane 2.
[0028] The average pore size of the porous substrate is, for example, 0.01 μm to 70 μm, preferably 0.05 μm to 25 μm. The average pore size of the porous substrate on the separation membrane side is 0.01 μm to 1 μm, preferably 0.05 μm to 0.5 μm. Regarding the distribution of pore size throughout the porous substrate, including the surface and interior, D5 is, for example, 0.01 μm to 50 μm, D50 is, for example, 0.05 μm to 70 μm, and D95 is, for example, 0.1 μm to 2000 μm. The porosity of the porous substrate on the separation membrane side is, for example, 25% to 50%. The average pore size of the porous substrate can be measured, for example, by a mercury porosimeter, palm porometer, or nanopalm porometer.
[0029] As shown in Figure 1, the base material 3 typically separates the first flow path 21 and the second flow path 22 described above. The base material 3 can take any suitable shape. Examples of the base material 3's shape include cylindrical, honeycomb, and flat plate shapes. In one embodiment, the base material 3 is a cylindrical base material 3a. Examples of cross-sectional shapes in the direction perpendicular to the longitudinal direction of the cylindrical base material 3a include triangles, quadrilaterals, pentagons, polygons with hexagons or more, circles, and ellipses, with a circle being preferred. The outer diameter and length of the cylindrical base material can be appropriately set depending on the purpose.
[0030] In this embodiment, the internal space of the cylindrical substrate 3a (the space defined by the inner circumferential surface of the cylindrical substrate) includes either the first flow path 21 or the second flow path 22, and the external space of the cylindrical substrate 3a (the space outside the outer circumferential surface of the cylindrical substrate) includes either the first flow path 21 or the second flow path 22. In the illustrated example, the internal space of the cylindrical substrate 3a includes the first flow path 21, and the external space of the cylindrical substrate 3a includes the second flow path 22.
[0031] In another embodiment, as shown in Figures 3 and 4, the base material 3 is a honeycomb base material 3b. The honeycomb base material 3b includes partition walls 33 that define a plurality of cells 34. The cells 34 are formed in a cylindrical shape so as to penetrate the honeycomb base material 3b in the longitudinal direction.
[0032] Cell 34 extends along the length (axial direction) of the honeycomb substrate 3b from the first end face E1 (inlet end face) to the second end face E2 (outlet end face) of the honeycomb substrate 3b (see Figure 4). Cell 34 has any suitable shape in a cross-section perpendicular to the length direction of the honeycomb substrate 3b. Examples of cell cross-sectional shapes include triangles, quadrilaterals, pentagons, polygons with hexagons or more, circles, and ellipses. The cross-sectional shapes and sizes of the cells may all be the same, or at least some may differ. Among such cell cross-sectional shapes, a circle is preferred.
[0033] The distance between the central axes of multiple cells 34 is, for example, 0.3 mm to 20 mm. The cell density (i.e., the number of cells 34 per unit area) in a cross-section perpendicular to the longitudinal direction of the honeycomb substrate can be appropriately set depending on the purpose. The cell density is, for example, 0.5 cells / cm 2 ~320 cells / cm 2This is possible. If the cell density is within this range, sufficient strength and effective GSA (geometric surface area) of the honeycomb substrate can be ensured.
[0034] The honeycomb substrate 3b has any suitable shape (overall shape). Examples of honeycomb substrate shapes include a cylindrical shape with a circular base, an elliptical columnar shape with an elliptical base, a prismatic columnar shape with a polygonal base, and a columnar shape with an irregular base. The honeycomb substrate 3b in the illustrated example has a cylindrical shape. The outer diameter and length of the honeycomb substrate can be appropriately set depending on the purpose.
[0035] In this embodiment, the internal space of each of the multiple cells 34 (the space defined by the inner circumferential surface of the cell) includes either the first flow path 21 or the second flow path 22, and the external space of the honeycomb substrate 3b (the space outside the outer circumferential surface of the honeycomb substrate) includes the other of the first flow path 21 or the second flow path 22. In the illustrated example, the internal space of the cell 34 includes the first flow path 21, and the external space of the honeycomb substrate 3b includes the second flow path 22.
[0036] B-1-2. Separation membrane The separation membrane 2 is typically provided directly on the surface of the substrate 3. The separation membrane 2 may face the first channel 21 (see Figures 1 and 4) or the second channel 22 (see Figure 5).
[0037] In one embodiment, the separation membrane 2 faces the first flow path 21. In Figure 1, the substrate 3 is a cylindrical substrate 3a, and the separation membrane 2 is formed on the inner surface of the cylindrical substrate 3a. In the illustrated example, the first channel 21 is formed in the portion of the cross-section of the separation membrane composite 10 where the separation membrane 2 is not formed (typically the central part). Furthermore, in Figure 4, the substrate 3 is a honeycomb-shaped substrate 3b, and the separation membrane 2 is formed on the inner surface of each of the multiple cells 34. The first channel 21 is formed in the portion of the cross-section of the cell 34 where the separation membrane 2 is not formed (typically the central part). The separation membrane 2 may be formed over the entire inner surface of the cylindrical substrate 3a or cell 34 (i.e., surrounding the first channel 21), as shown in the illustrated example, or it may be formed on a part of the inner surface of the cylindrical substrate 3a or cell 34. When the separation membrane is formed to surround the first channel, the separation efficiency can be improved.
[0038] Separation membrane 2 separates a specific substance from a mixture by, for example, utilizing differences in molecular size and / or adsorption properties.
[0039] The separation membrane 2 can be composed of any suitable material. Examples of materials for the separation membrane 2 include zeolite, MOF, silica, etc. These materials can be used individually or in combination.
[0040] When the adsorbed substance to be separated contains water, zeolite is preferably used as the material for the separation membrane 2. In one embodiment, the separation membrane 2 is a zeolite membrane.
[0041] A zeolite film is constructed by forming a zeolite film on the surface of a substrate. The zeolite film may contain two or more types of zeolites with different structures and compositions.
[0042] Examples of zeolites that make up a zeolite film include those in which the central atom (T atom) of the oxygen tetrahedron (TO4) constituting the zeolite is solely Si, or composed of Si and Al; AlPO-type zeolites in which the T atom is composed of Al and P; SAPO-type zeolites in which the T atom is composed of Si, Al and P; MAPSO-type zeolites in which the T atom is composed of magnesium (Mg), Si, Al and P; and ZnAPSO-type zeolites in which the T atom is composed of zinc (Zn), Si, Al and P. Some of the T atoms may be substituted with other elements.
[0043] Examples of the above-mentioned zeolites include AEI type, AEN type, AFN type, AFV type, AFX type, BEA type, CHA type, DDR type, ERI type, ETL type, FAU type (X type, Y type), GIS type, LEV type, LTA type, MEL type, MFI type, MOR type, PAU type, RHO type, SAT type, and SOD type zeolites. Among these zeolites, LTA-type zeolites are a notable example.
[0044] The maximum number of member rings in a zeolite is, for example, 12 or less, preferably 10 or less, more preferably 8 or less, and for example, 6 or more.
[0045] The zeolite film contains SiO2 and Al2O3. The zeolite film may further contain alkali metals. The alkali metals are, for example, sodium (Na) or potassium (K).
[0046] The molar ratio of SiO2 / Al2O3 in the zeolite film is, for example, 100 or less, preferably 10 or less, more preferably 5 or less, and even more preferably less than 5. When the molar ratio of SiO2 / Al2O3 in the zeolite film is below the above upper limit, the damage to the zeolite film can be suppressed more stably. The lower limit of the molar ratio of SiO2 / Al2O3 in the zeolite film is typically 2. The molar ratio of SiO2 / Al2O3 can be measured, for example, by scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDX; X-ray acceleration voltage 10kV).
[0047] The average pore size of the separation membrane 2 can be arbitrarily and appropriately selected depending on the substance to be separated. The average pore size of the separation membrane 2 is, for example, 0.2 nm to 1 nm, preferably 0.3 nm to 0.5 nm. Reducing the average pore size of the separation membrane 2 increases selectivity. The average pore size of the separation membrane 2 is smaller than the average pore size of the substrate 3. If the separation membrane 2 is a zeolite membrane, the average pore size is defined as the arithmetic mean of the short and long axes of the n-membered ring pores, where n is the maximum number of member rings in the zeolite. An n-membered ring pore is a pore where the number of oxygen atoms in the ring structure formed by oxygen atoms bonded to T atoms is n. If there are multiple n-membered ring pores with equal n, the average pore size of the zeolite is defined as the arithmetic mean of the short and long axes of all n-membered ring pores. The average pore size of a zeolite membrane is determined by the skeletal structure of the zeolite, and can be found in the International Zeolite Society's "Database of Zeolite Structures" [online], or via the Internet.<URL:http: / / www.iza-structure.org / databases / > It can be determined from the values disclosed.
[0048] The thickness of the separation membrane 2 is, for example, 0.05 μm to 30 μm, preferably 0.1 μm to 20 μm, and more preferably 0.5 μm to 10 μm. Increasing the thickness of the separation membrane increases selectivity. Increasing the thickness of the separation membrane increases the permeation rate.
[0049] The surface roughness (Ra) of the separation membrane 2 is, for example, 5 μm or less, preferably 2 μm or less, more preferably 1 μm or less, and even more preferably 0.5 μm or less. The surface roughness (Ra) can be measured, for example, in accordance with JIS B 0601.
[0050] The separation membrane 2 can be formed by any suitable method depending on the material constituting the membrane. For example, a zeolite membrane can be formed using zeolite as a seed crystal. Base materialZeolite can be obtained by immersing a substrate coated with a material and to which seed crystals are attached in a raw material solution, and growing zeolite using the seed crystals as nuclei by hydrothermal synthesis. The raw material solution includes, for example, a silica source, an alumina source, organic matter, an alkali source, and water. The heating temperature in hydrothermal synthesis is, for example, 60°C to 200°C. The heating time is, for example, 1 hour to 240 hours. Alternatively, a separation membrane may be formed using a raw material slurry obtained by mixing an organic binder, ceramic raw materials, and a solvent.
[0051] B-2. Other components The separation apparatus 1 described above may include any suitable elements in addition to the separation membrane complex 10. For example, it may include a supply unit for supplying fluids (gas supplied at startup, the mixture supplied after startup), a heating device for heating the fluids, and a recovery unit for recovering the fluids after they have passed through the separation membrane complex. Examples of heating devices include reactors involving chemical reactions, heaters, and heat exchangers. The separation apparatus 1 may further include a pressure adjustment unit capable of adjusting the pressure in the first flow path 21 and / or the second flow path 22 in the separation membrane complex 10. The separation apparatus 1 may further include a control unit capable of controlling the operation of the separation apparatus 1. Components of the separation apparatus other than the separation membrane complex are described, for example, in International Publication No. 2018 / 225325. The description in said publication is incorporated herein by reference.
[0052] In one embodiment, as shown in Figure 6, the separation apparatus 1 further comprises, in addition to the separation membrane complex 10, a supply unit 4 for supplying a mixture to the first channel 21 of the separation membrane complex 10; a first recovery unit 5 for recovering the fluid that has passed through the first channel 21; and a second recovery unit 6 for recovering the permeate material that has permeated through the separation membrane 2. The illustrated separation apparatus 1 is configured to allow adjustment of the temperature, pressure, and flow rate of the mixture passing through the first channel. Note that Figure 6 illustrates one embodiment of the present invention, and the present invention is not limited thereto.
[0053] The illustrated supply unit 4 is capable of adjusting the temperature and flow rate of the mixture supplied (flowing into) the first flow path 21. The supply unit 4 comprises a supply line 41, a heating device 42, and a flow rate regulator 43. The supply line 41 is a pipe for supplying the mixture to the first channel 21. The upstream end of the supply line 41 in the direction of mixture supply is connected to a storage tank for storing the mixture, although this is not shown in the diagram. The downstream end of the supply line 41 in the direction of mixture supply is connected to the inlet of the first channel 21 of the separation membrane complex 10. The heating device 42 is provided in the supply line 41 and is capable of heating the mixture passing through the supply line 41. The heating device 42 can employ any suitable configuration. The flow regulator 43 can adjust the flow rate of the mixture through the supply line 41. The flow regulator 43 can employ any suitable configuration. In the illustrated example, the flow regulator 43 is located in the supply line 41 between the heating device 42 and the separation membrane complex 10. The supply unit 4 may include other equipment as needed. For example, other equipment may be present between the flow regulator 43 and the separation membrane complex 10 in the supply line 41.
[0054] The first recovery unit 5 in the illustrated example is capable of adjusting the pressure in the first flow path 21. The first recovery unit 5 comprises a first recovery line 51 and a pressure regulating valve 52. The first recovery line 51 is a pipe through which the fluid that has passed through the first channel 21 of the separation membrane complex 10 passes. The upstream end of the first recovery line 51 in the direction of fluid passage is connected to the outlet of the first channel 21 of the separation membrane complex 10. The downstream end of the first recovery line 51 in the direction of fluid passage is connected to a storage tank, for example, although not shown in the figure. The pressure regulating valve 52 is located in the first recovery line 51. The pressure regulating valve 52 can adjust the opening degree of the first recovery line 51, and thereby adjust the pressure in the first flow path 21.
[0055] The second recovery unit 6 in the illustrated example includes a second recovery line 61. The second recovery line 61 is a pipe through which the fluid that has passed through the second flow path 22 of the separation membrane complex 10 passes. The upstream end of the second recovery line 61 in the direction of fluid passage is connected to the outlet of the second flow path 22 of the separation membrane complex 10. The downstream end of the second recovery line 61 in the direction of fluid passage is connected to a storage tank, for example, although not shown in the figure.
[0056] In the embodiment described above, the supply unit 4 upstream of the separation membrane complex 10 adjusts the temperature and flow rate of the mixture supplied (flowing into) the first channel 21, and the first recovery unit 5 downstream of the separation membrane complex 10 adjusts the pressure of the mixture in the first channel 21. However, the configuration of the separation apparatus 1 is not limited to this. The supply unit 4 may be configured to adjust the pressure of the mixture in the first channel 21. Also, the first recovery unit 5 may be configured to adjust the flow rate of the mixture passing through the first channel 21. [Industrial applicability]
[0057] The transient operation method of the separation apparatus according to the embodiment of the present invention can be used for the separation of a specific substance in a mixture, and can be particularly suitably used for the separation of water from a water-containing mixture. [Explanation of Symbols]
[0058] 1 Separation device 2 Separation membrane 3 Base material 21 First channel 22 Second channel
Claims
1. A transient operation method for a separation apparatus comprising a separation membrane composite having a separation membrane and a substrate disposed on one side of the separation membrane, The separation device has a first channel and a second channel, the first channel being located on the separation membrane side of the separation membrane complex, and the second channel being located on the substrate side of the separation membrane complex. This includes supplying gas to the first and second channels, and heating the separation membrane complex. The average relative humidity of gas A supplied to the first channel is higher than the average relative humidity of gas B supplied to the second channel. Transient operation method for a separation device.
2. A transient operation method for a separation apparatus according to claim 1, wherein the average relative humidity of the gas B is 10% or less.
3. A transient operation method for a separation apparatus according to claim 1 or 2, wherein the separation membrane is a zeolite membrane.
4. A transient operation method for a separation apparatus according to claim 3, wherein the zeolite membrane is composed of LTA-type zeolite.
5. A transient operation method for a separation apparatus comprising a separation membrane composite having a separation membrane and a substrate disposed on one side of the separation membrane, The separation device has a first channel and a second channel, the first channel being located on the separation membrane side of the separation membrane complex, and the second channel being located on the substrate side of the separation membrane complex. This includes supplying gas to the first and second channels, and heating the separation membrane complex. The relative humidity of gas A supplied to the first channel is higher than the relative humidity of gas B supplied to the second channel. Transient operation method for a separation device.
6. A transient operation method according to claim 1 or 2, which is a startup method.
7. A transient operation method according to claim 1 or 2, which is a stopping method.