WO2022255976A2 - Method of obtaining membranes and other functional films by aligned deposition of nanorod structured materials on porous surfaces via cross flow - Google Patents
Method of obtaining membranes and other functional films by aligned deposition of nanorod structured materials on porous surfaces via cross flow Download PDFInfo
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- WO2022255976A2 WO2022255976A2 PCT/TR2022/050489 TR2022050489W WO2022255976A2 WO 2022255976 A2 WO2022255976 A2 WO 2022255976A2 TR 2022050489 W TR2022050489 W TR 2022050489W WO 2022255976 A2 WO2022255976 A2 WO 2022255976A2
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- 239000002073 nanorod Substances 0.000 title claims abstract description 62
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000012528 membrane Substances 0.000 title claims abstract description 21
- 230000008021 deposition Effects 0.000 title abstract description 22
- 239000011148 porous material Substances 0.000 claims description 19
- 229920002678 cellulose Polymers 0.000 claims description 17
- 239000001913 cellulose Substances 0.000 claims description 17
- 239000002159 nanocrystal Substances 0.000 claims description 15
- 239000000725 suspension Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 13
- 230000008859 change Effects 0.000 claims description 7
- 238000004132 cross linking Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 125000000524 functional group Chemical group 0.000 claims description 6
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 3
- 150000004692 metal hydroxides Chemical class 0.000 claims description 3
- 239000002071 nanotube Substances 0.000 claims description 3
- 239000003431 cross linking reagent Substances 0.000 claims description 2
- 239000012510 hollow fiber Substances 0.000 claims description 2
- 239000003999 initiator Substances 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims description 2
- 238000000151 deposition Methods 0.000 description 23
- 230000008901 benefit Effects 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 239000004973 liquid crystal related substance Substances 0.000 description 6
- 230000000670 limiting effect Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
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- 239000007788 liquid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
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- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 229920001046 Nanocellulose Polymers 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000003098 cholesteric effect Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000004986 Cholesteric liquid crystals (ChLC) Substances 0.000 description 1
- 239000004988 Nematic liquid crystal Substances 0.000 description 1
- -1 PI: Feed pump Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 229920000891 common polymer Polymers 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000416 hydrocolloid Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000000614 phase inversion technique Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012465 retentate Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
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- 239000000758 substrate Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention relates to a method for obtaining membrane and other functional films by aligned deposition of nanorod structured materials on porous surfaces via cross flow.
Description
METHOD OF OBTAINING MEMBRANES AND OTHER FUNCTIONAL FILMS BY ALIGNED DEPOSITION OF NANOROD STRUCTURED MATERIALS ON POROUS SURFACES VIA CROSS FLOW
Field of the Invention
The invention relates to obtaining membranes and other functional films (films having anisotropic optical characteristics for applications such as decoration, camouflage, light filtering, three-dimensional barcode, and label, coatings having defined surface roughness for super-hydrophilic or super-hydrophobic surface coatings, material coatings having aligned conductivity) by aligned deposition of nanorod structured materials on porous surfaces via cross (tangential) flow.
State of the Art (Prior Art)
Commercial examples of porous structures such as membranes and adsorbents have a wide pore size distribution. Adjusting the pore size as desired needs to be done empirically and iteratively within the framework of fundamental principles governing the pore formation process. For example, the pore size of the membranes obtained in the phase inversion method, which is the most common method used in the production of polymeric membranes, can be adjusted by changing the composition of polymer solution and coagulation medium conditions. However, only the direction in which changes in these conditions can affect the pore size can typically be predicted in advance, and in some cases, even this cannot be predicted precisely (Yiicel et al., 2018, Journal of Membrane Science, 559, 54-62; Durmaz et al., 2018, Journal of Membrane Science, 178, 93-103, Guillen et al., 2011, Industrial and Engineering Chemistry Research, 50(7), 3798-3817). The main reason for this is that generally a production parameter has more than one effect, therefore the result of a change made in just a single parameter is not easily predictable. Adjusting the pore size by adjusting simple operating parameters (flow rate, concentration, pH, temperature, etc.) based on a theoretical background will provide flexibility and convenience to product design. A narrow pore size distribution will provide high selectivity for both products, thus increasing the
efficiency of various separation operations (e.g. the processes for the separation of materials of similar size such as different proteins, sugars, drugs, etc. from each other) and enabling more selective separations with less material consumption.
In the state of the art, membranes and adsorbents with narrow and controllable pore size distribution can be obtained by using special methods and/or materials (Yu et al., 2014, Angewandte Chemie - International Edition, 53(38), 10072-10076.). However, these often require materials and/or processes that are expensive and not easily synthesized.
Patent document numbered CN102703092A is related to a nanocellulose liquid crystal film and the application thereof, particularly cellulose nanocrystalline cholesteric liquid crystal material that belongs to the field of macromolecules and nanomaterials and the preparation method thereof. Here nanocellulose liquid crystal films are obtained by attaching cellulose nanocrystals to the surface of support materials.
Patent document numbered US 2019/0136033 Al is related to obtaining polymeric nanofibers through liquid crystallinity on the substrate under pressure.
However, in the state of the art, forming films with well-defined, controllable and designable structures by controlling the liquid crystal alignment of the nanorods during deposition on the porous surface and changing the pore size by simply adjusting the operating parameters (flow rate, concentration, pH, temperature, etc.) is not the case.
Brief Description and Objects of the Invention
The present invention is related to a method for obtaining membrane and other functional films by aligned deposition of nanorod structured (high aspect ratio) materials on porous surfaces via cross flow that meets the requirements above-mentioned, resolves all of the disadvantages and provides some additional advantages.
The primary object of the invention is to obtain films with well-defined, controllable and designable structures by controlling the liquid crystal alignment of the nanorods during deposition on the porous surface.
The object of the invention is to adjust the pore size of the films by adjusting only flow conditions, concentration, pH, temperature, etc. accordingly by controlling the liquid crystal alignment of the nanorods during deposition on the porous surface.
The nanorod materials used in the invention can be inexpensive materials such as cellulose nanocrystals, which can be obtained from cellulose, a natural and common polymer, in concentrated acid media. However, nanorod materials are not limited to cellulose nanocrystals.
It has been shown that the alignment can be increased by depositing cellulose nanocrystals on the surface at different flow rates. The distance between the nanorods can also be adjusted by the deposition conditions and a narrow pore size distribution can be obtained with nanorods having narrow size distribution.
In addition, the invention allows membrane production by using only water instead of organic solvents as a solvent in suspensions. Removing organic solvents that are relatively expensive and often have negative impacts on health and the environment from the production process is advantageous both in terms of cost and environmental impact.
With the invention, for the first time, aligned and porous films are obtained by using the liquid crystal alignment of nanorods with filtration carried out on the porous surface. The filtration parameters (flow rate and pressure) offer two new parameters for controlling the structure of the films, thereby enabling the controlled design of film structures consisting of aligned nanorods and pores.
The methods provided in the invention are fully scalable. The advantage of this is that the deposition is carried out in a controlled manner in large areas up to square meter scales. The advantage provided by this is that wider areas of use can be reached and commercialization is easier.
In addition to deposition on porous surfaces in the form of flat films, the method can also be used for deposition on porous surfaces such as patterned surfaces, and tubular, hollow fibers.
The synthesis of membranes and adsorbents with controllable and narrowly distributed pore sizes is achieved by using nanorods in the method and controlling their transition to the nematic liquid crystalline phase by flow conditions and suspension characteristics. The narrow pore size distribution increases the selectivity and improves the efficiency of the separation process, thus reducing the cost.
The surface deposition methods used in the invention are easily scalable. The advantage provided by this is that wider areas of use can be reached and commercialization is easier.
Description of the Figures of the Invention
The figures and related descriptions necessary for the subject matter of the invention to be understood better are given below.
Figure 1: Methods for aligned deposition of nanorods on the surface (a) and surface fixation by disrupting their colloidal stability (b)
Figure 2: Polarized microscope images of cellulose nanocrystal films obtained on porous support at 40 s 1 shear rate. The polarized filters are at 90 degrees to each other and the flow direction of the cellulose nanocrystal suspension is at 0, 45, 90 and 135 degrees from left to right with respect to the polarized filter direction, respectively. In the 1st and 3rd row images, since the alignment of the cellulose nanocrystals is in the same direction as the analyzer or polarizer, it does not cause a change in the polarization of the passing light, thereby resulting in a black microscope image.
Figure 3: Assemblies for the deposition of cellulose nanocrystals on porous surfaces. Tl: Cellulose nanocrystal suspension, PI: Feed pump, MEM: Filtration module designed to separate the feed (HI) and retentate (H3) and permeate or filtrate (H2) streams of the porous surface, Ml: Pressure gauge, VI: Pressure control valve, M2: Pressure gauge, P2: Suction pump suitable for creating negative pressure in H2 line
Detailed Description of the Invention
In this detailed description, obtaining membrane and other functional films by aligned deposition of nanorod structured materials on porous surfaces via cross flow is described only for a better understanding of the subject matter and without any limiting effect.
The method for obtaining a membrane or a functional film of the invention comprises the process steps of; a) Obtaining aligned nanorod layers by filtering the nanorod structured material suspensions on a porous surface by creating a pressure difference between two sides of the porous surface and under a cross (tangential) flow, b) Stabilizing the aligned nanorod layers by disrupting their colloidal stability via change in ionic strength, pH, temperature, pressure or solvent exchange or by cross-linking in case the nanorods have functional groups on their surfaces and thereby obtaining stable films
After step b, optionally the deposit turned into a stable film can be obtained in a free standing manner by dissolving the porous support material in a solvent that is capable of dissolving it.
Nanorod structured material can be metal, organic or inorganic, synthetic or natural rod shaped materials such as cellulose nanocrystal, metal hydroxide nanorod, and nanotube.
Suspensions of metal, organic or inorganic, synthetic or natural nanorod materials such as cellulose nanocrystals, metal hydroxide nanorods, and nanotubes in various solvents can show nematic liquid crystal alignment under flow. Factors such as flow rate, concentration of nanorods and ionic strength can be used to control the degree of alignment and the distance between the long axes of aligned nanorods. The transition from random arrangement to alignment in the flow direction depends on the characteristics of the material such as aspect ratio, density, etc., and will occur at different values for each nanorod. For example, for cellulose nanocrystals with a length of 180 nm and a diameter of 8 nm, there is an alignment on flow rates that provide a shear rate of 10 s 1. The concentration of the transition from the isotropic phase to the aligned nematic phase can also be found with the Onsager Model
depending on the aspect ratio and density of the nanorods (Qiao et al., 2016, Food Hydrocolloids, 55, 19-25).
The distance between the long axes of the aligned nanorods can be controlled by changing the ionic strength from zero to a concentration that causes the nanorods to aggregate and collapse for any given salt. For example, this concentration range is approximately 0 - 200 mM for cellulose nanocrystals and NaCl and approximately 0 - 25 mM for CaCb.
The first step of the invention is to deposit nanorods aligned in the direction of the flow on a porous support surface in a controlled manner by depositing them on the surface due to the pressure difference created between the two sides of the porous surface while flowing tangentially to the porous surface under flow conditions that will cause nanorod alignment (Figure l.a). The porous surface must have a pore size that does not allow the nanorods to penetrate therein. The pressure difference between the two sides of the surface can be provided by a valve placed at the outlet of the line through which the nanorod suspension flows tangential to the surface (Nataraj et al., 2008, Journal of Membrane Science, 308 (1-2), 152-161; Konca et al., 2019, Journal of Membrane Science, 587/9) (Figure 3. a)
The other side of the porous surface can be at atmospheric pressure or below atmospheric pressure, provided that it is at a lower pressure than the feed side. The fact that this side is below atmospheric pressure can be realized with a pump that provides suction to this line, thus allowing the solvent in the nanorod suspension to pass through the porous surface into this line (Miller et al., 2013, Review of Scientific Instruments, 84/3, 035003; Gen al et al., 2015, Journal of Membrane Science, 476, 224-233) (Figure 3.b). In this case, the other side of the surface containing the nanorods under cross flow can be at or above atmospheric pressure.
During this filtration operation, the concentration of nanorods on the surface is higher than that of the original suspension because the solvent, which is the continuous phase of the suspension, can pass through the pores while the nanorods are too large to pass through the
porous surface. This is the same phenomenon referred to as “concentration polarization” in tangential flow membrane filtration. When the pressure difference between the two sides of the porous support surface is gradually increased under constant flow conditions, it is seen that the flow rate through the unit membrane area does not change after a certain pressure. This is known as “limiting flux” in tangential flow membrane filtration. After the limiting flux is reached, increasing the pressure does not change the concentration of nanorods deposited on the surface, but only increases the thickness. Concentration polarization and subsequent limiting flux phenomena are used in the present invention to achieve aligned deposition of nanorods on the surface and to adjust the thickness of the deposit layer as desired. The degree of alignment of the nanorods in the deposit and the distance therebetween are also used to adjust the porosity and pore size in the film.
The pressure difference that needs to be created between the two sides of the porous surface to reach the limiting flux and realize deposition on the surface depends on the concentration of nanorods and the permeability of the porous surface. When the applied pressure difference is gradually increased with all other operating conditions being the same, the rate of transmission to the non-deposit side of the porous surface stabilizes after a certain pressure difference. At any pressure above the point where stabilization is seen, nanorods can be deposited on the surface.
The second step of the invention consists of coagulating the aligned nanorods deposited on the surface in such a way that they are not re-dispersed into the suspension, thus fixing the alignment on the surface (b). Fixation can be done by increasing the ionic strength of the solution or by adjusting properties such as temperature, pH, solvent, pressure, etc. in a way that decreases the colloidal stability of the nanorods. Furthermore, in case there are reactive groups on the surface of the nanorods, nanorods can be fixed by cross-linking these groups in such a way that their aligned deposition is not disrupted. The cross-linking of the functional groups on the surface of nanorods is carried out by forming covalent bonds directly between these functional groups or by a cross-linking agent to be added later, an initiator, temperature, pressure or light.
When these aligned films are prepared on a porous support surface, deposition is realized in such a way that the gaps between the nanorods are estimated to be around 3-5 nm according
to calculations made from experimental observations; films with pores of these sizes can function as membranes or adsorbents and can be used in processes for concentrating structures (polymers, proteins, drug molecules, nanoparticles, etc.) with sizes larger than the gaps in the structure in liquid media or for adsorbing smaller structures to the surface. Once these deposits are fixed on the porous support surface (by coagulation, cross-linking, etc.), they can be separated from the surfaces and used alone. Separation from the support surface can be achieved by dissolving the material forming the support surface in a suitable solvent. This solvent must be a solvent that does not dissolve the nanorods. Surfaces with depositions interact with light at visible wavelengths due to their controlled nematic and cholesteric alignment symmetries. Therefore, they can be used in optical applications, structural-colored surface coatings, light filters, three-dimensional barcode and label applications. Furthermore, they can also be used as a template for the synthesis of inorganic materials. In addition to these applications, anisotropic mechanical characteristics are also provided due to the anisotropic nanostructures of the materials. Due to these features, they can also be used in new robotics applications.
An advantage of the methods claimed in the invention is that they are scalable. Films having deposition on porous support with the controlled cross flow and pressure difference can be prepared on flat and tubular surfaces in square meter scales. This advantage is an important step towards the commercialization of the above-mentioned applications.
Deposition on the porous surface can also be carried out without tangential flow, simply by creating a pressure difference between the two sides of the porous surface. Under these conditions, all nanorods in suspension are deposited without alignment on the porous support surface. Films to be formed in this way from nanorod structured materials such as cellulose nanocrystals, etc., the suspensions of which above a certain concentration are in the cholesteric liquid crystalline phase, are the second variation of the method of the present invention. The flow rate and concentration profile of nanorods flowing towards the porous support surface due to the pressure difference can be controlled by the permeability of the porous surface, the applied pressure and the concentration and ionic strength of the suspension fed into the system. Fixation of the deposit on the surface can again be achieved by ionic strength, temperature, pH, solvent change or cross-linking chemically, thermally or photochemically (e.g. with UV light).
Claims
1. A method for obtaining a membrane or a functional film, characterized in that it comprises the process steps of; a) Obtaining aligned nanorod layers by filtering the nanorod structured material suspensions on a porous surface by creating a pressure difference between two sides of the porous surface and under a cross (tangential) flow, b) Stabilizing the aligned nanorod layers by disrupting their colloidal stability via change in ionic strength, pH, temperature, pressure or solvent exchange or by cross-linking in case the nanorods have functional groups on their surfaces and thereby obtaining stable films.
2. The method according to claim 1, characterized in that after process step b, the support beneath the deposit turned into a stable film is dissolved in a solvent that is capable of dissolving porous support material for obtaining the film in a free-standing manner.
3. The method according to claim 1, characterized in that said nanorod structured material is cellulose nanocrystal, metal hydroxide nanorod or nanotube.
4. The method according to claim 1, characterized in that the pore size of the porous support surface is such that it does not allow the nanorods to penetrate therein.
5. The method according to claim 1, characterized in that the cross-linking of the functional groups on the surface of nanorods is carried out by forming covalent bonds directly between these functional groups or by a cross-linking agent to be added later, an initiator, temperature, pressure or light.
6. The method according to claim 1, characterized in that the porous surface is flat, patterned, hollow fiber or tubular surfaces.
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| Application Number | Priority Date | Filing Date | Title |
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| EP22816574.2A EP4313846A2 (en) | 2021-05-31 | 2022-05-26 | Method of obtaining membranes and other functional films by aligned deposition of nanorod structured materials on porous surfaces via cross flow |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TR2021/008914 TR2021008914A1 (en) | 2021-05-31 | OBTAINING MEMBRANES AND OTHER FUNCTIONAL FILMS BY DIRECTED DEPOSITION OF NANOROD STRUCTURED MATERIALS ON POROUS SURFACES WITH CROSS FLOW | |
| TR2021008914 | 2021-05-31 |
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