Virus inactivating liquid agent and virus inactivating article

Abstract

Provided is a novel virus-inactivating liquid agent. This virus-inactivating liquid agent comprises a liquid medium and particles of a layered material including one or more layers, wherein the layers each include: a layer body represented by the formula of MmXn (in the formula, M is at least one metal belonging to group 3, 4, 5, 6, or 7, X is a carbon atom, a nitrogen atom, or a combination thereof, n is 1-4, and m is greater than n and at most 5); and a modification or terminal T (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom) present on the surface of the layer body.

Description

[Technical field]

[0001] The present disclosure relates to a virus inactivation liquid agent and a virus inactivation article. [Background technology]

[0002] Conventionally, various antibacterial agents and articles to which antibacterial agents are applied are known. For example, Patent Document 1 discloses an antibacterial sheet in which silver is used as the active ingredient of the antibacterial agent, and an antibacterial layer containing the antibacterial agent and a binder (the water contact angle of the binder alone is 20° or less) is disposed on a substrate. Patent Document 1 describes that the antibacterial agent is preferably one that exhibits a bactericidal effect against pathogenic bacteria such as Staphylococcus aureus and Escherichia coli.

[0003] On the other hand, it is known that liquid virus inactivating agents contain alcohol such as ethanol or 2-propanol as an active ingredient. The World Health Organization (WHO) recommends a prescription with an alcohol concentration of 80% by volume ethanol or 75% by volume 2-propanol as a hand disinfectant. However, it has been reported that a prescription with a lower alcohol concentration can also achieve the effect of virus inactivation. For example, Non-Patent Document 1 reports that a prescription with an ethanol or 2-propanol concentration of 30% by volume can achieve the effect of virus inactivation against SARS-CoV-2 (the so-called "novel coronavirus"). [Prior art documents] [Patent documents]

[0004] [Patent Document 1] International Publication No. 2016 / 047568 [Patent Document 2] International Publication No. 2017 / 083055 [Non-patent literature]

[0005] [Non-Patent Document 1] Annika Kratzel, et al., "Inactivation of Severe Acute Respiratory Syndrome Coronavirus 2 by WHO-Recommended Hand Rub Formulations and Alcohols", Emerging Infectious Diseases, 2020, Vol. 26, Issue 7, pp. 1592-1595 Summary of the Invention [Problem to be solved by the invention]

[0006] In recent years, MXene has been attracting attention as a new material. MXene is a type of so-called two-dimensional material, and as described below, it is a layered material having the form of one or more layers. In general, MXene has the form of particles of such layered materials (which may include powders, flakes, nanosheets, etc.).

[0007] Patent Document 2 discloses an antimicrobial agent containing MXene and an antimicrobial membrane in which the antimicrobial agent is coated on a polyvinylidene fluoride (PVDF) substrate. Patent Document 2 describes that the antimicrobial agent exhibits antimicrobial effects against Escherichia coli (E. coli) and Bacillus subtilis (B. subtilis).

[0008] As is generally known, bacteria are single-celled organisms, have a size on the order of microns, and are capable of self-propagation. In contrast, viruses are composed of nucleic acids (genes), capsids, and sometimes envelopes, have a size on the order of nanometers, are unable to self-propagate, and propagate by parasitizing cells (hosts). Thus, bacteria and viruses are completely different at least in terms of structure, size, and propagation mechanism. Even if a substance exhibits antibacterial effects, it cannot be determined by this alone whether the substance exhibits a virus inactivation effect. In fact, Patent Documents 1 and 2 do not mention viruses at all. Antibacterial properties can be evaluated according to JIS Z 2801, as described in Patent Document 1, for example. Although there is no specific standard for virus inactivation ability, it is possible to evaluate the virus inactivation ability by measuring the TCID 50 It can be evaluated by law.

[0009] There are many different types of viruses, and preventing the spread of infectious diseases caused by viruses has become an extremely important issue internationally. Under these circumstances, there is an increasing demand for novel virus inactivating liquid agents and virus inactivating products.

[0010] An object of the present disclosure is to provide a novel virus inactivation liquid agent and a novel virus inactivation article. [Means for solving the problem]

[0011] As a result of extensive research, the present inventors independently discovered that MXene has the ability to inactivate viruses, and have thus completed the present disclosure.

[0012] According to a first aspect of the present disclosure, there is provided a liquid virus inactivating agent, the liquid comprising: a liquid medium; and particles of a layered material comprising one or more layers; The layer comprises a compound having the following formula: M m X n (wherein M is at least one Group 3, 4, 5, 6, or 7 metal; X is a carbon atom, a nitrogen atom, or a combination thereof; n is 1 to 4, m is greater than n and less than or equal to 5) and a modification or terminal T (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom and an oxygen atom) present on the surface of the layer body.

[0013] In one embodiment of the first aspect of the present disclosure, the M m X n may be Ti3C2.

[0014] In one embodiment of the first aspect of the present disclosure, the particles may have an average thickness of 10 nm or less.

[0015] In one embodiment of the first aspect of the present disclosure, the liquid medium may include at least one of water and alcohol.

[0016] In one embodiment of the first aspect of the present disclosure, the virus inactivating liquid agent may further include at least one additive selected from the group consisting of a dispersant, a binder, an antioxidant, a viscosity modifier, and a fragrance.

[0017] In one embodiment of the first aspect of the present disclosure, the content of the particles in the virus inactivating liquid agent may be 0.5 mg / mL or more and 100 mg / mL or less.

[0018] In one embodiment of the first aspect of the present disclosure, the liquid medium may have a pH of 2.7 or more and 7.0 or less.

[0019] In one embodiment of the first aspect of the present disclosure, the particles may have a Li content of 20 ppm by mass or less.

[0020] In one embodiment of the first aspect of the present disclosure, the particles may have a total content of chlorine and bromine of 1,500 ppm by mass or less.

[0021] In one embodiment of the first aspect of the present disclosure, the particles may support at least one of a metal and a metal oxide, for example, titanium oxide.

[0022] According to a second aspect of the present disclosure, there is provided a virus inactivation article, comprising: A substrate; a virus inactivation layer disposed on the substrate; wherein the viral inactivation layer comprises particles of layered material comprising one or more layers; The layer comprises a compound having the following formula: M m X n (wherein M is at least one Group 3, 4, 5, 6, or 7 metal; X is a carbon atom, a nitrogen atom, or a combination thereof; n is 1 or more and 4 or less, m is greater than n and less than or equal to 5) and a modification or terminal T (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom) present on the surface of the layer body.

[0023] In one embodiment of the second aspect of the present disclosure, the substrate may be any one selected from the group consisting of a filter, a mask, a face shield, a bandage, a glove, a gown, a touch panel, a display, a film, and a seal.

[0024] In one embodiment of the second aspect of the present disclosure, the M m X n may be Ti3C2.

[0025] In one embodiment of the second aspect of the present disclosure, the particles may have an average thickness of 10 nm or less.

[0026] In one embodiment of the second aspect of the present disclosure, the virus inactivation article may further include at least one additive selected from the group consisting of a dispersant, a binder, an antioxidant, a viscosity modifier, and a fragrance.

[0027] In one embodiment of the second aspect of the present disclosure, the particles may have a Li content of 20 ppm by mass or less.

[0028] In one embodiment of the second aspect of the present disclosure, the particles may have a total content of chlorine and bromine of 1,500 ppm by mass or less.

[0029] In one embodiment of the second aspect of the present disclosure, the particles may support at least one of a metal and a metal oxide, for example, titanium oxide. Effect of the Invention

[0030] According to the present disclosure, the virus inactivation liquid agent and the virus inactivation layer of the virus inactivation article contain particles of a specific layered material (also referred to as "MXene" in this specification), which can inactivate viruses. Thus, according to the present disclosure, a novel virus inactivation liquid agent and a virus inactivation article are provided. [Brief description of the drawings]

[0031] [Figure 1] 1A and 1B are schematic cross-sectional views showing MXene, a layered material that can be used in one embodiment of the present disclosure, where (a) shows a single layer MXene and (b) shows a multi-layer (illustratively two-layer) MXene. [Diagram 2] FIG. 1 is a diagram illustrating a virus inactivation article in one embodiment of the present disclosure, in which (a) shows a schematic cross-sectional view of the virus inactivation article, and (b) shows a schematic perspective view of layered materials in a virus inactivation layer of the virus inactivation article. [Diagram 3]FIG. 1 shows SEM photographs showing the progress of partial oxidation in the heat treatment (oxidation treatment) of Example 2, where (a) is an SEM photograph of the solid content (particles) before treatment, and (b) is an SEM photograph of the solid content (particles) after treatment. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0032] (Embodiment 1: Virus inactivation liquid agent) A virus inactivating liquid agent in one embodiment of the present disclosure will be described in detail below, but the present disclosure is not limited to this embodiment.

[0033] The virus inactivating liquid agent of the present embodiment contains a liquid medium and particles of a predetermined layered material.

[0034] A particular layered material that may be used in this embodiment is MXene, which is defined as follows: 1. A layered material comprising one or more layers, the layers being represented by the following formula: M m X n where M is at least one group 3, 4, 5, 6, 7 metal and may include at least one selected from the group consisting of so-called early transition metals, such as Sc, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo and Mn; X is a carbon atom, a nitrogen atom, or a combination thereof; n is 1 or more and 4 or less, m is greater than n and less than or equal to 5) and a modification or termination T (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom) present on the surface of the layer body (more specifically, on at least one of the two opposing surfaces of the layer body). m X n T s", where s is any number, and conventionally, x is sometimes used in place of s). Typically, n can be 1, 2, 3, or 4, but is not limited thereto.

[0035] In the above formula for MXene, M is preferably at least one selected from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, and Mn, and more preferably at least one selected from the group consisting of Ti, V, Cr, and Mo.

[0036] MXene is a compound represented by the above formula: m X n However, it is known that it can be expressed as follows: Sc2C, Ti2C, Ti2N, Zr2C, Zr2N, Hf2C, Hf2N, V2C, V2N, Nb2C, Ta2C, Cr2C, Cr2N, Mo2C, Mo 1.3 C, Cr 1.3 C, (Ti,V)2C, (Ti,Nb)2C, W2C, W 1.3 C, Mo2N, Nb 1.3 C, Mo 1.3 Y 0.6 C (in the above formula, "1.3" and "0.6" mean approximately 1.3 (= 4 / 3) and approximately 0.6 (= 2 / 3), respectively), Ti3C2, Ti3N2, Ti3(CN), Zr3C2, (Ti,V)3C2, (Ti2Nb)C2, (Ti2Ta)C2, (Ti2Mn)C2, Hf3C2, (Hf2V)C2, (Hf2Mn)C2, (V2Ti)C2, (Cr2Ti)C2, (Cr2V)C 2, (Cr2Nb)C2, (Cr2Ta)C2, (Mo2Sc)C2, (Mo2Ti)C2, (Mo2Zr)C2, (Mo2Hf)C2, (Mo2V)C2, (Mo2Nb)C2, (Mo2Ta)C2, (W2Ti)C2, (W2Zr)C2, (W2Hf)C2, Ti4N3, V4C3, Nb4C3, Ta4C3, (Ti,Nb)4C3, (Nb,Zr)4C3, (Ti2Nb2)C3, (Ti2Ta2)C3, (V2Ti2)C3, (V2Nb2)C3, (V2Ta2)C3, (Nb2Ta2)C3, (Cr2Ti2)C3, (Cr 2V2)C3, (Cr2Nb2)C3, (Cr2Ta2)C3, (Mo2Ti2)C3, (Mo2Zr2)C3, (Mo2Hf2)C3, (Mo2V2)C3, (Mo2Nb2)C3, (Mo2Ta2)C3, (W2Ti2)C3, (W2Zr2)C3, (W2Hf2)C3

[0037] Typically, in the above formula, M can be titanium or vanadium, and X can be a carbon atom or a nitrogen atom. For example, the MAX phase is Ti3AlC2, and MXene is Ti3C2T s (In other words, M is Ti, X is C, n is 2, and m is 3). That is, the above formula: M m X n However, it is Ti3C2.

[0038] Such MXene particles (hereinafter simply referred to as "MXene particles") can be synthesized by selectively etching (removing and optionally layer-separating) A atoms (and optionally some of the M atoms) from the MAX phase. The MAX phase has the following formula: M m AX n (wherein M, X, n and m are as defined above, and A is at least one Group 12, 13, 14, 15, 16 element, usually a Group A element, typically Group IIIA and Group IVA, and more particularly may include at least one element selected from the group consisting of Al, Ga, In, Tl, Si, Ge, Sn, Pb, P, As, S and Cd, and is preferably Al). and M m X n(each X may have a crystal lattice in which it is located in the octahedral array of M) between which a layer composed of A atoms is located. In the MAX phase, typically when m=n+1, one layer of X atoms is arranged between each of the n+1 layers of M atoms (collectively referred to as "M m X n The MAX phase has a repeating unit in which a layer of A atoms (also referred to as an "A layer") is arranged as a layer next to the n+1th layer of M atoms, but is not limited thereto. The A atoms (and sometimes a part of the M atoms) are selectively etched (removed and sometimes layer separated) from the MAX phase, thereby removing the A atom layer (and sometimes a part of the M atoms) to expose the M m X n The surface of the layer is modified with hydroxyl groups, fluorine atoms, chlorine atoms, oxygen atoms, etc. present in the etching solution (usually, an aqueous solution of fluorine-containing acid is used, but is not limited to this) to terminate the surface.

[0039] The above etching is carried out in a fluorine-based resin container with an acid such as HF, HCl, HBr, HI, sulfuric acid, phosphoric acid, or nitric acid. - For example, a method using a mixed solution of lithium fluoride and hydrochloric acid, or a method using hydrofluoric acid may be used.

[0040] If desired, any suitable metal, such as Li, may be intercalated between the MXene layers, either separately after the etching process or in conjunction with the etching process.

[0041] Thereafter, layer separation of MXene (delamination, separation of multi-layered MXene into monolayered MXene) may be promoted by any suitable post-treatment (e.g., ultrasonic treatment, hand shaking, automatic shaker, etc.). For example, delamination treatment may be performed for a predetermined time using a mechanical shaker, vortex mixer, homogenizer, ultrasonic bath, etc. Next, the supernatant and precipitate are separated using a centrifuge, and the collected supernatant can be obtained as a dispersion of monolayered MXene particles. Note that ultrasonic treatment may destroy MXene due to excessive shear force, so when it is desired to obtain MXene particles (preferably monolayered MXene particles) having a two-dimensional shape with a larger aspect ratio, it is preferable to apply an appropriate shear force by hand shaking or an automatic shaker, etc.

[0042] In the present disclosure, the MXene particles may contain a relatively small amount of residual A atoms, for example, 10% by mass or less of the original A atoms. The amount of residual A atoms may be preferably 8% by mass or less, more preferably 6% by mass or less. However, even if the amount of residual A atoms exceeds 10% by mass, there may be cases where this is not a problem depending on the purpose of virus inactivation and the conditions of use.

[0043] The MXene particles 10 thus synthesized may be particles of layered material comprising one or more MXene layers 7a, 7b, as shown diagrammatically in FIG. 1 (non-limiting examples of MXene particles 10 include a single layer MXene particle 10a shown in FIG. 1(a) and a two layer MXene particle 10b shown in FIG. 1(b)). More specifically, the MXene layers 7a, 7b may be made of M m X n The layer body (M m X n The MXene layers 7a, 7b have "M m X n T s", where s is an arbitrary number. The MXene particle 10 may be one in which the MXene layers are individually separated and present as one layer (a monolayer structure shown in FIG. 1(a), so-called monolayer MXene particle 10a), a laminate in which a plurality of MXene layers are stacked at a distance from one another (a multilayer structure shown in FIG. 1(b), so-called multilayer MXene particle 10b), or a mixture thereof. The MXene particle 10 may be a particle (which may also be called a powder or flake) as an aggregate composed of monolayer MXene particles 10a and / or multilayer MXene particles 10b. In the case of a multilayer MXene particle, the two adjacent MXene layers (e.g., 7a and 7b) do not necessarily have to be completely separated, and may be partially in contact. In this embodiment, as described later, it is preferable that the MXene particle 10 contains as many monolayer MXene particles as possible (a high content of monolayer MXene particles) compared to the multilayer MXene particles.

[0044] Without being limiting to this embodiment, the thickness of each layer (corresponding to the above-mentioned MXene layers 7a, 7b) in the MXene particle is, for example, 0.8 nm or more and 5 nm or less, particularly 0.8 nm or more and 3 nm or less (which can vary mainly depending on the number of M atomic layers contained in each layer), and the maximum dimension in a plane parallel to the layer (two-dimensional sheet surface) is, for example, 0.1 μm or more and 200 μm or less, particularly 1 μm or more and 40 μm or less.

[0045] When the MXene particles are laminate (multilayer MXene) particles, the interlayer distance (or gap dimension, shown as Δd in Figure 1(b)) for each laminate is, for example, 0.8 nm or more and 10 nm or less, particularly 0.8 nm or more and 5 nm or less, more particularly about 1 nm, and the maximum dimension in a plane perpendicular to the stacking direction (two-dimensional sheet surface) is, for example, 0.1 μm or more and 100 μm or less, particularly 1 μm or more and 20 μm or less.

[0046] The total number of layers in the MXene particles may be 1 or 2 or more, for example, 1 to 100,000, particularly 1,000 to 20,000, and the thickness in the stacking direction is, for example, 0.1 to 200 μm, particularly 1 to 40 μm.

[0047] When the MXene particles are laminate (multilayer MXene) particles, the MXene particles preferably have a small number of layers. The term "small number of layers" refers to, for example, an MXene particle having 6 or fewer layers. The thickness in the stacking direction of the multilayer MXene particles having a small number of layers is preferably 10 nm or less. In this specification, this "multilayer MXene having a small number of layers" (multilayer MXene in the narrow sense) is also referred to as "few-layered MXene."

[0048] In this embodiment, the MXene particles are preferably particles (which may also be referred to as nanosheets) the majority of which is composed of monolayer MXene and / or few-layer MXene. In this specification, monolayer MXene and few-layer MXene may be collectively referred to as "monolayer / few-layer MXene".

[0049] In other words, the average thickness of the MXene particles is preferably 10 nm or less. This average thickness is more preferably 7 nm or less, and even more preferably 5 nm or less. On the other hand, when the thickness of a single-layer MXene particle is taken into consideration, the lower limit of the thickness of the MXene particles may be 1.0 nm. Thus, the average thickness of the MXene particles may be 1 nm or more.

[0050] From another perspective, the proportion of particles with a thickness of 10 nm or less in the stacking direction (single-layer MXene particles and / or few-layer MXene particles) in all MXene particles is preferably 90 vol. % or more, and more preferably 95 vol. % or more.

[0051] The above dimensions are determined as number average dimensions (e.g., number average of at least 40) based on photographs taken with a scanning electron microscope (SEM), a transmission electron microscope (TEM), or an atomic force microscope (AFM), or as distances in real space calculated from the position in reciprocal space of the (002) plane measured by X-ray diffraction (XRD).

[0052] On the other hand, any suitable liquid can be used as the liquid medium. For example, the liquid medium may be an aqueous medium. The aqueous medium is typically water, and may contain a relatively small amount of other liquid substances in addition to water (for example, 30% by mass or less, preferably 20% by mass or less based on the total aqueous medium). The liquid medium may be understood as a dispersion medium capable of dispersing MXene particles. The liquid medium may contain dissolved solutes such as ions.

[0053] Also, for example, the liquid medium may contain at least one of water and alcohol. Typically, the liquid medium is preferably water or a mixture of water and alcohol. The alcohol is not particularly limited, but may be, for example, methanol, ethanol, propanol (1-propanol, 2-propanol), etc. In the mixture of water and alcohol, when alcohol (methanol, ethanol, propanol, etc.) that is soluble / miscible with water is used, the content of alcohol based on the entire liquid medium is not particularly limited, and may be appropriately selected depending on the mode of use of the virus inactivating liquid agent, etc.

[0054] When the risk of flammability / ignition may be a problem in the use of the virus inactivating liquid agent, the liquid medium is preferably water or a mixture of water and a relatively small amount of alcohol, and more preferably water. Water is non-flammable and does not have the risk of flammability / ignition like alcohol. In contrast, in the case of conventional alcohol-based disinfectants (containing alcohol such as ethanol as an active ingredient), although it depends on the type and concentration of alcohol, the flash point may be within the range of room temperature, and there is a risk of ignition if there is an ignition source.

[0055] The virus inactivating liquid agent of this embodiment may further contain other components. For example, the virus inactivating liquid agent may further contain at least one additive selected from the group consisting of a dispersant, a binder, an antioxidant, a viscosity modifier, and a fragrance. The dispersant may be added to enhance the dispersibility of the MXene particles in the liquid medium. The binder may be added to enhance the adhesion strength between the MXene particles and the object (the substrate in the case of the second embodiment described later) after the virus inactivating liquid agent is applied to the object and dried (the liquid medium is at least partially removed), or to enhance the strength of the virus inactivating layer itself that may be formed from the virus inactivating liquid agent. The antioxidant may be added when it is desired to prevent oxidation of the MXene particles (more specifically, oxidation of the metal (M) that constitutes the MXene layer). The viscosity modifier may be added to adjust the viscosity of the virus inactivating liquid agent. More specific examples of additives include polyurethane (PU), polyvinyl alcohol (PVA), polyethylenedioxythiophene (PEDOT), sodium alginate (SA), polyamide resins (e.g., nylon), epoxy resins, acrylic resins, sodium hexametaphosphate, and polyallylamine.

[0056] Such other components may be added / mixed at any appropriate timing in the manufacturing process of the virus inactivating liquid agent. For example, other components may be added to a mixture (typically a slurry) containing synthesized MXene particles in a liquid medium, or may be added to synthesized MXene particles (typically in a clay or powder form) together with the liquid medium.

[0057] The virus inactivating liquid agent of this embodiment contains MXene particles having virus inactivation ability as an active ingredient. The fact that MXene particles have virus inactivation ability is a finding that was independently obtained by the present inventors. Although the present disclosure is not bound by any theory, the mechanism by which MXene particles inactivate viruses is believed to be as follows. MXene particles are m X nThe surface of the layer body represented by the formula (I) has a modification or a terminal T (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom), and such a configuration results in the presence of a site carrying a charge (negative or positive charge). Although this disclosure is not limited to this, specifically, the MXene particle may carry a negative charge in a plane (two-dimensional sheet surface) portion parallel to the layer, and may carry a positive charge at the end of the layer of the MXene particle. In general, viruses may also carry a charge (e.g., a positive charge), and are adsorbed by Coulomb force to a site carrying an opposite charge (e.g., a negative charge) present on the MXene particle. Since the MXene particle is conductive, when the virus is adsorbed to the above-mentioned site of the MXene particle, the virus is electrically neutralized, and as a result, the virus is instantly inactivated.

[0058] The above mechanism by which MXene particles inactivate viruses is fundamentally different from the mechanism by which MXene particles exert their antibacterial effect (inhibit bacterial growth). Bacteria are approximately the same size as or larger than MXene particles. Therefore, bacteria become surrounded by multiple MXene particles (rather than being adsorbed to MXene particles like viruses). In such a state, the effect of specific sites of MXene particles on bacteria is very small (compared to the effect on viruses). Furthermore, because bacteria have cell walls and cell membranes, being surrounded by multiple MXene particles does not immediately prevent them from growing, but rather their growth is gradually inhibited by the inhibition of life-sustaining activities such as nutrient intake.

[0059] From the above-mentioned mechanism by which MXene particles inactivate viruses, it is believed that the larger the specific surface area of ​​MXene particles, the higher the probability of contact with viruses and the greater the virus inactivation effect. From this viewpoint, and without being limiting to this embodiment, the MXene particles are preferably single-layer or few-layer MXene particles, and the average thickness of the MXene particles is preferably 10 nm or less.

[0060] The virus is not particularly limited. The virus may be composed of a nucleic acid (gene) and a capsid, and may be composed of an envelope in some cases, and generally has a size on the order of nanometers, for example, a size of several tens to several hundreds of nm. Examples of enveloped viruses (viruses having an envelope) include SARS-CoV-2 (so-called "new coronavirus"), influenza virus, herpes virus, rubella virus, hepatitis B virus, hepatitis C virus, and AIDS virus. Examples of non-envelope viruses (viruses without an envelope) include norovirus, rotavirus, poliovirus, and adenovirus. In addition, in the evaluation test of virus inactivation ability, feline calicivirus may be used as a substitute for norovirus.

[0061] In the present disclosure, "virus inactivation" (or inactivating a virus) means to eliminate the infectivity of a virus, and may also be expressed as "antiviral." Specifically, the virus infectivity is expressed as TCID 50 When evaluated by this method, if the virus infectivity is below the detection limit, it may be considered that "virus inactivation" has been achieved. The virus inactivation ability (ability to inactivate a virus) can be understood to be higher the shorter the action time required for the virus infectivity to become below the detection limit.

[0062] In addition, in the present disclosure, the term "liquid agent" refers to an agent having a liquid form as a whole. The liquid agent may be a dispersion (or suspension) in which MXene particles are dispersed (or suspended) in a liquid medium, and may be, for example, a sprayable slurry or a dispensable gel depending on the mode of use of the virus inactivating liquid agent.

[0063] The virus inactivating liquid agent of the present embodiment has a high virus inactivating ability, and can inactivate viruses in a short action time of, for example, 1 minute or less.In addition, since the virus inactivating liquid agent of the present embodiment contains MXene particles as an active ingredient, even if the liquid medium volatilizes due to exposure to air after the virus inactivating liquid agent is applied to an object, the MXene particles remain on the surface of the object, and the virus inactivating effect can be sustained for a long time, for example, even after 24 hours.In contrast, in the case of a conventional alcohol-based disinfectant, when the alcohol volatilizes, the virus inactivating effect can no longer be obtained.

[0064] The virus inactivating liquid agent of this embodiment exhibits sufficient virus inactivation effect even if the content of the MXene particles, which is the active ingredient, is small. The content of the MXene particles in the virus inactivating liquid agent can be, for example, 0.5 mg / mL or more, preferably 1 mg / mL or more, and more preferably 5 mg / mL or more. The upper limit of the content of the MXene particles in the virus inactivating liquid agent can be appropriately selected depending on the usage mode of the virus inactivating liquid agent, and when a dilute virus inactivating liquid agent is desired, the content can be, for example, 100 mg / mL or less, optionally 50 mg / mL or less, and further optionally 10 mg / mL or less.

[0065] In the virus inactivating liquid agent of this embodiment, the pH of the liquid medium can be appropriately selected depending on the desired properties and applications of the virus inactivating liquid agent, and can be, for example, 2.7 to 7.0. In the pH range of 2.7 to 7.0, the MXene particles can be stably dispersed in the liquid medium, and aggregation and / or sedimentation of the MXene particles can be prevented or reduced. Dispersion stability is important in using the virus inactivating liquid agent (applying it to a target object) and / or in obtaining a desired virus inactivation effect uniformly throughout the virus inactivating liquid agent (or a virus inactivation layer formed using it, etc.). In order to obtain higher dispersion stability for the MXene particles, the pH of the liquid medium is preferably 2.7 to 6.0.

[0066] In particular, the pH of the liquid medium is preferably 3.0 or more and 5.0 or less. In the pH range of 3.0 or more and 5.0 or less, not only is high dispersion stability of the MXene particles obtained, but the virus inactivation effect can be sustained for a longer period of time. Although the present disclosure is not bound by any theory, it is believed that in the pH range of 3.0 or more and 5.0 or less, the oxidation of the MXene particles is stabilized, thereby obtaining the above-mentioned effects. At a pH below the neutral range, hydrolysis may occur from the edge of the MXene layer of the MXene particles, and an oxide of the metal (M) constituting the MXene layer (e.g., Ti3C2T s In the case of the MXene particles represented by the formula (I), TiO2 may be produced, and CH4 and / or amorphous carbon may be produced as by-products. That is, the MXene particles, in the part where the oxidation occurs, have the M m X n The charged sites of the MXene particles are not maintained but are chemically decomposed and covered with an oxide of the metal (M) (hereinafter, such partial oxidation is also simply referred to as "partial oxidation"). Even if partial oxidation occurs to a certain extent in the MXene particles, the charged sites of the MXene particles are not all lost, so the virus inactivation effect is not significantly lost. In the pH range of 3.0 to 5.0, partial oxidation of the MXene particles may occur to a certain extent, but the oxidation is stabilized (in other words, the oxidation appears to be in a state where it does not substantially proceed), so that the virus inactivation effect can be prevented from being completely lost and can be sustained for a longer period of time at a level sufficient for virus inactivation. In addition, the stabilization of oxidation as described above, which prevents the decomposition of the MXene particles from apparently proceeding, is also thought to contribute to obtaining high dispersion stability.

[0067] From another perspective, there may be cases where a strong acidity is not preferable for the practical use of a liquid virus inactivating agent, in which case the pH of the liquid medium may be set to 3.0 or more and 7.0 or less (weakly acidic range pH = 3.0 or more and 6.0 or less, or neutral range pH = more than 6.0 and 7.0 or less).

[0068] The pH of the liquid medium can be adjusted by the type and concentration of ions dissolved in the liquid medium. Although this embodiment is not limited to this, for example, the pH of the liquid medium in the subsequently obtained virus inactivating liquid agent (typically, the slurry after delamination) can be adjusted by the etching and / or intercalation treatment conditions (for example, the type and charged concentration of acid and / or base). As described above, the intercalation treatment may be performed separately after the etching treatment or together with the etching treatment. In addition, for example, the pH of the liquid medium can be adjusted in advance when the synthesized MXene particles (typically, the clay or powder obtained by separating as a solid content after washing with water) are mixed with the liquid medium.

[0069] In the virus inactivating liquid agent of this embodiment, the Li content in the MXene particles is preferably 20 ppm by mass or less. It is known that Li can have an effect on living organisms when present in relatively large amounts, but the virus inactivating liquid agent of this embodiment can have high biocompatibility because the Li content in the MXene particles is 20 ppm by mass or less. The lower limit of the Li content in the MXene particles is not particularly limited and can be zero.

[0070] For example, even when Li intercalation is performed, the Li content in the MXene particles can be suppressed to 20 ppm by mass or less. In this case, the Li content in the MXene particles can be, for example, 1 ppm by mass or more.

[0071] When Li intercalation is performed, a virus inactivating liquid agent having a reduced Li content can be produced, for example, by the following first or second production method.

[0072] The first method for producing a virus inactivating liquid agent comprises: (a) providing a precursor comprised of a MAX phase; (b1) performing an etching treatment to remove at least a portion of the A atoms from the precursor using an etching solution; (c) performing a Li intercalation treatment, which includes a step of mixing and stirring the etched product obtained by the etching treatment with a Li-containing compound; (d) performing a delamination treatment, which includes a step of centrifuging the Li intercalation treatment product obtained by the Li intercalation treatment, discarding the supernatant, and then washing the remaining precipitate with water; (e) performing an acid treatment, the acid treatment comprising a step of mixing and stirring the delamination treated product obtained by the delamination treatment with an acid solution; (f) washing the acid-treated product obtained by the acid treatment with water to obtain MXene particles; and (g) Mixing the resulting MXene particles with a liquid medium to obtain a liquid virus inactivating agent. This production method makes it possible to produce a virus inactivating liquid agent having a Li content in the MXene particles of 0.0020% by mass (20 ppm by mass) or less.

[0073] The second method for producing a virus inactivating liquid agent comprises the steps of: (a) providing a precursor comprised of a MAX phase; (b2) etching at least a portion of the A atoms from the precursor using an etching solution containing a Li-containing compound and performing a Li intercalation process; (d) performing a delamination treatment, which includes a step of centrifuging the (etching + Li intercalation) treated product obtained by the etching and Li intercalation treatments, discarding the supernatant, and then washing the remaining precipitate with water; (e) performing an acid treatment, the acid treatment comprising a step of mixing and stirring the delamination treated product obtained by the delamination treatment with an acid solution; (f) washing the acid-treated product obtained by the acid treatment with water to obtain MXene particles; and (g) Mixing the resulting MXene particles with a liquid medium to obtain a liquid virus inactivating agent. This production method makes it possible to produce a virus inactivating liquid agent having a Li content in the MXene particles of 0.0020% by mass (20 ppm by mass) or less. Each step of the first and second production methods will be described in detail below. Step (a) and steps (d) to (g) common to these two production methods will be described together.

[0074] ·Process (a) First, a precursor composed of the MAX phase is prepared. The MAX phase is as described above. In addition to the MAX phase, the precursor may contain a trace amount of impurities that are inevitably mixed in.

[0075] ·Process (b1) In the first manufacturing method, an etching treatment is performed using an etching solution to remove at least a part of the A atoms from the precursor. The conditions of the etching treatment are not particularly limited, and known conditions can be used. The etching is performed using F - The etching can be carried out using an etching solution containing the above, for example, a method using hydrofluoric acid, a method using a mixed solution of lithium fluoride and hydrochloric acid, and a method using an etching solution further containing phosphoric acid or the like. In these methods, a method using a mixed solution with pure water as a solvent, for example, can be used. An example of the etched product obtained by the above etching treatment is a slurry.

[0076] ·Process (c) A Li intercalation treatment is carried out, which includes a step of mixing and stirring the etched product obtained by the etching treatment with a Li-containing compound.

[0077] The Li-containing compound may be a metal compound containing Li ions. As the Li-ion-containing metal compound, an ionic compound in which Li ions and cations are bonded may be used. For example, Li ions may include iodides, phosphates, sulfides including sulfates, nitrates, acetates, and carboxylates.

[0078] The content of the Li-containing compound in the intercalation treatment mixture is preferably 0.001% by mass or more. The content is more preferably 0.01% by mass or more, and even more preferably 0.1% by mass or more. On the other hand, from the viewpoint of ensuring dispersibility in the solution, the content of the Li-containing compound is preferably 10% by mass or less, and more preferably 1% by mass or less.

[0079] In step (c), for example, the slurry obtained by the etching treatment in step (b1) above is washed by repeating the process of centrifuging, removing the supernatant, adding pure water to the remaining precipitate, and then centrifuging again to obtain a water medium clay of MXene, which is then subjected to an intercalation treatment as an etching product.

[0080] The specific method of the intercalation treatment is not particularly limited, and for example, a Li-containing compound is mixed with the water medium clay of the MXene and stirred at room temperature, for example.

[0081] In the second production method, as described below, in step (b2), a precursor etching treatment and a Li intercalation treatment are carried out together.

[0082] ·Process (b2) In the second production method, at least a portion of the A atoms (and optionally a portion of the M atoms) are etched (removed and optionally layer-separated) from the precursor using an etching solution containing a Li-containing compound, and a Li intercalation treatment is performed.

[0083] In step (b2), upon etching (removal and optionally phase separation) of at least some of the A atoms (and optionally some of the M atoms) from the MAX phase, M m X n A Li intercalation process is performed to insert Li ions between the layers.

[0084] The content of the Li-containing compound in the etching solution is preferably 0.001% by mass or more. The content is more preferably 0.01% by mass or more, and even more preferably 0.1% by mass or more. On the other hand, from the viewpoint of ensuring dispersibility in the solution, the content of the Li-containing compound in the etching solution is preferably 10% by mass or less, and more preferably 1% by mass or less.

[0085] The etching solution in step (b2) is not particularly limited as long as it contains a Li-containing compound, and other components of the etching solution can be used under known conditions. For example, as described in step (b1) above, F - The etching may be performed using an etching solution further containing, for example, a method using hydrofluoric acid, a method using a mixed solution of lithium fluoride and hydrochloric acid, and a method using an etching solution further containing phosphoric acid or the like. In these methods, a method using a mixed solution with pure water as a solvent, for example, is included. The etched product obtained by the above etching process may be, for example, a slurry.

[0086] Of the first and second production methods, the first production method, in which the etching treatment step (b1) and the Li intercalation treatment step (c) are separated, is preferable because it is easier to form a monolayer of MXene.

[0087] ·Process (d) A delamination process is carried out, which includes a step of centrifuging the Li intercalation-treated product obtained by the Li intercalation process in the first manufacturing method, or the (etching + Li intercalation)-treated product obtained by the etching and Li intercalation processes in the second manufacturing method, discarding the supernatant, and then washing the remaining precipitate with water. The conditions for the delamination process are not particularly limited, and the delamination process can be carried out by a known method. For example, the delamination process can be carried out by the method shown below.

[0088] For example, a slurry-like Li intercalation-treated product or an (etching + Li intercalation)-treated product is centrifuged to discard the supernatant, and the remaining precipitate is washed with water by (i) adding pure water to the remaining precipitate after discarding the supernatant and stirring, (ii) centrifuging, and (iii) recovering the supernatant. The steps (i) to (iii) can be repeated at least once, preferably at least twice, but not more than 10 times to obtain a single-layered / single-layered MXene-containing supernatant before acid treatment as the delamination-treated product. Alternatively, the supernatant can be centrifuged, and the supernatant after centrifugation can be discarded to obtain a single-layered / single-layered MXene-containing clay before acid treatment as the delamination-treated product.

[0089] ·Process (e) The acid treatment includes a step of mixing and stirring the delamination-treated product (supernatant containing single-layer / few-layer MXene or clay containing single-layer / few-layer MXene) obtained by the delamination treatment with an acid solution. The acid used in the acid treatment is not limited, and for example, an inorganic acid such as a mineral acid and / or an organic acid can be used. The acid is preferably an inorganic acid alone or a mixed acid of an inorganic acid and an organic acid. The acid is more preferably an inorganic acid alone. As the inorganic acid, for example, one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, perchloric acid, hydroiodic acid, hydrobromic acid, hydrofluoric acid, etc. can be used. Preferably, one or more of hydrochloric acid and sulfuric acid can be used. As the organic acid, for example, acetic acid, citric acid, oxalic acid, benzoic acid, sorbic acid, etc. can be used. The concentration of the acid solution to be mixed with the delamination-treated product may be adjusted according to the amount and concentration of the delamination-treated product to be treated.

[0090] The delamination-treated material is mixed with the acid solution and stirred. Examples of the stirring method include stirring using a hand shake, an automatic shaker, a shear mixer, a pot mill, etc. The degree of stirring, such as the stirring speed and stirring time, may be adjusted according to the amount and concentration of the delamination-treated material to be treated.

[0091] When the acid solution is mixed and stirred, heating may be performed or not. The acid solution may be mixed and stirred without heating, or may be stirred while heating so that the liquid temperature is 80° C. or less.

[0092] After the stirring, for example, centrifugation is performed to remove the supernatant liquid, and the acid-treated product can be obtained as a slurry. The operation of mixing with the acid solution and stirring may be performed at least once. From the viewpoint of reducing the Li content in the MXene particles, it is preferable to perform the operation of mixing with the acid solution and stirring at least twice, for example, within a range of 10 times or less. As an embodiment of performing the operation of mixing with the acid solution and stirring multiple times, there can be mentioned a case where the steps (i) to (iii) of (i) mixing (the delamination-treated product or the remaining precipitate obtained in (iii) below) with an acid solution and stirring, (ii) centrifuging the stirred product, and (iii) discarding the supernatant liquid after centrifugation are performed at least twice, for example, within a range of 10 times or less.

[0093] The pH of the acid-treated product obtained by the acid treatment is preferably 2.5 or less. The pH is more preferably 2.0 or less, even more preferably 1.5 or less, and even more preferably 1.2 or less. The lower limit of the pH is not particularly limited, but is approximately 1.0. When the pH of the acid-treated product is sufficiently low in this way, the dispersibility of the MXene particles decreases, making the MXene particles difficult to handle in the subsequent steps. However, according to this method, this problem is solved by washing with water in the next step.

[0094] In the present disclosure, Li is actively removed by carrying out the acid treatment as described above, so that the Li content in the MXene particles can be further reduced.

[0095] ·Process (f) The acid-treated product obtained by the acid treatment is washed with water to obtain MXene particles. The amount of water to be mixed with the acid-treated product and the washing method are not particularly limited. For example, water may be added and stirring, centrifugation, etc. may be performed. Stirring methods include stirring using a hand shake, an automatic shaker, a shear mixer, a pot mill, etc. The degree of stirring, such as the stirring speed and stirring time, may be adjusted according to the amount and concentration of the acid-treated product to be treated. The washing with water may be performed one or more times. It is preferable to wash with water multiple times. For example, the steps (i) to (iii) of (i) adding water (to the acid-treated product or the remaining precipitate obtained in (iii) below) and stirring, (ii) centrifuging the stirred product, and (iii) discarding the supernatant after centrifugation may be performed two or more times, for example, 10 times or less.

[0096] ·Process (g) The MXene particles obtained as described above are mixed with a liquid medium to obtain a liquid virus inactivating agent. Details of the liquid medium are as described above. When the liquid medium is water, the water used in the washing step (f) (when washing with water is performed twice or more, the water used in the final washing step) may also serve as the liquid medium used in the step (g).

[0097] In the obtained virus inactivating liquid agent, the pH of the liquid medium may be 2.7 or more and 7.0 or less, as described above, preferably 2.7 or more and 6.0 or less, and more preferably 3.0 or more and 5.0 or less.

[0098] In this manner, even when Li intercalation is performed, a liquid virus inactivating agent having a Li content in the MXene particles of 20 ppm by mass or less can be produced.

[0099] The Li content in MXene particles can be measured by elemental (atomic) analysis such as inductively coupled plasma atomic emission spectrometry (ICP-AES) or X-ray fluorescence analysis (XRF).

[0100] In the virus inactivating liquid agent of this embodiment, the total content of chlorine and bromine in the MXene particles is preferably 1500 mass ppm or less. In the electronics industry and the like, as part of green procurement, it is required that the content of chlorine and bromine among halogens is suppressed to a certain level or less, that is, that the agent is "halogen-free". Since the total content of chlorine and bromine in the MXene particles is suppressed, the virus inactivating liquid agent of this embodiment can be suitably used in applications requiring halogen-free. The total content of chlorine and bromine is preferably 900 mass ppm or less, and most preferably 0 mass ppm or less. The lower limit of the total content of chlorine and bromine in the MXene particles is not particularly limited and may be zero.

[0101] A virus inactivating liquid agent in which the total content of chlorine and bromine is reduced can be produced, for example, by the following third production method.

[0102] The third method for producing a virus inactivating liquid agent comprises: (a) providing a precursor comprised of a MAX phase; (b3) etching A atoms from the precursor using an etching solution, wherein the etching solution satisfies at least one selected from the group consisting of a HPO concentration of 5.5M or more, a HI concentration of 5.0M or more, and a HSO concentration of 5.0M or more; and (g3) Mixing the obtained MXene particles with a liquid medium to obtain a virus inactivating liquid agent. Includes.

[0103] ·Process (a) First, a precursor composed of the MAX phase is prepared. This process is the same as in the first and second manufacturing methods.

[0104] ·Process (b3) The A atoms (and optionally some of the M atoms) are etched (removed and optionally layer separated) from the precursor using an etching solution that satisfies at least one of the group consisting of an H3PO4 concentration of 5.5M or more, an HI concentration of 5.0M or more, and an H2SO4 concentration of 5.0M or more.

[0105] In step (b3), the exposed M atoms are removed after etching (removal and optionally phase separation) of the A atoms (and optionally some of the M atoms) from the MAX phase. m X n The surface of the layer is etched with PO4 3- , I, and SO4 2- At least one selected from the group consisting of these PO4 3- etc. are M m X n When the MXene is adsorbed on the surface of the layer, the interlayer distance of the MXene increases due to steric hindrance, and the M m X n It is believed that the van der Waals forces between the layers are weakened. As a result, the multilayer M m X n Even without applying strong shear to the layer, M m X n It is believed that the layers can be easily made into a single layer. In addition, since there is no need to apply strong shear, M m X n Fracture in the plane of the layer is suppressed, resulting in a large monolayer M in the two-dimensional plane. m X n A layer can be obtained.

[0106] The etching solution does not contain hydrochloric acid, i.e., does not contain chlorine atoms. Note that the "chlorine atom-free" etching solution means that the chlorine concentration in the etching solution is 10 mass ppm or less when measured by, for example, combustion ion chromatography.

[0107] The etching solution does not need to contain hydrochloric acid, and may contain at least one of the above-mentioned predetermined amounts of H3PO4, etc. The other components of the etching solution are not particularly limited, and known conditions can be used. For example, F- For example, a method using a mixed solution of hydrofluoric acid (HF) and at least one of the above-mentioned predetermined amounts of H3PO4, etc. The concentration of hydrofluoric acid in this mixed solution may be 1 mass % or more and 50 mass % or less.

[0108] The higher the H3PO4 concentration, HI concentration, and H2SO4 concentration in the above etching solution, the better, so there are no particular limitations on the upper limits. For example, the H3PO4 concentration can be 13.2 M or less, the HI concentration can be 6.5 M or less, and the H2SO4 concentration can be 16.5 M or less.

[0109] The process after the etching is not particularly limited, and MXene particles can be obtained by a known method. For example, the slurry after the etching is washed by repeating the steps of centrifugation, removal of the supernatant, addition of pure water to the remaining precipitate, and centrifugation again, followed by intercalation and delamination treatments.

[0110] For example, after the step (b3), the steps (c) to (f) described above in the second production method may be carried out.

[0111] ·Process (g3) The MXene particles obtained as described above are mixed with a liquid medium to obtain a liquid virus inactivating agent. Details of the liquid medium are as described above. When the above-mentioned steps (c) to (f) are carried out after step (b3), the same explanation as for the above-mentioned step (g) can be applied to step (g3).

[0112] In this manner, a virus inactivating liquid agent can be produced in which the total chlorine and bromine content in the MXene particles is 1500 ppm by mass or less. When the above-mentioned steps (c) to (f) are carried out after step (b3), the Li content in the MXene particles can be reduced to 20 ppm by mass or less.

[0113] The respective chlorine and bromine contents in the MXene particles can be measured by combustion-ion chromatography.

[0114] In the first to third manufacturing methods, ultrasonic treatment is not performed as delamination after etching. Since ultrasonic treatment is not performed, particle destruction is unlikely to occur, and MXene particles containing single-layer and few-layer MXene with large two-dimensional surfaces can be obtained.

[0115] In the virus inactivating liquid agent of this embodiment, the MXene particles may support at least one of a metal and a metal oxide. This makes it possible to improve the virus inactivating ability and / or add other functions (antibacterial properties, catalytic functions, etc.) depending on the metal and / or metal oxide supported. The metal constituting the metal or metal oxide may be, for example, Ag. When the MXene particles support a metal, for example, metal particles may be supported on the MXene particles. When the MXene particles support a metal oxide, for example, metal oxide particles may be supported on the MXene particles, or the metal (M) constituting the MXene layer may be partially oxidized to support the metal oxide (produced by the partial oxidation) on the MXene particles. The fact that the MXene particles support a metal and / or metal oxide can be confirmed by detecting a peak specific to MXene and a peak specific to the metal and / or metal oxide in the XRD profile obtained by subjecting the particles to X-ray diffraction (XRD) measurement. The peak characteristic of MXene may be a peak of the (00l) plane of MXene (l is a natural number multiple of 2, i.e., l = 2, 4, 6, 8, 10, 12...), in particular the (002) plane. Detection of a peak characteristic of a metal and / or metal oxide in an XRD profile means that the content of the metal and / or metal oxide (based on the entire amount of the metal and / or metal oxide-supported MXene particles) is several mass % or more.

[0116] For example, the MXene particles may support titanium oxide. By supporting titanium oxide on the MXene particles, it is possible to impart antibacterial properties to the virus inactivating liquid agent. In this case, for example, the MXene particles may support titanium oxide particles, or Ti constituting the MXene layer may be partially oxidized to support titanium oxide (produced by the partial oxidation) on the MXene particles. Although this embodiment is not limited to this embodiment, specifically, the partial oxidation may be performed by heating in the presence of oxygen, for example, at 60 to 80°C (typically about 70°C) for 50 to 250 hours (typically 70 to 200 hours). The titanium oxide may be, but is not limited to, anatase type. For example, when the MXene particles are Ti3C2T s The Ti contained in this is partially oxidized to produce TiO2, and TiO2-supported Ti3C2T s When the particles are obtained, the particles are subjected to X-ray diffraction (XRD) measurement, and in the obtained XRD profile, Ti3C2T s This can be confirmed by detecting a peak of the (002) plane specific to TiO2 at around 2θ = 5 to 8°, and a peak specific to anatase type TiO2 at around 2θ = 24 to 26°.

[0117] Although excessive partial oxidation of the MXene particles is undesirable from the viewpoint of dispersion stability, as described above, even if partial oxidation occurs to a certain extent, the virus inactivation effect is not significantly lost. Depending on the desired properties and applications of the virus inactivating liquid agent, partial oxidation may be allowed to proceed moderately to achieve both the virus inactivation effect and antibacterial properties.

[0118] (Embodiment 2: Virus inactivation article) A virus inactivation article according to one embodiment of the present disclosure will be described in detail below, but the present disclosure is not limited to this embodiment.

[0119] Referring to FIG. 2, the virus inactivation article 20 of this embodiment is A substrate 11; A virus inactivation layer 13 disposed on the substrate 11; and the viral inactivation layer 13 comprises particles 10 of a predetermined layered material (MXene).

[0120] The substrate 11 may be any suitable article to which it may be desired to impart a viral inactivation function. The substrate 11 may also be understood as a support that supports the viral inactivation layer 13.

[0121] There are no particular limitations on the material and form of the substrate 11. For example, the substrate 11 may be made of fiber, glass, polymer / polymer composition (resin, plastic, etc.), ceramic, metal, or the like.

[0122] For example, the substrate 11 may be any one selected from the group consisting of a filter, a mask, a face shield, a bandage, a glove, a gown, a touch panel, a display (including a monitor), a film (including a protective film), and a sticker. The filter may be a filter used in an air purifier or an air conditioner, or a filter (membrane) used in a water purifier or a wastewater treatment facility. The mask, the face shield, the bandage, the glove, the gown, the touch panel, the display, the film, and the sticker may be general. Among them, the mask, the face shield, the bandage, the glove, the gown, the touch panel, and the display may be for medical use (used in a medical field), and are preferably used particularly when the person is likely to be exposed to a virus. The film and the sticker may have an adhesive layer on the side opposite to the surface on which the virus inactivation layer is disposed, and may be attached to any other article or other (for example, a touch panel, a display, a place where a large number of people may touch, etc.) via the adhesive layer. Alternatively, the film may not have an adhesive layer, and may be, for example, a porous film.

[0123] In this embodiment, the virus inactivation layer 13 can be formed using the virus inactivation liquid agent described above in embodiment 1. More specifically, the virus inactivation article 20 of this embodiment is (a) applying a virus inactivating liquid agent onto a substrate 11 to form a precursor of a virus inactivating layer containing particles of MXene; and (b) drying the precursor (in other words, at least partially removing the liquid medium) to form a virus inactivating layer 13; It can be produced by

[0124] In the above (a), the method for applying the liquid virus inactivating agent onto the substrate 11 is not particularly limited, and for example, spraying, spin casting, a blade method, printing, brush coating, immersion, etc. can be used.

[0125] The above steps (a) and (b) may be repeated a total of two or more times until a desired thickness of the virus inactivation layer is obtained.

[0126] The virus inactivation layer 13 may be substantially composed of only the MXene particles 10 (and the liquid medium that may remain in some cases), or may further contain at least one additive (not shown) selected from the group consisting of dispersants, binders, antioxidants, viscosity modifiers, and fragrances in addition to the MXene particles 10 (and the liquid medium that may remain in some cases). In order to obtain a high virus inactivation effect, when the substrate surface 11a is flat as shown in FIG. 2, it is preferable that the MXene particles 10 are oriented as parallel as possible to the substrate surface 11a (arranged flat) to form the virus inactivation layer 13, but this is not limited thereto. For example, when the substrate surface is not flat (has high surface roughness), the MXene particles 10 may be oriented along the state of the substrate surface to form the virus inactivation layer 13.

[0127] As a result, the surface 11a of the substrate 11 is coated with the virus inactivation layer 13. The virus inactivation layer 13 may coat the entire surface 11a of the substrate, or may coat only a part of the surface 11a. The thickness of the virus inactivation layer 13 may vary depending on the application of the virus inactivation article 20, and may be, for example, 0.1 μm or more and 1 mm or less.

[0128] According to the virus inactivation article 20 of this embodiment, the MXene particles can inactivate viruses through a mechanism similar to that described above in embodiment 1, and the virus inactivation effect can be sustained for a long period of time.

[0129] As for the rest, unless otherwise specified in this embodiment, the same explanation as in the first embodiment can be applied to this embodiment. EXAMPLES

[0130] Example 1 Example 1 relates to one example of the virus inactivating liquid agent described above in the first embodiment.

[0131] [Preparation of virus inactivating liquid agent] In Example 1, as described in detail below, a virus inactivating liquid agent was prepared by sequentially carrying out (1) preparation of a precursor (MAX), (2) etching of the precursor, (3) cleaning, (4) delamination, and (5) concentration adjustment.

[0132] (1) Preparation of precursor (MAX) TiC powder, Ti powder, and Al powder (all manufactured by Kojundo Chemical Laboratory Co., Ltd.) were mixed in a molar ratio of 2:1:1 in a ball mill containing zirconia balls for 24 hours. The mixed powder was sintered at 1350°C for 2 hours in an Ar atmosphere. The sintered body (block) was pulverized with an end mill to a maximum dimension of 40 μm or less. As a result, Ti3AlC2 particles were obtained as the precursor (MAX).

[0133] (2) Etching of Precursor Using the Ti3AlC2 particles (powder) prepared by the above method, etching was carried out under the following etching conditions to obtain a solid-liquid mixture (slurry) containing solid components derived from the Ti3AlC2 powder. (Etching conditions) Precursor: Ti3AlC2 (passed through a 45μm sieve) Etching solution composition: A mixture of 3g of LiF and 30mL of hydrochloric acid (9 mol / L). Precursor input: 3.0g Etching container: 100mL Eyeboy Etching temperature: 35℃ Etching time: 24h Stirrer speed: 400 rpm

[0134] (3) Cleaning The above slurry was divided into three parts and placed in three 50 mL centrifuge tubes, and centrifuged at a relative centrifugal force (RCF) of 3500G (which causes the clay to settle), after which the supernatant was separated and removed (discarded). 40 mL of pure water was added to each centrifuge tube (containing the remainder after the supernatant was separated and removed), and centrifuged again at 3500G to separate and remove the supernatant. This operation was repeated 11 times. Finally, MXene (Ti3C2T s ) particle-water medium clay was obtained.

[0135] (4) Delamination The above MXene (Ti3C2T s ) Particle-water medium 40 mL of pure water was added to the clay, and then it was stirred for 15 minutes on a shaker, centrifuged at 3500 G, and the supernatant was separated into single-layer and single-layer MXene (Ti3C2T s ) particle-containing liquid. s ) The average thickness of the MXene particles contained in the particle-containing liquid was 1 nm or more and 10 nm or less (the same applies to the following examples).

[0136] (5) Density adjustment The above single-layer and small-layer MXene (Ti3C2T s ) The particle-containing liquid was diluted with pure water so that the concentration of the particles (solid content) was adjusted to 5 mg / mL, thereby obtaining a virus inactivating liquid agent.

[0137] As a result, single-layer and few-layer MXene (Ti3C2T sA virus inactivating liquid agent of Example 1 was prepared containing 5 mg / mL of 1H-C18N-22N22O3 particles in pure water. The pH of the liquid medium in this virus inactivating liquid agent was 4.3. It was visually confirmed that the particles in this virus inactivating liquid agent were well dispersed without aggregation / sedimentation.

[0138] [Evaluation: Inactivation of enveloped viruses] The liquid virus inactivating agent obtained in Example 1 was used as a specimen (sample), and an inactivation test was performed on this specimen against an enveloped virus to evaluate the virus inactivation ability. Influenza virus was used as the enveloped virus. The details of the test are as follows.

[0139] (1) Viruses used in the test Test Virus: Influenza A virus (H1N1) A / PR / 8 / 34 ATCC VR-1469 Cells used: MDCK (NBL-2) cell JCRB 9029 strain Media used: Cell Growth Media Eagle's MEM medium "Nissui" (1) (Nissui Pharmaceutical Co., Ltd.) supplemented with 10% fetal bovine serum was used. Cell maintenance medium The following composition was used: Eagle MEM medium "Nissui" (1) 100mL 10% sodium bicarbonate 14mL L-glutamine (30g / L) 9.8mL Vitamin solution for MEM (100x) 30mL 10% albumin 20mL 0.25% trypsin 20mL

[0140] (2) Preparation of virus solution Cell culture The cells used were cultured as a monolayer in a cell culture flask using a cell growth medium. Virus inoculation After the monolayer culture, the cell growth medium was removed from the flask, and the test virus was inoculated. Next, the cell maintenance medium was added and the cells were cultured for 1 to 5 days in a carbon dioxide incubator (CO2 concentration: 5%) at 37°C ± 1°C. Preparation of virus solution After the above-mentioned culture, the morphology of the cells was observed using an inverted phase contrast microscope, and it was confirmed that the cells had undergone a morphological change (cytopathic effect). Next, the culture solution was centrifuged (3000 rpm, 10 minutes) to separate and collect the supernatant. The obtained supernatant was diluted 10 times with purified water to obtain a virus solution.

[0141] (3) Test operation 0.1 mL of the virus liquid was added to 1 mL of the sample (virus inactivation liquid agent) and mixed to obtain a mixed liquid (hereinafter referred to as the "working liquid"). The working solution was allowed to act by maintaining it at room temperature, and 1 minute, 5 minutes, 15 minutes, and 24 hours after the start, the working solution was diluted 1000 times with cell maintenance medium, and the virus infectivity was measured. (Note that in a preliminary test, it was previously confirmed that the virus infectivity could be measured without being affected by the sample by diluting the working solution 1000 times with cell maintenance medium.) As a control, a similar test was performed using purified water, and the virus infectivity was measured at the start (immediately after the start) and 1 minute, 5 minutes, 15 minutes, and 24 hours after the start.

[0142] (4) Measurement of virus infectivity After the cells were cultured in monolayer in a tissue culture microplate (96 wells) using cell growth medium, the cell growth medium was removed and 0.1 mL of cell maintenance medium was added (to each well). Next, the working solution after 100-fold dilution and the control were serially diluted 10-fold increments using cell maintenance medium. 0.1 mL of the resulting diluted solution was inoculated into 4 wells for each dilution ratio and cultured for 4 to 7 days in a carbon dioxide gas incubator (CO2 concentration: 5%) at 37°C ± 1°C. After the above incubation, the presence or absence of morphological changes in the cells (cytopathic effect) was observed using an inverted phase contrast microscope, and the 50% tissue culture infectious dose (TCID 50) was calculated to obtain the virus infectivity (log 10 TCID 50 The concentration was converted to 100 / mL. Viral infectivity (log 10 TCID 50 The results of the measurements (mg / mL) are shown in Table 1.

[0143] [Table 1] In the table, "<3.5" indicates that the result was below the lower limit of detection (viral infection was not detected).

[0144] As can be seen from Table 1, the virus inactivating liquid agent (specimen) of Example 1 had a virus infectivity below the lower limit of detection just one minute after the start of action, confirming that the agent can inactivate viruses in a short time. Furthermore, the virus inactivating liquid agent (specimen) of Example 1 had a virus infectivity below the lower limit of detection even 24 hours after the start of action, confirming that the agent can inactivate viruses sustainably. These results demonstrate that the virus inactivating liquid agent of Example 1 has high virus inactivation ability against enveloped viruses.

[0145] [Evaluation: Inactivation of non-enveloped viruses] The virus inactivating liquid agent of Example 1 is considered to have high virus inactivating ability even against non-enveloped viruses.

[0146] Example 2 The second embodiment relates to a modification of the first embodiment.

[0147] [Preparation of virus inactivating liquid agent] In Example 2, as described in detail below, after (4) delamination in Example 1, partial oxidation was carried out as an additional step, and then (5') concentration adjustment was carried out to prepare a virus inactivating liquid agent.

[0148] First, the same operations as those described in Example 1, including (1) preparation of the precursor (MAX), (2) etching of the precursor, (3) cleaning, and (4) delamination, were carried out to prepare single-layer and few-layer MXene (Ti3C2T s ) A particle-containing liquid was obtained.

[0149] The resulting single-layer and few-layer MXene (Ti3C2T s ) The particle-containing liquid had a particle concentration (solid content) of 125 mg / mL.

[0150] (Additional process) Partial oxidation The above single-layer and small-layer MXene (Ti3C2T s The particle-containing liquid was subjected to a heat treatment (oxidation treatment) at 70° C. in an oxygen-containing environment with a relative humidity of 90% to obtain a treated liquid. The treatment time was 194.5 hours.

[0151] In order to confirm that partial oxidation is progressing during the heat treatment (oxidation treatment), the single-layer and few-layer MXene (Ti3C2T s Solid matter (particles) were collected from the particle-containing liquid (before treatment) and the treatment liquid (after treatment), and observed under a scanning electron microscope (SEM). The SEM photographs obtained are shown in Figure 3. Compared to the state before treatment shown in Figure 3(a), the state after treatment shown in Figure 3(b) shows elongated images (observed as white elongated particles in the SEM photograph) that are characteristic of TiO2 obtained by low-temperature oxidation. In addition, the solid matter (particles) was subjected to X-ray diffraction (XRD) measurement to obtain an XRD profile. Compared to the XRD pattern of the solid matter (particles) before treatment, the XRD pattern of the solid matter (particles) after treatment showed that Ti3C2T s The height of the peak at 2θ=5~8° specific to anatase-type TiO2 decreased, and a new peak at 2θ=24~26° specific to anatase-type TiO2 was detected.

[0152] (5') Density adjustment The liquid after the heat treatment (oxidation treatment) was diluted with pure water so that the concentration of particles, which were solid contents, was adjusted to 5 mg / mL, thereby obtaining a virus inactivating liquid agent.

[0153] From the above, it was confirmed that TiO2-supported single-layer and few-layer MXene (Ti3C2T s A virus inactivating liquid agent of Example 2 was prepared containing 5 mg / mL of 1H-C18N-2O-2H-P2O4 particles in pure water. The pH of the liquid medium in this virus inactivating liquid agent was 4.3. It was visually confirmed that the particles in this virus inactivating liquid agent were well dispersed without aggregation / sedimentation.

[0154] [Evaluation: Inactivation of enveloped viruses] The virus inactivating liquid agent obtained in Example 2 was used as a specimen (sample), and an inactivation test of this specimen against enveloped viruses was performed in the same manner as in Example 1 to evaluate the virus inactivating ability. The results obtained showed that the virus inactivating liquid agent of Example 2 has high virus inactivating ability against enveloped viruses.

[0155] [Evaluation: Inactivation of non-enveloped viruses] The virus inactivating liquid agent of Example 2 is considered to have high virus inactivating ability even against non-enveloped viruses.

[0156] Example 3 Example 3 relates to the virus inactivation article described above in embodiment 2.

[0157] [Production of virus inactivation products] In Example 3, as described in detail below, a virus inactivating liquid agent was applied onto a substrate to form a virus inactivating layer, thereby producing a virus inactivation article in which a virus inactivating layer was disposed on a substrate.

[0158] First, the same procedure as in Example 1 was carried out except that the dilution rate with pure water was changed in the above (5) concentration adjustment, and single-layer and few-layer MXene (Ti3C2T s A liquid virus inactivation agent was prepared containing 34 mg / mL of the particles in pure water. In this virus inactivating liquid agent, the average thickness of the MXene particles was 1 nm or more and 10 nm or less, and the average dimension of the MXene particles within the plane of the two-dimensional sheet was 3 μm. This virus inactivation liquid agent is MXene (Ti3C2T s ) The particles are dispersed in pure water, and do not contain any additives such as binders or dispersants.

[0159] Separately, a glass substrate whose surface had been made hydrophilic by UV treatment was prepared as a base material.

[0160] The hydrophilized surface of the glass substrate was sprayed with the virus inactivating liquid agent prepared above, and then hot air was blown onto it using a dryer. This procedure was repeated 30 times, and then the substrate was pre-dried for 2 hours at 80°C in a normal pressure oven and then dried for 18 hours at 150°C in a vacuum oven (the liquid medium, pure water, was substantially removed by drying). As a result, monolayer and small layer MXene (Ti3C2T s A virus inactivation layer composed of 100 μm-sized particles was formed. The thickness of the virus inactivation layer was approximately 2 μm.

[0161] As a result, single-layer and few-layer MXene (Ti3C2T s As a result, the virus inactivation article of Example 3 was obtained, in which a virus inactivation layer composed of the .DELTA..DELTA..) particles was placed on a glass substrate.

[0162] [Evaluation: Inactivation of enveloped viruses] The virus inactivation article of Example 3 is considered to have high virus inactivation capacity against enveloped viruses.

[0163] [Evaluation: Inactivation of non-enveloped viruses] The virus inactivation article of Example 3 is considered to have high virus inactivation ability even against non-enveloped viruses.

[0164] Example 4 Example 4 relates to another example of the virus inactivating liquid agent described above in the first embodiment.

[0165] In Example 4, a virus inactivating liquid agent was prepared by sequentially carrying out the following steps, which are described in detail below: (1) preparation of a precursor (MAX), (2) etching of the precursor, (3) cleaning after etching, (4) intercalation of Li, and (5) delamination.

[0166] (1) Preparation of precursor (MAX) In the same manner as in Example 1, Ti3AlC2 particles were obtained as a precursor (powdered MAX).

[0167] (2) Etching of Precursor A solid-liquid mixture (slurry) containing a solid component derived from Ti3AlC2 powder was obtained in the same manner as in Example 1, except that the etching solution composition in the etching conditions was as follows. Etching solution composition: 49% HF 6mL H2O 18mL HCl (12M) 36mL

[0168] (3) Cleaning after etching The slurry was divided into two and placed in two 50 mL centrifuge tubes, respectively, in the same manner as in Example 1, except that MXene (Ti3C2T s ) particle-water medium clay was obtained.

[0169] (4) Li intercalation MXene (Ti3C2T s ) The particle-water medium clay was stirred for a specified time at a specified temperature range according to the conditions below to perform Li intercalation. (Li intercalation conditions) ·Feed composition: MXene (Ti3C2T s ) Particle-water medium clay: 0.75g solids LiCl 1.00g HCl approx. 0.67g Pure water 19.42g Intercalation vessel: 100mL Eye Boy ·Temperature: 20℃ or higher and 25℃ or lower (room temperature) ·Time: 12h Stirrer speed: 800 rpm

[0170] (5) Delamination The slurry obtained by Li intercalation was placed in a 50 mL centrifuge tube and centrifuged at 3500 G using a centrifuge, after which the supernatant was discarded. Next, (i) 40 mL of pure water was added to the remaining precipitate, and the mixture was stirred for 15 minutes using a shaker, (ii) centrifuged at 3500 G, and (iii) the supernatant was collected as a single-layer / sparse-layer MXene-containing solution. These steps (i) to (iii) were repeated four times in total to obtain a single-layer / sparse-layer MXene-containing supernatant. The supernatant was then centrifuged at 4300 G for 2 hours using a centrifuge, after which the supernatant was discarded to obtain a single-layer / sparse-layer MXene-containing clay. 1 mg of the clay thus obtained was taken and redispersed in 10 mL of pure water.

[0171] As a result, single-layer and few-layer MXene (Ti3C2T s A virus inactivating liquid agent of Example 4 was prepared containing approximately 3 mg / mL of 100% 100% 100% 15 ...

[0172] Example 5 Example 2 relates to a modification of Example 4.

[0173] In Example 5, a virus inactivating liquid agent was prepared in the same manner as in Example 4, except that in the above (4) Li intercalation, the charged composition under the Li intercalation conditions was as follows. ·Feed composition: MXene (Ti3C2T s ) Particle-water medium clay: 0.75g solids 0.97g LiCl LiOH+H2O approx. 0.03g Pure water 20.00g

[0174] As a result, single-layer and few-layer MXene (Ti3C2T s A virus inactivating liquid agent of Example 5 was prepared containing 2 mg / mL of 100% 1,000 μg / mL ...

[0175] Example 6 Example 6 relates to yet another example of the virus inactivating liquid agent described above in the first embodiment.

[0176] In Example 6, the same procedures as in Example 4 were carried out except that in the above (4) Li intercalation, the feed composition under the Li intercalation conditions was as follows, and the above (5) delamination was replaced with the following (5') delamination. Then, (6) acid treatment and (7) water washing were carried out in that order to prepare a virus inactivating liquid agent. (Li intercalation conditions) ·Feed composition: MXene (Ti3C2T s ) Particle-water medium clay: 0.75g solids 0.75g LiCl

[0177] (5') Delamination The slurry obtained by Li intercalation was placed in a 50 mL centrifuge tube and centrifuged at 3500 G using a centrifuge, after which the supernatant was discarded. Next, (i) 40 mL of pure water was added to the remaining precipitate and stirred for 15 minutes using a shaker, (ii) centrifuged at 3500 G, and (iii) the supernatant was collected as a single-layer / sparse-layer MXene-containing solution. These steps (i) to (iii) were repeated a total of four times to obtain a single-layer / sparse-layer MXene-containing supernatant. This supernatant was then centrifuged at 4300 G for 2 hours using a centrifuge, after which the supernatant was discarded to obtain a single-layer / sparse-layer MXene-containing clay.

[0178] (6) Acid treatment (i) 35 mL of 1.8 M hydrochloric acid was added to the above single-layered and few-layered MXene-containing clay, and then the clay was stirred for 5 minutes on a shaker. (ii) The clay was centrifuged at 3500 G, and (iii) the supernatant was discarded. The steps (i) to (iii) were repeated a total of five times.

[0179] (7) Water washing After the acid treatment, (i) 35 mL of water was added to the single-layered and few-layered MXene-containing clay, which was then stirred on a shaker for 5 minutes, (ii) centrifuged at 3,500 G, and (iii) the supernatant was discarded. These steps (i) to (iii) were repeated a total of five times to obtain a single-layered and few-layered MXene-containing clay as a single-layered and few-layered MXene-containing sample. It was confirmed that the pH of the supernatant was finally 4 or higher. 1 mg of the clay thus obtained was taken and redispersed in 10 mL of pure water.

[0180] As a result, single-layer and few-layer MXene (Ti3C2T s A virus inactivating liquid agent of Example 6 was prepared containing 3 mg / mL of 1H-Cyclohexyl 3H-pyridoxine (Cyclohexyl 3H-pyridoxine) particles in pure water. The pH of the liquid medium in this virus inactivating liquid agent was 4.3. It was visually confirmed that the particles in this virus inactivating liquid agent were well dispersed without aggregation / sedimentation.

[0181] [Measurement of Li content in MXene particles] MXene was dissolved by an alkali fusion method, and the Li content was measured by inductively coupled plasma atomic emission spectrometry ICP-AES (using Thermo Fisher Scientific's iCAP7400). As a result, the Li content was 4 ppm by mass.

[0182] Example 7 Example 7 relates to yet another example of the virus inactivating liquid agent described above in the first embodiment.

[0183] In Example 7, a virus inactivating liquid agent was prepared by sequentially carrying out the following steps, which are described in detail below: (1) preparation of a precursor (MAX), (2) etching of the precursor, (3) cleaning after etching, (4) intercalation of Li, and (5) delamination.

[0184] (1) Preparation of precursor (MAX) In the same manner as in Example 1, Ti3AlC2 particles were obtained as a precursor (powdered MAX).

[0185] (2) Etching of Precursor A solid-liquid mixture (slurry) containing a solid component derived from Ti3AlC2 powder was obtained in the same manner as in Example 1, except that the etching solution composition in the etching conditions was as follows. (Etching conditions) Etching solution composition: HF concentration 2.8M H3PO4 concentration 7.4M

[0186] (3) Cleaning after etching The slurry was divided into two and placed in two 50 mL centrifuge tubes, respectively, in the same manner as in Example 1, except that MXene (Ti3C2T s ) particle-water medium clay was obtained.

[0187] (4) Li intercalation MXene (Ti3C2T s) Li3PO4, H3PO4 and pure water were added to the particle-water medium clay and stirred at a specified temperature range for a specified time to perform Li intercalation. (Li intercalation conditions) ·Feed composition: MXene (Ti3C2T s ) Particle-water medium clay: 0.75g solids Li3PO4: 0.68g 85 mass%H3PO4:3.1mL Pure water: 31.9mL Intercalation vessel: 100mL Eye Boy ·Temperature: 20℃ or higher and 25℃ or lower (room temperature) ·Time: 15h Stirrer speed: 800 rpm

[0188] (5) Delamination The slurry obtained by Li intercalation was placed in a 50 mL centrifuge tube and centrifuged at 3500 G using a centrifuge, after which the supernatant was discarded. Next, 40 mL of pure water was added to the remaining precipitate after removing the supernatant, and the mixture was stirred for 15 minutes on a shaker, centrifuged at 3500 G, and the supernatant was collected as a single-layer / sparse-layer MXene-containing liquid. This procedure was repeated four times to obtain a single-layer / sparse-layer MXene-containing liquid.

[0189] As a result, single-layer and few-layer MXene (Ti3C2T s A virus inactivating liquid agent of Example 7 was prepared containing 3 mg / mL of 1H-Cyclohexyl 3H-pyridoxine (Cyclohexyl 3H-pyridoxine) particles in pure water. The pH of the liquid medium in this virus inactivating liquid agent was 4.3. It was visually confirmed that the particles in this virus inactivating liquid agent were well dispersed without aggregation / sedimentation.

[0190] [Measurement of chlorine and bromine contents in MXene particles] The chlorine content and bromine content in the MXene particles obtained in Example 7 were measured using a combustion-ion chromatography device (Dionex ICS-5000) manufactured by Thermo Fisher Scientific Inc. As a result, the chlorine content was 50 ppm by mass or less, and the bromine content was also 50 ppm by mass or less, that is, the total content of chlorine and bromine was 100 ppm by mass or less.

[0191] [Evaluation: Inactivation of viruses] The virus inactivating liquid agents of Examples 4 to 7, like the virus inactivating liquid agent of Example 1, are considered to have high virus inactivating ability against enveloped and non-enveloped viruses. [Industrial Applicability]

[0192] The virus inactivating liquid agent and virus inactivating article of the present disclosure can inactivate viruses and can therefore be used to prevent humans and other living organisms from becoming infected with viruses.

[0193] This application claims priority to application Ser. No. 63 / 129051, filed in the United States on December 22, 2020, the entire contents of which are incorporated herein by reference. [Explanation of symbols]

[0194] 1a, 1b layer body (M m X n layer) 3a, 5a, 3b, 5b Modified or terminal T 7a, 7b MXene layers 10, 10a, 10b MXene (layered material) particles 11 Base material 11a Base material surface 13 Virus inactivation layer 20 Virus inactivation products

Claims

1. A virus inactivating liquid agent, comprising: a liquid medium; and particles of layered material comprising one or more layers; The layer has the following formula: M ｍ X ｎ wherein M is at least one Group 3, 4, 5, 6, or 7 metal; X is a carbon atom, a nitrogen atom, or a combination thereof; n is 1 or more and 4 or less, m is greater than n and is equal to or less than 5. and a modification or terminal T (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom) present on the surface of the layer body, A virus inactivating liquid agent, wherein the particles have an average thickness of 10 nm or less.

2. Said M ｍ X ｎ But Ti ３ C ２ The virus inactivating liquid agent according to claim 1,

3. The virus inactivating liquid agent according to claim 1 or 2, wherein the liquid medium contains at least one of water and alcohol.

4. 4. The virus inactivating liquid agent according to claim 1, further comprising at least one additive selected from the group consisting of a dispersant, a binder, an antioxidant, a viscosity modifier and a fragrance.

5. 5. The virus inactivating liquid agent according to claim 1, wherein the content of the particles in the virus inactivating liquid agent is 0.5 mg / mL or more and 100 mg / mL or less.

6. The virus inactivating liquid agent according to any one of claims 1 to 5, wherein the liquid medium has a pH of 2.7 or more and 7.0 or less.

7. The virus inactivating liquid agent according to any one of claims 1 to 6, wherein the particles have a Li content of 20 ppm by mass or less.

8. The virus inactivating liquid agent according to any one of claims 1 to 7, wherein the particles have a total content of chlorine and bromine of 1,500 ppm by mass or less.

9. The virus inactivating liquid agent according to any one of claims 1 to 8, wherein the particles carry at least one of a metal and a metal oxide.

10. The virus inactivating liquid agent according to any one of claims 1 to 9, wherein the particles carry titanium oxide.

11. 1. A virus inactivation article comprising: A substrate; a virus inactivation layer disposed on the substrate; wherein the viral inactivation layer comprises particles of layered material comprising one or more layers; The layer has the following formula: M ｍ X ｎ wherein M is at least one Group 3, 4, 5, 6, or 7 metal; X is a carbon atom, a nitrogen atom, or a combination thereof; n is 1 or more and 4 or less, m is greater than n and is equal to or less than 5. and a modification or terminal T (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom) present on the surface of the layer body, A virus inactivation article, wherein the particles have an average thickness of 10 nm or less.

12. The virus inactivation article according to claim 11, wherein the substrate is any one selected from the group consisting of a filter, a mask, a face shield, a bandage, a glove, a gown, a touch panel, a display, a film, and a seal.

13. Said M ｍ X ｎ But Ti ３ C ２ The virus inactivation article according to claim 11 or 12,

14. The virus inactivation article according to any one of claims 11 to 13, further comprising at least one additive selected from the group consisting of a dispersant, a binder, an antioxidant, a viscosity modifier and a fragrance.

15. The virus inactivation article according to any one of claims 11 to 14, wherein the particle has a Li content of 20 ppm by mass or less.

16. The virus inactivation article according to any one of claims 11 to 15, wherein the total content of chlorine and bromine in the particles is 1500 ppm by mass or less.

17. The virus inactivation article according to any one of claims 11 to 16, wherein the particles carry at least one of a metal and a metal oxide.

18. The virus inactivation article according to any one of claims 11 to 17, wherein the particles carry titanium oxide.

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