Virus inactivation liquids and virus inactivation articles

Abstract

A novel virus inactivation liquid is provided. A virus inactivation liquid comprises a liquid medium and particles of a layered material comprising one or more layers, wherein the layers comprise: m X n A layer body represented by the formula (wherein, M is at least one metal of Groups 3, 4, 5, 6, or 7, X is a carbon atom, a nitrogen atom, or a combination thereof, n is greater than 1 and less than 4, and m is greater than n and less than 5); a modification or terminal T present on the surface of the layer body (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom).

Description

Technical Field

[0001] The present invention relates to a virus inactivation liquid and a virus inactivation article. Background Art

[0002] Various antimicrobial agents and articles using them are known. For example, Patent Document 1 discloses an antimicrobial sheet that uses silver as the active ingredient and comprises an antimicrobial layer containing the antimicrobial agent and a binder (the binder alone has a water contact angle of 20° or less) disposed on a substrate. Patent Document 1 describes the appropriate use of an antimicrobial agent that exhibits a bactericidal effect against pathogenic bacteria, such as Staphylococcus aureus and Escherichia coli.

[0003] On the other hand, it is known that virus-inactivating liquids contain alcohols such as ethanol and 2-propanol as active ingredients. The WHO (World Health Organization) recommends a formulation for hand sanitizers with an alcohol concentration of 80% by volume ethanol or 75% by volume 2-propanol. However, reports indicate that formulations with alcohol concentrations lower than these can also achieve virus inactivation. For example, Non-Patent Document 1 reports that a formulation with a concentration of 30% by volume of ethanol or 2-propanol can also achieve virus inactivation against SARS-CoV-2 (the so-called "new coronavirus").

[0004] Prior art literature

[0005] Patent Literature

[0006] Patent Document 1: International Publication No. 2016 / 047568

[0007] Patent Document 2: International Publication No. 2017 / 083055

[0008] Non-patent literature

[0009] Non-patent document 1: Annika Kratzel, et al., "Inactivation of Severe AcuteRespiratory Syndrome Coronavirus 2 by WHO-Recommended Hand Rub Formulationsand Alcohols", Emerging Infectious Diseases, 2020, Vol. 26, Issue 7, pp. 1592-1595 Summary of the Invention

[0010] Problems to be solved by the invention

[0011] In recent years, MXene has attracted attention as a new material. MXene is a so-called two-dimensional material. As described later, it is a layered material with one or more layers. Generally, MXene takes the form of particles (including powders, flakes, nanosheets, etc.) of these layered materials.

[0012] Patent Document 2 discloses an antimicrobial agent containing MXene and an antimicrobial film formed by coating this antimicrobial agent on a polyvinylidene fluoride (PVDF) substrate. Patent Document 2 states that this antimicrobial agent exhibits antimicrobial effects against Escherichia coli (E. coli) and Bacillus subtilis (B. subtilis).

[0013] As is known to all, bacteria are single-cell organisms, are micron-sized, and can reproduce on their own. In contrast, viruses are composed of nucleic acids (genetic factors) and capsids, and sometimes also envelopes, are nanometer-sized, cannot reproduce on their own, and must parasitize cells (hosts) to reproduce. In this way, bacteria and viruses are completely different at least in terms of structure, size, and reproduction mechanism. Even if a substance exhibits an antibacterial effect, it is impossible to judge whether the substance will show a virus inactivation effect based on this alone. In fact, in Patent Documents 1 and 2, there is no mention of viruses. Antibacterial properties can be evaluated in accordance with JIS Z 2801, for example, as described in Patent Document 1. There is no specific standard for virus inactivation ability, but for example, as described in Non-Patent Document 1, it can be evaluated based on TCID 50 Method for evaluation.

[0014] There are many different types of viruses, and preventing the spread of infectious diseases caused by viruses has become an extremely important issue internationally. In this context, the demand for new virus inactivation solutions and products is increasing.

[0015] The object of the present invention is to provide a novel virus inactivation liquid and virus inactivation article.

[0016] Means of solving the problem

[0017] As a result of the inventors' dedicated research, they independently discovered that MXene has the ability to inactivate viruses, which led to the completion of the present invention.

[0018] According to a first aspect of the present invention, there is provided a virus inactivation liquid comprising a liquid medium and particles comprising one or more layers of a layered material.

[0019] The layers include:

[0020] By the following formula: M m X nA layer body represented by (wherein, M is at least one metal of Groups 3, 4, 5, 6, or 7, X is a carbon atom, a nitrogen atom, or a combination thereof, n is 1 to 4, and m is greater than n and 5 or less);

[0021] The modification or terminal T present on the surface of the layer body (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom).

[0022] In one embodiment of the first aspect of the present invention, the M m X n It can be Ti3C2.

[0023] In one embodiment of the first aspect of the present invention, the average thickness of the particles may be 10 nm or less.

[0024] In one embodiment of the first aspect of the present invention, the liquid medium may include at least one of water and alcohol.

[0025] In one embodiment of the first aspect of the present invention, the virus inactivating liquid 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.

[0026] In one embodiment of the first aspect of the present invention, the content of the particles in the virus inactivating liquid may be 0.5 mg / mL or more and 100 mg / mL.

[0027] In one embodiment of the first aspect of the present invention, the pH of the liquid medium may be 2.7 or more and 7.0 or less.

[0028] In one embodiment of the first aspect of the present invention, the content of Li in the particles may be 20 mass ppm or less.

[0029] In one embodiment of the first aspect of the present invention, the total content of chlorine and bromine in the particles may be 1500 ppm by mass or less.

[0030] In one embodiment of the first aspect of the present invention, the particles may support at least one of a metal and a metal oxide. For example, the particles may support titanium oxide.

[0031] According to the second aspect of the present invention, there is provided a virus inactivation article, comprising:

[0032] substrate;

[0033] a virus inactivation layer disposed on the substrate,

[0034] The virus inactivating layer comprises particles of a layered material having one or more layers,

[0035] The layers include:

[0036] By the following formula: M m X n A layer body represented by (wherein, M is at least one metal of Groups 3, 4, 5, 6, or 7, X is a carbon atom, a nitrogen atom, or a combination thereof, n is 1 to 4, and m is greater than n and 5 or less);

[0037] The modification or terminal T present on the surface of the layer body (T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom).

[0038] In one embodiment of the second aspect of the present invention, the substrate may be any one selected from the group consisting of filters, masks, protective masks, bandages, gloves, protective clothing, touch screens, displays, films, and seals.

[0039] In one embodiment of the second aspect of the present invention, the M m X n It can be Ti3C2.

[0040] In one embodiment of the second aspect of the present invention, the average thickness of the particles may be 10 nm or less.

[0041] In one embodiment of the second aspect of the present invention, the virus-inactivated product 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.

[0042] In one embodiment of the second aspect of the present invention, the content of Li in the particles may be 20 mass ppm or less.

[0043] In one embodiment of the second aspect of the present invention, the total content of chlorine and bromine in the particles may be 1500 ppm by mass or less.

[0044] In one embodiment of the second aspect of the present invention, the particles may support at least one of a metal and a metal oxide. For example, the particles may support titanium oxide.

[0045] Effects of the Invention

[0046] According to the present invention, a virus-inactivating liquid and a virus-inactivating layer of a virus-inactivating article contain particles of a predetermined layered material (also referred to herein as "MXene"), thereby enabling virus inactivation. Thus, the present invention provides a novel virus-inactivating liquid and virus-inactivating article. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 11 and 2 are schematic cross-sectional views showing MXene as a layered material that can be used in one embodiment of the present invention. (a) shows a single-layer MXene, and (b) shows a multi-layer (for example, a double-layer) MXene.

[0048] Figure 2 The figures illustrate a virus inactivation article according to one embodiment of the present invention. (a) shows a schematic cross-sectional view of the virus inactivation article, and (b) shows a schematic perspective view of a layered material of a virus inactivation layer of the virus inactivation article.

[0049] Figure 3 These are SEM photographs showing the progress of partial oxidation in the heat treatment (oxidation treatment) of Example 2, (a) is a SEM photograph of the solid component (particles) before the treatment, and (b) is a SEM photograph of the solid component (particles) after the treatment. DETAILED DESCRIPTION

[0050] (Implementation 1: Virus Inactivation Liquid)

[0051] Hereinafter, a virus inactivating liquid according to one embodiment of the present invention will be described in detail, but the present invention is not limited to this embodiment.

[0052] The virus inactivating liquid of this embodiment includes a liquid medium and particles of a predetermined layered material.

[0053] The specified layered material that can be used in this embodiment is MXene, which is specified as follows:

[0054] A layered material containing one or more layers (which can be understood as a layered compound, also represented by "M m X n T s ", s is an arbitrary number. In the past, x was sometimes used instead of s). This layer includes:

[0055] By the following formula: M m X n (wherein M is at least one Group 3, 4, 5, 6, or 7 metal, 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; and m is greater than n and 5 or less.) A layer body (the layer body may have a lattice in which each X is located within an octahedral array of M); and a modified 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 a surface of the layer body (more specifically, on at least one of two opposing surfaces of the layer body). Typically, n is 1, 2, 3, or 4, but is not limited thereto.

[0056] In the above formula of 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.

[0057] It is known that Mxene is represented by the above formula: M m X n , expressed as follows.

[0058] 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.)

[0059] Ti3C2, Ti3N2, Ti3(CN), Zr3C2, (Ti, V)3C2, (Ti2Nb)C2, (Ti2Ta)C2, (Ti2Mn)C2, Hf3C2 , (Hf2V)C2, (Hf2Mn)C2, (V2Ti)C2, (Cr2Ti)C2, (Cr2V)C2, (Cr2Nb)C2, (Cr2Ta)C2, (Mo2 Sc)C2, (Mo2Ti)C2, (Mo2Zr)C2, (Mo2Hf)C2, (Mo2V)C2, (Mo2Nb)C2, (Mo2Ta)C2, (W2Ti)C2, (W2Zr)C2, (W2Hf)C2,

[0060] 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

[0061] Typically, in the above formula, M can be titanium or vanadium, and X can be a carbon atom or a nitrogen atom. For example, 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). m X n It is Ti3C2.

[0062] Such MXene particles (hereinafter, simply referred to as “MXene particles”) can be synthesized by selectively etching (removing and, if necessary, performing layer separation) A atoms (and, if necessary, a portion of M atoms) from the MAX phase.

[0063] MAX phase, by the following formula: M m AX n (wherein, M, X, n and m are as described above, A is at least one element of Groups 12, 13, 14, 15 and 16, usually an element of Group A, typically an element of Group IIIA and Group IVA, and more specifically may include at least one selected from the group consisting of Al, Ga, In, Tl, Si, Ge, Sn, Pb, P, As, S and Cd, preferably Al), and having a layer consisting of A atoms located between M m X n The MAX phase typically has a crystal structure between two layers (each X may have a lattice located within the octahedral array of M) when m=n+1. In the case of m=n+1, a MAX phase typically has a repeating unit in which a layer of X atoms is arranged one layer between each layer of n+1 layers of M atoms (these layers are collectively referred to as "M m X n The A-atom layer is a layer of A atoms ("A-atom layer") arranged as a layer next to the n+1-th M-atom layer, but the present invention is not limited thereto. By selectively etching (removing and, if necessary, performing layer separation) the A atoms (and, if necessary, a part of the M atoms) from the MAX phase, the A-atom layer (and, if necessary, a part of the M atoms) is removed, and the hydroxyl groups, fluorine atoms, chlorine atoms, oxygen atoms, etc. present in the etching solution (usually, an aqueous solution containing fluorine acid is used, but the present invention is not limited thereto) are oxidized to the exposed M atoms. m X n The surface of the layer is modified, with such a surface serving as the end.

[0064] The etching is carried out using a fluorine resin container and an acid such as HF, HCl, HBr, HI, sulfuric acid, phosphoric acid, or nitric acid. － The etching may be carried out using an etching solution such as a mixed solution of lithium fluoride and hydrochloric acid or a method using hydrofluoric acid.

[0065] If necessary, any suitable metal (e.g., Li) can be inserted between the MXene layers (intercalation). The intercalation treatment can be performed separately after the etching treatment or simultaneously with the etching treatment.

[0066] Thereafter, the layer separation (stratification, separating multilayer MXene into single-layer MXene) of MXene can be promoted by any appropriate post-treatment (such as ultrasonic treatment, manual shaking or automatic shaker, etc.). For example, a mechanical oscillator, a vortex mixer, a homogenizer, an ultrasonic bath, etc. can be used to perform a stratification treatment for a specified time. Then, the supernatant is separated from the precipitate by a centrifugal separator, and the recovered supernatant can be obtained as a dispersion of monolayered MXene particles. In addition, during ultrasonic treatment, if the shear force is too large, the MXene may be broken. Therefore, if you want to obtain MXene particles with a two-dimensional shape with a larger aspect ratio (preferably single-layer MXene particles), it is preferred to apply appropriate shear force by manual shaking or an automatic shaker.

[0067] Furthermore, in the present invention, MXene particles may contain a relatively small amount of residual A atoms, for example, 10% by mass or less relative to the original A atoms. The residual A atom content is preferably 8% by mass or less, and more preferably 6% by mass or less. However, even if the residual A atom content exceeds 10% by mass, it may not be a problem depending on the application and conditions of viral inactivation.

[0068] The MXene particles 10 synthesized in this way, such as Figure 1 Schematically, particles of layered materials (e.g., MXene particles 10, in FIG. Figure 1 (a) shows a single layer of MXene particles 10a. Figure 1 (b) shows two layers of MXene particles 10b, but is not limited to these examples). More specifically, the MXene layers 7a and 7b have: m X n The layer body represented by m X n Layers) 1a, 1b; modified or terminal T 3a, 5a, 3b, 5b present on the surface of the layer bodies 1a, 1b (more specifically, at least one of the two surfaces facing each other of each layer). Therefore, MXene layers 7a, 7b are also represented as "MXene". m X n T s ”, s is an arbitrary number. The MXene particle 10 may be such that each MXene layer is separated and exists as one layer ( Figure 1The single-layer structure shown in (a), so-called single-layer MXene particles 10a), can also be a stacked structure in which multiple MXene layers are separated from each other ( Figure 1 The multilayer structure shown in (b), the so-called multilayer MXene particles 10b), can also be a mixture thereof. The MXene particles 10 can be particles (also referred to as powder or flakes) as an aggregate composed of single-layer MXene particles 10a and / or multi-layer MXene particles 10b. In the case of multi-layer MXene particles, the two adjacent MXene layers (for example, 7a and 7b) do not have to be completely separated, but can be partially in contact. In this embodiment, as described later, the MXene particles 10 preferably have as many single-layer MXene particles as possible than multi-layer MXene particles (the content ratio of single-layer MXene particles is high).

[0069] Although not limiting to the present embodiment, the thickness of each layer of the MXene particles (equivalent to the above-mentioned MXene layers 7a and 7b) is, for example, not less than 0.8 nm and not more than 5 nm, and in particular can be not less than 0.8 nm and not more than 3 nm (mainly due to the number of M atomic layers contained in each layer), and the maximum size in a plane parallel to the layer (two-dimensional unfolded surface) is, for example, not less than 0.1 μm and not more than 200 μm, and in particular not less than 1 μm and not more than 40 μm.

[0070] When the MXene particles are laminated (multilayer MXene) particles, the interlayer distance (or gap size) of a single laminate is Figure 1 (represented by Δd in (b)), for example, is greater than 0.8 nm and less than 10 nm, particularly greater than 0.8 nm and less than 5 nm, more particularly is about 1 nm, and the maximum size in a plane perpendicular to the stacking direction (two-dimensional development surface) is, for example, greater than 0.1 μm and less than 100 μm, particularly greater than 1 μm and less than 20 μm.

[0071] The total number of layers of MXene particles may be 1 or 2 or more, for example, 1 or more and 100,000 or less, particularly 1,000 or more and 20,000 or less, and the thickness in the stacking direction may be, for example, 0.1 μm or more and 200 μm or less, particularly 1 μm or more and 40 μm or less.

[0072] When the MXene particles are laminated (multi-layer MXene) particles, MXene particles with a small number of layers are preferred. The term "small number of layers" refers to, for example, MXene particles with a stacking number of 6 or fewer layers. In addition, the thickness of the multi-layer MXene particles with a small number of layers in the stacking direction is preferably 10 nm or less. In this specification, this "multi-layer MXene with a small number of layers" (multi-layer MXene in a narrow sense) is also referred to as "few-layer MXene."

[0073] In this embodiment, the MXene particles are preferably particles (also referred to as nanosheets) whose majority is composed of single-layer MXene and / or few-layer MXene. In this specification, single-layer MXene and few-layer MXene are collectively referred to as "single-layer / few-layer MXene."

[0074] 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, considering the thickness of a single layer of MXene particles, the lower limit of the thickness of the MXene particles can be 1.0 nm. Therefore, the average thickness of the MXene particles can be 1 nm or more.

[0075] 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 the entire MXene particles is preferably 90% by volume or more, more preferably 95% by volume or more.

[0076] In addition, the above-mentioned dimensions can be obtained as the number average size (for example, the number average of at least 40) based on scanning electron microscope (SEM), transmission electron microscope (TEM) or atomic force microscope (AFM) photographs, or as the distance in real space calculated based on the position in the reciprocal lattice space of the (002) plane measured by the X-ray diffraction (XRD) method.

[0077] On the other hand, the liquid medium can use any appropriate liquid. For example, the liquid medium can be an aqueous medium. The aqueous medium is typically water, and depending on the circumstances, it can also contain other liquid substances other than water in a smaller amount (for example, 30% by mass or less, preferably 20% by mass or less, based on the overall standard of the aqueous medium). The liquid medium can be understood as a dispersion medium that can disperse MXene particles. Solutes such as ions can also be dissolved in the liquid medium.

[0078] For example, the liquid medium may also 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 and may be, for example, methanol, ethanol, or propanol (1-propanol, 2-propanol). When a water-soluble / miscible alcohol (such as methanol, ethanol, or propanol) is used in the water-alcohol mixture, the alcohol content relative to the total liquid medium is not particularly limited and may be appropriately selected based on the intended use of the virus inactivation solution.

[0079] In the use of viral inactivation liquids, when flammability / ignition risk is a concern, the liquid medium is preferably water, or a mixture of water and a relatively small amount of alcohol, with water being more preferred. Water is non-flammable and does not present the same flammability / ignition risk as alcohol. In contrast, conventional alcohol-based disinfectants (such as ethanol, which contain alcohols as active ingredients) have ignition points within the normal temperature range, although this varies depending on the type and concentration of the alcohol, posing a fire risk if there is an ignition source.

[0080] The virus inactivation liquid of this embodiment may also contain other ingredients. For example, the virus inactivation liquid may also 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 improve the dispersibility of the MXene particles in the liquid medium. The purpose of adding the binder is to improve the adhesion strength between the MXene particles and the object (the substrate in the case of embodiment 2 described later) after the virus inactivation liquid is applied to the object and dried (at least partially remove the liquid medium), or to improve the strength of the virus inactivation layer itself formed by the virus inactivation liquid. The antioxidant may be added when it is desired to prevent the oxidation of the MXene particles (more specifically, the oxidation of the metal (M) constituting the MXene layer). The viscosity modifier can be added to adjust the viscosity of the virus inactivation liquid. More specific examples of the additive include polyurethane (PU), polyvinyl alcohol (PVA), polyethylenedioxythiophene (PEDOT), sodium alginate (SA), polyamide resins (such as nylon), epoxy resins, acrylic resins, sodium hexametaphosphate, and polyacrylamine.

[0081] Such other components can be added / mixed at any appropriate time during the preparation of the viral inactivation liquid. For example, the other components can be added to a mixture containing the synthesized MXene particles in a liquid medium (typically a slurry), or can be added to the synthesized MXene particles (typically in a clay or powder form) along with the liquid medium.

[0082] The virus inactivation liquid of this embodiment contains MXene particles with virus inactivation ability as an active ingredient. The ability of MXene particles to inactivate viruses is an independent discovery made by the present inventors. Although the present invention is not bound by any theory, the mechanism by which MXene particles inactivate viruses is considered to be as follows. MXene particles, in the presence of MXene particles, m X nThe surface of the layer body represented has a modification or terminal T (T is at least one selected from the group consisting of hydroxyl groups, fluorine atoms, chlorine atoms, and oxygen atoms), and there are charged (negative or positive) sites under this structure. Although it does not limit the present invention, specifically, the MXene particles are partially negatively charged in the plane (two-dimensional unfolded surface) parallel to the layer, and are positively charged at the ends of the layer of the MXene particles. Generally speaking, viruses also have an electric charge (such as a positive charge), and are thus adsorbed on sites with opposite charges (such as negative charges) present on the MXene particles under the action of Coulomb force. Since MXene particles are conductive, if the virus is adsorbed on the above-mentioned sites of the MXene particles, the virus is electrically neutralized, resulting in the virus being immediately inactivated.

[0083] The mechanism by which MXene particles inactivate viruses is fundamentally different from the mechanism by which MXene particles exhibit an antimicrobial effect (inhibiting bacterial growth). Bacteria are of comparable or larger size than MXene particles. Therefore, the bacteria are surrounded by multiple MXene particles (rather than being adsorbed to the particles like viruses). In this state, the effect of the specific sites of MXene particles on bacteria is significantly smaller than that on viruses. Furthermore, because bacteria have cell walls and cell membranes, being surrounded by multiple MXene particles does not immediately prevent their growth. Instead, it inhibits their life-sustaining activities, such as nutrient uptake, and slows their growth.

[0084] Based on the aforementioned mechanism of virus inactivation by MXene particles, it is conceivable that a larger specific surface area of MXene particles increases the probability of contact with viruses, resulting in a higher viral inactivation effect. While not limiting to this embodiment, from this perspective, 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.

[0085] Viruses are not particularly limited. Viruses are composed of nucleic acids (genetic factors) and capsids, and sometimes also envelopes. Generally speaking, they have nanoscale dimensions, for example, they can be tens to hundreds of nm in size. Examples of enveloped viruses (viruses with an envelope) include SARS-CoV-2 (the so-called "new coronavirus"), influenza virus, herpes virus, rubella virus, hepatitis B virus, hepatitis C virus, HIV, etc. Examples of non-enveloped viruses (viruses without an envelope) include norovirus, rotavirus, poliovirus, adenovirus, etc. In addition, in the evaluation test of virus inactivation ability, feline calicivirus can be used as an alternative to norovirus.

[0086] In the present invention, the term "inactivation of viruses" (or inactivation of viruses) means that the virus loses its infectivity, which can also be expressed as "antiviral". Specifically, TCID 50 When evaluating viral infectivity titers, if the viral infectivity titer is below the detection limit, it can be considered that "virus inactivation" has been achieved. It can be understood that the shorter the exposure time required for the viral infectivity titer to fall below the detection limit, the higher the viral inactivation ability (the ability to inactivate the virus).

[0087] In the present invention, the term "liquid" refers to an agent that is generally liquid. A liquid agent can be a dispersion (or suspension) of MXene particles dispersed (or suspended) in a liquid medium. Depending on how the viral inactivation liquid agent is used, it can be, for example, a sprayable slurry or a dispensable gel.

[0088] The virus-inactivating liquid of this embodiment has a high virus-inactivating ability, for example, it can inactivate viruses in one minute or less. Furthermore, the virus-inactivating liquid of this embodiment contains MXene particles as an active ingredient. Therefore, after the virus-inactivating liquid is applied to an object, even if the liquid medium evaporates after exposure to air, the MXene particles can remain on the surface of the object, exerting a sustained virus-inactivating effect for a long time, for example, even after 24 hours. In contrast, conventional alcohol-based disinfectants fail to achieve virus-inactivating effects if the alcohol evaporates.

[0089] The virus inactivation liquid of this embodiment exhibits a sufficient virus inactivation effect even when the content of MXene particles, the active ingredient, is low. The content of MXene particles in the virus inactivation liquid is, for example, 0.5 mg / mL or greater, preferably 1 mg / mL or greater, and more preferably 5 mg / mL or greater. The upper limit of the MXene particle content in the virus inactivation liquid can be appropriately selected based on, for example, the intended use of the virus inactivation liquid. However, if a dilute virus inactivation liquid is desired, the above content is, for example, 100 mg / mL or less, 50 mg / mL or less if necessary, and 10 mg / mL or less if further desired.

[0090] In the virus inactivation liquid of this embodiment, the pH value of the liquid medium can be appropriately selected according to the characteristics and uses required for the virus inactivation liquid, for example, from 2.7 to 7.0. In the pH value region of from 2.7 to 7.0, the MXene particles can be stably dispersed in the liquid medium, which can prevent or reduce the aggregation and / or sedimentation of the MXene particles. Dispersion stability is important in obtaining the desired virus inactivation effect uniformly using the virus inactivation liquid (applied to the object) and / or in the virus inactivation liquid (or the virus inactivation layer formed therewith, etc.) as a whole. In order to achieve higher dispersion stability for MXene particles, the pH value of the liquid medium is preferably from 2.7 to 6.0.

[0091] In particular, it is preferred that the pH value of the liquid medium is 3.0 or more and 5.0 or less. In the pH range of 3.0 or more and 5.0 or less, in addition to obtaining high dispersion stability for the MXene particles, the virus inactivation effect can be continuously exerted for a longer period of time. Although the present invention is not bound by any theory, in the pH range of 3.0 or more and 5.0 or less, the oxidation stabilization of the MXene particles can be considered to obtain the above-mentioned effect. When the pH value is lower than the neutral range, the MXene particles will hydrolyze from the end of the MXene layer, and then, the oxide of the metal (M) constituting the MXene layer will be produced (for example, if it is composed of Ti3C2T s MXene particles represented by , TiO2 will be generated, and CH4 and / or amorphous carbon will be generated as by-products). That is, in the MXene particles, the MXene layer of the main body is m X n It cannot be maintained and chemical decomposition occurs, and it is covered by the oxide of the above-mentioned metal (M) (hereinafter, this partial oxidation is referred to as "partial oxidation"). In MXene particles, even if partial oxidation occurs to a certain extent, the sites of the MXene particles with the above-mentioned charge will not be completely lost, so the effect of virus inactivation will not disappear significantly. In the pH value range of 3.0 to 5.0, although partial oxidation of MXene particles occurs to a certain extent, because the oxidation is stable (in other words, apparently, it is a state where oxidation is not actually carried out), it is possible to prevent the virus inactivation effect from completely disappearing, and the effect can be continuously exerted for a longer time at a sufficient level of virus inactivation. In addition, as mentioned above, due to the oxidation stability, it can be considered that the decomposition of MXene particles does not appear to proceed, which also helps to obtain high dispersion stability.

[0092] From another perspective, strong acidity is not preferred in practical use of virus inactivation liquids. In such cases, the pH of the liquid medium can be 3.0 to 7.0 (weakly acidic pH = 3.0 to 6.0 or below, or neutral pH = above 6.0 to 7.0 or below).

[0093] The pH value of the liquid medium can be adjusted by the type and concentration of ions dissolved in the liquid medium. Although not limiting the present embodiment, for example, the pH value of the liquid medium in the virus inactivation liquid obtained thereafter (representatively, the slurry after layering) can be adjusted according to the processing conditions of etching and / or intercalation (e.g., the type and feed concentration of acid and / or alkali). As mentioned above, the intercalation treatment can be performed separately after the etching treatment or together with the etching treatment. In addition, for example, when the synthesized MXene particles (representatively, clay or powder obtained by separation as a solid component after washing with water) are mixed with the liquid medium, the pH value of the liquid medium can be pre-adjusted.

[0094] In the virus inactivation liquid of this embodiment, the Li content in the MXene particles is preferably 20 ppm by mass or less. While the presence of relatively large amounts of Li can affect living organisms, the virus inactivation liquid of this embodiment, with a Li content of 20 ppm by mass or less in the MXene particles, exhibits high biocompatibility. The lower limit of the Li content in the MXene particles is not particularly limited and can be 0.

[0095] For example, when Li intercalation is performed, the Li content in the MXene particles can be suppressed to 20 mass ppm or less. In this case, the Li content in the MXene particles can be, for example, 1 mass ppm or more.

[0096] The virus inactivation liquid in which the Li content is suppressed during Li intercalation can be produced, for example, by the following first production method or second production method.

[0097] A first method for producing a virus inactivating liquid comprises:

[0098] (a) a step of preparing a precursor consisting of a MAX phase,

[0099] (b1) performing an etching treatment using an etching solution to remove at least a portion of the A atoms from the precursor

[0100] (c) performing a Li intercalation treatment including a step of mixing and stirring the etched product obtained by the etching treatment and a Li-containing compound;

[0101] (d) performing a step of performing a layer separation process including centrifuging the Li intercalation product obtained by the Li intercalation process, discarding the supernatant, and washing the remaining precipitate with water,

[0102] (e) performing an acid treatment step comprising mixing and stirring the layered product obtained through the layering treatment with an acid solution,

[0103] (f) washing the acid-treated product obtained by the acid treatment with water to obtain MXene particles, and

[0104] (g) The step of mixing the obtained MXene particles with a liquid medium to obtain a virus inactivation liquid.

[0105] According to this production method, a virus inactivating liquid having a Li content of 0.0020 mass % (20 mass ppm) or less in MXene particles can be produced.

[0106] The second method for producing a virus-inactivating liquid comprises:

[0107] (a) a step of preparing a precursor consisting of a MAX phase,

[0108] (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 treatment,

[0109] (d) performing a demixing step comprising centrifuging the (etching + Li intercalation) product obtained by the etching and Li intercalation treatments, discarding the supernatant, and then washing the remaining precipitate with water,

[0110] (e) performing an acid treatment step comprising mixing and stirring the demixed product obtained through the demixing step with an acid solution,

[0111] (f) washing the acid-treated product obtained by the acid treatment with water to obtain MXene particles, and

[0112] (g) The step of mixing the obtained MXene particles with a liquid medium to obtain a virus inactivation liquid.

[0113] According to this production method, a virus inactivating liquid having a Li content of 0.0020 mass % (20 mass ppm) or less in MXene particles can be produced.

[0114] Hereinafter, each step of the first and second production methods will be described in detail, and the step (a) and steps (d) to (g) common to these two production methods will be summarized and described.

[0115] Process (a)

[0116] First, a precursor composed of a MAX phase is prepared. The MAX phase is as described above. The precursor may contain trace amounts of impurities that are inevitably mixed in addition to the MAX phase.

[0117] Process (b1)

[0118] In the first manufacturing method, an etching treatment is performed using an etching solution to remove at least a portion of the A atoms from the precursor. The etching conditions are not particularly limited, and known conditions can be used. － Examples of etching solutions include methods using hydrofluoric acid, methods using a mixture of lithium fluoride and hydrochloric acid, and methods using an etching solution further containing phosphoric acid or the like. Among these methods, methods using a mixture with pure water as a solvent are also possible. Examples of the etched product obtained through the above etching treatment include slurries.

[0119] Process (c)

[0120] A Li intercalation treatment is performed including a step of mixing and stirring the etched product obtained through the etching treatment with a Li-containing compound.

[0121] Examples of Li-containing compounds include metal compounds containing Li ions. Examples of Li-containing metal compounds include ionic compounds in which Li ions are bonded to cations. Examples include Li ion iodides, phosphates, sulfide salts containing sulfates, nitrates, acetates, and carboxylates.

[0122] The content of the Li-containing compound in the intercalation complex is preferably 0.001% by mass or greater. This content is more preferably 0.01% by mass or greater, and even more preferably 0.1% by mass or greater. On the other hand, from the perspective 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.

[0123] In step (c), for example, the slurry obtained by the etching treatment in the above step (b1) is subjected to repeated centrifugation, removal of the supernatant, addition of pure water to the remaining precipitate, and re-centrifugation to wash the obtained MXene aqueous medium clay as the etched product, which is then subjected to intercalation treatment.

[0124] The specific method of the intercalation treatment is not particularly limited. For example, a Li-containing compound may be mixed with the clay as the aqueous medium of the MXene, and the mixture may be stirred at room temperature.

[0125] In the second manufacturing method, as described below, in step (b2), etching treatment of the precursor and Li intercalation treatment are performed together.

[0126] Process (b2)

[0127] In the second manufacturing method, at least a portion of the A atoms (and optionally a portion of the M atoms) is etched (removed and optionally layer-separated) from the precursor using an etching solution containing a Li-containing compound, and Li intercalation treatment is performed.

[0128] In step (b2), Li intercalation treatment is performed, that is, when at least a part of the A atoms (and a part of the M atoms as needed) is etched (removed and layer-separated as needed) from the MAX phase, m X n Li ions are inserted between the layers.

[0129] The content of the Li-containing compound in the etching solution is preferably 0.001% by mass or greater. This content is more preferably 0.01% by mass or greater, and even more preferably 0.1% by mass or greater. On the other hand, from the perspective 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.

[0130] The etching solution of step (b2) may include a Li compound. The composition of the etching solution other than the Li compound is not particularly limited and known conditions can be used. For example, as described in step (b1), a solution containing F can be used. － Examples of etching methods include methods using hydrofluoric acid, methods using a mixture of lithium fluoride and hydrochloric acid, and methods using an etching solution containing phosphoric acid or the like. Among these methods, methods using a mixture of pure water as a solvent include methods. Examples of the etched product obtained through the above etching process include slurries.

[0131] Of the first and second production methods, the first production method, which is divided into the step (b1) etching treatment and the step (c) Li intercalation treatment, is preferred because it is easier to form a single layer of MXene.

[0132] Process (d)

[0133] A layered treatment is performed, which includes centrifuging the Li intercalation treated product obtained by the Li intercalation treatment of the first manufacturing method, or the (etching + Li intercalation) treated product obtained by the etching and Li intercalation treatment of the second manufacturing method, and after discarding the supernatant, washing the remaining precipitate with water. The conditions for the layered treatment are not particularly limited and can be performed using known methods. For example, it can be performed by the method shown below.

[0134] For example, as a process for centrifuging a slurry-like Li intercalation treated product or a (etching + Li intercalation) treated product, discarding the supernatant, and washing the remaining precipitate with water, the following steps can be listed: (i) adding pure water to the remaining precipitate after discarding the supernatant for stirring, (ii) performing centrifugal separation, and (iii) recovering the supernatant. The operations (i) to (iii) are repeated once or more, preferably more than twice and less than 10 times, to obtain a monolayer and few-layer MXene supernatant before acid treatment as a layered treated product. Alternatively, the supernatant can be centrifuged, the supernatant after centrifugation discarded, and a monolayer and few-layer MXene clay before acid treatment can be obtained as a layered treated product.

[0135] Process (e)

[0136] Acid treatment is performed, which includes a process of mixing and stirring the stratified product obtained by the stratification treatment (containing a supernatant containing a single layer or few layers of MXene or a clay containing a single layer or few layers of MXene) and an acid solution. The acid used for the above-mentioned acid treatment is not limited, for example, inorganic acids such as mineral acids, and / or organic acids can be used. The acid is preferably only an inorganic acid, or a mixed acid of an inorganic acid and an organic acid. The acid is more preferably only an inorganic acid. As the above-mentioned 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. As the above-mentioned organic acid. For example, acetic acid, citric acid, oxalic acid, benzoic acid, sorbic acid, etc. can be listed. The concentration of the acid solution mixed with the stratified product can be adjusted according to the amount and concentration of the stratified product to be treated.

[0137] The above-described layered product is mixed with the acid solution and stirred. Examples of stirring methods include manual shaking, automatic shaking, shear mixers, ball mills, and the like. The degree of stirring, such as the stirring speed and time, can be adjusted based on the amount and concentration of the layered product being treated.

[0138] The acid solution may be stirred without heating or heated while stirring at a temperature of 80°C or less.

[0139] After the above stirring, for example, centrifugation is performed to remove the supernatant, and an acid-treated product can be obtained as a slurry. The operation of mixing and stirring with the above-mentioned acid solution can be performed more than once. From the viewpoint of further reducing the Li content in the MXene particles, it is preferred that the operation of mixing and stirring with the above-mentioned acid solution is performed more than twice, for example, within a range of 10 times or less. As a method of performing the operation of mixing and stirring with the above-mentioned acid solution multiple times, there can be listed the steps of mixing and stirring (i) (the layered treated product or the remaining precipitate obtained by the following (iii)) with the solution, (ii) centrifuging the stirred product, and (iii) discarding the supernatant after centrifugation, and performing the steps (i) to (iii) more than twice, for example, within a range of 10 times or less.

[0140] The pH of the acid-treated product obtained by the above-mentioned acid treatment is preferably 2.5 or less. The pH is more preferably 2.0 or less, further 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 generally around 1.0. If the pH of the acid-treated product becomes very low, the dispersibility of the MXene particles will decrease, making the MXene particles difficult to handle in subsequent steps. However, according to this method, this problem can be eliminated by water washing in the next step.

[0141] In the present invention, since Li is actively removed by performing acid treatment as described above, the Li content in the MXene particles can be further reduced.

[0142] Process (f)

[0143] The acid-treated product obtained by acid treatment is washed with water to obtain MXene particles. The amount of water mixed with the acid-treated product and the washing method are not particularly limited. For example, stirring with water and centrifugal separation can be mentioned. As the stirring method, stirring using a hand shake, an automatic shaker, a shear mixer, a ball mill, etc. can be mentioned. The degree of stirring, such as the stirring speed and the stirring time, can be adjusted according to the amount and concentration of the acid-treated product to be treated. The washing with water can be performed more than once. Preferably, the washing with water is performed multiple times. For example, specifically, (i) adding water to (the acid-treated product or the remaining precipitate obtained in (iii) below) for stirring, (ii) centrifuging the stirred product, and (iii) discarding the supernatant after centrifugation can be listed, and the steps (i) to (iii) are performed more than twice, for example, within the range of less than 10 times.

[0144] Process (g)

[0145] The MXene particles obtained in this manner are mixed with a liquid medium to produce a virus inactivation liquid. Details of the liquid medium are described above. If the liquid medium is water, the water used for washing in step (f) (the water used for the last washing in the case of two or more water washings) can also be used as the liquid medium in step (g).

[0146] In the obtained virus inactivation liquid, the pH of the liquid medium can be 2.7 or higher and 7.0 or lower, as described above, preferably 2.7 or higher and 6.0 or lower, and more preferably 3.0 or higher and 5.0 or lower.

[0147] As described above, even when Li intercalation is performed, a virus inactivating solution having a Li content of MXene particles of 20 mass ppm or less can be produced.

[0148] The Li content of 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).

[0149] In the virus inactivation liquid of this embodiment, the combined chlorine and bromine content in the MXene particles is preferably 1500 ppm by mass or less. In industries such as electronic equipment, as part of green procurement, it is required to suppress the chlorine and bromine content of halogens to below a certain level, which is known as "halogen-free." Because the combined chlorine and bromine content in the MXene particles of this embodiment is suppressed, the virus inactivation liquid is suitable for applications requiring halogen-free use. The combined chlorine and bromine content is preferably 900 ppm by mass or less, and most preferably 0 ppm by mass or less. The lower limit of the combined chlorine and bromine content in the MXene particles is not particularly limited and can be 0.

[0150] The virus inactivating liquid in which the total content of chlorine and bromine is suppressed can be produced, for example, by the following third production method.

[0151] A third method for producing a virus-inactivating liquid comprises:

[0152] (a) a step of preparing a precursor consisting of a MAX phase,

[0153] (b3) etching the A atoms from the precursor using an etching solution, wherein the etching solution satisfies at least one condition selected from the group consisting of an H3PO4 concentration of 5.5M or greater, an HI concentration of 5.0M or greater, and an H2SO4 concentration of 5.0M or greater; and

[0154] (g3) A step of mixing the obtained MXene particles with a liquid medium to obtain a virus inactivation liquid.

[0155] Process (a)

[0156] First, a precursor composed of a MAX phase is prepared. This process is the same as that of the first and second manufacturing methods.

[0157] Process (b3)

[0158] The A atoms (and, if necessary, a portion of the M atoms) are etched (removed and, if necessary, layer-separated) from the precursor using an etching solution. The etching solution used is one that satisfies at least one condition selected from the group consisting of an H3PO4 concentration of 5.5 M or greater, an HI concentration of 5.0 M or greater, and an H2SO4 concentration of 5.0 M or greater.

[0159] In step (b3), after etching (removing and, if necessary, performing layer separation) the A atoms (and, if necessary, a part of the M atoms) from the MAX phase, the exposed M atoms m X n The surface of the layer adsorbs and binds PO4 in the etching solution. 3－ , I and SO4 2－ At least one of the groups is selected. Through these PO4 3－ Adsorbed on M m X n The surface of the layer is expanded by using steric hindrance to extend the distance between MXene layers, so that it can be considered that M m X n The van der Waals force between layers is weakened. As a result, it is believed that even for multilayer M m X n The M layer can be easily m X n In addition, since there is no need to apply strong shear, the M m X n The fracture in the plane of the layer results in a single layer of M with a large two-dimensional surface. m X n layer.

[0160] The etching solution does not contain hydrochloric acid, that is, does not contain chlorine atoms. The phrase "does not contain chlorine atoms" in the etching solution means that the chlorine concentration in the etching solution is 10 mass ppm or less, as measured by combustion-ion chromatography, for example.

[0161] The etching solution does not contain hydrochloric acid, but contains 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-containing －The etching solution can be implemented, for example, by using a mixed solution of hydrofluoric acid (HF) and at least one of the above-mentioned predetermined amounts of H3PO4, etc. The concentration of the hydrofluoric acid in the mixed solution can be 1% by mass or more and 50% by mass or less.

[0162] The higher the H3PO4 concentration, HI concentration, and H2SO4 concentration in the etching solution, the better. Therefore, there is no particular upper limit. For example, the H3PO4 concentration can be below 13.2M, the HI concentration can be below 6.5M, and the H2SO4 concentration can be below 16.5M.

[0163] The post-etching process is not particularly limited and can be performed using known methods to obtain MXene particles. For example, the etched slurry can be subjected to repeated centrifugation, removal of the supernatant, addition of pure water to the remaining precipitate, and further centrifugation and washing, followed by intercalation and delamination.

[0164] For example, after step (b3), the above-mentioned steps (c) to (f) may be carried out by the second production method.

[0165] Process (g3)

[0166] The MXene particles obtained in this manner are mixed with a liquid medium to produce a virus-inactivating liquid. Details of the liquid medium are as described above. After step (b3), if steps (c) to (f) are performed, step (g3) can be applied in the same manner as step (g).

[0167] As described above, a virus inactivation solution can be produced in which the combined chlorine and bromine content in the MXene particles is 1500 ppm by mass or less. Following step (b3), performing steps (c) to (f) can reduce the Li content in the MXene particles to 20 ppm by mass or less.

[0168] The contents of chlorine and bromine in MXene particles can be measured by combustion-ion chromatography.

[0169] Furthermore, in the first to third production methods, ultrasonic treatment is not performed after etching for delamination. This avoids particle breakage and allows the production of MXene particles containing single-layer or few-layer MXene with a large two-dimensional surface.

[0170] In the virus inactivation liquid of this embodiment, the MXene particles can carry at least one of a metal and a metal oxide. Thus, depending on the metal and / or metal oxide carried, the virus inactivation ability can be improved and / or other functions (antibacterial properties, catalytic functions, etc.) can be added. The metal constituting the metal or metal oxide can be, for example, Ag. When the MXene particles carry a metal, for example, the MXene particles can be made to carry metal particles. When the MXene particles carry a metal oxide, for example, the MXene particles can be made to carry metal oxide particles, or the metal (M) constituting the MXene layer can be partially oxidized, so that the MXene particles (generated by the above partial oxidation) carry a metal oxide. Whether the MXene particles carry a metal and / or metal oxide can be confirmed by subjecting the particles to X-ray diffraction (XRD) measurement, and in the resulting XRD line shape, peaks unique to MXene and peaks unique to the metal and / or metal oxide can be detected. Peaks unique to MXene can be peaks of the (001) plane of the MXene (l is a natural multiple of 2, i.e., l = 2, 4, 6, 8, 10, 12, etc.), particularly the (002) plane. Detection of peaks unique to metals and / or metal oxides in the XRD line profile indicates that the content of the metal and / or metal oxide (as a whole standard for the metal- and / or metal oxide-supported MXene particles) is at least several mass %.

[0171] For example, MXene particles can carry titanium oxide. By carrying titanium oxide on MXene particles, antibacterial properties can be added to the virus inactivation liquid. In this case, for example, the MXene particles can be made to carry titanium oxide particles, or the Ti constituting the MXene layer can be partially oxidized so that the MXene particles carry titanium oxide (generated by the above partial oxidation). Although not limited to this embodiment, specifically, the above partial oxidation can be carried out in the presence of oxygen, for example, by heating at 60 to 80°C (usually about 70°C) for 50 to 250 hours (usually 70 to 200 hours). Titanium oxide is not particularly limited and can be anatase-type. For example, the MXene particles are Ti3C2T s , so that the Ti contained therein is partially oxidized to generate TiO2, thereby obtaining Ti3C2T loaded with TiO2 s The condition of the particles can be confirmed by subjecting the particles to X-ray diffraction (XRD) measurement and detecting Ti3C2T in the XRD line shape obtained at 2θ=5-8°. s The peak of the unique (002) plane is detected near 2θ=24-26°, which is a peak unique to anatase TiO2.

[0172] While excessive partial oxidation of MXene particles is undesirable from the perspective of dispersion stability, as mentioned above, even with some degree of partial oxidation, the virus inactivation effect is not significantly diminished. By maintaining a moderate degree of partial oxidation, depending on the desired properties and intended use of the virus inactivation solution, both the virus inactivation effect and antimicrobial properties can be achieved.

[0173] (Implementation Method 2: Virus Inactivation Articles)

[0174] Hereinafter, a virus-inactivated article according to one embodiment of the present invention will be described in detail, but the present invention is not limited to this embodiment.

[0175] Reference Figure 2 The virus inactivation article 20 of this embodiment includes:

[0176] substrate 11;

[0177] The virus inactivation layer 13 is arranged on the substrate 11.

[0178] The virus inactivating layer 13 contains particles 10 of a predetermined layered material (MXene).

[0179] The substrate 11 can be any suitable article that is intended to be endowed with a virus inactivation function. The substrate 11 can also be understood as a support that supports the virus inactivation layer 13 .

[0180] The material and form of the substrate 11 are not particularly limited. For example, the substrate 11 can be made of fiber, glass, polymer / polymer composite (resin, plastic, etc.), ceramic, metal, etc.

[0181] For example, the substrate 11 can be any one selected from the group consisting of filters, masks, protective masks, bandages, gloves, protective clothing, touch screens, displays (including monitors), films (including protective films) and seals (stickers). The filter can be a filter used in air purifiers and air conditioners, a filter (diaphragm) used in water purifiers and wastewater treatment equipment, etc. The mask, protective mask, bandage, gloves, protective clothing, touch screens, displays, films and seals can be ordinary. Among them, the mask, protective mask, bandage, gloves, protective clothing, touch screens, displays can be medical (used at medical sites), and are particularly suitable for use in situations where they are easily exposed to viruses. The film and seal can have an adhesive layer on the opposite side of the side having the virus inactivation layer, and can be attached to any other article or other place (such as a touch screen, display, a place where a large number of people can be exposed, etc.) via the adhesive layer. Alternatively, the film can also be without an adhesive layer, for example, it can be a porous film.

[0182] In this embodiment, the virus inactivation layer 13 can be formed using the virus inactivation liquid described in Embodiment 1. More specifically, the virus inactivation article 20 of this embodiment can be manufactured as follows:

[0183] (a) applying a virus inactivation liquid to a substrate 11 to form a precursor of a virus inactivation layer containing MXene particles, and

[0184] (b) The precursor is dried (in other words, the liquid medium is at least partially removed) to form the virus inactivating layer 13 .

[0185] The method of applying the virus inactivating liquid to the substrate 11 in (a) above is not particularly limited, and examples thereof include spraying, spin coating, doctor blade coating, printing, brush coating, and dipping.

[0186] The above steps (a) and (b) may be repeated a total of two or more times until the desired thickness of the virus inactivating layer is obtained.

[0187] Even if the virus inactivation layer 13 is substantially composed of only the MXene particles 10 (and the liquid medium that may remain), in addition to the MXene particles 10 (and the liquid medium that may remain), it may further contain at least one additive (not shown) selected from the group consisting of a dispersant, a binder, an antioxidant, a viscosity modifier, and a fragrance. In addition, in order to achieve a high virus inactivation effect, Figure 2 As shown, when the substrate surface 11a is flat, the MXene particles 10 are preferably oriented as parallel as possible to the substrate surface 11a (arranged flatly) to form the virus inactivation layer 13, but the present invention is not limited thereto. For example, when the substrate surface is not flat (has a large surface roughness), the MXene particles 10 may be oriented along the substrate surface to form the virus inactivation layer 13.

[0188] Thus, the surface 11a of the substrate 11 is covered with the virus-inactivating layer 13. The virus-inactivating layer 13 may cover the entire surface 11a of the substrate, or may cover a portion of the surface 11a. The thickness of the virus-inactivating layer 13 may vary depending on the intended use of the virus-inactivated article 20, and may be, for example, from 0.1 μm to 1 mm.

[0189] According to the virus inactivation article 20 of this embodiment, based on the same mechanism as described in Embodiment 1, MXene particles can inactivate viruses and can continuously exert the virus inactivation effect for a long time.

[0190] Regarding other aspects, unless otherwise described in this embodiment, the same description as in Embodiment 1 can also be applied to this embodiment.

[0191] Example

[0192] (Example 1)

[0193] Example 1 relates to an example of the virus inactivation liquid described in embodiment 1.

[0194] [Preparation of virus inactivation solution]

[0195] In Example 1, as described in detail below, (1) preparation of a precursor (MAX), (2) etching of the precursor, (3) cleaning, (4) layering, and (5) concentration adjustment are performed in sequence to prepare a virus inactivation liquid.

[0196] (1) Preparation of precursor (MAX)

[0197] TiC powder, Ti powder, and Al powder (all manufactured by Kojundo Chemical Laboratory Co., Ltd.) were placed in a ball mill with zirconia balls at a molar ratio of 2:1:1 and mixed for 24 hours. The resulting mixed powder was sintered at 1350°C for 2 hours under an Ar atmosphere. The resulting sintered body (green body) was crushed with an end mill to a maximum size of 40 μm or less. This yielded Ti3AlC2 particles as a precursor (MAX).

[0198] (2) Etching of the precursor

[0199] The Ti 3 AlC 2 particles (powder) prepared by the above method were etched under the following etching conditions to obtain a solid-liquid mixture (slurry) containing a solid component derived from the Ti 3 AlC 2 powder.

[0200] (Etching Conditions)

[0201] Precursor: Ti3AlC2 (passing through a 45 μm sieve)

[0202] Etching solution composition: mixture of 3g LiF and 30mL hydrochloric acid (9 mol / L)

[0203] Precursor input amount: 3.0g

[0204] Etching container: 100mL bottle container

[0205] Etching temperature: 35°C

[0206] Etching time: 24h

[0207] Stirrer speed: 400rpm

[0208] (3) Cleaning

[0209] The slurry was divided into three equal parts and inserted into three 50 mL centrifuge tubes. After centrifugation at a relative centrifugal force (RCF) of 3500G using a centrifuge (so that the clay settles), the supernatant was separated and removed (discarded). 40 mL of pure water was added to each centrifuge tube (where there was a remaining portion after the supernatant was separated and removed), and the centrifugation was repeated at 3500G again to separate and remove the supernatant. The above operation was repeated 11 times. Finally, MXene (Ti3C2T s ) particle-water medium clay.

[0210] (4) Layering

[0211] For the above MXene (Ti3C2T s ) particle-water medium clay was added with 40 mL of pure water, stirred with a shaker for 15 minutes, and then centrifuged at 3500 G to recover the supernatant as a single-layer and few-layer MXene (Ti3C2T s ) particle liquid. Containing single-layer and few-layer MXene (Ti3C2T s ) The average thickness of the MXene particles contained in the particle liquid is greater than 1 nm and less than 10 nm (the same applies to the following embodiments).

[0212] (5) Concentration adjustment

[0213] The above-mentioned monolayer and few-layer MXene (Ti3C2T s ) particle liquid, adjust the concentration of the particles as the solid component to 5 mg / mL, and obtain a virus inactivation liquid.

[0214] According to the above, a 5 mg / mL monolayer and few-layer MXene (Ti3C2T s ) particles of Example 1. The pH of the liquid medium in this virus inactivation liquid was 4.3. Visual observation confirmed that the particles were well dispersed in this virus inactivation liquid without aggregation or sedimentation.

[0215] [Evaluation: Inactivation of enveloped viruses]

[0216] The virus inactivation liquid obtained in Example 1 was used as a sample (test material) to conduct an enveloped virus inactivation test to evaluate its virus inactivation ability. Influenza virus was used as the enveloped virus. The details of the test are as follows.

[0217] (1) Viruses used in the experiment

[0218] Test virus:

[0219] Influenza A virus(H1N1)A / PR / 8 / 34 ATCC VR-1469

[0220] Using cells:

[0221] MDCK (NBL-2) cell line JCRB 9029

[0222] Use culture medium:

[0223] Cell proliferation culture medium

[0224] Eagle MEM medium "Nissui" (1) (Nissui Pharmaceutical Co., Ltd.) supplemented with 10% fetal bovine serum was used.

[0225] Cell maintenance medium

[0226] The following composition was used.

[0227]

[0228] (2) Preparation of virus solution

[0229] Cell culture

[0230] In a cell culture flask, cells are cultured adherently using a cell growth medium.

[0231] Virus inoculation

[0232] After adherent culture, the cell growth medium is removed from the flask and the test virus is inoculated. Then, cell maintenance medium is added and cultured in a carbon dioxide incubator (CO2 concentration: 5%) at 37°C ± 1°C for 1 to 5 days.

[0233] Preparation of virus solution

[0234] After the above-mentioned culture, the morphology of the cells was observed using an inverted phase contrast microscope to confirm the occurrence of morphological changes in the cells (cytopathic effect). Next, the culture solution was centrifuged (3000 rpm, 10 minutes) to separate and recover the supernatant. The obtained supernatant was diluted 10 times with purified water to obtain a virus solution.

[0235] (3) Test operation

[0236] 0.1 mL of the above-mentioned virus solution was added and mixed with 1 mL of a sample (virus inactivation solution) to obtain a mixed solution (hereinafter referred to as "action solution").

[0237] The incubation solution was maintained at room temperature to allow it to incubate. After 1 minute, 5 minutes, 15 minutes, and 24 hours, the incubation solution was diluted 1000-fold with cell maintenance medium and the viral infectivity titer was measured. (In addition, preliminary tests can confirm that the viral infectivity titer can be measured without being affected by the sample by diluting the incubation solution 1000-fold with cell maintenance medium.)

[0238] In addition, the same test was performed using purified water as a control, and the virus infectivity titer was measured at the start (immediately after the start) and 1 minute, 5 minutes, 15 minutes, and 24 hours after the start.

[0239] (4) Measurement of viral infection titer

[0240] In a 96-well tissue culture microplate, adherent cells were cultured using cell growth medium. After the cells had adhered, the medium was removed and 0.1 mL of cell maintenance medium was added to each well. Next, the 100-fold diluted action solution and the control were diluted in 10-fold increments using cell maintenance medium. 0.1 mL of each dilution was inoculated into four wells at each dilution ratio and cultured in a carbon dioxide incubator (CO2 concentration: 5%) at 37°C ± 1°C for 4-7 days.

[0241] After the above culture, the cells were observed for morphological changes (cytopathic effect) using an inverted phase contrast microscope, and the 50% tissue culture infection dose (TCID) was calculated by the Reed-Muench method. 50 ), converted into virus infection titer per 1 mL of the working solution (log 10 TCID 50 / mL).

[0242] Virus infection titer (log 10 TCID 50 The measurement results of % RI / mL are shown in Table 1.

[0243]

Table 1

[0244]

[0245] In the table, “<3.5” means below the detection limit (no viral infection was detected).

[0246] As shown in Table 1, the virus inactivation solution (sample) of Example 1 had a viral infectivity titer below the detection limit just 1 minute after the start of application, confirming its ability to inactivate viruses within a short period of time. Furthermore, the viral infectivity titer of the virus inactivation solution (sample) of Example 1 remained below the detection limit 24 hours after the start of application, confirming its ability to continuously inactivate viruses. This result demonstrates that the virus inactivation solution of Example 1 has a high ability to inactivate enveloped viruses.

[0247] [Evaluation: Inactivation of non-enveloped viruses]

[0248] The virus inactivating liquid of Example 1 is considered to have a high virus inactivating ability even for non-enveloped viruses.

[0249] (Example 2)

[0250] Example 2 relates to a variation of Example 1.

[0251] [Preparation of virus inactivation solution]

[0252] In Example 2, as described in detail below, after the (4) separation in Example 1, partial oxidation was performed as an additional step, and then (5') concentration adjustment was performed to prepare a virus inactivation liquid.

[0253] 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) layering, were performed to obtain a single-layer or few-layer MXene (Ti3 C2T s ) particles contain liquid.

[0254] The obtained single-layer and few-layer MXene (Ti3 C2T s ) The particles contained liquid, and the concentration of the particles as the solid component was 125 mg / mL.

[0255] (Additional step) Partial oxidation

[0256] The above-mentioned single-layer and few-layer MXene (Ti3 C2T s ) particles containing liquid, and subjected to a heat treatment (oxidation treatment) at 70°C in an environment containing oxygen and having a relative humidity of 90% to obtain a treated liquid. The treatment time was 194.5 hours.

[0257] In order to confirm the progress of partial oxidation during the above-mentioned heat treatment (oxidation treatment), the above-mentioned single-layer and few-layer MXene (Ti3 C2T s ) The solid components (particles) were extracted from the particle-containing liquid (before treatment) and the above-mentioned treatment liquid (after treatment) and observed using a scanning electron microscope (SEM). The obtained SEM photographs are shown in Figure 3 In. With Figure 3 Compared with the state before treatment shown in (a), Figure 3 In the state after treatment shown in (b), the TiO2 obtained by low temperature oxidation can be confirmed to have a unique elongated image (white elongated particles can be observed in the SEM photograph). In addition, the XRD line shape of the solid component (particles) was obtained by X-ray diffraction (XRD) measurement. Compared with the XRD pattern of the solid component (particles) before treatment, the XRD pattern of the solid component (particles) after treatment shows that Ti3 C2T s The peak height near 2θ=5-8°, which is unique to anatase TiO2, is reduced, and the peak near 2θ=24-26°, which is unique to anatase TiO2, can be detected again.

[0258] (5') Concentration adjustment

[0259] The treatment liquid after the heat treatment (oxidation treatment) was diluted with pure water, and the concentration of the particles as the solid content was adjusted to 5 mg / mL to obtain a virus inactivation liquid.

[0260] Based on the above, single-layer and few-layer MXene (Ti3 C2T s ) particles to prepare the virus inactivation liquid of Example 2. The pH of the liquid medium in this virus inactivation liquid was 4.3. In this virus inactivation liquid, it was visually confirmed that the particles were well dispersed and there was no aggregation or sedimentation.

[0261] [Evaluation: Inactivation of enveloped viruses]

[0262] The virus inactivation liquid obtained in Example 2 was used as a sample (test material) to conduct an enveloped virus inactivation test on this sample in the same manner as in Example 1 to evaluate its virus inactivation ability. The results obtained thereby showed that the virus inactivation liquid of Example 2 had a high ability to inactivate enveloped viruses.

[0263] [Evaluation: Inactivation of non-enveloped viruses]

[0264] The virus inactivation liquid of Example 2 is considered to have a high virus inactivation ability even for non-enveloped viruses.

[0265] (Example 3)

[0266] Example 3 relates to the virus inactivation article described in Implementation 2.

[0267] [Manufacture of virus-inactivated products]

[0268] In Example 3, as described in detail below, a virus inactivating liquid was applied to a substrate to form a virus inactivating layer, thereby producing a virus inactivating article having a virus inactivating layer disposed on a substrate.

[0269] First, in the above (5) concentration adjustment, the same operation as in Example 1 was performed except that the dilution of pure water was changed. A single-layer and few-layer MXene (Ti3 C2T s ) particles to prepare a virus inactivation liquid.

[0270] In this virus inactivating liquid, the average thickness of the MXene particles is 1 nm to 10 nm, and the average size of the MXene particles in a two-dimensionally developed surface is 3 μm.

[0271] This virus inactivation liquid is MXene (Ti3C2T s ) particles dispersed in pure water, without additives such as binders and dispersants.

[0272] Separately, as a base material, a glass substrate whose surface was hydrophilized by UV treatment was prepared.

[0273] Then, the virus inactivation liquid prepared above was sprayed on the hydrophilized surface of the glass substrate, and then warm air was blown from a dryer. The above operation was repeated 30 times, and then pre-dried at 80°C for 2 hours in a normal pressure oven and formally dried at 150°C for 18 hours in a vacuum oven (the pure water as the liquid medium was substantially removed by drying). Thus, a single layer and a few layers of MXene (Ti3C2T s ) particles. The thickness of the virus inactivation layer is about 2 μm.

[0274] Based on the above, it is possible to obtain a monolayer or a few-layer MXene (Ti3C2T s ) particles are arranged on a glass substrate.

[0275] [Evaluation: Inactivation of enveloped viruses]

[0276] The virus inactivation article of Example 3 is considered to have a high virus inactivation ability against enveloped viruses.

[0277] [Evaluation: Inactivation of non-enveloped viruses]

[0278] The virus inactivation article of Example 3 is considered to have a high virus inactivation ability even for non-enveloped viruses.

[0279] (Example 4)

[0280] Example 4 relates to another example of the virus inactivation liquid described in embodiment 1.

[0281] In Example 4, the following detailed steps (1) preparation of the precursor (MAX), (2) etching of the precursor, (3) cleaning after etching, (4) Li intercalation, and (5) delamination were carried out in order to prepare a virus inactivation solution.

[0282] (1) Preparation of precursor (MAX)

[0283] As in Example 1, Ti3AlC2 particles were obtained as a precursor (powdered MAX).

[0284] (2) Etching of the precursor

[0285] A solid-liquid mixture (slurry) containing a solid component derived from the Ti 3 AlC 2 powder was obtained in the same manner as in Example 1 except that the etching liquid composition was changed to the following etching conditions.

[0286] Etching solution composition: 49% HF 6mL

[0287] H2O 18mL

[0288] HCl (12M) 36 mL

[0289] (3) Cleaning after etching

[0290] The slurry was divided into two equal parts and inserted into two 50 mL centrifuge tubes 2, respectively. Except for this, the same method as in Example 1 was used to obtain MXene (Ti3 C2T s ) particle-water medium clay.

[0291] (4) Li intercalation

[0292] For the MXene (Ti3 C2T s ) particles - water medium clay, as follows, stirring at a specified temperature range for a specified time, to carry out Li intercalation.

[0293] (Li intercalation conditions)

[0294] Ingredients:

[0295] MXene(Ti3C2T s ) Particle-water medium clay: solid content 0.75g

[0296] LiCl 1.00g

[0297] HCl about 0.67g

[0298] 19.42g pure water

[0299] Intercalation container: 100mL bottle container

[0300] Temperature: 20°C to 25°C (room temperature)

[0301] Duration: 12 hours

[0302] Stirrer speed: 800rpm

[0303] (5) Layering

[0304] The slurry obtained by Li intercalation was put into a 50 mL centrifuge tube, and after centrifugation at 3500G using a centrifuge, the supernatant was discarded. Then, (i) 40 mL of pure water was added to the remaining precipitate, and after stirring with a shaker for 15 minutes, (ii) centrifugation was performed at 3500G, and (iii) the supernatant was recovered as a single-layer / few-layer MXene-containing liquid. This operation (i) to (iii) was repeated 4 times in total to obtain a single-layer / few-layer MXene-containing supernatant. For this supernatant, a centrifuge was used to centrifuge at 4300G for 2 hours, and the supernatant was discarded to obtain a single-layer / few-layer MXene-containing clay. 1 mg of the clay thus obtained was taken and redispersed in 10 mL of pure water.

[0305] Based on the above, a single-layer and few-layer MXene (Ti3 C2T s ) particles of Example 4. The pH of the liquid medium of this virus inactivation liquid was 2.7. In this virus inactivation liquid, it was visually confirmed that the particles were well dispersed and did not aggregate or settle.

[0306] (Example 5)

[0307] Example 2 relates to a variation of Example 4.

[0308] In Example 5, a virus inactivation liquid was prepared in the same manner as in Example 4 except that the ingredients for the Li intercalation conditions in the above-mentioned (4) Li intercalation were as follows.

[0309] Ingredients:

[0310] MXene(Ti3 C2T s ) Particle-water medium clay: solid content 0.75g

[0311] LiCl 0.97g

[0312] LiOH+H2O about 0.03g

[0313] 20.00g pure water

[0314] Based on the above, a single-layer or few-layer MXene (Ti3 C2Ts ) particles of Example 5. The pH of the liquid medium in this virus inactivation liquid was 6.9. In this virus inactivation liquid, it was visually confirmed that the particles were well dispersed and did not aggregate or settle.

[0315] (Example 6)

[0316] Example 6 relates to another example of the virus inactivation liquid described in embodiment 1.

[0317] In Example 6, in the above-mentioned (4) Li intercalation, the ingredients for the Li intercalation conditions are as follows, and the following (5') layering is performed instead of the above-mentioned (5) layering. Except for this, the same procedures as in Example 4 are followed. Thereafter, (6) acid treatment and (7) water washing are performed in this order to prepare a virus inactivation liquid.

[0318] (Li intercalation conditions)

[0319] Ingredients:

[0320] MXene(Ti3 C2T s ) Particle-water medium clay: solid content 0.75g

[0321] LiCl 0.75g

[0322] (5') Layering

[0323] The slurry obtained by Li intercalation was put into a 50 mL centrifuge tube, and after centrifugation at 3500G using a centrifuge, the supernatant was discarded. Then, (i) 40 mL of pure water was added to the remaining precipitate, and after stirring with a shaker for 15 minutes, (ii) centrifugation was performed at 3500G, and (iii) the supernatant was recovered as a single-layer·few-layer MXene-containing liquid. The operations (i) to (iii) were repeated a total of 4 times to obtain a single-layer·few-layer MXene-containing supernatant. In addition, the supernatant was centrifuged at 4300G for 2 hours using a centrifuge to obtain a single-layer·few-layer MXene-containing clay.

[0324] (6) Acid treatment

[0325] To the above-mentioned single-layer / few-layer MXene-containing clay, (i) 35 mL of 1.8 M hydrochloric acid was added, followed by stirring with a shaker for 5 minutes, (ii) centrifugation at 3500 G, and (iii) discarding the supernatant. These steps (i) to (iii) were repeated a total of five times.

[0326] (7) Water cleaning

[0327] To the acid-treated monolayer / few-layer MXene-containing clay, (i) 35 mL of water was added, followed by agitation for 5 minutes, (ii) centrifugation at 3500 g, and (iii) the supernatant was discarded. These steps (i) to (iii) were repeated five times to obtain a monolayer / few-layer MXene-containing clay as a monolayer / few-layer MXene-containing sample. The final pH of the supernatant was confirmed to be 4 or higher. 1 mg of the resulting clay was redispersed in 10 mL of pure water.

[0328] Based on the above, a single-layer and few-layer MXene (Ti3 C2T s ) particles of Example 6. The pH of the liquid medium of this virus inactivation liquid was 4.3. In this virus inactivation liquid, it was visually confirmed that the particles were well dispersed and did not aggregate or settle.

[0329] [Measurement of Li Content in MXene Particles]

[0330] The MXene was melted by alkali fusion, and the Li content was measured by ICP-AES using inductively coupled plasma atomic emission spectrometry (using iCAP7400 manufactured by Thermo Fisher Scientific). The result showed that the Li content was 4 ppm by mass.

[0331] (Example 7)

[0332] Example 7 relates to another example of the virus inactivation liquid described in embodiment 1.

[0333] In Example 7, the following detailed steps (1) preparation of the precursor (MAX), (2) etching of the precursor, (3) cleaning after etching, (4) Li intercalation, and (5) delamination were carried out in order to prepare a virus inactivation solution.

[0334] (1) Preparation of precursor (MAX)

[0335] As in Example 1, Ti3AlC2 particles were obtained as a precursor (powdered MAX).

[0336] (2) Etching of the precursor

[0337] The etching conditions and the etching solution composition are as follows. Except for the above, the same procedures as in Example 1 were carried out to obtain a solid-liquid mixture (slurry) containing a solid component derived from the Ti3AlC2 powder.

[0338] (Etching Conditions)

[0339] Etching solution composition: HF concentration 2.8M

[0340] H3PO4 concentration 7.4M

[0341] (3) Cleaning after etching

[0342] The above slurry was divided into two equal parts and inserted into two 50 mL centrifuge tubes respectively. The same method as in Example 1 was used to obtain MXene (Ti3 C2T s ) particle-water medium clay.

[0343] (4) Li intercalation

[0344] For the MXene (Ti3 C2T s ) Particle-water medium clay, add Li3PO4, H3PO4 and pure water, stir for a specified time within a specified temperature range, and perform Li intercalation.

[0345] (Li intercalation conditions)

[0346] Ingredients:

[0347] MXene(Ti3 C2T s ) Particle-water medium clay: solid content 0.75g

[0348] Li3PO4: 0.68g

[0349] 85 mass% H3PO4: 3.1 mL

[0350] Pure water: 31.9 mL

[0351] Intercalation container: 100mL bottle container

[0352] Temperature: 20°C to 25°C (room temperature)

[0353] Duration: 15 hours

[0354] Stirrer speed: 800rpm

[0355] (5) Layering

[0356] The slurry obtained after Li intercalation was placed in a 50 mL centrifuge tube and centrifuged at 3500 G using a centrifuge. The supernatant was discarded. Next, 40 mL of pure water was added to the remaining precipitate after the supernatant was removed. The mixture was stirred for 15 minutes using a shaker and then centrifuged at 3500 G. The supernatant was recovered as a monolayer / few-layer MXene-containing liquid. This procedure was repeated four times to obtain a monolayer / few-layer MXene-containing liquid.

[0357] Based on the above, a single-layer and few-layer MXene (Ti3 C2T s) particles of Example 7. The pH of the liquid medium in this virus inactivation liquid was 4.3. In this virus inactivation liquid, it was visually confirmed that the particles were well dispersed and did not aggregate or settle.

[0358] [Measurement of chlorine and bromine content in MXene particles]

[0359] The chlorine and bromine contents of the MXene particles obtained in Example 7 were measured using a combustion ion chromatograph (Dionex ICS-5000) manufactured by Thermo Fisher Scientific. The results showed that the chlorine content was 50 ppm by mass or less, and the bromine content was also 50 ppm by mass or less. In other words, the combined chlorine and bromine content was 100 ppm by mass or less.

[0360] [Evaluation: Virus inactivation]

[0361] The virus inactivating liquids of Examples 4 to 7, like the virus inactivating liquid of Example 1, are considered to have high virus inactivation abilities against enveloped viruses and non-enveloped viruses.

[0362] Industrial applicability

[0363] The virus inactivating liquid and virus inactivating article of the present invention can inactivate viruses and therefore can be used to prevent humans and other organisms from being infected with viruses.

[0364] This application claims priority based on application No. 63 / 129,051 filed in the United States on December 22, 2020, the entire contents of which are incorporated by reference into this specification.

[0365] Explanation of symbols

[0366] 1a, 1b layer main body (M m X n layer)

[0367] 3a, 5a, 3b, 5b modification or terminal T

[0368] 7a, 7b MXene layers

[0369] 10, 10a, 10b MXene (layered material) particles

[0370] 11. Substrate

[0371] 11a Substrate surface

[0372] 13 Virus inactivation layer

[0373] 20 Virus inactivation items

Claims

1. Application of a virus inactivation liquid in the preparation of a virus inactivation agent, wherein: The virus inactivation liquid comprises a liquid medium and particles containing one or more layers of layered materials. The layers include: By the following formula: M m X n The layer body represented by Wherein, M is at least one metal of Groups 3, 4, 5, 6, or 7, X is a carbon atom, a nitrogen atom, or a combination of carbon and nitrogen atoms, n is 1 or more and 4 or less, m is greater than n and less than 5; and The modification or terminal T present on the surface of the main body of the layer, T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom, The average thickness of the particles is less than 10 nm. The virus inactivation liquid meets either or both of the following (i) and (ii): (i) the pH of the liquid medium is 2.7 or higher and 7.0 or lower, (ii) The Li content in the particles is 20 mass ppm or less.

2. The use according to claim 1, wherein The M m X n It is Ti3C2.

3. The use according to claim 1 or 2, wherein: The liquid medium includes at least one of water and alcohol.

4. The use according to claim 1 or 2, wherein: The composition further comprises at least one additive selected from the group consisting of a dispersant, a binder, an antioxidant, a viscosity modifier, and a fragrance.

5. The use according to claim 1 or 2, wherein: The content of the particles in the virus inactivating liquid is 0.5 mg / mL or more and 100 mg / mL or less.

6. The use according to claim 1 or 2, wherein: The total content of chlorine and bromine in the particles is 1500 ppm by mass or less.

7. The use according to claim 1 or 2, wherein: The particles support at least one of a metal and a metal oxide.

8. The use according to claim 1 or 2, wherein: The particles carry titanium oxide.

9. Use of a virus inactivation layer in the preparation of a virus inactivation article, wherein: The virus inactivation article comprises a substrate and a virus inactivation layer disposed on the substrate, wherein the virus inactivation layer comprises particles of a layered material having one or more layers. The layers include: By the following formula: M m X n The layer body represented by Wherein, M is at least one metal of Groups 3, 4, 5, 6, or 7, X is a carbon atom, a nitrogen atom, or a combination of carbon and nitrogen atoms, n is 1 or more and 4 or less, m is greater than n and less than 5; and The modification or terminal T present on the surface of the main body of the layer, T is at least one selected from the group consisting of a hydroxyl group, a fluorine atom, a chlorine atom, and an oxygen atom, The average thickness of the particles is less than 10 nm. The Li content in the particles is 20 mass ppm or less.

10. The use according to claim 9, wherein: The substrate is any one selected from the group consisting of filters, masks, protective masks, bandages, gloves, protective clothing, touch screens, displays, films and seals.

11. The use according to claim 9 or 10, wherein: The M m X n It is Ti3C2.

12. The use according to claim 9 or 10, wherein: The composition further comprises at least one additive selected from the group consisting of a dispersant, a binder, an antioxidant, a viscosity modifier, and a fragrance.

13. The use according to claim 9 or 10, wherein: The total content of chlorine and bromine in the particles is 1500 ppm by mass or less.

14. The use according to claim 9 or 10, wherein: The particles support at least one of a metal and a metal oxide.

15. The use according to claim 9 or 10, wherein: The particles carry titanium oxide.

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