Graphene fiber with core-shell structure

Abstract

The present application provides a fiber, in particular an oral care fiber, comprising a core and a shell surrounding the core wherein the weight ratio of graphene in the shell is greater than the weight ratio of graphene in the core. An oral care article is provided comprising the fiber. Under the condition that the fiber has the antibacterial performance brought by graphene, the fiber also has better physical properties such as rebound resilience, or also has good sharpened filament tip forming.

Description

Technical Field

[0001] The present application relates to the field of fibers, and more specifically to a core-shell structured graphene fiber. Background Art

[0002] Graphene is a two-dimensional carbon material composed of a layer of carbon atoms periodically and tightly stacked in a benzene ring structure (i.e., a hexagonal honeycomb structure). Graphene inactivates bacteria through various means such as physical cutting, oxidative stress, and interference with lipid molecules, and has a highly effective antibacterial effect.

[0003] Prior art has used graphene as an additive to fiber slices for blending and spinning, producing composite fibers containing graphene with antibacterial properties. The graphene is distributed both inside and on the outer surface of the fiber. The graphene on the outer surface of the fiber can inactivate bacteria, thus imparting the fiber's antibacterial properties.

[0004] However, the graphene distributed within the fiber cannot come into contact with bacteria and thus cannot play an antibacterial role. Therefore, a large amount of graphene must be added to impart a certain degree of antibacterial properties to the fiber, and the antibacterial properties are still unstable. Furthermore, as the amount of graphene added increases, the fiber's physical properties, such as resilience, decrease, leading to a decrease in the fiber's overall performance.

[0005] The sharpened wire is formed by hydrolyzing the polyester fiber material with a strong base (such as sodium hydroxide) to form a sharp point (sharpened), such as Figure 9 However, when such fibers are used as sharpened wires, graphene also affects the tip formation of the sharpened wires. Summary of the Invention

[0006] In one aspect, the present application provides a fiber, in particular a fiber for oral care, comprising:

[0007] a core; and

[0008] a shell portion, surrounding the core portion,

[0009] The weight ratio of graphene in the shell portion is greater than the weight ratio of graphene in the core portion.

[0010] In one aspect, the present application provides a method for preparing fiber, particularly fiber for oral care, comprising:

[0011] providing a core; and

[0012] providing a shell portion surrounding the core portion,

[0013] The weight ratio of graphene in the shell portion is greater than the weight ratio of graphene in the core portion.

[0014] In one aspect, the present application provides an oral care product comprising the fiber of the present application. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] By describing the exemplary embodiments in detail with reference to the accompanying drawings, the features will become apparent to those skilled in the art. However, the various technical features in the drawings are not drawn to scale. For the purpose of clearly illustrating this application, the dimensions of the various features in the drawings may be arbitrarily enlarged or reduced. The dimensions of the various components or their proportional relationships in the drawings are not intended to limit the dimensions of the various components or their proportional relationships in this application.

[0016] Figure 1 This is a schematic diagram of a partial structure of a fiber in some embodiments of the present application.

[0017] Figure 2 This is a schematic cross-sectional view of a fiber along a cross section perpendicular to its extending direction (ie, axial direction) in some embodiments of the present application.

[0018] Figure 3 Schematic cross-sectional view of a fiber along a cross section perpendicular to its extending direction in some other embodiments of the present application.

[0019] Figure 4 The ends of the fibers are shown in some embodiments of the present application.

[0020] Figure 5 The ends of fibers in other embodiments of the present application are shown.

[0021] Figure 6 An oral care product of the present application is shown, including the fiber of the present application.

[0022] Figure 7 The figures show the ends of several sharpened wires of the comparative examples of the present application observed under an electron magnifying glass.

[0023] Figure 8 Fiber cross sections of some embodiments of the present application observed under an electron magnifying glass are shown.

[0024] Figure 9 Schematic diagram of a sharpened wire according to the general technology in this field.

[0025] The following are the descriptions of the reference numerals:

[0026] 100: fiber; 101: tip; 110: core; 111: protrusion; 112: radial protrusion; 120: shell; 200: toothbrush; 210: toothbrush body; 300: dental floss; z: extension direction (axial direction); ρ: radial direction; Circumferential direction; D1, D2: diameter; L, L′: length. DETAILED DESCRIPTION

[0027] In order to further illustrate the technical means and effects adopted by this application to achieve the intended purpose, the specific implementation methods, structures, features and effects of this application are described in detail below in combination with the accompanying drawings and examples.

[0028] The following will describe specific embodiments or implementations of the elements and their structural relationships to simplify the content of this application, and use specific language to describe the embodiments or implementations of the present application as exemplified in the accompanying drawings, so that those skilled in the art can implement the different features of the technical solutions of this application. However, it should be understood that these embodiments are merely exemplary and are not intended to limit the scope of this application. For those skilled in the art, any changes or modifications to the described embodiments and any further applications of the principles described in this application can be considered as general and common situations.

[0029] Terms and Definitions

[0030] The present application repeats reference numerals throughout the various embodiments. This repetition is for simplicity and clarity and is not intended to limit the relationships between the elements and their structural relationships among the various embodiments of the present application. Even if features of one embodiment share the same reference numeral, this does not necessarily mean that features of one embodiment must be used in another embodiment.

[0031] For ease of description, spatially relative terms (such as "lower," "beneath," "below," "lower," "upper," "above," "above," or similar terms) may be used herein to describe the relationship of one element or feature to another element (or elements) or feature (or features) shown in the various figures. In addition to the directions depicted in the various figures, such spatially relative terms should be deemed to include different orientations of the device in use or operation. The technical solutions of the present application can be oriented in other ways (rotated 90 degrees, 180 degrees, mirrored, etc.) and the spatially relative terms used herein can be interpreted similarly.

[0032] As used herein, a cylindrical coordinate system is used to describe the spatial relativity of the structure of the fibers of this application. The term "axial direction" should be understood in its common meaning in this field and refers to the direction in which the fibers of this application extend. It is not intended to limit the fibers of this application to being rigid and extending only in one direction. The fibers of this application, depending on their material, should possess a certain degree of plasticity and bendability. The terms "radial direction" and "circumferential direction" should be understood in their common meaning in this field.

[0033] As used herein, descriptions such as "forming a first feature 'over' or 'on' a second feature" may include embodiments in which the first and second features are formed in direct contact, and may also include embodiments in which an additional feature may be formed between the first and second features so that the first and second features are not in direct contact. Unless otherwise specified, this application should be deemed to disclose embodiments in which the first and second features are formed in direct contact and embodiments in which the first and second features are not in direct contact, respectively.

[0034] As used herein, singular terms refer to one or more than one. For example, "element" or "an element" refers to one element or more than one element. As used herein, the term "plurality" refers to at least two.

[0035] As used herein, the term "about" refers to approximation, in the range of about or near. When the term "about" is used in conjunction with a numerical range, it modifies the range by expanding the limit above or below the provided numerical value. In general, the term "about" is used herein to change the numerical value up and down by 10% from the provided value. On the one hand, the term "about" refers to adding or subtracting 20% ​​of the numerical value of the number it modifies. For example, "about 50%" refers to within the range of 45%-55%. The numerical ranges mentioned herein by endpoints include all integers and fractions contained in the range (e.g., "1 to 5" includes 1, 1.5, 2, 2.75, 3, 3.90, 4, and 5). It should also be understood that all integers and fractions thereof are considered to be modified by the term "about".

[0036] As used herein, the terms "comprise", "include", or "contain", as non-exclusive or open terms, are intended to indicate that a combination (e.g., a device, composition, method, etc.) includes the listed elements (e.g., each unit of the device, each component of the composition, the substantial steps of the method, etc.), but does not exclude other elements. As used herein, the term "substantially consisting of..." when used to define compositions and methods means excluding other elements that have any substantial impact on the combination of the stated purpose, but does not exclude other elements that do not substantially affect the basic and novel features of the present application. As used herein, the term "consisting of..." refers to a combination (unit, component, substantial step, etc.) excluding other elements, but unless otherwise stated, it is not intended to exclude trace amounts of unavoidable impurities. The embodiments defined by each of these connecting terms are within the scope of the present application. As specific embodiments thereof, the disclosure of a technical solution including the terms "comprise", "include", or "contain" should also be deemed to simultaneously disclose the corresponding technical solutions including the terms "substantially consisting of..." and "consisting of..."

[0037] As used herein, the term "and / or" refers to and encompasses any and all possible combinations of one or more of the associated listed items. When used in a list of two or more items, the term "and / or" means that any one of the listed items may be included alone, or may include any combination of two or more of the listed items. For example, if a group, combination, or composition, etc., is described as including (or comprising) components A, B, C, and / or D, the composition may include A alone; B alone; C alone; D alone; the combination of A and B; the combination of A and C; the combination of A and D; the combination of B and C; the combination of B and D; the combination of C and D; the combination of A, B, and C; the combination of A, B, and D; the combination of A, C, and D; or the combination of A, B, C, and D.

[0038] Unless otherwise defined and not conflicting with the context, the content ratios used herein shall be preferably regarded as weight ratios, and the content percentages shall be preferably regarded as weight percentages (wt %).

[0039] As used herein, the term "core-shell" or "core-sheath" means that in the fiber of the present application, at least a portion (e.g., at least 50%, particularly at least 60%, 70%, 75%, 80%, 85%, 90% or 95%, more particularly 100%) of the core in its extending direction, i.e., the axial direction, is surrounded by a shell (sheath). As used herein, the term "surrounding" means that the shell (sheath) is formed on at least a portion (e.g., at least 50%, particularly at least 60%, 70%, 75%, 80%, 85%, 90% or 95%, more particularly 100%) of the core in the radial direction, and the core portion on which the shell (sheath) is formed is covered by the shell and is not exposed. As used herein, the terms "shell" and "sheath" should be understood identically and can be used interchangeably when describing the fiber of the present application.

[0040] Implementation Method

[0041] Fiber (brush wire)

[0042] Figure 1 This is a schematic diagram of a partial structure of a fiber 100 in some embodiments of the present application; Figure 2 This is a cross-sectional view of the fiber 100 along the section AA perpendicular to the extending direction z (ie, the axial direction) thereof in some embodiments of the present application.

[0043] like Figure 2As shown, the fiber 100 may include a core 110 and a shell 120 surrounding the core 110 (forming (covering) at least a portion of the core 110 in the radial direction, for example, at least 50%, particularly at least 60%, 70%, 75%, 80%, 85%, 90%, or 95%, and more particularly 100%). In some embodiments, the fiber 100 is composed of the core 110 and the shell 120. In some embodiments, the fiber 100 may include a core 110 composed of a polymer fiber and a shell 120 composed of a graphene polymer fiber and surrounding the core 110.

[0044] In some embodiments, the surrounding is contact surrounding or non-contact surrounding, in particular contact surrounding. In some embodiments, the shell 120 contacts and surrounds the core 110, that is, the shell 120 is directly formed (contact covered) on at least a portion of the core 110 in the radial direction.

[0045] In some embodiments, the core 110 may have a further core-shell structure.

[0046] In some embodiments, the core 110 may include polymer fibers. In some embodiments, the core 110 may include or consist of polyolefin fibers, polyfluoroolefin fibers, polyester fibers, or polyamide fibers. In some embodiments, the core 110 may include or consist of polyethylene (PE), polypropylene (PP), polytetrafluoroethylene (PTFE), polyethylene terephthalate (PET), polybutylene terephthalate (PBT), nylon (e.g., nylon N6, nylon N66, nylon 610, nylon 612, nylon 1010, etc.), or combinations thereof.

[0047] In some embodiments, the core 110 may be composed of a single polyolefin fiber, polyfluoroolefin fiber, polyester fiber, or polyamide fiber, or a combination of multiple polyolefin fibers, polyfluoroolefin fibers, polyester fibers, or polyamide fibers.

[0048] In some embodiments, the shell 120 may include polymer fibers. In some embodiments, the shell 120 may include polyolefin fibers, polyfluoroolefin fibers, polyester fibers, or polyamide fibers. In some embodiments, the shell 120 may include polyethylene, polypropylene, polytetrafluoroethylene, polyethylene terephthalate, polybutylene terephthalate, nylon (e.g., nylon N6, nylon N66, nylon 610, nylon 612, nylon 1010, etc.), or combinations thereof, but is not limited thereto.

[0049] In some embodiments, the shell 120 may be composed of graphene polyolefin fibers, graphene polyfluoroolefin fibers, graphene polyester fibers, or graphene polyamide fibers.

[0050] graphene

[0051] In some embodiments, the core 110 and / or the shell 120 may include graphene. In some embodiments, the weight ratio of graphene in the shell 120 is greater than the weight ratio of graphene in the core 110. In some embodiments, the weight ratio of graphene in the shell 120 may be 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.8, 2, 2.5, 3, 4, 5, 6, 8, or 10 times greater than the weight ratio of graphene in the core 110. In some embodiments, the weight ratio of graphene in the core 110 may be 0.9, 0.8, 0.7, 0.6, 0.5, 0.4, 0.3, 0.2, or less than 0.1 times the weight ratio of graphene in the shell 120.

[0052] In some embodiments, the core 110 may include 0.6 wt % or less, specifically 0.5 wt %, 0.4 wt %, 0.3 wt %, 0.2 wt %, or 0.1 wt % or less of graphene.

[0053] In some embodiments, the core 110 may not include graphene.

[0054] In some embodiments, the shell 120 may include more than 0.4 wt%, and particularly more than 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, or 4.0 wt% graphene. In some embodiments, the shell 120 can include 0.4–4.0 wt%, specifically 0.6–4.0 wt%, 0.8–4.0 wt%, 0.4–3.0 wt%, 0.6–3.0 wt%, 0.8–3.0 wt%, 0.4–2.4 wt%, 0.6–2.4 wt%, 0.8–2.4 wt%, 0.4–1.6 wt%, 0.6–1.6 wt%, or 0.8–1.6 wt% graphene.

[0055] In some embodiments, the fiber 100 may include greater than 0.2 wt%, particularly greater than 0.25, 0.3, 0.35, 0.4, 0.45, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, or 3.0 wt% graphene. In some embodiments, the fiber 100 may include less than 3.0 wt%, specifically 2.9 wt%, 2.8 wt%, 2.7 wt%, 2.6 wt%, 2.5 wt%, 2.4 wt%, 2.3 wt%, 2.2 wt%, 2.1 wt%, 1.0 wt%, 1.9 wt%, 1.8 wt%, 1.7 wt%, 1.6 wt%, 1.5 wt%, 1.4 wt%, 1.3 wt%, 1.2 wt%, 1.1 wt%, 1.0 wt%, 0.9 wt%, 0.8 wt%, 0.7 wt%, 0.6 wt%, 0.5 wt%, 0.45 wt%, 0.4 wt%, 0.35 wt%, 0.3 wt%, 0.25 wt%, or less than 0.2 wt% graphene. In some embodiments, the fiber 100 may include 0.2-2.0 wt%, specifically 0.3-2.0 wt%, 0.4-2.0 wt%, 0.5-2.0 wt%, 0.2-1.7 wt%, 0.3-1.7 wt%, 0.4-1.7 wt%, 0.5-1.7 wt%, 0.2-1.3 wt%, 0.3-1.3 wt%, 0.4-1.3 wt%, 0.5-1.3 wt%, 0.2-0.8 wt%, 0.3-0.8 wt%, 0.4-0.8 wt%, or 0.5-0.8 wt% graphene.

[0056] In some embodiments, the graphene may be graphene oxide, reduced graphene, or a combination thereof.

[0057] In some embodiments, the core 110 and / or the shell 120, particularly the shell 120, may further include an antimicrobial agent. In some embodiments, the antimicrobial agent may be, for example, silver ions, zinc ions, or activated carbon.

[0058] Fiber proportions, shapes, and sizes

[0059] Figure 3 This is a cross-sectional view of the fiber 100 along a cross section perpendicular to its extending direction z in some embodiments of the present application.

[0060] Please refer to Figure 3 (a)–(b). Figure 3 The cross-sectional area of ​​the core 110a in (a) occupies a larger proportion of the cross-sectional area of ​​the entire fiber 100a. In other words, the cross-sectional area of ​​the shell 120a occupies a smaller proportion of the cross-sectional area of ​​the entire fiber 100a. Conversely, Figure 3 In (b), the cross-sectional area of ​​the core 110b accounts for a smaller proportion of the cross-sectional area of ​​the entire fiber 100b. In other words, the cross-sectional area of ​​the shell 120b accounts for a larger proportion of the cross-sectional area of ​​the entire fiber 100b. By adjusting the ratio of the cross-sectional area of ​​the core 110 / shell 120 to the cross-sectional area of ​​the entire fiber 100, the weight percentage of the core 110 / shell 120 in the entire fiber 100 can be adjusted, and the weight percentage of the components of the core 110 / shell 120 in the entire fiber can be further adjusted.

[0061] In some embodiments, in a radial direction p perpendicular to the extension direction z, the diameter of the core 110 may be more than 10% of the diameter of the shell 120 (or the diameter of the fiber 100), in particular, more than 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, or 90%. In some embodiments, in a radial direction p perpendicular to the extension direction z, the diameter of the core 110 may be less than 90% of the diameter of the shell 120 (or the diameter of the fiber 100), in particular, less than 85%, 80%, 75%, 70%, 65%, 60%, 55%, 50%, 45%, 40%, 35%, 30%, 25%, 20%, 15%, or 10%. In some embodiments, in the radial direction ρ perpendicular to the extension direction z, the diameter of the core 110 may be 40% to 90% of the diameter of the shell 120 (or the diameter of the fiber 100), in particular 45% to 90%, 50% to 90%, 55% to 90%, 40% to 80%, 45% to 80%, 50% to 80%, 55% to 80%, 40% to 75%, 45% to 75%, 50% to 75%, or 55% to 75%.

[0062] In some embodiments, in the radial direction ρ perpendicular to the extension direction z, the cross-sectional area of ​​the shell 120 may be more than 10% of the cross-sectional area of ​​the fiber 100 (or in particular the sum of the cross-sectional area of ​​the shell 120 and the cross-sectional area of ​​the core 110), in particular 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, or 90% or more. In some embodiments, in the radial direction ρ perpendicular to the extension direction z, the cross-sectional area of ​​the shell 120 may be less than 90% of the cross-sectional area of ​​the fiber 100 (or in particular the sum of the cross-sectional area of ​​the shell 120 and the cross-sectional area of ​​the core 110), in particular 85%, 80%, 75%, 70%, 65%, 60%, 55%, 50%, 45%, 40%, 35%, 30%, 25%, 20%, 15%, or 10% or less. In some embodiments, in the radial direction ρ perpendicular to the extension direction z, the cross-sectional area of ​​the shell 120 may be 20% to 90% of the cross-sectional area of ​​the fiber 100 (or in particular the sum of the cross-sectional area of ​​the shell 120 and the cross-sectional area of ​​the core 110), in particular 30% to 90%, 35% to 90%, 40% to 90%, 20% to 80%, 30% to 80%, 35% to 80%, 40% to 80%, 20% to 75%, 30% to 75%, 35% to 75%, or 40% to 75%.

[0063] In some embodiments, the weight of the shell 120 can be greater than 20%, particularly greater than 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, or 90%, of the weight of the fiber 100 (or particularly the sum of the weight of the shell 120 and the weight of the core 110). In some embodiments, the weight of the shell 120 can be less than 90%, particularly less than 85%, 80%, 75%, 70%, 65%, 60%, 55%, 50%, 45%, 40%, 35%, 30%, 25%, or 20%, of the weight of the fiber 100 (or particularly the sum of the weight of the shell 120 and the weight of the core 110). In some embodiments, the weight of the shell 120 can be 20% to 90%, particularly 30% to 90%, 35% to 90%, 40% to 90%, 20% to 80%, 30% to 80%, 35% to 80%, 40% to 80%, 20% to 75%, 30% to 75%, 35% to 75%, or 40% to 75% of the weight of the fiber 100 (or particularly the sum of the weight of the shell 120 and the weight of the core 110).

[0064] In some embodiments, the diameter of the core 110 may be greater than 50% of the diameter of the shell 120 (or the diameter of the fiber 100), and the shell 120 may include greater than 0.8 wt % graphene. In some embodiments, the diameter of the core 110 may be greater than 50% of the diameter of the shell 120 (or the diameter of the fiber 100), and the fiber 100 may include greater than 0.6 wt % graphene. In some embodiments, the diameter of the core 110 may be greater than 55% of the diameter of the shell 120 (or the diameter of the fiber 100), and the shell 120 may include greater than 2.4 wt % graphene. In some embodiments, the diameter of the core 110 may be greater than 55% of the diameter of the shell 120 (or the diameter of the fiber 100), and the shell 100 may include greater than 1.6 wt % graphene.

[0065] In some embodiments, the cross-sectional area of ​​the shell 120 may be less than 75% of the cross-sectional area of ​​the fiber 100 (or, in particular, the sum of the cross-sectional area of ​​the shell 120 and the cross-sectional area of ​​the core 110), and the shell 120 may include 0.8 wt% or more of graphene. In some embodiments, the cross-sectional area of ​​the shell 120 may be less than 75% of the cross-sectional area of ​​the fiber 100 (or, in particular, the sum of the cross-sectional area of ​​the shell 120 and the cross-sectional area of ​​the core 110), and the fiber 100 may include 0.6 wt% or more of graphene. In some embodiments, the cross-sectional area of ​​the shell 120 may be less than 70% of the cross-sectional area of ​​the fiber 100 (or, in particular, the sum of the cross-sectional area of ​​the shell 120 and the cross-sectional area of ​​the core 110), and the shell 120 may include 2.4 wt% or more of graphene. In some embodiments, the cross-sectional area of ​​shell 120 may be less than 70% of the cross-sectional area of ​​fiber 100 (or particularly the sum of the cross-sectional area of ​​shell 120 and the cross-sectional area of ​​core 110), and shell 100 may include more than 1.6 wt% graphene.

[0066] In some embodiments, the diameter of the core 110 may be 45% to 90%, in particular 50% to 90%, of the diameter of the shell 120 (or the diameter of the fiber 100), and the shell 120 may include 0.8 wt % to 4.0 wt % graphene; in particular, the percentage of the diameter of the core 110 relative to the diameter of the shell 120 minus 40% may be greater than about 6.25 times the weight percentage of the graphene in the shell 120.

[0067] In some embodiments, the cross-sectional area of ​​the shell 120 may be 20% to 80%, particularly 20% to 75%, of the cross-sectional area of ​​the fiber 100 (or particularly the sum of the cross-sectional area of ​​the shell 120 and the cross-sectional area of ​​the core 110), and the shell 120 may include 0.8 wt % to 4.0 wt % graphene; particularly, 85% minus the percentage of the cross-sectional area of ​​the shell 120 relative to the cross-sectional area of ​​the fiber 100 may be greater than about 6.25 times the weight percentage of the graphene in the shell 120.

[0068] In some embodiments, the cross-section of the fiber 100 in the vertical extension direction z may be circular or non-circular, for example, a circle, an ellipse, a convex polygon (for example, a triangle, a quadrilateral, a pentagon, a hexagon, a heptagon, an octagon, etc.) or a concave polygon (for example, a star, such as a five-pointed star, a six-pointed star, a seven-pointed star, or an eight-pointed star, etc.).

[0069] Please refer to Figure 3 (a)-(d) show the shape of the fiber 100 or a portion thereof (ie, the appearance of the shell 120) or the shape of the core 110 in some embodiments of the present application. Figure 3 As shown in (a)–(d), Figure 3 The fiber 100 (shell portion 120) in (a) and (b) may include a cylinder (ie, its cross section is circular), Figure 3 The fiber 100 (shell portion 120) in (c) may include a pentagonal column (ie, its cross section is a pentagon), Figure 3 The fiber 100 (shell 120) in (d) may include a triangular prism (i.e., its cross-section is triangular). However, the present application is not limited thereto, and the shape of the fiber 100 (i.e., the appearance of the shell 120) or the shape of the core 110 may be any shape feasible in the art.

[0070] In some embodiments, the length L of the fiber 100 can be 10 mm to 34 mm, specifically 15 mm to 20 mm, more specifically 16 mm to 17 mm, or specifically 10 mm to 15 mm, more specifically 11 mm to 13 mm, or specifically 20 mm to 34 mm, more specifically 26 mm to 30 mm.

[0071] In some embodiments, the diameter (e.g., the diameter at the thickest point) D of the fiber 100 may be 0.50 mm or less, particularly 0.35 mm or less, more particularly 0.30 mm, 0.25 mm, 0.22 mm, 0.20 mm, 0.19 mm, 0.18 mm, 0.17 mm, 0.16 mm, 0.15 mm, 0.14 mm, 0.13 mm, 0.12 mm, 0.11 mm, 0.10 mm, 0.09 mm, 0.08 mm, 0.075 mm, 0.07 mm, 0.06 mm, 0.05 mm, 0.04 mm, 0.06 mm, 0.08 mm, 0.09 ... and / or may be 0.01 mm or more, in particular 0.02 mm, 0.03 mm, 0.04 mm, 0.05 mm, 0.06 mm, 0.07 mm, 0.075 mm, 0.08 mm, 0.09 mm, 0.10 mm, 0.11 mm, 0.12 mm, 0.13 mm, 0.14 mm, 0.15 mm, 0.16 mm, 0.17 mm, 0.18 mm, 0.19 mm, 0.20 mm, 0.22 mm, 0.25 mm, 0.30 mm, or 0.35 mm or more.

[0072] In some embodiments, the diameter (e.g., the diameter at the thickest point) D of the fiber 100 may be 0.075 mm to 0.25 mm, particularly 0.10 mm to 0.18 mm, more particularly 0.11 mm to 0.14 mm, more particularly 0.12 mm to 0.13 mm, or particularly 0.14 mm to 0.16 mm, more particularly 0.145 mm to 0.155 mm, or particularly 0.16 mm to 0.18 mm, more particularly 0.17 mm to 0.18 mm.

[0073] Fiber end

[0074] Please refer to Figure 4 , illustrates the end of a fiber 100 in some embodiments of the present application. In some embodiments, the core 110 of the fiber 100 (e.g., a sharpened wire) may include a protrusion 111 that protrudes from the shell 120 in the extension direction z (i.e., the axial direction). That is, the protrusion 111 is the portion of the core 110 that is not radially covered by the shell 120. In some embodiments, the length of the protrusion 111 in the extension direction z may be at least 5%, specifically at least 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, or 50%, of the length of the core 110 in the extension direction z. In some embodiments, the shape of the protrusion 111 may be cylindrical, conical, truncated conical, or a combination thereof. In some embodiments, the shape of the protrusion 111 may be cylindrical, conical, truncated conical, or a combination thereof.

[0075] In some embodiments, the fiber 100 (e.g., a sharpened wire) may include a tip 101. In some embodiments, the tip 101 has a cross-sectional area perpendicular to the extension direction z that decreases along the extension direction z. In some embodiments, the length of the tip 101 along the extension direction z may be at least 5%, particularly at least 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, or 50%, of the length of the fiber 100 along the extension direction z. In some embodiments, the shape of the tip 101 may be conical, frustoconical, or a combination thereof. In some embodiments, the shape of the tip 101 may be conical, frustoconical, or a combination thereof.

[0076] In some embodiments, tip portion 101 may include protrusion 111; in other words, protrusion 111 constitutes at least a portion of tip portion 101. In some embodiments, protrusion 111 may include tip portion 101; in other words, tip portion 101 constitutes at least a portion of protrusion 111.

[0077] In some embodiments, as Figure 4 As shown, the tip portion 101 may include a protrusion 111; and the tip portion 101 may include a portion of the shell 120 and a portion of the core 110, and in particular may include a portion of the shell 120, a portion of the core 110 that does not belong to the protrusion 111, and (the entire) protrusion 111.

[0078] Please refer to Figure 5 , showing the end of the fiber 100 in some embodiments of the present application.

[0079] In some embodiments, as Figure 5 As shown in (a), the protrusion 111 may include the tip portion 101, and in particular, the protrusion 111 may include the (entire) tip portion 101 and a portion of the core 110 that does not belong to the tip portion 101. The tip portion 101 may be shaped like a cone, a truncated cone, or a combination thereof, in particular, like a cone, a truncated cone, or a combination thereof.

[0080] In some embodiments, as Figure 5 As shown in (b), the protrusion 111 may be columnar, particularly cylindrical. In some embodiments, the protrusion 111 may not have the tip 101.

[0081] In some embodiments, as Figure 5As shown in (c), the protrusion 111 may be composed of the tip portion 101, and / or the tip portion 101 may be composed of the protrusion 111. In some embodiments, the core 110 may include a radial protrusion 112, wherein the cross-sectional area of ​​the core 110 perpendicular to the extension direction z of the radial protrusion 112 is larger than the cross-sectional area of ​​the portion of the core 110 perpendicular to the extension direction z outside the protrusion 111. In some embodiments, the core 110 and the shell 120 contact each other in the extension direction z.

[0082] In some embodiments, as Figure 5 As shown in (d), the fiber 100 may not include the protrusion 111, and / or the fiber 100 may not include the tip 101. In some embodiments, one end of the core 110 and the shell 120 in the extension direction z (for example, the end away from the toothbrush body 210) is flush with each other. In some embodiments, both ends of the core 110 and the shell 120 in the extension direction z are flush with each other.

[0083] In some embodiments, the core 110 does not protrude beyond the shell 120 in the extension direction z. In some embodiments, the shell 120 does not protrude beyond the core 110 in the extension direction z.

[0084] In some embodiments, the diameter of the fiber 100, particularly the tip 101, at a distance of 0.01 mm from one end thereof is less than 0.04 mm. In some embodiments, the diameter of the fiber 100, particularly the tip 101, at a distance of 0.5 mm from one end thereof is less than 0.08 mm.

[0085] Applications and properties of fibers

[0086] In some embodiments, the fiber 100 is a brush filament, more particularly a toothbrush filament, and more particularly a toothbrush sharpening filament. In some embodiments, the fiber 100 is used in oral care products, particularly oral hygiene products, more particularly tooth cleaning products, and more particularly a toothbrush. In some embodiments, the fiber 100 is an oral care fiber, particularly an oral hygiene fiber, more particularly a tooth cleaning fiber, and more particularly a toothbrush filament, and especially a toothbrush sharpening filament. In some embodiments, an oral care product, particularly an oral hygiene product, more particularly a tooth cleaning product, and more particularly a toothbrush, is provided, comprising the fiber 100 and an optional oral care product body. In some embodiments, the fiber 100 is used in a hygiene product, particularly an oral hygiene product.

[0087] Please refer to Figure 6 , shows oral care products in some embodiments of the present application.

[0088] Figure 6(a) shows a toothbrush 200 in some embodiments of the present application. In some embodiments, the toothbrush 200 may include the fiber 100 of the present application as a brush filament. In some embodiments, more than 50% of the brush filaments in the toothbrush 200 are the fiber 100 of the present application. In some embodiments, the toothbrush 200 may further include a toothbrush body 210, wherein the fiber 100 is disposed on the toothbrush body 210. In some embodiments, the length L′ of the fiber 100 protruding from the toothbrush body 210 may be 10 mm to 15 mm, in particular 11 mm to 13 mm.

[0089] Figure 6 (b) shows a dental floss 300 in some embodiments of the present application. In some embodiments, the dental floss 300 may include or consist of the fiber 100 of the present application.

[0090] In some embodiments, the toothbrush 200 includes sharpened filaments disposed on the toothbrush body 210. In some embodiments, more than 50%, particularly more than 60%, 65%, 70%, 75%, 80%, 85%, 90%, or 95% of the sharpened filaments in the toothbrush 200 may be fibers 100 of the present application, and the diameter of the fibers 100 at a distance of 0.01 mm from one end (particularly the end distal to the toothbrush body 210) may be 0.04 mm or less. In some embodiments, more than 50%, particularly more than 60%, 65%, 70%, 75%, 80%, 85%, 90%, or 95% of the sharpened filaments in the toothbrush 200 may be fibers 100 of the present application, and the diameter of the fibers 100 at a distance of 0.5 mm from one end (particularly the end distal to the toothbrush body 210) may be 0.08 mm or less.

[0091] In some embodiments, the single-filament recovery rate of the fiber 100 measured according to the method of GB 19342-2013 is greater than 60%.

[0092] In some embodiments, the fiber 100 has an antibacterial rate of 90% or higher against Escherichia coli 8099 as tested according to the method of GB / T 36391-2018. In some embodiments, the fiber 100 has an antibacterial rate of 90% or higher against Staphylococcus aureus ATCC 6538 as tested according to the method of GB / T 36391-2018. In some embodiments, the fiber 100 has an antibacterial rate of 90% or higher against Candida albicans ATC 10231 as tested according to the method of GB / T 36391-2018. In some embodiments, the fiber 100 has an antibacterial rate of 90% or higher against beta-hemolytic Streptococcus CMCC 32210 as tested according to the method of GB / T 36391-2018. In some embodiments, the fiber 100 has an antibacterial rate of 90% or higher against Klebsiella pneumoniae ATCC 4352 as tested according to the method of GB / T 36391-2018.

[0093] In some embodiments, the fiber having the structure of the present application not only has the antibacterial properties brought by graphene, but also has good physical properties, especially resilience (single fiber recovery rate).

[0094] In some embodiments, fibers having the core-to-shell ratio and / or graphene addition amount of the present application, and fibers having the structure of the present application, while having the antibacterial properties brought by graphene, also have good physical properties, especially resilience (single filament recovery rate).

[0095] In some embodiments, the fiber having the structure of the present application not only has the antibacterial properties brought by graphene, but also has a good sharpened wire tip shape.

[0096] In some embodiments, fibers having the core-to-shell ratio and / or graphene addition amount of the present application, fibers having the structure of the present application, in addition to having the antibacterial properties brought by graphene, also have good sharpened wire tip formation.

[0097] Example

[0098] In the following examples and comparative examples:

[0099] - The test for single filament recovery rate is conducted in accordance with the test method in Section 5.5.5 (single filament bending recovery rate) of the Chinese national standard GB 19342-2013 "Toothbrush". This standard stipulates that a single filament recovery rate of 60% or higher is considered satisfactory.

[0100] Antibacterial performance testing is based on the requirements of Section 5.3.1 (Antibacterial Performance) of the Chinese national standard GB / T 36391-2018, "Antibacterial Toothbrush," and is conducted according to the methods specified in Appendix B (Material Antibacterial Performance Test Method - Oscillation Method) of the Chinese national standard GB / T 21510-2008, "Nano-Inorganic Antibacterial Performance Test Method." This standard stipulates that for Escherichia coli, an antibacterial rate of ≥90% is considered satisfactory; for Staphylococcus aureus, an antibacterial rate of ≥90% is considered satisfactory.

[0101] The diameter of the sharpened wire tip was examined by observing the tip of the sharpened wire under an electronic magnifying microscope at 400–500 magnification. A minimum of 90% of the fibers had a diameter ≤0.08 mm at a distance of 0.5 mm from the tip, meeting the requirements described in the following Examples and Comparative Examples. The Chinese national standard GB / T 36391-2018, "Antibacterial Toothbrush," stipulates that a minimum of 70% of the fibers had a diameter ≤0.04 mm at a distance of 0.01 mm from the tip, and a minimum of 90% of the fibers had a diameter ≤0.08 mm at a distance of 0.5 mm from the tip, meeting the requirements.

[0102] Comparative Example 1

[0103] Fiber preparation

[0104] 8 wt% of graphene is added to PBT raw material particles, mixed and granulated to obtain graphene masterbatch.

[0105] 5 wt % of graphene masterbatch was added to the PBT raw material particles, mixed, extruded and spun to obtain fibers with an actual added graphene content of 0.4 wt %, which is the fiber of Comparative Example 1.

[0106] The tip of the fiber of Comparative Example 1 was immersed in a sodium hydroxide aqueous solution with a concentration of 30% to 70% for 20 to 30 minutes to obtain the sharpened wire of Comparative Example 1.

[0107] Fiber test results

[0108] After testing, the percentage of the fibers with a diameter of 0.5 mm from the tip of the sharpened wire in comparative example 1 that was ≤ 0.08 mm reached more than 90%, meeting the requirements.

[0109] The single fiber recovery rate of the fiber of comparative example 1 was tested to be 66.56%, which met the requirements of GB 19342-2013.

[0110] The antibacterial performance test results are shown in Tables 1A and 1B. Tables 1A and 1B show that the antibacterial rates of the fiber of Comparative Example 1 against Escherichia coli 8099 and Staphylococcus aureus ATCC 6538 were 33% and 41%, respectively, which do not meet the requirements of GB / T 36391-2018.

[0111] Table 1A Antibacterial rate test results of the fiber of comparative example 1 against Escherichia coli 8099

[0112]

[0113] Table 1B Antibacterial rate test results of the fiber of comparative example 1 against Staphylococcus aureus ATCC 6538

[0114]

[0115] Comparative Example 2

[0116] Fiber preparation

[0117] The graphene masterbatch was prepared using the same method as in Comparative Example 1.

[0118] 10 wt% of graphene masterbatch was added to the PBT raw material particles, mixed, extruded and spun to obtain fibers with an actual added graphene content of 0.8 wt%, which is the fiber of Comparative Example 2.

[0119] The sharpened wire of Comparative Example 2 was prepared from the fibers of Comparative Example 2 using the same method used to prepare the sharpened wire of Comparative Example 1 from the fibers of Comparative Example 1.

[0120] Fiber test results

[0121] The test showed that the percentage of the fibers with a diameter of ≤0.08 mm at a distance of 0.5 mm from the tip of the sharpened wire in Comparative Example 2 did not reach more than 90%, which did not meet the requirements. Figure 7 The figures show the ends of several sharpened wires of the comparative examples of the present application observed under an electron magnifying glass.

[0122] The single fiber recovery rate of the fiber of Comparative Example 2 was tested to be 57.56%, which did not meet the requirements of GB 19342-2013.

[0123] The antibacterial performance test results are shown in Tables 2A to 2E. Tables 2A to 2E show that the fiber of Comparative Example 2 had an antibacterial rate of 62% against Escherichia coli 8099 and 99% against Staphylococcus aureus ATCC 6538, with the antibacterial rate against Staphylococcus aureus meeting the requirements of GB / T 36391-2018. The antibacterial rate against Candida albicans ATC 10231 was 74%, against beta-hemolytic Streptococcus CMCC 32210 was 77%, and against Klebsiella pneumoniae ATCC 4352 was 36%.

[0124] Table 2A Antibacterial rate test results of the fiber of comparative example 2 against Escherichia coli 8099

[0125]

[0126] Table 2B Antibacterial rate test results of the fiber of comparative example 2 against Staphylococcus aureus ATCC 6538

[0127]

[0128] Table 2C Antibacterial rate test results of the fiber of comparative example 2 against Candida albicans ATCC 10231

[0129]

[0130] Table 2D Antibacterial rate test results of the fiber of comparative example 2 against beta-hemolytic Streptococcus CMCC 32210

[0131]

[0132]

[0133] Table 2E Antibacterial rate test results of the fiber of comparative example 2 against Klebsiella pneumoniae ATCC 4352

[0134]

[0135] Comparative Example 3

[0136] Fiber preparation

[0137] The graphene masterbatch was prepared using the same method as in Comparative Example 1.

[0138] 15 wt% of graphene masterbatch was added to the PBT raw material particles, mixed, extruded and spun to obtain fibers with an actual added graphene content of 1.2 wt%, which is the fiber of Comparative Example 3.

[0139] The sharpened wire of Comparative Example 3 was prepared from the fibers of Comparative Example 3 using the same method as that used to prepare the sharpened wire of Comparative Example 1 from the fibers of Comparative Example 1.

[0140] Fiber test results

[0141] The test showed that the percentage of the fibers with a diameter of ≤0.08 mm at a distance of 0.5 mm from the tip of the sharpened wire in Comparative Example 3 did not reach more than 90%, which did not meet the requirements.

[0142] The single fiber recovery rate of the fiber of Comparative Example 3 was tested to be 53.78%, which did not meet the requirements of GB 19342-2013.

[0143] The antibacterial performance test results are shown in Tables 3A to 3E. Tables 3A to 3E show that the fiber of Comparative Example 3 had an antibacterial rate of 58% against Escherichia coli 8099 and 99% against Staphylococcus aureus ATCC 6538, with the antibacterial rate against Staphylococcus aureus meeting the requirements of GB / T 36391-2018. The antibacterial rate against Candida albicans ATC 10231 was 78%, against beta-hemolytic Streptococcus CMCC 32210 was 76%, and against Klebsiella pneumoniae ATCC 4352 was 40%.

[0144] Table 3A Antibacterial rate test results of the fiber of comparative example 3 against Escherichia coli 8099

[0145]

[0146] Table 3B Antibacterial rate test results of the fiber of comparative example 3 against Staphylococcus aureus ATCC 6538

[0147]

[0148] Table 3C Antibacterial rate test results of the fiber of comparative example 3 against Candida albicans ATCC 10231

[0149]

[0150]

[0151] Table 3D Antibacterial rate test results of the fiber of comparative example 3 against beta-hemolytic Streptococcus CMCC 32210

[0152]

[0153] Table 3E Antibacterial rate test results of the fiber of comparative example 3 against Klebsiella pneumoniae ATCC 4352

[0154]

[0155] It can be seen that although 1.2 wt% of graphene is added in Comparative Example 3, the overall antibacterial rate of the fiber is not significantly improved compared with Comparative Example 2 in which 0.8 wt% of graphene is added.

[0156] Example 1

[0157] Fiber preparation

[0158] The graphene masterbatch was prepared using the same method as in Comparative Example 1.

[0159] 10 wt% graphene masterbatch was added to PBT raw material particles to serve as the shell material; PBT raw material without the graphene masterbatch was used as the core material. The shell and core materials were extruded and spun through a double-barrel extruder to obtain a core-shell structure fiber with a shell graphene content of 0.8 wt%, which is the fiber of Example 1.

[0160] The sharpened wire of Example 1 was prepared from the fibers of Example 1 using the same method as that used to prepare the sharpened wire of Comparative Example 1 from the fibers of Comparative Example 1.

[0161] Fiber test results

[0162] Figure 8 Figure 2 shows a cross section of the fiber of Example 1 observed under an electron microscope at 400-500 magnification. It can be seen that the fiber of Example 1 exhibits a clear double-layer structure, which consists of a core 110 and a shell 120, wherein the cross-sectional shape of the core 110 is close to a circle. Five fibers of Example 1 were selected and the diameter D' of the core 110 and the diameter D of the shell 120 (which is also the diameter of the fiber 100) were measured. Figure 2 The ratio D' / D of the core diameter D' to the shell diameter D was calculated. The results are shown in Table 4. It can be seen that the average value of the core diameter / shell diameter ratio of the fiber of Example 1 is 0.695.

[0163] Table 4 Measurement results of the core diameter and shell diameter of the fiber of Example 1

[0164]

[0165]

[0166] Based on this, the core diameter / shell diameter ratio D′ / D of Example 1 can be used to estimate that the cross-sectional area of ​​the shell of the fiber of Example 1 accounts for 1–(D′ / D)2, assuming that the fiber and core cross-section of Example 1 are circular. It can also be further estimated that the mass ratio of the shell of the fiber of Example 1 is also approximately 1–(D′ / D). 2 , it is calculated that the graphene content of the entire fiber of Example 1 is approximately (0.8wt%×(1–(D′ / D)2))≈0.41%.

[0167] After testing, the sharpened wires of Example 1 had a diameter of 0.5 mm at the tip of the wire that was less than or equal to 0.08 mm, accounting for more than 90%, which met the requirements.

[0168] After testing, the single fiber recovery rate of the fiber of Example 1 was 64.34%, which met the requirements of GB 19342-2013.

[0169] The antibacterial performance test results are shown in Tables 5A and 5B. Tables 5A and 5B show that the fiber of Example 1 has an antibacterial rate of 99% against Escherichia coli 8099 and an antibacterial rate of >99% against Staphylococcus aureus ATCC 6538, both meeting the requirements of GB / T 36391-2018.

[0170] Table 5A Antibacterial rate test results of the fiber of Example 1 against Escherichia coli 8099

[0171]

[0172] Table 5B Antibacterial rate test results of the fiber of Example 1 against Staphylococcus aureus ATCC 6538

[0173]

[0174] Example 2

[0175] Fiber preparation

[0176] The graphene masterbatch was prepared using the same method as in Comparative Example 1.

[0177] 20 wt% graphene masterbatch was added to the PBT raw material particles as the shell material; and PBT raw material without the graphene masterbatch was used as the core material. Using the same method as used to prepare the fiber of Example 1 from the shell and core materials of Example 1, a core-shell structured fiber with a shell graphene content of 1.6 wt% (the overall graphene content of the fiber was approximately 0.83%) was prepared from the shell and core materials of Example 2, which is the fiber of Example 2.

[0178] The sharpened wire of Example 2 was prepared from the fibers of Example 2 using the same method as that used to prepare the sharpened wire of Comparative Example 1 from the fibers of Comparative Example 1.

[0179] Fiber test results

[0180] After testing, the sharpened wires of Example 2 had a diameter of 0.5 mm at the tip of the wire that was less than or equal to 0.08 mm, accounting for more than 90%, which met the requirements.

[0181] After testing, the single fiber recovery rate of the fiber of Example 2 was 61.56%, which met the requirements of GB 19342-2013.

[0182] The antibacterial performance test results are shown in Tables 6A and 6B. Tables 6A and 6B show that the fiber of Example 2 has an antibacterial rate of >99% against Escherichia coli 8099 and >99% against Staphylococcus aureus ATCC 6538, both meeting the requirements of GB / T 36391-2018.

[0183] Table 6A Antibacterial rate test results of the fiber of Example 2 against Escherichia coli 8099

[0184]

[0185]

[0186] Table 6B Antibacterial rate test results of the fiber of Example 2 against Staphylococcus aureus ATCC 6538

[0187]

[0188] Example 3

[0189] Fiber preparation

[0190] The graphene masterbatch was prepared using the same method as in Comparative Example 1.

[0191] 5 wt% graphene masterbatch was added to the PBT raw material particles as the shell material; and PBT raw material without the graphene masterbatch was used as the core material. Using the same method as used to prepare the fiber of Example 1 from the shell and core materials of Example 1, a core-shell structured fiber with a shell graphene content of 0.4 wt% (the overall graphene content of the fiber was approximately 0.21%) was prepared from the shell and core materials of Example 3. This fiber is referred to as Example 3.

[0192] The sharpened wire of Example 3 was prepared from the fibers of Example 3 using the same method as that used to prepare the sharpened wire of Comparative Example 1 from the fibers of Comparative Example 1.

[0193] Fiber test results

[0194] After testing, the sharpened wires of Example 3 had a diameter of 0.5 mm at the tip of the wire that was less than or equal to 0.08 mm, accounting for more than 90%, which met the requirements.

[0195] After testing, the single fiber recovery rate of the fiber of Example 3 was 67.12%, which met the requirements of GB 19342-2013.

[0196] The antibacterial performance test results are shown in Tables 6A and 6B. Tables 6A and 6B show that the fiber of Example 3 has an antibacterial rate of 72% against Escherichia coli 8099 and an antibacterial rate of 99% against Staphylococcus aureus ATCC 6538. The antibacterial rate against Staphylococcus aureus meets the requirements of GB / T 36391-2018.

[0197] Example 4 Effect of core and shell diameters on fiber properties

[0198] As shown in Comparative Examples 1-3 and Examples 1-3, as the amount of graphene added increases, the single filament recovery rate of the fiber decreases.

[0199] Example 4 studies the lower limit of the fiber shell cross-sectional area ratio (i.e., the upper limit of the core diameter to shell diameter ratio) when the addition ratio of graphene masterbatch in the shell is 10%, 20%, and 30%, respectively, in order to meet the condition that the single fiber recovery rate is above 60%.

[0200] In Example 4, graphene masterbatch was prepared using the same method as Comparative Examples 1-3 and Examples 1-3.

[0201] In Example 4, graphene masterbatch in various proportions as listed in Table 7 was added to PBT raw material pellets to serve as the shell material for Examples 4A–4D; and PBT raw material without the graphene masterbatch was used as the core material for Examples 4A–4D. Using a method similar to that used to prepare the fibers of Examples 1–3 from the shell and core materials of Examples 1–3, adjusting the ratio of core to shell diameter, core-shell structured fibers with varying graphene contents and varying core-to-shell diameter ratios were prepared from the shell and core materials of Examples 4A–4D, respectively. These fibers, i.e., the fibers of Examples 4A–4D, were obtained.

[0202] The test results of the single fiber recovery rates of the fibers of Examples 4A-4D are shown in Table 7.

[0203] Table 7

[0204]

[0205] As shown in Table 7, as the ratio of the core diameter to the shell diameter increases (the fiber shell cross-sectional area ratio decreases), the addition ratio of the graphene masterbatch can be increased accordingly to obtain a fiber with sufficient single-filament recovery rate; conversely, if the addition ratio of the graphene masterbatch needs to be reduced, a lower core diameter to shell diameter ratio (a higher fiber shell cross-sectional area ratio) can be selected to ensure that the fiber has a sufficient single-filament recovery rate.

[0206] Specifically:

[0207] - With respect to the relationship between the core diameter / shell diameter ratio D′ / D and the shell graphene content w, as shown in Examples 4A and 4B, for example, when the core diameter / shell diameter ratio D′ / D is approximately 0.5 and / or the shell graphene content w is approximately 1.6 wt% or less, for example, 0.8 wt% to 1.6 wt%, sufficient single filament recovery can be achieved. As shown in Example 4C, for example, when the core diameter / shell diameter ratio D′ / D is approximately 0.5 and / or the shell graphene content w is approximately 2.4 wt% or less, for example, 0.8 wt% to 2.4 wt%, sufficient single filament recovery can be achieved. Alternatively, based on a combination of Examples 4B and 4C, a sufficient single filament recovery can be achieved when the core diameter / shell diameter ratio D′ / D minus 40% is approximately 6.25 times or more of the shell graphene content w.

[0208] - With respect to the relationship between the fiber shell cross-sectional area ratio 1-(D′ / D)2 and the shell graphene content w, as shown in Examples 4A and 4B, for example, when the fiber shell cross-sectional area ratio 1-(D′ / D)2 is approximately 0.75 and / or the shell graphene content w is approximately 1.6 wt% or less, for example, 0.8 wt% to 1.6 wt%, sufficient single fiber recovery rate can be obtained; as shown in Example 4C, for example, when the fiber shell cross-sectional area ratio 1-(D′ / D)2 is approximately 0.75 and / or the shell graphene content w is approximately 1.6 wt% or less, for example, 0.8 wt% to 1.6 wt%. 2 The ratio of the cross-sectional area of ​​the fiber shell to that of the shell is about 0.7, and / or the graphene content w of the shell is about 2.4 wt% or less, for example, 0.8 wt% to 2.4 wt%, to obtain a sufficient single filament recovery rate; or, based on Examples 4B and 4C, 85% minus the proportion of the fiber shell cross-sectional area 1–(D′ / D)2 is about 6.25 times or more of the graphene content w of the shell, to obtain a sufficient single filament recovery rate.

[0209] The above-mentioned embodiments are only preferred embodiments of the present application and cannot be used to limit the scope of protection of the present application. Any non-substantial changes and replacements made by technicians in this field based on the present application shall fall within the scope of protection required by the present application.

Claims

1. A fiber for oral care, characterized in that include: core; as well as a shell portion, surrounding the core portion, The weight ratio of graphene in the shell portion is greater than the weight ratio of graphene in the core portion.

2. A method for preparing oral care fiber, characterized in that: include: providing a core; as well as providing a shell portion surrounding the core portion, The weight ratio of graphene in the shell portion is greater than the weight ratio of graphene in the core portion.

3. The fiber or the method for preparing the fiber according to any one of claims 1 to 2, wherein: The shell comprises 0.4-4.0 wt%, in particular 0.6-4.0 wt%, 0.8-4.0 wt%, 0.4-3.0 wt%, 0.6-3.0 wt%, 0.8-3.0 wt%, 0.4-2.4 wt%, 0.6-2.4 wt%, 0.8-2.4 wt%, 0.4-1.6 wt%, 0.6-1.6 wt%, or 0.8-1.6 wt% graphene; and / or The fibers comprise 0.2–2.0 wt%, in particular 0.3–2.0 wt%, 0.4–2.0 wt%, 0.5–2.0 wt%, 0.2–1.7 wt%, 0.3–1.7 wt%, 0.4–1.7 wt%, 0.5–1.7 wt%, 0.2–1.3 wt%, 0.3–1.3 wt%, 0.4–1.3 wt%, 0.5–1.3 wt%, 0.2–0.8 wt%, 0.3–0.8 wt%, 0.4–0.8 wt%, or 0.5–0.8 wt% of graphene; Optionally, the graphene is graphene oxide, reduced graphene, or a combination thereof.

4. The fiber or the method for preparing the fiber according to any one of claims 1 to 3, wherein: the diameter of the core is 40% to 90%, in particular 45% to 90%, 50% to 90%, 55% to 90%, 40% to 80%, 45% to 80%, 50% to 80%, 55% to 80%, 40% to 75%, 45% to 75%, 50% to 75%, or 55% to 75% of the diameter of the shell; and / or The cross-sectional area of ​​the shell is 20% to 90%, specifically 30% to 90%, 35% to 90%, 40% to 90%, 20% to 80%, 30% to 80%, 35% to 80%, 40% to 80%, 20% to 75%, 30% to 75%, 35% to 75%, or 40% to 75% of the cross-sectional area of ​​the fiber.

5. The fiber or the method for preparing the fiber according to any one of claims 1 to 2, wherein: The diameter of the core is 45% to 90%, in particular 50% to 90%, of the diameter of the shell, and the shell comprises 0.8 wt % to 4.0 wt % of graphene; Optionally, the percentage of the diameter of the core relative to the diameter of the shell minus 40% is greater than 6.25 times the weight percentage of the graphene in the shell; and / or The cross-sectional area of ​​the shell portion is 20% to 80%, in particular 20% to 75%, of the cross-sectional area of ​​the fiber, and the shell portion comprises 0.8 wt % to 4.0 wt % of graphene; Optionally, the percentage of 85% minus the cross-sectional area of ​​the shell portion relative to the cross-sectional area of ​​the fiber is greater than 6.25 times the weight percentage of the graphene in the shell portion.

6. The fiber or the method for preparing the fiber according to any one of claims 1 to 5, wherein: The core comprises or consists of polymer fibers, in particular polyolefin fibers, polyfluoroolefin fibers, polyester fibers, or polyamide fibers; and / or The shell comprises polymer fibers, in particular polyolefin fibers, polyfluoroolefin fibers, polyester fibers, or polyamide fibers, Optionally, The core comprises or consists of polyethylene, polypropylene, polytetrafluoroethylene, polyethylene terephthalate, polybutylene terephthalate, nylon N6, nylon N66, nylon 610, nylon 612, nylon 1010, or a combination thereof; and / or The shell includes polyethylene, polypropylene, polytetrafluoroethylene, polyethylene terephthalate, polybutylene terephthalate, nylon N6, nylon N66, nylon 610, nylon 612, nylon 1010, or a combination thereof.

7. The fiber or the method for preparing the fiber according to any one of claims 1 to 6, wherein: The core portion includes a protrusion protruding from the shell portion in the extending direction of the fiber; Optionally, the length of the protrusion in the extension direction is at least 5%, in particular at least 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, or 50% of the length of the core in the extension direction; Optionally, the protrusion 111 is in a shape of a column, a cone, a frustum, or a combination thereof.

8. The fiber or the method for preparing the fiber according to any one of claims 1 to 7, wherein: The fiber includes a tip portion having a cross-sectional area perpendicular to the extending direction that decreases in the extending direction of the fiber; Optionally, the length of the tip portion in the extension direction is at least 5%, in particular at least 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, or 50% of the length of the fiber in the extension direction; Optionally, the tip portion is shaped like a cone, a truncated cone, or a combination thereof. Optionally, the diameter of the tip portion at a distance of 0.01 mm from one end thereof is less than 0.04 mm. Optionally, the diameter of the tip portion at a distance of 0.5 mm from one end thereof is less than 0.08 mm.

9. The fiber or the method for preparing the fiber according to any one of claims 1 to 8, wherein: The length of the fibers is from 10 mm to 35.0 mm, in particular from 15 mm to 20 mm, more in particular from 16 mm to 17 mm, or in particular from 10 mm to 15 mm, more in particular from 11 mm to 13 mm, or in particular from 20 mm to 34 mm, more in particular from 26 mm to 30 mm; and / or The fibers have a diameter of 0.075 to 0.25 mm, in particular 0.10 to 0.18 mm, more in particular 0.11 to 0.14 mm, more in particular 0.12 to 0.13 mm, or in particular 0.14 to 0.16 mm, more in particular 0.145 to 0.155 mm, or in particular 0.16 to 0.18 mm, more in particular 0.17 to 0.18 mm; and / or The cross section of the fiber perpendicular to its extension direction is circular or non-circular, in particular circular, elliptical, convex polygonal, or concave polygonal; and / or The core and / or shell also includes an antimicrobial agent; Optionally, the shell further comprises an antimicrobial agent; Optionally, the antimicrobial agent is silver ion, zinc ion, or activated carbon; and / or The fiber has a single fiber recovery rate of 60% or more as measured by the method of GB 19342-2013; and / or The fiber has an antibacterial rate of 90% or more against Escherichia coli 8099 according to the method of GB / T 36391-2018; and / or The fiber has an antibacterial rate of 90% or more against Staphylococcus aureus ATCC 6538 as tested according to the method of GB / T 36391-2018; and / or the fiber has an antibacterial rate of 90% or more against Candida albicans ATC 10231 as tested according to the method of GB / T 36391-2018; and / or the fiber has an antibacterial rate of 90% or more against beta-hemolytic Streptococcus CMCC 32210 as tested according to the method of GB / T 36391-2018; and / or The fiber has an antibacterial rate of more than 90% against Klebsiella pneumoniae ATCC 4352 when tested according to the method of GB / T 36391-2018.

10. An oral care product, characterized in that: The oral care fiber comprises the oral care fiber according to any one of claims 1 or 3 to 9 or the oral care fiber prepared by the preparation method according to any one of claims 2 to 9; Optionally, the oral care product is a tooth cleaning product, in particular a toothbrush or dental floss, more in particular a toothbrush.

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