WO2021125029A1 - シート状物およびその製造方法 - Google Patents
シート状物およびその製造方法 Download PDFInfo
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- WO2021125029A1 WO2021125029A1 PCT/JP2020/046006 JP2020046006W WO2021125029A1 WO 2021125029 A1 WO2021125029 A1 WO 2021125029A1 JP 2020046006 W JP2020046006 W JP 2020046006W WO 2021125029 A1 WO2021125029 A1 WO 2021125029A1
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- polymer elastic
- sheet
- precursor
- elastic body
- fiber
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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
- D06N3/145—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes two or more layers of polyurethanes
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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
- D06N3/146—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes characterised by the macromolecular diols used
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2201/00—Chemical constitution of the fibres, threads or yarns
- D06N2201/02—Synthetic macromolecular fibres
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- D06N2205/00—Condition, form or state of the materials
- D06N2205/20—Cured materials, e.g. vulcanised, cross-linked
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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/12—Permeability or impermeability properties
- D06N2209/126—Permeability to liquids, absorption
- D06N2209/128—Non-permeable
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- D06N2209/00—Properties of the materials
- D06N2209/16—Properties of the materials having other properties
- D06N2209/1635—Elasticity
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- D06N2209/00—Properties of the materials
- D06N2209/16—Properties of the materials having other properties
- D06N2209/1685—Wear resistance
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- D06N2211/00—Specially adapted uses
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- D06N2211/00—Specially adapted uses
- D06N2211/12—Decorative or sun protection articles
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- D06N2211/00—Specially adapted uses
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- D06N2211/26—Vehicles, transportation
- D06N2211/263—Cars
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- D06N2211/00—Specially adapted uses
- D06N2211/12—Decorative or sun protection articles
- D06N2211/26—Vehicles, transportation
- D06N2211/265—Trains
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- D06N2211/00—Specially adapted uses
- D06N2211/12—Decorative or sun protection articles
- D06N2211/26—Vehicles, transportation
- D06N2211/267—Aircraft
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- D06N2213/00—Others characteristics
- D06N2213/03—Fibrous web coated on one side with at least two layers of the same polymer type, e.g. two coatings of polyolefin
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- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/24—Polyamides; Polyurethanes
- D06P3/241—Polyamides; Polyurethanes using acid dyes
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- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
- D06P3/54—Polyesters using dispersed dyestuffs
Definitions
- the present invention relates to a sheet-like material and a method for producing the same, particularly a sheet-like material having excellent flexibility, chemical resistance and dyeing resistance, and a method for producing the same.
- Sheet-like materials mainly composed of fibrous base materials such as non-woven fabrics and polyurethane have excellent characteristics not found in natural leather, and are widely used in various applications such as artificial leather.
- sheet-like materials using polyester-based fibrous base materials have excellent moldability, and therefore their use has been expanding year by year for clothing, upholstery, automobile interior materials, and the like.
- the fibrous base material is impregnated with an organic solvent solution of polyurethane, and then the obtained fibrous base material is immersed in water or an aqueous solution of an organic solvent which is a non-solvent of polyurethane.
- an organic solvent which is the solvent of polyurethane a water-miscible organic solvent such as N, N-dimethylformamide (hereinafter, may also be referred to as “DMF”) is used.
- DMF water-miscible organic solvent
- organic solvents are generally highly harmful to the human body and the environment, there is a strong demand for a method that does not use organic solvents in the production of sheet-like products.
- a method of using a water-dispersed polyurethane in which a polyurethane resin is dispersed in water is being studied instead of the conventional organic solvent-based polyurethane.
- a water-dispersible polyurethane liquid containing a foaming agent has been applied to a fibrous base material such as a sheet made of a cloth such as a non-woven fabric.
- a method has been proposed in which a gas is generated in the polyurethane by applying and heating to make the structure of the polyurethane in the fibrous substrate a porous structure (see Patent Document 1).
- a water-dispersible polyurethane liquid containing a foaming agent is applied to a fibrous base material containing ultrafine fiber-expressing fibers, and then ultrafine fibers are expressed from the ultrafine fiber-expressing fibers, and then the water-dispersed polyurethane liquid is again expressed.
- a method of granting is proposed. (See Patent Document 2.).
- the size of the polyurethane resin is reduced by impregnating the fibrous base material in a solution containing water-dispersible polyurethane and a thickener and immersing it in hot water, and the gripping force of the confounded portion of the fibers by the water-dispersible polyurethane is increased.
- a method for lowering the amount has been proposed (see Patent Document 3).
- the coagulation method of the organic solvent-based polyurethane liquid is a so-called wet coagulation method in which polyurethane molecules dissolved in an organic solvent are solvent-substituted with water to coagulate. Is formed. Therefore, even when polyurethane is impregnated in the fibrous base material and solidified, the adhesive area between the fiber and polyurethane is reduced, resulting in a soft sheet-like material.
- the mainstream of water-dispersed polyurethane is a so-called moist heat coagulation method in which the hydrated state of the water-dispersed polyurethane dispersion is disrupted by heating and the polyurethane emulsions are coagulated to coagulate.
- the polyurethane film structure to be obtained is a dense non-porous film. Therefore, the fibrous base material and the polyurethane are closely adhered to each other, and the entangled portion of the fibers is strongly gripped, so that the texture becomes hard.
- Patent Document 1 by making the water-dispersible polyurethane porous, the adhesive area between the fiber and the polyurethane is reduced, the gripping force at the entangled point of the fiber is weakened, and the tactile sensation is flexible. It is possible to obtain a sheet-like material having a texture, but it tends to be less flexible as compared with the case where an organic solvent-based polyurethane is added.
- Patent Document 3 by making the water-dispersible polyurethane porous, the adhesive area between the fiber and the polyurethane is reduced, the gripping force at the entanglement point of the fiber is weakened, and the tactile sensation is flexible. It is possible to obtain a sheet-like material having a good texture, but since a divalent cation-containing inorganic salt is used as a heat-sensitive coagulation adjuster, the occurrence of impregnation unevenness due to gelation of the impregnating liquid is a problem.
- an object of the present invention is to provide a sheet-like material having excellent flexibility, chemical resistance and dyeing resistance, and a method for producing the same, in view of the background of the above-mentioned prior art.
- the present inventors have undergone a first polymer elastic body precursor impregnation step, an ultrafine fiber expression step, and a second polymer elastic precursor precursor impregnation step. It has been found that flexibility, chemical resistance and dyeing resistance can be improved by giving a specific functional group to the polymer elastic body by producing a sheet-like material or the like. Furthermore, it was also found that this sheet-like material can reduce the amount of fiber waste during washing.
- the sheet-like material of the present invention is a sheet-like material having a fibrous base material made of ultrafine fibers and a polymer elastic body, and the average single fiber diameter of the ultrafine fibers is 0.1 ⁇ m or more and 10.0 ⁇ m or less.
- the above-mentioned polymer elastic body has a hydrophilic group and an N-acylurea bond and / or an isourea bond, and satisfies the following conditions 1 and 2.
- Condition 1 JIS L1096: 2010
- the longitudinal rigidity specified by the A method (45 ° cantilever method) described in "8.21 Rigidity" of "Fabric test method for woven fabrics and knits" is 40 mm.
- the polymer elastic body contains two types, a polymer elastic body A and a polymer elastic body B different from the polymer elastic body A.
- the tensile strength of the sheet-like material when wet is 75% or more when dry.
- the tensile strength and elongation of the sheet-like material when wet is 100% or more when dry.
- condition 3 is further satisfied in the sheet-like material.
- Condition 3 When the raised surface of the sheet-like material is placed on a hot plate heated to 150 ° C. and pressed with a pressing load of 2.5 kPa for 10 seconds, the retention rate of the L value is 90% or more and 100% or less. is there.
- condition 4 is further satisfied in the sheet-like material.
- Condition 4 At the time of the washing test according to the ISO 6330 C4N method, the washing test of one sheet-like material is carried out, and after the test, the fiber debris adhering to the collection bag attached to the drain hose is captured by using a membrane filter. The amount of fiber waste when collected is 10.0 (mg / sheet-like material 100 cm 2 ) or less.
- the method for producing a sheet-like product of the present invention includes the following steps (1) to (3) in this order.
- a fibrous base material made of ultrafine fiber-expressing fibers is impregnated with an aqueous dispersion containing a polymer elastic precursor having a hydrophilic group, a monovalent cation-containing inorganic salt, and a cross-linking agent.
- the temperature of the fibrous base material impregnated with the aqueous dispersion is set to 100 ° C. or higher and 180 ° C. or lower and heat-drying treatment is performed to form a polymer elastic body.
- the first polymer elastic precursor wherein the content of the monovalent cation-containing inorganic salt in the aqueous dispersion is 10 parts by mass or more and 100 parts by mass or less with respect to 100 parts by mass of the polymer elastic precursor.
- Impregnation step (2) Ultrafine fiber expression step of expressing ultrafine fibers from the ultrafine fiber-expressing fibers to form a fibrous substrate composed of the ultrafine fibers (3) Fibrous substrate composed of the ultrafine fibers Is impregnated with an aqueous dispersion containing a polymer elastic precursor having a hydrophilic group, a monovalent cation-containing inorganic salt, and a cross-linking agent, and then impregnated with the aqueous dispersion.
- the second polymer elastic precursor impregnation step in which the content of the inorganic salt is 10 parts by mass or more and 100 parts by mass or less with respect to 100 parts by mass of the polymer elastic precursor.
- the polymer elastic precursor impregnation step of the first polymer elastic precursor impregnation step and the polymer elastic precursor precursor impregnation step of the second polymer elastic precursor precursor step are the same polymer elastic precursor.
- the polymer elastic precursor contains a polyether diol and / or a polycarbonate diol.
- the polymer elastic precursor in the first polymer elastic precursor impregnation step is the polymer elastic precursor A, and the first polymer elastic precursor is described above.
- the polymer elastic precursor used in the polymer elastic precursor in the step of impregnating the polymer elastic precursor of No. 2 is a polymer elastic precursor B different from the polymer elastic precursor A.
- the polymer elastic precursor A contains a polyether diol as a constituent component.
- the polymer elastic precursor B contains a polycarbonate diol as a constituent component.
- the cross-linking agent is a carbodiimide-based cross-linking agent and / or a blocked isocyanate cross-linking agent.
- the monovalent cation-containing inorganic salt is sodium chloride and / or sodium sulfate.
- a sheet-like material having excellent flexibility, chemical resistance and dyeing resistance can be obtained.
- the sheet-like material of the present invention is a sheet-like material having a fibrous base material made of ultrafine fibers and a polymer elastic body, and the average single fiber diameter of the ultrafine fibers is 0.1 ⁇ m or more and 10.0 ⁇ m or less.
- the above-mentioned polymer elastic body has a hydrophilic group and an N-acylurea bond and / or an isourea bond, and satisfies the following conditions 1 and 2.
- Condition 1 JIS L1096: 2010
- the longitudinal rigidity specified by the A method (45 ° cantilever method) described in "8.21 Rigidity" of "Fabric test method for woven fabrics and knits" is 40 mm.
- N, N-dimethylformamide or more Method E according to "8.19 Abrasion strength and frictional discoloration" of JIS L1096: 2010 "Fabric test method for woven fabrics and knitted fabrics” after immersion in N, N-dimethylformamide.
- the wear test is grade 4 or higher, and the wear loss is 25 mg or less. As long as it does not exceed the gist, it is not limited to the scope described below.
- the sheet-like material of the present invention has a fibrous base material made of ultrafine fibers.
- Examples of the resin that can be used for the ultrafine fibers include polyester resin and polyamide resin from the viewpoint of excellent durability, particularly mechanical strength, heat resistance and chemical resistance.
- polyester resin when a polyester resin is used as the resin used for the ultrafine fibers, polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate and copolymers thereof can be used. Further, the polyester resin can be obtained from, for example, a dicarboxylic acid and / or an ester-forming derivative thereof and a diol.
- Examples of the dicarboxylic acid and / or its ester-forming derivative used in the polyester resin include terephthalic acid, isophthalic acid, 2,6-naphthalenedicarboxylic acid, diphenyl-4,4'-dicarboxylic acid and its ester-forming derivative. And so on.
- the ester-forming derivative referred to in the present invention is a lower alkyl ester of a dicarboxylic acid, an acid anhydride, an acyl chloride or the like. Specifically, methyl ester, ethyl ester, hydroxy ethyl ester and the like are preferably used.
- a more preferred embodiment of the dicarboxylic acid and / or ester-forming derivative thereof used in the present invention is terephthalic acid and / or a dimethyl ester thereof.
- diol used in the polyester resin examples include ethylene glycol, 1,3-propanediol, 1,4-butanediol, cyclohexanedimethanol and the like. Of these, ethylene glycol is preferably used.
- polyamide 6 polyamide 66, polyamide 56, polyamide 610, polyamide 11, polyamide 12, and copolymerized polyamide can be used.
- the resin used for the ultrafine fibers includes inorganic particles such as titanium oxide particles, a lubricant, a pigment, a heat stabilizer, an ultraviolet absorber, and conductivity as long as the object of the present invention is achieved according to various purposes. It can contain agents, heat storage agents, antibacterial agents and the like.
- the resin used for the ultrafine fibers of the present invention contains a component derived from a biomass resource.
- the component derived from the biomass resource when a polyester resin is used as the resin used for the ultrafine fibers, the component derived from the biomass resource may be used as the component dicarboxylic acid or its ester-forming derivative.
- a component derived from a biomass resource may be used as the diol, but from the viewpoint of reducing the environmental load, it is preferable to use a component derived from the biomass resource for both the dicarboxylic acid or its ester-forming derivative and the diol.
- the polyamide 56 and the polyamide can be obtained from the viewpoint of economically advantageous availability of the raw material derived from the biomass resource and the physical characteristics of the fiber.
- 610 and polyamide 11 are preferably used.
- the cross-sectional shape of the ultrafine fiber either a round cross section or a deformed cross section can be adopted.
- Specific examples of the irregular cross section include polygons such as ellipses, flats, and triangles, sectors, and crosses.
- the average single fiber diameter of the ultrafine fibers is 0.1 ⁇ m or more and 10 ⁇ m or less.
- the sheet-like material can be made more flexible. Further, when the sheet-like material has fluff, the quality of the fluff can be improved.
- the average single fiber diameter of the ultrafine fibers is 0.1 ⁇ m or more, preferably 0.3 ⁇ m or more, more preferably 0.7 ⁇ m or more, a sheet-like material having excellent color development after dyeing can be obtained. .. Further, when the sheet-like material has fluff, it is possible to improve the ease of dispersing and the ease of handling of the ultrafine fibers existing in the bundle shape when the fluff treatment by buffing is performed.
- the average single fiber diameter referred to in the present invention is measured by the following method. That is, (1) The cross section of the obtained sheet-like material cut in the thickness direction is observed with a scanning electron microscope (SEM). (2) The fiber diameters of any 50 ultrafine fibers in the observation surface are measured in three directions in each ultrafine fiber cross section. However, when ultrafine fibers having a modified cross section are used, the cross-sectional area of the single fiber is first measured, and the diameter of the circle having the cross-sectional area is calculated by the following formula. The diameter obtained from this is taken as the single fiber diameter of the single fiber.
- SEM scanning electron microscope
- Single fiber diameter ( ⁇ m) (4 ⁇ (cross-sectional area of single fiber ( ⁇ m 2 )) / ⁇ ) 1/2 (3) Calculate the arithmetic mean value ( ⁇ m) of the total of 150 points obtained, and round off to the second decimal place.
- the fibrous base material used in the present invention comprises the above-mentioned ultrafine fibers. It is permissible for the fibrous base material to be a mixture of ultrafine fibers made of different raw materials.
- a non-woven fabric formed by entwining each of the above-mentioned ultrafine fibers or a non-woven fabric formed by entwining fiber bundles of ultrafine fibers can be used.
- a non-woven fabric formed by entwining fiber bundles of ultrafine fibers is preferably used from the viewpoint of strength and texture of a sheet-like material.
- a non-woven fabric in which the ultrafine fibers constituting the fiber bundle of the ultrafine fibers are appropriately separated from each other and has voids is preferably used.
- the non-woven fabric in which the fiber bundles of the ultrafine fibers are entangled can be obtained, for example, by entwining the ultrafine fiber-expressing fibers in advance and then expressing the ultrafine fibers.
- the non-woven fabric in which the ultrafine fibers constituting the fiber bundle of the ultrafine fibers are appropriately separated from each other and have voids is, for example, a sea-island type composite fiber capable of forming voids between the island components by removing the sea component. It can be obtained by using it.
- the non-woven fabric may be either a short-fiber non-woven fabric or a long-fiber non-woven fabric, but the short-fiber non-woven fabric is more preferably used from the viewpoint of the texture and quality of the sheet-like material.
- the fiber length of the short fiber is preferably in the range of 25 mm or more and 90 mm or less.
- the fiber length is preferably in the range of 25 mm or more and 90 mm or less.
- the fiber length is set to 25 mm or more, more preferably 35 mm or more, still more preferably 40 mm or more, it becomes easy to obtain a sheet-like material having excellent wear resistance due to entanglement.
- the fiber length is set to 90 mm or less, more preferably 80 mm or less, still more preferably 70 mm or less, a sheet-like material having more excellent texture and quality can be obtained.
- the non-woven fabric or knitted fabric when a non-woven fabric is used as the fibrous base material, the non-woven fabric or knitted fabric can be inserted, laminated, or lined inside the non-woven fabric for the purpose of improving the strength.
- the average single fiber diameter of the fibers constituting such a woven fabric or knitted fabric is more preferably 0.3 ⁇ m or more and 10 ⁇ m or less because damage at the time of needle punching can be suppressed and strength can be maintained.
- polyesters such as "polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate, and polylactic acid", and "polyamide 6 and polyamide 66, polyamide 56, polyamide 610, polyamide 11, and polyamide.” 12.
- Synthetic fibers made of thermoplastic resins typified by polyamides such as "12 and copolymerized polyamides", regenerated fibers such as cellulose-based polymers, and natural fibers such as cotton and hemp can be used.
- a fibrous base material made of ultrafine fibers it is preferable to prepare a fibrous base material using ultrafine fiber-expressing type fibers and adopt a method of expressing ultrafine fibers by means described later.
- the ultrafine fiber-expressing fiber a thermoplastic resin having two components (two or three components when the island fiber is a core-sheath composite fiber) having different solvent solubility is used as a sea component and an island component, and the above sea component is used as a solvent.
- a sea-island type composite fiber in which the island component is an ultrafine fiber by dissolving and removing the sea component an appropriate void is provided between the island components, that is, between the ultrafine fibers inside the fiber bundle when the sea component is removed. Therefore, it is preferable from the viewpoint of the texture and surface quality of the sheet-like material.
- sea-island type composite fiber a polymer mutual arrangement in which two components of the sea component and the island component (three components when the island fiber is a core-sheath composite fiber) are reciprocally arranged and spun using a sea-island type composite base is used.
- the method used is preferable from the viewpoint of obtaining ultrafine fibers having a uniform single fiber fineness.
- polyethylene, polypropylene, polystyrene, copolymerized polyester obtained by copolymerizing sodium sulfoisophthalic acid, polyethylene glycol, etc., polylactic acid, etc. can be used. From this point of view, polystyrene and copolymerized polyester are preferably used.
- the dissolution and removal of the sea component is performed after the first polymer elastic precursor impregnation step.
- the mass ratio of the sea component is 10% by mass or more, the island component is likely to be sufficiently refined. Further, when the mass ratio of the sea component is 80 mass or less, the ratio of the eluted component is small, so that the productivity is improved.
- the fibrous base material made of ultrafine fiber-expressing fibers preferably takes the form of a non-woven fabric, and can be used as either a so-called short-fiber non-woven fabric or a long-fiber non-woven fabric. It is preferable because the number of fibers facing the thickness direction is larger than that of the long-fiber non-woven fabric, and a high degree of denseness can be obtained on the surface of the sheet-like material when raised.
- the obtained ultrafine fiber-expressing fibers are preferably crimped and cut to a predetermined length to obtain raw cotton. obtain.
- a known method can be used for the crimping process and the cutting process.
- the obtained raw cotton is made into a fiber web by a cloth wrapper or the like, and entangled to obtain a short fiber non-woven fabric.
- a needle punching process, a water jet punching process, or the like can be used as a method of entwining the fiber webs to obtain a short fiber non-woven fabric.
- the obtained short fiber non-woven fabric and woven fabric are laminated and entangled and integrated.
- the woven fabric is laminated on one or both sides of the short-fiber non-woven fabric, or the woven fabric is sandwiched between multiple short-fiber non-woven fabric webs, and then needle punching or water jet is performed.
- the short fiber non-woven fabric and the fibers of the woven fabric can be entangled with each other by punching or the like.
- Apparent density of the short-fiber nonwoven fabric composed of the composite fiber after needle punching or water jet punching is preferably 0.15 g / cm 3 or more 0.45 g / cm 3 or less.
- the apparent density is preferably 0.15 g / cm 3 or more, the sheet-like material can obtain sufficient morphological stability and dimensional stability.
- the apparent density is set to preferably 0.45 g / cm 3 or less, a sufficient space for forming the polymer elastic body can be maintained.
- the short fiber non-woven fabric thus obtained is preferably shrunk by dry heat, moist heat, or both to further increase the density. Further, the short fiber non-woven fabric can be compressed in the thickness direction by a calendar treatment or the like.
- the sheet-like material of the present invention has a polymer elastic body.
- This polymer elastic body is formed by reacting a polymer elastic precursor with a cross-linking agent. The details will be further described below.
- the polymer elastic precursor according to the present invention has a hydrophilic group.
- “having a hydrophilic group” means “having a group having active hydrogen” itself.
- Specific examples of the group having active hydrogen include a hydroxyl group, a carboxyl group, a sulfonic acid group, an amino group and the like.
- this polymer elastic precursor examples include water-dispersible silicone resin, water-dispersible acrylic resin, water-dispersible urethane resin, and copolymers thereof.
- a water-dispersible polyurethane resin is preferably used from the viewpoint of texture.
- it is prepared by reacting a polymer polyol described later, an organic diisocyanate, and an active hydrogen component-containing compound having a hydrophilic group to form a hydrophilic prepolymer, and then adding and reacting a chain extender.
- Water-dispersible polyurethane resin is more preferably used. Details of these will be described below.
- polymer polyols examples include polyether-based polyols, polyester-based polyols, and polycarbonate-based polyols.
- the polyether-based polyol a polyol obtained by adding and polymerizing a monomer such as ethylene oxide, propylene oxide, butylene oxide, styrene oxide, tetrahydrofuran, epichlorohydrin and cyclohexylene using a polyhydric alcohol or polyamine as an initiator, and a polyol obtained by addition and polymerization.
- Specific examples thereof include polyethylene glycol, polypropylene glycol, polytetramethylene glycol, and copolymerized polyols in which these are combined.
- examples of the polyester-based polyol include a polyester polyol obtained by condensing various low-molecular-weight polyols with a polybasic acid, a polyol obtained by depolymerizing a lactone, and the like.
- polyester-based polyol examples include "ethylene glycol, 1,3-propylene glycol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, 1,7-".
- Linear alkylene glycols such as heptanediol, 1.8-octanediol, 1,9-nonanediol, 1,10-decanediol, and neopentyl glycol, 3-methyl-1,5-pentanediol, 2, Branched alkylene glycols such as 4-diethyl-1,5-pentanediol, 2-methyl-1,8-octanediol, alicyclic diols such as 1,4-cyclohexanediol, and 1,4-bis ( ⁇ -).
- aromatic dihydric alcohols such as hydroxyethoxy) benzene and the like can be mentioned.
- an adduct obtained by adding various alkylene oxides to bisphenol A can also be used as a low molecular weight polyol.
- examples of the polybasic acid used in the polyester-based polyol include succinic acid, maleic acid, adipic acid, glutaric acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, dodecanecarboxylic acid, phthalic acid, and isophthalic acid.
- succinic acid maleic acid, adipic acid, glutaric acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, dodecanecarboxylic acid, phthalic acid, and isophthalic acid.
- terephthalic acid hexahydroisophthalic acid and the like can be mentioned.
- polycarbonate-based polyol examples include compounds obtained by reacting a polyol with a carbonate compound, such as a polyol and a dialkyl carbonate, or a polyol and a diallyl carbonate.
- the polyol used for the polycarbonate-based polyol the low molecular weight polyol used for the polyester-based polyol can be used.
- the dialkyl carbonate dimethyl carbonate, diethyl carbonate or the like can be used, and as the diaryl carbonate, diphenyl carbonate or the like can be used.
- the number average molecular weight of the polymer polyol preferably used in the present invention is preferably 500 or more and 5000 or less.
- the number average molecular weight of the polymer polyol is preferably 500 or more and 5000 or less.
- organic diisocyanates As the organic diisocyanates preferably used in the present invention, aromatic diisocyanates having 6 or more and 20 or less carbon atoms (excluding carbon in the isocyanate group, the same applies hereinafter) and fats having 2 or more and 18 or less carbon atoms are used. Group diisocyanates, alicyclic diisocyanates having 4 to 15 carbon atoms, aromatic aliphatic diisocyanates having 8 to 15 carbon atoms, modified products of these diisocyanates (carbodiimide modified products, urethane modified products, uretdione modified products, etc.) And a mixture of two or more of these.
- aromatic diisocyanate having 6 or more and 20 or less carbon atoms include 1,3- and / or 1,4-phenylenediocyanate, 2,4- and / or 2,6-tolylene diisocyanate, 2, 4'-and / or 4,4'-diphenylmethane diisocyanate (hereinafter sometimes abbreviated as MDI), 4,4'-diisocyanatobiphenyl, 3,3'-dimethyl-4,4'-diisocyanate Examples thereof include biphenyl, 3,3'-dimethyl-4,4'-diisocyanatodiphenylmethane, and 1,5-naphthylene diisocyanate.
- MDI 4,4'-diisocyanatobiphenyl
- Examples thereof include biphenyl, 3,3'-dimethyl-4,4'-diisocyanatodiphenylmethane, and 1,5-naphthylene diisocyanate.
- aliphatic diisocyanate having 2 or more and 18 or less carbon atoms include ethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, dodecamethylene diisocyanate, 2,2,4-trimethylhexamethylene diisocyanate, lysine diisocyanate, 2, 6-Diisocyanatomethyl caproate, bis (2-isocyanatoethyl) carbonate, 2-isocyanatoethyl-2,6-diisocyanatohexaate and the like can be mentioned.
- alicyclic diisocyanate having 4 or more and 15 or less carbon atoms include isophorone diisocyanate, dicyclohexylmethane-4,4'-diisocyanate, cyclohexylene diisocyanate, methylcyclohexylene diisocyanate, and bis (2-isocyanatoethyl).
- examples include -4-cyclohexylene-1,2-dicarboxylate, and 2,5- and / or 2,6-norbornane diisocyanate.
- aromatic aliphatic diisocyanate having 8 or more and 15 or less carbon atoms include m- and / or p-xylylene diisocyanate, ⁇ , ⁇ , ⁇ ', and ⁇ '-tetramethylxylylene diisocyanate. Be done.
- the more preferable organic diisocyanate is an alicyclic diisocyanate having 4 or more and 15 or less carbon atoms.
- a particularly preferable organic diisocyanate is dicyclohexylmethane-4,4'-diisocyanate (hereinafter, may be abbreviated as hydrogenated MDI).
- Active hydrogen component-containing compound having a hydrophilic group examples include a nonionic group and / or an anionic group and / or a cationic group and active hydrogen. Examples thereof include compounds containing and. These active hydrogen component-containing compounds can also be used in the form of salts neutralized with a neutralizing agent. By using this active hydrogen component-containing compound having a hydrophilic group, the stability of the aqueous dispersion used in the method for producing a sheet-like product can be enhanced.
- Examples of the compound having a nonionic group and active hydrogen include a compound containing two or more active hydrogen components or two or more isocyanate groups and having a polyoxyethylene glycol group having a molecular weight of 250 to 9000 in the side chain. And triols such as trimethylolpropane and trimethylolbutane can be mentioned.
- Examples of the compound having an anionic group and active hydrogen include carboxyl group-containing compounds such as 2,2-dimethylol propionic acid, 2,2-dimethylolbutanoic acid, and 2,2-dimethylol valerate and their derivatives, and 1 , 3-Phenylenediamine-4,6-disulfonic acid, 3- (2,3-dihydroxypropoxy) -1-propanesulfonic acid and other compounds containing sulfonic acid groups and their derivatives, and neutralizing these compounds. Examples include salts neutralized with an agent.
- Examples of the compound containing a cationic group and active hydrogen include a tertiary amino group-containing compound such as 3-dimethylaminopropanol, N-methyldiethanolamine, and N-propyldiethanolamine, and derivatives thereof.
- chain extender examples include water, "ethylene glycol, propylene glycol, 1,3-butylene glycol, 1,4-butanediol, 1,6-hexanediol, diethylene glycol and the like.
- Low molecular weight diols such as neopentyl glycol, alicyclic diols such as 1,4-bis (hydroxymethyl) cyclohexane, aromatic diols such as 1,4-bis (hydroxyethyl) benzene, ethylene diamines, etc.
- Aliphatic diamines "isophorone diamines, etc.” alicyclic diamines, “4,4-diaminodiphenylmethane, etc.” aromatic diamines, “xylenideamines, etc.” aromatic aliphatic diamines, “ethanolamine, etc.” alkanolamines , Hydrazine, dihydrazides such as “dihydrazide adipate", and mixtures of two or more of these.
- chain extenders are water, low molecular weight diols, aromatic diamines, more preferably water, ethylene glycol, 1,4-butanediol, 4,4'-diaminodiphenylmethane and two of these.
- the above mixture can be mentioned.
- the water-dispersed polyurethane resin preferably used in the present invention comprises the above-mentioned high molecular weight polyol, an organic diisocyanate, and an active hydrogen component-containing compound having a hydrophilic group. It is prepared by reacting to form a hydrophilic prepolymer, and then adding and reacting a chain extender.
- the polymeric elastic precursor according to the present invention preferably contains a polyether diol and / or a polycarbonate diol as constituent components.
- a contains B as a constituent component means "containing B as a monomer component and an oligomer component constituting A”.
- the polymer elastic precursor according to the present invention contains this polyether diol as a constituent component, the degree of freedom of the ether bond is high, the glass transition temperature is low, and the cohesive force is weak, so that the flexibility is excellent. It can be a polymer elastic body.
- the polycarbonate diol as a constituent component, it is possible to obtain a polymer elastic body having excellent water resistance, heat resistance and weather resistance due to the high cohesive force of the carbonate group.
- the number average molecular weight of the polymer elastic precursor used in the present invention is preferably 20,000 or more and 500,000 or less.
- the strength of the polymer elastic body can be increased by 20,000 or more, more preferably 30,000 or more.
- it is 500,000 or less, more preferably 150,000 or less, the stability of viscosity can be improved and the workability can be improved.
- the number average molecular weight of the polymer elastic precursor can be determined by gel permeation chromatography (GPC), and is measured under the following conditions, for example.
- GPC gel permeation chromatography
- cross-linking agent a polymer compound having a carbodiimide group, an isocyanate group, an oxazoline group, an epoxy group, a melamine resin, a silanol group and the like can be used.
- an N-acylurea bond and / or an N-acylurea bond and / or a carbodiimide cross-linking agent containing a carbodiimide group and a blocked isocyanate cross-linking agent in which an isocyanate group is expressed by heating are used. It is preferable to form an isocyanate bond.
- the N-acylurea bond and / or the isourea bond which are excellent in physical properties such as light resistance, heat resistance, and abrasion resistance, and flexibility, are formed in the molecule of the polymer elastic body in the sheet-like material.
- a dimensional crosslinked structure can be imparted, and physical properties such as abrasion resistance can be dramatically improved while maintaining the flexibility of the sheet-like material.
- the polymer elastic body of the sheet-like material of the present invention is formed by reacting the above-mentioned polymer elastic body precursor with a cross-linking agent.
- the polymer elastic body of the present invention has a hydrophilic group derived from the polymer elastic precursor, and further has an N-acylurea bond and / or an isourea bond.
- the presence of the above N-acylurea group and isourea group in the polymer elastic body means that the cross section of the sheet-like material is mapped by, for example, time-of-flight secondary ion mass spectrometry (TOF-SIMS analysis).
- TOF-SIMS analysis time-of-flight secondary ion mass spectrometry
- Processing for example, "TOF.SIMS 5" manufactured by ION-TOF as an analytical instrument
- infrared spectroscopic analysis for example, "FT / IR 4000 series” manufactured by Nippon Spectroscopy Co., Ltd. as an analytical instrument
- the polymer elastic material according to the present invention preferably contains a polyether diol and / or a polycarbonate diol as a constituent component.
- the polymer elastic body according to the present invention contains this polyether diol as a constituent component, the degree of freedom of its ether bond is high, the glass transition temperature is low, and the cohesive force is weak, so that the polymer is excellent in flexibility. It can be an elastic body.
- the polycarbonate diol as a constituent component, it is possible to obtain a polymer elastic body having excellent water resistance, heat resistance and weather resistance due to the high cohesive force of the carbonate group.
- the polymer elastic body may be composed of a polymer elastic body A containing a polyether diol as a constituent component and a polymer elastic body B containing a polycarbonate diol as a constituent component.
- a polymer elastic body A containing a polyether diol as a component having excellent flexibility and a polymer elastic body B containing a polycarbonate diol as a component having excellent durability against external stimuli such as light and heat. By including it inside the material, it becomes easy to obtain a sheet-like material that is flexible and has excellent durability.
- the polymer elastic body having a hydrophilic group used in the present invention appropriately grips fibers in a sheet-like material, and preferably has fluff on at least one side of the sheet-like material. It is a preferred embodiment that it exists inside the.
- the sheet-like material of the present invention is rigid in the vertical direction defined by the method A (45 ° cantilever method) described in "8.21 Rigidity and softness" of JIS L1096: 2010 "Fabric test method for woven fabrics and knitted fabrics".
- the softness is 40 mm or more and 140 mm or less.
- By setting the rigidity and softness in this range a sheet-like material having appropriate flexibility and resilience can be obtained.
- By setting the rigidity to 50 mm or more, more preferably 55 mm or more a more generalized sheet-like material can be obtained.
- the rigidity to 120 mm or less, more preferably 110 mm or less, a more flexible sheet-like material can be obtained.
- the "vertical direction" in the sheet-like material of the present invention means the direction in which the sheet-like material is brushed in the manufacturing process of the sheet-like material.
- a method of searching for the direction in which the brushing treatment is performed it can be appropriately adopted depending on the constituent components of the sheet-like material such as visual confirmation when tracing with a finger and SEM photography. That is, when traced with a finger, the direction in which the fluffy fibers can be laid down or erected is the vertical direction. Further, by SEM-imaging the surface of the sheet-like object traced with a finger, the direction in which the lying nap fibers are most oriented becomes the vertical direction.
- the horizontal direction in the sheet-like object of the present invention is referred to as the horizontal direction in the sheet-like object surface with respect to the vertical direction.
- the sheet-like material of the present invention is described in "8.19 Abrasion strength and frictional discoloration" of JIS L1096: 2010 "Fabric test method for woven fabrics and knitted fabrics” after being immersed in N, N-dimethylformamide for 24 hours.
- the wear test under the pressing load of 12.0 kPa and the number of frictions of 20000 times specified by the E method (Martindale method)
- the wear test is grade 4 or higher, and the wear loss is 25 mg or less.
- the surface grade and wear loss after immersion in N, N-dimethylformamide for 24 hours are within this range, so that it can be used for a long time in a harsh environment where it is exposed to organic solvents, acids, alkaline solutions or sunlight.
- This wear loss is preferably 23 mg or less, and more preferably 20 mg or less, because deterioration of the appearance of the sheet-like material can be suppressed.
- the sheet-like material of the present invention preferably has a tensile strength when wet is 75% or more when dry.
- a tensile strength during wetting is within this range, deterioration of physical properties during dyeing and post-processing can be suppressed, and the durability of the product can be further enhanced.
- the tensile strength at the time of wetting is 77% or more, more preferably 80% or more, deterioration of the sheet-like material can be further suppressed.
- the sheet-like material of the present invention preferably has a tensile strength and elongation when wet and 100% or more when dry.
- a tensile strength and elongation during wetting are within this range, deterioration of physical properties during dyeing and post-processing can be suppressed, and the durability of the product can be further enhanced.
- the tensile strength and elongation at the time of wet and wet to 105% or more, more preferably 110% or more, deterioration of the sheet-like material can be further suppressed.
- the tensile strength and tensile strength / elongation of the sheet-like material when dried or wet are determined by "6.3 Tensile strength and elongation (ISO method)" of JIS L1913: 2010 "General Nonwoven Fabric Test Method". Refers to the value measured and calculated according to the following procedure.
- the sheet-like material of the present invention is placed on a hot plate in which the raised surface of the sheet-like material is heated to 150 ° C. and pressed with a pressing load of 2.5 kPa for 10 seconds to retain the L value (hereinafter referred to as “L value retention rate”). It is preferable that the L value retention rate) is 90% or more and 100% or less. Above all, when the L value retention rate is 90% or more, more preferably 92% or more, still more preferably 95% or more, the sheet-like material has high heat resistance.
- the "brushed surface of the sheet-like material” refers to the surface of the sheet-like material that has been brushed.
- the L value is an L value defined by the Commission International on Illumination (CIE), but the L value retention rate in the present invention is a change in brightness under heating / pressing conditions. Is a small ratio, that is, it is an index indicating how much a sheet-like material having a bright color before heating / pressing does not become dark after heating / pressing.
- the L value retention rate refers to a value measured and calculated by the procedure as follows.
- the sheet-like material is cut, and the L value of the cut test piece is measured using a color difference meter (for example, "CR-410" manufactured by Konica Minolta Co., Ltd.).
- the test piece is placed on a hot plate heated to 150 ° C. (for example, "CHP-250DN” manufactured by AS ONE Corporation) with the raised surface of the test piece facing down.
- An indenter adjusted so that the pressing load is 2.5 kPa is placed on the test piece and held for 10 seconds.
- the L value retention rate is calculated from the following formula.
- L value retention rate (%) (L value measured in (1)) / (L value measured in (4)) ⁇ 100
- the washing test of one sheet-like material is carried out, and after the test, the fiber debris adhering to the collection bag attached to the drain hose is removed.
- the amount of fiber waste collected using a membrane filter can be 10.0 (mg / sheet-like material 100 cm 2 ) or less.
- the sheet-like material has less fiber shedding during washing and has a smaller environmental load.
- the washing test of one sheet-like material was carried out, and after the test, the fiber dust adhering to the collection bag attached to the drain hose was removed by using a membrane filter.
- the amount of fiber waste when collected using is a value calculated by measuring according to the following procedure. First, the washing machine is washed according to the ISO 6330 C4N method without putting the object to be washed and the detergent in the washing machine. Next, wash one sheet to be evaluated with a collection bag manufactured using NY10-HC (manufactured by Flon Industries Co., Ltd.), a "nylon screen" with a 10 ⁇ m opening, attached to the drain hose of the washing machine.
- the fiber debris adhering to the "nylon screen” is suction-filtered using a polycarbonate membrane (K040A047A Advantech Toyo Co., Ltd.) whose weight has been measured in advance.
- the polycarbonate membrane after filtration and the fiber waste are dried at 105 ° C. for 1 hour, the weight is measured, and the difference from the weight before filtration is defined as the amount of fiber waste during washing.
- a sheet-like product can be produced through a first polymer elastic precursor impregnation step, an ultrafine fiber expression step, and a second polymer elastic precursor impregnation step, which will be described later.
- a first polymer elastic precursor impregnation step By impregnating the first polymer elastic precursor and then undergoing an ultrafine fiber expression step, it can be formed in the gap between the ultrafine fibers and the polymer elastic, and a flexible texture can be easily obtained.
- the polymer elastic body applied for the first time can be reinforced, and the chemical resistance and dyeing resistance can be easily improved. ..
- the heat-sensitive coagulation temperature of the aqueous dispersion within the range described below, uneven distribution (migration) of polyurethane to the surface of the sheet-like material due to water evaporation is suppressed, deterioration due to thermal pressing of polyurethane is suppressed, and the L value is maintained. The rate can be increased.
- the sheet-like material of the present invention includes interior materials, shirts, jackets, which have a very elegant appearance as furniture, chairs and wall materials, and skin materials such as seats, ceilings and interiors in vehicle interiors such as automobiles, trains and aircraft. Industry of uppers, trims, bags, belts, wallets, etc. of shoes such as casual shoes, sports shoes, men's shoes and women's shoes, and clothing materials used for some of them, wiping cloths, polishing cloths, CD curtains, etc. It can be suitably used as a material.
- the method for producing a sheet-like product of the present invention includes the following steps (1) to (3) in this order.
- a fibrous base material made of ultrafine fiber-expressing fibers is impregnated with an aqueous dispersion containing a polymer elastic precursor having a hydrophilic group, a monovalent cation-containing inorganic salt, and a cross-linking agent.
- the temperature of the fibrous base material impregnated with the aqueous dispersion is set to 100 ° C. or higher and 180 ° C. or lower and heat-drying treatment is performed to form a polymer elastic body.
- the first polymer elastic precursor wherein the content of the monovalent cation-containing inorganic salt in the aqueous dispersion is 10 parts by mass or more and 100 parts by mass or less with respect to 100 parts by mass of the polymer elastic precursor.
- Impregnation step (2) Ultrafine fiber expression step of expressing ultrafine fibers from the ultrafine fiber-expressing fibers to form an ultrafine fibrous substrate composed of the ultrafine fibers (3) Fibrous group composed of the ultrafine fibers The material is impregnated with an aqueous dispersion containing a polymer elastic precursor having a hydrophilic group, a monovalent cation-containing inorganic salt, and a cross-linking agent, and then impregnated with the aqueous dispersion.
- the second polymer elastic precursor impregnation step in which the content of the contained inorganic salt is 10 parts by mass or more and 100 parts by mass or less with respect to 100 parts by mass of the polymer elastic precursor. explain.
- a polymer elastic precursor having a hydrophilic group and a monovalent cation-containing inorganic substance are formed on a fibrous substrate made of ultrafine fiber-expressing fibers.
- a polymer elastic body is formed by impregnating an aqueous dispersion containing a salt and a cross-linking agent, and then heat-drying the fibrous substrate impregnated with the aqueous dispersion at a temperature of 100 ° C. or higher and 180 ° C. or lower. Let me.
- the water dispersion used in this step contains the above-mentioned polymer elastic precursor having a hydrophilic group, a monovalent cation-containing inorganic salt, and a cross-linking agent. ..
- the concentration of the polymer elastic precursor in this aqueous dispersion is preferably 5% by mass or more and 50% by mass or less in the aqueous dispersion.
- concentration of the polymer elastic precursor in the aqueous dispersion is preferably 5% by mass or more, more preferably 10% by mass or more, the cohesiveness becomes good, and the polymer elastic body aggregates in a large mass, which is good. It becomes abrasion resistant.
- concentration to 50% by mass or less, more preferably 40% by mass or less, the polymer elastic body can be uniformly applied to the fibrous base material.
- the aqueous dispersion contains a monovalent cation-containing inorganic salt.
- a monovalent cation-containing inorganic salt By containing a monovalent cation-containing inorganic salt, it is possible to impart heat-sensitive coagulation to the aqueous dispersion.
- the heat-sensitive coagulation property means that when the aqueous dispersion is heated, the fluidity of the aqueous dispersion decreases and solidifies when a certain temperature (hereinafter, this temperature is referred to as a heat-sensitive coagulation temperature) is reached.
- the heat-sensitive coagulation temperature of this aqueous dispersion is preferably 55 ° C. or higher and 80 ° C. or lower.
- the dry heat coagulation temperature is preferably 55 ° C. or higher, more preferably 60 ° C. or higher.
- the stability of the aqueous dispersion during storage is improved, and the adhesion of the polymer elastic body to the manufacturing equipment during operation is suppressed. be able to.
- 80 ° C. or lower more preferably 70 ° C. or lower, it is possible to suppress the migration phenomenon in which the polymer elastic body migrates to the surface of the fibrous substrate as the water evaporates.
- the monovalent cation-containing inorganic salt is preferably sodium chloride and / or sodium sulfate.
- an inorganic salt having a divalent cation such as magnesium sulfate or calcium chloride has been preferably used as the heat-sensitive coagulant.
- these inorganic salts greatly affect the stability of the aqueous dispersion even when added in a small amount, depending on the type of the polymer elastic precursor, the heat-sensitive gelation temperature by adjusting the addition amount is strict. It is difficult to control, and there is a problem in that the aqueous dispersion may gel during preparation or storage.
- the monovalent cation-containing inorganic salt having a small ionic valence has a relatively small effect on the stability of the aqueous dispersion, and the stability of the aqueous dispersion can be ensured by adjusting the addition amount.
- the heat-sensitive solidification temperature can be strictly controlled.
- the monovalent cation-containing inorganic salt is contained in an amount of 10 parts by mass or more and 100 parts by mass or less with respect to 100 parts by mass of the polymer elastic precursor in the aqueous dispersion.
- a large amount of ions present in the aqueous dispersion act uniformly on the polymer elastic particles, so that coagulation is rapidly performed at a specific heat-sensitive coagulation temperature.
- the coagulation of the polymer elastic body can proceed in a state where the fibrous base material contains a large amount of water. As a result, it is possible to achieve good flexibility and resilience similar to natural leather.
- the content in the above range, it is possible to prevent the polymer elastic body from being excessively aggregated and hardened, and to prevent the formation of a film-like substance of the polymer elastic body. ..
- the content is 100 parts by mass or less, the polymer elastic body is cured in an appropriate size, so that deterioration of physical properties can be suppressed.
- the stability of the aqueous dispersion can be maintained.
- the aqueous dispersion contains a cross-linking agent.
- the cross-linking agent By using the cross-linking agent, the polymer elastic body has a three-dimensional network structure, and the sheet-like material has excellent wear resistance and the like. Furthermore, when used in combination with the above-mentioned monovalent cation-containing inorganic salt, the solidification of the polymer elastic precursor and the reaction between the polymer elastic precursor and the cross-linking agent proceed simultaneously, resulting in a dense three-dimensional network structure. It is possible to form and control the adhesive structure of fibers, to make the sheet-like material more flexible, and to achieve high physical properties, high light resistance, and high heat resistance of the sheet-like material.
- the aqueous dispersion contains 40% by mass of a water-soluble organic solvent such as a ketone solvent such as acetone, ethylmethylketone, and diethylketone in 100% by mass of the aqueous dispersion in order to improve storage stability and film formation. It may be contained below. However, from the viewpoint of preserving the working environment, collecting wastewater, and the like, the content of the organic solvent is preferably 1% by mass or less.
- the temperature of the fibrous base material in this heat-drying treatment is 100 ° C. or higher and 180 ° C. or lower.
- the temperature of the fibrous substrate is 100 ° C. or higher, preferably 120 ° C. or higher, more preferably 140 ° C. or higher.
- the polymer elastic precursor is rapidly solidified, and the polymer elastic body is formed on the lower surface of the sheet due to its own weight. It is possible to prevent uneven distribution.
- the cross-linking reaction between the polymer elastic precursor and the cross-linking agent can be sufficiently promoted to form a three-dimensional network structure, and the physical characteristics, light resistance and heat resistance of the sheet-like material can be improved.
- the temperature of the fibrous base material is 180 ° C. or lower, preferably 175 ° C. or lower, it is possible to prevent the polymer elastic body from being thermally deteriorated.
- ultrafine fiber expression step In this step, ultrafine fibers are expressed from the ultrafine fiber-expressing type fibers to form a fibrous base material composed of the ultrafine fibers.
- the ultrafine fibers after the first polymer elastic material precursor impregnation step that is, after applying the polymer elastic material once, for example, when the ultrafine fiber-expressing type fibers are sea-island type composite fibers. Since the voids formed by dissolving the island components can be formed, the polymer elastic body does not firmly restrain the ultrafine fibers, and the texture of the sheet-like material becomes more flexible.
- the fiber ultra-fine fiber treatment can be performed by immersing the sea-island type composite fiber in a solvent and squeezing the liquid. It can.
- a solvent for dissolving the sea component an alkaline aqueous solution such as sodium hydroxide or hot water can be used.
- devices such as a continuous dyeing machine, a vibro washer type dewatering machine, a liquid flow dyeing machine, a Wins dyeing machine and a Jigger dyeing machine can be used for the expression of ultrafine fibers.
- an alkaline aqueous solution or the like is used after the ultrafine fiber expression step, it is preferable to perform a sufficient washing step after the treatment.
- a sufficient washing step By going through the cleaning process, it is possible to process the sheet without leaving alkali or excess monovalent cation-containing inorganic salt adhering to the sheet on the sheet, and it is possible to process without affecting the production equipment. It is preferable to use water as the cleaning liquid in consideration of the environment and safety.
- Second Polymer Elastic Precursor Impregnation Step a polymeric elastic precursor having a hydrophilic group, a monovalent cation-containing inorganic salt, and a fibrous substrate made of ultrafine fibers are added.
- An aqueous dispersion containing a cross-linking agent is impregnated, and then the fibrous substrate impregnated with the aqueous dispersion is heat-dried at a temperature of 100 ° C. or higher and 180 ° C. or lower to further form a polymer elastic body. ..
- the aqueous dispersion used in this step is the same as the aqueous dispersion used in the first polymer elastic precursor impregnation step.
- the same polymer elastic precursor may be used, or different polymer elastic precursors may be used.
- the first polymer elastic precursor is the polymer elastic precursor A containing a polyether diol as a component
- the second polymer elastic precursor contains a polycarbonate diol as a component.
- the heat-drying treatment in this step is the same as the heat-drying treatment performed in the first polymer elastic precursor impregnation step.
- At least one surface of the sheet-like material may be brushed to form fluff on the surface.
- the method for forming the naps is not particularly limited, and various methods usually used in the art such as buffing with sandpaper or the like can be used. If the fluff length is too short, it is difficult to obtain an elegant appearance, and if it is too long, pilling tends to occur. Therefore, the fluff length is preferably 0.2 mm or more and 1 mm or less.
- the sheet-like material can be dyed.
- various methods usually used in the art can be adopted.
- a method using a liquid flow dyeing machine is preferable because the sheet-like material can be softened by giving a kneading effect at the same time as dyeing the sheet-like material.
- the dyeing temperature is preferably 80 ° C. or higher and 150 ° C. or lower, although it depends on the type of fiber. By setting the dyeing temperature to 80 ° C. or higher, more preferably 110 ° C. or higher, dyeing to the fibers can be efficiently performed. On the other hand, by setting the dyeing temperature to 150 ° C. or lower, more preferably 130 ° C. or lower, deterioration of the polymer elastic body can be prevented.
- the dye used in the present invention may be selected according to the type of fiber constituting the fibrous base material and is not particularly limited. For example, if it is a polyester fiber, a disperse dye can be used, and a polyamide fiber can be used. If so, acid dyes and gold-containing dyes can be used, and combinations thereof can be used. When dyed with a disperse dye, reduction cleaning may be performed after dyeing.
- a dyeing aid at the time of dyeing.
- a dyeing aid By using a dyeing aid, the uniformity and reproducibility of dyeing can be improved.
- a finishing agent treatment using, for example, a softener such as silicone, an antistatic agent, a water repellent agent, a flame retardant, a light resistant agent, an antibacterial agent, or the like can be applied in the same bath as the dyeing or after the dyeing.
- the present invention will be specifically described based on Examples. However, the present invention is not limited to these examples. In addition, in the measurement of each physical property, if there is no particular description, the measurement is performed based on the above method.
- Average single fiber diameter of ultrafine fibers As a scanning electron microscope, 50 singles were randomly extracted within a field of view of 30 ⁇ m ⁇ 30 ⁇ m by observing the ultrafine fibers constituting the sheet-like material at a magnification of 3000 using “VE-7800 type” manufactured by KEYENCE CORPORATION. The fiber diameter was measured in ⁇ m units to the first decimal place.
- the temperature at which the liquid level of the aqueous dispersion lost its fluidity was defined as the heat-sensitive solidification temperature of the aqueous dispersion. This measurement was performed three times for each type of aqueous dispersion, and the average value was calculated.
- Appearance grade of sheet-like material The surface quality of the obtained sheet-like material was evaluated by 10 panelists, evaluated according to the following criteria, and the evaluation result with the largest number of people was adopted.
- the sheet-like object 3 is placed on the inspection table 2 located at a position parallel to the floor surface 1, and the line 4 connecting the visually confirmed position and the sheet-like object is formed.
- the sheet-like object 3 was visually confirmed and judged at an angle of 45 ° from the inspection table plane with respect to the sheet-like object 3 so that the distance was 50 cm.
- a 32W fluorescent lamp 6 was installed 150 cm above the upper surface of the inspection table in the vertical direction.
- the surface quality evaluation was carried out by placing the sheet-like object 3 directly below the fluorescent lamp 6, that is, at a position where a perpendicular line 7 from the sheet-like object to the fluorescent lamp can be drawn.
- the 4th to 5th grades were considered to be good.
- Grade 5 Uniform fiber fluff was present, the fiber dispersion was good, and the appearance was good.
- Grade 4 Evaluation between grade 5 and grade 3.
- Grade 3 The dispersed state of the fibers was somewhat poor, but the fibers had fluff and the appearance was reasonably good.
- 2nd grade Evaluation between 3rd grade and 1st grade.
- Grade 1 The fluff of the fiber was small, the dispersed state of the fiber was very poor as a whole, and the appearance was poor.
- Wear loss (mg) mass before wear (mg) -mass after wear (mg) (7)
- Tension strength retention rate and tensile strength elongation retention rate (staining resistance) when wet As a constant speed extension type tensile tester, Illinois Tool Works Inc. Manufactured by "Instron 3343" was used.
- the type of inorganic salt was identified by using an ion chromatograph device of "ICS-3000 type" manufactured by Dionex Co., Ltd. for the aqueous solution containing the inorganic salt.
- Amount of fiber waste during washing A 10 cm ⁇ 10 cm (100 cm 2 ) test piece was cut out from the sheet, and a washing test was carried out by the above method to calculate the amount of fiber waste. The measurement was performed twice, and the average value was taken as the amount of fiber waste at the time of washing.
- aqueous dispersion Wa of polymer elastic precursor a Polytetramethylene ether glycol having a number average molecular weight (Mn) of 2000 as a high molecular weight polyol, MDI as an organic diisocyanate, and 2,2-dimethylol propionic acid as an active hydrogen component-containing compound having a hydrophilic group are used in a toluene solvent. Made a prepolymer in. Further, ethylene glycol and ethylenediamine were added as chain extenders, and polyoxyethylene nonylphenyl ether and water were added as external emulsifiers, and the mixture was stirred. Toluene was removed by reducing the pressure to obtain an aqueous dispersion Wa of the polymer elastic precursor a.
- the polymer elastic precursor a is a polymer elastic precursor corresponding to the polymer elastic body A.
- aqueous dispersion Wb of polymer elastic precursor b Polyhexamethylene carbonate having a number average molecular weight (Mn) of 2000 as a high molecular weight polyol, hydrogenated MDI as an organic diisocyanate, a diol compound having polyethylene glycol in the side chain as an active hydrogen component-containing compound having a hydrophilic group, and 2,2. -A prepolymer was prepared in an acetone solvent using dimethylol propionic acid. Ethylene glycol, ethylenediamine and water were added as chain extenders, and the mixture was stirred. Acetone was removed by reducing the pressure to obtain an aqueous dispersion Wb of the polymer elastic precursor b.
- the polymer elastic precursor b is a polymer elastic precursor corresponding to the polymer elastic body B.
- Example 1 (Ultrafine fiber expression type non-woven fabric)
- the sea component polyethylene terephthalate obtained by copolymerizing 8 mol% of sodium 5-sulfoisophthalate was used, and as the island component, polyethylene terephthalate was used.
- the sea component was 20% by mass and the island component was 80% by mass.
- Sea-island type composite fibers having 16 islands / 1 filament and an average fiber diameter of 20 ⁇ m were obtained.
- the obtained sea-island type composite fiber was cut into a fiber length of 51 mm to form a staple, a fiber web was formed through a curd and a cloth wrapper, and a non-woven fabric was obtained by needle punching.
- the non-woven fabric thus obtained was immersed in hot water at a temperature of 97 ° C. for 2 minutes to shrink, and dried at a temperature of 100 ° C. for 5 minutes.
- the obtained sheet-like material having fluff was dyed with a black dye using a liquid flow dyeing machine under a temperature condition of 120 ° C. Then, it was dried with a drier to obtain a sheet-like material having an average single fiber fineness of 4.4 ⁇ m.
- the obtained sheet-like material has a rigidity of 84 mm, a surface grade of 5 grade, a wear resistance after DMF treatment of grade 4.5 grade / wear weight loss of 7.6 mg, and a tensile strength retention rate of 83% / tension when wet. It had a strong elongation retention rate of 119%, a soft texture, and excellent chemical resistance and dyeing resistance.
- polyether bond there were a polyether bond, a polycarbonate bond, an N-acylurea bond and an isourea bond inside the polymer elastic body.
- having an N-acylurea bond and / or an isourea bond inside the polymer elastic body means that the polymer elastic body has an N-acylurea bond and / or an isourea bond.
- the amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection. Further, the L value retention rate was 97%, and it had excellent heat resistance.
- the amount of fiber waste during washing was 2.9 (mg / sheet-like material 100 cm 2 ), which had a small environmental load.
- Example 2 In Example 1 (addition of the first polymer elastic resin), 3 parts by mass of a carbodiimide-based cross-linking agent was added as a cross-linking agent, but 3 parts by mass of a blocked isocyanate-based cross-linking agent was added. Except for this, a sheet-like product having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1. The obtained sheet-like material has a rigidity of 94 mm, a surface grade of 5 grade, a wear resistance after DMF treatment of grade 4.5 grade / wear weight loss of 7.8 mg, and a tensile strength retention rate of 81% / tension when wet.
- Example 3 In Example 1 (addition of the second polymer elastic resin), 3 parts by mass of the carbodiimide-based cross-linking agent was added as the cross-linking agent, but 3 parts by mass of the blocked isocyanate-based cross-linking agent was added. Except for this, a sheet-like product having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1. The obtained sheet-like material has a rigidity of 89 mm, a surface grade of 5 grade, a wear resistance after DMF treatment of grade 4.5 grade / wear weight loss of 8.5 mg, and a tensile strength retention rate of 80% / tension when wet.
- Example 4 In Example 1 (application of the second polymer elastic resin), the polymer elastic precursor b was used as the polymer elastic precursor, but the polymer elastic precursor a was used instead.
- a sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the changes were made.
- the obtained sheet-like material has a rigidity of 82 mm, a surface grade of 4.5 grade, a wear resistance after DMF treatment of grade 4 / wear weight loss of 8.8 mg, and a tensile strength retention rate of 77% / tension when wet. It had a strong elongation retention rate of 122%, a soft texture, and excellent chemical resistance and dyeing resistance.
- a polyether bond, an N-acylurea bond and an isourea bond were present inside the polymer elastic body.
- the amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection. Further, the L value retention rate was 93%, and it had excellent heat resistance. In addition, the amount of fiber waste during washing was 3.4 (mg / sheet-like material 100 cm 2 ), which had a small environmental load.
- Example 5 In Example 1 (application of the first polymer elastic resin), the polymer elastic precursor a was used as the polymer elastic precursor, but the polymer elastic precursor b was used instead.
- a sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the changes were made.
- the obtained sheet-like material has a rigidity of 98 mm, a surface grade of 4 grade, a wear resistance after DMF treatment of grade 4.5 grade / wear weight loss 7.7 mg, and a tensile strength retention rate of 84% / tension when wet. It had a strong elongation retention rate of 111%, a soft texture, and excellent chemical resistance and dyeing resistance.
- a polycarbonate bond, an N-acylurea bond and an isourea bond were present inside the polymer elastic body.
- the amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection. Further, the L value retention rate was 96%, and it had excellent heat resistance. In addition, the amount of fiber waste during washing was 2.8 (mg / sheet-like material 100 cm 2 ), which had a small environmental load.
- Example 6 In Example 1 (addition of the first polymer elastic resin), 35 parts by mass of sodium sulfate was added as a heat-sensitive coagulant, but 12 parts by mass was added, and the heat-sensitive coagulation temperature was changed to 70 ° C. A sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the fine fibers were adjusted to 4.4 ⁇ m. The obtained sheet-like material has a rigidity of 94 mm, a surface grade of 4 grade, a wear resistance after DMF treatment of grade 4 / wear weight loss of 7.7 mg, a tensile strength retention rate of 83% when wet, and tensile strength elongation.
- the degree retention rate was 117%, and it had a soft texture and excellent chemical resistance and dyeing resistance. Further, there were a polyether bond, a polycarbonate bond, an N-acylurea bond and an isourea bond inside the polymer elastic body. The amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection. Further, the L value retention rate was 90%, and it had excellent heat resistance. In addition, the amount of fiber waste during washing was 2.8 (mg / sheet-like material 100 cm 2 ), which had a small environmental load.
- Example 7 In Example 1 (addition of the first polymer elastic resin), 35 parts by mass of sodium sulfate was added as a heat-sensitive coagulant, but 86 parts by mass was changed, and the heat-sensitive coagulation temperature was set to 60 ° C. A sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the fine fibers were adjusted to 4.4 ⁇ m. The obtained sheet-like material has a rigidity of 80 mm, a surface grade of 4 grades, a wear resistance after DMF treatment of grade 4 grade / wear weight loss 13.5 mg, a tensile strength retention rate of 80% when wet, and tensile strength elongation.
- Example 8 In Example 1 (addition of the second polymer elastic resin), 35 parts by mass of sodium sulfate was added as the heat-sensitive coagulant, but 12 parts by mass was added, and the heat-sensitive coagulation temperature was changed to 70 ° C. A sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the fine fibers were adjusted to 4.4 ⁇ m.
- the obtained sheet-like material has a rigidity of 98 mm, a surface grade of 4th grade, a wear resistance after DMF treatment of a 4th grade / wear weight loss of 8.0 mg, and a tensile strength retention rate of 83% / tensile strength and elongation when wet. It had a degree retention of 114%, a soft texture, and excellent chemical resistance and dyeing resistance. Further, there were a polyether bond, a polycarbonate bond, an N-acylurea bond and an isourea bond inside the polymer elastic body. The amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection. Further, the L value retention rate was 91%, and it had excellent heat resistance. In addition, the amount of fiber waste during washing was 2.6 (mg / sheet-like material 100 cm 2 ), which had a small environmental load.
- Example 9 In Example 1 (addition of the second polymer elastic resin), 35 parts by mass of sodium sulfate was added as a heat-sensitive coagulant, but 86 parts by mass was changed, and the heat-sensitive coagulation temperature was set to 60 ° C. A sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the fine fibers were adjusted to 4.4 ⁇ m.
- the obtained sheet-like material has a rigidity of 88 mm, a surface grade of 4 grade, a wear resistance after DMF treatment of grade 4 grade / wear weight loss 14.1 mg, a tensile strength retention rate of 81% when wet, and a tensile strength elongation.
- the degree retention rate was 113%, and it had a soft texture and excellent chemical resistance and dyeing resistance.
- the amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection.
- the L value retention rate was 93%, and it had excellent heat resistance.
- the amount of fiber waste during washing was 5.8 (mg / sheet-like material 100 cm 2 ), which had a small environmental load.
- Example 10 In Example 1 (adding the first polymer elastic resin), 35 parts by mass of sodium sulfate was added as a heat-sensitive coagulant, and 30 parts by mass of sodium chloride (described as “NaCl” in Table 1) was added. Instead of adding, the heat-sensitive coagulation temperature was adjusted to 65 ° C., and in (addition of the second polymer elastic resin), 35 parts by mass of sodium sulfate was added as a heat-sensitive coagulant, and the portion was chloride. A sheet-like product having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the heat-sensitive coagulation temperature was adjusted to 65 ° C. by adding 30 parts by mass of sodium.
- the obtained sheet-like material has a rigidity of 86 mm, a surface grade of 5 grade, a wear resistance after DMF treatment of grade 4.5 grade / wear weight loss of 7.4 mg, and a tensile strength retention rate of 83% / tension when wet. It had a strong elongation retention rate of 119%, a soft texture, and excellent chemical resistance and dyeing resistance. Further, there were a polyether bond, a polycarbonate bond, an N-acylurea bond and an isourea bond inside the polymer elastic body. The amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection. Further, the L value retention rate was 96%, and it had excellent heat resistance. The amount of fiber waste during washing was 2.9 (mg / sheet-like material 100 cm 2 ), which had a small environmental load.
- Example 1 A sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the step of Example 1 (application of the second polymer elastic resin) was not performed. ..
- the obtained sheet-like material has a rigidity of 81 mm, a surface grade of 5, the wear resistance after DMF treatment is a series 2 / wear weight loss of 33.5 mg, and a tensile strength retention rate of 72% / tensile strength and elongation when wet.
- the degree retention rate was 103%, the texture was flexible, and the L value retention rate was 93%, which was excellent heat resistance, but the chemical resistance and dyeing resistance were inferior.
- the amount of fiber waste during washing was 12.5 (mg / sheet-like material 100 cm 2 ), which had a large environmental load.
- a polyether bond, an N-acylurea bond and an isourea bond were present inside the polymer elastic body.
- the amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection.
- Comparative Example 2 In Comparative Example 1 (application of the first polymer elastic resin), the average of the ultrafine fibers was the same as in Comparative Example 1 except that the polymer elastic precursor b was used as the polymer elastic precursor. A sheet-like material having a single fiber fineness of 4.4 ⁇ m was obtained. The obtained sheet-like material has a rigidity of 92 mm, a surface grade of 3.5 grade, a wear resistance after DMF treatment of grade 2 / wear loss of 29.9 mg, and a tensile strength retention rate of 73% / tension when wet. The strong elongation retention rate was 101%, the texture was flexible, and the L value retention rate was 94%, which was excellent heat resistance, but the chemical resistance and dyeing resistance were inferior.
- the amount of fiber waste during washing was 11.4 (mg / sheet-like material 100 cm 2 ), which had a large environmental load.
- a polycarbonate bond, an N-acylurea bond and an isourea bond were present inside the polymer elastic body.
- the amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection.
- Example 3 The average single fiber fineness of the ultrafine fibers was 4.4 ⁇ m in the same manner as in Example 1 except that the heat-sensitive coagulant was not added in Example 1 (addition of the first polymer elastic resin). A sheet was obtained.
- the obtained sheet-like material has a rigidity of 150 mm or more, a surface grade of 2nd grade, a wear resistance after DMF treatment of grade 4 / wear loss of 7.4 mg, and a tensile strength retention rate of 84% / tensile strength when wet.
- the elongation retention rate is 109%, the chemical resistance and dyeing resistance are good, the amount of fiber waste during washing is 2.8 (mg / sheet-like material 100 cm 2 ), and the environmental load is small.
- the L value retention rate was 84%, and the heat resistance was not sufficient.
- Example 4 In Example 1 (addition of the second polymer elastic resin), the average single fiber fineness of the ultrafine fibers was 4.4 ⁇ m in the same manner as in Example 1 except that the heat-sensitive coagulant was not added. A sheet was obtained.
- the obtained sheet-like material has a rigidity of 150 mm or more, a surface grade of 2nd grade, a wear resistance after DMF treatment of grade 4 / wear weight loss of 7.1 mg, and a tensile strength retention rate of 82% / tensile strength when wet. Elongation retention rate is 110%, chemical resistance and dyeing resistance are good, and the amount of fiber waste during washing is 3.0 (mg / sheet-like material 100 cm 2 ), which has a small environmental load.
- the L value retention rate was 86%, and the heat resistance was not sufficient.
- Example 5 In Example 1 (addition of the first polymer elastic resin), 35 parts by mass of sodium sulfate was added as a heat-sensitive coagulant, but 5 parts by mass was added, and the heat-sensitive coagulation temperature was set to 85 ° C. A sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the fine fibers were adjusted to 4.4 ⁇ m. The obtained sheet-like material has a rigidity of 144 mm, a surface grade of 2.5 grade, a wear resistance after DMF treatment of grade 4 / wear weight loss of 8.0 mg, and a tensile strength retention rate of 82% / tension when wet.
- Example 6 In Example 1 (addition of the first polymer elastic resin), 35 parts by mass of sodium sulfate was added as a heat-sensitive coagulant, but 120 parts by mass was changed to add 120 parts by mass, and the heat-sensitive coagulation temperature was set to 50 ° C. A sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the fine fibers were adjusted to 4.4 ⁇ m. The obtained sheet-like material has a rigidity of 84 mm, a surface grade of 1.5 grade, a wear resistance after DMF treatment of grade 3 / wear loss of 21.2 mg, and a tensile strength retention rate of 80% when wet / tension.
- N-acylurea bond and isourea bond existed inside the polymer elastic body. Further, there were a polyether bond, a polycarbonate bond, an N-acylurea bond and an isourea bond inside the polymer elastic body. The amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection.
- Example 7 In Example 1 (addition of the second polymer elastic resin), 35 parts by mass of sodium sulfate was added as the heat-sensitive coagulant, but 5 parts by mass was added, and the heat-sensitive coagulation temperature was set to 85 ° C. A sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the fine fibers were adjusted to 4.4 ⁇ m. The obtained sheet-like material has a rigidity of 148 mm, a surface grade of 2.5 grade, a wear resistance after DMF treatment of grade 4 / wear loss of 7.8 mg, and a tensile strength retention rate of 77% / tension when wet.
- the strength retention rate is 120%, the chemical resistance and dyeing resistance are good, the amount of fiber waste during washing is 2.6 (mg / sheet-like material 100 cm 2 ), and the environmental load is small. Although it was, it had a hard texture. Further, the L value retention rate was 87%, and the heat resistance was not sufficient.
- Example 8 In Example 1 (addition of the second polymer elastic resin), 35 parts by mass of sodium sulfate was added as a heat-sensitive coagulant, but 120 parts by mass was changed to add 120 parts by mass, and the heat-sensitive coagulation temperature was set to 50 ° C. A sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained in the same manner as in Example 1 except that the fine fibers were adjusted to 4.4 ⁇ m. The obtained sheet-like material has a rigidity of 86 mm, a surface grade of 1.5 grade, a wear resistance after DMF treatment of grade 3 / wear weight loss of 32.7 mg, and a tensile strength retention rate of 74% / tension when wet.
- the amount of fiber waste during washing was 12.1 (mg / sheet-like material 100 cm 2 ), which had a large environmental load.
- Example 9 Except that the cross-linking agent was not added in (the first addition of the polymer elastic resin) of Example 1 and the cross-linking agent was not added in (the addition of the second polymer elastic resin). Obtained a sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers in the same manner as in Example 1.
- the obtained sheet-like material has a rigidity of 96 mm, a surface grade of 3 grades, a wear resistance after DMF treatment of grade 2 / wear weight loss of 32.0 mg, and a tensile strength retention rate of 71% / tensile strength and elongation when wet.
- the degree retention rate was 97%, and although the texture was good, the chemical resistance and dyeing resistance were inferior.
- the L value retention rate was 88%, and the heat resistance was not sufficient.
- the amount of fiber waste during washing was 13.6 (mg / sheet-like material 100 cm 2 ), which had a large environmental load. There were no polyether bond, polycarbonate bond, N-acylurea bond or isourea bond inside the polymer elastic body. The amount of inorganic salt inside the polymer elastic body was less than the lower limit of detection.
- Example 10 Example 1 except that in Example 1 (addition of the first polymer elastic resin), the place where the heat-sensitive coagulant was added was changed to the addition of 3% by mass of the foaming agent (AIBN). In the same manner as above, a sheet-like material having an average single fiber fineness of 4.4 ⁇ m was obtained.
- the obtained sheet-like material has a rigidity of 145 mm, a surface grade of 2nd grade, a wear resistance after DMF treatment of grade 3 / wear loss of 19.5 mg, and a tensile strength retention rate of 77% / tensile strength and elongation when wet.
- the degree retention rate was 107%, the dyeing resistance was excellent, and the amount of fiber waste during washing was 9.1 (mg / sheet-like material 100 cm 2 ), which had a small environmental load, but the texture and quality. , The chemical resistance was inferior. Further, the L value retention rate was 88%, and the heat resistance was not sufficient.
- Example 11 In Example 1 (addition of the second polymer elastic resin), except that a polycarbonate-based polymer elastic precursor dissolved in DMF was used as the polymer elastic precursor, the same as in Example 1. Similarly, a sheet-like material having an average single fiber fineness of 4.4 ⁇ m of ultrafine fibers was obtained. The obtained sheet-like material has a rigidity of 97 mm, a surface grade of 3 grades, a wear resistance after DMF treatment of grade 2 / wear loss of 42.7 mg, a tensile strength retention rate of 81% when wet, and tensile strength and elongation.
- Example 12 In Example 1 (addition of the second polymer elastic resin), 35 parts by mass of sodium sulfate was added as a heat-sensitive coagulant, and 35 parts by mass of magnesium sulfate (described as “Crosslink 4 ” in Table 1) was added. Instead of adding a part, 3% by mass of a carbodiimide-based cross-linking agent was added, and the whole was adjusted to 11% by mass with water to obtain an aqueous dispersion containing the polymer elastic body a. It gelled and could not impart a polymer elastic body to the non-woven fabric.
- the sheet-like material of the present invention includes furniture, chairs and wall coverings, seats in vehicle interiors such as automobiles, trains and aircraft, skin materials such as ceilings and interiors, interior materials having a very elegant appearance, and clothing and industry. It can be suitably used as a material or the like.
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Abstract
Description
条件1:JIS L1096:2010「織物及び編物の生地試験方法」の「8.21 剛軟度」に記載のA法(45°カンチレバー法)にて規定される縦方向の剛軟度が、40mm以上140mm以下である
条件2:N,N-ジメチルホルムアミドに24時間浸漬後のJIS L1096:2010「織物及び編物の生地試験方法」の「8.19 摩耗強さ及び摩擦変色性」に記載のE法(マーチンデール法)で規定される押圧荷重12.0kPa、摩擦回数20000回における摩耗試験において4級以上であり、摩耗減量が25mg以下である。
条件3:前記のシート状物の起毛面を150℃に加熱したホットプレート上に載置し、押圧荷重2.5kPaで10秒間押圧した際のL値の保持率が90%以上100%以下である。
条件4:ISO 6330 C4N法に従う洗濯試験時において、前記のシート状物1枚の洗濯試験を実施し、試験後に排水ホースに取り付けた捕集袋に付着した繊維屑を、メンブレンフィルターを用いて捕集した場合の繊維屑量が10.0(mg/シート状物100cm2)以下である。
(1) 極細繊維発現型繊維からなる繊維質基材に、親水性基を有する高分子弾性体前駆体と、1価陽イオン含有無機塩と、架橋剤とを含有する水分散液を含浸せしめ、次いで水分散液を含浸させた繊維質基材の温度を100℃以上180℃以下として加熱乾燥処理を行って高分子弾性体を形成させる第1の高分子弾性体前駆体含浸工程であって、前記の水分散液における1価陽イオン含有無機塩の含有量を高分子弾性体前駆体100質量部に対して10質量部以上100質量部以下とする、第1の高分子弾性体前駆体含浸工程
(2) 前記の極細繊維発現型繊維から極細繊維を発現させて前記の極細繊維からなる繊維質基材を形成する、極細繊維発現工程
(3) 前記の極細繊維からなる繊維質基材に、親水性基を有する高分子弾性体前駆体と、1価陽イオン含有無機塩と、架橋剤とを含有する水分散液を含浸せしめ、次いで水分散液を含浸させた繊維質基材の温度を100℃以上180℃以下として加熱乾燥処理を行って、さらに高分子弾性体を形成させる第2の高分子弾性体前駆体含浸工程であって、前記の水分散液における1価陽イオン含有無機塩の含有量が高分子弾性体前駆体100質量部に対して10質量部以上100質量部以下とする、第2の高分子弾性体前駆体含浸工程。
条件1:JIS L1096:2010「織物及び編物の生地試験方法」の「8.21 剛軟度」に記載のA法(45°カンチレバー法)にて規定される縦方向の剛軟度が、40mm以上140mm以下である
条件2:N,N-ジメチルホルムアミドに浸漬後のJIS L1096:2010「織物及び編物の生地試験方法」の「8.19 摩耗強さ及び摩擦変色性」に記載のE法(マーチンデール法)で規定される押圧荷重12.0kPa、摩擦回数20000回における摩耗試験において4級以上であり、摩耗減量が25mg以下である
以下にこの構成要素について詳細に説明するが、本発明はその要旨を超えない限り、以下に説明する範囲に何ら限定されるものではない。
まず、本発明のシート状物は、極細繊維からなる繊維質基材を有する。
(1)得られたシート状物を厚み方向に切断した断面を走査型電子顕微鏡(SEM)により観察する。
(2)観察面内の任意の50本の極細繊維の繊維直径をそれぞれの極細繊維断面において3方向で測定する。ただし、異型断面の極細繊維を採用した場合には、まず単繊維の断面積を測定し、当該断面積となる円の直径を以下の式で算出する。これより得られた直径をその単繊維の単繊維直径とする
単繊維直径(μm)=(4×(単繊維の断面積(μm2))/π)1/2
(3)得られた合計150点の算術平均値(μm)を算出し、小数点以下第二位で四捨五入する。
次に、本発明のシート状物は、高分子弾性体を有する。この高分子弾性体は、高分子弾性体前駆体と架橋剤とが反応して形成されるものである。以下、この詳細について、さらに説明する。
まず、本発明に係る高分子弾性体前駆体は、親水性基を有する。本発明において「親水性基を有する」とは、そのものが「活性水素を有する基を有する」ことを指す。この活性水素を有する基の具体例としては、水酸基やカルボキシル基、スルホン酸基、アミノ基等が挙げられる。
本発明で好ましく用いられる高分子ポリオールは、ポリエーテル系ポリオール、ポリエステル系ポリオール、ポリカーボネート系ポリオール等を挙げることができる。
本発明で好ましく用いられる有機ジイソシアネートとしては、炭素数(イソシアネート基中の炭素を除く、以下同様。)が6以上20以下の芳香族ジイソシアネート、炭素数が2以上18以下の脂肪族ジイソシアネート、炭素数が4以上15以下の脂環式ジイソシアネート、炭素数が8以上15以下の芳香脂肪族ジイソシアネート、これらのジイソシアネートの変性体(カーボジイミド変性体、ウレタン変性体、ウレトジオン変性体など。)およびこれらの2種以上の混合物等が挙げられる。
本発明で好ましく用いられる親水性基を有する活性水素成分含有化合物としては、ノニオン性基および/またはアニオン性基および/またはカチオン性基と活性水素とを含有する化合物等が挙げられる。これらの活性水素成分含有化合物は、中和剤で中和した塩の状態でも用いることができる。この親水性基を有する活性水素成分含有化合物を用いることによって、シート状物の製造方法で用いられる水分散液の安定性を高めることができる。
本発明で好ましく用いられる鎖伸長剤としては、水、「エチレングリコール、プロピレングリコール、1,3-ブチレングリコール、1,4-ブタンジオール、1,6-ヘキサンジオール、ジエチレングリコールおよびネオペンチルグリコールなど」の低分子ジオール、「1,4-ビス(ヒドロキシメチル)シクロヘキサンなど」の脂環式ジオール、「1,4-ビス(ヒドロキシエチル)ベンゼンなど」の芳香族ジオール、「エチレンジアミンなど」の脂肪族ジアミン、「イソホロンジアミンなど」の脂環式ジアミン、「4,4-ジアミノジフェニルメタンなど」の芳香族ジアミン、「キシレンジアミンなど」の芳香脂肪族ジアミン、「エタノールアミンなど」のアルカノールアミン、ヒドラジン、「アジピン酸ジヒドラジドなど」のジヒドラジド、および、これらの2種以上の混合物が挙げられる。
前記のとおり、本発明で好ましく用いられる水分散型ポリウレタン樹脂は、前記の高分子ポリオールと、有機ジイソシアネートと、親水性基を有する活性水素成分含有化合物とを反応させて親水性プレポリマーを形成し、その後に鎖伸長剤を添加・反応させることによって調製される。
本発明に係る高分子弾性体前駆体は、ポリエーテルジオールおよび/またはポリカーボネートジオールを構成成分として含有することが好ましい。なお、本明細書において、「AがBを構成成分として含有する」とは、「Aを構成するモノマー成分、オリゴマー成分として、Bを含有する」ことを指す。
・機器:東ソー株式会社製「HLC-8220」
・カラム:東ソーTSKgel α-M
・溶媒:N,N-ジメチルホルムアミド(DMF)
・温度:40℃
・校正:ポリスチレン。
続いて、本発明に係る架橋剤は、カルボジイミド基、イソシアネート基、オキサゾリン基、エポキシ基、メラミン樹脂、およびシラノール基などを有する高分子化合物を用いることができる。
本発明のシート状物を高分子弾性体は、前記の高分子弾性体前駆体と架橋剤とが反応して形成されるものである。この反応によって、本発明の高分子弾性体は、高分子弾性体前駆体由来の親水性基と、さらに、N-アシルウレア結合および/またはイソウレア結合とを有するものとなる。これらの結合を有することによって、前記のとおり、シート状物の柔軟性を保持しながら、耐摩耗性等の物性を飛躍的に向上させることができる。
本発明のシート状物は、JIS L1096:2010「織物及び編物の生地試験法」の「8.21 剛軟度」に記載のA法(45°カンチレバー法)にて規定される縦方向の剛軟度が、40mm以上140mm以下である。剛軟度をこの範囲とすることで、適度な柔軟性と反発性を有するシート状物とすることができる。この剛軟度を50mm以上、より好ましくは55mm以上とすることで、より汎発性のあるシート状物とすることができる。一方、剛軟度を120mm以下、より好ましくは110mm以下とすることで、より柔軟性のあるシート状物とすることができる。
(A)乾燥時
(1) 室温18℃以上28℃以下、湿度35%以上75%以下の条件下で1時間以上静置する。
(2) シート状物から幅20mm、長さ300mm(うち、つかみ間隔200mm)の縦方向の試験片を5枚採取する。
(3) 試験片を初荷重(試験片を手でたるみが生じない程度に引っ張った状態の荷重)で定速伸長型引張試験機につかみ間隔200mmで取り付ける。
(4) 100mm/分の引張速度で試験片が切断するまで荷重を加える。
(5) 試験片の最大荷重時の強さ(N)を0.1N単位まで測定するとともに、最大荷重時の伸びを1mmまで測定する。この伸びから伸び率を求める。
(6) 各試験片について同様に測定し、最大荷重時の強さ(N)を試験片幅(cm)で除した値の算術平均値を引張強力(N/cm)、伸び率の算術平均値を引張強伸度(%)とする。
(B)湿潤時
(1) 室温18℃以上28℃以下、湿度35%以上75%以下の条件下で1時間以上静置する。
(2) シート状物を常温の水に10分間浸漬させる。
(3) シート状物から幅20mm、長さ300mm(うち、つかみ間隔200mm)の縦方向の試験片を5枚採取する。
(4) 試験片を初荷重(試験片を手でたるみが生じない程度に引っ張った状態の荷重)で定速伸長型引張試験機につかみ間隔200mmで取り付ける。
(5) 100mm/分の引張速度で試験片が切断するまで荷重を加える。
(6) 試験片の最大荷重時の強さ(N)を0.1N単位まで測定するとともに、最大荷重時の伸びを1mmまで測定する。この伸びから伸び率を求める。
(7) 各試験片について同様に測定し、最大荷重時の強さ(N)を試験片幅(cm)で除した値の算術平均値を引張強力(N/cm)、伸び率の算術平均値を引張強伸度(%)とする。
湿潤時の引張強力保持率(%)=湿潤時の引張強力(N/cm)/乾燥時の引張強力(N/cm)×100
湿潤時の引張強伸度保持率(%)=湿潤時の引張強伸度(%)/乾燥時の引張強伸度(%)×100。
(1) シート状物を裁断し、裁断した試験片のL値を色差計(例えば、コニカミノルタ株式会社製「CR-410」など)を用いて測定する。
(2) 試験片の起毛面を下にして、試験片を150℃に熱したホットプレート(例えば、アズワン株式会社製「CHP-250DN」など)上に載置する。
(3) 試験片上に、押圧荷重が2.5kPaとなるように調整した圧子を載置し、10秒間保持する。
(4) 試験片上の圧子を外し、試験片の起毛面のL値を前記の色差計で測定する。
(5) L値保持率を以下の式より算出する。
本発明のシート状物は、さらに、ISO 6330 C4N法に従う洗濯試験時において、前記のシート状物1枚の洗濯試験を実施し、試験後に排水ホースに取り付けた捕集袋に付着した繊維屑を、メンブレンフィルターを用いて捕集した場合の繊維屑量が10.0(mg/シート状物100cm2)以下とすることもできる。中でも、8.0(mg/シート状物100cm2)以下、より好ましくは6.0(mg/シート状物100cm2)以下、さらに好ましくは5.0(mg/シート状物100cm2)以下であることによって、シート状物が洗濯時に繊維脱落が少なく、環境負荷の少ないものとなる。
本発明のシート状物の製造方法は、下記(1)~(3)の工程をこの順に含む。
(1) 極細繊維発現型繊維からなる繊維質基材に、親水性基を有する高分子弾性体前駆体と、1価陽イオン含有無機塩と、架橋剤とを含有する水分散液を含浸せしめ、次いで水分散液を含浸させた繊維質基材の温度を100℃以上180℃以下として加熱乾燥処理を行って高分子弾性体を形成させる第1の高分子弾性体前駆体含浸工程であって、前記の水分散液における1価陽イオン含有無機塩の含有量を高分子弾性体前駆体100質量部に対して10質量部以上100質量部以下とする、第1の高分子弾性体前駆体含浸工程
(2) 前記の極細繊維発現型繊維から極細繊維を発現させて前記の極細繊維からなる極細繊維質基材を形成する、極細繊維発現工程
(3) 前記の極細繊維からなる繊維質基材に、親水性基を有する高分子弾性体前駆体と、1価陽イオン含有無機塩と、架橋剤とを含有する水分散液を含浸せしめ、次いで水分散液を含浸させた繊維質基材の温度を100℃以上180℃以下として加熱乾燥処理を行って、さらに高分子弾性体を形成させる第2の高分子弾性体前駆体含浸工程であって、前記の水分散液における1価陽イオン含有無機塩の含有量が高分子弾性体前駆体100質量部に対して10質量部以上100質量部以下とする、第2の高分子弾性体前駆体含浸工程
以下に、これについて、詳細を順に説明する。
本工程では、極細繊維発現型繊維からなる繊維質基材に、親水性基を有する高分子弾性体前駆体と、1価陽イオン含有無機塩と、架橋剤とを含有する水分散液を含浸せしめ、次いで水分散液を含浸させた繊維質基材の温度を100℃以上180℃以下として加熱乾燥処理を行って高分子弾性体を形成させる。
まず、本工程で用いられる水分散液は、前記の親水性基を有する高分子弾性体前駆体と、1価陽イオン含有無機塩と、架橋剤とを含有する。
本工程では、前記の極細繊維発現型繊維からなる繊維質基材に、前記の水分散液を含浸せしめ、次いで水分散液を含浸させた繊維質基材の温度を100℃以上180℃以下として加熱乾燥処理を行い、高分子弾性体を形成させる。
本工程では、前記の極細繊維発現型繊維から極細繊維を発現させて前記の極細繊維からなる繊維質基材を形成する。
本工程では、極細繊維からなる繊維質基材に、親水性基を有する高分子弾性体前駆体と、1価陽イオン含有無機塩と、架橋剤とを含有する水分散液を含浸せしめ、次いで水分散液を含浸させた繊維質基材の温度を100℃以上180℃以下として加熱乾燥処理を行って、さらに高分子弾性体を形成させる。
本発明では、シート状物の少なくとも一面を起毛処理して表面に立毛を形成させてもよい。立毛を形成する方法は、特に限定されず、サンドペーパー等によるバフィング等、当分野で通常行われる各種方法を用いることができる。立毛長は短すぎると優美な外観が得られにくく、長すぎると、ピリングが発生しやすくなる傾向にあることから、立毛長は0.2mm以上1mm以下とすることが好ましい。
(1)極細繊維の平均単繊維直径:
走査型電子顕微鏡として、株式会社キーエンス製「VE-7800型」を用いてシート状物を構成する極細繊維を3000倍で観察し、30μm×30μmの視野内で無作為に抽出した50本の単繊維直径をμm単位で、小数第1位まで測定した。
JIS L1096:2010「織物および編物の生地試験方法」の8.21「剛軟度」の8.21.1に記載のA法(45°カンチレバー法)に基づき、縦方向へ2×35cmの試験片を5枚作成し、45°の角度の斜面を有する水平台へ置き、試験片を滑らせて試験片の一端の中央点が斜面と接したときのスケールを読み、5枚の平均値を求めた。
各実施例、比較例で調製される水分散液20gを内径12mmの試験管に入れ、温度計を先端が液面よりも下になるように差し込んだ後、試験管を封止し、95℃の温度の温水浴に水分散液の液面が温水浴の液面よりも下になるように浸漬した。温度計により試験管内の温度の上昇を確認しつつ、適宜1回あたり5秒以内の時間、試験管を引き上げて水分散液の液面の流動性の有無を確認できる程度に揺すり、水分散液の液面が流動性を失った温度を水分散液の感熱凝固温度とした。この測定を、水分散液1種につき3回ずつ行い、平均値を算出した。
上記シート状物より分離した高分子弾性体について、日本分光株式会社製「FT/IR 4000 series」を用いて、赤外分光分析により結合種を同定した。
得られたシート状物の表面品位は10人のパネラーによる評価で行い、下記の基準で評価して、最も人数の多かった評価結果を採用した。なお、表面品位の評価は、図1に示すように床面1と平行の位置にある検査台2の上にシート状物3を置き、目視確認する位置とシート状物とを結ぶ線4の距離が50cmとなるように、シート状物3に対して検査台平面から45°の角度でシート状物3を目視確認して判断した。また、検査台には、検査台上面から垂直方向に150cm上部に32Wの蛍光灯6が設置されていた。その蛍光灯6の真下、すなわち、シート状物から蛍光灯への垂線7を引くことができる位置にシート状物3を置いて表面品位評価を実施した。外観品位は、4級~5級を良好であるものとした。
5級:均一な繊維の立毛があり、繊維の分散状態は良好で、外観は良好であった。
4級:5級と3級の間の評価である。
3級:繊維の分散状態はやや良くない部分があったが、繊維の立毛はあり、外観はまずまず良好であった。
2級:3級と1級の間の評価である。
1級:繊維の立毛は少なく、また、全体的に繊維の分散状態は非常に悪く、外観は不良であった。
摩耗評価に用いるマーチンデール摩耗試験機として、James H.Heal&Co.社製の「Model 406」を用い、標準摩擦布として同社の「ABRASTIVE CLOTH SM25」を用いた。評価基準は、シート状物の外観が摩耗前と全く変化が無かったものを5級とし、直径1mm以上の毛玉が30個以上発生したものを1級とし、その間を0.5級ずつに区切った。また、摩耗前後のシート状物の質量を用いて、下記の式により、摩耗減量を算出した。
(7)湿潤時の引張強力保持率および引張強伸度保持率(耐染色性):
定速伸長型引張試験機として、Illinois Tool Works Inc.製「Instron 3343」を用いた。
シート状物をN,N-ジメチルホルムアミドに一晩浸漬させ、高分子弾性体および無機塩を溶出させた溶液を140℃での加熱乾燥により濃縮し、固形化させた。得られた固形物に対し、蒸留水を加え、無機塩のみを溶出させた。この無機塩を含む水溶液を加熱乾燥した上で、シート状物中に含まれる無機塩の量を測定した。また、固形化した高分子弾性体についても加熱乾燥の上、重量を測定し、高分子弾性体質量対比での無機塩重量を算出した。ただし、数値の有効性の観点から高分子弾性体対比で0.1質量%未満は、検出下限未満とする。
ホットプレートとして、アズワン株式会社製「CHP-250DN」を用い、色差計として、コニカミノルタ株式会社製「CR-410」を用い、前記の方法によって測定、算出を行った。
シート状物から10cm×10cm(100cm2)の試験片を切り出し、前記の方法にて洗濯試験を実施し、繊維屑量を算出した。測定は2回行い、その平均値を洗濯時の繊維屑量とした。
高分子ポリオールとして数平均分子量(Mn)が2000のポリテトラメチレンエーテルグリコール、有機ジイソシアネートとしてMDI、親水性基を有する活性水素成分含有化合物として、2,2-ジメチロールプロピオン酸を用い、トルエン溶媒中でプレポリマーを作成した。さらに、鎖伸長剤としてエチレングリコールとエチレンジアミン、外部乳化剤としてポリオキシエチレンノニルフェニルエーテルと水を添加して、攪拌した。減圧化でトルエンを除去して、高分子弾性体前駆体aの水分散液Waを得た。なお、高分子弾性体前駆体aは、高分子弾性体Aに対応する高分子弾性体前駆体である。
高分子ポリオールとして数平均分子量(Mn)が2000のポリヘキサメチレンカーボネート、有機ジイソシアネートとして水添MDI、親水性基を有する活性水素成分含有化合物として、側鎖にポリエチレングリコールを有するジオール化合物および2,2-ジメチロールプロピオン酸を用い、アセトン溶媒中でプレポリマーを作成した。鎖伸長剤としてエチレングリコールとエチレンジアミンと水を添加して、攪拌した。減圧化でアセトンを除去して高分子弾性体前駆体bの水分散液Wbを得た。なお、高分子弾性体前駆体bは、高分子弾性体Bに対応する高分子弾性体前駆体である。
(極細繊維発現型不織布)
海成分として、5-スルホイソフタル酸ナトリウムを8モル%共重合したポリエチレンテレフタレートを用い、島成分として、ポリエチレンテレフタレートを用い、海成分が20質量%で島成分が80質量%の複合比率で、島数16島/1フィラメント、平均繊維直径が20μmの海島型複合繊維を得た。得られた海島型複合繊維を、繊維長51mmにカットしてステープルとし、カードおよびクロスラッパーを通して繊維ウェブを形成し、ニードルパンチ処理により不織布とした。このようにして得られた不織布を、97℃の温度の湯中に2分間浸漬させて収縮させ、100℃の温度で5分間乾燥させた。
高分子弾性体前駆体aを100質量部として、感熱凝固剤として硫酸ナトリウム(表1では「Na2SO4」と記載)を35質量部添加し、カルボジイミド系架橋剤を3質量部加え、水によって全体を固形分11質量%となるように、高分子弾性体前駆体aを含む水分散液Waを調製した。感熱凝固温度は、65℃であった。得られた繊維質基材用不織布を、前記の水分散液に浸漬し、次いで160℃の温度の熱風で20分間乾燥することにより、繊維重量に対して高分子弾性体Aが10質量%付与された高分子弾性体付与不織布を得た。
得られた高分子弾性体付与不織布を、95℃の温度に加熱した濃度8g/Lの水酸化ナトリウム水溶液に浸漬して30分間処理を行い、海島型複合繊維の海成分を除去した極細繊維からなるシート(高分子弾性体付与極細繊維不織布)を得た。
高分子弾性体前駆体bを100質量部として、感熱凝固剤として硫酸ナトリウムを35質量部添加し、カルボジイミド系架橋剤を3質量部加え、水によって全体を固形分11質量%となるように、高分子弾性体前駆体bを含む水分散液Wbを調製した。感熱凝固温度は、65℃であった。得られた繊維質基材用不織布を、前記の水分散液に浸漬し、次いで160℃の温度の熱風で20分間乾燥することにより、繊維重量に対して高分子弾性体Bが10質量%付与された高分子弾性体付与不織布を得た。
得られた高分子弾性体樹脂付与シートを厚さ方向に垂直に半裁し、半裁面の反対側をサンドペーパー番手240番のエンドレスサンドペーパーで研削することにより、厚みが0.7mmの立毛を有するシート状物を得た。
得られた立毛を有するシート状物を、液流染色機を用いて120℃の温度条件下で黒色染料を用いて染色を行った。次いで乾燥機で乾燥を行い、極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は84mm、表面品位は5級、DMF処理後の耐摩耗性は級数4.5級/摩耗減量7.6mg、湿潤時の引張強力保持率83%/引張強伸度保持率119%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。ここで、高分子弾性体内部にN-アシルウレア結合および/またはイソウレア結合を有するとは、高分子弾性体がN-アシルウレア結合および/またはイソウレア結合を有することを表す。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は97%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は2.9(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第1の高分子弾性体樹脂の付与)において、架橋剤としてカルボジイミド系架橋剤を3質量部加えていたところを、ブロックイソシアネート系架橋剤を3質量部添加することに変えたこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は94mm、表面品位は5級、DMF処理後の耐摩耗性は級数4.5級/摩耗減量7.8mg、湿潤時の引張強力保持率81%/引張強伸度保持率119%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は93%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は3.1(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第2の高分子弾性体樹脂の付与)において、架橋剤としてカルボジイミド系架橋剤を3質量部加えていたところを、ブロックイソシアネート系架橋剤を3質量部添加することに変えたこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は89mm、表面品位は5級、DMF処理後の耐摩耗性は級数4.5級/摩耗減量8.5mg、湿潤時の引張強力保持率80%/引張強伸度保持率114%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は94%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は3.4(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第2の高分子弾性体樹脂の付与)において、高分子弾性体前駆体として高分子弾性体前駆体bを用いていたところを、高分子弾性体前駆体aを用いることに変えたこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は82mm、表面品位は4.5級、DMF処理後の耐摩耗性は級数4級/摩耗減量8.8mg、湿潤時の引張強力保持率77%/引張強伸度保持率122%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリエーテル結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は93%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は3.4(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第1の高分子弾性体樹脂の付与)において、高分子弾性体前駆体として高分子弾性体前駆体aを用いていたところを、高分子弾性体前駆体bを用いることに変えたこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は98mm、表面品位は4級、DMF処理後の耐摩耗性は級数4.5級/摩耗減量7.7mg、湿潤時の引張強力保持率84%/引張強伸度保持率111%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は96%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は2.8(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第1の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを12質量部添加することに変えて、感熱凝固温度を70℃に調整したこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は94mm、表面品位は4級、DMF処理後の耐摩耗性は級数4級/摩耗減量7.7mg、湿潤時の引張強力保持率83%/引張強伸度保持率117%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は90%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は2.8(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第1の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを86質量部添加することに変えて、感熱凝固温度を60℃に調整したこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は80mm、表面品位は4級、DMF処理後の耐摩耗性は級数4級/摩耗減量13.5mg、湿潤時の引張強力保持率80%/引張強伸度保持率115%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は91%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は5.4(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第2の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを12質量部添加することに変えて、感熱凝固温度を70℃に調整したこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は98mm、表面品位は4級、DMF処理後の耐摩耗性は級数4級/摩耗減量8.0mg、湿潤時の引張強力保持率83%/引張強伸度保持率114%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は91%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は2.6(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第2の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを86質量部添加することに変えて、感熱凝固温度を60℃に調整したこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は88mm、表面品位は4級、DMF処理後の耐摩耗性は級数4級/摩耗減量14.1mg、湿潤時の引張強力保持率81%/引張強伸度保持率113%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は93%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は5.8(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第1の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを塩化ナトリウム(表1では「NaCl」と記載)を30質量部添加することに変えて、感熱凝固温度を65℃に調整し、さらに、(第2の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを塩化ナトリウムを30質量部添加することに変えて、感熱凝固温度を65℃に調整したこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は86mm、表面品位は5級、DMF処理後の耐摩耗性は級数4.5級/摩耗減量7.4mg、湿潤時の引張強力保持率83%/引張強伸度保持率119%であり、柔軟な風合いと優れた耐薬品性および耐染色性を有していた。また、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。さらに、L値保持率は96%であり、優れた耐熱性を有していた。また、洗濯時の繊維屑量は2.9(mg/シート状物100cm2)であり、環境負荷の小さいものであった。
実施例1の(第2の高分子弾性体樹脂の付与)の工程を経ないこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は81mm、表面品位は5級、DMF処理後の耐摩耗性は級数2級/摩耗減量33.5mg、湿潤時の引張強力保持率72%/引張強伸度保持率103%であり、柔軟な風合いであり、L値保持率も93%と優れた耐熱性を有していたが、耐薬品性および耐染色性が劣位であった。また、洗濯時の繊維屑量は12.5(mg/シート状物100cm2)であり、環境負荷の大きいものであった。なお、高分子弾性体内部にポリエーテル結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
比較例1の(第1の高分子弾性体樹脂の付与)において、高分子弾性体前駆体として高分子弾性体前駆体bを用いたこと以外は、比較例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は92mm、表面品位は3.5級、DMF処理後の耐摩耗性は級数2級/摩耗減量29.9mg、湿潤時の引張強力保持率73%/引張強伸度保持率101%であり、柔軟な風合いであり、L値保持率も94%と優れた耐熱性を有していたが、耐薬品性および耐染色性が劣位であった。また、洗濯時の繊維屑量は11.4(mg/シート状物100cm2)であり、環境負荷の大きいものであった。なお、高分子弾性体内部にポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第1の高分子弾性体樹脂の付与)において、感熱凝固剤の添加をしなかったこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は150mm以上、表面品位は2級、DMF処理後の耐摩耗性は級数4級/摩耗減量7.4mg、湿潤時の引張強力保持率84%/引張強伸度保持率109%であり、耐薬品性および耐染色性は良好であり、洗濯時の繊維屑量は2.8(mg/シート状物100cm2)であって、環境負荷の小さいものであったものの、硬い風合いであった。さらに、L値保持率は84%であり、耐熱性は十分なものではなかった。なお、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第2の高分子弾性体樹脂の付与)において、感熱凝固剤の添加をしなかったこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は150mm以上、表面品位は2級、DMF処理後の耐摩耗性は級数4級/摩耗減量7.1mg、湿潤時の引張強力保持率82%/引張強伸度保持率110%であり、耐薬品性および耐染色性は良好であり、洗濯時の繊維屑量は3.0(mg/シート状物100cm2)であって、環境負荷の小さいものであったものの、硬い風合いであった。さらに、L値保持率は86%であり、耐熱性は十分なものではなかった。なお、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第1の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを5質量部添加することに変えて、感熱凝固温度を85℃に調整したこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は144mm、表面品位は2.5級、DMF処理後の耐摩耗性は級数4級/摩耗減量8.0mg、湿潤時の引張強力保持率82%/引張強伸度保持率111%であり、耐薬品性および耐染色性は良好であり、洗濯時の繊維屑量は2.6(mg/シート状物100cm2)であって、環境負荷の小さいものであったものの、硬い風合いであった。さらに、L値保持率は85%であり、耐熱性は十分なものではなかった。なお、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第1の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを120質量部添加することに変えて、感熱凝固温度を50℃に調整したこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は84mm、表面品位は1.5級、DMF処理後の耐摩耗性は級数3級/摩耗減量21.2mg、湿潤時の引張強力保持率80%/引張強伸度保持率114%であり、柔軟な風合い、良好な耐染色性であって、L値保持率も90%と一定の耐熱性を有しており、また、洗濯時の繊維屑量は8.8(mg/シート状物100cm2)であり、環境負荷の小さいものであったが、耐薬品性および品位が劣位であった。なお、高分子弾性体内部にN-アシルウレア結合とイソウレア結合が存在した。また、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第2の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを5質量部添加することに変えて、感熱凝固温度を85℃に調整したこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は148mm、表面品位は2.5級、DMF処理後の耐摩耗性は級数4級/摩耗減量7.8mg、湿潤時の引張強力保持率77%/引張強伸度保持率120%であり、耐薬品性および耐染色性は良好であり、洗濯時の繊維屑量は2.6(mg/シート状物100cm2)であって、環境負荷の小さいものであったものの、硬い風合いであった。さらに、L値保持率は87%であり、耐熱性は十分なものではなかった。なお、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第2の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを120質量部添加することに変えて、感熱凝固温度を50℃に調整したこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は86mm、表面品位は1.5級、DMF処理後の耐摩耗性は級数3級/摩耗減量32.7mg、湿潤時の引張強力保持率74%/引張強伸度保持率113%であり、柔軟な風合い、良好な耐染色性であるが、耐薬品性および品位が劣位であった。さらに、L値保持率は89%であり、耐熱性は十分なものではなかった。また、洗濯時の繊維屑量は12.1(mg/シート状物100cm2)であり、環境負荷の大きいものであった。なお、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N‐アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第1の高分子弾性体樹脂の付与)において、架橋剤の添加をせず、(第2の高分子弾性体樹脂の付与)においても架橋剤の添加をしなかったこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は96mm、表面品位は3級、DMF処理後の耐摩耗性は級数2級/摩耗減量32.0mg、湿潤時の引張強力保持率71%/引張強伸度保持率97%であり、良好な風合いであるものの、耐薬品性、耐染色性が劣位であった。さらに、L値保持率は88%であり、耐熱性は十分なものではなかった。また、洗濯時の繊維屑量は13.6(mg/シート状物100cm2)であり、環境負荷の大きいものであった。なお、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合は存在しなかった。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第1の高分子弾性体樹脂の付与)において、感熱凝固剤を添加していたところを発泡剤(AIBN)を3質量%添加することに変えたこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は145mm、表面品位は2級、DMF処理後の耐摩耗性は級数3級/摩耗減量19.5mg、湿潤時の引張強力保持率77%/引張強伸度保持率107%であり、耐染色性に優れ、洗濯時の繊維屑量は9.1(mg/シート状物100cm2)であって、環境負荷の小さいものであったものの、風合い、品位、耐薬品性が劣位であった。さらに、L値保持率は88%であり、耐熱性は十分なものではなかった。なお、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第2の高分子弾性体樹脂の付与)において、高分子弾性体前駆体としてDMFに溶解しているポリカーボネート系高分子弾性体前駆体を用いたこと以外は、実施例1と同様にして極細繊維の平均単繊維繊度が4.4μmのシート状物を得た。得られたシート状物の剛軟度は97mm、表面品位は3級、DMF処理後の耐摩耗性は級数2級/摩耗減量42.7mg、湿潤時の引張強力保持率81%/引張強伸度保持率118%であり、柔軟な風合いと優れた耐染色性を有しており、洗濯時の繊維屑量は2.7(mg/シート状物100cm2)であって、環境負荷の小さいものであったが耐薬品性が劣位であった。さらに、L値保持率は88%であり、耐熱性は十分なものではなかった。なお、高分子弾性体内部にポリエーテル結合、ポリカーボネート結合、N-アシルウレア結合およびイソウレア結合が存在した。また、高分子弾性体内部の無機塩量は検出下限未満であった。
実施例1の(第2の高分子弾性体樹脂の付与)において、感熱凝固剤として硫酸ナトリウムを35質量部添加していたところを硫酸マグネシウム(表1では「MgSO4」と記載)を35質量部添加することに変え、カルボジイミド系架橋剤3質量%加え、水によって全体を固形分11質量%に調製し、高分子弾性体aを含む水分散液を得たが、加工中に不織布表面でゲル化し、不織布に高分子弾性体を付与することができなかった。
2: 検査台
3: シート状物
4: 目視確認する位置とシート状物とを結ぶ線
5: 目視確認する位置
6: 蛍光灯
7: シート状物から蛍光灯への垂線
Claims (14)
- 極細繊維からなる繊維質基材と、高分子弾性体とを有するシート状物であって、前記極細繊維の平均単繊維直径は0.1μm以上10.0μm以下であり、前記高分子弾性体が親水性基とN-アシルウレア結合および/またはイソウレア結合とを有し、以下の条件1および条件2を満たす、シート状物。
条件1:JIS L1096:2010「織物及び編物の生地試験方法」の「8.21 剛軟度」に記載のA法(45°カンチレバー法)にて規定される縦方向の剛軟度が、40mm以上140mm以下である
条件2:N,N-ジメチルホルムアミドに24時間浸漬後のJIS L1096:2010「織物及び編物の生地試験方法」の「8.19 摩耗強さ及び摩擦変色性」に記載のE法(マーチンデール法)で規定される押圧荷重12.0kPa、摩擦回数20000回における摩耗試験において4級以上であり、摩耗減量が25mg以下である - 前記高分子弾性体が高分子弾性体Aおよび該高分子弾性体Aとは異なる高分子弾性体Bの2種を含む、請求項1に記載のシート状物。
- 前記シート状物の湿潤時の引張強力が乾燥時の75%以上である、請求項1または2に記載のシート状物。
- 前記シート状物の湿潤時の引張強伸度が乾燥時の100%以上である、請求項1~3のいずれかに記載のシート状物。
- 前記シート状物において、さらに以下の条件3を満たす、請求項1~4のいずれかに記載のシート状物。
条件3:前記シート状物の起毛面を150℃に加熱したホットプレート上に載置し、押圧荷重2.5kPaで10秒間押圧した際のL値の保持率が90%以上100%以下である - 前記シート状物において、さらに以下の条件4を満たす、請求項1~5のいずれかに記載のシート状物。
条件4:ISO 6330 C4N法に従う洗濯試験時において、前記シート状物1枚の洗濯試験を実施し、試験後に排水ホースに取り付けた捕集袋に付着した繊維屑を、メンブレンフィルターを用いて捕集した場合の繊維屑量が10.0(mg/シート状物100cm2)以下である - 下記(1)~(3)の工程をこの順に含む、請求項1に記載のシート状物の製造方法。
(1) 極細繊維発現型繊維からなる繊維質基材に、親水性基を有する高分子弾性体前駆体と、1価陽イオン含有無機塩と、架橋剤とを含有する水分散液を含浸せしめ、次いで水分散液を含浸させた繊維質基材の温度を100℃以上180℃以下として加熱乾燥処理を行って高分子弾性体を形成させる第1の高分子弾性体前駆体含浸工程であって、前記水分散液における1価陽イオン含有無機塩の含有量を高分子弾性体前駆体100質量部に対して10質量部以上100質量部以下とする、第1の高分子弾性体前駆体含浸工程
(2) 前記極細繊維発現型繊維から極細繊維を発現させて前記極細繊維からなる繊維質基材を形成する、極細繊維発現工程
(3) 前記極細繊維からなる繊維質基材に、親水性基を有する高分子弾性体前駆体と、1価陽イオン含有無機塩と、架橋剤とを含有する水分散液を含浸せしめ、次いで水分散液を含浸させた繊維質基材の温度を100℃以上180℃以下として加熱乾燥処理を行って、さらに高分子弾性体を形成させる第2の高分子弾性体前駆体含浸工程であって、前記水分散液における1価陽イオン含有無機塩の含有量が高分子弾性体前駆体100質量部に対して10質量部以上100質量部以下とする、第2の高分子弾性体前駆体含浸工程 - 前記第1の高分子弾性体前駆体含浸工程の高分子弾性体前駆体と前記第2の高分子弾性体前駆体含浸工程の高分子弾性体前駆体とで用いられる高分子弾性体前駆体が同一の高分子弾性体前駆体である、請求項7に記載のシート状物の製造方法。
- 前記高分子弾性体前駆体がポリエーテルジオールおよび/またはポリカーボネートジオールを含む、請求項7または8に記載のシート状物の製造方法。
- 前記第1の高分子弾性体前駆体含浸工程の高分子弾性体前駆体が高分子弾性体前駆体Aであり、前記第2の高分子弾性体前駆体含浸工程の高分子弾性体前駆体とで用いられる高分子弾性体前駆体が該高分子弾性体前駆体Aとは異なる高分子弾性体前駆体Bである、請求項7に記載のシート状物の製造方法。
- 前記高分子弾性体前駆体Aが構成成分としてポリエーテルジオールを含む、請求項10に記載のシート状物の製造方法。
- 前記高分子弾性体前駆体Bが構成成分としてポリカーボネートジオールを含む、請求項10または11に記載のシート状物の製造方法。
- 前記架橋剤がカルボジイミド系架橋剤および/またはブロックイソシアネート架橋剤である、請求項7~12のいずれかに記載のシート状物の製造方法。
- 前記1価陽イオン含有無機塩が塩化ナトリウムおよび/または硫酸ナトリウムである、請求項7~13のいずれかに記載のシート状物の製造方法。
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PCT/JP2020/046006 WO2021125029A1 (ja) | 2019-12-20 | 2020-12-10 | シート状物およびその製造方法 |
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US (1) | US20230009350A1 (ja) |
EP (1) | EP4079961A4 (ja) |
JP (1) | JP6904494B1 (ja) |
KR (1) | KR20220111272A (ja) |
CN (1) | CN114829701B (ja) |
WO (1) | WO2021125029A1 (ja) |
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EP3951047A4 (en) * | 2019-03-29 | 2022-12-28 | Toray Industries, Inc. | LEAF-FORM ARTICLE AND METHOD OF MANUFACTURE THEREOF |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2011214210A (ja) | 2010-03-16 | 2011-10-27 | Toray Ind Inc | シート状物およびその製造方法 |
WO2013065608A1 (ja) * | 2011-10-31 | 2013-05-10 | 東レ株式会社 | シート状物およびその製造方法 |
WO2014042241A1 (ja) * | 2012-09-14 | 2014-03-20 | 東レ株式会社 | シート状物の製造方法及びこの製造方法より得られるシート状物 |
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JP4093777B2 (ja) * | 2002-03-14 | 2008-06-04 | 旭化成せんい株式会社 | スエード調人工皮革 |
JP2013112905A (ja) * | 2011-11-28 | 2013-06-10 | Toray Ind Inc | シート状物 |
US20160002835A1 (en) * | 2013-02-12 | 2016-01-07 | Kuraray Co., Ltd. | Hard sheet and method for producing the same |
JP6180873B2 (ja) * | 2013-08-30 | 2017-08-16 | 株式会社クラレ | 繊維複合シート、研磨パッド及びその製造方法 |
WO2015129602A1 (ja) | 2014-02-27 | 2015-09-03 | 東レ株式会社 | シート状物およびその製造方法 |
JP6267590B2 (ja) * | 2014-06-05 | 2018-01-24 | 株式会社クラレ | 繊維複合シートの製造方法 |
EP3604667B1 (en) * | 2017-03-29 | 2024-06-26 | Toray Industries, Inc. | Sheet-like material |
CN111918998A (zh) * | 2018-04-12 | 2020-11-10 | 东丽株式会社 | 片状物及其制造方法 |
JP7322573B2 (ja) * | 2019-07-30 | 2023-08-08 | 東レ株式会社 | シート状物およびその製造方法 |
WO2022114041A1 (ja) * | 2020-11-30 | 2022-06-02 | 東レ株式会社 | 人工皮革およびその製造方法 |
-
2020
- 2020-12-10 WO PCT/JP2020/046006 patent/WO2021125029A1/ja active Application Filing
- 2020-12-10 JP JP2020569211A patent/JP6904494B1/ja active Active
- 2020-12-10 CN CN202080086970.1A patent/CN114829701B/zh active Active
- 2020-12-10 EP EP20902145.0A patent/EP4079961A4/en active Pending
- 2020-12-10 KR KR1020227018851A patent/KR20220111272A/ko unknown
- 2020-12-10 US US17/784,749 patent/US20230009350A1/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2011214210A (ja) | 2010-03-16 | 2011-10-27 | Toray Ind Inc | シート状物およびその製造方法 |
WO2013065608A1 (ja) * | 2011-10-31 | 2013-05-10 | 東レ株式会社 | シート状物およびその製造方法 |
WO2014042241A1 (ja) * | 2012-09-14 | 2014-03-20 | 東レ株式会社 | シート状物の製造方法及びこの製造方法より得られるシート状物 |
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See also references of EP4079961A4 |
Also Published As
Publication number | Publication date |
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TW202132388A (zh) | 2021-09-01 |
KR20220111272A (ko) | 2022-08-09 |
EP4079961A4 (en) | 2024-01-24 |
CN114829701A (zh) | 2022-07-29 |
US20230009350A1 (en) | 2023-01-12 |
EP4079961A1 (en) | 2022-10-26 |
JPWO2021125029A1 (ja) | 2021-12-23 |
CN114829701B (zh) | 2023-10-20 |
JP6904494B1 (ja) | 2021-07-14 |
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