JPH09188975A - Leathery sheet-like article and its production - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a leathery sheet-like article excellent in flexibility and touch feeling, with natural appearance and dampish touch, having smooth surface as compared to those of conventional analogous articles, highly excellent in air and moisture permeability. SOLUTION: This article is a sheet-like article provided with a coat at least on one side of a fibrous base material. The coat has microjoint structure 2. This article is obtained by forming a continuous film at least on one side of the base material followed by mechanically and/or chemically finely dividing the continuous film.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a leather-like sheet material having a soft and moist feel, which has never existed before, and a method for producing the same.

[0002]

2. Description of the Related Art As a leather-like sheet material, there is known one in which a film-like continuous film is formed by coating or transferring a polymer elastic material or the like as a coating layer on the surface of a woven or knitted or non-woven fabric substrate. However, regarding the texture and flexibility,
It is hard, film-like, has no natural appearance and touch, is plastic-like, breathable,
There is also a problem that the moisture permeability is insufficient.

Among the above problems, as a method of softening the texture, a method of using a flexible material for the film forming the surface coating layer is known, but such a film is weak against abrasion and is durable. There was a problem of low sex. Further, although a certain degree of flexibility can be obtained by using a microporous structure film of a polymeric elastic body, it is not yet satisfactory and there is a drawback that the texture becomes rubber-like. Further, as a method for improving the appearance and touch, a method is known in which after forming a surface layer, embossing, or after forming a film on a release paper having skin-texture-like unevenness, transferring it onto a substrate. There is. All of these tried to imitate the irregularities of natural leather, but after all, only a regular and artificial appearance was obtained. Furthermore, a method of forming random irregularities on the sheet surface by mixing fine particles during film formation is known, but this method also has some effect, but only an artificial and plastic-like appearance is obtained. I couldn't do it. Known methods for improving air permeability and moisture permeability include a method in which the coating layer has a microporous structure and a method in which a hydrophilic substance is added to the coating layer. Although breathability and moisture permeability are improved to some extent by these methods,
Since the coating layer impairs the air permeability and moisture permeability of the substrate, satisfactory performance has not been obtained.

Incidentally, JP-A-6-33577 suggests a method for obtaining a leather sheet in which an elastic polymer and naps are mixed on the surface. In this method, an elastic polymer is applied to the surface of a fibrous sheet, and then the polymer on the surface of the fiber is buffed until at least one part is left to form naps, and then the fibrous sheet is contracted. Since it is provided, the obtained sheet-like material is a nubuck-like one having fluffs due to buffing and fine creases due to contraction of the base material on the silver surface, and is not a smooth and smooth surface. In addition, in addition, since the nubuck-like leather sheet-like material is a composite of a low-shrinkage elastic polymer and a high-shrinkage fiber, residual strain occurs and unevenness occurs on the surface due to dry cleaning. There was one.

As described above, there is no means for fundamentally solving the conventional problems, and much less means for solving them at the same time.

[0006]

In view of the problems of the prior art, the present invention has excellent flexibility and texture, has a natural appearance and a moist touch, and has a smoother and smoother surface than conventional products. And a leather-like sheet having excellent breathability and moisture permeability, and a method for producing the same.

[0007]

The present invention employs the following means to solve the above-mentioned problems. That is,
The leather-like sheet material of the present invention is a sheet material having a coating layer on at least one side of a base material, wherein the coating layer has a microjoint structure,
Further, the method for producing such a leather-like sheet is a substrate containing fibers, in the method for producing a leather-like sheet having a coating layer on at least one side, after forming a continuous film on at least one side of the substrate, It is characterized in that the continuous film is mechanically and / or chemically finely divided.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention has been earnestly studied in view of the problems of the above-mentioned technology, and the problems are that the surface of the substrate is covered with a film-like uniform continuous film. By investigating the cause, and making the coating layer a specific structural form, it is a leather-like sheet excellent in flexibility, texture, appearance as well as breathability and moisture permeability compared to conventional products. It has succeeded in providing goods.

The micro joint structure as used in the present invention means
It consists of a minute unit film and a micro joint. ◎ On the contrary, in the conventional artificial leather with silver, the surface of the base material was covered with a continuous film or film to give a sheet-like appearance to leather.

That is, contrary to such a conventional one,
The microjoint structure of the present invention is an assembly of minute unit films as shown in FIG. 1, and by having a microjoint portion between the unit films, a scratch resistance of the silver surface, which has not been obtained conventionally, It is a new skin-sensing artificial leather that combines flexibility, touch and, by extension, an extremely natural appearance.

The unit film referred to here is a film independent of the unit film, and is a film in which the surface of the base material is coated or integrated with the base material. In addition, the micro joint portion mentioned here exists between the unit membranes and has a function of freely bending.

The size of the unit film of the present invention is not particularly limited, but in terms of quality, it is preferable that the unit film at first glance looks like one continuous film, so that the area is 0.1.
Square centimeters or less are preferred and 0.01 square centimeters or less are most preferred. In addition, it is preferable that the size is small from the viewpoint of reducing the wrinkles in terms of quality. Therefore, when it is used for clothing, it is better to make it as small as possible, but when it is used for shoes and the like, it is not necessarily required to be 0.1 square centimeter or less. The unit membrane and the unit membrane may be completely separated or partly connected.

Further, the unit membranes may be connected by a softer substance. Further, as shown in FIG. 1, those having different sizes and shapes may be included, or as shown in FIG. 2, an aggregate of the same shapes may be included.

The substance constituting the unit membrane is not particularly limited, but polyester, polyamide, polyvinyl chloride, polyacrylic acid ester copolymer, polyamino acid,
Polyamino acid polyurethane copolymers, silicone resins and the like can be used, but elastic high molecular polymers, particularly polyurethanes are preferable from the viewpoint of softening the texture. The type of polyurethane is not particularly limited, and for example, polyether type, polyester type, polycarbonate type urethane can be used.

Further, it is preferable to add a cross-linking agent if necessary, since the durability of the sheet-like material is improved and the micro joint structure is easily formed. In addition, it is preferable that the unit film has a multi-layered structure in order to satisfy characteristics such as adhesiveness with a substrate, scratch resistance, and appearance. Also, if necessary,
Proteins such as collagen and fibroin, weathering agents such as antioxidants and ultraviolet absorbers, pigments, dyes, flame retardants, water repellents and the like can be included.

The micro joint portion of the present invention has a property of following the bending of the base material and not impairing the flexibility of the base material. Specifically, it may be one that connects the unit membranes with a material that is softer than the unit membrane, or the same material as the unit membrane may have weak adhesion to the base material, or a portion that is not adhered to the base material, It does not matter if there are only voids. Although the size of the micro joint is not particularly limited, it is preferably 0.1 mm or less, and most preferably 0.01 mm or less in terms of surface quality. On the other hand, from the viewpoint of flexibility, the size is preferably ⅓ or more of the film thickness, more preferably the film thickness or more, and most preferably twice or more the film thickness.

Therefore, it is necessary to appropriately select the material according to the material and thickness of the base material and the film, the desired flexibility, and the like. The ratio of the area of the micro joint part to the whole is 1 to
30% is preferred. If it is 1% or less, the effect of the present invention cannot be obtained, and if it is 30% or more, the quality and surface durability are deteriorated.

It is preferable that the fluff or fluffy fibers are exposed from the micro joints in order to improve the surface touch of the sheet-like material. As a result, fluff or fluff is generated on the surface, and a comfortable touch can be obtained when touched. This kind of touch is different from conventional silver, suede, and nubuck, and is unique to natural leather, and if you dare to say, it is a skin-like touch.

The length of the fiber is not particularly limited, and when it is longer than the film thickness, it is effective only by touching the surface, whereas
When the length is short, the effect is exhibited only when the sheet-like material is bent. In any case, a comfortable touch can be obtained and can be appropriately selected according to the purpose. The thickness of the napped fibers is preferably 0.5d or less. When it is 0.5d or less, hair fall becomes smooth, and a smoother and more comfortable feel is obtained.

In order to achieve the object of the present invention, the thickness of the unit film is not particularly limited, but is preferably 10 μm or less. The thinner the unit film, the more flexible and breathable, and a more natural appearance can be obtained. In forming such a micro joint structure, there is no particular limitation as long as the effect of the present invention is not impaired.

That is, the coating layer having the micro joint structure may be formed on the surface of the base material in one step, or the coating layer having the micro joint structure may be formed once and then transferred onto the base material. . Alternatively, it can be formed relatively easily by a method in which a continuous film is once formed and then microjoined as illustrated below.

First, as a method for forming a continuous film, either a dry method or a wet method may be used as long as the object of the present invention is satisfied. Further, either a method of directly coating on the surface of the base material or a method of forming the base material and the film separately and then bonding the both may be used.

As a method for directly coating the surface of the substrate,
Reverse roll coating, knife coating, gravure coating, slit coating, spraying and the like can be used. In addition, as a method of laminating the base material and the film separately and then bonding them together, a method of forming the film alone and then integrating it with the base material, or a method of forming the film on release paper and then transferring the film onto the base material A method can be adopted.

As a method of mechanically dividing the continuous film into microjoints, a kneading process in a dry state, a kneading process in a liquid, a rubbing process, or the like can be used.

It is preferable to crystallize by heat treatment or chemicals, add a cross-linking agent at the time of film formation, or carry out the dividing treatment under cooling in order to facilitate the dividing, before the microjoining treatment.

The method of removal by dissolution is not particularly limited. For example, a method of mixing components that can be removed later at the time of film formation and removing after forming the coating layer can be adopted. Further, for example, a micro joint can be formed relatively easily by performing a kneading process while heating in an alkaline aqueous solution.

The substrate used in the present invention is exemplified below, but other than that, the material and structure are not particularly limited as long as the object of the present invention can be achieved. For example, as the structure, a non-woven fabric, a woven fabric, a knitted fabric, a composite of these, or a base material to which a resin serving as a binder is added can be used. Whether or not a binder is applied to such a substrate can be appropriately selected depending on the important characteristics. For example, when importance is attached to morphological stability and texture, a binder can be added.

The binder is not particularly limited, but for example, a polymeric elastic material such as polyurethane, or a polyacrylic acid ester resin, a silicone resin, or the like can be applied in a solution or emulsion state.
When importance is attached to air permeability and flexibility, it is desirable not to add a binder.

In particular, the silver surface having a microjoint structure of the present invention is extremely flexible and highly breathable as compared with the silver surface of a conventional continuous film due to the presence of voids between the unit films. When combined with a base material that does not contain a binder, it is possible to obtain a leather-like sheet material that is flexible and has excellent air permeability.

The above-mentioned non-woven fabric is not particularly limited and may be a short fiber non-woven fabric or a long fiber non-woven fabric. Further, as a manufacturing method, spunbonding, meltblowing, flash spinning, needle punching, hydroentanglement, papermaking method, etc. can be appropriately adopted. There is no limitation on the structure and density of the woven fabric, and a plain weave or a twill weave can be appropriately used.
There is no particular limitation on the yarn processing of the woven yarn constituting the woven fabric, and a woven yarn can be appropriately selected according to the purpose from false twisting, crimping, non-twisting, sweet twisting to strong twisting. The same applies to knitted fabrics.

As the material for the base material, nylon 6, polyamide such as nylon 6,6, polyethylene terephthalate, polyethylene terephthalate containing a copolymerization component, polybutylene terephthalate, polyacrylonitrile, cotton, etc. may be used alone or in combination. Can be used.

In addition to the usual round cross section, the fiber constituting the substrate has a hollow cross section, a triangular or Y-shaped irregular cross section, or a composite yarn of two or more kinds of polymers, a sea-island type fiber, A blended yarn or the like can be appropriately selected according to the purpose. There is no particular limitation on the method for forming the fiber, and a normal spinning / drawing step can be adopted,
A super draw method, a method of spinning two or more kinds of components and then separating them by separation can be employed. In particular, when a method in which at least one component is dissolved and removed after spinning two or more polymers having different solubilities together, a space is formed between the fibers, and thus a sheet-like material having excellent flexibility is obtained. You can As a removing component in such a case, for example, polyethylene, polystyrene, copolymerized polystyrene, polyester, copolymerized polyester and the like can be used.

Further, it is preferable that the base material is made of ultrafine fibers and / or ultrafine fiber bundles of 0.2 d or less, and the distance between the entanglement points of the ultrafine fibers is 200 μm or less in order to achieve the object of the present invention. That is, when the fiber thickness is 0.2 d or less and the inter-entanglement point distance is 200 μm or less, unit membranes and micro joints are finely and uniformly generated, and the surface appearance and flexibility are significantly improved. Furthermore, since the thickness of the fiber is 0.2 d or less, the smoothness of the surface of the base material is improved, and the inter-entanglement point distance of 200 μm or less means that the ultrafine fibers are densely entangled. Yes, it has the effect of reinforcing the unit membrane. As a result, the unit film can be thinned, and a leather-like sheet material having excellent flexibility, breathability and moisture permeability can be obtained.

The inter-entanglement point distance referred to here is a value obtained by the following method, and the smaller the value is as one measure showing the denseness of the entanglement of fibers, the denser the entanglement is. Is shown.

FIG. 1 is an enlarged schematic view of the constituent fibers when the constituent fibers in the coating layer are observed from the surface side. The constituent fibers are f 1, f 2, f 3 ..., The point at which any two fibers f 1, f 2 are entangled is a 1, and the upper fiber f 2 at a 1 is the other fiber. Follow the intersection to the bottom and cross the intersection at a2 (f2
And the intersection of f3). Similarly, a3, a4, a5 ...
And Next, the distance straight line horizontal distances a1a2, a2a3, a3a4 ... Between the inter-entangled points thus obtained are measured, the average value of a large number of these measured values is obtained, and this is set as the fiber inter-entangled point distance.

Further, the above-mentioned base material is composed of ultrafine fibers and / or ultrafine fiber bundles of 0.2d or less and a woven or knitted fabric, and the distance between the entanglement points of the ultrafine fibers is 200 μm or less, and the ultrafine fibers and / or ultrafine fiber bundles It is preferable that the woven and knitted fabrics are integrated with each other in terms of flexibility and morphological stability of the sheet-shaped product.

In the case of the conventional leather-like sheet material, the morphological stability may be imparted to some extent by the surface coating layer. In the case of the coating layer of the present invention, it may be inferior in morphological stability as compared with the conventional coating layer, but by combining with the base material integrated with the woven or knitted material, the morphological stability is improved particularly when wet, and wet. Rubbing can be applied in the state.
As a result, flexibility is greatly improved. Further, it is needless to say that the improved morphological stability provides excellent properties as a material for clothing and materials.

There are no particular restrictions on the type of woven or knitted fabric as long as it satisfies the object of the present invention.

As the fibers to be used, natural fibers such as cotton, semi-synthetic fibers such as rayon, synthetic fibers such as polyamide and polyethylene terephthalate can be appropriately selected according to the purpose.

In addition to the usual round cross section, the shape of the thread may be a hollow cross section, a triangular or Y-shaped irregular cross section, a composite thread of two or more kinds of polymers, a sea-island type fiber, a blended thread, etc. depending on the purpose. Can be appropriately selected.

The yarn processing is also not particularly limited, and can be appropriately selected from false twisted yarn, crimped yarn, untwisted, sweet twist to strong twist depending on the purpose.

There is no limitation on the structure and density of the woven fabric, and a plain weave or a twill weave can be appropriately used. The same applies to knitted fabrics.

The method for integrating the ultrafine fibers and / or the ultrafine fiber bundles with the woven or knitted fabric is not particularly limited, but for example, a method of laminating with an adhesive or the like, a needle punch or a high-pressure columnar water stream can be used for entangling. It is possible to adopt a method of combining. In particular, by using a base material integrated by entanglement of fibers without using a binder, flexibility,
It is possible to obtain a sheet-shaped material having excellent breathability. The woven or knitted material may be present inside the substrate or on the surface without the coating layer.

[0044]

EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited thereto. Example 1 A 0.4 denier polyethylene terephthalate fiber was crimped, cut into 51 mm, made into a web using a card and a cross wrapper, and further needle-punched to obtain a nonwoven fabric. Polyurethane obtained by reacting a mixed diol of polyethylene adipate and polybutylene adipate with p, p'-diphenylmethane diisocyanate and diluting with a polyurethane DMF-toluene mixed solvent obtained by chain extension with ethylene glycol Then
It was a 10% solution. The nonwoven fabric was impregnated with the polyurethane DMF solution, and the content of polyurethane was adjusted to 35% based on the weight of the nonwoven fabric. Then, polyurethane was wet-solidified, immediately pressed and dried to obtain a substrate. The same polyurethane as above was applied to the substrate with a knife coater, dried and then pressed with a heating embossing roll at 180 ° C. It was rubbed and processed in an aqueous sodium hydroxide solution at 95 ° C. and 10 g / l.

The obtained product was thoroughly washed with water and then dyed with a disperse dye at 120 ° C. The surface has an average area of about 0.07
The square millimeter unit membrane formed the microjoint structure. The ratio of the micro joint part to the whole was about 15%.

The obtained leather-like sheet had a natural appearance and flexibility. Comparative Example 1 A leather-like sheet material was obtained by the same steps as in Example 1 except that rubbing was not performed in an aqueous sodium hydroxide solution.

The surface of the obtained sheet-like material was covered with a continuous film of polyurethane, and neither a unit film nor a micro joint part was present. The texture of the sheet-like product was harder than that of the sheet-like product of Example 1, and the touch and appearance were plastic-like. Example 2 4.0 of a mixed spun fiber in which a single filament contains a large number of ultrafine fiber components at a ratio of 50 parts polystyrene as a sea component and 50 parts nylon 6 as an ultrafine component.
A denier, 51 mm staple was used to form a web through a card and a cross wrapper, and then needle punching was performed to make a nonwoven fabric. The density of this non-woven fabric was about 450 g / m 2.

This non-woven fabric has 0.4 holes with a diameter of 1.0 mm.
A water stream was sprayed from the nozzles arranged at a pitch of mm at a pressure of 130 kg / square centimeter three times on each side.

Next, the non-woven fabric was pressed to a thickness of 1/3 with a mirror surface roll heated to 130 ° C. Example 1
The polyurethane used in step 2 was diluted with a DMF-toluene mixed solvent to give a 25% solution. A product obtained by adding trifunctional isocyanate and carbon black as a cross-linking agent was applied to the above-mentioned non-woven fabric with a gravure coater so that the applied amount was 100 g / square meter, and dried. Then, the coated surface was preheated with a heating embossing roll at 180 ° C.

Next, dipping in trichloroethylene and repeated squeezing to completely remove the polystyrene were followed by drying. Further, rubbing was performed at 10 ° C. below zero to form fine cracks on the surface. The fibers of the nonwoven fabric were exposed on the surface from the cracks, and the average thickness was about 0.01 denier. Then, it was dyed black with an acid dye at 95 ° C.

On the surface, a unit membrane having an average area of about 0.02 cm 2 formed a micro joint structure. About 19% of the total micro joints
Met. The polyurethane layer of the sheet was removed with a solvent, and the distance between the entanglement points of the fibers was measured.
It was 0 μm.

The obtained leather-like sheet had a natural appearance and flexibility, and the surface was moist and good. Example 3 Instead of the polyurethane used in Example 1, a polycarbonate-based polyurethane and a polyester-based polyurethane were used.
A sheet-like product was obtained through the same steps up to the removal of polystyrene, except that a mixture of 0: 1 was used. The sheet-like material was treated in an aqueous sodium hydroxide solution at 95 ° C. and 50 g / l for 15 minutes to dissolve and remove a part of the polyester-based polyurethane portion to form fine cracks on the surface. After that, acid dye at 95 ℃
It was dyed black with.

On the surface, a unit membrane having an average area of about 0.03 cm 2 formed a micro joint structure. About 11% of the total micro joints
Met.

The leather-like sheet obtained had a natural appearance and flexibility, and the surface was moist and good. Example 4 When needle-punching the web used in Example 2, needle-punching was performed by stacking it on a plain fabric woven with nylon yarns of 75 denier in both length and width. Other than that, a sheet-like material was obtained through the same steps as in Example 2 until dyeing. The sheet-like material was kneaded by a jet dyeing machine in a sodium hydroxide aqueous solution of 95 ° C. at 5 g / l, and further kneaded in warm water of 80 ° C. On the surface, a unit membrane having an average area of about 0.005 cm 2 formed a micro joint structure. The ratio of the micro joint part to the total is about 8
%Met.

The leather-like sheet material obtained had a natural appearance and flexibility, and the surface was moist and good. Further, the dimensional change of the sheet-like material before and after the rubbing process was 3% or less, and the surface quality was not deteriorated. Comparative Example 2 A sheet-like product was obtained by the same treatment as in Example 4, except that the treatment with an aqueous sodium hydroxide solution and the kneading treatment in warm water were not performed.

The coating layer of the obtained sheet-like material was continuous 1.
It was in the shape of a sheet of film, and had a harder texture than the sheet-like material obtained in Example 4, and had an appearance and touch similar to artificial plastic. Comparative Example 3 A sheet-like product was obtained by using the same web and plain woven fabric as in Example 4 except that the treatment with an aqueous sodium hydroxide solution was not performed.

The coating layer of the obtained sheet-like material was continuous 1.
Although it is in the shape of a sheet of film and is more flexible than the sheet-like article obtained in Comparative Example 2, the texture is harder than the sheet-like article obtained in Example 4, and the appearance and touch are It was an artificial plastic-like thing.

[0058]

The effects of the leather-like sheet material of the present invention will be described in detail below. ◎ First, the first effect is that both high scratch resistance and flexibility are achieved. That is, with respect to scratch resistance, the unit film is hardened to improve durability, and at the same time, flexibility can be obtained by bending the micro joint portion with respect to bending of the sheet-like material.

The second effect is a moist touch and a natural appearance. That is, since the unit film and the micro joint portion are mixed, a moist, natural touch and appearance are obtained instead of the conventional uniform and plastic-like one.

The third effect is high air permeability and moisture permeability. That is, since there is a gap between the unit membranes, it is possible to impart a function that allows gases such as air and water vapor to pass through very easily.

[Brief description of the drawings]

FIG. 1 is a schematic view of an example of a micro joint structure of the present invention.

FIG. 2 is a schematic view of another example of the micro joint structure of the present invention.

FIG. 3 is a schematic view of another example of the micro joint structure of the present invention.

FIG. 4 is an enlarged photograph of an example of an embodiment of the micro joint structure of the present invention.

[Explanation of symbols]

 1: Unit membrane 2: Micro joint

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[Procedure amendment]

[Submission date] April 4, 1996

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] Brief description of drawings

[Correction method] Change

[Correction contents]

[Brief description of the drawings]

FIG. 1 is a schematic view of an example of a micro joint structure of the present invention.

FIG. 2 is a schematic view of another example of the micro joint structure of the present invention.

FIG. 3 is a schematic view of an example of a micro joint structure of the present invention.

FIG. 4 is a micro example of a micro joint structure of the present invention.
It is a microscope picture figure which shows the shape of the fiber in a joint part .

Claims (10)

[Claims] 1. A leather-like sheet having a coating layer on at least one side of a substrate, wherein the coating layer has a micro joint structure. 2. The leather-like sheet material according to claim 1, wherein the joint portion of the micro joint structure occupies 1 to 30% of the surface. 3. The leather-like sheet material according to claim 2, wherein fluff or napped fibers are exposed from at least a part of the joint structure. 4. The thickness of fluff or napped fiber is 0.5.
The leather-like sheet material according to claim 3, wherein the thickness is d or less. 5. The leather-like sheet material according to claim 1, wherein the base material is formed by only entanglement of fibers without substantially containing a binder therein. 6. The base material is composed of ultrafine fibers and / or ultrafine fiber bundles having a length of 0.2 d or less, and the distance between entanglement points of the entanglement of the ultrafine fibers is 200 μm or less. The leather-like sheet material according to item 5. 7. The leather-like sheet material according to claim 5, wherein the base material is an ultrafine fiber of 0.2 d or less and / or an ultrafine fiber bundle and a woven or knitted fabric are entangled and integrated with each other. . 8. The leather-like sheet material according to claim 1, wherein the coating layer has a thickness of 10 μm or less. 9. A method for producing a leather-like sheet material having a coating layer on at least one side of a substrate containing fibers, wherein a continuous film is formed on at least one side of the substrate, and then the continuous film is mechanically and / or mechanically Alternatively, a method for producing a leather-like sheet material is characterized in that it is chemically minutely divided. 10. The method for producing a leather-like sheet according to claim 9, wherein the step of dividing the continuous film is a treatment with an alkaline aqueous solution.