CN110629559A - 3D super-hydrophobic microfiber suede leather and manufacturing method thereof - Google Patents
3D super-hydrophobic microfiber suede leather and manufacturing method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- 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
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0004—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using ultra-fine two-component fibres, e.g. island/sea, or ultra-fine one component fibres (< 1 denier)
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- D—TEXTILES; PAPER
- 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
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/004—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using flocked webs or pile fabrics upon which a resin is applied; Teasing, raising web before resin application
-
- D—TEXTILES; PAPER
- 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
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
-
- D—TEXTILES; PAPER
- 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
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
-
- D—TEXTILES; PAPER
- 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention discloses a 3D super-hydrophobic microfiber suede leather and a manufacturing method thereof, and is characterized in that a nano precursor is dispersed into base cloth impregnating waterborne polyurethane to prepare wet impregnation slurry, sea-island type microfiber non-woven fabric impregnated with the slurry is placed into a water solution with the pH value of 2 ~ 3 for solidification, then a sea component is removed through an alkali reduction process, water washing and drying are carried out, and finally a hydrophobic treatment agent is used for treatment to obtain the super-hydrophobic microfiber suede leather.
Description
Technical Field
The invention particularly relates to 3D super-hydrophobic super-fiber suede leather and a manufacturing method thereof, and belongs to the field of synthetic leather manufacturing.
Background
The superfine fiber synthetic leather is a composite material developed based on sea-island superfine fibers and consists of superfine fibers and polyurethane. The superfine fibers have the titer and the structure similar to those of collagen fibers, so that the superfine fibers have similar characteristics in the aspects of surface morphology and mechanical property; the polyurethane is filled between the fiber bundles, and the polyurethane is not simply filled in the leather body, but has a plurality of round and needle-shaped microporous foaming structures which are in a three-dimensional net shape to form a fine transparent structure, so that the leather body has certain air and moisture permeability and compression elasticity. Due to high physical properties, durability and flexibility, the superfine fiber synthetic leather has become a high-simulation substitute of natural leather.
The superfine fiber leather industry in China starts in the 80 th 20 th century, the superfine fiber leather industry develops rapidly in recent years, but a plurality of products with high physical properties and functionality are still in the exploration and development period. At present, the superfine fiber synthetic leather products in China are in the middle and low grade positions of the similar products internationally, and have gaps compared with the products of companies such as Japan Asahi formation and Colorado and the like with technical advantages. Therefore, only by accelerating the technical innovation and the industrial upgrading of the superfine fiber synthetic leather in China, the market competitiveness of the superfine fiber synthetic leather products in China can be improved. The functional superfine fiber synthetic leather is the mainstream trend of high-end products of superfine fiber synthetic leather in the future.
Along with the improvement of the living quality of people and the improvement of the consciousness of environmental protection, people hope that the microfiber leather has excellent hydrophobic performance. Chinese patent publication No. CN 106811984A discloses hydrophobic microfiber suede leather and a preparation method thereof. Immersing the microfiber synthetic leather into a hydrophobic finishing agent and a softening agent for treatment, and constructing a layer of nano structure on the surface of the microfiber suede leather by a sol-gel technology to further improve the waterproof performance of the microfiber suede leather. On one hand, the hydrophobic component is only printed on the surface of the microfiber synthetic leather in a physical mode, and the hydrophobic component is easy to migrate and separate out in the using process, so that the hydrophobic effect is reduced, and the durability is insufficient; on the other hand, the nano particles exist only on the surface layer, so that the nano particles only have a 1D hydrophobic effect, and the leather loses hydrophobicity after the surface layer is damaged. Chinese patent publication No. CN 109763337A discloses a waterproof superfine fiber suede leather and a preparation method thereof, wherein a sea-island type non-woven fabric is immersed in a solvent type polyurethane impregnating solution for waterproof leather, and the waterproof superfine fiber suede leather is obtained through toluene decrement and post-treatment. However, the impregnating resin used by the method is solvent type polyurethane, so that the content of VOCs is high and the environmental pollution is serious.
Disclosure of Invention
Aiming at the defects of the prior art, the 3D super-hydrophobic microfiber suede leather and the manufacturing method thereof provided by the invention are characterized by comprising the following steps:
(1) preparing impregnated polyurethane slurry:
the impregnated polyurethane slurry is prepared according to the following proportion by weight
Aqueous polyurethane resin: 100 portions of
15 portions to 15 ~ 30 portions of nano precursor
1 part of water-based thickener 1 ~ 5
0.5 ~ 3 parts of foam cell regulating auxiliary agent
Color paste 0 ~ 5 parts
The nano precursor is any one or the combination of tetraethoxysilane, tetrabutyl orthosilicate and tetrabutyl titanate;
(2) dipping and solidifying, namely putting the sea-island type superfine fiber non-woven fabric into the dipping polyurethane slurry prepared in the step (1) for dipping, extruding by a roller, scraping the surface dipping solution by a scraper, then putting the dipped non-woven fabric into an aqueous solution with the pH value of 2 ~ 3 for solidifying, hydrolyzing the nano precursor in situ to generate nano particles, and filling fiber gaps after polyurethane is solidified to obtain the porous wet substrate;
(3) reducing and sizing, namely placing the porous wet-process substrate prepared in the step (2) into a sodium hydroxide solution reducing tank with the concentration of 4 ~ 10%, reducing and removing sea components at the temperature of 85 ~ 95 ℃, and then washing, drying and sizing to obtain the microfiber suede leather base cloth;
(4) performing hydrophobic treatment, namely soaking the base cloth prepared in the step (3) in a normal hexane solution of 0.1 ~ 2% of hydrophobic treatment agent in parts by weight after leather grinding treatment for normal temperature treatment for 30 ~ 60 min, recycling the solvent, and washing and sizing the mixture to obtain the 3D super-hydrophobic microfiber suede leather;
the hydrophobic treatment agent is fluorochlorosilane, preferably any one or combination of perfluorododecyl trichlorosilane, 1H,2H, 2H-perfluorooctyl dimethylchlorosilane, 1H,2H, 2H-perfluorooctyl methyldichlorosilane, 1H,2H, 2H-perfluorodecyl dimethylchlorosilane.
The solid content of the waterborne polyurethane resin is 20 ~ 30%, and the waterborne polyurethane resin is any one or the combination of alkaline hydrolysis resistant aliphatic or aromatic waterborne polyurethane.
The sea-island type superfine fiber non-woven fabric is any one of COPET/PA6 type, PET/PA6 type and COPET/PET type.
Compared with the prior art, the invention has the following innovation points:
(1) according to the 3D super-hydrophobic microfiber suede leather prepared by the invention, the nano precursor generates nano particles in situ in the process of coagulating the microfiber non-woven fabric, so that the nano particles are immobilized by the porous polyurethane and are uniformly distributed on the surface of the superfine fiber and the inner and outer surfaces of the porous polyurethane, on one hand, the mechanical property of the super-hydrophobic microfiber suede leather is improved, on the other hand, the multi-level micro-nano rough structure is jointly constructed by the nano particles, the superfine fiber and the porous polyurethane, the surface and the inner part of the leather are kept consistent, and the multi-level micro-nano rough structure constructed by bionics (lotus leaves) endows the microfiber suede leather with special 3D super-hydrophobicity and lasting hydrophobicity. The apparent contact angle of the prepared 3D super-hydrophobic microfiber suede leather is more than 160 degrees, the water contact angle can still be kept more than 150 degrees after the surface layer is ground through a friction test, and the super-hydrophobic microfiber suede leather prepared by the technology has a 3D hydrophobic effect and is durable in hydrophobic effect;
(2) according to the 3D super-hydrophobic microfiber suede leather prepared by the invention, the traditional solvent-based impregnated polyurethane is replaced by the water-based impregnated polyurethane, so that the emission of VOCs in the preparation process of the microfiber suede leather is greatly reduced, and the microfiber suede leather has the outstanding characteristics of environmental friendliness, health, safety and the like.
Detailed Description
The present invention is described in detail below by way of examples, and it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 13D Superhydrophobic microfiber clothing leather
(1) Preparing the aqueous polyurethane slurry for impregnation:
according to weight, the polyurethane impregnating slurry is prepared according to the following proportion
20% of solid aliphatic waterborne polyurethane resin: 100 portions of
Ethyl orthosilicate: 15 portions of
An aqueous thickener: 5 portions of
Cell regulating aid: 0.5 portion
Color paste: 0 portion of
(2) Dipping and solidifying: placing the PET/PA6 sea-island superfine fiber non-woven fabric into the impregnated polyurethane slurry prepared in the step (1) for impregnation, extruding by a roller, scraping off the surface impregnation solution by a scraper, then placing the impregnated non-woven fabric into an aqueous solution with the pH value of 3 for solidification, hydrolyzing the nano precursor in situ to generate nano particles, and filling fiber gaps after polyurethane solidification to obtain a porous wet substrate;
(3) reducing and sizing: placing the porous wet-process substrate prepared in the step (2) in a sodium hydroxide solution decrement tank with the concentration of 8%, reducing and removing sea components at 95 ℃, and then washing, drying and sizing to prepare the porous microfiber suede leather base cloth;
(4) and (3) hydrophobic treatment: and (3) after the base cloth prepared in the step (3) is subjected to leather grinding treatment, soaking the base cloth in a 1H,1H,2H, 2H-perfluorooctyl dimethylchlorosilane normal hexane solution with the mass fraction of 0.1% for 30min, recycling the solvent, and washing and shaping to obtain the 3D super-hydrophobic microfiber suede leather.
The super-hydrophobic superfine fiber suede leather has a water contact angle of 162.5 degrees, has excellent and lasting hydrophobicity, is soft to form leather, and can still keep the super-hydrophobicity after being scratched by a knife.
Example 23D Superhydrophobic microfiber automotive interior leather
(1) Preparing the aqueous polyurethane slurry for impregnation:
according to weight, the polyurethane impregnating slurry is prepared according to the following proportion
30% solid content of aromatic aqueous polyurethane resin: 100 portions of
Butyl titanate: 30 portions of
An aqueous thickener: 1 part of
Cell regulating aid: 1 part of
Color paste: 3 portions of
(2) Dipping and solidifying: placing the COPET/PET sea-island superfine fiber non-woven fabric into the impregnated polyurethane slurry prepared in the step (1) for impregnation, extruding by a roller, scraping off the surface impregnation solution by a scraper, then placing the impregnated non-woven fabric into an aqueous solution with the pH value of 2 for solidification, hydrolyzing butyl titanate in situ to generate nano particles, and filling fiber gaps after polyurethane solidification to obtain a porous wet substrate;
(3) reducing and sizing: placing the porous wet-process substrate prepared in the step (2) in a sodium hydroxide solution decrement tank with the concentration of 4%, reducing and removing sea components at 95 ℃, and then washing, drying and sizing to prepare the porous microfiber suede leather base cloth;
(4) and (3) hydrophobic treatment: and (4) after the base cloth prepared in the step (3) is subjected to leather grinding treatment, soaking the base cloth in a 1% perfluorododecyl trichlorosilane normal hexane solution in parts by weight for 60 min, recycling the solvent, and washing and shaping to obtain the 3D super-hydrophobic microfiber suede leather.
The water contact angles of the surface and the cross section of the 3D super-hydrophobic microfiber suede leather are both larger than 160 degrees, and after 50 times of washing tests, the water contact angles of the surface and the cross section of the 3D super-hydrophobic microfiber suede leather are still larger than 150 degrees.
Example 33D Superhydrophobic microfiber sofa leather
(1) Preparing the aqueous polyurethane slurry for impregnation:
according to weight, the polyurethane impregnating slurry is prepared according to the following proportion
Aliphatic waterborne polyurethane resin with solid content of 25%: 100 portions of
Butyl orthosilicate: 25 portions of
An aqueous thickener: 3 portions of
Cell regulating aid: 3 portions of
Color paste: 5 portions of
(2) Dipping and solidifying: placing COPET/PA6 sea-island superfine fiber non-woven fabric into the impregnated polyurethane slurry prepared in the step (1) for impregnation, extruding by a roller, scraping off the surface impregnation solution by a scraper, then placing the impregnated non-woven fabric into an aqueous solution with the pH value of 2 for solidification, hydrolyzing ethyl orthosilicate in situ to generate nano particles, and filling fiber gaps after polyurethane solidification to obtain a porous wet substrate;
(3) reducing and sizing: placing the porous wet-process substrate prepared in the step (2) in a sodium hydroxide solution decrement tank with the concentration of 10%, reducing and removing sea components at 85 ℃, and then washing, drying and sizing to prepare the porous microfiber suede leather base cloth;
(4) and (3) hydrophobic treatment: and (3) after the base cloth prepared in the step (3) is subjected to leather grinding treatment, soaking the base cloth in 2% of 1H,1H,2H, 2H-perfluorodecyl methyl dichlorosilane normal hexane solution for 30min, recycling the solvent, and washing and shaping to obtain the 3D super-hydrophobic microfiber suede leather.
The 3D super-hydrophobic super-microfiber suede leather has a water contact angle of 165.7 degrees and excellent hydrophobicity. The Martindale wear resistance test shows that the contact angle of the microfiber suede leather prepared by the method is still more than 150 degrees after the abrasive material is rubbed for 400 times, namely the lower layer of the microfiber suede leather still has superhydrophobicity, and the prepared microfiber suede leather has 3D hydrophobic performance.
Claims (3)
1. A3D super-hydrophobic microfiber suede leather and a manufacturing method thereof are characterized by comprising the following steps:
(1) preparing impregnated polyurethane slurry:
the impregnated polyurethane slurry is prepared according to the following proportion by weight
Aqueous polyurethane resin: 100 portions of
15 portions to 15 ~ 30 portions of nano precursor
1 part of water-based thickener 1 ~ 5
0.5 ~ 3 parts of foam cell regulating auxiliary agent
Color paste 0 ~ 5 parts
The nano precursor is any one or the combination of tetraethoxysilane, tetrabutyl orthosilicate and tetrabutyl titanate;
(2) dipping and solidifying, namely putting the sea-island type superfine fiber non-woven fabric into the dipping polyurethane slurry prepared in the step (1) for dipping, extruding by a roller, scraping the surface dipping solution by a scraper, then putting the dipped non-woven fabric into an aqueous solution with the pH value of 2 ~ 3 for solidifying, hydrolyzing the nano precursor in situ to generate nano particles, and filling fiber gaps after polyurethane is solidified to obtain the porous wet substrate;
(3) reducing and sizing, namely placing the porous wet-process substrate prepared in the step (2) into a sodium hydroxide solution reducing tank with the concentration of 4 ~ 10%, reducing and removing sea components at the temperature of 85 ~ 95 ℃, and then washing, drying and sizing to obtain the microfiber suede leather base cloth;
(4) performing hydrophobic treatment, namely soaking the base cloth prepared in the step (3) in a normal hexane solution of 0.1 ~ 2% of hydrophobic treatment agent in parts by weight after leather grinding treatment for normal temperature treatment for 30 ~ 60 min, recycling the solvent, and washing and sizing the mixture to obtain the 3D super-hydrophobic microfiber suede leather;
the hydrophobic treatment agent is fluorochlorosilane, preferably any one or combination of perfluorododecyl trichlorosilane, 1H,2H, 2H-perfluorooctyl dimethylchlorosilane, 1H,2H, 2H-perfluorooctyl methyldichlorosilane, 1H,2H, 2H-perfluorodecyl dimethylchlorosilane.
2. The 3D superhydrophobic microfiber suede leather and the manufacturing method thereof according to claim 1, wherein the aqueous polyurethane resin is any one or combination of aliphatic or aromatic aqueous polyurethane with solid content of 20 ~ 30% and alkali hydrolysis resistance.
3. The 3D superhydrophobic microfiber suede leather and manufacturing method thereof according to claim 1, wherein said sea-island type microfiber non-woven fabric is any one of COPET/PA6 type, PET/PA6 type and COPET/PET type.
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| CN104179031A (en) * | 2014-08-01 | 2014-12-03 | 陕西科技大学 | Successively-impregnating after-finishing method of suede-like superfine fiber synthetic leather |
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