CN107881798B - Waterborne polyurethane synthetic leather and preparation method thereof - Google Patents
Waterborne polyurethane synthetic leather and preparation method thereof Download PDFInfo
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- CN107881798B CN107881798B CN201711215945.5A CN201711215945A CN107881798B CN 107881798 B CN107881798 B CN 107881798B CN 201711215945 A CN201711215945 A CN 201711215945A CN 107881798 B CN107881798 B CN 107881798B
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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
- D06N3/12—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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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/003—Treatment with radio-waves or microwaves
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/59—Polyamides; Polyimides
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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
- 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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- 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
- D06N3/0011—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 non-woven fabrics
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- 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
- D06N3/0045—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 obtained by applying a ready-made foam layer; obtained by compressing, crinkling or crushing a foam layer, e.g. Kaschierverfahren für Schaumschicht
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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
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
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- 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
- D06N3/0095—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 by inversion technique; by transfer processes
- D06N3/0097—Release surface, e.g. separation sheets; Silicone papers
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- D06N2205/00—Condition, form or state of the materials
- D06N2205/02—Dispersion
- D06N2205/023—Emulsion, aqueous dispersion, latex
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- D06N2209/00—Properties of the materials
- D06N2209/10—Properties of the materials having mechanical properties
- D06N2209/103—Resistant to mechanical forces, e.g. shock, impact, puncture, flexion, shear, compression, tear
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- D06N2211/00—Specially adapted uses
- D06N2211/12—Decorative or sun protection articles
- D06N2211/28—Artificial leather
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Abstract
The invention belongs to the technical field of synthetic leather manufacturing, and particularly relates to waterborne polyurethane synthetic leather and a preparation method thereof. The preparation method comprises the following steps: (1) dipping the non-woven fabric into the pre-impregnation solution, and then rolling and drying to obtain a pre-treated non-woven fabric; (2) dipping the pretreated non-woven fabric into the aqueous polyurethane slurry to obtain a dipped non-woven fabric; (3) solidifying the impregnated non-woven fabric under the microwave condition, and then washing and drying to form a non-woven fabric sheet; (4) and (4) veneering the non-woven fabric sheet to obtain the waterborne polyurethane synthetic leather. The solidification is carried out under the microwave, so that local polyurethane is prevented from drying and forming a film on the surface of the fiber, and the adhesion between the polyurethane and the fiber is reduced, thereby preparing the polyurethane synthetic leather with soft hand feel and excellent folding resistance.
Description
Technical Field
The invention belongs to the technical field of synthetic leather manufacturing, and particularly relates to waterborne polyurethane synthetic leather and a preparation method thereof.
Background
Nonwoven fabric, also known as nonwoven fabric, is a fabric formed without the need for woven gauze by orienting or randomly arranging woven staple fibers or filaments to form a web structure, which is then consolidated by mechanical, thermal or chemical means, etc. The non-woven fabric has the characteristics of moisture resistance, air permeability, light weight, rich colors and the like, and is widely applied to the preparation of synthetic leather. The front and back surfaces of the leather are very similar to leather, have certain air permeability and are closer to natural leather than common artificial leather, so that the leather is widely applied to the fields of manufacturing shoes, boots, cases, automobile seats, sofas and the like. The synthetic leather is usually polyurethane synthetic leather, which is generally prepared by impregnating woven cloth and non-woven fabric to simulate a net layer of natural leather, and a polyurethane microporous layer to simulate a grain surface layer of the natural leather.
Chinese patent document CN101725052A discloses a waterborne polyurethane resin superfine fiber leather and a manufacturing method thereof, the process flow comprises the processing of non-woven fabrics, the wet processing and the post-finishing processing, the concrete process flow is that alkali-soluble polyester and polyamide sea-island fibers are carded into a net by a carding machine, then the net is paved by a lapping machine, finally the non-woven fabrics with three-dimensional structure are punctured up and down by a needle machine for many times, the non-woven fabrics are dipped by hot pressing skin or polyvinyl alcohol solution and then dried and shaped, then ground to process into processed original cloth with uniform thickness, stable shape and smooth surface, the processed original cloth is dipped and coated by the wet polyurethane resin, heated and solidified, the sea component of the sea-island fibers is extracted by alkali decrement to form the base cloth of the sea-island fibers, the obtained base cloth is ground, dyed or embossed to obtain the waterborne polyurethane resin superfine fiber synthetic leather, according to the preparation method, an organic solvent is not used, pollution is reduced to the greatest extent, the prepared waterborne polyurethane superfine fiber leather meets the application requirements, but the heating and solidification time is long, the water loss is high, the polyurethane can be dried on the surface of the fiber to form a film, and the polyurethane and the fiber are bonded together, so that the prepared waterborne polyurethane superfine fiber has poor flexibility and folding resistance.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect of poor flexibility and folding endurance of the waterborne polyurethane synthetic leather in the prior art, so that the waterborne polyurethane synthetic leather with excellent flexibility and folding endurance and the preparation method thereof are provided.
The technical scheme of the invention is as follows:
a preparation method of waterborne polyurethane synthetic leather comprises the following steps: (1) dipping the non-woven fabric into the pre-impregnation solution, and then rolling and drying to obtain a pre-treated non-woven fabric; (2) dipping the pretreated non-woven fabric into the aqueous polyurethane slurry to obtain a dipped non-woven fabric; (3) solidifying the impregnated non-woven fabric under microwave, and then washing and drying to form a non-woven fabric sheet; (4) and (3) veneering the non-woven fabric sheet to obtain the waterborne polyurethane synthetic leather.
The microwave frequency for solidification in the step (3) is 500-3000MHz, the temperature is 50-130 ℃, and the time is 1-5 min.
The microwave frequency for solidification in the step (3) is 1000-2500MHz, the temperature is 60-110 ℃, and the time is 1-3 min.
The aqueous polyurethane slurry comprises 10-50% of aqueous polyurethane, 40-90% of thickening agent and 0.15% of wetting agent.
The aqueous polyurethane slurry also comprises 1 percent of sodium chloride aqueous solution with the mass fraction of 30 percent and 0.5 percent of curing agent.
The waterborne polyurethane is nonionic waterborne polyurethane or anionic nonionic mixed waterborne polyurethane.
The pre-impregnation solution is one of polyvinyl alcohol aqueous solution, polyester aqueous solution or modified cellulose water solubility.
The concentration of the pre-impregnation solution is 5-25%, and the viscosity is 100-3000 CPs.
The facing comprises the following steps: (1) coating the surface layer slurry on release paper by a scraping way and drying to obtain a surface layer; (2) coating the foaming slurry on the surface layer by scraping and drying to obtain a composite layer of a foaming layer and the surface layer; (3) and coating the bottom layer slurry on the foaming layer of the composite layer by scraping, and attaching the non-woven fabric sheet on the bottom layer slurry for drying.
The surface layer slurry comprises 96.2% of waterborne polyurethane, 3% of color paste, 0.3% of thickening agent and 0.5% of cross-linking agent.
The foaming slurry comprises 94% of waterborne polyurethane, 3% of a foam stabilizer, 2% of a foaming agent, 0.5% of a cross-linking agent and 0.5% of a thickening agent.
The bottom layer slurry comprises 99% of waterborne polyurethane, 0.5% of cross-linking agent and 0.5% of thickening agent.
The waterborne polyurethane synthetic leather is prepared by the preparation method of the waterborne polyurethane synthetic leather.
The technical scheme of the invention has the following advantages:
1. in the conventional solidification method, local polyurethane is dried on the fiber surface to form a film, so that fibers in the non-woven fabric are adhered together, free movement among the fibers is limited, the non-woven fabric is hardened, the distribution of the waterborne polyurethane is not uniform due to long solidification time, and the non-woven fabric is also hardened; and the polyurethane is solidified under microwave, so that the waterborne polyurethane is uniformly distributed, and the prepared waterborne polyurethane synthetic leather has good hand feeling.
2. According to the preparation method of the waterborne polyurethane synthetic leather provided by the invention, the viscosity of the prepared waterborne polyurethane slurry is in a reasonable range, so that the superfine fiber non-woven fabric can be wetted, and the hand feeling of the product is not hard and solid.
3. According to the preparation method of the waterborne polyurethane synthetic leather provided by the invention, waterborne polyurethane is used as a main body, solvent type polyurethane resin is replaced, the problems of volatilization and residue of an organic solvent are avoided, the whole production process is environment-friendly and pollution-free, and real clean production is realized.
4. The preparation method of the waterborne polyurethane synthetic leather provided by the invention is simple in process, short in solidification time and easier to realize industrial production.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The Impranil DLU in the examples and comparative examples was a Cosmark waterborne polyurethane, Tego 5211 was a Dekker wetting agent, Aquolin161 was a Wanhua curing agent, the black paste was Yongfeng LR-01, the black paste was Yongcheng L75N and the Black paste was a thickener of borchers, Permutex XR-2500 was a crosslinker of Statalr, Netherlands were aqueous polyurethanes of CF106, CF601, CF605 and CF402, respectively, Zhejiang Feng, Sappi Bufalino-107, a polyvinyl alcohol was Fenpu PURE015, and CF053 and CF4 were 05Fencyx foam stabilizer and foaming agent, respectively.
Example 1
Dipping 220 g per square meter of common polyester non-woven fabric with the thickness of 0.9mm in a polyvinyl alcohol aqueous solution with the concentration of 5% and the viscosity of 100CPs, carrying out full pressure through two-dipping and two-rolling rollers, then placing the non-woven fabric into 130 ℃ for baking for 4 minutes to obtain a pre-treated non-woven fabric, dipping the pre-treated non-woven fabric in a slurry of waterborne polyurethane, carrying out full pressure through the rollers, then dipping the pre-treated non-woven fabric in the slurry of waterborne polyurethane again, controlling the gap between the rollers to be 60% for carrying out gap rolling to obtain a dipped non-woven fabric, solidifying the dipped non-woven fabric for 2 minutes under the conditions of the microwave frequency of 500MHz and the temperature of 130 ℃, then washing and baking the dipped non-woven fabric for 3 minutes at 140 ℃ to obtain a non-woven fabric sheet, scraping the surface slurry on release paper to obtain a scraping thickness of 0.12mm, placing the non-woven fabric sheet into an oven to be sequentially baked at 80 ℃, respectively for one minute for the surface layer at 130 ℃, scraping the foamed slurry on the release paper to obtain a surface layer, and (3) sequentially baking for one minute in a baking oven at 70 ℃, 90 ℃, 100 ℃, 120 ℃ and 140 ℃ to obtain a composite layer of a surface layer, scraping and coating a bottom slurry on the surface layer of the composite layer, then laminating a non-woven fabric sheet with the bottom slurry, and baking for one minute at 70 ℃, 90 ℃, 110 ℃ and 140 ℃ to obtain the waterborne polyurethane synthetic leather.
Preparing aqueous polyurethane slurry: uniformly mixing 1% of carboxymethyl cellulose aqueous solution prepared from 10g of Impranil DLU, 0.15g of Tego 5211, 0.5g of Aquolin161 and 90g of carboxymethyl cellulose and 1g of NaCl aqueous solution with the mass fraction of 30% to obtain the waterborne polyurethane slurry with the viscosity of 1500 cps.
Preparing surface layer slurry: 96.2g CF106, 3g LR-01, 0.3g Borchigel L75N and 0.5g Permutex XR-2500 were mixed well to give a topcoat slurry with a viscosity of 3890 cps.
Preparing foaming slurry: 50g CF601, 44g CF605, 3g CF053, 2g CF054, 0.5g BorchigelALA and 0.5g Permutex XR-2500 were mixed well and mechanically foamed to give 500g/L of foamed slurry.
Preparing bottom layer slurry: 99g of CF402, 0.5g of Permutex XR-2500 and 0.5g of Borchigel ALA were mixed well to give a base slurry with a viscosity of 12000 cps.
Example 2
Dipping 220 g per square meter of common polyester non-woven fabric with the thickness of 0.9mm in a polyvinyl alcohol aqueous solution with the concentration of 10% and the viscosity of 670CPs, carrying out full pressure through two-dipping and two-rolling rollers, then placing the non-woven fabric into 130 ℃ for baking for 4 minutes to obtain a pre-treated non-woven fabric, dipping the pre-treated non-woven fabric in a slurry of waterborne polyurethane, carrying out full pressure through the rollers, then dipping the pre-treated non-woven fabric in the slurry of waterborne polyurethane again, controlling the gap between the rollers to be 60% for carrying out gap rolling to obtain a dipped non-woven fabric, solidifying the dipped non-woven fabric for 3 minutes under the conditions that the microwave frequency is 1500MHz and the temperature is 70 ℃, then washing and baking the dipped non-woven fabric for 3 minutes at 140 ℃ to obtain a non-woven fabric sheet, scraping the surface slurry on release paper to obtain a scraping thickness of 0.12mm, placing the non-woven fabric sheet into an oven to be sequentially baked at 80 ℃, surface layers for one minute respectively at 130 ℃, scraping the foaming slurry on the release paper to obtain a surface layer with the, and (3) sequentially baking for one minute in a baking oven at 70 ℃, 90 ℃, 100 ℃, 120 ℃ and 140 ℃ to obtain a composite layer of a surface layer, scraping and coating a bottom slurry on the surface layer of the composite layer, then laminating a non-woven fabric sheet with the bottom slurry, and baking for one minute at 70 ℃, 90 ℃, 110 ℃ and 140 ℃ to obtain the waterborne polyurethane synthetic leather.
Preparing aqueous polyurethane slurry: a1% carboxymethyl cellulose aqueous solution prepared from Impranil DLU 15g, Tego 5211 0.5g, Aquolin161, 83.35g carboxymethyl cellulose and 1g of a 30% NaCl aqueous solution are uniformly mixed to obtain the waterborne polyurethane slurry with the viscosity of 1900 cps.
Preparing surface layer slurry: 96.2g of CF106, 3g of LR01, 0.3g of Borchigel L75N and 0.5g of Permutex XR-2500 were mixed well to give a topcoat slurry with a viscosity of 3890 cps.
Preparing foaming slurry: 50g CF601, 44g CF605, 3g CF053, 2g CF054, 0.5g BorchigelALA and 0.5g Permutex XR-2500 were mixed well and mechanically foamed to give 500g/L of foamed slurry.
Preparing bottom layer slurry: 99g of CF402, 0.5g of Permutex XR-2500 and 0.5g of Borchigel ALA were mixed well to give a base slurry with a viscosity of 12000 cps.
Example 3
Dipping 220 g per square meter of common polyester non-woven fabric with the thickness of 0.9mm in a polyvinyl alcohol aqueous solution with the concentration of 12% and the viscosity of 800CPs, carrying out full pressure through two-dipping and two-rolling rollers, then placing the non-woven fabric into 130 ℃ for baking for 4 minutes to obtain a pre-treated non-woven fabric, dipping the pre-treated non-woven fabric into a slurry of waterborne polyurethane, carrying out full pressure through the rollers, then dipping the pre-treated non-woven fabric into the slurry of waterborne polyurethane again, controlling the gap between the rollers to be 60% for carrying out gap rolling to obtain a dipped non-woven fabric, solidifying the dipped non-woven fabric for 1 minute under the conditions that the microwave frequency is 2500MHz and the temperature is 60 ℃, then washing and baking the dipped non-woven fabric for 3 minutes at 140 ℃ to obtain a non-woven fabric sheet, scraping the surface slurry on release paper to obtain a scraping thickness of 0.12mm, placing the non-woven fabric sheet into an oven to be sequentially baked at 80 ℃, surface layers for one minute respectively at 130 ℃, scraping the foaming slurry to obtain a surface layer with the thickness of 0., and (3) sequentially baking for one minute in a baking oven at 70 ℃, 90 ℃, 100 ℃, 120 ℃ and 140 ℃ to obtain a composite layer of a surface layer, scraping and coating a bottom slurry on the surface layer of the composite layer, then laminating a non-woven fabric sheet with the bottom slurry, and baking for one minute at 70 ℃, 90 ℃, 110 ℃ and 140 ℃ to obtain the waterborne polyurethane synthetic leather.
Preparing aqueous polyurethane slurry: uniformly mixing 1% aqueous solution prepared from 10g of Impranil DLU, 0.15g of Tego 5211, 0.5g of Aquolin161 and 78.35g of sodium carboxymethylcellulose and 1g of NaCl aqueous solution with the mass fraction of 30% to obtain the aqueous polyurethane slurry with the viscosity of 2500 cps
Preparing surface layer slurry: 96.2g CF106, 3g LR01, 0.3g Borchigel L75N and 0.5g Permutex XR-2500 were mixed well to give a topcoat slurry with a viscosity of 3890 cps.
Preparing foaming slurry: 50g CF601, 44g CF605, 3g CF053, 2g CF054, 0.5g BorchigelALA and 0.5g Permutex XR-2500 were mixed well and mechanically foamed to give 500g/L of foamed slurry.
Preparing bottom layer slurry: 99g of CF402, 0.5g of Permutex XR-2500 and 0.5g of Borchigel ALA were mixed well to give a base slurry with a viscosity of 12000 cps.
Example 4
Dipping 220 g per square meter of common polyester non-woven fabric with the thickness of 0.9mm in a polyvinyl alcohol aqueous solution with the concentration of 15% and the viscosity of 1100CPs, carrying out full pressure through two-dipping and two-rolling rollers, then placing the non-woven fabric into 130 ℃ for baking for 4 minutes to obtain a pre-treated non-woven fabric, dipping the pre-treated non-woven fabric into a slurry of waterborne polyurethane, carrying out full pressure through the rollers, then dipping the pre-treated non-woven fabric into the slurry of waterborne polyurethane again, controlling the gap between the rollers to be 60% for carrying out gap rolling to obtain a dipped non-woven fabric, solidifying the dipped non-woven fabric for 3 minutes under the conditions that the microwave frequency is 1500MHz and the temperature is 50 ℃, then washing and baking the dipped non-woven fabric for 3 minutes at 140 ℃ to obtain a non-woven fabric sheet, scraping the surface slurry on release paper to obtain a scraping thickness of 0.12mm, placing the non-woven fabric sheet into an oven to be sequentially baked at 80 ℃, surface layers for one minute respectively at 130 ℃, scraping the foamed slurry to obtain a surface layer with the thickness of 0., and (3) sequentially baking for one minute in a baking oven at 70 ℃, 90 ℃, 100 ℃, 120 ℃ and 140 ℃ to obtain a composite layer of a surface layer, scraping and coating a bottom slurry on the surface layer of the composite layer, then laminating a non-woven fabric sheet with the bottom slurry, and baking for one minute at 70 ℃, 90 ℃, 110 ℃ and 140 ℃ to obtain the waterborne polyurethane synthetic leather.
Preparing aqueous polyurethane slurry: a1% carboxymethyl cellulose aqueous solution prepared from 20g of Impranil DLU, 0.15g of Tego 5211, 0.5g of Aquolin161 and 68.35g of carboxymethyl cellulose and 1g of a 30% NaCl aqueous solution are uniformly mixed to obtain an aqueous polyurethane slurry with the viscosity of 2800 cps.
Preparing surface layer slurry: 96.2g CF106, 3g LR01, 0.3g Borchigel L75N and 0.5g Permutex XR-2500 were mixed well to give a topcoat slurry with a viscosity of 3890 cps.
Preparing foaming slurry: 50g CF601, 44g CF605, 3g CF053, 2g CF054, 0.5g BorchigelALA and 0.5g Permutex XR-2500 were mixed well and mechanically foamed to give 500g/L of foamed slurry.
Preparing bottom layer slurry: 99g of CF402, 0.5g of Permutex XR-2500 and 0.5g of Borchigel ALA were mixed well to give a base slurry with a viscosity of 12000 cps.
Example 5
Dipping 220 g per square meter of common polyester non-woven fabric with the thickness of 0.9mm in a polyvinyl alcohol aqueous solution with the concentration of 18% and the viscosity of 1500CPs, carrying out full pressure through two-dipping and two-rolling rollers, then placing the non-woven fabric into 130 ℃ for baking for 4 minutes to obtain a pre-treated non-woven fabric, dipping the pre-treated non-woven fabric into a slurry of waterborne polyurethane, carrying out full pressure through the rollers, then dipping the pre-treated non-woven fabric into the slurry of waterborne polyurethane again, controlling the gap between the rollers to be 60% for carrying out gap rolling to obtain a dipped non-woven fabric, solidifying the dipped non-woven fabric for 2 minutes under the conditions that the microwave frequency is 2000MHz and the temperature is 90 ℃, then washing and baking the dipped non-woven fabric for 3 minutes at 140 ℃ to obtain a non-woven fabric sheet, scraping the surface slurry on release paper to obtain a scraping thickness of 0.12mm, placing the non-woven fabric sheet into an oven to be sequentially baked at 80 ℃, surface layers for one minute respectively at 130 ℃, scraping the foaming slurry to obtain a surface layer with the thickness of 0., and (3) sequentially baking for one minute in a baking oven at 70 ℃, 90 ℃, 100 ℃, 120 ℃ and 140 ℃ to obtain a composite layer of a surface layer, scraping and coating a bottom slurry on the surface layer of the composite layer, then laminating a non-woven fabric sheet with the bottom slurry, and baking for one minute at 70 ℃, 90 ℃, 110 ℃ and 140 ℃ to obtain the waterborne polyurethane synthetic leather.
Preparing aqueous polyurethane slurry: 40g of Impranil DLU, 0.15g of Tego 5211, 0.5g of Aquolin161, 58.35g of carboxymethyl cellulose prepared into 1 percent of carboxymethyl cellulose aqueous solution and 1g of 30 percent of NaCl aqueous solution are uniformly mixed to obtain the waterborne polyurethane slurry with the viscosity of 3200 cps.
Preparing surface layer slurry: 96.2g CF106, 3g LR01, 0.3g Borchigel L75N and 0.5g Permutex XR-2500 were mixed well to give a topcoat slurry with a viscosity of 3890 cps.
Preparing foaming slurry: 50g CF601, 44g CF605, 3g CF053, 2g CF054, 0.5g BorchigelALA and 0.5g Permutex XR-2500 were mixed well and mechanically foamed to give 500g/L of foamed slurry.
Preparing bottom layer slurry: 99g of CF402, 0.5g of Permutex XR-2500 and 0.5g of Borchigel ALA were mixed well to give a base slurry with a viscosity of 12000 cps.
Example 6
Dipping 220 g per square meter of common polyester non-woven fabric with the thickness of 0.9mm in a polyvinyl alcohol aqueous solution with the concentration of 20% and the viscosity of 2100CPs, carrying out full pressure through two-dipping and two-rolling rollers, then placing the non-woven fabric into 130 ℃ for baking for 4 minutes to obtain a pre-treated non-woven fabric, dipping the pre-treated non-woven fabric in a slurry of waterborne polyurethane, carrying out full pressure through the rollers, then dipping the pre-treated non-woven fabric in the slurry of waterborne polyurethane again, controlling the gap between the rollers to be 60% for carrying out gap rolling to obtain a dipped non-woven fabric, solidifying the dipped non-woven fabric for 2 minutes under the conditions of a microwave frequency of 3000MHz and a temperature of 110 ℃, then washing and baking the dipped non-woven fabric for 3 minutes at 140 ℃ to obtain a non-woven fabric sheet, scraping the surface slurry on release paper to obtain a scraping thickness of 0.12mm, placing the non-woven fabric sheet into an oven to be sequentially baked at 80 ℃, surface layers for one minute respectively at 130 ℃, scraping the foamed slurry on the release paper to obtain a surface layer with the, and (3) sequentially baking for one minute in a baking oven at 70 ℃, 90 ℃, 100 ℃, 120 ℃ and 140 ℃ to obtain a composite layer of a surface layer, scraping and coating a bottom slurry on the surface layer of the composite layer, then laminating a non-woven fabric sheet with the bottom slurry, and baking for one minute at 70 ℃, 90 ℃, 110 ℃ and 140 ℃ to obtain the waterborne polyurethane synthetic leather.
Preparing aqueous polyurethane slurry: 50g of Impranil DLU, 0.15g of Tego 5211, 0.5g of Aquolin161 and 1g of a 1% carboxymethyl cellulose aqueous solution prepared from 48.35g of carboxymethyl cellulose and 1g of a 30% NaCl aqueous solution are mixed uniformly to obtain the waterborne polyurethane slurry with the viscosity of 3500 cps.
Preparing surface layer slurry: 96.2g CF106, 3g LR01, 0.3g Borchigel L75N and 0.5g Permutex XR-2500 were mixed well to give a topcoat slurry with a viscosity of 3890 cps.
Preparing foaming slurry: 50g CF601, 44g CF605, 3g CF053, 2g CF054, 0.5g BorchigelALA and 0.5g Permutex XR-2500 were mixed well and mechanically foamed to give 500g/L of foamed slurry.
Preparing bottom layer slurry: 99g of CF402, 0.5g of Permutex XR-2500 and 0.5g of Borchigel ALA were mixed well to give a base slurry with a viscosity of 12000 cps.
Example 7
Dipping 220 g per square meter of common polyester non-woven fabric with the thickness of 0.9mm in a polyvinyl alcohol aqueous solution with the concentration of 25% and the viscosity of 3000CPs, carrying out full pressure through two-dipping and two-rolling rollers, then placing the non-woven fabric into 130 ℃ for baking for 4 minutes to obtain a pre-treated non-woven fabric, dipping the pre-treated non-woven fabric into a slurry of waterborne polyurethane, carrying out full pressure through the rollers, then dipping the pre-treated non-woven fabric into the slurry of waterborne polyurethane again, controlling the gap between the rollers to be 60% for carrying out gap rolling to obtain a dipped non-woven fabric, solidifying the dipped non-woven fabric under the conditions of the microwave frequency of 1000MHz and the temperature of 80 ℃ for 5 minutes, then washing and baking at 140 ℃ for 3 minutes to obtain a non-woven fabric sheet, scraping the surface slurry onto release paper to obtain a scraping thickness of 0.12mm, placing the non-woven fabric into an oven to bake surface layer at 80 ℃, respectively for one minute at 100 ℃, scraping the foaming slurry onto a release paper to obtain a surface layer with the thickness of 0.35mm, and (3) sequentially baking for one minute in a baking oven at 70 ℃, 90 ℃, 100 ℃, 120 ℃ and 140 ℃ to obtain a composite layer of a surface layer, scraping and coating a bottom slurry on the surface layer of the composite layer, then laminating a non-woven fabric sheet with the bottom slurry, and baking for one minute at 70 ℃, 90 ℃, 110 ℃ and 140 ℃ to obtain the waterborne polyurethane synthetic leather.
Preparing aqueous polyurethane slurry: uniformly mixing a 1% carboxymethyl cellulose aqueous solution prepared from 30g of Impranil DLU, 0.15g of Tego 5211, 0.5g of Aquolin161 and 40g of carboxymethyl cellulose with 1g of a 30% NaCl aqueous solution to obtain the aqueous polyurethane slurry with the viscosity of 3600 cps.
Preparing surface layer slurry: 96.2g CF106, 3g LR01, 0.3g Borchigel L75N and 0.5g Permutex XR-2500 were mixed well to give a topcoat slurry with a viscosity of 3890 cps.
Preparing foaming slurry: 50g CF601, 44g CF605, 3g CF053, 2g CF054, 0.5g BorchigelALA and 0.5g Permutex XR-2500 were mixed well and mechanically foamed to give 500g/L of foamed slurry.
Preparing bottom layer slurry: 99g of CF402, 0.5g of Permutex XR-2500 and 0.5g of Borchigel ALA were mixed well to give a base slurry with a viscosity of 12000 cps.
Comparative example 1
Dipping a common polyester non-woven fabric with the thickness of 0.9mm in a polyvinyl alcohol aqueous solution with the concentration of 18% and the viscosity of 1500CPs, performing full-pressure treatment through two dipping and two rolling rollers, placing the non-woven fabric in a 130 ℃ baking environment for 4 minutes, dipping the non-woven fabric in a slurry of waterborne polyurethane, performing full-pressure treatment through the rollers, then dipping the non-woven fabric in the slurry of waterborne polyurethane again, performing gap rolling by controlling the gap between the rollers to be 60% to obtain a dipped non-woven fabric, sequentially performing coagulation on the dipped non-woven fabric at the temperature of 80 ℃ for 3 minutes, at the temperature of 100 ℃ for 2 minutes, at the temperature of 120 ℃ for 2 minutes and at the temperature of 140 ℃ for 2 minutes, then performing water washing and baking at the temperature of 140 ℃ for 3 minutes to obtain a non-woven fabric sheet, performing scraping coating on release paper by using the surface slurry, wherein the thickness of the scraping is 0.12mm, and sequentially performing one-time baking on the surface layer in an 80 ℃ baking oven, 100 ℃ and 130 ℃ respectively, scraping and coating the foaming slurry on a surface layer, wherein the scraping and coating thickness is 0.35mm, and placing the surface layer into a baking oven to be sequentially baked for one minute at 70 ℃, 90 ℃, 100 ℃, and 140 ℃ to obtain a composite layer of the surface layer, scraping and coating the bottom slurry on the surface layer of the composite layer, then attaching the non-woven fabric sheet to the bottom slurry, and baking the non-woven fabric sheet for one minute at 70 ℃, 90 ℃, 110 ℃ and 140 ℃ to peel off the release paper to obtain the waterborne polyurethane synthetic leather.
Preparing aqueous polyurethane slurry: 40g of Impranil DLU, 0.15g of Tego 5211, 0.5g of Aquolin161, 58.35g of carboxymethyl cellulose prepared into 1 percent of carboxymethyl cellulose aqueous solution and 1g of 30 percent of NaCl aqueous solution are uniformly mixed to obtain the waterborne polyurethane slurry with the viscosity of 3200 cps.
Preparing surface layer slurry: 96.2g CF106, 3g LR01, 0.3g Borchigel L75N and 0.5g Permutex XR-2500 were mixed well to give a topcoat slurry with a viscosity of 3890 cps.
Preparing foaming slurry: 50g CF601, 44g CF605, 3g CF053, 2g CF054, 0.5g BorchigelALA and 0.5g Permutex XR-2500 were mixed well and mechanically foamed to give 500g/L of foamed slurry.
Preparing bottom layer slurry: 99g of CF402, 0.5g of Permutex XR-2500 and 0.5g of Borchigel ALA were mixed well to give a base slurry with a viscosity of 12000 cps.
Experimental example 1
Comparing the nonwoven fabric sheets obtained in example 1 with those obtained in comparative example 1, it was found that the sheet obtained in example 1 had better hand and elasticity.
The aqueous polyurethane synthetic leathers obtained in the examples and comparative examples were subjected to a flexural test in accordance with DIN EN ISO32100, and the results are shown in Table 1:
TABLE 1
| Folding endurance (ten thousands) (25C) | Folding endurance (ten thousands) (-20C) | |
| Example 1 | 5 | 1.8 |
| Example 2 | 25 | 8 |
| Example 3 | 9 | 3 |
| Example 4 | 18 | 6 |
| Example 5 | 30 | 10 |
| Example 6 | 12 | 4 |
| Example 7 | 6 | 2 |
| Comparative example 1 | 3 | 1.5 |
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (8)
1. A preparation method of waterborne polyurethane synthetic leather is characterized by comprising the following steps:
(1) dipping the non-woven fabric into a pre-impregnation solution, and then rolling and drying to obtain a pre-treated non-woven fabric, wherein the pre-impregnation solution is one of a polyvinyl alcohol aqueous solution, a polyester aqueous solution or a modified cellulose aqueous solution, the concentration of the pre-impregnation solution is 5-25%, and the viscosity of the pre-impregnation solution is 100-;
(2) the pre-treated non-woven fabric is soaked in the aqueous polyurethane slurry, is subjected to full pressure through a roller, is then soaked in the aqueous polyurethane slurry again, and is subjected to gap rolling by controlling the gap between the rollers to be 60% to obtain the soaked non-woven fabric, wherein the aqueous polyurethane slurry comprises, by weight percentage of raw materials, 10% -50% of aqueous polyurethane, 40% -83.35% of thickening agent, 0.15% of wetting agent, 1% of sodium chloride aqueous solution with the mass fraction of 30% and 0.5% of curing agent;
(3) solidifying the dipped non-woven fabric under microwave, washing and drying to form a non-woven fabric sheet, wherein the frequency of the solidified microwave is 500-3000MHz, the temperature is 50-130 ℃, and the time is 1-5 min;
(4) and (3) veneering the non-woven fabric sheet to obtain the waterborne polyurethane synthetic leather.
2. The preparation method of the waterborne polyurethane synthetic leather according to claim 1, wherein the microwave frequency for solidification in the step (3) is 1000-2500MHz, the temperature is 60-110 ℃, and the time is 1-3 min.
3. The method for preparing the waterborne polyurethane synthetic leather according to claim 1, wherein the waterborne polyurethane is nonionic waterborne polyurethane or anionic nonionic mixed waterborne polyurethane.
4. A method for preparing an aqueous polyurethane synthetic leather according to any one of claims 1 to 3, wherein the overlay comprises the steps of:
(1) coating the surface layer slurry on release paper by a scraping way and drying to obtain a surface layer;
(2) coating the foaming slurry on the surface layer by scraping and drying to obtain a composite layer of a foaming layer and the surface layer;
(3) and coating the bottom layer slurry on the foaming layer of the composite layer by scraping, and attaching the non-woven fabric sheet on the bottom layer slurry for drying.
5. The preparation method of the waterborne polyurethane synthetic leather according to claim 4, wherein the surface layer slurry comprises 96.2% of waterborne polyurethane, 3% of color paste, 0.3% of thickening agent and 0.5% of cross-linking agent according to the weight percentage of the raw materials.
6. The preparation method of the waterborne polyurethane synthetic leather according to claim 4, wherein the foaming slurry comprises 94 weight percent of waterborne polyurethane, 3 weight percent of foam stabilizer, 2 weight percent of foaming agent, 0.5 weight percent of cross-linking agent and 0.5 weight percent of thickening agent.
7. The preparation method of the waterborne polyurethane synthetic leather according to claim 4, wherein the primer slurry comprises 99% of waterborne polyurethane, 0.5% of cross-linking agent and 0.5% of thickening agent according to the weight percentage of the raw materials.
8. The aqueous polyurethane synthetic leather prepared by the preparation method of the aqueous polyurethane synthetic leather according to any one of claims 1 to 7.
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| CN109056362A (en) * | 2018-09-21 | 2018-12-21 | 兰州科天水性高分子材料有限公司 | A kind of aqueous PU shoe lining leather bass, preprocess method and preparation method thereof |
| CN109652980A (en) * | 2019-01-28 | 2019-04-19 | 陕西科技大学 | A kind of biology base superfine fiber chemical leather and preparation method thereof |
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