CN112195663B - Regenerated silk water-based solvent-free polyurethane synthetic leather for packaging and preparation method thereof - Google Patents
Regenerated silk water-based solvent-free polyurethane synthetic leather for packaging and preparation method thereof Download PDFInfo
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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
- D06N3/0002—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
- D06N3/0015—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 fibres of specified chemical or physical nature, e.g. natural silk
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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
- D06N3/0056—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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- D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
- D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
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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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- 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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- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
- D06N3/146—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes characterised by the macromolecular diols used
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- 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
- D06N3/147—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes characterised by the isocyanates used
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Abstract
The invention provides a regenerated silk water-based solvent-free polyurethane synthetic leather for packaging and a preparation method thereof. The polyurethane synthetic leather sequentially comprises a waterborne surface layer polyurethane layer, a waterborne middle polyurethane layer, a polyester and polycaprolactone blended solvent-free polyurethane layer and a PET regenerated silk fiber layer from top to bottom; the polyester polycaprolactone blended solvent-free polyurethane layer comprises the following raw materials in parts by mass: 100 parts of polyester dihydric alcohol and polycaprolactone dihydric alcohol blend, 9-15 parts of chain extender, 0.05-0.5 part of catalyst and 90-130 parts of isocyanate prepolymer. The invention combines the recycled PET regenerated fiber with the pollution-free advantage of waterborne polyurethane, and develops the high-performance environment-friendly polyurethane synthetic leather for electronic packaging by utilizing the performances of solvent-free chemical resistance, wear resistance and high strength.
Description
Technical Field
The invention belongs to the technical field of synthetic leather, and particularly relates to polyurethane synthetic leather for regenerated silk water-based solvent-free packaging and a preparation method thereof.
Background
The waste PET has no toxic or harmful effect, but has long degradation period in natural environment, and the waste PET causes huge environmental pollution and resource waste due to the large-scale use of the waste PET. And the waste PET is recycled, so that the environmental pollution can be reduced, and the waste can be changed into valuable.
In addition, with the continuous progress of the times, scientific development is changing day by day, and scientific intelligence is integrated into life, electronic products are gradually driven together with living necessities, the life quality of people is improved, the electronic products become necessary tools and partners of people, and the time for more than 80% of testees to use electronic products such as mobile phones and tablet computers is counted to exceed 4 hours every day. Along with the change of living habits and aesthetic tastes of consumers, the polyurethane synthetic leather is gradually applied to digital electronic products and is in close contact with the consumers. The conventional polyurethane synthetic leather adopts a large amount of organic solvents, pollutes the environment, is inflammable and explosive, and has certain potential safety hazards in storage, transportation and operation. Meanwhile, the prepared synthetic leather has residual solvent, and the long-term contact with the human body will influence the health of the human body.
The traditional polyurethane synthetic leather is thick and heavy, has poor touch fineness and poor wear resistance and scratch resistance, is easy to be corroded and dyed by daily living goods, has poor experience feeling after being contacted with consumers for a long time, and can not meet the requirements of the consumers.
Disclosure of Invention
Aiming at the problems, the invention provides a regenerated silk waterborne solvent-free polyurethane synthetic leather for packaging, which sequentially comprises a waterborne surface layer polyurethane layer, a waterborne middle polyurethane layer, a polyester-polycaprolactone blended solvent-free polyurethane layer and a PET regenerated silk fiber layer from top to bottom; the polyester polycaprolactone blended type solvent-free polyurethane layer comprises the following raw materials in parts by mass: 100 parts of polyester dihydric alcohol and polycaprolactone dihydric alcohol blend, 9-15 parts of chain extender, 0.05-0.5 part of catalyst and 90-130 parts of isocyanate prepolymer.
Further, the preparation raw materials of the waterborne surface layer polyurethane layer comprise the following components in parts by mass: 100 parts of water-based polycarbon polyether composite polyurethane resin, 0.2-2 parts of thickening agent, 0.2-2 parts of defoaming agent, 0.5-3 parts of flatting agent, 8-40 parts of pigment and 1-5 parts of water-based curing agent.
Further, the chain extender is one or more of ethylene glycol, propylene glycol and 1, 4-butanediol; the catalyst is one or more of organometallic catalysts BICAT8106, BICAT3228 and BICAT 4232.
Further, the thickening agent is one or more of cellulose, hydrophobic modified acrylate and polyurethane; the leveling agent is an organic silicon surfactant; the defoaming agent is polyether modified silicone; the water-based curing agent is one or more of an open isocyanate curing agent, a closed isocyanate curing agent, a carbodiimide curing agent and an aziridine curing agent.
A preparation method of regenerated silk water-based solvent-free polyurethane synthetic leather for packaging comprises the following steps:
step a, coating a layer of water-based surface layer polyurethane resin on release paper, and drying to form a water-based surface layer polyurethane layer;
step b, coating a layer of waterborne middle layer polyurethane resin on the waterborne surface layer polyurethane layer, and drying to form a waterborne middle polyurethane layer;
c, coating a layer of polyester-polycaprolactone blended solvent-free polyurethane resin on the waterborne intermediate polyurethane layer, and forming a polyester-polycaprolactone blended solvent-free polyurethane layer after pre-reaction;
d, laminating the PET regenerated silk fiber layer and the polyester polycaprolactone blended solvent-free polyurethane layer by using a compression roller, and curing in an oven;
e, coiling the PET regenerated silk fiber layer cured by the oven and the polyester polycaprolactone blended solvent-free polyurethane layer laminate together, and curing for 24-48h by a curing chamber; and (4) peeling off the release paper after the secondary curing is finished to obtain the regenerated silk water-based solvent-free packaging polyurethane synthetic leather.
Further, the viscosity of the waterborne surface layer polyurethane resin in the step a is 4000-8000 cps at 25 ℃, the coating thickness is 0.12-0.18mm, and the drying temperature is 70-130 ℃.
Further, in the step b, the viscosity of the waterborne middle layer polyurethane resin at 25 ℃ is 4000 to 8000cps, the coating thickness is 0.12 to 0.2mm, and the drying temperature is 70 to 130 ℃.
Further, the thickness of the polyester and polycaprolactone blended solvent-free polyurethane resin in the step c is 0.18-0.3mm, and the pre-reaction condition is pre-reaction for 2-3min at 100-130 ℃.
Further, in the step d, the oven curing condition is that the oven curing is carried out for 10-15min at the temperature of 130-150 ℃; the thickness of the PET regenerated silk fiber layer is 0.2-0.4 mm.
Compared with the prior art, the invention has the following advantages:
1. the prepared regenerated silk aqueous solvent-free packaging polyurethane synthetic leather adopts 100% recycled PET regenerated silk fiber as a base material, so that the environmental pollution can be reduced, the regenerated silk aqueous solvent-free packaging polyurethane synthetic leather can be used as a treasure by waste, the resource is saved, and the sustainable development of the industry is improved;
2. the polyurethane synthetic leather prepared by the invention has a four-layer structure, the thickness of the product is only 0.35-0.5mm, and the gram weight is 160-300g/m 2 The packaging structure is assembled on an electronic product, has strong coating property, is light, thin and fashionable;
3. the invention adopts the polyurethane resin of the surface layer and the middle layer compounded by the water-based polycarbon polyether, takes water as a solvent, does not contain toxic organic chemical solvent, and has no harm to human bodies and environment because the main body volatilized in the production process is water vapor, thereby greatly reducing the environmental pollution; in physical properties, the paint has the properties of water resistance, solvent resistance, wear resistance, scratch resistance and the like;
4. the polyester polycaprolactone blended solvent-free polyurethane resin adopted by the invention endows the product with excellent hydrolysis resistance, high wear resistance and excellent chemical resistance, and can meet the requirements of high-grade electronic packaging materials;
5. the invention adopts the water-based and solvent-free combined process for preparation, and the preparation method and equipment are advanced, so that the production process can be simplified, the advantages of high efficiency and low energy consumption are achieved, the volatilization and residue problems of the organic solvent (DMF is less than or equal to 5ppm) are reduced, and the green and environment-friendly development trend of the synthetic leather industry is met.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 shows a schematic structural diagram of a polyurethane synthetic leather for a regenerated silk aqueous solvent-free package in an embodiment of the invention.
In the figure: 1-waterborne surface layer polyurethane layer, 2-waterborne intermediate polyurethane layer, 3-polyester polycaprolactone blending type solvent-free polyurethane layer and 4-PET regenerated silk fiber layer.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious 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 invention combines the advantages of recycled PET regenerated fiber and waterborne polyurethane in no pollution, and develops the high-performance environment-friendly polyurethane synthetic leather for electronic packaging by utilizing the performances of solvent-free chemical resistance, wear resistance and high strength.
The invention discloses a regenerated silk waterborne solvent-free packaging polyurethane synthetic leather, which sequentially comprises a waterborne surface layer polyurethane layer 1, a waterborne middle polyurethane layer 2, a polyester and polycaprolactone blended solvent-free polyurethane layer 3 and a PET regenerated silk fiber layer 4 from top to bottom.
Illustratively, the PET recycled filament fiber layer 4 is a thin 100% recycled PET recycled filament fiber, which is qualified as GRS recycled material.
Illustratively, the layer of PET regenerated filament fibers 4 is 0.30mm thick gauge regenerated filament.
The polyester polycaprolactone blended solvent-free polyurethane layer 3 comprises the following raw materials in parts by weight: 100 parts of polyester dihydric alcohol and polycaprolactone dihydric alcohol blend, 9-15 parts of chain extender, 0.05-0.3 part of catalyst and 90-130 parts of isocyanate prepolymer.
Illustratively, the chain extender is used for increasing the hard segment content in the polyurethane resin and improving the strength of the polyurethane resin; the catalyst is used for improving the reaction speed and the curing effect of the solvent-free AB material; the isocyanate prepolymer is solvent-free material B, and reacts with the dimethyl polycarbonate diol to generate polyurethane.
Illustratively, the blending average molecular weight of the polyester diol and the polycaprolactone diol is 1000-4000 g/mol; the chain extender is one or more of ethylene glycol, propylene glycol and 1, 4-butanediol; the catalyst is one or more of organometallic catalysts BICAT8106, BICAT3228 and BICAT 4232; the isocyanate prepolymer is isocyanate-terminated polyurethane resin prepolymer, and the viscosity of the isocyanate prepolymer is 3000-6000cps at 25 ℃.
The preparation raw materials of the waterborne surface layer polyurethane layer 1 comprise the following components in parts by mass: 100 parts of water-based polycarbon polyether composite polyurethane resin, 0.2-2 parts of thickening agent, 0.2-2 parts of defoaming agent, 0.5-3 parts of flatting agent, 8-40 parts of pigment and 1-5 parts of water-based curing agent.
Illustratively, thickeners are used to adjust the viscosity of the aqueous formulation; the defoaming agent is used for eliminating bubbles generated in the stirring process of the aqueous formula and reducing the generation of air holes; the leveling agent is used for reducing the surface tension of the water-based material, improving the coating leveling of the water-based material on release paper and avoiding the problem of fisheye diffusion; the aqueous curing agent is used for improving intermolecular force after drying the aqueous resin and improving film-forming strength.
The preparation raw materials of the waterborne intermediate polyurethane layer 2 comprise the following components in parts by mass: 100 parts of water-based polycarbon polyether composite polyurethane resin, 0.2-2 parts of thickening agent, 0.2-2 parts of defoaming agent, 0.6-3 parts of flatting agent, 8-40 parts of pigment and 1-5 parts of water-based curing agent.
Exemplary waterborne polycarbonate polyether composite polyurethane resins have a 100% modulus of 30 to 90kg/cm 2 The solid content of the waterborne polycarbon polyether composite polyurethane resin is 30-50%; the thickening agent is one or more of cellulose, hydrophobic modified acrylate and polyurethane; the flatting agent is organic silicon surfactant; the defoaming agent is polyether modified silicone; the water-based curing agent is one or more of an open isocyanate curing agent, a closed isocyanate curing agent, a carbodiimide curing agent and an aziridine curing agent; the pigment is water-based color paste.
Exemplary, the aqueous polycarbonate polyether composite polyurethane resin model is polyferyl polyurethane new materials ltd (WT-13); the thickener is U-605 produced by Tantaowawa; the model of the defoaming agent is Pico chemical BYK-141; the model of the flatting agent is BYK-300 in Pico chemical industry; the type of the water-based curing agent is Dismann CX-100; the model of the isocyanate prepolymer is Hefei Anli polyurethane new material Co., Ltd (AL-5050B).
A preparation method of regenerated silk water-based solvent-free polyurethane synthetic leather for packaging comprises the following steps:
step a, coating a layer of water-based surface layer polyurethane resin on release paper, and drying to form a water-based surface layer polyurethane layer 1;
wherein: the preparation raw materials of the waterborne surface layer polyurethane layer 1 comprise the following components in parts by mass: 100 parts of water-based polycarbopolyether composite polyurethane resin, 0.2-2 parts of thickening agent, 0.2-2 parts of defoaming agent, 0.5-3 parts of flatting agent, 8-40 parts of pigment and 1-5 parts of water-based curing agent;
the viscosity of the waterborne surface layer polyurethane resin at 25 ℃ is 4000-8000 cps, and the coating thickness is 0.12-0.18 mm; the drying temperature is 70-130 ℃;
b, coating a layer of waterborne intermediate layer polyurethane resin on the waterborne surface layer polyurethane layer 1, and drying to form a waterborne intermediate polyurethane layer 2;
wherein: the preparation raw materials of the waterborne intermediate polyurethane layer comprise the following components in parts by mass: 100 parts of water-based polycarbon polyether composite polyurethane resin, 0.2-2 parts of thickening agent, 0.2-2 parts of defoaming agent, 0.5-3 parts of flatting agent, 8-40 parts of pigment and 1-5 parts of water-based curing agent;
the viscosity of the waterborne middle layer polyurethane resin at 25 ℃ is 4000-8000 cps, the coating thickness is 0.12-0.2mm, and the drying temperature is 70-130 ℃;
c, coating a layer of polyester-polycaprolactone blended solvent-free polyurethane resin on the waterborne intermediate polyurethane layer 2, and forming a polyester-polycaprolactone blended solvent-free polyurethane layer 3 after pre-reaction;
wherein: the polyester polycaprolactone blended type solvent-free polyurethane layer 3 comprises the following raw materials in parts by weight: 100 parts of polyester dihydric alcohol and polycaprolactone dihydric alcohol blend, 9-15 parts of chain extender, 0.05-0.3 part of catalyst and 90-130 parts of isocyanate prepolymer;
the thickness of the polyester-polycaprolactone blended solvent-free polyurethane resin is 0.18-0.3mm, and the pre-reaction condition is pre-reaction for 2-3min at 100-130 ℃;
d, laminating the PET regenerated silk fiber layer 4 and the polyester polycaprolactone blended solvent-free polyurethane layer 3 by using a compression roller, and curing in an oven; the oven curing condition is that the oven curing is carried out for 10-15min at the temperature of 130-150 ℃; the thickness of the PET regenerated silk fiber layer 4 is 0.2-0.4 mm;
e, coiling the PET regenerated silk fiber layer cured by the oven and the polyester polycaprolactone blended solvent-free polyurethane layer laminate together, and curing for 24-48h by a curing chamber, wherein the curing temperature is 70 ℃; and (4) peeling off the release paper after the secondary curing is finished to obtain the regenerated silk water-based solvent-free packaging polyurethane synthetic leather.
The present invention is further illustrated by the following three specific examples, but it should be noted that the specific material ratios, process conditions, results, etc. described in the examples of the present invention are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Example one
A preparation method of regenerated silk water-based solvent-free polyurethane synthetic leather for packaging comprises the following steps:
step a, coating a layer of water-based surface layer polyurethane resin on release paper, and drying to form a water-based surface layer polyurethane layer 1;
wherein: the preparation raw materials of the waterborne surface layer polyurethane layer 1 comprise the following components in parts by mass: 100 parts of water-based polycarbon polyether composite polyurethane resin, 0.5 part of thickening agent, 0.5 part of defoaming agent, 0.7 part of flatting agent, 10 parts of pigment and 2 parts of water-based curing agent;
the viscosity of the waterborne surface layer polyurethane resin at 25 ℃ is 5000cps, and the coating thickness is 0.13 mm; the drying temperature is 120 ℃;
b, coating a layer of waterborne intermediate layer polyurethane resin on the waterborne surface layer polyurethane layer 1, and drying to form a waterborne intermediate polyurethane layer 2;
wherein: the preparation raw materials of the waterborne intermediate polyurethane layer comprise the following components in parts by mass: 100 parts of water-based polycarbon polyether composite polyurethane resin, 0.5 part of thickening agent, 0.5 part of defoaming agent, 0.7 part of flatting agent, 10 parts of pigment and 2 parts of water-based curing agent;
the viscosity of the waterborne middle layer polyurethane resin at 25 ℃ is 5000cps, the coating thickness is 0.15mm, and the drying temperature is 130 ℃;
c, coating a layer of polyester-polycaprolactone blended solvent-free polyurethane resin on the waterborne intermediate polyurethane layer 2, and forming a polyester-polycaprolactone blended solvent-free polyurethane layer 3 after pre-reaction;
wherein: the polyester polycaprolactone blended solvent-free polyurethane layer 3 comprises the following raw materials in parts by weight: 100 parts of polyester dihydric alcohol and polycaprolactone dihydric alcohol blend, 9 parts of ethylene glycol, 0.1 part of catalyst (BICAT8106) and 90 parts of isocyanate prepolymer;
the thickness of the polyester-polycaprolactone blended solvent-free polyurethane resin is 0.2mm, and the pre-reaction condition is pre-reaction for 3min at 110 ℃;
d, laminating the PET regenerated silk fiber layer 4 and the polyester polycaprolactone blended solvent-free polyurethane layer 3 by using a compression roller, and curing in an oven; the curing condition of the oven is oven curing 10 at 140 ℃; the thickness specification of the PET regenerated silk fiber layer 4 is 0.3 mm;
e, coiling the PET regenerated silk fiber layer cured by the oven and the polyester polycaprolactone blended solvent-free polyurethane layer laminate together, and curing the PET regenerated silk fiber layer and the polyester polycaprolactone blended solvent-free polyurethane layer laminate in a curing chamber at the temperature of 70 ℃; and (4) peeling off the release paper after the secondary curing is finished to obtain the regenerated silk water-based solvent-free packaging polyurethane synthetic leather.
Example two
A preparation method of regenerated silk water-based solvent-free polyurethane synthetic leather for packaging comprises the following steps:
step a, coating a layer of water-based surface layer polyurethane resin on release paper, and drying to form a water-based surface layer polyurethane layer 1;
wherein: the preparation raw materials of the waterborne surface layer polyurethane layer 1 comprise the following components in parts by mass: 100 parts of water-based polycarbopolyether composite polyurethane resin, 0.4 part of thickening agent, 0.3 part of defoaming agent, 0.8 part of flatting agent, 15 parts of pigment and 4 parts of water-based curing agent;
the viscosity of the waterborne surface layer polyurethane resin at 25 ℃ is 4500cps, and the coating thickness is 0.15 mm; the drying temperature is 110 ℃;
b, coating a layer of waterborne intermediate layer polyurethane resin on the waterborne surface layer polyurethane layer 1, and drying to form a waterborne intermediate polyurethane layer 2;
wherein: the preparation raw materials of the waterborne intermediate polyurethane layer comprise the following components in parts by mass: 100 parts of water-based polycarbon polyether composite polyurethane resin, 0.4 part of thickening agent, 0.3 part of defoaming agent, 0.8 part of flatting agent, 15 parts of pigment and 4 parts of water-based curing agent;
the viscosity of the waterborne middle layer polyurethane resin at 25 ℃ is 4500cps, the coating thickness is 0.18mm, and the drying temperature is 130 ℃;
c, coating a layer of polyester-polycaprolactone blended solvent-free polyurethane resin on the waterborne intermediate polyurethane layer 2, and forming a polyester-polycaprolactone blended solvent-free polyurethane layer 3 after pre-reaction;
wherein: the polyester polycaprolactone blended solvent-free polyurethane layer 3 comprises the following raw materials in parts by weight: 100 parts of polyester dihydric alcohol and polycaprolactone dihydric alcohol, 12 parts of ethylene glycol, 0.1 part of catalyst (BICAT3228) and 110 parts of isocyanate prepolymer;
the thickness of the polyester polycaprolactone blended solvent-free polyurethane resin is 0.18mm, and the pre-reaction condition is pre-reaction for 3min at 100 ℃;
d, laminating the PET regenerated silk fiber layer 4 and the polyester polycaprolactone blended solvent-free polyurethane layer 3 by using a compression roller, and curing in an oven; the oven curing condition is 130 oven curing for 10 min; the thickness of the PET regenerated silk fiber layer 4 is 0.35 mm;
e, coiling the PET regenerated silk fiber layer cured by the oven and the polyester polycaprolactone blended solvent-free polyurethane layer laminate together, and curing for 24 hours in a curing chamber, wherein the curing temperature is 70 ℃; and (4) peeling off the release paper after the secondary curing is finished to obtain the regenerated silk water-based solvent-free packaging polyurethane synthetic leather.
EXAMPLE III
A preparation method of regenerated silk water-based solvent-free polyurethane synthetic leather for packaging comprises the following steps:
step a, coating a layer of waterborne surface layer polyurethane resin on release paper, and drying to form a waterborne surface layer polyurethane layer 1;
wherein: the preparation raw materials of the waterborne surface layer polyurethane layer 1 comprise the following components in parts by mass: 100 parts of water-based polycarbopolyether composite polyurethane resin, 0.8 part of thickening agent, 0.4 part of defoaming agent, 0.8 part of flatting agent, 20 parts of pigment and 5 parts of water-based curing agent;
the viscosity of the aqueous surface layer polyurethane resin at 25 ℃ is 7000cps, and the coating thickness is 0.16 mm; the drying temperature is 130 ℃;
b, coating a layer of waterborne intermediate layer polyurethane resin on the waterborne surface layer polyurethane layer 1, and drying to form a waterborne intermediate polyurethane layer 2;
wherein: the preparation raw materials of the waterborne intermediate polyurethane layer comprise the following components in parts by mass: 100 parts of water-based polycarbon polyether composite polyurethane resin, 0.8 part of thickening agent, 0.4 part of defoaming agent, 0.8 part of flatting agent, 20 parts of pigment and 5 parts of water-based curing agent;
the viscosity of the waterborne middle layer polyurethane resin at 25 ℃ is 7000cps, the coating thickness is 0.2mm, and the drying temperature is 130 ℃;
c, coating a layer of polyester-polycaprolactone blended solvent-free polyurethane resin on the waterborne intermediate polyurethane layer 2, and forming a polyester-polycaprolactone blended solvent-free polyurethane layer 3 after pre-reaction;
wherein: the polyester polycaprolactone blended solvent-free polyurethane layer 3 comprises the following raw materials in parts by weight: 100 parts of polyester dihydric alcohol and polycaprolactone dihydric alcohol, 12 parts of ethylene glycol, 0.1 part of catalyst (BICAT3228) and 110 parts of isocyanate prepolymer;
the thickness of the polyester-polycaprolactone blended solvent-free polyurethane resin is 0.25mm, and the pre-reaction condition is pre-reaction for 2min at 110 ℃;
d, laminating the PET regenerated silk fiber layer 4 and the polyester polycaprolactone blended solvent-free polyurethane layer 3 by using a compression roller, and curing in an oven; the curing condition of the oven is that the oven is cured for 10min at 150 ℃; the thickness of the PET regenerated silk fiber layer 4 is 0.25 mm;
e, coiling the PET regenerated silk fiber layer cured by the oven and the polyester polycaprolactone blended solvent-free polyurethane layer laminate together, and curing the PET regenerated silk fiber layer and the polyester polycaprolactone blended solvent-free polyurethane layer laminate in a curing chamber at the temperature of 70 ℃; and (4) peeling off the release paper after the secondary curing is finished to obtain the regenerated silk water-based solvent-free packaging polyurethane synthetic leather.
To verify the effect of the present invention, the samples prepared in examples 1 to 3 above were subjected to a detection test: no cracking after being bent for 10 ten thousand times at 25 ℃; the CS-10 of the Taber test is carried out, the load is 1Kg, and 200 turns are carried out; the leather surface is not pulverized and cracked when placed for 7 weeks in a constant temperature and humidity box at 70 ℃ and the humidity is 95%; and (3) detecting chemicals: sweat, perfume, alcohol and the like are coated on the leather surface, and the leather surface does not obviously change under the conditions of 70 ℃ 95% RH 72 h; the DMF content of the samples 1 to 3 is detected, the content of the sample 1 is 3ppm, the content of the sample 2 is 2ppm, and the content of the sample 3 is 4ppm, which all meet the industrial requirements.
According to the regenerated silk waterborne solvent-free polyurethane synthetic leather material for electronic packaging, no organic solvent is added and used in the processing process, and meanwhile, the regenerated silk waterborne solvent-free polyurethane synthetic leather material is high in wear resistance, scratch resistance and chemical resistance; the invention is mainly used in high-end electronic protective sleeve products, and can meet the requirements of forming processes of die cutting, molding and the like of electronic packaging products.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. The regenerated silk waterborne solvent-free packaging polyurethane synthetic leather is characterized by sequentially comprising a waterborne surface layer polyurethane layer, a waterborne middle polyurethane layer, a polyester and polycaprolactone blended solvent-free polyurethane layer and a PET regenerated silk fiber layer from top to bottom;
the polyester polycaprolactone blended solvent-free polyurethane layer comprises the following raw materials in parts by mass: 100 parts of polyester diol and polycaprolactone diol blend, 9-15 parts of chain extender, 0.05-0.5 part of catalyst and 90-130 parts of isocyanate prepolymer;
the preparation raw materials of the waterborne surface layer polyurethane layer comprise the following components in parts by mass: 100 parts of water-based polycarbopolyether composite polyurethane resin, 0.2-2 parts of thickening agent, 0.2-2 parts of defoaming agent, 0.5-3 parts of flatting agent, 8-40 parts of pigment and 1-5 parts of water-based curing agent;
the preparation raw materials of the waterborne intermediate polyurethane layer comprise the following components in parts by mass: 100 parts of water-based polycarbon polyether composite polyurethane resin, 0.2-2 parts of thickening agent, 0.2-2 parts of defoaming agent, 0.5-3 parts of flatting agent, 8-40 parts of pigment and 1-5 parts of water-based curing agent;
the thickness of the polyurethane synthetic leather is 0.35-0.5mm, and the gram weight is 160-300g/m 2 。
2. The regenerated silk aqueous solvent-free polyurethane synthetic leather for packaging as claimed in claim 1, wherein the chain extender is one or more of ethylene glycol, propylene glycol and 1, 4-butanediol; the catalyst is one or more of organometallic catalysts BICAT8106, BICAT3228 and BICAT 4232.
3. The regenerated silk aqueous solvent-free packaging polyurethane synthetic leather according to claim 1, wherein the thickener is one or more of celluloses, hydrophobically modified acrylates and polyurethanes; the leveling agent is an organic silicon surfactant; the defoaming agent is polyether modified silicone; the water-based curing agent is one or more of an open isocyanate curing agent, a closed isocyanate curing agent, a carbodiimide curing agent and an aziridine curing agent.
4. A method for preparing the regenerated silk aqueous solvent-free polyurethane synthetic leather for packaging according to any one of claims 1 to 3, which comprises the following steps:
step a, coating a layer of waterborne surface layer polyurethane resin on release paper, and drying to form a waterborne surface layer polyurethane layer;
b, coating a layer of waterborne intermediate layer polyurethane resin on the waterborne surface layer polyurethane layer, and drying to form a waterborne intermediate polyurethane layer;
c, coating a layer of polyester-polycaprolactone blended solvent-free polyurethane resin on the waterborne intermediate polyurethane layer, and forming a polyester-polycaprolactone blended solvent-free polyurethane layer after pre-reaction;
d, laminating the PET regenerated silk fiber layer and the polyester polycaprolactone blended solvent-free polyurethane layer by using a compression roller, and curing in an oven;
e, coiling the PET regenerated silk fiber layer cured by the oven and the polyester polycaprolactone blended solvent-free polyurethane layer laminate together, and curing for 24-48h by a curing chamber; and (4) peeling off the release paper after the secondary curing is finished to obtain the regenerated silk water-based solvent-free packaging polyurethane synthetic leather.
5. The preparation method of the regenerated silk waterborne solvent-free packaging polyurethane synthetic leather as claimed in claim 4, wherein the viscosity of the waterborne surface layer polyurethane resin at 25 ℃ in the step a is 4000 to 8000cps, the coating thickness is 0.12 to 0.18mm, and the drying temperature is 70 to 130 ℃.
6. The method for preparing the regenerated silk aqueous solvent-free packaging polyurethane synthetic leather as claimed in claim 4, wherein in the step b, the viscosity of the aqueous middle layer polyurethane resin at 25 ℃ is 4000 to 8000cps, the coating thickness is 0.12 to 0.2mm, and the drying temperature is 70 to 130 ℃.
7. The preparation method of the regenerated silk water-based solvent-free polyurethane synthetic leather for packaging, according to claim 4, characterized in that in the step c, the thickness of the polyester and polycaprolactone blended solvent-free polyurethane resin is 0.18-0.3mm, and the pre-reaction condition is pre-reaction at 100-130 ℃ for 2-3 min.
8. The preparation method of the regenerated silk aqueous solvent-free polyurethane synthetic leather for packaging according to claim 4, characterized in that the oven curing condition in the step d is oven curing at 130-150 ℃ for 10-15 min; the thickness of the PET regenerated silk fiber layer is 0.2-0.4 mm.
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