CN108219656B - Aqueous suede leather slurry, method for processing suede leather by wet process and application - Google Patents
Aqueous suede leather slurry, method for processing suede leather by wet process and application Download PDFInfo
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- CN108219656B CN108219656B CN201711397671.6A CN201711397671A CN108219656B CN 108219656 B CN108219656 B CN 108219656B CN 201711397671 A CN201711397671 A CN 201711397671A CN 108219656 B CN108219656 B CN 108219656B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
-
- 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
-
- 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
- D06N3/146—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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention provides a water-based suede leather slurry, a method for processing suede leather by a wet process and application thereof, wherein the water-based suede leather slurry comprises the following components in parts by mass: 70-95 parts by mass of an aqueous polyurethane dispersion, preferably 80-90 parts by mass; 5-30 parts by mass of water-based acrylic emulsion, preferably 10-25 parts by mass; 1-5 parts by mass of a foam stabilizer, preferably 2-3 parts by mass; 1 to 5 parts by mass of a foaming agent, preferably 2 to 3 parts by mass. The processing slurry prepared by foaming the aqueous suede leather slurry is particularly suitable for processing suede leather by a wet process, the obtained suede leather is particularly suitable for the field of electronic packaging, the aqueous suede leather slurry is environment-friendly and pollution-free, and the suede leather prepared by the wet process has better hand feeling.
Description
Technical Field
The invention relates to the field of aqueous suede leather slurry, further relates to slurry applicable to electronic packaging suede leather processing, and particularly relates to aqueous suede leather slurry applicable to suede leather processing by a wet process, and a preparation method and application thereof.
Background
With the rapid development of electronic industry in China, the demand of electronic products such as mobile phone covers, tablet personal computer protective covers and the like for electronic packages is increasingly vigorous. Most of the traditional electronic packaging leather is made of PVC material or oily PU material, and the traditional process is a method for replacing DMF by oily PU to prepare the electronic packaging leather. The traditional process has the defects that DMF (dimethyl formamide) is a substance harmful to human bodies and the environment in the production process of the oily PU material, and the prepared product has residual solvent, is not environment-friendly and also brings threat to the health of production workers and consumers. The preparation method for developing the water-based electronic packaging innovation can replace an oil-based PU material, and has great potential commercial value.
The published patent application 201320013758.X describes an aqueous polyurethane electronic packaging leather, wherein a traditional packaging leather prepared by a release paper method is only compounded with knitted cloth and aqueous polyurethane, and belongs to a lower-end leather in the field of packaging leather. Published patent application 201410523751.1 describes a polyurethane synthetic leather for high-grade electronic packaging and certificates, which is prepared by coating a layer of colorless transparent sizing material on the outer surface of a polyurethane synthetic leather base layer, drying and curing to obtain the polyurethane synthetic leather, and preparing the electronic packaging leather by adopting a traditional solvent wet curing method instead of the prior method, mainly playing a certain antifouling role and still being a traditional and environmentally-friendly preparation method. Published patent application 201310008066.0 describes a method for making aqueous electronic packaging microfiber, wherein microfiber cloth is immersed in aqueous polyurethane slurry, and directly dried and formed; the preparation method has no solvent, and the whole process is a non-solvent aqueous environment; but the prepared electronic microfiber leather has poor hand feeling and low softness. Published patent application 201210164124.4 describes a high-permeability environment-friendly waterborne polyurethane suede synthetic leather and a preparation method thereof, wherein waterborne polyurethane glue is coated on napping knitted fabrics, and the leather is directly dried and shaped, so that the leather has excellent permeability, but the cost is high, and the leather is mostly suitable for shoe leather and is not suitable for the field of electronic packaging. Published patent application 201110302564.7 describes a method for producing synthetic leather for electronic products, which produces a large amount of solvents such as dimethylformamide which pollute the environment and is not environment-friendly.
Therefore, the development of the slurry for the electronic packaging suede leather which can meet the requirements that the slurry does not contain an organic solvent, a finished product is soft in hand feeling and strong in suede feeling, and can be processed by a wet process is needed, and the suede leather obtained by processing the slurry can meet the requirements of the electronic packaging suede leather in mobile phone covers, tablet computer protective covers and the like.
Disclosure of Invention
The processing slurry prepared by foaming the aqueous suede leather slurry is particularly suitable for processing suede leather by a wet process, the obtained suede leather is particularly suitable for the field of electronic packaging, the aqueous suede leather slurry is environment-friendly and pollution-free, and the suede leather prepared by the wet process has better hand feeling.
The invention provides a water-based suede leather slurry which comprises the following components in parts by mass:
70-95 parts by mass of an aqueous polyurethane dispersion, preferably 80-90 parts by mass;
5-30 parts by mass of water-based acrylic emulsion, preferably 10-25 parts by mass;
1-5 parts by mass of a foam stabilizer, preferably 2-3 parts by mass;
1 to 5 parts by mass of a foaming agent, preferably 2 to 3 parts by mass.
Preferably, the aqueous polyurethane dispersion is an isocyanate-terminated prepolymer obtained by reacting raw materials including isocyanate, polyol and a chain extender, and is obtained by neutralizing and dispersing the isocyanate-terminated prepolymer in water; preferably, the particle size of the aqueous polyurethane dispersion is 200-350nm, which is beneficial to improving the stability of a slurry system and is beneficial to solidification by adopting a metal salt ion flocculation method in a wet process; preferably, the hydrophilic chain extender is used in an amount of 1 to 10%, preferably 1.5 to 4%, based on the total mass of raw materials for preparing the aqueous polyurethane dispersion, in order to obtain an aqueous polyurethane dispersion of a preferred particle size. The solid content of the aqueous polyurethane dispersion is preferably 40-50%, and the aqueous polyurethane dispersion is easy to mechanically foam, associate and thicken and has better construction performance.
Preferably, the isocyanate is selected from one or more of aromatic, aliphatic and cycloaliphatic diisocyanates; further preferred are isophorone diisocyanate (IPDI) and 4,4' -dicyclohexylmethane diisocyanate (H)12One or more of MDI), Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI) and Hexamethylene Diisocyanate (HDI), and more preferably Toluene Diisocyanate (TDI), is added into the slurry formula system, so that a product with good elasticity and toughness and excellent hand feeling can be obtained, the high-temperature high-humidity water resistance (jungle hydrolysis resistance) of the product can be improved, and the high-temperature high-humidity water resistance can reach the 4-week standard.
Preferably, the polyol is selected from one or more of polyether polyol, polyester polyol and polycarbonate polyol; further preferably polyether polyol with the number average molecular weight of 300-. The polyether polyol is preferably one or more of polytetrahydrofuran polyol, polyethylene glycol polyol, polypropylene glycol polyol, polyethylene glycol-propylene glycol copolyol, polyoxypropylene polyol and PO/EO copolymerized polyether polyol. In the PO/EO copolymerized polyether polyol, the EO content is preferably not more than 30% by mass of the polyether polyol. More preferably, the polyol is a polyoxypropylene polyol, and/or a PO/EO copolymerized polyether polyol, such as WANOL C2010, WANOL C2056, WANOL C2140, and the like, available from wawa chemical melway polyurethane ltd. In a more preferable scheme, the polyol is a polyether polyol copolymerized by PO/EO, an EO chain segment is introduced in the ring opening polymerization of PO, the hydrophilicity and the miscibility of the polyether polyol with water and polyisocyanate can be improved, the preferable polyol is favorable for obtaining the aqueous polyurethane dispersion with controllable particle size, and the skin fullness of the suede leather obtained by processing can be improved.
Preferably, the chain extender comprises a hydrophilic chain extender, and preferably also comprises a glycol chain extender; the glycol chain extender may be, for example, but not limited to, one or more of ethylene glycol, 1, 4-butanediol, neopentyl glycol, 1, 6-hexanediol, etc., and the hydrophilic chain extender is preferably an anionic chain extender, and may be one or more of dimethylolpropionic acid (DMPA), dimethylolbutyric acid, dihydroxy half ester, and sodium ethylene diamine sulfonate, and more preferably one or two of dimethylolpropionic acid and dimethylolbutyric acid.
The aqueous suede leather slurry disclosed by the invention preferably comprises the following components in parts by mass in raw materials for preparing the aqueous polyurethane dispersion: 5-20 parts of isocyanate, 75-95 parts of polyol, 0-5 parts of glycol chain extender and 1.5-4 parts of hydrophilic chain extender. The aqueous polyurethane dispersion prepared by adopting the optimized raw material proportion is matched with other components in a slurry formula system, so that the soft and non-sticky hand feeling can be obtained. The specific preparation process of the aqueous polyurethane dispersion is the prior art in the field, and the detailed description is omitted; for example, one particularly preferred preparation step comprises: adding isocyanate, polyol, a hydrophilic chain extender, a dihydric alcohol chain extender and a solvent (such as acetone and the like) into a reactor to react at 60-90 ℃ to reach the theoretical value of NCO (approximately reacting for 3-6 hours), neutralizing (such as adding triethylamine and the like) after the reaction is finished, and adding water to disperse under stirring; optionally, a small molecule amine chain extender (for example, 0 to 4 parts by mass) can be added to continue chain extension (for example, chain extension is 10 min); finally, the solvent is removed. The small molecule amine chain extender can be, for example, ethylenediamine, isophoronediamine, and the like.
According to the water-based suede leather slurry, the preferable water-based acrylic emulsion is the acrylic emulsion crosslinked by metal ions, and the preferable water-based acrylic emulsion is added into the slurry formula system, so that the water-based suede leather slurry and the water-based polyurethane in the formula have good compounding stability, and the opening time of the slurry can be ensured; on the other hand, the two have combined action, have excellent sanding property, are dispersed in the base cloth suede, are easy to sand in the sanding process, do not stick sand paper, and can obtain fine hand feeling of the suede.
In the aqueous suede leather slurry of the present invention, it is further preferred that the metal ion crosslinked acrylate emulsion is a product of Vanhua chemical Co
4316 the styrene-acrylic emulsion or the metal ion crosslinked acrylate emulsion is prepared from the following raw materials in parts by mass to obtain more excellent sanding property: 10-30 parts of methyl methacrylate, 5-15 parts of styrene, 5-15 parts of butyl acrylate, 1-5 parts of methacrylic acid, 5-15 parts of zinc ammonia solution, 0.5-2 parts of emulsifier, 0.1-0.5 part of initiator and 50-70 parts of water. The emulsifier and the initiator used therein may be corresponding reagents commonly used in the art, and are not particularly limited, for example, the emulsifier may be one or more of sodium dodecyl diphenyl oxide disulfonate, sodium dodecyl sulfate, etc., and the initiator may be at least one of ammonium persulfate, potassium persulfate, sodium persulfate, etc.
Preferably, the mass percent of zinc oxide in the zinc-ammonia solution is 5-25%, the mass percent of ammonia water is 5-10%, and the balance is water.
The preparation process of the metal ion crosslinked acrylate emulsion can be the existing preparation process in the field, and details are not repeated. In a preferred embodiment of the present invention, the emulsion is prepared by the steps of: pre-emulsifying an emulsifier, water, methyl methacrylate, styrene, butyl acrylate and methacrylic acid to obtain a pre-emulsion; taking 1-10 wt% of the pre-emulsion as seeds, adding 10-60 wt% of the total amount of the initiator to initiate polymerization (the reaction time can be 15-60min) when the temperature reaches 50-90 ℃ to obtain seed emulsion; and (3) dropwise adding the rest pre-emulsion and the rest initiator into the seed emulsion (the dropwise adding time can be 1-3h), keeping the temperature for 0.5-3h, cooling to below 45 ℃, and adding a zinc ammonia solution. Further preferably, when the pre-emulsification is performed, 10 to 70 wt% of the total amount of the emulsifier and 70 to 90 wt% of the total amount of the water are added to stir, and then the rest of the emulsifier and the water, as well as methyl methacrylate, styrene, butyl acrylate and methacrylic acid are added to perform pre-emulsification.
The aqueous suede leather slurry of the invention preferably further comprises one or more of the following components: the pigment is characterized by comprising a filler, a dispersing agent, color paste and a thickening agent, wherein the filler, the dispersing agent and the thickening agent are preferably at least added.
The filler preferably includes but is not limited to one or more of wood powder, titanium dioxide, calcium carbonate, talcum powder, kaolin, white carbon black, carbon black and calcium sulfate. The invention further discloses a preparation method of the sizing agent, wherein the talc powder is more preferable, the mesh number is preferably 500-4000 meshes, and the application discovers that the talc powder added into the sizing agent formula system has a layered crystal structure, has the tendency of easy cracking into scales and the lubricating property, can obtain the oily feeling similar to the real leather, and has better hand feeling.
The dispersant preferably comprises one or more of polyacid homopolymer, hydrophilic polyacid copolymer and hydrophobic polyacid copolymer, particularly but not limited to Rohm and Hass OROTAN 731A or nopilex dispersant SN 5040, and the like, can obtain excellent overall compatibility and has good matching property with polyurethane thickener.
The foaming agent may be any foaming agent known in the art, and may preferably include surfactants such as sodium lauryl sulfate, sodium fatty alcohol-polyoxyethylene ether sulfate, rosin soap, stearates, silicone polyether emulsions, and the like, more preferably an amine stearate foaming agent, such as but not limited to, those of acesulfame
STA, etc.
The foam stabilizer can be the foam stabilizer existing in the field, preferably comprises succinate foam stabilizer, and particularly, but not limited to, the foam stabilizer can be the foam stabilizer of pythate
SR, and the like.
The thickening agent is one or more of inorganic thickening agents such as celluloses, bentonite and the like, alkaline acrylic acid, hydrophobic modified acrylic acid and nonionic associated polyurethane thickening agents; preferably one or more of nonionic associative polyurethanes; in particular, but not exclusively, associative thickeners of Wanhua chemistry
U605/
U300 or Ningbeidi thickener PS166, Rohm and Haas Dow RM-8w, Rohm and Haas Dow RM-12w, etc. More preferred are high shear thickeners (e.g., Wanhua chemistry)
U300, etc.) and low shear thickeners (e.g., Wanhua chemistry
U605, etc.), the preferred mass ratio of the two is 3: 7-7: 3, the high-shear thickening agent is used for adjusting the slurry to be easy to foam, the low-shear viscosity enables the foamed slurry to be difficult to break foam, the viscosity is stable, and the high-shear thickening agent and the low-shear viscosity are synergistic, so that the preparation of the slurry is facilitated, and the storage stability of the slurry is improved. The shear rate range of the high-shear thickening agent is more than or equal to 1000S-1E.g. 1000S-1-10000S-1Said low shear thickening agent having a shear rate in the range of 0.001 to 0.1S-1。
The color paste is not particularly limited, and a person skilled in the art can select the required color paste according to actual needs.
In a preferred embodiment of the present invention, in the aqueous suede slurry, the filler is preferably 1 to 10 parts by mass, and more preferably 2 to 5 parts by mass; the dispersant is preferably 0.2 to 0.5 part by mass, and more preferably 0.3 to 0.4 part by mass; the color paste is preferably 3 to 10 parts by mass, and more preferably 4 to 6 parts by mass; the thickener is preferably 0.5 to 3 parts by mass, and more preferably 1 to 2 parts by mass.
In a preferred embodiment, the aqueous suede leather slurry comprises the following components in parts by mass so as to obtain better comprehensive performance of the product:
70-95 parts by mass of an aqueous polyurethane dispersion, preferably 80-90 parts by mass;
5-30 parts by mass of water-based acrylic emulsion, preferably 10-25 parts by mass;
1-5 parts by mass of a foam stabilizer, preferably 2-3 parts by mass;
1 to 5 parts by mass of a foaming agent, preferably 2 to 3 parts by mass.
1-10 parts by mass of a filler, preferably 2-5 parts by mass;
0.2 to 0.5 part by mass of a dispersant, preferably 0.3 to 0.4 part by mass;
3-10 parts of color paste, preferably 4-6 parts;
0.5 to 3 parts by mass of a thickener, preferably 1 to 2 parts by mass.
The invention provides a preparation method of aqueous suede leather processing slurry, which comprises the following steps: uniformly mixing and dispersing all components of the aqueous suede leather slurry, and then foaming, wherein the foaming multiplying power is 1-5 multiplying power, preferably 2-3 multiplying power; by adopting the optimal foaming multiplying power, on one hand, the sizing agent is solidified on the surface of the napped fabric in a porous structure, the hand feeling can be effectively improved, and the fine foam structure can ensure that the napped fabric is flawless and uniformly distributed with the napped fabric; on the other hand, the sizing amount is reduced, the cost performance is improved, and the cost is close to that of solvent type electronic packaging suede leather sizing agent. The foaming viscosity may be 3000-7000cp, preferably 4000-6000 cp.
In a specific embodiment, the aqueous polyurethane dispersion and the aqueous acrylic emulsion in the aqueous suede leather slurry are mixed, stirred and dispersed, the dispersing agent and the filler are added under the stirring condition for dispersion (specifically, the stirring can be carried out at the rotating speed of 600 plus 800 rpm, the dispersing agent can be added firstly, the stirring is carried out for 10-20 minutes, the stirring is carried out for 20-30 minutes after the filler is added), the foaming agent, the foam stabilizer and the color paste are added after the uniform dispersion is carried out, the stirring is continued (specifically, the stirring can be carried out for 10-20 minutes), then the thickening agent is added for adjusting the viscosity, and then the foaming is carried out.
The third aspect of the invention provides a method for processing suede leather by adopting a wet process, which comprises the following steps: performing water repellency treatment on the napped cloth, drying, and preferably performing rolling treatment after the water repellency treatment and before the drying; applying the aqueous suede leather slurry to (specifically, blade coating and the like) napped cloth, then immersing the napped cloth into a solidification liquid for solidification, and then performing water washing, drying (preferably performing rolling treatment after the water washing and before the drying) and sanding; the aqueous suede leather slurry is the aqueous suede leather processing slurry prepared by the preparation method. The sanding process can be performed by using grinding wheels with 100-240 meshes, and is selected according to actual requirements.
Preferably, the water repellent treatment is to treat the suede leather by adopting a water repellent agent, wherein the water repellent agent is one or more of a quaternary ammonium salt compound, an organic silicon compound and a fluorine-containing compound; more preferably, the water repellent agent is a cationic quaternary ammonium salt, for example, water repellent agent PF, Ahaore DTM-648, or the like. In the wet process, in order to achieve good hand feeling, the water repellent agent is adopted to form a hydrophobic molecular layer on the surface of the fabric in the pretreatment of the base fabric, so that the surface energy of the fiber is reduced, the coating floats on the surface of the fluff, and the excellent hand feeling can be achieved after the fluff is ground; a large number of pores are still reserved among fibers and among yarns of the fabric after the cationic quaternary ammonium salt water repellent agent is finished, so that the slurry can be effectively prevented from permeating into the back of the base material, the slurry coated by blade coating is arranged between the pile face and the bottom face, the hard handfeel of the board can be avoided, the pile feel is improved, and good air permeability and moisture permeability are still maintained.
Preferably, the coagulating liquid is a mixed solution of soluble metal salts, the soluble metal salts preferably include but are not limited to one or more of calcium chloride dihydrate, aluminum chloride hexahydrate, calcium chloride, aluminum chloride and the like, and the concentration of the coagulating liquid is preferably 0.2-5 wt%. According to the wet process, after the slurry is applied, the slurry is solidified, and preferably, the waterborne polyurethane in the slurry is subjected to flocculation and solidification through metal salt ions, so that on one hand, a stable surface coating with a porous structure can be obtained, on the other hand, the coating strength can be provided through flocculation, and then most of moisture of the waterborne slurry is extruded by matching with a rolling method, and the drying speed is effectively improved.
In a fourth aspect, the present invention provides a suede leather produced by the method described above, preferably a suede leather suitable for electronic packaging.
The technical scheme provided by the invention has the following beneficial effects:
the aqueous suede leather slurry does not contain a plasticizer or an organic solvent in production and use, so that harm to production personnel caused by the plasticizer or the organic solvent can be avoided. The suede leather obtained by the water-based suede leather slurry through a wet process is plump in hand feeling, fine and smooth, excellent in jungle hydrolysis resistance, easy to grind, high in production efficiency, free of any VOC (volatile organic compound) residue and very environment-friendly; the requirements of electronic products such as mobile phone covers, tablet personal computer protective covers and the like on higher and higher requirements can be met.
By adopting the aqueous suede leather slurry, suede leather with excellent elasticity, full hand feeling and fine and smooth suede can be obtained through a wet process and sanding processing.
The aqueous suede leather slurry is particularly suitable for processing suede leather by adopting a wet process, and can replace the traditional oily PU and PVC for manufacturing electronic packaging leather; and a brand new wet production process without solvent and pollution can be used, so that the method is quite friendly to production personnel and environment.
Detailed Description
In order to better understand the technical solution of the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
The main raw materials used in the examples are described below:
OROTAN 731A (polyacrylic acid sodium salt aqueous pigment dispersant, roman hass);
TSELR22(TSE LR series for the color paste for synthetic leather, Suzhou Shiming science)
WANOL C2056: pure PO, wanhua chemistry;
WANOL C2140: PO/EO copolymerized polyether polyol, EO amount about 20% by weight, Wanhua chemistry;
solidifying liquid: 2 parts by mass of calcium chloride dihydrate, 0.2 part by mass of aluminum chloride hexahydrate and 97.8 parts by mass of deionized water are dispersed to obtain a solution.
The synthetic resins referred to in the examples are as follows:
preparation of aqueous polyurethane dispersion a:
223g of WANOL C2056 (polyether polyol), 44g of TDI80 (toluene diisocyanate), 5g of 1, 4-butanediol (diol chain extender), 5g of dimethylolpropionic acid (hydrophilic chain extender) and 50g of acetone (solvent) were added to a 1L four-necked round-bottomed flask equipped with a nitrogen inlet and outlet, and the mixture was stirred at 75 ℃ until NCO reached 1.3% by weight. The temperature is reduced to 40-45 ℃, 231g of acetone and 3.8g of triethylamine are added for neutralization for about 5min, then the mixture is dispersed by adding 420g of water, 4g of isophorone diamine (small molecule amine chain extender) is added after dispersion is finished, and chain extension is continued for 10min under stirring. After further separation of the acetone by distillation, a solvent-free dispersion was obtained having a solids content of 43% by weight, an average particle diameter of 220nm and a pH of 8.4.
Preparation of aqueous polyurethane dispersion B:
400g of WANOL C2140 (polyether polyol), 40g of TDI80 (toluene diisocyanate), 3g of neopentyl glycol (diol chain extender), 8g of dimethylolpropionic acid (hydrophilic chain extender) and 50g of acetone were added to a 1L four-necked round-bottomed flask equipped with a nitrogen port and the mixture was stirred at 75 ℃ until NCO reached 0.70% by weight. The temperature is reduced to 40-45 ℃, 380g of acetone and 6.0g of triethylamine are added for neutralization for about 5min, then the mixture is dispersed by adding 420g of water, after the dispersion is finished, 3.5g of isophorone diamine is added, and the chain extension is continued for 10min under stirring. After further separation of the acetone by distillation, a solvent-free dispersion was obtained having a solids content of 46% by weight, an average particle diameter of 270nm and a pH of 8.5.
Preparation of aqueous polyurethane dispersion C:
223g of WANOL C2056 (polyether polyol), 44g of HDI (hexamethylene diisocyanate), 5g of 1, 4-butanediol (glycol chain extender), 5g of dimethylolpropionic acid (hydrophilic chain extender) and 50g of acetone (solvent) were added to a 1L four-necked round-bottomed flask equipped with a nitrogen inlet and outlet, and the mixture was stirred at 75 ℃ until NCO reached 1.5% by weight. The temperature is reduced to 40-45 ℃, 231g of acetone and 3.8g of triethylamine are added for neutralization for about 5min, then the mixture is dispersed by adding 420g of water, 4.8g of isophorone diamine is added after dispersion is finished, and chain extension is continued for 10min under stirring. After further separation of the acetone by distillation, a solvent-free dispersion was obtained having a solids content of 44.2% by weight, an average particle diameter of 201nm and a pH of 8.8.
Preparation of aqueous acrylic emulsion E:
adding 0.7 part of emulsifier SDS and 50 parts of deionized water into a reaction kettle, starting stirring and heating; adding 0.3 part of SDS emulsifier, 10 parts of deionized water, 20 parts of methyl methacrylate, 10 parts of styrene, 10 parts of butyl acrylate and 4 parts of methacrylic acid into a pre-emulsification kettle for pre-emulsification; taking 5 wt% of the pre-emulsion as a seed, adding the seed into a reaction kettle, adding 0.2 part of APS (ammonium persulfate) as an initiator when the temperature is raised to 80 ℃, and initiating polymerization for 25 min; after the seed reaction is finished, beginning to dropwise add the residual pre-emulsion and 0.2 part of initiator for 2 hours; after the dropwise adding, keeping the temperature for 2 hours; cooling to below 45 deg.c, adding 10 portions of zinc ammonia solution, filtering and discharging. The zinc ammonia solution comprises the following components: 20 wt% of zinc oxide, 10 wt% of ammonia water and 70 wt% of water.
Preparation of aqueous acrylic emulsion F (without metal ion crosslinking):
adding 0.7 part of emulsifier SDS and 50g of deionized water into a reaction kettle, starting stirring and heating; adding 0.3 part of SDS emulsifier, 10g of deionized water, 20 parts of methyl methacrylate, 10 parts of styrene, 10 parts of butyl acrylate and 4 parts of methacrylic acid into a pre-emulsification kettle for pre-emulsification; taking 5% of the pre-emulsion as seeds, adding the seeds into a reaction kettle, adding 0.2 part of APS (ammonium sulfate) as an initiator to initiate polymerization when the temperature is raised to 80 ℃, and reacting for 25 min; after the seed reaction is finished, beginning to dropwise add the residual pre-emulsion and 0.2 part of initiator for 2 hours; after the dropwise adding, keeping the temperature for 2 hours; cooling to below 45 deg.c, filtering and discharging.
Example 1
All the parts mentioned in the formula of the embodiment refer to parts by mass, and the same is true for other embodiments, and the description is omitted.
In this example, aqueous polyurethane dispersion A was mixed with
4316 dispersant: (A)
731A) Stirring at 600 rpm for 10min, adding pulvis Talci (mesh number 2000), stirring at 800 rpm for 15 min, and adding foaming agent: (
STA), foam stabilizer (C: (B) ((C))
SR), water-based red paste (Shiming science and technology TSELR22), thickening agent (VesmodyU 3)00, aqueous polyurethane thickener), thickener (VesmodyU605, aqueous polyurethane thickener), was stirred at 1000 rpm for 15 minutes to prepare a slurry having a viscosity of about 4000cp, and the foaming ratio was 2 times using a mechanical foaming machine (MICROMIX/14, GEMAT foaming machine, italy).
Example 2
In this example, aqueous polyurethane dispersion B was mixed with
4316 dispersant: (A)
731A) Stirring at 600 rpm for 10min, adding pulvis Talci (mesh number 2000), stirring at 800 rpm for 15 min, and adding foaming agent: (
STA), foam stabilizer (C: (B) ((C))
SR), aqueous red paste (Shiming science and technology TSELR22), thickening agent (VesmodyU300, aqueous polyurethane thickening agent), thickening agent (VesmodyU605, aqueous polyurethane thickening agent), stirring for 15 minutes at the rotating speed of 1000 revolutions per minute to prepare slurry with the viscosity of about 4000 cp; the foaming ratio was 2 times that of a mechanical foaming machine.
Example 3
In this example, aqueous polyurethane dispersion A was mixed with
4316 dispersant: (A)
731A) Stirring at 600 rpm for 10min, adding pulvis Talci (mesh number 2000), stirring at 800 rpm for 15 min, and adding foaming agent: (
STA), foam stabilizer (C: (B) ((C))
SR), aqueous red paste (Shiming science and technology TSELR22), thickening agent (VesmodyU300, aqueous polyurethane thickening agent), thickening agent (VesmodyU605, aqueous polyurethane thickening agent), stirring for 15 minutes at the rotating speed of 1000 revolutions per minute to prepare slurry with the viscosity of about 4000 cp; the foaming ratio was 4 times that of a mechanical foaming machine.
Example 4
In this example, aqueous polyurethane dispersion A, aqueous acrylic emulsion E, and aqueous dispersant(s) ((s))
731A) Stirring at 600 rpm for 10min, adding pulvis Talci (mesh number 2000), stirring at 800 rpm for 15 min, and adding foaming agent: (
STA), foam stabilizer (C: (B) ((C))
R), aqueous red paste (Shiming science TSELR22), thickener (VesmodyU300, aqueous polyurethane thickener), thickener (VesmodyU605, aqueous polyurethane thickener), stirring for 15 minutes at a rotation speed of 1000 revolutions per minuteAnd (3) preparing slurry with the viscosity of about 4000cp, and using a mechanical foaming machine to expand the slurry by 2 times.
Example 5
In this example, aqueous polyurethane dispersion C was mixed with
4316 dispersant: (A)
731A) Stirring at 600 rpm for 10min, adding pulvis Talci (mesh number 2000), stirring at 800 rpm for 15 min, and adding foaming agent: (
STA), foam stabilizer (C: (B) ((C))
SR), aqueous red paste (Shiming science and technology TSELR22), thickening agent (VesmodyU300, aqueous polyurethane thickening agent), thickening agent (VesmodyU605, aqueous polyurethane thickening agent), stirring for 15 minutes at the rotating speed of 1000 revolutions per minute to prepare slurry with the viscosity of about 4000 cp; the foaming ratio was 2 times that of a mechanical foaming machine.
Example 6
In this example, aqueous polyurethane dispersion A was mixed with
4316 adding foaming agent
STA), foam stabilizer (C: (B) ((C))
SR), aqueous red paste (Shiming science and technology TSELR22), thickening agent (VesmodyU300, aqueous polyurethane thickening agent), thickening agent (VesmodyU605, aqueous polyurethane thickening agent), stirring for 15 minutes at the rotating speed of 1000 revolutions per minute to prepare slurry with the viscosity of about 4000 cp; the foaming ratio was 2 times that of a mechanical foaming machine.
Example 7
In this example, aqueous polyurethane dispersion A was mixed with
4316 dispersant: (A)
731A) Stirring at 600 rpm for 10min, adding pulvis Talci (mesh number 2000), stirring at 800 rpm for 15 min, and adding foaming agent: (
STA), foam stabilizer (C: (B) ((C))
SR), water-based red paste (Shiming science and technology TSELR22), thickening agent (VesmodyU300), stirring for 15 minutes at the rotating speed of 1000 rpm to prepare slurry with the viscosity of about 4000 cp; the foaming ratio was 2 times that of a mechanical foaming machine.
Comparative example 1
All parts of the formula of the comparative example refer to parts by mass, and the rest of the comparative examples are similar to the formula of the comparative example, so that the detailed description is omitted.
The preparation process was substantially the same as in example 1 except that the expansion ratio of the foam obtained by foaming with the mechanical foaming agent was 0.
Comparative example 2
The procedure was essentially the same as in example 1, except that no aqueous acrylic emulsion was added.
Example 8
The preparation process is the same as that of example 1 and is not repeated.
The following describes the performance testing method:
viscosity test, Bolifei, LV, GB/T2794-
Particle size testing: the Zeta potential and nano-particle size analyzer is adopted to carry out emulsion particle size test, the concentration of the dispersion is diluted to 0.1 percent, the test temperature is 25 ℃, and the laser scattering angle is 90 degrees.
The jungle hydrolysis resistance test method comprises the following steps: performing water repellent treatment on the napped cloth by using a waterproof agent PF, wherein the liquid rate is 50%, and drying in an oven at 80 ℃; respectively blade-coating the aqueous suede leather processing slurry prepared in the above examples and comparative examples on a napped cloth, controlling the thickness to be 0.8mm, then immersing the napped cloth in a solidification solution for solidification, washing and drying after 5min, and sanding with 200-mesh sand paper; and obtaining the electronic packaging suede leather. Standing for 1 day, rolling, placing into a constant temperature and humidity box with temperature of 70 deg.C and humidity of 95%, taking out every week on time, taking control group (not scraping water-based suede leather processing slurry, the other operations are the same), and judging properties such as surface and sticking stickiness. Surface properties the fuzz was observed primarily for uniformity and defects. Sticking performance to a sticker: and (3) oppositely attaching a 4 cm-4 cm sample cloth under the pressure of 3kg, placing the sample cloth in a constant temperature and humidity box for 24h, taking out the sample cloth, and judging the force after the sample cloth is uncovered.
Stability test method (slurry storage stability): taking 1 kg of slurry into a 1 kg plastic bottle, sealing, standing at normal temperature, and observing viscosity change and bubble breaking phenomenon;
and (3) comparison test:
the contrast material was solvent-based suede packaging leather, available from Glan leather Co., Ltd, Dongguan, having a Korea imitated microfiber thickness of 0.4mm, a breadth of 137cm and a color of No. 17.
The appearance test method comprises the following steps: the eye is judged to have defects and covering power. By comparing the scores of the solvent-based packaging leather, the evaluation grades are shown in the table 1;
the hand feeling test method comprises the following steps: hand feeling judgment is carried out through hand grasping and touch, and the hand feeling judgment comprises tactile senses such as texture, fullness, toughness and the like; by comparing the scores of the solvent-based packaging leather, the evaluation grades are shown in the table 1;
the velvet feeling test method comprises the following steps: the fluff is uniform and fine by touching with hands; the evaluation grades are given in table 1 by comparison with solvent-based packaging leather scores.
TABLE 1 evaluation rating reference Table
The performance test results of the obtained waterborne polyurethane electronic suede packaging leather are shown in table 2.
TABLE 2
From the above experimental results it can be seen that: of examples 1-8, the example using the preferred isocyanate TDI when preparing the aqueous polyurethane dispersion had better resistance to jungle hydrolysis than example 5, which did not use the preferred isocyanate. Example 6, which did not use talc as a filler, had a slightly poor hand, while the other examples all had a wet and slippery hand. The product prepared by adopting the slurry system combining the low-shear thickening agent and the high-shear thickening agent has better storage performance and more stable foam; whereas example 7 has relatively poor memory performance. Comparative example 1 is no foaming, the expansion ratio is 0, and compared with the examples of the present invention, it is difficult to form a cell structure, and the hand panel is hard after sanding. Compared with the embodiment of the invention, the effect is poorer in the sanding process, and the obtained suede leather has poorer hand feeling and downy feeling. Example 8 compared to the other examples, the aqueous acrylic emulsion not crosslinked with the preferred metal ions had a slightly inferior sanding property and produced suede leather products having a slightly inferior hand feel.
It will be appreciated by those skilled in the art that modifications or adaptations to the invention may be made in light of the teachings of the present specification. Such modifications or adaptations are intended to be within the scope of the present invention as defined in the claims.
Claims (24)
1. The water-based suede leather slurry is characterized by comprising the following components in parts by mass:
70-95 parts by mass of an aqueous polyurethane dispersion;
5-30 parts of water-based acrylic emulsion;
1-5 parts of a foam stabilizer;
1-5 parts by mass of a foaming agent;
1-10 parts by mass of a filler;
0.2-0.5 parts by mass of a dispersant;
3-10 parts of color paste;
0.5-3 parts of thickening agent;
moreover, the foaming multiplying power of the water-based suede leather slurry is 1-5 multiplying power;
wherein the aqueous acrylic emulsion is a metal ion crosslinked acrylate emulsion; the filler is talcum powder;
the aqueous polyurethane dispersion is an isocyanate-terminated prepolymer obtained by reacting raw materials including isocyanate, polyol and a chain extender, and is obtained by neutralizing and dispersing the isocyanate-terminated prepolymer in water; the isocyanate is selected from toluene diisocyanate; the polyol is selected from one or more of polyether polyol, polyester polyol and polycarbonate polyol; the chain extender comprises a hydrophilic chain extender.
2. The aqueous suede leather slurry according to claim 1,
the polyol is selected from polyether polyols having a number average molecular weight of 300-.
3. The aqueous suede leather slurry according to claim 2, wherein the polyether polyol is one or more of polytetrahydrofuran polyol, polyethylene glycol polyol, polypropylene glycol polyol, polyethylene glycol-propylene glycol copolyol, polyoxypropylene polyol and PO/EO copolymerized polyether polyol; the PO/EO copolymerized polyether polyol has an EO content of not more than 30% by mass of the polyether polyol.
4. The aqueous suede leather slurry of claim 1, wherein the chain extender further comprises a glycol chain extender; the dihydric alcohol chain extender is one or more of ethylene glycol, 1, 4-butanediol, neopentyl glycol and 1, 6-hexanediol.
5. The aqueous suede leather slurry according to claim 4, wherein the hydrophilic chain extender is an anionic chain extender.
6. The aqueous suede leather slurry according to claim 5, wherein the hydrophilic chain extender is one or more of dihydroxypropionic acid, dimethylolbutyric acid, dihydroxy half ester, sodium ethylene diamine ethanesulfonate.
7. The aqueous suede leather slurry according to any one of claims 1-6, wherein the particle size of the aqueous polyurethane dispersion is 200-350 nm; the solid content is 40-50%.
8. The aqueous suede leather slurry according to claim 7, wherein the hydrophilic chain extender is used in an amount of 1-10% based on the total mass of raw materials for preparing the aqueous polyurethane dispersion.
9. The aqueous suede leather slurry according to claim 8, wherein the hydrophilic chain extender is used in an amount of 1.5-4% based on the total mass of raw materials for preparing the aqueous polyurethane dispersion.
10. The aqueous suede leather slurry according to any one of claims 4-6, wherein the raw materials for preparing the aqueous polyurethane dispersion comprise the following components in parts by mass: 5-20 parts of isocyanate, 75-95 parts of polyol, 0-5 parts of glycol chain extender and 1.5-4 parts of hydrophilic chain extender.
11. The aqueous suede leather slurry according to claim 1, wherein the metal ion crosslinked acrylate emulsion is from Vanhua chemical company
4316 styrene-acrylic emulsion; or the metal ion crosslinked acrylate emulsion is prepared from the following raw materials in parts by mass: 10-30 parts of methyl methacrylate, 5-15 parts of styrene, 5-15 parts of butyl acrylate, 1-5 parts of methacrylic acid, 5-15 parts of zinc ammonia solution, 0.5-2 parts of emulsifier, 0.1-0.5 part of initiator and 50-70 parts of water.
12. The aqueous suede leather slurry according to claim 11, wherein in the zinc ammonia solution, the mass percent of zinc oxide is 5-25%, the mass percent of ammonia water is 5-10%, and the balance is water.
13. The aqueous suede leather slurry according to claim 11, wherein the step of preparing the metal ion crosslinked acrylate emulsion comprises: pre-emulsifying an emulsifier, water, methyl methacrylate, styrene, butyl acrylate and methacrylic acid to obtain a pre-emulsion; taking 1-10 wt% of the pre-emulsion as seeds, adding 10-60 wt% of the total amount of the initiator when the temperature reaches 50-90 ℃ to initiate polymerization to obtain seed emulsion; and (3) dropwise adding the rest pre-emulsion and the rest initiator into the seed emulsion, keeping the temperature for 0.5-3h, cooling to below 45 ℃, and adding a zinc ammonia solution.
14. The aqueous suede leather slurry according to claim 13, wherein in the pre-emulsification, 10-70 wt% of the total amount of the emulsifier and 70-90 wt% of the total amount of water are added to be stirred, and then the rest of the emulsifier and water, and methyl methacrylate, styrene, butyl acrylate and methacrylic acid are added to be pre-emulsified.
15. The aqueous suede slurry according to any one of claims 1-6,
the filler is talcum powder with the mesh number of 500-4000;
the dispersant is selected from one or more of polyacid homopolymer, hydrophilic polyacid copolymer and hydrophobic polyacid copolymer;
the foaming agent is selected from one or more of lauryl sodium sulfate, fatty alcohol-polyoxyethylene ether sodium sulfate, rosin soaps, stearamides and silicone polyether emulsion surfactants;
the foam stabilizer is selected from succinate foam stabilizers;
the thickening agent is selected from one or more of inorganic thickening agents, alkaline acrylic acid, hydrophobic modified acrylic acids and nonionic associated polyurethane thickening agents.
16. The aqueous suede leather slurry according to claim 15, wherein the thickener is a nonionic associative polyurethane thickener.
17. The aqueous suede slurry according to claim 16, wherein the thickener is a combination of both a high shear thickener and a low shear thickener, the high shear thickener having a shear rate in the range of 1000S or more-1Said low shear thickening agent having a shear rate in the range of 0.001 to 0.1S-1。
18. The aqueous suede leather slurry according to claim 15, which is characterized by comprising the following components in parts by mass:
80-90 parts by mass of an aqueous polyurethane dispersion;
10-25 parts by mass of a water-based acrylic emulsion;
2-3 parts of a foam stabilizer;
2-3 parts of foaming agent;
2-5 parts of a filler;
0.3-0.4 parts by mass of a dispersant;
4-6 parts of color paste;
1-2 parts of thickening agent.
19. The preparation method of the aqueous suede leather processing slurry is characterized by comprising the following steps: the aqueous suede leather slurry according to any one of claims 1-18, wherein the components are uniformly mixed and dispersed, and then foaming is carried out, and the foaming ratio is 1-5.
20. The production method according to claim 19, wherein the expansion ratio is 2 to 3.
21. A method for processing suede leather by adopting a wet process is characterized by comprising the following steps:
1) performing water repellency treatment on the napped cloth, and drying;
2) applying the aqueous suede leather processing slurry to napped cloth, then immersing the napped cloth into a solidification solution for solidification, and then performing washing, drying and sanding; the aqueous suede leather processing slurry is prepared by the preparation method of claim 19 or 20;
the water repellent treatment is to treat the suede leather by adopting a water repellent agent, wherein the water repellent agent is one or more of a quaternary ammonium salt compound, an organic silicon compound and a fluorine-containing compound;
the coagulating liquid is a mixed solution of soluble metal salts.
22. A method according to claim 21, wherein in step 1), a rolling treatment is further performed after the water-repellent treatment;
in the step 2), rolling treatment is also carried out after water washing;
the water repellent is a cationic quaternary ammonium salt water repellent; the soluble metal salt comprises one or more of calcium chloride dihydrate, aluminum chloride hexahydrate, calcium chloride and aluminum chloride, and the concentration of the solidification liquid is 0.2-5 wt%.
23. Suede leather produced by the method of claim 21 or 22.
24. The suede leather of claim 23, which is suede leather adapted for electronic packaging.
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| CN114174469A (en) * | 2019-07-18 | 2022-03-11 | 赢创运营有限公司 | Combined use of polyol ethers and cationic polyelectrolytes in aqueous polyurethane dispersions |
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