CN109537301A - A method of synthetic leather functional coating is prepared with solution casting method final finishing technology - Google Patents

A method of synthetic leather functional coating is prepared with solution casting method final finishing technology Download PDF

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CN109537301A
CN109537301A CN201811415196.5A CN201811415196A CN109537301A CN 109537301 A CN109537301 A CN 109537301A CN 201811415196 A CN201811415196 A CN 201811415196A CN 109537301 A CN109537301 A CN 109537301A
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synthetic leather
solution
coating
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郭艳
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Bengbu Star Scintillation New Material Technology Co Ltd
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Bengbu Star Scintillation New Material Technology Co Ltd
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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
    • D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
    • D06N3/005—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers obtained by blowing or swelling agent
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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
    • D06N3/121—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 polyesters, polycarbonates, alkyds
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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
    • D06N3/142—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 mixture of polyurethanes with other resins in the same layer
    • D06N3/143—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 mixture of polyurethanes with other resins in the same layer with polyurethanes and other polycondensation or polyaddition products, e.g. aminoplast
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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
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    • D06N3/142—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 mixture of polyurethanes with other resins in the same layer
    • D06N3/144—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 mixture of polyurethanes with other resins in the same layer with polyurethane and polymerisation products, e.g. acrylics, PVC
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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a kind of methods for preparing synthetic leather functional coating with solution casting method final finishing technology, blend solution is uniformly mixed with gained modified nano-titanium dioxide, graphene modified aqueous polyurethane slurry, high dispersive silica-unsaturated polyester coating, obtains coating solution；Coating solution is poured over by synthetic leather surface using solution casting method, solvent flashing is dried in vacuo, film, melt process is made, then cultivated and made annealing treatment, functional coating is made on synthetic leather surface.Using triethylamine as catalyst, nano-titanium dioxide is modified with Silane coupling agent KH550, modified nano-titanium dioxide, which is added, can be improved the antistatic property of coating solution, improve the gas permeability and water vapor permeability of synthetic leather, hence it is evident that improve wear-resisting, the folding resistance of synthetic leather.

Description

A method of synthetic leather functional coating is prepared with solution casting method final finishing technology
Technical field
The invention belongs to artificial leather fields, and in particular to a kind of to prepare synthetic leather function with solution casting method final finishing technology The method of property coating.
Background technique
Using textile fabric as base, polyurethane is that the synthetic leather of coating has the developing history of many years, is widely used in people Live in various aspects.Using solvent borne polyurethane as the conventional urethane synthetic leather of main material production, there are organic molten The problem of agent volatilization and pollution.It is to close at this stage using environment-friendly water-based and functional modification material preparation high-performance multi-functional coatings The new and high technology that finished leather industry is given priority to.Aqueous polyurethane has nontoxic, environmentally protective advantage, but its using water as medium There is poor mechanical property, wear no resistance, intolerant to hydrolysis the problems such as.As the nova in carbon nanomaterial field, graphene has Excellent mechanical property and electric property, can be used for improving mechanical property, thermal stability, electric conductivity of polyurethane matrix etc., Therefore graphene modified aqueous polyurethane becomes the research hotspot of researcher, and the need of country and industry value chain It asks.
Unsaturated polyester resin is one of the most widely used thermosetting resin, have low cost, low-density,
The advantages that highly corrosion resistant and excellent processing performance.It, which often needs to add filler in use, is modified, benefit The problem of being commonly present dispersibility and poor compatibility with inoganic particle modified unsaturated polyester resin.
The functionalization of high molecular material is its following developing direction, is risen to the development of the high-technology fields such as advanced manufacture Important impetus.Important branch of the synthetic leather as high molecular material has wide in the every field of national economy Market, in recent years the functionalization high-end market such as forward conduction, damping and electrochromism develop.Study synthetic leather surface Functional coating with performances such as ferroelectricity, dielectric and pyroelectricities has the application field for developing and widen functional synthetic leather There is important theoretical and practical significance.Currently, it is good in processing performance and have ferroelectricity and medium electrical property high polymer coating material in, gather Vinylidene occupies consequence, and strand construction is special, and outside the property for having both resins for universal use and fluororesin, there are also excellent Ferroelectricity and the performances such as pyroelectricity.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of solution casting method final finishing technology preparation synthesis is provided Remove from office functional coating method, according to this method production synthetic leather have excellent antistatic property, wearability, folding resistance and thoroughly Gas, water vapor permeability and dielectric properties.
The present invention is achieved by the following technical solutions:
A method of synthetic leather functional coating is prepared with solution casting method final finishing technology, which is characterized in that including as follows Step:
(1) modified nano-titanium dioxide:
3-4 parts of nano-titanium dioxide powders are dried in vacuo 20-25h at 90-110 DEG C, acetone is added in 1:7-8 in mass ratio, 0.1-0.2 parts of KH550 and 0.1-0.2 parts of triethylamines, mechanical stirring 1-2h is added in ultrasonic disperse 30-40min under nitrogen protection Afterwards, flow back modified 2-3h, and filtering after washing extraction 3-5 times with dehydrated alcohol, is dried in vacuo 1-2h, mechanical grinding at 80-85 DEG C Grind to obtain modified nano-titanium dioxide；
(2) graphene modified aqueous polyurethane:
90-100 parts of aqueous polyurethanes, 0.5-2 parts of thickeners, 1-2 parts of foaming agents, 5-7 parts of carbon are added into graphene dispersing solution Sour calcium, stirs, and graphene modified aqueous polyurethane slurry is made；
(3) high dispersive silica-unsaturated polyester coating preparation:
4-6 parts of high dispersive silica flatting silicas, high shear mixing emulsion dispersion are added into 30-40 parts of unsaturated polyester resins 5-10min stands 3-5min, and 0.3-0.4 parts of promotors are added and stir evenly, adds 0.4-0.6 parts of initiators and stirs evenly, High dispersive silica-unsaturated polyester coating is made；
(4) preparation of synthetic leather functional coating:
By gained graphene modified aqueous polyurethane slurry in gained modified nano-titanium dioxide in blend solution and (1), (2), (3) gained high dispersive silica-unsaturated polyester coating is uniformly mixed in, obtains coating solution；It will using solution casting method Coating solution is poured over synthetic leather surface, is dried in vacuo solvent flashing, film coating is made, the melt process at 190-200 DEG C 10-15min is cultivated and is made annealing treatment 1-2h at 130-158 DEG C, and functional coating is made on synthetic leather surface.
Further, in step (2) graphene dispersion: be added into 0.5-1 parts of dispersing aid polyvinylpyrrolidones Deionized water, stirring and dissolving are made the dispersant solution that concentration is 1-2mg/mL, 1-2 parts of graphenes, ultrasonic disperse 50- are added The graphene dispersing solution that concentration is 0.5-1mg/mL is made in 60min.
Further, promotor is cobalt naphthenate in step (3), and initiator is methyl ethyl ketone peroxide.
Further, blend solution is prepared using solution blended process in step (4): by 50-90 parts of Kynoar, 10- 50 parts of poly adipate succinic acid ester mixing, add 1-1.8 parts of ionic liquid fuse salt [BMIM] PF6It is blended, solvent N is added, The blend solution that concentration is 4-6mg/mL is made in dinethylformamide, stirring and dissolving.
The present invention has the advantage that compared with prior art
(1) using triethylamine as catalyst, nano-titanium dioxide is modified with Silane coupling agent KH550, modified Nano is added The antistatic property of coating solution can be improved in titanium dioxide, improves the gas permeability and water vapor permeability of synthetic leather, hence it is evident that improves synthetic leather Wear-resisting, folding resistance.
(2) stable graphene aqueous solution is prepared as dispersing aid using polyvinylpyrrolidone, using the side of solution blending Method prepares graphene modified aqueous polyurethane slurry, and graphene may be homogenously dispersed in aqueous polyurethane, composite membrane tensile strength, Elongation at break is improved, and the addition of graphene can improve the mechanical property and electric property of aqueous polyurethane, improves The wearability of coating.
(3) high dispersive silica flatting silica is dispersed in unsaturated polyester resin using emulsifying manner, is prepared Low thickening antiglossing pigment, can play preferable extinction effect to class coating material, and resistance to blocking is 5 grades.
(4) Kynoar-poly adipate succinic acid ester-ionic liquid fuse salt [BMIM] is prepared using solution blended process PF6Blend solution, the poly adipate succinic acid ester in compound system can promote Kynoar Crystallization more stable Structure, the addition of poly adipate succinic acid ester can enhance the ferroelectricity of composite material, improve coercive field and maximum polarization is strong Degree is conducive to increase on-off ratio of the composite material as memory；Ionic liquid can improve the hydrophily and dielectricity of synthetic leather Energy.
Specific embodiment
Embodiment 1
A method of synthetic leather functional coating is prepared with solution casting method final finishing technology, which is characterized in that including as follows Step:
(1) modified nano-titanium dioxide:
3 parts of nano-titanium dioxide powders are dried in vacuo 20h at 90-110 DEG C, acetone, ultrasonic disperse is added in 1:7 in mass ratio 0.1 part of KH550 and 0.1 part of triethylamine is added in 30min under nitrogen protection, and after mechanical stirring 1h, flow back modified 2h, and filtering is used After dehydrated alcohol washing extraction 3 times, 1h is dried in vacuo at 80-85 DEG C, mechanical lapping obtains modified nano-titanium dioxide；
(2) graphene modified aqueous polyurethane:
90 parts of aqueous polyurethanes, 0.5 part of thickener, 1 part of foaming agent, 5 parts of calcium carbonate are added into graphene dispersing solution, sufficiently stir It mixes uniformly, graphene modified aqueous polyurethane slurry is made；
(3) high dispersive silica-unsaturated polyester coating preparation:
4 parts of high dispersive silica flatting silicas of addition into 30 parts of unsaturated polyester resins, high shear mixing emulsion dispersion 5min, 3min is stood, 0.3 part of promotor is added and stirs evenly, adds 0.4 part of initiator and stirs evenly, high dispersive titanium dioxide is made Silicon-unsaturated polyester coating；
(4) preparation of synthetic leather functional coating:
By gained graphene modified aqueous polyurethane slurry in gained modified nano-titanium dioxide in blend solution and (1), (2), (3) gained high dispersive silica-unsaturated polyester coating is uniformly mixed in, obtains coating solution；It will using solution casting method Coating solution is poured over synthetic leather surface, is dried in vacuo solvent flashing, film coating is made, the melt process at 190-200 DEG C 10min is cultivated and is made annealing treatment 1h at 130-158 DEG C, and functional coating is made on synthetic leather surface.
Further, in step (2) graphene dispersion: be added and go into 0.5 part of dispersing aid polyvinylpyrrolidone The dispersant solution that concentration is 1mg/mL is made in ionized water, stirring and dissolving, and 1 part of graphene is added, and ultrasonic disperse 50min is made Concentration is the graphene dispersing solution of 0.5mg/mL.
Further, promotor is cobalt naphthenate in step (3), and initiator is methyl ethyl ketone peroxide.
Further, blend solution is prepared using solution blended process in step (4): 50 parts of Kynoar, 10 parts are gathered Tetramethylene adipate mixing, adds 1 part of ionic liquid fuse salt [BMIM] PF6It is blended, solvent N, N- dimethyl methyl is added The blend solution that concentration is 4mg/mL is made in amide, stirring and dissolving.
Embodiment 2
A method of synthetic leather functional coating is prepared with solution casting method final finishing technology, which is characterized in that including as follows Step:
(1) modified nano-titanium dioxide:
4 parts of nano-titanium dioxide powders are dried in vacuo 25h at 90-110 DEG C, acetone, ultrasonic disperse is added in 1:8 in mass ratio 0.2 part of KH550 and 0.2 part of triethylamine is added in 40min under nitrogen protection, and after mechanical stirring 2h, flow back modified 3h, and filtering is used After dehydrated alcohol washing extraction 5 times, 2h is dried in vacuo at 80-85 DEG C, mechanical lapping obtains modified nano-titanium dioxide；
(2) graphene modified aqueous polyurethane:
100 parts of aqueous polyurethanes, 2 parts of thickeners, 2 parts of foaming agents, 7 parts of calcium carbonate are added into graphene dispersing solution, sufficiently stir It mixes uniformly, graphene modified aqueous polyurethane slurry is made；
(3) high dispersive silica-unsaturated polyester coating preparation:
6 parts of high dispersive silica flatting silicas, high shear mixing emulsion dispersion are added into 40 parts of unsaturated polyester resins 10min stands 5min, 0.4 part of promotor is added and stirs evenly, adds 0.6 part of initiator and stirs evenly, and high dispersive two is made Silica-unsaturated polyester coating；
(4) preparation of synthetic leather functional coating:
By gained graphene modified aqueous polyurethane slurry in gained modified nano-titanium dioxide in blend solution and (1), (2), (3) gained high dispersive silica-unsaturated polyester coating is uniformly mixed in, obtains coating solution；It will using solution casting method Coating solution is poured over synthetic leather surface, is dried in vacuo solvent flashing, film coating is made, the melt process at 190-200 DEG C 15min is cultivated and is made annealing treatment 2h at 130-158 DEG C, and functional coating is made on synthetic leather surface.
Further, in step (2) graphene dispersion: into 1 part of dispersing aid polyvinylpyrrolidone be added go from Sub- water, stirring and dissolving are made the dispersant solution that concentration is 2mg/mL, 2 parts of graphenes are added, ultrasonic disperse 60min is made dense Degree is the graphene dispersing solution of 1mg/mL.
Further, promotor is cobalt naphthenate in step (3), and initiator is methyl ethyl ketone peroxide.
Further, blend solution is prepared using solution blended process in step (4): 90 parts of Kynoar, 50 parts are gathered Tetramethylene adipate mixing, adds 1.8 parts of ionic liquid fuse salt [BMIM] PF6It is blended, solvent N, N- dimethyl is added The blend solution that concentration is 6mg/mL is made in formamide, stirring and dissolving.
Comparative example 1
This comparative example 1 compared with Example 1, does not carry out any modification to nano-titanium dioxide in step (1), removes Furthermore method and step is all the same.
Comparative example 2
This comparative example 2 compared with Example 2, unused unsaturated polyester resin, promotor, initiator pair in step (3) High dispersive silica flatting silica carries out emulsion dispersion, and method and step in addition to this is all the same.
Control group blank synthetic leather
It is real to above-described embodiment 1, embodiment 2, comparative example 1, comparison in order to compare the performance of synthetic leather produced by the present invention It applies the corresponding synthetic leather obtained of 2 method of example and the corresponding synthetic leather of control group and carries out performance detection according to professional standard, specifically Correlation data is as shown in table 1 below:
Table 1
There is excellent antistatic property, wearability, folding resistance and gas permeability, vapor pervious according to the synthetic leather of the method for the present invention production Property；Any modification is not carried out to nano-titanium dioxide in comparative example 1, leads to the gas permeability and vapor pervious of synthetic leather Property reduce, but still be better than blank synthetic leather gas permeability and water vapor permeability；The unused unsaturated polyester (UP) tree in comparative example 2 Rouge, promotor, initiator carry out emulsion dispersion to high dispersive silica flatting silica, and the dullness of synthetic leather is caused to reduce, but Still better than blank synthetic leather.

Claims (4)

1. a kind of method for preparing synthetic leather functional coating with solution casting method final finishing technology, which is characterized in that including such as Lower step:
(1) modified nano-titanium dioxide:
3-4 parts of nano-titanium dioxide powders are dried in vacuo 20-25h at 90-110 DEG C, acetone is added in 1:7-8 in mass ratio, 0.1-0.2 parts of KH550 and 0.1-0.2 parts of triethylamines, mechanical stirring 1-2h is added in ultrasonic disperse 30-40min under nitrogen protection Afterwards, flow back modified 2-3h, and filtering after washing extraction 3-5 times with dehydrated alcohol, is dried in vacuo 1-2h, mechanical grinding at 80-85 DEG C Grind to obtain modified nano-titanium dioxide；
(2) graphene modified aqueous polyurethane:
90-100 parts of aqueous polyurethanes, 0.5-2 parts of thickeners, 1-2 parts of foaming agents, 5-7 parts of carbon are added into graphene dispersing solution Sour calcium, stirs, and graphene modified aqueous polyurethane slurry is made；
(3) high dispersive silica-unsaturated polyester coating preparation:
4-6 parts of high dispersive silica flatting silicas, high shear mixing emulsion dispersion are added into 30-40 parts of unsaturated polyester resins 5-10min stands 3-5min, and 0.3-0.4 parts of promotors are added and stir evenly, adds 0.4-0.6 parts of initiators and stirs evenly, High dispersive silica-unsaturated polyester coating is made；
(4) preparation of synthetic leather functional coating:
By gained graphene modified aqueous polyurethane slurry in gained modified nano-titanium dioxide in blend solution and (1), (2), (3) gained high dispersive silica-unsaturated polyester coating is uniformly mixed in, obtains coating solution；It will using solution casting method Coating solution is poured over synthetic leather surface, is dried in vacuo solvent flashing, film coating is made, the melt process at 190-200 DEG C 10-15min is cultivated and is made annealing treatment 1-2h at 130-158 DEG C, and functional coating is made on synthetic leather surface.
2. a kind of side for preparing synthetic leather functional coating with solution casting method final finishing technology according to claim 1 Method, which is characterized in that the dispersion of graphene in step (2):
Deionized water is added into 0.5-1 parts of dispersing aid polyvinylpyrrolidones, stirring and dissolving, it is 1-2mg/mL that concentration, which is made, Dispersant solution, be added 1-2 part graphenes, ultrasonic disperse 50-60min, be made concentration be 0.5-1mg/mL graphene divide Dispersion liquid.
3. a kind of side for preparing synthetic leather functional coating with solution casting method final finishing technology according to claim 1 Method, which is characterized in that promotor is cobalt naphthenate in step (3), and initiator is methyl ethyl ketone peroxide.
4. a kind of side for preparing synthetic leather functional coating with solution casting method final finishing technology according to claim 1 Method, which is characterized in that prepare blend solution using solution blended process in step (4):
50-90 parts of Kynoar, 10-50 parts of poly adipate succinic acid esters are mixed, 1-1.8 parts of ionic liquid meltings are added Salt [BMIM] PF6It is blended, solvent n,N-Dimethylformamide is added, it is molten that the blending that concentration is 4-6mg/mL is made in stirring and dissolving Liquid.
CN201811415196.5A 2018-11-26 2018-11-26 A method of synthetic leather functional coating is prepared with solution casting method final finishing technology Withdrawn CN109537301A (en)

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