CN110565395B - Production process of PU synthetic leather - Google Patents
Production process of PU synthetic leather Download PDFInfo
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- CN110565395B CN110565395B CN201910678972.9A CN201910678972A CN110565395B CN 110565395 B CN110565395 B CN 110565395B CN 201910678972 A CN201910678972 A CN 201910678972A CN 110565395 B CN110565395 B CN 110565395B
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- 239000002649 leather substitute Substances 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000002585 base Substances 0.000 claims abstract description 58
- 239000004744 fabric Substances 0.000 claims abstract description 58
- 239000003513 alkali Substances 0.000 claims abstract description 34
- 229920004933 Terylene® Polymers 0.000 claims abstract description 32
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 32
- 229920000728 polyester Polymers 0.000 claims abstract description 29
- 238000012986 modification Methods 0.000 claims abstract description 28
- 230000004048 modification Effects 0.000 claims abstract description 28
- 238000010306 acid treatment Methods 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 24
- 108010022355 Fibroins Proteins 0.000 claims abstract description 19
- 238000007598 dipping method Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 11
- 239000004814 polyurethane Substances 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 claims description 16
- 238000007711 solidification Methods 0.000 claims description 16
- 230000008023 solidification Effects 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 10
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 10
- 238000007865 diluting Methods 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- 229920003009 polyurethane dispersion Polymers 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 229920013822 aminosilicone Polymers 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 5
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 5
- RNSLCHIAOHUARI-UHFFFAOYSA-N butane-1,4-diol;hexanedioic acid Chemical compound OCCCCO.OC(=O)CCCCC(O)=O RNSLCHIAOHUARI-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 5
- 229920000962 poly(amidoamine) Polymers 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 229920001451 polypropylene glycol Polymers 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 238000007790 scraping Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 abstract description 9
- 238000000576 coating method Methods 0.000 abstract description 9
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 55
- 239000000835 fiber Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000010985 leather Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 229920002635 polyurethane Polymers 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 239000012790 adhesive layer Substances 0.000 description 3
- -1 cerium ions Chemical class 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 239000000412 dendrimer Substances 0.000 description 2
- 229920000736 dendritic polymer Polymers 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004597 plastic additive Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
- D06M11/65—Salts of oxyacids of nitrogen
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
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- D—TEXTILES; PAPER
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/325—Amines
- D06M13/332—Di- or polyamines
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/15—Proteins or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—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
- D06N3/0036—Polyester fibres
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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
- D06N3/12—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
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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- D06N2209/00—Properties of the materials
- D06N2209/10—Properties of the materials having mechanical properties
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- D06N2209/00—Properties of the materials
- D06N2209/16—Properties of the materials having other properties
- D06N2209/1664—Releasability
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention discloses a production process of PU synthetic leather, which has the technical scheme key points that the production process comprises the following steps: s1 acid treatment: soaking the terylene base cloth in an acid treatment solution at the temperature of 70-80 ℃ for 15-20min, and then drying the terylene base cloth in vacuum at the temperature of 90-95 ℃; s2 alkali treatment: soaking the terylene base cloth subjected to S1 acid treatment in an alkali treatment solution at the temperature of 75-85 ℃ for 30-40min, and washing and drying the terylene base cloth to constant weight after the treatment is finished; hydrophilic modification of S3: immersing the terylene base cloth subjected to the alkali treatment of S2 in a modification solution at the temperature of 25-35 ℃ for 80-100min, pre-drying after the treatment is finished, baking at the temperature of 130-140 ℃ for 2-3min, and then washing and drying, wherein the modification solution comprises 5-7% of silk fibroin; s4 dipping; s5 is solidified. The silk fibroin is arranged before the polyester base cloth is soaked in PU, so that the formed PU coating has good adhesive force, is not easy to peel off and has long service life.
Description
Technical Field
The invention relates to synthetic leather, in particular to a production process of PU synthetic leather.
Background
Artificial leather is a kind of plastic product with appearance and hand feeling similar to leather and capable of replacing it, and is produced by coating fabric as base with synthetic resin and various plastic additives. The artificial leather mainly comprises PVC artificial leather and PU synthetic leather, wherein the PU synthetic leather has the advantages of attractive appearance and good care and is an ideal substitute of natural leather.
Common production methods of PU synthetic leather include a dry method and a wet method. The dry process comprises the following steps: preparing PU resin into sol with certain solid content and certain viscosity, coating the sol on release paper serving as a carrier, heating the sol in an oven to volatilize a solvent so as to form a film, coating an adhesive layer on the film, compounding the adhesive layer with base cloth, drying, curing, cooling, then stripping the adhesive layer from the release paper, and finally carrying out processes such as printing treatment to obtain the synthetic leather. The wet process comprises the following steps: directly soaking the base cloth in the prepared PU resin, washing and curing the base cloth by DMF aqueous solution, washing the base cloth by hot water, and finally drying and post-treating the base cloth to obtain the PU synthetic leather.
Although the appearance of the PU synthetic leather is very close to that of genuine leather and has excellent cold resistance and aging resistance, the wear resistance of the PU synthetic leather relative to genuine leather is still poor, and the PU epidermis is easy to peel off after long-term use and needs to be improved.
Disclosure of Invention
Aiming at the technical defects, the invention aims to provide a production process of PU synthetic leather, and the PU coating has high adhesive force and is not easy to peel off.
In order to achieve the purpose, the invention provides the following technical scheme:
a production process of PU synthetic leather comprises the following steps:
s1 acid treatment: soaking the terylene base cloth in an acid treatment solution at the temperature of 70-80 ℃ for 15-20min, and then drying the terylene base cloth in vacuum at the temperature of 90-95 ℃;
s2 alkali treatment: soaking the terylene base cloth subjected to S1 acid treatment in an alkali treatment solution at the temperature of 75-85 ℃ for 30-40min, and washing and drying the terylene base cloth to constant weight after the treatment is finished;
hydrophilic modification of S3: immersing the terylene base cloth subjected to the alkali treatment of S2 in a modification solution at the temperature of 25-35 ℃ for 80-100min, pre-drying after the treatment is finished, baking at the temperature of 130-140 ℃ for 2-3min, and then washing and drying, wherein the modification solution comprises 5-7% of silk fibroin;
s4 dipping: soaking the polyester base fabric subjected to hydrophilic modification by S3 into PU dipping solution, and scraping redundant slurry;
s5 solidification: and (3) immersing the polyester base fabric soaked in the S4 into a solidification solution, taking out the polyester base fabric, washing with water, drying, and rolling to obtain the PU synthetic leather, wherein the solidification solution comprises 20-25% of DMF.
By adopting the technical scheme, after the terylene base cloth is subjected to S1 acid treatment, the surface of the terylene fiber is primarily damaged to form obvious micro-holes; after the alkali treatment of S2, the surface of the polyester fiber is etched by strong alkali, the micro-hole grooves are deepened, and a plurality of micro-holes which are mutually penetrated are generated on the surface and inside of the fiber; through S3 hydrophilic modification, silk fibroin is coated on the surface of polyester fiber in a crosslinking way, on one hand, the crosslinking performance of silk fibroin and polyurethane is good, and silk fibroin contains a large number of hydrophilic groups, so that the hydrophilicity of the surface of the polyester fiber is improved, the impregnation effect of impregnation liquid is conveniently improved, the crosslinking reaction range is widened, the adhesion effect of a PU coating is further improved, on the other hand, the polyester base cloth is softer and more elastic after finishing, and the hand feeling of synthetic leather is closer to that of real leather; and (3) forming a PU coating on the surface of the terylene base cloth by S4 dipping and S5 solidification.
The invention is further configured to: the acid treatment solution comprises 8-10% of HCl and 6-9% of citric acid.
By adopting the technical scheme, carboxyl is grafted on micro-holes of the polyester fiber, so that a protection effect is achieved, and the trouble that the mechanical property of the fabric is reduced due to the damage of S2 alkali treatment on the internal structure of the polyester fiber is avoided; meanwhile, the silk fibroin is combined with the polyester fiber.
The invention is further configured to: the alkali treatment liquid comprises 6-8% of sodium hydroxide and 2-3% of sodium tert-butoxide.
By adopting the technical scheme, the sodium tert-butoxide has good modification effect on the surface of the polyester fiber, but is easy to damage the internal structure of the polyester fiber as organic strong base, and the etching degree of the polyester fiber is controlled due to the protection of acid groups.
The invention is further configured to: the alkali treatment liquid also comprises 0.8-1.6% of ethylenediamine.
By adopting the technical scheme, the alkali amine has a synergistic effect during alkali treatment, and is beneficial to promoting the formation of deeper cracks and grooves.
The invention is further configured to: the modified liquid also comprises 1-1.5% of amino silicone oil.
By adopting the technical scheme, the amino silicone oil has good hydrophilicity.
The invention is further configured to: the modifying solution also comprises 0.6-0.8% of cerium nitrate.
By adopting the technical scheme, the coordination relationship exists between cerium ions and silk fibroin, so that the stability of the silk fibroin can be improved, the compactness of the molecular arrangement of the silk fibroin coating layer can be improved, and the adhesion performance of the silk fibroin coating layer and the adhesion performance of the PU coating layer can be improved; the cerium ions and the amino silicone oil have a coordination relationship, so that the stability of the cerium ions and the amino silicone oil is improved.
The invention is further configured to: the modified liquid also comprises 0.2-0.4% of penetrating agent JFC.
By adopting the technical scheme, the polyester base cloth can be favorably soaked by the modified liquid.
The invention is further configured to: the preparation process of the PU impregnating solution is as follows:
firstly, mixing 22-28 parts of polypropylene oxide glycol and 26-30 parts of polyethylene glycol adipate-1, 4-butanediol glycol, heating to 100-105 ℃, and treating for 60-80 min;
secondly, adding 20-23 parts of IPDI, 3-4 parts of dimethylolpropionic acid and 0.2-0.4 part of dibutyl tin dilaurate, heating to 85-90 ℃, and reacting for 2-3 h;
thirdly, adding 2-3 parts of 1, 4-butanediol and 4-6 parts of N-methyl-2-pyrrolidone, reacting for 2-3 hours, cooling to 40-45 ℃, diluting with acetone during cooling, adding 2-3 parts of triethylamine, and uniformly stirring to obtain a polyurethane dispersion;
and fourthly, finally, adding 0.2-0.4 part of 15-20% PAMAM solution into the polyurethane dispersion, uniformly stirring, performing reduced pressure evaporation to remove acetone, and diluting with water to obtain the PU impregnation solution.
By adopting the technical scheme, on one hand, the raw material of the polyalcohol has good hydrophilicity, the formed waterborne polyurethane has good dispersion in water, can easily soak the hydrophilic modified polyester base fabric, and has tighter crosslinking with silk fibroin; on the other hand, the wear resistance of the PU coating is improved by introducing the polyamide-amine dendritic polymer into the molecular structure of the waterborne polyurethane and utilizing the structural advantages of the polyamide-amine dendritic polymer.
In conclusion, the invention has the following beneficial effects:
1. the silk fibroin is finished before the polyester base cloth is soaked in PU, so that the formed PU coating has good adhesive force, is not easy to peel and has long service life;
2. the cross-linking degree of silk fibroin and the terylene base cloth is improved by acid treatment and alkali treatment before silk fibroin finishing of the terylene base cloth;
and 3, the PU dipping solution has excellent performance, and the prepared synthetic leather has good mechanical performance and hand feeling and is close to real leather.
Drawings
Fig. 1 is a schematic flow chart of the first to third embodiments.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The first embodiment is as follows:
a production process of PU synthetic leather is shown in figure 1, and comprises the following steps:
s1 acid treatment: immersing the terylene base cloth into an acid treatment solution, wherein the bath ratio is 1:5, the temperature is 70 ℃, the treatment time is 15min, and then the terylene base cloth is dried in vacuum at 90 ℃, and the acid treatment solution comprises 8% of HCl, 6% of citric acid and the balance of water;
s2 alkali treatment: immersing the terylene base cloth subjected to S1 acid treatment in an alkali treatment solution, wherein the bath ratio is 1:10, the temperature is 75 ℃, the treatment time is 30min, after the treatment is finished, the terylene base cloth is washed by water and dried to constant weight, and the alkali treatment solution comprises 6% of sodium hydroxide, 2% of sodium tert-butoxide, 0.8% of ethylenediamine and the balance of water;
hydrophilic modification of S3: immersing the polyester base fabric subjected to the alkali treatment of S2 in a modifying solution, wherein the bath ratio is 1:10 at 25 ℃ for 80min, pre-drying at 75 ℃ for 10min after treatment, baking at 130 ℃ for 2min, washing with water, and drying, wherein the modification solution comprises 5% of silk fibroin, 1% of amino silicone oil, 0.6% of cerium nitrate, 0.2% of penetrating agent JFC, and the balance of water, and the pH value of the modification solution is 6.5;
s4 dipping: soaking the polyester base fabric subjected to hydrophilic modification by S3 in PU dipping solution at room temperature for 2min, and scraping off redundant slurry;
s5 solidification: and (3) immersing the polyester base fabric soaked in the S4 into a solidification solution, at the temperature of 25 ℃ for 15min, taking out, washing with water, drying and rolling to obtain the PU synthetic leather, wherein the solidification solution comprises 20% of DMF.
The preparation process of the PU impregnating solution is as follows:
firstly, mixing 22 parts of polypropylene oxide glycol and 26 parts of polyethylene glycol adipate-1, 4-butanediol glycol, heating to 100 ℃, and treating for 60 min;
secondly, adding 20 parts of IPDI, 3 parts of dimethylolpropionic acid and 0.2 part of dibutyl tin dilaurate, heating to 85 ℃, and reacting for 2 hours;
thirdly, adding 2 parts of 1, 4-butanediol and 4 parts of N-methyl-2-pyrrolidone, reacting for 2 hours, cooling to 40 ℃, diluting with acetone during cooling, adding 2 parts of triethylamine, and uniformly stirring to obtain a polyurethane dispersion;
and fourthly, finally, adding 0.2 part of 15% G1 PAMAM solution into the polyurethane dispersion, uniformly stirring, then carrying out reduced pressure evaporation to remove acetone, and then mixing the mixture according to the mass ratio of water to polyurethane of 5: 1 diluting to obtain PU dipping solution.
Example two:
a production process of PU synthetic leather is shown in figure 1, and comprises the following steps:
s1 acid treatment: immersing the terylene base cloth into an acid treatment solution, wherein the bath ratio is 1:5, the temperature is 80 ℃, the treatment time is 20min, and then the terylene base cloth is dried in vacuum at the temperature of 95 ℃, and the acid treatment solution comprises 10% of HCl, 9% of citric acid and the balance of water;
s2 alkali treatment: immersing the terylene base cloth subjected to S1 acid treatment in an alkali treatment solution, wherein the bath ratio is 1:10, the temperature is 85 ℃, the treatment time is 40min, after the treatment is finished, the terylene base cloth is washed by water and dried to constant weight, and the alkali treatment solution comprises 8% of sodium hydroxide, 3% of sodium tert-butoxide, 1.6% of ethylenediamine and the balance of water;
hydrophilic modification of S3: immersing the polyester base fabric subjected to the alkali treatment of S2 in a modifying solution, wherein the bath ratio is 1:10 at 35 ℃ for 100min, pre-drying at 75 ℃ for 10min after treatment, baking at 140 ℃ for 3min, washing with water, and drying, wherein the modification solution comprises 7% of silk fibroin, 1.5% of amino silicone oil, 0.8% of cerium nitrate, 0.4% of penetrating agent JFC, and the balance of water, and the pH value of the modification solution is 6.5;
s4 dipping: soaking the polyester base fabric subjected to hydrophilic modification by S3 in PU dipping solution at room temperature for 2min, and scraping off redundant slurry;
s5 solidification: and (3) immersing the polyester base fabric soaked in the S4 into a solidification solution, at the temperature of 25 ℃, for 15min, taking out, washing with water, drying, and rolling to obtain the PU synthetic leather, wherein the solidification solution comprises 25% of DMF.
The preparation process of the PU impregnating solution is as follows:
firstly, mixing 28 parts of polypropylene oxide glycol and 30 parts of polyethylene glycol adipate-1, 4-butanediol glycol, heating to 105 ℃, and treating for 80 min;
secondly, adding 23 parts of IPDI, 4 parts of dimethylolpropionic acid and 0.4 part of dibutyl tin dilaurate, heating to 90 ℃, and reacting for 3 hours;
thirdly, adding 3 parts of 1, 4-butanediol and 6 parts of N-methyl-2-pyrrolidone, reacting for 3 hours, cooling to 45 ℃, diluting with acetone during cooling, adding 3 parts of triethylamine, and uniformly stirring to obtain a polyurethane dispersion;
and fourthly, finally, adding 0.4 part of 20% G1 PAMAM solution into the polyurethane dispersion, uniformly stirring, performing reduced pressure evaporation to remove acetone, and then performing water/polyurethane mass ratio of (5): 1 diluting to obtain PU dipping solution.
Example three:
a production process of PU synthetic leather is shown in figure 1, and comprises the following steps:
s1 acid treatment: immersing the terylene base cloth into an acid treatment solution, wherein the bath ratio is 1:5, the temperature is 75 ℃, the treatment time is 18min, and then the terylene base cloth is dried in vacuum at the temperature of 92 ℃, and the acid treatment solution comprises 9% of HCl, 7% of citric acid and the balance of water;
s2 alkali treatment: immersing the terylene base cloth subjected to S1 acid treatment in an alkali treatment solution, wherein the bath ratio is 1:10, the temperature is 80 ℃, the treatment time is 35min, and after the treatment is finished, the terylene base cloth is washed and dried to constant weight, and the alkali treatment solution comprises 7% of sodium hydroxide, 2.5% of sodium tert-butoxide, 1.2% of ethylenediamine and the balance of water;
hydrophilic modification of S3: immersing the polyester base fabric subjected to the alkali treatment of S2 in a modifying solution, wherein the bath ratio is 1:10 at 30 ℃ for 90min, pre-drying at 75 ℃ for 10min after treatment, baking at 135 ℃ for 2.5min, washing with water, and drying, wherein the modification solution comprises 6% of silk fibroin, 1.2% of amino silicone oil, 0.7% of cerium nitrate, 0.3% of penetrating agent JFC, and the balance of water, and the pH value of the modification solution is 6.5;
s4 dipping: soaking the polyester base fabric subjected to hydrophilic modification by S3 in PU dipping solution at room temperature for 2min, and scraping off redundant slurry;
s5 solidification: and (3) immersing the polyester base fabric soaked in the S4 into a solidification solution, at the temperature of 25 ℃ for 15min, taking out, washing with water, drying and rolling to obtain the PU synthetic leather, wherein the solidification solution comprises 22% of DMF.
The preparation process of the PU impregnating solution is as follows:
firstly, mixing 25 parts of polypropylene oxide glycol and 28 parts of polyethylene glycol adipate-1, 4-butanediol glycol, heating to 103 ℃, and treating for 70 min;
secondly, adding 21 parts of IPDI, 3.5 parts of dimethylolpropionic acid and 0.3 part of dibutyl tin dilaurate, heating to 88 ℃, and reacting for 2.5 h;
thirdly, adding 2.5 parts of 1, 4-butanediol and 5 parts of N-methyl-2-pyrrolidone, reacting for 2.5 hours, cooling to 42 ℃, diluting with acetone during cooling, adding 2.5 parts of triethylamine, and uniformly stirring to obtain a polyurethane dispersion;
and fourthly, finally, adding 0.3 part of 18% G1 PAMAM substitute solution into the polyurethane dispersion, uniformly stirring, performing reduced pressure evaporation to remove acetone, and then performing water/polyurethane mass ratio of (5): 1 diluting to obtain PU dipping solution.
Example four:
the difference from the third example is that the modification liquid does not include cerium nitrate.
Example five:
the difference from the third example is that the modifying liquid does not include amino silicone oil.
Example six:
the difference from example three is that the alkali treatment solution does not include ethylenediamine.
Comparative example one:
the difference from example three is that the alkali treatment solution does not include sodium tert-butoxide.
Comparative example two:
the difference from example three is that the alkaline treatment solution does not include sodium tert-butoxide and ethylenediamine.
Comparative example three:
the difference from example three is that acid treatment of S1 and alkali treatment of S2 are not included.
Comparative example four:
the difference from the third example is that acid treatment of S1, alkali treatment of S2, and hydrophilic modification of S3 are not included.
Comparative example five:
the difference from the third example is that the sample is the common PU wet-process synthetic leather sold in the market.
And (3) performance testing:
according to the method recorded in QB/T5143-.
And (3) touch test: the synthetic leathers of examples one to three had the closest hand and appearance to the real leather.
Table 1 synthetic leather performance test result recording table
| Abrasion resistance/grade | Peeling load/N | |
| Example one | 0 | 60.7 |
| Example two | 0 | 58.2 |
| EXAMPLE III | 0 | 61.5 |
| Example four | 0 | 51.1 |
| EXAMPLE five | 0 | 55.9 |
| EXAMPLE six | 0 | 58.3 |
| Comparative example 1 | 0 | 51.6 |
| Comparative example No. two | 0 | 49.7 |
| Comparative example No. three | 1 | 34.5 |
| Comparative example No. four | 2 | 20.3 |
| Comparative example five | 2 | 16.5 |
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (2)
1. A production process of PU synthetic leather is characterized by comprising the following steps:
s1 acid treatment: immersing the terylene base cloth into an acid treatment solution, wherein the temperature is 70-80 ℃, the treatment time is 15-20min, and then the terylene base cloth is dried in vacuum at the temperature of 90-95 ℃, and the acid treatment solution comprises 8-10% of HCl and 6-9% of citric acid;
s2 alkali treatment: immersing the terylene base cloth subjected to S1 acid treatment in an alkali treatment solution, wherein the temperature is 75-85 ℃, the treatment time is 30-40min, and after the treatment is finished, the terylene base cloth is washed by water and dried to constant weight, and the alkali treatment solution comprises 6-8% of sodium hydroxide, 2-3% of sodium tert-butoxide and 0.8-1.6% of ethylenediamine;
hydrophilic modification of S3: immersing the terylene base cloth subjected to the alkali treatment of S2 in a modification solution at the temperature of 25-35 ℃ for 80-100min, pre-drying after the treatment, baking at the temperature of 130-140 ℃ for 2-3min, washing with water, and drying, wherein the modification solution comprises 5-7% of silk fibroin, 0.6-0.8% of cerium nitrate, and 1-1.5% of amino silicone oil;
s4 dipping: soaking the polyester base fabric subjected to hydrophilic modification by S3 into PU dipping solution, and scraping redundant slurry;
s5 solidification: soaking the polyester base fabric soaked in the S4 into a solidification solution, taking out the polyester base fabric, washing with water, drying, and rolling to obtain PU synthetic leather, wherein the solidification solution comprises 20-25% of DMF;
the preparation process of the PU impregnating solution is as follows:
firstly, mixing 22-28 parts of polypropylene oxide glycol and 26-30 parts of polyethylene glycol adipate-1, 4-butanediol glycol, heating to 100-105 ℃, and treating for 60-80 min;
secondly, adding 20-23 parts of IPDI, 3-4 parts of dimethylolpropionic acid and 0.2-0.4 part of dibutyl tin dilaurate, heating to 85-90 ℃, and reacting for 2-3 h;
thirdly, adding 2-3 parts of 1, 4-butanediol and 4-6 parts of N-methyl-2-pyrrolidone, reacting for 2-3 hours, cooling to 40-45 ℃, diluting with acetone during cooling, adding 2-3 parts of triethylamine, and uniformly stirring to obtain a polyurethane dispersion;
and fourthly, finally, adding 0.2-0.4 part of 15-20% PAMAM solution into the polyurethane dispersion, uniformly stirring, performing reduced pressure evaporation to remove acetone, and diluting with water to obtain the PU impregnation solution.
2. The production process of PU synthetic leather according to claim 1, characterized in that: the modified liquid also comprises 0.2-0.4% of penetrating agent JFC.
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| CN111793981A (en) * | 2020-07-10 | 2020-10-20 | 温州厚德服饰有限公司 | Moisture permeable cotton-padded clothes |
| CN111875770B (en) * | 2020-07-10 | 2022-06-10 | 温州厚德服饰有限公司 | Waterproof cotton-padded clothes |
| CN115787314B (en) * | 2022-11-04 | 2024-08-16 | 安徽安利材料科技股份有限公司 | High-durability water-based solvent-free double-color polyurethane synthetic leather and preparation method and application thereof |
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| GB1428873A (en) * | 1973-03-31 | 1976-03-17 | Kuraray Co | Production of simulated leather |
| WO2017012239A1 (en) * | 2015-07-22 | 2017-01-26 | 江苏国信复合材料科技股份有限公司 | Low voc polyurethane synthetic leatherand manufacturing method therefor |
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| CN1920162B (en) * | 2006-09-15 | 2010-04-07 | 浙江大学 | Method of coating polyester piece goods by silk fibroin combination liquid |
| CN102776602A (en) * | 2012-07-27 | 2012-11-14 | 烟台万华超纤股份有限公司 | Figured island superfine fiber, figured island superfine fiber synthetic leather base cloth, suede leather for clothes, smooth synthetic leather for clothes and production method of fiber, base cloth, suede leather and smooth synthetic leather |
| CN103774455A (en) * | 2012-10-15 | 2014-05-07 | 李翠平 | Water-based polyurethane superfine fiber synthetic leather and preparation method thereof |
| CN103087285B (en) * | 2013-01-24 | 2015-04-22 | 陕西科技大学 | Method for preparing solvent-free wet-process foaming polyurethane for synthetic leather and method for preparing synthetic leather by using solvent-free wet-process foaming polyurethane |
| CN107383315A (en) * | 2017-08-10 | 2017-11-24 | 山东泽辉新材料股份有限公司 | A kind of environment-friendly type waterborne polyurethane for synthetic leather and preparation method |
| CN108978179A (en) * | 2018-07-10 | 2018-12-11 | 安徽玉然经编科技有限公司 | A kind of plasma of dacron-chitosan base load silver-nano-titanium oxide antibacterial hydrophilic finiss technique |
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| GB1428873A (en) * | 1973-03-31 | 1976-03-17 | Kuraray Co | Production of simulated leather |
| WO2017012239A1 (en) * | 2015-07-22 | 2017-01-26 | 江苏国信复合材料科技股份有限公司 | Low voc polyurethane synthetic leatherand manufacturing method therefor |
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Denomination of invention: A kind of production process of PU synthetic leather Effective date of registration: 20220816 Granted publication date: 20220603 Pledgee: Taizhou Bank Co.,Ltd. Wenzhou Ouhai small and micro enterprise franchise sub branch Pledgor: Wenzhou Zhenjin Clothing Co.,Ltd. Registration number: Y2022330001761 |