CN114277582A - High-cold-resistance wear-resistant synthetic leather and preparation method thereof - Google Patents
High-cold-resistance wear-resistant synthetic leather and preparation method thereof Download PDFInfo
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- 239000002649 leather substitute Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 238000002156 mixing Methods 0.000 claims abstract description 54
- 239000002344 surface layer Substances 0.000 claims abstract description 53
- 239000011248 coating agent Substances 0.000 claims abstract description 51
- 238000000576 coating method Methods 0.000 claims abstract description 51
- 239000002131 composite material Substances 0.000 claims abstract description 48
- 238000005187 foaming Methods 0.000 claims abstract description 44
- 239000002002 slurry Substances 0.000 claims abstract description 43
- 238000003756 stirring Methods 0.000 claims abstract description 42
- 239000000839 emulsion Substances 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 34
- 239000010410 layer Substances 0.000 claims abstract description 33
- 239000004088 foaming agent Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 29
- 239000004744 fabric Substances 0.000 claims abstract description 26
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 239000002562 thickening agent Substances 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 239000000853 adhesive Substances 0.000 claims abstract description 15
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- 239000003381 stabilizer Substances 0.000 claims abstract description 11
- 239000006260 foam Substances 0.000 claims abstract description 10
- 241001518926 Cladrastis Species 0.000 claims abstract description 9
- 238000010409 ironing Methods 0.000 claims abstract description 9
- 238000005096 rolling process Methods 0.000 claims abstract description 9
- 235000007063 yellowwood Nutrition 0.000 claims abstract description 9
- 238000010030 laminating Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical class [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 27
- 239000004814 polyurethane Substances 0.000 claims description 24
- 239000002023 wood Substances 0.000 claims description 23
- 239000003995 emulsifying agent Substances 0.000 claims description 21
- 229920002635 polyurethane Polymers 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 18
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 14
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 14
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 239000002518 antifoaming agent Substances 0.000 claims description 8
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 7
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 235000013312 flour Nutrition 0.000 claims description 4
- 238000004513 sizing Methods 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 238000003825 pressing Methods 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000007761 roller coating Methods 0.000 abstract 1
- 238000005299 abrasion Methods 0.000 description 12
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- 239000010954 inorganic particle Substances 0.000 description 4
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
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- 239000003960 organic solvent Substances 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
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- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
Abstract
The invention discloses high cold-resistant wear-resistant synthetic leather and a preparation method thereof, wherein the preparation method comprises the following steps: mixing the PUA composite emulsion, the thickening agent, the foaming agent, the foam stabilizer and the modified yellow wood powder, uniformly stirring, and mechanically foaming to obtain foaming layer slurry; cleaning the base fabric, airing and ironing, blade-coating a layer of surface layer slurry on the surface of the base fabric through a blade coating machine, and drying in an oven to obtain the foaming bass; coating the surface layer slurry on the separation paper, and then putting the separation paper in an oven for drying to obtain a surface layer; and (3) roller-coating a layer of adhesive on the surface layer, baking for 2 minutes in an oven, laminating with the foaming base and rolling to obtain the high cold-resistant wear-resistant synthetic leather. The high cold-resistant and wear-resistant synthetic leather prepared by the invention has excellent wear resistance and folding resistance, can still maintain better folding resistance at low temperature, has excellent cold resistance and high economic benefit, and is suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of synthetic leather, and particularly relates to high-cold-resistance wear-resistant synthetic leather and a preparation method thereof.
Background
Synthetic leather is a plastic product that mimics the composition and structure of natural leather and can be used as a substitute material for natural leather. Synthetic leather is generally manufactured by taking impregnated non-woven fabric as a bottom layer and a microporous polyurethane layer as a surface layer, and has certain air permeability. With the development of the market, the requirements of people on synthetic leather are more and more strict, and the wear resistance and cold resistance of the existing synthetic leather can not meet the requirements.
Chinese patent CN110685166A discloses a cold-resistant wear-resistant synthetic leather, which comprises a coating liquid, wherein the coating liquid is prepared from the following components in parts by weight: 60% of waterborne polyurethane, 13% of light calcium carbonate, 3% -10% of foaming agent, 7% of foam stabilizer, 1% of graphene, 0.5% -10% of waterborne color paste, 0.5% -10% of leveling agent, 1% -2% of thickening agent and 1% -3% of cold-resistant agent. However, the cold-resistant and wear-resistant synthetic leather has poor cold-resistant effect by adding the cold-resistant agent.
Chinese CN102168387A discloses a high cold-resistant synthetic leather and a preparation method thereof, the synthetic leather is prepared by a calendering method by using high cold-resistant slurry, and the high cold-resistant slurry is prepared from the following components in parts by weight: 100 parts of PVC resin powder, 10-20 parts of TPU resin, 5-10 parts of cold-resistant agent, 40-60 parts of epoxidized soybean oil, 2-10 parts of color cake, 3-7 parts of stabilizer and foaming agent and 10-40 parts of superfine filler. However, the synthetic leather prepared by the patent has poor cold resistance and wear resistance.
Disclosure of Invention
In view of this, the invention provides a high cold-resistant wear-resistant synthetic leather and a preparation method thereof, so as to solve the technical problems.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of high cold-resistant wear-resistant synthetic leather comprises the following steps:
step S10, mixing 100 parts of PUA composite emulsion, 0.4-1.6 parts of thickening agent, 2.5-7.5 parts of foaming agent, 0.14-0.85 part of foam stabilizer and 1.2-2.4 parts of modified yellow wood powder, uniformly stirring, and mechanically foaming for 30 minutes to obtain foaming layer slurry;
step S20, uniformly mixing 10 to 30 parts of polyurethane, 0.12 to 0.82 part of thickening agent, 0.12 to 0.22 part of defoaming agent, 0.15 to 0.32 part of flatting agent and 3.5 to 15 parts of modified hydroxyapatite, performing centrifugal defoaming at the rotating speed of 2600 to 2800r/min for 5 minutes, and standing for 40 minutes to obtain surface layer slurry;
step S30, cleaning the base fabric, airing and ironing, blade-coating a layer of surface layer sizing agent on the surface of the base fabric through a blade coating machine, and controlling the coating weight to be 110g/m2～135g/m2Drying in an oven to obtain foamed shellS;
step S40, coating the surface layer slurry on the separation paper, and then putting the separation paper in an oven for drying to obtain a surface layer;
and S50, coating a layer of adhesive on the surface layer, baking the surface layer in an oven at 100 ℃ for 2 minutes, and then laminating and rolling the surface layer and the foamed base obtained in the S30 to obtain the high cold-resistant wear-resistant synthetic leather.
Further, in step S10, the preparation method of the PUA composite emulsion includes:
step i, stirring and mixing 10 parts of methyl methacrylate, 8-12 parts of butyl acrylate, 0.12-0.8 part of composite emulsifier and 40 parts of water, heating to 78-82 ℃, dropwise adding 1-5 parts of potassium persulfate aqueous solution, and carrying out constant temperature treatment for 45-70 minutes to obtain a premixed solution A;
step ii, mixing 2-12 parts of waterborne polyurethane emulsion, 15 parts of methyl methacrylate, 10-15 parts of butyl acrylate, 0.15-0.7 part of composite emulsifier and 20-40 parts of water, heating to 65-72 ℃, and continuously stirring and mixing for 30-50 minutes to obtain a premixed solution B;
and iii, dropwise adding the premixed liquid B obtained in the step ii, 1.5-3.5 parts of acrylic acid and 2-8 parts of potassium persulfate aqueous solution into the premixed liquid A at the temperature of 80 ℃, adjusting the pH value to be 4-5 after dropwise adding, carrying out heat preservation treatment for 2 hours, cooling to room temperature, and then carrying out filtration treatment to obtain the PUA composite emulsion.
Wherein, the properties of PU and PA are combined, the cold resistance and the organic solvent resistance of PU and the aging resistance and the water resistance of PA are exerted, and a composite emulsion with excellent water resistance, low-temperature film-forming property and strong adhesive force is synthesized; furthermore, the premix A is taken as a core, and the surface of the premix A is coated with a layer of aqueous polyurethane shell structure, so that the storage stability and the transparency of the composite emulsion are improved.
Further, in the step ii, the composite emulsifier is a mixture of sodium dodecyl benzene sulfonate and dodecyl phenol polyoxyethylene ether in a weight ratio of 1: 4-5.
Further, in step S10, the method for preparing the modified wood flour comprises: 50 parts of wood powder, 0.4-1.6 parts of silane coupling agent and 10-20 parts of diatomite are mixed, heated to 50-65 ℃, stirred and mixed for 20-30 minutes, dispersed at high speed, dried and crushed to 200 meshes to 500 meshes to obtain the modified wood powder. The wood flour is subjected to surface modification treatment by a silane coupling agent, so that the dispersibility of the wood flour in an organic phase and the binding force with the organic phase are improved.
Further, in step S10, the foaming agent is a mixture of a foaming agent ST and sodium lauryl sulfate mixed in a weight ratio of 3: 5; the foaming amount was adjusted to control the foaming ratio to about 150%. According to the foaming agent, the foaming pores are small in size and uniform in distribution by selecting and adjusting the weight and the proportion of the foaming agent, the specific surface area of the pores in the substrate is enhanced, and the permeability and the air permeability of the substrate are ensured.
Further, in step S20, the method for preparing modified hydroxyapatite includes: adding hydroxyapatite into water, heating and stirring in a water bath at 75-85 ℃ for 30 minutes, standing at the temperature of the water bath for 20 minutes, adding a octadecyl trimethyl ammonium chloride solution, stirring at a high speed for 1.5-2.5 hours, controlling the temperature of the water bath to be 78-82 ℃, carrying out suction filtration on a reaction solution, cleaning for 2-3 times, then placing a filter cake into an oven for drying for 24 hours, and grinding and crushing to obtain the modified hydroxyapatite.
The filler can reduce the cost and endow the synthetic leather with certain wear resistance while adjusting the microporous structure in the foaming layer. When hydroxyapatite is used as a filler, the number of the pores formed by foaming is large, the uniformity of the pores is high, the surface evenness of the membrane is high, the influence of the modified filler on the permeability of bass is small, and high water vapor permeability can be still ensured. The hydroxyapatite has higher chemical stability and wear resistance, but the problem of compatibility between the hydroxyapatite serving as an inorganic particle and a polymer matrix interface can cause the fracture of the inorganic particle and an organic interface due to lack of adhesive force, so that the mechanical property is influenced.
Further, in step S30, the drying process includes: the temperature is raised to 65 ℃, then raised to 95-105 ℃ at the heating rate of 0.5 ℃/min, and kept constant for 20-45 minutes. As described above.
In step S30, the thickness of the slurry applied to the base fabric is 0.4mm to 0.7 mm.
Further, in step S50, the pressure for bonding is controlled to 2.2kg/m2～4.5kg/m2。
The invention also aims to provide high cold-resistant and wear-resistant synthetic leather prepared by the preparation method.
The technical scheme can show that the invention has the advantages that:
1. the foaming layer of the high cold-resistant wear-resistant synthetic leather prepared by the invention uses the PUA composite emulsion, combines the properties of PU and PA, exerts the cold resistance and organic solvent resistance of PU and the aging resistance and water resistance of PA, and realizes the composite emulsion with excellent water resistance, low-temperature film forming property and strong adhesive force; the premixed liquid A is taken as a core, and a layer of shell structure of waterborne polyurethane is coated on the surface of the premixed liquid A, so that the storage stability and the transparency of the composite emulsion are improved;
2. the filler of the high cold-resistant wear-resistant synthetic leather prepared by the invention is modified hydroxyapatite which has higher chemical stability and wear resistance, but the problem of compatibility of the inorganic particles and the interface of a polymer matrix can cause the fracture of the inorganic particles and the organic interface due to lack of adhesive force, so that the mechanical property is influenced, the dispersibility of the synthetic leather in an organic phase and the compatibility of the synthetic leather with the organic phase are improved after organic modification treatment, and the internal adhesive force is greatly improved;
3. the high cold-resistant and wear-resistant synthetic leather prepared by the invention has excellent wear resistance and folding resistance, can still maintain better folding resistance at low temperature, has excellent cold resistance and high economic benefit, and is suitable for large-scale production.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below.
Detailed Description
The following detailed description of embodiments of the invention, but the invention can be practiced in many different ways, as defined and covered by the claims.
Example 1
High-cold-resistance wear-resistant synthetic leather and preparation method thereof
The preparation method of the high cold-resistant wear-resistant synthetic leather comprises the following steps:
step S10, mixing 100 parts of PUA composite emulsion, 0.4 part of thickening agent, 2.5 parts of foaming agent, 0.14 part of foam stabilizer and 1.2 parts of modified yellow wood powder, uniformly stirring, and mechanically foaming for 30 minutes to obtain foaming layer slurry; the foaming agent is a mixture of a foaming agent ST and sodium dodecyl sulfate which are mixed according to the weight ratio of 3:5, and the foaming amount is controlled to be 150 percent; the preparation method of the modified wood powder comprises the following steps: mixing 50 parts of wood powder, 0.4 part of silane coupling agent and 10 parts of diatomite, heating to 50 ℃, stirring and mixing for 20 minutes, dispersing at a high speed, drying and crushing to 200-mesh and 500-mesh to obtain modified wood powder;
step S20, uniformly mixing 10 parts of polyurethane, 0.12 part of thickening agent, 0.12 part of defoaming agent, 0.15 part of flatting agent and 3.5 parts of modified hydroxyapatite, performing centrifugal defoaming at the rotating speed of 2600r/min for 5 minutes, and standing for 40 minutes to obtain surface layer slurry; the preparation method of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into water, heating in a water bath at 75 ℃ and stirring for 30 minutes, standing at the temperature of 75 ℃ for 20 minutes, adding an octadecyl trimethyl ammonium chloride solution, stirring at a high speed for 1.5 hours, controlling the water bath temperature at 78 ℃, carrying out suction filtration on a reaction solution, cleaning for 2 times, then putting a filter cake into an oven, drying for 24 hours, and grinding and crushing to obtain modified hydroxyapatite;
step S30, cleaning the base fabric, airing and ironing, blade-coating a layer of surface layer slurry on the surface of the base fabric through a blade coating machine, wherein the blade-coating thickness of the slurry on the base fabric is 0.4mm, and the coating weight is controlled to be 110g/m2Then drying in an oven to obtain the foaming bass; the drying process comprises the following steps: firstly heating to 65 ℃, then heating to 95 ℃ at the heating rate of 0.5 ℃/min, and keeping the temperature for 20 minutes;
step S40, coating the surface layer slurry on the separation paper, and then putting the separation paper in an oven for drying to obtain a surface layer;
s50, coating a layer of adhesive on the surface layer, baking in an oven at 100 ℃ for 2 minutes, and mixing with the adhesive obtained in the step S30Bonding with foamed bass and rolling, and controlling bonding pressure at 2.2kg/m2And obtaining the high cold-resistant wear-resistant synthetic leather.
In step S10, the preparation method of the PUA composite emulsion includes:
step i, stirring and mixing 10 parts of methyl methacrylate, 8 parts of butyl acrylate, 0.12 part of composite emulsifier and 40 parts of water, heating to 78 ℃, dropwise adding 1 part of potassium persulfate aqueous solution, and carrying out constant-temperature treatment for 45 minutes to obtain a premixed solution A;
step ii, mixing 2 parts of waterborne polyurethane emulsion, 15 parts of methyl methacrylate, 10 parts of butyl acrylate, 0.15 part of composite emulsifier and 20 parts of water, heating to 65 ℃, and continuously stirring and mixing for 30 minutes to obtain a premixed solution B; the composite emulsifier is prepared by mixing sodium dodecyl benzene sulfonate and dodecyl phenol polyoxyethylene ether in a weight ratio of 1: 4;
and iii, dropwise adding the premixed liquid B obtained in the step ii, 1.5 parts of acrylic acid and 2 parts of a potassium persulfate aqueous solution into the premixed liquid A at the temperature of 80 ℃, adjusting the pH value to be 4-5 after dropwise adding, carrying out heat preservation treatment for 2 hours, cooling to room temperature, and carrying out filtration treatment to obtain the PUA composite emulsion.
The high cold-resistant wear-resistant synthetic leather prepared by the invention is subjected to performance test, the folding endurance at 25 ℃ is 5 grade, and the folding endurance at-40 ℃ is more than 1500 times; and a Taber abrasion resistance tester is used for testing, and the abrasion resistance is greater than 5000 turns.
Example 2
High-cold-resistance wear-resistant synthetic leather and preparation method thereof
The preparation method of the high cold-resistant wear-resistant synthetic leather comprises the following steps:
step S10, mixing 100 parts of PUA composite emulsion, 1.6 parts of thickening agent, 7.5 parts of foaming agent, 0.85 part of foam stabilizer and 2.4 parts of modified yellow wood powder, uniformly stirring, and mechanically foaming for 30 minutes to obtain foaming layer slurry; the foaming agent is a mixture of a foaming agent ST and sodium dodecyl sulfate in a weight ratio of 3: 5; the foaming amount is adjusted by controlling the foaming rate to be about 120 percent; the preparation method of the modified wood powder comprises the following steps: mixing 50 parts of wood powder, 1.6 parts of silane coupling agent and 20 parts of diatomite, heating to 65 ℃, stirring and mixing for 30 minutes, dispersing at a high speed, drying and crushing to 200-mesh and 500-mesh to obtain modified wood powder;
step S20, uniformly mixing 30 parts of polyurethane, 0.82 part of thickening agent, 0.22 part of defoaming agent, 0.32 part of flatting agent and 15 parts of modified hydroxyapatite, performing centrifugal defoaming at the rotating speed of 2800r/min for 5 minutes, and standing for 40 minutes to obtain surface layer slurry; the preparation method of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into water, heating in a water bath at 85 ℃ and stirring for 30 minutes, standing at the temperature of 85 ℃ for 20 minutes, adding a octadecyl trimethyl ammonium chloride solution, stirring at a high speed for 2.5 hours, controlling the temperature of the water bath at 82 ℃, carrying out suction filtration on a reaction solution, cleaning for 3 times, then putting a filter cake into an oven to dry for 24 hours, and grinding and crushing to obtain modified hydroxyapatite;
step S30, cleaning the base fabric, airing and ironing, blade-coating a layer of surface layer slurry on the surface of the base fabric through a blade coating machine, wherein the blade-coating thickness of the slurry on the base fabric is 0.7mm, and the coating weight is controlled to be 135g/m2Then drying in an oven to obtain the foaming bass; the drying process comprises the following steps: firstly heating to 65 ℃, then heating to 105 ℃ at the heating rate of 0.5 ℃/min, and keeping the temperature for 45 minutes;
step S40, coating the surface layer slurry on the separation paper, and then putting the separation paper in an oven for drying to obtain a surface layer;
s50, coating a layer of adhesive on the surface layer, baking in a baking oven at 100 ℃ for 2 minutes, bonding the surface layer with the foamed base obtained in the S30, and rolling, wherein the bonding pressure is controlled to be 4.5kg/m2And obtaining the high cold-resistant wear-resistant synthetic leather.
In step S10, the preparation method of the PUA composite emulsion includes:
step i, stirring and mixing 10 parts of methyl methacrylate, 12 parts of butyl acrylate, 0.8 part of composite emulsifier and 40 parts of water, heating to 82 ℃, dropwise adding 5 parts of potassium persulfate aqueous solution, and carrying out constant-temperature treatment for 70 minutes to obtain a premixed solution A;
step ii, mixing 12 parts of waterborne polyurethane emulsion, 15 parts of methyl methacrylate, 15 parts of butyl acrylate, 0.7 part of composite emulsifier and 40 parts of water, heating to 72 ℃, and continuously stirring and mixing for 50 minutes to obtain a premixed solution B; the composite emulsifier is prepared by mixing sodium dodecyl benzene sulfonate and dodecyl phenol polyoxyethylene ether in a weight ratio of 1: 5;
and iii, dropwise adding the premixed liquid B obtained in the step ii, 3.5 parts of acrylic acid and 8 parts of potassium persulfate aqueous solution into the premixed liquid A at the temperature of 80 ℃, adjusting the pH value to be 4-5 after dropwise adding, carrying out heat preservation treatment for 2 hours, cooling to room temperature, and carrying out filtration treatment to obtain the PUA composite emulsion.
The high cold-resistant wear-resistant synthetic leather prepared by the invention is subjected to performance test, the folding endurance at 25 ℃ is 5 grade, and the folding endurance at-40 ℃ is more than 1500 times; and a Taber abrasion resistance tester is used for testing, and the abrasion resistance is greater than 5000 turns.
Example 3
High-cold-resistance wear-resistant synthetic leather and preparation method thereof
The preparation method of the high cold-resistant wear-resistant synthetic leather comprises the following steps:
step S10, mixing 100 parts of PUA composite emulsion, 0.6 part of thickening agent, 6.5 parts of foaming agent, 0.7 part of foam stabilizer and 1.5 parts of modified yellow wood powder, uniformly stirring, and mechanically foaming for 30 minutes to obtain foaming layer slurry; the foaming agent is a mixture of a foaming agent ST and sodium dodecyl sulfate in a weight ratio of 3: 5; the foaming amount is adjusted by controlling the foaming rate to be about 150 percent; the preparation method of the modified wood powder comprises the following steps: mixing 50 parts of wood powder, 1.2 parts of silane coupling agent and 12 parts of diatomite, heating to 60 ℃, stirring and mixing for 28 minutes, dispersing at a high speed, drying and crushing to 200-mesh and 500-mesh to obtain modified wood powder;
step S20, uniformly mixing 15 parts of polyurethane, 0.25 part of thickening agent, 0.15 part of defoaming agent, 0.3 part of flatting agent and 12 parts of modified hydroxyapatite, carrying out centrifugal defoaming at the rotating speed of 2650r/min for 5 minutes, and standing for 40 minutes to obtain surface layer slurry; the preparation method of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into water, heating in a water bath at 77 ℃ and stirring for 30 minutes, standing at the temperature of 77 ℃ for 20 minutes, adding an octadecyl trimethyl ammonium chloride solution, stirring at a high speed for 2.0 hours, controlling the water bath temperature at 79 ℃, carrying out suction filtration on a reaction solution, cleaning for 3 times, then putting a filter cake into an oven to dry for 24 hours, and grinding and crushing to obtain modified hydroxyapatite;
step S30, cleaning the base fabric, airing and ironing, blade-coating a layer of surface layer slurry on the surface of the base fabric through a blade coating machine, wherein the blade-coating thickness of the slurry on the base fabric is 0.6mm, and the coating weight is controlled to be 130g/m2Then drying in an oven to obtain the foaming bass; the drying process comprises the following steps: firstly heating to 65 ℃, then heating to 102 ℃ at the heating rate of 0.5 ℃/min, and keeping the temperature for 40 minutes;
step S40, coating the surface layer slurry on the separation paper, and then putting the separation paper in an oven for drying to obtain a surface layer;
s50, coating a layer of adhesive on the surface layer, baking in a baking oven at 100 ℃ for 2 minutes, bonding the surface layer with the foamed base obtained in the S30, and rolling, wherein the bonding pressure is controlled to be 4.0kg/m2And obtaining the high cold-resistant wear-resistant synthetic leather.
In step S10, the preparation method of the PUA composite emulsion includes:
step i, stirring and mixing 10 parts of methyl methacrylate, 11 parts of butyl acrylate, 0.6 part of composite emulsifier and 40 parts of water, heating to 79 ℃, dropwise adding 4 parts of potassium persulfate aqueous solution, and carrying out constant-temperature treatment for 45-70 minutes to obtain a premixed solution A;
step ii, mixing 10 parts of waterborne polyurethane emulsion, 15 parts of methyl methacrylate, 14 parts of butyl acrylate, 0.25 part of composite emulsifier and 25 parts of water, heating to 70 ℃, and continuously stirring and mixing for 45 minutes to obtain a premixed solution B; the composite emulsifier is prepared by mixing sodium dodecyl benzene sulfonate and dodecyl phenol polyoxyethylene ether in a weight ratio of 1: 4.8;
and iii, dropwise adding the premixed liquid B obtained in the step ii, 3.0 parts of acrylic acid and 4 parts of potassium persulfate aqueous solution into the premixed liquid A at the temperature of 80 ℃, adjusting the pH value to be 4-5 after dropwise adding, carrying out heat preservation treatment for 2 hours, cooling to room temperature, and carrying out filtration treatment to obtain the PUA composite emulsion.
The high cold-resistant wear-resistant synthetic leather prepared by the invention is subjected to performance test, the folding endurance at 25 ℃ is 5 grade, and the folding endurance at-40 ℃ is more than 1500 times; and a Taber abrasion resistance tester is used for testing, and the abrasion resistance is greater than 5000 turns.
Example 4
High-cold-resistance wear-resistant synthetic leather and preparation method thereof
The preparation method of the high cold-resistant wear-resistant synthetic leather comprises the following steps:
step S10, mixing 100 parts of PUA composite emulsion, 1.0 part of thickening agent, 5 parts of foaming agent, 0.5 part of foam stabilizer and 1.8 parts of modified yellow wood powder, uniformly stirring, and mechanically foaming for 30 minutes to obtain foaming layer slurry; the foaming agent is a mixture of a foaming agent ST and sodium dodecyl sulfate in a weight ratio of 3: 5; the foaming amount is adjusted by controlling the foaming rate to be about 150 percent; the preparation method of the modified wood powder comprises the following steps: mixing 50 parts of wood powder, 1.0 part of silane coupling agent and 15 parts of diatomite, heating to 58 ℃, stirring and mixing for 25 minutes, dispersing at a high speed, drying and crushing to 200-mesh and 500-mesh to obtain modified wood powder;
step S20, uniformly mixing 20 parts of polyurethane, 0.5 part of thickening agent, 0.17 part of defoaming agent, 0.23 part of flatting agent and 9 parts of modified hydroxyapatite, centrifugally defoaming at the rotating speed of 2700r/min for 5 minutes, and standing for 40 minutes to obtain surface layer slurry; the preparation method of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into water, heating in a water bath at 80 ℃ and stirring for 30 minutes, standing at the temperature of 80 ℃ for 20 minutes, adding a octadecyl trimethyl ammonium chloride solution, stirring at a high speed for 2.0 hours, controlling the water bath temperature at 80 ℃, carrying out suction filtration on a reaction solution, cleaning for 3 times, then putting a filter cake into an oven to dry for 24 hours, and grinding and crushing to obtain modified hydroxyapatite;
step S30, cleaning the base fabric, airing and ironing, blade-coating a layer of surface layer slurry on the surface of the base fabric through a blade coating machine, wherein the blade-coating thickness of the slurry on the base fabric is 0.6mm, and the coating weight is controlled to be 120g/m2Then drying in an oven to obtain the foaming bass; the drying process comprises the following steps: firstly heating to 65 ℃, then heating to 10 ℃ at the heating rate of 0.5 ℃/min, and keeping the temperature for 35 minutes;
step S40, coating the surface layer slurry on the separation paper, and then putting the separation paper in an oven for drying to obtain a surface layer;
s50, coating a layer of adhesive on the surface layer, baking in an oven at 100 ℃ for 2 minutes, bonding with the foamed base obtained in the S30, rolling, and adheringThe resultant pressure was controlled to 3.2kg/m2And obtaining the high cold-resistant wear-resistant synthetic leather.
In step S10, the preparation method of the PUA composite emulsion includes:
step i, stirring and mixing 10 parts of methyl methacrylate, 10 parts of butyl acrylate, 0.46 part of composite emulsifier and 40 parts of water, heating to 80 ℃, dropwise adding 3 parts of potassium persulfate aqueous solution, and carrying out constant-temperature treatment for 55 minutes to obtain a premixed solution A;
step ii, mixing 7 parts of waterborne polyurethane emulsion, 15 parts of methyl methacrylate, 12 parts of butyl acrylate, 0.42 part of composite emulsifier and 30 parts of water, heating to 68 ℃, and continuously stirring and mixing for 40 minutes to obtain a premixed solution B; the composite emulsifier is prepared by mixing sodium dodecyl benzene sulfonate and dodecyl phenol polyoxyethylene ether in a weight ratio of 1: 4.5;
and iii, dropwise adding the premixed liquid B obtained in the step ii, 2.5 parts of acrylic acid and 5 parts of potassium persulfate aqueous solution into the premixed liquid A at the temperature of 80 ℃, adjusting the pH value to be 4-5 after dropwise adding, carrying out heat preservation treatment for 2 hours, cooling to room temperature, and carrying out filtration treatment to obtain the PUA composite emulsion.
The high cold-resistant wear-resistant synthetic leather prepared by the invention is subjected to performance test, the folding endurance at 25 ℃ is 5 grade, and the folding endurance at-40 ℃ is more than 1500 times; and a Taber abrasion resistance tester is used for testing, and the abrasion resistance is greater than 5000 turns.
Comparative example 1
High-cold-resistance wear-resistant synthetic leather and preparation method thereof
The preparation method of the high cold-resistant wear-resistant synthetic leather comprises the following steps:
step S10, mixing 100 parts of polyurethane emulsion, 1.0 part of thickening agent, 5 parts of foaming agent, 0.5 part of foam stabilizer and 1.8 parts of modified yellow wood powder, uniformly stirring, and mechanically foaming for 30 minutes to obtain foaming layer slurry; the foaming agent is a mixture of a foaming agent ST and sodium dodecyl sulfate in a weight ratio of 3: 5; the foaming amount is adjusted by controlling the foaming rate to be about 150 percent; the preparation method of the modified wood powder comprises the following steps: mixing 50 parts of wood powder, 1.0 part of silane coupling agent and 15 parts of diatomite, heating to 58 ℃, stirring and mixing for 25 minutes, dispersing at a high speed, drying and crushing to 200-mesh and 500-mesh to obtain modified wood powder;
step S20, uniformly mixing 20 parts of polyurethane, 0.5 part of thickening agent, 0.17 part of defoaming agent, 0.23 part of flatting agent and 9 parts of modified hydroxyapatite, centrifugally defoaming at the rotating speed of 2700r/min for 5 minutes, and standing for 40 minutes to obtain surface layer slurry; the preparation method of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into water, heating in a water bath at 80 ℃ and stirring for 30 minutes, standing at the temperature of 80 ℃ for 20 minutes, adding a octadecyl trimethyl ammonium chloride solution, stirring at a high speed for 2.0 hours, controlling the water bath temperature at 80 ℃, carrying out suction filtration on a reaction solution, cleaning for 3 times, then putting a filter cake into an oven to dry for 24 hours, and grinding and crushing to obtain modified hydroxyapatite;
step S30, cleaning the base fabric, airing and ironing, blade-coating a layer of surface layer slurry on the surface of the base fabric through a blade coating machine, wherein the blade-coating thickness of the slurry on the base fabric is 0.6mm, and the coating weight is controlled to be 120g/m2Then drying in an oven to obtain the foaming bass; the drying process comprises the following steps: firstly heating to 65 ℃, then heating to 10 ℃ at the heating rate of 0.5 ℃/min, and keeping the temperature for 35 minutes;
step S40, coating the surface layer slurry on the separation paper, and then putting the separation paper in an oven for drying to obtain a surface layer;
s50, coating a layer of adhesive on the surface layer, baking in a baking oven at 100 ℃ for 2 minutes, bonding the surface layer with the foamed base obtained in the S30, and rolling, wherein the bonding pressure is controlled to be 3.2kg/m2And obtaining the high cold-resistant wear-resistant synthetic leather.
The high cold-resistant wear-resistant synthetic leather prepared by the invention is subjected to performance test, the folding endurance at 25 ℃ is 4 grade, and the folding endurance at-40 ℃ is 1200 times; and a Taber abrasion resistance tester is used for testing, and the abrasion resistance is greater than 5000 turns.
Comparative example 2
High-cold-resistance wear-resistant synthetic leather and preparation method thereof
The preparation method of the high cold-resistant wear-resistant synthetic leather comprises the following steps:
step S10, mixing 100 parts of PUA composite emulsion, 1.0 part of thickening agent, 5 parts of foaming agent, 0.5 part of foam stabilizer and 1.8 parts of yellow wood powder, uniformly stirring, and mechanically foaming for 30 minutes to obtain foaming layer slurry; the foaming agent is a mixture of a foaming agent ST and sodium dodecyl sulfate in a weight ratio of 3: 5; the foaming amount is adjusted by controlling the foaming rate to be about 150 percent;
step S20, uniformly mixing 20 parts of polyurethane, 0.5 part of thickening agent, 0.17 part of defoaming agent, 0.23 part of flatting agent and 9 parts of hydroxyapatite, centrifugally defoaming at the rotating speed of 2700r/min for 5 minutes, and standing for 40 minutes to obtain surface layer slurry;
step S30, cleaning the base fabric, airing and ironing, blade-coating a layer of surface layer slurry on the surface of the base fabric through a blade coating machine, wherein the blade-coating thickness of the slurry on the base fabric is 0.6mm, and the coating weight is controlled to be 120g/m2Then drying in an oven to obtain the foaming bass; the drying process comprises the following steps: firstly heating to 65 ℃, then heating to 10 ℃ at the heating rate of 0.5 ℃/min, and keeping the temperature for 35 minutes;
step S40, coating the surface layer slurry on the separation paper, and then putting the separation paper in an oven for drying to obtain a surface layer;
s50, coating a layer of adhesive on the surface layer, baking in a baking oven at 100 ℃ for 2 minutes, bonding the surface layer with the foamed base obtained in the S30, and rolling, wherein the bonding pressure is controlled to be 3.2kg/m2And obtaining the high cold-resistant wear-resistant synthetic leather.
In step S10, the preparation method of the PUA composite emulsion includes:
step i, stirring and mixing 10 parts of methyl methacrylate, 10 parts of butyl acrylate, 0.46 part of composite emulsifier and 40 parts of water, heating to 80 ℃, dropwise adding 3 parts of potassium persulfate aqueous solution, and carrying out constant-temperature treatment for 55 minutes to obtain a premixed solution A;
step ii, mixing 7 parts of waterborne polyurethane emulsion, 15 parts of methyl methacrylate, 12 parts of butyl acrylate, 0.42 part of composite emulsifier and 30 parts of water, heating to 68 ℃, and continuously stirring and mixing for 40 minutes to obtain a premixed solution B; the composite emulsifier is prepared by mixing sodium dodecyl benzene sulfonate and dodecyl phenol polyoxyethylene ether in a weight ratio of 1: 4.5;
and iii, dropwise adding the premixed liquid B obtained in the step ii, 2.5 parts of acrylic acid and 5 parts of potassium persulfate aqueous solution into the premixed liquid A at the temperature of 80 ℃, adjusting the pH value to be 4-5 after dropwise adding, carrying out heat preservation treatment for 2 hours, cooling to room temperature, and carrying out filtration treatment to obtain the PUA composite emulsion.
The high cold-resistant wear-resistant synthetic leather prepared by the invention is subjected to performance test, the folding endurance at 25 ℃ is 4 grade, and the folding endurance times at-40 ℃ are 1300 times; the abrasion resistance was 3200 revolutions using a Taber abrasion tester.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the high cold-resistant wear-resistant synthetic leather is characterized by comprising the following steps:
step S10, mixing 100 parts of PUA composite emulsion, 0.4-1.6 parts of thickening agent, 2.5-7.5 parts of foaming agent, 0.14-0.85 part of foam stabilizer and 1.2-2.4 parts of modified yellow wood powder, uniformly stirring, and mechanically foaming for 30 minutes to obtain foaming layer slurry;
step S20, evenly mixing 10 to 30 parts of polyurethane, 0.12 to 0.82 part of thickening agent, 0.12 to 0.22 part of defoaming agent, 0.15 to 0.32 part of flatting agent and 3.5 to 15 parts of modified hydroxyapatite, then centrifugally defoaming at the rotating speed of 2600 to 2800r/min for 5 minutes, and standing for 40 minutes to obtain surface layer slurry;
step S30, cleaning the base fabric, airing and ironing, blade-coating a layer of surface layer sizing agent on the surface of the base fabric through a blade coating machine, and controlling the coating weight to be 110g/m2～135g/m2Then drying in an oven to obtain the foaming bass;
step S40, coating the surface layer slurry on the separation paper, and then putting the separation paper in an oven for drying to obtain a surface layer;
and S50, coating a layer of adhesive on the surface layer, baking the surface layer in an oven at 100 ℃ for 2 minutes, and then laminating and rolling the surface layer and the foamed base obtained in the S30 to obtain the high cold-resistant wear-resistant synthetic leather.
2. The method according to claim 1, wherein in step S10, the PUA composite emulsion is prepared by a method comprising:
step i, stirring and mixing 10 parts of methyl methacrylate, 8-12 parts of butyl acrylate, 0.12-0.8 part of composite emulsifier and 40 parts of water, heating to 78-82 ℃, dropwise adding 1-5 parts of potassium persulfate aqueous solution, and carrying out constant temperature treatment for 45-70 minutes to obtain a premixed solution A;
step ii, mixing 2 to 12 parts of aqueous polyurethane emulsion, 15 parts of methyl methacrylate, 10 to 15 parts of butyl acrylate, 0.15 to 0.7 part of composite emulsifier and 20 to 40 parts of water, heating to 65 to 72 ℃, and continuously stirring and mixing for 30 to 50 minutes to obtain a premixed solution B;
and iii, dropwise adding the premixed liquid B obtained in the step ii, 1.5-3.5 parts of acrylic acid and 2-8 parts of potassium persulfate aqueous solution into the premixed liquid A at the temperature of 80 ℃, adjusting the pH value to be 4-5 after dropwise adding, carrying out heat preservation treatment for 2 hours, cooling to room temperature, and carrying out filtration treatment to obtain the PUA composite emulsion.
3. The preparation method of claim 1, wherein in the step ii, the composite emulsifier is a mixture of sodium dodecyl benzene sulfonate and dodecyl phenol polyoxyethylene ether in a weight ratio of 1: 4-5.
4. The method of claim 1, wherein the modified wood flour is prepared by the method of step S10, comprising: 50 parts of wood powder, 0.4-1.6 parts of silane coupling agent and 10-20 parts of diatomite are mixed, heated to 50-65 ℃, stirred and mixed for 20-30 minutes, dispersed at high speed, dried and crushed to 200 meshes to 500 meshes to obtain the modified wood powder.
5. The method according to claim 1, wherein in step S10, the foaming agent is a mixture of a foaming agent ST and sodium lauryl sulfate mixed in a weight ratio of 3: 5.
6. The method according to claim 1, wherein in step S20, the method for preparing the modified hydroxyapatite comprises: adding hydroxyapatite into water, heating and stirring in a water bath at 75-85 ℃ for 30 minutes, standing at the temperature of the water bath for 20 minutes, adding a octadecyl trimethyl ammonium chloride solution, stirring at a high speed for 1.5-2.5 hours, controlling the temperature of the water bath to be 78-82 ℃, carrying out suction filtration on reaction liquid, cleaning for 2-3 times, then putting a filter cake into an oven, drying for 24 hours, and grinding and crushing to obtain the modified hydroxyapatite.
7. The method according to claim 1, wherein in step S30, the drying process is: the temperature is raised to 65 ℃, then raised to 95-105 ℃ at the heating rate of 0.5 ℃/min, and kept constant for 20-45 minutes. The method is as follows.
8. The method according to claim 1, wherein in step S30, the thickness of the slurry applied on the base fabric is 0.4mm to 0.7 mm.
9. The method of claim 1, wherein in step S50, the applying pressure is controlled to 2.2kg/m2～4.5kg/m2。
10. High cold-resistant wear-resistant synthetic leather prepared by the preparation method of any one of claims 1 to 9.
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