CN114016301A - PVC wear-resistant leather and preparation method thereof - Google Patents
PVC wear-resistant leather and preparation method thereof Download PDFInfo
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- CN114016301A CN114016301A CN202111198802.4A CN202111198802A CN114016301A CN 114016301 A CN114016301 A CN 114016301A CN 202111198802 A CN202111198802 A CN 202111198802A CN 114016301 A CN114016301 A CN 114016301A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—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 by reactions only involving carbon-to-carbon unsaturated bonds
- D06N3/06—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 by reactions only involving carbon-to-carbon unsaturated bonds with polyvinylchloride or its copolymerisation products
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
- D06N3/005—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers obtained by blowing or swelling agent
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0061—Organic fillers or organic fibrous fillers, e.g. ground leather waste, wood bark, cork powder, vegetable flour; Other organic compounding ingredients; Post-treatment with organic compounds
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
- D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
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- D06N2209/04—Properties of the materials having electrical or magnetic properties
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- D06N2209/00—Properties of the materials
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- D06N2211/00—Specially adapted uses
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Abstract
The invention discloses a PVC wear-resistant leather and a preparation method thereof, wherein the PVC wear-resistant leather comprises the following raw materials in parts by weight: 50-70 parts of PVC resin, 1-3 parts of methyl triethyl silicane, 10-20 parts of epoxidized soybean oil, 1-5 parts of polyurethane, 2-4 parts of tributyl citrate, 10-15 parts of modified alumina, 3-7 parts of silicon carbide, 1-3 parts of antistatic agent, 5-8 parts of wear-resistant agent and 1-5 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder, and the components of the raw materials are matched in a synergistic manner, and the preparation method is combined, so that compared with the common PVC leather, the PVC leather finally prepared by the invention is soft in hand feeling, excellent in wear resistance and aging resistance, simple in preparation method, easy to operate, safe and environment-friendly.
Description
Technical Field
The invention relates to the technical field of leather processing, in particular to PVC (polyvinyl chloride) wear-resistant leather and a preparation method thereof.
Background
Leather is mainly used for automobile seat surfaces, armrest surfaces and the like in automobile interior trim, and leather covers the outer surfaces of instrument panels, steering wheels, inner walls of compartments and the like of some high-grade automobiles. Leather used in automotive interiors is mainly divided into genuine leather, artificial leather, furs; compared with the artificial leather made of chemical fiber materials, the inner decoration made of the leather material has soft hand feeling, smoothness and flatness and excellent tensile strength, and is mainly used in high-grade luxury automobile models. Artificial leather including PVC leather, PU leather, microfiber PU leather, etc. is an industrial product produced by coating different fiber fabrics with different coating materials. Among them, polyvinyl chloride (PVC) leather, as an artificial leather used in the largest amount at present, is similar to natural leather, has product performances such as soft hand feeling and wear resistance, and is highly popular with consumers. At present, the PVC automobile interior leather has poor wear resistance and short service life, and is easy to soften, harden and embrittle.
Chinese patent CN106582258A discloses a wear-resistant PVC decorative artificial leather, which is prepared by calendering wear-resistant PVC slurry, wherein the wear-resistant PVC slurry is prepared from the following components in parts by weight: 112-116 PVC resin powder, 30-35 modified epoxidized soybean oil, 4-6 color cakes, 1-3 stabilizers, 1-5 foaming agents, 18-24 modified pitchstone and 5-7 camphorwood powder. This patent is through the synergism of modified pitchstone with the camphorwood powder through handling, can very big improvement synthetic leather's wear resistance to its wearability can not descend along with the time increase, very big improvement life. The oil resistance of the artificial leather can be greatly improved by modifying epoxidized soybean oil and pitchstone, and the problem of poor oil resistance of the traditional artificial leather is solved. However, the direct addition of pitchstone to the PVC slurry results in a decrease in the softness and resistance to bending of the leather product.
Chinese patent CN108112846A discloses a high-strength wear-resistant coated PVC artificial leather, which comprises a base cloth layer, an intermediate layer and a PVC surface layer, wherein the base cloth layer and the intermediate layer are bonded through an adhesive layer, the intermediate layer is a reinforcing agent layer, a PVC foaming layer is coated on the intermediate layer, and the PVC surface layer is formed after drying at 180-180 ℃; coating a film coating agent on the PVC surface layer to form a coating layer; the coating agent is prepared from the following components in parts by weight: 3-10 parts of silicone oil emulsion, 10-15 parts of film-forming resin, 0.5-2 parts of dispersing agent, 0.7-1.5 parts of antioxidant, 5-10 parts of graphene and 1-3 parts of stabilizer. According to the coating, a coating layer is formed by coating a water-based coating agent on a PVC surface layer, and the coating agent is sprayed on the surface of genuine leather in the using process, so that a flexible and transparent coating layer can be formed on the surface of the genuine leather. The graphene is added into the film coating agent as a modifier, so that the strength and the wear resistance of the PVC leather are greatly improved. However, the coating layer is adopted to treat the PVC surface to form a protective layer on the PVC surface, but the method can only indirectly solve the wear-resisting problem of the PVC leather in a short time and cannot fundamentally solve the defect of poor wear resistance of the PVC leather, and the wear-resisting protective layer formed by the coating agent gradually loses efficacy along with the time, so that the PVC leather or the genuine leather is directly abraded.
Disclosure of Invention
In view of the above, the present invention provides a PVC wear-resistant leather and a preparation method thereof, so as to solve the above technical problems.
The invention provides the following technical scheme:
the PVC wear-resistant leather comprises the following raw materials in parts by weight: 50-70 parts of PVC resin, 1-3 parts of methyl triethyl silicane, 10-20 parts of epoxidized soybean oil, 1-5 parts of polyurethane, 2-4 parts of tributyl citrate, 10-15 parts of modified alumina, 3-7 parts of silicon carbide, 1-3 parts of antistatic agent, 5-8 parts of wear-resistant agent and 1-5 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
Preferably, the PVC wear-resistant leather comprises the following raw materials in parts by weight: 55 to 68 parts of PVC resin, 1.5 to 2.5 parts of methyl triethyl silicane, 12 to 18 parts of epoxidized soybean oil, 1.5 to 4 parts of polyurethane, 2.5 to 3.5 parts of tributyl citrate, 12 to 14 parts of modified alumina, 4 to 6 parts of silicon carbide, 1.2 to 2.5 parts of antistatic agent, 6 to 7.5 parts of wear-resistant agent and 2 to 4 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
More preferably, the PVC wear-resistant leather comprises the following raw materials in parts by weight: 60 parts of PVC resin, 2 parts of methyl triethyl silane, 17 parts of epoxidized soybean oil, 3 parts of polyurethane, 2 parts of tributyl citrate, 15 parts of modified alumina, 5 parts of silicon carbide, 2 parts of antistatic agent, 5 parts of wear-resisting agent and 3 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
Preferably, the preparation of the modified alumina comprises the following steps:
s1, transferring alumina into a pulverizer to be ground into alumina powder with the average grain diameter of 40 mu m, adding the alumina powder into absolute ethyl alcohol, ultrasonically stirring until the alumina powder is uniformly dispersed, then sequentially adding magnesium aluminate and an ammonia water solution, ultrasonically dispersing uniformly, adding a polyethylene glycol solution, stirring to react until gel appears, continuously stirring until the gel is completely dispersed, taking out and filtering, repeatedly washing with absolute ethyl alcohol, placing in an oven to dry to constant weight, transferring into a sintering furnace to roast, taking out and cooling to obtain pretreated alumina;
s2, adding the pretreated aluminum oxide obtained in the step (2) into deionized water, placing the mixture in a constant-temperature water bath, stirring the mixture for 30-50 min at a constant temperature of 80-80 ℃, adding a modifier, adjusting the pH value to 8-8 by using ammonia water, heating the mixture to 110 ℃, stirring the mixture for 50-80 min at a constant temperature of 400-600 r/min, precipitating and filtering the mixture, taking out the mixture, cooling the mixture to room temperature, repeatedly washing the mixture by using absolute ethyl alcohol, then placing the mixture in a drying oven, and drying the mixture for 3-5 h at 110 ℃ to obtain the modified aluminum oxide.
More preferably, in S1, the concentration of the aqueous ammonia solution is 10%; the concentration of the polyethylene glycol solution is 10%.
More preferably, in S1, the temperature of the oven is 100 ℃; the roasting temperature is 700-800 ℃, and the roasting time is 5-7 h.
More preferably, in S2, the preparation of the modifier comprises the steps of: adding liquid butyl titanate into deionized water, and stirring and mixing at the rotating speed of 200r/min to obtain a white butyl titanate suspension; adding liquid dodecyl dimethyl betaine into deionized water, and stirring and mixing at a rotating speed of 100r/min to obtain dodecyl dimethyl betaine solution; mixing the butyl titanate white suspension with dodecyl dimethyl betaine solution, adding 1, 2-propylene glycol, stirring and mixing for 1-2 h, then heating to 70-80 ℃, continuing stirring for 2-3.5 h, and distilling under reduced pressure to obtain the modifier.
More preferably, the volume ratio of the liquid butyl titanate to the deionized water is 0.04-0.35: 1; the density of the liquid butyl titanate is 0.866g/cm3(ii) a The volume ratio of the liquid dodecyl dimethyl betaine to the deionized water is 0.002-0.05: 1; the density of the liquid dodecyl dimethyl betaine is 0.56g/cm3。
More preferably, the volume ratio of the butyl titanate white suspension to the dodecyl dimethyl betaine solution to the 1, 2-propylene glycol is 1: 0.01-0.25: 15-20.
The invention also aims to provide a preparation method of the PVC wear-resistant leather, which comprises the following steps:
mixing the modified aluminum oxide, the silicon carbide, the antistatic agent and the wear-resisting agent in parts by weight, and fully grinding to obtain a mixture; kneading the PVC resin, the methyltriethylsilane, the polyurethane, the tributyl citrate, the foaming agent and the mixture in parts by weight at a high speed at 100-110 ℃, adding the epoxidized soybean oil in parts by weight, stirring at a high speed, uniformly mixing, and banburying at 150-170 ℃ to obtain the wear-resistant PVC slurry; and (3) laminating the obtained wear-resistant PVC slurry on a base fabric through a calender, then carrying out foaming embossing treatment, and standing and cooling to obtain the PVC wear-resistant leather.
According to the technical scheme, the invention has the beneficial effects that:
(1) according to the invention, the modified aluminum oxide, the silicon carbide and the wear-resistant agent polyvinyl chloride powder are compounded for use, so that the wear resistance of the PVC leather is obviously improved, the wear resistance of the PVC leather is not reduced along with the lapse of time, the service life of the PVC leather is prolonged, and the softness and the bending strength of the PVC leather are not reduced. The modified aluminum oxide is modified to be uniformly dispersed in the wear-resistant PVC slurry, the modified aluminum oxide is a modifier prepared by complexing dodecyl dimethyl betaine and butyl titanate, the dispersion uniformity and stability of the aluminum oxide can be improved, long-chain carboxyl in the modifier is combined with a PVC matrix, and the modified aluminum oxide powder can migrate to offset friction load and reduce friction damage when the PVC leather is subjected to external friction force, so that the wear resistance of the PVC leather is greatly improved, the heat resistance of the aluminum oxide powder is good, and the aging resistance of the PVC leather can be effectively improved. The epoxidized soybean oil has good compatibility with PVC, has obvious improvement effect on PVC performance, and can improve the tensile strength, thermal stability and aging resistance of the product.
(2) According to the invention, by combining the synergistic cooperation of the raw materials and the preparation method, compared with common PVC leather, the PVC leather finally prepared by the invention has soft hand feeling, excellent wear resistance and aging resistance, simple preparation method, easy operation, safety and environmental protection.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. The exemplary embodiments and descriptions of the present invention are provided to explain the present invention, but not to limit the present invention.
Example 1
PVC wear-resistant leather and preparation method thereof
The PVC wear-resistant leather comprises the following raw materials in parts by weight: 50 parts of PVC resin, 1 part of methyl triethyl silicane, 10 parts of epoxidized soybean oil, 1 part of polyurethane, 2 parts of tributyl citrate, 10 parts of modified alumina, 3 parts of silicon carbide, 1 part of antistatic agent, 5-8 parts of wear-resisting agent and 1-5 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
The preparation of the modified alumina comprises the following steps:
s1, transferring alumina into a pulverizer to be ground into alumina powder with the average grain diameter of 40 microns, adding the alumina powder into absolute ethyl alcohol, ultrasonically stirring until the alumina powder is uniformly dispersed, then sequentially adding magnesium aluminate and 10% ammonia water solution, ultrasonically dispersing uniformly, adding 10% polyethylene glycol solution, stirring to react until gel appears, continuously stirring until the gel is complete, taking out and filtering, repeatedly washing with absolute ethyl alcohol, drying in an oven at 100 ℃ to constant weight, transferring into a sintering furnace at 700 ℃ to roast for 7 hours, taking out and cooling to obtain pretreated alumina;
s2, adding the pretreated aluminum oxide obtained in the step (2) into deionized water, placing the mixture in a constant-temperature water bath, stirring the mixture for 30min at a constant temperature of 80 ℃, adding a modifier, adjusting the pH value to 8 by using ammonia water, heating the mixture to 110 ℃, stirring the mixture for 50min at a constant temperature of 400r/min, precipitating and filtering the mixture, taking the mixture out, cooling the mixture to room temperature, repeatedly washing the mixture by using absolute ethyl alcohol, then placing the mixture in an oven, and drying the mixture for 3h at 110 ℃ to obtain the modified aluminum oxide.
S2, the preparation of the modifier comprises the following steps: adding liquid butyl titanate into deionized water, and stirring and mixing at the rotating speed of 200r/min to obtain a white butyl titanate suspension; adding liquid dodecyl dimethyl betaine into deionized water, and stirring and mixing at a rotating speed of 100r/min to obtain dodecyl dimethyl betaine solution; and (2) mixing the butyl titanate white suspension with dodecyl dimethyl betaine solution, adding 1, 2-propylene glycol, stirring and mixing for 1h, heating to 70 ℃, continuously stirring for 2h, and distilling under reduced pressure to obtain the modifier.
The volume ratio of the liquid butyl titanate to the deionized water is 0.04: 1; the density of the liquid butyl titanate is 0.866g/cm3(ii) a The volume ratio of the liquid dodecyl dimethyl betaine to the deionized water is 0.002: 1; the density of the liquid dodecyl dimethyl betaine is 0.56g/cm3. The volume ratio of the butyl titanate white suspension to the dodecyl dimethyl betaine solution to the 1, 2-propylene glycol is 1:0.01: 15.
The preparation method of the PVC wear-resistant leather comprises the following steps:
mixing the modified aluminum oxide, the silicon carbide, the antistatic agent and the wear-resisting agent in parts by weight, and fully grinding to obtain a mixture; kneading the PVC resin, the methyltriethylsilane, the polyurethane, the tributyl citrate, the foaming agent and the mixture in parts by weight at a high speed at 100 ℃, adding the epoxidized soybean oil in parts by weight, stirring at a high speed, uniformly mixing, and banburying at 150 ℃ to obtain the wear-resistant PVC slurry; and (3) laminating the obtained wear-resistant PVC slurry on a base fabric through a calender, then carrying out foaming embossing treatment, and standing and cooling to obtain the PVC wear-resistant leather.
Example 2
PVC wear-resistant leather and preparation method thereof
The PVC wear-resistant leather comprises the following raw materials in parts by weight: 55 parts of PVC resin, 1.5 parts of methyl triethyl silane, 12 parts of epoxidized soybean oil, 1.5 parts of polyurethane, 2.5 parts of tributyl citrate, 12 parts of modified aluminum oxide, 4 parts of silicon carbide, 1.2 parts of antistatic agent, 6 parts of wear-resisting agent and 2 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
The preparation of the modified alumina comprises the following steps:
s1, transferring alumina into a pulverizer to be ground into alumina powder with the average grain diameter of 40 microns, adding the alumina powder into absolute ethyl alcohol, ultrasonically stirring until the alumina powder is uniformly dispersed, then sequentially adding magnesium aluminate and 10% ammonia water solution, ultrasonically dispersing uniformly, adding 10% polyethylene glycol solution, stirring to react until gel appears, continuously stirring until the gel is complete, taking out and filtering, repeatedly washing with absolute ethyl alcohol, drying in an oven at 100 ℃ to constant weight, transferring into a sintering furnace at 700 ℃ to roast for 6 hours, taking out and cooling to obtain pretreated alumina;
s2, adding the pretreated aluminum oxide obtained in the step (2) into deionized water, placing the mixture in a constant-temperature water bath, stirring the mixture at a constant temperature of 85 ℃ for 35min, adding a modifier, adjusting the pH value to 8-8 by using ammonia water, heating the mixture to 110 ℃, stirring the mixture at a constant temperature of 400r/min for 55min, precipitating and filtering the mixture, taking the mixture out, cooling the mixture to room temperature, repeatedly washing the mixture by using absolute ethyl alcohol, then placing the mixture in an oven, and drying the mixture at 110 ℃ for 3.5h to obtain the modified aluminum oxide.
S2, the preparation of the modifier comprises the following steps: adding liquid butyl titanate into deionized water, and stirring and mixing at the rotating speed of 200r/min to obtain a white butyl titanate suspension; adding liquid dodecyl dimethyl betaine into deionized water, and stirring and mixing at a rotating speed of 100r/min to obtain dodecyl dimethyl betaine solution; and (3) mixing the butyl titanate white suspension with dodecyl dimethyl betaine solution, adding 1, 2-propylene glycol, stirring and mixing for 1.5h, heating to 70 ℃, continuously stirring for 2h, and distilling under reduced pressure to obtain the modifier.
The volume ratio of the liquid butyl titanate to the deionized water is 0.08: 1; the density of the liquid butyl titanate is 0.866g/cm3(ii) a The volume ratio of the liquid dodecyl dimethyl betaine to the deionized water is 0.008: 1; the density of the liquid dodecyl dimethyl betaine is 0.56g/cm3. The volume ratio of the butyl titanate white suspension to the dodecyl dimethyl betaine solution to the 1, 2-propylene glycol is 1:0.08: 16.
The preparation method of the PVC wear-resistant leather comprises the following steps:
mixing the modified aluminum oxide, the silicon carbide, the antistatic agent and the wear-resisting agent in parts by weight, and fully grinding to obtain a mixture; kneading the PVC resin, the methyltriethylsilane, the polyurethane, the tributyl citrate, the foaming agent and the mixture in parts by weight at a high speed at 100 ℃, adding the epoxidized soybean oil in parts by weight, stirring at a high speed, uniformly mixing, and banburying at 150 ℃ to obtain the wear-resistant PVC slurry; and (3) laminating the obtained wear-resistant PVC slurry on a base fabric through a calender, then carrying out foaming embossing treatment, and standing and cooling to obtain the PVC wear-resistant leather.
Example 3
PVC wear-resistant leather and preparation method thereof
The PVC wear-resistant leather comprises the following raw materials in parts by weight: 60 parts of PVC resin, 2 parts of methyl triethyl silane, 17 parts of epoxidized soybean oil, 3 parts of polyurethane, 2 parts of tributyl citrate, 15 parts of modified alumina, 5 parts of silicon carbide, 2 parts of antistatic agent, 5 parts of wear-resisting agent and 3 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
The preparation of the modified alumina comprises the following steps:
s1, transferring alumina into a pulverizer to be ground into alumina powder with the average grain diameter of 40 microns, adding the alumina powder into absolute ethyl alcohol, ultrasonically stirring until the alumina powder is uniformly dispersed, then sequentially adding magnesium aluminate and 10% ammonia water solution, ultrasonically dispersing uniformly, adding 10% polyethylene glycol solution, stirring to react until gel appears, continuously stirring until the gel is complete, taking out and filtering, repeatedly washing with absolute ethyl alcohol, drying in an oven at 100 ℃ to constant weight, transferring into a sintering furnace to roast for 5 hours at 800 ℃, taking out and cooling to obtain pretreated alumina;
s2, adding the pretreated aluminum oxide obtained in the step (2) into deionized water, placing the mixture in a constant-temperature water bath, stirring the mixture for 45min at a constant temperature of 80 ℃, adding a modifier, adjusting the pH value to 8-8 by using ammonia water, heating the mixture to 110 ℃, stirring the mixture for 60min at a constant temperature of 500r/min, precipitating and filtering the mixture, taking the mixture out, cooling the mixture to room temperature, repeatedly washing the mixture by using absolute ethyl alcohol, then placing the mixture in an oven, and drying the mixture for 5h at 110 ℃ to obtain the modified aluminum oxide.
S2, the preparation of the modifier comprises the following steps: adding liquid butyl titanate into deionized water, and stirring and mixing at the rotating speed of 200r/min to obtain a white butyl titanate suspension; adding liquid dodecyl dimethyl betaine into deionized water, and stirring and mixing at a rotating speed of 100r/min to obtain dodecyl dimethyl betaine solution; and (2) mixing the butyl titanate white suspension with dodecyl dimethyl betaine solution, adding 1, 2-propylene glycol, stirring and mixing for 1h, heating to 80 ℃, continuously stirring for 2h, and distilling under reduced pressure to obtain the modifier.
The volume ratio of the liquid butyl titanate to the deionized water is 0.25: 1; the density of the liquid butyl titanate is 0.866g/cm3(ii) a The volume ratio of the liquid dodecyl dimethyl betaine to the deionized water is 0.03: 1; the density of the liquid dodecyl dimethyl betaine is 0.56g/cm3. The volume ratio of the butyl titanate white suspension to the dodecyl dimethyl betaine solution to the 1, 2-propylene glycol is 1:0.2: 20.
The preparation method of the PVC wear-resistant leather comprises the following steps:
mixing the modified aluminum oxide, the silicon carbide, the antistatic agent and the wear-resisting agent in parts by weight, and fully grinding to obtain a mixture; kneading the PVC resin, the methyltriethylsilane, the polyurethane, the tributyl citrate, the foaming agent and the mixture in parts by weight at a high speed at 110 ℃, adding the epoxidized soybean oil in parts by weight, stirring at a high speed, uniformly mixing, and banburying at 165 ℃ to obtain the wear-resistant PVC slurry; and (3) laminating the obtained wear-resistant PVC slurry on a base fabric through a calender, then carrying out foaming embossing treatment, and standing and cooling to obtain the PVC wear-resistant leather.
Example 4
PVC wear-resistant leather and preparation method thereof
The PVC wear-resistant leather comprises the following raw materials in parts by weight: 68 parts of PVC resin, 2.5 parts of methyl triethyl silane, 18 parts of epoxidized soybean oil, 4 parts of polyurethane, 3.5 parts of tributyl citrate, 14 parts of modified aluminum oxide, 6 parts of silicon carbide, 2.5 parts of antistatic agent, 7.5 parts of wear-resisting agent and 2 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
The preparation of the modified alumina comprises the following steps:
s1, transferring alumina into a pulverizer to be ground into alumina powder with the average grain diameter of 40 microns, adding the alumina powder into absolute ethyl alcohol, ultrasonically stirring until the alumina powder is uniformly dispersed, then sequentially adding magnesium aluminate and 10% ammonia water solution, ultrasonically dispersing uniformly, adding 10% polyethylene glycol solution, stirring to react until gel appears, continuously stirring until the gel is complete, taking out and filtering, repeatedly washing with absolute ethyl alcohol, drying in an oven at 100 ℃ to constant weight, transferring into a sintering furnace to be roasted at 800 ℃ for 6 hours, taking out and cooling to obtain pretreated alumina;
s2, adding the pretreated aluminum oxide obtained in the step (2) into deionized water, placing the mixture in a constant-temperature water bath, stirring the mixture for 45min at a constant temperature of 85 ℃, adding a modifier, adjusting the pH value to 8 by using ammonia water, heating the mixture to 110 ℃, stirring the mixture for 75min at a constant temperature of 500r/min, precipitating and filtering the mixture, taking the precipitate out, cooling the precipitate to room temperature, repeatedly washing the precipitate by using absolute ethyl alcohol, then placing the precipitate in a drying oven, and drying the precipitate for 3h to 5h at 110 ℃ to obtain the modified aluminum oxide.
S2, the preparation of the modifier comprises the following steps: adding liquid butyl titanate into deionized water, and stirring and mixing at the rotating speed of 200r/min to obtain a white butyl titanate suspension; adding liquid dodecyl dimethyl betaine into deionized water, and stirring and mixing at a rotating speed of 100r/min to obtain dodecyl dimethyl betaine solution; and (3) mixing the butyl titanate white suspension with dodecyl dimethyl betaine solution, adding 1, 2-propylene glycol, stirring and mixing for 1.8h, heating to 80 ℃, continuously stirring for 3h, and distilling under reduced pressure to obtain the modifier.
The volume ratio of the liquid butyl titanate to the deionized water is 0.30: 1; the density of the liquid butyl titanate is 0.866g/cm3(ii) a The volume ratio of the liquid dodecyl dimethyl betaine to the deionized water is 0.04: 1; the density of the liquid dodecyl dimethyl betaine is 0.56g/cm3. The white suspension of butyl titanate, dodecyl dimethyl betaine solution and 1, 2-propylene glycolThe volume ratio is 1:0.20: 18.
The preparation method of the PVC wear-resistant leather comprises the following steps:
mixing the modified aluminum oxide, the silicon carbide, the antistatic agent and the wear-resisting agent in parts by weight, and fully grinding to obtain a mixture; kneading the PVC resin, the methyltriethylsilane, the polyurethane, the tributyl citrate, the foaming agent and the mixture in parts by weight at a high speed at 110 ℃, adding the epoxidized soybean oil in parts by weight, stirring at a high speed, uniformly mixing, and banburying at 160 ℃ to obtain the wear-resistant PVC slurry; and (3) laminating the obtained wear-resistant PVC slurry on a base fabric through a calender, then carrying out foaming embossing treatment, and standing and cooling to obtain the PVC wear-resistant leather.
Example 5
PVC wear-resistant leather and preparation method thereof
The PVC wear-resistant leather comprises the following raw materials in parts by weight: 70 parts of PVC resin, 3 parts of methyl triethyl silane, 20 parts of epoxidized soybean oil, 1-5 parts of polyurethane, 4 parts of tributyl citrate, 15 parts of modified alumina, 7 parts of silicon carbide, 3 parts of antistatic agent, 8 parts of wear-resisting agent and 5 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
The preparation of the modified alumina comprises the following steps:
s1, transferring alumina into a pulverizer to be ground into alumina powder with the average grain diameter of 40 microns, adding the alumina powder into absolute ethyl alcohol, ultrasonically stirring until the alumina powder is uniformly dispersed, then sequentially adding magnesium aluminate and 10% ammonia water solution, ultrasonically dispersing uniformly, adding 10% polyethylene glycol solution, stirring to react until gel appears, continuously stirring until the gel is complete, taking out and filtering, repeatedly washing with absolute ethyl alcohol, drying in an oven at 100 ℃ to constant weight, transferring into a sintering furnace to roast for 5 hours at 800 ℃, taking out and cooling to obtain pretreated alumina;
s2, adding the pretreated aluminum oxide obtained in the step (2) into deionized water, placing the mixture in a constant-temperature water bath, stirring the mixture for 50min at a constant temperature of 80 ℃, adding a modifier, adjusting the pH value to 8 by using ammonia water, heating the mixture to 110 ℃, stirring the mixture for 80min at a constant temperature of 600r/min, precipitating and filtering the mixture, taking the precipitate out, cooling the precipitate to room temperature, repeatedly washing the precipitate by using absolute ethyl alcohol, placing the precipitate in an oven, and drying the precipitate for 5h at 110 ℃ to obtain the modified aluminum oxide.
S2, the preparation of the modifier comprises the following steps: adding liquid butyl titanate into deionized water, and stirring and mixing at the rotating speed of 200r/min to obtain a white butyl titanate suspension; adding liquid dodecyl dimethyl betaine into deionized water, and stirring and mixing at a rotating speed of 100r/min to obtain dodecyl dimethyl betaine solution; mixing the butyl titanate white suspension with dodecyl dimethyl betaine solution, adding 1, 2-propylene glycol, stirring and mixing for 2h, then heating to 80 ℃, continuing stirring for 3.5h, and distilling under reduced pressure to obtain the modifier.
The volume ratio of the liquid butyl titanate to the deionized water is 0.35: 1; the density of the liquid butyl titanate is 0.866g/cm3(ii) a The volume ratio of the liquid dodecyl dimethyl betaine to the deionized water is 0.05: 1; the density of the liquid dodecyl dimethyl betaine is 0.56g/cm3. The volume ratio of the butyl titanate white suspension to the dodecyl dimethyl betaine solution to the 1, 2-propylene glycol is 1:0.25: 20.
The preparation method of the PVC wear-resistant leather comprises the following steps:
mixing the modified aluminum oxide, the silicon carbide, the antistatic agent and the wear-resisting agent in parts by weight, and fully grinding to obtain a mixture; kneading the PVC resin, the methyltriethylsilane, the polyurethane, the tributyl citrate, the foaming agent and the mixture in parts by weight at a high speed at 110 ℃, adding the epoxidized soybean oil in parts by weight, stirring at a high speed, uniformly mixing, and banburying at 170 ℃ to obtain the wear-resistant PVC slurry; and (3) laminating the obtained wear-resistant PVC slurry on a base fabric through a calender, then carrying out foaming embossing treatment, and standing and cooling to obtain the PVC wear-resistant leather.
Comparative example 1
The difference from the example 3 is only that the raw materials of the PVC wear-resistant leather do not comprise modified alumina, and specifically, the PVC wear-resistant leather comprises the following raw materials in parts by weight: 60 parts of PVC resin, 2 parts of methyl triethyl silane, 17 parts of epoxidized soybean oil, 3 parts of polyurethane, 2 parts of tributyl citrate, 15 parts of aluminum oxide, 5 parts of silicon carbide, 2 parts of antistatic agent, 5 parts of wear-resisting agent and 3 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
The preparation method of the PVC wear-resistant leather comprises the following steps:
mixing the aluminum oxide, the silicon carbide, the antistatic agent and the wear-resisting agent in parts by weight, and fully grinding to obtain a mixture; kneading the PVC resin, the methyltriethylsilane, the polyurethane, the tributyl citrate, the foaming agent and the mixture in parts by weight at a high speed at 110 ℃, adding the epoxidized soybean oil in parts by weight, stirring at a high speed, uniformly mixing, and banburying at 165 ℃ to obtain the wear-resistant PVC slurry; and (3) laminating the obtained wear-resistant PVC slurry on a base fabric through a calender, then carrying out foaming embossing treatment, and standing and cooling to obtain the PVC wear-resistant leather.
Comparative example 2
The difference from the example 3 is only that the raw materials of the PVC wear-resistant leather do not comprise modified alumina and silicon carbide, and the rest conditions are the same.
Comparative example 3
The modified alumina is different from the modified alumina in example 3 only in that the modified alumina is the alumina powder modified by a silane coupling agent, and specifically, the preparation of the modified alumina comprises the following steps: adding alumina powder with average particle size of 40 μm into anhydrous ethanol, ultrasonically dispersing, adding silane coupling agent KH570, stirring, heating to reflux, reacting for 8 hr, centrifuging, and vacuum drying. Washing with absolute ethyl alcohol repeatedly to remove residual silane coupling agent KH570, and drying in a vacuum drying oven to obtain the alumina powder modified by silane coupling agent.
Comparative example 4
Commercially available PVC leather.
Test examples
In order to determine the performance of the PVC wear-resistant leather prepared by the invention, the performance tests are respectively carried out on the PVC wear-resistant leather prepared in the examples 1-5, the PVC wear-resistant leather prepared in the comparative examples 1-3 and the commercial PVC leather in the comparative example 4.
Taber abrasion resistance performance test: the products of the above examples and comparative examples were cut to the same size and placed on a Taber abrasion tester for testing, the results of which are shown in table 1:
TABLE 1
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the embodiment of the present invention by 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 (9)
1. The PVC wear-resistant leather is characterized by comprising the following raw materials in parts by weight: 50-70 parts of PVC resin, 1-3 parts of methyl triethyl silicane, 10-20 parts of epoxidized soybean oil, 1-5 parts of polyurethane, 2-4 parts of tributyl citrate, 10-15 parts of modified alumina, 3-7 parts of silicon carbide, 1-3 parts of antistatic agent, 5-8 parts of wear-resistant agent and 1-5 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
2. The PVC wear-resistant leather as claimed in claim 1, which comprises the following raw materials in parts by weight: 60 parts of PVC resin, 2 parts of methyl triethyl silane, 17 parts of epoxidized soybean oil, 3 parts of polyurethane, 2 parts of tributyl citrate, 15 parts of modified alumina, 5 parts of silicon carbide, 2 parts of antistatic agent, 5 parts of wear-resisting agent and 3 parts of foaming agent; the wear-resisting agent is polyvinyl chloride powder.
3. The PVC abrasion-resistant leather according to claim 1, wherein the preparation of the modified alumina comprises the following steps:
s1, transferring alumina into a pulverizer to be ground into alumina powder with the average grain diameter of 40 mu m, adding the alumina powder into absolute ethyl alcohol, ultrasonically stirring until the alumina powder is uniformly dispersed, then sequentially adding magnesium aluminate and an ammonia water solution, ultrasonically dispersing uniformly, adding a polyethylene glycol solution, stirring to react until gel appears, continuously stirring until the gel is completely dispersed, taking out and filtering, repeatedly washing with absolute ethyl alcohol, placing in an oven to dry to constant weight, transferring into a sintering furnace to roast, taking out and cooling to obtain pretreated alumina;
s2, adding the pretreated aluminum oxide obtained in the step (2) into deionized water, placing the mixture in a constant-temperature water bath, stirring the mixture for 30-50 min at a constant temperature of 80-90 ℃, adding a modifier, adjusting the pH value to 8-9 by using ammonia water, heating the mixture to 110 ℃, stirring the mixture for 50-80 min at a constant temperature of 400-600 r/min, precipitating and filtering the mixture, taking out the mixture, cooling the mixture to room temperature, repeatedly washing the mixture by using absolute ethyl alcohol, then placing the mixture in a drying oven, and drying the mixture for 3-5 h at 110 ℃ to obtain the modified aluminum oxide.
4. The PVC wear-resistant leather of claim 3, wherein in S1, the concentration of the ammonia water solution is 10%; the concentration of the polyethylene glycol solution is 10%.
5. The PVC wear-resistant leather according to claim 3, wherein in S1, the temperature of the oven is 100 ℃; the roasting temperature is 700-800 ℃, and the roasting time is 5-7 h.
6. The PVC abrasion-resistant leather according to claim 3, wherein in S2, the preparation of said modifier comprises the following steps: adding liquid butyl titanate into deionized water, and stirring and mixing at the rotating speed of 200r/min to obtain a white butyl titanate suspension; adding liquid dodecyl dimethyl betaine into deionized water, and stirring and mixing at a rotating speed of 100r/min to obtain dodecyl dimethyl betaine solution; mixing the butyl titanate white suspension with dodecyl dimethyl betaine solution, adding 1, 2-propylene glycol, stirring and mixing for 1-2 h, then heating to 70-80 ℃, continuing stirring for 2-3.5 h, and distilling under reduced pressure to obtain the modifier.
7. The PVC wear-resistant leather of claim 6, wherein the volume ratio of the liquid butyl titanate to the deionized water is 0.04-0.35: 1; the density of the liquid butyl titanate is 0.966g/cm3(ii) a The volume ratio of the liquid dodecyl dimethyl betaine to the deionized water is 0.002-0.05: 1; the density of the liquid dodecyl dimethyl betaine is 0.56g/cm3。
8. The PVC wear-resistant leather of claim 6, wherein the volume ratio of the butyl titanate white suspension to the dodecyl dimethyl betaine solution to the 1, 2-propylene glycol is 1: 0.01-0.25: 15-20.
9. The preparation method of the PVC wear-resistant leather according to any one of claims 1 to 8, which is characterized by comprising the following steps: mixing the modified aluminum oxide, the silicon carbide, the antistatic agent and the wear-resisting agent in parts by weight, and fully grinding to obtain a mixture; kneading the PVC resin, the methyltriethylsilane, the polyurethane, the tributyl citrate, the foaming agent and the mixture in parts by weight at a high speed at 100-110 ℃, adding the epoxidized soybean oil in parts by weight, stirring at a high speed, uniformly mixing, and banburying at 150-170 ℃ to obtain the wear-resistant PVC slurry; and (3) laminating the obtained wear-resistant PVC slurry on a base fabric through a calender, then carrying out foaming embossing treatment, and standing and cooling to obtain the PVC wear-resistant leather.
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