CN113637238B - Coarsening-free sports sole and preparation method thereof - Google Patents
Coarsening-free sports sole and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
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- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B13/00—Soles; Sole-and-heel integral units
- A43B13/02—Soles; Sole-and-heel integral units characterised by the material
- A43B13/04—Plastics, rubber or vulcanised fibre
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- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B13/00—Soles; Sole-and-heel integral units
- A43B13/02—Soles; Sole-and-heel integral units characterised by the material
- A43B13/12—Soles with several layers of different materials
- A43B13/122—Soles with several layers of different materials characterised by the outsole or external layer
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- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B13/00—Soles; Sole-and-heel integral units
- A43B13/02—Soles; Sole-and-heel integral units characterised by the material
- A43B13/12—Soles with several layers of different materials
- A43B13/125—Soles with several layers of different materials characterised by the midsole or middle layer
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- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43D—MACHINES, TOOLS, EQUIPMENT OR METHODS FOR MANUFACTURING OR REPAIRING FOOTWEAR
- A43D25/00—Devices for gluing shoe parts
- A43D25/06—Devices for gluing soles on shoe bottoms
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Abstract
The invention provides a rough-free sports sole and a preparation method thereof, wherein the sole comprises a midsole and an outsole; the midsole comprises the following raw materials in parts by weight: 30-50 parts of EVA, 0-20 parts of OBC, 10-20 parts of POE, 0-10 parts of SEBS, 0-10 parts of EPDM, 5-20 parts of ethylene-carbon monoxide copolymer, 1-15 parts of ethylene-acrylic acid copolymer, 1-10 parts of ethylene-methacrylic acid ionized resin, 0.5-1 part of peroxide cross-linking agent, 3.5 parts of foaming agent, 1-3 parts of zinc oxide, 0.8 part of stearic acid and 1 part of zinc stearate; the outsole comprises 50-70 parts of natural rubber, 20-40 parts of butadiene rubber, 1-10 parts of polyacrylate rubber, 30-50 parts of white carbon black, 1.5 parts of silane coupling agent, 10 parts of softening oil, 3 parts of zinc oxide, 2.5 parts of composite accelerator and 2.5 parts of sulfur. The sole does not need to be roughened, and has higher adhesive strength.
Description
Technical Field
The invention belongs to the technical field of sole materials, and particularly relates to a roughening-free sports sole and a preparation method thereof.
Background
In recent years, along with the hot trend of body building exercises of the whole people, more and more people are in the middle of various exercises, the requirements on the sports shoes are higher and higher, and consumers want to have a pair of perfect sports shoes which integrate light weight, high elasticity, softness, shock absorption, durability and wear resistance.
However, with the improvement of performance requirements, non-polar polymers such as OBC (block ethylene copolymer), POE (random ethylene-butylene/octene copolymer), EPDM (ethylene propylene diene monomer), metallocene PE (polyethylene), SEBS (styrene-butadiene copolymer) and the like are gradually introduced into the formula, and the polymers improve the rebound resilience, shock absorption property, durability and the like of the foaming material, but bring new problems to the adhesive force of the sole. The higher the content of the nonpolar polymer in the formula, the worse the adhesive force, the easier the sole is to open, and sole factories can only roughen the foamed midsole and the rubber outsole by adding oily glue and the like to attach, thus not only increasing the production cost and reducing the production efficiency, but also the dust generated in the roughening procedure, the harmful solvent in the oily glue and the like are not beneficial to the health and the environment of human bodies.
Therefore, there is an urgent need to develop a sports shoe sole that is free of roughening but yet has a strong adhesive strength.
Disclosure of Invention
In view of the above, the present invention aims to provide a sole for sports without roughening and a method for preparing the same, wherein the sole is free from roughening, and the midsole and the outsole have high adhesion strength.
The invention provides a rough-free sports sole, which comprises a midsole and an outsole;
the midsole comprises the following raw materials in parts by weight:
30-50 parts of EVA, 0-20 parts of OBC, 10-20 parts of POE, 0-10 parts of SEBS, 0-10 parts of EPDM, 5-20 parts of ethylene-carbon monoxide copolymer, 1-15 parts of ethylene-acrylic acid copolymer, 1-10 parts of ethylene-methacrylic acid ionized resin, 0.5-1 part of peroxide cross-linking agent, 3.5 parts of foaming agent, 1-3 parts of zinc oxide, 0.8 part of stearic acid and 1 part of zinc stearate;
the outsole comprises the following raw materials:
50-70 parts of natural rubber, 20-40 parts of butadiene rubber, 1-10 parts of polyacrylate rubber, 30-50 parts of white carbon black, 1.5 parts of silane coupling agent, 10 parts of softening oil, 3 parts of zinc oxide, 1.5 parts of thiazole accelerator, 0.6 part of diphenyl guanidine accelerator, 0.025 part of thiuram accelerator and 2.5 parts of sulfur.
Preferably, the VA content in the EVA is 12-33%;
the content of the hard segment in the SEBS is 13-33 mol%;
the EPDM has a crystallinity of <5%;
the acrylate content of the vinyl acid ester-carbon monoxide copolymer is >20mol%;
the ethylene acrylic acid copolymer has an acrylic acid content of >8 mole%.
Preferably, the EVA is selected from one or more of EVA33121, EVA26061 and EVA 7350M;
the vinyl ester-carbon monoxide copolymer is selected from Elvaloy AC 3427 and/or Elvaloy AC 1125;
the ethylene-acrylic acid copolymer is selected from Fusabond 514D and/or Nucrel 925;
the peroxide crosslinking agent is selected from dicumyl peroxide and/or 1, 4-di-tert-butyl peroxyisopropyl benzene;
the foaming agent is selected from one or more of azodicarbonamide, expanded microspheres and 4, 4-oxo-diphenyl sulfonyl hydrazine;
the ethylene-methacrylic acid ionizing resin is selected from ethylene-sodium methacrylate.
Preferably, the natural rubber has a Mooney viscosity of 80.+ -.20 (ML1+4@100℃);
the Mooney viscosity of the butadiene rubber is 45+/-3 (ML1+4@100 ℃);
the Mooney viscosity of the polyacrylate rubber is 45+ -5 (ML1+4@100℃).
Preferably, the specific surface area of the white carbon black is 160-180 m 2 /g；
The silane coupling agent is selected from one or more of Si-50, KH550 and KH 570;
the softening oil is selected from paraffinic oil and/or naphthenic oil;
the accelerator is selected from the group consisting of mixtures of diphenyl guanidine, dibenzothiazyl disulfide and tetramethylthiuram monosulfide.
The invention provides a preparation method of the roughening-free sports sole, which comprises the following steps:
EVA, OBC, POE, SEBS, EPDM, an ethylene acid ester-carbon monoxide copolymer, an ethylene-acrylic acid copolymer and an ethylene-methacrylic acid ionized resin are mixed, heated to 75-85 ℃, zinc oxide, stearic acid and zinc stearate are added, then heated to 85-95 ℃, a peroxide cross-linking agent and a foaming agent are added, heated to 100-105 ℃, and uniformly mixed to obtain a mixed material; granulating the mixed materials, and foaming to obtain a semi-finished product; standing the semi-finished product, molding, and cooling to obtain a midsole foaming material;
mixing natural rubber, butadiene rubber and polyacrylate rubber, and banburying to obtain a rubber base material; discharging the rubber base material, standing for 4-8 h, mixing with white carbon black, a silane coupling agent, softening oil and zinc oxide, and banburying again to obtain a sizing material; mixing the sizing material with thiazole accelerators, diphenyl guanidine accelerators, thiuram accelerators and sulfur, discharging tablets, and vulcanizing to obtain a outsole material;
and respectively processing the midsole foaming material and the outsole material, and then attaching to obtain the rough-free sports sole.
Preferably, the foaming temperature is 175 ℃ and the foaming time is 650-670 s;
the molding temperature is 175 ℃, and the molding time is 410-430 s.
Preferably, the process of attaching the midsole foaming material and the outsole material after being respectively treated comprises the following steps:
cleaning, soaking and irradiating the midsole foaming material to obtain a midsole;
cleaning the outsole material, adding a treating agent, and drying to obtain an outsole;
and brushing the rubber on the midsole and the outsole respectively, drying, attaching and pressing.
According to the invention, polymers such as ethylene acid ester-carbon monoxide copolymer, ethylene-acrylic acid copolymer, ethylene-methacrylic acid ionized resin and the like are added into the midsole foaming material for blending foaming, so that the polarity of the foaming midsole is greatly improved, and the roughening procedure of the midsole is saved; the addition of the polyacrylate rubber (ACM rubber) in the rubber outsole also improves the polarity of the rubber outsole, saves the roughening procedure of the outsole, avoids the roughening procedure of the midsole and the outsole, improves the production efficiency, reduces the production cost, also avoids the damage of dust in the roughening procedure to the health of operators, and truly achieves low carbon and environmental protection; the polarity of the midsole and the outsole is synchronously increased, the effect of coarse bonding without beating with the midsole is better realized, and the problem of easy glue opening of the midsole and the outsole is solved. The experimental results show that: the bonding strength of the sole of the roughening-free sports shoe provided by the invention is more than or equal to 30N/cm.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a midsole foam material according to an embodiment of the present invention;
FIG. 2 shows a process for implementing a rubber outsole material in accordance with an embodiment of the invention;
fig. 3 is a schematic diagram of a lamination process according to an embodiment of the invention.
Detailed Description
The invention provides a rough-free sports sole, which comprises a midsole and an outsole;
the midsole comprises the following raw materials in parts by weight:
30-50 parts of EVA, 0-20 parts of OBC, 10-20 parts of POE, 0-10 parts of SEBS, 0-10 parts of EPDM, 5-20 parts of ethylene-carbon monoxide copolymer, 1-15 parts of ethylene-acrylic acid copolymer, 1-10 parts of ethylene-methacrylic acid ionized resin, 0.5-1 part of peroxide cross-linking agent, 3.5 parts of foaming agent, 1-3 parts of zinc oxide, 0.8 part of stearic acid and 1 part of zinc stearate;
the outsole comprises the following raw materials:
50-70 parts of natural rubber, 20-40 parts of butadiene rubber, 1-10 parts of polyacrylate rubber, 30-50 parts of white carbon black, 1.5 parts of silane coupling agent, 10 parts of softening oil, 3 parts of zinc oxide, 1.5 parts of thiazole accelerator, 0.6 part of diphenyl guanidine accelerator, 0.025 part of thiuram accelerator and 2.5 parts of sulfur.
According to the invention, polymers such as ethylene acid ester-carbon monoxide copolymer, ethylene-acrylic acid copolymer, ethylene-methacrylic acid ionized resin and the like are added into the midsole foaming material for blending foaming, so that the polarity of the foaming midsole is greatly improved, and the roughening procedure of the midsole is saved; the polyacrylate rubber (ACM rubber) is added into the rubber outsole, so that the polarity of the rubber outsole is improved, and the roughening process of the outsole is saved; the middle sole and the outsole avoid the roughening process, the production efficiency is improved, the production cost is reduced, the damage of dust in the roughening process to the health of operators is avoided, and the low-carbon environment protection is truly achieved; the polarity of the midsole and the outsole is synchronously increased, the effect of coarse bonding without beating with the midsole is better realized, and the problem of easy glue opening of the midsole and the outsole is solved.
The roughening-free sports shoe sole provided by the invention comprises a midsole, wherein the midsole comprises the following raw materials in parts by weight: 30-50 parts of EVA, 0-20 parts of OBC, 10-20 parts of POE, 0-10 parts of SEBS, 0-10 parts of EPDM, 5-20 parts of ethylene-carbon monoxide copolymer, 1-15 parts of ethylene-acrylic acid copolymer, 1-10 parts of ethylene-methacrylic acid ionized resin, 0.5-1 part of peroxide cross-linking agent, 3.5 parts of foaming agent, 1-3 parts of zinc oxide, 0.8 part of stearic acid and 1 part of zinc stearate.
EVA in the raw material of the midsole is ethylene-vinyl acetate copolymer; the VA content in the EVA is 12-33%; the EVA is preferably one or more selected from EVA33121, EVA26061 and EVA 7350M. In a specific example, the EVA has a VA mass content of 33 mole percent and a hardness of 65A, and is purchased from Asian Polymer Co., ltd.
The OBC in the raw material of the midsole is an ethylene-butene block copolymer, and the OBC is preferably selected from Inform 9107.
The POE in the raw material of the midsole is an ethylene-octene random copolymer, and the POE is preferably selected from Engage 8003.
The SEBS in the raw material of the midsole is a styrene-butadiene copolymer, wherein a styrene structural unit is a hard segment, and the content of the hard segment is 13-33 mol%. The SEBS is preferably from YH688.
The EPDM in the raw material of the midsole is a terpolymer of ethylene, propylene and non-conjugated diene; the EPDM has a crystallinity of <5%. In a specific embodiment, the EPDM is selected from EPDM5565.
The ethylene acid ester-carbon monoxide copolymer in the raw materials of the midsole is an ethylene terpolymer pushed by DuPont company, and the chemical composition of the ethylene terpolymer is as follows: vinyl-acrylate-carbon monoxide can be classified as ethylene-methacrylate (EMA), ethylene-ethyl acrylate (EEA), ethylene-butyl acrylate (EBA) copolymers, depending on the comonomer. The acrylate content of the vinyl acid ester-carbon monoxide copolymer is >20%. The carbon monoxide has strong polarity and obvious effect of improving adhesive force, and the Elvaloy has higher melt strength, low-temperature flexibility and medium-strength polar acrylic ester, and the performances are superior to EVA. The vinyl ester-carbon monoxide copolymer is preferably selected from Elvaloy AC 3427 (ethylene-butyl acrylate, acrylate content 27%) or Elvaloy AC 1125 (ethylene-methacrylate, acrylate content 25%).
The ethylene-acrylic acid copolymer in the raw material of the midsole is a binary copolymer of DuPont company, and the carboxyl in the ethylene-acrylic acid copolymer has strong polarity, so that the higher the acrylic acid content is, the stronger the polarity is; the acrylic acid content of the ethylene-acrylic acid copolymer is preferably >8%. The ethylene-acrylic acid copolymer is preferably selected from Fusabond 514D (9% methacrylic acid content) and/or Nucrel 925 (15% methacrylic acid content).
The ethylene-methacrylic acid ionized resin in the raw material of the midsole is purchased from DuPont company, and the acidified metal ions have stronger polarity. The ethylene-methacrylic acid ionizing resin is selected from ethylene-sodium methacrylate or ethylene-zinc methacrylate, more preferably ethylene-sodium methacrylate; in a specific embodiment, the ethylene-methacrylic acid ionizing resin is Surlyn 1601.
The peroxide cross-linking agent in the raw material of the midsole is selected from dicumyl peroxide and/or 1, 4-di-tert-butyl peroxyisopropyl benzene; the peroxide crosslinking agent is selected from DCP PERCADOX BC-FF and/or BIBP PERCADOX 14S-FL.
The foaming agent in the raw materials of the midsole is one or more selected from azodicarbonamide, expansion microspheres and 4, 4-oxo-diphenyl sulfonyl hydrazine; in a specific embodiment, the foaming agent is selected from AC6000H.
The zinc oxide in the raw material of the midsole is selected from ZnO 997.
Stearic acid and zinc stearate in the raw materials of the midsole serve as activating agents.
The roughening-free sports shoe sole provided by the invention comprises an outsole, wherein the outsole comprises the following raw materials: 50-70 parts of natural rubber, 20-40 parts of butadiene rubber, 1-10 parts of polyacrylate rubber, 30-50 parts of white carbon black, 1.5 parts of silane coupling agent, 10 parts of softening oil, 3 parts of zinc oxide, 1.5 parts of thiazole accelerator, 0.6 part of diphenyl guanidine accelerator, 0.025 part of thiuram accelerator and 2.5 parts of sulfur.
Natural rubber, butadiene rubber and polyacrylate rubber (ACM) are adopted as the raw materials of the outsole, wherein the Mooney viscosity of the natural rubber is 80+/-20 (ML1+4@100 ℃); the Mooney viscosity of the butadiene rubber is 45+/-3 (ML1+4@100 ℃); the Mooney viscosity of the polyacrylate rubber is 45+ -5 (ML1+4@100℃). In a specific embodiment, the natural rubber is NR SVR-3L; butadiene rubber is BR9000; the ACM rubber is AVM-2212.
The specific surface area of the white carbon black in the raw material of the outsole is preferably 160-180 m 2 In a specific embodiment, the model number of the white carbon black is WL-180.
The silane coupling agent in the raw material of the outsole is preferably selected from one or more of Si-50, KH550 and KH570, more preferably Si-50.
The softening oil in the outsole feedstock is preferably selected from paraffinic and/or naphthenic oils. In a specific embodiment, the softening oil is selected from naphthenic oils 4006.
The specific surface area of zinc oxide in the raw material of the outsole is 25+/-5 m 2 Preferably from ZnO945.
The invention provides a preparation method of the roughening-free sports sole, which comprises the following steps:
EVA, OBC, POE, SEBS, EPDM, an ethylene acid ester-carbon monoxide copolymer, an ethylene-acrylic acid copolymer and an ethylene-methacrylic acid ionized resin are mixed, heated to 75-85 ℃, zinc oxide, stearic acid and zinc stearate are added, then heated to 85-95 ℃, a peroxide cross-linking agent and a foaming agent are added, heated to 100-105 ℃, and uniformly mixed to obtain a mixed material; granulating the mixed materials, and foaming to obtain a semi-finished product; standing the semi-finished product, molding, and cooling to obtain a midsole foaming material;
mixing natural rubber, butadiene rubber and polyacrylate rubber, and banburying to obtain a rubber base material; discharging the rubber base material, standing for 4-8 h, mixing with white carbon black, a silane coupling agent, softening oil and zinc oxide, and banburying again to obtain a sizing material; mixing the sizing material with thiazole accelerators, diphenyl guanidine accelerators, thiuram accelerators and sulfur, discharging tablets, and vulcanizing to obtain a outsole material;
and respectively processing the midsole foaming material and the outsole material, and then attaching to obtain the rough-free sports sole.
EVA, OBC, POE, SEBS, EPDM, an ethylene acid ester-carbon monoxide copolymer, an ethylene-acrylic acid copolymer and an ethylene-methacrylic acid ionized resin are mixed, the temperature is raised to 75-85 ℃, zinc oxide, stearic acid and zinc stearate are added, the temperature is raised to 85-95 ℃, a peroxide cross-linking agent and a foaming agent are added, the temperature is raised to 100-105 ℃, and the mixture is obtained after uniform mixing; granulating the mixed materials, and foaming to obtain a semi-finished product; and standing the semi-finished product, molding, and cooling to obtain the midsole foaming material.
In the invention, the foaming temperature is 175 ℃ and the foaming time is 650-670 s; the foaming ratio is 175-180%. The molding temperature is 175 ℃, and the molding time is 410-430 s. The cooling temperature is 25 ℃, and the cooling time is 420s.
Mixing natural rubber, butadiene rubber and polyacrylate rubber, and banburying to obtain a rubber base material; discharging the rubber base material, standing for 4-8 h, mixing with white carbon black, a silane coupling agent, softening oil and zinc oxide, and banburying again to obtain a sizing material; mixing the sizing material with thiazole accelerators, diphenyl guanidine accelerators, thiuram accelerators and sulfur, discharging tablets, and vulcanizing to obtain the outsole material.
According to the invention, the midsole foaming material and the outsole material are respectively treated and then attached to obtain the rough-free sports sole.
In the invention, the midsole foaming material is treated by an irradiation treatment agent, wherein the irradiation treatment agent adopts commercial products, the solid content is 0.8-1.5%, the irradiation treatment agent comprises vinyl chloride-vinyl acetate resin, methyl methacrylate, acrylic acid, a photoinitiator and a solvent, and the solvent comprises ethyl acetate, toluene, acetone and butanone. The midsole foaming material and the outsole material both contain acrylic acid/acrylic acid ester molecular monomers, and the acrylic acid/acrylic acid ester molecular monomers are similar molecular structure monomers with methyl methacrylate and acrylic acid in the irradiation treatment agent, and according to a similar compatibility principle, polymers of acrylic acid/acrylic acid ester components in the formula of the EVA midsole and the rubber outsole and small molecules such as methyl methacrylate and acrylic acid in the midsole irradiation agent play a stealth bypass role, so that a better bonding effect is achieved. The EVA midsole is soaked by the irradiation treatment agent and then is subjected to UV irradiation within 2 hours;
in the invention, after the midsole foaming material and the outsole material are respectively treated, respectively brushing water-based PU glue, drying, attaching and pressing to obtain the sole. And (3) drying the shoe soles subjected to glue brushing in an oven assembly line, wherein the drying temperature is 60-70 ℃, and the rotating speed of the oven assembly line is 300-400 rpm. The bonding temperature is preferably 50℃or higher. Pressing at 45-50 ℃ and finishing the time from the lamination to the pressing within 60 s; the invention preferably carries out strong pressure and then spot pressure; the pressure of the strong pressure is 35kg-40kg, and the time of the strong pressure is 7-8 seconds; the pressure of the spot pressing is 30-35 kg, and the time of the spot pressing is 2-3 s.
In order to further illustrate the present invention, the following examples are provided to illustrate a roughening-free sports shoe sole and a method for making the same, but they should not be construed to limit the scope of the present invention.
Example 1
1) Preparation of midsole foam material
The implementation steps of fig. 1 are illustrated:
weighing: the cross-linking agent and the foaming agent are weighed according to the amount of the formulation shown in tables 1 and 2; weighing zinc oxide, stearic acid and zinc stearate as a second group; the remaining materials were weighed for the third group.
And (3) mixing: firstly, pouring the third group of materials into a scouring machine, and opening the machine until the temperature is increased to 75-85 ℃; pouring a second group of materials; pouring a third material when the temperature is raised to 85-95 ℃; and pouring out the mixed materials when the temperature is raised to 100-105 ℃.
And (3) material manufacturing: mixing the materials; pouring the mixture into a material making machine, and respectively adjusting the temperatures of a first zone, a second zone, a third zone and a fourth zone to be: 75 ℃, 80 ℃,85 ℃ and 90 ℃, and the screw is adjusted to 40-50 rpm, and the blanking is adjusted to 15-20 rpm.
Small foaming: pouring the manufactured granules into a flat-plate mould pressing small foaming mould to finish the first foaming, wherein the foaming temperature is as follows: 175 ℃; the foaming time is as follows: 660 seconds; the foaming ratio was 175%.
And (3) mould pressing: after standing and cooling the small foamed semi-finished product for 24 hours, pressing the small foamed semi-finished product into a flat plate mould pressing die to finish finished product mould pressing, and obtaining the midsole foaming material; the hot pressing temperature is as follows: 175 ℃; the hot pressing time is as follows: 420 seconds; the cooling water temperature is: the cooling time at 25 ℃ is as follows: 420 seconds.
Table 1 raw material formulation tables of examples 1 to 4 and comparative examples 1 to 3
Table 2 raw material formulation tables of examples 5 to 11
Wherein, EVA 33121: the VA mass content was 33%, hardness 65A, asian Polymer Co., ltd.
EVA7350M: the VA mass content is 18%, the hardness is 84A, and the molding is performed.
Inuse 9107: hardness 60A, crystallinity 10.6%, melting point 120 ℃, dow chemical.
Engage 8003: hardness 84A, crystallinity 25%, dow chemical.
SEBS YH 688: hardness 45A, hard segment content 13%, and Baling petrochemical.
EPDM 5565: ethylene content 50%, crystallinity <1%, dow chemical.
Elvaloy AC 3427: acrylic ester content 27%, hardness 81A, melting point 94 ℃, duPont.
Elvaloy AC 1125: 25% acrylate, 78A hardness, 92℃melting point, duPont.
Nucrel 925: hardness 50D, acrylic content 15%, melting point 92 ℃, duPont company.
Fusabond 514D: hardness 53D, crystallinity 45%, acrylic content 9%, tear strength 91N/mm, duPont company.
Surlyn 1601: hardness 60D, acrylic content 6%, duPont company.
ZnO 997: the relative density of the white stone plate zinc oxide is 4.42-4.45.
BIBP PERCADOX 14S-FL: ackersinobell.
Stearic acid 1801: indonesia Du Kuda.
Zinc stearate: the new chemical company of water chestnut lake in Huzhou city is expected.
Foaming agent AC6000H: hangzhou sea iridescence fine chemical Co., ltd.
Physical property data of the midsole foam material prepared above are shown in table 3:
table 3 physical property data of the midsole foam materials of examples 1 to 4 and comparative example
Table 4 physical property data of the midsole foam materials of examples 5 to 11
2) Preparation of rubber outsole material:
the rubber substrate material implementation steps are shown in fig. 2:
description of implementation steps:
mixing 1: according to the raw material formulation of Table 5, the base rubber was poured into an internal mixer, the internal mixer was started, and the mixture was kneaded for 8 minutes to thoroughly mix the various rubbers, and when the internal mixer temperature was raised to 110 ℃, the mixed rubber was poured out.
And (3) discharging a sheet 1: and (3) placing the mixed sizing material into an open mill, continuously rolling for 5-10 times, forming a sheet with the thickness of 3CM, and standing for 4-8 hours for later use.
And (3) mixing 2: pouring the mixed sizing material which is parked for 4-8 hours into an internal mixer again, pouring white carbon black, a silane coupling agent, softening oil and zinc oxide into the internal mixer together, mixing for 8 minutes, and pouring out the mixed sizing material when the temperature of the internal mixer is raised to 110 ℃.
And (3) discharging a sheet 2: pouring the mixed sizing material into an open mill, continuously rolling for 5-8 times, adding the accelerator and the cross-linking agent sulfur, and obtaining the sheet with the thickness of 4 cm.
Vulcanizing: cutting a sheet with the thickness of 4cm into a size required by a mould, putting the sheet into the mould, vulcanizing the sheet for 250 seconds by using a flat vulcanizing machine at 160 ℃, and taking out the vulcanized rubber product.
Table 5 raw material formulation table for rubber outsole material
Wherein NR SVR-3L: mooney viscosity 80+ -20 (ML1+4@100℃), vietnam standard gum.
BR 9000: mooney viscosity 45.+ -.3 (ML1+4@100℃), yan Shangao bridge Co.
NBR1052: mooney viscosity 52.+ -.3 (ML1+4@100℃), nandi corporation.
BIIR X2: mooney viscosity 32.+ -.3 (ML1+4@100℃), langsheng Co.
ACM-2212: mooney viscosity 40.+ -.5 (ML1+4@100℃), dumet rubber technologies Co., ltd.
WL-180: BET specific surface area 180m 2 And/g, win the company.
Si-50: hua Xiang chemical trade company, inc.
ZnO945: BET specific surface area 25.+ -.5 m 2 The trade name of/g, taixiang company.
Naphthenic oil 4006: xinjiang Kelamani company.
S-80: rubber master batch prepared from 80% of sulfur and 20% of EPDM rubber is available from Dongguan Euro New Material Co.
Accelerator DM: utilin, new Material technology, inc.
Accelerator D: utilin, new Material technology, inc.
Accelerator TS: utilin, new Material technology, inc.
Physical property data of the rubber outsole material are shown in table 6:
TABLE 6 physical Property data of rubber outsole Material
3) The attaching flow is shown in fig. 3:
description of implementation steps:
EVA sole: (1) cleaning: putting the EVA midsole into a cleaning assembly line, and after the working procedures of soaking liquid medicine (oxalic acid 2%/ethanol 10% and water 88%) +ultrasonic cleaning+clear water cleaning+air knife water scraping and the like, framing, placing and airing, wherein the assembly line temperature is as follows: the water washing time is more than 8 minutes at 50+/-5 ℃, and the air drying time is more than 4 hours. (2) Soaking: the EVA midsole after airing is put into midsole irradiation treating agent liquid medicine (treating agent component: solid content: 0.8-1.5%, including vinyl chloride-vinyl acetate resin, methyl methacrylate, acrylic acid, photoinitiator, etc., solvent: ethyl acetate, toluene, acetone, butanone) to be soaked for 5-10 seconds, and then is framed and aired for 30min. (3) And (3) irradiation: the EVA midsole is treated by the treating agent and then is irradiated by UV within 2 hours, the irradiation intensity of the irradiation machine (strong light for light soles, energy of 0.50-0.60W/cm) 2 The method comprises the steps of carrying out a first treatment on the surface of the Dim light for dark soles with energy of 0.42-0.50W/cm 2 。
Rubber sole: (1) cleaning: soaking with oxalic acid solution cleaner for 20-30 seconds to remove surface oil, and naturally airing for 4 hours. (2) And (3) an upper treating agent: brushing a treating agent on the dried rubber sole, wherein the treating agent comprises the following components: trichloroisocyanuric acid powder + solvent (toluene, acetone, butanone, ethyl acetate). (3) And (3) drying: putting the rubber sole on which the treating agent is applied on an oven assembly line for drying, wherein the temperature of the oven is 45-50 ℃, and the rotation speed of the assembly line is as follows: 350-450rad/min.
And (3) laminating: (1) brushing glue: brushing water-based PU glue on the treated EVA midsole and the treated rubber outsole. (2) And (3) drying: oven assembly line is advanced to the sole after the brush is glued and is dried, oven temperature: 60-70 ℃, oven assembly line rotating speed: 300-400rad/min. (3) And (3) laminating: the assembly line oven is in time laminated, oven temperature: 60-70 ℃, oven assembly line rotating speed: 300-400rad/min. The bonding temperature is usually kept above 50 ℃, and the glue ensures drying. (4) Pressing: the press outsole is finished within 60 seconds from the lamination to the press under the heat preservation environment (the temperature of a humidity preservation box is 45-50 ℃), and cold pressing is stopped: the pressure is firstly strong (the pressure is 35kg-40kg, the strong pressure is 7-8 seconds), and then the spot pressure is carried out (the pressure is 30kg-35kg, the spot pressure is 2-3 seconds).
The invention adopts the method described in GB/T21396-2008 to test the bonding strength of the sole of the roughening-free sports shoe, and the result is shown in Table 7:
table 7 results of adhesive strength test of the coarsely-removed sports sole
As can be seen from table 7 above: (1) The middle sole is not subjected to a roughening procedure before being attached. In general, the adhesive strength of the outsole in the sports shoe needs to be larger than 25N/mm, and the risk of the sole being glued is low. From the adhesive strength test data of various midsole formulas, even if the EVA foam midsole is pure, if the EVA foam midsole is directly attached to the rubber midsole without roughening, the final adhesive strength is less than 25N/mm, but the EVA foam midsole cannot be pure EVA, and nonpolar polymers like POE/OBC/EPDM/SEBS are added, so that the adhesive strength is lower (like comparative example 2+comparative example 4 or comparative example 3+comparative example 4);
(2) The adhesion of the EVA midsole formula without adding strong polar polymers such as ethylene acid ester-carbon monoxide copolymer, ethylene-acrylic acid copolymer and ethylene-methacrylic acid ionized resin and the like to the rubber outsole formula with or without adding polyacrylate ACM rubber is higher than that of the EVA midsole formula without adding ACM rubber, and the adhesion is continuously improved along with the increase of the addition amount of the ACM rubber, but the adhesion is higher than 25N/mm only when the addition amount of the ACM rubber is higher than 10 parts;
(3) The EVA midsole formula is added with one or more polymers with strong polarity such as ethylene-carbon monoxide copolymer, ethylene-acrylic acid copolymer, ethylene-methacrylic acid ionized resin and the like, and the bonding condition that the polyacrylate ACM rubber (comparative example 4) is not added in the rubber outsole formula is that the bonding strength of the ethylene-acrylic acid copolymer and the ethylene-methacrylic acid ionized resin with the strongest polarity is higher than that of the ethylene-carbon monoxide copolymer with the weaker polarity, and the bonding strength is higher as the addition amount of the polar polymer is larger;
(4) The EVA midsole formula is added with one or more polymers with strong polarity such as ethylene acid ester-carbon monoxide copolymer, ethylene-acrylic acid copolymer, ethylene-methacrylic acid ionized resin and the like, and the adhesive strength is improved to 30-43N/mm compared with that of the EVA midsole without the ACM rubber when the same EVA midsole formula is used for bonding with the ACM rubber (example 14);
(5) The two or three kinds of compound effects are better compared with the situation that one or more polymers such as ethylene acid ester-carbon monoxide copolymer, ethylene-acrylic acid copolymer, ethylene-methacrylic acid ionized resin and the like are added into the EVA foaming midsole. The compound proportion range is: 5-20 parts of ethylene acid ester-carbon monoxide copolymer, 1-15 parts of ethylene-acrylic acid copolymer and 1-10 parts of ethylene-methacrylic acid ionized resin;
(6) Therefore, the invention is beneficial to obtaining soles with higher bonding strength by comprehensively controlling the components of the midsole foaming material and the rubber outsole material, and greatly reduces the risk of avoiding rough bonding but not opening rubber.
As can be seen from the above embodiments, the present invention provides a roughening-free sports shoe sole comprising a midsole and an outsole; the midsole comprises the following raw materials in parts by weight: 30-50 parts of EVA, 0-20 parts of OBC, 10-20 parts of POE, 0-10 parts of SEBS, 0-10 parts of EPDM, 5-20 parts of ethylene-carbon monoxide copolymer, 1-15 parts of ethylene-acrylic acid copolymer, 1-10 parts of ethylene-methacrylic acid ionized resin, 0.5-1 part of peroxide cross-linking agent, 3.5 parts of foaming agent, 1-3 parts of zinc oxide, 0.8 part of stearic acid and 1 part of zinc stearate; the outsole comprises the following raw materials: 50-70 parts of natural rubber, 20-40 parts of butadiene rubber, 1-10 parts of polyacrylate rubber, 30-50 parts of white carbon black, 1.5 parts of silane coupling agent, 10 parts of softening oil, 3 parts of zinc oxide, 1.5 parts of thiazole accelerator, 0.6 part of diphenyl guanidine accelerator, 0.025 part of thiuram accelerator and 2.5 parts of sulfur. According to the invention, polymers such as ethylene acid ester-carbon monoxide copolymer, ethylene-acrylic acid copolymer, ethylene-methacrylic acid ionized resin and the like are added into the midsole foaming material for blending foaming, so that the polarity of the foaming midsole is greatly improved, and the roughening procedure of the midsole is saved; the addition of the polyacrylate rubber (ACM rubber) in the rubber outsole also improves the polarity of the rubber outsole, saves the roughening procedure of the outsole, avoids the roughening procedure of the midsole and the outsole, improves the production efficiency, reduces the production cost, also avoids the damage of dust in the roughening procedure to the health of operators, and truly achieves low carbon and environmental protection; the polarity of the midsole and the outsole is synchronously increased, the effect of coarse bonding without beating with the midsole is better realized, and the problem of easy glue opening of the midsole and the outsole is solved. The experimental results show that: the bonding strength of the sole of the roughening-free sports shoe provided by the invention is more than or equal to 30N/cm.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. An exercise sole without roughening, comprising a midsole and an outsole;
the midsole comprises the following raw materials in parts by weight:
30-50 parts of EVA, 0-20 parts of ethylene-butene block copolymer, 10-20 parts of ethylene-octene random copolymer, 0-10 parts of styrene-butadiene copolymer, 0-10 parts of EPDM, 5-20 parts of vinyl-acrylic ester-carbon monoxide terpolymer, 1-15 parts of ethylene-acrylic acid copolymer, 1-10 parts of ethylene-methacrylic acid ionizing resin, 0.5-1 part of peroxide crosslinking agent, 3.5 parts of foaming agent, 1-3 parts of zinc oxide, 0.8 part of stearic acid and 1 part of zinc stearate;
the outsole comprises the following raw materials:
50-70 parts of natural rubber, 20-40 parts of butadiene rubber, 1-10 parts of polyacrylate rubber, 30-50 parts of white carbon black, 1.5 parts of a silane coupling agent, 10 parts of softening oil, 3 parts of zinc oxide, 1.5 parts of a thiazole accelerator, 0.6 part of a diphenyl guanidine accelerator, 0.025 part of a thiuram accelerator and 2.5 parts of sulfur.
2. The roughening-free athletic sole of claim 1, wherein VA content in the EVA is 12-33 mol%;
the styrene structural unit in the styrene-butadiene copolymer is a hard segment, and the content of the hard segment in the styrene-butadiene copolymer is 13-33 mol%;
the EPDM has a crystallinity of <5%;
the content of acrylate in the vinyl-acrylate-carbon monoxide terpolymer is >20mol%;
the ethylene-acrylic acid copolymer has an acrylic acid content of >8%.
3. The roughening-free athletic sole of claim 1 wherein the EVA is selected from one or more of EVA33121, EVA26061 and EVA 7350M;
the vinyl-acrylate-carbon monoxide terpolymer is selected from Elvaloy AC 3427 and/or Elvaloy AC 1125;
the ethylene-acrylic acid copolymer is selected from Fusabond 514D and/or Nucrel 925;
the peroxide crosslinking agent is selected from dicumyl peroxide and/or 1, 4-di-tert-butyl peroxyisopropyl benzene;
the foaming agent is selected from one or more of azodicarbonamide, expanded microspheres and 4, 4-oxo-diphenyl sulfonyl hydrazine;
the ethylene-methacrylic acid ionizing resin is selected from ethylene-sodium methacrylate.
4. The roughening-free athletic shoe sole of claim 1, wherein the natural rubber has a mooney viscosity of 80±20 under test conditions of ml1+4@100 ℃;
the Mooney viscosity of the butadiene rubber is 45+/-3, and the test condition is ML1+4@100 ℃;
the Mooney viscosity of the polyacrylate rubber is 45+/-5, and the test condition is ML1+4@100 ℃.
5. The roughening-free sports shoe sole of claim 1, wherein the white carbon black has a specific surface area of 160-180 m 2 /g；
The silane coupling agent is selected from one or more of Si-50, KH550 and KH 570;
the softening oil is selected from paraffinic oil and/or naphthenic oil;
the accelerator is selected from the group consisting of mixtures of diphenyl guanidine, dibenzothiazyl disulfide and tetramethylthiuram monosulfide.
6. A method for preparing the roughening-free sports shoe sole according to any one of claims 1 to 5, comprising the following steps:
mixing EVA, ethylene-butene block copolymer, ethylene-octene random copolymer, styrene-butadiene copolymer, EPDM, vinyl-acrylic ester-carbon monoxide terpolymer, ethylene-acrylic acid copolymer and ethylene-methacrylic acid ionized resin, heating to 75-85 ℃, adding zinc oxide, stearic acid and zinc stearate, heating to 85-95 ℃, adding peroxide cross-linking agent and foaming agent, heating to 100-105 ℃, and uniformly mixing to obtain a mixed material; granulating the mixed materials, and foaming to obtain a semi-finished product; standing the semi-finished product, molding, and cooling to obtain a midsole foaming material;
mixing natural rubber, butadiene rubber and polyacrylate rubber, and banburying to obtain a rubber base material; discharging the rubber base material, standing for 4-8 hours, mixing with white carbon black, a silane coupling agent, softening oil and zinc oxide, and banburying again to obtain a sizing material; mixing the sizing material with thiazole accelerators, diphenyl guanidine accelerators, thiuram accelerators and sulfur, discharging tablets, and vulcanizing to obtain a outsole material;
and respectively processing the midsole foaming material and the outsole material, and then attaching to obtain the rough-free sports sole.
7. The preparation method according to claim 6, wherein the foaming temperature is 175 ℃ and the foaming time is 650-670 s;
the molding temperature is 175 ℃, and the molding time is 410-430 s.
8. The method according to claim 6, wherein the process of attaching the midsole foaming material and the outsole material after the respective treatments comprises:
cleaning, soaking and irradiating the midsole foaming material to obtain a midsole;
cleaning the outsole material, adding a treating agent, and drying to obtain an outsole;
and brushing the rubber on the midsole and the outsole respectively, drying, attaching and pressing.
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