CN110894317A - Preparation method of light wear-resistant sole material - Google Patents
Preparation method of light wear-resistant sole material Download PDFInfo
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- CN110894317A CN110894317A CN201911267316.6A CN201911267316A CN110894317A CN 110894317 A CN110894317 A CN 110894317A CN 201911267316 A CN201911267316 A CN 201911267316A CN 110894317 A CN110894317 A CN 110894317A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a preparation method of a light wear-resistant sole material, and particularly relates to the technical field of shoe materials, 1, 5-naphthalene diisocyanate is reacted with hydroxyl on the surface of nano-zinc composite aerogel through isocyanate groups, 1, 5-naphthalene diisocyanate is grafted to the surface of the nano-zinc composite aerogel, naphthalene rings and the isocyanate groups are introduced, wherein the isocyanate groups are reacted and crosslinked with the hydroxyl in saponified ethylene-vinyl acetate, so that the mechanical property of the obtained material is greatly improved, and meanwhile, the naphthalene rings are introduced into the obtained material through chemical bonds, so that the wear resistance of the obtained material is improved.
Description
Technical Field
The invention belongs to the technical field of shoe materials, and particularly relates to a preparation method of a light wear-resistant sole material.
Background
Shoes are articles commonly used in daily life, and soles are indispensable parts for manufacturing the shoes, wherein EVA (ethylene vinyl acetate) sports soles are popular among consumers and are accepted by the good plasticity, elasticity and processability of ethylene-vinyl acetate copolymers (EVA) because of the advantages of lightness, good elasticity, strong toughness and comfortable foot feel after entering the Chinese market, and foamed materials have the advantages of low density, good mechanical property, easy coloring and the like, so the EVA sports soles are widely applied to sole materials, but the EVA materials have the defect that the wear resistance is not as good as that of rubber shoe materials, so the application of parts of the EVA sports soles is limited.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a preparation method of a light wear-resistant sole material.
The invention is realized by the following technical scheme:
(1) ball-milling 10-12 parts by weight of nano zinc oxide at 80-100 ℃ for 10-20min, then adding the nano zinc oxide into 20-30 parts by weight of methyl cellulose solution with the mass fraction of 10-14%, carrying out ultrasonic dispersion at 30-35 ℃ and 40-42KHz for 20-30min, then adding 5-7 parts of kaolin, continuing to carry out ultrasonic treatment for 30-40min, carrying out freeze drying, and pulverizing the obtained powder to the particle size of 100-500nm to obtain a nano zinc oxide compound;
(2) adding 30-50 parts of tetraethyl orthosilicate into 40-60 parts of absolute ethyl alcohol, stirring for 20-30min at 35-40 ℃ and 200-0.01 rpm, then adding 3-4 parts of oxalic acid solution with the concentration of 0.007-0.01mol/L, stirring for 10-11h at 54-56 ℃ and 200-300rpm, then adding 1-2 parts of saturated ammonia water, stirring for 3-5min at 600-800rpm, then adding 10-12 parts of the nano zinc oxide compound obtained in the step (1), continuously stirring for 20-30min, standing for 2-3min at 30-36 ℃ in a forward direction, then standing for 2-3min in a reverse direction, then alternately soaking the obtained gel by using absolute ethyl alcohol and n-hexane for 10-11h each time, alternately soaking for 6-8 times, changing the forward and reverse directions of the gel when the solvent is replaced every time, then freeze-drying at-45 to-50 ℃, and crushing and ball-milling until the particle size is 100-500nm to obtain the nano-zinc composite aerogel;
(3) dissolving 4-5 parts of 1, 5-naphthalene diisocyanate in tetrahydrofuran with the volume 2-3 times of that of the 1, 5-naphthalene diisocyanate, stirring at the temperature of 50-60 ℃ and the speed of 400rpm for 8-10min, adding 10-12 parts of the nano zinc composite aerogel obtained in the step (2), continuously stirring for 5-10min, adding 0.04-0.05 part of triethanolamine, and reacting at the temperature of 83-87 ℃ and the speed of 500rpm for 3-5h to obtain the isocyanate grafted nano zinc composite aerogel.
(4) Adding 80-100 parts of ethylene-vinyl acetate resin into 150-200 parts of toluene, stirring for 20-30min, adding 15-20 parts of sodium hydroxide ethanol solution with the mass fraction of 3-5%, refluxing and condensing for 6-9h at the temperature of 115 ℃ and the speed of 400rpm of 113-115 ℃, cooling, neutralizing by using hydrochloric acid solution with the mass fraction of 2-3%, then adding 10-15 parts of the obtained product in the step (3) and 0.5-0.6 part of triethanolamine, reacting for 5-8h at the temperature of 86-88 ℃ and the speed of 500rpm of 400-53 ℃, removing the solvent by rotary evaporation, drying the obtained product in vacuum at the temperature of 50-53 ℃, adding the obtained product into an internal mixer together with 10-15 parts of glycerol and 15-18 parts of ethylene acrylic acid for plastication for 5-8min, then transferring into a plasticator, adding 5-7 parts of dicumyl peroxide into a plasticator, 4-6 parts of azodicarbonamide, open milling for 15-20min, and foaming at 176-178 ℃.
The invention has the beneficial effects that: the sole material prepared by the method has good wear resistance, excellent mechanical property, light weight, heat preservation, lightness and convenience. Firstly, preparing a compound by utilizing nano zinc oxide, methyl cellulose and kaolin, and combining the viscosity of the methyl cellulose and the light weight characteristic of the kaolin to obtain composite particles with light weight and good dispersibility; then coating a layer of silicon dioxide aerogel on the surface of the nano zinc oxide compound, introducing a large number of hydroxyl groups to the surface of the nano zinc oxide compound, and simultaneously enabling the obtained product to have higher hardness, wear resistance and lower density; 1, 5-naphthalene diisocyanate is reacted with hydroxyl on the surface of the nano-zinc composite aerogel through isocyanate groups, 1, 5-naphthalene diisocyanate is grafted to the surface of the nano-zinc composite aerogel, naphthalene rings and the isocyanate groups are introduced, wherein the isocyanate groups are reacted and crosslinked with the hydroxyl in the saponified ethylene-vinyl acetate, the mechanical property of the obtained material is greatly improved, and meanwhile, the naphthalene rings are introduced into the obtained material through chemical bonds, so that the wear resistance of the obtained material is improved.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
(1) Ball-milling 11 parts by weight of nano zinc oxide at 90 ℃ for 15min, then adding the nano zinc oxide into 25 parts by weight of methyl cellulose solution with the mass fraction of 12%, carrying out ultrasonic dispersion at 32 ℃ and 41KHz for 25min, then adding 6 parts of kaolin, continuing to carry out ultrasonic treatment for 35min, carrying out freeze drying, and crushing the obtained product until the particle size is 100-500nm to obtain a nano zinc oxide compound;
(2) adding 40 parts of tetraethyl orthosilicate into 50 parts of absolute ethyl alcohol, stirring at 38 ℃ and 260rpm for 25min, then adding 4 parts of oxalic acid solution with the concentration of 0.009mol/L, then stirring at 55 ℃ and 250rpm for 11h, then adding 2 parts of saturated ammonia water, stirring at 700rpm for 4min, then adding 11 parts of the nano zinc oxide compound obtained in the step (1), continuously stirring for 25min, forward standing at 35 ℃ for 3min, then reversely standing for 3min, then alternately soaking the obtained gel by using the absolute ethyl alcohol and the normal hexane for 10h and 7 times each time, changing the forward and reverse directions of the gel when the solvent is changed each time, then freeze-drying at-47 ℃, crushing and ball-milling until the particle size is 100-500nm, and obtaining the nano zinc compound aerogel;
(3) and (2) dissolving 5 parts of 1, 5-naphthalene diisocyanate in tetrahydrofuran with the volume 3 times of that of the 1, 5-naphthalene diisocyanate, stirring at 55 ℃ and 350rpm for 9min, adding 11 parts of the nano zinc composite aerogel obtained in the step (2), continuously stirring for 8min, adding 0.05 part of triethanolamine, and reacting at 85 ℃ and 450rpm for 4h to obtain the isocyanate grafted nano zinc composite aerogel.
(4) Adding 90 parts of ethylene-vinyl acetate resin into 180 parts of toluene, stirring for 25min, adding 18 parts of ethanol solution of sodium hydroxide with the mass fraction of 4%, refluxing and condensing at 114 ℃ and 300rpm for 8h, cooling, neutralizing by using hydrochloric acid solution with the mass fraction of 3%, adding 12 parts of the product obtained in the step (3) and 0.55 part of triethanolamine, reacting at 87 ℃ and 450rpm for 7h, removing the solvent by rotary evaporation, drying the product in vacuum at 52 ℃, adding the dried product, 13 parts of glycerol and 16 parts of ethylene acrylic acid into an internal mixer for plastication for 7min, transferring the plastication into a plasticator, adding 6 parts of dicumyl peroxide and 5 parts of azodicarbonamide, opening for 18min, and then foaming at 177 ℃.
The tensile strength was 4.2MPa, the tear strength was 26.8kg/cm, and the Akron abrasion index was 9.3.
Example 2
(1) Ball-milling 11 parts by weight of nano zinc oxide at 90 ℃ for 15min, then adding the nano zinc oxide into 25 parts by weight of methyl cellulose solution with the mass fraction of 12%, carrying out ultrasonic dispersion at 32 ℃ and 41KHz for 25min, then adding 6 parts of kaolin, continuing to carry out ultrasonic treatment for 35min, carrying out freeze drying, and crushing the obtained product until the particle size is 100-500nm to obtain a nano zinc oxide compound;
(2) dissolving 5 parts of 1, 5-naphthalene diisocyanate in tetrahydrofuran with the volume 3 times of that of the 1, 5-naphthalene diisocyanate, stirring at 55 ℃ and 350rpm for 9min, adding 11 parts of the nano zinc composite obtained in the step (1), continuously stirring for 8min, adding 0.05 part of triethanolamine, and reacting at 85 ℃ and 450rpm for 4h to obtain the isocyanate grafted nano zinc composite aerogel.
(3) Adding 90 parts of ethylene-vinyl acetate resin into 180 parts of toluene, stirring for 25min, adding 18 parts of ethanol solution of sodium hydroxide with the mass fraction of 4%, refluxing and condensing at 114 ℃ and 300rpm for 8h, cooling, neutralizing by using hydrochloric acid solution with the mass fraction of 3%, adding 12 parts of the product obtained in the step (2) and 0.55 part of triethanolamine, reacting at 87 ℃ and 450rpm for 7h, removing the solvent by rotary evaporation, drying the product in vacuum at 52 ℃, adding the dried product, 13 parts of glycerol and 16 parts of ethylene acrylic acid into an internal mixer for plastication for 7min, transferring the plastication into a plasticator, adding 6 parts of dicumyl peroxide and 5 parts of azodicarbonamide, opening for 18min, and then foaming at 177 ℃.
The tensile strength was 2.5MPa, the tear strength was 20.4kg/cm, and the Akron abrasion index was 11.6.
Example 3
(1) Ball-milling 11 parts by weight of nano zinc oxide at 90 ℃ for 15min, then adding the nano zinc oxide into 25 parts by weight of methyl cellulose solution with the mass fraction of 12%, carrying out ultrasonic dispersion at 32 ℃ and 41KHz for 25min, then adding 6 parts of kaolin, continuing to carry out ultrasonic treatment for 35min, carrying out freeze drying, and crushing the obtained powder until the particle size is 100-500nm to obtain a nano zinc oxide compound;
(2) adding 40 parts of tetraethyl orthosilicate into 50 parts of absolute ethyl alcohol, stirring at 38 ℃ and 260rpm for 25min, then adding 4 parts of oxalic acid solution with the concentration of 0.009mol/L, then stirring at 55 ℃ and 250rpm for 11h, then adding 2 parts of saturated ammonia water, stirring at 700rpm for 4min, then adding 11 parts of the nano zinc oxide compound obtained in the step (1), continuously stirring for 25min, forward standing at 35 ℃ for 3min, then reversely standing for 3min, then alternately soaking the obtained gel by using the absolute ethyl alcohol and the normal hexane for 10h and 7 times each time, changing the forward and reverse directions of the gel when the solvent is changed each time, then freeze-drying at-47 ℃, crushing and ball-milling until the particle size is 100-500nm, and obtaining the nano zinc compound aerogel;
(3) adding 90 parts of ethylene-vinyl acetate resin into 180 parts of toluene, stirring for 25min, adding 18 parts of ethanol solution of sodium hydroxide with the mass fraction of 4%, refluxing and condensing at 114 ℃ and 300rpm for 8h, cooling, neutralizing by using hydrochloric acid solution with the mass fraction of 3%, adding 12 parts of the product obtained in the step (2) and 0.55 part of triethanolamine, reacting at 87 ℃ and 450rpm for 7h, removing the solvent by rotary evaporation, drying the product in vacuum at 52 ℃, adding the dried product, 13 parts of glycerol and 16 parts of ethylene acrylic acid into an internal mixer for plastication for 7min, transferring the plastication into a plasticator, adding 6 parts of dicumyl peroxide and 5 parts of azodicarbonamide, opening for 18min, and then foaming at 177 ℃.
The tensile strength was 2.3MPa, the tear strength was 19.7kg/cm, and the Akron abrasion index was 11.7.
The specific test method is as follows:
and (3) testing tensile property: according to the national GB/T1040-92 standard, the testing environment temperature is 22-28 ℃, the relative humidity is 20% -30% RH, and the testing speed is 100 mm/min.
And (3) testing the tearing performance: the type C tear test was carried out according to GB/T529-1999 standard at a test speed of 100 mm/min.
And (3) testing the wear resistance: the Akron abrasion index is tested according to GB/T9867-2008 standard, and the lower the value, the stronger the abrasion resistance is.
Each set was set to 5 parallel runs and the average was taken.
Claims (3)
1. The preparation method of the light wear-resistant sole material is characterized by comprising the following steps of:
(1) ball-milling 10-12 parts by weight of nano zinc oxide at 80-100 ℃ for 10-20min, then adding the nano zinc oxide into 20-30 parts by weight of methyl cellulose solution with the mass fraction of 10-14%, carrying out ultrasonic dispersion at 30-35 ℃ and 40-42KHz for 20-30min, then adding 5-7 parts of kaolin, continuing to carry out ultrasonic treatment for 30-40min, carrying out freeze drying, and pulverizing the obtained powder to the particle size of 100-500nm to obtain a nano zinc oxide compound;
(2) adding 30-50 parts of tetraethyl orthosilicate into 40-60 parts of absolute ethyl alcohol, stirring for 20-30min at 35-40 ℃ and 200-0.01 rpm, then adding 3-4 parts of oxalic acid solution with the concentration of 0.007-0.01mol/L, stirring for 10-11h at 54-56 ℃ and 200-300rpm, then adding 1-2 parts of saturated ammonia water, stirring for 3-5min at 600-800rpm, then adding 10-12 parts of the nano zinc oxide compound obtained in the step (1), continuously stirring for 20-30min, standing for 2-3min at 30-36 ℃ in a forward direction, then standing for 2-3min in a reverse direction, then alternately soaking the obtained gel by using absolute ethyl alcohol and n-hexane for 10-11h each time, alternately soaking for 6-8 times, then freeze-drying at-45-50 ℃, and grinding and ball-milling until the particle size is 100-500nm to obtain the nano-zinc composite aerogel;
(3) further processing the nano-zinc composite aerogel obtained in the step (2) to obtain isocyanate grafted nano-zinc composite aerogel;
(4) adding 80-100 parts of ethylene-vinyl acetate resin into 150-200 parts of toluene, stirring for 20-30min, adding 15-20 parts of sodium hydroxide ethanol solution with the mass fraction of 3-5%, refluxing and condensing for 6-9h at the temperature of 115 ℃ and the speed of 400rpm of 113-115 ℃, cooling, neutralizing by using hydrochloric acid solution with the mass fraction of 2-3%, then adding 10-15 parts of the obtained product in the step (3) and 0.5-0.6 part of triethanolamine, reacting for 5-8h at the temperature of 86-88 ℃ and the speed of 500rpm of 400-53 ℃, removing the solvent by rotary evaporation, drying the obtained product in vacuum at the temperature of 50-53 ℃, adding the obtained product into an internal mixer together with 10-15 parts of glycerol and 15-18 parts of ethylene acrylic acid for plastication for 5-8min, then transferring into a plasticator, adding 5-7 parts of dicumyl peroxide into a plasticator, 4-6 parts of azodicarbonamide, open milling for 15-20min, and foaming at 176-178 ℃.
2. The method for preparing a lightweight wear-resistant sole material according to claim 1, wherein the alternate soaking in step (2) is to change the forward and reverse directions of the gel each time the solvent is changed.
3. The preparation method of the lightweight wear-resistant sole material as claimed in claim 1, wherein the specific treatment method in step (3) is as follows: dissolving 4-5 parts of 1, 5-naphthalene diisocyanate in tetrahydrofuran with the volume 2-3 times of that of the 1, 5-naphthalene diisocyanate, stirring at the temperature of 50-60 ℃ and the speed of 400rpm for 8-10min, adding 10-12 parts of the nano zinc composite aerogel obtained in the step (2), continuously stirring for 5-10min, adding 0.04-0.05 part of triethanolamine, and reacting at the temperature of 83-87 ℃ and the speed of 500rpm for 3-5h to obtain the isocyanate grafted nano zinc composite aerogel.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112265330A (en) * | 2020-11-05 | 2021-01-26 | 杭州盛得新材料有限公司 | Fabric laminate with recycled modified PVB and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112265330A (en) * | 2020-11-05 | 2021-01-26 | 杭州盛得新材料有限公司 | Fabric laminate with recycled modified PVB and preparation method thereof |
| CN112265330B (en) * | 2020-11-05 | 2021-06-25 | 杭州盛得新材料有限公司 | Fabric laminate with recycled modified PVB and preparation method thereof |
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