CN111253673A - High-elastic wear-resistant rubber sole material - Google Patents
High-elastic wear-resistant rubber sole material Download PDFInfo
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- CN111253673A CN111253673A CN202010246427.5A CN202010246427A CN111253673A CN 111253673 A CN111253673 A CN 111253673A CN 202010246427 A CN202010246427 A CN 202010246427A CN 111253673 A CN111253673 A CN 111253673A
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- 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
- C08J9/30—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by mixing gases into liquid compositions or plastisols, e.g. frothing with air
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
- B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
- B29B7/12—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with single shaft
- B29B7/16—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with single shaft with paddles or arms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/22—Component parts, details or accessories; Auxiliary operations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/22—Component parts, details or accessories; Auxiliary operations
- B29B7/26—Component parts, details or accessories; Auxiliary operations for discharging, e.g. doors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/22—Component parts, details or accessories; Auxiliary operations
- B29B7/28—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
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- 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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Abstract
The invention discloses a high-elasticity wear-resistant rubber sole material, which is prepared by selecting chlorohydrin rubber with excellent elasticity and air tightness and isoprene rubber with high elasticity and good tensile strength as main rubber components, using EVA particles as a main resin component, matching with an elastomer olefin block copolymer, a hydrophobic wear-resistant agent and PVDF resin powder, using sodium dodecyl sulfate as a foaming agent and magnesium oxide as a flame retardant, and obtaining a rubber material with good elasticity, light weight, high wear resistance, tear resistance and high water resistance under the action of a crosslinking agent, a vulcanization accelerator and a vulcanization activator, wherein the rubber material is suitable for being used as a material for wear-resistant outdoor shoes; during preparation, a matched internal mixer is adopted for high-temperature pressurization and internal mixing, and the rubber sole material with high uniformity and high purity is obtained through sheet discharging, extrusion and granulation.
Description
Technical Field
The invention relates to the technical field of rubber materials for shoes, in particular to a high-elasticity wear-resistant rubber sole material.
Background
The rubber has the advantages of good elasticity, high strength and strong wear resistance, is more suitable to be used as a raw material of the sole, but has poor oxidation resistance, cannot prevent fire and limits the application to a certain extent. In order to solve the above problems, plastics are often added or the amount of synthetic rubber in the raw materials is increased, so that although the performance of the sole material can be enhanced, the overall comfort of the sole material is reduced, and the hardness of the sole material is increased easily, which makes the sole material unsuitable for long-term wearing.
The patent of publication No. CN104788750A provides a high-elasticity high-wear-resistance rubber sole and a preparation method thereof, which is prepared from natural rubber, talcum powder, carbon tetraiodide, polyacetylene, polyethylene resin, a defoaming agent, a plasticizer, wear-resistant particles and white factice. The sole has the characteristics of softness, comfort, low carbon, environmental protection, skid resistance, wear resistance and low temperature resistance. The patent of publication No. CN109337181A discloses an ultra-light high-elasticity wear-resistant sole and a preparation process, the sole is composed of 75-85% of rubber-plastic composition and 18-22% of rubber-plastic auxiliary agent, the rubber-plastic composition is composed of ethylene-vinyl acetate copolymer, isoprene rubber, ethylene-methacrylic acid copolymer and olefin block copolymer; the rubber-plastic auxiliary agent component is composed of wear-resisting agent, filling agent, vulcanization accelerator, vulcanization activator, cross-linking agent, foaming agent and color developing agent. The following problems are found to remain: 1) rubber materials with good elasticity, light weight, high wear resistance, tear resistance and high water resistance cannot be obtained, and rubber sole materials with high uniformity and high purity cannot be prepared; 2) the common wear-resistant filler cannot improve the hydrophobicity through modification so as to further improve the waterproof performance of the rubber material; 3) in the preparation process, the internal mixer cannot promote the circulation and the sufficient shearing and crushing of materials, and the quality of rubber materials cannot be guaranteed.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a high-elasticity wear-resistant rubber sole material.
By selecting chlorohydrin rubber with excellent elasticity and air tightness and isoprene rubber with high elasticity and good tensile strength as main rubber components, EVA particles as main resin components, elastomer olefin block copolymer, hydrophobic wear-resisting agent and PVDF resin powder, sodium dodecyl sulfate as a foaming agent and magnesium oxide as a flame retardant, under the action of a crosslinking agent, a vulcanization accelerator and a vulcanization activator, the rubber material with good elasticity, light weight, high wear resistance, tear resistance and high water resistance is obtained and is suitable for being used as a material for wear-resistant outdoor shoes; during preparation, a matched internal mixer is adopted for high-temperature pressurization and internal mixing, and the rubber sole material with high uniformity and high purity is obtained through sheet discharging, extrusion and granulation.
As the surfaces of the nano silicon dioxide and the nano titanium dioxide contain hydroxyl functional groups, the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane is hydrolyzed to obtain Si-OH groups, chemical bonds of Si-O-Si are obtained through condensation reaction, carbon-carbon double bonds of styrene are introduced to the surfaces of nano particles of the silicon dioxide and the titanium dioxide, and are subjected to free radical polymerization with styrene monomers under the action of an inorganic peroxide initiator ammonium persulfate to obtain the composite microsphere with the silicon dioxide and the titanium dioxide particles as cores and the polystyrene as shells, thereby exerting good hydrophobic and wear-resistant properties.
The telescopic rod is driven by the cylinder to stretch up and down, the pressurizing plate is driven to move in the vertical direction, so that the air pressure in the extrusion cavity is adjusted, the pressure is injected into the stirring and shearing cavity, meanwhile, the pressure gauge can monitor the air pressure in the stirring and shearing cavity at any time, and the accuracy and timeliness of air pressure control are improved; the first belt pulley is driven to rotate through the servo motor, the belt and the second belt pulley are driven to rotate, and the stirring shaft drives the stirring frame and the shearing blade to mix, stir and shear the materials; the ejection of compact board that the slope set up has made things convenient for the ejection of compact of rubber material, and the material that returns through second valve, return pipe simultaneously falls along the discharge gate under the cylinder drives the air pressure that the pressure plate downwardly moving produced, has promoted the circulation of material and has fully sheared the smashing, has improved rubber materials's purity.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a high-elasticity wear-resistant rubber sole material which is prepared from the following components in parts by weight: 15-22 parts of chlorohydrin rubber, 45-60 parts of EVA (ethylene-vinyl acetate copolymer) particles, 8-15 parts of isoprene rubber, 25-36 parts of talcum powder, 8-13 parts of olefin block copolymer, 3.5-6 parts of hydrophobic wear-resisting agent, 5-10 parts of PVDF (polyvinylidene fluoride) resin powder, 1.5-3 parts of sodium dodecyl sulfate, 1-2 parts of magnesium oxide, 1-3 parts of crosslinking agent, 2.2-3.6 parts of vulcanization accelerator and 2.5-3.5 parts of vulcanization activator;
wherein the density of EAV particles is 0.95-0.96g/cm3The tensile breaking strength is 142-146kg/cm2The tensile elongation at break is 700-800%; the density of the olefin block copolymer is 1.29 to 1.31g/cm3The tensile strength is 9.68-9.73MPa, and the elongation at break is 400-430%; the density of the PVDF resin powder is 1.75-1.77g/cm3The thermal decomposition temperature is 385-390 ℃.
As a further aspect of the present invention, the hydrophobic anti-wear agent is prepared by the following method: adding 20-30 parts of nano silicon dioxide and 6-11 parts of nano titanium dioxide into 800 parts of 600-one-wall dimethyl carbonate, ultrasonically dispersing for 20-30min, adding into a reaction bottle, stirring and refluxing at the temperature of 92-95 ℃, dropwise adding 35-50 parts of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, performing reflux reaction for 40-50min after dropwise adding, slowly dropwise adding 25-36 parts of styrene, dropwise adding 10-20 parts of ammonium persulfate, and stirring and reacting for 2-2.5 hours; filtering, drying at low temperature, and grinding.
As a further embodiment of the invention, the cross-linking agent is one or more of dicumyl peroxide, dicumyl hydroperoxide, benzoyl peroxide, 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and di-tert-butyl diisopropylbenzene peroxide.
As a further scheme of the invention, the vulcanization accelerator is stearic acid, and the vulcanization activator is calcium stearate.
As a further scheme of the invention, the preparation method of the high-elasticity wear-resistant rubber sole material comprises the following steps:
s1, adding chlorohydrin rubber, EVA particles, isoprene rubber, olefin block copolymer, PVDF resin powder, vulcanization accelerator and vulcanization activator into a stirring and shearing cavity along a feed hopper of an internal mixer, driving a first belt pulley to rotate by a servo motor, driving a belt and a second belt pulley to rotate, and driving a stirring frame and a shearing blade to mix, stir and shear the materials by a stirring shaft; the cylinder drives the telescopic rod to stretch up and down to drive the pressurizing plate to move in the vertical direction so as to adjust the air pressure in the extrusion cavity and inject the pressure into the stirring and shearing cavity; carrying out heat preservation and banburying at the temperature of 210 ℃ and 220 ℃ for 20-30min to obtain a mixture a;
s2, adding talcum powder, hydrophobic wear-resistant agent and magnesium oxide into the mixture a, heating the internal mixer to 190 ℃ plus materials, carrying out heat preservation and internal mixing for 5-10min, heating to 200 ℃ plus materials, carrying out heat preservation and internal mixing for 10-15min, adding sodium dodecyl sulfate and cross-linking agent, heating the internal mixer to 220 ℃ plus materials, continuing internal mixing for 20-30min, and carrying out sheet discharging, extrusion and granulation to obtain the high-elasticity wear-resistant rubber sole material.
As a further scheme of the invention, the internal mixer comprises a reaction shell, an anti-seismic base and a pressurizing shell, wherein a funnel-shaped extrusion cavity is arranged above an inner cavity of the reaction shell, a stirring and shearing cavity is arranged below the inner cavity, the bottom of the extrusion cavity is communicated with the top of the stirring and shearing cavity, a cylinder with a telescopic rod vertically downward is arranged at the top of the extrusion cavity, the bottom of the telescopic rod of the cylinder is connected with a pressurizing plate, the pressurizing plate is cuboid, and the length of the cross section of the pressurizing plate is smaller than that of the cross section of the extrusion; the top of the side wall of the stirring and shearing cavity is connected with a pressure gauge and a feed hopper, the bottom of the other side wall is provided with a servo motor, a motor shaft of the servo motor is coaxially connected with a first belt pulley, a second belt pulley is arranged above the first belt pulley, and a belt is arranged around the peripheries of the first belt pulley and the second belt pulley.
As a further scheme of the invention, the two sides of the bottom of the stirring and shearing cavity are obliquely provided with discharge plates, and the center position of the bottom of the stirring and shearing cavity is connected with a discharge pipe obliquely extending out of the reaction shell through a first valve; one of the discharge plates is connected with a second valve through a return pipe, and the return pipe extends into the inner cavity at the top of the stirring and shearing cavity after extending through the outer wall of the stirring and shearing cavity; a plurality of discharge ports are arranged on the material returning pipe extending into the inner cavity of the top part at equal intervals.
The invention has the beneficial effects that:
1. the high-elasticity wear-resistant rubber sole material selects chlorohydrin rubber with excellent elasticity and air tightness and isoprene rubber with high elasticity and good tensile strength as main rubber components, EVA particles are used as main resin components, elastomer olefin block copolymer, hydrophobic wear-resistant agent and PVDF resin powder are matched, sodium dodecyl sulfate is used as foaming agent, magnesium oxide is used as flame retardant, and under the action of crosslinking agent, vulcanization accelerator and vulcanization activator, the high-elasticity wear-resistant rubber sole material is obtained and is suitable for being used as a material of wear-resistant outdoor shoes; the preparation method comprises the steps of carrying out high-temperature pressurization and banburying by using a matched banbury mixer, carrying out sheet discharging and extrusion granulation to obtain the rubber sole material with high uniformity and purity, wherein the Shore hardness A reaches 52-59 in a performance test, and the DIN abrasion resistance reaches 74-86cm3The tensile strength reaches 56.2-57.4MPa, and the rebound resilience reaches 57.9-59.7%.
2. According to the preparation method of the hydrophobic wear-resisting agent, the surfaces of the nano silicon dioxide and the nano titanium dioxide contain hydroxyl functional groups, the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane is hydrolyzed to obtain Si-OH groups, chemical bonds of Si-O-Si are obtained through condensation reaction, carbon-carbon double bonds of styrene are introduced to the surfaces of nano particles of the silicon dioxide and the titanium dioxide, and are subjected to free radical polymerization with styrene monomers under the action of an inorganic peroxide initiator ammonium persulfate to obtain the composite microspheres with the silicon dioxide and the titanium dioxide particles as cores and the polystyrene as shells, so that good hydrophobic and wear-resisting properties are exerted.
3. In the banburying process of the rubber material, the telescopic rod is driven by the air cylinder to stretch up and down, and the pressurizing plate is driven to move in the vertical direction so as to adjust the air pressure in the extrusion cavity, so that the pressure is injected into the stirring and shearing cavity, and meanwhile, the pressure gauge can monitor the air pressure in the stirring and shearing cavity at any time, thereby improving the accuracy and timeliness of air pressure control; the first belt pulley is driven to rotate through the servo motor, the belt and the second belt pulley are driven to rotate, and the stirring shaft drives the stirring frame and the shearing blade to mix, stir and shear the materials; the ejection of compact board that the slope set up has made things convenient for the ejection of compact of rubber material, and the material that returns through second valve, return pipe simultaneously falls along the discharge gate under the cylinder drives the air pressure that the pressure plate downwardly moving produced, has promoted the circulation of material and has fully sheared the smashing, has improved rubber materials's purity.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of the internal mixer of the present invention.
Fig. 2 is a partial enlarged view of the invention at a in fig. 1.
FIG. 3 is a schematic view of the connection structure of the stirring shaft, the stirring frame and the shear blade of the present invention.
In the figure: 1. a reaction housing; 2. a shock-resistant base; 3. a pressurized housing; 4. an extrusion chamber; 5. a stirring and shearing cavity; 6. a cylinder; 7. a pressurizing plate; 8. a pressure gauge; 9. a feed hopper; 10. a servo motor; 11. a first pulley; 12. a second pulley; 13. a belt; 14. a stirring shaft; 15. a stirring frame; 16. a shearing blade; 17. a crushing knife; 18. a discharge plate; 19. a first valve; 20. a discharge pipe; 21. a material returning pipe; 22. a second valve; 23. a discharge port; 24. clamping a hoop; 25. a hydraulic damper.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A high-elasticity wear-resistant rubber sole material is prepared from the following components in parts by weight: 17 parts of chlorohydrin rubber, 53 parts of EVA (ethylene-vinyl acetate copolymer) particles, 12 parts of isoprene rubber, 30 parts of talcum powder, 12 parts of olefin block copolymer, 4.5 parts of hydrophobic wear-resisting agent, 8 parts of PVDF (polyvinylidene fluoride) resin powder, 2.2 parts of sodium dodecyl sulfate, 1.5 parts of magnesium oxide, 2 parts of crosslinking agent, 3.3 parts of vulcanization accelerator and 2.7 parts of vulcanization activator;
wherein the density of EAV particles is 0.95-0.96g/cm3The tensile breaking strength is 142-146kg/cm2The tensile elongation at break is 700-800%; the density of the olefin block copolymer is 1.29 to 1.31g/cm3The tensile strength is 9.68-9.73MPa, and the elongation at break is 400-430%; the density of the PVDF resin powder is 1.75-1.77g/cm3The thermal decomposition temperature is 385-390 ℃.
The preparation method of the hydrophobic anti-wear agent comprises the following steps: adding 26 parts by weight of nano silicon dioxide and 9 parts by weight of nano titanium dioxide into 700 parts by weight of dimethyl carbonate, performing ultrasonic dispersion for 26min, adding the mixture into a reaction bottle, stirring and refluxing at 93 ℃, dropwise adding 46 parts by weight of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, performing reflux reaction for 46min after the dropwise adding is finished, slowly dropwise adding 30 parts by weight of styrene, dropwise adding 16 parts by weight of ammonium persulfate, and performing stirring reaction for 2.2 hours; filtering, drying at low temperature, and grinding. The cross-linking agent is hydrogen peroxide diisopropylbenzene. The vulcanization accelerator is stearic acid, and the vulcanization activator is calcium stearate.
The preparation method of the high-elasticity wear-resistant rubber sole material comprises the following steps:
s1, adding chlorohydrin rubber, EVA particles, isoprene rubber, olefin block copolymer, PVDF resin powder, vulcanization accelerator and vulcanization activator into a stirring and shearing cavity 5 along a feed hopper 9 of an internal mixer, driving a first belt pulley 11 to rotate by a servo motor 10, driving a belt 13 and a second belt pulley 12 to rotate, and driving a stirring frame 15 and a shearing blade 16 to mix, stir and shear the materials by a stirring shaft 14; the cylinder 6 drives the telescopic rod to stretch up and down and drives the pressurizing plate 7 to move in the vertical direction so as to adjust the air pressure in the extrusion cavity 4 and inject the pressure into the stirring and shearing cavity 5; carrying out heat preservation and banburying at the temperature of 216 ℃ for 26min to obtain a mixture a;
s2, adding talcum powder, hydrophobic wear-resistant agent and magnesium oxide into the mixture a, heating the mixture a to 188 ℃ by an internal mixer, carrying out heat preservation and banburying for 7min, heating to 198 ℃, carrying out heat preservation and banburying for 12min, adding sodium dodecyl sulfate and cross-linking agent, heating the internal mixer to 216 ℃, continuing banburying for 25min, and carrying out sheet extrusion, extrusion and granulation to obtain the high-elasticity wear-resistant rubber sole material.
Example 2
A high-elasticity wear-resistant rubber sole material is prepared from the following components in parts by weight: 21 parts of chlorohydrin rubber, 55 parts of EVA (ethylene-vinyl acetate copolymer) particles, 14 parts of isoprene rubber, 32 parts of talcum powder, 12 parts of olefin block copolymer, 5.5 parts of hydrophobic wear-resisting agent, 8 parts of PVDF (polyvinylidene fluoride) resin powder, 2.5 parts of sodium dodecyl sulfate, 1.8 parts of magnesium oxide, 2.5 parts of crosslinking agent, 3.3 parts of vulcanization accelerator and 3.0 parts of vulcanization activator;
wherein the density of EAV particles is 0.95-0.96g/cm3The tensile breaking strength is 142-146kg/cm2The tensile elongation at break is 700-800%; the density of the olefin block copolymer is 1.29 to 1.31g/cm3The tensile strength is 9.68-9.73MPa, and the elongation at break is 400-430%; the density of the PVDF resin powder is 1.75-1.77g/cm3The thermal decomposition temperature is 385-390 ℃.
The preparation method of the hydrophobic anti-wear agent comprises the following steps: adding 28 parts by weight of nano silicon dioxide and 10 parts by weight of nano titanium dioxide into 750 parts by weight of dimethyl carbonate, performing ultrasonic dispersion for 28min, adding the mixture into a reaction bottle, stirring and refluxing at 95 ℃, dropwise adding 45 parts by weight of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, performing reflux reaction for 48min after the dropwise adding is finished, slowly dropwise adding 33 parts by weight of styrene, dropwise adding 15 parts by weight of ammonium persulfate, and performing stirring reaction for 2.3 hours; filtering, drying at low temperature, and grinding. The cross-linking agent is formed by mixing dicumyl peroxide and di-tert-butylperoxydiisopropylbenzene according to the mass ratio of 1: 1. The vulcanization accelerator is stearic acid, and the vulcanization activator is calcium stearate.
The preparation method of the high-elasticity wear-resistant rubber sole material comprises the following steps:
s1, adding chlorohydrin rubber, EVA particles, isoprene rubber, olefin block copolymer, PVDF resin powder, vulcanization accelerator and vulcanization activator into a stirring and shearing cavity 5 along a feed hopper 9 of an internal mixer, driving a first belt pulley 11 to rotate by a servo motor 10, driving a belt 13 and a second belt pulley 12 to rotate, and driving a stirring frame 15 and a shearing blade 16 to mix, stir and shear the materials by a stirring shaft 14; the cylinder 6 drives the telescopic rod to stretch up and down and drives the pressurizing plate 7 to move in the vertical direction so as to adjust the air pressure in the extrusion cavity 4 and inject the pressure into the stirring and shearing cavity 5; keeping the temperature at 218 ℃ and banburying for 25min to obtain a mixture a;
s2, adding talcum powder, hydrophobic wear-resistant agent and magnesium oxide into the mixture a, heating the mixture a to 190 ℃ by an internal mixer, carrying out heat preservation and banburying for 10min, heating the mixture to 200 ℃, carrying out heat preservation and banburying for 15min, adding sodium dodecyl sulfate and cross-linking agent, heating the internal mixer to 216 ℃, continuing banburying for 28min, and carrying out sheet extrusion, extrusion and granulation to obtain the high-elasticity wear-resistant rubber sole material.
Example 3
A high-elasticity wear-resistant rubber sole material is prepared from the following components in parts by weight: 21 parts of chlorohydrin rubber, 56 parts of EVA particles, 13 parts of isoprene rubber, 35 parts of talcum powder, 12 parts of olefin block copolymer, 5.2 parts of hydrophobic wear-resisting agent, 9 parts of PVDF resin powder, 2.8 parts of sodium dodecyl sulfate, 1.6 parts of magnesium oxide, 2.5 parts of crosslinking agent, 3.5 parts of vulcanization accelerator and 3.2 parts of vulcanization activator;
wherein the density of EAV particles is 0.95-0.96g/cm3The tensile breaking strength is 142-146kg/cm2The tensile elongation at break is 700-800%; the density of the olefin block copolymer is 1.29 to 1.31g/cm3The tensile strength is 9.68-9.73MPa, and the elongation at break is 400-430%; the density of the PVDF resin powder is 1.75-1.77g/cm3The thermal decomposition temperature is 385-390 ℃.
The preparation method of the hydrophobic anti-wear agent comprises the following steps: adding 25 parts by weight of nano silicon dioxide and 9 parts by weight of nano titanium dioxide into 780 parts by weight of dimethyl carbonate, ultrasonically dispersing for 28min, adding into a reaction bottle, stirring and refluxing at 94 ℃, dropwise adding 46 parts by weight of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, reacting for 50min in a refluxing manner after dropwise adding, slowly dropwise adding 32 parts by weight of styrene, dropwise adding 15 parts by weight of ammonium persulfate, and reacting for 2.4 hours in a stirring manner; filtering, drying at low temperature, and grinding. The cross-linking agent is formed by mixing benzoyl peroxide and 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide according to the mass ratio of 2: 1. The vulcanization accelerator is stearic acid, and the vulcanization activator is calcium stearate.
The preparation method of the high-elasticity wear-resistant rubber sole material comprises the following steps:
s1, adding chlorohydrin rubber, EVA particles, isoprene rubber, olefin block copolymer, PVDF resin powder, vulcanization accelerator and vulcanization activator into a stirring and shearing cavity 5 along a feed hopper 9 of an internal mixer, driving a first belt pulley 11 to rotate by a servo motor 10, driving a belt 13 and a second belt pulley 12 to rotate, and driving a stirring frame 15 and a shearing blade 16 to mix, stir and shear the materials by a stirring shaft 14; the cylinder 6 drives the telescopic rod to stretch up and down and drives the pressurizing plate 7 to move in the vertical direction so as to adjust the air pressure in the extrusion cavity 4 and inject the pressure into the stirring and shearing cavity 5; keeping the temperature at 218 ℃ and banburying for 30min to obtain a mixture a;
s2, adding talcum powder, hydrophobic wear-resistant agent and magnesium oxide into the mixture a, heating the mixture a to 190 ℃ by an internal mixer, carrying out heat preservation and banburying for 10min, heating the mixture to 200 ℃, carrying out heat preservation and banburying for 15min, adding sodium dodecyl sulfate and cross-linking agent, heating the internal mixer to 220 ℃, continuing banburying for 26min, and carrying out sheet extrusion, extrusion and granulation to obtain the high-elasticity wear-resistant rubber sole material.
Example 4
A high-elasticity wear-resistant rubber sole material is prepared from the following components in parts by weight: 21 parts of chlorohydrin rubber, 56 parts of EVA particles, 14 parts of isoprene rubber, 32 parts of talcum powder, 12 parts of olefin block copolymer, 5.5 parts of hydrophobic wear-resisting agent, 9 parts of PVDF resin powder, 2.8 parts of sodium dodecyl sulfate, 2 parts of magnesium oxide, 3 parts of crosslinking agent, 3.5 parts of vulcanization accelerator and 3.4 parts of vulcanization activator;
wherein the density of EAV particles is 0.95-0.96g/cm3The tensile breaking strength is 142-146kg/cm2The tensile elongation at break is 700-800%; the density of the olefin block copolymer is 1.29 to 1.31g/cm3The tensile strength is 9.68-9.73MPa, and the elongation at break is 400-430%; the density of the PVDF resin powder is 1.75-1.77g/cm3The thermal decomposition temperature is 385-390 ℃.
The preparation method of the hydrophobic anti-wear agent comprises the following steps: adding 30 parts of nano silicon dioxide and 10 parts of nano titanium dioxide into 760 parts of dimethyl carbonate, ultrasonically dispersing for 26min, adding into a reaction bottle, stirring and refluxing at 95 ℃, dropwise adding 48 parts of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, reacting for 45min in a refluxing manner after dropwise adding, slowly dropwise adding 32 parts of styrene, dropwise adding 18 parts of ammonium persulfate, and reacting for 2.5 hours in a stirring manner; filtering, drying at low temperature, and grinding. The cross-linking agent is bis-tert-butylperoxydiisopropylbenzene. The vulcanization accelerator is stearic acid, and the vulcanization activator is calcium stearate.
The preparation method of the high-elasticity wear-resistant rubber sole material comprises the following steps:
s1, adding chlorohydrin rubber, EVA particles, isoprene rubber, olefin block copolymer, PVDF resin powder, vulcanization accelerator and vulcanization activator into a stirring and shearing cavity 5 along a feed hopper 9 of an internal mixer, driving a first belt pulley 11 to rotate by a servo motor 10, driving a belt 13 and a second belt pulley 12 to rotate, and driving a stirring frame 15 and a shearing blade 16 to mix, stir and shear the materials by a stirring shaft 14; the cylinder 6 drives the telescopic rod to stretch up and down and drives the pressurizing plate 7 to move in the vertical direction so as to adjust the air pressure in the extrusion cavity 4 and inject the pressure into the stirring and shearing cavity 5; carrying out heat preservation and banburying at the temperature of 210 ℃ and 220 ℃ for 30min to obtain a mixture a;
s2, adding talcum powder, hydrophobic wear-resistant agent and magnesium oxide into the mixture a, heating the mixture a to 190 ℃ by an internal mixer, carrying out heat preservation and banburying for 7min, heating the mixture to 200 ℃, carrying out heat preservation and banburying for 12min, adding sodium dodecyl sulfate and cross-linking agent, heating the internal mixer to 218 ℃, continuing banburying for 25min, and carrying out sheet extrusion, extrusion and granulation to obtain the high-elasticity wear-resistant rubber sole material.
Comparative example 1
This comparative example differs from example 1 in that no hydrophobic anti-wear agent was added.
Comparative example 2
This comparative example differs from example 1 in that no olefin block copolymer was added.
Comparative example 3
This comparative example differs from example 1 in that no EVA particles were added, 57 parts of chlorohydrin rubber and 25 parts of isoprene rubber were added.
Examples of the experiments
The high-elasticity wear-resistant rubber sole materials prepared in the experimental examples 1 to 4 and the comparative examples 1 to 3 are subjected to performance tests, wherein the Shore hardness A is determined according to ISO 7619: 1997 test, DIN abrasion resistance according to TM 174: 1994, tensile strength according to ISO 37: 2005 test, specific test results are shown in table 1:
TABLE 1 high elastic abrasion-resistant rubber sole material performance test results
| Item | Shore hardness A | DIN abrasion (cm)3) | Tensile Strength (MPa) | Rebound resilience (%) |
| Example 1 | 59 | 74 | 57.4 | 59.7 |
| Example 2 | 58 | 78 | 56.8 | 58.2 |
| Example 3 | 56 | 82 | 56.7 | 57.9 |
| Example 4 | 52 | 86 | 56.2 | 58.4 |
| Comparative example 1 | 37 | 127 | 43.8 | 42.8 |
| Comparative example 2 | 48 | 118 | 45.7 | 45.1 |
| Comparative example 3 | 41 | 107 | 48.5 | 47.8 |
As can be seen from the table above, the rubber sole material provided by the embodiment of the invention has the advantages of good hardness, excellent wear resistance, good tensile strength and good rebound rate, and is suitable for being used as a material for wear-resistant outdoor shoes.
Example 5
Referring to fig. 1-3, this embodiment provides an internal mixer for the compounding of rubber raw materials, the pressurization is cuted, including reaction housing 1, antidetonation base 2, pressurization housing 3, reaction housing 1's inner chamber top is equipped with hourglass hopper-shaped extrusion chamber 4, the inner chamber below is equipped with stirring shearing chamber 5, the bottom in extrusion chamber 4 and the top intercommunication in stirring shearing chamber 5, the top in extrusion chamber 4 is equipped with the cylinder 6 that the telescopic link is vertical decurrent, the telescopic link bottom of cylinder 6 is connected with pressure plate 7, pressure plate 7 is cuboid form and cross section length is less than the section length in extrusion chamber 4. The top of the side wall of the stirring and shearing cavity 5 is connected with a pressure gauge 8 and a feed hopper 9, the bottom of the other side wall is provided with a servo motor 10, a motor shaft of the servo motor 10 is coaxially connected with a first belt pulley 11, a second belt pulley 12 is arranged above the first belt pulley 11, and a belt 13 is arranged around the peripheries of the first belt pulley 11 and the second belt pulley 12. The cylinder 6 drives the telescopic rod to stretch up and down, so that the pressurizing plate 7 can be driven to move in the vertical direction to adjust the air pressure in the extrusion cavity 4, the pressure is injected into the stirring and shearing cavity 5, and meanwhile, the pressure gauge 8 can monitor the air pressure in the stirring and shearing cavity 5 at any time; the servo motor 10 drives the first belt pulley 11 to rotate, drives the belt 13 and the second belt pulley 12 to rotate, and the stirring shaft 14 drives the stirring frame 15 and the shearing blade 16 to mix, stir and shear the materials.
The axial center position of the second belt pulley 12 is connected with a stirring shaft 14 extending into the stirring and shearing cavity 5, the periphery of the stirring shaft 14 is sleeved with a cylindrical stirring frame 15, a plurality of circles of shearing blades 16 are equidistantly distributed on the periphery of the stirring frame 15, the number of the shearing blades 16 in each circle is 8, the extending directions of the adjacent shearing blades 16 are opposite, and a plurality of crushing cutters 17 are arranged on the cutting edge parts, opposite to the adjacent shearing blades 16. The shearing blades 16 promote stirring and mixing of materials, the crushing blades 17 promote shearing and crushing of the materials in different areas, adhesion and hardening between the materials are avoided, and uniformity of material mixing is improved.
The two sides of the bottom of the stirring and shearing cavity 5 are obliquely provided with discharge plates 18, and the central position of the bottom of the stirring and shearing cavity 5 is connected with a discharge pipe 20 obliquely extending out of the reaction shell 1 through a first valve 19. One of the discharging plates 18 is connected with a second valve 22 through a return pipe 21, and the return pipe 21 extends into the top inner cavity of the stirring and shearing cavity 5 after extending through the outer wall of the stirring and shearing cavity 5. A plurality of discharge holes 23 are equidistantly arranged on the material returning pipe 21 extending into the inner cavity of the top part. The return pipe 21 located on the outer wall of the mixing and shearing chamber 5 is fastened by a plurality of clamps 24 arranged from top to bottom. The section of the anti-seismic base 2 is isosceles trapezoid, and a plurality of hydraulic dampers 25 are arranged in the cavity. The ejection of compact board 18 that the slope set up has made things convenient for the ejection of compact of rubber material, and the material that returns through second valve 22, return pipe 21 simultaneously drives the pressure plate 7 and under the atmospheric pressure that the downstream produced at cylinder 6, falls along discharge gate 23, has promoted the circulation of material and has cuted crushing, has improved the purity of rubber material.
The working method of the internal mixer of the embodiment comprises the following steps:
1) adding raw materials of synthetic rubber into the stirring and shearing cavity 5 along the feed hopper 9, driving the first belt pulley 11 to rotate by the servo motor 10, driving the belt 13 and the second belt pulley 12 to rotate, and driving the stirring frame 15 and the shearing blade 16 to mix, stir and shear the materials by the stirring shaft 14;
2) the cylinder 6 drives the telescopic rod to stretch up and down, and can drive the pressurizing plate 7 to move in the vertical direction so as to adjust the air pressure in the extrusion cavity 4, so that the pressure is injected into the stirring and shearing cavity 5, and meanwhile, the pressure gauge 8 can monitor the air pressure in the stirring and shearing cavity 5 at any time;
3) the materials returned by the second valve 22 and the material returning pipe 21 fall along the discharge port 23 under the air pressure generated by the downward movement of the pressurizing plate 7 driven by the cylinder 6, so that the circulation and the sufficient shearing and crushing of the materials are promoted; after the material is completely reacted, the material is discharged through a first valve 19 and a discharge pipe 20.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. The high-elasticity wear-resistant rubber sole material is characterized by being prepared from the following components in parts by weight: 15-22 parts of chlorohydrin rubber, 45-60 parts of EVA (ethylene-vinyl acetate copolymer) particles, 8-15 parts of isoprene rubber, 25-36 parts of talcum powder, 8-13 parts of olefin block copolymer, 3.5-6 parts of hydrophobic wear-resisting agent, 5-10 parts of PVDF (polyvinylidene fluoride) resin powder, 1.5-3 parts of sodium dodecyl sulfate, 1-2 parts of magnesium oxide, 1-3 parts of crosslinking agent, 2.2-3.6 parts of vulcanization accelerator and 2.5-3.5 parts of vulcanization activator;
wherein the density of EAV particles is 0.95-0.96g/cm3The tensile breaking strength is 142-146kg/cm2The tensile elongation at break is 700-800%; the density of the olefin block copolymer is 1.29 to 1.31g/cm3The tensile strength is 9.68-9.73MPa, and the elongation at break is 400-430%; the density of the PVDF resin powder is 1.75-1.77g/cm3The thermal decomposition temperature is 385-390 ℃.
2. The high-elasticity abrasion-resistant rubber sole material according to claim 1, wherein the hydrophobic abrasion-resistant agent is prepared by the following method: adding 20-30 parts of nano silicon dioxide and 6-11 parts of nano titanium dioxide into 800 parts of 600-one-wall dimethyl carbonate, ultrasonically dispersing for 20-30min, adding into a reaction bottle, stirring and refluxing at the temperature of 92-95 ℃, dropwise adding 35-50 parts of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, performing reflux reaction for 40-50min after dropwise adding, slowly dropwise adding 25-36 parts of styrene, dropwise adding 10-20 parts of ammonium persulfate, and stirring and reacting for 2-2.5 hours; filtering, drying at low temperature, and grinding.
3. The high resilience abrasion resistant rubber sole material according to claim 1, wherein the cross-linking agent is one or more of dicumyl peroxide, benzoyl peroxide, 2, 5-dimethyl-2, 5-di-tert-butylperoxyhexane, di-tert-butylperoxydiisopropylbenzene.
4. The high elastic abrasion resistant rubber sole material according to claim 1, wherein said vulcanization accelerator is stearic acid, and said vulcanization activator is calcium stearate.
5. The highly elastic abrasion resistant rubber sole material according to claim 1, wherein the method for preparing the highly elastic abrasion resistant rubber sole material comprises the steps of:
s1, adding chlorohydrin rubber, EVA particles, isoprene rubber, olefin block copolymer, PVDF resin powder, vulcanization accelerator and vulcanization activator into a stirring and shearing cavity (5) along a feed hopper (9) of an internal mixer, driving a first belt pulley (11) to rotate by a servo motor (10) to drive a belt (13) and a second belt pulley (12) to rotate, and driving a stirring frame (15) and a shearing blade (16) to mix, stir and shear the materials by a stirring shaft (14); the cylinder (6) drives the telescopic rod to stretch up and down to drive the pressurizing plate (7) to move in the vertical direction so as to adjust the air pressure in the extrusion cavity (4) and inject the pressure into the stirring and shearing cavity (5); carrying out heat preservation and banburying at the temperature of 210 ℃ and 220 ℃ for 20-30min to obtain a mixture a;
s2, adding talcum powder, hydrophobic wear-resistant agent and magnesium oxide into the mixture a, heating the internal mixer to 190 ℃ plus materials, carrying out heat preservation and internal mixing for 5-10min, heating to 200 ℃ plus materials, carrying out heat preservation and internal mixing for 10-15min, adding sodium dodecyl sulfate and cross-linking agent, heating the internal mixer to 220 ℃ plus materials, continuing internal mixing for 20-30min, and carrying out sheet discharging, extrusion and granulation to obtain the high-elasticity wear-resistant rubber sole material.
6. The high-elasticity wear-resistant rubber sole material according to claim 5, wherein the internal mixer comprises a reaction shell (1), a shock-resistant base (2) and a pressurizing shell (3), a funnel-shaped extrusion cavity (4) is arranged above an inner cavity of the reaction shell (1), a stirring and shearing cavity (5) is arranged below the inner cavity, the bottom of the extrusion cavity (4) is communicated with the top of the stirring and shearing cavity (5), a cylinder (6) with a vertically downward telescopic rod is arranged at the top of the extrusion cavity (4), a pressurizing plate (7) is connected to the bottom of the telescopic rod of the cylinder (6), and the pressurizing plate (7) is cuboid and has a cross section length smaller than that of the extrusion cavity (4); the top of the side wall of the stirring and shearing cavity (5) is connected with a pressure gauge (8) and a feed hopper (9), the bottom of the other side wall is provided with a servo motor (10), a motor shaft of the servo motor (10) is coaxially connected with a first belt pulley (11), a second belt pulley (12) is arranged above the first belt pulley (11), and a belt (13) is arranged around the peripheries of the first belt pulley (11) and the second belt pulley (12).
7. The high-elasticity wear-resistant rubber sole material according to claim 6, wherein discharge plates (18) are obliquely arranged on two sides of the bottom of the stirring and shearing cavity (5), and a discharge pipe (20) obliquely extending out of the reaction shell (1) is connected to the center of the bottom of the stirring and shearing cavity (5) through a first valve (19); one of the discharging plates (18) is connected with a second valve (22) through a return pipe (21), and the return pipe (21) extends into the top inner cavity of the stirring and shearing cavity (5) after extending through the outer wall of the stirring and shearing cavity (5); a plurality of discharge holes (23) are equidistantly arranged on the material returning pipe (21) extending into the top inner cavity.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113004590A (en) * | 2021-03-05 | 2021-06-22 | 亚罗斯建材（江苏）有限公司 | Environment-friendly and fireproof rubber plastic material for ships and processing method thereof |
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