CN115010999B - Wear-resistant sole rubber formula and manufacturing process - Google Patents

Wear-resistant sole rubber formula and manufacturing process Download PDF

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CN115010999B
CN115010999B CN202110237607.1A CN202110237607A CN115010999B CN 115010999 B CN115010999 B CN 115010999B CN 202110237607 A CN202110237607 A CN 202110237607A CN 115010999 B CN115010999 B CN 115010999B
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rubber
temperature
feeding
aging agent
sole
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CN115010999A (en
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陈志勇
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Xiamen Greentouch Co ltd
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Xiamen Greentouch Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L7/00—Compositions of natural rubber
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
    • Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction 

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The wear-resistant sole rubber formula and the manufacturing process thereof, wherein the formula comprises the following components: 48-60phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:13 to 20phr; butadiene rubber KBR01:27 to 32phr; carbon black N330:58-65phr; zinc oxide: 3 to 4.5phr; stearic acid: 2 to 3phr; anti-aging agent 264:2.5 to 4.5phr; anti-aging agent RD:1 to 2.5phr; 1.3 to 3.6phr of antioxidant AW; accelerator TBBS:0.6 to 1.2phr; rubber microcrystalline wax: 0.5 to 1.5phr; insoluble sulfur IS HD-OT-20:2.3 to 4.2phr; 2.4 to 4.3phr of coumarone resin; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 3.5 to 6.5phr; the basalt fiber bulked yarn as the skeleton material and the new technology are added in the sole rubber formula, so that the tear resistance, the wear resistance and the bending resistance of the finished product are enhanced.

Description

Wear-resistant sole rubber formula and manufacturing process
Technical Field
The invention belongs to the technical field of rubber materials for shoes, and particularly relates to a wear-resistant sole rubber formula and a manufacturing process thereof.
Background
The existing sole rubber material has various formulas, and even each company has a unique material formula. These formulations mainly emphasize the properties of the rubber materials, such as abrasion resistance, slip resistance, elasticity, tear resistance, aging resistance, corrosion resistance. Among them, wear resistance is particularly important for work shoes, as well as for mountain climbing shoes, basketball shoes for outsourcing, shoes for outdoor crossing, etc., where outdoor use is a playing field, because it involves durability of the sole, and wear resistance of the sole is even vital in outdoor use and in some terrains where the environment is bad. However, the existing formulation is often defective due to cost or technical reasons, so it is important to develop a high-strength wear-resistant sole rubber formulation. The general wear resistance improvement of the common sole is mainly improved by the change of the rubber content and the formulation of the carbon black, but the improvement of the wear resistance is limited by the improvement mode. The tire for automobile has its overall structural strength reinforced and abrasion resistance improved by adding cords and cords to the rubber material. Through the suggestion of this concept, we tried to improve the wear resistance and overall strength of the sole by adding two ways of adjusting the carcass material and the overall rubber formulation to the rubber material for the sole.
Disclosure of Invention
The invention provides a wear-resistant sole rubber formula and a manufacturing process thereof, which have high wear resistance and lower cost.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a wear-resistant sole rubber formulation, which comprises the following components:
48-60phr of natural rubber; styrene-butadiene rubber: 13 to 20phr; butadiene rubber: 27 to 32phr; carbon black: 58-65phr; zinc oxide: 3 to 4.5phr; stearic acid: 2 to 3phr; anti-aging agent 264:2.5 to 4.5phr; anti-aging agent RD:1 to 2.5phr; 1.3 to 3.6phr of antioxidant AW; accelerator TBBS:0.6 to 1.2phr; rubber microcrystalline wax: 0.5 to 1.5phr; insoluble sulfur: 2.3 to 4.2phr; 2.4 to 4.3phr of coumarone resin; basalt fiber bulked yarn: 3.5 to 6.5phr.
Further, the natural rubber is TSR20LM; the styrene-butadiene rubber is SBR 1712E; the butadiene rubber is KBR01; the carbon black is N330; the insoluble sulfur IS IS HD-OT-20; the basalt fiber bulked yarn has the length of 3MM and the diameter of 6-17um.
Further, the formula comprises the following components:
60phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:13phr; butadiene rubber KBR01:27phr; carbon black N330:58phr; zinc oxide: 3.5phr; stearic acid: 2.5phr; anti-aging agent 264:3phr; anti-aging agent RD:2phr; 2.5phr of antioxidant AW; accelerator TBBS:1.0phr; rubber microcrystalline wax: 0.8phr; insoluble sulfur IS HD-OT-20:4phr; 3.5phr of coumarone resin; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 5.5phr.
Further, the formula comprises the following components:
48phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:20phr; butadiene rubber KBR01:32phr; carbon black N330:65phr; zinc oxide: 4phr; stearic acid: 3phr; anti-aging agent 264:4phr; anti-aging agent RD:2phr; 2phr of antioxidant AW; accelerator TBBS:0.8phr; rubber microcrystalline wax: 1.2phr; insoluble sulfur IS HD-OT-20:3phr; 3phr of coumarone resin; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 4.5phr.
Further, the 3MM length diameter 6-17um basalt fiber bulked yarn is replaced by chopped recycled carbon fiber.
Further, the 3MM length diameter 6-17um basalt fiber bulked yarn is replaced with pretreated para-polyamide chopped fiber 1414.
Further, the manufacturing process comprises an internal mixing process and an open mixing process;
the process conditions of the banburying flow are as follows: the air pressure is 6 KG/square meter, the rotating speed is 150-170R/MIN, the upper bolt pressure is 0.6-0.8MPA, and the filling coefficient is 0.6-0.7, comprising the following steps:
(1) Feeding: 48-60phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:13 to 20phr; the temperature is 110-120 ℃ and the time is 1-1.5MIN;
(2) Feeding II: butadiene rubber KBR01:27 to 32phr; the temperature is 110-120 ℃ and the time is 2-2.5MIN;
(3) And (3) feeding: zinc oxide: 3 to 4.5phr; anti-aging agent 264:2.5 to 4.5phr; anti-aging agent RD:1 to 2.5phr; rubber microcrystalline wax: 0.5 to 1.5phr; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 3.5 to 6.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(4) Feeding four: carbon black N330:58-65phr; 1.3 to 3.6phr of antioxidant AW; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(5) Feeding fifth: 2.4 to 4.3phr of coumarone resin; stearic acid: 2 to 3phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(6) Discharging: air cooling or water cooling is carried out for more than 2H until the temperature of the sizing material is lower than 45 ℃;
the technological conditions of the open mill flow are as follows: the temperature of the front roller is 50-55 ℃, the temperature of the rear roller is 45-50 ℃, and the roller speed is as follows: front roller 27.5, rear roller 33, speed ratio 1:1.2, comprising the steps of:
(1) Wrapping the roller for 3-4MIN;
(2) Adding an accelerator TBBS:0.6 to 1.2phr;
(3) Turning: left and right cutters are separated for 20-30 seconds for 2 times;
(4) Adding insoluble sulfur IS HD-OT-20:2.3 to 4.2phr;
(5) Cutting, narrowing the roll gap to the required thickness of mould pressing, packing in a triangular bag, and carrying out thin ventilation for 5-7 times;
(6) And (5) blanking.
Cutting the rubber into the required size for mould pressing after refining and blanking, standing for 12-24 hours, and then entering a sole mould for mould pressing and vulcanization processing, wherein the mould pressing and vulcanization conditions are as follows: the temperature is 1450C-1550C for 5 minutes. And trimming and blanking after die pressing to obtain a sole finished product.
The natural rubber TSR20LM has good physical and mechanical properties and processability, has low Mooney, is easy to mix with other raw materials, and reduces banburying time.
The styrene-butadiene rubber is synthetic rubber, adopts the environment-friendly SBR 1712E model, and has the relative molecular mass and distribution, molecular structure and physical and mechanical properties which are basically the same as those of the common styrene-butadiene rubber; but the plasticity is better than that of the traditional rubber in the same series, which is more beneficial to processing and passing the stricter environmental protection test standard of foreign shoes. In addition, the use amount of natural rubber can be reduced, and the cost is reduced.
Butadiene rubber is synthetic rubber, is of Korean KBR01 type, is particularly excellent in cold resistance, wear resistance and elasticity after vulcanization, generates little heat under dynamic load, has good ageing resistance, and is easy to be compounded with natural rubber. Is favorable for passing stricter foreign shoe environmental protection test standards. The usage amount of natural rubber can be reduced, and the cost is reduced.
The carbon black is a rubber reinforcing agent, is superior to channel carbon black, and can endow colloidal particles with better stretching performance, tear resistance, wear resistance and elasticity, and the model N330 is used for reinforcing wear resistance.
Zinc oxide acts to improve the efficiency of vulcanization and reduce the vulcanization time. And simultaneously, the crosslinking density is improved, and the ageing resistance of the vulcanized rubber is improved.
The stearic acid has the functions of softening and plasticizing, improving the activity of zinc oxide and accelerator, and accelerating hardening.
The antioxidant 264 acts as a stabilizer, and has a protective effect on the thermo-oxidative aging of rubber, and also can prevent the damage of weather to vulcanized rubber. And is also beneficial to the later storage of vulcanized rubber.
The anti-aging agent RD is mainly used as a rubber anti-aging agent. Is suitable for natural rubber and synthetic rubber such as butyronitrile, butylbenzene, ethylene-propylene and neoprene. The protective effect on aging caused by heat and oxygen is excellent, but the protective effect on flex aging is poor. The rubber product is used together with antioxidant AW or p-phenylenediamine as one common antioxidant.
The anti-aging agent AW is used for preventing the rubber products from cracking caused by ozone, is suitable for the rubber products used under dynamic conditions, and has the effect of reinforcing the antioxidation.
The accelerator TBBS acts as a post-effect accelerator, is safe at the operation temperature, has strong scorch resistance, high vulcanization speed and high stretching strength, and can improve the use proportion of the synthetic adhesive. Low toxicity, high efficiency and forms a good vulcanization system together with other raw materials.
The rubber microcrystalline wax is used as special wax for protecting rubber products from being corroded and aged by light, oxygen and ozone, and is also an anti-aging agent.
Insoluble sulfur IS HD-OT-20 IS used as accelerator and vulcanizing agent to prevent the frosting of the finished sizing material and improve the heat resistance and wear resistance of the finished product.
The coumarone resin has good compatibility with rubber, is a solvent tackifier, a plasticizer and a softener, and is also an organic reinforcing agent of synthetic rubber.
In the selection of the framework material, three different materials are adopted by taking physical properties of the raw material and mixing processability of the raw material and rubber material into consideration, and economic and cost considerations, namely basalt fiber bulked yarn, recycled carbon fiber and pretreated para-polyamide chopped fiber 1414.
The basalt fiber bulked yarn has good heat stability, flame retardance, electrical insulation, chemical stability and the like, and has good heat resistance, high elastic modulus, high strength, good dimensional stability and the like. The main functions of the formula are skeleton materials, so that the tearing strength, the wear resistance and the bending strength of the finished product are enhanced.
As a high-strength high-modulus fiber, carbon fiber is used as a fiber, and the application field of the composite material is expanding continuously, so that the problem of recycling waste is also attracting attention. Due to the difficulty of filament carbon fibers in subsequent processing of the post sole after compression vulcanization, chopped materials are preferred in the application of sole materials.
The pretreated para-polyamide chopped fiber 1414 also has good thermal stability, flame retardance, electrical insulation, chemical stability, radiation resistance and the like, and has good heat resistance, high elastic modulus, high strength, good dimensional stability and the like. And are therefore also within the framework material considerations.
The wear-resistant sole is used on the sole of the shoes applied to outdoor sites, the wear resistance of the sole is improved, the cost is reduced, and the excellent sole performance can be beneficial to common consumers and can better guarantee the consumers.
Detailed Description
The following examples describe the novel process of the present invention in detail, but are not meant to limit the scope of the invention.
Example 1:
60phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:13phr; butadiene rubber KBR01:27phr; carbon black N330:58phr; zinc oxide: 3.5phr; stearic acid: 2.5phr; anti-aging agent 264:3phr; anti-aging agent RD:2phr; 2.5phr of antioxidant AW; accelerator TBBS:1.0phr; rubber microcrystalline wax: 0.8phr; insoluble sulfur IS HD-OT-20:4phr; 3.5phr of coumarone resin; 3MM length, 6-17um diameter basalt fiber bulked yarn (chopped recycled carbon fiber/pretreated para-polyamide chopped fiber 1414): 5.5phr.
The preparation method comprises an internal mixing process and an open mixing process, wherein the process conditions and the feeding process are as follows:
the process conditions of the banburying flow are as follows: the air pressure is 6 KG/square meter, the rotating speed is 150-170R/MIN, the upper bolt pressure is 0.6-0.8MPA, and the filling coefficient is 0.6-0.7, comprising the following steps:
(1) Feeding: 60phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:13phr; the temperature is 110-120 ℃ and the time is 1-1.5MIN;
(2) Feeding II: butadiene rubber KBR01:27phr; the temperature is 110-120 ℃ and the time is 2-2.5MIN;
(3) And (3) feeding: zinc oxide: 3.5phr; anti-aging agent 264:3phr; anti-aging agent RD:2phr; rubber microcrystalline wax: 0.8phr; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 5.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(4) Feeding four: carbon black N330:58phr; anti-aging agent AW:2.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(5) Feeding fifth: 3.5phr of coumarone resin; stearic acid: 2.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(6) Discharging: air cooling or water cooling for 2H to the temperature of the sizing material of 45 ℃;
the technological conditions of the open mill flow are as follows: the temperature of the front roller is 50-55 ℃, the temperature of the rear roller is 45-50 ℃, and the roller speed is as follows: front roller 27.5, rear roller 33, speed ratio 1:1.2, comprising the steps of:
(1) Wrapping the roller for 3-4MIN;
(2) Adding an accelerator TBBS:1.0phr;
(3) Turning: left and right cutters are separated for 20-30 seconds for 2 times;
(4) Adding insoluble sulfur IS HD-OT-20:4phr;
(5) Cutting, narrowing the roll gap to the required thickness of mould pressing, packing in a triangular bag, and carrying out thin ventilation for 5-7 times;
(6) And (5) blanking.
Cutting the rubber into the required size for mould pressing after refining and blanking, standing for 12-24 hours, and then entering a sole mould for mould pressing and vulcanization processing, wherein the mould pressing and vulcanization conditions are as follows: the temperature is 145-155 ℃ and the time is 5 minutes. And trimming and blanking after die pressing to obtain a sole finished product.
Example 2:
48phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:20phr; butadiene rubber KBR01:32phr; carbon black N330:65phr; zinc oxide: 4phr; stearic acid: 3phr; anti-aging agent 264:4phr; anti-aging agent RD:2phr; 2phr of antioxidant AW; accelerator TBBS:0.8phr; rubber microcrystalline wax: 1.2phr; insoluble sulfur IS HD-OT-20:3phr; 3phr of coumarone resin; 3MM length, 6-17um diameter basalt fiber bulked yarn (chopped recycled carbon fiber/pretreated para-polyamide chopped fiber 1414): 4.5phr.
The preparation method comprises an internal mixing process and an open mixing process, wherein the process conditions and the feeding process are as follows:
the process conditions of the banburying flow are as follows: the air pressure is 6 KG/square meter, the rotating speed is 150-170R/MIN, the upper bolt pressure is 0.6-0.8MPA, and the filling coefficient is 0.6-0.7, comprising the following steps:
(1) Feeding: 48phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:20phr; the temperature is 110-120 ℃ and the time is 1-1.5MIN;
(2) Feeding II: butadiene rubber KBR01:32phr; the temperature is 110-120 ℃ and the time is 2-2.5MIN;
(3) And (3) feeding: zinc oxide: 4phr; anti-aging agent 264:4phr; anti-aging agent RD:2phr; rubber microcrystalline wax: 1.2phr; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 4.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(4) Feeding four: carbon black N330:65phr; anti-aging agent AW:2phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(5) Feeding fifth: 3phr of coumarone resin; stearic acid: 3phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(6) Discharging: air cooling or water cooling for 2H to the temperature of the sizing material of 45 ℃;
the technological conditions of the open mill flow are as follows: the temperature of the front roller is 50-55 ℃, the temperature of the rear roller is 45-50 ℃, and the roller speed is as follows: front roller 27.5, rear roller 33, speed ratio 1:1.2, comprising the steps of:
(1) Wrapping the roller for 3-4MIN;
(2) Adding an accelerator TBBS:0.8phr;
(3) Turning: left and right cutters are separated for 20-30 seconds for 2 times;
(4) Adding insoluble sulfur IS HD-OT-20:3phr;
(5) Cutting, narrowing the roll gap to the required thickness of mould pressing, packing in a triangular bag, and carrying out thin ventilation for 5-7 times;
(6) And (5) blanking.
Cutting the rubber into the required size for mould pressing after refining and blanking, standing for 12-24 hours, and then entering a sole mould for mould pressing and vulcanization processing, wherein the mould pressing and vulcanization conditions are as follows: the temperature is 145-155 ℃ and the time is 5 minutes. And trimming and blanking after die pressing to obtain a sole finished product.
To contrast with the examples, two experimental comparative example formulations were specifically set:
comparative example 1:
65phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:12phr; butadiene rubber KBR01:23phr; carbon black N330:62phr; zinc oxide: 4phr; stearic acid: 2.5phr; anti-aging agent 264:3.5phr; anti-aging agent RD:1.5phr; 2.5phr of antioxidant AW; accelerator TBBS:0.8phr; rubber microcrystalline wax: 1.0phr; insoluble sulfur IS HD-OT-20:3.2phr; 3phr of coumarone resin; 3MM length, 6-17um diameter basalt fiber bulked yarn (chopped recycled carbon fiber/pretreated para-polyamide chopped fiber 1414): 8phr.
The preparation method comprises an internal mixing process and an open mixing process, wherein the process conditions and the feeding process are as follows:
the process conditions of the banburying flow are as follows: the air pressure is 6 KG/square meter, the rotating speed is 150-170R/MIN, the upper bolt pressure is 0.6-0.8MPA, and the filling coefficient is 0.6-0.7, comprising the following steps:
(1) Feeding: 65phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:12phr; the temperature is 110-120 ℃ and the time is 1-1.5MIN;
(2) Feeding II: butadiene rubber KBR01:23phr; the temperature is 110-120 ℃ and the time is 2-2.5MIN;
(3) And (3) feeding: zinc oxide: 4phr; anti-aging agent 264:3.5phr; anti-aging agent RD:1.5phr; rubber microcrystalline wax: 1.0phr; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 8phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(4) Feeding four: carbon black N330:62phr; anti-aging agent AW:2.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(5) Feeding fifth: 3phr of coumarone resin; stearic acid: 2.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(6) Discharging: air cooling or water cooling for 2H to the temperature of the sizing material of 45 ℃;
the technological conditions of the open mill flow are as follows: the temperature of the front roller is 50-55 ℃, the temperature of the rear roller is 45-50 ℃, and the roller speed is as follows: front roller 27.5, rear roller 33, speed ratio 1:1.2, comprising the steps of:
(1) Wrapping the roller for 3-4MIN;
(2) Adding an accelerator TBBS:0.8phr;
(3) Turning: left and right cutters are separated for 20-30 seconds for 2 times;
(4) Adding insoluble sulfur IS HD-OT-20:3.2phr;
(5) Cutting, narrowing the roll gap to the required thickness of mould pressing, packing in a triangular bag, and carrying out thin ventilation for 5-7 times;
(6) And (5) blanking.
Cutting the rubber into the required size for mould pressing after refining and blanking, standing for 12-24 hours, and then entering a sole mould for mould pressing and vulcanization processing, wherein the mould pressing and vulcanization conditions are as follows: the temperature is 145-155 ℃ and the time is 5 minutes. And trimming and blanking after die pressing to obtain a sole finished product.
Comparative example 2:
natural rubber TSR20LM 43phr; styrene butadiene rubber SBR 1712E:25phr; butadiene rubber KBR01:32phr; carbon black N330:58phr; zinc oxide: 3.5phr; stearic acid: 2.5phr; anti-aging agent 264:3.0phr; anti-aging agent RD:2phr; 2phr of antioxidant AW; accelerator TBBS:1.0phr; rubber microcrystalline wax: 1.5phr; insoluble sulfur IS HD-OT-20:3phr; 3.5phr of coumarone resin; 3MM length, 6-17um diameter basalt fiber bulked yarn (chopped recycled carbon fiber/pretreated para-polyamide chopped fiber 1414): 2.5phr.
The preparation method comprises an internal mixing process and an open mixing process, wherein the process conditions and the feeding process are as follows:
the process conditions of the banburying flow are as follows: the air pressure is 6 KG/square meter, the rotating speed is 150-170R/MIN, the upper bolt pressure is 0.6-0.8MPA, and the filling coefficient is 0.6-0.7, comprising the following steps:
(1) Feeding: natural rubber TSR20LM 43phr; styrene butadiene rubber SBR 1712E:25phr; the temperature is 110-120 ℃ and the time is 1-1.5MIN;
(2) Feeding II: butadiene rubber KBR01:32phr; the temperature is 110-120 ℃ and the time is 2-2.5MIN;
(3) And (3) feeding: zinc oxide: 3.5phr; anti-aging agent 264:3.0phr; anti-aging agent RD:2phr; rubber microcrystalline wax: 1.5phr; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 2.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(4) Feeding four: carbon black N330:58phr; anti-aging agent AW:2.0phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(5) Feeding fifth: 3.5phr of coumarone resin; stearic acid: 2.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(6) Discharging: air cooling or water cooling for 2H to the temperature of the sizing material of 45 ℃;
the technological conditions of the open mill flow are as follows: the temperature of the front roller is 50-55 ℃, the temperature of the rear roller is 45-50 ℃, and the roller speed is as follows: front roller 27.5, rear roller 33, speed ratio 1:1.2, comprising the steps of:
(1) Wrapping the roller for 3-4MIN;
(2) Adding an accelerator TBBS:1.0phr;
(3) Turning: left and right cutters are separated for 20-30 seconds for 2 times;
(4) Adding insoluble sulfur IS HD-OT-20:3phr;
(5) Cutting, narrowing the roll gap to the required thickness of mould pressing, packing in a triangular bag, and carrying out thin ventilation for 5-7 times;
(6) And (5) blanking.
Cutting the rubber into the required size for mould pressing after refining and blanking, standing for 12-24 hours, and then entering a sole mould for mould pressing and vulcanization processing, wherein the mould pressing and vulcanization conditions are as follows: the temperature is 145-155 ℃ and the time is 5 minutes. And trimming and blanking after die pressing to obtain a sole finished product.
Example 1 example 2 and comparative example 1 comparative example 2 the physical properties of the finished soles prepared by the test data are compared as follows:
example 1 example 2 physical property test data are compared with national standard requirement data as follows:
note that:
tear strength test conditions:
1. room temperature (23.+ -. 2 ℃ C.), humidity (50%.+ -. 10%)
2. The distance between the two markings was 25mm.
3. The speed of the tensile machine test is 500mm/min.
4. The distance between the clamps is 50mm
5. The test sample is allowed to stand at room temperature for at least 3 hours
Test machine: single-column electronic tensile testing machine
The test meets the standard: ASTM, ISO and EN standards
Elongation at break test conditions:
1. room temperature (23.+ -. 2 ℃ C.), humidity (50%.+ -. 10%)
2. The distance between the two markings was 25mm.
3. The speed of the tensile machine test is 500mm/min.
4. The distance between the clamps is 50mm
5. The test sample is allowed to stand at room temperature for at least 3 hours
Test machine: single-column electronic tensile testing machine
The test meets the standard: ASTM, ISO and EN standards
Bending resistance test conditions:
temperature- - - (normal temperature 23.+ -. 2 ℃ low temperature-20 ℃ C.)
Relative humidity (65.+ -. 2)%,
bending at normal temperature for 10 ten thousand times and at low temperature for 5 ten thousand times
The frequency was 230 times/min.
Test machine: bending test machine and vernier caliper
The test meets the standard: GB/T20991-2007EN 344ISO 20344
Abrasion test conditions: room temperature (23+ -2 ℃ C.)
The test times after 15min of premilled mill are 3418 revolutions (sample mill 1.61 km)
Test instrument: acle abrasion machine, specific gravity tester and electronic balance
The test meets the standard: DIN-53516DIS-4649GB-9867
Anti-skid test conditions: room temperature/square brick floor/dry/wet type
Anti-skid test machine: anti-skid tester
The test meets the standard: BS EN 13287SATRA TM 144
Aging test conditions: test temperature 700C
Experimental time 72H
Aging test machine: UV aging test box
The test meets the standard: GB/T16422.3-1997 ASTMG154
Frosting test conditions: temperature 700C
Humidity 95%, distilled water used for test
Test time 72H
Frosting test machine: constant temperature humidity control box
Test compliance with Standard GB/T20991DIN 53543 SARA CM44
From a combination of several test data of example 1, example 2 and comparative example 1, comparative example 2, a basalt fiber bulked yarn (chopped recycled carbon fiber/pretreated para-polyamide chopped fiber 1414) as a framework material is added in the sole rubber formula, so that the tear resistance, the wear resistance and the bending resistance of the finished product are enhanced. Particularly, the abrasion test data can be greatly improved on the data required by national standards, which has great practical significance in the shoes such as working shoes, mountain climbing shoes taking the outdoors as a playing field, basketball shoes for the outfield, shoes for the outdoor crossing and the like, means that the sole is more wear-resistant and stronger, and provides greater protection for people moving and working under severe environments. The abrasion test data in comparative example 1 was also greatly improved, but the slip resistance and flex resistance were reduced due to the change of other formulation components, and the cost was increased. In comparative example 2, the amount of basalt fiber bulked yarn (chopped recycled carbon fiber/pretreated para-polyamide chopped fiber 1414) as a framework material is too small, although the abrasion data can reach the national standard, the improvement is not great, the practical significance is lost, and the anti-skid and low-temperature bending performance is reduced due to the change of the formula components.
In the selection of three framework materials:
1: the basalt fiber bulked yarn is preferred for economic reasons of sole finished products, and is further subjected to chopped recovery of carbon fiber and is further subjected to pretreatment of para-polyamide chopped fiber 1414.
2: because the sole sizing material is required to enter a sole mold for mold pressing vulcanization processing after refining, and because the processing mold has some finer fonts and some fine structures, the diameter of the framework material is selected to be 6-17um for the best choice on the fonts, the fine structures and the integrity of sole biting, and the choice of the diameter also has better guarantee on the appearance finish of sole finished products. Since the elasticity, shear force and bulkiness of the three materials have influence on the appearance and the integrity of the finished product, the three materials are preferably basalt fiber bulked yarns, and the pretreatment is performed on para-polyamide chopped fibers 1414, and the chopped recycled carbon fibers are further performed.
3: after the sole is manufactured into a sole finished product through mould pressing and vulcanization, the sole is required to be subjected to post-processing of processes such as demoulding, trimming, paint repairing, knife changing and the like, the processing process is not smooth due to overlong fiber length in the post-processing, and the wear resistance and the strength of the sole are reduced due to overlong fiber length, so that the expected skeleton material effect is not achieved. The fiber length was tested and then 3MM length was chosen as the appropriate length.
4: the three framework materials are selected to be basalt fiber bulked yarns optimally through overall consideration, and then chopped and recycled carbon fibers are used for preprocessing para-polyamide chopped fibers 1414.
While the foregoing description illustrates and describes the preferred embodiments of the present invention, as noted above, it is to be understood that the invention is not limited to the forms disclosed herein but is not to be construed as excluding other embodiments, and that various other combinations, modifications and environments are possible and may be made within the scope of the inventive concepts described herein, either by way of the foregoing teachings or by those of skill or knowledge of the relevant art. And that modifications and variations which do not depart from the spirit and scope of the invention are intended to be within the scope of the appended claims.

Claims (4)

1. The wear-resistant sole rubber is characterized by comprising the following components:
60phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:13phr; butadiene rubber KBR01:27phr; carbon black N330:58phr; zinc oxide: 3.5phr; stearic acid: 2.5phr; anti-aging agent 264:3phr; anti-aging agent RD:2phr; 2.5phr of antioxidant AW; accelerator TBBS:1.0phr; rubber microcrystalline wax: 0.8phr; insoluble sulfur IS HD-OT-20:4phr; 3.5phr of coumarone resin; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 5.5phr.
2. The wear-resistant sole rubber is characterized by comprising the following components:
48phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:20phr; butadiene rubber KBR01:32phr; carbon black N330:65phr; zinc oxide: 4phr; stearic acid: 3phr; anti-aging agent 264:4phr; anti-aging agent RD:2phr; 2phr of antioxidant AW; accelerator TBBS:0.8phr; rubber microcrystalline wax: 1.2phr; insoluble sulfur IS HD-OT-20:3phr; 3phr of coumarone resin; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 4.5phr.
3. A manufacturing process of a wear-resistant sole rubber formula is characterized by comprising the following steps of: the method comprises an internal mixing process and an open mixing process, wherein the process conditions and the feeding process are as follows:
technological conditions of the banburying process: the air pressure is 6 KG/square meter, the rotating speed is 150-170R/MIN, the upper bolt pressure is 0.6-0.8MPA, and the filling coefficient is 0.6-0.7, comprising the following steps:
(1) Feeding: 60phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:13phr; the temperature is 110-120 ℃ and the time is 1-1.5MIN;
(2) Feeding II: butadiene rubber KBR01:27phr; the temperature is 110-120 ℃ and the time is 2-2.5MIN;
(3) And (3) feeding: zinc oxide: 3.5phr; anti-aging agent 264:3phr; anti-aging agent RD:2phr; rubber microcrystalline wax: 0.8phr; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 5.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(4) Feeding four: carbon black N330:58phr; anti-aging agent AW:2.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(5) Feeding fifth: 3.5phr of coumarone resin; stearic acid: 2.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(6) Discharging: air cooling or water cooling for 2H to the temperature of the sizing material of 45 ℃;
technological conditions of the open mill flow are as follows: the temperature of the front roller is 50-55 ℃, the temperature of the rear roller is 45-50 ℃, and the roller speed is as follows: front roller 27.5, rear roller 33, speed ratio 1:1.2, comprising the steps of:
(1) Wrapping the roller for 3-4MIN;
(2) Adding an accelerator TBBS:1.0phr;
(3) Turning: left and right cutters are separated for 20-30 seconds for 2 times;
(4) Adding insoluble sulfur IS HD-OT-20:4phr;
(5) Cutting, narrowing the roll gap to the required thickness of mould pressing, packing in a triangular bag, and carrying out thin ventilation for 5-7 times;
(6) The lower part of the upper part is provided with a lower part,
cutting the rubber into the required size for mould pressing after refining and blanking, standing for 12-24 hours, and then entering a sole mould for mould pressing and vulcanization processing, wherein the mould pressing and vulcanization conditions are as follows: the temperature is 145-155 ℃ for 5 minutes, and the finished sole is obtained after trimming and blanking after die pressing.
4. A manufacturing process of a wear-resistant sole rubber formula is characterized by comprising the following steps of: the method comprises an internal mixing process and an open mixing process, wherein the process conditions and the feeding process are as follows:
technological conditions of the banburying process: the air pressure is 6 KG/square meter, the rotating speed is 150-170R/MIN, the upper bolt pressure is 0.6-0.8MPA, and the filling coefficient is 0.6-0.7, comprising the following steps:
(1) Feeding: 48phr of natural rubber TSR20LM; styrene butadiene rubber SBR 1712E:20phr; the temperature is 110-120 ℃ and the time is 1-1.5MIN;
(2) Feeding II: butadiene rubber KBR01:32phr; the temperature is 110-120 ℃ and the time is 2-2.5MIN;
(3) And (3) feeding: zinc oxide: 4phr; anti-aging agent 264:4phr; anti-aging agent RD:2phr; rubber microcrystalline wax: 1.2phr; basalt fiber bulked yarn with 3MM length and diameter of 6-17 um: 4.5phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(4) Feeding four: carbon black N330:65phr; anti-aging agent AW:2phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(5) Feeding fifth: 3phr of coumarone resin; stearic acid: 3phr; the temperature is 110-120 ℃ and the time is 1.5-2MIN;
(6) Discharging: air cooling or water cooling for 2H to the temperature of the sizing material of 45 ℃;
technological conditions of the open mill flow are as follows: the temperature of the front roller is 50-55 ℃, the temperature of the rear roller is 45-50 ℃, and the roller speed is as follows: front roller 27.5, rear roller 33, speed ratio 1:1.2, comprising the steps of:
(1) Wrapping the roller for 3-4MIN;
(2) Adding an accelerator TBBS:0.8phr;
(3) Turning: left and right cutters are separated for 20-30 seconds for 2 times;
(4) Adding insoluble sulfur IS HD-OT-20:3phr;
(5) Cutting, narrowing the roll gap to the required thickness of mould pressing, packing in a triangular bag, and carrying out thin ventilation for 5-7 times;
(6) The lower part of the upper part is provided with a lower part,
cutting the rubber into the required size for mould pressing after refining and blanking, standing for 12-24 hours, and then entering a sole mould for mould pressing and vulcanization processing, wherein the mould pressing and vulcanization conditions are as follows: the temperature is 145-155 ℃ for 5 minutes, and the finished sole is obtained after trimming and blanking after die pressing.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304239A (en) * 2011-09-07 2012-01-04 际华三五三七制鞋有限责任公司 Black bi-vulcanized rubber outsole for mat high-modulus shoe and preparation method thereof
CN103570992A (en) * 2013-10-18 2014-02-12 青岛科技大学 Sole material for sports shoes for body-building and mountaineering and preparation method thereof
CN107955235A (en) * 2017-11-29 2018-04-24 际华三五五皮革皮鞋有限公司 A kind of basalt fibre rubber soles and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304239A (en) * 2011-09-07 2012-01-04 际华三五三七制鞋有限责任公司 Black bi-vulcanized rubber outsole for mat high-modulus shoe and preparation method thereof
CN103570992A (en) * 2013-10-18 2014-02-12 青岛科技大学 Sole material for sports shoes for body-building and mountaineering and preparation method thereof
CN107955235A (en) * 2017-11-29 2018-04-24 际华三五五皮革皮鞋有限公司 A kind of basalt fibre rubber soles and preparation method thereof

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* Cited by examiner, † Cited by third party
Title
碳纤维增强橡胶复合材料;贺福;《化工新型材料》;第09卷;第12-15页 *

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