CN105086013A - No-blooming wear-resistant rubber and preparing method thereof - Google Patents

No-blooming wear-resistant rubber and preparing method thereof Download PDF

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CN105086013A
CN105086013A CN201510498714.4A CN201510498714A CN105086013A CN 105086013 A CN105086013 A CN 105086013A CN 201510498714 A CN201510498714 A CN 201510498714A CN 105086013 A CN105086013 A CN 105086013A
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wear
rubber
blooming
parts
agent
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李贝贝
焦占磊
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Jihua 3514 Leather and Footware Co Ltd
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Jihua 3514 Leather and Footware Co Ltd
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Abstract

The invention discloses no-blooming wear-resistant rubber and a preparing method thereof. White carbon black is adopted as a reinforcing agent, multiple activating agents are mixed for activating the reinforcing agent to adjust the vulcanization speed, semi-transparent products or products of any color can be prepared, and pollution is avoided; an anti-fogging agent is not used in the wear-resistant rubber, while the same no-blooming effect can be achieved, the provided materials are low in cost, the processing technology is simple, and the wear-resistant rubber can be produced easily in an industrialized mode; the no-blooming wear-resistant rubber finally prepared is moderate in hardness, the wearing value is small, shore A hardness is 66-69, and Akron wear is 0.08-0.09 cm<3>/1.61 km. The no-blooming wear-resistant rubber is suitable for preparing local wear-resisting blocks of rubber outsoles or overall rubber soles of shoes and boots, rubber soles composited with EVA, outsoles of dual-density rubber shoes and boots and the like.

Description

Wear-resisting glue of no blooming and preparation method thereof
Technical field
The invention belongs to shoe-making field, relate to a kind of rubber and preparation method thereof, be specifically related to wear-resisting glue of a kind of no blooming and preparation method thereof.
Background technology
Material for sole of shoe is most based on thermoplastic elastomer and elastomeric material.At the bottom of city shoe, by adding a large amount of reclaimed rubber, rubber powder or weighting agent in the plastic to reduce costs, shaping through hot compression molding, wear resistance is general, pliability, expandability and good bandability.But with rubber phase ratio, thermostability and weathering resistance poor, easily brittle, elasticity and wear resistance far less than the latter, and if possess at some application requirements that some is functional, such as oil resistant, high temperature resistant, resistance toly to subdue etc., the former limitation is mutually just to greatly.Also have some to be high-pressure polyethylene rubber-sole at present, the sole being major ingredient with high-pressure polyethylene and rubber, rubber and plastics are also used.
Chinese invention patent application CN102181081A discloses " a kind of high abrasion-resistant rubber for soles and preparation method thereof ", is made up of the raw material comprising following weight: 5 ~ 20 parts, SBR styrene-butadiene rubber(SBR), BR cis-1,4-polybutadiene rubber 70 ~ 100 parts, White Carbon black 35 ~ 55 parts, naphthenic oil 5 ~ 8 parts, promoting agent 3 ~ 6 parts, 4 ~ 7 parts, zinc oxide, stearic acid 0.8 ~ 1.5 part, promotor 2 ~ 3 parts, antifogging agent 0.4 ~ 0.6 part, 2 ~ 3 parts, sulphur.High abrasion glue has advantage wear-resisting significantly than traditional sole rubber.In this application, adopt butadiene-styrene rubber and cis-butadiene cement to be material of main part, processing technology is poor; Softening strengthening agent consumption is little, slightly high on cost; Also use antifogging agent in this invention, in the preparation of wear-resisting glue, the use of antifogging agent whether, actively affects not quite the anti-bloom of glue itself, but if improper use, on the contrary can accelerated deterioration.What this invention adopted is conventional vulcanization system, and post vulcanization is given prominence to, and postcure has hardness to become trend that is large, elongation step-down, is unfavorable for that the standing storage of cross-linked rubber uses.In general, be main formula for cis-butadiene cement, adopt SE curing system the most suitable.
Chinese invention patent application CN104448423A discloses " at the bottom of a kind of wear-resisting glue and preparation method thereof ", be prepared from by following two portions raw material: first part is prepared from by the raw material of following weight part: natural rubber 10-12, cis-1,4-polybutadiene rubber 4-46, zinc oxide 2-3, octadecanoic acid 1.66-1.68, N-sec.-propyl-N '-diphenyl-para-phenylene diamine 0.59-0.61,2,2,4-trimethylammonium-1,2-dihyaroquinoline 0.61-0.62, strengthening agent 32-34, all the other are solvent; Second section is the add-on on first part every kilogram basis, and it is sulphur 300g, captax 90-110g, accelerant CZ 190-210g, Vulcanization accelerator TMTD 20-30g.This application takes inverse compounding process, first the main ingredients beyond vulcanizing agent is dropped into banburying, and then drop into broken-(down)rubber mixing, finally add remainder reinforcing filler, flat machine adds vulcanizing agent, the rubber compounding after mixing is like this even, does not have bubble.Through detecting at the bottom of the glue that this formula makes, the abrasion DIN index of sizing material is 90cm3, is better than national standard, serves abrasion resistant effect.But the anti-aging agent wherein used is contaminative composition, and can not be used for light sizing material, range of application is limited to.
Chinese invention patent application CN102898694A discloses " a kind of super abrasive glue for sole and preparation method thereof ", is obtained: natural rubber 20-25 part, synthetic rubber 70-80 part, white carbon black 50-60 part, naphthenic oil 6-7 part, sulphur 1.5-2.5 part, vulcanization leveller 4-5 part, vulcanization accelerator 1.8-2.5 part, zinc oxide 4-6 part, stearic acid 1-1.5 part, antifogging agent 0.3-0.8 part, anti-wear agent 1-1.5 part, anti-aging agent 1-1.5 part by the raw material of following weight part; Synthesis super abrasive glue is made by these raw material banburyings being processed and inserting high-temperature pressurizing sulfuration in mould.This super abrasive glue being used for sole substantially increases the antiwear property of sole, and work-ing life.But it is main sizing material that conventional vulcanization system generally shall not be applied to cis-butadiene cement, and this is general knowledge, under hardening, flexibility, degradation drawback can show in the postcure phase; Do not use white carbon black activator to activate it, its vulcanization rate can be very slow, and be unfavorable for enhancing productivity, during sulfuration, energy consumption increase corresponding to labour cost is many.
Chinese invention patent application CN104059253A discloses " a kind of tire tread abrasion resistant compound combination and preparation method thereof ", and size composition comprises natural rubber, styrene-butadiene rubber(SBR), cis-butadiene cement, carbon black, zinc oxide, stearic acid, anti-aging agent, sulphur, aromatic hydrocarbon oil, promotor, strengthening agent, tackifier and dispersion agent, aromatic hydrocarbon oil is high hydrocarbon oil, tackifier are C5 resin, and carbon black is N110 and N234; This application combination can also add white carbon black; By plasticating, mixing and open the steps such as refining and make.The sizing material that tire fabric combination and preparation method thereof obtains has better tensile strength at yield, tensile strength and hardness.But the kind of carbon black particle diameter used is very little, and rubber mixing technique is not good, and operation easier is large and loaded down with trivial details; Employ carbon black and high hydrocarbon oil, have pollution, black sizing material can only be used for.
Summary of the invention
The technical problem to be solved in the present invention, is to provide wear-resisting glue of a kind of no blooming and preparation method thereof, adopts white carbon black as strengthening agent, be aided with multiple actives to activate it, regulate vulcanization rate, goods that are translucent or other any color and lusters can be made, pollution-free; Do not use antifogging agent can reach the effect of no blooming equally in the present invention, and provide that the cost of material is low, complete processing is simple, is easy to suitability for industrialized production; Final obtained no blooming abrasive rubber hardness is moderate, and wear(ing)value is little, Shore A hardness 63-69, Akron abrasion 0.08-0.09cm 3/ 1.61km.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
The wear-resisting glue of a kind of no blooming, it comprises the raw material of following parts by weight:
Natural rubber 20 ~ 25 parts, cis-1,4-polybutadiene rubber 75 ~ 80 parts, 5.7 ~ 6.8 parts, activator,
0.8 ~ 1.9 part, anti-aging agent, 6.0 ~ 9.0 parts, white carbon black activator, white carbon black 58 ~ 70 parts,
Look rubber master batch 0.5 ~ 5.0 part, non-polluting tenderizer 20 ~ 30 parts, vulcanizing agent 1.0 ~ 1.5 parts,
Promotor 2.2 ~ 3.7 parts, anti-wear agent 2.0 ~ 4.5 parts;
Wherein, activator comprises zinc oxide and stearic acid.
Limit as one of the present invention, described zinc oxide and stearic ratio of weight and number are 3.5 ~ 5.0:1.
Limit as another kind of the present invention, described anti-aging agent is SP-P;
Described white carbon black activator comprises polyoxyethylene glycol and glycol ether;
Described non-polluting tenderizer is white oil or naphthenic oil;
Described vulcanizing agent is sulphur;
Described promotor comprises the N-tertiary butyl-2-[4-morpholinodithio time yellow acid amides, MBT and tetramethylthiuram monosulfide;
Described anti-wear agent is SI-50.
As the further restriction of above-mentioned restriction, described polyoxyethylene glycol and the ratio of weight and number of glycol ether are 3.0 ~ 4.0:1.
Another kind as above-mentioned restriction limits further, and the ratio of weight and number of the described N-tertiary butyl-2-[4-morpholinodithio time yellow acid amides, MBT and tetramethylthiuram monosulfide is 4.0 ~ 5.0:1.2 ~ 2.0:1.
Another kind as above-mentioned restriction limits further, described SI-50 to be ratio of weight and number be 1:1 two-(the silica-based propyl group of γ-triethoxy) tetrasulfide and caoutchouc elasticity carrier.
Present invention also offers the method for the wear-resisting glue of the above-mentioned no blooming of preparation, it carries out according to following steps order:
1) checking that natural rubber reaches plasticity number is 0.40-0.46;
2) first natural rubber and cis-1,4-polybutadiene rubber are dropped into Banbury mixer, and refine 1-2min, lift floating weight, add activator, anti-aging agent, non-polluting tenderizer, white carbon black and white carbon black activator and start banburying, lift floating weight during 65-70 DEG C and turn over glue, cleaning residual powder once, lift floating weight during 85-90 DEG C and binder removal;
3) mill roll spacing is adjusted to 5 ~ 8mm, bottom sheet, water-cooled, and extension dries in the air, obtained rubber unvulcanizate;
4) rubber unvulcanizate adds vulcanizing agent, promotor, anti-wear agent and look rubber master batch, and cutter is turned over each five times in left and right, plays five triangle bags, cut-parts;
5) weigh, in vulcanizing press die cavity, carry out sulfuration, curing temperature is 150 ~ 155 DEG C, and the time is 5min, and pressure is 6 ~ 10kg/cm 2;
6) cross-linked rubber leaves standstill 10h, does Akron abrasion and DIN abrasion, the final obtained wear-resisting glue of no blooming.
The effect of the technical parameter in the formula of raw material used in the present invention and making method is specific as follows:
In general polydiene, the abrasion resistance after cis-butadiene cement sulfuration is better, and major cause is that its molecular chain kindliness is good, elasticity is high, second-order transition temperature lower (-95 ~-105 DEG C); But resist to fall block ability low during its main drawback pressurized, for this reason by natural gum and cis-butadiene cement by a certain percentage with the use of, better effect can be reached.
What select is fine particle precipitated silica, uses polyoxyethylene glycol and glycol ether to activate, can improve the tear strength of cross-linked rubber, add good heat resistance, be particularly useful for the environment of high-temperature wearable.Use coupling agent SI-50, the interface cohesion of filler/rubber can be strengthened, reduce white carbon black and assemble, improve dispersion, reduce the hysteresis loss of cross-linked rubber, greatly improve wear resistance.
There is after rubber vulcanization certain rigidity, use procedure is mainly based on fatigue abrasion and pounding wear, a large number of experiments show that, natural rubber and cis-1,4-polybutadiene rubber and the cracking resistance mouth propagation rate of cross-linked rubber and fatigue durability, higher than the blend compounds of natural rubber and styrene-butadiene rubber(SBR).
Bloom be liquid or solid Synergist S-421 95 by the phenomenon of rubber internal migration to rubber surface, cause the immanent cause of bloom to be that supersaturation or incompatible occurs some Synergist S-421 95 in sizing material.Through test of many times checking, formula vulcanization system of the present invention and processing condition reasonable in design, without bloom phenomenon.
Owing to have employed above-mentioned technical scheme, compared with prior art, acquired technical progress is in the present invention:
The present invention adopts white carbon black as strengthening agent, is aided with one or more promoting agents and activates it, regulates vulcanization rate, can make goods that are translucent or other any color and lusters, pollution-free; Furthermore, adopt glue based on natural rubber and cis-1,4-polybutadiene rubber, optimize strengthening agent and tenderizer consumption, then add physical whipping agent, proportion can be made less and at the bottom of the mold pressing that wear resistance is good.SE curing system provided by the present invention design, both ensure that cross-linked rubber had good intensity and wear resistance, simultaneously in standing storage on postcure again without affecting, decrease the risk of bloom, cross-linked rubber also can not be hardening; Do not use antifogging agent can reach the effect of no blooming equally in the present invention, and provide that the cost of material is low, complete processing is simple, is easy to suitability for industrialized production; Final obtained no blooming abrasive rubber hardness is moderate, and wear(ing)value is little, Shore A hardness 63 ~ 69, Akron abrasion 0.08 ~ 0.09cm 3/ 1.61km, DIN wear(ing)value 55 ~ 58mm 3.
The present invention be applicable to footwear boots rubber sole local wear-resistant block or with the rubber-sole of EVA compound and the preparation at the dual-density rubber footwear boots large end.
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment
embodiment 1 one kinds of wear-resisting glue of no blooming and preparation method thereof
The wear-resisting glue of a kind of no blooming, make with following raw material:
Natural rubber 25g, cis-1,4-polybutadiene rubber 75g, zinc oxide 4.7g, stearic acid 1g, SP-P0.8g, polyoxyethylene glycol 7.0g, glycol ether 2.0g, white carbon black 58g, look rubber master batch 1.0g, white oil 20g, sulphur 1.0g, the N-tertiary butyl-2-[4-morpholinodithio time yellow acid amides 1.4g, MBT 0.5g, tetramethylthiuram monosulfide 0.35g, SI-502.0g;
Wherein, described SP-P is the powdery solid that styrenated phenol is adsorbed in mineral filler by a certain percentage, Shanghai rubber ingredients factory, Kirin.
Prepare the method for the wear-resisting glue of above-mentioned no blooming, it is characterized in that it carries out according to following steps order:
1) checking that natural rubber reaches plasticity number is 0.45;
2) first natural rubber and cis-1,4-polybutadiene rubber are dropped into Banbury mixer, and refine 1min, lift floating weight, add activator, anti-aging agent, non-polluting tenderizer, white carbon black and white carbon black activator and start banburying, lift floating weight when 70 DEG C and turn over glue, cleaning residual powder once, when 90 DEG C, lift floating weight and binder removal;
3) mill roll spacing is adjusted to 7mm, bottom sheet, water-cooled, and extension dries in the air, obtained rubber unvulcanizate;
4) rubber unvulcanizate adds vulcanizing agent, promotor, anti-wear agent and look rubber master batch, and its ratio is 1:2.2:2:1, and cutter is turned over each five times in left and right, plays five triangle bags, cut-parts;
5) weigh, in vulcanizing press die cavity, carry out sulfuration, curing temperature is 150 DEG C, and the time is 5min, and pressure is 8kg/cm 2;
6) cross-linked rubber leaves standstill 10h, and do Akron abrasion and DIN abrasion, the Shore A hardness finally recorded is 69, Akron abrasion 0.09cm 3/ 1.61km, DIN abrasion are 58mm 3.
wear-resisting glue of embodiment 2-6 no blooming and preparation method thereof
Embodiment 2-6 is respectively wear-resisting glue of a kind of no blooming and preparation method thereof, and its raw material is similar to embodiment 1 to preparation method, and difference is only that technical parameter involved in the consumption of raw material and preparation method is different, shown in table specific as follows:
the wear test of embodiment 7 no blooming
The wear-resisting glue of no blooming obtained in embodiment 1-6 is carried out no blooming wear test, 1#-6# sulfuration blob of viscose is put into hydrothermal aging case (95% humidity, 70 DEG C, 72h) respectively, take out, after drenching solid carbon dioxide vapour, observe surface without atomization or whiting.
The wear-resisting glue of no blooming obtained by another Example 1, small drilling machine is used to cut into diameter for 16mm, the cylindric blob of viscose of thickness >=6mm, DIN wear testing machine is used to survey its wear loss respectively, according to the proportion of sizing material, calculate wear volume value, repeat said process three times, final wear(ing)value all gets the mean value of three test-results.
Contrast with prior art, result is as shown in the table:
as can be seen from the above table, the wear(ing)value of embodiment 1 is little, namely means that wear resistance at the bottom of cross-linked rubber is good.Compare the disclosed patent of other application, have larger technical superiority.
Analysis reason is as follows: what embodiment 1 adopted is SE curing system (0.8<S≤1.5), postcure phenomenon is negligible, cross-linked rubber quality is with the prolongation of storage period, test piece through 100 DEG C × 12h xeothermic aging after, the conservation rate of intensity and elongation reaches 85%; In Chinese patent CN102181081, employing be conventional vulcanization system (S≤1.8), post vulcanization is obvious, under equal simulation aging condition, maintenance Shuai≤50% of intensity and elongation, decay is very fast; In Chinese patent CN104448423, DIN wear(ing)value is much larger than example 1, and hardness is large.
Chinese patent CN104059253 and CN102898694, employing be conventional vulcanization system (S≤1.8), post vulcanization is obvious, and hardness is too large, and during sulfuration, required pressure is at least at more than 1.5MPa; Example 1 Shore A hardness is only 69, comfortable and easy to wear, and rubber vulcanization speed is fast, and can realize high temperature fast cure (160 DEG C × 4min), during dull and stereotyped pressure P≤0.5MPa, decorative pattern can be made clear, and production efficiency is high.
The above is only preferred embodiment of the present invention, is not restriction the present invention being made to other form, and any those skilled in the art may utilize above-mentioned technology contents to be changed or be modified as the Equivalent embodiments of equivalent variations as enlightenment.But everyly do not depart from technical solution of the present invention content, according to technical spirit of the present invention to the simple modification done by above embodiment, equivalent variations and remodeling, still belong to the protection domain of the claims in the present invention.

Claims (7)

1. the wear-resisting glue of no blooming, it is characterized in thatit comprises the raw material of following parts by weight:
Natural rubber 20 ~ 25 parts, cis-1,4-polybutadiene rubber 75 ~ 80 parts, 5.7 ~ 6.8 parts, activator,
0.8 ~ 1.9 part, anti-aging agent, 6.0 ~ 9.0 parts, white carbon black activator, white carbon black 58 ~ 70 parts,
Look rubber master batch 0.5 ~ 5.0 part, non-polluting tenderizer 20 ~ 30 parts, vulcanizing agent 1.0 ~ 1.5 parts,
Promotor 2.2 ~ 3.7 parts, anti-wear agent 2.0 ~ 4.5 parts;
Wherein, activator comprises zinc oxide and stearic acid.
2. the wear-resisting glue of no blooming according to claim 1, it is characterized in that:described zinc oxide and stearic ratio of weight and number are 3.5 ~ 5.0:1.
3. the wear-resisting glue of no blooming according to claim 1, it is characterized in that:described anti-aging agent is SP-P;
Described white carbon black activator comprises polyoxyethylene glycol and glycol ether;
Described non-polluting tenderizer is white oil or naphthenic oil;
Described vulcanizing agent is sulphur;
Described promotor comprises the N-tertiary butyl-2-[4-morpholinodithio time yellow acid amides, MBT and tetramethylthiuram monosulfide;
Described anti-wear agent is SI-50.
4. the wear-resisting glue of no blooming according to claim 3, it is characterized in that:described polyoxyethylene glycol and the ratio of weight and number of glycol ether are 3.0 ~ 4.0:1.
5. the wear-resisting glue of no blooming according to claim 3, it is characterized in that:the ratio of weight and number of the described N-tertiary butyl-2-[4-morpholinodithio time yellow acid amides, MBT and tetramethylthiuram monosulfide is 4.0 ~ 5.0:1.2 ~ 2.0:1.
6. the wear-resisting glue of no blooming according to claim 3, it is characterized in that:described SI-50 to be ratio of weight and number be 1:1 two-(the silica-based propyl group of γ-triethoxy) tetrasulfide and caoutchouc elasticity carrier.
7. prepare a method for the wear-resisting glue of no blooming according to any one of claim 1-6, it is characterized in that it carries out according to following steps order:
1) checking that natural rubber reaches plasticity number is 0.40-0.46;
2) first natural rubber and cis-1,4-polybutadiene rubber are dropped into Banbury mixer, and refine 1-2min, lift floating weight, add activator, anti-aging agent, non-polluting tenderizer, white carbon black and white carbon black activator and start banburying, lift floating weight during 65-70 DEG C and turn over glue, cleaning residual powder once, lift floating weight during 85-90 DEG C and binder removal;
3) mill roll spacing is adjusted to 5-8mm, bottom sheet, water-cooled, and extension dries in the air, obtained rubber unvulcanizate;
4) rubber unvulcanizate adds vulcanizing agent, promotor, anti-wear agent and look rubber master batch, and cutter is turned over each five times in left and right, plays five triangle bags, cut-parts;
5) weigh, in vulcanizing press die cavity, carry out sulfuration, curing temperature is 150 ~ 155 DEG C, and the time is 5min, and pressure is 6 ~ 10kg/cm 2;
6) cross-linked rubber leaves standstill 10h, does Akron abrasion and DIN abrasion, the final obtained wear-resisting glue of no blooming.
CN201510498714.4A 2015-08-14 2015-08-14 No-blooming wear-resistant rubber and preparing method thereof Pending CN105086013A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106220911A (en) * 2016-08-30 2016-12-14 浙江中瑞橡胶高分子材料股份有限公司 A kind of density vulcanized rubber shoes less than 1 molds big-sole formula
CN107841147A (en) * 2017-11-24 2018-03-27 东莞新东方科技有限公司 No blooming not bleed hot press moulding conduction button silicon rubber and preparation method thereof
CN111995797A (en) * 2019-10-25 2020-11-27 江苏卡欧化工股份有限公司 Anti-bluing agent for shoe material and preparation method thereof
CN118027526A (en) * 2024-01-19 2024-05-14 诚天科技实业(广东)有限公司 Outdoor anti-skid wear-resistant sole and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102212216A (en) * 2010-04-09 2011-10-12 中国皮革和制鞋工业研究院 Sneaker sole material with high wear resistance and low hardness and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102212216A (en) * 2010-04-09 2011-10-12 中国皮革和制鞋工业研究院 Sneaker sole material with high wear resistance and low hardness and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106220911A (en) * 2016-08-30 2016-12-14 浙江中瑞橡胶高分子材料股份有限公司 A kind of density vulcanized rubber shoes less than 1 molds big-sole formula
CN107841147A (en) * 2017-11-24 2018-03-27 东莞新东方科技有限公司 No blooming not bleed hot press moulding conduction button silicon rubber and preparation method thereof
CN111995797A (en) * 2019-10-25 2020-11-27 江苏卡欧化工股份有限公司 Anti-bluing agent for shoe material and preparation method thereof
CN118027526A (en) * 2024-01-19 2024-05-14 诚天科技实业(广东)有限公司 Outdoor anti-skid wear-resistant sole and preparation method thereof
CN118027526B (en) * 2024-01-19 2024-09-17 诚天科技实业(广东)有限公司 Outdoor anti-skid wear-resistant sole and preparation method thereof

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