WO2023152774A1 - A rubber composition using natural fibers for tyre tread and method thereof - Google Patents

A rubber composition using natural fibers for tyre tread and method thereof Download PDF

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Publication number
WO2023152774A1
WO2023152774A1 PCT/IN2023/095001 IN2023095001W WO2023152774A1 WO 2023152774 A1 WO2023152774 A1 WO 2023152774A1 IN 2023095001 W IN2023095001 W IN 2023095001W WO 2023152774 A1 WO2023152774 A1 WO 2023152774A1
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Prior art keywords
phr
rubber composition
rubber
highway
tyre tread
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PCT/IN2023/095001
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French (fr)
Inventor
Brindha Senthilraja
Arthi P.S
Kadambanathan THIAGARAJAN
Viswanathan Sivaramakrishnan
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Tvs Srichakra Limited
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Publication of WO2023152774A1 publication Critical patent/WO2023152774A1/en

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • C08L9/06Copolymers with styrene
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B60VEHICLES IN GENERAL
    • B60CVEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
    • B60C1/00Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
    • B60C1/0016Compositions of the tread

Definitions

  • the present invention relates to the field of Polymer Technology.
  • the present invention in particular relates to an environment- friendly off highway tyre tread rubber composition and its method of preparation.
  • Off highway tyres also termed as all terrain tyres (on and off roads) need to provide maximum grip on the loose surfaces. Cut and chip resistance and abrasion resistance of off highway tyre is most important, where the tyres are in contact with gravel, rock soil and in uneven terrain surfaces. Excessive tread wear is also common cause in off highway tyres. The wear that causes due to fatigue and it further change into abrasive wear. Then the abrasive wear turns into cutting and chipping in tyre treads.
  • the tread of the tire is in direct contact with the ground, braking characteristics are important to prepare for unexpected or sudden situations, and, in terms of economy, wear resistance can be used for a long time is important.
  • the abrasion resistance of the tread of an off highway tire is determined by the nature of the tread surface layer in contact with the ground, and heat generated during high-speed driving causes deterioration of the physical properties of the tread and deterioration of the abrasion resistance.
  • CN109181144 discloses a wood-plastic composite material added with sunflower leaf fiber and an application thereof and relates to the technical field of wood-plastic profiles.
  • the material contains the following raw materials: polyvinyl chloride resin powder SG-4, hydroxypropyl methacrylate, the Chinese fan palm leaf fiber, niobium yttrium tailing powder, nano bismuth vanadate powder, JYM-087B rubber powder, tributoxyethyl phosphate, compound dispersant, a compound coupling agent, a compound foaming agent and an antioxygen anti-aging agent.
  • the wood-plastic composite material disclosed by the invention has the advantages that the mechanical strength, the physical stability, the purification ability, the antibacterial property, the shielding property and the like are remarkably improved; the overall performance is more excellent; the applicability is better; and the service life is more guaranteed.
  • WO2014159805 relates to a coated rubber composition includes a rubber composition coated with a liquid refresh agent selected from the group consisting of one or more liquid terpenes, limonene, carvone, pinene, pine needle oil, citral, orange oil, C9-C15 aliphatics, C9-C15 cyclo aliphatic s, ethyl lactate, dipentene, 1,8-cineole, eucalyptol, citronellol, geraniol, citronellene, terpinen-4-ol, and combinations thereof.
  • a method of application and a coated rubber composition are also disclosed.
  • PAF pineapple Leaf fibers
  • PP Polypropylene
  • MAPP Maleated Polyolefin
  • PALF/Glass fiber PP hybrid composites Improved interfacial adhesion in case of PALF/Glass fiber PP hybrid composites was confirmed with considerably lesser fiber pull out and gaps between the fibers and the PP matrix.
  • the mechanical performance and the durability of PALF fiber reinforced PP composites can be enhanced by hybridization with the addition of glass fibers for use in high performance engineering applications.
  • US409608 relates to a new and useful vegetable fiber produced from the leaves or pine-needles, as they are commonly termed, of the Pinus Australis or other coniferous trees by both chemical and mechanical treatment, whereby obtain a new product or article of manufacture termed by pine fiber, a fiber which will felt or can be spun and woven with substantially the same facility as ordinary wool.
  • a tire tread rubber composition comprises a petroleum resin 1 ⁇ 10 parts by weight having a flash point 270-300 °C, softening point 105+5 °C, and specific gravity 1.0+0.3 based on the base rubber 100.0 parts by weight; pyroligneous liquor 1—10 parts by weight obtained from one or more selected from the group consisting of pine, larch, oak, cryptomeria japonica, big-cone pine, fir, korean fir, oak tree, spruce and bamboo; and at least one reinforcing filler 10-80 parts by weight selected from the group consisting of titanium dioxide, clay, layered silicate, tungsten and talc.
  • Publication No. CA2576167 relates to a process for producing a conjugated diene copolymer rubber which comprise s initiating a copolymerization reaction in a reaction system containing a first conjugated diene compound and a first aromatic vinyl compound and completing the reaction, adding a first polyfunctional monomer to the reaction system, optionally further adding a second conjugated diene compound and a second aromatic vinyl compound, and further conducting copolymerization reaction, and adding a modifier to the reaction system to react the modifier with the copolymer.
  • a rubber composition having excellent processability, exhibiting sufficient hardness even after vulcanization, and possessing reduced rolling resistance can be obtained.
  • JP6382793 relates to a rubber composition with excellent reinforcement properties by improving the dispersibility of fibers in a rubber component when the fibers are added to the rubber, a method for manufacturing the same, a vulcanized rubber, and a tire.
  • a rubber composition comprising a rubber component and short fibers, wherein the short fibers are cationized.
  • a method for manufacturing the rubber composition comprising a mixing step for mixing cationized short fibers and rubber latex to prepare a rubber- short fiber mixed solution, and a drying step for drying the rubber- short fiber mixed solution to give a rubber composition.
  • JP2021004293 relates to a rubber composition for a tire that enables improvement of water-resistant adhesiveness while reducing viscosity.
  • the rubber composition for a tire is produced by blending, based on 100 pts. mass of diene rubber including 50 mass% or more of natural rubber, 25 pts. mass to 140 pts. mass of carbon black having an iodine adsorption amount of 30 g/kg to 130 g/kg, 2 pts. mass to 10 pts. mass of sulfur and 0.2 pt. mass to 3.5 pts. mass of pine tar and blending 0.05 pt. mass to 1 pt.
  • Publication No. GB453299 relates to rubber - bituminous compositions, which when diluted with water may be used as a paint, are emulsions, each containing a stabilizing agent such as casein, by incorporating with the latex and with the emulsion separately finely divided solid non-colloidal mineral filling material in such proportion that each becomes of a plastic consistency and then mixing together in the cold the two resulting plastics.
  • Filling materials specified are talc, loomite, burnt fireclay, barytes, slate dust, whinstone flour; different filling materials may be added to the latex and to the emulsion prepared from rubber latex and aqueous bituminous. Up to about 60 per cent by weight of filling material may be added to the latex and up to about 40 per cent may be added to the emulsion.
  • the latex plastic and the bitumen plastic may be mixed in proportions varying from 50—50 per cent to 90—10 per cent by weight, although the amount of bitumen plastic present may exceed the amount of latex plastic.
  • Publication No. CN103570968 relates to an environmentally -friendly high-tenacity tire reclaimed rubber making method.
  • the method sequentially comprises the following steps: selecting materials and crushing; carrying out sieving magnetic separation; carrying out charging stirring; desulphurizing; plasticating; refining; filtering; and molding.
  • the invention discloses a formula of a composition of an environmentally -friendly high-tenacity tire reclaimed rubber.
  • the formula comprises, by weight, 100 parts of rubber powder, 7-10 parts of an environmentally-friendly rubber softener, and 1-2 parts of an adhesion agent.
  • CN107915879 relates to a composition of a long-service-life automobile tire inner tube.
  • Raw materials of the composition comprise, by weight, 20-40 parts of butadiene styrene rubber, 20-40 parts of chloroprene rubber, 15-25 parts of phenolic aldehyde tackifying resin, 15-25 parts of rosin soft butylbenzene, 5-10 parts of N33O carbon black, 5-10 parts of light calcium carbonate, 5-10 parts of stearic acid, 4-8 parts of anti-aging agent, 4-8 parts of tackifier, 4-8 parts of softener, 1-5 parts of aromatic hydrocarbon oil, 1-5 parts of pine tar, 0.6- 1 part of accelerant, 0.6-1 part of foaming agent and 0.6-1 part of active agent.
  • the compressive strength and flexibility of the inner tube can be improved, the damping effect can be achieved, accordingly, the service life of a tire is prolonged, and the requirement of current development is met
  • a sidewall rubber composition with improved blooming resistance comprises 100 parts by weight of a base rubber and 5 ⁇ 10 parts by weight of vegetable oil-based softeners modified with alkyl oxide-based light base.
  • the alkyl oxidebased light base is one or more selected from the group consisting of CH2CO3, ethylene oxide, and alkylbenzoate.
  • the vegetable oil-based softener is one or more selected from the group consisting of castor oil, linseed oil, pine tar, tall oil, and palm oil.
  • the composites were prepared using two-roll mill and were cured using compression moulding with keeping the fiber orientation. These composites were characterized using moving die rheometer (MDR), dynamic mechanical thermal analysis (DMTA) and tensile testing. The morphology after cryogenic fracture was observed using scanning electron microscopy (SEM). The effect of NBR from 0 to 20 phr of total rubber content was investigated. NBR is proposed to encase PALF leading to higher stress transfer between matrix and PALF. The method of mixing was also studied. For the fiber surface treatment, propylsilane, allylsilane and silane-69 were treated on the alkali-treated fiber.
  • MDR moving die rheometer
  • DMTA dynamic mechanical thermal analysis
  • SEM scanning electron microscopy
  • Treated fibers were characterized using Fourier-Transform infrared spectroscopy (FTIR), x- ray photoelectron spectroscopy (XPS) and SEM.
  • FTIR Fourier-Transform infrared spectroscopy
  • XPS x- ray photoelectron spectroscopy
  • SEM SEM
  • Silane-69 treatment of fiber increased the modulus at low deformation more than the incorporation of NBR of NR/PALF composites due to the chemical crosslinking between rubber and fiber from silane-treatment rather than the physical interaction of NR, NBR and fiber.
  • reinforcement by fiber reduced the deformation at break.
  • carbon black was also incorporated into NR/NBR/PALF and NR/surface-treated PALF composites to improve the ultimate properties. By incorporation of carbon black 30 phr in both composites, the mechanical properties of composites were improved and can be controlled at both low and high deformations.
  • the present invention aims to provide an environmentfriendly off highway tyre tread composition and its method of preparation. Also, to provide an off highway tire tread rubber composition with abrasion resistance and cut-and-chip performance.
  • the principal object of the present invention is to provide environment friendly off-highway tyre tread composition and its method of preparation.
  • Another object of the present invention is to provide off highway tyre tread composition having improved abrasion resistance.
  • Yet another object of the present invention is to provide off highway tyre tread composition which provides better cut and chip resistance and high hardness.
  • Yet another object of the present invention is to provide off highway tyre tread rubber composition which provides better wet and dry grip.
  • NR natural rubber
  • SBR Styrene butadiene rubber
  • PBR PolyButadiene Rubber
  • MC wax Microcrystalline wax
  • primary accelerators is selected from n- cyclohexyl-2-benzothiazole sulfonamide (CBS).
  • First stage as mastication of rubber at a temperature of 70+5 degree Celsius; blending of natural fiber selected from screw pine leaf fiber having length of 1-5 mm in two roll mill; Second stage as loading first stage rubber compound in Banbury mixer and mixing for 0-35 seconds at a temperature 65-80°C; further add 75% carbon black, 100% silica, rubber chemicals MC wax, wood rosin, and TDAE oil for 90 to 230 seconds; sweeping down in the orifice and mixing for 80 to 102 seconds; further mixing is continued until dump temperature in the range between 130 and 160°C and sheet out; third stage as addition of 25% carbon black, zinc oxide, 6PPD, and mix for 60 - 180 seconds, and dump at a temperature range between
  • processing parameters include rotational speed of 55 to 60 rpm for master batch, preparation of final batch: mixing of master batch rubber compound and curatives for 60-90 seconds, dumped at temperature range between 95 °C and 115°C, and sheet out, wherein the rubbers are selected from natural rubber (NR), Styrene butadiene rubber (SBR), Poly Butadiene Rubber (PBR), and combinations thereof, preferably in a weight ratio of NR: SBR: PBR - 30-85:5-40:10-30 phr.
  • NR natural rubber
  • SBR Styrene butadiene rubber
  • PBR Poly Butadiene Rubber
  • Figure 1 represents the screw pine leaf fibre blend with polymers.
  • the present invention relates to a high quality off highway tyre tread composition and its method of preparation.
  • Screw pine leaf fibre is used in natural rubber and synthetic rubber triblend (NR:SBR: PBR) based rubber composition to provide off highway tyre tread composition.
  • the present invention uses screw pine leaf fibre in off highway tyre tread rubber composition to provide better cut and chip resistance, abrasion resistance and higher hardness.
  • An off highway tyre tread rubber composition comprises one or more rubbers ; reinforcing filler carbon black: 20 to 60 phr; silica: 0 to 15 phr; 0.5 to 10 phr of screw pine leaf fibre, presence of screw pine leaf fibre in rubber compound reduces the rubber chain mobility and it makes the rubber compound more rigid which turns into better reinforcement properties of rubber vulcanizate; wood rosin; activators; anti-degradants; vulcanization agent; primary accelerators; and process aid.
  • Natural Rubber - RSS 3 Natural Rubber - Ribbed Smoke Sheet
  • Carbon black - ASTM grade N234 is from ASTM Grade Aljubail Carbon, Saudi Arabia. It is the reinforcing filler ISAF, Intermediate Superior Abrasion Furnace having the Iodine adsorption No. 115 to 125 mg/gm, tinting strength value between 114 to 124 % ITRB, statistical thickness surface area value between 107 to 117 m 2 /gm
  • Wood rosin -It is a tackifier resin from Kanchi Karpooram Ltd, Kanchipuram, India
  • Zinc Oxide from POCL Enterprises Limited, India. It is an activator added to the rubber compound to activate sulphur vulcanization
  • Stearic acid from 3F Industries Ltd., India. It is used as a Process aid. Also, Zinc oxide and Stearic acid are added to form zinc soap, improves the solubility of zinc oxide in the compound, and with the accelerator to form a complex, this complex reacts with sulphur to produce a strong cure activating system.
  • MC Wax - Microcrystalline wax is used to provide a physical barrier on the surface of a tire. This physical barrier prevents attack on the rubber from ozone present in the atmosphere.
  • 6PPD - (N-(l,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine) is an antidegradant from Nocil Limited, India.
  • TDAE Oil- Treated Distillate Aromatic Extract Oil is a non-carcinogenic mineral oil. It is from Panama Petrochem Ltd, India.
  • CBS N-cyclohexyl-2-benzothiazolesulfenamide from Nocil Limited, India. It is a delayed action accelerator suitable for diene rubbers.
  • Sulphur is the vulcanizing agent from The Standard Chemical Co. Pvt Ltd, India.
  • Rubber composition - Method of Preparation A rubber composition prepared by a thermo mechanical process which comprises the sequential mixing steps, Thermomechanically mixing with the preparatory mixing step - master batch is as follows:
  • Step I Mixing in Two roll mill
  • Rubber is masticated in a two-roll mill with the roll temp 70+/-5 deg C to form a band on roll and then the screw pine leaf fibre with the length of 1 to 5 mm is added into the masticated rubber to attain uniform orientation of screw pine leaf fibre in rubber blend.
  • Step II Mixing in Banbury Mixer
  • Mixing has been done with the head temperature of the Banbury maintained between 65 to 80°C and the unloaded rotor speed maintained between 55 to 60 rpm.
  • the mixing cycle is to be followed as: a) Mixing chamber has been charged with step I rubber compound (rubber + screw pine leaf fibre blend) and allowed to mix for 0 to 35 seconds b) and further, 75% of carbon black, 100% of silica, rubber chemicals MC wax, wood rosin, TDAE oil, and allowed to mix for 90 to 230 seconds, c) sweeping has been done in the orifice and allowed to mix for another 80 to 102 seconds, the compound has been dumped at the temperature in the range of 130°C to 165°C and sheeted out in the laboratory two roll mill.
  • Step III Add the step II master batch in the Lab Banbury Mixer and add remaining 25% of carbon black, Zinc oxide, 6PPD and mix it for 60 seconds to 180 seconds and the compound has been dumped at the temperature in the range of 125 °C to 155 °C and sheeted out in the laboratory two roll mill.
  • Thermomechanical mixing in at least one preparatory mixing step - final batch is as follows: Mixing chamber charged with the master batch rubber compound and the curatives, and allowed to mix for 60 to 90 seconds and the compound has been dumped at the temperature in the range of upto the temperature 95 °C to 115°C. The final batch sheet out has been done in the laboratory two roll mill.
  • rubber composition Fl is prepared based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre against rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers is prepared and evaluated.
  • rubber composition F2 is prepared based on NR: SBR 1739: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black is replaced with 5 phr of screw pine leaf fibre against rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers is prepared and evaluated.
  • the present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre hardness value is 70 Shore A.
  • the present invention provides a 100 parts by weight of rubber composition F2, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black is replaced with 5 phr of screw pine leaf fibre provides hardness value is 66 Shore A (Note: Silica filler in not used).
  • the present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides scorch time ts value is 26.42 minutes (Ideal value of scorch time is 15 minutes).
  • present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides scorch time ts value is 29.30minutes (Ideal value of scorch time is 15 minutes).
  • the present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides abrasion loss value lowered by 9.61% (i.e., better abrasion resistance) when compared to rubber composition Cl based on NR:SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
  • the present invention provides a 100 parts by weight of rubber composition F2, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black is replaced with 5 phr of screw pine leaf fibre provides abrasion loss value lowered by 7.45% (i.e., better abrasion resistance) when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
  • the present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR 1739: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides weight loss and diameter loss value lowered by 1.60% and 28.72% respectively (i.e., better cut and chip resistance) when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
  • the present invention provides a 100 parts by weight of rubber composition F2, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black is replaced with 5 phr of screw pine leaf fibre provides weight loss and diameter value lowered by 28.72 % and 36.84 % respectively (i.e., better cut and chip resistance) when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
  • the present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR 1739: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides tan delta value at 0 deg C is improved by 11.26% when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
  • the present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides tan delta value at 25 deg C is improved by 6.48 % when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
  • the present invention provides a 100 parts by weight of rubber composition, NR: SBR: PBR (40 phr: 30 phr: 30 phr) triblend based rubber composition reinforced by carbon black containing 5 phr of pineapple leaf fibre provides better abrasion resistance (wear resistance) and cut and chip resistance along with better process safety.
  • the present invention provides a 100 parts by weight of rubber composition, NR: SBR: PBR (40 phr: 30 phr: 30 phr) triblend based rubber composition reinforced by carbon black and silica filler containing 5 phr of screw pine leaf fibre provides better wet grip and dry grip property.
  • the resulting vulcanized rubber compositions shall be evaluated for
  • Mooney Scorch time at 125 deg C, t5 value is measured in accordance with ASTM D1646 in Mooney Viscometer MV2000, Alpha technologies, USA.
  • Shore A Hardness of the Rubber Vulcanizate is assessed in accordance with ASTM D 2240.
  • M3 Abrasion loss in mm 3 is measured using Din Abrader in accordance with ASTM D 5963.
  • M4 Cut and chip resistance of the rubber vulcanizate is measured to understand the relative service life of the off highway tyre subjected to uneven terrains (i.e., to predict service performance of the tyre tread that are subjected to contacting surfaces containing sharp objects such as rocks, gravels etc.,) using Goodrich Cut and Chip Tester. Cutting takes place when the tyre tread hits a sharp object with the sufficient force that the surface is cut, creating a new surface area. Chipping follows cutting and involves fracturing away of a piece of rubber from the surface. Test specimen Speed: 760 rpm; Cut chip cycle-Frequency: 60HZ; Test cycle - 10 Minutes. Weight loss and diameter reduction are measured after 10 minutes of test time.
  • Dynamic properties/Visco elastic properties of the Rubber vulcanizate The dynamic properties of the rubber vulcanizate are measured on a dynamic mechanical analyzer (DMA Metravib +1000) in tension mode with the temperature sweep -40 to 100 °C, Dynamic strain: 0.3%, Static strain:0.6%, Frequency: 10 Hz.
  • Tan delta at 0°C is a predictor for wet grip (Higher tan delta value at 0 °C is good for wet grip property) and tan delta at 25 °C is a predictor for dry grip (Higher tan delta value at 25 °C is good for dry grip property).

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Abstract

The present invention relates to an off highway tyre tread composition and its method of preparation and the rubber composition of an Off highway tyre tread which includes 100 phr of natural rubber and synthetic rubber blends, and 20 to 60 phr of reinforcing filler carbon black and 0 to 15 phr of reinforcing filler silica and 0.5 - 10 phr of screw pine leaf fibre and the said rubber composition is to provide better abrasion resistance and an improved cut and chip resistance.

Description

A RUBBER COMPOSITION USING NATURAE FIBERS FOR TYRE TREAD AND METHOD THEREOF
FIELD OF THE INVENTION
The present invention relates to the field of Polymer Technology. The present invention in particular relates to an environment- friendly off highway tyre tread rubber composition and its method of preparation.
BACKGROUND OF THE INVENTION
The performance required for Off highway tyres varies greatly depending on the site function and end use of the tire. Off highway tyres also termed as all terrain tyres (on and off roads) need to provide maximum grip on the loose surfaces. Cut and chip resistance and abrasion resistance of off highway tyre is most important, where the tyres are in contact with gravel, rock soil and in uneven terrain surfaces. Excessive tread wear is also common cause in off highway tyres. The wear that causes due to fatigue and it further change into abrasive wear. Then the abrasive wear turns into cutting and chipping in tyre treads. Since the tread of the tire is in direct contact with the ground, braking characteristics are important to prepare for unexpected or sudden situations, and, in terms of economy, wear resistance can be used for a long time is important. The abrasion resistance of the tread of an off highway tire is determined by the nature of the tread surface layer in contact with the ground, and heat generated during high-speed driving causes deterioration of the physical properties of the tread and deterioration of the abrasion resistance.
Reference made to the following inventions:
Publication No. CN109181144 discloses a wood-plastic composite material added with sunflower leaf fiber and an application thereof and relates to the technical field of wood-plastic profiles. The material contains the following raw materials: polyvinyl chloride resin powder SG-4, hydroxypropyl methacrylate, the Chinese fan palm leaf fiber, niobium yttrium tailing powder, nano bismuth vanadate powder, JYM-087B rubber powder, tributoxyethyl phosphate, compound dispersant, a compound coupling agent, a compound foaming agent and an antioxygen anti-aging agent. The wood-plastic composite material disclosed by the invention has the advantages that the mechanical strength, the physical stability, the purification ability, the antibacterial property, the shielding property and the like are remarkably improved; the overall performance is more excellent; the applicability is better; and the service life is more guaranteed.
Publication No. WO2014159805 relates to a coated rubber composition includes a rubber composition coated with a liquid refresh agent selected from the group consisting of one or more liquid terpenes, limonene, carvone, pinene, pine needle oil, citral, orange oil, C9-C15 aliphatics, C9-C15 cyclo aliphatic s, ethyl lactate, dipentene, 1,8-cineole, eucalyptol, citronellol, geraniol, citronellene, terpinen-4-ol, and combinations thereof. A method of application and a coated rubber composition are also disclosed.
IN Publication No. 308/KOL/2007 relates to pineapple Leaf fibers (PALF) reinforced Polypropylene (PP) composites and PALF/Glass fiber reinforced PP hybrid composites were fabricated using melt blending followed by injection moulding. Maleated Polyolefin (MAPP) was used as a coupling agent to improve the adhesion between the hydrophilic fibers and hydrophobic PP matrix. Incorporation of upto 20 weight % of glass fibers into PALF-PP composites at 20 weight % of PALF and 2 weight % of MAPP, the mechanical strength increased substantially, compared to those of PALF-PP composites. The sorption behaviour and effects of environmental ageing on tensile properties were also dramatically reduced with incorporation of glass fibers. Improved interfacial adhesion in case of PALF/Glass fiber PP hybrid composites was confirmed with considerably lesser fiber pull out and gaps between the fibers and the PP matrix. The mechanical performance and the durability of PALF fiber reinforced PP composites can be enhanced by hybridization with the addition of glass fibers for use in high performance engineering applications.
Publication No. US409608 relates to a new and useful vegetable fiber produced from the leaves or pine-needles, as they are commonly termed, of the Pinus Australis or other coniferous trees by both chemical and mechanical treatment, whereby obtain a new product or article of manufacture termed by pine fiber, a fiber which will felt or can be spun and woven with substantially the same facility as ordinary wool.
Publication No. KR100917446 relates to a tire tread rubber composition to improve cut and chip performance and exothermic performance and to increase abrasion resistance by comprising petroleum resin and pyroligneous liquor. A tire tread rubber composition comprises a petroleum resin 1~ 10 parts by weight having a flash point 270-300 °C, softening point 105+5 °C, and specific gravity 1.0+0.3 based on the base rubber 100.0 parts by weight; pyroligneous liquor 1—10 parts by weight obtained from one or more selected from the group consisting of pine, larch, oak, cryptomeria japonica, big-cone pine, fir, korean fir, oak tree, spruce and bamboo; and at least one reinforcing filler 10-80 parts by weight selected from the group consisting of titanium dioxide, clay, layered silicate, tungsten and talc.
Publication No. CA2576167 relates to a process for producing a conjugated diene copolymer rubber which comprise s initiating a copolymerization reaction in a reaction system containing a first conjugated diene compound and a first aromatic vinyl compound and completing the reaction, adding a first polyfunctional monomer to the reaction system, optionally further adding a second conjugated diene compound and a second aromatic vinyl compound, and further conducting copolymerization reaction, and adding a modifier to the reaction system to react the modifier with the copolymer. A rubber composition having excellent processability, exhibiting sufficient hardness even after vulcanization, and possessing reduced rolling resistance can be obtained.
Publication No. JP6382793 relates to a rubber composition with excellent reinforcement properties by improving the dispersibility of fibers in a rubber component when the fibers are added to the rubber, a method for manufacturing the same, a vulcanized rubber, and a tire. A rubber composition comprising a rubber component and short fibers, wherein the short fibers are cationized. A method for manufacturing the rubber composition, comprising a mixing step for mixing cationized short fibers and rubber latex to prepare a rubber- short fiber mixed solution, and a drying step for drying the rubber- short fiber mixed solution to give a rubber composition.
Publication No. JP2021004293 relates to a rubber composition for a tire that enables improvement of water-resistant adhesiveness while reducing viscosity. The rubber composition for a tire is produced by blending, based on 100 pts. mass of diene rubber including 50 mass% or more of natural rubber, 25 pts. mass to 140 pts. mass of carbon black having an iodine adsorption amount of 30 g/kg to 130 g/kg, 2 pts. mass to 10 pts. mass of sulfur and 0.2 pt. mass to 3.5 pts. mass of pine tar and blending 0.05 pt. mass to 1 pt. mass of a resin acid cobalt salt as a metallic cobalt content. Publication No. GB453299 relates to rubber - bituminous compositions, which when diluted with water may be used as a paint, are emulsions, each containing a stabilizing agent such as casein, by incorporating with the latex and with the emulsion separately finely divided solid non-colloidal mineral filling material in such proportion that each becomes of a plastic consistency and then mixing together in the cold the two resulting plastics. Filling materials specified are talc, loomite, burnt fireclay, barytes, slate dust, whinstone flour; different filling materials may be added to the latex and to the emulsion prepared from rubber latex and aqueous bituminous. Up to about 60 per cent by weight of filling material may be added to the latex and up to about 40 per cent may be added to the emulsion. The latex plastic and the bitumen plastic may be mixed in proportions varying from 50—50 per cent to 90—10 per cent by weight, although the amount of bitumen plastic present may exceed the amount of latex plastic.
Publication No. CN103570968 relates to an environmentally -friendly high-tenacity tire reclaimed rubber making method. The method sequentially comprises the following steps: selecting materials and crushing; carrying out sieving magnetic separation; carrying out charging stirring; desulphurizing; plasticating; refining; filtering; and molding. The invention discloses a formula of a composition of an environmentally -friendly high-tenacity tire reclaimed rubber. The formula comprises, by weight, 100 parts of rubber powder, 7-10 parts of an environmentally-friendly rubber softener, and 1-2 parts of an adhesion agent. The use of severe-pollution and high-aromatic hydrocarbon-content additives comprising coal tar, aromatic hydrocarbon oil, pine tar and the like in the prior art is prevented and the environmentally-friendly rubber softener and the adhesion agent are used in the reclaimed rubber production process, regeneration is carried out at a high temperature under a normal pressure, and regeneration activators comprising 420 and 450 are not added in the regeneration process, so thorough desulphurization is realized, the tenacity of the reclaimed rubber is improved, harmful substances are not contained.
Publication No. CN107915879 relates to a composition of a long-service-life automobile tire inner tube. Raw materials of the composition comprise, by weight, 20-40 parts of butadiene styrene rubber, 20-40 parts of chloroprene rubber, 15-25 parts of phenolic aldehyde tackifying resin, 15-25 parts of rosin soft butylbenzene, 5-10 parts of N33O carbon black, 5-10 parts of light calcium carbonate, 5-10 parts of stearic acid, 4-8 parts of anti-aging agent, 4-8 parts of tackifier, 4-8 parts of softener, 1-5 parts of aromatic hydrocarbon oil, 1-5 parts of pine tar, 0.6- 1 part of accelerant, 0.6-1 part of foaming agent and 0.6-1 part of active agent. According to the composition of the long-service-life automobile tire inner tube, the compressive strength and flexibility of the inner tube can be improved, the damping effect can be achieved, accordingly, the service life of a tire is prolonged, and the requirement of current development is met.
Publication No. KR20110083385 relates to a sidewall rubber composition with improved blooming resistance and tire using the same to improve the appearance of tire by improving a blooming phenomenon using a large amount of vegetable oil-based softeners modified with alkyl oxide-based light base. A sidewall rubber composition with improved blooming resistance comprises 100 parts by weight of a base rubber and 5 ~10 parts by weight of vegetable oil-based softeners modified with alkyl oxide-based light base. The alkyl oxidebased light base is one or more selected from the group consisting of CH2CO3, ethylene oxide, and alkylbenzoate. The vegetable oil-based softener is one or more selected from the group consisting of castor oil, linseed oil, pine tar, tall oil, and palm oil.
The article entitled “Pineapple leaf fibers and palf-reinforced polymer composites” by S. M. Sapuan; A. R Mohamed; Januar Parlaungan Siregar; Mohamad Ridzwan Ishak; Cellulose Fibers: Bio- and Nano-Polymer Composites (pp.325-343); 2011 talks about a survey of research works carried out on PALF and PALF -reinforced composites. It reviews PALF extraction, fiber characterization, and PALF applications, modification of PALF, and manufacture and properties of PALF -reinforced composites. With increasing importance of pineapple and pineapple plantation area, value-added applications of PALF as reinforcing fibers in polymer composites must be developed in order to increase “resource potential” of pineapple and consequently energize the utilization of PALF.
The article entitled “Development of green natural rubber composites : Effect of nitrile rubber, fiber surface treatment and carbon black on properties of pineapple leaf fiber reinforced natural rubber composites” by Nuttapong Hariwongsanupab; Universite De Haute Alsace, France & Mahidol University, Thailand; tel.archives-ouvertes; 16 March 2018 talks about the effects of nitrile rubber (NBR), fiber surface treatment and carbon black on properties of pineapple leaf fiber-reinforced natural rubber composites (NR/PALF). The incorporation of NBR and surface treatment of fiber were used to improve the mechanical properties of composites at low deformation, whereas carbon black was used to improve these properties at high deformation. The fiber content was fixed at 10 phr. The composites were prepared using two-roll mill and were cured using compression moulding with keeping the fiber orientation. These composites were characterized using moving die rheometer (MDR), dynamic mechanical thermal analysis (DMTA) and tensile testing. The morphology after cryogenic fracture was observed using scanning electron microscopy (SEM). The effect of NBR from 0 to 20 phr of total rubber content was investigated. NBR is proposed to encase PALF leading to higher stress transfer between matrix and PALF. The method of mixing was also studied. For the fiber surface treatment, propylsilane, allylsilane and silane-69 were treated on the alkali-treated fiber. Treated fibers were characterized using Fourier-Transform infrared spectroscopy (FTIR), x- ray photoelectron spectroscopy (XPS) and SEM. Silane-69 treatment of fiber increased the modulus at low deformation more than the incorporation of NBR of NR/PALF composites due to the chemical crosslinking between rubber and fiber from silane-treatment rather than the physical interaction of NR, NBR and fiber. However, reinforcement by fiber reduced the deformation at break. Hence, carbon black was also incorporated into NR/NBR/PALF and NR/surface-treated PALF composites to improve the ultimate properties. By incorporation of carbon black 30 phr in both composites, the mechanical properties of composites were improved and can be controlled at both low and high deformations.
Hence, there needed improved tread rubber composition for off highway tyres that can improve abrasion resistance by using it.
To overcome the above listed prior arts, the present invention aims to provide an environmentfriendly off highway tyre tread composition and its method of preparation. Also, to provide an off highway tire tread rubber composition with abrasion resistance and cut-and-chip performance.
OBJECT OF THE INVENTION
The principal object of the present invention is to provide environment friendly off-highway tyre tread composition and its method of preparation.
Another object of the present invention is to provide off highway tyre tread composition having improved abrasion resistance.
Yet another object of the present invention is to provide off highway tyre tread composition which provides better cut and chip resistance and high hardness.
Yet another object of the present invention is to provide off highway tyre tread rubber composition which provides better wet and dry grip.
SUMMARY OF THE INVENTION
One or more problems of the conventional prior arts may be overcome by various embodiments of the present invention.
It is a primary aspect of the present invention to provide a tyre tread rubber composition using natural fibers for off-highway tyres, comprising of:
Polymer matrix- 100 phr; reinforcing filler - 20-75 phr; natural fiber - 0.5-10 phr; wood rosin - 1-7 phr; activators - 1.5 - 10 phr; antiozonants / anti-degradants - 0-5 phr; vulcanization agent - 1.3 - 2.7 phr; primary accelerators - 1.2 - 3 phr; and process aid - 1-15 phr, wherein the natural fiber is selected from screw pine leaf fiber having the length of 1-5 mm.
It is another aspect of the present invention to provide a tyre tread rubber composition using natural fibers for off-highway tyres, wherein the polymer matrix comprises of rubbers selected from natural rubber (NR), Styrene butadiene rubber (SBR), PolyButadiene Rubber (PBR), and combinations thereof, preferably in a weight ratio of NR:SBR: PBR - 30-85:5-40:10-30 phr.
It is another aspect of the present invention to provide a tyre tread rubber composition using natural fibers for off-highway tyres, wherein the reinforcing filler is selected from carbon black, silica and combinations thereof, preferably carbon black - 20-60 phr and silica - 0-15 phr.
It is another aspect of the present invention to provide a tyre tread rubber composition using natural fibers for off highway tyres, wherein the activators are selected from zinc oxide, stearic acid and combinations thereof, preferably zinc oxide - 3-5 phr and stearic acid- 1.5 - 5 phr.
It is another aspect of the present invention to provide a tyre tread rubber composition using natural fibers for off highway tyres, wherein anti-degradants are selected from Microcrystalline wax (MC wax), N(l,3-dimethyl-butyl)-N’-phenylenediamine (6PPD) and combinations thereof, preferably MC wax- 0 - 2phr and 6PPD - 0-3 phr.
It is another aspect of the present invention to provide a tyre tread rubber composition using natural fibers for off highway tyres, wherein vulcanization agent is sulphur.
It is another aspect of the present invention to provide a tyre tread rubber composition using natural fibers for off highway tyres, wherein primary accelerators is selected from n- cyclohexyl-2-benzothiazole sulfonamide (CBS).
It is another aspect of the present invention to provide a tyre tread rubber composition using natural fibers for off highway tyres, wherein the process aid is selected from TDAE oil.
It is another aspect of the present invention to provide a method for preparation of a tyre tread rubber composition using natural fibers from screw pine leaf fiber for off highway tyres, comprising of steps: preparation of master batch in three stages:
First stage as mastication of rubber at a temperature of 70+5 degree Celsius; blending of natural fiber selected from screw pine leaf fiber having length of 1-5 mm in two roll mill; Second stage as loading first stage rubber compound in Banbury mixer and mixing for 0-35 seconds at a temperature 65-80°C; further add 75% carbon black, 100% silica, rubber chemicals MC wax, wood rosin, and TDAE oil for 90 to 230 seconds; sweeping down in the orifice and mixing for 80 to 102 seconds; further mixing is continued until dump temperature in the range between 130 and 160°C and sheet out; third stage as addition of 25% carbon black, zinc oxide, 6PPD, and mix for 60 - 180 seconds, and dump at a temperature range between
125 °C and 155 °C and sheet out; wherein the processing parameters include rotational speed of 55 to 60 rpm for master batch, preparation of final batch: mixing of master batch rubber compound and curatives for 60-90 seconds, dumped at temperature range between 95 °C and 115°C, and sheet out, wherein the rubbers are selected from natural rubber (NR), Styrene butadiene rubber (SBR), Poly Butadiene Rubber (PBR), and combinations thereof, preferably in a weight ratio of NR: SBR: PBR - 30-85:5-40:10-30 phr.
BRIEF DESCRIPTION OF DRAWINGS
Figure 1 represents the screw pine leaf fibre blend with polymers.
DETAILED DESCRIPTION OF THE INVENTION
At the outset of the description that follows, it is to be understood that the ensuing description only illustrates a particular form of this invention. However, such a particular form is only an exemplary embodiment and is not intended to be taken restrictively to imply any limitation on the scope of the present invention.
Source and geographical origin of biological material: Screw pine leaf fibre from Sree Ram Agencies Old No. 2, (New No. IB) Palmal Cross Street, Near Mahal South, Madurai, India.
The present invention relates to a high quality off highway tyre tread composition and its method of preparation. Screw pine leaf fibre is used in natural rubber and synthetic rubber triblend (NR:SBR: PBR) based rubber composition to provide off highway tyre tread composition. The present invention uses screw pine leaf fibre in off highway tyre tread rubber composition to provide better cut and chip resistance, abrasion resistance and higher hardness. An off highway tyre tread rubber composition comprises one or more rubbers ; reinforcing filler carbon black: 20 to 60 phr; silica: 0 to 15 phr; 0.5 to 10 phr of screw pine leaf fibre, presence of screw pine leaf fibre in rubber compound reduces the rubber chain mobility and it makes the rubber compound more rigid which turns into better reinforcement properties of rubber vulcanizate; wood rosin; activators; anti-degradants; vulcanization agent; primary accelerators; and process aid.
Table 1: Rubber Composition in Phr
Figure imgf000012_0001
Figure imgf000013_0001
1. Natural Rubber - RSS 3 (Natural Rubber - Ribbed Smoke Sheet) from Southland Global PTE Ltd, Thailand.
2. SBR 1739 - Styrene butadiene rubber oil extended with 37.5 % TDAE oil
3. Polybutadiene rubber - It is from Reliance Industries Ltd, India.
4. Carbon black - ASTM grade N234 is from ASTM Grade Aljubail Carbon, Saudi Arabia. It is the reinforcing filler ISAF, Intermediate Superior Abrasion Furnace having the Iodine adsorption No. 115 to 125 mg/gm, tinting strength value between 114 to 124 % ITRB, statistical thickness surface area value between 107 to 117 m2/gm
5. Precipitated Silica- Ultrasil VN3 silica from Insilico Ltd, Evonik Industries GmbH, India. It is the reinforcing filler having nitrogen surface area value 170 to 190 m2/gm.
6. Wood rosin -It is a tackifier resin from Kanchi Karpooram Ltd, Kanchipuram, India
7. Screw pine leaf fibre from Sree Ram Agencies Old No. 2, (New No. IB) Palmal Cross Street, Near Mahal South, Madurai, India.
8. Zinc Oxide from POCL Enterprises Limited, India. It is an activator added to the rubber compound to activate sulphur vulcanization
9. Stearic acid - from 3F Industries Ltd., India. It is used as a Process aid. Also, Zinc oxide and Stearic acid are added to form zinc soap, improves the solubility of zinc oxide in the compound, and with the accelerator to form a complex, this complex reacts with sulphur to produce a strong cure activating system.
10. MC Wax - Microcrystalline wax is used to provide a physical barrier on the surface of a tire. This physical barrier prevents attack on the rubber from ozone present in the atmosphere.
11. 6PPD - (N-(l,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine) is an antidegradant from Nocil Limited, India.
12. TDAE Oil- Treated Distillate Aromatic Extract Oil is a non-carcinogenic mineral oil. It is from Panama Petrochem Ltd, Gujarat, India.
13. CBS N-cyclohexyl-2-benzothiazolesulfenamide) from Nocil Limited, India. It is a delayed action accelerator suitable for diene rubbers.
14. Sulphur is the vulcanizing agent from The Standard Chemical Co. Pvt Ltd, India.
Rubber composition - Method of Preparation: A rubber composition prepared by a thermo mechanical process which comprises the sequential mixing steps, Thermomechanically mixing with the preparatory mixing step - master batch is as follows:
Step I: Mixing in Two roll mill
Rubber is masticated in a two-roll mill with the roll temp 70+/-5 deg C to form a band on roll and then the screw pine leaf fibre with the length of 1 to 5 mm is added into the masticated rubber to attain uniform orientation of screw pine leaf fibre in rubber blend.
Step II: Mixing in Banbury Mixer
Mixing has been done with the head temperature of the Banbury maintained between 65 to 80°C and the unloaded rotor speed maintained between 55 to 60 rpm. The mixing cycle is to be followed as: a) Mixing chamber has been charged with step I rubber compound (rubber + screw pine leaf fibre blend) and allowed to mix for 0 to 35 seconds b) and further, 75% of carbon black, 100% of silica, rubber chemicals MC wax, wood rosin, TDAE oil, and allowed to mix for 90 to 230 seconds, c) sweeping has been done in the orifice and allowed to mix for another 80 to 102 seconds, the compound has been dumped at the temperature in the range of 130°C to 165°C and sheeted out in the laboratory two roll mill.
Step III: Add the step II master batch in the Lab Banbury Mixer and add remaining 25% of carbon black, Zinc oxide, 6PPD and mix it for 60 seconds to 180 seconds and the compound has been dumped at the temperature in the range of 125 °C to 155 °C and sheeted out in the laboratory two roll mill.
Thermomechanical mixing in at least one preparatory mixing step - final batch is as follows: Mixing chamber charged with the master batch rubber compound and the curatives, and allowed to mix for 60 to 90 seconds and the compound has been dumped at the temperature in the range of upto the temperature 95 °C to 115°C. The final batch sheet out has been done in the laboratory two roll mill.
Results:
Table 2: Characterization of Cured Rubber Vulcanizate and Uncured Rubber Compound:
Figure imgf000015_0001
Table: 3 Characterization of Cured Rubber Vulcanizate and Uncured Rubber Compound
Figure imgf000015_0002
Results
Measurements and tests (Table 2):
The purpose of these tests is to measure the improved properties of the tyre tread rubber composition related to the invention against control tread rubber composition. For this, rubber composition Fl is prepared based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre against rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers is prepared and evaluated.
Similarly, rubber composition F2 is prepared based on NR: SBR 1739: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black is replaced with 5 phr of screw pine leaf fibre against rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers is prepared and evaluated.
The present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre hardness value is 70 Shore A.
Also, the present invention provides a 100 parts by weight of rubber composition F2, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black is replaced with 5 phr of screw pine leaf fibre provides hardness value is 66 Shore A (Note: Silica filler in not used).
The present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides scorch time ts value is 26.42 minutes (Ideal value of scorch time is 15 minutes).
Also, present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides scorch time ts value is 29.30minutes (Ideal value of scorch time is 15 minutes). The present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides abrasion loss value lowered by 9.61% (i.e., better abrasion resistance) when compared to rubber composition Cl based on NR:SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
Similarly, the present invention provides a 100 parts by weight of rubber composition F2, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black is replaced with 5 phr of screw pine leaf fibre provides abrasion loss value lowered by 7.45% (i.e., better abrasion resistance) when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
The present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR 1739: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides weight loss and diameter loss value lowered by 1.60% and 28.72% respectively (i.e., better cut and chip resistance) when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
Similarly, the present invention provides a 100 parts by weight of rubber composition F2, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black is replaced with 5 phr of screw pine leaf fibre provides weight loss and diameter value lowered by 28.72 % and 36.84 % respectively (i.e., better cut and chip resistance) when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
Results:
Measurements and Tests (Table 3)
The present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR 1739: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides tan delta value at 0 deg C is improved by 11.26% when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers. Also, the present invention provides a 100 parts by weight of rubber composition Fl, NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers containing 5 phr of screw pine leaf fibre provides tan delta value at 25 deg C is improved by 6.48 % when compared to rubber composition Cl based on NR: SBR: PBR (40 phr :30 phr: 30 phr) triblend rubber composition reinforced by carbon black and silica fillers.
Overall, the present invention provides a 100 parts by weight of rubber composition, NR: SBR: PBR (40 phr: 30 phr: 30 phr) triblend based rubber composition reinforced by carbon black containing 5 phr of pineapple leaf fibre provides better abrasion resistance (wear resistance) and cut and chip resistance along with better process safety. The present invention provides a 100 parts by weight of rubber composition, NR: SBR: PBR (40 phr: 30 phr: 30 phr) triblend based rubber composition reinforced by carbon black and silica filler containing 5 phr of screw pine leaf fibre provides better wet grip and dry grip property.
Characterization of Rubber Vulcanizate:
The resulting vulcanized rubber compositions shall be evaluated for
Measurements and Tests:
Better processability (Process Requirements) of a Rubber Compound:
Mooney Scorch time at 125 deg C, t5 value is measured in accordance with ASTM D1646 in Mooney Viscometer MV2000, Alpha technologies, USA.
M2. Shore A Hardness of the Rubber Vulcanizate:
Shore A Hardness of the Rubber Vulcanizate is assessed in accordance with ASTM D 2240. M3: Abrasion loss in mm3 is measured using Din Abrader in accordance with ASTM D 5963. M4: Cut and chip resistance of the rubber vulcanizate is measured to understand the relative service life of the off highway tyre subjected to uneven terrains (i.e., to predict service performance of the tyre tread that are subjected to contacting surfaces containing sharp objects such as rocks, gravels etc.,) using Goodrich Cut and Chip Tester. Cutting takes place when the tyre tread hits a sharp object with the sufficient force that the surface is cut, creating a new surface area. Chipping follows cutting and involves fracturing away of a piece of rubber from the surface. Test specimen Speed: 760 rpm; Cut chip cycle-Frequency: 60HZ; Test cycle - 10 Minutes. Weight loss and diameter reduction are measured after 10 minutes of test time.
M5. Dynamic properties/Visco elastic properties of the Rubber vulcanizate: The dynamic properties of the rubber vulcanizate are measured on a dynamic mechanical analyzer (DMA Metravib +1000) in tension mode with the temperature sweep -40 to 100 °C, Dynamic strain: 0.3%, Static strain:0.6%, Frequency: 10 Hz.
Tan delta at 0°C is a predictor for wet grip (Higher tan delta value at 0 °C is good for wet grip property) and tan delta at 25 °C is a predictor for dry grip (Higher tan delta value at 25 °C is good for dry grip property).

Claims

WE CLAIM:
1. A tyre tread rubber composition using natural fibers for off-highway tyres, comprising of:
Polymer matrix- 100 phr; reinforcing filler - 20-75 phr; natural fiber - 0.5-10 phr; wood rosin - 1-7 phr; activators - 1.5 - 10 phr; antiozonants / anti-degradants - 0-5 phr; vulcanization agent - 1.3 - 2.7 phr; primary accelerators - 1.2 - 3 phr; and process aid - 1-15 phr, wherein the natural fiber is selected from screw pine leaf fiber having the length of 1-5 mm.
2. The tyre tread rubber composition using natural fibers for off-highway tyres as claimed in claim 1, wherein the polymer matrix comprises of rubbers selected from natural rubber (NR), Styrene butadiene rubber (SBR), PolyButadiene Rubber (PBR), and combinations thereof, preferably in a weight ratio of NR:SBR: PBR - 30-85:5-40:10-30 phr.
3. The tyre tread rubber composition using natural fibers for off-highway tyres as claimed in claim 1, wherein the reinforcing filler is selected from carbon black, silica and combinations thereof, preferably carbon black - 20-60 phr and silica - 0-15 phr.
4. The tyre tread rubber composition using natural fibers for off-highway tyres as claimed in claim 1, wherein the activators are selected from zinc oxide, stearic acid and combinations thereof, preferably zinc oxide - 3-5 phr and stearic acid- 1.5 - 5 phr.
5. The tyre tread rubber composition using natural fibers for off-highway tyres as claimed in claim 1, wherein anti-degradants are selected from Microcrystalline wax (MC wax), N(l,3- dimethyl-butyl)-N’ -phenylenediamine (6PPD) and combinations thereof, preferably MC wax- 0 - 2phr and 6PPD - 0-3 phr.
6. The tyre tread rubber composition using natural fibers for off-highway tyres as claimed in claim 1, wherein vulcanization agent is sulphur.
7. The tyre tread rubber composition using natural fibers for off-highway tyres as claimed in claim 1, wherein primary accelerators is selected from n-cyclohexyl-2-benzothiazole sulfonamide (CBS).
8. The tyre tread rubber composition using natural fibers for off-highway tyres as claimed in claim 1, wherein the process aid is selected from TDAE oil.
9. A method for preparation of a tyre tread rubber composition using natural fibers from screw pine leaf fiber for off highway tyres, comprising of steps: preparation of master batch in three stages:
First stage as mastication of rubber at a temperature of 70+5 degree Celsius; blending of natural fiber selected from screw pine leaf fiber having length of 1-5 mm in two roll mill;
Second stage as loading first stage rubber compound in Banbury mixer and mixing for 0-35 seconds at a temperature 65-80°C; further add 75% carbon black, 100% silica, rubber chemicals MC wax, wood rosin, and TDAE oil for 90 to 230 seconds; sweeping down in the orifice and mixing for 80 to 102 seconds; further mixing is continued until dump temperature in the range between 130 and 160°C and sheet out; third stage as addition of 25% carbon black, zinc oxide, 6PPD, and mix for 60
- 180 seconds, and dump at a temperature range between
125 °C and 155 °C and sheet out; wherein the processing parameters include rotational speed of 55 to 60 rpm for master batch, preparation of final batch: mixing of master batch rubber compound and curatives for 60-90 seconds, dumped at temperature range between 95 °C and 115°C, and sheet out, wherein the rubbers are selected from natural rubber (NR), Styrene butadiene rubber (SBR), PolyButadiene Rubber (PBR), and combinations thereof, preferably in a weight ratio of NR:SBR:PBR - 30-85:5-40:10-30 phr.
PCT/IN2023/095001 2022-02-09 2023-02-07 A rubber composition using natural fibers for tyre tread and method thereof WO2023152774A1 (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0527396A1 (en) * 1991-08-02 1993-02-17 Pirelli Armstrong Tire Corporation Tire tread rubber composition
WO2016104815A1 (en) * 2014-12-26 2016-06-30 Compagnie Generale Des Etablissements Michelin A tire having a tread comprising rubber composition comprising short fibers
EP3795374A1 (en) * 2019-09-20 2021-03-24 Kraton Polymers Research B.V. Tire composition and method for making thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0527396A1 (en) * 1991-08-02 1993-02-17 Pirelli Armstrong Tire Corporation Tire tread rubber composition
WO2016104815A1 (en) * 2014-12-26 2016-06-30 Compagnie Generale Des Etablissements Michelin A tire having a tread comprising rubber composition comprising short fibers
EP3795374A1 (en) * 2019-09-20 2021-03-24 Kraton Polymers Research B.V. Tire composition and method for making thereof

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