WO2022029791A1 - Rubber composition for motor cycle tyre treads using moringa oleifera oil and method thereof - Google Patents

Rubber composition for motor cycle tyre treads using moringa oleifera oil and method thereof Download PDF

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Publication number
WO2022029791A1
WO2022029791A1 PCT/IN2021/050435 IN2021050435W WO2022029791A1 WO 2022029791 A1 WO2022029791 A1 WO 2022029791A1 IN 2021050435 W IN2021050435 W IN 2021050435W WO 2022029791 A1 WO2022029791 A1 WO 2022029791A1
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Prior art keywords
rubber
rubber composition
phr
oil
moringa oleifera
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PCT/IN2021/050435
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French (fr)
Inventor
Brindha Senthilraja
Sankaran Kumar
Kadambanathan THIAGARAJAN
Viswanathan Sivaramakrishnan
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Tvs Srichakra Ltd
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Publication of WO2022029791A1 publication Critical patent/WO2022029791A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
    • B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
    • B60C1/0016—Compositions of the tread
    • 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 

Definitions

  • the present invention relates to the field of rubber, rubber processing and rubber compounding. More particularly, the present invention relates to a rubber composition for motor cycle tyre treads using naturally occurring Moringa oleifera oil for better winter traction along with dry traction and lower rolling resistance property.
  • a tyre tread has to meet, in a known way, a large number of often conflicting technical requirements, including a low rolling resistance, a high wear resistance, a high dry grip and a high wet grip.
  • wet grip ability is now improving, although this approach improves the tire's wet traction capabilities, but the wear performance of the tire but also therefore reduced tire life accordingly reduced.
  • Tires are generally designed to provide high speed performance. Achievement of good winter performance is obtained at the cost of a reduction of handling; good dry traction of a tire can only be obtained by a reduction of winter performance.
  • Aromatic oil is added into the rubber composition for improving the processing characteristics and grip properties of the rubber vulcanizate.
  • Conventional oil processing aids have been used in many tire components: tread compounds often contain polybutadiene rubber (“BR”), oil-extended polybutadiene rubber (“OE- BR”), styrene -butadiene rubber (“SBR”), oil-extended styrenebutadiene rubber (“OE-SBR”), isoprene-butadiene rubber (“IBR”), and styrene-isoprene -butadiene rubber (“SIBR”); sidewall and ply coats can contain butyl rubber and SBR and may use free aromatic oils as processing aids; internal components, such as the steel belt skim coat, gum strips, cushions, barriers, bases, and wedges, contain predominantly natural rubber and aromatic oils.
  • any alternative to conventional processing oils such as naphthenic, paraffinic, and aromatic oils must be compatible with the rubbers, not interfere with cure, be easily dispersed in all tire compounds, be cost effective, and not adversely impact tire performance.
  • CN108948444 A discloses a multifunctional foamed insole which is prepared from the following raw materials in parts by weight: 100 parts of natural rubber, 15-17 parts of terpene resin, 15-17 parts of jute fibers, 10-12 parts of shell powder, 13-15 parts of talc powder, 19-22 parts of jade powder, 8-10 parts of palygorskite, 7-9 parts of radiobarite powder, 6-8 parts of cortex moriradicis, 3-5 parts of moringa tree roots, 14-16 parts of diatomite, 7-8 parts of a coupling agent, 3-4 parts of azodicarbonamide, 3-5 parts of nano zinc oxide, 1-2 parts of stearic acid, 2-2.5 parts of sulfur, 1- 1.5part of an accelerant and 1.5-2 parts of an antiageing agent.
  • CN104817740A discloses a high-wet-grip tire rubber composition which comprises environmentfriendly emulsion-polymerized oil-extended styrene -butadiene rubber SBR 1723, novel solution- polymerized oil-extended styrene-butadiene rubber TUFDENE F3440, medium super abrasion furnace black N-220, processing oil V-500, a novel modified petroleum resin OPPERA PR373, an anti-aging agent 6PPD, an anti-aging agent 3100, microcrystalline wax, an activator zinc oxide, an activator industrial stearic acid, sulfur, an accelerator CZ, an accelerator TT and an anti-scorching agent PVI.
  • US20140235751 discloses a tire having an improved wet grip, in particular for a passenger vehicle, a van, or a two-wheel vehicle, includes a tread formed of a rubber composition.
  • the rubber composition includes at least (phr meaning parts by weight per hundred parts of elastomer): as a first diene elastomer, from 55 to 95 phr of natural rubber or synthetic polyisoprene; as a second diene elastomer, from 5 to 45 phr of a polybutadiene or butadiene copolymer having a glass transition temperature (Tg) which is greater than -70° C.; as a reinforcing filler, more than 90 phr and less than 150 phr of an inorganic filler; and as a plasticizer, more than 10 phr of a thermoplastic hydrocarbon resin exhibiting a glass transition temperature (Tg) greater than 20° C.
  • EP0940462 discloses high aromatic oil characterized by that a glass transition point is -45 to - 20 DEG C and an aromatic component measured by Clay-Gel method accounts for 55 to 90 % by weight and that a polycyclic aromatic compound measured by IP 346 method accounts for less than 3 % by weight based on the whole components of hydrocarbons contained in the oil.
  • This high aromatic oil can suitably be used for various rubber compositions such as tires, rubber vibration insulators and fenders, oil extended synthetic rubbers, printing inks and writing inks.
  • CN104059329A discloses a rubber characterized by including the following substances by weight: 14-20 parts of furfuryl alcohol resin, 21-30 parts of urea formaldehyde resin, 26-29 parts of polytetrafluoroethylene gum, 4-8 parts of silicon carbide, 9-14 parts of a formaldehyde solution, 16- 17 parts of glacial acetic acid, 3-9 parts of resorcinol, 1-4 parts of paraformaldehyde, 1-9 parts of precipitated barium sulfate, 2-8 parts of Hoveniaacerba sawdust, 3-7 parts of camellia oleifera sawdust, 4-8 parts of Eucalyptus globules sawdust, 1-2 parts of anatase titanium dioxide, 0.5-1 part of nano-organic montmorillonite, and 3-4 parts of talcum powder.
  • EP2143755 Al discloses methods for making shapeable composite materials or shaped articles from recycled materials comprising forming a crumb slurry by, in any order, increasing the particle size of a composition comprising white water waste from one or more emulsion or dispersion polymer and combining the white water waste polymer with one or more waste thermoset material, preferably, ground tire rubber (GTR), and, then processing the combined material wet or dry as a thermoplastic to form the composite material or article.
  • Useful coagulating agents include any known coagulation agents such as, for example, any chosen from a salt, such as sodium chloride or iron (ferric) chloride, i.e. FeC13, , iron (ferrous) sulfate, i.e.
  • Other chemical coagulants may include alumina, aluminium chlorohydrate, calcium oxide, polyacrylamide, sodium aluminate, and sodium silicate, and the like; and natural product coagulants may include chitosan, moringa oleifera seeds, papain, strychnos seeds, and is in glass, among others.
  • US2017273313A1 relates to compositions comprising a vehicle such as a polymer base, moringa oil and neem oil.
  • the combination of the two oils is in an amount sufficient to prevent the establishment or proliferation of a microorganism, such as a mildew, on the surface of an inanimate object.
  • the moringa oil and neem oil combination can be advantageously admixed with a paint base, a solvent system, or other vehicle base for the treatment of wood, dry wall, or other porous or non- porous surface that is susceptible to a biological infestation.
  • US2010167013A1 discloses thermoplastic roofing membranes comprising particles of cross linked rubber and an aqueous (co)polymer dispersion.
  • thermoplastic roofing membranes are formed by combining particles of cross linked rubber and a suspension polymer dispersion, or a coagulated aqueous latex (co)polymer dispersion, to form a mixture in aqueous dispersion, which aqueous dispersion mixture is subjected to solid state shear pulverization to form materials that can be processed as thermoplastics at cross linked rubber concentrations of from 10 wt. % to as high as 95 wt. %, based on the total solids of the material.
  • the method may further comprise kneading the pulverized product, followed by extrusion to form roofing membranes.
  • Suitable methods of coagulation may include the addition of an acid, such as formic acid or sulfuric acid, or a salt, such as sodium chloride or iron (ferric) chloride.
  • Other chemical coagulants may include alum, alumina, aluminiumchlorohydrate, aluminium sulfate, calcium oxide, iron (ferrous) sulfate, magnesium sulfate, polyacrylamide, sodium aluminate, and sodium silicate, and the like; and natural product coagulants may include chitosan, Moringa oleifera seeds, papain, strychnos seeds, and isinglass, among others.
  • AU2009202787A1 relates to methods of making shapeable composites in the form of finely divided materials or articles and the materials and articles produced by the methods, the methods comprising forming mixtures by (i) treating an aqueous thermoplastic acrylic or vinyl polymer to increase the particle size thereof to a weight average particle size of 1 pm or more, and, optionally, dewatering to form a crumb mixture; and (ii) combining a thermoplastic acrylic or vinyl polymer with one or more waste rubber vulcanizate having a sieve particle size ranging from 10 to 600 pm in the amount of from 15 to 95 wt.%, based on the total weight of polymer and rubber to form a crumb slurry, such that (ii) can take place before, during, after (i) but before any dewatering, or after any dewatering; and (iii) thermoplastic processing the mixture.
  • Useful coagulating agents include any known coagulation agents such as, for example, any chosen from a salt, such as sodium chloride or iron (ferric) chloride, i.e. FeC13, iron (ferrous) sulfate, i.e. Fe2(SO4)-, alum, i.e. A12(SO4)3, magnesium sulfate, or preferably FeC13; an acid, such as a carboxylic acid, e.g. formic acid, or sulfuric acid to reduce the pH of the acrylic or vinyl polymer to 4.5 or less, preferably 4.0 or less; a chemical coagulant and mixtures thereof.
  • a salt such as sodium chloride or iron (ferric) chloride, i.e. FeC13, iron (ferrous) sulfate, i.e. Fe2(SO4)-, alum, i.e. A12(SO4)3, magnesium sulfate, or preferably FeC13
  • an acid such as a carboxylic acid,
  • US2010016456A1 relates to methods of making composite materials comprising combining particles of crosslinked rubber with coagulated aqueous polymer dispersions to form a mixture in aqueous dispersion, and subjecting the aqueous dispersion mixture to solid state shear pulverization to form materials that can be processed as thermoplastics at crosslinked rubber concentrations of from 10 to as high as 95 wt.
  • the method may further comprise kneading the pulverized product to form useful articles, such as roofing membranes and shoe soles.
  • Suitable methods of coagulation may include the addition of an acid, such as formic acid or sulfuric acid, or a salt, such as sodium chloride or iron (ferric) chloride.
  • Other chemical coagulants may include alum, alumina, aluminiumchlorohydrate, aluminium sulfate, calcium oxide, iron (ferrous) sulfate, magnesium sulfate, polyacrylamide, sodium aluminate, and sodium silicate, and the like; and natural product coagulants may include chitosan, moringa oleifera seeds, papain, strychnos seeds, and isinglass, among others.
  • results showed that both moringa components improved thermal properties and reduced the crystalline phase of the mixture.
  • the addition of PMO had improved the biodegradation capacity up to five times while MO had improved it up to three times.
  • the results showed the greatest influence of moringa components on biodegradation of mixtures with cited polymers [Cristiane Medina Finzi-Quintao, KatiaMonteiro Novack, Ana Claudia Bernardes-Silva, Thais Dhayane Silva, Lucas Emiliano Souza Moreira, LuizaEduardaMoraes Braga; Polimeros vol.28 no.4 Sao Carlos, Aug./Sept. 2018].
  • said anti-degradants comprises of N-(l,3-Dimethylbutyl)-N’-phenyl-phenylenediamine 7-(6PPD), 2,2,4-trimethyl- 1 ,2-dihydroquinoline (TDQ).
  • the primary accelerator is selected from N-cyclohexyl-2-benzthiazolesulfenamide and guanidines, thiazoles, sulphenamides and thiuram sulphides or its mixtures.
  • Step I mixing of rubber component and adding 80 - 90% of the reinforcing filler; adding 80 - 90 % of inorganic reinforcing filler silica and silane coupling agent; mixing the added ingredients for silanisation at around 105 to 125 °C at 20 to 30 rpm; addition of remaining reinforcing fillers, rubber chemicals except N-(1,3-Dimethylbutyl)-N’- phenyl -phenylenediamine and zinc oxide and Moringa oleiferaoil; sweeping down in the orifice and allowing to mix for time period of 50 - 60 seconds; dumping the compound at temperature range between 135 and 160 °C; sheeting out the rubber compound to yield master batch.
  • Step I master batch Mixing of activators and anti -degrandants with Step I master batch at a temperature range between 135 °C and 150°C; sheeting out the rubber compound;
  • Step III mixing of Step II master batch; dump at a temperature range between 135°C and 150 °C; sheeting out the rubber compound; final batch preparation by:
  • step III master batch compounds with curatives
  • Figure 1 represents the ATR FTIR spectra of Moringa oleifera oil.
  • the present invention relates to the field of rubber processing for tyres.
  • the present invention relates to rubber composition for motor cycle tyre treads using naturally occurring Moringa oleifera oil.
  • the present invention also provides a tyre produced using this rubber composition, capable of providing better winter traction along with dry traction and lower rolling resistance property.
  • the rubber composition of tyre tread includes 100 parts by weight of a rubber, preferably with the blend of natural rubber, styrene butadiene rubber and butadiene rubber, preferably natural rubbers 20 - 55 phr, non- oil extended styrene butadiene rubber 20 - 75 phr and poly butadiene rubber 10 - 35 phr, 30 to 80 parts of the reinforcing filler such as carbon black, preferably with carbon black with the iodine surface area of 114 to 126 mg/gm at a concentration of 25-55 phr, and preferably silica 5-30 phr, along with the use of 2 to 20 parts of a naturally occurring Moringa oleifera oil with high oleic acid 60-80gm/100gm and also with the flash point greater than 260°C which is higher than aromatic oil and TDAE oil.
  • the invention also relates to the better processing properties of the rubber compound.
  • rubber composition for motor cycle tyre tread consists of the rubbers selected from one or more of natural rubber, non-oil extended styrene butadiene rubber and poly-butadiene rubber, preferably in a weight ratio for combination of rubbers are natural rubber 20 - 55 parts, Non-oil extended styrene butadiene rubber 20 - 75 parts, and poly-butadiene rubber 10 - 35 parts and 2 to 20 parts of a naturally occurring Moringa oleifera oil.
  • the rubber composition also consists of reinforcing fillers - 20 - 80 phr; coupling agent - 2 - 8.50 phr; activators - 2 - 10 phr; anti-degrandants - 0.5 - 6phr; primary accelerators - 1- 3 phr; and vulcanization agent - 1- 3.0 phr.
  • An embodiment of the present invention discloses the method of preparation of a rubber composition comprising of naturally occurring Moringa oleifera oil.
  • a rubber composition prepared by a thermomechanical process is as follows: For exemplification, a particular batch of the rubber composition is prepared in Banbury mixer.
  • Step I Preparation of masterbatch has been performed with the rotation speed of the mixer between 55 to 65 rpm and with the head temperature of the banbury maintained between 55 to 65° C.
  • Mixing chamber has been charged with the selected rubbers, and allowed to mix for 0 to 30 seconds
  • the remaining carbon black and silica, along with Moringa oleifera oil or aromatic oil, rubber chemicals except 6PPD and zinc oxide are added, and allowed to mix for 50 to 60 seconds e) sweeping done in the orifice and allowed to mix for 50 to 60 seconds and the compound has been dumped at the temperature in the range of 135 °C to 160 °C.
  • Step II Mixing chamber of banbury charged with the Step I master batch, chemicals zinc oxide and 6PPD, and allowed to mix for 120 seconds and dumped in the temperature range of 135°C to 150°C.
  • the rubber compound has been sheeted out in the laboratory two-roll mill.
  • Step III Mixing chamber of banbury charged with the Step II master batch, and allowed to mix for 120 seconds and dumped at the temperature range of 135°C to 150°C.
  • the rubber compound has been sheeted out in the laboratory two-roll mill.
  • Preparation of Final Batch Mixing chamber charged with the Step III master batch and the curatives, and allowed to mix for 50 to 80 seconds and dumped at the temperature range of 85 °C to 120°C.
  • Final batch sheet out of the rubber compound has been done in the laboratory two roll mill.
  • the present invention related to the rubber composition for motor cycle tyre treads using naturally occurring Moringa oleifera oil and to rubber compositions according to Table 1 manufacture thereof.
  • the rubber composition according to the invention comprises of: a.
  • the Moringa oleifera oil 10 used in the NR: SBR: BR blend (25:65:10) based rubber composition is to provide better winter traction along with dry traction and lower rolling resistance of a motor cycle tyre tread have the essential characteristics i) the iodine value lesser than 70 ii) viscosity using U tube viscometer C is greater than 85 cSt iii) Flashpoint greater than 260°C, and iv) density @ 20°C is 0.8956 gm/ml.
  • the most common fatty acids present in the Moringa oleifera oil are palmitic acid (C16:0), palmitoleic acid - C16:l, stearic acid (C18:0) - 5.99%, oleic acid (C18: l) - 68.36%, linoleic acid (C18:2) - 1.36%, arachidic acid (C20:0) - 3.66%, gadoleic acid -2.10% and behenic acid (C22:0) - 6.0%.
  • the Moringa oleifera oil identified the spectrum 3476.98 cm’ 1 which refers to hydroxyl groups formed by triglyceride hydrolysis.
  • Polycyclic aromatic hydrocarbons PAH
  • Benz(a)anthracene is less than 0.5pg/kg
  • Benzo(a)pyrene is less than 0.5pg/kg
  • Benzo(b)fluoranthene is less than 0.5pg/kg
  • the Figure 1. represents the Attenuated total reflectance - Fourier transform infrared (ATR- FTIR) spectra of Moringa oleifera Oil.
  • Aromatic oil 9 , Elasto 710 grade is used in the compound is to compare with the Moringa oleifera oil used in the present invention to provide better winter traction along with dry traction and lower rolling resistance property.
  • the other ingredients selected for the present invention is based on the conventional motor y cycle tyre tread composition activator zinc oxide and stearic acid, antidegradant 6PPD , TDQ 8 g.
  • the vulcanization system used in the present invention is based on sulphur and on a primary accelerator CBS 11 .
  • 6- Si75 is a bifunctional, sulfur-containing organosilane from Evonik Resource efficiency GmbH, Germany.
  • Mooney Scorch Characteristics pre-vulcanization characteristics using large rotor for processability: The Mooney Scorch measurements are carried out with a Mooney Viscometer (MV 2000 Alpha technologies, USA) according to ASTM DI 646. MV indicates the minimum viscosity, ts indicates the time to scorch (MV+5) which indicates the processing properties (process safety) and t35 indicates the time to cure (MV+35).
  • t5 scorch time (ts) - the time interval (measured from rotor start) corresponding to a viscosity increase of 5 Mooney units over MV, measured at rotor start.
  • the t5 value indicates the prevulcanization tendency of the compound.
  • Shore A Hardness of the Rubber Vulcanizate is assessed in accordance with ASTM D 2240. Shore Hardness is a measure of the resistance a material has to indentation. The test carried out for rubber vulcanizate using Shore A Durometer instrument. The Hardness unit for rubber materials is Shore A.
  • the dynamic properties of the rubber vulcanizate are measured in accordance with ASTM D5992 on a dynamic mechanical analyzer (DMA Metravib +1000) with a dynamic strain 0.1%, temperature sweep from -120 to +100°C, frequency: 20Hz in tension mode.
  • a. Storage Modulus E’ at a temperature in the region of -20°C in tension mode is used as a predictor for winter traction. Lower the E’ Storage modulus value at -20°C, better the winter traction.
  • Loss compliance J” @ 30°C is commonly used as a predictor for dry traction. Higher the J” value is better the dry traction.
  • Tan delta at 60°C is used as a predictor for Lower Rolling Resistance. Lower the tan delta value at 60° C is lower the rolling resistance.
  • compositions related to invention F3 against the control composition Fl, F2.
  • Three compositions Fl, F2, F3 were prepared based on NR: SBR: BR blend (25:65: 10) blend reinforced by carbon black and silica containing Moringa oleifera Oil (F3) against NR: SBR: BR blend (25:65:10) blend reinforced by carbon black and silica without oil (Fl) and containing 10 phr aromatic oil (F2) are prepared and evaluated.
  • the present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65:10) blend based rubber composition containing 10 phr Moringa oleifera oil gave mooney viscosity value lowered by 31.38% when compared to NR: SBR: BR blend (25:65:10) based rubber composition without oil, Fl (Control) whereas NR: SBR: BR blend (25:65: 10) based rubber composition containing 10 phr aromatic oil, F2 gave mooney viscosity value lowered by 24.95%.
  • Mooney Scorch test performed at 125 °C. In general the t5 value @ 125 °C for tread compounds ideally should be greater than 15 minutes.
  • the Moringa olifera oil added tread composition F3 gave process safety.
  • the present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65:10) blend based rubber composition containing 10 phr Moringa oleifera oil gave Shore A hardness value lowered by 9.09 % when compared to NR: SBR: BR blend (25:65: 10) based rubber composition without oil Fl (Control) whereas NR: SBR: BR blend (25:65:10) based rubber composition containing 10 phr aromatic oil F2 gave Shore A hardness value lowered by 6.06%.
  • the present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65: 10) blend based rubber composition containing 10 phr Moringa oleifera oil containing rubber composition, F3 gave lower hardness and lower mooney viscosity which indicates Moringa oleifera oil is having better compatibility with the polymer blend used in the present invention when compared to aromatic oil containing rubber composition, F2.
  • the present invention provides a 100 parts by weight of rubber composition, NR: SBR: BR blend (25:65: 10) blend based rubber composition containing 10 phr. Moringa oleifera oil gave process safety, 15 ⁇ 35 value improved by 21.70% & 18.98% respectively when compared to NR: SBR: BR blend (25:65: 10) based rubber composition containing no oil, Fl (Control).
  • the present invention relates to a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65: 10) blend based rubber composition containing 10 phr of Moringa oleifera oil gave 31.70% lowered E’ Storage modulus value @ -20°C i.e., better winter traction along with 38.60% improved dry traction when compared to when compared to NR: SBR: BR blend (25:65:10) based rubber composition containing no oil, Fl (Control) whereas NR: SBR: BR blend (25:65: 10) based rubber composition containing 10 phr aromatic oil, F2 gave 10.61 % lowered E’ Storage modulus value @ -20°C along with 33.30 % improved dry traction when compared to NR: SBR: BR blend (25:65: 10) based rubber composition containing no oil, Fl (Control).
  • the present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65:10) blend based rubber composition containing 10 phrMoringa oleifera oil, F3 gave 23.60% lowered E’ storage modulus value @ -20°C i.e., better winter traction along with 3.80 % improved dry traction when compared to NR: SBR: BR blend (25:65: 10) based rubber composition containing 10 phr aromatic oil, F2.
  • the present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65:10) blend based rubber composition containing 10 phrMoringa oleifera oil, F3 gave

Abstract

The present invention relates to the field of rubber, rubber processing and rubber compounding. Particularly, the present invention relates to a rubber composition for motor cycle tyre treads using naturally occurring Moringa oleifera oil. The composition comprises of reinforcing fillers, comprising of carbon black, silica, coupling agents, activators, anti-degradants, vulcanizing agents, primary accelerators and naturally occurring Moringa olifera oil that eliminates the use of aromatic oil and provides better winter traction along with dry traction and lower rolling resistance property.

Description

RUBBER COMPOSITION FOR MOTOR CYCLE TYRE TREADS USING MORINGA
OLEIFERA OIL AND METHOD THEREOF
FIELD OF THE INVENTION
The present invention relates to the field of rubber, rubber processing and rubber compounding. More particularly, the present invention relates to a rubber composition for motor cycle tyre treads using naturally occurring Moringa oleifera oil for better winter traction along with dry traction and lower rolling resistance property.
BACKGROUND OF THE INVENTION
A tyre tread has to meet, in a known way, a large number of often conflicting technical requirements, including a low rolling resistance, a high wear resistance, a high dry grip and a high wet grip. By adding reinforcing filler silica in rubber composition, wet grip ability is now improving, although this approach improves the tire's wet traction capabilities, but the wear performance of the tire but also therefore reduced tire life accordingly reduced. Tires are generally designed to provide high speed performance. Achievement of good winter performance is obtained at the cost of a reduction of handling; good dry traction of a tire can only be obtained by a reduction of winter performance.
Aromatic oil is added into the rubber composition for improving the processing characteristics and grip properties of the rubber vulcanizate. Conventional oil processing aids have been used in many tire components: tread compounds often contain polybutadiene rubber ("BR"), oil-extended polybutadiene rubber ("OE- BR"), styrene -butadiene rubber ("SBR"), oil-extended styrenebutadiene rubber ("OE-SBR"), isoprene-butadiene rubber ("IBR"), and styrene-isoprene -butadiene rubber ("SIBR"); sidewall and ply coats can contain butyl rubber and SBR and may use free aromatic oils as processing aids; internal components, such as the steel belt skim coat, gum strips, cushions, barriers, bases, and wedges, contain predominantly natural rubber and aromatic oils. Generally, the raw ingredients and materials used in tire compounding impact all tire performance variables, thus, any alternative to conventional processing oils, such as naphthenic, paraffinic, and aromatic oils must be compatible with the rubbers, not interfere with cure, be easily dispersed in all tire compounds, be cost effective, and not adversely impact tire performance. CN108948444 A discloses a multifunctional foamed insole which is prepared from the following raw materials in parts by weight: 100 parts of natural rubber, 15-17 parts of terpene resin, 15-17 parts of jute fibers, 10-12 parts of shell powder, 13-15 parts of talc powder, 19-22 parts of jade powder, 8-10 parts of palygorskite, 7-9 parts of radiobarite powder, 6-8 parts of cortex moriradicis, 3-5 parts of moringa tree roots, 14-16 parts of diatomite, 7-8 parts of a coupling agent, 3-4 parts of azodicarbonamide, 3-5 parts of nano zinc oxide, 1-2 parts of stearic acid, 2-2.5 parts of sulfur, 1- 1.5part of an accelerant and 1.5-2 parts of an antiageing agent.
CN104817740A discloses a high-wet-grip tire rubber composition which comprises environmentfriendly emulsion-polymerized oil-extended styrene -butadiene rubber SBR 1723, novel solution- polymerized oil-extended styrene-butadiene rubber TUFDENE F3440, medium super abrasion furnace black N-220, processing oil V-500, a novel modified petroleum resin OPPERA PR373, an anti-aging agent 6PPD, an anti-aging agent 3100, microcrystalline wax, an activator zinc oxide, an activator industrial stearic acid, sulfur, an accelerator CZ, an accelerator TT and an anti-scorching agent PVI.
US20140235751 discloses a tire having an improved wet grip, in particular for a passenger vehicle, a van, or a two-wheel vehicle, includes a tread formed of a rubber composition. The rubber composition includes at least (phr meaning parts by weight per hundred parts of elastomer): as a first diene elastomer, from 55 to 95 phr of natural rubber or synthetic polyisoprene; as a second diene elastomer, from 5 to 45 phr of a polybutadiene or butadiene copolymer having a glass transition temperature (Tg) which is greater than -70° C.; as a reinforcing filler, more than 90 phr and less than 150 phr of an inorganic filler; and as a plasticizer, more than 10 phr of a thermoplastic hydrocarbon resin exhibiting a glass transition temperature (Tg) greater than 20° C.
EP0940462 (A2) discloses high aromatic oil characterized by that a glass transition point is -45 to - 20 DEG C and an aromatic component measured by Clay-Gel method accounts for 55 to 90 % by weight and that a polycyclic aromatic compound measured by IP 346 method accounts for less than 3 % by weight based on the whole components of hydrocarbons contained in the oil. This high aromatic oil can suitably be used for various rubber compositions such as tires, rubber vibration insulators and fenders, oil extended synthetic rubbers, printing inks and writing inks. CN104059329A discloses a rubber characterized by including the following substances by weight: 14-20 parts of furfuryl alcohol resin, 21-30 parts of urea formaldehyde resin, 26-29 parts of polytetrafluoroethylene gum, 4-8 parts of silicon carbide, 9-14 parts of a formaldehyde solution, 16- 17 parts of glacial acetic acid, 3-9 parts of resorcinol, 1-4 parts of paraformaldehyde, 1-9 parts of precipitated barium sulfate, 2-8 parts of Hoveniaacerba sawdust, 3-7 parts of camellia oleifera sawdust, 4-8 parts of Eucalyptus globules sawdust, 1-2 parts of anatase titanium dioxide, 0.5-1 part of nano-organic montmorillonite, and 3-4 parts of talcum powder.
Natural product chitosan, moringa oleifera seeds, papain, strychnos seeds, have been used as coagulants.
EP2143755 Al discloses methods for making shapeable composite materials or shaped articles from recycled materials comprising forming a crumb slurry by, in any order, increasing the particle size of a composition comprising white water waste from one or more emulsion or dispersion polymer and combining the white water waste polymer with one or more waste thermoset material, preferably, ground tire rubber (GTR), and, then processing the combined material wet or dry as a thermoplastic to form the composite material or article. Useful coagulating agents include any known coagulation agents such as, for example, any chosen from a salt, such as sodium chloride or iron (ferric) chloride, i.e. FeC13, , iron (ferrous) sulfate, i.e. Fe2(SO4)3, alum, i.e. A12(SO4)3, magnesium sulfate, or preferably FeC13; an acid, such as a carboxylic acid, e.g. formic acid, or sulfuric acid to reduce the pH of the white water polymer to 4.5 or less, preferably 4.0 or less; a chemical coagulant and mixtures thereof. Other chemical coagulants may include alumina, aluminium chlorohydrate, calcium oxide, polyacrylamide, sodium aluminate, and sodium silicate, and the like; and natural product coagulants may include chitosan, moringa oleifera seeds, papain, strychnos seeds, and is in glass, among others.
US2017273313A1 relates to compositions comprising a vehicle such as a polymer base, moringa oil and neem oil. The combination of the two oils is in an amount sufficient to prevent the establishment or proliferation of a microorganism, such as a mildew, on the surface of an inanimate object. The moringa oil and neem oil combination can be advantageously admixed with a paint base, a solvent system, or other vehicle base for the treatment of wood, dry wall, or other porous or non- porous surface that is susceptible to a biological infestation. US2010167013A1 discloses thermoplastic roofing membranes comprising particles of cross linked rubber and an aqueous (co)polymer dispersion. The thermoplastic roofing membranes are formed by combining particles of cross linked rubber and a suspension polymer dispersion, or a coagulated aqueous latex (co)polymer dispersion, to form a mixture in aqueous dispersion, which aqueous dispersion mixture is subjected to solid state shear pulverization to form materials that can be processed as thermoplastics at cross linked rubber concentrations of from 10 wt. % to as high as 95 wt. %, based on the total solids of the material. The method may further comprise kneading the pulverized product, followed by extrusion to form roofing membranes. Suitable methods of coagulation may include the addition of an acid, such as formic acid or sulfuric acid, or a salt, such as sodium chloride or iron (ferric) chloride. Other chemical coagulants may include alum, alumina, aluminiumchlorohydrate, aluminium sulfate, calcium oxide, iron (ferrous) sulfate, magnesium sulfate, polyacrylamide, sodium aluminate, and sodium silicate, and the like; and natural product coagulants may include chitosan, Moringa oleifera seeds, papain, strychnos seeds, and isinglass, among others.
AU2009202787A1 relates to methods of making shapeable composites in the form of finely divided materials or articles and the materials and articles produced by the methods, the methods comprising forming mixtures by (i) treating an aqueous thermoplastic acrylic or vinyl polymer to increase the particle size thereof to a weight average particle size of 1 pm or more, and, optionally, dewatering to form a crumb mixture; and (ii) combining a thermoplastic acrylic or vinyl polymer with one or more waste rubber vulcanizate having a sieve particle size ranging from 10 to 600 pm in the amount of from 15 to 95 wt.%, based on the total weight of polymer and rubber to form a crumb slurry, such that (ii) can take place before, during, after (i) but before any dewatering, or after any dewatering; and (iii) thermoplastic processing the mixture. Useful coagulating agents include any known coagulation agents such as, for example, any chosen from a salt, such as sodium chloride or iron (ferric) chloride, i.e. FeC13, iron (ferrous) sulfate, i.e. Fe2(SO4)-, alum, i.e. A12(SO4)3, magnesium sulfate, or preferably FeC13; an acid, such as a carboxylic acid, e.g. formic acid, or sulfuric acid to reduce the pH of the acrylic or vinyl polymer to 4.5 or less, preferably 4.0 or less; a chemical coagulant and mixtures thereof. Other chemical coagulants may include alumina, aluminiumchlorohydrate, calcium oxide, polyacrylamide, sodium aluminate, and sodium silicate, and the like; and natural product coagulants may include chitosan, moringa oleifera seeds, papain, strychnos seeds, and isinglass, among others. US2010016456A1 relates to methods of making composite materials comprising combining particles of crosslinked rubber with coagulated aqueous polymer dispersions to form a mixture in aqueous dispersion, and subjecting the aqueous dispersion mixture to solid state shear pulverization to form materials that can be processed as thermoplastics at crosslinked rubber concentrations of from 10 to as high as 95 wt. %, based on the total solids of the material. The method may further comprise kneading the pulverized product to form useful articles, such as roofing membranes and shoe soles. Suitable methods of coagulation may include the addition of an acid, such as formic acid or sulfuric acid, or a salt, such as sodium chloride or iron (ferric) chloride. Other chemical coagulants may include alum, alumina, aluminiumchlorohydrate, aluminium sulfate, calcium oxide, iron (ferrous) sulfate, magnesium sulfate, polyacrylamide, sodium aluminate, and sodium silicate, and the like; and natural product coagulants may include chitosan, moringa oleifera seeds, papain, strychnos seeds, and isinglass, among others.
The article entitled “Influence of Moringa oleifera derivates in blends of PBAT/PLA with LDPE” talks about the polymerization of moringa oil (MO) was carried out assisted by microwaves without catalysts presence. There studies about the polymerization of MO using microwaves technology. Moringa’ s oil and its polymer (PMO) were used as a biodegrading agent for mixtures of low density polyethylene (LDPE) with poly (butylene adipate-co-terephthalate)/poly (lactic acid) (PBAT/PLA). The mixtures producted films that were characterized and submitted to biodegradation analysis in order to discuss the influence of moringa components. Results showed that both moringa components improved thermal properties and reduced the crystalline phase of the mixture. The addition of PMO had improved the biodegradation capacity up to five times while MO had improved it up to three times. The results showed the greatest influence of moringa components on biodegradation of mixtures with cited polymers [Cristiane Medina Finzi-Quintao, KatiaMonteiro Novack, Ana Claudia Bernardes-Silva, Thais Dhayane Silva, Lucas Emiliano Souza Moreira, LuizaEduardaMoraes Braga; Polimeros vol.28 no.4 Sao Carlos, Aug./Sept. 2018].
The alternatives to aromatic processing oils that are now being used by rubber processors are of petroleum origin and thus consist of a non-renewable resource.
Further, there is a global approach to use a larger proportion of renewable materials in all manufactured goods and products to minimize the use of processing oils that contain polynuclear aromatic compounds. Accordingly, there exists a need for a rubber composition for motor cycle tyre treads using naturally occurring Moringa oleifera oil that eliminates the use of aromatic oil and provides better winter traction along with dry traction and lower rolling resistance property.
OBJECTS OF THE INVENTION
It is the principal object of the present invention to provide rubber composition for tyre treads using naturally occurring Moringa oleifera oil.
It is another object of the present invention to provide a tyre produced using the rubber composition, capable of providing better winter traction along with dry traction and lower rolling resistance property.
It is another object of the present invention to provide a tyre produced using the rubber composition, capable of providing better rubber processing properties.
It is another object of the present invention to eliminate the use of aromatic oil.
SUMMARY OF THE INVENTION
One or more of the problems of the conventional prior art may be overcome by various embodiments of the present invention.
It is a primary aspect of the present invention to provide a rubber composition for tyre treads, comprising of: one or more rubbers - 100 phr; reinforcing fillers comprising carbon black in the range of 25-55 phr and silica in the range of 5-30 phr; coupling agent - 2 - 8.50 phr; activators - 2 - 10 phr; anti-degradants- 0.5 - 6phr; vulcanization agent - 1 - 3 phr; primary accelerators - 1 - 3 phr; naturally occurring Moringa oleifera oil 1 - 20 phr, wherein the Moringa oleifera oil comprises of high oleic acid 60 - 80 gm / 100 gm with a flash point greater than 260°C.
It is another aspect of the present invention to provide a rubber composition for tyre tread, wherein said rubbers are selected from one or more of natural rubbers, non-oil extended styrene butadiene rubber, poly butadiene rubber, diene rubbers namely SSBR, OESBR, OEBR, ENR or blend of two or three diene rubbers. It is another aspect of the present invention to provide a rubber composition for tyre tread, wherein said rubbers comprises by weight of natural rubbers 20-55 phr, non- oil extended styrene butadiene rubber 20-75 phr and poly butadiene rubber 10-35 phr.
It is another aspect of the present invention to provide a rubber composition for tyre tread, wherein said reinforcing fillers comprises of carbon black grades N100 series, N200 series, N300 series or blend of any of these two carbon black grades, inorganic filler silica and combinations thereof.
It is another aspect of the present invention to provide a rubber composition for tyre tread, wherein said coupling agent is bifunctional, sulfur containing organosilane or Si69 bis3- triethoxysilylpropyltetrasulfide
It is another aspect of the present invention to provide a rubber composition for tyre tread, wherein said activators comprises of zinc oxide, stearic acid and combinations thereof.
It is another aspect of the present invention to provide a rubber composition for tyre tread, wherein said anti-degradants comprises of N-(l,3-Dimethylbutyl)-N’-phenyl-phenylenediamine 7-(6PPD), 2,2,4-trimethyl- 1 ,2-dihydroquinoline (TDQ).
It is another aspect of the present invention to provide a rubber composition for tyre tread, wherein the vulcanization agent is sulphur.
It is another aspect of the present invention to provide a rubber composition for tyre tread, wherein the primary accelerator is selected from N-cyclohexyl-2-benzthiazolesulfenamide and guanidines, thiazoles, sulphenamides and thiuram sulphides or its mixtures.
It is another aspect of the present invention to provide a method of preparation of rubber composition for tyre tread, comprising of steps: master batch preparation by:
Step I: mixing of rubber component and adding 80 - 90% of the reinforcing filler; adding 80 - 90 % of inorganic reinforcing filler silica and silane coupling agent; mixing the added ingredients for silanisation at around 105 to 125 °C at 20 to 30 rpm; addition of remaining reinforcing fillers, rubber chemicals except N-(1,3-Dimethylbutyl)-N’- phenyl -phenylenediamine and zinc oxide and Moringa oleiferaoil; sweeping down in the orifice and allowing to mix for time period of 50 - 60 seconds; dumping the compound at temperature range between 135 and 160 °C; sheeting out the rubber compound to yield master batch.
Step II
Mixing of activators and anti -degrandants with Step I master batch at a temperature range between 135 °C and 150°C; sheeting out the rubber compound;
Step III mixing of Step II master batch; dump at a temperature range between 135°C and 150 °C; sheeting out the rubber compound; final batch preparation by:
Mixing of step III master batch compounds with curatives;
Dumping at a temperature range between 85 °C and 120 °C;
Sheeting out the rubber compound.
It is another aspect of the present invention to provide a method of preparation of rubber composition for tyre tread, wherein the processing parameters for master batch preparation are rotation speed of mixer between 55 and 65 rpm and the head temperature of the mixer maintained between 55°C and 65°C.
It is another aspect of the present invention to provide a rubber composition for tyre tread containing 10 phr of Moringa Oleifera Oil, wherein the hardness of the rubber vulacanizate is 60 Shore A.
It is another aspect of the present invention to provide a rubber composition of tyre tread containing 10 phr of Moringa Oleifera oil as claimed in claim 1, wherein the winter traction E’ at -20°C is 57.3 MPa.
It is another aspect of the present invention to provide a rubber composition of tyre tread containing 10 phr of Moringa Oleifera Oil as claimed in claim 1, where in dry traction, loss compliance J”@30°C is 0.0079 MPa-1. It is another aspect of the present invention to provide a rubber composition of tyre tread containing 10 phr of Moringa oleifera oil as claimed in claim 1, wherein LRR, tan delta at 60 °C is 0.158 (no unit)
It is another aspect of the present invention to provide a rubber composition of tyre tread containing 10 phr of Moringa Oleifera oil as claimed in claim I, wherein Mooney viscosity of the final batch rubber compound is 36.30 MU (Mooney unit).
BRIEF DESCRIPTION OF DRAWINGS
Figure 1: represents the ATR FTIR spectra of Moringa oleifera oil.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to the field of rubber processing for tyres. The present invention relates to rubber composition for motor cycle tyre treads using naturally occurring Moringa oleifera oil. The present invention also provides a tyre produced using this rubber composition, capable of providing better winter traction along with dry traction and lower rolling resistance property. The rubber composition of tyre tread includes 100 parts by weight of a rubber, preferably with the blend of natural rubber, styrene butadiene rubber and butadiene rubber, preferably natural rubbers 20 - 55 phr, non- oil extended styrene butadiene rubber 20 - 75 phr and poly butadiene rubber 10 - 35 phr, 30 to 80 parts of the reinforcing filler such as carbon black, preferably with carbon black with the iodine surface area of 114 to 126 mg/gm at a concentration of 25-55 phr, and preferably silica 5-30 phr, along with the use of 2 to 20 parts of a naturally occurring Moringa oleifera oil with high oleic acid 60-80gm/100gm and also with the flash point greater than 260°C which is higher than aromatic oil and TDAE oil. The invention also relates to the better processing properties of the rubber compound.
In accordance with the present invention, rubber composition for motor cycle tyre tread consists of the rubbers selected from one or more of natural rubber, non-oil extended styrene butadiene rubber and poly-butadiene rubber, preferably in a weight ratio for combination of rubbers are natural rubber 20 - 55 parts, Non-oil extended styrene butadiene rubber 20 - 75 parts, and poly-butadiene rubber 10 - 35 parts and 2 to 20 parts of a naturally occurring Moringa oleifera oil. In accordance with the present invention, the rubber composition also consists of reinforcing fillers - 20 - 80 phr; coupling agent - 2 - 8.50 phr; activators - 2 - 10 phr; anti-degrandants - 0.5 - 6phr; primary accelerators - 1- 3 phr; and vulcanization agent - 1- 3.0 phr.
Method of preparation of rubber composition comprising of naturally occurring Moringa oleifera oil:
An embodiment of the present invention discloses the method of preparation of a rubber composition comprising of naturally occurring Moringa oleifera oil.
Mixing Sequence:
Using a mixer a rubber composition prepared by a thermomechanical process is as follows: For exemplification, a particular batch of the rubber composition is prepared in Banbury mixer.
Preparation of master batch:
Step I: Preparation of masterbatch has been performed with the rotation speed of the mixer between 55 to 65 rpm and with the head temperature of the banbury maintained between 55 to 65° C. a) Mixing chamber has been charged with the selected rubbers, and allowed to mix for 0 to 30 seconds b) Further by adding 80 to 90% of the reinforcing filler carbon black and 80 to 90% of the reinforcing filler silica, silane coupling agent Si75, and allowed to mix for 60 seconds for silanisation at around 105 to 125° C, c) the process of silanisation has been done with the reduced the rotor speed 20 to 30 rpm d) The remaining carbon black and silica, along with Moringa oleifera oil or aromatic oil, rubber chemicals except 6PPD and zinc oxide are added, and allowed to mix for 50 to 60 seconds e) sweeping done in the orifice and allowed to mix for 50 to 60 seconds and the compound has been dumped at the temperature in the range of 135 °C to 160 °C. The master batch rubber compound has been sheeted out in the laboratory two-roll mill.
Step II: Mixing chamber of banbury charged with the Step I master batch, chemicals zinc oxide and 6PPD, and allowed to mix for 120 seconds and dumped in the temperature range of 135°C to 150°C. The rubber compound has been sheeted out in the laboratory two-roll mill.
Step III: Mixing chamber of banbury charged with the Step II master batch, and allowed to mix for 120 seconds and dumped at the temperature range of 135°C to 150°C. The rubber compound has been sheeted out in the laboratory two-roll mill. Preparation of Final Batch: Mixing chamber charged with the Step III master batch and the curatives, and allowed to mix for 50 to 80 seconds and dumped at the temperature range of 85 °C to 120°C. Final batch sheet out of the rubber compound has been done in the laboratory two roll mill.
Example
The present invention will be explained further by examples, but the scope of the present invention, is not limited to these examples.
The present invention related to the rubber composition for motor cycle tyre treads using naturally occurring Moringa oleifera oil and to rubber compositions according to Table 1 manufacture thereof. The rubber composition according to the invention comprises of: a. The motor cycle tyre tread composition acccording to the invention, which can be used for the manufacture of a tyre, comprising 100 parts by weight of a rubber(s), 25 parts by weight of a natural rubber1 ISNR 20 with the massed raw rubber mooney viscosity ML (1+4) @
2 100°C of 73 to 87 mooney units, 65 parts of the non oil extended styrene butadiene rubber SBR1502 with 22.5 to 24.5% of styrene content and 10 parts by weight of a PBR 1220 a polybutadiene rubber with the 96% cis 1, 4 configuration. b. Reinforcing filler, Carbon Black ISAF (Intermediate Superior Abrasion Furnace) ASTM grade N2204, or any of the ASTM grades of Carbon Black having the Iodine adsorption No. 116 to 126 mg/gm, tinting strength value between 110 to 129 % ITRB, statistical thickness surface area value between 102 to 117 m /gm and with the blend of another reinforcing inorganic filler silica, Ultrasil VN35 grade with the nitrogen surface area value 170 to 190 m /gm used for the present invention is to provide better dry traction and LRR property. c. In order to couple the inorganic filler silica to the diene elastomer, bi functional organosilane coupling agent SI756 is used to provide a satisfactory bonding of, chemical/or physical nature between the inorganic filler and diene elastomer(s). d. In accordance to the present invention, the Moringa oleifera oil10 used in the NR: SBR: BR blend (25:65:10) based rubber composition is to provide better winter traction along with dry traction and lower rolling resistance of a motor cycle tyre tread have the essential characteristics i) the iodine value lesser than 70 ii) viscosity using U tube viscometer C is greater than 85 cSt iii) Flashpoint greater than 260°C, and iv) density @ 20°C is 0.8956 gm/ml. The most common fatty acids present in the Moringa oleifera oil are palmitic acid (C16:0), palmitoleic acid - C16:l, stearic acid (C18:0) - 5.99%, oleic acid (C18: l) - 68.36%, linoleic acid (C18:2) - 1.36%, arachidic acid (C20:0) - 3.66%, gadoleic acid -2.10% and behenic acid (C22:0) - 6.0%. Also the Moringa oleifera oil identified the spectrum 3476.98 cm’1 which refers to hydroxyl groups formed by triglyceride hydrolysis. The absorption band at 3004 - 3009 cm’1 is typical of fatty acids as oleic acid and indicates the cis stretching of double bond (=C-H).
Polycyclic aromatic hydrocarbons (PAH) Benz(a)anthracene is less than 0.5pg/kg, Benzo(a)pyrene is less than 0.5pg/kg, Benzo(b)fluoranthene is less than 0.5pg/kg and Chrysene 1.29 pg/kg.
The above PAH’s in accordance with EC regulation 835/2011 as regards to maximum levels for Polycyclic Aromatic Hydrocarbons.
The Figure 1. represents the Attenuated total reflectance - Fourier transform infrared (ATR- FTIR) spectra of Moringa oleifera Oil. e. Aromatic oil9, Elasto 710 grade is used in the compound is to compare with the Moringa oleifera oil used in the present invention to provide better winter traction along with dry traction and lower rolling resistance property. f. The other ingredients selected for the present invention is based on the conventional motor y cycle tyre tread composition activator zinc oxide and stearic acid, antidegradant 6PPD , TDQ8 g. The vulcanization system used in the present invention is based on sulphur and on a primary accelerator CBS11.
Table 1:
Rubber composition in phr:
Figure imgf000013_0001
Figure imgf000014_0001
1- Indian Standard Natural Rubber ISNR 20 with the Mooney Viscosity, ML (1+4) @ 100°C is 75 MU.
2- Non-oil extended styrene butadiene Rubber, SBR1502
3- Poly butadiene rubber , PBR 1220
4- ASTM Grade N220 from Birla Carbon, India
5- Ultrasil VN3 Silica having nitrogen surface area from Insilco Ltd, Evonik Industries GmbH, India.
6- Si75 is a bifunctional, sulfur-containing organosilane from Evonik Resource efficiency GmbH, Germany.
7- 6PPD (N-(l,3-dimethylbutyl)-N’ -phenyl -p-phenylenediamine) from Nocil Limited, India
8- TDQ 2, 2, 4-trimethyl- 1 , 2-dihydroquinoline from Lanxess, India
9- Aromatic Oil from Indian Oil Corporation Limited, India.
10- Moringa oleifera Oil from Miracle Tree Life Science, Madurai, India.
11- CBS (N-cyclohexyl-2-benzothiazolesulfenamide) from Nocil Limited, India.
Results
Characterization of Cured Rubber Vulcanizate and Uncured Rubber Compound:
The compound properties are listed in Table 2 below-
Measurements and Tests:
Better processability (Process Requirements) of a Rubber Compound:
Ml. Mooney Scorch Characteristics (pre-vulcanization characteristics using large rotor) for processability: The Mooney Scorch measurements are carried out with a Mooney Viscometer (MV 2000 Alpha technologies, USA) according to ASTM DI 646. MV indicates the minimum viscosity, ts indicates the time to scorch (MV+5) which indicates the processing properties (process safety) and t35 indicates the time to cure (MV+35).
The test is carried out through Mooney Viscometer. t5 scorch time (ts) - the time interval (measured from rotor start) corresponding to a viscosity increase of 5 Mooney units over MV, measured at rotor start. The t5 value indicates the prevulcanization tendency of the compound.
M2. Shore A Hardness:
Shore A Hardness of the Rubber Vulcanizate is assessed in accordance with ASTM D 2240. Shore Hardness is a measure of the resistance a material has to indentation. The test carried out for rubber vulcanizate using Shore A Durometer instrument. The Hardness unit for rubber materials is Shore A.
Dynamic properties of the rubber vulcanizate:
M3. The dynamic properties of the rubber vulcanizate are measured in accordance with ASTM D5992 on a dynamic mechanical analyzer (DMA Metravib +1000) with a dynamic strain 0.1%, temperature sweep from -120 to +100°C, frequency: 20Hz in tension mode. a. Storage Modulus E’ at a temperature in the region of -20°C in tension mode is used as a predictor for winter traction. Lower the E’ Storage modulus value at -20°C, better the winter traction. b. Loss compliance J” @ 30°C is commonly used as a predictor for dry traction. Higher the J” value is better the dry traction. c. Tan delta at 60°C is used as a predictor for Lower Rolling Resistance. Lower the tan delta value at 60° C is lower the rolling resistance.
Table 2: Properties of Rubber Compounds
Figure imgf000015_0001
Figure imgf000016_0001
RESULTS
The purpose of these tests is to measure the rubber compound properties of the compositions related to invention F3, against the control composition Fl, F2. Three compositions Fl, F2, F3 were prepared based on NR: SBR: BR blend (25:65: 10) blend reinforced by carbon black and silica containing Moringa oleifera Oil (F3) against NR: SBR: BR blend (25:65:10) blend reinforced by carbon black and silica without oil (Fl) and containing 10 phr aromatic oil (F2) are prepared and evaluated. The present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65:10) blend based rubber composition containing 10 phr Moringa oleifera oil gave mooney viscosity value lowered by 31.38% when compared to NR: SBR: BR blend (25:65:10) based rubber composition without oil, Fl (Control) whereas NR: SBR: BR blend (25:65: 10) based rubber composition containing 10 phr aromatic oil, F2 gave mooney viscosity value lowered by 24.95%. In the present invention Mooney Scorch test performed at 125 °C. In general the t5 value @ 125 °C for tread compounds ideally should be greater than 15 minutes. In the present invention, the Moringa olifera oil added tread composition F3 gave process safety.
The present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65:10) blend based rubber composition containing 10 phr Moringa oleifera oil gave Shore A hardness value lowered by 9.09 % when compared to NR: SBR: BR blend (25:65: 10) based rubber composition without oil Fl (Control) whereas NR: SBR: BR blend (25:65:10) based rubber composition containing 10 phr aromatic oil F2 gave Shore A hardness value lowered by 6.06%.
Hence, the present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65: 10) blend based rubber composition containing 10 phr Moringa oleifera oil containing rubber composition, F3 gave lower hardness and lower mooney viscosity which indicates Moringa oleifera oil is having better compatibility with the polymer blend used in the present invention when compared to aromatic oil containing rubber composition, F2.
The present invention provides a 100 parts by weight of rubber composition, NR: SBR: BR blend (25:65: 10) blend based rubber composition containing 10 phr. Moringa oleifera oil gave process safety, 15 ^35 value improved by 21.70% & 18.98% respectively when compared to NR: SBR: BR blend (25:65: 10) based rubber composition containing no oil, Fl (Control).
The present invention relates to a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65: 10) blend based rubber composition containing 10 phr of Moringa oleifera oil gave 31.70% lowered E’ Storage modulus value @ -20°C i.e., better winter traction along with 38.60% improved dry traction when compared to when compared to NR: SBR: BR blend (25:65:10) based rubber composition containing no oil, Fl (Control) whereas NR: SBR: BR blend (25:65: 10) based rubber composition containing 10 phr aromatic oil, F2 gave 10.61 % lowered E’ Storage modulus value @ -20°C along with 33.30 % improved dry traction when compared to NR: SBR: BR blend (25:65: 10) based rubber composition containing no oil, Fl (Control).
Hence, the present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65:10) blend based rubber composition containing 10 phrMoringa oleifera oil, F3 gave 23.60% lowered E’ storage modulus value @ -20°C i.e., better winter traction along with 3.80 % improved dry traction when compared to NR: SBR: BR blend (25:65: 10) based rubber composition containing 10 phr aromatic oil, F2.
Also, the present invention provides a 100 parts by weight of rubber composition F3, NR: SBR: BR blend (25:65:10) blend based rubber composition containing 10 phrMoringa oleifera oil, F3 gave
5.95% lowered rolling resistance when compared to NR: SBR: BR blend (25:65:10) based rubber composition containing 10 phr aromatic oil, F2.

Claims

WE CLAIM:
1. A rubber composition for tyre treads, comprising of: one or more rubbers - 100 phr; reinforcing fillers comprising carbon black in the range of 25-55 phr and silica in the range of 5-30 phr; coupling agent - 2 - 8.50 phr; activators - 2 - 10 phr; anti-degradants- 0.5 - 6phr; vulcanization agent - 1 - 3 phr; primary accelerators - 1 - 3 phr; and naturally occurring Moringa oleifera oil 1 - 20 phr, wherein the Moringa oleifera oil comprises of high oleic acid 60 - 80 gm / 100 gm with a flash point greater than 260°C.
2. The rubber composition for tyre tread as claimed in claim 1, wherein said rubbers are selected from one or more of natural rubbers, non-oil extended styrene butadiene rubber, poly butadiene rubber, diene rubbers namely SSBR, OESBR, OEBR, ENR or blend of two or three diene rubbers.
3. The rubber composition for tyre treads as claimed in claim 1, wherein said rubbers comprises by weight of natural rubbers 20-55 phr, non- oil extended styrene butadiene rubber 20-75 phr and poly butadiene rubber 10-35 phr.
4. The rubber composition for tyre treads as claimed in claim 1, wherein said reinforcing fillers comprises of carbon black grades N100 series, N200 series, N300 series or blend of any of these two carbon black grades, inorganic filler silica and combinations thereof.
5. The rubber composition for tyre treads as claimed in claim 1, wherein said coupling agent is bifunctional, sulfur containing organosilane or Si69 bis3-triethoxysilylpropyltetrasulfide.
6.The rubber composition for tyre treads as claimed in claim 1, wherein said activators comprises of zinc oxide, stearic acid and combinations thereof.
7. The rubber composition for tyre treads as claimed in claim 1, wherein said anti -degradants comprises of N-( 1 ,3-Dimethylbutyl)-N’ -phenyl-phenylenediamine
7-(6PPD), 2,2,4-trimethyl-l,2-dihydroquinoline (TDQ).
8. The rubber composition for tyre treads as claimed in claim 1, wherein said vulcanization agent is sulphur.
9. The rubber composition for tyre treads as claimed in claim 1, wherein said primary accelerator is selected from N-cyclohexyl-2-benzthiazolesulfenamide and guanidines, thiazoles, sulphenamides and thiuram sulphides or its mixtures.
10. A method of preparation of rubber composition for tyre tread, comprising of steps: master batch preparation by:
Step I mixing of rubber component and adding 80 - 90% of the reinforcing filler; adding 80 - 90 % of inorganic reinforcing filler silica and silane coupling agent; mixing the added ingredients for silanisation at around 105 to 125 °C at 20 to 30 rpm; addition of remaining reinforcing fillers, rubber chemicals except N-(l,3- Dimethylbutyl)- N’ -phenyl-phenylenediamine and zinc oxide and Moringa oleiferaoil; sweeping down in the orifice and allowing to mix for time period of 50 - 60 seconds; dumping the compound at temperature range between 135 and 160 °C; sheeting out the rubber compound to yield master batch;
Step II
Mixing of activators and anti -degrandants with Step I master batch at a temperature range between 135 °C and 150°C; sheeting out the rubber compound;
Step III mixing of Step II master batch; dump at a temperature range between 135°C and 150 °C; sheeting out the rubber compound; final batch preparation by:
Mixing of step III master batch compounds with curatives;
Dumping at a temperature range between 85 °C and 120°C; and Sheeting out the rubber compound.
11. The method of preparation of rubber composition for tyre tread as claimed in claim 10, wherein the processing parameters for master batch preparation are rotation speed of mixer between 55 and 65 rpm and the head temperature of the mixer maintained between 55°C and 65°C.
12. The rubber composition for tyre tread containing 10 phr of Moringa Oleifera Oil as claimed in claim 1 , wherein the hardness of the rubber vulacanizate is 60 Shore A.
13. The rubber composition of tyre tread containing 10 phr of Moringa Oleifera oil as claimed in claim 1, wherein the winter traction E’ at -20°C is 57.3 MPa.
14. The rubber composition of tyre tread containing 10 phr of Moringa Oleifera Oil as claimed in claim 1, where in dry traction, loss compliance J”@30°C is 0.0079 MPa-1.
15. The rubber composition of tyre tread containing 10 phr of Moringa oleifera oil as claimed in claim 1, wherein LRR, tan delta at 60°C is 0.158 (no unit)
16. The rubber composition of tyre tread containing 10 phr of Moringa Oleifera oil as claimed in claim 1, wherein Mooney viscosity of the final batch rubber compound is 36.30 MU (Mooney unit).
PCT/IN2021/050435 2020-08-05 2021-05-05 Rubber composition for motor cycle tyre treads using moringa oleifera oil and method thereof WO2022029791A1 (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2231769A1 (en) * 2007-12-27 2010-09-29 Société de Technologie Michelin Rubber composition for the tread of a winter tyre
CN103221466A (en) * 2010-11-26 2013-07-24 米其林集团总公司 Tyre tread
WO2016131704A1 (en) * 2015-02-17 2016-08-25 Compagnie Generale Des Etablissements Michelin Tyre, the tread of which includes a phenolic compound

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2231769A1 (en) * 2007-12-27 2010-09-29 Société de Technologie Michelin Rubber composition for the tread of a winter tyre
CN103221466A (en) * 2010-11-26 2013-07-24 米其林集团总公司 Tyre tread
WO2016131704A1 (en) * 2015-02-17 2016-08-25 Compagnie Generale Des Etablissements Michelin Tyre, the tread of which includes a phenolic compound

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