DESC:FIELD OF INVENTION
The present invention relates to the field of Polymer technology particularly, relates to the tyre rubber composition with bamboo leaf ash as a filler material and its method of preparation thereof.
BACKGROUND OF THE INVENTION
Rubbers or elastomers have remarkable properties and can be transformed and tailored to give extremely useful products in a wide range of applications by embedding particles, short or long fibres or textiles. Such rubber composites have major changes in force-deformation behavior strength, fatigue and wear characteristics.
The most predominant reinforcing filler is Carbon Black used in rubber compounds, which imparts the necessary durability and strength to the products for longer lifetime and improved performance. It distributes and absorbs stress applied to a rubber component and improves its tensile strength, tear strength and abrasion resistance. It also imparts electrical conductivity / resistivity to a rubber compound for dissipating static charge in dynamic applications. However, according to the current International Agency for Research on Cancer (IARC), "Carbon black is possibly carcinogenic to humans and short-term exposure to high concentrations of carbon black dust may produce discomfort to the upper respiratory tract, through mechanical irritation.
Hence natural fibres also have reinforcing capability, which holds many advantages over synthetic fibres, as they are widely abundant, less costly, biodegradable and nonabrasive. The automotive industries in Europe and North America have been manufacturing vehicles with partially biodegradable parts, made from fibres such as kenaf, jute, flax and hemp and petroleum thermoplastics such as polypropylene and polyethylene. Cellulose fibre from pulp has also been studied and incorporated into composites with various applications. Composites reinforced by fiber have a brittle and strong fibrous reinforcing phase, surrounded by a more ductile matrix phase. Addition of fibres to a matrix phase improves strength, stiffness and fatigue resistance, as most of the force applied to the composite is carried by the fibre phase.
Reference made for the following:
Publication No.1067/MUM/2015 relates to a biofiller for rubber reinforcement; said biofiller is surface treated up to 10% by weight of microcrystalline lignocellulose with aldehyde and / or ketone. The said bio-filler has economic significance as well as reduces pollution as it replaces 2 % carbon black with the rubber composition which is substantial amount after reviewing overall use of carbon black in rubber industries such as tyre industry, worldwide. A rubber composition comprises the said bio filler and its various applications such as tyre, shoes, bags, belts, etc. whereas the present invention discusses the use of a nano bio filler as a filler material for tyre rubber composition.
Publication No. JP2011162627 relates to improve working environment at manufacturing of a rubber composition by reducing odor caused by a natural rubber, to also reduce odor of a rubber product after vulcanization, and to also suppress reduction of reinforcement property of the rubber product further in the method for manufacturing the rubber composition, a masticated rubber is produced by performing mixing operation of a first stage by formulating 0.05-5 pts. Mass of a powder having an average particle diameter of 500 µm or less comprising a porous carbide (for example, bamboo coal) of a plant based on 100 pts. Mass of a diene-based rubber containing 50 pts. mass or more of the natural rubber, and mixing operation of a second stage is performed by formulating a compounding agent containing a filler to the obtained masticated rubber whereas the present invention discusses about the use of bamboo leaf ash as a filler material for tyre rubber composition. Publication No. KR100917446 relates to a tyre tread rubber composition is provided to improve cut and chip performance and exothermic performance and to increase abrasion resistance by comprising petroleum resin and pyroligneous liquor. A tyre 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 whereas the present invention discusses about the use of a nano bio filler as a filler material for tyre rubber composition.
Publication No. CN103709455 relates to an automotive suspension rubber composition. The automotive suspension rubber composition consists of the following raw materials in parts by weight: 100-104 parts of natural rubber SVR3L, 10-20 parts of clay, 2-3 parts of boron oxide, 1-2 parts of phthalic anhydride, 4-6 parts of calcium carbonate whisker, 1-2 parts of benzotriazole, 1-2 parts of a dispersant NNO, 0.6-1 part of hydrogenated castor oil, 2-4 parts of anhydrous calcium chloride, 1-2 parts of Tri ethylene glycol, 4-7 parts of bamboo charcoal powder, 1-1.6 parts of sulfur, 1-2 parts of a promoter NOBS, 1-2 parts of an anti-aging agent 3100, and 24-30 parts of a composite filler. The automotive suspension rubber composition disclosed by the invention has excellent resistance to high temperature fatigue, low ratio of dynamic stiffness and static stiffness, strong corrosion resistance and acid and alkali resistance, good compression resistance, and superior comprehensive performance whereas the present invention discusses the use of a nano bio filler as a filler material for tyre rubber composition.
Publication No. JP2007126524 relates a rubber composition for a tyre, having effectively improved properties on ice by a comparatively small, compounded amount, and having excellent properties on the ice and excellent abrasion resistance in the rubber composition compounded with bamboo charcoal suitable for a studless tyre. the method for producing the rubber composition for the tyre comprises a mixing step (a) for charging a diene rubber, a reinforcing filler (carbon black and silica) and a liquid additive (oil, a coupling agent and the like) to a mixer, and mixing them, and a mixing step (b) for adding and mixing a vulcanizing agent and the bamboo charcoal powder having 10-500 µm average particle diameter to and with the mixed composition comprising the diene rubber, the reinforcing filler and the liquid additive by a mixer whereas the present invention discusses about the use of a nano bio filler as a filler material for tyre rubber composition.
Publication No. NL1020294 relates to the composition contains cellulosic material chips obtained from softwoods, hardwoods, bamboo and plant stems, in addition to from more than 10 vol.% to less than 95 vol.% additives such as glass shards, natural stone, rubber, plastic, ceramic, earth, metal and similar material granules. An independent claim is also included for a method for preparing the composition, comprising the following steps: adding adhesive to a mixture of cellulosic material and additives; adding the mixture to a mould and vibrating the mould in order to remove air bubbles; pressing the mixture at elevated temperature and pressure to form a board; coarse grinding the board until the grain is clearly visible; filling in the holes with transparent filler; grinding the filler; polishing; and painting mixer whereas the present invention discusses about the use of a nano bio filler bamboo leaf ash as a filler material for tyre rubber composition.
IN Publication No. 4368/DELNP/2014 relates to a moulding element of a mould for moulding and curing a tread of a tyre said tread comprising a tread surface intended to make contact with the ground during the rotation of the tyre. The moulding element comprises a moulding surface intended to mould part of the tread surface of the tyre and a blade of length L and height H intended to mould an incision or groove in the tread. The above-mentioned blade comprises a rounded end extending along the length of the blade in the direction of extension X. The moulding element also comprises two cutting means disposed on each side of the blade at a certain distance therefrom. Each cutting means includes an edge extending along the direction of extension and forming an acute angle in a cutting plane perpendicular to the direction of extension the height of said edge being greater than or equal to the height of the blade whereas the present invention discusses the use of a nano bio filler bamboo leaf ash as a filler material for tyre rubber composition.
IN Publication No. 3556/DELNP/2014 relates to a tyre having a tread comprising a felt characterized in that the fibres of the felt are fibres selected from the group made up of textile fibres mineral fibres and mixtures of same whereas the present invention discusses about the use of a nano bio filler as a filler material for tyre rubber composition.
IN Publication No. 3519/DELNP/2014 relates to a tyre having a tread characterized in that the tread comprises a felt impregnated with a thermoplastic elastomer material and in that the fibres of the felt are selected from the group containing textile fibres mineral fibres and mixtures thereof whereas the present invention discusses the use of a nano bio filler as a filler material for tyre rubber composition.
Reference may be to an article entitled “Preparation and characterization of natural rubber composites highly filled with brewers' spent grain/ground tyre rubber hybrid reinforcement” by Lukasz Zedler, Xavier Colom, Mohmmad Reza Saeb, Krzysztof Formela, Composites Part B: Engineering Volume 145, 15 July 2018 talks about the brewers' spent grain (BSG) and ground tyre rubber (GTR) were applied as low-cost hybrid reinforcement natural rubber (NR). The impact of BSG/GTR ratio (in range: 100/0, 75/25, 50/50, 25/75 and 0/100 phr) on processing and performance properties of highly filled natural rubber composites was evaluated by oscillating disc rheometer, Fourier-transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, swelling behavior, tensile tests and impedance tube measurements. It was found that increasing content of GTR in NR/BSG/GTR composites accelerate cross- linking reactions during their preparation, which resulted in decrease of scorch time and optimal cure time. Simultaneously, higher content of GTR fillers in NR/BSG/GTR composites significantly improved their physio-mechanical, thermal, morphological and acoustic properties. This indicates better compatibility between natural rubber matrix and GTR than with BSG, which is related to correlation between two factors. The first factor is obvious differences in particles size and polarity of GTR and BSG, which affected physical interactions into phase boundary between NR matrix and BSG/GTR hybrid reinforcement. The second factor is possible migration of unreacted curing additives and carbon black particles from GTR filler to NR matrix, which played a significant role in processing and final properties of NR/BSG/GTR composites whereas the present invention discusses the use of a nano bio filler as a filler material for tyre rubber composition.
Reference may be to an entitled “Compressive strength and durability of bamboo leaf ash concrete” by G. Dhinakaran and Gangava Hari Chandana; 1/25/2015;
Jordan Journal of Civil Engineering, Volume 10 talks about the feasibility of calcined bamboo leaf ash as a partial substitute to cement and its effect on compressive strength, pozzolanic activity, sorptivity and porosity characteristics in hardened concrete. Cement was replaced with BLA with a percentage of 10% to 30% with a uniform increment of 5%. Fallen dry bamboo leaves burnt in an open atmosphere were heated in a muffle furnace for 4 hours at 500°C to induce pozzolanic activity. The grade of concrete was taken in such a way that it will give a characteristic compressive strength of 20 MPa. The chemical composition of BLA was obtained by XRF analysis. The nature of BLA was assessed by XRD analysis and found to have an amorphous structure. The pozzolanic activity was ensured by ASTM lime test (ASTM C311 and ASTM C109). Other durability characteristics, like sorptivity and porosity, were performed as per ASTM guidelines (ASTM C1545 and ASTM C127) to assess the resistance of BLA concrete against sorption and the volume of voids. From the experiments conducted, it was understood that cement could be replaced with BLA till 15% with a little compromise in strength and durability characteristics and that this replacement was found to be an optimum one whereas the present invention discusses about the use of a nano bio filler as a filler material for tyre rubber composition.
Reference may be to an entitled “Bioresources fillers for rubber composite sustainability: Current development and future opportunities” by Boon Peng Chang; Arvind Gupta; Rajendran Muthuraj; Tizazu H. Mekonnen; 6/18/2021; Green Chemistry talks about the recent developments in the innovation and utilization of sustainable biofillers for rubber composite applications, emphasizing the effect of the filler on the structure-processing-property relationship in rubber composites. A wide range of bio fillers with an array of structure, morphology, and physicochemical properties and their various attributes in different rubbers are intensively reviewed and discussed. Effective fabrication strategies and surface modifications platforms on the different bio fillers to develop high- performance sustainable rubber bio composites were critically reviewed. Finally, future perspectives for bio fillers in rubber composite applications and challenges are discussed whereas the present invention discusses the use of a nano bio filler as a filler material for tyre rubber composition.
Reference may be to an entitled “Mechanical properties and microstructure of High-Performance Concrete with bamboo leaf ash as additive” by S.O. Odeyemi, O.D. Atoyebi, O.S. Kegbeyale, M.A. Anifowose, O.T. Odeyemi, A.G. Adeniyi, O.A. Orisadare, Cleaner Engineering and Technology Volume 6, 2/1/2022 talks about the demand for High-Performance Concrete (HPC) is on the increase for its good workability, high strength, and better durability. HPC are obtained by incorporating supplementary Cementitious Materials (SCM) into concrete to attain a long-term strength and durability performance. Though several SCM have been investigated in HPC, the use of Bamboo Leave Ash (BLA) in HPC as an SCM has not been considered. Thus, this research investigated the use of BLA as SCM in HPC. The bamboo leaves were calcined in an electric furnace at a temperature of 700 °C. The ash was characterized by using Energy Dispersive X-ray Fluorescence (EDXRF) and was found to possess pozzolanic properties with silica content above 70%. Cement was replaced by BLA at 5%, 10%, 15%, and 20% by weight of cement. Concrete made from these combinations were tested for compressive and splitting tensile strengths at 7, 28 and 56 days of curing. It was observed that optimum strength was attained at 5% replacement at 56 days of curing. The microstructures of the concrete revealed that at 5% incorporation of BLA in concrete, there was a better interlocking of concrete grain. It was concluded that cement can be replaced with 5% BLA in High Performance Concrete whereas the present invention discusses the use of as a filler material for tyre rubber composition.
Hence there is a need for a rubber composition which can have improved performance on road surface. In order to overcome the above listed prior art, the present invention aims to provide a tyre tread rubber composition containing a nano bio-filler with not less than 70% silica content which is obtained from bamboo leaf extract which is derived from bamboo leaf ash and its method of preparation thereof.
OBJECTS OF THE INVENTION
The principal object of the present invention is to provide a tyre rubber composition containing a nano bio-filler with not less than 70% silica content which is obtained from bamboo leaf extract which is derived from bamboo leaf ash and its method of preparation thereof.
Another object of the present invention is to provide a tyre rubber composition to provide improved dynamic mechanical properties.
Still another object of the present invention is to provide a tyre tread rubber composition containing bio filler bamboo leaf ash to replace carbon black reinforcing filler.
Yet another object of the present invention is to provide bio fillers from renewable resources.
Yet another object of the present invention is to reduce carbon footprint.
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.
SUMMARY OF THE INVENTION
In one aspect of the present invention, it pertains to a tire rubber composition containing a nano bio filler having atleast 70% of silica content which is obtained from bamboo leaf extract which is derived from bamboo leaf ash and its preparation method thereof.
In another aspect of the present invention, the rubber composition includes elastomeric matrix, carbon black reinforcing filler, a nano bio filler, activator, antidegradant, microcrystalline wax, process oil, vulcanization agent, primary and secondary accelerators. In an aspect of the present invention, a nano bio filler (Particle size passes through 40 # Mesh) having atleast 70% of silica content which is obtained from bamboo leaf extract which is derived from bamboo leaf ash as a reinforcing filler having specific surface area (multipoint BET) ranging from 364.30 m2/gm to 369.30 m2/gm, bulk density ranging from 0.3 g/ml to 0.80 g/ml and it is obtained from renewable resources and it is used as a partial replacement for reinforcing carbon black filler.
In an aspect of the present invention, the rubber composition for tyre tread contains 100 parts per hundred rubbers (phr) comprising both natural and synthetic rubbers, the selection of synthetic rubbers can be from SBR & PBR and its combination thereof. SBR can be selected based on Tg values ranging from -21 Deg C to -50 Deg C and the selected SBR can be from solution or emulsion polymerized techniques, Oil extended or non-oil extended SBR, functionalized SBR, polybutadiene rubber and the selected polybutadiene rubber can be catalyzed by Neodymium or lithium, 20-80 phr of reinforcing filler carbon black can be from ASTM grades N110, N121, N134, N234, N220, N231, N330, N339, N347, N375, N326, N550, N660 and the combinations thereof, inorganic fillers, functionalized organic or inorganic fillers etc., and a nano bio filler is added in the rubber composition and the rubber composition can be designed in order to achieve 55 to 78 Shore A of tyre tread rubber hardness.
Antidegradants can be from amine or phenolic types (staining or non-staining). Process aid can be selected from MES oil or TDAE oil or RAE oil or resins type of C5 or C5/C9 or hydrocarbon resin or combination thereof.
Accelerators can be from delayed action sulfenamides, thiazoles, thiuram sulfides, dithiocarbonates and guanidine’s and combinations thereof.
Vulcanizer can be selected from soluble or insoluble sulphur.
BRIEF DESCRIPTION OF DRAWINGS
Figure 1 represents the ATR FTIR spectra of a nano bio filler having at least 70% of silica content (40 Mesh) which is obtained from bamboo leaf extract which is derived from bamboo leaf ash.
Figure 2 represents the TEM image at 20 nm of a nano bio filler having at least 70% of silica content (40 Mesh) which is obtained from bamboo leaf extract which is derived from bamboo leaf ash.
Figure 3 represents the TEM image at 200 nm of a nano bio filler having at least 70% of silica content (40 Mesh) which is obtained from bamboo leaf extract which is derived from bamboo leaf ash.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Various embodiments of the disclosure are discussed in detail below. While specific implementations are discussed, it should be understood that this is done for illustration purposes only. A person skilled in the relevant art will recognize that other components and configurations may be used without parting from the spirit and scope of the disclosure. Thus, the following description and drawings are illustrative and are not to be construed as limiting. Numerous specific details are described to provide a thorough understanding of the disclosure. However, in certain instances, known details are not described in order to avoid obscuring the description.
References to one or an embodiment in the present disclosure can be references to the same embodiment or any embodiment; and such references mean at least one of the embodiments. Reference to "one embodiment", "an embodiment", “one aspect”, “some aspects”, “an aspect” means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the disclosure. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Moreover, various features are described which may be exhibited by some embodiments and not by others.
The terms used in this specification generally have their ordinary meanings in the art, within the context of the disclosure, and in the specific context where each term is used. Alternative language and synonyms may be used for any one or more of the terms discussed herein, and no special significance should be placed upon whether or not a term is elaborated or discussed herein. In some cases, synonyms for certain terms are provided.
A recital of one or more synonyms does not exclude the use of other synonyms. The use of examples anywhere in this specification including examples of any terms discussed herein is illustrative only and is not intended to further limit the scope and meaning of the disclosure or of any example term. Likewise, the disclosure is not limited to various embodiments given in this specification. Without intent to limit the scope of the disclosure, examples of instruments, apparatus, methods and their related results according to the embodiments of the present disclosure are given below. Note that titles or subtitles may be used in the examples for convenience of a reader, which in no way should limit the scope of the disclosure. Unless otherwise defined, technical and scientific terms are used. Herein have the meaning as commonly understood by one of ordinary skill in the art to which this disclosure pertains. In the case of conflict, the present document, including definitions, will be controlled.
Additional features and advantages of the disclosure will be set forth in the description which follows, and in part will be obvious from the description, or can be learned by practice of the herein disclosed principles. The features and advantages of the disclosure can be realized and obtained by means of the instruments and combinations particularly pointed out in the appended claims. These and other features of the disclosure will become more fully apparent from the following description and appended claims or can be learned by the practice of the principles set forth herein.
As mentioned before, there is a need for technology that overcomes these drawbacks associated with the prior arts. The present disclosure, therefore, also provides a tyre rubber composition containing a nano bio filler with not less than 70% of silica content which is obtained from bamboo leaf extract which is derived from with bamboo leaf ash is provided. Figure 1 describes the FTIR ATR spectra of a nano bio filler. The X-axis provides the absorption number. The Y-axis is labelled as "Percent Transmittance”. A small absorption peak at a wave number of 3401.58 cm-1, which represents the OH stretching vibrations from SiOH. Also, a sharp absorption peak at the wavenumber 1069.55 cm -1 indicates asymmetrical stretching vibration of Si–O–Si. The absorption peak at 1633.18 cm-1 indicates the Si-OH bending vibration in the silanol group. Furthermore, the absorption peaks at wave numbers 970.26 cm -1 corresponds to Si OH group and 797.38 cm-1, which represents the presence of Si-C group.
The present disclosure also provides a method for preparing the tyre rubber composition containing a renewable filler with not less than 70% of silica content which is obtained from bamboo leaf extract which is derived from with bamboo leaf ash is provided.
The present invention relates to diene based rubber composition containing a nano bio filler with not less than 70% of silica content (40 Mesh) which is obtained from bamboo leaf extract which is derived from bamboo leaf ash as a filler provides improved dynamic mechanical properties on rubber vulcanizate, and tyre made of using this tyre tread rubber composition improves the performance of the tyre on road surface.
The composition for tyre treads comprises elastomeric matrix; a nano bio filler with not less than 70% of silica content (40 Mesh) which is obtained from bamboo leaf extract which is derived from bamboo leaf ash carbon black or silica, combination of carbon black and silica; coupling agent; activators; anti-degradants; vulcanization agent; primary accelerator.
Table: 1 Tyre Tread Rubber Composition in phr

Ingredients Control (Comparative Example), C1 Formulation related to invention (Example), F1
SSBR 1 65.0 65.0
NdBR 2 15.0 15.0
NR, ISNR 20 3 30.0 30.0
Nano Bio filler, Bamboo leaf Extract (Silica not less than 70%) 4 - 5.0
Precipitated Silica 5 - -
Carbon Black, N234 6 70.0 65.0
Coupling Agent SI75 7 - 0.5
Zinc oxide 8 2.7 2.7
Stearic acid 9 1.7 1.7
LOW PCA OIL 10 4.0 4.0
MC WAX 11 1.4 1.4
6PPD 12 2.2 2.2
DPG 13 1.0 1.0
CBS 14 1.0 1.0
Sulphur 15 1.3 1.3
1. SSBR - HPR 355 HR is non-oil extended solution styrene butadiene rubber (SSBR) with 26 – 28 % of styrene content, 55.5 % to 59.5% of vinyl content and Tg of -21°C to -27°C (HPR 355 HR from JSR corporation).
2. NdBR: NDBR 40 Kumho NdBR is ultra-high cis polybutadiene rubber, produced by 1, 3-butadiene polymerization with a novel neodymium catalyst having more than 97% of 1,4-cis content and its glass transition temperature (Tg) is -100? from Kumho Petrochemical.
3. NR, ISNR 20-Indian Standard Natural Rubber ISNR 20 with the Mooney Viscosity, ML (1+4) at 100°C is 76 MU.
4. Nano bio filler: Bamboo leaf extract 70% of silica content which is derived from bamboo leaf ash Pore Volume – 1.07841, Pore diameter – 9.244 nm which implies the materials contains mesopores (Mesoporous materials have pore diameter between 2nm to 50 nm), external Surface area (statistical surface area) ranging from 308 to 318 m2/gm. A small absorption peak at a wave number of 3401.58 cm-1, which represents the OH stretching vibrations from SiOH. Also, a sharp absorption peak at the wavenumber 1069.55 cm -1 indicates asymmetrical stretching vibration of Si–O–Si. The absorption peak at 1633.18 cm-1 indicates the Si-OH bending vibration in the silanol group. Furthermore, the absorption peaks at wave numbers 970.26 cm -1 corresponds to Si OH group and 797.38 cm-1, which represents the presence of Si-C group. Particle size of bio nano filler is measured from TEM image and its diameter in the range of 62.4 nm to 107.7 nm.
5. Precipitated Silica - Madhu Silica pvt ltd, Gujarat having the specific surface area ranging from 165 to 180 m2/gm .
6. Carbon Black-ASTM Grade N234 from Himadri Carbon, India. It is the reinforcing filler HAF, High Abrasion Furnace having the Iodine adsorption No. 125 to 115 mg/gm, tinting strength value between 118 to 109 % ITRB, nitrogen surface area value between 114 to 124 m2/gm and COAN value ranges between 97 to 107 cc/100 gm.
7. Coupling agent - Si75 is a bifunctional, sulfur containing organosilane from Nanjing Shuguang Silane Chemical Co Ltd, China
8. Zinc oxide -It is used as an activator for the sulphur vulcanization of rubbers enhances the vulcanization efficiency and reduces the vulcanization time from Ambica Dhatu Private Limited, India.
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. MES oil– Mild Extracted Solvate or Low PCA oil is used to improve the processability of rubber compounds from IOCL Limited, India.
11. MC Wax- (Microcrystalline wax) from GPL, India
12. 6PPD (N-(1,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine) from Nocil Limited, India. It is added to the rubber composition to provide resistance to thermo-oxidative ageing of elastomers.
13. DPG – Diphenylguanidine - It is secondary accelerator, used to activate the primary accelerator) from PMC Rubber Chemicals India Pvt ltd, India.
14. 1CBS- (N-cyclohexyl-2-benzothiazolesulfenamide) It is a delayed action accelerator suitable for diene rubbers from Nocil Limited, India.
15. Sulphur is the vulcanizing agent from The Standard Chemical Co. Pvt Ltd, India.
Mixing Sequence:
Using a Banbury mixer with a tangential rotor, a rubber composition prepared by the thermomechanical process is as follows:
The method of preparation of the Rubber Composition includes the following:
Step I: Mixing has been done with the head temperature of the Banbury mixer maintained between 70 to 90°C and the unloaded rotor speed maintained between 55 to 65 rpm. The mixing cycle is to be followed as: a) Mixing chamber has been charged with rubbers and allowed to mix for 30 to 60 seconds. b) further reinforcing fillers and a nano bio filler having at least 70% of silica content which is from bamboo leaf extract, and it is derived from bamboo leaf ash are added and allow to mix it for 60 to 200 seconds. c) process of silanization is carried out with reduced rotor speed of 20 to 30 rpm. d) and further, rubber chemicals, process oil, stearic acid, MC wax (except zinc oxide and 6PPD) are added and allowed it to mix for time period of 100 to 300 seconds, e) sweeping has been done in the orifice and allowed it to mix for the time period of 100 to 320 seconds, the compound has been dumped at the temperature in the range of 145°C to 165°C and sheeted out in the laboratory two roll mill.
Step II: Add zinc oxide and 6PPD along with the step I master batch in the Lab Banbury Mixer and allowed to mix it for 80 seconds to 180 seconds and the compound has been dumped at the temperature in the range of 120°C to 155°C and sheeted out in the laboratory two roll mill.
Step III: Add step II master batch in the Lab Banbury Mixer and allow to mix it for 100 seconds to 220 seconds and the compound has been dumped at the temperature in the range of 120°C to 155°C and sheeted out in the laboratory two roll mill.
Preparation of Final Batch:
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 primary accelerator and sulphur as vulcanizing agent are allowed to mix for 60 to 100 seconds and the compound has been dumped at the temperature range of 95°C to 120°C. The final batch sheet out has been done in the laboratory two roll mill.
The compound properties are listed in Table 2 below.
Measurements and Tests:
The purpose of these tests is to measure the improved properties of the composition related to the invention against control composition. For this, a rubber composition F1 is prepared based on SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black and a nano bio filler, that is, silica obtained from bamboo leaf extract which is derived from bamboo leaf ash against SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black (C1) are prepared and evaluated.
The present invention provides a 100 parts by weight of rubber composition F1, a rubber composition F1 is prepared based on SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black and a nano bio filler, that is, silica obtained from bamboo leaf extract which is derived from bamboo leaf ash , t90 value lowers by 48.93 % (i.e., good) when compared to SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black (C1). In general, incorporation of silica filler in polymer matrix increases the t90. In the present invention, lower t90 is obtained with a nano bio filler containing compound which helps in improving the productivity of tyre manufacturing process and saves energy consumption.
The present invention provides a 100 parts by weight of rubber composition F1, a rubber composition F1 is prepared based on SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black and a nano bio filler, that is, silica obtained from bamboo leaf extract which is derived from bamboo leaf ash gave lowered E’ at -20 Deg C by 5.24 % (ie., good) which implies better winter traction when compared to SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black (C1).
The present invention provides a 100 parts by weight of rubber composition F1, a rubber composition F1 is prepared based on SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black and a nano bio filler, that is, silica obtained from bamboo leaf extract which is derived from bamboo leaf ash gave higher tan delta at -10 Deg C improved by 2.90% (ie., good) which implies better ice traction when compared to SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black (C1).
The present invention provides a 100 parts by weight of rubber composition F1, a rubber composition F1 is prepared based on SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black and a nano bio filler, that is, silica obtained from bamboo leaf extract which is derived from bamboo leaf ash gave higher tan delta at 0 Deg C improved by 2.67% (ie., good) which implies better wet traction when compared to SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black (C1).
The present invention provides a 100 parts by weight of rubber composition F1, a rubber composition F1 is prepared based on SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black and a nano bio filler, that is, silica obtained from bamboo leaf extract which is derived from bamboo leaf ash gave higher tan delta at 25 Deg C improved by 4.22% (ie., good) which implies better wet traction when compared to SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black (C1).
The present invention provides a 100 parts by weight of rubber composition F1, a rubber composition F1 is prepared based on SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend reinforced by carbon black and a nano bio filler, that is, silica obtained from bamboo leaf extract which is derived from bamboo leaf ash gave 69 Shore A.
Hence, SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend-based rubber composition containing a nano bio filler partially replaced with reinforcing filler carbon black gave improved winter traction, ice traction, wet and dry traction when compared to SSBR: NdBR: NR (65 phr: 15phr: 30 phr) blend-based rubber composition containing reinforcing filler carbon black. Also, a nano bio filler containing rubber compounds having capability to provide better productivity in tyre manufacturing process.
Table 2: Characterization of Rubber Vulcanizate
Properties Control, C1 F1, Formulation related to invention Index
M1. Hardness of a Rubber Vulcanizate
Hardness, Shore A 72 69 -
M2. Dynamic Mechanical Properties of the Rubber Vulcanizate
Winter traction, E’ -20 Deg C, Mpa (Lower the index value is better) 157.21 148.98 94.76
Ice Traction, tan delta at -10 Deg C (Higher the index value is better) 0.482 0.496 102.90
Wet Grip, tan delta at 0°C
(Higher the index value is better) 0.375 0.385 102.67
Dry Grip, tan delta at 25°C
(Higher the index value is better) 0.213 0.222 104.22
Rheological properties at 190 Deg C
t90, minutes: minutes
(Lower the cure time is better for productivity improvement) 2.33 1.14 48.93
M1. Shore A Hardness:
Shore A Hardness of the Rubber Vulcanizate is assessed in accordance with ASTM D 2240.
M2. Dynamic properties of the rubber vulcanizate:
The dynamic properties of the rubber vulcanizate are measured on a dynamic mechanical analyzer (DMA Metravib +1000) with a dynamic strain 0.3% and a static strain – 0.6% temperature sweep from - 40 to +80°C, frequency: 10Hz in tension mode as per ASTM D5992.
E’ at – 20 °C is commonly used as a predictor of tyre winter/snow traction. Lower the E’ value at -20°C, better the winter/snow traction.
Tan delta at -10°C is commonly used as a predictor of tyre ice traction. Higher the tan delta value at -10°C, better the ice traction.
Tan delta at 0°C is commonly used as a predictor of tyre wet traction. Higher the tan delta value at 0°C, better the wet traction.
M3. Rheological properties of rubber compound is measured in accordance with ASTM D 5289.
Advantages:
To reduce carbon footprint.
To provide improved winter traction/snow traction along with ice traction, wet traction along with dry traction.
To provide a nano bio filler obtained from renewable resources to replace reinforcing carbon black filler.
To provide high performance motorcycle tyre tread rubber composition.

The implementation set forth in the foregoing description does not represent all implementations consistent with the subject matter described herein. Instead, they are merely some examples consistent with aspects related to the described subject matter. Although a few variations have been described in detail above, other
modifications or additions are possible. In particular, further features and/or variations can be provided in addition to those set forth herein. For example, the implementation described can be directed to various combinations and sub combinations of the disclosed features and/or combinations and sub combinations of the several further features disclosed above. In addition, the logic flows
depicted in the accompany figures and/or described herein do not necessarily require the particular order shown, or sequential order, to achieve desirable results. Other implementations may be within the scope of the following claims.
,CLAIMS:A tyre rubber composition, comprising:
An elastomeric matrix: 100 parts by weight (phr), consisting of:
-Solution styrene-butadiene rubber (SSBR): 50-90 phr, selected based on Tg values ranging from -21°C to -50°C, and
-Neodymium catalyzed polybutadiene rubber (NdBR): 10-50 phr;
- Natural rubber:10-30 phr;
-Nano bio filler: 1-20 phr, having at least 70% silica content, derived from bamboo leaf extract obtained from bamboo leaf ash, with a particle size passing through a 40-mesh sieve, a specific surface area ranging from 364.30 to 369.30 m²/g; particle size of diameter in the range of 62.4 nm to 107.7 nm
-Reinforcing fillers: 10-80 phr, selected from carbon black and/or silica,
wherein Carbon black is present in the range of 20-70 phr
-Silica is present in the range of 0-40 phr;
-Coupling agent: 0.5-4 phr;
-Activators: 2-8 phr, comprising zinc oxide and stearic acid;
-Process oil: 2-8 phr;
-Anti-degradants: 0.5-5 phr;
-Vulcanization agent: 1.0-3 phr, and
-Accelerators: 1.0-2.5 phr, selected from sulfenamides and guanidines, thiazoles, or thiuram sulfides.
2. The tyre rubber composition as claimed in claim 1, wherein the process oil is selected from MES oil, TDAE oil, or RAE oil in the range of 2-8 phr.
3. The tyre rubber composition as claimed in claim 1, wherein the coupling agent comprises a silane, such as Si75: 0.5-4 phr.
4.The tyre rubber composition as claimed in claim 1, wherein the anti-degradants are selected from amine types, phenolic types, or a combination thereof, preferably 6PPD: 1-2 phr, and microcrystalline wax: 0-2 phr.
5. The tyre rubber composition as claimed in claim 1, wherein the vulcanization agent is selected from soluble or insoluble sulfur: 1-3 phr.
6. The tyre rubber composition as claimed in claim 1, wherein the accelerator is selected from sulfenamides and guanidines.
7. The tyre rubber composition as claimed in claim 1, wherein the reinforcing filler carbon black having the Iodine adsorption No. 125 to 115 mg/gm, tinting strength value between 118 to 109 % ITRB, nitrogen surface area value between 114 to 124 m2/gm and COAN value ranges between 97 to 107 cc/100 gm and the reinforcing filler silica having the specific surface area ranging from 85 to 180 m2/gm.
8. A method for preparing the tyre rubber composition, comprising:
Preparation of Master Batch:
Step I as Mixing elastomers, including solution styrene-butadiene rubber (SSBR) and polybutadiene rubber (NdBR) and natural rubber for 30- 60 secs, further adding a nano bio filler containing at least 70% silica, derived from bamboo leaf extract obtained from bamboo leaf ash, and reinforcing fillers such as carbon black and/or silica in a Banbury mixer;
Maintaining the head temperature between 70°C and 90°C, rotor speed at 55-65 rpm, and mixing for 60-200 seconds;
Conducting silanization of the nano bio filler and coupling agent silane by reducing the rotor speed to 20-30 rpm and further adding rubber chemicals, process oil, stearic acid, MC wax (except zinc oxide and 6PPD) are added continuing mixing for 100-300 seconds, sweeping has been done in the orifice and allowed it to mix for the time period of 100 to 320 seconds, the compound has been dumped at the temperature in the range of 145°C to 165°C and sheeted out in the laboratory two roll mill.
Step II: Adding zinc oxide and 6PPD along with the step I master batch in the Banbury Mixer and allowed to mix it for 80 seconds to 180 seconds and the compound has been dumped at the temperature in the range of 120°C to 155°C and sheeted out in the laboratory two roll mill.
Step III: Adding step II master batch in the Banbury Mixer and allow to mix it for 100 seconds to 220 seconds and the compound has been dumped at the temperature in the range of 120°C to 155°C and sheeted out in the laboratory two roll mill.
Dumping the batch at a temperature range of 145°C to 165°C and sheet-out using a two-roll mill.
Preparation of Final Batch:
Mixing the master batch rubber compound prepared in Step 3 with curatives, including primary accelerators (e.g., CBS) and vulcanization agents (e.g., sulfur), in a Banbury mixer;
Maintaining the temperature between 95°C and 120°C and mixing for 60-100 seconds and dumping the final batch rubber compound and sheet-out in a laboratory two-roll mill.