Abstract: The disclosed is a tire tread rubber composition includes elastomers of 100 parts, containing reinforcing filler carbon black ranging from 0 – 60 phr is replaced with biomass derived reinforcing renewable filler sugarcane bagasse ash ranging from 5- 60 phr to provide high rubber elasticity, lower rolling resistance along with better processing properties or biomass derived reinforcing renewable filler sugarcane bagasse ash is used along with reinforcing filler carbon black is to provide better wet grip and dry grip along with better processing properties. The present disclosure also relates to a method of preparation of the tire tread rubber composition.
DESC:TECHNICAL FIELD
The present disclosure relates to the field of tyre. More particularly, the present disclosure relates to reinforcing renewable filler derived from biomass containing tyre tread rubber composition and its method for preparation.
BACKGROUND
Currently marketed tires are manufactured from materials derived from petroleum resources such that these materials account for half or more of the total weight of the tire. For example, common radial tires for passenger cars contain, based on the total weight of the tire, about 20% of synthetic rubber and about 20% of carbon black as well as aromatic oil and synthetic fibers. Thus, they contain at least 50% of petroleum-derived materials as a whole.
The recent emphasis on the environmental issues, however, has led to tighter CO2 emission restrictions. Moreover, since petroleum raw material is a limited resource and the amount of the material supplied is decreasing year by year, oil prices are expected to escalate in the future and thus the use of petroleum-derived materials has a limit.
Hence, the people's desire to construct a sound material-cycle society has recently become stronger. Accordingly, there is a need for a departure from fossil fuel dependence in the material field as well as in the energy field, and the use of biomass has been focused on.
WO2015054685 discloses rubber composites containing macro, micro and nano-sized fillers made from agricultural, industrial, and food processing wastes, methods of making the same, and articles fabricated there from. The referred patent discusses about the use of agricultural, industrial waste and processing waste as filler in the rubber composite.
EP2861655 discloses methods for the removal of organic solvents from wet bagasse. The use of the method results in dried bagasse that contains no more than one weight percent organic solvents. The referred patent discusses about the method for removal of organic solvents from wet bagasse.
IN202027045216 discloses a polymer composition may include elastomeric ethylene-vinyl acetate, in which at least a portion of ethylene from the elastomeric ethylene-vinyl acetate is obtained from a renewable source of carbon. The referred patent discusses about the process of producing the polymer composition in EVA (ethylene vinyl acetate) with a renewable source of carbon.
IN202117023066 discloses a rubber composition with an excellent grip force; a method of producing the rubber composition; a shoe sole, a shoe, and a tire each using the rubber composition; and a method of improving a frictional force of a rubber component. The referred patent discusses about the use of rubber composition with lignin and specified amine compound in shoe sole in order to improve the frictional force of the component.
US2019185645 discloses a pneumatic tire that provides a balanced improvement of abrasion resistance, wet grip performance, and fuel economy. The referred patent discusses about the method of preparation of copolymers, its polymerization technique and experimental carbon black process set parameters and its process, method of preparation of zinc carrier. The composition of the rubber component that contains aromatic vinyl - conjugated diene copolymer with different molecular weight having Tg more than 10 deg C with the styrene content 40% by mass and vinyl bond content 24% by mass, 0-70% by mass of an isoprene-based rubber along with experimental carbon black and silica with different surface area for a balanced improvement of abrasion resistance, wet grip performance and fuel economy.
US2019185644 discloses the method of preparation of copolymers, its polymerization technique and experimental carbon black process set parameters and its process, method of preparation of zinc carrier. The rubber composition containing the copolymer containing aromatic vinyl units and conjugated diene units, 1 to 90% by mass of the copolymer (copolymers- aromatic vinyl - conjugated diene copolymer with different molecular weight having Tg more than 10 deg C with the styrene content 40% by mass and vinyl bond content 24% by mass) and 0 to 40% by mass of an isoprene-based rubber. Also, the rubber composition containing 10 parts by mass or more of the silica per 100 parts by mass of the rubber component along with experimental carbon black and silica with different surface area for a balanced performance of wet grip and fuel economy.
US2019185643 discloses the method of preparation of copolymers, its polymerization technique and experimental carbon black process set parameters and its process, method of preparation of zinc carrier. The rubber composition containing the copolymer containing aromatic vinyl units and conjugated diene units, 1 to 90% by mass of the copolymer (copolymers- aromatic vinyl - conjugated diene copolymer with different molecular weight having Tg more than 10 deg C with the styrene content 40% by mass and vinyl bond content 24% by mass) , 20-64% by mass of the high-cis polybutadiene rubber, and 35-60% by mass of the isoprene-based rubber, the rubber composition containing 5 parts by mass or more of the silica per 100 parts by mass of the rubber component for a balanced improvement of abrasion resistance, grip performance on ice and fuel economy.
US2019184746 discloses the composition of the rubber component that contains 1-60% by mass of the copolymer and 0-99% by mass of an isoprene-based rubber, the rubber composition containing 10 parts by mass or more of the silica per 100 parts by mass of the rubber component for a balanced improvement of abrasion resistance, wet grip performance, and fuel economy in a pneumatic tyre.
US2019184745 discloses the composition of the rubber component based on 100% by mass thereof, based on 100% by mass thereof, 10% by mass or more of the copolymer, the rubber composition containing 10 parts by mass or more of the silica per 100 parts by mass of the rubber component for a balanced improvement of tensile strength and fuel economy in pneumatic tire.
US2019169314 discloses the resin composition blended with modified cellulose fibers for various industrial applications and household electric appliance’s part.
US2019134930 discloses a sealant composition for use with tires, a tire having at least one component with at least one surface at least partially coated with the sealant composition, and related methods for applying the sealant composition to tires. The referred patent discusses about the use of sealant composition in which bio-rubber and a softener (plant resin) is used.
US2019100643 discloses a tire assuring that variation with time of hardness is inhibited and ride comfort performance can be maintained for a long period of time. The tire is provided with a tread composed of a rubber composition comprising 2 to 20 parts by mass of a liquid farnesene resin and 10 to 150 parts by mass of silica based on 100 parts by mass of a rubber component, wherein a total content of the liquid farnesene resin and a plasticizer is 2 to 100 parts by mass. The referred patent discusses about the performance of tire ride comfort for a longer period of time with the use of liquid farnesene resin with silica.
US2018244806 discloses rubber composition containing a rubber and modified cellulose fibers, wherein one or more substituents selected from substituents represented by the following general formulas (1) and (2): —CH2—CH(OH)—R1 (1), —CH2—CH(OH)—CH2—(OA)n—O—R1 (2), wherein each R1 in the general formulas (1) and (2) is independently a linear or branched alkyl group having 3 or more carbon atoms and 30 or less carbon atoms; n in the general formula (2) is a number of 0 or more and 50 or less; and A is a linear or branched, divalent saturated hydrocarbon group having 1 or more carbon atoms and 6 or less carbon atoms are bonded to cellulose fibers via an ether bond, wherein the modified cellulose fibers have a cellulose I crystal structure. The referred patent discusses about the resin composition blended with modified cellulose fibers for various industrial applications and household electric appliance’s part.
US3734766 discloses treating bagasse with an aqueous solution of alum and defibrated to give a fibrous product suitable for the reinforcement of resin bodies. The fiber can also be pulverized to yield a flour suitable for use as a filler in resin bodies. The referred patent discusses about the use of pulverized filler of bagasse in resin bodies for the application of insulation and acoustical materials.
US2015126698 discloses rubber compositions for tires capable of providing tire components and pneumatic tires having low-temperature properties and abrasion resistance that are equivalent to those of tire components and pneumatic tires formed from conventional synthetic rubber, respectively, while meeting the demand for a sound material-cycle society. The referred patent discusses about the rubber composition for tires containing a biomass derived rubber capable of providing low temperature properties and abrasion resistance similar to the conventional synthetic rubber.
US2015148458 discloses rubber compositions for tires capable of providing tire components and pneumatic tires having low-temperature properties and abrasion resistance that are equivalent to those of tire components and pneumatic tires formed from conventional synthetic rubber, respectively, while meeting the demand for a sound material-cycle society. The referred patent discusses about the production method of polysaccharide fibers to suppress the carbon disulphide emissions and the tire containing these fibers has good tire characteristics.
US2016009877 discloses a method for manufacturing a rubber composition, which method can give a rubber composition provided with excellent reinforcement properties by improving the dispersibility of fibers in a rubber component when the fibers are added to the rubber, a rubber composition obtained using this method, a vulcanized rubber, and a tire. The referred patent discusses about the use of short fibers (cellulose nano fibers) and its method of dispersion in the rubber composition for attaining the better reinforcement.
US2015266988 discloses a rubber compositions for tires capable of providing tire components and pneumatic tires that have the same level of fuel efficiency and wet grip performance (particularly, wet grip performance) as those of tire components and pneumatic tires containing conventional synthetic rubber, while satisfying the requirements for a sound material-cycle society. The referred patent discusses about the biomass derived rubber that is polymerized from aromatic vinyl compound and a diene and has a PMC (percent modern carbon) to provide same level fuel efficiency and wet grip performance.
US2016168757 discloses process for producing purified polysaccharide fiber of the present disclosure includes bringing a polysaccharide solution, which is obtained by dissolving a polysaccharide raw material in a liquid containing an ionic liquid, into contact with a solidification liquid containing an ionic liquid, and performing dry-wet spinning on polysaccharide, in which the concentration of the ionic liquid in the solidification liquid is 0.4% by weight to 70% by weight, and a distance D from a site where the polysaccharide solution is extruded in the form of fiber to a site where the extruded polysaccharide solution comes into contact with the solidification liquid is 50 mm to 120 mm The referred patent discusses about the production method of polysaccharide fibers to suppress the carbon disulphide emissions and the tire containing these fibers has good tire characteristics.
US2016122515 discloses an automotive tire containing from 0.1 wt % to 50 wt % hydrophobic nanocellulose. Hydrophobic nanocellulose may include lignin-coated nanocellulose and/or a chemically modified surface to increase hydrophobicity. The referred patent discusses the use of lignin coated nanocellulose which is chemically modified to increase the hydrophobicity for the various tire components.
US2017253740 discloses lignin derivative extracted from biomass and used for rubber reinforcement or used in a molding material. The referred patent discusses about the use of lignin resin in the rubber composition for better tensile properties and good low hysteresis loss.
US2017137599 discloses a rubber composition that shows a balanced improvement in fuel economy and abrasion resistance while having good processability, and a pneumatic tyre formed from the rubber composition. The referred patent discusses about the rubber composition containing a structural unit derived from a conjugated diene monomer, a structural unit derived from a conjugated diene monomer, a structural unit derived from a conjugated diene monomer, a structural unit derived from farnesene provides balanced improvement in fuel economy and abrasion resistance.
US2013090445 discloses a synthesis system that can synthesize aniline and/or styrene efficiently, a synthesis system that can synthesize butadiene (1,3-butadiene) efficiently, a rubber chemical for a tire which is synthesized from the aniline obtained by the synthesis system, a synthetic rubber for a tire which is synthesized from the styrene and/or butadiene obtained by the synthesis systems, and a pneumatic tire produced using the rubber chemical for a tire and/or the synthetic rubber for a tire. The referred patent discusses about the synthesis of rubber chemicals from the aniline obtained by the synthesis system and a pneumatic tyre produced using these rubber chemicals are capable to provide comparable wet grip performance, abrasion resistance, dry grip performance and rolling resistance.
US2009062433 discloses a rubber composition that attains both low heat generating property and high reinforcement property simultaneously at high levels, is capable of attaining low fuel consumption through the tire, is excellent in durability, and is good in workability and surface property. The referred patent discusses about the NR: BR (60: 40) blend rubber composition rubber composition with bagasse charcoal (incomplete combustion) as filler along with carbon black and silica reinforcing fillers to provide lower rolling resistance.
US2016194484 discloses a pneumatic tire having high productivity and achieving a balanced improvement in fuel economy, rubber strength, abrasion resistance, wet-grip performance, and handling stability. The referred patent discusses about the improved performance of tire with the use of farnesene resin along with silica in the styrene butadiene, polybutadiene and polyisoprene blend based rubber composition.
N109181038 discloses a preparation method for a modified white carbon black tread rubber and belongs to the technical field of preparation of tire materials. The referred patent discusses about the modified white carbon black (using bagasse as a raw material) in tread rubber composition as an advantage of low sliding resistance, high crack resistance and wide application prospect.
GB721205 discloses a bend for use in furniture, radio cabinets or the like comprises a radially-continuous bent filler piece three of an easily-bendable material, extending at least around the curve and preferably to some distance on either side, and an outer layer six glued to the filler piece and extending beyond it and into union with the timber side-pieces one on either side of the bend, the filler piece being of substantially the same thickness as the side-pieces. The referred patent discusses about the use of adhesives and natural fillers in the field of multi layered composites.
GB560492 discloses the use of lignin coated nanocellulose which is chemically modified to increase the hydrophobicity for the various tire components.
CA1318741 discloses the use of sustainable materials like bagasse, peat moss, cane trash, olive pulp and coffee bean waste in the rubber product as filler. It is mainly discussed about the fly ash or furnace ash obtained from bagasse and it is used as an additive in NBR based O ring rubber composition i.e., automotive sealing application.
IN201917016465 discloses a shoe sole rubber composition using a specific lignin degradation product as an anti-ageing agent is having ability to provide excellent grip force in both wet and dry conditions.
IN10349/DELNP/2014 discloses the production method of polysaccharide fibers to suppress the carbon disulphide emissions and the tire containing this fiber rubber complex has good tire characteristics.
IN10754/DELNP/2015 discloses the production method of polysaccharide fibers to suppress the carbon disulphide emissions and the tire containing this fiber rubber complex has good tire characteristics.
IN201717016883 discloses the use of lignin coated nanocellulose which is chemically modified to increase the hydrophobicity for the various tire components.
IN2896/KOLNP/2012 discloses the synthesis of rubber chemicals from the aniline obtained by the synthesis system and a pneumatic tire produced using these rubber chemicals are capable to provide comparable wet grip performance, abrasion resistance, dry grip performance and rolling resistance.
The article entitled “Potential of carbonized bagasse filler in rubber products” by Journal of Emerging Trends in Engineering and Applied Sciences Vol. 1, No. 2. The technical paper discusses about the use of carbonized bagasse in natural rubber composite for the improvement of physical properties like tensile strength, compression set, hardness and elongation at break and it can be used as an alternative filler material in natural rubber to provide low cost.
The article entitled “Sugarcane bagasse fiber as semi-reinforcement filler in natural rubber composite sandals” by Journal of Material Cycles and Waste Management volume 21, pages 326–335 (2019). The technical publication discusses about the use of bagasse fibers in the footwear application where the bagasse fibre is treated with the alkali for the better incorporation in the rubber composites to provide better mechanical properties.
The article entitled “Sugarcane bagasse ash: new filler to natural rubber composite:” by Polímeros 24 (6) Dec 2014. The referred patent discusses about the use of bagasse ash in the rubber composite with a blend of NR/SBA in which the SBA (sugarcane bagasse ash) is prepared in open cylinder with the vulcanization agents for better reinforcing to achieve good mechanical properties.
The article entitled “Potential eco-friendly application of sugarcane bagasse ash in the rubber industry” Published 3 January 2021; Materials Science; Waste and Biomass Valorization. The referred patent discusses about the use of sugarcane bagasse ash in natural rubber with the use of coupling agent (TESPT) and thiuram as the curing alternative system for better physical properties.
Hence there is a need for low-cost, biomass derived reinforcing renewable filler sugarcane bagasse ash for use in rubber compounds that equal or surpass the performance of current carbon-based fillers and lowers the rolling resistance.
Therefore, there is a need for a biomass-derived tyre tread rubber composition that provides lower rolling resistance along with better processing.
OBJECTS OF THE DISCLOSURE:
The principal object of the present disclosure is to provide a biomass derived tyre tread rubber composition and its method of preparation.
Another object of the present disclosure is to provide a tyre tread rubber composition using biomass derived reinforcing renewable filler sugarcane bagasse ash and its method of preparation.
Another object of the present disclosure is to use biomass derived reinforcing renewable filler sugarcane bagasse ash as a replacement of reinforcing filler carbon black or addition of biomass derived reinforcing renewable filler sugarcane bagasse ash along with reinforcing filler carbon black.
Yet another object of the present disclosure is to eliminate/reduce the carbon footprint in the environment with sustainable approach.
Yet another object of the present disclosure is to provide a tyre tread composition having lower rolling resistance along with better processing properties.
Yet another object of the present disclosure is to provide lower hysteresis in the tire treads.
Yet another object of the present disclosure is to provide better wet grip and dry grip in tyre treads.
Yet another objection of the present disclosure is to provide lower rolling tyre tread compound for two wheeler application.
SUMMARY OF THE DISCLOSURE:
In one aspect of the present disclosure, a tire tread rubber composition is provided.
The composition includes elastomers – 100 parts per hundred (phr). The composition further includes reinforcing filler ranging from 0 – 60 phr. The composition further includes reinforcing renewable filler ranging from 5- 60 phr. The composition further includes coupling agent X50S ranging from 0 – 9.6 phr. The composition further includes process aid ranging from 0 – 40 phr. The composition further includes struktol 40MS ranging from 0.5 – 2 phr. The composition further includes cure activators ranging from 0.5 – 5 phr. The composition further includes anti-degradants ranging from 1-4 phr. The composition further includes vulcanization agent ranging from 1.2 – 1.7 phr. The composition further includes accelerator ranging from 0.5- 1.2 phr, wherein the reinforcing renewable filler is sugarcane bagasse ash.
It is another aspect of the present disclosure to provide a tyre tread rubber composition using reinforcing renewable filler, such that the elastomers is ranging from 70 – 100 parts of natural rubber and 0 – 30 parts of neodymium catalyst polymerized polybutadiene rubber.
It is another aspect of the present disclosure to provide a tyre tread rubber composition using reinforcing renewable filler, such that the elastomers is 70 – 100 parts of emulsion polymerized non-oil extended styrene butadiene rubber and 0 –30 parts of neodymium catalyst polymerized polybutadiene rubber.
It is another aspect of the present disclosure to provide a tyre tread rubber composition using reinforcing renewable filler, such that the reinforcing filler is carbon black having iodine surface area value ranges from 77 m2/gm to 87 m2/gm, oil absorption number value ranges from 97 cc/100 gm to 107 cc/100 gm, tinting strength values ranges from 99 to 109 % ITRB.
It is another aspect of the present disclosure to provide a tyre tread rubber composition using reinforcing renewable filler, such that the process aid is mild extract solvate (MES) oil.
It is another aspect of the present disclosure to provide a tyre tread rubber composition using reinforcing renewable filler, such that the cure activators are zinc oxide and stearic acid, in a weight ratio of 1- 3.5 phr: 0.5 – 1.5 phr.
It is another aspect of the present disclosure to provide a tyre tread rubber composition using reinforcing renewable filler, such that the anti-degradants are MC wax and 6PPD, in a weight ratio of 1- 2 phr: 1- 2 phr.
It is another aspect of the present disclosure to provide a tyre tread rubber composition using reinforcing renewable filler, such that the vulcanization agent is sulphur.
It is another aspect of the present disclosure to provide a tyre tread rubber composition using reinforcing renewable filler, such that the accelerator is CBS.
It is another aspect of the present disclosure to provide a tyre tread rubber composition using reinforcing renewable filler, such that the coupling agent X50S is a blend of the bifunctional, sulfur containing organo silane coupling agent Si69 and N330 type carbon black in the ratio 1:1 by weight. The coupling agent X50S enhance the polymer filler interaction.
In second aspect of the present disclosure, a method for preparation of a tire tread rubber composition containing sugarcane bagasse ash as biomass derived reinforcing renewable filler is provided.
Master Batch Stage 1: The method includes adding elastomers, reinforcing renewable filler, coupling agent X50S and 50% of carbon black in the Banbury mixer chamber is allowed to mix. The method further includes mixing ingredients in the chamber of Banbury by maintaining a temperature of the chamber between 120°C-125°C and ram pressure maintained between 4.5 to 6.0 kP/cm2. The method further includes additionally adding stearic acid, MC wax, Struktol 40MS, and the remaining 50% of carbon black in the chamber of Banbury mixer is allowed to mix. The method further includes mixing of ingredients in Banbury mixer by maintaining chamber temperature between 140°C-145°C. The method further includes allowing the mixture to silanization process for a time period of 20 to 30 seconds at a maintained rotor speed of 20 rpm. The method further includes reducing the rotor speed to 16 rpm and allowing to mix the ingredients in the Banbury mixer for a period of 30 to 40 seconds. The method further includes increasing rotor speed at a maintained range between 45-60rpm and allowing the ingredients to mix in the Banbury mixture for a period of 20-30 seconds. The method further includes dumping the rubber compound at a temperature up to 160°C to obtain a first rubber compound. The method further includes maintaining the first rubber compound for maturation for a period of 6-8 hours.
Master batch Stage 2: The method further includes adding zinc oxide and 6PPD to the obtained rubber compound. The method further includes allowing to mix the ingredients in the Banbury mixer for a period of 120 seconds. The method further includes dumping the rubber compound at a temperature maintained between 150°C-160°C to obtain a second rubber compound. The method further includes sheeting out the obtained second rubber compound in the two roll mills by maintaining the rotor speed between 50-60 rpm and rotor temperature maintained between 55°C to 65°C. The method further includes maintaining the second rubber compound for maturation for a period of 4-6 hours.
Final Batch: The method further includes adding cure chemicals vulcanizer Sulphur and accelerator CBS to the second rubber compound and mixing ingredients in the Banbury mixer for a period of 120 – 140 seconds by a maintained rotor speed between 25-45 rpm. The method further includes maintaining the chamber temperature between 100°C-105°C and ram pressure maintained between 4.0 to 4.5 kP/cm2. The method further includes dumping the rubber and sheeting out using two roll mill.
BRIEF DESCRIPTION OF DRAWINGS
The accompanying drawings, which are incorporated in and constitute a part of this specification, show certain aspects of the subject matter disclosed herein and, together with the description, help explain some of the principles associated with the disclosed implementations. In the drawing,
Figure 1 illustrates SEM image that depicts morphology of Sugarcane Bagasse Ash as biomass-derived reinforcing filler aggregates and its nature of porosity at 10 µm magnification, in accordance with an aspect of the present disclosure;
Figure 2 illustrates SEM image that depicts the morphology of Sugarcane Bagasse Ash as biomass-derived reinforcing filler aggregates and its nature of porosity at 100 µm magnification, in accordance with an aspect of the present disclosure;
Figure 3 illustrates TEM image that depicts the particle shape and size of Sugarcane Bagasse Ash as biomass-derived reinforcing filler at 50 nm, in accordance with an aspect of the present disclosure; and
Figure 4 illustrates TEM image that depicts the particle shape and size of Sugarcane Bagasse Ash as biomass derived reinforcing filler at 100 nm, in accordance with an aspect of the present disclosure.
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 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 control.
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.
The term “Phr” abbreviates as “Parts per hundred rubber” and is interchangeably used across the context.
As mentioned before, there is a need for technology that overcomes these drawbacks by enhancing lower rolling resistance of the rubber composition. The present disclosure aims to addresses the aforementioned needs by providing a biomass-derived tyre tread rubber composition that incorporates Sugarcane bagasse ash as a biomass derived reinforcing renewable filler, along with various other components.
The present disclosure relates to the tyre tread rubber composition and its method of preparation to provide lower rolling resistance along with better processing properties. Sugarcane bagasse ash as a biomass derived reinforcing renewable filler is used in tyre tread rubber composition which provide lower rolling resistance along with better processing properties.
The use of bagasse ash (complete combustion) as a reinforcing renewable filler in a tire tread rubber composition containing blend of NR: PBR or ESBR: PBR blend based rubber composition to provide low rolling resistance along with better processing properties. The biomass derived reinforcing filler sugarcane bagasse ash without any chemical modification is used in tyre tread rubber composition to provide lower rolling resistance along with better processing properties.
The composition comprises an elastomeric matrix; reinforcing filler carbon black; activators; anti-degradants; vulcanization agent; primary accelerators; process aid; biomass derived reinforcing renewable filler sugarcane bagasse ash.
The present disclosure relates to the tire tread rubber composition having lower rolling resistance by using biomass derived reinforcing renewable filler sugarcane bagasse ash in the tread rubber composition and its method thereof.
The present disclosure comprising 70 to 100 parts of natural rubber, and neodymium catalyst polymerized polybutadiene rubber comprising 0 to 30 parts is used. Emulsion polymerized non-oil extended styrene butadiene rubber of 70 to 100 parts and neodymium catalyst polymerized polybutadiene rubber comprising 0 to 30 parts is used. Reinforcing filler, ASTM grades of carbon black having iodine adsorption No.85 to 95 mg/gm is used.
Biomass derived reinforcing renewable filler sugarcane bagasse ash a residue obtained from the burning of bagasse in the sugar industry. It is a renewable and biodegradable filler. The chemical composition of sugarcane bagasse ash having elements mainly in the weight percentage of carbon – 43.13%, oxygen -38.25%, Silicon -7.61% and other elements like magnesium, aluminium, sulfur, potassium, calcium, phosphorous, iron is in the weight percentage range between 0.5% to 3.45% and the said values are obtained from SEM EDAX TEAM measurement. Also, SEM (Figure 1 & 2) image shows the presence of Sclerenchyma tissue i.e., dead cells with lignified walls (i.e., lignin) in the sugar bagasse ash which gives protection to the rubber matrix against degradation processes during mixing at high mechanical and thermo-oxidative stresses.
As the inorganic biomass derived renewable reinforcing filler sugarcane bagasse ash is used in the tyre tread rubber composition, a suitable coupling agent X50S is used to enhance better polymer to filler interaction. It is a blend of the bifunctional, sulfur containing organo silane coupling agent Si69 and N330 type carbon black in the ratio 1:1 by weight.
MES oil (Mild extract solvate) oil is used as a processing aid in the tyre tread rubber composition, and it act as a plasticizer in the tyre tread rubber composition to reduce viscosity, better filler dispersion and to improve processing characteristics. Struktol 40MS improves the homogeneity of elastomers.
Zinc oxide and Stearic acid acts as an activator in the rubber composition. It activates the rubber composition for the vulcanization process and acts as mold release agent in-situ to the rubber composition. 6PPD [N-(1,3-Dimethylbutyl)-N’-phenyl-p-phenylenediamine-quinone] is an antidegradant which acts as an antioxidant and an antiozonant for natural and synthetic polymers. Microcrystalline Wax is used as an antiozonant in the tyre tread rubber composition.
Soluble Sulphur is used for the rubber composition for the vulcanization process. CBS [N-Cyclohexyl-2-benzthiazole sulphenamide] is added as an accelerator in the rubber composition, to accelerate the vulcanization process in the rubber composition.
Table 1: Rubber composition in phr
Ingredients Control, C1 Formulation related to disclosure
F1, phr F3, phr F4, phr
NR1 80.00 80.00 80.00 80.00
SBR 15022 - - - -
PBR-Nd3 20.00 20.00 20.00 20.00
Carbon black 4 60.00 45.00 25.00 -
Bagasse ash5 - 15.00 35.00 60.00
X50S6 - 2.40 5.60 9.60
MES Oil7 5.00 5.00 5.00 5.00
Struktol 40MS8 2.00 2.00 2.00 2.00
Zinc oxide9 3.00 3.00 3.00 3.00
Stearic acid10 1.50 1.50 1.50 1.50
MC Wax11 2.00 2.00 2.00 2.00
6PPD12 2.00 2.00 2.00 2.00
Sulphur13 1.50 1.50 1.50 1.50
CBS14 1.00 1.00 1.00 1.00
Total, Phr 178.00 180.40 183.60 187.60
Table 2: Rubber composition in phr
Ingredients Control
Formulation related to disclosure
C2 F2, phr
NR1 - -
SBR 15022 80.00 80.00
PBR-Nd3 20.00 20.00
Carbon black 4 50.00 50.00
Bagasse ash5 - 50.00
X50S6 - 8.00
MES Oil7 5.00 30.00
Struktol 40MS8 2.00 2.00
Zinc oxide9 3.00 3.00
Stearic acid10 1.50 1.50
MC Wax11 2.00 2.00
6PPD12 2.00 2.00
Sulphur13 1.50 1.50
CBS14 1.00 1.00
Total, Phr 168.00 251.00
Ingredients used in rubber compounding (Table 1 & 2) is as follows:
1. “NR - Indian Standard Natural Rubber, ISNR 20 grade” is from Alpharub Trading and Manufacturing Private Ltd., India.
2. “SBR 1502 – Emulsion polymerized non-oil extended styrene butadiene rubber” is from Reliance Industries, India.
3. “PBR-Nd – Neodymium catalyst polymerized polybutadiene rubber” is from Kumho Petrochemical Co. Ltd., SEOUL, Korea and It is an ultra-high cis polybutadiene rubber grade. It is produced by 1, 3-butadiene polymerization with a novel neodymium catalyst.
4. “Carbon black – ASTM grade N330 Carbon black” is from Epsilon Carbon private Limited, India.
5. “Bagasse Ash - Biomass derived reinforcing renewable filler” is obtained from sugarcane bagasse ash. Sugarcane bagasse ash (SCBA) is a residue obtained from the burning of bagasse in the sugar industry. It is from Sree Ram Agencies New No. 51b, (Old No. 1b) Palmal Cross Street, Near Mahal South, Madurai-625 001. Tamilnadu.
6. “Coupling agent X50S” is a blend of the bifunctional, sulfur containing organo silane coupling agent Si69 and N330 type carbon black in the ratio 1:1 by weight is from Evonik India Private Limited, India
7. “MES Oil – Mild extract solvate (MES)” is a process aid, which is purchased from Indian Oil Corporation Ltd, India.
8. “Struktol 40MS” is a homogenizer used to improve the homogeneity of elastomers is from Lanxess India Private Limited, India.
9. “Zinc oxide” which acts as an activator of the vulcanization of the rubber compound is from POCL Enterprises Ltd., India
10. “Stearic acid” is used as a Process aid is from 3F Industries Limited, Andhra Pradesh. 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.
11. “MC Wax - Microcrystalline wax” is used to protect against degradation by ozone from Gujarat Parafins pvt ltd., India.
12. “6PPD-(N-(1,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine)” is an antidegradant and added to the rubber composition to provide resistance to thermo-oxidative ageing of elastomers is from Lanxess India Private Limited.
13. “Sulphur” is purchased from Southern Minerals and Chemicals, Kerala. It is a vulcanizing agent
14. “CBS- N-cyclohexyl-2-benzothiazolesulfenamide”, is a delayed action accelerator, is from PMC Rubber Chemicals India Private Limited, West Bengal, India.
The method of preparing rubber compositions includes following:
Mixing Sequence:
Banbury mixer (Internal Mixer) with tangential rotor of capacity 2 liters is used for mixing of rubber compound and two roll mill is used for rubber compound sheeting out purpose. These are the two polymer mixing machineries used for the master batch and final preparation of rubber compounds.
A rubber composition prepared by a process which comprises sequential mixing stages, thermo-mechanically mixing of master batch. The mixing stages are as follows:
Master Batch Stage 1:
Mixing has been done with the head temperature of the Banbury maintained between 55 to 65°C, the unloaded rotor speed maintained between 45 to 65 rpm and the ram pressure is to be maintained at 4.5 to 6.0 Kp/cm2.
The mixing cycle is to be followed as: a) mixing chamber has been charged with natural rubber, neodymium catalyst polybutadiene rubber, a reinforcing renewable filler bagasse ash, coupling agent X50S and 50% of carbon black and allowed it to mix upto the temperature range between 120°C-125°C b) further mixing chamber has been charged with the ingredients like stearic acid, MC wax, Struktol 40MS and remaining 50% of carbon black is added and mixed up to temperature range between 140°C to 145°C and c) the rotor rpm is changed into 20 rpm for silanization process for allow it to mix for 20 to 30 seconds and the ram pressure maintained between 4.5 to 6.0 kP/cm2 throughout the process. The rotor rpm is reduced to 16 rpm and allow it to mix for 30 to 40 seconds and e) further the rotor rpm is increased to 45 to 60 rpm and mixed for 20 seconds to 30 seconds and the compound has been dumped by not exceeding the temperature of 160°C.
Master Batch Stage 2:
The stage 1 master batch compound maturation time has been maintained between 6 to 8 hours and then the stage 1 master batch rubber compound has been charged into the Banbury internal mixer with zinc oxide and 6PPD and mixed for 120 seconds and the master batch rubber compound has been dumped in the temperature range of 150°C to 160°C and further the rubber compound is sheeted out in two roll mill.
Final Batch Stage 3:
Thermo mechanically mixing of final batch is as follows:
Mixing has been done with the head temperature of the Banbury maintained between 100 to 105°C, the unloaded rotor speed maintained between 25 to 45 rpm and the ram pressure is to be maintained at 4.0 to 4.5 Kp/cm2.
The stage 2 master batch rubber compound maturation time is maintained between 4 to 6 hours and then stage 2 master batch rubber compound is charged into the Banbury internal mixer and then add cure chemicals like vulcanizer sulphur and an accelerator CBS are charged and allow it to mix for 120 to 140 seconds, and the final batch rubber compound has been dumped and sheeted out in the two roll mill.
Results:
Characterization of Cured Rubber Vulcanizate and Uncured Rubber Compound. The compound properties are listed in Table 3 & Table 4 as below:
Table 3: Properties of uncured Rubber Compound and Cured Rubber Vulcanizate
Properties Control Rubber Composition Formulation related to disclosure Index
C1 F1 F3 F4 F1 F3 F4
M1. Better Processability of a Rubber Compound
a) Mooney Viscosity of a Rubber Compound ML (1+4) @125 deg C
ML (1+4) @125 deg C, MU 78.90 38.00 36.40 36.50 48.16 46.13 46.13
b) Mooney Scorch @ 125°C
t5, minutes: minutes
(Ideal t5 value of tread compound is greater than or equal to 18 minutes) 23.80 31.53 33.60 39.93 - - -
c) Payne Effect of a Rubber Compound
Payne effect, Mpa (G’@0.07% - G’@10% Strain
(Lower the index value is better) 0.87 0.20 0.05 0.04 22.99 5.75 4.59
M2. Rebound Resilience of the Rubber Vulcanizate
Rebound Resilience at 25+/- 2 deg C, % 56.38 62.60 70.30 76.15 110.03 124.69 135.07
M3. Visco elastic properties of a Rubber Vulcanizate
a) Rolling resistance of a Rubber Vulcanizate
Tan delta at 60 deg C
(Lower the index value is better) 0.144 0.103 0.067 0.055 71.53
46.52
38.19
b) Hysteresis of a Rubber Vulcanizate
B) Tan delta @ 80 deg C (Lower index value is better) 0.135 0.101 0.070 0.055 74.81
51.85
40.74
Table 4: Properties of uncured Rubber Compound and Cured Rubber Vulcanizate
Properties Control Rubber Composition, C2 Formulation related to disclosure, F2 Index
M1. Better Processability of a Rubber Compound
a) Mooney Viscosity of a rubber Compound
ML (1+4) @125 deg C, MU
(Lower the index value is better) 38.20 26.90 70.41
b) Mooney Scorch @ 125°C
t5, minutes: minutes
(Ideal t5 value of tread compound is greater than or equal to 18 minutes) 53.43 43.93 -
c) Payne effect of a Rubber compound
Payne effect (G’@0.07% - G’@10% Strain), MPa
(Lower the index value is better) 0.28 0.20 71.43
M3. Visco elastic properties of a Rubber Vulcanizate
Tan delta at 0 deg C
(Higher the index value is better) 0.202 0.253 125.24
Tan delta at 25 deg C
(Higher the index value is better) 0.188 0.229 121.80
The purpose of these tests is to measure the improved properties of the formulations related to the disclosure against control formulation. For this, NR: Nd PBR blend based tyre tread rubber compositions F1, F3, F4 containing reinforcing filler carbon black grade N330 (60 phr) is replaced by 15 phr, 35 phr, 60 phr of bagasse ash as a biomass derived reinforcing renewable filler are prepared against NR: Nd PBR blend based tyre tread rubber composition containing reinforcing filler carbon black grade N330 (60 phr) C1 Control is prepared and evaluated.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F1, F3, F4) NR: Nd PBR blend reinforced by reinforcing filler N330 (60 phr) is replaced by 15 phr, 35 phr, 60 phr of bagasse ash as a biomass derived reinforcing renewable filler gave master batch Mooney viscosity values 38.0, 36.4 and 36.5 respectively when compared to NR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C1) gave Mooney viscosity value is 78.90 MU (Refer Table 3). From the data, it infers lower Mooney viscosity value is good for better processability i.e., 51.84%, 53.87%, 53.87% improvement from the control rubber composition.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F1, F3, F4) NR: Nd PBR blend reinforced by reinforcing filler N330 (60 phr) is replaced by 15 phr, 35 phr, 60 phr of bagasse ash as a biomass derived reinforcing renewable filler gave t5 values 31.53 minutes, 33.60 minutes, 39.90 minutes (Note: Ideal value of tyre tread rubber compound is 18 minutes) when compared to NR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C1) gave t5 value is 23.80 minutes (Refer Table 3). Rubber composition related to disclosure F1, F3 & F4 gave higher t5 values than control rubber composition which indicates process safety.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F1, F3, F4) NR: Nd PBR blend reinforced by reinforcing filler N330 (60 phr) is replaced by 15 phr, 35 phr, 60 phr of bagasse ash as a biomass derived reinforcing renewable filler gave Payne effect values 0.20 Mpa, 0.05 Mpa and 0.04 Mpa when compared to NR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C1) gave Payne effect value is 0.87 Mpa (Refer Table 3). Lower Payne effect value provides better rubber-filler interaction rather than filler-filler interaction. Therefore, the rubber compositions related to disclosure provides better rubber filler interaction than control rubber composition, C1 and the data in Table 2 (lower Payne effect value) infers the silanization process is effective while mixing of rubber compounds.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F1, F3, F4) NR: Nd PBR blend reinforced by reinforcing filler N330 (60 phr) is replaced by 15 phr, 35 phr, 60 phr of bagasse ash as a biomass derived reinforcing renewable filler gave rebound resilience 56.38%, values 0.20 Mpa, 0.05 Mpa and 0.04 Mpa when compared to NR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C1) gave Payne effect value is 0.87 Mpa (Lower Payne effect value provides better rubber-filler interaction (i.e., 25.19%, 48.15%, 59.26% improvement from control rubber composition) rather than filler-filler interaction. Therefore, the rubber compositions related to disclosure provides better rubber filler interaction than control rubber composition C1 and the data (lower Payne effect value) infers the better silanization process while mixing the rubber compounds (Refer: Table 3).
The present disclosure provides a tyre tread rubber compositions related to disclosure (F1, F3, F4) NR: Nd PBR blend reinforced by reinforcing filler N330 (60 phr) is replaced by 15 phr, 35 phr, 60 phr of bagasse ash as a biomass derived reinforcing renewable filler gave improvement of 10.03%, 24.69% and 35.07% rebound resilience % respectively when compared to NR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C1). Higher rebound value % provides high rubber elasticity.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F1, F3, F4) NR: Nd PBR blend reinforced by reinforcing filler N330 (60 phr) is replaced by 15 phr, 35 phr, 60 phr of bagasse ash as a biomass derived reinforcing renewable filler gave lower rolling resistance 28.47 %, 53.48% and 61.81% respectively when compared to NR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C1). Lower tan delta at 60 deg C values provides lower rolling resistance.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F1, F3, F4) NR: Nd PBR blend reinforced by reinforcing filler N330 (60 phr) is replaced by 15 phr, 35 phr, 60 phr of bagasse ash as a biomass derived reinforcing renewable filler gave lower hysteresis i.e., improved by 25.19 %, 48.19% and 59.26% respectively when compared to NR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C1). Lower tan delta at 80 deg C values indicates lower hysteresis and also higher rebound resilience % indicates lower hysteresis.
The purpose of these tests is to measure the improved properties of the formulations related to the disclosure against control rubber formulation. For this, SBR: Nd BR blend based tyre tread rubber compositions F2, containing reinforcing filler carbon black grade N330 (50 phr) along with 50 phr of bagasse ash as a biomass derived reinforcing renewable filler and 25 phr of process aid MES oil are prepared against SBR: Nd BR blend based tyre tread rubber composition containing reinforcing filler carbon black grade N330 (50 phr) along with 5 phr of process aid MES oil , C2 Control is prepared and evaluated.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F2) SBR: Nd PBR blend reinforced by reinforcing filler N330 (50 phr) along with 50 phr of bagasse ash as a biomass derived reinforcing renewable filler along with 25 phr of process aid MES oil gave master batch Mooney viscosity value 26.90 MU (i.e., 29.59% improvement) when compared to SBR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C2) along with 5 phr of process aid MES oil gave Mooney viscosity value is 38.20 MU (Refer Table 4). Lower Mooney viscosity value is good for better processability.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F2) SBR: Nd PBR blend reinforced by reinforcing filler N330 (50 phr) along with 50 phr of bagasse ash as a biomass derived reinforcing renewable filler along with 25 phr of process aid MES oil gave t5 value 43.93 minutes (Note: Ideal value of tyre tread rubber compound is 18 minutes) when compared to SBR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C2) along with 5 phr of process aid MES oil gave t5 value is 53.43 minutes.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F2) SBR: Nd PBR blend reinforced by reinforcing filler N330 (50 phr) along with 50 phr of bagasse ash as a biomass derived reinforcing renewable filler along with 25 phr of process aid MES oil gave t5 value 43.93 minutes (Note: Ideal value of tyre tread rubber compound is 18 minutes) when compared to SBR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C2) along with 5 phr of process aid MES oil gave t5 value is 53.43 minutes.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F2) SBR: Nd PBR blend reinforced by reinforcing filler N330 (50 phr) along with 50 phr of bagasse ash as a biomass derived reinforcing renewable filler along with 25 phr of process aid MES oil gave 28.57 % improvement in Payne effect when compared to SBR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C2) along with 5 phr of process aid MES oil.
The present disclosure provides a tyre tread rubber compositions related to disclosure (F2) SBR: Nd PBR blend reinforced by reinforcing filler N330 (50 phr) along with 50 phr of bagasse ash as a biomass derived reinforcing renewable filler along with 25 phr of process aid MES oil provides improvement in wet grip by 25.24 % and dry grip by 21.80% when compared to SBR: Nd PBR blend based tyre tread rubber composition reinforced by reinforcing filler N330 (Control C2) along with 5 phr of process aid MES oil.
Hence, the present disclosure provides a tyre tread rubber composition reinforced by reinforcing filler carbon black grade N330 replaced by a reinforced filler bio mass derived renewable filler Sugarcane bagasse ash provides lower rolling resistance, lower hysteresis, high rubber elasticity along with better processing properties and the tyre rubber composition is suitable for motorcycle and scooter low rolling resistance tyre tread application. Also, the present disclosure provides a tyre tread rubber composition reinforced by reinforcing filler carbon black grade N330 along with a biomass derived reinforcing renewable filler sugarcane bagasse ash provides combination of improved wet and dry grip along with better processability and the tyre rubber composition is suitable for high performance motorcycle and scooter tyre tread application.
Characteristics of cured Rubber vulcanizate and uncured Rubber compound:
Measurements and Tests:
M1. Better processability of a Rubber Compound
a) Mooney Viscosity of a Rubber Compound
Mooney Viscosity of a Rubber compound is measured for master batch compound (Stage 2 master batch compound) at ML (1+4) @ 125 deg C in Mooney Viscometer, Alpha technologies USA in accordance with ASTM D 1646. Mooney viscosity of a rubber compound is measured to understand the rubber compound flowability during process. Lower the Mooney viscosity is better for Processability.
b) Mooney Scorch characteristics of a Rubber Compound
Mooney Scorch properties of a Rubber compound is measured for final batch rubber compound (Stage 3 i.e., Final batch compound) at 125 deg C is measured in Mooney Viscometer, Alpha technologies USA in accordance with ASTM D 1646. Mooney scorch (pre vulcanization characteristics) of a rubber compound is measured to understand the rubber compound processing time i.e., which indicates the first incipient crosslinking. Higher the Mooney Scorch value is better for processability.
c) Payne Effect
The RPA (Rubber Process Analyzer) is a dynamic mechanical rheological tester to analyze unvulcanized (uncured) compounds.
The Payne effect is an effective way of studying deagglomeration of fully reinforcing carbon black during the rubber compound mixing process. It should be an effective way of relating to carbon black aggregate—aggregate attraction vs. the carbon black aggregate attraction to the specific rubber hydrocarbon medium.
The Payne effect is the difference in storage modulus (G’) at relatively low elongation rates. The difference (G’@0.7% - G’ @ 10%) is caused by 'filler-filler interaction'. During mixing, the filler should be dispersed homogeneously through the compound, which indicates a break-up of agglomerates into primary particles, resulting in a filler network within the polymer network. Lower the difference (G’@0.7% - G’ @ 10%) value is lower the Payne effect which implies lower filler- filler interaction and better polymer -filler interaction.
The Payne Effect Strain (Test conditions: Sweep test, Strain Angle 0.07 to 300.00%, Temperature: 70°C, Frequency: 1Hz) is measured through Rubber Process Analyzer RPA 2000 premier from Alpha Technologies, USA in accordance with ASTM D 8059.
M2. Rebound Resilience of a Rubber Vulcanizate:
It is a percentage of a cured rubber vulcanizate is measured using Rebound Resilience tester (Schob type Rebound Pendulam) from Zwick Roell 5109 Rebound resilience tester in accordance with ASTMD 7121. Higher the Rebound resilience % value is higher the rubber elasticity. Highly resilient compound prevents excessive heat build-up in service of the product i.e., Higher resilience percentage value is an indication of lower hysteresis compound.
M3. Visco elastic properties of a Rubber Vulcanizate:
The dynamic properties of the rubber vulcanizate are measured on a dynamic mechanical analyzer (DMA Metravib +1000) with a 0.3% dynamic strain, 0.6% static strain%, temperature -40 deg C to +80 deg C, and 10Hz frequency as per ASTM D5992.
a) Tan delta at 60°C is commonly used as a predictor of tyre rolling resistance. Also, lower the tan delta value at 60°C indicates lower rolling resistance.
b) Tan delta at 80 deg C is used as a predictor for hysteresis. Lowe tan delta value at 60 deg C indicates lower hysteresis.
c) Tan delta at 0°C is commonly used as a predictor of tyre wet traction. Also, higher the tan delta value at 0°C indicates higher wet grip.
d) Tan delta at 25°C is commonly used as a predictor of tyre dry grip. Also, higher the tan delta value at 25°C indicates higher dry grip.
,CLAIMS:I/We claim (s):
1. A tire tread rubber composition comprising:
elastomers – 100 parts;
reinforcing filler – 0 – 60 phr;
reinforcing renewable filler – 5- 60 phr;
coupling agent X50S – 0 – 9.6 phr;
process aid – 0 – 40 phr;
struktol 40MS – 0.5 – 2 phr;
cure activators – 0.5 – 5 phr;
anti-degradants – 1-4 phr;
vulcanization agent – 1.2 – 1.7 phr; and
accelerator – 0.5- 1.2 phr;
wherein the biomass derived reinforcing renewable filler is sugarcane bagasse ash.
2. The tire tread rubber composition as claimed in claim 1, wherein the elastomers is 70 – 100 parts of natural rubber and 0 – 30 parts of neodymium catalyst polymerized polybutadiene rubber.
3. The tire tread rubber composition as claimed in claim 1, wherein the elastomers is 70 – 100 parts of emulsion polymerized non-oil extended styrene butadiene rubber and 0 –30 parts of neodymium catalyst polymerized polybutadiene rubber.
4. The tire tread rubber composition as claimed in claim 1, wherein the reinforcing filler is carbon black having iodine surface area value ranges from 77 m2/gm to 87 m2/gm, oil absorption number value ranges from 97 cc/100 gm to 107 cc/100 gm, tinting strength values ranges from 99 to 109 % ITRB.
5. The tire tread rubber composition as claimed in claim 1, wherein the process aid is mild extract solvate (MES) oil.
6. The tire tread rubber composition as claimed in claim 1, wherein the cure activators are zinc oxide and stearic acid, in a weight ratio of 1- 3.5 phr: 0.5 – 1.5 phr.
7. The tire tread rubber composition as claimed in claim 1, wherein the anti-degradants are MC wax and 6PPD, in a weight ratio of 1- 2 phr: 1- 2 phr.
8. The tire tread rubber composition as claimed in claim 1, wherein the vulcanization agent is sulphur.
9. The tire tread rubber composition as claimed in claim 1, wherein the accelerator is CBS.
10. The tire tread rubber composition as claimed in claim 1, wherein the coupling agent X50S is a blend of the bifunctional, sulfur containing organo silane coupling agent Si69 and N330 type carbon black in the ratio 1:1 by weight. The coupling agent X50S enhance the polymer filler interaction.
11. A method for preparation of a tire tread rubber composition containing sugarcane bagasse ash as biomass derived reinforcing renewable filler, comprising:
a) Master batch Stage 1: adding elastomers, reinforcing renewable filler, coupling agent X50S and 50% of carbon black in the Banbury mixer chamber is allowed to mix;
b) mixing ingredients obtained at step-a in the chamber of Banbury by maintaining a temperature of the chamber between 120°C-125°C and ram pressure maintained between 4.5 to 6.0 kP/cm2;
c) additionally adding stearic acid, MC wax, Struktol 40MS, and the remaining 50% of carbon black in the chamber of Banbury mixer mixture is allowed to mix;
d) mixing of ingredients in Banbury mixer by maintaining chamber temperature between 140°C-145°C;
e) allowing the mixture to silanization for a time period of 20 to 30 seconds at a maintained rotor speed of 20 rpm;
f) reducing the rotor speed to 16 rpm and allowing to mix the ingredients in the Banbury mixer for a period of 30 to 40 seconds;
g) increasing rotor speed at a maintained range between 45-60 rpm and allowing the ingredients to mix in the Banbury mixture for a period of 20-30 seconds;
h) dumping the rubber compound at a temperature up to 160°C to obtain a first rubber compound;
i) maintaining the first rubber compound obtained at step-h for maturation for a period of 6-8 hours;
j) Master batch Stage 2: adding zinc oxide and 6PPD to rubber compound obtained at step-i;
k) allowing to mix the ingredients in the Banbury mixer for a period of 120 seconds;
l) dumping the rubber compound at a temperature maintained between 150°C-160°C to obtain a second rubber compound;
m) sheeting out the second rubber compound obtained at step-l in the two roll mills by maintaining the rotor speed between 50-60 rpm and rotor temperature maintained between 55°C to 65°C;
n) maintaining the second rubber compound for maturation for a period of 4-6 hours;
o) Final batch: adding cure chemicals vulcanizer Sulphur and accelerator CBS to the second rubber compound obtained at step-n;
p) mixing ingredients of step-o in the Banbury mixer for a period of 120 – 140 seconds by a maintained rotor speed between 25-45 rpm;
q) maintaining the chamber temperature between 100°C-105°C and ram pressure maintained between 4.0 to 4.5 kP/cm2; and
r) dumping the rubber obtained at step-q and sheeting out using two roll mill.
| # | Name | Date |
|---|---|---|
| 1 | 202241040085-STATEMENT OF UNDERTAKING (FORM 3) [13-07-2022(online)].pdf | 2022-07-13 |
| 2 | 202241040085-PROVISIONAL SPECIFICATION [13-07-2022(online)].pdf | 2022-07-13 |
| 3 | 202241040085-FORM-26 [13-07-2022(online)].pdf | 2022-07-13 |
| 4 | 202241040085-FORM 1 [13-07-2022(online)].pdf | 2022-07-13 |
| 5 | 202241040085-DECLARATION OF INVENTORSHIP (FORM 5) [13-07-2022(online)].pdf | 2022-07-13 |
| 6 | 202241040085-Information under section 8(2) [13-07-2023(online)].pdf | 2023-07-13 |
| 7 | 202241040085-DRAWING [13-07-2023(online)].pdf | 2023-07-13 |
| 8 | 202241040085-CORRESPONDENCE-OTHERS [13-07-2023(online)].pdf | 2023-07-13 |
| 9 | 202241040085-COMPLETE SPECIFICATION [13-07-2023(online)].pdf | 2023-07-13 |
| 10 | 202241040085-FORM 18 [09-01-2025(online)].pdf | 2025-01-09 |