DESC:TECHNICAL FIELD OF INVENTION
The present disclosure relates to the field of polymer technology. More particularly, the present disclosure relates to the invention of a tire tread rubber composition using oil-treated Fuller's Earth and its method of preparation.

BACKGROUND OF INVENTION
The invention broadly belongs to the domain of polymer engineering, particularly focusing on the development and innovation of tire compositions. This field primarily involves studying, manufacturing, and applying various compositions to enhance the physical properties and performance of tires.
One area the field explores is the integration of different enhancements, such as the utilization of oil- treated Fuller's Earth, to improve the characteristics and efficiency of the tread rubber. This field also encompasses the methodology involved in creating such improved rubber compositions, optimizing the efficiency of the production process, and augmenting the overall tire quality.
IN202041049202 describes a rubber nanocomposite for motorcycle tyres, comprised of rubbers and a nanofiller. This nanofiller features naturally occurring, unmodified Fuller’s earth, which reduces rolling resistance while enhancing rubber elasticity. The invention also outlines a method for preparing this rubber nanocomposite along with a tyre tread using the same. However, the current invention is centered on the use of oil-treated Fuller's earth in tyre tread rubber composition to improve dynamic mechanical properties.
IN201941012523 describes a development of a cured elastomeric composite made up of un-modified fuller’s earth clay acting as a reinforcing filler. The patent discloses a nanocomposite that includes an elastomeric compound and fuller’s earth nano clay, resulting in high thermal stability and mechanical properties. The processability of the uncured compound also reportedly increases marginally with the addition of the filler. The patent relates to cured silica or carbon black reinforced, or gum elastomer compounds used in various elastomer products, functioning as a compression set regulator, hardness modifier, and as a reinforcing material.
IN3377/MUM/2010 describes the use of oil-treated carbon black utilizing naturally occurring rice bran oil to achieve low rolling resistance. The focal point of this patent is on the specific application of this substance in tyre tread rubber compositions to deliver dynamic mechanical properties. It is unique in its approach of leveraging oil-treated fuller's earth as a crucial aspect of this composition.
IN202141030054 describes a tyre bead rubber composition that contains polymer-coated CNT in a carbon black filled system. This composition provides superior thermal stability, a high modulus, and low gas permeability. However, it does not address the use of oil treated fuller’s earth in the tyre tread rubber composition for enhancing dynamic mechanical properties as per the present invention. This poses an opportunity for innovation and improvement.
PH12016500630 describes the use of fatty acid treated filler in rubber composition. However, the current invention is distinct as it discusses the utilization of oil-treated fuller's earth in tyre tread rubber composition, aiming to enhance dynamic mechanical properties. EP4122984 describes the use of two different functionalized silica fillers with varied surface area ranges, intended to provide low rolling resistance and improved wet traction. This practice is exhibited in the prior art. However, the patent in discussion here pertains to the incorporation of oil-treated fuller’s earth in tyre tread rubber compositions to enhance dynamic mechanical properties.
WO2020218601 discloses a rubber composition featuring an elastomeric matrix, reinforcing inorganic filler, and a plasticizing agent. This agent includes a hydrocarbon resin and a liquid plasticizer, contributing to a balance between durability and hysteresis characteristics. However, it does not address the usage of oil-treated fuller's earth in tyre tread rubber composition to enhance dynamic mechanical properties, as proposed in the current invention.
WO2016032010 describes a rubber composition containing a diene elastomer, a minimum of 60 phr of an inorganic reinforcing filler, and between 20 to 100 phr of a plasticizer which incorporates more than 4 phr of mercapto-modified silicone oil. The disclosed composition aims to lower rolling resistance and enhance wear resistance of tires. The present invention, however, focuses on oil-treated fuller's earth being used in a tire tread rubber composition to provide improved dynamic mechanical properties. BG109150 discloses a method of tyre pyrolysis, which is a process of thermal decomposition of tires. The method outlined in this patent involves applying heat to tires in an oxygen-free environment to break them down into oils and gases. However, the current invention diverges from this by discussing the use of oil treated fuller’s earth in tyre tread rubber composition to enhance its dynamic mechanical properties.
KR20060134335 describes a bead filler rubber composition for the radial tire of a truck or a bus. The focus of this prior art is on improving the blow-out characteristics, hardness, and heat build-up characteristics in radial tires. However, it does not address or contemplate the use of oil-treated Fuller’s earth in tyre tread rubber composition for enhancing dynamic mechanical properties, as discussed in the present invention.
KR20090106287 describes an insert rubber composition for reinforcing the sidewall of run-flat tires, serving to enhance modulus and tear strength properties of the rubber. The invention detailed in this patent involves the use of the rubber composition in the sidewall area and does not mention the utilization of any additives like oil treated fuller's earth. The primary focus appears to be on the reinforcement and strength enhancements of tire sidewall via the described rubber composition. This prior art doesn't provide information about the use of the rubber composition in the tread area, or the potential impacts on dynamic mechanical properties.
KR20010081361 discloses a rubber composition for tire rim flange exhibiting high hardness with improved anti-abrasion, anti-aging by heat resistance and compression set against atmospheric factors and ozone. This is achieved by utilizing free sulfur or oil-treated sulfur for vulcanization. However, the current invention steers away from the previously described approach, introducing the use of oil-treated fuller's earth in tire tread rubber composition to enhance dynamic mechanical properties.
JP2005023219 describes a rubber composition for a tire tread that uses silicone oil treated silica as a reinforcing filler. This composition aids in significantly improving the breaking performances of a tire on ice and on a wet road surface. However, it should be noted that the current invention under consideration uses oil treated fuller’s earth in the tyre tread rubber composition to enhance its dynamic mechanical properties.
IN7939/DELNP/2006 describes a cross-linkable or cross-linked rubber composition with improved hysteresis properties in the cross-linked state, which can be used to create a tyre tread with reduced rolling resistance. The focus of the prior art is more on improving the characteristics of the rubber composition, specifically its hysteresis properties. On the other hand, the present invention introduces the concept of oil treated fuller’s earth in tyre tread rubber composition to enhance its dynamic mechanical properties.
IN2128/DELNP/2006 describes the utilization of a crosslinked elastomeric material placed between tyre components, the resultant material having a dynamic elastic modulus (E'), measured at 70°C, preferably ranging from 25 MPa to 50 Mpa. This earlier patent primarily focused on the properties imparted by the elastomeric material onto the tyre components. However, the present invention diverts to discuss the application of oil-treated fuller’s earth in tyre tread rubber composition to augment its dynamic mechanical properties.
JP2002097311 describes a rubber composition characterized by compounding a rubber component with staple fibers and a filler containing silica heat-treated with silicone oil. This composition is known to produce tires with high initial dry steering stability and wet steering stability. However, it doesn't discuss the use of oil treated fuller's earth. The current invention addresses the utilization of oil-treated fuller's earth in tire tread rubber composition to enhance dynamic mechanical properties.
IN202221029284 discloses a synergistic tire tread formulation that broadly includes neat rubber; zinc oxide; stearic acid; modified calcium carbonate; carbon black; paraffinic oil; 2,2,4-trimethyl-1,2-dihydroquinoline; sulphur; N-cyclohexyl- 2-benzothiazolesulfenamide; and tetramethylthiuram disulphide. This formulation provides advantages such as improved fuel efficiencies and reduced rolling resistance. However, the present invention introduces the use of oil-treated fuller's earth in the tire tread rubber composition to improve dynamic mechanical properties.
IN202217012465 discloses a method for chemically adhering a diene rubber with a piezoelectric polymer used for tyre innerliners. However, the present invention diverts from this approach and instead presents a novel method of using oil-treated fuller’s earth in the composition of tyre tread rubber with the aim of enhancing its dynamic mechanical properties.

OBJECTS OF THE INVENTION:
The principal object of the present invention is to provide tyre tread rubber composition using oil treated Fuller’s Earth nano clay.
Another object of the present invention is to provide a method of preparation of oil treated Fuller’s Earth nano clay in tyre tread rubber composition.
Yet another object of the present invention is the process oil used for treating the unmodified Fuller’s Earth nano clay belongs to TDAE oil or MES oil or any other naturally occurring oils.
Yet another object of the present invention is the process oil used for treating the unmodified Fuller’s Earth nano clay belongs naturally occurring Mustard Oil.
Yet another object of the present invention is to provide a tyre tread rubber composition to provide improved dynamic mechanical properties.
Yet another object of the present invention to provide reduce carbon footprint.

SUMMARY OF THE INVENTION
One or more of the problems of the conventional prior art may be overcome by various embodiments of the present disclosure.
In one aspect of the present invention, a rubber composition is provided. This rubber composition comprises Natural Rubber, Polybutadiene Rubber or Neodymium Catalyzed Butadiene Rubber, Styrene butadiene rubber or Solution Styrene-Butadiene Rubber, Carbon Black, and Oil treated Fullers Earth. It may include Precipitated Silica, at least one of Natural resin, C5 type resin, or C5/C9 type resin, a coupling agent, Zinc oxide, Stearic acid, 2,2,4-Trimethyl-1,2-dihydroquinoline, N-(1,3-dimethylbutyl)-N'- phenyl-phenylenediamine, Microcrystalline Wax, Sulphur, Diphenylguanidine, and N-cyclohexyl-2-benzothiazolesulfenamide. Strikingly, this rubber composition is devoid of process oil as an additional ingredient. The process oil used for treating the unmodified fuller’s earth nano clay in the present invention belongs to MES oil or TDAE oil or any other naturally occurring oils.
In another aspect of the present invention, the rubber composition wherein the Carbon Black is present in a certain amount ranging that enhances the inventive rubber composition's properties.
In another aspect of the present invention, the rubber composition is further improved by incorporating an amount of Oil treated Fullers Earth nano clay that ranges to enrich the properties of the inventive rubber composition.
In another aspect of the present invention, the rubber composition may include a certain amount of Precipitated Silica to optimize its rubber composition.
In another aspect of the present disclosure, a method for preparing a rubber composition for tyre tread is disclosed. This process involves preparing a master batch using a thermo-mechanical process in a Banbury mixer, following a sequence of steps detailed in the patent claim. The master batch is then mixed with zinc oxide and 6PPD in the second stage, before charging the mixing chamber with the master batch and adding curatives to mix and form the final batch rubber compound. This procedure ensures an optimal composition for the rubber tire tread, providing better performance characteristics compared to traditional methods.

DETAILED DESCRIPTION OF DRAWINGS
Figure 1: Fourier Transform Infrared (FTIR) Spectroscopy (FTIR) Attenuated Total Reflectance (ATR) spectra of Unmodified Fuller’s Earth nano clay
Figure 2: FTIR ATR spectra of Mustard Oil
Figure 3: FTIR ATR spectra of Mustard Oil treated Fuller’s Earth nano clay
Figure 4: Overlay of Figure 1, Figure 2 and Figure 3

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. 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.

The present invention relates to the field of tyres. The present invention relates to rubber composition for motorcycle tyre treads using Mustard oil treated fuller’s Earth Nano Clay. The present invention also provides a tyre produced using this rubber composition, capable of providing better ice traction along with wet traction and lower rolling resistance property. The present invention also relates to the better processing properties of the rubber compound. The rubber composition of motor cycle tyre tread includes 100 parts by weight of a rubber, preferably with the blend of natural rubber, neodymium catalyzed butadiene rubber and solution styrene butadiene rubber , preferably natural rubber 45-55 phr, neodymium catalyzed butadiene rubber 15 to 25 phr and solution styrene butadiene rubber 25 – 35 phr, 10 to 30 parts of the reinforcing filler such as carbon black, preferably with carbon black with the iodine surface area of 140 to 150 mg/gm and the reinforcing filler dosage can be adjusted based on the tyre tread hardness requirement ranging from 58 to 65 Shore A, and preferably silica 5-15 phr, along with the use of 30 to 80 parts of mustard oil treated fuller’s earth nano clay and the oil treated filler dosage can be adjusted based on the tyre tread hardness requirement ranging from 58 to 69 Shore A. Further, the present invention rubber composition containing 3- 6 phr of natural resin or C5 type resin, or C5/C9 type resin, 0.1 to 8.0 phr of coupling agent,1-3 phr of zinc oxide, 1-3 phr of Stearic acid, 0.1 to 3 phr of 2,2,4-Trimethyl-1,2-dihydroquinoline (TMQ), 1-4 phr of N-(1,3-dimethylbutyl)-N'-phenyl-p- phenylenediamine (6PPD), 1-3phr of Microcrystalline Wax, 1-3.5 phr of sulphur, 0-2.0 phr of Diphenylguanidine (DPG), and 1.0-3.0 phr of N-cyclohexyl-2-benzothiazolesulfenamide (CBS).

Table 1: Rubber Composition in phr
Ingredients Control Rubber Composition Formulation related to invention Control Rubber Composition Formulation related to invention
C1, phr F1, phr
C2, phr
F2, phr

NR 1 50 50 50 50
NdBR 2 20 20 20 20
SSBR 3 30 30 30 30
Carbon Black N110 4 20 20 20 20
Unmodified Fuller’s Earth Nano Clay 5 40 30
Mustard Oil treated Fuller’s Earth 6 48.0 36
Precipitated Silica 7 10 10
Impera resin 1504 8 3 3 3 3
Coupling agent, Si 69 9 1 1
Mustard Oil 10 10 10
Zinc oxide 11 2.5 2.5 2.5 2.5
Stearic acid 12 1.5 1.5 1.5 1.5
TMQ 13 0.5 0.5 0.5 0.5
6PPD 14 1.5 1.5 1.5 1.5
MC Wax 15 1.2 1.2 1.2 1.2
Sulphur 16 1.8 1.8 1.8 1.8
DPG 17 0.5 0.5 0.5 0.5
CBS 18 1.3 1.3 1.3 1.3
1.NR - Indian Standard Natural Rubber ISNR 20 with the Mooney Viscosity, ML (1+4) at 100°C is 70 to 80 MU and it is obtained from Mamparambil Rubber India Pvt Ltd, India.
2.NdBR - It is an 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.
3. SSBR SLR 563 - It is a non-oil extended solution polymerized styrene butadiene rubber with a vinyl content of 55% and bound styrene content of 20% and a polymer Tg of -36 Deg C.
4. Carbon Black N110 - Carbon Black –ASTM Grade N110 is the reinforcing filler SAF, Superior Abrasion Furnace having the Iodine adsorption No. 140 to 150 mg/gm, tinting strength value between 118 to 128 % ITRB, nitrogen surface area value between 122 to 132 m2/gm and COAN value ranges between 92 to 102 cc/100 gm.
5. Unmodified Fuller’s Earth Nano Clay - Unmodified fuller’s Earth is a nano clay with the acicular particles in diameter 1 to 5 nm and length 10 to 5000 nm with the aspect ratio is in the range of 5 to 45 measured in HR TEM image at 50 nm magnification and it is having specific surface area of 100.3 m2/gm. The FTIR ATR spectrum of Unmodified fuller’s earth nano clay corresponds to 982.97 cm-1, 912.91 cm-1, 1641.5 cm-1, 796.13 cm-1, 693.4 cm-1, 2925.8 cm-1, 2855.8 cm-1 corresponds to unmodified Fuller’s Earth nano clay (Figure 1)
6. Mustard Oil treated Fuller’s Earth Nano Clay – Unmodified fuller’s Earth is a nano clay with the acicular particles in diameter 1 to 5 nm and length 10 to 5000 nm with the aspect ratio is in the range of 5 to 45 measured in HR TEM image at 50 nm magnification. The present invention treated the Unmodified Fuller’s Earth nano clay with naturally occurring mustard oil (Refer: Figure 4) along with coupling agent Si 69. The FTIR ATR spectra of mustard oil clearly indicates the miscibility of mustard oil treatment with unmodified fuller’s earth nano clay and its major peaks corresponds to 1744.2 cm-1, 1459.3 cm-1, 726.1 cm-1 corresponds to mustard oil (Figure 2) and 982.97 cm-1, 912.91cm-1, 796.15 cm-1, 693.4 cm-1 and its major peaks corresponds to unmodified fuller’s earth nano clay (Figure 1)
7. Precipitated Silica– It is from Madhu Silica Private Ltd, India. It is the reinforcing filler having nitrogen surface area value 170 to 190 m2/gm and it is used for the present invention is to provide a high performance motor cycle tyre treads.
8. Impera Resin 1504 – It is a hydrocarbon resin having the softening point of 85 Deg C and a Tg of 40 Deg C.
9. Coupling agent – Si69 is a bifunctional, sulfur- containing organosilane from Nanjing Shuguang Silane Chemical Co Ltd, China. It is used to provide a satisfactory bonding of, chemical/or physical nature between the inorganic filler and diene elastomer(s).
10. Mustard Oil-It is a naturally occurring oil is having 12% oleic acid, 6% of omega-3 alpha-linolenic acid and 15% of omega-6 linoleic acid and its iodine value ranges from 121.0 to 121.6 g/100 gm. The FTIR ATR spectra of mustard oil peaks corresponds to 3005.2 cm-1, 2925.8 cm-1, 2855.8 cm-1, 1744.2 cm-1, 1459.3 cm-1,160.4 cm-1,1099.7 cm-1, 726 cm-1. It is obtained from Sree Ram Agencies, New No: 18 Palmal Cross Street, Near Mahal South, Madurai, Tamilnadu, India.
11.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.
12.Stearic acid - Stearic acid- It is 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.
13.TMQ – It is 2,2,4-trimethyl-1,2-dihydroquinoline used as an antioxidant. TMQ act as a radical scavenger in elastomers to protect against oxidative aging.
14.6PPD -It is N-(1,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine from Finorchem Limited, India. It is added to the rubber composition to provide resistance to thermo-oxidative ageing of elastomers.
15. MC Wax - (Microcrystalline wax) from GPL, India. It is used to protect against degradation by ozone.
16.Sulphur - Sulphur is the vulcanizing agent from The Standard Chemical Co. Pvt Ltd, India.
17. DPG- Diphenylguanidine It is secondary accelerator, used to activate the primary accelerator) from PMC Rubber Chemicals India Pvt ltd, India.
18. CBS- (N-cyclohexyl-2-benzothiazolesulfenamide) It is a delayed action accelerator suitable for diene rubbers from Nocil Limited, India
Characterization of Uncured Rubber Compound and Cured Vulcanizate:
The compound properties are listed in Table 2 below-
Measurements and Tests:
The purpose of these tests was measured to understand the properties of rubber composition properties of formulation related to invention over the control rubber composition. Rubber composition F1 is prepared, and the properties are compared against a control rubber composition (C1). The control rubber composition comprises of NR: Nd BR: SSBR (50 phr: 20 phr: 30 phr) blend reinforced with 20 phr of carbon black and 40 phr of unmodified Fuller’s Earth nano clay along with 10 phr of mustard oil is compared against with the rubber composition comprises of NR: Nd BR: SSBR (50 phr: 20 phr: 30 phr) blend reinforced with 20 phr of carbon black and 48 phr of oil treated Fuller’s Earth nano clay.

The present invention provides a 100 parts by weight of rubber composition F1, NR: Nd BR: SSBR (50 phr: 20 phr: 30 phr) blend reinforced with 20 phr of carbon black and 48 phr of mustard oil treated Fuller’s Earth nano clay gave process safety, t5 value is 21.48 minutes (t5 value greater than 15 minutes is ideal value for tread compound) and the hardness of F1 tread compound is 58 Shore A when compared to NR: Nd BR: SSBR (50 phr: 20 phr: 30 phr) blend reinforced with 20 phr of carbon black and 40 phr of unmodified Fuller’s Earth nano clay along with 10 phr of mustard oil based rubber composition C1 (Control) and its hardness is 55 Shore A. Improvement in hardness in F1 rubber composition which indicates the higher polymer filler interaction than control rubber composition C1 and also it demonstrates the oil treated Fuller’s Earth containing compounds can increase the durability and mechanical integrity of the tyre tread rubber. The balanced hardness ensures that these compositions meet the rigorous requirements for tyre tread applications in particular lower rolling resistance applications.
The tyre tread rubber compositions F1 showed remarkable improvements in ice traction properties. Ice traction is improved by 8.49% when compared to the control rubber composition F2. Additionally, wet traction is improved by 3.85%. These enhancements indicate the superior grip and handling in diverse conditions, particularly in icy and wet environments. Moreover, low rolling resistance (LRR) improved remarkably by 14.29% contributing to better fuel efficiency and reduced energy consumption during vehicle operation.
Further, Rubber composition F2 is prepared, and the properties are compared against a control rubber composition (C2). The control rubber composition comprises of NR: Nd BR: SSBR (50 phr: 20 phr: 30 phr) blend reinforced with 20 phr of carbon black, 10 phr of reinforcing filler silica and 30 phr of unmodified Fuller’s Earth nano clay along with phr of mustard oil is compared against with the rubber composition comprises of NR: Nd BR: SSBR (50 phr: 20 phr: 30 phr) blend reinforced with 20 phr of carbon black, 10 phr of silica and 36 phr of oil treated Fuller’s Earth nano clay.
The present invention provides a 100 parts by weight of rubber composition F2, NR: Nd BR: SSBR (50 phr: 20 phr: 30 phr) blend reinforced with 20 phr of reinforcing filler carbon black, 10 phr of reinforcing filler silica and 36 phr of mustard oil treated Fuller’s Earth nano clay gave process safety, t5 value is 19.67 minutes (t5 value greater than 18 minutes is ideal value for tread compound) and the hardness of F1 tread compound is 59 Shore A when compared to NR: Nd BR: SSBR (50 phr: 20 phr: 30 phr) blend reinforced with 20 phr of carbon black, 10 phr of reinforcing filler silica and 30 phr of unmodified Fuller’s Earth nano clay along with 10 phr of mustard oil based rubber composition C2 (Control) and its hardness is 57 Shore A. Improvement in hardness in F2 rubber composition which indicates the higher polymer filler interaction than control rubber composition C2 and also it demonstrates the oil treated Fuller’s Earth containing compounds can increase the durability and mechanical integrity of the tyre tread rubber. The balanced hardness ensures that these compositions meet the rigorous requirements for tyre tread applications in particular lower rolling resistance applications.
The tyre tread rubber compositions F2 showed optimum properties in terms of ice traction, wet traction and lower rolling resistance over control rubber composition F2.
The mustard oil treated Fuller’s Earth nano clay enhances the properties of ice traction, wet traction and lower rolling resistance along with processability characteristics which implies the incorporation of process oil in filler itself enhances the reinforcement characteristics & dynamic mechanical properties and it provides a better solution in rubber compounding.
The compound properties are listed in Table 2 below-
Table 2: Properties of Cured Rubber Vulcanizate and Uncured Rubber Compound
Properties Control, C1 F1 Index Control, C2 F2 Index
M1. Processability Characteristics of Rubber Compound
t5@ 125 Deg C, minute: minute
(Ideal value is greater than 15 minutes) 16.02 21.48 - 15.45 19.67 -
M2. Hardness of a Rubber Vulcanizate
Hardness, Shore A 55 58 - 57 59 -
M3. Dynamic Mechanical Properties of the Rubber Vulcanizate
Ice Traction, tan delta at -10 Deg C (Higher the index value is better) 0.212 0.230 108.49 0.222 0.222 100.0
Wet traction, tan delta at 0°C
(Higher the index value is better) 0.182 0.189 103.85 0.190 0.190 100.0
Rolling resistance, tan delta 60 Deg C
(Lower the index value is better) 0.161 0.138 85.71 0.156 0.156 100.0
Measurements:
Mooney Scorch Characteristics (M1):
The Mooney Scorch test, conducted using a Mooney Viscometer (MV 2000), assessed the pre-vulcanization characteristics of the rubber compounds. The higher t5 value indicated that F1 and F2 compositions had better processability compared to the control composition (C1 & C2). The higher t5 values reflected easier mixing and handling during manufacturing, which contributed to improved process safety and efficiency.
Shore A Hardness (M2):
The Shore A Hardness of the rubber vulcanizate was measured according to ASTM D2240. The results showed that F1 and F2 compositions achieved hardness values between 57 and 59 Shore A. This range ensured that the compositions maintained adequate durability . The findings confirmed that incorporation of Oil treated fuller’s earth nano clay did not compromise the mechanical integrity of the tread rubber compound.
Dynamic Properties of Rubber Vulcanizate (M3)
The dynamic properties were evaluated using a dynamic mechanical analyzer (DMA), which provided predictive insights into the tyre's performance in specific conditions:
The tan delta values at -10°C were higher and optimal for F1 and F2 than for C1 & C2, demonstrating enhanced safety on icy surfaces.
The results showed higher tan delta values at 0°C for F1 and F2, which indicated better wet traction, contributing to improved handling and braking performance in wet conditions.
The tan delta values at 60°C were lower for F1 and F2 than for C1 & C2 reflecting reduced rolling resistance. This improvement translated into better fuel efficiency and energy savings during tyre usage.
Advantages:
The present disclosure provides a composition and preparing a rubber composition that reduces carbon footprint.
The present disclosure provides a rubber composition that improves ice traction, wet traction along with lower rolling resistance (LRR) property.
The present disclosure provides a rubber composition that provides better processing properties.
The present invention depicts the method of preparation of Oil treated Fuller’s Earth Nano Clay. The method includes the following process.
Unmodified Fuller’s Earth nano clay is taken in a container which was dried at 125 Deg C in air oven and removed any moisture content present in it.
For 100 gm of unmodified Fuller’s Earth nano clay 20 ml of mustard oil is taken and it is mixed with 0.1% Si 69 Coupling agent of a given dosage (20 ml) of mustard oil. Further the obtained mixture, M1 (mustard oil and Si 69 coupling agent) is diluted with a solvent toluene and stirred vigorously in order to obtain mixture M2.
Thus, mixture M2 is sprayed (Sprayer contains the nozzle 0.1mm) on unmodified Fuller’s Earth Nano Clay and allowed to rest in room temperature for 24 hours in order to evaporate the solvent toluene from it. Further, mustard oil treated Unmodified Fuller’s Earth nano Clay is kept in air oven 50 Deg C for 2 hours and remove the mustard oil treated Unmodified Fuller’s Earth nano clay from oven and cool it.
Now the Unmodified Fuller’s Earth Nano Clay is ready for rubber compounding.
The present invention depicts a method for preparing a rubber composition for tyre tread is provided, in accordance with an aspect of the present disclosure. The method includes the following process:
At Step A: Preparing a master batch by a thermo-mechanical process in a Banbury mixer, the process comprising:
Charging the mixing chamber with elastomers and mixing at a rotation speed between 45 to 65 rpm and a head temperature maintained between 80°C to 95°C
for 20 to 50 seconds.
adding 100% of the reinforcing fillers, which include carbon black, oil treated Fuller's Earth nano clay, and/or silica, along with a coupling agent, and mixing for 90 to 150 seconds.
conducting a silanisation process by reducing the rotor speed to 20 to 30 rpm at a
temperature of approximately 110°C to 140°C for 60-120 seconds, adding the remaining rubber chemicals TMQ, MC Wax, stearic acid, and mixing for 40 to 60 seconds.
sweeping down in the orifice, mixing for an additional 40 to 60 seconds, and dumping the compound at a temperature in the range of 150°C to 165°C.
sheeting out the rubber compound on a laboratory two-roll mill.
At Step B: Mixing the master batch prepared in Step A with zinc oxide and 6PPD in the Banbury mixer for 120 to 130 seconds and dumping the mixture at a temperature range of 125°C to 145°C, followed by sheeting out the rubber compound on a laboratory two-roll mill.
At step C: Charging the mixing chamber with the master batch from Step B and
adding curatives including Sulphur, CBS, and DPG, mixing for 40 to 90 seconds, and dumping the mixture at a temperature range of 90°C to 115°C, followed by sheeting out the final batch rubber compound on a laboratory mill. ,CLAIMS:We Claim
1. A rubber composition for tyre tread, comprising:
a polymer matrix – 100 parts by weight;
a reinforcing filler such as carbon black – 10 to 30 parts by weight;
a reinforcing nano filler – oil-treated Fuller’s Earth nanoclay – 30 to 80 parts by weight;
a resin – 0.5 to 5 parts by weight;
a coupling agent – 0.1 to 8 parts by weight;
an activator – 1.5 to 6 parts by weight;
an anti-degradant – 0.5 to 5 parts by weight;
a vulcanizing agent – 0.5 to 5 parts by weight; and
a primary accelerator – 0.5 to 3 parts by weight;
a secondary accelerator – 0-2.0 parts by weight;
wherein the oil-treated Fuller’s Earth nanoclay has a specific surface area ranging from 100 to 110 m²/gm and comprises acicular particles having an aspect ratio of 5 to 45, and wherein the oil treatment can be performed using mustard oil, treated distillate aromatic extract (TDAE) oil, or other natural oils in the presence of a silane coupling agent.
2. The rubber composition for tyre tread as claimed in claim 1, wherein the polymer matrix comprises a triblend elastomer composition comprising 50 parts by weight of natural rubber, 30 parts by weight of solution styrene-butadiene rubber (SBR), and 20 parts by weight of Neodymium catalyzed high-cis polybutadiene rubber (Nd BR).
3. The rubber composition for tyre tread as claimed in claim 1, wherein the resin is selected from naturally occurring resin, C5 resin, or a C5/C9 resin and has a softening point ranging from 70°C to 85°C.
4. The rubber composition for tyre tread as claimed in claim 1, wherein the oil-treated Fuller’s Earth nanoclay is modified using mustard oil containing oleic acid and linolenic acid, in combination with a silane coupling agent and solvent evaporation method.
5. The rubber composition for tyre tread as claimed in claim 1, wherein the anti-degradant is selected from 2,2,4-trimethyl-1,2-dihydroquinoline (TMQ), 6PPD and MC Wax.
6. The rubber composition for tyre tread as claimed in claim 1, wherein the vulcanizing agent is sulfur.
7. The rubber composition for tyre tread as claimed in claim 1, wherein the primary accelerator is selected from N-cyclohexyl-2-benzothiazole sulfenamide (CBS).
8. The rubber composition for tyre tread as claimed in claim 1, wherein the reinforcing filler carbon black has a nitrogen surface area (N2SA) ranging from 122 to 132 m²/g and an iodine adsorption number ranging from 140 to 150 mg/g.
9. A method for preparing the rubber composition as claimed in claim 1, comprising:
as a step A: mixing natural rubber and synthetic rubbers in a Banbury mixer at 50–60 rpm and 85–90°C for 20–40 seconds;
adding carbon black, oil-treated Fuller’s Earth nanoclay along with a coupling agent and mixing for 90–150 seconds to achieve homogeneous dispersion and the silanization process is carried out from 130 to 140 Deg C for 30 to 120 seconds at reduced rotor speed 20 to 30 rpm;
adding rubber chemicals stearic acid, 6PPD, TMQ, MC Wax and mixing for another 50–60 seconds, sweeping down the mixture and dumping at 150–165°C;
sheeting the rubber on a two-roll mill to form a step A master batch;
as step B: mixing step A obtained masterbatch compound along with zinc oxide and 6PPD for 120 to 130 seconds and dumping at 125 -145°C;
sheeting the rubber compound on a two-roll mill to form a Step B master batch;
subsequently mixing with sulfur and primary accelerator for 50–80 seconds, dumping at 85–110°C, and sheeting out to obtain the final rubber compound with a Shore A hardness in the range of 58–64 Shore A.