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Environment Friendly Vulcanizable Elastomer Composition, And Implementations Thereof

Abstract: The present disclosure discloses a vulcanizable elastomer composition comprising: at least one diene elastomer; tapioca flour; and at least one crosslinking agent. Also disclosed is a process for obtaining the vulcanizable elastomer as described herein. The present disclosure further discloses a vulcanized composition obtained by a process as disclosed herein.

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Notices, Deadlines & Correspondence

Patent Information

Application #
Filing Date
02 November 2018
Publication Number
19/2020
Publication Type
INA
Invention Field
POLYMER TECHNOLOGY
Status
Email
iprdel@lakshmisri.com
Parent Application
Patent Number
Legal Status
Grant Date
2024-02-08
Renewal Date

Applicants

CEAT LIMITED
RPG HOUSE, 463, Dr. Annie Besant Road, Worli, Mumbai 400 030, India

Inventors

1. BHADRA, Sambhu
CEAT Ltd; At: Getmuwala; PO: Chandrapura; Ta: Halol Dist.: Panchamahal, Gujarat 389350, India
2. NAIR, Sujith Sasidharan
CEAT Ltd; At: Getmuwala; PO: Chandrapura; Ta: Halol Dist.: Panchamahal, Gujarat 389350, India
3. Nitin Mohan
CEAT Ltd; At: Getmuwala; PO: Chandrapura; Ta: Halol Dist.: Panchamahal, Gujarat 389350, India

Specification

FORM 2
THE PATENTS ACT, 1970 (39 of 1970)
&
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(See section 10, rule 13)
1. Title of the invention: ENVIRONMENT-FRIENDLY VULCANIZABLE ELASTOMER
COMPOSITION, AND IMPLEMENTATIONS THEREOF
2. Applicant(s)

NAME NATIONALITY ADDRESS
CEAT LIMITED Indian RPG HOUSE, 463, Dr. Annie Besant Road, Worli, Mumbai 400 030, India
3. Preamble to the description
COMPLETE SPECIFICATION
The following specification particularly describes the invention and the manner in which it
is to be performed.

TECHNICAL FIELD
[0001] The subject matter described herein in general relates to vulcanizable
elastomer composition and in particular relates to elastomer composition comprising
bio-products.
BACKGROUND OF INVENTION
[0002] Vulcanizable elastomer compositions are used to obtain vulcanized elastomer which in turn has numerous applications in the field. Vulcanization is a chemical process which comprises heating elastomers in the presence of a cross-linking agent at a specific temperature range so as to result in cross-linking between rubber polymers, to obtain the vulcanized product. The vulcanization process results in enhanced tensile strength, elasticity, viscosity, resilience, and hardness of the vulcanized product. Sulphur is generally used as the cross-linker which initiates the cross-linking among the polymers. Since the invention of the vulcanization process by Charles Goodyear in 1839, cross-linking reactions have considerably improved as a result of constant research in the area of activators, retarders, accelerators, which can modulate the cross-linking reactions to yield products with improved mechanical properties.
[0003] Zinc oxide and stearic acid are well-known activators of the vulcanization process for achieving optimum mechanical properties. Sulphur is the most commonly used cross-linking agent used in case of elastomers and particularly in case of diene rubbers. Sulphur can initiate cross-linking even in absence of any promoters provided it has an optimum temperature range for the reaction. Vulcanizable elastomers further comprise certain ingredients that can be used as fillers like carbon black and silica which add bulk to the composition.
[0004] Owing to the increasing environmental concerns over the disposal of such vulcanized elastomers, constant research is ongoing to arrive at improved compositions which when vulcanized shall give rise to an environmentally benign vulcanized elastomer.

[0005] US6274662 discloses vulcanizable elastomeric compositions having enhanced dampening properties, among other things, in which the elastomeric composition contains surface-treated barium sulfate particles formed of a plurality of barium sulfate particles and a reaction product of the barium sulfate and silicon-hydride containing polysiloxane integrally located on the surfaces of the barium sulfate particles.
[0006] US20120316283 discloses elastomer compositions comprising reclaimed elastomer material (micronized rubber powder) of broad particle size distribution, which is less expensive than traditional reclaimed elastomer material with narrow particle size distribution.
[0007] In view of the shortcomings of the prior art, the present disclosure provides an environmentally-friendly vulcanizable composition.
SUMMARY OF THE INVENTION
[0008] In an aspect of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent.
[0009] In another aspect of the present disclosure, there is provided a process for preparing the vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, said process comprising: (i) obtaining at least one diene elastomer; (ii) obtaining tapioca flour; (iii) obtaining at least one crosslinking agent; and (iv) contacting the at least one diene elastomer, the tapioca flour, and the at least one crosslinking agent, to obtain the composition.
[0010] These and other features, aspects, and advantages of the present subject matter will be better understood with reference to the following description and appended claims. This summary is provided to introduce a selection of concepts in a simplified form. This summary is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter.
DETAILED DESCRIPTION OF THE INVENTION

[0011] Those skilled in the art will be aware that the present disclosure is subject to
variations and modifications other than those specifically described. It is to be
understood that the present disclosure includes all such variations and modifications.
The disclosure also includes all such steps, features, compositions, and compounds
referred to or indicated in this specification, individually or collectively, and any and
all combinations of any or more of such steps or features.
Definitions
[0012] For convenience, before further description of the present disclosure, certain
terms employed in the specification, and examples are delineated here. These
definitions should be read in the light of the remainder of the disclosure and
understood as by a person of skill in the art. The terms used herein have the meanings
recognized and known to those of skill in the art, however, for convenience and
completeness, particular terms and their meanings are set forth below.
[0013] The articles “a”, “an” and “the” are used to refer to one or to more than one
(i.e., to at least one) of the grammatical object of the article.
[0014] The terms “comprise” and “comprising” are used in the inclusive, open sense,
meaning that additional elements may be included. It is not intended to be construed
as “consists of only”.
[0015] Throughout this specification, unless the context requires otherwise the word
“comprise”, and variations such as “comprises” and “comprising”, will be
understood to imply the inclusion of a stated element or step or group of element or
steps but not the exclusion of any other element or step or group of element or steps.
[0016] The term “including” is used to mean “including but not limited to”.
“Including” and “including but not limited to” are used interchangeably.
[0017] Ratios, concentrations, amounts, and other numerical data may be presented
herein in a range format. It is to be understood that such range format is used merely
for convenience and brevity and should be interpreted flexibly to include not only
the numerical values explicitly recited as the limits of the range, but also to include
all the individual numerical values or sub-ranges encompassed within that range as
if each numerical value and sub-range is explicitly recited. For example, a
temperature range of about 80–250℃ should be interpreted to include not only the

explicitly recited limits of about 80℃ to about 250℃, but also to include sub-ranges, such as 80-200℃, 85-250℃, and so forth, as well as individual amounts, including fractional amounts, within the specified ranges, such as 80.2 ℃, and 240.5 ℃, for example.
[0018] The term “at least one” is used to mean one or more and thus includes individual components as well as mixtures/combinations.
[0019] For the purposes of the present disclosure, the term “tapioca flour” is used to refer to flour obtained from cassava root. It is intended to cover flour obtained from any process using cassava root in any manner. Cassava is the common name for Manihot esculenta, the utility of the tapioca flour as used in the present disclosure is not limited to a particular variety of M esculenta from which flour is processed. The tapioca flour used as part of the present disclosure was procured commercially. ‘Bio-product’ refers to a product obtained from a biological source. [0020] For the purposes of the present disclosure, the term “phr” refers to parts per hundred rubber, it is a unit well used in the field of rubber technology to define the amount of ingredients used.
[0021] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the disclosure, the preferred methods, and materials are now described. All publications mentioned herein are incorporated herein by reference.
[0022] The present disclosure is not to be limited in scope by the specific embodiments described herein, which are intended for the purposes of exemplification only. Functionally-equivalent products, compositions, and methods are clearly within the scope of the disclosure, as described herein. [0023] Addressing the need of the hour to produce environmentally benign products, the present disclosure discloses vulcanizable elastomer composition comprising tapioca flour. The composition of the present disclosure provides a solution in terms of producing environment-friendly vulcanized elastomers, which can further be used in various products having day-to-day applications. The present disclosure, thereby,

discloses a composition comprising a bio-degradable material that is easily available
and abundant in supply. Further, the disclosure identifies the criticality of
vulcanizable elastomer composition by providing the specific concentration ranges
of tapioca flour that can be used in the composition. Additionally, the effect of
tapioca flour in comparison with other known flour on the properties of the
vulcanized composition has been provided for indicating the surprising effect
achieved.
[0024] The present disclosure discloses a vulcanizable elastomer composition
comprising diene elastomer, tapioca flour, crosslinking agent, and additives
including activator, processing aid, antioxidant, filler, coupling agent, accelerator,
and retarder. The present disclosure also discloses a process for obtaining the
vulcanizable elastomer composition as disclosed herein. Also disclosed is a
vulcanized composition obtained from the vulcanizable elastomer composition as
described herein along with a process to obtain the same.
[0025] In an embodiment of the present disclosure, there is provided a vulcanizable
elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour;
and (c) at least one crosslinking agent.
[0026] In an embodiment of the present disclosure, there is provided a vulcanizable
elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour;
and (c) at least one crosslinking agent, wherein the tapioca flour has a concentration
in a range of 5-20 phr. In another embodiment, the tapioca flour has a concentration
in a range of 6-15 phr.
[0027] In an embodiment of the present disclosure, there is provided a vulcanizable
elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour;
and (c) at least one crosslinking agent, wherein the tapioca flour has a concentration
in a range of 7.5-20 phr.
[0028] In an embodiment of the present disclosure, there is provided a vulcanizable
elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour;
and (c) at least one crosslinking agent, wherein the tapioca flour has a concentration
in a range of 5-20 phr, and wherein the at least one crosslinking agent is present in a
range of 1.0-3.0 phr.

[0029] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, wherein the tapioca flour has a concentration in a range of 5-16 phr. In another embodiment, the tapioca flour has a concentration in a range of 6-12 phr. In yet another embodiment, the tapioca flour has a concentration in a range of 6-10 phr.
[0030] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition as described herein, wherein the at least one diene elastomer is selected from a group consisting of styrene butadiene elastomer (SBR), butadiene elastomer, polyisoprene, polychloroprene, ethylene propylene diene monomer rubber (EPDM), and combinations thereof.
[0031] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition as described herein, wherein the at least one diene elastomer is a combination of styrene butadiene elastomer (SBR) and butadiene elastomer. [0032] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition as described herein, wherein the at least one crosslinking agent is selected from a group consisting of sulphur, peroxides, acetoxysilanes, urethanes, metal oxides, and combinations thereof.
[0033] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition as described herein, wherein the at least one crosslinking agent is sulphur.
[0034] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof.
[0035] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, wherein the tapioca flour has a

concentration in a range of 5-20 phr. In another embodiment, the tapioca flour has a concentration in a range of 5-15 phr. In yet another embodiment, the tapioca flour has a concentration in a range of 6-10 phr. In an alternate embodiment, the tapioca flour has a concentration in a range of 7-9 phr.
[0036] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, wherein the tapioca flour has a concentration in a range of 7.5-20 phr.
[0037] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, wherein the activator is selected from a group consisting of zinc oxide, stearic acid, and combinations thereof, having a concentration in a range of 3-8 phr; the processing aid is selected from a group consisting of treated distillate aromatic extracted (TDAE) oil, aromatic oil, paraffinic oil, naphthenic oil, heavy naphthenic oil, spinder oil & RAE (residual aromatic extract), and combinations thereof, having a concentration in a range of 5-30 phr; the antioxidant is selected from a group consisting of N-(1,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine (6PPD), wax, 2,2,4-trimethyl-1,2-dihydroquinoline (TMQ), 1,2-dihydro-2,2,4-trimethylquinoline (TMDQ) and N-isopropyl-N’-phenyl-P-phenylenediamine (IPPD), and combinations thereof, having a concentration in a range of 1-5 phr; the filler is selected from a group consisting of carbon black, silica, talc, clay, calcium carbonate, carbon fibre, glass, polyester, polyamide, natural fibers, and combinations thereof, having a concentration in a range of 10-80 phr; the coupling agent is silane, having a concentration in a range of 0.5-10 phr; the accelerator is selected from a group consisting of diphenylguanidine (DPG), N-cyclohexyl-2-benzothiazole sulfenamide (CBS), and combinations thereof, having a

concentration in a range of 0.5-3.5 phr; the retarder is N-cyclohexylthio-phthalimide (CTP), having a concentration in a range of 0.05-0.8 phr.
[0038] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition as described herein, wherein the at least one crosslinking agent is present in a range of 1.0-3.0 phr.
[0039] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer selected from a group consisting of styrene butadiene elastomer (SBR), butadiene elastomer, polyisoprene, polychloroprene, ethylene propylene diene monomer rubber (EPDM), and combinations thereof; (b) tapioca flour; and (c) at least one crosslinking agent selected from a group consisting of sulphur, peroxides, acetoxysilanes, urethanes, metal oxides, and combinations thereof, wherein the tapioca flour has a concentration in a range of 5-20 phr.
[0040] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer selected from a group consisting of styrene butadiene elastomer (SBR), butadiene elastomer, polyisoprene, polychloroprene, ethylene propylene diene monomer rubber (EPDM), and combinations thereof; (b) tapioca flour; and (c) at least one crosslinking agent selected from a group consisting of sulphur, peroxides, acetoxysilanes, urethanes, metal oxides, and combinations thereof, wherein the tapioca flour has a concentration in a range of 5-20 phr, and wherein the at least one crosslinking agent is present in a range of 1.0-3.0 phr.
[0041] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer selected is a combination of styrene butadiene elastomer (SBR) and butadiene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent selected from a group consisting of sulphur, peroxides, acetoxysilanes, urethanes, metal oxides, and combinations thereof, wherein the tapioca flour has a concentration in a range of 5-20 phr. In another embodiment, the at least one crosslinking agent is sulphur.
[0042] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour;

(c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, wherein the tapioca flour has a concentration in a range of 5-20 phr.
[0043] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, wherein the tapioca flour has a concentration in a range of 5-20 phr, and wherein the at least one crosslinking agent is present in a range of 1.0-3.0 phr.
[0044] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer selected from a group consisting of styrene butadiene elastomer (SBR), butadiene elastomer, polyisoprene, polychloroprene, ethylene propylene diene monomer rubber (EPDM), and combinations thereof; (b) tapioca flour; (c) at least one crosslinking agent selected from a group consisting of sulphur, peroxides, acetoxysilanes, urethanes, metal oxides, and combinations thereof; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, wherein the tapioca flour has a concentration in a range of 5-20 phr, and wherein the at least one crosslinking agent is present in a range of 1.0-3.0 phr.
[0045] In an embodiment of the present disclosure, there is provided a vulcanizable elastomer composition comprising: (a) at least one diene elastomer selected from a group consisting of styrene butadiene elastomer (SBR), butadiene elastomer, polyisoprene, polychloroprene, ethylene propylene diene monomer rubber (EPDM), and combinations thereof; (b) tapioca flour; (c) at least one crosslinking agent selected from a group consisting of sulphur, peroxides, acetoxysilanes, urethanes, metal oxides, and combinations thereof; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, wherein the tapioca flour has a

concentration in a range of 5-20 phr, and wherein the at least one crosslinking agent
is present in a range of 1.0-3.0 phr, and wherein the activator is selected from a group
consisting of zinc oxide, stearic acid, and combinations thereof, having a
concentration in a range of 3-8 phr; the processing aid is selected from a group
consisting of treated distillate aromatic extracted (TDAE) oil, steric acid, aromatic
oil, paraffinic oil, naphthenic oil, heavy naphthenic oil, spinder oil, residual aromatic
extract (RAE), and combinations thereof, having a concentration in a range of 5-30
phr; the antioxidant N-(1,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine (6PPD),
wax, 2,2,4-trimethyl-1,2-dihydroquinoline (TMQ), 1,2-dihydro-2,2,4-
trimethylquinoline (TMDQ) and N-isopropyl-N’-phenyl-P-phenylenediamine (IPPD), and combinations thereof, having a concentration in a range of 1-5 phr; the filler is selected from a group consisting of carbon black, silica, talc, clay, calcium carbonate, carbon fibre, glass, polyester, polyamide, natural fibers, and combinations thereof, having a concentration in a range of 10-80 phr; the coupling agent is silane, having a concentration in a range of 0.5-10 phr; the accelerator is selected from a group consisting of diphenylguanidine (DPG), N-cyclohexyl-2-benzothiazole sulfenamide (CBS), and combinations thereof, having a concentration in a range of 0.5-3.5 phr; the retarder is N-cyclohexylthio-phthalimide (CTP), having a concentration in a range of 0.05-0.8 phr. In another embodiment, the activator has a concentration in a range of 4-7 phr; the processing aid has a concentration in a range of 7-25 phr; the antioxidant has a concentration in a range of 1-3 phr; the filler has a concentration in a range of 30-80 phr; the coupling agent has a concentration in a range of 5-10 phr; the accelerator has a concentration in a range of 1.5-3.5 phr; the retarder has a concentration in a range of 0.1-0.7 phr.
[0046] In an embodiment of the present disclosure, there is provided a vulcanized elastomer obtained from a vulcanizable elastomer as described herein.
[0047] In an embodiment of the present disclosure, there is provided a vulcanized elastomer obtained from a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent. [0048] In an embodiment of the present disclosure, there is provided a vulcanized elastomer obtained from a vulcanizable elastomer composition comprising: (a) at

least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, wherein the tapioca flour has a concentration in a range of 5-20 phr. In another embodiment, the tapioca flour has a concentration in a range of 6-15 phr. [0049] In an embodiment of the present disclosure, there is provided a vulcanized elastomer obtained from a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, wherein the tapioca flour has a concentration in a range of 7.5-20 phr.
[0050] In an embodiment of the present disclosure, there is provided a vulcanized elastomer obtained from a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, wherein the tapioca flour has a concentration in a range of 5-20 phr, and wherein the at least one crosslinking agent is present in a range of 1.0-3.0 phr.
[0051] In an embodiment of the present disclosure, there is provided a vulcanized elastomer obtained from a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof. [0052] In an embodiment of the present disclosure, there is provided a vulcanized elastomer obtained from a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, wherein the tapioca flour has a concentration in a range of 5-20 phr.
[0053] In an embodiment of the present disclosure, there is provided a vulcanized elastomer obtained from a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, wherein the tapioca flour has a concentration in a range of 5-20 phr, and wherein the at least one crosslinking agent is present in a range of 1.0-3.0 phr. In another embodiment, the activator is selected from a group consisting of zinc oxide, stearic

acid, and combinations thereof, having a concentration in a range of 3-8 phr; the
processing aid is selected from a group consisting of treated distillate aromatic
extracted (TDAE) oil, steric acid, aromatic oil, paraffinic oil, naphthenic oil, heavy
naphthenic oil, spinder oil, residual aromatic extract (RAE), and combinations
thereof, having a concentration in a range of 5-30 phr; the antioxidant N-(1,3-
dimethylbutyl)-N’-phenyl-p-phenylenediamine (6PPD), wax, 2,2,4-trimethyl-1,2-
dihydroquinoline (TMQ), 1,2-dihydro-2,2,4-trimethylquinoline (TMDQ) and N-
isopropyl-N’-phenyl-P-phenylenediamine (IPPD), and combinations thereof, having
a concentration in a range of 1-5 phr; the filler is selected from a group consisting of
carbon black, silica, talc, clay, calcium carbonate, carbon fibre, glass, polyester,
polyamide, natural fibers, and combinations thereof, having a concentration in a
range of 10-80 phr; the coupling agent is silane, having a concentration in a range of
0.5-10 phr; the accelerator is selected from a group consisting of diphenylguanidine
(DPG), N-cyclohexyl-2-benzothiazole sulfenamide (CBS), and combinations
thereof, having a concentration in a range of 0.5-3.5 phr; the retarder is N-
cyclohexylthio-phthalimide (CTP), having a concentration in a range of 0.05-0.8 phr.
[0054] In an embodiment of the present disclosure, there is provided a vulcanized
elastomer obtained from a vulcanizable elastomer composition comprising: (a) at
least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and
(d) at least one additive selected from a group consisting of activator, processing aid,
antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof,
wherein the activator is selected from a group consisting of zinc oxide, stearic acid,
and combinations thereof, having a concentration in a range of 3-8 phr; the
processing aid is selected from a group consisting of treated distillate aromatic
extracted (TDAE) oil, aromatic oil, paraffinic oil, naphthenic oil, heavy naphthenic
oil, spinder oil & residual aromatic extract (RAE), and combinations thereof, having
a concentration in a range of 5-30 phr; the antioxidant is selected from a group
consisting of N-(1,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine (6PPD), wax,
2,2,4-trimethyl-1,2-dihydroquinoline (TMQ), 1,2-dihydro-2,2,4-trimethylquinoline
(TMDQ) and N-isopropyl-N’-phenyl-P-phenylenediamine (IPPD), and
combinations thereof, having a concentration in a range of 1-5 phr; the filler is

selected from a group consisting of carbon black, silica, talc, clay, calcium carbonate, carbon fibre, glass, polyester, polyamide, natural fibers, and combinations thereof, having a concentration in a range of 10-80 phr; the coupling agent is silane, having a concentration in a range of 0.5-10 phr; the accelerator is selected from a group consisting of diphenylguanidine (DPG), N-cyclohexyl-2-benzothiazole sulfenamide (CBS), and combinations thereof, having a concentration in a range of 0.5-3 phr; the retarder is N-cyclohexylthio-phthalimide (CTP), having a concentration in a range of 0.05-0.8 phr.
[0055] In an embodiment of the present disclosure, there is provided a process for preparing a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, said process comprising: (i) obtaining at least one diene elastomer; (ii) obtaining tapioca flour; (iii) obtaining at least one crosslinking agent; and (iv) contacting the at least one diene elastomer, the tapioca flour, and the at least one crosslinking agent, to obtain the composition.
[0056] In an embodiment of the present disclosure, there is provided a process for preparing a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, said process comprising: (i) obtaining at least one diene elastomer; (ii) obtaining tapioca flour; (iii) obtaining at least one crosslinking agent; and (iv) contacting the at least one diene elastomer, the tapioca flour, and the at least one crosslinking agent, to obtain the composition, wherein the tapioca flour has a concentration in a range of 5-20 phr. [0057] In an embodiment of the present disclosure, there is provided a process for preparing a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, said process comprising: (i) obtaining at least one diene elastomer; (ii) obtaining tapioca flour; (iii) obtaining at least one crosslinking agent; (iv) obtaining at least one additive; and (v) contacting the at least one diene elastomer, the tapioca flour, the at least one additive, and the at least one crosslinking agent, to obtain the composition.

[0058] In an embodiment of the present disclosure, there is provided a process for preparing a vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, said process comprising: (i) obtaining at least one diene elastomer; (ii) obtaining tapioca flour; (iii) obtaining at least one crosslinking agent; (iv) obtaining at least one additive; and (v) contacting the at least one diene elastomer, the tapioca flour, the at least one additive, and the at least one crosslinking agent, to obtain the composition, wherein the tapioca flour has a concentration in a range of 7.5-20 phr. [0059] In an embodiment of the present disclosure, there is provided a process for preparing a vulcanizable elastomer composition as described herein, wherein the temperature is maintained in a range of 120°C-170°C.
[0060] In an embodiment of the present disclosure, there is provided a process for preparing a vulcanizable elastomer composition as described herein, wherein the rpm is maintained in a range of 40 rpm-75 rpm.
[0061] In an embodiment of the present disclosure, there is provided a process for obtaining a vulcanized elastomer from the vulcanizable elastomer composition as described herein, said process comprising: (a) obtaining the composition as described herein; and (b) thermally treating the composition at a temperature in a range of 80 - 250 ℃ to obtain the vulcanized elastomer.
[0062] In an embodiment of the present disclosure, there is provided a process for obtaining a vulcanized elastomer from the vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, said process comprising: (i) obtaining the vulcanizable elastomer composition; and (ii) thermally treating the composition at a temperature in a range of 80 - 250 ℃ to obtain the vulcanized elastomer.
[0063] In an embodiment of the present disclosure, there is provided a process for obtaining a vulcanized elastomer from the vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; (c) at least one crosslinking agent; and (d) at least one additive selected from a group consisting of

activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof, said process comprising: (i) obtaining the vulcanizable elastomer composition; and (b) thermally treating the composition at a temperature in a range of 80 - 250 °C to obtain the vulcanized elastomer. [0064] In an embodiment of the present disclosure, there is provided a process for obtaining a vulcanized elastomer from the vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, said process comprising: (i) obtaining the vulcanizable elastomer composition; and (ii) thermally treating the composition at a temperature in a range of 80 - 250 °C to obtain the vulcanized elastomer, wherein the tapioca flour has a concentration in a range of 5-20 phr. In another embodiment, the tapioca flour has a concentration in a range of 6-15 phr.
[0065] In an embodiment of the present disclosure, there is provided a process for obtaining a vulcanized elastomer from the vulcanizable elastomer composition comprising: (a) at least one diene elastomer; (b) tapioca flour; and (c) at least one crosslinking agent, said process comprising: (i) obtaining the vulcanizable elastomer composition; and (ii) thermally treating the composition at a temperature in a range of 80 - 250 °C to obtain the vulcanized elastomer, wherein the tapioca flour has a concentration in a range of 5-20 phr, and wherein the at least one crosslinking agent is present in a range of 1.0-3.0 phr.
[0066] In an embodiment of the present disclosure, there is provided a process for obtaining a vulcanized elastomer from the vulcanizable elastomer composition comprising: (a) at least one diene elastomer; selected from a group consisting of styrene butadiene elastomer (SBR), butadiene elastomer, polyisoprene, polychloroprene, ethylene propylene diene monomer rubber (EPDM), and combinations thereof; (b) tapioca flour; and (c) at least one crosslinking agent selected from a group consisting of sulphur, peroxides, acetoxysilanes, urethanes, metal oxides, and combinations thereof, said process comprising: (i) obtaining the vulcanizable elastomer composition; and (ii) thermally treating the composition at a temperature in a range of 80 - 250 °C to obtain the vulcanized elastomer, wherein the tapioca flour has a concentration in a range of 5-20 phr, and wherein the at least

one crosslinking agent is present in a range of 1.0-3.0 phr. In another embodiment, treating the composition is done at a temperature in a range of 90 - 200 ℃ to obtain the vulcanized elastomer. In yet another embodiment, treating the composition is done at a temperature in a range of 95 - 180 ℃ to obtain the vulcanized elastomer. [0067] In an embodiment of the present disclosure, there is provided a vulcanized elastomer as described herein, wherein the vulcanized elastomer for use in products including not limited to tires, hose, conveyor belt, boat, dock fenders, mats, hot water bags, O rings, rail pads, rubber rollers, and similar vulcanizable elastomeric products.
EXAMPLES
[0068] The disclosure will now be illustrated with working examples, which is intended to illustrate the working of disclosure and not intended to take restrictively to imply any limitations on the scope of the present disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood to one of ordinary skill in the art to which this disclosure belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice of the disclosed methods and compositions, the exemplary methods, devices and materials are described herein. It is to be understood that this disclosure is not limited to particular methods, and experimental conditions described, as such methods and conditions may apply.
[0069] The present disclosure provides a vulcanizable elastomer (mix) comprising tapioca flour, to improve ageing properties and fatigue properties of the vulcanized composition. Furthermore, the addition of tapioca flour results in the acceleration of sulphur curing reaction during the vulcanization of diene elastomers. The following examples depict the properties of vulcanized elastomer composition obtained from using different concentrations of tapioca flour along with additives as mentioned in the present disclosure.
Example 1
Process for preparation of the vulcanizable elastomer composition
[0070] Elastomer composition was selected containing a diene elastomer, more
specifically, solution of styrene butadiene elastomer (SBR) and another diene

elastomer, more specifically, butadiene elastomer (BR). Furthermore, zinc oxide (ZnO) as activator, stearic acid (St-acid) as processing aid, N-(1,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine (6 PPD) and wax as antioxidant, carbon black and silica as filler, silane as coupling agent for silica filler, treated distillate aromatic extracted oil (TDAE oil) as processing aid, sulphur as crosslinking agent, N-cyclohexyl-2-benzothiazole sulfonamide (CBS) and diphenylguanidine (DPG) as accelerator, and N-cyclohexylthio-phthalimide (CTP) as retarder were used. Tapioca flour was used in the composition to improve the characteristics of vulcanized elastomer obtained after vulcanizing the composition.
[0071] Kobelco intermix, Mixtron BB-L3200 IM, Kobe, Japan was employed to melt and mix the elastomer in the vulcanization mix. A fill factor (FF) of 62% was employed. The mixing was carried out in three steps; (i) preparation of master, (ii) repass, (iii) final mixing with curatives.
[0072] Step 1- Preparation of master: At first, all rubbers/elastomers were incorporated and mixed for 45 seconds at a speed of 60 rpm. Then half of all ingredients (except curative system- i.e. sulphur, CBS, DPG and CTB) were incorporated and mixed again for 60 seconds at a speed of 60 rpm. After that, the remaining half of the ingredients were incorporated and mixed again for 45 seconds at a speed of 60 rpm. Finally, the mixing was continued for 340 seconds to obtain the master. At this stage, the rpm was varied to maintain the temperature at 150 °C. [0073] Step 2- Repass: The master was kept overnight for relaxation. Next day, it was re-mixed for 210 seconds at 70 rpm.
[0074] Step 3- Final mixing with curatives: All the master and curatives were incorporated and mixed for 200 seconds to obtain the vulcanization mix. At this stage, the temperature was maintained below 100 °C through rpm control. The vulcanization mix was cured/vulcanized by thermally treating the mix at 160 °C for T90 + 5 minutes to obtain the vulcanized elastomers (T90 is the time required to complete 90% vulcanization).
Example 2
Characterization and testing of the vulcanized elastomer

[0075] After final mixing, the rheometric tests were performed at 160 °C using Moving Die Rheometer, MDR 3000, MonTech, and Mooney viscosity (ML 1+4) at 100 °C using Mooney Viscometer, and VR-1132, Ueshima, Japan. As mentioned above, the vulcanization mix was cured/vulcanized by thermally treating the mix at 160 °C for T90 + 5 minutes. Stress vs. strain and tear test were performed using Universal testing machine (UTM), Strograph AE, Toyoseiki and hardness was measured using Durometer, MonTech. Fatigue to failure (FTFT) test was performed using FTFT-Monsanto, SG 48, SG Electricals and Electronics, India, heat buildup was tested using Flexometer, FT-1260, Ueshima, Japan, H-adhesion test was performed using Zwick-Roell, ALLROUND Z010, Zwick, Germany, DMA test was performed using Eplexor 500N, Gabo, Germany. A tabulation of the ingredients used and various parameters established are listed below in Table 1.
Table 1: Table listing the effect of the presence of tapioca flour on the properties of vulcanized composition

Step 1: M1
RM Code ↓ Sample No → 1 3
Sample description→ Control Tapioca flour
SBR 70.00 70.00
BR 30.00 30.00
ZnO 3.00 3.00
Stearic acid 2.00 2.00
6 PPD 2.50 2.50
Wax 2.00 2.00
Tapioca flour 0.00 10.00
Carbon black 10.00 10.00
Silica 60.00 60.00
Silane coupling agent 9.60 9.60
TDAE oil 20.00 20.00
Step 2: Repass
Step 3: Final mixing with M1
Sulphur 1.818 1.818
CBS 1.400 1.400
DPG 1.800 1.800
CTP 0.200 0.200
PROPERTIES
Specific Gravity 1.1727 1.1902
RHEO (MDR): 160°CX45'
ML (dN-m) 1.71 1.73
MHF/MHR/MH (dN-m) 19.52 19.46

MH-ML (dN-m) 17.81 17.73
FINAL S' (dN-m) 19.51 19.44
ts - 1 Mins 2.74 1.93
ts - 2 Mins 3.86 2.44
ts - 10 Mins 3.68 2.35
ts - 30 Mins 5.16 3.04
ts - 50 Mins 6.01 3.64
ts - 90 Mins 15.89 9.56
ts - 95 Mins 23.05 13.47
t'max Mins 44.76 44.52
MIN - TAN DELTA 1.02 1.04
TAN - DELTA @ t 95 0.2 0.23
S" @ t 95 (dN-m) 3.74 4.3
S" @ ML (dN-m) 1.74 1.79
ML (1+4) @ 100oC 70.6 68.5
Mooney Scorch @ 125oC
ML (1 + 4) 45.6 45.4
MV 41.8 42.8
ML 5 UP Mins 43.1 25
Curing (T90 + 5 min)
STRESS-STRAIN (Ambient)
50% MODULUS (Kg/cm2) 13.65 14.48
100% MODULUS (Kg/cm2) 23.40 25.18
200% MODULUS (Kg/cm2) 54.09 57.74
300% MODULUS (Kg/cm2) 99.42 98.31
400% MODULUS (Kg/cm2) 148.61 139.90
TENSILE STRENGTH (Kg/cm2) 167.41 152.05
ELONGATION AT BREAK % 440.2 420.4
M300% / M50% 7.28 6.78
TENSILE STRENGTH SD 12.36 9.91
HARDNESS SHORE A 66 67
STRESS-STRAIN (after ageing)
50% MODULUS (Kg/cm2) 15.80 16.44
100% MODULUS (Kg/cm2) 27.30 29.51
200% MODULUS (Kg/cm2) 62.03 67.67
300% MODULUS (Kg/cm2) 109.7 111.5
400% MODULUS (Kg/cm2) 0 157.0
TENSILE STRENGTH (Kg/cm2) 150.2 166.2
ELONGATION AT BREAK % 385.8 428.2
M300% / M50% 6.94 6.78
TENSILE STRENGTH SD 6.80 4.93
HARDNESS (Shore A) 68 68
Changes after aging (%)
Change in 300% MODULUS 10.42 13.43
Change in TENSILE STR. -10.26 9.31
% Change in ELONGATION -12.35 1.85
Change in Hardness (Shore A) 2 1
DMA, ISOTHERMAL AT 60oC
Storage modulus, E’ (MPa) 9.229 9.996
Loss modulus, E” (MPa) 1.132 1.301
Tan delta 0.123 0.130
H ADHESION

CORD DETAILS 1680/2 1680/2
PULL-OUT FORCE (Kgs) 20.983 19.500
CORD CONDITION SR SR
Angle Tear (T): Ambient: ORI-SC
ANGLE TEAR STRENGTH (Kg/cm) 40.60 38.22
EXTENSION % 140.05 120.92
Min 36 35
Max 42 40
Angle Tear (T): B1
ANGLE TEAR STRENGTH (Kg/cm) 39.50 36.86
EXTENSION % 115.34 105.46
Min 37 36
Max 41 38
TGA
Volatile 11.1 15.1
Rubber 1 0 0
Rubber 2 100 100
Carbon black 14.6 15.5
Ash 49.4 49.8
Total 175.1 180.4
Flexometer HBU Constant Strain
After 10 min
TANDELTA 0.1709 0.17325
E1(Mpa) 9.6705 9.8155
E2(Mpa) 1.6605 1.7005
TEMP(C) 81.9 81.45
CREEP (%) 17.65 17.2
Average Heat Build-up 31.9 31.45
After 20 Min.
TAN DELTA 0.1691 0.17175
E1(Mpa) 9.6985 9.815
E2(Mpa) 1.64 1.6865
TEMP(C) 83.25 83
CREEP (%) 17.75 17.4
Average Heat Build-up 33.25 33
FTFT
ORIGINAL 100% (AVH3) KC 27 39
ORIGINAL 100% (GMH3) KC 22 39
ORIGINAL 100% (MEDAIN6) KC 14 34
S.D 17 8
HIGH-LOW 51-9 66-27
[0076] Sample 1 lacks tapioca flour and sample 2 has a concentration of 10 phr of tapioca flour. As observed from Table 1, the elastomer containing 10 phr of tapioca flour (Sample no. 1) was found to display high tensile strength (166.2 Kg/cm2) and elongation at break (428.2%) after ageing at 80oC for 7 days. Also, fatigue to failure

(FTFT) property is enhanced for sample 2 (39) than that of sample 1 (27). The observations indicate that the addition of tapioca flour improves the FTFT property of the vulcanized diene elastomer composition. The data also indicate that on the addition of tapioca flour, tensile strength and elongation at break increases after ageing. Further, as per the T50 (ts-50 minutes) and T90 (ts-90 minutes) data (T50 and T90 is the time required to complete 50% and 90% vulcanization respectively) shown in Table 1, it can be appreciated that upon addition of 10 phr of tapioca flour, reduction in curing time can be observed, suggesting that tapioca flour helps in accelerating the curing time. Overall, the elastomer containing 10 phr tapioca flour was found to yield high-quality vulcanized elastomer displaying better mechanical properties after ageing.
Example 3
Elastomer compositions comprising other elements other than tapioca flour
[0077] The properties of elastomer composition were studied by using rice flour
and maize flour independently instead of tapioca flour.
[0078] Table 2 depicts the properties of composition made using rice flour and
maize flour versus tapioca flour.

Step 1: M1
RM Name Grade Code Control Maize flour Rice flour Tapioca flour
S-SBR R4601 70.0 70.0 70.0 70.0
BR 1678 30.0 30.0 30.0 30.0
ZnO 135 3.0 3.0 3.0 3.0
St-acid 224 2.0 2.0 2.0 2.0
6 PPD 727 2.5 2.5 2.5 2.5
Wax 582 2.0 2.0 2.0 2.0
- - 0.0 10.0 10.0 10.0
Carbon black N234 N234 10.0 10.0 10.0 10.0
Silica 7000GR 3029 60.0 60.0 60.0 60.0
Silane Si266 6266 9.6 9.6 9.6 9.6
TDAE oil 6311 20.0 20.0 20.0 20.0
Step 2: Repass
Step 3: Final mixing with M1
Sulphur 5299 1.82 1.82 1.82 1.82
CBS 327 1.4 1.4 1.4 1.4
DPG 146 1.8 1.8 1.8 1.8
CTP 774 0.2 0.2 0.2 0.2
Properties

Rheological
TC 50 (min) 5.9 6.1 6.2 4.6
TC 90 (min) 17 18.9 19.2 13.3
MH – ML (dN.m) 20 21.8 21.7 20.1
STRESS-STRAIN (Cured at T90 time + 5 min)
50% MODULUS (Kg/cm2) 14.4 16.9 16.8 15.4
100% MODULUS (Kg/cm2) 23.4 28.2 27.6 25.3
200% MODULUS (Kg/cm2) 50.8 58.7 53.3 55.0
300% MODULUS (Kg/cm2) 89.9 91.6 87.2 89
400% MODULUS (Kg/cm2) 134 131 126 130
TENSILE STRENGTH (Kg/cm2) 162 144 139 144
ELONGATION AT BREAK % 462 433 434 437
M300% / M50% 6.2 5.4 5.2 5.8
TENSILE STRENGTH SD 7.9 8.3 7.4 8.8
HARDNESS SHORE A 67 73 72 69
[0079] For each elastomer composition, wherever flour has been added it has been added at a concentration of 10 phr. The properties of the vulcanized elastomer has been compared to that of control and to that of the composition comprising tapioca flour. The data as depicted in Table 2 suggests that the composition comprising tapioca flour has lower T50 and T90 values (4.6 and 13.3 respectively) as compared to that of the control (5.9 and 17 respectively) and as well as the composition comprising either rice flour (6.2 and 19.2 respectively) or maize flour (6.1 and 18.9 respectively). Thus, indicating the acceleration achieved in curing times. Further, the values of tensile strength and elongation at break are higher for the composition comprising tapioca flour as compared to that of rice flour. Also, the values of elongation at break for composition comprising tapioca flour is higher as compared to the composition comprising maize flour. Therefore, it can be inferred that the desired properties of vulcanized elastomer can only be achieved by using tapioca flour and not by using rice or maize flour. Thus, establishing the experimental effort in arriving at the composition of the present disclosure.
[0080] The properties of tapioca flour along with rice flour and maize flour have been listed out in Table 3 below. Table 3 depicts properties of different type of flours used in the present study:

Maize flour Rice flour Tapioca flour
Test Name

FTIR (Fourier-transform infrared spectroscopy)
% co-relation with maize flour 100 95.86 81.69
DSC (Differential Scanning Calorimetry)
Melting Point (peak) / oC 298 302.42 279.9
Degradation point (peak) /oC 399.2 390.25 417.84
PSA (Particle size analysis)
Particle size D10 9.72 7.92 11.9
Particle size D50 14.68 14.58 25.87
Particle size D90 21.35 126.42 193.16
Halogen moisture analyser
%Moisture 10.98 13.04 9.99
pH 5.6 6.3 6.2
Example 4
Compositions comprising different concentrations of tapioca flour
[0081] Properties of the vulcanized elastomer were studied in the presence of
different concentrations of tapioca flour.
Table 4: Properties of the vulcanized products comprising different concentrations
of tapioca flour.

Step 1: M1
RM Code Sample No→ 1 2 3 4 5
SBR 70.00 70.00 70.00 70.00 70.00
BR 30.00 30.00 30.00 30.00 30.00
ZnO 3.00 3.00 3.00 3.00 3.00
Stearic acid 2.00 2.00 2.00 2.00 2.00
6 PPD 2.50 2.50 2.50 2.50 2.50
Wax 2.00 2.00 2.00 2.00 2.00
Tapioca flour 0.00 5.00 7.50 10.00 20.00
Carbon black 10.00 10.00 10.00 10.00 10.00
Silica 60.00 60.00 60.00 60.00 60.00
Silane coupling agent 9.60 9.60 9.60 9.60 9.60
TDAE oil 10.00 10.00 10.00 10.00 10.00
Step 2: Repass
Step 3: Final m ixing with M1
Sulphur 1.818 1.818 1.818 1.818 1.818
CBS 1.400 1.400 1.400 1.400 1.400
DPG 1.800 1.800 1.800 1.800 1.800
CTP 0.200 0.200 0.200 0.200 0.200

PROPERTIES
Specific Gravity 1.202 1.209 1.194 1.208 1.219
RHEO (MDR): 160°CX45'
ML (dN-m) 1.97 2.02 1.91 1.94 2.11
MHF/MHR/MH (dN-m) 22.01 22.92 22.92 22.96 24.87
MH-ML (dN-m) 20.04 20.9 21.01 21.02 22.76
FINAL S' (dN-m) 21.99 22.92 22.92 22.95 24.87
ts - 1 Mins 3.11 2.73 2.71 2.71 2.27
ts - 2 Mins 4.31 3.8 3.77 3.71 3.15
ts - 10 Mins 4.31 3.86 3.84 3.77 3.31
ts - 30 Mins 5.75 5.12 5.05 4.9 4.4
ts - 50 Mins 6.58 5.95 5.81 5.64 5.23
ts - 90 Mins 16.18 15 14.28 13.96 13.86
ts - 95 Mins 23.09 21.56 20.37 19.86 20.88
t'max Mins 44.78 44.66 44.51 44.83 44.53
MIN - TAN DELTA 1.01 1.01 1.02 1.05 1.07
TAN - DELTA @ t 95 0.24 0.25 0.24 0.24 0.27
S" @ t 95 (dN-m) 5 5.39 5.2 5.28 6.4
S" @ ML (dN-m) 1.99 2.05 1.96 2.02 2.26
ML(1+4) @ 100oC 73.5 73.5 71.3 72.4 73.5
Mooney Scorch @ 125oC
ML ( 1 + 4 ) 40.4 59.4 57.8 58.1 59.1
MV 37.4 55.3 54 54.4 55.8
ML 5 UP Mins 51.1 30.8 28 27.7 24.4
Curing T90 + 5 min)
STRESS-STRAIN (Ambient)
50% MODULUS (Kg/cm2) 16.64 17.28 17.6 18.28 22.21
100% MODULUS (Kg/cm2) 28.97 30.59 31.44 33.31 40.63
200% MODULUS (Kg/cm2) 67.19 72.69 78.61 82.2 89.79
300% MODULUS (Kg/cm2) 122.3 127.1 136 137.3 139.7
400% MODULUS (Kg/cm2) 0 0 0 0 0
TENSILE STRENGTH (Kg/cm2) 153.1 145.8 167.9 168.9 152.8
ELONGATION AT BREAK % 355.3 338 359 359.4 331.9
M300% / M50% 7.3 7.3 7.7 7.5 6.3
TENSILE STRENGTH SD 5.94 14.11 7.77 9.4 14.7
HARDNESS SHORE A 71.3 72.5 72.7 74.7 75.9
STRESS-STRAIN (C2-ageing)
50% MODULUS (Kg/cm2) 23.63 24.52 24.69 25.87 30.82
100% MODULUS (Kg/cm2) 44.68 47.03 47 50.68 60.37
200% MODULUS (Kg/cm2) 106.3 113.4 116.8 122.8 131.1
300% MODULUS (Kg/cm2) 0 0 0 0 0
400% MODULUS (Kg/cm2) 0 0 0 0 0
TENSILE STRENGTH (Kg/cm2) 133.1 143.1 166.7 146.7 145.2
ELONGATION AT BREAK % 241.1 243.9 272.3 237 227.6
M300% / M50% 0 0 0 0 0
TENSILE STRENGTH SD 5.2 6.51 8.15 8.45 9.93
HARDNESS (Shore A) 79 78 79 81 82

Changes after aging (%)
Change in 300% MODULUS 100.0 100.0 100.0 100.0 100.0
Change in TENSILE STR. -13.1 -1.9 -0.7 -13.2 -5.0
% Change in ELONGATION -32.1 -27.8 -24.2 -34.1 -31.4
Change in Hardness (Shore A) 7.70 5.50 6.30 6.30 6.10
FTFT
ORI 100% 30 32 126 74 64
ORIGINAL 100% (AVH3) KC 29 32 120 71 63
ORIGINAL 100% (GMH3) KC 25 25 96 54 50
ORIGINAL 100% (MEDAIN6) KC 8 8 51 26 24
[0082] Table 4 depicts the data for five samples, namely control-sample 1 (without tapioca flour), and samples 2 to 5 comprising 5 phr, 7.5 phr, 10 phr, and 20 phr respectively, of tapioca flour. Referring to Table 4, it can be appreciated that samples 2-5 display better qualities in terms of tensile strength after ageing and FTFT analysis as compared to control-sample 1. Also, the samples 2-5 display an acceleration in curing as depicted by T50 and T90 values as compared to the control. Further, it can be observed that sample 3 comprising 7.5 phr of tapioca flour displays better tensile strength and elongation at break values both before and after ageing as compared to the other samples comprising tapioca flour. Sample 3 also shows better values for FTFT analysis as compared to the other samples. Therefore, it can be inferred that although all the samples comprising tapioca flour shows better properties as compared to the control, however, sample 3 comprising 7.5 phr of tapioca flour shows the best result. It should be noted that the preparation of the elastomer composition comprising more than 20 phr of tapioca flour did not yield good results in terms of desirable properties as compared to the control sample.
[0083] The examples as depicted in the present disclosure succinctly establish the use of tapioca flour in vulcanizable elastomer composition for displaying better mechanical properties in terms of tensile strength and FTFT analysis. Also, it provides a composition which has lower curing time attributed to the presence of tapioca flour in the composition. The vulcanizable elastomer composition as

disclosed in the present disclosure show improvement in aged properties of the vulcanized composition.
Advantages of the present disclosure:
[0084] The present disclosure discloses a vulcanizable elastomer composition comprising tapioca flour for achieving high-quality vulcanized elastomers displaying better mechanical properties in terms of ageing and FTFT. Significant advantages of using tapioca flour include its low-cost, and abundant availability. Also, tapioca flour can be used in its unmodified form in the vulcanizable elastomer composition, thus imparting ease of use along with the economic advantage of avoiding any processing steps. Since tapioca flour is environment-friendly and a biodegradable product, the composition of the present disclosure provides a solution to address the rising environmental concerns regarding pollution caused by rubber products. Also, the final properties of vulcanizates are not compromised upon the addition of tapioca flour.

I/We Claim:
1. A vulcanizable elastomer composition comprising:
a) at least one diene elastomer;
b) tapioca flour; and
c) at least one crosslinking agent.

2. The composition as claimed in claim 1, wherein the tapioca flour has a concentration in a range of 5-20 phr.
3. The composition as claimed in claim 1, wherein the tapioca flour has a concentration in a range of 6-15 phr.
4. The composition as claimed in claim 1, wherein the at least one diene elastomer is selected from a group consisting of styrene butadiene elastomer (SBR), butadiene elastomer, polyisoprene, polychloroprene, ethylene propylene diene monomer rubber (EPDM), and combinations thereof.
5. The composition as claimed in claim 1, wherein the at least one diene elastomer is a combination of styrene butadiene elastomer (SBR) and butadiene elastomer.
6. The composition as claimed in claim 1, wherein the at least one crosslinking agent is selected from a group consisting of sulphur, peroxides, acetoxysilanes, urethanes, metal oxides, and combinations thereof.
7. The composition as claimed in claim 1, wherein the composition further comprises at least one additive selected from a group consisting of activator, processing aid, antioxidant, filler, coupling agent, accelerator, retarder, and combinations thereof.
8. The composition as claimed in claim 7, wherein the activator is selected from a group consisting of zinc oxide, stearic acid, and combinations thereof, having a concentration in a range of 3-8 phr; the processing aid is selected from a group consisting of treated distillate aromatic extracted (TDAE) oil, steric acid, aromatic oil, paraffinic oil, naphthenic oil, heavy naphthenic oil, spinder oil, residual aromatic extract (RAE), and combinations thereof, having a concentration in a range of 5-30 phr; the antioxidant N-(1,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine (6PPD), wax, 2,2,4-

trimethyl-1,2-dihydroquinoline (TMQ), 1,2-dihydro-2,2,4-
trimethylquinoline (TMDQ) and N-isopropyl-N’-phenyl-P-
phenylenediamine (IPPD), and combinations thereof, having a concentration in a range of 1-5 phr; the filler is selected from a group consisting of carbon black, silica, talc, clay, calcium carbonate, carbon fibre, glass, polyester, polyamide, natural fibers, and combinations thereof, having a concentration in a range of 10-80 phr; the coupling agent is silane, having a concentration in a range of 0.5-10 phr; the accelerator is selected from a group consisting of diphenylguanidine (DPG), N-cyclohexyl-2-benzothiazole sulfenamide (CBS), and combinations thereof, having a concentration in a range of 0.5-3.5 phr; the retarder is N-cyclohexylthio-phthalimide (CTP), having a concentration in a range of 0.05-0.8 phr.
9. The composition as claimed in claim 1, wherein the at least one crosslinking agent is present in a range of 1.0-3.0 phr.
10. A vulcanized elastomer obtained from the compositions as claimed in any one of the claims 1-9.
11. A process for preparing the composition as claimed in claim 1, said process comprising:

a) obtaining at least one diene elastomer;
b) obtaining tapioca flour;
c) obtaining at least one crosslinking agent; and
d) contacting the at least one diene elastomer, the tapioca flour, and the at least one crosslinking agent, to obtain the composition.
12. A process for preparing the composition as claimed in claim 7, said process
comprising:
a) obtaining at least one diene elastomer;
b) obtaining tapioca flour;
c) obtaining at least one crosslinking agent;
d) obtaining at least one additive; and

e) contacting the at least one diene elastomer, the tapioca flour, the at least one crosslinking agent, and the at least one additive, to obtain the composition.
13. A process for obtaining the vulcanized elastomer as claimed in claim 10, said process comprising:
a) obtaining the composition as claimed in any one of the claims 1-9; and
b) thermally treating the composition at a temperature in a range of 80 -250 ℃ to obtain the vulcanized elastomer.

Documents

Orders

Section Controller Decision Date

Application Documents

# Name Date
1 201821041672-IntimationOfGrant08-02-2024.pdf 2024-02-08
1 201821041672-STATEMENT OF UNDERTAKING (FORM 3) [02-11-2018(online)].pdf 2018-11-02
2 201821041672-PatentCertificate08-02-2024.pdf 2024-02-08
2 201821041672-PROVISIONAL SPECIFICATION [02-11-2018(online)].pdf 2018-11-02
3 201821041672-Written submissions and relevant documents [25-10-2023(online)].pdf 2023-10-25
3 201821041672-POWER OF AUTHORITY [02-11-2018(online)].pdf 2018-11-02
4 201821041672-FORM 1 [02-11-2018(online)].pdf 2018-11-02
4 201821041672-Correspondence to notify the Controller [10-10-2023(online)].pdf 2023-10-10
5 201821041672-Proof of Right (MANDATORY) [19-12-2018(online)].pdf 2018-12-19
5 201821041672-FORM-26 [06-10-2023(online)].pdf 2023-10-06
6 201821041672-US(14)-ExtendedHearingNotice-(HearingDate-11-10-2023).pdf 2023-10-06
6 201821041672-CORRESPONDENCE-OTHERS [25-10-2019(online)].pdf 2019-10-25
7 201821041672-Correspondence to notify the Controller [05-10-2023(online)].pdf 2023-10-05
7 201821041672-COMPLETE SPECIFICATION [25-10-2019(online)].pdf 2019-10-25
8 201821041672-US(14)-HearingNotice-(HearingDate-09-10-2023).pdf 2023-09-05
8 201821041672-ORIGINAL UR 6(1A) FORM 1-261218.pdf 2019-11-21
9 201821041672--ORIGINAL UR 6(1A) FORM 1-261218.pdf 2019-11-21
9 201821041672-CLAIMS [05-05-2023(online)].pdf 2023-05-05
10 201821041672-FER_SER_REPLY [05-05-2023(online)].pdf 2023-05-05
10 201821041672-FORM 18 [12-10-2022(online)].pdf 2022-10-12
11 201821041672-FER.pdf 2022-11-16
12 201821041672-FER_SER_REPLY [05-05-2023(online)].pdf 2023-05-05
12 201821041672-FORM 18 [12-10-2022(online)].pdf 2022-10-12
13 201821041672--ORIGINAL UR 6(1A) FORM 1-261218.pdf 2019-11-21
13 201821041672-CLAIMS [05-05-2023(online)].pdf 2023-05-05
14 201821041672-ORIGINAL UR 6(1A) FORM 1-261218.pdf 2019-11-21
14 201821041672-US(14)-HearingNotice-(HearingDate-09-10-2023).pdf 2023-09-05
15 201821041672-COMPLETE SPECIFICATION [25-10-2019(online)].pdf 2019-10-25
15 201821041672-Correspondence to notify the Controller [05-10-2023(online)].pdf 2023-10-05
16 201821041672-CORRESPONDENCE-OTHERS [25-10-2019(online)].pdf 2019-10-25
16 201821041672-US(14)-ExtendedHearingNotice-(HearingDate-11-10-2023).pdf 2023-10-06
17 201821041672-FORM-26 [06-10-2023(online)].pdf 2023-10-06
17 201821041672-Proof of Right (MANDATORY) [19-12-2018(online)].pdf 2018-12-19
18 201821041672-Correspondence to notify the Controller [10-10-2023(online)].pdf 2023-10-10
18 201821041672-FORM 1 [02-11-2018(online)].pdf 2018-11-02
19 201821041672-Written submissions and relevant documents [25-10-2023(online)].pdf 2023-10-25
19 201821041672-POWER OF AUTHORITY [02-11-2018(online)].pdf 2018-11-02
20 201821041672-PROVISIONAL SPECIFICATION [02-11-2018(online)].pdf 2018-11-02
20 201821041672-PatentCertificate08-02-2024.pdf 2024-02-08
21 201821041672-STATEMENT OF UNDERTAKING (FORM 3) [02-11-2018(online)].pdf 2018-11-02
21 201821041672-IntimationOfGrant08-02-2024.pdf 2024-02-08

Search Strategy

1 SearchHistoryE_16-11-2022.pdf

ERegister / Renewals

3rd: 02 May 2024

From 02/11/2020 - To 02/11/2021

4th: 02 May 2024

From 02/11/2021 - To 02/11/2022

5th: 02 May 2024

From 02/11/2022 - To 02/11/2023

6th: 02 May 2024

From 02/11/2023 - To 02/11/2024

7th: 02 May 2024

From 02/11/2024 - To 02/11/2025

8th: 16 Oct 2025

From 02/11/2025 - To 02/11/2026