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Process For Preparing Elastomer Composite

Abstract: ABSTRACT PROCESS FOR PREPARING ELASTOMER COMPOSITE The present disclosure provides a continuous process for the preparation of an elastomer composite, said process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone to obtain the elastomer composite. Also disclosed herein is a formulation comprising an elastomer composite.

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Patent Information

Application #
Filing Date
07 October 2019
Publication Number
15/2021
Publication Type
INA
Invention Field
POLYMER TECHNOLOGY
Status
Email
iprdel@lakshmisri.com
Parent Application

Applicants

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

Inventors

1. BHADRA, Sambhu
H 103, Earth Artica, Vasna, Vadodara 390007, India
2. NAIR, Sujith Sasidharan
A402, Fortune heights, Mangal Pandey Road, Sama, Vadodara 390008, India
3. PUROHIT, Vivek
A 204, Orchid Harmony, behind Ambe vidyalya, Sama savli road, Vemali, Vadodara 390008, India
4. SAHA, Tuhin
102, Shyam Residency, Near Anushakti Nagar, Vadodara 390024, 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: PROCESS FOR PREPARING ELASTOMER COMPOSITE
2. Applicant(s)
NAME NATIONALITY ADDRESS
CEAT LIMITED Indian RPG HOUSE, 463, Dr. Annie Besant Road, Worli, Mumbai -Maharashtra 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.

FIELD OF INVENTION
[001] The present disclosure broadly relates the field of rubber composites and
particularly refers to a method of preparing elastomer composites.
BACKGROUND OF INVENTION
[002] Elastomers are polymers that exhibits exceptional elasticity properties Elastomer finds various applications in various fields, including the manufacturing of tires, tubes, medical products, sport equipment’s, and the like. Incorporation of particulate filler into an elastomeric composition provides reinforcement and improves resilience, tear-strength, conductivity and other physical properties to the elastomer. Different mixing processes have been utilized for incorporating particulate filler into an elastomer to obtain the elastomer compositions. [003] Over the years, a wide variety of mixing processes and devices have evolved in the rubber industry. The standard mixing processes generally utilize two-roll mills that helps to modify the basic properties of elastomer and also helps to incorporate enhancing ingredients such as reinforcing agents, modifying oils and curatives. Another processing device that has been disclosed in the literature utilizes internal mixer such as the Banbury-type mixer. The internal mixer mixes the components to form the elastomer composition through a discontinuous process. This process may require several steps to arrive at the final rubber composition.
[004] For instance, US3897070A discloses a banbury type mixer for processing rubber compounds and the like. The document also discloses a method of improving service time availability of a Banbury type mixer by mixing rubber compounds in the region surrounding the connection between the ram and the ram-weight in a Banbury mixer.
[005] EP1035958B1 discloses a simple and an efficient process and automated system that utilises an internal mixer. The internal mixer is provided for controlled mixing of polymeric material and additive materials to obtain quality products and batch to batch product uniformity.

[006] The batch wise process performed by the means of various batch mixing devices as disclosed in the literature are used for producing elastomeric compositions. However, they seem to suffer a significant failure when it comes to meeting the commercial quality standards and high market demands. Thus, there arises a dire need in the present state of art for developing an elastomer producing process that is not only economic in terms of time and cost of processing but also produces quality products.
SUMMARY OF THE INVENTION
[007] In a first aspect of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone to obtain the elastomer composite.
[008] In a second aspect of the present disclosure, there is provided a formulation comprising the elastomer composite prepared by the process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone to obtain the elastomer composite.
[009] 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.
BRIEF DESCRIPTION OF ACCOMPANYING DRAWINGS
[0010] The following drawings form a part of the present specification and are
included to further illustrate aspects of the present disclosure. The disclosure may be
better understood by reference to the drawings in combination with the detailed
description of the specific embodiments presented herein.
[0011] Figure 1 illustrates the schematic diagram of a co-rotating twin screw
extruder (CRTSE) used for the preparing the first mix, in accordance with an
implementation of the present disclosure.
[0012] Figure 2 illustrates the schematic diagram of a co-rotating twin screw
extruder (CRTSE) used for preparing the elastomer composite, in accordance with an
implementation of the present disclosure.
DETAILED DESCRIPTION OF THE INVENTION
[0013] 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
[0014] 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.

[0015] 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.
[0016] 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”.
[0017] 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. [0018] The term “including” is used to mean “including but not limited to”. “Including” and “including but not limited to” are used interchangeably. [0019] For the purposes of the present disclosure, the term “particulate filler” or “filler” may be a carbon black (CB) slurry or any other suitable filler in a suitable carrier fluid. The terms “particulate filler” and “filler” have been used interchangeably in the present disclosure. Selection of the carrier fluid will depend largely upon the choice of particulate filler and upon system parameters. Both aqueous and nonaqueous liquids may be used, with water being preferred in many embodiments in view of its cost, availability and suitability of use in the production of carbon black and certain other filler slurries. Small amounts of water-miscible organic solvents may also be included in aqueous carrier fluids. Selection of the filler or mixture of fillers will depend largely upon the intended use of the elastomer masterbatch product. As used herein, filler can include any material which is appropriate for use in the masterbatch process. Conventional fillers such as zinc oxide (ZnO), silica, clay, calcium carbonate, talc and other functional equivalent thereof are within the scope of the fillers of the present disclosure.
[0020] The term “phr” used herein refers to parts per hundred rubber/resin. It is a unit well defined in the field of rubber technology to define the amount of ingredients used. The unit “phr” can also be interchangeably used with the unit “gram” as both denote phr/gram of ingredient per 100 phr/gram of rubber.
[0021] The term “rpm” used herein refers to rotations/revolutions per minute. It is a unit well used in the field of rubber technology to define the speed of any rotating

part of the machine, in this disclosure especially for co-rotating twin screw extruder (CRTSE).
[0022] The term “elastomer latex” used herein refers to an elastic polymer in the latex form.
[0023] The term “dry rubber content” used herein refers to the amount in grams of a rubber per 100 grams of the latex.
[0024] The term “natural rubber latex” used herein refers to an elastic substance obtained naturally from the latex (milky tree sap) derived from bark of trees. [0025] The term “surfactant” used herein refers to the substances used for decreasing surface tension between particulate dispersion ingredients and the elastomer latex. Examples include, but are not limited to, ammonium laurate, dispersol. [0026] The term “crosslinking agent” used herein refers to substances that can form chemical bonds between two molecular chains by a chemical reaction. Rubber cross linking/vulcanization is highly essential is the field or rubber industry and is well known to a person known to a person skilled in the art. It is commonly performed by adding sulfur or soluble sulfur to an unvulcanised rubber sample.
[0027] The term “activator” used herein refers to the substances that activate the crosslinking/vulcanisation process of rubbers. Examples include, but are not limited to, zinc oxide.
[0028] The term “accelerator” used herein refers to the substances used with a cross-linking agent to increase the speed of vulcanization of rubber and enhance its physical properties.
[0029] The term “antioxidant” used herein refers to the substances that are used to protect rubber articles against the attack of oxygen.
[0030] The term “antiozonant” used herein refers to the substances that prevent the degradation due to ozone cracking. Examples include ethylene di-urea, microcrystalline wax, and others.
[0031] The term “peptizer” used herein refers to the substances which break down polymer chains and reduce rubber viscosity during its processing.

[0032] The term “processing aid” used herein refers to the substances which reduce viscosity of a rubber compound and help in rubber processing. Examples include, but are not limited to, stearic acid, wood rosin.
[0033] The term “inhibitor” used herein refers to the substances added to rubber compounds to delay premature vulcanization during its processing. Examples include, but are not limited to, pre-vulcanization inhibitors (PVI). [0034] 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 100 °C - 250 °C should be interpreted to include not only the explicitly recited limits of about 100 °C to about 250 °C, but also to include sub-ranges, such as 120 °C, 140 °C, 180 °C, 200 °C and so forth, as well as individual amounts, including fractional amounts, within the specified ranges, such as 120.4 °C, and 140.8 °C, for example.
[0035] 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.
[0036] 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. [0037] With the advent of different machineries such as internal mixers, mills, and batches in the market, the elastomer composites have now been extensively manufactured. However, there are few limitations associated with these machines and processes deployed by them for preparing the elastomer composite. The

limitations are as follows: (a) The principal limitation associated with them is the batch or unit production nature of the process carried out by them. The process that is carried out by the aforementioned machines require several steps for mixing all ingredients to obtain the elastomer composite. Different factors contribute to a batch process, such as variation in the weights of individual ingredients, order and timing of adding different components to arrive at the final rubber composition, temperature maintained at each step, and different apparatus involved at each step. (b) The quality of the final rubber compound gets degraded which renders the final rubber composition unacceptable for further application in producing various rubber products in the industry. The quality of the final rubber compound gets degraded because the rubber latex is processed into bale/sheet form through various steps which degrades the polymer chains of the elastomer compound. (c) The carbon particles are dispersed into the mixture containing elastomer only up to a certain range, beyond which the carbon particles are not distributed and dispersed properly in the mixture. Therefore, the final rubber compound achieved do not exhibit acceptable properties. (d) The fillers such as carbon black, and silica is weighed manually and fed through a feed hoper which does not give desired dispersion. (e) Acid is added at the final step to coagulate the rubber mixture. The addition of acid decreases the curing rate of rubber mixture, thereby, degrading the properties of the rubber mixture, which further limits their use in various industrial products in the long run. The overall process of handling carbon black makes the entire production area dirty, and the power that is consumed during the entire process is also very high. Therefore, the apparatus and methods that are disclosed in the literature are complex, labor-intensive, requires lot of time, and high cost of manufacturing is involved therein.
[0038] The present disclosure overcomes the aforementioned disadvantages associated with mixing process by providing a continuous process for preparing an elastomer composite through a single-step mixing in a co-rotating twin screw extruder (CRTSE). The process as disclosed in the present disclosure comprises: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone to obtain a first mix; b)

allowing the first mix from the first zone through a second zone to coagulate to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone to obtain the elastomer composite.
[0039] The present disclosure discloses a single step and continuous process which involves a single apparatus for mixing all the ingredients. The process of sequentially adding the particulate dispersion ingredients and surfactants into the elastomer in liquid state helps to facilitate the desired adsorption of the particles on the elastomer surface area and achieve a final well-dispersed and homogenous elastomer composite. The elastomer latex that is directly used in the present disclosure is mixed under mild conditions that does not involve intensive mixing procedures which prevents the elastomer chains from undergoing any mechanical or thermal degradation. The present disclosure allows efficient dispersion of carbon particles separately in water that is highly stable and does not settle down for even 2 weeks of storage. Further, since the carbon particles slurry is incorporated directly into the apparatus, therefore, the production floor remains clear. The coagulation of the mixture containing an elastomer and carbon particles is carried out without using any acid, and instead a thermomechanical method is employed for the same. The resulting elastomer composite is of high quality with moisture content less than 3 %. Therefore, the process of obtaining the elastomer composite as disclosed in the present disclosure, is a simple, cost-effective, energy-efficient, and a time-efficient process that can successfully substitute the conventionally used complex and time-consuming processes.
[0040] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d)

continuously passing the third mix from the third zone to a granulating zone to obtain the elastomer composite. In one another embodiment of the present disclosure, continuously passing the second mix from the second zone to a third zone is carried out at a temperature in the range of 150 °C - 240 °C to obtain a third mix. In yet another embodiment of the present disclosure, continuously passing the second mix from the second zone to a third zone is carried out at a temperature in the range of 190 °C - 210 °C to obtain a third mix.
[0041] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone at a temperature in the range of 30°C - 50°C at high shear mixing to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone to obtain the elastomer composite. In another embodiment of the present disclosure, contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone is carried out at a temperature in the range of 40°C - 50°C at high shear mixing to obtain a first mix. In yet another embodiment of the present disclosure, contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone is carried out at a temperature of 40°C at high shear mixing to obtain a first mix. [0042] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone at a temperature in the range of 30°C - 50°C at high shear mixing carried out in a co-rotating twin screw extruder at a screw speed in the range of 200 - 1000 rpm to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at

a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone to obtain the elastomer composite. In another embodiment of the present disclosure, the contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone is carried out at a temperature in the range of 35°C - 45°C at high shear in a co-rotating twin screw extruder at a screw speed in the range of 400 - 700 rpm mixing to obtain a first mix. In yet another embodiment of the present disclosure, the contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone is carried out at a temperature of 40°C at high shear in a co-rotating twin screw extruder at a screw speed of 500 rpm mixing to obtain a first mix. [0043] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate at a temperature in the range of 100 - 250°C to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone to obtain the elastomer composite. In another embodiment of the present disclosure, allowing the first mix from the first zone through a second zone to coagulate is carried out at a temperature in the range of 100 - 150°C to obtain a second mix. In yet another embodiment of the present disclosure, allowing the first mix from the first zone through a second zone to coagulate is carried out at a temperature of 100°C to obtain a second mix. [0044] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate to obtain a second mix; c) continuously passing the second mix from the second zone to a third

zone at a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone at a temperature in the range of 150 - 250°C to obtain the elastomer composite. In another embodiment of the present disclosure, continuously passing the third mix from the third zone to a granulating zone is carried out at a temperature in the range of 200 -250°C to obtain the elastomer composite. In yet another embodiment of the present disclosure, continuously passing the third mix from the third zone to a granulating zone is carried out at a temperature of 200°C to obtain the elastomer composite. [0045] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone at a temperature in the range of 30°C - 50°C at high shear mixing carried out in a co-rotating twin screw extruder at a screw speed in the range of 200 - 1000 rpm to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate at a temperature in the range of 100 - 250°C to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at a temperature in the range of 100 °C -250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone at a temperature in the range of 150 - 250°C to obtain the elastomer composite.
[0046] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein the at least one surfactant is selected from the group consisting of cationic surfactant, anionic surfactant, non-ionic surfactants, and combinations thereof. In another embodiment of the present disclosure, the at least one surfactant is a combination of dispersol and ammonium laurate.
[0047] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein the at least one particulate dispersion ingredient is selected from the group consisting of carbon black dispersion, coarse-grained carbon black dispersion, fillers, activators, accelerators, antioxidant, antiozonant, peptizer, processing aid,

inhibitor, and combinations thereof. In one another embodiment of the present disclosure, the at least one particulate dispersion ingredient is a combination of carbon black dispersion, fillers, activators, accelerators, antioxidant, antiozonant, peptizer, processing aid, and inhibitor. In yet another embodiment of the present disclosure, the filler is carbon black, the activator is zinc oxide, the accelerator is N-Cyclohexyl-2-benzothiazole sulfenamide (CBS), the antioxidant is a combination of 1,2-dihydro-2,2,4-trimethyl-quinoline (TMQ) and N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine (6PPD), the antiozonant is microcrystalline wax, the processing aid is a combination of wood rosin and stearic acid, and the inhibitor is pre-vulcanization inhibitor.
[0048] In an embodiment of the present disclosure, there is a provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein the at least one particulate dispersion ingredient further includes at least one cross linking agent. In another embodiment of the present disclosure, the at least one cross linking agent is selected from sulfur or soluble sulfur.
[0049] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein the at least one particulate dispersion ingredient has a concentration in the range of 0.1 phr - 150 phr. In one another embodiment of the present disclosure, the at least one particulate dispersion ingredient has a concentration in the range of 0.15 phr - 100 phr. In yet one another embodiment of the present disclosure, the at least one particulate dispersion ingredient has a concentration in the range of 0.2 phr - 90 phr.
[0050] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein the at least one elastomer latex is selected from the group consisting of natural rubber latex, styrene butadiene rubber latex, butadiene rubber latex, acrylonitrile butadiene rubber latex, and combinations thereof. In another embodiment of the present disclosure, the at least one elastomer latex is natural rubber latex.

[0051] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein the at least one elastomer latex is a derivative of the at least one elastomer latex selected from the group consisting of natural rubber latex, styrene butadiene rubber latex, butadiene rubber latex, acrylonitrile butadiene rubber latex, and combinations thereof.
[0052] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein the at least one elastomer latex has a concentration in the range of 15 - 20 % with respect to the elastomer composite. In another embodiment of the present disclosure, the at least one elastomer latex has a concentration of 20 % with respect to the elastomer composite.
[0053] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein the at least one elastomer latex has a dry rubber content (DRC) in a range of 10 - 60 % with respect to the at least one elastomer latex. In another embodiment of the present disclosure, the at least one elastomer latex has a dry rubber content (DRC) of 60 % with respect to the at least one elastomer latex. [0054] In an embodiment of the present disclosure, there is provided a formulation comprising the elastomer composite prepared by the continuous process comprising: a) contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone to obtain a first mix; b) allowing the first mix from the first zone through a second zone to coagulate to obtain a second mix; c) continuously passing the second mix from the second zone to a third zone at a temperature in the range of 100 °C - 250 °C to obtain a third mix; and d) continuously passing the third mix from the third zone to a granulating zone to obtain the elastomer composite.
[0055] In an embodiment of the present disclosure, there is provided a use of the elastomer composite prepared by the continuous process as described herein, in manufacturing elastomeric products selected from tires, hose, conveyor belt, boat, dock fenders, mats, hot water bags, O rings, rail pads, or rubber rollers.

[0056] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein concentration of combination of at least one particulate dispersion ingredients in a particulate dispersion is in the range of 1 – 30 %. In one another embodiment of the present disclosure, concentration of combination of at least one particulate dispersion ingredients in a particulate dispersion is in the range of 5 – 20 %. In yet one another embodiment of the present disclosure, concentration of combination of at least one particulate dispersion ingredients in a particulate dispersion is 10 %.
[0057] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein percentage of kneading block in the co-rotating twin screw extruder is in the range of 10 – 90 %.
[0058] In an embodiment of the present disclosure, there is provided a continuous process for the preparation of an elastomer composite, said process as described herein, wherein the at least one elastomer latex in liquid state is in the form of a solution or dispersion.
[0059] Although the subject matter has been described in considerable detail with reference to certain examples and implementations thereof, other implementations are possible.
EXAMPLES
[0060] 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.
Materials and methods
[0061] For the purpose of the present disclosure, carbon black was procured from Philips carbon black. Surfactant was procured from BASF. Natural rubber latex was procured from Harrisons Malayalam Limited (HML).
EXAMPLE 1
Process for preparation of the elastomer composite
[0062] In order to prepare the elastomer composite of the present disclosure, a 10 %
particulate dispersion of a mixture of ingredients as mentioned in Table 1 was
prepared for which, 44 phr carbon black, 0.7 phr TMQ, 2 phr 6PPD, 1 phr
microcrystalline wax, 1 phr wood rosin, 2 phr soluble sulfur, 2 phr stearic acid, 3.5
phr zinc oxide, 0.75 phr CBS, 0.88 phr dispersol, 0.22 phr ammonium laurate, and
0.25 phr pre-vulcanization inhibitor were added in 504.9 phr water. All the
particulate dispersion ingredients were premixed for 1 hour using a mechanical
stirrer. The premix thus formed was then fed into a CRTSE at the rate of 80g/min
using a first liquid feeding pump and processed at screw speed 500 rpm and 40oC to
make a stable particulate dispersion. The schematic diagram for the preparation of
the particulate dispersion in a non-solvent liquid is illustrated in Figure 1.
[0063] Then, 166.7 g natural rubber latex, having 60 % dry rubber content and 20 %
concentration was fed into the CRTSE along with the particulate dispersion using a
second liquid feeding pump (at the feeding rate of 71.25 g/min). Both the liquids
were thoroughly mixed at a low temperature of 50oC (or less) and at a high shear
mixing speed of 500 rpm in first zone of CRTSE to obtain a first mix. Figure 2
illustrates the schematic diagram for the preparation of elastomer composites
indicating the second liquid feeding pumps and barrel demarcation.
[0064] Mixing in the first zone was continued up to barrel 7 post which, the first mix
was further passed to barrel 8 (second zone) where the temperature was increased to
100oC for partial evaporation of water. Because of the thermomechanical force and

evaporation of water, the first mix started getting coagulated. Thus, a second mix in the coagulated form was obtained which was continuously passed into barrel 10 (third zone) where complete evaporation of water was achieved at 150oC temperature. Finally, the obtained solid mass (third mix) was sent to the granulation zone at the end of the extruder where the third mix was granulated at 200oC to obtain the elastomer composite.
Table 1

Material Ingredient Concentration (phr)
Filler Carbon black 44
Antioxidant 1,2-dihydro-2,2,4-trimethyl-quinoline (TMQ) 0.7

N-(1,3-dimethylbutyl)-N'- phenyl-p-phenylenediamine (6PPD) 2.0
Inhibitor Pre-vulcanization inhibitor (PVI) 0.25
Accelerator N-Cyclohexyl-2-benzothiazole sulfenamide (CBS) 0.75
Activator Zinc oxide (ZnO) 3.5
Antiozonant Microcrystalline wax 1.0
Processing aid Stearic acid 2.0

Wood rosin 1.0
Dispersing medium Water 504.9
Cross linking agent Soluble sulfur 2.0
Surfactant Dispersol 0.88

Ammonium laurate 0.22
[0065] By following the process as described above, a continuous production of a well-dispersed elastomer composite was achieved. The elastomer composite obtained did not show any signs of thermal or mechanical degradation of the polymer chains. Also, the elastomer composite displayed remarkable results in terms of

highly reduced moisture content of less than 3 %. Further, the carbon black slurry prepared with water also remained stable for up to 2 weeks. Hence, by using the process disclosed in the present disclosure, a high-quality elastomer composite was obtained which can successfully pave a way in the realm of presently known elastomer composite producing processes.
Advantages of the present disclosure
[0066] The present disclosure discloses a continuous process for the preparation of an elastomer composite using one single equipment (co-rotating twin screw extruder) for mixing, coagulating, drying, and granulating in a single step. The liquid phase mixing of the elastomer latex and particulate dispersion ingredients along with water and surfactants imparts excellent dispersion and complete homogenization of the mixture. All the extrusion processes in different zones of the CRTSE are carried out at lower temperatures below 250oC which makes it an energy efficient process. A separate preparation of the highly stable carbon black dispersion eliminates chances of polymer chain breakdown during downsizing of carbon black. The use of thermomechanical method facilitates proper curing of the elastomers and ensures long-lasting properties in the rubber compound produced therefrom. The formulation comprising the elastomer composite prepared by the process as disclosed herein, can also be used for manufacturing several rubber products including tires, hose, conveyor belt, boat, dock fenders, mats, hot water bags, O rings, rail pads, rubber rollers, and the like. Overall, the present disclosure provides a simple, cost-effective and a time saving process for the continuous production of a high-quality elastomer composite.

I/We Claim:
1. A continuous process for the preparation of an elastomer composite, said process
comprising:
a. contacting at least one particulate dispersion ingredient, at least one
surfactant, and at least one elastomer latex in liquid state in a first zone to
obtain a first mix;
b. allowing the first mix from the first zone through a second zone to coagulate
to obtain a second mix;
c. continuously passing the second mix from the second zone to a third zone at
a temperature in the range of 100 °C - 250 °C to obtain a third mix; and
d. continuously passing the third mix from the third zone to a granulating zone
to obtain the elastomer composite.
2. The process as claimed in claim 1, wherein the contacting at least one particulate dispersion ingredient, at least one surfactant, and at least one elastomer latex in liquid state in a first zone is carried out in the temperature range of 30°C - 50°C at high shear mixing.
3. The process as claimed in claim 2, wherein the high shear mixing is carried out in a co-rotating twin screw extruder at a screw speed in the range of 200 - 1000 rpm.
4. The process as claimed in claim 1, wherein the allowing the first mix from the first zone through a second zone to coagulate is carried out in the temperature range of 100 - 250°C.
5. The process as claimed in claim 1, wherein the continuously passing the third mix from the third zone to a granulating zone is carried out in a temperature range of 150 - 250°C to obtain the elastomer composite
6. The process as claimed in claim 1, wherein the at least one particulate dispersion ingredient is selected from the group consisting of carbon black dispersion, coarse-grained carbon black dispersion, fillers, activators, accelerators, antioxidant, antiozonant, peptizer, processing aid, inhibitor, and combinations thereof.

7. The process as claimed in claim 6, wherein the at least one particulate dispersion ingredient has a concentration in the range of 0.1 phr - 150 phr.
8. The process as claimed in claim 1, wherein the at least one surfactant is selected from the group consisting of cationic surfactant, anionic surfactant, non-ionic surfactants, and combinations thereof.
9. The process as claimed in claim 1, wherein the at least one elastomer latex is selected from the group consisting of natural rubber latex, styrene butadiene rubber latex, butadiene rubber latex, acrylonitrile butadiene rubber latex, and combinations thereof.

10. The process as claimed in claim 9, wherein the at least one elastomer latex has a concentration in the range of 15 – 20 % with respect to the elastomer composite.
11. The process as claimed in claim 1, wherein the at least one elastomer latex has a dry rubber content (DRC) in a range of 10 – 60 % with respect to the at least one elastomer latex.
12. A formulation comprising the elastomer composite prepared by the process as claimed in any one of the claims 1-11.

Documents

Application Documents

# Name Date
1 201921040612-FORM 18 [12-09-2023(online)].pdf 2023-09-12
1 201921040612-STATEMENT OF UNDERTAKING (FORM 3) [07-10-2019(online)].pdf 2019-10-07
2 Abstract1.jpg 2021-10-19
2 201921040612-PROVISIONAL SPECIFICATION [07-10-2019(online)].pdf 2019-10-07
3 201921040612-POWER OF AUTHORITY [07-10-2019(online)].pdf 2019-10-07
3 201921040612-COMPLETE SPECIFICATION [05-10-2020(online)].pdf 2020-10-05
4 201921040612-CORRESPONDENCE-OTHERS [05-10-2020(online)].pdf 2020-10-05
4 201921040612-FORM 1 [07-10-2019(online)].pdf 2019-10-07
5 201921040612-DRAWING [05-10-2020(online)].pdf 2020-10-05
5 201921040612-DRAWINGS [07-10-2019(online)].pdf 2019-10-07
6 201921040612-Proof of Right (MANDATORY) [22-10-2019(online)].pdf 2019-10-22
6 201921040612-ORIGINAL UR 6(1A) FORM 1-041119.pdf 2019-11-06
7 201921040612-Proof of Right (MANDATORY) [22-10-2019(online)].pdf 2019-10-22
7 201921040612-ORIGINAL UR 6(1A) FORM 1-041119.pdf 2019-11-06
8 201921040612-DRAWINGS [07-10-2019(online)].pdf 2019-10-07
8 201921040612-DRAWING [05-10-2020(online)].pdf 2020-10-05
9 201921040612-FORM 1 [07-10-2019(online)].pdf 2019-10-07
9 201921040612-CORRESPONDENCE-OTHERS [05-10-2020(online)].pdf 2020-10-05
10 201921040612-COMPLETE SPECIFICATION [05-10-2020(online)].pdf 2020-10-05
10 201921040612-POWER OF AUTHORITY [07-10-2019(online)].pdf 2019-10-07
11 201921040612-PROVISIONAL SPECIFICATION [07-10-2019(online)].pdf 2019-10-07
11 Abstract1.jpg 2021-10-19
12 201921040612-STATEMENT OF UNDERTAKING (FORM 3) [07-10-2019(online)].pdf 2019-10-07
12 201921040612-FORM 18 [12-09-2023(online)].pdf 2023-09-12
13 201921040612-FER.pdf 2025-09-04
14 201921040612-FORM 3 [08-10-2025(online)].pdf 2025-10-08

Search Strategy

1 201921040612_SearchStrategyNew_E_201921040612searchE_29-08-2025.pdf