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Process For Preparation Of Polymer, And Implementations Thereof

Abstract: The instant disclosure provides a process for the production of poly €-olefins. The process comprises: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to form a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12.

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Patent Information

Application #
Filing Date
23 November 2018
Publication Number
22/2020
Publication Type
INA
Invention Field
POLYMER TECHNOLOGY
Status
Email
tarun@khuranaandkhurana.com
Parent Application
Patent Number
Legal Status
Grant Date
2024-04-05
Renewal Date

Applicants

HINDUSTAN PETROLEUM CORPORATION LIMITED
PETROLEUM HOUSE, 17 JAMSHEDJI TATA ROAD, CHURCHGATE, MUMBAI, MAHARASHTRA 400020, INDIA

Inventors

1. CHIKKALI, Samir Hujur
CSIR-National Chemical Laboratory, Dr. Homi Bhabha Road, Pune Maharashtra, 411008, India
2. MANDAL, Dipa
CSIR-National Chemical Laboratory, Dr. Homi Bhabha Road, Pune Maharashtra, 411008, India
3. GOTE, Ravindra
CSIR-National Chemical Laboratory, Dr. Homi Bhabha Road, Pune Maharashtra, 411008, India
4. CHELLIAHN, Bennet
HINDUSTAN PETROLEUM GREEN R&D CENTRE, KIADB INDUSTRIAL AREA, TARABANAHALLI, DEVANAGUNDI, HOSKOTE TALUK, BANGALORE-560067, INDIA
5. KADAM, Pravin
HINDUSTAN PETROLEUM GREEN R&D CENTRE, KIADB INDUSTRIAL AREA, TARABANAHALLI, DEVANAGUNDI, HOSKOTE TALUK, BANGALORE-560067, INDIA
6. KOTTARI, Naresh
HINDUSTAN PETROLEUM GREEN R&D CENTRE, KIADB INDUSTRIAL AREA, TARABANAHALLI, DEVANAGUNDI, HOSKOTE TALUK, BANGALORE-560067, INDIA
7. RAO, Bojja Ramachandra
HINDUSTAN PETROLEUM GREEN R&D CENTRE, KIADB INDUSTRIAL AREA, TARABANAHALLI, DEVANAGUNDI, HOSKOTE TALUK, BANGALORE-560067, INDIA
8. CHOUDHARY, Nettem Venkateswarlu
HINDUSTAN PETROLEUM GREEN R&D CENTRE, KIADB INDUSTRIAL AREA, TARABANAHALLI, DEVANAGUNDI, HOSKOTE TALUK, BANGALORE-560067, INDIA
9. GANDHAM, Sri Ganesh
HINDUSTAN PETROLEUM GREEN R&D CENTRE, KIADB INDUSTRIAL AREA, TARABANAHALLI, DEVANAGUNDI, HOSKOTE TALUK, BANGALORE-560067, 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 PREPARATION OF POLYMER, AND
IMPLEMENTATIONS THEREOF
2. Applicant(s)
NAME NATIONALITY ADDRESS
HINDUSTAN PETROLEUM Indian PETROLEUM HOUSE, 17
CORPORATION LIMITED JAMSHEDJI TATA ROAD,
CHURCHGATE, MUMBAI,
MAHARASHTRA 400020, INDIA
COUNCIL OF SCIENTIFIC Indian Anusandhan Bhawan, 2 Rafi Marg,
AND INDUSTRIAL New Delhi 110 001, India
RESEARCH an Indian registered body incorporated under the Regn. of Soc. Act (Act XXI of 1860)

FIELD OF THE INVENTION
[001] The present disclosure generally relates to the oil and gas industry, and in particular to processes for producing drag reducing additives.
BACKGROUND OF THE INVENTION
[002] Drag is the resistive force by a fluid on a surface acting in the opposite direction to the relative motion of the fluid. In pipelines for the transportation of a fluid, drag on pipe results in pressure drop, thereby increases the pumping costs or limiting the throughput. In order to maintain throughput or reduce the pumping costs, drag reducing additives, DRA's (usually specialized polymers) are being used. Polymer-based drag reduction is a phenomenon in which by adding polymers (few ppm by weight), 30-80% drag reduction in turbulent flow could be obtained (US4289679A). [003] Polv(α-olefins) (PAOs) are commonly used as DRA to reduce friction or drag during the transportation of refinery fluids through pipelines. Drag reducing effects are most pronounced when the polymers are flexible with ultra-high molecular weight (UHMW) (Mw> 106). Generally, PAOs are amorphous, soluble in common hydrocarbon solvents and commonly synthesized using organometallic catalysis. US6649670 reveals a continuous process using a stirred tank reactor for formation of PAO which incorporates grinding as part of the method in order to obtain PAO which is finely dispersed in the fluid. EP0595565 reveals a catalyst composition comprising titanium, magnesium and a halogen along with a second component which is selected from the group consisting of zeolite, alumina, titania, silica, and zirconia. [004] In recent years, there has been a tremendous increase in demand pertaining to energy resources. The corresponding load on efficient processing of the oil and gas has meant that the energy-efficient transport of oil via pipelines has evolved into an important criterion for revenue generation. In accordance, newer and more efficient methods for obtaining additives such as drag reducing agents that are able to improve efficiency of oil transport are of utmost importance.
SUMMARY OF THE INVENTION

[005]In an aspect of the present disclosure, there is provided a process for preparing a polymer, said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 -C12.
[006] 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 THE DRAWINGS
[007] The detailed description is described with reference to the accompanying figures.
In the figures, the left-most digit(s) of a reference number identifies the figure in which
the reference number first appears. The same numbers are used throughout the drawings
to reference like features and components.
[008] Figure 1 depicts the 1H NMR spectrum of poly(1-decene) in CDCl3 at 25 ºC, in
accordance with an implementation of the present subject matter.
[009] Figure 2 depicts the 1H NMR spectrum of poly(1-decene) in CDCl3 at 25 ºC, in
accordance with an implementation of the present subject matter.
[0010] Figure 3a-3d depict the gel permeation chromatography (GPC) spectrum of
poly(1-decene) in CDCl3 at 25 ºC, in accordance with an implementation of the present
subject matter.
[0011] Figure 4a-4b depict the differential scanning chromatography (DSC) spectrum,
in accordance with an implementation of the present subject matter.
[0012] Figure 5 depicts the shear rate as a function of viscosity for the polymer, in
accordance with an implementation of the present subject matter.
[0013] Figure 6 depicts the drag reducing ability of the polymer, in accordance with an
implementation of the present subject matter.

[0014] Figure 7 depicts a plot of viscosity versus shear of the polymer, in accordance
with an implementation of the present subject matter.
[0015] Figure 8 depicts a plot of percentage drag versus Reynolds number of the
polymer, in accordance with an implementation of the present subject matter.
[0016] Figure 9 depicts a plot of viscosity versus shear of the polymer, in accordance
with an implementation of the present subject matter.
[0017] Figure 10 depicts a plot of percentage drag versus Reynolds number of the
polymer, in accordance with an implementation of the present subject matter.
DETAILED DESCRIPTION OF THE INVENTION
[0018] 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:
[0019] For convenience, before further description of the present disclosure, certain
terms employed in the specification, and examples are collected 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.
[0020] 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.
[0021] 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",
[0022] 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 steps.
[0023] The term "including" is used to mean "including but not limited to", "including" and "including but not limited to" are used interchangeably. [0024] 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 or testing of the disclosure, the preferred methods, and materials are now described. All publications mentioned herein are incorporated herein by reference.
[0025] 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 60 °C to about 100 °C should be interpreted to include not only the explicitly recited limits of about 60 °C to about 100 °C, but also to include sub-ranges, such as 60 °C to 95 °C, 65 °C to 100 °C, and so forth, as well as individual amounts, including fractional amounts, within the specified ranges, such as 60.5 °C, 81.1 °C, and 92.9 °C, for example.
[0026] 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 scope of the disclosure, as described herein.
[0027] As mentioned previously, to address the problem of poor transportation efficiency in oil and gas pipelines, there is need in the art to provide additives that are able to reduce drag and hence in-turn increase transport efficiency. Improvements in process for production of such additives is sought-after. The present disclosure provides a process for the preparation of ultra-high molecular weight (UHMW) PAOs that would

be effective as drag reducing agent (DRA), using a modified organometallic catalytic system in presence of co-catalyst methylaluminoxane (MAO).
[0028] In an embodiment of the present disclosure, there is provided a process for preparing a polymer, said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one a-olefin has a carbon chain length in the range of C8 - C12. In another embodiment of the present disclosure, the at least one a-olefin has a carbon chain length of C10.
[0029] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin is carried out at a temperature in the range of -10 to 0 °C for a period in the range of 24 - 72 hours to obtain the first mixture. In another embodiment of the present disclosure, contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin is carried out at a stirring in the range of 50 - 300 rpm. In yet another embodiment of the present disclosure, contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin is carried out at a temperature of 0 °C for a period in the range of 48 hours to obtain the first mixture. In yet another embodiment of the present disclosure, contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin is carried out at a temperature in the range of -5 to 0 °C for a period in the range of 30 - 60 hours under a stirring in the range of 70-250 rpm to obtain the first mixture. [0030] In an embodiment of the present disclosure, there is provided a process for preparing a polymer, said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin is carried out at a temperature in the range of -10 to 0 °C for a period in the range of 24 - 72 hours to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one a-olefin has a carbon chain length in the range of C8 - C12.

[0031] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein the first aluminium compound is selected from the group consisting of aluminoxane, trialkylaluminium, and combinations thereof. In another of the present disclosure, the trialkylaluminium is selected from the group consisting of trimethylaluminium, triethylaluminium, tri-n-butylaluminium, tri-n-propylaluminium, triisobutylaluminium, tri-tert-butylaluminum, tri-n-hexylaluminum, tri-n-octylaluminum, and combinations thereof. In yet another embodiment of the present disclosure, the first aluminium compound is an aluminoxane. [0032] In an embodiment of the present disclosure, there is provided a process for preparing a polymer, said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and the first aluminium compound is selected from the group consisting of aluminoxane, trialkylaluminium, and combinations thereof.
[0033] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein the aluminoxane is selected from the group consisting of methylaluminoxane (MAO), modified-methylaluminoxane (MMAO), and combinations thereof. In another embodiment of the present disclosure, the aluminoxane is methylaluminoxane. In yet another embodiment of the present disclosure, the aluminoxane is modified-methylaluminoxane.
[0034] In an embodiment of the present disclosure, there is provided a process for preparing a polymer, said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and the first aluminium compound is selected from the group consisting of methylaluminoxane (MAO), modified-methylaluminoxane (MMAO), and combinations thereof.

[0035] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein the polymer has a weight (Mw) range in the range of 106 - 107 g/mol. In another embodiment of the present disclosure, the polymer has a weight (Mw) of at least 106 g/mol.
[0036] In an embodiment of the present disclosure, there is provided a process for preparing a polymer, said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and the polymer has a weight (Mw) range in the range of 106 - 107 g/mol. [0037] In an embodiment of the present disclosure, there is provided a polymer obtained by a process as described herein, said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and the polymer has a polydispersity index in the range of 1 - 3.5.
[0038] In an embodiment of the present disclosure, there is provided a polymer obtained by a process as described herein, said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and the polymer has a polydispersity index in the range of 1 - 3.5 and the weight (Mw) of the polymer is in the range of 106 t 107 g/mol.
[0039] In an embodiment of the present disclosure, there is provided a polymer as described herein, wherein the polymer has an application selected from the group consisting of friction modifiers, drag reducing agents, oil pipeline additives, and combinations thereof.

[0040] In an embodiment of the present disclosure, there is provided a polymer obtained by a process as described herein, said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and the polymer has an application selected from the group consisting of friction modifiers, drag reducing agents, oil pipeline additives, and combinations thereof.
[0041] In an embodiment of the present disclosure, there is provided a polymer as described herein, wherein the polymer is used in pipelines as drag reducing agent. [0042] In an embodiment of the present disclosure, there is provided a polymer obtained by a process as described herein, wherein said process comprising the steps of: a) obtaining at least one pre-catalyst; b) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and c) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and the polymer is used in pipelines as drag reducing agent.
[0043] In an embodiment of the present disclosure, there is provided a process for preparing a polymer, wherein obtaining the at least one pre-catalyst comprises: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst, wherein the at least one magnesium halide to the compound of Formula M(OR)x mole ratio is in the range of 1:10 - 1:20.
[0044] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound

to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one €α-olefin has a carbon chain length in the range of C8 - C12 and the at least one magnesium halide to the compound of Formula M(OR)x mole ratio is in the range of 1:10 - 1:20.
[0045] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein the alkyl aluminium compound to the compound of Formula M(OR)x mole ratio is in the range of 1:8 - 1:16. In another embodiment of the present disclosure, the alkyl aluminium compound to the compound of Formula M(OR)x mole ratio is in the range of 1:12 - 1:13.
[0046] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and the at least one magnesium halide to the compound of Formula M(OR)x mole ratio is in the range of 1:10 - 1:20 and the alkyl aluminium compound to the compound of Formula M(OR)x mole ratio is in the range of 1:8 - 1:16. [0047] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein M of the compound of Formula M(OR)x is at least one transition metal (M) selected from the group consisting of group IV-B metals, group V-B metals, and combinations thereof. In another embodiment of the present disclosure, M is a IV-B metal. In another embodiment of the present disclosure, M is a V-B metal.

[0048] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and M of the compound of Formula M(OR)x is at least one transition metal (M) selected from the group consisting of group IV-B metals, group V-B metals, and combinations thereof.
[0049] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein first aluminium compound to the compound of Formula M(OR)x mole ratio is in the range of 1:2 - 1:20. In another embodiment of the present disclosure, the compound of Formula M(OR)x mole ratio is in the range of 1:5 - 1:18. In another embodiment of the present disclosure, the compound of Formula M(OR)x mole ratio is 1:10.
[0050] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one α€-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and first aluminium compound to the compound of Formula M(OR)x mole ratio is in the range of 1:2 - 1:20.

[0051] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein M of the compound Formula M(OR)x is at least one transition metal (M) selected from Ti, Zr, Hf, V, Nb, or Ta. In another embodiment of the present disclosure, the at least one transition metal is Ti. In yet another embodiment of the present disclosure, the at least one transition metal is Zr. [0052] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and M of the compound Formula M(OR)x is at least one transition metal (M) selected from Ti, Zr, Hf, V, Nb, or Ta.
[0053] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein R of the compound of Formula M(OR)x is selected from the group consisting of C1-15 alkyl, C5-15 aryl, C1-15 haloalkyl, C3-12 cycloalkyl, C1-20 heteroaryl, and C1-20 heterocyclyl, wherein C5-15 aryl is optionally substituted with 1 - 3 groups selected from halogen, C1-8 alkyl or C1-8 alkoxy; x is 2 to 5. In another embodiment of the present disclosure, R of the compound of Formula M(OR)x is selected from the group consisting of C1-12 alkyl, C5-15 aryl, C1-14 haloalkyl, C3-10 cycloalkyl, C1-18 heteroaryl, and C1-18 heterocyclyl, wherein C5-12 aryl is optionally substituted with 1 - 3 groups selected from halogen, C1-8 alkyl or C1-8 alkoxy; x is 3 to 5.
[0054] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-

mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and R of the compound of Formula M(OR)x is selected from the group consisting of C1-15 alkyl, C5-15 aryl, C1-15 haloalkyl, C3-12 cycloalkyl, C1-20 heteroaryl, and C1-20 heterocyclyl, wherein C5-15 aryl is optionally substituted with 1 - 3 groups selected from halogen, C1-8 alkyl or C1-8 alkoxy; x is 2 to 5.
[0055] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein R of the compound Formula M(OR)x is selected from the group consisting of C1-8 alkyl and C5-12 aryl; x is 4. In another embodiment of the present disclosure, R of the compound Formula M(OR)x is selected from the group consisting of C1-5 alkyl; x is 4. In another embodiment of the present disclosure, R of the compound Formula M(OR)x is selected from the group consisting of C2 alkyl; x is 4.
[0056] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and R of the compound Formula M(OR)x is selected from the group consisting of C1-8 alkyl and C5-12 aryl; x is 4.
[0057] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula

M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one α-olefin has a carbon chain length in the range of C8 - C12; M of the compound Formula M(OR)x is at least one transition metal (M) selected from Ti, Zr, Hf, V, Nb, or Ta; and R of the compound Formula M(OR)x is selected from the group consisting of C1-8 alkyl and C5-12 aryl; x is 4. [0058] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein the at least one alkyl aluminium compound has a Formula AlR'nCl3-n.
[0059] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one a-olefin has a carbon chain length in the range of C8 - C12 and the at least one alkyl aluminium compound has a Formula AlR'nCl3-n.
[0060] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein R' is C1-5 alkyl; n is 1 to 2. In another embodiment of the present disclosure, R' is selected from the group consisting of C1-3 alkyl; n is 2. In another embodiment of the present disclosure, R' is selected from the group consisting of C2 alkyl; n is 2.
[0061] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of:

a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one a-olefin has a carbon chain length in the range of C8 - C12 and R' is selected from the group consisting of C1-5 alkyl; n is 1 to 2. [0062] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein the solvent has a formula CmH2m+2; wherein m is 5 to 12. In another embodiment of the present disclosure, the solvent has a formula CmH2m+2; wherein m is 5 to 8. In yet another embodiment of the present disclosure, the solvent has a formula CmH2m+2; wherein m is 6.
[0063] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one a-olefin has a carbon chain length in the range of C8 - C12 and the solvent has a formula CmH2m+2; wherein m is 5 to 12. [0064] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein the magnesium halide is a magnesium salt of at least one halide selected from the group consisting of fluoride, chloride, bromide, iodide, and combinations thereof. In another embodiment of the present disclosure, the at least one halide is chloride. In yet another embodiment of the present disclosure, the magnesium halide is magnesium chloride having a particle size in the range of 0.15-2.0 mm.

[0065] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 t C12 and the magnesium halide is a magnesium salt of at least one halide selected from the group consisting of fluoride, chloride, bromide, iodide, and combinations thereof.
[0066] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein the at least one pre-catalyst has a a) transition metal content (M) in the range of 2.5 - 6 wt.% with respect to the at least one pre-catalyst; b) elemental magnesium content in the range of 10 - 12 wt.% with respect to the at least one pre-catalyst; and c) elemental aluminium in the range of 0.8 - 1.1 wt.% with respect to the at least one pre-catalyst.
[0067] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one €-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one €-olefin has a carbon chain length in the range of C8 - C12 and the at least one pre-catalyst has a a) transition metal content (M) in the range of 2.5 - 6 wt.% with respect to the at least one pre-catalyst; b) elemental magnesium content in the range of 10 - 12 wt.% with respect to the at least one pre-

catalyst; and c) elemental aluminium in the range of 0.8 - 1.1 wt.% with respect to the at least one pre-catalyst.
[0068] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein the a-olefin to the compound of Formula M(OR)x mole ratio is in the range of 200 - 1000. In another embodiment of the present disclosure, the α-olefin to the compound of Formula M(OR)x mole ratio is in the range of 200 - 500. In yet another embodiment of the present disclosure, the a-olefin to the compound of Formula M(OR)x mole ratio is in the range of 200 - 350. [0069] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one a-olefin has a carbon chain length in the range of C8 - C12 and the a-olefin to the compound of Formula M(OR)x mole ratio is in the range of 200- 1000.
[0070] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein contacting the compound having Formula MORx with at least one magnesium halide in the presence of the solvent is carried out at a temperature in the range of 60 - 100 °C for a period in the range of 0,5 - 2 hours to obtain a pre-mixture 1. In another embodiment of the present disclosure, contacting the compound having Formula MORx with at least one magnesium halide in the presence of the solvent is carried out at a temperature in the range of 70 - 90 °C for a period in the range of 0.5 - 1.5 hours to obtain a pre-mixture 1. In yet another embodiment of the present disclosure, contacting the compound having Formula MORx with at least one magnesium halide in the presence of the solvent is carried out at a temperature of 80 °C for a period of 1 hour to obtain a pre-mixture 1.

[0071] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent is carried out at a temperature in the range of 60-100 °C for a period in the range of 0,5 - 2 hours to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one a-olefin has a carbon chain length in the range of C8-C12.
[0072] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein contacting the pre-mixture 1 with at least one alkyl aluminium compound is carried out at a temperature in the range of 30 -100 °C for a period in the range of 0.2 - 3 hours to obtain a pre-mixture 2. In another embodiment of the present disclosure, contacting the pre-mixture 1 with at least one alkyl aluminium compound is carried out at a temperature in the range of 30 - 90 °C for a period in the range of 1 - 3 hours to obtain a pre-mixture 2. In yet another embodiment of the present disclosure, contacting the pre-mixture 1 with at least one alkyl aluminium compound is carried out ins a step-wise manner, step 1) at a temperature of 40 °C for a period in the range of 0.5 hours followed by step 2) at a temperature of 80 °C for a period in the range of 2 hours to obtain a pre-mixture 2.
[0073] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound is carried out at a temperature in the range of 30 - 100 °C for a period in the range of 0.2 - 3 hours to obtain a pre-mixture 2; d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium

compound and at least one a-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one a-olefin has a carbon chain length in the range of C8-C12.
[0074] In an embodiment of the present disclosure, there is provided a process for preparing a polymer as described herein, wherein said process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent is carried out at a temperature in the range of 60-100 °C for a period in the range of 0,5 - 2 hours to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound is carried out at a temperature in the range of 30 - 100 °C for a period in the range of 0.2 - 3 hours to obtain a pre-mixture 2; d) processing the pre-mixture 2 to obtain the at least one pre-catalyst; e) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin to obtain a first mixture; and f) processing the first mixture to obtain the polymer, wherein the at least one a-olefin has a carbon chain length in the range of C8-C12.
[0075] In an embodiment of the present disclosure, there is provided the at least one pre-catalyst obtained by a process as described herein, wherein the process comprising the steps of: a) obtaining a compound of Formula M(OR)x; b) contacting the compound of Formula M(OR)x with at least one magnesium halide in the presence of a solvent to obtain a pre-mixture 1; c) contacting the pre-mixture 1 with at least one alkyl aluminium compound to obtain a pre-mixture 2; and d) processing the pre-mixture 2 to obtain the at least one pre-catalyst.
[0076] Although the subject matter has been described in considerable detail with reference to certain preferred embodiments thereof, other embodiments are possible.
EXAMPLES
[0077] 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.
[0078] There is need in the art for efficient processes that are able to provide poly a-olefins (PAOs) or drag reducing agents. The present disclosure provides a process for polymerization of higher a-olefins (like 1-octene, 1-decene, 1-dodecene etc.) to produce super high molecular weight PAO. The synthesis of active catalyst system for polymerization of a-olefins (like 1-octene, 1-decene, 1-dodecene etc.) comprises: a) reacting of metal alkoxide/aryloxide with anhydrous magnesium chloride in a suitable hydrocarbon solvent to form slurry; and b) activating the compound by treating with an organo-aluminum compound followed by purifying the mixture to obtain PAO. [0079] A combination of a pre-catalyst as described in the present disclosure, along with an methylaluminoxane or MAO (first aluminium compound or co-catalyst) characteristics are defined as follows:
a) The catalyst component comprises of a transition metals alcholate/phenolate of general formula M(OR)4, wherein M is either Ti or Zr.
b) R denotes a straight chain or branched alkyl group containing 1 to 8 carbon atoms, such as methyl, ethyl, iso-propyl, tert-butyl etc. or an aryl or substituted aryl group, such as phenyl, p-methylphenyl, p-methoxyphenyl, 2,4,6 bromophenyl, 2,4,6 triethoxyphenyl group etc.
c) Organoaluminum compound of general formula AlR'nCl3-n, wherein n is between 1-2; R = methyl or ethyl
d) The mole ratio of Mg/M was 10 to 20.
e) The mole ratio of Al/M was 8 to 16 preferably 12 to 13.
f) Typically the solid pre-catalysts contained 2.5 to 6 weight % M (Ti or Zr), 10 to 12 weight % Mg and 0.8 to 1.1 weight % Al.

g) The pre-catalyst thus prepared according to the process of the present disclosure was used for the polymerization of €-olefins of general formula CnH2n where n is 8 to 12 in presence of suitable co-catalyst.
h) Co-catalysts useful in the present disclosure were trialkylaluminium compounds,
representative examples of such compounds are trimethylaluminium,
triethylaluminium, tri-n-butylaluminium, tri-n-propylaluminium,
triisobutylaluminium, tri-tert-butylaluminum, tri-n-hexylaluminium, tri-n-octylaluminium or aluminoxanes compounds, like methylaluminoxane (MAO) or modified methylaluminoxane (MMAO).
i) For polymerization the mole ratio of Al/M was 2 to 20, preferably 10.
j) The mole ratio of monomer or €α-olefin/M was 200 to 1000, preferably 250-300.
k) The polymerization temperature is at 0 to [-10] °C, preferably at 0 °C for 24 to 72 h, preferably for 48 h.
l) The particle size of magnesium chloride was in the range of 0.15 to 2.0 mm.
Example 1- Synthesis of catalyst comprising zirconium (pre-catalyst 1) [0080] To a two necked reactor equipped with a magnetic bar nitrogen inlet and outlet addition funnel 100 ml of dry n-hexane (solvent) was added, followed by 1.15 g (4.24 mmol) zirconium(IV) ethoxide and 6.2 g (65 mmol) of anhydrous magnesium chloride. The mixture was stirred at 80 °C for one hour (pre-mixture 1). The temperature was brought to 40 °C and 6.2 g (6.5 ml) of diethyl aluminium chloride in 20 ml of n-hexane was added dropwise over period of half an hour (pre-mixture 2). The temperature was raised to 80 °C and maintained for two hours. The obtained greenish black slurry was cooled to room temperature and washed with dry n-hexane (50 ml three times). Finally, the solid catalyst was dried under vacuum and stored in glove box for further use. The solid catalyst was characterized using solid-state NMR and elemental analyses were done using ICP. The catalyst component contained following percentage by weight: Zr 5.37%; Al 0.77%; Mg 16.99%. Said example corresponds to Polymer S.No 1 of Table 1 below.
Example 2- Synthesis of catalyst comprising titanium (pre-catalyst 2)

[0081] Titanium(IV) ethoxide (1 g, 4.4 mmol), anhydrous magnesium chloride (6.1 g, 64 mmol) were reacted with 6.34 g (6.6 ml) of diethyl aluminium chloride and the reaction was carried out in similar manner as mentioned for pre-catalyst 1. The brownish black obtained catalyst component contained following percentage by weight: Ti 3.02 %; Al 0.87%; Mg 11.57%. Said example corresponds to Polymer S.No 2 of Table 2 below.
Example 3
General procedure for preparation of polymer- polymerization of a-olefins (1-
decene)
[0082] In a 250 ml jacketed reactor equipped with a magnetic bar,1 g of pre-catalyst was loaded in glove box or under argon and closed properly with septum. Then 30 ml of dry 1-decene was added to it through septum under argon atmosphere followed by 2ml of MAO (for M [Ti or Zr]:Al= 10) (first aluminium compound) and suitable monomer (first mixture). The polymerization was carried out for 48 hours by stirring reaction mixture gently at 0° C. The polymerization reaction was quenched by adding acidified methanol. The obtained polymer was dissolved in toluene and reprecipitated from methanol solution. The white polymer was filtered and dried under vacuum to a constant weight. The polymers were characterized using NMR spectral analysis (Figure 1-2). The molecular weights (Mw and Mn) and PDI values were obtained from GPC (Figure 3); viscosity average molecular weights are obtained using a Cannon-Ubbelohde four bulb shear dilution viscometer (in THF solvent at 25° C) and melting temperatures are obtained from DSC curves (Figure 4). The polymerization results are given below in Table 1. Said example corresponds to Polymer S.No 3 of Table 3 below. Table 1: Polymerization data of 1-decene using pre-catalysts 1 and 2 and cocatalyst MAOa.

Polymer S. No. Pre-cat.
1 [M]: Al* [M]: Monomer Mvb Mwc Mnc Mw/Mnc [PDI] Melting Temp.d (ºC)
1
1:10 1:300 5.9×104 1.32×106 8.05×105 1.64 106, 117





2.78×103 2.08×103 1.35

2 1
2 2 1
2
2 1
2 1:20 1:300 6.64×105 2.07×105 3.21





1.7×103 1.1×103 1.55
3
1:10 1:250 2.88×105 1.02×106 5.21×105 1.96 101, 127
4
1:20 1:250 2.98×105 1.01×106 5.01×105 2.01
5
Withou t MAO 1:300 No polymerization observed
6
Withou t MAO 1:250 No polymerization observed
7
1:20 1:2500 7.9×105
8
Withou t MAO 1:300 No polymerization observed
9
Withou t MAO 1:250 No polymerization observed
*-Al refers to Aluminium from first aluminium or MAO and M refers to Ti or Zr; apolymerization conditions as described in Example 3; bobtained from intrinsic viscosity obtained by Mark-Houwink equation with K = 5.19×10-3 mL/g and a = 0,77 in THF at 25 ºC; cmeasured by GPC in CHCl3at 25 ºC (Figures 3a-d); dobtained from DSC curve (from 1st heating cycle with a heating and cooling rate of 10 K min1) (Figures 4a-b). [0083] The 1H, 13C NMR spectra of poly(1-decene) (500 MHz, RT, CDCl3) were recorded and provided in Figures 1-2. The 13C NMR spectrum was found to be in good agreement with the reported values of poly(1-decene), obtained from the related literature (J. Polym. Sci. Part A: Polym. Chem. 2009, 47, 4314). Furthermore, it is noted that polymer S.No 1 reveals two species. Without being bound by theory, it is suggested that this could be due to multisite nature of the catalyst. If two catalytic species exist in the same polymerization system, then two different types of polymers can form.
Example 4
Drag reducing ability of polymers
[0084] The extent of drag reduction by the polymer was evaluated using rheological
experiments wherein, the polymer concentration was varied between 10 and 50 ppm in
diesel (hydrocarbon liquid) (Petrol Sci Technol 2015, 33, 943).

[0085] All rheological experiments were performed in Anton-Paar MCR 302 rotational rheometer equipped with a Couette-type cell (CC27/T200/SS). The liquid sample volume (20 mL) was kept fixed, and in the isothermal experiments, the temperature was maintained at 25,00 ± 0.01°C by a constant temperature circulating apparatus. The torque ratio with and without polymer addition was measured up to a Reynolds number (Re) of 3000.
[0086] Equations used for the conversion of Torque to Drag Reduction (Equation 1) and Shear Rate to Reynolds Number (Equation 2) are also mentioned below.

Where:
%DR is the Drag Reduction (%),
Ts is the Torque measured for DRA solution,
Tp is the Torque measured for the pure solvent (Diesel in our case),
Ts and Tp values are to be taken of solution and solvent at the same Reynolds Number
(Re)

Where:
. Re is the Reynolds Number
• y is the shear rate (1/s),
. Ro (28.912 mm) and Ri (26.656 mm) are respectively the outer and inner radii of the cylinders,
• P is the density (810 kg/m3), and
. ή is the dynamic viscosity (mPa.s)

[0087] Accordingly, torque (mN.m) and shear rate (s-1) data was converted to drag reduction (%) and Reynolds number (unitless), respectively. (J. Non-Newton Fluid Mech. 2001, 97, 1; J. Appl. Polym. Sci. 2016, 133).
[0088] Figure 5 is a plot of viscosity vs shear for Polymer 1 (Example 1 above); whereas, the plot of % drag reduction vs Reynolds number is shown in Figure 6. [0089] Figure 7 is a plot of viscosity vs shear for Polymer 2 (Example 2 above); whereas, the plot of % drag reduction vs Reynolds number is shown in Figure 8. [0090] Figure 9 is a plot of viscosity vs shear for Polymer 3 (Example 3 above); whereas, the plot of % drag reduction vs Reynolds number is shown in Figure 10.
Table 2: Percentage drag reduction obtained for Polymers 1 to 3

Percentage drag reduction
Polymer S. No. 10ppm 50ppm
1 4 18
2 3 16
3 8 23
[0091] The polymer 1-3 (from Table 1) were added onto to diesel in two different concentrations, namely 10 and 50 ppm. As can be seen from Figures 5, 7 and 9, the addition of polymer significantly reduced the viscosity of diesel. Furthermore, the associated drag reduction data (Figures 5, 7 and 10) also revealed enhanced reduction upon the addition of said polymers. The results of the percentage drag reduction have been summarized above in Table 2. Polymer 3 was found to perform best affecting a drag reduction of 8% and 23% upon addition of 10 and 50 ppm polymer into diesel. [0092] Although the subject matter has been described in considerable detail with reference to certain examples and implementations thereof, other implementations are possible.
Advantages gained from the present disclosure

[0093] The present disclosure reveals a convenient process to obtain ultra-high molecular weight polyolefins. Said process combines the use of a pre-catalyst and a first aluminium compound which ensures the polymer has a weight (Mw) range in the range of 106 - 107 g/mol. Said polymers are valuable as drag reducing agents.

I/We Claim:
1. A process for preparing a polymer, said process comprising the steps of:
(a) obtaining at least one pre-catalyst;
(b) contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin to obtain a first mixture; and
(c) processing the first mixture to obtain the polymer,
wherein the at least one a-olefin has a carbon chain length in the range of C8 -
C12.
2. The process as claimed in claim 1, wherein contacting the at least one pre-catalyst with a first aluminium compound and at least one a-olefin is carried out at a temperature in the range of -10 to 0 °C for a period in the range of 24 - 72 hours to obtain the first mixture.
3. The process as claimed in claim 1, wherein the first aluminium compound is selected from the group consisting of aluminoxane, trialkylaluminium, and combinations thereof.
4. The process as claimed in claim 3, wherein the aluminoxane is selected from the group consisting of methylaluminoxane (MAO), modified-methylaluminoxane (MMAO), and combinations thereof.
5. The process as claimed in any one of the claims 1-4, wherein the polymer has a weight (Mw) range in the range of 106 - 107 g/mol.
6. A polymer obtained from the process as claimed in any one of the claims 1-5, wherein the polymer has a polydispersity index in the range of 1-3.5.
7. The polymer as claimed in claim 6, wherein the polymer has an application selected from the group consisting of friction modifiers, drag reducing agents, oil pipeline additives, and combinations thereof.
8. The polymer as claimed in claim 6, for use in pipelines as drag reducing agent.
9. The process as claimed in claim 1, wherein obtaining the at least one pre-catalyst comprises:
a) obtaining a compound of Formula M(OR)x;

b) contacting the compound of Formula M(OR)x with at least one
magnesium halide in the presence of a solvent to obtain a pre-mixture 1;
c) contacting the pre-mixture 1 with at least one alkyl aluminium
compound to obtain a pre-mixture 2; and
d) processing the pre-mixture 2 to obtain the at least one pre-catalyst,
wherein the at least one magnesium halide to the compound of Formula
M(OR)x mole ratio is in the range of 1:10 - 1:20.
10. The process as claimed in claim 9, wherein the alkyl aluminium compound to the compound of Formula M(OR)x mole ratio is in the range of 1:8 - 1:16.
11. The process as claimed in claim 9, wherein M of the compound of Formula M(OR)x is at least one transition metal (M) selected from the group consisting of group IV-B metals, group V-B metals, and combinations thereof.
12. The process as claimed in claims 1 and 9, wherein the first aluminium compound to the compound of Formula M(OR)x mole ratio is in the range of 1:2 - 1:20.
13. The process as claimed in claim 11, wherein M of the compound Formula M(OR)x is at least one transition metal (M) selected from Ti, Zr, Hf, V, Nb, or Ta.
14. The process as claimed in claim 9, wherein R of the compound of Formula
M(OR)x is selected from the group consisting of C1-15 alkyl, C5-15 aryl, C1-15
haloalkyl, C3-12 cycloalkyl, C1-20 heteroaryl, and C1-20 heterocyclyl, wherein C5-
15 aryl is optionally substituted with 1 - 3 groups selected from halogen, C1-8
alkyl or C1-8 alkoxy; x is 2 to 5.
15. The process as claimed in claim 14, wherein R of the compound Formula M(OR)x is selected from the group consisting of C1-8 alkyl and C5-12 aryl; x is 4.
16. The process as claimed in claim 9, wherein the at least one alkyl aluminium compound has a Formula AlR'nCl3-n and wherein R' is Cl-5 alkyl; n is 1 to 2.
17. The process as claimed in claim 9, wherein the solvent has a formula CmH2m+2; wherein m is 5 to 12.

18. The process as claimed in claim 9, wherein the magnesium halide is a magnesium salt of at least one halide selected from the group consisting of fluoride, chloride, bromide, iodide, and combinations thereof.
19. The process as claimed in claim 9, wherein the at least one pre-catalyst has a a) transition metal content (M) in the range of 2.5 - 6 wt.% with respect to the at least one pre-catalyst; b) elemental magnesium content in the range of 10 - 12 wt.% with respect to the at least one pre-catalyst; and c) elemental aluminium in the range of 0.8 - 1.1 wt.% with respect to the at least one pre-catalyst.
20. The process as claimed in any of the claims 1-14, wherein the a-olefin to the compound of Formula M(OR)x mole ratio is in the range of 200 - 1000.
21. The process as claimed in claim 9, wherein contacting the compound having Formula MORx with at least one magnesium halide in the presence of the solvent is carried out at a temperature in the range of 60-100 °C for a period in the range of 0.5 - 2 hours to obtain a pre-mixture 1.
22. The process as claimed in claim 9, wherein contacting the pre-mixture 1 with at least one alkyl aluminium compound is carried out at a temperature in the range of 30 - 100 °C for a period in the range of 0.2 - 3 hours to obtain a pre-mixture 2.
23. The at least one pre-catalyst obtained by a process as claimed in claim 9.

Documents

Orders

Section Controller Decision Date
25(1) Amarendra Samal 2024-04-05
25(1) Amarendra Samal 2024-04-05

Application Documents

# Name Date
1 201821044261-FORM 4 [03-01-2025(online)].pdf 2025-01-03
1 201821044261-STATEMENT OF UNDERTAKING (FORM 3) [23-11-2018(online)].pdf 2018-11-23
2 201821044261-REQUEST FOR EXAMINATION (FORM-18) [23-11-2018(online)].pdf 2018-11-23
2 201821044261-IntimationOfGrant05-04-2024.pdf 2024-04-05
3 201821044261-PatentCertificate05-04-2024.pdf 2024-04-05
3 201821044261-FORM 18 [23-11-2018(online)].pdf 2018-11-23
4 201821044261-FORM 1 [23-11-2018(online)].pdf 2018-11-23
4 201821044261-Annexure [11-03-2024(online)].pdf 2024-03-11
5 201821044261-Written submissions and relevant documents [11-03-2024(online)].pdf 2024-03-11
5 201821044261-DRAWINGS [23-11-2018(online)].pdf 2018-11-23
6 201821044261-DECLARATION OF INVENTORSHIP (FORM 5) [23-11-2018(online)].pdf 2018-11-23
6 201821044261-Correspondence to notify the Controller [23-02-2024(online)].pdf 2024-02-23
7 201821044261-FORM-26 [23-02-2024(online)].pdf 2024-02-23
7 201821044261-COMPLETE SPECIFICATION [23-11-2018(online)].pdf 2018-11-23
8 201821044261-PreGrant-ExtendedHearingNotice-(HearingDate-26-02-2024).pdf 2024-01-24
8 201821044261-FORM-26 [25-02-2019(online)].pdf 2019-02-25
9 201821044261-REQUEST FOR ADJOURNMENT OF HEARING UNDER RULE 129A [19-01-2024(online)]-1.pdf 2024-01-19
9 201821044261-Proof of Right (MANDATORY) [27-02-2019(online)].pdf 2019-02-27
10 201821044261-ORIGINAL UR 6(1A) FORM 26-050319.pdf 2019-12-27
10 201821044261-REQUEST FOR ADJOURNMENT OF HEARING UNDER RULE 129A [19-01-2024(online)].pdf 2024-01-19
11 201821044261-ORIGINAL UR 6(1A) FORM 1-050319.pdf 2019-12-27
11 201821044261-PreGrant-HearingNotice-(HearingDate-24-01-2024).pdf 2023-12-22
12 201821044261- CORRESPONDENCE(IPO)-(DAE LETTER)-(06-07-2020).pdf 2020-07-06
12 201821044261-AMMENDED DOCUMENTS [10-11-2023(online)].pdf 2023-11-10
13 201821044261-Annexure [10-11-2023(online)].pdf 2023-11-10
13 201821044261-FER.pdf 2020-08-12
14 201821044261-FORM 13 [10-11-2023(online)].pdf 2023-11-10
14 201821044261-PRE GRANT OPPOSITION FORM [27-08-2020(online)].pdf 2020-08-27
15 201821044261-MARKED COPIES OF AMENDEMENTS [10-11-2023(online)].pdf 2023-11-10
15 201821044261-PRE GRANT OPPOSITION DOCUMENT [27-08-2020(online)].pdf 2020-08-27
16 201821044261-FORM-26 [28-08-2020(online)].pdf 2020-08-28
16 201821044261-Statement and Evidence [10-11-2023(online)].pdf 2023-11-10
17 201821044261- Notice Of Opposition.pdf 2023-09-14
17 201821044261-Response to office action [24-10-2020(online)].pdf 2020-10-24
18 201821044261-FORM 13 [11-04-2022(online)].pdf 2022-04-11
18 201821044261-RELEVANT DOCUMENTS [02-11-2020(online)].pdf 2020-11-02
19 201821044261-POA [11-04-2022(online)].pdf 2022-04-11
19 201821044261-FORM-26 [02-11-2020(online)].pdf 2020-11-02
20 201821044261-FORM 13 [02-11-2020(online)].pdf 2020-11-02
20 201821044261-RELEVANT DOCUMENTS [11-04-2022(online)].pdf 2022-04-11
21 201821044261-ORIGINAL UR 6(1A) FORM 26-271120.pdf 2021-10-18
21 201821044261-OTHERS [10-02-2021(online)].pdf 2021-02-10
22 201821044261-CLAIMS [10-02-2021(online)].pdf 2021-02-10
22 201821044261-FER_SER_REPLY [10-02-2021(online)].pdf 2021-02-10
23 201821044261-DRAWING [10-02-2021(online)].pdf 2021-02-10
24 201821044261-CLAIMS [10-02-2021(online)].pdf 2021-02-10
24 201821044261-FER_SER_REPLY [10-02-2021(online)].pdf 2021-02-10
25 201821044261-OTHERS [10-02-2021(online)].pdf 2021-02-10
25 201821044261-ORIGINAL UR 6(1A) FORM 26-271120.pdf 2021-10-18
26 201821044261-RELEVANT DOCUMENTS [11-04-2022(online)].pdf 2022-04-11
26 201821044261-FORM 13 [02-11-2020(online)].pdf 2020-11-02
27 201821044261-FORM-26 [02-11-2020(online)].pdf 2020-11-02
27 201821044261-POA [11-04-2022(online)].pdf 2022-04-11
28 201821044261-FORM 13 [11-04-2022(online)].pdf 2022-04-11
28 201821044261-RELEVANT DOCUMENTS [02-11-2020(online)].pdf 2020-11-02
29 201821044261- Notice Of Opposition.pdf 2023-09-14
29 201821044261-Response to office action [24-10-2020(online)].pdf 2020-10-24
30 201821044261-FORM-26 [28-08-2020(online)].pdf 2020-08-28
30 201821044261-Statement and Evidence [10-11-2023(online)].pdf 2023-11-10
31 201821044261-MARKED COPIES OF AMENDEMENTS [10-11-2023(online)].pdf 2023-11-10
31 201821044261-PRE GRANT OPPOSITION DOCUMENT [27-08-2020(online)].pdf 2020-08-27
32 201821044261-FORM 13 [10-11-2023(online)].pdf 2023-11-10
32 201821044261-PRE GRANT OPPOSITION FORM [27-08-2020(online)].pdf 2020-08-27
33 201821044261-Annexure [10-11-2023(online)].pdf 2023-11-10
33 201821044261-FER.pdf 2020-08-12
34 201821044261- CORRESPONDENCE(IPO)-(DAE LETTER)-(06-07-2020).pdf 2020-07-06
34 201821044261-AMMENDED DOCUMENTS [10-11-2023(online)].pdf 2023-11-10
35 201821044261-ORIGINAL UR 6(1A) FORM 1-050319.pdf 2019-12-27
35 201821044261-PreGrant-HearingNotice-(HearingDate-24-01-2024).pdf 2023-12-22
36 201821044261-ORIGINAL UR 6(1A) FORM 26-050319.pdf 2019-12-27
36 201821044261-REQUEST FOR ADJOURNMENT OF HEARING UNDER RULE 129A [19-01-2024(online)].pdf 2024-01-19
37 201821044261-REQUEST FOR ADJOURNMENT OF HEARING UNDER RULE 129A [19-01-2024(online)]-1.pdf 2024-01-19
37 201821044261-Proof of Right (MANDATORY) [27-02-2019(online)].pdf 2019-02-27
38 201821044261-PreGrant-ExtendedHearingNotice-(HearingDate-26-02-2024).pdf 2024-01-24
38 201821044261-FORM-26 [25-02-2019(online)].pdf 2019-02-25
39 201821044261-FORM-26 [23-02-2024(online)].pdf 2024-02-23
39 201821044261-COMPLETE SPECIFICATION [23-11-2018(online)].pdf 2018-11-23
40 201821044261-DECLARATION OF INVENTORSHIP (FORM 5) [23-11-2018(online)].pdf 2018-11-23
40 201821044261-Correspondence to notify the Controller [23-02-2024(online)].pdf 2024-02-23
41 201821044261-Written submissions and relevant documents [11-03-2024(online)].pdf 2024-03-11
41 201821044261-DRAWINGS [23-11-2018(online)].pdf 2018-11-23
42 201821044261-FORM 1 [23-11-2018(online)].pdf 2018-11-23
42 201821044261-Annexure [11-03-2024(online)].pdf 2024-03-11
43 201821044261-FORM 18 [23-11-2018(online)].pdf 2018-11-23
43 201821044261-PatentCertificate05-04-2024.pdf 2024-04-05
44 201821044261-IntimationOfGrant05-04-2024.pdf 2024-04-05
44 201821044261-REQUEST FOR EXAMINATION (FORM-18) [23-11-2018(online)].pdf 2018-11-23
45 201821044261-FORM 4 [03-01-2025(online)].pdf 2025-01-03
45 201821044261-STATEMENT OF UNDERTAKING (FORM 3) [23-11-2018(online)].pdf 2018-11-23

Search Strategy

1 SearchstrategyE_03-07-2020.pdf
2 SCREENSHOTAE_09-12-2022.pdf

ERegister / Renewals

3rd: 03 Jan 2025

From 23/11/2020 - To 23/11/2021

4th: 03 Jan 2025

From 23/11/2021 - To 23/11/2022

5th: 03 Jan 2025

From 23/11/2022 - To 23/11/2023

6th: 03 Jan 2025

From 23/11/2023 - To 23/11/2024

7th: 03 Jan 2025

From 23/11/2024 - To 23/11/2025

8th: 21 Nov 2025

From 23/11/2025 - To 23/11/2026

9th: 21 Nov 2025

From 23/11/2026 - To 23/11/2027

10th: 21 Nov 2025

From 23/11/2027 - To 23/11/2028