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Process For Preparation Of Soap Noodles

Abstract: The present disclosure discloses a process for fatty acid neutralization comprising sequential addition of the following ingredients to a reactor followed by processing: (a) a first brine solution; (b) a first part of distilled fatty acids; (c) a first part of caustic solution; (d) lauric acid flakes or palm kernel based fatty acids or coconut fatty acids or mixed fatty acids of C12-C14 chain length; (e) second part of distilled fatty acids and a second part of caustic solution; and (f) additives and a second brine solution, to obtain soap noodle having color units in the range of 0.6 to 1.3.

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Patent Information

Application #
Filing Date
29 December 2017
Publication Number
27/2019
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
iprdel@lakshmisri.com
Parent Application

Applicants

ITC LIMITED
ITC LIFE SCIENCES & TECHNOLOGY CENTRE #3. 1ST Main, Peenya Industrial Area, Phase -1, Bangalore 560 058, India

Inventors

1. KOTA, Lakshmi Sravanthi
ITC LIMITED, ITC LIFE SCIENCES & TECHNOLOGY CENTRE, PEENYA INDUSTRIAL AREA, PHASE 1, BANGALORE 560058, India
2. GEORGE, Rikku Sarah
ITC LIMITED, ITC LIFE SCIENCES & TECHNOLOGY CENTRE, PEENYA INDUSTRIAL AREA, PHASE 1, BANGALORE 560058.
3. JAYAPRAKASH, Doss
ITC LIMITED, ITC LIFE SCIENCES & TECHNOLOGY CENTRE, PEENYA INDUSTRIAL AREA, PHASE 1, BANGALORE 560058.

Specification

FILED OF INVENTION
[001] The present disclosure broadly relates to the field of cosmetics and personal hygiene and particularly relates to process for preparing soap noodle.
BACKGROUND OF INVENTION
[002] Preparation of soap requires two major raw materials: fat and alkali. Animal fat or vegetable oils comprise fat and sodium hydroxide or potassium hydroxide comprises alkali matter. A commonly followed process involves generating distilled fatty acids (DFA) by hydrolyzing fats and oils under high pressure followed by purification by distillation. The distilled fatty acids are further neutralized with an alkali to produce soap and water. Generating the distilled fatty acids provides benefit of using different types of fatty acids in preparation of soap rather than directly using animal fat.
[003] One of the most important step during manufacture of soap using distilled fatty acids is neutralization of the fatty acids. The distilled fatty acids are neutralized to obtain soap noodles which is further mixed with additives, fragrance, and color to obtain the final soap product. Many of the problems associated with quality, color, texture of the soap noodles finds their root causes in the manner in which fatty acid neutralization is carried out.
[004] Fatty acid neutralization at industrial scale for the manufacture of soap noodles is carried out in large reactors called crutchers. Typically, crutchers are equipped with provisions for addition of raw materials which include distilled fatty acids, alkali amongst other components. Various types of crutchers have been in use that employ different mechanisms to introduce caustic (alkali) during fatty acid neutralization process.
[005] The conventional fatty acid neutralization process in a typical crutcher suffers from numerous shortcomings which include: charring of fatty acid such as lauric acid flakes during mixing with hot DFA; and pocket formation or lump formation during fatty acid neutralization resulting in a product with inferior color profiles. Further, there is always a possibility of blockage of the outlet of the crutcher on account of improper mixing or improper temperature regulation during

the fatty acid neutralization process. The charring of lauric acid flakes during the conventional neutralization process leads to formation of brown spots in the soap noodles, which is considered undesirable. Also, it is observed that considerable amount of time is invested in the process of fatty acid neutralization thereby increasing the operating costs in manufacturing soaps. Thus, the conventional process of neutralization of fatty acid is not desirable for obtaining soap noodles to manufacture final soap product.
[006] WO2008140432 discloses a process for removal of free fatty acids (FFA) content of industrial and/or edible vegetable oils by using a chemical method and a new reactor configuration.
[007] US5990074 discloses a process for producing soap from a mixed feedstock of at least one triglyceride and at least one free fatty acid which comprises contacting at least one triglyceride and at least one free fatty acid with strong alkali at an elevated temperature.
[008] Therefore, there exists a need for a method that overcomes the above-mentioned problems and simultaneously improves the color of the resulting soap noodles.
SUMMARY OF THE INVENTION
[009] In an aspect of the present invention, there is provided a process of neutralizing fatty acid content to obtain soap noodle, said method comprising: (a) adding a first brine solution to a reactor; (b) contacting a first part of distilled fatty acid with the first brine solution to obtain a first mixture; (c) contacting a first part of caustic solution with the first mixture to obtain a second mixture; (d) contacting at least one fatty acid selected from the group consisting of Cn fatty acid, mixture of C12-C14 fatty acid, palm kernel based fatty acid, coconut fatty acid, and combinations thereof, with the second mixture to obtain a third mixture; (e) contacting a second part of distilled fatty acid and a second part of caustic solution with the third mixture to obtain a fourth mixture; (f) contacting at least one additive and a second brine solution with the fourth mixture to obtain a fifth mixture; and (g) processing the fifth mixture, wherein the first brine solution occupies 2% to

15% volume of the reactor, and wherein the process leads to neutralization of fatty acid content to obtain soap noodle having color units in the range of 0.6 to 1.3. [0010] In an aspect of the present invention, there is provided a process of neutralizing fatty acid content to obtain soap noodle, said method comprising: (a) adding a first brine solution having a concentration of sodium chloride in the range of 0.5%-0.6% w/v to a reactor at a temperature in the range of 60°C-65°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm, wherein the first brine solution occupies 2%-15% of volume of the reactor; (b) contacting a first part of distilled fatty acid having a weight percentage in the range of 5%-25% with respect to total distilled fatty acid with the first brine solution at a temperature in the range of 70°C-80°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm to obtain a first mixture; (c) contacting a first part of caustic solution having a concentration of sodium hydroxide (NaOH) in the range of 25% w/v to 47% w/v with the first mixture to obtain a second mixture; (d) contacting at least one fatty acid selected from the group consisting of Cn fatty acid, mixture of C12-C14 fatty acid, palm kernel based fatty acid, coconut fatty acid, and combinations thereof having a weight percentage in the range of 5%-40% with respect to fatty acid content of the soap noodle with the second mixture at a temperature in the range of 65°C-75°C for a time period in the range of 15-30 minutes under continuous agitation at 80-120 rpm to obtain a third mixture, wherein the at least one fatty acid occupies 5%-10% volume of the reactor; (e) contacting a second part of distilled fatty acid having a weight percentage in the range of 25%-55% with respect to total distilled fatty acid and a second part of caustic solution with the third mixture for a time period in the range of 10-20 minutes under continuous agitation at 80-120 rpm to obtain a fourth mixture; (f) contacting at least one additive having a weight percentage in the range of 0.04%-0.07%) with respect to total soap composition selected from the group consisting of EDTA (ethyl enediaminetetraacetic acid), EHDP (ethane 1-hydroxy-1, 1-diphosphonate), and combinations thereof, and a second brine solution having a concentration of sodium chloride (NaCl) in the range of 0.15%-0.2% w/v to the fourth mixture for a time period in the range of 5-10 minutes under continuous

agitation at 80-120 rpm to obtain a fifth mixture; and (g) processing the fifth mixture, wherein the distilled fatty acid is selected from the group consisting of C16-C20 fatty acid, and combinations thereof, and wherein the process leads to neutralization of fatty acid content to obtain soap noodle having color units in the range of 0.6 to 1.3.
[0011] 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
[0012] 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.
[0013] Figure 1 depicts soap noodle obtained by following the process disclosed in the present invention, in accordance with an embodiment of the present disclosure. [0014] Figure 2 depicts soap noodle obtained through conventional process, in accordance with an embodiment of the present disclosure.
DETAILED DESCRIPTION OF THE INVENTION
[0015] 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

[0016] 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.
[0017] 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.
[0018] 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".
[0019] 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.
[0020] The term "including" is used to mean "including but not limited to".
"Including" and "including but not limited to" are used interchangeably.
[0021] Typically, formation of soap involves neutralization of sodium hydroxide
with fatty acids. Free caustic alkali is the amount of unreacted sodium hydroxide
present in the soap composition.
[0022] For the purposes of present document, color is measured using a Lovibond®
Tintometer® instrument. The sample is measured in a 5 1/4 " cell of the instrument
and according to the color of the sample a unit is assigned.
[0023] For the purposes of the present document, a reactor should be construed
broadly to define a crutcher or a mixer. A reactor can be a crutcher with or without
a conical bottom, and can come in different configurations as is known in the art.
[0024] For the purposes of the present document, fatty acid content of soap noodle
comprises distilled fatty acid selected from group consisting of C16-C20 fatty acid,
and combinations thereof; and at least one fatty acid selected from the group

consisting of C12 fatty acid, mixture of C12-C14 fatty acid, palm kernel based fatty acid, coconut fatty acid, and combinations thereof.
[0025] 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. [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 the scope of the disclosure, as described herein. [0027] The process as disclosed comprises sequential addition of the following ingredients to a reactor followed by processing: (a) a first brine solution; (b) a first part of distilled fatty acids; (c) a first part of caustic solution; (d) lauric acid flakes or palm kernel based fatty acids or coconut fatty acids or mixed fatty acids of C12-C14 chain length; (e) second part of distilled fatty acids and a second part of caustic solution; and (f) additives and a second brine solution. The distilled fatty acids comprise fatty acids having broad chain length of C16-C20, preferably C16-C18 fatty acids. Hence, different types of fatty acids are added in a particular sequence in a specific temperature range as disclosed to ensure better mixing of alkali with fatty acids during neutralization process to obtain soap noodle having desirable characteristics. The process as disclosed in the present disclosure helps in avoiding charring of lauric acid flakes during the neutralization process thus, improves the color and texture of soap noodles. Additionally, the method as disclosed herein not only avoids choking of the outlet at the bottom of the reactor but it also avoids pocket formation during mixing.
[0028] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle, said process comprising: (a) adding a first brine solution to a reactor; (b) contacting a first part of distilled fatty acid with the first brine solution to obtain a first mixture; (c) contacting a first part

of caustic solution with the first mixture to obtain a second mixture; (d) contacting at least one fatty acid selected from the group consisting of C12 fatty acid, mixture of C12-C14 fatty acid, palm kernel based fatty acid, coconut fatty acid, and combinations thereof, with the second mixture to obtain a third mixture; (e) contacting a second part of distilled fatty acid and a second part of caustic solution with the third mixture to obtain a fourth mixture; (f) contacting at least one additive and a second brine solution with the fourth mixture to obtain a fifth mixture; and (g) processing the fifth mixture, wherein the first brine solution occupies 2% to 15% volume of the reactor, and wherein the process leads to neutralization of fatty acid content to obtain soap noodle having color units in the range of 0.6 to 1.3. [0029] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the process leads to neutralization of fatty acid content to obtain soap noodle having color units in the range of 0.6 to 1.1.
[0030] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the first brine solution has a concentration of sodium chloride (NaCl) in the range of 0.5%-0.6% w/v. In another embodiment of the present disclosure, the first brine solution has a concentration of sodium chloride (NaCl) in the range of 0.51%-0.59% w/v.
[0031] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the first part of distilled fatty acid has a weight percentage in the range of 5%-25% with respect to distilled fatty acid content of the soap noodle. In another embodiment of the present disclosure, the first part of distilled fatty acid has a weight percentage in the range of 10%-20% with respect to distilled fatty acid content of the soap noodle.
[0032] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the distilled fatty acid is in liquid state and the at least one fatty acid is in solid state in form of flakes.

[0033] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the at least one fatty acid is lauric acid in form of flakes.
[0034] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the distilled fatty acid is selected from the group consisting of C16-C20 fatty acid, and combinations thereof.
[0035] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the distilled fatty acid is selected from the group consisting of C16-C18 fatty acid, and combinations thereof.
[0036] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the distilled fatty acid comprises mono-unsaturated and poly-unsaturated fatty acid. [0037] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the distilled fatty acid is selected from the group consisting of C16-C20 fatty acid, and combinations thereof, and wherein the first part of distilled fatty acid has a weight percentage in the range of 5%-25% with respect to distilled fatty acid content of the soap noodle, and second part of distilled fatty acid has a weight percentage in the range of 75%-95% with respect to distilled fatty acid content of the soap noodle.
[0038] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the distilled fatty acid comprises saturated C16-C18 fatty acids, and unsaturated Ci8:i, Ci8:2, and Ci8:3 fatty acids.
[0039] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the fatty acid content of the soap noodle comprises a combination of distilled fatty acid and the at least one fatty acid in a w/w ratio in the range of 9:1 to 3:2. In another embodiment of the present disclosure, the fatty acid content of the soap

noodle comprises a combination of distilled fatty acid and the at least one fatty acid
in a w/w ratio in the range of 7.5:1 to 3:1.
[0040] In an embodiment of the present disclosure, there is provided a process of
neutralizing fatty acid content to obtain soap noodle as described herein, wherein
caustic solution has a concentration in the range of 25% to 47% w/v. In another
embodiment of the present disclosure, the caustic solution has a concentration in
the range of 30% to 40% w/v.
[0041] In an embodiment of the present disclosure, there is provided a process of
neutralizing fatty acid content to obtain soap noodle as described herein, wherein
caustic solution has a concentration in the range of 25% to 47% w/v.
[0042] In an embodiment of the present disclosure, there is provided a process of
neutralizing fatty acid content to obtain soap noodle as described herein, wherein
the at least one fatty acid has a weight percentage in the range of 5%-40% with
respect to fatty acid content of the soap noodle. In another embodiment of the
present disclosure, the at least one fatty acid has a weight percentage in the range
of 10%-30% with respect to fatty acid content of the soap noodle. In yet another
embodiment of the present disclosure, the at least one fatty acid has a weight
percentage in the range of 15%-25% with respect to fatty acid content of the soap
noodle.
[0043] In an embodiment of the present disclosure, there is provided a process of
neutralizing fatty acid content to obtain soap noodle as described herein, wherein
the first part of distilled fatty acid occupies 5%-25% volume of the reactor. In
another embodiment of the present disclosure, the first part of distilled fatty acid
occupies 10%-20% volume of the reactor.
[0044] In an embodiment of the present disclosure, there is provided a process of
neutralizing fatty acid content to obtain soap noodle as described herein, wherein
the second part of distilled fatty acid has a weight percentage in the range of 75%-
95%) with respect to distilled fatty acid content of the soap noodle. In another
embodiment of the present disclosure, the second part of distilled fatty acid has a
weight percentage in the range of 80%-90% with respect to distilled fatty acid
content of the soap noodle.

[0045] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the at least one additive is selected from the group consisting of EDTA (ethylenediaminetetraacetic acid) having a weight percentage in the range of 0.04%-0.07% with respect to soap noodle, and EHDP (ethane 1-hydroxy-l, 1-diphosphonate) having a weight percentage in the range of 0.12%-0.23% with respect to soap noodle. In another embodiment of the present disclosure, the at least one additive is selected from the group consisting of EDTA (ethylenediaminetetraacetic acid) having a weight percentage in the range of 0.05%-0.06% with respect to soap noodle, and EHDP (ethane 1-hydroxy-l, 1-diphosphonate) having a weight percentage in the range of 0.15%-0.20% with respect to soap noodle.
[0046] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the second brine solution has a concentration of sodium chloride (NaCl) in the range of 0.15%-0.2% w/v. In another embodiment of the present disclosure, the second brine solution has a concentration of sodium chloride (NaCl) in the range of 0.16%-0.19%w/v.
[0047] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein adding the first brine solution is carried out at a temperature in the range of 60°C-65°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm. In another embodiment of the present disclosure, adding the first brine solution is carried out at a temperature in the range of 62°C-64°C for a time period in the range of 6-8 minutes under continuous agitation at 90-110 rpm. [0048] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein contacting a first part of distilled fatty acid with the first brine solution is carried out at a temperature in the range of 70°C-80°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm. In another embodiment of the present disclosure, contacting a first part of distilled fatty acid with the first brine

solution is carried out at a temperature in the range of 72°C-78°C for a time period in the range of 6-8 minutes under continuous agitation at 90-110 rpm. [0049] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein contacting the at least one fatty acid with the second mixture is carried out at a temperature in the range of 65°C-75°C for a time period in the range of 15-30 minutes under continuous agitation at 80-120 rpm. In another embodiment of the present disclosure, contacting the at least one fatty acid with the second mixture is carried out at a temperature in the range of 67°C-72°C for a time period in the range of 20-25 minutes under continuous agitation at 90-110 rpm.
[0050] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein contacting the second part of distilled fatty acid and a second part of caustic solution with the third mixture is carried out for a time period in the range of 10-20 minutes under continuous agitation at 80-120 rpm. In another embodiment of the present disclosure, contacting the second part of distilled fatty acid and a second part of caustic solution with the third mixture is carried out for a time period in the range of 12-18 minutes under continuous agitation at 90-110 rpm. [0051] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein contacting the at least one additive and the second brine solution with the fourth mixture is carried out for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm. In another embodiment of the present disclosure, contacting the at least one additive and the second brine solution with the fourth mixture is carried out for a time period in the range of 6-8 minutes under continuous agitation at 90-110 rpm.
[0052] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the soap noodle has free caustic alkali concentration in the range of 0.02-0.08% with respect to the soap noodle. In another embodiment of the present disclosure,

the soap noodle has free caustic alkali concentration in the range of 0.03-0.07% with respect to the soap noodle.
[0053] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the process leads to homogenous mixing during neutralization of the fatty acid content to obtain the soap noodle.
[0054] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the contacting at least one fatty acid with the second mixture leads to decomposition of the at least one fatty acid in the range of 0.01%-0.1% with respect to the at least one fatty acid. The low percentage of decomposition of the at least one fatty acid indicates minimal charring of the fatty acid in the process thereby avoiding appearance of brown spots and imparting acceptable color to the soap noodle.
[0055] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle, said process comprising: (a) adding a first brine solution to a reactor; (b) contacting a first part of distilled fatty acid with the first brine solution to obtain a first mixture; (c) contacting a first part of caustic solution with the first mixture to obtain a second mixture; (d) contacting at least one fatty acid selected from the group consisting of Cn fatty acid, mixture of C12-C14 fatty acid, palm kernel based fatty acid, coconut fatty acid, and combinations thereof, with the second mixture to obtain a third mixture; (e) contacting a second part of distilled fatty acid and a second part of caustic solution with the third mixture to obtain a fourth mixture; (f) contacting at least one additive and a second brine solution with the fourth mixture to obtain a fifth mixture; and (g) processing the fifth mixture, wherein the first brine solution occupies 2% to 15% volume of the reactor, and wherein the process leads to neutralization of fatty acid content to obtain soap noodle having color units in the range of 0.6 to 1.3, and wherein the contacting at least one fatty acid with the second mixture leads to decomposition of the at least one fatty acid in the range of 0.01%-0.1% with respect to the at least one fatty acid.

[0056] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle, said method comprising: (a) adding a first brine solution having a concentration of sodium chloride in the range of 0.5%-0.6% w/v to a reactor at a temperature in the range of 60°C-65°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm, wherein the first brine solution occupies 2%-15% of volume of the reactor; (b) contacting a first part of distilled fatty acid having a weight percentage in the range of 5%-25% with respect to total distilled fatty acid with the first brine solution at a temperature in the range of 70°C-80°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm to obtain a first mixture; (c) contacting a first part of caustic solution having a concentration of sodium hydroxide (NaOH) in the range of 25% w/v to 47% w/v with the first mixture to obtain a second mixture, (d) contacting at least one fatty acid selected from the group consisting of Cn fatty acid, mixture of C12-C14 fatty acid, palm kernel based fatty acid, coconut fatty acid, and combinations thereof having a weight percentage in the range of 5%-40% with respect to fatty acid content of the soap noodle with the second mixture at a temperature in the range of 65°C-75°C for a time period in the range of 15-30 minutes under continuous agitation at 80-120 rpm to obtain a third mixture, wherein the at least one fatty acid occupies 5%-10% volume of the reactor; (e) contacting a second part of distilled fatty acid having a weight percentage in the range of 25%-55% with respect to total distilled fatty acid and a second part of caustic solution with the third mixture for a time period in the range of 10-20 minutes under continuous agitation at 80-120 rpm to obtain a fourth mixture; (f) contacting at least one additive having a weight percentage in the range of 0.04%-0.07%) with respect to total soap composition selected from the group consisting of EDTA, EHDP, and combinations thereof, and a second brine solution having a concentration of sodium chloride (NaCl) in the range of 0.15%>-0.2%> w/v to the fourth mixture for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm to obtain a fifth mixture; and (g) processing the fifth mixture, wherein the distilled fatty acid is selected from the group consisting of C16-C20 fatty acid, and combinations thereof, and wherein the process leads to

neutralization of fatty acid content to obtain soap noodle having color units in the range of 0.6 to 1.3. In another embodiment of the present disclosure, the process leads to neutralization of fatty acid content to obtain soap noodle having color units in the range of 0.7 to 1.2.
[0057] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle, said method comprising: (a) adding a first brine solution having a concentration of sodium chloride in the range of 0.5%-0.6% w/v to a reactor at a temperature in the range of 60°C-65°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm, wherein the first brine solution occupies 2%-15% of volume of the reactor; (b) contacting a first part of distilled fatty acid having a weight percentage in the range of 5%-25% with respect to total distilled fatty acid with the first brine solution at a temperature in the range of 70°C-80°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm to obtain a first mixture; (c) contacting a first part of caustic solution having a concentration of sodium hydroxide (NaOH) in the range of 25% w/v to 47% w/v with the first mixture to obtain a second mixture; (d) contacting lauric acid flakes having a weight percentage in the range of 5%>-40%) with respect to fatty acid content of the soap noodle with the second mixture at a temperature in the range of 65°C-75°C for a time period in the range of 15-30 minutes under continuous agitation at 80-120 rpm to obtain a third mixture, wherein the lauric acid flakes occupies 5%-10% volume of the reactor; (e) contacting a second part of distilled fatty acid having a weight percentage in the range of 25%>-55%> with respect to total distilled fatty acid and a second part of caustic solution with the third mixture for a time period in the range of 10-20 minutes under continuous agitation at 80-120 rpm to obtain a fourth mixture; (f) contacting at least one additive having a weight percentage in the range of 0.04%-0.07%) with respect to total soap composition selected from the group consisting of EDTA, EHDP, and combinations thereof, and a second brine solution having a concentration of sodium chloride (NaCl) in the range of 0.15%-0.2% w/v to the fourth mixture for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm to obtain a fifth mixture; and (g) processing the fifth

mixture, wherein the distilled fatty acid comprises saturated C16-C18 fatty acids, unsaturated Ci8:i, Ci8:2 and Ci8:3 fatty acids, and wherein the process leads to neutralization of fatty acid content to obtain soap noodle having color units in the range of 0.6 to 1.3. In another embodiment of the present disclosure, the first part of distilled fatty acid has a weight percentage in the range of 10%-20% with respect to total distilled fatty acid, and lauric acid flakes has a weight percentage in the range of 10%-25% with respect to fatty acid content of the soap noodle. In yet another embodiment of the present disclosure, the process leads to neutralization of fatty acid content to obtain soap noodle having color units in the range of 0.7 to 1.2.
[0058] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the process optionally includes contacting the fifth mixture with at least one benefit agent selected from the group consisting of humectants, surfactants, electrolytes, and combinations thereof.
[0059] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the humectants is selected from the group consisting of glycerine, sorbitol, propylene glycol, and combinations thereof, and the humectants is present in a weight percentage in the range of 1 to 10% w/w with respect to the soap noodle, the surfactants is selected from the group consisting of alfa olefin sulphonates, sodium lauryl ether sulphate, cocoamido propyl betaine, decyl glucoside, and combinations thereof, and the surfactant is present in a weight percentage in the range of 1 to 7% w/w with respect to the soap noodles, and the electrolytes is selected from the group consisting of chloride, sulphate, meta bisulphate, citrate salts of sodium or potassium, and the electrolytes is present in a weight percentage in the range of 0.2 to 0.6% w/w with respect to the soap noodles. [0060] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein contacting a first part of caustic solution with the first mixture is carried out in a gradual manner through distributor rings. In another embodiment of the present

disclosure, contacting a first part of caustic solution with the first mixture is carried out by pipes controlled by valves.
[0061] In an embodiment of the present disclosure, there is provided a process of neutralizing fatty acid content to obtain soap noodle as described herein, wherein the reactor is a crutcher with a conical bottom.
[0062] Although the subject matter has been described in considerable detail with reference to certain examples and implementations thereof, other implementations are possible. EXAMPLES
[0063] 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. [0064] The examples will be discussed in the succeeding sections highlighting the working and non-working examples. The non-working examples include carrying out fatty acid neutralization by adding various ingredients in a sequence differing in a manner as compared to the disclosed process. One of the non-working example displays the effect of not adding brine solution before the commencement of fatty acid neutralization process, another non-working example displays the undesirable characteristics of soap noodles obtained upon pre-melting lauric acid flakes along with distilled fatty acids. The working example displays the desirable characteristics of soap noodle in terms of color, odor, FCA (Free Caustic Alkali) content and SAST (Super Accelerated Stability Test) results obtained by the process as disclosed in the present disclosure.
Example 1

Process of fatty acid neutralization
[0065] The process as disclosed in the present disclosure involves fatty acid neutralization in a crutcher. The ingredients required are depicted in Table 1 and the steps are depicted in the following paragraphs. Table 1: Ingredients required for the process

[0066] Step 1 comprises adding the first brine solution to a crutcher at a temperature in the range of 60°C-65°C for a time period in the range of 5-10 minutes with continuous agitation at 80-120 rpm. The first brine solution is to be added in a volume so as to occupy 10%-30% volume of the crutcher.
[0067] Step 2 comprises contacting a first part of distilled fatty acid having a weight percentage in the range of 5%-25% with respect to total distilled fatty acid with the first brine solution at a temperature in the range of 70°C-80°C for a time period in the range of 5-10 minutes with continuous agitation at 80-120 rpm. It is important that only one part of total distilled fatty acid be added at this step which contacts the first brine solution to form a first mixture.

[0068] Step 3 comprises introducing a first part of caustic solution in a gradual manner into the crutcher. The first part of caustic solution forms a second mixture upon contacting the first mixture of previous step. Neutralization of distilled fatty acids is initiated at the present step.
[0069] Step 4 comprises addition of lauric acid flakes to the second mixture of previous step to facilitate neutralization of the lauric acid flakes. The addition of lauric acid flakes to be carried out a temperature in the range of 65°C-75°C for a time period in the range of 15-30 minutes with continuous agitation at 80-120 rpm. The lauric acid flakes is to be added so as to occupy 5%-10% of volume of the crutcher and the addition of lauric acid flakes forms a third mixture. [0070] Step 5 comprises addition of a second part of distilled fatty acid having a weight percentage in the range of 25%-55% with respect to total distilled fatty acid. A second part of caustic solution is also added in this step to further facilitate complete neutralization of fatty acid content. The step is to be carried out for a time period in the range of 10-20 minutes with continuous agitation at 80-120 rpm. [0071] Step 6 comprises addition of additives (EDTA and EHDP) and a second brine solution having a concentration of sodium chloride (NaCl) in the range of 0.15%-0.2% w/v for a time period in the range of 5-10 minutes with continuous agitation at 80-120 rpm.
[0072] The mixture obtained after step 6 is further processed by extruding and cutting to obtain soap noodle having the desired characteristics. [0073] The addition of distilled fatty acids in two separate steps and addition of lauric acid flakes separately from the distilled fatty acids ensure homogenous neutralization of the fatty acids thereby resulting in soap noodle with better sensorial as compared to the soap noodle obtained by conventional fatty acid neutralization process. The following working examples describe the properties of soap noodle obtained by following the disclosed process. The non-working examples describe the properties of soap noodle obtained by a deviated process. Example 2 Working Examples

[0074] The soap noodle obtained by a process as described in the Working
Example 1 as mentioned previously was assessed for various parameters of color,
odor, and free caustic alkali (FCA) content. The color, odor, and profile of the
obtained soap noodles are evaluated using Super Accelerated Stability Test
(SAST).
[0075] Estimation of FCA content - The acceptable FCA range in the obtained
soap noodle was considered as 0.02%-0.05% with respect to the soap noodle.
[0076] Procedure for SAST - Twenty-five grams of soap noodles was taken and
grated using a grater. The grated soap noodle was added to a conical flask and
sealed with a Teflon tape. The flask was placed in a hot air oven at 90°C for 16
hours. Post the incubation time, the flask was removed and allowed to reach room
temperature. Once the room temperature was attained the soap noodles were
evaluated for odor intensity, profile, and color.
[0077] Parameters for evaluating quality of soap noodle:
[0078] Color: Color of soap noodle was evaluated prior and post SAST. The color
was evaluated using Lovibond Tintometer and was assigned particular units
according to the color. A maximum of 1.3 units was acceptable post SAST for
desirable soap noodle.
[0079] Odor: A dry sniff test was performed by trained technician to evaluate
soap noodle based on fatty odor. A strong fatty odor was considered unacceptable.
[0080] FCA content: The FCA content was measured in accordance with BIS
Standard [METHODS OF SAMPLING AND TEST FOR SOAPS (Second
Revision; Fifth Reprint JULY 2007 (Including Amendment Nos. 1, 2, 3 & 4)]
[0081] Soap noodle was obtained following the procedure detailed in Example 1.
The soap noodle underwent color analysis (pre- and post SAST) in Lovibond
tintometer, and was analyzed for FCA content. The results obtained are depicted in
Table 2.
[0082] Table 2: parameters of soap noodle



[0083] Referring to Table 2, it can be appreciated that the color of all prototype soap noodle is within the acceptable range of 1.3 units in Lovibond tintometer. Also, as per the SAST odor was found to be acceptable. The analyzed FCA content post SAST of all the prototypes of soap noodles was found within the acceptable limit of 0.05%. The low acceptable FCA content signifies the mildness of soap noodle and is a testimony of complete neutralization achieved by the disclosed process. The process of the present invention describes use of lauric acid flakes for manufacturing soap noodles, it is a fact that flakes have increased surface area and it renders them particularly susceptible to charring in case of minor temperature fluctuations. The present invention has arrived at a process with due experimentation, that is specifically adapted to avoid any charring or pocketing of solid fatty acid components which results in undesirable brown spot formation.

[0084] The Figure 1 depicts soap noodle obtained through the process of the present disclosure, it can be appreciated that the soap noodles are devoid of any brown spots and is acceptable in terms of other sensorial parameters. The Figure 2 depicts soap noodle obtained by conventional process, brown spots can be observed in the soap noodle which is not a desirable feature. Thus, the process of present disclosure provides an efficient solution for obtaining soap noodle with improved color and devoid of any brown spots caused by charring of fatty acids. The process as disclosed in the present disclosure has been compared with conventional processes (non-working examples) in practice for neutralizing fatty acid.
[0085] Thus, preparation of soap noodles by the process as disclosed in the present disclosure leads to manufacturing of soap noodle having the desirable characteristics of color (absence of brown spots), odor, and low FCA content. The process ensures homogenous and complete neutralization of fatty acids used in the preparation of soap. Example 3
Non-working examples
[0086] The non-working examples depicted follow a different sequence of preparation of soap noodles than as disclosed in the Example 1. The non-working examples are conventional processes employed for neutralizing fatty acids. Non-working example - Set A
[0087] The present soap noodle prototype was prepared by adding brine after the commencement of fatty acid neutralization. Rest of the process remains same as depicted in Example 1. The obtained soap noodle underwent SAST followed by color analysis, odor analysis, and percentage FCA analysis. Table 3 depicts the parameters of soap noodle obtained by the process. Table 3: Parameters of Set A


[0088] Referring to Table 3, it can be appreciated that the color of soap noodle obtained by the present process is although acceptable for prototype 183 but on a higher side as compared to that of the working examples depicted in Table 2. The prototype 182 was unacceptable in terms of color post SAST. Also, brown spots are observed post SAST. Odor of soap noodle for both the prototypes was also found to be unacceptable. The prototypes 182 and 183 are also unacceptable in terms of the FCA content which is below the working range. Non-working example - Set B
[0089] The present non-working example includes analysis of soap noodles prepared by a process in which lauric acid flakes are pre-melted with distilled fatty acid instead of adding separately in form of flakes. Rest of the process for preparing soap noodles is the same as described in Example 1. The obtained soap noodle underwent SAST followed by color analysis, odor analysis, and percentage FCA analysis. Table 4 depicts the parameters of soap noodle obtained by the process. [0090] Table 4:

[0091] Table 4 summarizes the parameters analyzed for the soap noodle obtained by the present process. According to Table 4, the color of the soap noodle for both

the prototypes is not within the acceptable range of 1.3 units. Prototype 184 displays the color unit of 1.7 (post SAST), and prototype 185 displays the color unit of 1.8 (post SAST). On performing dry sniff test post SAST, it is found that the odor is acceptable for both the prototypes and also no brown spots are observed in the present case. The FCA contents of the prototypes are also below the acceptable range. Non-working examples - Set C
[0092] The present set of non-working examples depict the parameters of soap noodle obtained by a process in which lauric acid flakes are added to the crutcher followed by the addition of distilled fatty acids and brine solution. Table 5 depicts the parameters of soap noodle obtained by following the present process. [0093] Table 5:

[0094] Inconsistencies with reference to the percentage of FCA can be observed from Table 5. The acceptable range of FCA content is 0.02%-0.08% with respect to

the soap noodle composition. Except for prototype 115, the FCA content of all other prototypes are below the minimum percentage of 0.02%, and the color is also unacceptable in all of the prototypes. The higher values for color are attributed to a higher extent of charring and pocket formation of the Laurie acid flakes. A very low level of FCA may not be desirable since color is not acceptable in such cases. [0095] Thus, in case of non-working examples - Set A, the prototypes are considered unacceptable based on their odor, and appearance of brown spots. In case of non-working examples - Set B, the prototypes are considered undesirable because of the color of soap noodle. In case of Set C, the prototypes are undesirable because of the higher values of color units and lower FCA values which are not within the desired range and also inconsistencies can be observed with respect to color of soap noodle. Therefore, the non-working prototypes assert the importance of the steps disclosed in the present disclosure for fatty acid neutralization for obtaining soap noodle with desired parameters. Advantages of the present disclosure:
[0096] The present disclosure discloses a process for neutralizing fatty acids to obtain soap noodle having improved color, odor, and low FCA content as compared to that obtained by conventional process. The present process forms soap noodle having low FCA content thus being less abrasive and at the same time retains all other sensorial parameters of improved color and odor. Also, the conventional process comes with a risk of reactor choking and pocket formation during neutralization but the present process overcomes the mentioned drawbacks and ensures homogenous neutralization of the fatty acid content. Following the process and regulating the temperature of the reactor during mixing ensures efficient mixing of caustic during fatty acid neutralization and avoids the formation of brown spots in the obtained soap noodle thereby improving the color of the soap noodle.

I/We Claim:
1. A process of neutralizing fatty acid content to obtain soap noodle, said
method comprising:
a) adding a first brine solution to a reactor;
b) contacting a first part of distilled fatty acid with the first brine solution to obtain a first mixture;
c) contacting a first part of caustic solution with the first mixture to obtain a second mixture;
d) contacting at least one fatty acid selected from the group consisting of C12 fatty acid, mixture of C12-C14 fatty acid, palm kernel based fatty acid, coconut fatty acid, and combinations thereof, with the second mixture to obtain a third mixture;
e) contacting a second part of distilled fatty acid and a second part of caustic solution with the third mixture to obtain a fourth mixture;
f) contacting at least one additive and a second brine solution with the fourth mixture to obtain a fifth mixture; and
g) processing the fifth mixture,
wherein the first brine solution occupies 2% to 15% volume of the reactor, and wherein the process leads to neutralisation of fatty acid content to obtain soap noodle having color units in the range of 0.6 to 1.3.
2. The process as claimed in claim 1, wherein the first brine solution has a concentration of sodium chloride (NaCl) in the range of 0.5%-0.6% w/v.
3. The process as claimed in claim 1, wherein the first part of distilled fatty acid has a weight percentage in the range of 5%-25% with respect to distilled fatty acid content of the soap noodle.
4. The process as claimed in claim 1, wherein the distilled fatty acid is in liquid state and the at least one fatty acid is in solid state in form of flakes.
5. The process as claimed in claims 1 and 4, wherein the at least one fatty acid is lauric acid in form of flakes.

6. The process as claimed in claim 1, wherein the distilled fatty acid is selected from the group consisting of C16-C20 fatty acid, and combinations thereof.
7. The process as claimed in claim 6, wherein the distilled fatty acid is selected from the group consisting of C16-C18 fatty acid, and combinations thereof.
8. The process as claimed in claims 6 and 7, wherein the distilled fatty acid comprises mono-unsaturated and poly-unsaturated fatty acid.
9. The process as claimed in claim 1, wherein the fatty acid content of the soap noodle comprises a combination of distilled fatty acid and the at least one fatty acid in a w/w ratio in the range of 9:1 to 3:2.
10. The process as claimed in claim 1, wherein caustic solution has a concentration in the range of 25% to 47% w/v.
11. The process as claimed in claim 1, wherein at least one fatty acid has a weight percentage in the range of 5%-40% with respect to fatty acid content of the soap noodle.
12. The process as claimed in claim 1, wherein the first part of distilled fatty acid occupies 5%-25% volume of the reactor.
13. The process as claimed in claim 1, wherein the at least one additive is selected from the group consisting of EDTA (ethylenediaminetetraacetic acid) having a weight percentage in the range of 0.04%-0.07% with respect to soap noodle, EHDP (ethane 1-hydroxy-1, 1-diphosphonate) having a weight percentage in the range of 0.12%-0.23% with respect to soap noodle.
14. The process as claimed in claim 1, wherein the second brine solution has a concentration of sodium chloride (NaCl) in the range of 0.15%-0.2% w/v.
15. The process as claimed in claim 1, wherein adding the first brine solution is carried out at a temperature in the range of 60°C-65°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm.
16. The process as claimed in claim 1, wherein contacting a first part of distilled fatty acid with the first brine solution is carried out at a temperature

in the range of 70°C-80°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm.
17. The process as claimed in claim 1, wherein contacting the at least one fatty acid with the second mixture is carried out at a temperature in the range of 65°C-75°C for a time period in the range of 15-30 minutes under continuous agitation at 80-120 rpm.
18. The process as claimed in claim 1, wherein contacting the second part of distilled fatty acid and a second part of caustic solution with the third mixture is carried out for a time period in the range of 10-20 minutes under continuous agitation at 80-120 rpm.
19. The process as claimed in claim 1, wherein contacting the at least one additive and the second brine solution with the fourth mixture is carried out for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm.
20. The process as claimed in claim 1, wherein the soap noodle has free caustic alkali concentration in the range of 0.02-0.08% with respect to the soap noodle.
21. The process as claimed in claim 1, wherein the process leads to homogenous mixing during neutralisation of the fatty acid content to obtain the soap noodle.
22. The process as claimed in claim 1, wherein contacting at least one fatty acid with the second mixture leads to decomposition of the at least one fatty acid in the range of 0.01%-0.1% with respect to the at least one fatty acid.
23. A process of neutralizing fatty acid content to obtain soap noodle, said method comprising:
a) adding a first brine solution having a concentration of sodium chloride in the range of 0.5%-0.6% w/v to a reactor at a temperature in the range of 60°C-65°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm, wherein the first brine solution occupies 2%-15% of volume of the reactor;

b) contacting a first part of distilled fatty acid having a weight percentage in the range of 5%-25% with respect to total distilled fatty acid with the first brine solution at a temperature in the range of 70°C-80°C for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm to obtain a first mixture;
c) contacting a first part of caustic solution having a concentration of sodium hydroxide (NaOH) in the range of 25% w/v to 47% w/v with the first mixture to obtain a second mixture,
d) contacting at least one fatty acid selected from the group consisting of C12 fatty acid, mixture of C12-C14 fatty acid, palm kernel based fatty acid, coconut fatty acid, and combinations thereof having a weight percentage in the range of 5%-40% with respect to fatty acid content of the soap noodle with the second mixture at a temperature in the range of 75°C-80°C for a time period in the range of 15-30 minutes under continuous agitation at 80-120 rpm to obtain a third mixture, wherein the at least one fatty acid occupies 5%-10% volume of the reactor;
e) contacting a second part of distilled fatty acid having a weight
percentage in the range of 75%-95% with respect to total distilled
fatty acid and a second part of caustic solution with the third
mixture for a time period in the range of 10-20 minutes under
continuous agitation at 80-120 rpm to obtain a fourth mixture,
f) contacting at least one additive having a weight percentage in the range of 0.04%-0.23% with respect to total soap composition selected from the group consisting of EDTA, EHDP, and combinations thereof, and a second brine solution having a concentration of sodium chloride (NaCl) in the range of 0.15%-0.2%) w/v to the fourth mixture for a time period in the range of 5-10 minutes under continuous agitation at 80-120 rpm to obtain a fifth mixture; and
g) processing the fifth mixture,

wherein the distilled fatty acid is selected from the group consisting of C16-C20 fatty acid, and combinations thereof, and wherein the process leads to neutralisation of fatty acid content to obtain soap noodle having color units in the range of 0.6 to 1.3.
24. The process as claimed in any of the claims 1 and 23, wherein the process optionally includes contacting the fifth mixture with at least one benefit agent selected from the group consisting of humectants, surfactants, electrolytes, and combinations thereof.
25. The process as claimed in claim 24, wherein the humectants is selected from the group consisting of glycerine, sorbitol, propylene glycol, and combinations thereof, and the humectants is present in a weight percentage in the range of 1 to 10% w/w with respect to the soap noodle, the surfactants is selected from the group consisting of alfa olefin sulphonates, sodium lauryl ether sulphate, cocoamido propyl betaine, decyl glucoside, and combinations thereof, and the surfactant is present in a weight percentage in the range of 1 to 7% w/w with respect to the soap noodles, and the electrolytes is selected from the group consisting of chloride, sulphate, meta bi sulphate, citrate salts of sodium or potassium, and the electrolytes is present in a weight percentage in the range of 0.2 to 0.6% w/w with respect to the soap noodles.
26. The process as claimed in any of the claims 1 and 23, wherein contacting a first part of caustic solution with the first mixture is carried out in a gradual manner through distributor rings.

Documents

Application Documents

# Name Date
1 201741047354-STATEMENT OF UNDERTAKING (FORM 3) [29-12-2017(online)].pdf 2017-12-29
2 201741047354-FORM 1 [29-12-2017(online)].pdf 2017-12-29
3 201741047354-DRAWINGS [29-12-2017(online)].pdf 2017-12-29
4 201741047354-DECLARATION OF INVENTORSHIP (FORM 5) [29-12-2017(online)].pdf 2017-12-29
5 201741047354-COMPLETE SPECIFICATION [29-12-2017(online)].pdf 2017-12-29
6 abstract_201741047354.jpg 2018-01-02
7 201741047354-Proof of Right (MANDATORY) [01-03-2018(online)].pdf 2018-03-01
8 201741047354-FORM-26 [01-03-2018(online)].pdf 2018-03-01
9 Correspondence by Agent_Form26-Proof of Right_06-03-2018.pdf 2018-03-06