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Nanomaterial Based Cosmetic Products

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Patent Information

Application #
Filing Date
07 March 2012
Publication Number
35/2016
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
Parent Application
Patent Number
Legal Status
Grant Date
2018-04-02
Renewal Date

Applicants

ITC LIMITED
37  J.L.Nehru Road  Kolkata – 700 071  State of West Bengal  India.

Inventors

1. PANIGRAHI Sudipa
ITC Limited  ITC R&D Centre  No.3  1st Main Road  Peenya Industrial Area  Phase I  Bengaluru -560 058  India
2. RAMAMURTHI Suresh
ITC Limited  ITC R&D Centre  No.3  1st Main Road  Peenya Industrial Area  Phase I  Bengaluru -560 058  India
3. KRISHNAN Venkat
ITC Limited  ITC R&D Centre  No.3  1st Main Road  Peenya Industrial Area  Phase I  Bengaluru -560 058  India
4. SRIMATHI P
ITC Limited  ITC R&D Centre  No.3  1st Main Road  Peenya Industrial Area  Phase I  Bengaluru -560 058  India
5. JAYAPRAKASH Doss
ITC Limited  ITC R&D Centre  No.3  1st Main Road  Peenya Industrial Area  Phase I  Bengaluru -560 058  India

Specification

F O R M 2
THE PATENTS ACT, 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10; rule 13)
1. Title of the invention –
NANOMATERIAL BASED COSMETIC PRODUCTS
2. Applicant(s)
(a) NAME: ITC LIMITED
(b) NATIONALITY : An Indian Company
(c) ADDRESS : 37, J.L.Nehru Road,
Kolkata – 700 071,
State of West Bengal,
India.
3. PREAMBLE TO THE DESCRIPTION
The following specification particularly describes the invention and the manner in
which it is to be performed:
2
Field of the invention
The present invention relates to a composition for coloring human hair fibres.
More particularly, the present invention relates to a composition comprising
nanoparticles with a hydrophobic group at the surface with improved binding
ability to the hair.
Background and prior art
Currently used hair dyes are of two types- direct dyes impart a colour to the hair
that is the combination of natural hair colour plus the colour added by the dye and
oxidative dyes that require the hair that is to be dyed to be a shade lighter than
what it is. The dyeing procedure first eliminates the natural shade of the hair
through bleaching with an oxidizing agent such as alkaline hydrogen peroxide.
Then the desired shade is obtained on the hair by contacting it with the oxidation
dye. It is also possible to simultaneously bleach and colour the hair. In this case
the dyestuff penetrates through the damaged hair follicles to impart colour to the
hair. This eventually releases substances from the reaction with the dye with the
peroxide, which causes allergies to the scalp.
Further conventional hair dyeing products not only require longer time in
colouring but also, leave some acceptable marks on the scalp or skin. These dyes
come out easily through washing and go to the waste water system which, create
environmental pollution. Moreover, pre-treatment of hair can make permanent
damage by removing its natural gloss.
US 7186274 (D1) teaches the use of organomodified metallic nanoparticles
preferably bearing at their surface a self-assembled monolayer of organosulphur
compounds. The inventors of D1 have found that it is possible to increase the
remanence of metallic nanoparticles at the surface of the hair and thus to maintain
their cosmetic effect even after shampooing several times by using not “naked”
metallic nanoparticles. According to D1 the diversity of organic groups that may
be attached to the surface of the metallic nanoparticles makes it possible to
provide several routes for immobilizing the particles at the surface of human
3
keratin fibers. This diversity allows great freedom in modifying the various
surface parameters, such as electric charge or the hydrophobic nature, and thus in
modifying the forces of interaction with the cosmetic substrate and of increasing
in particular the remanence of the deposit of metallic particles.
US 7276088 (D2) teaches hair colouring and cosmetic compositions comprising
chemically functionalized or physically modified carbon nanotubes as a black
pigment. The carbon nanotubes of D2 may be physically modified with a
modifying agent such as a polymer, which has affinity for hair. According to D2,
the term “physically modified carbon nanotubes” refers to carbon nanotubes that
have been dispersed by physical means or have been coated with or are associated
with a modifying agent. The term modifying agent refers to reagents used to coat
carbon nanotubes nanotubes to disperse them in aqueous solution. Modifying
agents include nanoparticles including metallic, semiconductor or polymer
particles. Further D2 teaches that the physical modification of the nanotubes
accomplishes two purposes. First, the modifying agent forms a place of
attachment for ligands or for a hair substrate. Secondly, the modifying agent often
disperses the nanotubes allowing for facile handling.
However, the compositions as taught in D1 and D2 require longer time for
colouration when compared to the present invention. The present invention uses
metallic nanoparticles such as gold, silver, copper, platinum, palladium etc as hair
colourants. The present invention also relates to a method to prepare the metallic
nanoparticles of various shapes and sizes including but not limited to spherical,
rod etc and using cosmetically acceptable non-toxic reagents. Incorporation of the
nanomaterial into a cosmetic product formulation especially hair care products
remain challenging because of the aggregation of the nanomaterial in the
formulation. The nanomaterial due to its small size is prone to aggregation if there
is any change in the chemical/physical environment surrounding it. Hydrophilic
surface on the nanomaterial cannot provide maximum stability and are much more
susceptible to such changes compared to their hydrophobic analogue.
In order to overcome the above drawbacks, according to the present invention the
surface chemistry of the nanomaterial are modified with long hydrophobic group,
4
which binds to the hair effectively unlike the hydrophilic surface. Further the
present invention preludes any pre and/or post treatment required to impart the
desired colour to hair. Moreover, present formulation containing the nanomaterial
imparts the desired colour to a maximum extent in a short interval with very low
concentration. Unlike the conventional hair dyes, the nanomaterial based
colourants of the present invention can impart effective antimicrobial activity
along with enhanced gloss, conditioning and smoothness to the hair. The present
formulation does not leave any mark to the scalp or skin and is easily washable
through soap or shampoo.
Object of the invention
The object of the present invention is to overcome the drawbacks of the prior art.
It is another object of the present invention to provide a composition comprising
nanomaterial as hair colourants.
It is yet another object of the present invention to provide hydrophobically
modified nanoparticles in microgram concentration to impart the desired colour to
hair, without any pre and/or post treatment in a short interval.
Summary of the invention
The present invention relates to a cosmetic composition comprising:
at least one cosmetically active component; and
a metallic nanoparticle composite material comprising a metal and at least
one of semiconductors, polymers, fatty acids, fatty alcohols, long chain
amides and esters;
wherein said metallic nanoparticles are hydrophobically modified.
5
Brief description of the accompanying figures:
Figure 1 represents cotton fibres treated with (a) hydrophobically modified gold
nanorods; (b) hydrophillically modified gold nanorods treated for same time
interval
Figure 2 represents white hair fivers treated with (a) hydrophobically modified
silver nanoparticles, (b) hydrophilically modified silver nanoparticles treated for
same time interval
Figure 3 represents white hair fibers treated with hydrophobically modified silver
nanoparticles dispersed in different surfactants and silicones for same time
interval
Figure 4 represents SEM images of (a) untreated and (b) treated (with
nanoparticle) hair fibers. The inset shows the high resolution micrograph of the
same
Figure 5 represents SEM image of the hair fiber treated with nanoparticles with
(a) hydrophobically modified gold nanoparticles and and (b) with hydrophilically
modified gold nanoparticles
Detailed description of the invention
The present invention relates to hair colourant compositions comprising metallic
nanoparticles, such as gold, silver, copper, platinum, palladium etc., as hair
colourants. It also provides compositions comprising metallic oxides and
chalcogenides as a colouring agent for human hair fiber.
According to the present invention the surface chemistry of the nanomaterial is
modified with long hydrophobic groups, which binds to the hair effectively unlike
the hydrophilic surface. It is surprisingly found that nanoparticles with a
6
hydrophobic group at the surface binds to hair better compared to their
hydrophilic analogue. The synthesized hydrophobic nanoparticles are soluble in
oil and give colour to the hair when treated for even a short period of time. It was
further found that the hydrophobic nanoparticles impart conditioning and
smoothness to the hair. The scattering properties of the metals enhance the gloss
of the hair.
The present invention demonstrates that the importance of the surface chemistry
of the nanoparticles to determine its adsorption to the hair surface. Specifically
hydrophobicity of the nanoparticle surface facilitates the adsorption to the hair
unlike the hydrophilic surface. Further the hydrophobic surface imparts more
stability to the nanoparticles and in turn prevents them from aggregation. The
nanomaterials are incorporated in microgram concentration in hair oil, silicone oil
shampoo, conditioner, serum to impart colours. White/grey hair when treated with
the nanomaterials of the present invention imparts the desired colour, gloss,
conditioning and antimicrobial properties in a very short interval. The
hydrophobically modified nanoparticles impart a better colour when dispersed in
cationic surfactants compared to their anionic and non-ionic counterpart. The
present invention further provides a higher extent of colouration when disperse in
hydrophobically modified compared to their hydrophilic counterpart.
The present formulation containing hydrophobically modified nanoparticles in
microgram concentration imparts the desired colour to hair, without any pre
and/or post treatment in a short interval. Yet another object of the present
invention is that the formulation does not contain any toxic dyes/hair colourants
such as ammonia, hydrogen peroxide or the like. Furthermore, the present
invention shows that the formulation containing hydrophobic metallic
nanoparticles enhances the smoothness, conditioning and hydrophobicity of the
hair. It also imparts antimicrobial properties unlike the conventional hair dyes.
Further according to the present invention, the hydrophobically modified
nanoparticles impart better colour through hydrophobic silicones and cationic
surfactant compared to hydrophilic silicones and anionic or non-ionic surfactants.
7
According to the present invention the amount of nanoparticles deposited on hair
increases with increase in time of treatment
The present invention discloses that the time required to achieve a particular
intensity of colour that is much less than that of prior arts. It is to be noted the
time required to achieve a particular intensity of colour is less when the particles
are hydrophobically modified compared to their hydrophilic counterpart. Figure 1
demonstrates cotton fibres treated with hydrophobically and hydrophilically
modified gold nanorods. Figure 2 demonstrates cotton fibres treated with
hydrophobically and hydrophilically modified silver nanoparticles.
It was observed that the cationic surfactants provides a better colour to the hair
fibre compared to non-ionic or anionic surfactants with a same concentration of
hydrophobically modified metal nanoparticles. The following table shows the
details result while 2% hydrophobically modified silver nanoparticles were
dispersed in different surfactant system and silicones.
Table 1: Extent of colouration through hydrophobically modified silver
nanoparticles dispersed in different surfactants and silicones
The normal hair colours are organic dye which degrades in presence of light.
While the present invention discloses the use of hydrophobically modified metal
nanoparticles which does not degrade in presence of light and hence can impart
the colour for a longer time. Also the common hair dyes are hydrophilic in nature
and hence goes out while washing giving a lighter shade of colour. While the
present invention discloses the use of hydrophobically modified nanoparticles and
hence would not go easily while washing with water.
8
It may be noted that when the hair samples were treated with hydrophobically
modified silicone, the hair get damaged after a few treatments. Further the
hydrophobic components come out of the hair surface after washing off with any
rinse off product like shampoo. However, according to the present invention, it is
surprisingly found that hydrophobically modified nanoparticle surface does not
comes out easily even after several wash with shampoo.
System Concentration
of Silver
Nanoparticles
Time of
Treatment
(minutes)
Extent of
Colouration
Anionic Surfactant
(SLES)
2% 15 No
colouration
Non-Ionic Surfactant (Tween-
80)
2% 15 Very light
colouration
Cationic Surfactant
Cetyl Pyridinium Chloride
(CPC)
2% 15 Light
colouration
Cationic Surfactant
Cetyltrimethylammonium
Chloride-30 (CTC-30)
2% 15 Medium
colouration
Cationic Surfactant
Cetyltrimethylammonium
Bromide (CTAB)
2% 15 Light
colouration
Polyethylene Glycol – 400 2% 15 No
colouration
Silicone
Decamethylcyclopentasiloxane
(DC-245)
2% 15 Dark
colouration
9
Further as the hair surface is negatively charged it was expected that positively
charged hydrophilic surface (charged surface) will demonstrate better adsorbtion
and provide a better colour to the hair. However, it is surprisingly found that
hydrophobically modified nanoparticle surface (having no charge) adsorbs more
to the hair surface compared to hydrophilically modified nanoparticle surface.
Table 2: Percentage of nanoparticles present on hair fiber treated for different time
interval as quantified by EDX analysis
Sample Time of
treatment
Percentage of
nanoparticles
Percentage of
sulfur
Untreated hair 0 minute 0% 100%
Treated hair -1 30 minutes 37.02 62.98
Treated hair -2 60 minutes 55.91 44.09
Treated hair -3 120 minutes 66.84 37.47
It can be seen from Table 2 that with the increase in time of treatment, the
amount of nanoparticles deposited on hair increases. Presence of
nanoparticles on hair fibers was confirmed by SEM analysis.
Synthesis of hydrophobic silver nanoparticles using long chain fatty
acids/alcohols/amines
A mixture of silver salt (silver nitrate, silver acetate, silver sulfate, silver
acetylacetonate etc.) and long chain fatty acids/amines/alcohols were taken in a
round bottomed flask in 1:3.4 molar ratio and were heated to 120°C under
nitrogen atmosphere for 30 minutes under continuous stirring. Then the
temperature was increased to 150°C and the reducing agent (e.g., primary amine
and or secondary amines and or tertiary amines or a mixture of these) was added
10
to it under continuous stirring. The heating was continued for 2 hours and the
mixture was allowed to cool to 50°C and a mixture of toluene and methanol were
added to it. Finally the whole mixture was allowed to cool to room temperature.
The mixture was then centrifuged and the supernatant was discarded. The black
coloured precipitate were re-dispersed in methanol and centrifuged again. The redispersion
and centrifugation cycle was followed for 7-8 times. Finally the
product was put in the oven at 60°C for 7-8 hours to completely dry and to get the
hydrophobic silver nanoparticles in powder form. The black powder is then stored
under dark and used for product formation.
Synthesis of hydrophobic silver nanoparticles using cocoamide MEA
A mixture of silver salt and cocoamide MEA in water was taken in a round
bottom flask and was heated to 70°C under nitrogen atmosphere under continuous
stirring for 30 minutes. Then the reducing agent (primary amine and/or secondary
amine and/or tertiary amine or a mixture of these, sodium borohydride, reducing
sugars) is added to it under continuous stirring. The reaction was continued for 30
minutes and then allowed to cool to room temperature and then non-polar solvents
(toluene, hexane, heptanes, butane etc.) or oil was added to it. The mixture was
left undisturbed for a couple of hours to facilitate the phase separation. Once the
phases are separated, the non-aqueous phase containing the hydrophobic
nanoparticles were separated from the aqueous phase using a separating funnel.
Finally methanol was added to the non-aqueous phase to precipitate the
nanoparticles. The mixture was then centrifuged and the precipitate was and the
precipitate was collected and re-dispersed in methanol and further centrifuged.
The centrifugation and re-dispersion cycle was repeated several times to ensure
that the product is free from any unreacted chemicals or impurities. Finally the
product was put in the oven at 60°C for 7-8 hours to completely dry and to get the
hydrophobic silver nanoparticles in powder form. The black powder was stored
under dark and used for product formulation.
The present invention is further described by way of suitable working examples.
11
Example 1
Synthesis of silver nanoparticles using stearic acid as the stabilizer
A mixture of 1.68 gm of silver acetate and 5.68 gm of stearic acid were taken in a
round bottomed flask and were heated to 120°C under nitrogen atmosphere for 30
minutes under continuous stirring. Then the temperature was increased to 150°C
under continuous stirring 10gm of triethylamine was added to it using a syringe.
The heating was continued for 2 hours. Finally the mixture was allowed to cool to
50°C and a mixture of 10 mL of toluene and 50 mL of methanol was added to it.
Finally the whole mixture was allowed to cool to room temperature (25°C). The
mixture was then centrifuged at 6000 rpm for 10 minutes and the supernatant was
discarded. The black coloured precipitate were re-dispersed in methanol and
centrifuged again. The re-dispersion and centrifugation cycle was followed for 7-8
times and finally the product was put in the oven at 60°C for 7-8 hours to
completely dry and get the hydrophobic silver nanoparticles in powder form. The
synthesized silver nanoparticles were hydrophobic in nature and are dispersible in
any non-polar solvent or oil. The silver nanoparticles when dispersed in toluene
show a bright yellow colour due to the surface plasmon band of silver
nanoparticles. The product was characterized by UV-vis spectroscopy which
shows at λmax at 413 nm at a concentration of 0.01mg/mL. The black powder was
stored under dark and used for the product formulation.
Example 2
Synthesis of silver nanoparticles using cocamide MEA as stabilizer
A mixture of 0.169 gm of silver nitrate and 1.4 gm of cocamide MEA were taken
in a round bottomed flask and were heated to 70°C under nitrogen atmosphere for
10 minutes under continuous stirring. Then 5 gm of triethylamine was added to it
using a syringe. The mixture turned yellow after 5 minutes indicating the onset of
evolution of silver nanoparticles. The reaction was continued for 30 minutes and
12
then allowed to cool to room temperature (25°C) and then 20 mL of toluene was
added to it. The mixture was left undisturbed for four hours to facilitate the phase
separation. Once the phases are separated, the non-aqueous phase containing the
hydrophobic nanoparticles were separated from the aqueous phase using a
separating funnel. Finally 20 mL of methanol was added to the toluene phase to
precipitate the nanoparticles. The mixture was then centrifuged at 6000 rpm for 20
minutes and the supernatant was discarded. The black coloured precipitate were
re-dispersed in methanol and centrifuged again. The re-dispersion and
centrifugation cycle was followed for 7-8 times and finally the product was put in
the oven at 60°C for 7-8 hours to completely dry and get the hydrophobic silver
nanoparticles in powder form. The synthesized silver nanoparticles were
hydrophobic in nature and are dispersible in any non-polar solvent or oil. The
silver nanoparticles when dispersed in tolune show a bright yellow colour due to
the surface plasmon band of silver nanoparticles. The product was characterized
by UV-vis spectroscopy which shows at λmax at 425 nm at a concentration of
0.01mg/mL. The black powder was stored under dark and used for the product
formulation.
Example 3
Shampoo composition containing 2% hydrophobic silver nanoparticles
Shampoo formulation was prepared containing 2.0% of hydrophobically modified
silver nanoparticles. A bunch of 5 gm of white/gray hair were treated with 0.5 gm
of shampoo for 2 minutes and washed off with water and dried. The colour
intensity was measured by measuring the L*a*b* value of the hair bunches both
before and after treatment and the ΔE values were calculated to measure the
extent of colouration (Table 4). The formulation details are given below Table 3.
Table 3: Formulation details of the shampoo containing 2% hydrophobically
modified silver nanoparticles as an example
13
It is to be noted that one objective of the present invention is to provide colour
through a cleansing product e.g. shampoo. The colour intensity was measured by
measuring the L*a*b* value of the hair bunches.
Table 4 provides the change in colour of white hair fibres after different time of
washing.
Table 4: Change in the ΔE (change in colour of white hair fibres after
different time of washing) value with number of washes by shampoo
containing 2% hydrophobically modified silver nanoparticles
Ingredient Weight in % Amount, gm
SLES(2EO) 40.500 40.500
Galaxy 780 10.410 10.410
Lamesoft Po65 2.000 2.000
Hydrophobic Silver Nanoparticles 2.000 2.000
Catinal HC-100 0.200 0.200
DI water 5.000 5.000
Sc-60 0.100 0.100
Di water 5.000 5.000
ITC-27 2.000 2.000
H-81 0.200 0.200
Zn PCA 0.020 0.020
Hydrovance 1.500 1.500
CAPB 5.000 5.000
Aqua SF-1 5.000 5.000
DI water 5.000 5.000
DI Water 16.0700 16.070
Total formula 100.0000 100.0000
14
SI No No of washes with
shampoo
ΔE
1 1st wash 65.86
2 2nd wash 54.86
3 3rd wash 53.91
4 4th wash 50.93
5 5th wash 50.87
6 6th wash 49.19
7 7th wash 48.76
From the above Table 4 it is clear that with increased number of washes the
colour intensity increases which is reflected by the decrease in ΔE value.
Degree of conditioning can be determined by measuring the advancing and
receding angles on the treated hair in comparison to the untreated hair sample.
Table 5 and 6 show that hair treated with a silicone oil with hydrophobic silver
nanoparticles show a higher advancing and receding value as compared with
untreated hair and hair treated with silicone oil minus the nanoparticles.
Table 5: 1st advancing angle of all the hair samples
No of washes
Washed with the
shampoo without the
hydrophobically modified
silver nanoparticles
Washed with shampoo
containing 2%
hydrophobically modified
silver nanoparticles
1st wash 93.07 99.34
2nd wash 90.66 100.46
3rd wash 88.60 97.32
4th wash 87.48 98.19
5th wash 85.63 98.51
6th wash 84.45 97.80
15
7th wash 81.32 95.80
Table 6: 1st receding angle of contact for all the hair samples
No of washes
Washed with the shampoo
without the
hydrophobically modified
silver nanoparticles
Washed with shampoo
containing 2%
hydrophobically modified
silver nanoparticles
1st wash 61.20 69.94
2nd wash 58.32 70.01
3rd wash 54.37 73.57
4th wash 50.77 74.10
5th wash 48.18 73.82
6th wash 45.89 71.23
7th wash 44.61 69.25
Example 4
Conditioner composition containing 2.0% hydrophobic silver nanoparticles
Conditioner formulation was prepared containing 2.0% of hydrophobically
modified silver nanoparticles. A bunch of 5 gm of white/gray hair was treated
with 0.5 gm of shampoo for 2 minutes and rinse off with water. Finally, 0.5 gm of
conditioner was applied to the wet hair for 3 minutes and washed off with water
and dried. The formulation details are given below Table 7.
Table 7: Formulation details of the conditioner containing 2%
hydrophobically modified silver nanoparticles as an example:
16
The colour intensity was measured by measuring the L*a*b* value of the hair
bunches both before and after treatment and the ΔE values were calculated to
measure the extent of colouration. The change in ΔE values are given in Table 8.
Table 8: Change in the ΔE (change in colour of white hair fibres after
different treatment with hair conditioner) value with number of treatment by
hair conditioner containing 2% hydrophobically modified silver
nanoparticles
Ingredients Amount, % Amount, gm
Structure XL 1.600 3.2
Softcat SKM 0.100 0.20
Distilled water 72.790 143.38
EDTA 2Na 0.100 0.20
Distilled water 2.00 4.00
Cetostearyl alcohol 4.00 8.00
GMS(NSE) 1.00 2.00
CM 1000 1.500 3.00
Behenyl TMS 0.500 1.00
Hydrophobic Silver Nanoparticles 2.000 4.00
CTC 30 3.300 6.60
Crodamol STS 1.000 2.00
KCG 0.090 0.18
D-Panthenol 0.300 0.60
Distilled water 10.820 21.64
Total formula 100.00 200.00
17
SI No No of treatment with
hair conditioner
ΔE
1 1st treatment 26.64
2 2nd treatment 24.75
3 3rd treatment 23.13
4 4th treatment 19.36
5 5th treatment 15.40
Example 5
Serum composition containing 2% hydrophobic silver nanoparticles
Serum formulation was prepared containing 2.0% of hydrophobically modified
silver nanoparticles. A bunch of 5 gm of white/gray hair were treated with 1 gm of
serum for overnight and washed off with water and dried. The formulation details
are given below Table 9.
Table 9: Formulation details of the hair serum containing 2%
hydrophobically modified silver nanoparticles as an example.
Ingredient Amount,% Amount, gm
DC1411 30.00 30.00
C12-C15 Alkyl
Benzoate 3.00
3.00
DC-245 65.00 65.00
Hydrophobic Silver
nanoparticles
2.00 2.00
Total formula 100.00 100.00
The colour intensity was measured by measuring the L*a*b* value of the hair
bunches both before and after treatment and the ΔE values were calculated to
18
measure the extent of colouration. The change in ΔE values during treatment is
given in Table 10.
Table 10: Change in the ΔE (change in colour of white hair fibres after
different treatment with hair serum) value with number of treatment by hair
serum containing 2% hydrophobically modified silver nanoparticles
SI No No of treatment with
hair serum
ΔE
1 1st treatment 21.07
2 2nd treatment 16.09
3 3rd treatment 13.40
4 4th treatment 8.62
5 5th treatment 5.32
Example 6
Hair oil composition containing 2% hydrophobic silver nanoparticles
1 gm of hydrophobic silver nanoparticles were dispersed in 50 mL of olive oil and
the mixture was sonicated for 30 minutes to disperse the nanoparticles in olive oil.
Then 5 gm of white/gray hairs was treated with 0.5 gm of olive oil containing
hydrophobic silver nanoparticles. The hair bunch was left overnight and washed
off with 0.5 gm of shampoo and dried. The colour intensity was measured by
measuring the L*a*b* value of the hair bunches both before and after treatment
and the ΔE values were calculated to measure the extent of colouration. The
change in ΔE is given in Table 11.
Table 11: Change in the ΔE (change in colour of white hair fibres after
different treatment with hair oil) value with number of treatment by hair oil
containing 2% hydrophobically modified silver nanoparticles
19
SI No No of treatment with
hair oil
ΔE
1 1st treatment 28.23
2 2nd treatment 22.23
3 3rd treatment 18.25
4 4th treatment 14.81
5 5th treatment 11.13
Example 7
Deposition of hydrophobic silver nanoparticles on hair through silicone oil
1 gm of hydrophobic silver nanoparticles were dispersed in 50 mL of silicone oil
through ultra sonication for 5 minutes. Then 5 gm of white/gray hairs was treated
with 0.5 gm of solicone oil containing hydrophobic silver nanoparticles. The hair
bunch was treated for 15 minutes and then washed off with 0.5 gm of shampoo
and dried. The colour intensity was measured by measuring the L*a*b* value of
the hair bunches both before and after treatment and the ΔE values were
calculated to measure the extent of colouration. The change in ΔE values during
treatment is given in Table 12.
Table 12: Change in the ΔE (change in colour of white hair fibres after
different treatment with silicone oil) value with number of treatment by
silicone oil containing 2% hydrophobically modified silver nanoparticles
SI No No of treatment with
silicone oil
ΔE
1 1st treatment 62.99
2 2nd treatment 55.65
3 3rd treatment 52.45
4 4th treatment 48.22
5 5th treatment 42.31
20
Example 8
Deposition of hydrophobic silver nanoparticles and measurement of the
contact angle of hair
0.5 gm of hydrophobic silver nanoparticles were dispersed in 100 mL of silicone
oil through ultra sonication for 5 minutes. Then 5 gm of white/gray hairs was
treated with 0.5 gm of silicone oil containing hydrophobic silver nanoparticles.
The hair bunch was treated for 15 minutes and then washed off with 0.5 gm of
shampoo and dried. The contact angle of the hair was measured for both the
treated and untreated. For each time the samples were treated for 15 minutes.
Table 5 demonstrates the detail contact angle data (1st advancing angle) for both
treated and untreated samples along with control. Table 6 demonstrates the detail
contact angle data (1st receding angle) for both treated and untreated samples
along with control.
Degree of conditioning can be determined by measuring the advancing and
receding angles on the treated hair in comparison to the untreated hair sample.
Table 13 and 14 show that hair treated with a silicone oil with hydrophobic silver
nanoparticles show a higher advancing and receding value as compared with
untreated hair and hair treated with silicone oil minus the nanoparticles.
Table 13: 1st advancing angle of all the hair samples
Samples
1st
treatment
2nd
treatment
3rd
treatment
Untreated 94.01 91.07 88.03
Treated with silicone oil 94.25 94.82 95.21
Treated with hydrophobic silver nanoparticles
(0.5%) dispersed in silicone oil 97.5 99.23 102.42
21
Table 14: 1st receding angle of contact for all the hair samples
Samples
1st
treatment
2nd
treatment
3rd
treatment
Untreated 54.9 50.21 48.22
Treated with silicone oil 61.47 54.09 53.87
Treated with hydrophobic silver nanoparticles
(0.5%) dispersed in silicone oil 62.76 68.83 72.32
22
We claim:
1. A cosmetic composition comprising:
at least one cosmetically active component; and
a metallic nanoparticle composite material comprising a metal and at least
one of semiconductors, polymers, fatty acids, fatty alcohols, long chain
amides and esters;
wherein said metallic nanoparticles are hydrophobically modified.
2. The cosmetic composition as claimed in claim 1, wherein the said
composition provides colouring effect to hair.
3. The cosmetic composition as claimed in claim 1, wherein the said
composition provides conditioning and antimicrobial effect to hair.
4. The cosmetic composition as claimed in any of the preceding claims,
wherein said composition comprises hydrophobic silicones and cationic
surfactants.
5. The cosmetic composition as claimed in the preceding claims, wherein the
said nanoparticle is non-spherical in shape including but not limited to
rods, prism, nanowires, cubes and platelets.
6. The cosmetic composition as claimed in the preceding claims, wherein the
size of the hydrophobically modified metallic nanoparticle is preferably 1
to 100 nm, more preferably 10 to 80 nm and most preferably 5 to 30 nm.
7. The cosmetic composition as claimed in the preceding claims, wherein the
hydrophobically modified metallic nanoparticle provides coloring effect to
hair within about 2 minutes of time interval.
8. The cosmetic composition as claimed in the preceding claims, wherein the
hydrophobically modified metallic nanoparticle is incorporated into a
personal care product such as shampoos, conditioners, cream, gel, lotion,
serum, emulsion, hair spray or the like.
9. The cosmetic composition as claimed in the preceding claims is a rinse off
product, wherein the colouring can be achieved through rinse off products.
23
10. The cosmetic composition as claimed in the preceding claims is a leave on
product, wherein the colouring can be achieved through or leave on
products.
Dated this 7th day of March 2012
A.K. Chakraborty
of S. MAJUMDAR & CO.
Applicant’s Agent
24
Abstract
NANOMATERIAL BASED COSMETIC PRODUCTS
The present invention discloses cosmetic compositions containing
hydrophobically modified nanomaterials as hair colourants. The present
invention also discloses cosmetic compositions (both rinse off and leave on) to
achieve the desired hair colour in a short time interval without any
pretreatment. The nanomaterial based colourants of the present invention can
impart effective antimicrobial activity along with enhanced gloss,
conditioning and smoothness to the hair.
Applicant: ITC LIMITED 3 SHEETS
SHEET 1
A. K. Chakraborty
Of S. MAJUMDAR & CO.
(Applicant’s Agent)
Figure 1
Control A B
Figure 2
Control A B
Applicant: ITC LIMITED 3 SHEETS
SHEET 2
A. K. Chakraborty
Of S. MAJUMDAR & CO.
(Applicant’s Agent)
Figure 3
Figure 4
Applicant: ITC LIMITED 3 SHEETS
SHEET 3
A. K. Chakraborty
Of S. MAJUMDAR & CO.
(Applicant’s Agent)
Figure 5

Documents

Application Documents

# Name Date
1 244-KOL-2012-(07-03-2012)-POWER OF AUTHORITY.pdf 2012-03-07
2 244-KOL-2012-(07-03-2012)-FORM-3.pdf 2012-03-07
3 244-KOL-2012-(09-03-2012)-FORM-18.pdf 2012-03-09
4 244-KOL-2012-(13-04-2012)-FORM-1.pdf 2012-04-13
5 244-KOL-2012-(13-04-2012)-CORRESPONDENCE.pdf 2012-04-13
6 Other Patent Document [19-12-2016(online)].pdf 2016-12-19
7 244-KOL-2012-FER.pdf 2016-12-22
8 Other Document [22-06-2017(online)].pdf 2017-06-22
9 Examination Report Reply Recieved [22-06-2017(online)].pdf 2017-06-22
10 Claims [22-06-2017(online)].pdf 2017-06-22
11 244-KOL-2012-HearingNoticeLetter.pdf 2017-09-11
12 244-KOL-2012-Written submissions and relevant documents (MANDATORY) [20-10-2017(online)].pdf 2017-10-20
13 244-KOL-2012-RELEVANT DOCUMENTS [20-10-2017(online)].pdf 2017-10-20
14 244-KOL-2012-MARKED COPIES OF AMENDEMENTS [20-10-2017(online)].pdf 2017-10-20
15 244-KOL-2012-Annexure (Optional) [20-10-2017(online)].pdf 2017-10-20
16 244-KOL-2012-AMMENDED DOCUMENTS [20-10-2017(online)].pdf 2017-10-20
17 244-KOL-2012-Amendment Of Application Before Grant - Form 13 [20-10-2017(online)].pdf 2017-10-20
18 244-KOL-2012-PatentCertificate02-04-2018.pdf 2018-04-02
19 244-KOL-2012-IntimationOfGrant02-04-2018.pdf 2018-04-02
20 244-KOL-2012-RELEVANT DOCUMENTS [31-03-2019(online)].pdf 2019-03-31
21 244-KOL-2012-FORM 4 [29-06-2019(online)].pdf 2019-06-29
22 244-KOL-2012-RELEVANT DOCUMENTS [25-03-2020(online)].pdf 2020-03-25
23 244-KOL-2012-RELEVANT DOCUMENTS [23-09-2021(online)].pdf 2021-09-23
24 244-KOL-2012-RELEVANT DOCUMENTS [27-09-2022(online)].pdf 2022-09-27

Search Strategy

1 244kol2012searchstrategy_22-12-2016.pdf

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