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Patent 2894928 Summary

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(12) Patent Application: (11) CA 2894928
(54) English Title: ANTI-MICROBIAL LAUNDRY DETERGENT PRODUCT
(54) French Title: PRODUIT DETERGENT ANTIMICROBIEN DE LESSIVE
Status: Dead
Bibliographic Data
(51) International Patent Classification (IPC):
  • C11D 1/12 (2006.01)
  • C11D 1/66 (2006.01)
(72) Inventors :
  • GUO, YU (China)
  • OHTANI, RYOHEI (Japan)
  • ISHIDA, YOSHIKI (Japan)
  • WENDT, HANS (China)
  • EIKE, DAVID MICHAEL (United States of America)
(73) Owners :
  • THE PROCTER & GAMBLE COMPANY (United States of America)
(71) Applicants :
  • THE PROCTER & GAMBLE COMPANY (United States of America)
(74) Agent: TORYS LLP
(74) Associate agent:
(45) Issued:
(86) PCT Filing Date: 2012-12-13
(87) Open to Public Inspection: 2014-06-19
Examination requested: 2015-06-12
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): Yes
(86) PCT Filing Number: PCT/CN2012/086574
(87) International Publication Number: WO2014/089808
(85) National Entry: 2015-06-12

(30) Application Priority Data: None

Abstracts

English Abstract

The use of a laundry detergent composition for providing an anti-microbial benefit. The laundry detergent composition comprises at least 2.9%, preferably from 3.2% to 30%, more preferably from 4.3% to 20%, by weight of the composition, of a linear alkylbenzene sulfonate (LAS), and the laundry detergent composition is capable of delivering a free LAS monomer level of more than 60 ppm, preferably from 67 ppm to 500 ppm, more preferably from 88 ppm to 300 ppm, in a laundry washing liquor.


French Abstract

L'invention concerne l'utilisation d'une composition détergente antimicrobienne de lessive produisant un effet antimicrobien bénéfique. La composition détergente de lessive comprend au moins 2,9 %, de préférence de 3,2 % à 30 %, et idéalement de 4,3% à 20 % en poids d'une composition de sulfonate d'alkylbenzène linéaire (LAS), et permet d'obtenir un niveau de monomère à LAS libre de plus de 60 ppm, de préférence de 67 ppm à 500 ppm, et idéalement de 88 à to 300 ppm dans une liqueur de lavage de linge.

Claims

Note: Claims are shown in the official language in which they were submitted.



27

CLAIMS

What is claimed is:

1. The use of a laundry detergent composition for providing an anti-microbial
benefit, said
laundry detergent composition comprising at least 2.9%, preferably from 3.2%
to 30%, more
preferably from 4.3% to 20%, by weight of the composition, of a linear
alkylbenzene sulfonate
(LAS), wherein said laundry detergent composition is capable of delivering a
free LAS monomer
level of more than 60 ppm, preferably from 67 ppm to 500 ppm, more preferably
from 88 ppm to
300 ppm, in a laundry washing liquor.
2. The use according to Claim 1, wherein said anti-microbial benefit is
determined by the QB/T
2738-2005 method.
3. The use according to Claim 2, wherein said laundry detergent composition is
substantially free
of a co-surfactant.
4. The use according to Claim 2, wherein said laundry detergent composition
further comprises
from 0.001% to 25.4%, preferably from 0.001% to 13.5%, by weight of the
composition, of a
nonionic surfactant.
5. The use according to Claim 2, wherein said laundry detergent composition
further comprises
from 0.001% to 53.6%, preferably from 0.001% to 25.5%, by weight of the
composition, of a
sulphated fatty alcohol ethoxylate (AES).
6. The use according to Claim 2, wherein said laundry detergent composition is
substantially free
of an anti-microbial agent.
7. The use according to Claim 2, wherein said laundry detergent composition
provides said anti-
microbial benefit against gram positive bacteria.
8. The use according to Claim 7, wherein said laundry detergent composition
provides a bacteria
killing rate of at least 50% in a 2069 ppm aqueous solution against
Staphylococcus aureus for a
20 minutes contact time as determined by the QB/T 2738-2005 method.


28

9. The use according to Claim 8, wherein said laundry detergent composition is
capable of
delivering a free LAS monomer level of more than 60 ppm, and wherein said
laundry detergent
composition provides a bacteria killing rate of at least 50% in a 2069 ppm
aqueous solution
having a temperature of above 35°C against Staphylococcus aureus for a
20 minutes contact time
as determined by the QB/T 2738-2005 method.
10. The use according to Claim 8, wherein said laundry detergent composition
is capable of
delivering a free LAS monomer level of more than 67 ppm, and wherein said
laundry detergent
composition provides a bacteria killing rate of at least 50% in a 2069 ppm
aqueous solution
against Staphylococcus aureus for a 20 minutes contact time as determined by
the QB/T 2738-
2005 method.
11. A laundry detergent product comprising a laundry detergent composition
contained within a
container,
wherein said laundry detergent composition comprises at least 2.9%, preferably
from 3.2% to
30%, more preferably from 4.3% to 20%, by weight of the composition, of a LAS,
wherein said
laundry detergent composition is capable of delivering a free LAS monomer
level of more than
60 ppm, preferably from 67 ppm to 500 ppm, more preferably from 88 ppm to 300
ppm, in a
laundry washing liquor; and
wherein said container comprises instructions instructing the user of the anti-
microbial benefit
of said laundry detergent composition.
12. The laundry detergent product according to Claim 11, wherein said laundry
detergent
composition is substantially free of a co-surfactant.
13. The laundry detergent product according to Claim 11, wherein said laundry
detergent
composition further comprises from 0.001% to 25.4%, preferably from 0.001% to
13.5%, by
weight of the composition, of a nonionic surfactant.
14. The laundry detergent product according to Claim 11, wherein said laundry
detergent
composition further comprises from 0.001% to 53.6%, preferably from 0.001% to
25.5%, by
weight of the composition, of an AES.


29

15. The laundry detergent product according to Claim 11, wherein said laundry
detergent
composition is substantially free of an anti-microbial agent.
16. The laundry detergent product according to Claim 11, wherein said laundry
detergent
composition is a liquid laundry detergent composition, and wherein said
container is a bottle
comprising a dosing cap, wherein said dosing cap is configured to hold a
volume of from 60 g to
120 g, wherein said container further comprises instructions instructing the
user to dose from 5 g
to 60 g of said laundry detergent composition into a hand washing basin or
from 60 g to 120 g of
said laundry detergent composition into a washing machine via said dosing cap.
17. The laundry detergent product according to Claim 16, wherein said
container further
comprises instructions instructing the user to use said laundry detergent
composition for a hand
washing.
18. The laundry detergent product according to Claim 11, wherein said
container comprises
instructions instructing the user of the anti-microbial benefit of said
laundry detergent
composition against gram positive bacteria.
19. A method of using the laundry detergent product according to any one of
Claims 11 - 18 to
treat a fabric with an anti-microbial benefit comprising the step of
administering from 5 g to 120
g of said laundry detergent composition into a laundry washing basin
comprising water to form
an aqueous solution, wherein said aqueous solution has a free LAS monomer
level of more than
60 ppm, preferably from 67 ppm to 500 ppm, more preferably from 88 ppm to 300
ppm.
20. The method according to Claim 19, further comprising the step of
contacting a fabric with
said aqueous solution, wherein said fabric is in need of an anti-microbial
treatment.

Description

Note: Descriptions are shown in the official language in which they were submitted.


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ANTI-MICROBIAL LAUNDRY DETERGENT PRODUCT
FIELD OF THE INVENTION
The present invention relates to the use of a laundry detergent composition
for providing
an anti-microbial benefit. The present invention also relates to a laundry
detergent product
comprising a laundry detergent composition contained within a container and a
method of using
the laundry detergent product to treat a fabric with an anti-microbial
benefit.
BACKGROUND OF THE INVENTION
Consumer products have evolved to address user needs for an anti-microbial
benefit, in
addition to their original intended functions. For example, an anti-microbial
laundry detergent
product is desired by users as it cleans fabrics whilst having an anti-
microbial benefit on fabrics.
Currently, the typical approach to deliver an anti-microbial benefit is the
incorporation of anti-
microbial agents into the consumer product formulations. Such anti-microbial
agents either
damage the bacteria envelope to kill bacteria, or denature the bacteria
envelope to prevent
bacteria growth or reproduction, thereby delivering the anti-microbial
benefit.
However, the incorporation of anti-microbial agents into a consumer product
leads to
several challenges. Firstly, in terms of formulation design of a consumer
product, some anti-
microbial agents are not compatible or react with other ingredients (e.g.,
perfume oils)
incorporated in the same formulation to cause a stability issue. Moreover,
many consumer
products comprising anti-microbial agents are harsh or irritating to the skin
due to the nature of
the chemicals utilized to provide the anti-microbial benefit.
Thus, there is a need for a laundry detergent product that provides an anti-
microbial benefit
without the need of incorporating an anti-microbial agent.
It is an advantage of the present invention to provide an anti-microbial
laundry detergent
product that is gentle to the skin.
It is a further advantage of the present invention to provide a stable anti-
microbial laundry
detergent product.
SUMMARY OF THE INVENTION
In one aspect, the present invention is directed to the use of a laundry
detergent composition
for providing an anti-microbial benefit, the laundry detergent composition
comprising at least
2.9%, preferably from 3.2% to 30%, more preferably from 4.3% to 20%, by weight
of the

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composition, of a LAS, wherein the laundry detergent composition is capable of
delivering a free
LAS monomer level of more than 60 ppm, preferably from 67 ppm to 500 ppm, more
preferably
from 88 ppm to 300 ppm, in a laundry washing liquor.
In another aspect, the present invention is directed to a laundry detergent
product
comprising a laundry detergent composition contained in a container, wherein
the laundry
detergent composition comprises at least 2.9%, preferably from 3.2% to 30%,
more preferably
from 4.3% to 20%, by weight of the composition, of a linear alkylbenzene
sulfonate (LAS),
wherein the laundry detergent composition is capable of delivering a free LAS
monomer level of
more than 60 ppm, preferably from 67 ppm to 500 ppm, more preferably from 88
ppm to 300
ppm, in a laundry washing liquor, and wherein the container comprises
instructions instructing
the user of the anti-microbial benefit of the laundry detergent composition.
In yet another aspect, the present invention is directed to a method of using
the laundry
detergent product to treat a fabric with an anti-microbial benefit, comprising
the step of
administering from 5 g to 120 g of the laundry detergent composition into a
laundry washing
basin comprising water to form an aqueous solution, wherein the aqueous
solution has a free
LAS monomer level of more than 60 ppm, preferably from 67 ppm to 500 ppm, more
preferably
from 88 ppm to 300 ppm.
DETAILED DESCRIPTION OF THE INVENTION
Definitions
As used herein, the term "laundry detergent product" means a product relating
to cleaning
fabrics.
As used herein, the term "anti-microbial agent" refers to a chemical compound
of which the
principle intended function is to kill bacteria or to prevent their growth or
reproduction. Those
chemical compounds that do not have a principle intended function as anti-
microbial agents but
impart the anti-microbial benefit for some time are not considered as the anti-
microbial agent of
the present invention. For example, LAS in a laundry detergent composition is
not considered as
an anti-microbial agent because the principle intended function of LAS is a
cleaning surfactant,
even though it may impart an anti-microbial benefit in certain circumstances
(as illustrated in the
present invention).
As used herein, the term "free LAS monomer" refers to the linear alkylbenzene
sulfonate
(LAS) monomers that do not aggregate to form micelles. It is known that, LAS
starts to form
micelles when its concentration in water achieves or exceeds its critical
micelle concentration

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(CMC). Thus, in a laundry washing liquor, LAS typically comprises those
forming micelles and
the left free LAS monomers. The free LAS monomer level in an aqueous solution
can be
calculated or measured by any method known in the prior art. Preferably, the
free LAS monomer
level is calculated by the Calculation Method of Free LAS Monomer as described
hereinafter.
As used herein, the term "laundry washing liquor" refers to the typical amount
of aqueous
solution used for one cycle of laundry washing, preferably from 1 L to 50 L,
alternatively from 1
L to 20 L for hand washing and from 20 L to 50 L for machine washing.
As used herein, the term "co-surfactant" refers to a coexistent surfactant in
the laundry
detergent composition of the present invention, in addition to the LAS. In one
embodiment, the
co-surfactant is selected from the group consisting of an anionic surfactant
except the LAS (e.g.,
sulphated fatty alcohol ethoxylated (AES)), a cationic surfactant, a nonionic
surfactant, a
zwitterionic surfactant, and a combination thereof. A surfactant system is
formed from the
combination of the LAS and the co-surfactant.
As used herein, when a composition is "substantially free" of a specific
ingredient, it is
meant that the composition comprises less than a trace amount, alternatively
less than 0.1%,
alternatively less than 0.01%, alternatively less than 0.001%, by weight of
the composition of the
specific ingredient.
As used herein, the articles including "a" and "an" when used in a claim, are
understood to
mean one or more of what is claimed or described.
As used herein, the terms "comprise", "comprises", "comprising", "include",
"includes",
"including", "contain", "contains", and "containing" are meant to be non-
limiting, i.e., other
steps and other ingredients which do not affect the end of result can be
added. The above terms
encompass the terms "consisting of' and "consisting essentially of'.
Laundry Detergent Composition
The laundry detergent composition of the present invention comprises at least
2.9%,
preferably from 3.2% to 30%, more preferably from 4.3% to 20%, by weight of
the composition,
of a LAS. In a laundry washing liquor, the laundry detergent composition is
capable of
delivering a free LAS monomer level of more than 60 ppm, preferably from 67
ppm to 500 ppm,
more preferably from 88 ppm to 300 ppm.
In the present invention, applicant has surprisingly found that the level of
the free LAS
monomers in a laundry washing liquor constitutes the key to delivering an anti-
microbial benefit.
Only when the level of the free LAS monomers is above a specific level in a
laundry washing

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liquor, is when an anti-microbial benefit is achieved. Specifically, a level
of the free LAS
monomers of more than 60 ppm in a laundry washing liquor provides a bacteria
killing rate of at
least 50% according to the QB/T 2738-2005 method. In one embodiment, a level
of the free
LAS monomers of more than 60 ppm in a laundry washing liquor having a
temperature of above
35 C provides a bacteria killing rate of at least 50% according to the QB/T
2738-2005 method.
In an alternative embodiment, a level of the free LAS monomers of more than 67
ppm in a
laundry washing liquor (e.g., at 25 C) provides a bacteria killing rate of at
least 50% according to
the QB/T 2738-2005 method. Preferably, a level of the free LAS monomers of
more than 88
ppm in a laundry washing liquor (e.g., at 25 C) provides a bacteria killing
rate of at least 90%
according to the QB/T 2738-2005 method. Without wishing to be bound by theory,
it is believed
that a sufficient amount of the free LAS monomers in a laundry washing liquor
(namely, more
than 60 ppm, preferably more than 67 ppm, more preferably more than 88 ppm of
the free LAS
monomers in the laundry washing liquor) enables at least a portion of the free
LAS monomers to
penetrate into and damage the bacteria envelope, thereby achieving the anti-
microbial benefit.
Furthermore, laundry detergent compositions with such an anti-microbial
benefit delight users by
providing a fresh, treated fabric due to less amounts of bacteria left on the
fabric.
The laundry detergent composition herein may be of any suitable temperature
for washing
fabrics, preferably the temperatures of the laundry washing liquor range from
5 C to 60 C.
Applicant has found that a higher temperature of the laundry washing liquor
helps in the anti-
microbial benefit, thereby enabling a lower level of the free LAS monomers to
achieve the same
anti-microbial efficacy. For example, in order to achieve a bacteria killing
rate of at least 50%
according to the QB/T 2738-2005 method, the level of the free LAS monomers in
a laundry
washing liquor having a temperature of 25 C is required to be more than 67
ppm. Nevertheless,
a free LAS monomer level of 60 ppm in a laundry washing liquor having a
temperature of above
35 C provides a bacteria killing rate of more than 50% according to the QB/T
2738-2005 method.
The laundry detergent composition herein provides anti-microbial benefits
against both
gram positive bacteria (e.g., Staphylococcus aureus) and gram negative
bacteria (e.g.,
Escherichia colt). In particular, the laundry detergent composition provides
good anti-microbial
efficacy against gram positive bacteria.
There are a variety of factors that may determine the level of the free LAS
monomers in a
laundry washing liquor. Such factors include but are not limited to: CMC of
the laundry
detergent composition, the level of the LAS in the laundry detergent
composition, the presence of
co-surfactants and their levels in the laundry detergent composition, the
ratio of the LAS to co-

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surfactants, the presence of adjunct ingredients in the laundry detergent
composition, and
conditions of the water supplied for the laundry washing liquor (e.g., the
water hardness). These
factors may affect each other. Thus, by adjusting these factors, a wide
variety of combinations
between LAS and co-surfactants or other ingredients are suitable herein
provided the
5 combinations deliver a free LAS monomer level of more than 60 ppm in a
laundry washing
liquor.
In one embodiment, the laundry detergent composition herein comprises LAS and
is
substantially free of a co-surfactant, preferably substantially free of AES, a
nonionic surfactant, a
cationic surfactant, and a zwitterionic surfactant. Preferably, the laundry
detergent composition
comprises at least 2.9% of the LAS and is substantially free of a co-
surfactant, which delivers a
free LAS monomer level of more than 60 ppm in a laundry washing liquor. More
preferably, the
laundry detergent composition comprises at least 3.2% of the LAS and is
substantially free of a
co-surfactant, which delivers a free LAS monomer level of more than 67 ppm in
a laundry
washing liquor. Even more preferably, the laundry detergent composition
comprises at least 4.3%
of the LAS and is substantially free of a co-surfactant, which delivers a free
LAS monomer level
of more than 88 ppm in a laundry washing liquor.
In an alternative embodiment, the laundry detergent composition further
comprises a co-
surfactant selected from the group consisting of an anionic surfactant except
the LAS (e.g., AES),
a nonionic surfactant, a cationic surfactant, a zwitterionic surfactant, and a
combination thereof.
Without wishing to be bound by theory, with the introduction of the co-
surfactant, the CMC of
the laundry detergent composition is significantly reduced and surfactants
start to form micelles
at a lower concentration. As a result, the amount of the left free LAS
monomers is reduced.
Therefore, in order to achieve a free LAS monomer level of more than 60 ppm,
the level of the
LAS in the laundry detergent composition having such a surfactant system needs
to be slightly
higher than the aforementioned laundry detergent composition that is free of a
co-surfactant.
In one preferred embodiment, the laundry detergent composition comprises the
combination
of LAS and a co-surfactant of AES. Preferably, the AES is present at a level
of from 0.001% to
53.6%, preferably from 0.001% to 25.5%, by weight of the composition. For
example, in a
laundry washing liquor, a laundry detergent composition having the LAS at a
level of 3.9% and
the AES at a level of 5.0% delivers a free LAS monomer of 60 ppm, a laundry
detergent
composition having the LAS at a level of 4.6% and the AES at a level of 5.0%
delivers a free
LAS monomer of 67 ppm, a laundry detergent composition having the LAS at a
level of 20.0%
and the AES at a level of 25.5% delivers a free LAS monomer of 88 ppm, and a
laundry

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detergent composition having the LAS at a level of 20.0% and the AES at a
level of 44.5%
delivers a free LAS monomer of 67 ppm. A relatively low level of the AES in
the laundry
detergent composition is preferred as it requires a lower level of the LAS to
achieve the free LAS
monomer level of more than 60 ppm in a laundry washing liquor.
In another preferred embodiment, the laundry detergent composition comprises
the
combination of LAS and a co-surfactant of nonionic surfactant. Preferably, the
nonionic
surfactant is present at a level of from 0.001% to 25.4%, preferably from
0.001% to 13.5%, by
weight of the composition. For example, in a laundry washing liquor, a laundry
detergent
composition having the LAS at a level of 3.5% and the nonionic surfactant at a
level of 0.6%
delivers a free LAS monomer of 60 ppm, a laundry detergent composition having
the LAS at a
level of 4.0% and the nonionic surfactant at a level of 0.6% delivers a free
LAS monomer of 67
ppm, a laundry detergent composition having the LAS at a level of 20.0% and
the nonionic
surfactant at a level of 13.5% delivers a free LAS monomer of 88 ppm, and a
laundry detergent
composition having the LAS at a level of 20.0% and the nonionic surfactant at
a level of 21.7%
delivers a free LAS monomer of 67 ppm. Similar to the AES, a relatively low
level of the
nonionic surfactant in the laundry detergent composition is preferred as it
requires a lower level
of the LAS to achieve the free LAS monomer level of more than 60 ppm in a
laundry washing
liquor.
In yet another preferred embodiment, the laundry detergent composition
comprises the
combination of LAS and co-surfactants of AES and nonionic surfactant.
Preferably, the nonionic
surfactant is present at a level of from 0.001% to 25.4%, preferably from
0.001% to 13.5%, the
AES is present at a level of from 0.001% to 53.6%, preferably from 0.001% to
25.5%, by weight
of the composition, and the laundry detergent composition delivers a free LAS
monomer level of
more than 67 ppm in a laundry washing liquor. For example, in a laundry
washing liquor, a
laundry detergent composition having the LAS at a level of 11.5%, the AES at a
level of 8.2%,
and the nonionic surfactant at a level of 0.2% delivers a free LAS monomer of
97 ppm.
The laundry detergent composition herein may be acidic or alkali or pH
neutral, depending
on the ingredients incorporated in the composition. The pH range of the
laundry detergent
composition is preferably from 5 to 11. It is known that an acidic or alkali
laundry detergent
composition achieves better anti-microbial efficacy than a pH neutral laundry
detergent
composition. Thus, the laundry detergent composition of the present invention
that delivers a
free LAS monomer level of more than 60 ppm in a laundry washing liquor
achieves even better

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anti-microbial efficacy under either acidic or alkali conditions versus under
a neutral pH
condition.
The laundry detergent composition may be a liquid or granular laundry
detergent
composition, preferably is a liquid laundry detergent composition. The term
"liquid laundry
detergent composition", as used herein, refers to compositions that are in a
form selected from
the group consisting of pourable liquid, gel, cream, and combinations thereof.
The liquid laundry
detergent composition may be anisotropic, isotropic and combinations thereof.
Anionic Surfactant
LAS is a required anionic surfactant for the laundry detergent composition of
the present
invention. The LAS herein can be any LAS classes known in the art. C10-C16 LAS
is preferred.
The LAS is normally prepared by sulfonation (using SO2 or SO3) of
alkylbenzenes followed by
neutralization. Suitable alkylbenzene feedstocks can be made from olefins,
paraffins or mixtures
thereof using any suitable alkylation scheme, including sulfuric and HF-based
processes. By
varying the precise alkylation catalyst, it is possible to widely vary the
position of covalent
attachment of benzene to an aliphatic hydrocarbon chain. Accordingly the LAS
herein can vary
widely in 2-phenyl isomer and/or internal isomer content.
In addition to the LAS, non-limiting examples of anionic surfactants useful as
a co-
surfactant herein include: C10-C20 primary, branched-chain and random alkyl
sulfates (AS); C10-
C18 secondary (2,3) alkyl sulfates; AES, preferably C10-C18 alkyl alkoxy
sulfates (AES) wherein
preferably x is from 1-30, more preferably x is 1-3; C10-C18 alkyl alkoxy
carboxylates preferably
comprising 1-5 ethoxy units; mid-chain branched alkyl sulfates as discussed in
US 6,020,303 and
US 6,060,443; mid-chain branched alkyl alkoxy sulfates as discussed in US
6,008,181 and US
6,020,303; modified alkylbenzene sulfonate (MLAS) as discussed in WO 99/05243,
WO
99/05242, and WO 99/05244; methyl ester sulfonate (MES); and alpha-olefin
sulfonate (AOS).
AES is the preferred anionic surfactant as a co-surfactant.
Nonionic Surfactant
Non-limiting examples of nonionic surfactants include: C12-C18 alkyl
ethoxylates, such as
Neodol nonionic surfactants available from Shell; C6-C12 alkyl phenol
alkoxylates wherein the
alkoxylate units are a mixture of ethyleneoxy and propyleneoxy units; C12-C18
alcohol and C6-
C12 alkyl phenol condensates with ethylene oxide/propylene oxide block alkyl
polyamine
ethoxylates such as PLURONIC available from BASF; C14-C22 mid-chain branched
alcohols,
BA, as discussed in US 6,150,322; C14-C22 mid-chain branched alkyl
alkoxylates, BAEx,
wherein x is from 1-30, as discussed in US 6,153,577, US 6,020,303 and US
6,093,856;

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alkylpolysaccharides as discussed in U.S. 4,565,647 Llenado, issued January
26, 1986;
specifically alkylpolyglycosides as discussed in US 4,483,780 and US
4,483,779; polyhydroxy
fatty acid amides as discussed in US 5,332,528; and ether capped
poly(oxyalkylated) alcohol
surfactants as discussed in US 6,482,994 and WO 01/42408. Also useful herein
as nonionic
surfactants are alkoxylated ester surfactants such as those having the formula

R1C(0)0(R20)nR3 wherein R1 is selected from linear and branched C6-C22 alkyl
or alkylene
moieties; R2 is selected from C2H4 and C3H6 moieties and R3 is selected from
H, CH3, C2H5
and C3H7 moieties; and n has a value between 1 and 20.Such alkoxylated ester
surfactants
include the fatty methyl ester ethoxylates (MEE) and are well-known in the
art; see for example
US 6,071,873; US 6,319,887; US 6,384,009; US 5,753,606; WO 01/10391, WO
96/23049. The
preferred nonionic surfactant as a co-surfactant is C12-C115 alcohol
ethoxylated with 7 moles of
ethylene oxide (e.g., Neodol 25-7 available from Shell).
Cationic Surfactant
Non-limiting examples of cationic surfactants include: the quaternary ammonium
surfactants, which can have up to 26 carbon atoms include: alkoxylate
quaternary ammonium
(AQA) surfactants as discussed in US 6,136,769; dimethyl hydroxyethyl
quaternary ammonium
as discussed in 6,004,922; dimethyl hydroxyethyl lauryl ammonium chloride;
polyamine cationic
surfactants as discussed in WO 98/35002, WO 98/35003, WO 98/35004, WO
98/35005, and WO
98/35006; cationic ester surfactants as discussed in US Patents Nos.
4,228,042, 4,239,660
4,260,529 and US 6,022,844; and amino surfactants as discussed in US 6,221,825
and WO
00/47708, specifically amido propyldimethyl amine (APA).
Adjunct Ingredients
The laundry detergent composition herein may comprise adjunct ingredients.
Suitable
adjunct materials include but are not limited to: builders, chelating agents,
dye transfer inhibiting
agents, dispersants, enzymes, and enzyme stabilizers, catalytic materials,
bleach activators,
hydrogen peroxide, sources of hydrogen peroxide, preformed peracids, polymeric
dispersing
agents, clay soil removal/anti-redeposition agents, brighteners, suds
suppressors, dyes,
photobleaches, perfumes, structure elasticizing agents, fabric softeners,
carriers, hydrotropes,
processing aids, solvents, hueing agents, structurants and/or pigments. In
addition to the
disclosure below, suitable examples of such other adjuncts and levels of use
are found in U.S.
Patent Nos. 5,576,282, 6,306,812 B1 and 6,326,348 B1 that are incorporated by
reference. The
precise nature of these adjunct ingredients and the levels thereof in the
laundry detergent

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9
composition will depend on the physical form of the composition and the nature
of the cleaning
operation for which it is to be used.
The laundry detergent composition herein may or may not comprise an anti-
microbial agent.
Preferably, the laundry detergent composition is substantially free of an anti-
microbial agent.
Without the incorporation of an anti-microbial agent, the laundry detergent
composition avoids
the issues caused by anti-microbial agents, e.g., formulation stability, skin
irritation.
Nevertheless, it should be understood and appreciated that the anti-microbial
agent can be
incorporated into the laundry detergent composition in certain circumstances,
e.g., to kill a
particular type of bacteria.
Container
The laundry detergent product of the present invention comprises a container
containing the
laundry detergent composition, wherein the container comprises instructions
instructing the user
of the anti-microbial benefit of the laundry detergent composition. Non-
limiting examples of the
instructions include: anti-microbial detergent, bacteria killing, bacteria
removal, and the like. In
one embodiment, the container comprises instructions instructing the user of
the anti-microbial
benefit of the laundry detergent composition against gram positive bacteria.
The container herein can be of any suitable size known in the art. In one
embodiment, the
container is configured to have an internal volume of from 250 cm3 to 10,000
cm3, preferably
from 500 cm3 to 3,000 cm3.
The container can be made of any suitable material, such as glass, metal,
polymer, and the
like. In one embodiment, the container is made of a polymeric material
selected from the group
consisting of polypropylene (PP), polyethylene (PE), polycarbonate (PC),
polyamides (PA)
polyethylene terephthalate (PET), polyvinylchloride (PVC), polystyrene (PS),
and a combination
thereof.
The container herein can be of any form known in the art, such as bottle, box,
bag, and
pouch. In one embodiment, the laundry detergent composition is a liquid
laundry detergent
composition, and the container is a bottle. Preferably, the container is a
bottle comprising a
dosing cap, wherein the dosing cap is configured to hold a volume of from 30 g
to 150 g,
preferably from 60 g to 120 g.
Preferably, the container further comprises instructions instructing the user
to dose a
suitable amount of the laundry detergent composition, depending on factors
including the nature
and the amount of the fabrics or surfaces that are going to be cleaned, the
washing type, the

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amount of water used for cleaning, etc. For example, the instructions instruct
the user to dose
from 5 g to 60 g of the laundry detergent composition into a hand washing
basin (e.g., 4L) or
from 60 g to 120 g of the laundry detergent composition into a washing machine
(e.g., 30L). In
the execution of the bottle comprising a dosing cap, the instructions instruct
the user to dose from
5 5 g to 60 g of the laundry detergent composition into a hand washing
basin or from 60 g to 120 g
of the laundry detergent composition into a washing machine via the dosing
cap.
The container may further comprise instructions instructing the user to use
the laundry
detergent composition for a hand washing. In particular, when the laundry
detergent composition
is substantially free of an anti-microbial agent, the container comprises
instructions instructing
10 the user to use the laundry detergent composition for a hand washing.
For example, such
instructions could be: gentle to the skin, not harsh to your hand, and the
like.
The container may further comprise instructions instructing the user to wash a
fabric with
the laundry detergent composition for certain time, preferably from 1 minute
to 90 minutes, more
preferably from 3 minutes to 60 minutes, even more preferably from 20 minutes
to 50 minutes,
alternatively at least 20 minutes. For example, such instructions could be:
wash your fabric with
the laundry detergent composition for at least 20 minutes to deliver a better
anti-microbial benefit.
The container may further comprise instructions instructing the user to pre-
treat a fabric
with the laundry detergent composition for certain time, preferably from 1
minute to 10 minutes.
The instructions herein may be applied to, preferably printed onto, any
portions of the
outward facing side of the container, e.g., the front, the back, the side, the
cap. In one
embodiment, the instructions related to the anti-microbial benefit are applied
to the front of the
container, and the instructions related to the dosing amount are applied to
the back of the
container.
Composition Preparation
The laundry detergent composition of the present invention is generally
prepared by
conventional methods such as those known in the art of making laundry
detergent compositions.
Such methods typically involve mixing the essential and optional ingredients
in any desired order
to a relatively uniform state, with or without heating, cooling, application
of vacuum, and the like,
thereby providing laundry detergent compositions containing ingredients in the
requisite
concentrations.
The Use

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One aspect of the present invention is directed to the use of the laundry
detergent
composition for providing an anti-microbial benefit. The laundry detergent
composition
comprises at least 2.9%, preferably from 3.2% to 30%, more preferably from
4.3% to 20%, by
weight of the composition, of a LAS, wherein the laundry detergent composition
is capable of
delivering a free LAS monomer level of more than 60 ppm, preferably from 67
ppm to 500 ppm,
more preferably from 88 ppm to 300 ppm, in a laundry washing liquor.
Preferably, the anti-microbial benefit is determined by the QB/T 2738-2005
method. More
preferably, the laundry detergent composition provides a bacteria killing rate
of at least 50% in a
2069 ppm aqueous solution against Staphylococcus aureus for a 20 minutes
contact time as
determined by the QB/T 2738-2005 method. In one preferred embodiment, the
laundry detergent
composition comprises at least 2.9%, by weight of the composition, of a LAS,
is capable of
delivering a free LAS monomer level of more than 60 ppm in a laundry washing
liquor, and
provides a bacteria killing rate of at least 50% in a 2069 ppm aqueous
solution having a
temperature of above 35 C against Staphylococcus aureus for a 20 minutes
contact time as
determined by the QB/T 2738-2005 method. In an alternative embodiment, the
laundry detergent
composition comprises from 3.2% to 30%, by weight of the composition, of a
LAS, is capable of
delivering a free LAS monomer level of from 67 ppm to 300 ppm in a laundry
washing liquor,
and provides a bacteria killing rate of at least 50% in a 2069 ppm aqueous
solution against
Staphylococcus aureus for a 20 minutes contact time as determined by the QB/T
2738-2005
method. In a more preferred embodiment, the laundry detergent composition
comprises from 4.3%
to 20%, by weight of the composition, of a LAS, is capable of delivering a
free LAS monomer
level of from 88 ppm to 300 ppm in a laundry washing liquor, and provides a
bacteria killing rate
of at least 90% in a 2069 ppm aqueous solution against Staphylococcus aureus
for a 20 minutes
contact time as determined by the QB/T 2738-2005 method.
Method of Use
Another aspect of the present invention is directed to a method of using the
laundry
detergent product to treat a fabric with an anti-microbial benefit. The method
comprises the step
of administering from 5 g to 120 g of the laundry detergent composition into a
laundry washing
basin comprising water to form an aqueous solution, wherein the aqueous
solution has a free
LAS monomer level of more than 60 ppm, preferably from 67 ppm to 500 ppm, more
preferably
from 88 ppm to 300 ppm. The aqueous solution in a laundry washing basin herein
has the same
volume as the laundry washing liquor, preferably from 1 L to 50 L,
alternatively from 1 L to 20 L

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for hand washing and from 20 L to 50 L for machine washing. The required
dosing amount of
the laundry detergent composition by the present invention, namely, from 5 g
to 120 g of the
laundry detergent composition, is capable of delivering a free LAS monomer
level of more than
60 ppm in a laundry washing liquor of from 1 L to 50 L. Preferably, the anti-
microbial benefit
herein is determined by the QB/T 2738-2005 method. The temperatures of the
laundry washing
liquor preferably range from 5 C to 60 C
The dosing amount in the method herein may be different depending on the
washing type.
In one embodiment, the method comprises administering from 5 g to 60 g of the
laundry
detergent composition into a hand washing basin (e.g., 4 L). In an alternative
embodiment, the
method comprises administering from 60 g to 120 g of the laundry detergent
composition into a
washing machine (e.g., 30 L).
Preferably, the method herein further comprises the step of contacting a
fabric with the
aqueous solution, wherein the fabric is in need of an anti-microbial
treatment. For example, the
presence of gram positive bacteria and/or gram negative bacteria is suspected
on the fabric. The
step of contacting the fabric with the aqueous solution is preferably after
the step of
administering the laundry detergent composition in a laundry washing basin.
The method may
further comprise the step of contacting a fabric with the laundry detergent
composition prior to
the step of administering the laundry detergent composition in a laundry
washing basin, i.e., pre-
treat the fabric with the laundry detergent composition for certain time,
preferably from 1 minute
to 10 minutes.
Calculation Method of Free LAS Monomer
The calculation model of CMC and monomer-micelle composition is based on the
Pseudo-
phase Separation Model and the Regular Solution Theory. The Pseudo-phase
Separation Model
is described in "Non-ideal multicomponent mixed micelle model", Holland, P.
M.; Rubingh, D.
N., J. Phys. Chem. 1983, 87 (11), 1984-1990. The Regular Solution Theory is
described in
"Micellization of mixed nonionic surface-active agents", Clint J. H., J. Chem.
Soc., Faraday
Trans. 1 1975, 71, 1327-1334. The inputs to the calculation model are the
composition of the
surfactant formulation, CMCs of individual surfactants, and the interaction
between the
surfactants in a mixed micelle (i.e., beta parameters).
The Pseudo-phase Separation Model is used to calculate the CMC of a surfactant
mixture.
In this model, above the CMC the surfactants are assumed to exist in two
phases in equilibrium
with each other: aggregated micellar phase and non-aggregated monomeric phase.
Based on this

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two phase approximation, the chemical potential of a given surfactant species
in each phase can
be calculated as:
[iron
For monomeric phase, = 1.11Qm(m RT111Cr1' (1)
For micellar phase, [tric = [tiQmic + RT1nxiyi (2)
Also, for a pure surfactant solution at and above its CMC, the monomer
concentration is
fixed equal to the CMC concentration. Since the solution and micelle chemical
potentials are
equal, the following relationship is established for a pure system:
111 = [ti
0,mic 0,mon RT1nCCmc
(3)
At equilibrium, the chemical potential for a given species is equal in the two
phases, i.e., (1)
= (2). Therefore, obtain the following relationship by combining equations
(1), (2) and (3):
Clnon = xiyomc
(4)
For the mixture CMC, the following relationship is valid:
crn = aicmCNilxCture
(5)
Combining equations (4) and (5), and summing over the species, the CMC of the
mixture is
calculated as:
)-1
CcMc = (En 6)
mixture 1=1 rcmc,, (
yi
In order to calculate the activity coefficient,Ti in equation (6), the Regular
Solution Theory
is referred to. From the Regular Solution Theory, a simple activity
coefficient model is derived
as:
25vi-i (0 , m 0
lnYi = Pii x? + En j=i Pik ¨ Pjk)XjXk
(7)
(i#0 (i#i#k)
The Regular Solution Theory allows specific interactions between types of
surfactants to be
coarsely but successfully captured by a single interaction parameter. Quite
often in real
surfactant mixtures, the beta parameter is negative representing synergistic
interactions between
surfactants.

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In "Surfactants and Interfacial Phenomena", Rosen, M. J., Wiley Interscience:
New York,
1989, the beta parameters are clustered into groups based on surfactant type,
as summarized in
Table 1.
Table 1
ANIONIC CATIONIC NONIONIC ZWITTERIONIC
ANIONIC 0 -8 -2 -4
CATIONIC -8 0 -2 -4
NONIONIC -2 -2 0 0
ZWITTERIONIC -4 -4 0 0
To calculate the non-ideal mixture CMC, combine equation (7) with the
following equations
and solve iteratively.
Rewrite equation (4) for species i and j,
,cmc
xi ccik-j Yj
(8)
xj aJ Ccmcy
Sum over species j in equation (8),
,cmc
yj
____________________ = 1 (9)
xi j#1 alqmcy
Equations (7), (8) and (9) are then iteratively solved starting with an
estimate value for
activity coefficients. Specifically, steps involved in iterations include:
1) Initially, make an estimate of the activity coefficients. One option is to
start by assuming
an ideal micelle, where all activity coefficients are unity.
2) Based on a set of activity coefficients, solve (9) to calculate a new
estimate of micelle
mole fraction for a reference component, xi. Use xi with (8) to calculate new
estimates for
remaining micelle components.
3) Use the new micelle compositions with (7) to generate new activity
coefficients. If the
old and new activity coefficients have converged then a self-consistent
solution is achieved.
Otherwise, return to step 2 and continue to iterate until convergence.
Once the non-ideal CMC is known, the next step is to calculate the amount of
each species
present as monomers and in micelles. Below the CMC, the system is present
fully as monomers,

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and the monomer concentrations are equal to the bulk values. Above the CMC,
the following
relationship is needed to relate the micelle mole fraction of a given species
to a reference species:
aiCtotal
X = ccmcv _ccmcy +a ctotalix,
(10)
1 /1
5 The following relationship is based on the constraint that mole fractions
sum to one:
¨ ¨ = 1
xi - xi
Substituting (10) into (11) yields an expression to solve for reference mole
fraction xi based
on an estimate of activity coefficients. Therefore, the same solution steps as
used for non-ideal
10 CMC can be used, except (10)-(11) take the place of (8)-(9). Once
micelle mole fractions and
activity coefficients have been self-consistently determined, (4) is used to
yield monomer
concentrations.
Wherein in the above equations (1) to (11):
Symbol Meaning
CFmc critical micelle concentration of pure component i
Cure critical micelle concentration of mixed system
Clnon concentration of species i present as monomer
Grata' total concentration of all species in overall mixed
system
mole fraction of species i in mixed micelle
Xi mole fraction of a class of species i, in mixed micelle
mole fraction of species i in overall mixed system
Pii interaction parameter between species or species classes
i and j in mixed
Yi activity coefficient for species i in mixed micelle
0,mon standard chemical potential of species i in monomeric
state
o,rnic standard chemical potential of species i in pure micelle
pron chemical potential of species i as monomer in solution
r ic chemical potential of species i in mixed micelle
15 Therefore, for a surfactant mixture or an aqueous solution comprising
LAS, the level of the
free LAS monomers can be calculated as described above, wherein species i
represents LAS and
species j and k represent one or more co-surfactants.
Test Method

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The anti-microbial efficacy for laundry detergent compositions is determined
by the method
of simulation of washing machine as defined in the QB/T 2738-2005 method.
1. Microorganism Preparation:
A. Aseptically add certain amount of nutrient broth into a lyophilized culture
of
Staphylococcus aureus. Dissolve and suspend the culture in the nutrient broth
to obtain a
suspension. Apply some of the suspension into a tube containing 5.0 mL to 10.0
mL of nutrient
broth, and incubate at 37 C for 18 hours to 24 hours to obtain a first
generation subculture of
bacterial suspension. Streak a loop of the first generation subculture of
bacterial suspension on a
nutrient agar plate, and incubate at 37 C for 18 hours to 24 hours to obtain a
second generation
subculture of bacterial suspension. Inoculate a colony of the second
generation subculture of
bacterial suspension on a nutrient agar slant, incubate at 37 C for 18 hours
to 24 hours to obtain a
third generation subculture of bacterial suspension.
B. Use 3.0 mL to 5.0 mL of a dilution to purge colonies of the third
generation subculture to
the fourteenth generation subculture of bacterial suspension on a nutrient
agar slant. Transfer the
purge solution into another sterile tube, and vortex to mix for 20 seconds or
shake with hand for
80 times to obtain a preliminary working culture.
C. Adjust the bacterial concentration of the preliminary working culture to
the required
bacterial concentration with Spectrophotometer to obtain a working culture.
D. Store the working culture at 4 C. The working culture cannot be stored
overnight.
2. Assay Protocol:
A. Boil 300 g of a test fabric (32 yarn/cmx32 yarn/cm, plain weave cotton) in
3 L of a
washing solution for 1 hour. The washing solution is prepared by 1.5 g of a
nonionic soaked
agent, 1.5 g of sodium carbonate, and 3000 mL of distilled water. The nonionic
soaked agent is
prepared by 5.0 g of alkylphenol ethoxylate, 5 g of sodium carbonate, and 1000
mL of distilled
water. Rinse the test fabric in boiled deionized water for 5 minutes. Place
the test fabric in cool
deionized water for 5 minutes, and indoor dry.
B. Cut the treated test fabric to a strip having a width of 5 cm width and
weight of 15 1 g.
Fix one end of the test fabric strip onto a stainless steel spindle at an
outer position along the
horizontal extension of the stainless steel spindle. The stainless steel
spindle has 3 horizontal
stands that are connected to one another. Wrap the test fabric strip around
the 3 horizontal stands
of the stainless steel spindle with sufficient tension to obtain a fabric
wrapped spindle having 12
laps of fabric. Fix the other end of the test fabric strip onto the outer lap
of the 12 laps of fabric
via a pin. Sterilize the fabric wrapped spindle with pressure steam at 121 C
for 15 minutes.

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C. Dilute the working culture obtained from step 1D using a phosphate buffered
solution
(PBS) to achieve a concentration of from 1x104 cfu/ml to 9x104 cfu/ml. Add a
bovine serum
albumin solution (BSA) with the same volume to obtain a bacterial suspension.
The PBS is
prepared by dissolving 2.83 g of disodium hydrogen phosphate, anhydrous and
1.36 g of
potassium dihydrogen phosphate in 1000 mL of distilled water, until completely
dissolved
adjusting the pH of the solution to 7.2 to 7.4, and then sterilizing the
solution with pressure steam
at 121 C for 20 minutes. The BSA is prepared by dissolving 3.0 g bovine serum
albumin in 100
mL of distilled water, filtered the solution with a microporous membrane
having a pore size of
0.45 lam and preserved in a refrigerator.
D. Prepare 3 fabric carriers, each fabric carrier having a width of 2.5 cm to
3.8 cm. Treat the
fabric carriers with the same method as treating the test fabric, as described
herein above in step
2A. Inoculate each fabric carrier with 20 [t.L of the bacterial suspension
obtained from step 2C.
Place the inoculated fabric carrier in a petri dish with cover. Dry the
inoculated fabric carriers in
an incubator at (35 2) C for 20 minutes.
E. 20 minutes prior to testing, place an exposure chamber containing 265 mL of
standard
hard water in a water bath to achieve the test temperature of (25 1) C. The
exposure chamber is
sterilized with pressure steam at 121 C for 15 minutes. The standard hard
water is prepared by
dissolving 0.034 g of calcium chloride and 0.139 g of magnesium chloride
hexahydrate in 1000
mL of distilled water, and then sterilizing the solution with pressure steam
at 121 C for 20
minutes. Add sufficient amount of sample into the exposure chamber to obtain a
mixed solution
having a concentration of 2069 ppm.
F. Place the 2 inoculated fabric carriers in the position between the 6th lap
and the 7th lap of
the 12 laps of fabric, and place the 3rd inoculated fabric carrier into the
position between the 7th
lap and the 8th lap of the 12 laps of fabric.
G. Aseptically place the spindle unit (including the fabric wrapped spindle
and the
inoculated fabric carriers) into the exposure chamber, and close the exposure
chamber with a lid.
H. Fix the exposure chamber onto a shaker. Rotate the shaker for 20 minutes.
Remove the
exposure chamber from the shaker.
I. Aseptically remove the spindle unit out of the exposure chamber and remove
the 3
inoculated fabric carriers from the fabric wrapped spindle. Place each fabric
carrier into a
separate tube containing 30 mL of a neutralizer, vortex to mix for 10 seconds,
shake for 100
times, and 10 times serially dilute using PBS. The neutralizer is prepared by
37.8 g of letheen
broth base modified (available as 110405 from Merck), 30 g of Tween 80, 2.3 g
of lecithin, 5 g

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of sodium thiosulfate, and 1000 mL of distilled water. Tween 80 is
polyoxyethylene (20)
sorbitan monooleate. Plate appropriate dilution of the sample into TSB with
duplicate form a
TSB plate.
J. In step 2E, use a PBS containing 0.5% Tween 80 instead of the sample as
control.
K. Incubate the TSB plates of the sample and the control reversely in a
incubator at
(35 2) C for (48 4) hours. Plate counting.
L. Repeat 3 times, and obtain average results.
3. Calculation of Bacteria Killing Rate
Bacteria Killing Rate (%) = (A-B)/Ax100%
wherein: A: Counting of control group
B: Counting of sample group
A Bacteria Killing Rate of greater than 50% represents acceptable anti-
microbial efficacy,
of greater than 90% represents good anti-microbial efficacy, and of greater
than 99% represents
excellent anti-microbial efficacy. And a Bacterial Killing Rate of lower than
50% indicates
unacceptable poor anti-microbial efficacy.
Example
The Examples herein are meant to exemplify the present invention but are not
used to limit
or otherwise define the scope of the present invention. Examples 1A - 1X and
2A - 2D are
examples according to the present inventions, and Examples 3A - 3B are
comparative examples.
Example 1A - 1X: Formulations of laundry detergent compositions
The following compositions in liquid forms shown in Table 2 are made
comprising the
listed ingredients in the listed proportions (weight %). The calculated level
of the free LAS
monomers in a 2069 ppm aqueous solution according to the Calculation Method of
Free LAS
Monomer as described above is listed for each composition.
Table 2
1A 1B 1C 1D 1E 1F 1G 1H
CH-Cu LAS 2.9 3.2 4.3 11 3.9 4.6 7.3 4.5
C12-C14AE35 0 0 0 0 5.0 5.0 5.0 1.0
Neodol 25-7 a 0 0 0 0 0 0 0 0
Add to Add to Add to Add to Add to Add to Add to Add to
Water
100 100 100 100 100 100 100 100

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Free LAS
60 67 88 133 60 67 88 88
monomer (ppm)
Table 2 (continued)
11 1J 1K 1L 1M 1N 10 1P
C11-C13 LAS 3.7 20.0 20.0 30.0 3.5 4.0 7.9
5.6
C12-C14AE35 1.0 53.6 44.5 25.5 0 0 0 0
Neodol 25-7 a 0 0 0 0 0.6 0.6 5.0 0.6
Add to Add to Add to Add to Add to Add to Add to Add to
Water
100 100 100 100 100 100 100
100
Free LAS
76 60 67 88 60 67 67 88
monomer (ppm)
Table 2 (continued)
1Q 1R is 1T 1U 1V 1W 1X
CH-Cu LAS 11.3 20.0 20.0 20.0 6.5 9.0 11.0
11.5
C12-C14AE35 0 0 0 0 9.8 7.0 5.5 8.2
Neodol 25-7 a 5.0 25.4 21.7 13.5 1.4 0.6 0.6
0.2
Add to Add to Add to Add to Add to Add to Add to Add to
Water
100 100 100 100 100 100 100
100
Free LAS
88 60 67 88 60 87 101 97
monomer (ppm)
a Neodol 25-7 is C12-C115 alcohol ethoxylated with 7 moles of ethylene oxide
as a nonionic surfactant,
available from Shell
Preparation of the compositions of Example 1A - 1X
The compositions of Example 1A - 1X are prepared by mixing the ingredients
listed for
each composition with a shear of 250 rpm, respectively.
Example 2A - 2D: Formulations of laundry detergent compositions
The following compositions in liquid forms shown in Table 3 are made
comprising the
listed ingredients in the listed proportions (weight %). The calculated level
of the free LAS

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monomers in a 2069 ppm aqueous solution according to the Calculation Method of
Free LAS
Monomer as described above is listed for each composition.
Table 3
2A 2B 2C 2D
CH-Cu LAS 9.0 11.0 11.5 6.5
C12-C14AE35 7.0 8.0 8.2 9.8
Neodol 25-7 a 0.6 0.6 0.2 1.4
Citric acid 1 0.5 0 2.4
C12-C18 fatty acid 1.2 1.3 0 1.3
Chelant b 0.2 0.4 0 0.4
1, 2 propanediol 2 4 0 2.5
Tri ethanol amine 0 0 1.8 0
NaOH 2.9 2.9 0 3.2
Dye 0.002 0.002 0.002 0.002
Perfume 0.5 0.7 0.5 0.5
Add to Add to Add to Add to
Water
100 100 100 100
Free LAS monomer
87 93 97 60
(PPm)
a Neodol 25-7 is C12-C115 alcohol ethoxylated with 7 moles of ethylene oxide
as a nonionic surfactant,
5 available from Shell
b diethylene triamine penta acetate
Preparation of the composition of Example 2A
The composition of Example 2A is prepared by the following steps:
10 a) mixing a combination of NaOH, 1, 2 propanediol, and water in a mixer
by applying a
shear of 200 rpm;
b) adding Citric acid, Neodol 25-7, and Chelant in sequence into the
combination obtained
in step a), keeping on mixing by applying a shear of 200 rpm;
c) increasing the mixing shear to 250 rpm, and maintaining the temperature of
the
15 combination obtained in step b) to be under 45 C;
d) mixing the combination obtained in step c) with LAS by applying a shear of
250 rpm;

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e) once the temperature of the combination obtained in step d) is below 35 C,
adding AES
into the combination and mixing by applying a shear of 250 rpm until the
combination is
homogeneously mixed;
f) adding C12-C18 fatty acid into the combination obtained in step e), keeping
on mixing by
applying a shear of 250 rpm for 5 minutes;
g) adding Perfume and Dye into the combination obtained in step f), keeping on
mixing by
applying a shear of 250 rpm for 5 minutes, thus forming a liquid laundry
detergent
composition,
wherein in the composition, each ingredient is present in the amount as
specified for
Example 2A in Table 3.
Preparation of the composition of Example 2B
The composition of Example 2B is prepared by the same steps as preparing the
composition
of Example 2A, except for that each ingredient is present in the amount as
specified for Example
2B in Table 3.
Preparation of the composition of Example 2C
The composition of Example 2C is prepared by the following steps:
a) mixing a combination of Tri ethanol amine and water in a mixer by applying
a shear of
200 rpm;
b) adding Neodol 25-7 into the combination obtained in step a), keeping on
mixing by
applying a shear of 200 rpm;
c) increasing the mixing shear to 250 rpm, and maintaining the temperature of
the
combination obtained in step b) to be under 45 C;
d) mixing the combination obtained in step c) with LAS by applying a shear of
250 rpm;
e) once the temperature of the combination obtained in step d) is below 35 C,
adding AES
into the combination and mixing by applying a shear of 250 rpm until the
combination is
homogeneously mixed;
f) adding Perfume and Dye into the combination obtained in step e), keeping on
mixing by
applying a shear of 250 rpm for 5 minutes, thus forming a liquid laundry
detergent
composition,
wherein in the composition, each ingredient is present in the amount as
specified for
Example 2C in Table 3.

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22
Preparation of the composition of Example 2D
The composition of Example 2D is prepared by the same steps as preparing the
composition
of Example 2A, except for that each ingredient is present in the amount as
specified for Example
2D in Table 3.
Comparative Example 3A - 3B: Comparative Formulations of laundry detergent
compositions
The following comparative compositions in liquid forms shown in Table 4 are
made
comprising the listed ingredients in the listed proportions (weight %). The
calculated level of the
free LAS monomers in a 2069 ppm aqueous solution according to the Calculation
Method of
Free LAS Monomer as described above is listed for each composition.
Table 4
3A 3B
CH-Cu LAS 1.9 6.0
C12-C14AE1_35 11.3 9.0
Neodol 25-7 a 1.2 7.0
Citric acid 1.4 1.7
C12-C18 fatty acid 1.2 1.7
Chelant b 0.2 0
1, 2 propanediol 1.2 1.2
Tri ethanol amine 0 1.3
NaOH 2.5 2.0
Dye 0.002 0.002
Perfume 0.5 0.5
Add to Add to
Water
100 100
Free LAS monomer
40
(PPm)
a Neodol 25-7 is C12-C115 alcohol ethoxylated with 7 moles of ethylene oxide
as a nonionic surfactant,
15 available from Shell
b diethylene triamine penta acetate

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23
Preparation of the composition of Comparative Example 3A
The composition of Comparative Example 3A is prepared by the following steps:
a) mixing a combination of NaOH, 1, 2 propanediol, and water in a mixer by
applying a
shear of 200 rpm;
b) adding Citric acid, Neodol 25-7, and Chelant in sequence into the
combination obtained
in step a), keeping on mixing by applying a shear of 200 rpm;
c) increasing the mixing shear to 250 rpm, and maintaining the temperature of
the
combination obtained in step b) to be under 45 C;
d) mixing the combination obtained in step c) with LAS by applying a shear of
250 rpm;
e) once the temperature of the combination obtained in step d) is below 35 C,
adding AES
into the combination and mixing by applying a shear of 250 rpm until the
combination is
homogeneously mixed;
f) adding C12-C18 fatty acid into the combination obtained in step e), keeping
on mixing by
applying a shear of 250 rpm for 5 minutes;
g) adding Perfume and Dye into the combination obtained in step f), keeping on
mixing by
applying a shear of 250 rpm for 5 minutes, thus forming a liquid laundry
detergent
composition,
wherein in the composition, each ingredient is present in the amount as
specified for
Comparative Example 3A in Table 4.
Preparation of the composition of Comparative Example 3B
The composition of Comparative Example 3B is prepared by the following steps:
a) mixing a combination of NaOH, 1, 2 propanediol, Tri ethanol amine, and
water in a
mixer by applying a shear of 200 rpm;
b) adding Citric acid and Neodol 25-7 in sequence into the combination
obtained in step a),
keeping on mixing by applying a shear of 200 rpm;
c) increasing the mixing shear to 250 rpm, and maintaining the temperature of
the
combination obtained in step b) to be under 45 C;
d) mixing the combination obtained in step c) with LAS by applying a shear of
250 rpm;
e) once the temperature of the combination obtained in step d) is below 35 C,
adding AES
into the combination and mixing by applying a shear of 250 rpm until the
combination is
homogeneously mixed;

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24
f) adding C12-C18 fatty acid into the combination obtained in step e), keeping
on mixing by
applying a shear of 250 rpm for 5 minutes;
g) adding Perfume and Dye into the combination obtained in step f), keeping on
mixing by
applying a shear of 250 rpm for 5 minutes, thus forming a liquid laundry
detergent
composition,
wherein in the composition, each ingredient is present in the amount as
specified for
Comparative Example 3B in Table 4.
Comparative Data of Examples 2 and 3
Comparative experiments of measuring the anti-microbial efficacy of the
compositions of
Examples 2A - 2C and Comparative Examples 3A - 3B are conducted, according to
the QB/T
2738-2005 method as described herein above. The experimental results are shown
in Table 5.
Table 5
Example Free LAS monomer (ppm) Bacteria Killing Rate (%)
2A 87 93
2B 93 96
2C 97 99
3A 20 -50
3B 40 21
As shown in Table 5, the laundry detergent compositions according to the
present invention
(Examples 2A, 2B, and 2C) demonstrate good anti-microbial efficacy, whereas
the comparative
compositions (Comparative Examples 3A and 3B) show poor anti-microbial
efficacy. Moreover,
for the laundry detergent compositions according to the present invention, the
degree of the anti-
microbial efficacy is correlated to the free LAS monomer level, i.e., a higher
level of free LAS
monomers in a laundry washing liquor leads to a higher Bacteria Killing Rate.
Data of Example 2D under varying temperature conditions
Experiments of measuring the anti-microbial efficacy of the composition of 2D
under
varying temperature conditions are conducted, according to the QB/T 2738-2005
method as
described herein above. The test temperatures in steps 2E to 2H (i.e., the
temperature of the
standard hard water contained in the exposure chamber) are set to be (25 1) C,
(35 1) C, and

CA 02894928 2015-06-12
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(60 1) C, respectively. The test temperature of control is the same as the
corresponding sample.
The experimental results are shown in Table 6.
Table 6
Temperature Free LAS monomer (ppm) Bacteria Killing Rate (%)
25 C 60 33
35 C 60 72
60 C 60 84
5
As shown in Table 6, higher test temperatures (namely, 35 C and 60 C) enable a
lower level
of the free LAS monomers in a laundry washing liquor to achieve acceptable
anti-microbial
efficacy.
Unless otherwise indicated, all percentages, ratios, and proportions are
calculated based on
10
weight of the total composition. All temperatures are in degrees Celsius ( C)
unless otherwise
indicated. All measurements made are at 25 C, unless otherwise designated. All
component or
composition levels are in reference to the active level of that component or
composition, and are
exclusive of impurities, for example, residual solvents or by-products, which
may be present in
commercially available sources.
15
It should be understood that every maximum numerical limitation given
throughout this
specification includes every lower numerical limitation, as if such lower
numerical limitations
were expressly written herein. Every minimum numerical limitation given
throughout this
specification will include every higher numerical limitation, as if such
higher numerical
limitations were expressly written herein. Every numerical range given
throughout this
20
specification will include every narrower numerical range that falls within
such broader
numerical range, as if such narrower numerical ranges were all expressly
written herein.
The dimensions and values disclosed herein are not to be understood as being
strictly
limited to the exact numerical values recited. Instead, unless otherwise
specified, each such
dimension is intended to mean both the recited value and a functionally
equivalent range
25
surrounding that value. For example, a dimension disclosed as "40 mm" is
intended to mean
"about 40 mm."
Every document cited herein, including any cross referenced or related patent
or application,
is hereby incorporated herein by reference in its entirety unless expressly
excluded or otherwise
limited. The citation of any document is not an admission that it is prior art
with respect to any

CA 02894928 2015-06-12
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26
invention disclosed or claimed herein or that it alone, or in any combination
with any other
reference or references, teaches, suggests or discloses any such invention.
Further, to the extent
that any meaning or definition of a term in this document conflicts with any
meaning or
definition of the same term in a document incorporated by reference, the
meaning or definition
assigned to that term in this document shall govern.
While particular embodiments of the present invention have been illustrated
and described,
it would be obvious to those skilled in the art that various other changes and
modifications can be
made without departing from the spirit and scope of the invention. It is
therefore intended to
cover in the appended claims all such changes and modifications that are
within the scope of this
invention.

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Administrative Status

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Administrative Status

Title Date
Forecasted Issue Date Unavailable
(86) PCT Filing Date 2012-12-13
(87) PCT Publication Date 2014-06-19
(85) National Entry 2015-06-12
Examination Requested 2015-06-12
Dead Application 2018-12-13

Abandonment History

Abandonment Date Reason Reinstatement Date
2017-12-13 FAILURE TO PAY APPLICATION MAINTENANCE FEE
2018-02-28 R30(2) - Failure to Respond

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Request for Examination $800.00 2015-06-12
Registration of a document - section 124 $100.00 2015-06-12
Application Fee $400.00 2015-06-12
Maintenance Fee - Application - New Act 2 2014-12-15 $100.00 2015-06-12
Maintenance Fee - Application - New Act 3 2015-12-14 $100.00 2015-12-02
Maintenance Fee - Application - New Act 4 2016-12-13 $100.00 2016-11-29
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
THE PROCTER & GAMBLE COMPANY
Past Owners on Record
None
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Abstract 2015-06-12 1 59
Claims 2015-06-12 3 125
Description 2015-06-12 26 1,268
Cover Page 2015-08-03 1 29
Amendment 2017-05-10 15 690
Description 2017-05-10 26 1,210
Claims 2017-05-10 4 152
Examiner Requisition 2017-08-28 4 260
Patent Cooperation Treaty (PCT) 2015-06-12 4 206
International Preliminary Report Received 2015-06-12 5 199
International Search Report 2015-06-12 3 72
National Entry Request 2015-06-12 9 322
Examiner Requisition 2016-11-08 3 206