Note: Descriptions are shown in the official language in which they were submitted.
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BLEACHING COMPOSITIONS
Technical field
The pres~. ~l invention relates to stable peroxygen bleach-containing
co..-~,osilio.-s particularly suitable to be used as pr~l,ed~er.
Background
Peroxygen bleach-containing compositions have been extensively
described in laundry applications as laundry detergen~s, laundry
additives or evsn laundry pretrea~er~.
15 Indeed, it is known to use liquid CGI..pOSiliG..s co.--"r;sing a peroxygen
bleach and a bleach activator in laundry p(~l~eal,.,ent applications.
Although said liquid bleaching co~.posilions providc good bleaching
pe.rGr---ance when used to pr~lreat a soiled fabric, there is still some
room to further improve them regarding for example the stains/soils
20 removal performance 'elivereJ when prel.edli..g said soiled fabric.
It is thus an aspectof the present inventiGn to provide improved stain
rem~Dval p~rformance on a variety of stains/soils under prel(ea~ e,)t
cDnditions, i.c., when ap~lis~ directly onto the soiled fabrics, and left t
25 act onto said fabrics before washing said fabrics. More particularly, it is
an aspect of the ~r~s~-t invent;a.. to provide liquid compositions
containing a peroxygen bleach and a liquid h ydrophobic bleach
activator, which deliver improved stain removal "crror---ance on a
varhty of stains/soils under pretreat. . .ent conditions while not
3 0 CG. ~ ~pn:~- n;si- ~~ on their bleaching per ror- ~ ~ance.
It has now been found that the above aspect can be met by using a
liquid co.l-posit.Dn co~ risi--g a polyhydroxy fatty acid amid~ surfactant
to prelr~at soiled tabrics. Indeed, it has been found that the addition of
35 a polyhydroxy fatty acid amide surfactant, as defined hereinafter, in a
liquid cc,~ osiliO--, e.g., in a liquid co,--posilion comprising a peroxygen
bleach and optionally a liquid hydrophobic bleach activator, allows tO
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deliver improved stain removal performance on fabrics under
pretreatment conditions, as compared to the stain removal performance
delivered by the same composition without said polyhydroxy fatty acid
amide surfactant, or to the same composition but with another
surfactant like for instance a nonionic ethoxylated surfactant (C14-C1s
7E0) instead of said polyhydroxy fatty acid amide surfactant. Thus, in
its broadest aspect, the present invention encompasses the use of said
polyhydroxy fatty acid amide surfactant, in a liquid composition, for
improving the stain removal performance of said composition under
pretreatment conditions, on a variety of stains. The present invention
also er.co,.,passes liquid compositions comprising said polyhydroxy fatty
acid amide surfactant, a peroxygen-bleach and a liquid hydrophobic
bleach activator. Indeed, it has further been found that the addition of
said polyhydroxy fatty acid amide surfactants, in the liquid peroxygen
bleach-containing compositions of the present invention comprising said
liquid hydrophobic bleach activator, contributes to emulsify said
hydrophobic bleach activator so that said compositions are formulated
either as microemulsions or as emulsions. Thus, the compositions
according to the present invention allow to provide improved stain
removal performance when pretreating soiled fabrics while exhibiting
also excellent chemical stability, even upon prolonged storage periods.
An advantage of the present invention is that the improved stain
removal performance obtained when pretreating fabrics with the
compositions of the present invention is noticeable on a variety of
stains/soils including greasy/oil stains, like make-up, lipstick, dirty motor
oil and mineral oil, greasy food like mayonnaise and spaghetti sauce,
bleachable stains like tea and enzymatic stains like blood and grass.
EP-A- 598 170 discloses an emulsion comprising hydrogen peroxide or a
source thereof, a hydrophobic liquid ingredient and an emulsifying
system comprising two nonionic surfactants with different HLB
(hydrophilic lipophilic balance). No polyhydroxy fatty acid amide
surfactants are disclosed.
Co-pending European patent application number 95203330.6 discloses
a liquid bleaching composition comprising hydrogen peroxide, a liquid
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hydrophobic bleach activator, said composition being formulated as a
microemulsion of said hydrophobic liquid bleach activator in a matrix
o comprising water, said hydrogen peroxide, a hydrophilic surfactant
system comprising a nonionic surfactant and an anionic surfactant. No
polyhydroxy fatty acid amide surfactants are disclosed.
Summarv of the invention
The present invention encompasses a liquid composition comprising a
peroxygen bleach, a liquid hydrophobic bleach activator and a
polyhydroxy fatty acid amide surfactant according to the formula
R2 - C(O) - N(R1) Z
wherein R1 is H, or C1 C4 alkyl, C1 C4 hydrocarbyl, 2-hydroxy ethyl, 2-
hydroxy propyl or a mixture thereof, R2 is Cs C31 hydrocarbyl, and Z is
a polyhydroxyhydrocarbyl having a linear hydrocarbyl chain with at least
3 hydroxyls directly connected to the chain, or an alkoxylated derivative
thereof, said composition beirlg formulated either as a microemulsion or
as an emulsion.
The present invention also encompasses a process of pretreating soiled
fabrics with a liquid composition comprising a polyhydroxy fatty acid
amide surfactant according to the formula
R2 C(O) - N(R1 ) - Z,
wherein R1 is H, or C1 C4 alkyl, C1 C4 hydrocarbyl, 2-hydroxy ethyl, 2-
hydroxy propyl or a mixture thereof, R2 is Cs C31 hydrocarbyl, and Z is
a polyhydroxyhydrocarbyl having a linear hydrocarbyl chain with at least
3 hydroxyls directly connected to the chain, or an alkoxylated derivative
thereof, said process comprising the steps of applying said composition
in its neat form onto the fabric and allowing said composition to remain
in contact with said fabric, before said fabric is washed.
The present invention further encompasses the use of a polyhydroxy
fatty acid amide surfactant according to the formula
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R2 C(O) - N(R1) Z
wherein R1 is H, or C1 C4 alkyl, C1 C4 hydrocarbyl, 2-hydroxy ethyl, 2-
hydroxy propyl or a mixture thereof, R2 is Cs C31 hydrocarbyl, and Z is
a polyhydroxyhydrocarbyl having a linear hydrocarbyl chain with at least
3 hydroxyls directly connected to the chain, or an alkoxylated derivative
thereof, in a liquid composition, preferably in a liquid peroxygen bleach-
containing composition, for improving the stain removal performance of
said composition under prel,edL~,ent conditions, i.e., when pretreating a
soiled fabric with said composition before said fabric is washed.
Detailed descrintion of the invention
As an essential element the compositions of the present invention
comprise a peroxygen bleach. Preferred peroxygen bleach is hydrogen
peroxide, or a water soluble source thereof, or mixtures thereof.
Hydrogen peroxide is most preferred to be used in the compositions of
the present invention. Indeed, the presence of peroxygen bleach,
preferably hydrogen peroxide, provides strong cleaning benefits which
are particularly noticeable in laundry applications. As used herein a
hydrogen peroxide source refers to any compound which produces
hydrogen peroxide when said compound is in contact with water.
Suitable water-soluble sources of hydrogen peroxide for use herein
include percarbonates, persilicate, persulphate such as monopersulfate,
perborates, peroxyacids such as diperoxydodecandioic acid ~DPDA),
magnesium perphtalic acid, perbenzoic and alkylperbenzoic acids, and
mixtures thereof.
Typically, the compositions of the present invention comprise from
0.01% to 20% by weight of the total composition of said peroxygen
bleach or mixtures thereof, preferably from 1% to 15 %, and most
preferably from 2% to 10%.
As another ingredient, the compositions of the present invention
comprise a liquid hydrophobic bleach activator or mixtures thereof. By
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"bleach activatorn, it is meant herein a compound which reacts with
hydrogen peroxide to form a peracid. The peracid thus formed
constitutes the activated bleach. By "hydrophobic bleach activator", it
is meant herein a bleach activator which is not substantially and stably
miscible with water. Typically, such hydrophobic bleach activators
have a secondary HLB (hydrophilic lipophilic balance) below 11,
preferably below 10. Secondary HLB is known to those skilled in the
art and is defined for example in "Emulsions theory and practice" by P.
Becher, Reinhold, New York, 1957, or in "Emulsion science" by P.
Sherman, Academic Press, London, 1969.
Suitable hydrophobic bleach activators to be used herein include those
belonging to the class of esters, amides, imides, or anhydrides.
Examples of suitable compounds of this type are disclosed in British
Patent GB 1 586 769 and GB 2 143 231 and a method for their
formation into a prilled form is described in European Published Patent
Application EP-A-62 523. Suitable examples of such compounds to be
used herein are tetracetyl ethylene diamine (TAED), sodium 3,5,5
~ "elhyl hexanoyloxybenzene sulphonate, diperoxy dodecanoic acid as
described for instance in US 4 818 425 and nonylamide of peroxyadipic
acid as described for instance in US 4 259 201 and n-
nonanoyloxybenzenesulphonate (NOBS). Also suitable are N-acyl
caprolactams selected from the group consisting of substituted or
unsubstituted benzoyl caprolactam, octanoyl caprolactam, nonanoyl
caprolactam, hexanoyl caprolactam, decanoyl caprolactam, undecenoyl
caprolactam, formyl caprolactam, acetyl caprolactam, propanoyl
caprolactam, butanoyl caprolactam pentanoyl caprolactam or mixtures
thereof. A particular family of bleach activators of interest was
disclosed in EP 624 154, and particularly preferred in that family is
acetyl triethyl citrate (ATC). Acetyl triethyl citrate has the advantage
that it is environmentally friendly as it eventually degrades into citric
acid and alcohol. Furthermore, acetyl triethyl citrate has a good
hydrolytical stability in the product upon storage and it is an efficient
bleach activator. Finally, it provides good building capacity to the
composition.
The compositions according to the present invention comprise from
0.1 % to 20% by weight of the total composition of said liquid
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hydrophobic bleach activator, or mixtures thereof, preferably from 1%
to 10%, and more preferably from 1.5% to 7%.
As another essential ingredient, the compositions of the present
invention comprise a polyhydroxy fatty acid amide surfactant, or
mixtures thereof, according to the formula
R2 C(O) - N(R 1 ) - Z
wherein R1 is H, or C1 C4 alkyl, C1 C4 hydrocarbyl, 2-hydroxy ethyl, 2-
hydroxy propyl or a mixture thereof, R2 j5 Cs C31 hydrocarbyl, and Z is
a polyhydroxyhydrocarbyl having a linear hydrocarbyl chain with at least
3 hydroxyls directly connected to the chain, or an alkoxylated derivative
thereof.
Preferably, R1 is C1 C4 alkyl, more preferably C1 or C2 alkyl and most
preferably methyl, R2 is a straight chain C7 C1g alkyl or alkenyl,
preferably a straight chain Cg C1g alkyl or alkenyl, more preferably a
straight chain C11 C1g alkyl or alkenyl, and most preferably a straight
chain C11 C14 alkyl or alkenyl, or mixtures thereof. Z preferably will be
derived from a reducing sugar in a reductive amination reaction; more
preferably Z is a glycityl. Suitable reducing sugars include glucose,
fructose, maltose, lactose, galactose, mannose and xylose. As raw
materials, high dextrose corn syrup, high fructose corn syrup, and high
",allose corn syrup can be utilised as well as the individual sugars listed
above. These corn syrups may yield a mix of sugar components for Z.
It should be understood that it is by no means intended to exclude other
suitable raw materials. Z prt:ferably will be selected from the group
consisting of -CH2-(CHOH)n-CH20H, -CH(CH20H)-(CHOH)n 1-CH20H, -
CH2-(CHOH)2-(CHOR')(CHOH)-CH20H, where n is an integer from 3 to
5, inclusive, and R' is H or a cyclic or aliphatic monosaccharide, and
alkoxylated derivatives thereof. Most preferred are glycityls wherein n
is 4, particularly CH2-(CHOH)4-CH20H.
In formula R2 - C(O) - N(R1) - Z, R1 can be, for example, N-methyl, N-
ethyl, N-propyl, N-isopropyl, N-butyl, N-2-hydroxy ethyl, or N-2-hydroxy
propyl.
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R2 C(O) - N< can be, for example, cocamide, stearamide, oleamide,
Iauramide, myristamide, capricamide, palmitamide, tallowamide and the
like.
Z can be 1-deoxyglucityl, 2-deoxyfructityl, 1-deoxymaltityl, 1-
deoxylactityl, 1-deoxygalactityl, 1-deoxymannityl, 1-deoxymaltotriotityl
and the like.
Suitable polyhydroxy fatty acid amide surfactants to be used herein
may be commercially available under the trade name HOE~) from
Hoechst.
Methods for making polyhydroxy fatty acid amide surfactants are known
in the art. In general, they can be made by reacting an alkyl amine with
a reducing sugar in a reductive amination reaction to form a
corresponding N-alkyl polyhydroxyamine, and then reacting the N-alkyl
polyhydroxyamine with a fatty aliphatic ester or triglyceride in a
condensation/amidation step to form the N-alkyl, N-polyhydroxy fatty
acid amide product. Processes for making compositions containing
polyhydroxy fatty acid amides are disclosed for example in GB patent
specification 809,060, published February 18, 1959, by Thomas Hedley
& Co., Ltd., US patent 2,965,576, issued December 20, 1960 to E.R.
Wilson, US patent 2,703,798, Anthony M. Schwartz, issued March 8,
1955, US patent 1,985,424, issued December 25, 1934 to Pi990K and
W092/06070, each of which is incorporated herein by reference.
Typically, the compositions of the present invention comprise from
0.01 % to 30% by weight of the total composition of said polyhydroxy
fatty acid amide surfactants, or mixtures thereof, preferably from 0.1%
to 20%, and more preferably from 0.5% to 15%.
It has now been found that by adding said polyhydroxy fatty acid amide
surfactant in a liquid composition comprising a peroxygen bleach and a
liquid hydrophobic bleach activator, improved stain removal
performance is obtained with said composition when used to pretreat a
soiled fabric before said fabric is washed, as compared to the stain
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removal performance delivered with the same composition without said
polyhydroxy fatty acid amide surfactant, or to the same composition
with another hydrophilic surfactant like for instance nonionic
ethoxylated surfactant (C14/C15 7E0) instead of said polyhydroxy fatty
acid amide surfactant.
By "stain removal performance" it is meant herein stain removal
performance on a variety of stains/soils such as greasy/oily stains
and/or bleachable stains and/or enzymatic stains.
By "greasy/oily stains" it is meant herein any soil and stain of greasy
nature that can be found on a fabric like dirty motor oil, mineral oil,
make-up, lipstick vegetal oil, spaghetti sauce, mayonnaise and the like.
Examples of bleachable stains include tea, coffee, wine and the like.
Examples of enzymatic stains include grass, chocolate and blood.
The stain removal performance of a composition on a soiled fabric under
pretreatment conditions may be evaluated by the following test method.
A composition according to the present invention is first applied to a
fabric, preferably to the stained portion of said fabric, left to act from
about 1 to about 10 minutes, preferably 5 minutes, and said pretreated
fabric is then washed according to common washing conditions, at a
temperature of from 30~C to 70~C for a period of time sufficient to
bleach said fabric. The stain removal performance is then evaluated by
comparing side by side the soiled fabric pretreated with the composition
according to the present invention with those pretreated with the
reference, e.g. the same compositions but without any polyhydroxy
fatty acid amide surfactants according to the present invention. A
visual grading scale may be used to assign differences in panel score
units (psu), in a range from 0 to 4.
Actually, it has now been found that improved stain removal
performance, is achieved with said polyhydroxy fany acid amide
surfactants when contacting them directly to fabrics before
washing/rinsing them. Thus the stain removal performance associated to
said polyhydroxy fatty acid amide surfactants is not matrix dependent.
-
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Thus, in its broadest aspect, the present invention encompasses the use
of a polyhydroxy fatty acid amide surfactant as defined herein, in a
liquid composition, preferably in a peroxygen bleach-containing liquid
composition, for improving the stain removal performance of said
composition under pretreatment conditions, i.e., when prel-ealing a
soiled fabric with said composition before said fabric is washed.
The peroxygen bleach-containing compositions according to the present
invention comprise a liquid hydrophobic bleach activator and are thus
formulated either as aqueous emulsions of said liquid hydrophobic
bleach activator in a matrix comprising water, the peroxygen bleach and
an emulsifying surfactant system comprising said polyhydroxy fatty acid
amide surfactant (as a hydrophilic surfactant having an HLB above 10),
or as microemulsions of said liquid hydrophobic bleach activator in a
matrix comprising water, the peroxygen bleach and a hydrophilic
surfactant system comprising at least said polyhydroxy fatty acid amide
surfactant.
In the embodiment of the present invention where the peroxygen
bleach-containing compositions of the present invention are formulated
as aqueous emulsions, said polyhydroxy fatty acid amide surfactant
may be used, as sole emulsifying surfactant, to emulsify said
hydrophobic bleach activator. Accordingly, if said polyhydroxy fatty
acid amide surfactant is present in said emulsions as the sole
emulsifying surfactant, it is preferably present at a level of from 1% to
6% by weight of the total composition.
It has now been observed that the polyhydroxy fatty acid amide
surfactants as defined herein, even at low levels, allow to improve the
physical stability of the emulsions of the present invention, even at
c higher temperatures (up to 40~C), as compared to the physical stability
of the same compositions without said polyhydroxy fatty acid amide
surfactants. Thus, another aspect of the present invention is, the use of
a polyhydroxy fatty acid amide surfactant as defined herein, in a liquid
emulsion preferably comprising a peroxygen bleach, or a source thereof,
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and a liquid hydrophobic bleach activator, to improve the physical
stability of said emulsion.
Preferred peroxygen bleach-containing emulsions herein comprise an
emulsifying surfactant system of at least two different surfactants, i.e.
at least a hydrophobic surfactant having an HLB up to 9.5 or mixtures
thereof, and at least a hydrophilic surfactant having an HLB above 10,
or mixtures thereof, in order to emulsify the liquid hydrophobic bleach
activator. Plefer-ed herein, said two different surfactants should have
different HLB values (hydrophilic / lipophilic balance) in order to form
stable emulsions, and preferably the difference in value of the HLBs of
said two surfactants is at least 1, preferably at least 2. Indeed, by
appropriately combining at least two of said surfactants with different
HLBs in water, emulsions will be formed which do not subsLd,-Lially
separate into distinct layers, upon standing for at least two weeks at
40~C.
The prefe, ~ ecl emulsions according to the present invention comprise
from 1 % to 50 % by weight of the total composition of said
hydrophilic and hydrophobic surfactants, more preferably from 5 % to
40 % and most preferably from 8 % to 30 %. The preferred emulsions
according to the present invention comprise at least from 0.01 % by
weight of the total emulsion of said hydrophobic surfactant, or mixtures
thereof, preferably at least 2 % and more preferably at least 4 % and at
least from 0.01 % by weight of the total emulsion of said hydrophilic
surfactant, or mixtures thereof, preferably at least 2%, and more
preferably at least 4 %.
The hydrophilic surfactants having an HLB above 10 to be used in said
emulsions herein are said polyhydroxy fatty acid amide surfactants
alone or in mixture with other hydrophilic surfactants having an HLB
above 10, preferably hydrophilic nonionic surfactants having an HLB
above 10 and more preferably above 10.~. Preferred to be used herein
as the hydrophobic surfactants are the hydrophobic nonionic
surfactants. Said hydrophobic nonionic surfactants to be used herein
have an HLB up to 9.5, preferably below 9.5, more preferably below 9.
Indeed, the hydrophobic nonionic surfactants to be used herein have
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excellent grease cutting properties, i.e. they have a solvent effect which
contributes to hydrophobic soils removal. The hydrophobic surfactants
act as carrier of the hydrophobic brighteners onto the fabrics allowing
thereby said brighteners to work in close proximity with the fabrics
surface since the beginning of the wash.
Suitable nonionic surfactants for use herein include alkoxylated fatty
alcohols preferably, fatty alcohol ethoxylates and/or propoxylates.
Indeed, a great variety of such alkoxylated fatty alcohols are
commercially available which have very different HLB values
(hydrophilic / lipophilic balance). The HLB values of such alkoxylated
nonionic surfactants depend essentially on the chain length o~ the fatty
alcohol, the nature of the alkoxylation and the degree of alkoxylation.
Hydrophilic nonionic surfactants tend to have a high degree of
alkoxylation and a short chain fatty alcohol, while hydrophobic
surfactants tend to have a !ow degree of alkoxylation and a long chain
fatty alcohol. Surfactants catalogs are available which list a number of
surfactants including nonionics, together with their respective HLB
values.
Suitable chemical processes for preparing the nonionic surfactants for
use herein include condensation of corresponding alcohols with
alkylene oxide, in the desired proportions. Such processes are well-
known to the man skilled in the art and have been extensively
described in the art. As an alternative, a great variety of alkoxylated
alcohols suitable for use herein is commercially available frorn various
suppliers.
Preferred hydrophobic nonionic surfactants to be used in the emulsions
according to the present invention are surfactants having an HLB up to
9 and being according to the formula R~-(C2H4~)n(C3H6~)mH~
wherein R is a C6 to C22 alkyl chain or a C6 to C28 alkyl benzene
chain, and wherein n+m is from 0.5 to 5 and n is from O to 5 and m is
from O to 5 and preferably n+m is from 0.5 to 4.5 and, n and m are
from O to 4.5. The preferred R chains for use herein are the C8 to C22
alkyl chains. Accordingly, suitable hydrophobic nonionic surfactants
for use herein are Dobanol R 91-2.5 (HLB= 8.1; R is a mixture of Cg
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and C11 alkyl chains, n is 2.5 and m is O), or Lutensol R T03 (HLB=8;
R is a mixture of C13 and C1 s alkyl chains, n is 3 and m is O), or
Tergitol R 25L3 ~HLB= 7.7; R is in the range of C12 to C1s alkyl chain
length, n is 3 and m is O), or Dobanol R 23-3 (HLB=8.1; R is a mixture
of C12 and C13 alkyl chains, n is 3 and m is O), or Dobanol R 23-2
(HLB= 6.2; R is a mixture of C12 and C13 alkyl chains, n is 2 and m is
O), or mixtures thereof. Preferred herein are Dobanol R 23-3, or
Dobanol R 23-2, Lutensol R T03, or mixtures thereof. These Dobanol
R surfactants are commercially available from SHELL. These Lutensol
R surfactants are commercially available from BASF and these Tergitol
R surfactants are commercially available from UNION CARBIDE. Other
suitable hydrophobic nonionic surfactants to be used herein are non
alkoxylated surfactants. An example is Dobanol R 23 (HLBc3).
Preferred hydrophilic nonionic surfactants to be used in the emulsions
according to the present invention are surfactants having an HLB above
10 and being according to the formula R~-(C2H4~)n(C3H6~)mH~
wherein R is a C6 to C22 alkyl chain or a C6 to C2g alkyl benzene chain,
and wherein n + m is from 5 to 11 and n is from O to 11 and m is from O
to 11, preferably n+m is from 6 to 10 and, n and m are from O to 10.
Throughout this description n and m refer to the average degree of the
ethoxylation/propoxylation. The preferred R chains for use herein are the
C8 to C22 alkyl chains. Accordingly, suitable hydrophilic nonionic
surfactants for use herein are Dobanol R 23-6.5 (HLB = 11.9 ; R is a
mixture ~f C12 and C13 alkyl chains, n is 6.5 and m is O), or Dobanol R
25-7 (HLB= 12; R is a mixture of C12 to C1s alkyl chains, n is 7 and m
is O), or Dobanol R 45 7 (HLB=11.6; R is a mixture of C14 and C1s
alkyl chains, n is 7 and m is O), or Dobanol R 91-5 (HLB=11.6; R is a
mixture of Cg to C11 alkyl chains, n is 5 and m is O), or Dobanol R 91-6
(HLB= 12.5; R is a mixture of Cg to C11 alkyl chains, n is 6 and m is O),
or Dobanol R 91-8 (HLB=13.7; R is a mixture of Cg to C11 alkyl chains,
n is 8 and m is O), or Dobanol R 91-10 (HLB= 14.2; R is a mixture of
Cg to C11 alkyl chains, n is 10 and m is O), or mixtures thereof.
Rlerer.ed herein are Dobanol R 91-10, or Dobanol R 45 7, Dobanol R
23-6.5, or mixtures thereof. These Dobanol R surfactants are
commercially available from SHELL. Apart from the hydrophilic nonionic
surfactants other hydrophilic surfactants may further be used in the
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emulsions of the present invention such as anionic surfactants described
hereinafter.
The emulsions according to the present invention may further comprise
other surfactants on top of said polyhydroxy fatty acid amide surfactant
alone or in an emulsifying system further comprising hydrophobic
surfactants and optional other hydrophilic surfactants, which should
however not significantly alter the weighted average HLB value of the
overall emulsion.
In a particularly preferred embodiment of the emulsions of the present
invention, wherein the emulsions comprise acetyl triethyl citrate as the
bleach activator, an adequate nonionic emulsifying surfactant system on
top of said polyhydroxy faKy acid amide surfactant, would comprise a
hydrophobic nonionic surfactant with for instance an HLB of 6, such as
a Dobanol R 23-2 and a hydrophilic nonionic surfactant with for
instance an HLB of 15, such as a Dobanol R 91-10. Other suitable
nonionic surfactant systems comprise for example a Dobanol R 23-6.5
(HLB about 12) and a Dobanol R 23 (HLB below 6) or a Dobanol R 45 7
(HLB=11.6) and a Dobanol 23-3 (HLB=8.1).
The preferred making of the preferred emulsions of the present
invention, which comprise a liquid hydrophobic bleach activator,
includes: (i) premixing the hydrophobic surfactants with the bleach
activator and other non-water miscible ingredients if present; (ii)
premixing the hydrophilic surfactants (i.e. said polyhydroxy fatty acid
amide surfactants with optional other hydrophilic surfactants like
hydrophilic nonionic surfactants) with water and subsequently adding
the other water soluble ingredients if present; (iii) trimming the pH to
preferred value; (iv) including a peroxygen bleach, e.g., hydrogen
peroxide, and the hydrophobic phase prepared in step (i). It is important
that during the mixing of the two phases, the emulsions be constantly
kept under stirring under relatively low stirring energies, preferably 30
minutes at 550 rpm, most preferably 30 minutes at 450 rpm.
In the embodiment of the present invention where the compositions are
formulated as emulsions said compositions are opaques. In
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centrifugation examination, it was observed that said emulsions herein
showed no phase separation after 15 minutes at 6000 rpm. Under
microscopic examination, said emulsions appeared as a dispersion of
droplets in a matrix.
In the embodiment of the ,~resent invention where the peroxygen
bleach-containing compositions of the present invention are formulated
as microemulsions, said peroxygen bleach-containing microemulsions
according to the present invention comprise a hydrophilic surfactant
system comprising said polyhydroxy fatty acid amide surfactant.
Accordingly, if said polyhydroxy fatty acid amide surfactant is present
in said microemulsions as the sole emulsifying surfactant, it is preferably
present at a level of more than 6% of the total composition up to 15%.
A key factor in order to stably incorporate the hydrophobic bleach
activator is that said polyhydroxy fatty acid amide surfactant has a
different HLB value to that of the hydrophobic activator.
It has now been observed that the polyhydroxy fatty acid amide
surfactants as defined herein, even at low levels, allow to improve the
physical stability of the microemulsions of the present invention, even at
higher temperatures (up to 40~C), as compared to the physical stability
of the same compositions without said polyhydroxy fatty acid amide
surfactants. Thus, another aspect of the present invention is, the use of
a polyhydroxy fatty acid amide surfactant as defined herein, in a liquid
microemulsion preferably comprising a peroxygen bleach, or a source
thereof, and a liquid hydrophobic bleach activator, to improve the
physical stability of said microemulsion.
The hydrophilic surfactant system emulsifying said hydrophobic bleach
activator in the microemulsions of the present invention may further
comprise other hydrophilic surfactants like other nonionic hydrophilic
surfactants andlor anionic surfactants. A key factor in order to stably
incorporate the hydrophobic activator in said microemulsions is that at
least one of said surfactants of the hydrophilic surfactant system must
have a different HLB value to that of the hydrophobic activator. Indeed,
if all said surfactants had the same HLB value as that of the hydrophobic
activator, a continuous single phase might be formed, thus lowering the
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chemical stability of the bleach/bleach activator system. Preferably, at
least one of said surfactants has an HLB value which differs by at least
1.0 HLB unit, preferably 2.0 to that of said bleach activator.
- Suitable anionic surfactants to be further added in the compositions
herein include water soluble salts or acids of the formula ROS03M
wherein R preferably is a C10-C24 hydrocarbyl, preferably an alkyl or
hydroxyalkyl having a C1 0-c20 alkyl component, more preferably a
C12-C1g alkyl or hydroxyalkyl, and M is H or a cation, e.g., an alkali
metal cation (e.g., sodium, potassium, lithium~, or ammonium or
substituted ammonium (e.g., methyl-, dimethyl-, and trimethyl
ammonium cations and quaternary ammonium cations, such as
tetramethyl-ammonium and dimethyl piperdinium cations and quaternary
ammonium cations derived from alkylamines such as ethylamine,
diethylamine, triethylamine, and mixtures thereof, and the like).
Typically, alkyl chains of C12-16 are preferred for lower wash
temperatures (e.g., below about 50~C) and C1 6-18 alkyl chains are
preferred for higher wash temperatures (e.g., above about 50~C).
Other suitable anionic surfactants for use herein are water soluble salts
or acids of the formula RO(A)mS03M wherein R is an unsubstituted
C10-C24 alkyl or hydroxyalkyl group having a C1o-C24 alkyl
component, preferably a C12-C20 alkyl or hydroxyalkyl, more preferably
C1 2-C1 8 alkyl or hydroxyalkyl, A is an ethoxy or propoxy unit, m is
greater than zero, typically between about 0.5 and about 6, more
preferably between about 0.5 and about 3, and M is H or a ca~ion which
can be, for example, a metal cation (e.g., sodium, potassiurn, lithium,
calcium, magnesium, etc.), ammonium or substituted-ammonium cation.
Alkyl ethoxylated sulfates as well as alkyl propoxylated sulfates are
contemplated herein. Specific examples of substituted ammonium
cations include methyl-, dimethyl-, trimethyl-ammonium and quaternary
ammonium cations, such as tetramethyl-ammonium, dimethyl
piperdinium and cations derived from alkanolamines such as ethylamine,
diethylamine, triethylamine, mixtures thereof, and the like. Exemplary
surfactants are C1 2-C1 8 alkyl polyethoxylate (1.0) sulfate, C1 2-
C1 gE(1 .O)M), C1 2-C18 alkyl polyethoxylate (2.25) sulfate, C1 2-
C1 gE(2.25)M), C1 2-C1 8 alkyl polyethoxylate (3.0) sulfate C1 2-
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16
C1 8E(3-0), and C1 2-C1 8 alkyl polyethoxylate (4.0) sulfate C1 2-
C1 gE(4.0)M), wherein M is conveniently selected from sodium and
potassium .
Other anionic surfactants useful for detersive purposes can also be used
herein. These can include salts (including, for example, sodium,
potassium, ammonium, and substituted ammonium salts such as mono-,
di- and triethanolamine salts) of soap, Cg-C20 linear
alkylbenzenesulfonates, Cg-C22 primary or secondary alkanesulfonates,
Cg-C24 olefinsulfonates, sulfonated polycarboxylic acids prepared by
sulfonation of the pyrolyzed product of alkaline earth metal citrates,
e.g., as described in British patent specification No. 1,082,179, Cg-C24
alkylpolyglycolethersulfates (containing up to 10 moles of ethylene
oxide); alkyl ester sulfonates such as C14-16 methyl ester sulfonates;
acyl glycerol sulfonates, fatty oleyl glycerol sulfates, alkyl phenol
ethylene oxide ether sulfa~es, paraffin sulfonates, alkyl phosphates,
isethionates such as the acyl isethionates, N-acyl taurates, alkyl
succinamates and sulfosuccinates, monoesters of sulfosuccinate
(especially saturated and unsaturated C12-C18 monoesters) diesters of
sulfosuccinate (especially saturated and unsaturated C6-C14 diesters),
sulfates of alkylpolysaccharides such as the sulfates of
alkylpolyglucoside (the nonionic nonsulfated compounds being described
below), branched primary alkyl sulfates, alkyl polyethoxy carboxylates
such as those of the formula RO(CH2CH20)kCH2COO-M~ wherein R is
a C8-C22 alkyl, k is an integer from 0 to 10, and M is a soluble salt-
forming cation. Resin acids and hydrogenated resin acids are also
suitable, such as rosin, hydrogenated rosin, and resin acids and
hydrogenated resin acids present in or derived from tall oil. Further
examples are given in ~Surface Active Agents and Detergents" (Vol. I
and ll by Schwartz, Perry and Berch). A variety of such surfactants are
also generally disclosed in U.S. Patent 3,929,678, issued December 30,
1975 to Laughlin, et al. at Column 23, line 58 through Column 29, line
23 (herein incorporated by reference).
Other suitable anionic surfactants to be used herein also include acyl
sarcosinate or mixtures thereof, in its acid and/or salt form, preferably
long chain acyl sarcosinates having the following formula:
-
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PCTrUS96/10906
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~,OM
CH3 0
-
wherein M is hydrogen or a cationic moiety and wherein R is an alkyl
group of from 1 1 to 15 carbon atoms, preferably of from 1 1 to 13
carbon atoms. Preferred M are hydrogen and alkali metal salts, especially
sodium and potassium. Said acyl sarcosinate surfactants are derived
from natural fatty acids and the amino-acid sarcosine (N-methyl glycine).
They are suitable to be used as aqueous solution of their salt or in their
acidic form as powder. Being derivatives of natural fatty acids, said acyl
sarcosinates are rapidly and completely biodegradable and have good
skin compatibility.
Accordingly, particularly preferred long chain acyl sarcosinates to be
used herein include C1 2 acyl sarcosinate (i.e. an acyl sarcosinate
according to the above formula wherein M is hydrogen and R is an alkyl
group of 11 carbon atoms) and C14 acyl sarcosinate (i.e. an acyl
sarcosinate according to the above formula wherein M is hydrogen and R
is an alkyl group of 13 carbon atoms). C1 2 acyl sarcosinate is
commercially available, for example, as Hamposyl L-30(~) supplied by
Hampshire. C14 acyl sarcosinate is commerc~ally available, for example,
as Hamposyl M-30~ supplied by Hampshire.
Suitable other nonionic surfactants for use in the microemulsions herein
include the hydrophilic nonionic surfactants as defined herein before for
the emulsions.
The preferred making of the microemulsions of the present invention
which comprises a liquid hydrophobic bleach activator includes
premixing the surfactants with water and subsequently adding the other
ingredients including the peroxygen bleach, e.g., hydrogen peroxide,
and said hydrophobic bleach activator. Irrespective of this preferred
order of addition, it is important that during the mixing of the
ingredients, the microemulsions be constantly kept under stirring under
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relatively high stirring energies, preferably 30 minutes at 750 rpm, most
preferably 30 minutes at 1000 rpm.
In the embodiment of the present invention where the compositions are
formulated as microemulsions said compositions are macroscopically
transparent in the absence of opacifiers and dyes. In centrifugation
examination, it was observed that said microemulsions herein showed
no phase separation after 15 minutes at 6000 rpm. Under microscopic
- examination, said microemulsions appeared as a dispersion of droplets
in a matrix. The matrix is the hydrophilic matrix described
hereinbefore, and the droplets are constituted by the liquid
hydrophobic bleach activator. We have observed that the particles had
a size which is typically around or below 3 micron diameter.
The peroxygen bleach-containing compositions of the present invention
formulated in the form of emulsions or microemulsions are chemically
stable. By "chemically stable" it is meant herein that said composition of
the present invention comprising a peroxygen bleach does not undergo
more than 10% available oxygen loss at 50~C in 2 weeks. The
concentration of available oxygen can be measured by chemical titration
methods known in the art, such as the iodimetric method, the
permanganometric method and the cerimetric method. Said methods
and the criteria for the choice of the appropriate method are described
for example in ~Hydrogen Peroxide", W. C. Schumb, C. N. Satterfield
and R. L. Wentworth, Reinhold Publishing Corporation, New York, 1955
and "Organic Peroxides", Daniel Swern, Editor Wiley Int. Science, 1970.
Alternatively, the stability of said compositions may also be evaluated
by a bulging test method.
Accordingly, said peroxygen bleach-containing compositions of the
present invention may be packaged in a given deformable
container/bottle without compromising the stability of said
container/bottle comprising it upon standing, for long periods of time.
The peroxygen-bleach containing compositions of the present invention
formulated either as an emulsion or as a microemulsion may further
comprise other surfactants known to those skilled in the art including
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cationic, zwitterionic and/or amphotheric surfactants. For example, the
peroxygen bleach-containing compositions of the present invention may
further comprise an amine oxide surfactant according to the formula
RlR2R3NO, wherein each of R1, R2 and R3 is independently a C1-C30,
- preferably a C1-C20, most preferably a C1 -C1 6 hydrocarbon chain.
Indeed, we have observed that improved chemical stability, i.e., lower
decomposition of the bleach and the bleach activator is obtained by
adding such an amine oxide. It is believed that such stability is due to
the capacity of the amine-oxide to limit interactions between the bleach
and the bleach activator possibly through emulsification. It is believed
that this stabilising effect is matrix independent. Amine oxides may be
preferably present in amounts up to 10 % by weight of the total
composition, more preferably from 1% to 3%.
The compositions according to the present invention are aqueous liquid
cleaning compositions. Said aqueous compositions should be formulated
in the acidic pH up to the neutral pH(pH=7~, preferably at a pH of from
O to 6, more preferably at a pH of from 1 to 6, and most preferably of
from 1 to 5. Formulating the compositions of the present invention in
the acidic pH range contributes to the stability of said compositions. The
pH of the compositions of the present invention can be adjusted by using
organic or inorganic acids, or alkalinising agents.
The compositions of the present invention may further comprise optional
ingredients like stabilisers, chelating agents, radical scavengers, builders,
soil suspenders, dye transfer agents, solvents, brighteners, perfumes,
foam suppressors or dyes or mixtures thereof.
The peroxygen bleach-containing compositions of the present invention
may comprise a chelating agent or mixtures thereof, as a highly preferred
optional ingredient. Chelating agents suitable to be used herein include
chelating agents selected from the group of phosphonate chelating
agents, amino carboxylate chelating agents, polyfunctionally-substituted
aromatic chelating agents, and further chelating agents like glycine,
salicylic acid, aspartic acid, glutamic acid, malonic acid, or mixtures
thereof. Chelating agents when used, are typically present herein in
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amounts ranging from 0.001% to 5% by weight of the total composition
and preferably from 0.05% to 2% by weight.
Suitable phosphonate chelating agents to be used herein may include
ethydronic acid as well as amino phosphonate compounds, including
amino alkylene poly (alkylene phosphonate), alkali metal ethane 1-
hydroxy diphosphonates, nitrilo trimethylene phosphonates, ethylene
diamine tetra methylene phosphonates, and diethylene triamine penta
methylene phosphonates. The phosphonate compounds may be present
either in their acid form or as salts of different cations on some or all of
their acid functionalities. Preferred phosphonate chelating agents to be
used herein are diethylene triamine penta methylene phosphonates.
Such phosphonate chelating agents are commercially available from
Monsanto under the trade name DEQUEST~)-
Polyfunctionally-substituted aromatic chelating agents may also be
useful in the compositions herein. See U.S. patent 3,812,044, issued
May 21, 1974, to Connor et al. Preferred compounds of this type in
acid form are dihydroxydisulfobenzenes such as 1,2-dihydroxy -3,5-
disulfobenzene.
A preferred biodegradable chelating agent for use herein is ethylene
diamine N,N'- disuccinic acid, or alkali metai, or alkaline earth,
ammonium or substitutes ammonium salts thereof or mixtures thereof.
Ethylenediamine N,N'- disuccinic acids, especially the (S,S) isomer have
been extensively described in US patent 4, 704, 233, November 3,
1987, to Hartman and Perkins. Ethylenediamine N,N'- disuccinic acids is,
for instance, commercially available under the tradename ssEDDS(~) from
Palmer Research Laboratories.
Suitable amino carboxylates to be used herein include ethylene diamine
tetra acetates, diethylene triamine pentaace~aLes, diethylene triamine
pentaacetate (DTPA),N- hydroxyethylethylenediamine triacetates,
nitrilotri-acetates, ethylenediamine tetrapropionates,
triethylenetetraaminehexa-acetates, ethanol-diglycines, propylene
diamine tetracetic acid (PDTA) and methyl glycine di-acetic acid
(MGDA), both in their acid form, or in their alkali metal, ammonium, and
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substituted ammonium salt forms. Particularly suitable amino
carboxylates to be used herein are diethylene triamine penta acetic acid,
propylene diamine tetracetic acid (PDTA) which is, for instance,
commercially available from BASF under the trade name Trilon FS(~) and
methyl glycine di-acetic acid (MGDA).
Particularly preferred chelating agents to be used herein are diethylene
triamine methylene phosphonate, ethylene N,N'-disuccinic acid,
diethylene triamine pantaacetate, glycine, salicylic acid, aspartic acid,
glutamic acid, malonic acid or mixtures thereof and highly preferred is
salicylic acid. Salicylic acid may be commercially available from Rhone-
Poulenc under the name Salicylic Acid~.
The peroxygen bleach-containing compositions of the present invention
may further comprise a radical scavenger, or mixtures thereof, as a
highly preferred optional ingredient. Suitable radical scavengers for use
herein include the well-known substituted mono and dihydroxy benzenes
and their analogs, alkyl and aryl carboxylates and mixtures thereof.
Preferred such radical scavengers for use herein include di-tert-butyl
hydroxy toluene (BHT), hydroquinone, di-tert-butyl hydroquinone, mono-
tert-butyl hydroquinone, tert-butyl-hydroxy anysole, benzoic acid, toluic
acid, catechol, t-butyl catechol, benzylamine, 1,1,3-tris~2-methyl-4-
hydroxy-5-t-butylphenyl) butane, n-propyl-gallate or mixtures thereof and
highly preferred is di-tert-butyl hydroxy toluene. Radical scavengers
when used, are typically present herein in amounts ranging from 0.001%
to 2% by weight of the total composition and preferably from 0.001% to
0.5% by weight.
The presence of chelating agents and/or radical scavengers allows to
provide compositions that are particularly safe to the fabrics treated
therewith and to the color, even when used for pretreating a soiled fabric
upon prolonged contact times before washing said fabric.
The peroxygen bleach-containing compositions of the present invention
may further comprise up to 10%, preferably from 2% to 4% by weight
of the total composition of an alcohol according to the formula HO -
CR'R" - OH, wherein R' and R" are independently H or a C2-C1o
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hydrocarbon chain and/or cycle. Preferred alcohol according to that
formula is propanediol. Indeed, we have observed that these alcohols in
general and propanediol in particular also improve the chemical stability
of the compositions, i.e. Iower the decomposition of the bleach and the
bleach activator, as the amine oxides herein above. In addition, said
alcohols lower the surface tension of the product, thus preventing
superficial film or gel formation. Thus, said alcohols improve the
aesthetics of the compositions herein. It is believed that the chemical
stabilising effect of said alcohols is twofold. Firstly, they may v~~ork as
radical scavengers and secondly, they may interact with the hydrogen
peroxide preventing or limiting hydrolysis, therefore reducing the rate of
peroxide decomposition. It is believed that this improvement in chemical
stability obtained by said alcohols is matrix independent.
The peroxygen bleach-containing compositions according to the present
invention may further comprise a foam suppressor such as 2-alkyl
alkanol, or mixtures thereof, as an optional ingredient. Particularly
suitable to be used in the present invention are the 2-alkyl alkanols
having an alkyl chain comprising from 6 to 16 carbon atoms, preferably
from 8 to 12 and a terminal hydroxy group, said alkyl chain being
substituted in the a position by an alkyl chain comprising from 1 to 10
carbon atoms, preferably from 2 to 8 and more preferably 3 to 6. Such
suitable compounds are commercially available, for instance, in the
Isofol~) series such as Isofol(~) 12 (2-butyl octanol) or Isofol~3) 16 (2-
hexyl decanol). Typically, the compositions of the present invention
comprise up to 2 % by weight of the total composition of a 2-alkyl
alkanol, or mixtures thereof, preferably from 0.05 % to 1.5 % and more
preferably from 0.1 % to 0.8 %.
Although the prefer.ed application of the compositions described herein
is laundry pretreatment, the compositions according to the present
invention may also be used as a laundry detergent or as a laundry
detergent booster and as a household cleaner in the bathroom or in the
kitchen.
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The present invention further encompasses a process of prelrealing
soiled fabrics with a liquid composition comprising a polyhydroxy fatty
acid amide surfactant according to the formula
R2 C(O) - N(R1) z
wherein R1 is H, or C1 C4 alkyl, C1 C4 hydrocarbyl, 2-hydroxy ethyl, 2-
hydroxy propyl or a mixture thereof, R2 is C~ C31 hydrocarbyl, and Z is
a polyhydroxyhydrocarbyl having a linear hydrocarbyl chain with at least
3 hydroxyls directly connected to the chain, or an alkoxylated derivative
thereof, said process comprises the steps of applying said composition
in its neat form onto the fabric and allowing said composition to remain
in contact with said fabric preferably without leaving said composition
to dry onto said fabric, before said fabric is washed. Said composition
may remain in contact with said fabric, typically for a period of 1 minute
to several hours, preferably 1 minute to 1 hour, more preferably 1
minutes to 30 minutes, and most preferably 2 to 10 minutes.
Optionally, when the fabric is soiled with encrusted stains/soils which
otherwise would be relatively difficult to remove, said compositions may
be rubbed and/or brushed more or less intensively, for example, by
means of a sponge or a brush or simply by rubbing two pieces of fabric
each against the other. In the preferred process of prel-ealing soiled
fabrics herein the compositions according to the present invention are
used.
By "washing" it is to be understood herein to simply rinse the fabrics
with water, or the fabrics may be washed with conventional
compositions comprising at least one surface active agent, this by the
means of a washing machine or simply by hand.
By "in its neat form" it is to be understood that the liquid compositions
~ are applied directly onto the fabrics to be pre-treated without
undergoing any dilution, e.g., the compositions according to the present
invention are applied as described herein.
According to the process of pretreating soiled fabrics of the present
invention, the liquid compositions according to the present invention
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24
used in said process should preferably not be left to dry onto the
fabrics. Indeed, it has been found that water evaporation contributes to
increase the concentration of free radicals onto the surface of the
fabrics and, consequently, the rate of chain reaction. It is also
speculated that an auto-oxidation reaction occurs upon evaporation of
water when the liquid compositions are left to dry onto the fabrics.
Said reaction of auto-oxidation generates peroxy-radicals which may
contribute to the de~-adaLion of cellulose. Thus, not leaving said liquid
peroxygen bleach-containing compositions to dry onto the fabric, in the
process of prel~ealing soiled fabrics according to the present invention,
may reduce fabric damage what may otherwise result from prolonged
contact time between said fabrics and liquid peroxygen bleach-
containing compositions.
The present invention will be further illustrated by the followin~7Hbleach-
examples. 1 578YExamDles
The following compositions were made by mixing the listed ingredients
in the listed proportions (weight % unless otherwise specified).
Co".posilions I ll lll IV V Vl Vll
Alkyl Glucose Amide 4 2.0 2.0 3.0 12 3.0 3.0
Dobanol~ 45-7 - 6.4 6.4 6.4 - 6.0
Dobanol~9 23-3 - 8.6 8.6 8.6
Dobanol~ 23-6.5 - - - - - 6.0
C25-AE-2. 5-S - - 4.0 9 .0 - 6.0 6.0
ATC~ 3-5 3-5 3-5 3-5 3-5 3-5 3-5
H2~2 4.0 4.0 4.0 4.0 6.0 6.0 6.0
Water and minors up to 100~,C
H2504 up to pH 4
~ ATC is acetyl triethyl citrate.
Dobanol ~ 23-3 is a C12-C13 nonionic ethoxylated surfactant with HLB
of 8.1.
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Dobanol ~ 23-6.5 is a C12-C13 nonionic ethoxylated surfactant with
HLB of 11.9.
Dobanol (~ 45-7 is a C14-C15 nonionic ethoxylated surfactant with HLB
of 11.6.
Compositions I to IV are emuisions according to the present invention
and compositions V to Vll are microemulsions according to the present
invention. Excellent stain removal performance has been obtained on a
variety of stains including greasy/oily stains like dirty motor oil, make-
up, lipstick, spaghetti sauce, bleachable stains like tea and enzymatic
stains like grass, blood, when pretreating soiled fabrics with
compositions I to Vll, as described above, e.g., when leaving said
compositions to act onto the fabrics for a contact period of about 5
minutes, before washing said fabrics.
