Note: Descriptions are shown in the official language in which they were submitted.
' CA 02306376 2000-04-20
~Hand dishwashing detergent coataiaing
microcapsule8n
Field of the Invention
The invention relates to thickened aqueous surfactant-
containing compositions, in particular hand dishwashing
detergents, containing anionic surfactant, amphoteric
surfactant, polymer and microcapsules.
Background of the Invention
Attempts, using traditional means, to incorporate
certain active ingredients (inter alia additives which
improve the feel on the skin or care additives, such
as, for example, liposomes, proteins, vitamins, plant
extracts, etc.; performance-enhancing additives, such
as, for example, acetic acid, etc.; antibacterial
additives, such as, for example, lactic acid, benzoic
acid, etc.; aesthetics (in particular additives which
improve odor and appearance and tactile properties,
such as, for example, perfume oils, dyes, etc.)) in an
exactly dosable, excellently cleaning, skin-compatible,
temperature- and storage-stable, pourable and
ecologically particularly compatible hand dishwashing
detergent can - as a result of direct action of the
surfactant components on the active ingredient -
rapidly lead to losses in activity (e.g. in the case of
liposomes). Other problems include difficulties in
stably incorporating active ingredients into the
detergent formulation (e.g. in the case of perfumes or
antibacterial active ingredients), discolorations (e. g.
in the case of plant extracts or proteins), odor
problems (e. g. in the case of the addition of vinegar,
antibacterial active ingredients or plant extracts) or
incompatibilities between the active ingredient
component and the detergent.
An elegant method for incorporating sensitive,
chemically or physically incompatible, and volatile
ingredients consists in the use of microcapsules in
which these ingredients are included in storage- and
transportation-stable form, and from which they are
' CA 02306376 2000-04-20
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mechanically, chemically, thermally or enzymatically
released for or during use.
Microcapsules are finely disperse liquid or solid
phases coated with film-forming polymers, during the
preparation of which the polymers, following
emulsification and coacervation and interfacial
polymerization, deposit on the material (active
ingredient) to be coated. In the process, the active
ingredient is coated by a solid membrane in a type of
shell (microcapsule in the narrower sense) or is
enclosed by a matrix (microsphere or sphere). In 'the
text below, the term "microcapsule" is used for both
variants in the collective sense, or in some cases both
terms are placed one after the other. The
microscopically small capsules, also called nano-
capsules, can be dried like powders. In this way it is
possible, for example, to convert petroleum spirit,
water, alcohol, pharmaceuticals, solvents, vitamins,
enzymes, liquid crystals, food flavorings and perfumes
into a dry mass which cannot dry up. Microencapsulation
can be used, for example, for perfume powders which are
easier to handle and are effective for a longer period
than microcapsules.
German Laid-Open Specification DT 2 215 441 (Unilever
N.Y.) discloses aqueous liquid dishwashing detergents
containing 20 to 45% by weight of anionic and/or
nonionic surfactants, 3 to 10% by weight of electrolyte
and capsules having a diameter of 1 to 4000 ~m of the
polymers carrageenan, polyvinyl alcohol or cellulose
ethers, where the polymers and the electrolyte
concentration are chosen such that the stability of the
capsules in the composition and also dissolution of the
capsules upon dilution with water are ensured. Such a
dishwashing detergent comprises, for example, 10% by
weight of capsules having a diameter of 4000 Vim, 25% by
weight of sodium dodecylbenzenesulfonate, 5% by weight
of cocomonoethanolamide, 7% by weight of sodium
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sulfate, 1.5% by weight of synthetic clay, or 5% by
weight of capsules having a diameter of 4000 Etm, 20% by
weight of sodium alkylbenzenesulfonate, 5% by weight of
sodium Cla-ls-a-olefinsulfonate, 5% by weight of lauric
acid diethanolamide, 7% by weight of sodium
xylenesulfonate, 3% by weight of ethanol, 1% by weight
of potassium chloride, 1% by weight of synthetic clay
and 0.2% by weight of EDTA.
DE 36 15 514 A1 (Lion Corp.) discloses an, aqueous hand
dishwashing detergent containing 22% by weight of
sodium a-olefinsulfonate, 6% by weight of magnesium
alkylbenzenesulfonate, 2% by weight of sodium sulfate,
0.725% by weight of sodium chloride, 3% by weight of
ethanol, 0.5% by weight of fragrance and 1.5% by weight
of fragrance-containing microcapsules having a size of
from 200 to 500 Vim, which dissolve upon dilution with
water.
British Patent Specification 1 471 406 (Unilever Ltd. )
relates to liquid aqueous detergents which comprise at
least 2% by weight of triethanolamine lauryl sulfate
and a total of from 8 to 50% by weight of surfactant,
and 0.5 to 2% by weight of water-soluble crosslinked
polyacrylic acid having a molecular weight of more than
1,000,000 and 0.1 to 5% by weight of a suspended phase,
e.g. spheroidal capsules having a diameter of from 0.1
to 5 mm, and have a pH of from 5.5 to 11.
Summary of the Invention
The object of the invention was then to provide an
exactly dosable, excellently cleaning, skin-compatible,
temperature- and storage-stable, pourable hand
dishwashing detergent in which the optionally
physically or chemically incompatible or sensitive
ingredients are incorporated in temperature-, storage-
and transportation-stable, easy-to-handle and optically
pleasing form, and which releases. these ingredients
only directly prior to or during use.
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The invention provides a thickened aqueous surfactant-
containing composition, in particular hand dishwashing
detergent, comprising anionic surfactant, amphoteric
surfactant, polymer and microcapsules in which one or
more ingredients of the composition are completely or
partially included.
In contrast to the ingredients based on the overall
hand dishwashing detergent, the term "active
ingredients" means merely the fraction thereof present
in the microcapsules.
The present invention likewise provides for the use of
the composition according to the invention as hand
dishwashing detergent.
As well as crockery, the composition is, however,
equally as effective in cleaning hard surfaces made of
glass, ceramic, plastic or metal for domestic and
commercial use. Accordingly, the present invention
further provides for the use of the composition
according to the invention as a hard-surface cleaner.
The combination of anionic surfactant and amphoteric
surfactant on the one hand brings about a particularly
advantageous cleaning action, and on the other hand, in
conjunction with the polymer, effects a spatially
particularly stable suspension of the microcapsules.
The otherwise customary use of relatively large amounts
of electrolyte salt for stabilizing the microcapsul~~s
is therefore not necessary. Visible microcapsules
permit particularly accurate, reproducible dosing by
counting out the microcapsules present in the metered
amount of hand dishwashing detergent.
Unless stated otherwise, for the purposes of the
present invention, fatty acids or. fatty alcohols or
derivatives thereof are representative of branched or
unbranched carboxylic acids or alcohols or derivatives
CA 02306376 2000-04-20
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thereof respectively having, preferably, from 6 to 22
carbon atoms. Because of their vegetable base and
because they are based on renewable raw materials, the
first-mentioned are preferred for ecological reasons,
without, however, the teaching according to the
invention being limited thereto. In particular, the oxo
alcohols, obtainable, for example, according to the
ROELEN oxo synthesis, or derivatives thereof can,
accordingly, also be used.
Whenever the text below mentions alkaline earth metals
as counterions for monovalent anions, this means that
the alkaline earth metal is of course present only in
half of the amount - i.e. in an amount sufficient to
balance the charge - of the anion.
The indication INCI means that the designation which
follows - or in some cases which precedes - is a name
in accordance with the International Dictionary of
Cosmetic Ingredients from The Cosmetic, Toiletry, and
Fragrance Association (CTFA). The indication CAS means
that the numeral sequence which follows is a
designation of the Chemical Abstracts Service.
Detailed Description of the Invention
Polymer
Polymers for the purposes of the present invention are
polycarboxylates, preferably homo- and copolymers of
acrylic acid, in particular acrylic acid copolymers,
such as acrylic acid-methacrylic acid copolymers, and
polysaccharides, in particular heteropolysaccharides,
and other customary polymeric thickeners.
Suitable polysaccharides and heteropolysaccharides are
the polysaccharide gums, for example gum arabic, agar,
alginate, carrageens and their salts, guar, guaran,
tragacanth, gellan, ramsan, dextran or xanthan and
their derivatives, e.g. propoxylated guar, and their
mixtures. Other polysaccharide thickeners, such as
starches or cellulose derivatives, can be used
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alternatively, but are preferably used in addition to a
polysaccharide gum, for example starches of very
different origins and starch derivatives, e.g.
hydroxyethyl starch, starch phosphate ester or starch
acetates, or carboxymethylcellulose or its sodium salt,
methyl-, ethyl-, hydroxyethyl-, hydroxypropyl-,
hydroxypropyl-methyl- or hydroxyethyl-methyl-cellulose
or cellulose acetate.
A preferred polymer is the microbial anionic
heteropoly-saccharide xanthan gum, which is produced
from Xanthomonas campestris and some other species
under aerobic conditions and has a molecular weight of
2-15 x 106 and is available, for example, from Kelco
under the trade name Keltrol ~, e.g. as cream-colored
powder Keltrol ~ T (Transparent) or as white granules
Keltrol ~ RD (Readily Dispersible).
Suitable acrylic acid polymers are, for example,
homopolymers of acrylic acid (INCI Carbomer)
crosslinked with a polyalkenyl polyether, in particular
an allyl ether of sucrose, pentaerythritol or
propylene, which are also referred to as carboxyvinyl
polymers. Such polyacrylic acids are obtainable inter
alia from BF Goodrich under the trade name Carbopol ~,
e.g. Carbopol ~ 940 (molecular weight about 4,000,000),
Carbopol ~ 941 (molecular weight about 1,250,000) or
Carbopol ~ 934 (molecular weight about 3,000,000).
Particularly suitable polymers are, however, the
following acrylic acid copolymers: (i) copolymers of
two or more monomers from the group of acrylic acid,
methacrylic acid and its simple esters, preferably
formed with C1_4-alkanols (INCI Acrylates Copolymer), to
which, for example; the copolymers of methacrylic acid,
butyl acrylate and methyl methacrylate (CAS 25035-69-2)
or of butyl acrylate and methyl methacrylate (CAS
25852-37-3) belong and which are available, for
example, from Rohm & Haas under the trade names Aculyn0
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and Acusol ~, e.g. the anionic nonassociative polymers
AculynO 33 (crosslinked) , Acusol~ 810 and Acusol~ 830
(CAS 25852-37-3); (ii) crosslinked high molecular
weight acrylic acid copolymers, to which, for example,
the copolymers of Clo-ao-alkyl acrylates, crosslinked
with an allyl ether of sucrose or of pentaerythritol,
having one or more monomers from the group of acrylic
acid, methacrylic acid and its simple esters,
preferably formed with Cl_4-alkanols (INCI
Acrylates/C10-30 Alkyl Acrylate Crosspolymer) belong
and which are obtainable, for example, from BFGoodrich
under the trade name Carpopol ~ e.g. the hydrophobicized
Carbopol~ ETD 2623 and Carbopol~ 1382 (INCI
Acrylates/C10-30 Alkyl Acrylate Crosspolymer), and
Carbopol~ AQUA 30 (previously Carbopol~ EX 473) .
The content of polymer is customarily between 0.01 and
8% by weight, preferably between 0.1 and 7% by weight,
particularly preferably between 0.5 and 6% by weight,
in particular between 1 and 5% by weight and most
preferably between 1.5 and 4% by weight, for example
between 2 and 2.5% by weight. The viscosity of the
compositions according to the invention is essentially
set or controlled via the polymer content, the required
amount varying from polymer to polymer. The surfactant
composition used also plays a role in the choice of
amount.
Surfactants
As surfactants, the hand dishwashing detergent
according to the invention comprises a combination of
at least one anionic surfactant and at least one
amphoteric surfactant. In a particular embodiment of
the invention, at least one nonionic surfactant is
additionally present. Overall, the surfactants are
customarily used in amounts of from 0.2 to 60% by
weight, preferably from 1 to ~ 55% by weight,
particularly preferably 3 to 50% by weight and most
preferably 5 to 45% by weight.
' CA 02306376 2000-04-20
_ g _
In one embodiment which is preferable for the
relatively high use concentration of, for example,
about 0.8 g of the composition according to the
invention per liter of wash liquor, the surfactant
content is customarily 5 to 35% by weight, preferably
to 30% by weight, in particular 14 to 25% by weight.
In a concentrated embodiment which is preferable for a
relatively low use concentration of, for example, about
0.4 g of the composition according to the invention per
liter of wash liquor, the surfactant content is, by
contrast, customarily 30 to 60% by weight, preferably
35 to 55% by weight, in particular 38 to 52% by weight.
Anionic surfactants
Anionic surfactants according to the invention can be
aliphatic sulfates, such as fatty alcohol sulfates,
fatty alcohol ether sulfates, dialkyl ether sulfates,
monoglyceride sulfates and aliphatic sulfonates, such
as alkanesulfonates, olefinsulfonates, ether
sulfonates, n-alkyl ether sulfonates, ester sulfonates
and lignin sulfonates. For the purposes of the present
invention, use can also be made of alkylbenzene-
sulfonates, fatty acid cyanamides, sulfosuccinic
esters, fatty acid isethionates, acylaminoalkane-
sulfonates (fatty acid tauride), fatty acid
sarcosinates, ether carboxylic acids and alkyl (ether)
phosphates.
For the purposes of the present invention, particular
preference is given to fatty alcohol ether sulfates.
Fatty alcohol ether sulfates are products of sulfating
reactions with alkoxylated alcohols. In this
connection, the person skilled in the art generally
understands by the term "alkoxylated alcohols" the
reaction products of alkylene . oxide, preferably
ethylene oxide, with alcohols, for the purposes of the
present invention, preferably with longer-chain
CA 02306376 2000-04-20
_ g _
alcohols. Generally, n moles of ethylene oxide and one
mole of alcohol form, depending on the reaction
conditions, a complex mixture of addition products of
varying degrees of ethoxylation. A further embodiment
of the alkoxylation consists of the use of mixtures of
the alkylene oxides, preferably the mixture of ethylene
oxide and propylene oxide. For the purposes of the
present invention, very particular preference is given
to fatty alcohols with a low degree of ethoxylation
having from 1 to 4 ethylene oxide units (EO), in
particular 1 to 2 EO, for example 1.3 EO.
Preferably, the anionic surfactants, in particular
fatty alcohol ether sulfates, are used in amounts of
from 0.2 to 49.8% by weight, particularly preferably 5
to 45% by weight, in particular 8 to 40% by weight and
most preferably 10 to 36% by weight.
In a particular embodiment of the teaching according to
the invention, the composition comprises, as the sole
anionic surfactant or, preferably, as an additional
anionic surfactant, in particular in combination with
fatty alcohol ether sulfates, fatty alcohol sulfates,
where, preferably, between 0.5 and 15% by weight of
fatty alcohol sulfates are present.
Amphoteric surfactants
Amphoteric surfactants (zwitterionic surfactants) which
can be used according to the invention include
betaines, amine oxides, alkylamidoalkylamines, alkyl-
substituted amino acids, acylated amino acids and
biosurfactants, of which the betaines are particularly
preferred within the meaning of the teaching according
to the invention.
Betaines
Suitable betaines are the alkylbetaines, the alkyl-
amidobetaines, the imidazoliniumbetaines, the sulfo-
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betaines (INCI Sultaines) and the phosphobetaines and
preferably satisfy formula I,
R1- [CO-X- (CHz) n~ x-N+ (Rz) (R3) - (CHz) m- [CH (OH) -CHz] Y-Y- (I )
in which is a saturated or unsaturated Cs_zz-alkyl
Rl
radical, preferably Ce_18-alkyl radical,
in particular a saturated Clo-ls-alkyl
radical, for example a saturated Clz_14-
alkyl radical,
X is NH, NR4 with the Cl_4-alkyl radical R4
,
0 or S,
n is a number from 1 to 10, preferably 2
to 5, in particular 3,
x is 0 or 1, preferably 1,
Rz, R3 independently of one another are a Cl_4-
alkyl radical, optionally hydroxy-
substituted, such as, for example, a
hydroxyethyl radical, but in particular
a methyl radical,
m is a number from 1 to 4, in particular
1, 2 or 3,
y is 0 or 1 and
Y is COO, S03, OPO (OR5) O or P (0) (OR5) O,
where RS is a hydrogen atom H or a Cl_4-
alkyl radical.
The alkyl- and alkylamidobetaines, betaines of the
formula I containing a carboxylate group (Y' - COO') are
also c-.fled carbobetaines.
Preferred amphoteric surfactants are the alkylbetaines
of the formula (Ia), the alkylamidobetaines of the
formula (Ib), the sulfobetaines of the formula (Ic) and
the amidosulfobetaines of the formula (Id),
Rl-N+(CH3)z-CH2C00- _ (Ia)
R1-CO-NH- (CHz) 3-N+ (CH3) z-CH2C00- , (Ib)
Rl-N+ (CH3) z-CHzCH (OH) CH2S03- (Ic)
Rl-CO-NH- (CHz) 3-N+(CH3) z-CHZCH (OH) CHzS03- (Id)
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in which Rl has the same meaning as in formula I.
Particularly preferred amphoteric surfactants are the
carbobetaines, in particular the carbobetaines of the
formula (Ia) and (Ib), most preferably the alkylamido-
betaines of the formula (Ib) .
Examples of suitable betaines and sulfobetaines are the
following compounds named in accordance with INCI:
Almondamidopropyl Betaine, Apricotamidopropyl Betaine,
Avocadamidopropyl Betaine, Babassuamidopropyl Betaine,
Behenamidopropyl Betaine, Behenyl Betaine, Hetaine,
Canolamidopropyl Betaine, Capryl/Capramidopropyl
Betaine, Carnitine, Cetyl Betaine, Cocamidoethyl
Hetaine, Cocamidopropyl Betaine, Cocamidopropyl
Hydroxysultaine, Coco-Hetaine, Coco-Hydroxysultaine,
Coco/Oleamidopropyl Hetaine, Coco-Sultaine, Decyl
Betaine, Dihydroxyethyl Oleyl Glycinate, Dihydroxyethyl
Soy Glycinate, Dihydroxyethyl Stearyl Glycinate,
Dihydroxyethyl Tallow Glycinate, Dimethicone Propyl
PG-Betaine, Erucamidopropyl Hydroxysultaine,
Hydrogenated Tallow Betaine, Isostearamidopropyl
Betaine, Lauramidopropyl Betaine, Lauryl Hetaine,
Lauryl Hydroxysultaine, Lauryl Sultaine,
Milkamidopropyl Betaine, Minkamidopropyl Betaine,
Myristamidopropyl Betaine, Myristyl Betaine,
Oleamidopropyl Hetaine, Oleamidopropyl Hydroxysultaine,
Oleyl Hetaine, Olivamidopropyl Betaine, Palmamidopropyl
Hetaine, Palmitamidopropyl Betaine, Palmitoyl
Carnitine, Palm Kernelamidopropyl Hetaine,
Polytetrafluoroethylene Acetoxypropyl Betaine,
Ricinoleamidopropyl Betaine, Sesamidopropyl Betaine,
Soyamidopropyl Betaine, Stearamidopropyl Hetaine,
Stearyl Betaine, Tallowamidopropyl Hetaine,
Tallowamidopropyl Hydroxysultaine, Tallow Betaine,
Tallow Dihydroxyethyl Betaine, Undecylenamidopropyl
Hetaine and Wheat Germamidopropyi Betaine.
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Amine oxides
The amine oxides which are suitable according to the
invention include alkylamine oxides, in particular
alkyldimethylamine oxides, alkylamidoamine oxides and
alkoxyalkylamine oxides. Preferred amine oxides satisfy
formula II,
RsR7ReN+-O (II)
Rs- ICO-NH- (CH2) wl z-N+ (R') (Re) -O- (II)
in which Rs is a saturated or unsaturated Cs_z2-alkyl
radical, preferably Ce_18-alkyl radical,
in particular a saturated Clo-is-alkyl
radical, for example a saturated Clz-14-
alkyl radical, which is bonded to the
nitrogen atom N in the alkylamidoamine
oxides via a carbonylamidoalkylene group
-CO-NH-(CH2)Z- and in the alkoxyalkyl-
amine oxides via an oxaalkylene group
-O-(CHZ)Z-, where z is in each case a
number from 1 to 10, preferably 2 to 5,
in particular 3,
R',R8 independently of one another are a C1_4-
alkyl radical, optionally hydroxy-
substituted, such as, for example, a
hydroxyethyl radical, in particular a
methyl radical.
Examples of suitable amine oxides are the following
compounds named in accordance with INCI:
Almondamidopropylamine Oxide, Babassuamidopropylamine
Oxide, Behenamine Oxide, Cocamidopropyl Amine Oxide,
Cocamidopropylamine Oxide, Cocamine Oxide, Coco-
Morpholine Oxide, Decylamine Oxide,
Decyltetradecylamiae Oxide, Diaminopyrimidine Oxide,
Dihydroxyethyl C8-10 Alkoxypropylamine Oxide,
Dihydroxyethyl C9-11 Alkoxypropylamine Oxide,
Dihydroxyethyl C12-15 Alkoxypropylamine Oxide,
Dihydroxyethyl Cocamine Oxide, Dihydroxyethyl Lauramine
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Oxide, Dihydroxyethyl Stearamine Oxide, Dihydroxyethyl
Tallowamine Oxide, Hydrogenated Palm Kernel Amine
Oxide, Hydrogenated Tallowamine Oxide, Hydroxyethyl
Hydroxypropyl C12-15 Alkoxypropylamine Oxide,
Isostearamidopropylamine Oxide, Isostearamidopropyl
Morpholine Oxide, Lauramidopropylamine Oxide, Lauramine
Oxide, Methyl Morpholine Oxide, Milkamidopropyl Amine
Oxide, Minkamidopropylamine Oxide, Myristamido-
propylamine Oxide, Myristamine Oxide, Myristyl/Cetyl
Amine Oxide, Oleamidopropylamine Oxide, Oleamine Oxide,
Olivamidopropylamine Oxide, Palmitamidopropylamine
Oxide, Palmitamine Oxide, PEG-3 Lauramine Oxide,
Potassium Dihydroxyethyl Cocamine Oxide Phosphate,
Potassium Trisphosphonomethylamine Oxide, Sesamido-
propylamine Oxide, Soyamidopropylamine Oxide,
Stearamidopropylamine Oxide, Stearamine Oxide,
Tallowamidopropylamine Oxide, Tallowamine Oxide,
Undecylenamidopropylamine Oxide and Wheat
Germamidopropylamine Oxide.
Alkylamidoalkylamines
The alkylamidoalkylamines (INCI Alkylamido Alkylamines)
are amphoteric surfactants of the formula (III),
R9-CO-NR1°- (CH2) i-N (R11) - (CHZCHzO) j- (CHz) k- [CH (OH) ] 1-CHZ-Z-
OM ( I I I )
in which R9 is a saturated or unsaturated C6_z2-alkyl
radical, preferably C8_~e-alkyl radical,
in particular a saturated Clo-ls-alkyl
radical, for example a saturated C12_~a-
alkyl radical,
R1° is a hydrogen atom H or a C1_4-alkyl
radical, preferably H,
i is a number from 1 to 10, preferably 2
to ~, in particular 2 or 3,
R11 is a hydrogen atom H or CH2COOM (for M
see below),
j is a number from 1 to 4, preferably 1 or
2, in particular 1,
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k is a number from 0 to 4, preferably 0 or
1,
1 i s 0 or 1, where k = 1, when 1 = 1,
Z is CO, SOZ, OPO (OR12) or P (O) (OR12) , where
Rl2 is a Cl_4-alkyl radical or M (see
below), and
M is hydrogen, an alkali metal, an
alkaline earth metal or a protonated
alkanolamine, e.g. protonated mono-, di-
or triethanolamine.
Preferred representatives satisfy the formulae IIIa to
IIId,
R9-CO-NH- (CHZ) Z-N (Rll) -CHZCHzO-CHz-COOM (Ills)
R9-CO-NH- (CHZ) ~-N(Rll) -CHzCHzO-CHZCHz-LOOM (IIIb)
R9-CO-NH- (CHz) Z-N (Rll) -CHzCH~O-CHZCH (OH) CHZ-S03M (IIIc)
R9-CO-NH- (CH2) 2-N (Rll) -CHzCHZO-CHZCH (OH) CHZ-OPOjHM (IIId)
in which Rll and M have the same meaning as in formula
(III) .
Examples of alkylamidoalkylamines are the following
compounds named in accordance with INCI:
Cocoamphodipropionic Acid, Cocobetainamido
Amphopropionate, DEA-Cocoamphodipropionate, Disodium
Caproamphodiacetate, Disodium Caproamphodipropionate,
Disodium Capryloamphodiacetate, Disodium Capryloampho-
dipropionate, Disodium Cocoamphocarboxyethylhydroxy-
propylsulfonate, Disodium Cocoamphodiacetate, Disodium
Cocoamphodipropionate, Disodium Isostearoampho-
diacetate, Disodium Isostearoamphodipropionate,
Disodium Laureth-5 Carboxyamphodiacetate, Disodium
Lauroamphodiacetate, Disodium Lauroamphodipropionate,
Disodium Oleoamphodipropionate, Disodium PPG-2-
Isodeceth-7 Carboxyamphodiacetate, Disodium
Stearoamphodiacetate, Disodium Tallowamphodiacetate,
Disodium Wheatgermamphodiacetate, Lauroamphodipropionic
Acid, Quaternium-85, Sodium Caproamphoacetate, Sodium
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Caproamphohydroxypropylsulfonate, Sodium Capro-
amphopropionate, Sodium Capryloamphoacetate, Sodium
Capryloamphohydroxypropylsulfonate, Sodium Caprylo-
amphopropionate, Sodium Cocoamphoacetate, Sodium
Cocoamphohydroxypropylsulfonate, Sodium Cocoampho-
propionate, Sodium Cornamphopropionate, Sodium
Isostearoamphoacetate, Sodium Isostearoamphopropionate,
Sodium Lauroamphoacetate, Sodium Lauroampho-
hydroxypropylsulfonate, Sodium Lauroampho PG-Acetate
Phosphate, Sodium Lauroamphopropionate, Sodium
Myristoamphoacetate, Sodium Oleoamphoacetate, Sodium
Oleoamphohydroxypropylsulfonate, Sodium Oleoampho-
propionate, Sodium Ricinoleoamphoacetate, Sodium
Stearoamphoacetate, Sodium Stearoamphohydroxy-
propylsulfonate, Sodium Stearoamphopropionate, Sodium
Tallamphopropionate, Sodium Tallowamphoacetate, Sodium
Undecylenoamphoacetate, Sodium Undecyleno-
amphopropionate, Sodium Wheat Germamphoacetate and
Trisodium Lauroampho PG-Acetate Chloride Phosphate.
Alky3-substituted amino acids
Alkyl-substituted amino acids (INCI Alkyl-Substituted
Amino Acids) preferred according to the invention are
monoalkyl-substituted amino acids according to formula
(IV) ,
R13-NH-CH (R14) - (CH2) u-COOM' (IV)
in which R13 is a saturated or unsaturated Cs_zz-alkyl
radical, preferably Ce_la-alkyl radical,
in particular a saturated Clo-ls-alkyl
radical, for example a saturated Clz_14-
alkyl radical,
R14 is a hydrogen atom H or a Cl_4-alkyl
radical, preferably H,
a is a number from 0 to 4, preferably 0 or
1, in particular l, and
M' is hydrogen, an alkali metal, an
alkaline earth metal or a protonated
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alkanolamine, e.g. protonated mono-, di-
or triethanolamine,
alkyl-substituted imino acids according to formula (V),
R15-N- C (CHz) ~-COOM" J z (V)
in which R15 is a saturated or unsaturated Cs_zz-alkyl
radical, preferably CB_18-alkyl radical,
in particular a saturated Clo_ls-alkyl
radical, for example a saturated Clz_la-
alkyl radical,
v is a number from 1 to 5, preferably 2 or
3, in particular 2, and
M" is hydrogen, an alkali metal, an
alkaline earth metal or a protonated
alkanolamine, e.g. protonated mono-, di-
or triethanolamine, where M" in the two
carboxyl groups can have the same
meanings or two di f f erent meanings , a . g .
hydrogen and sodium or 2 x sodium,
and mono- or dialkyl-substituted natural amino acids
according to formula (VI),
Rls-N (R1') -CH (Rl8) -COOM' ' ' (VI )
in which Rls is a saturated or unsaturated Cs_zz-alkyl
radical, preferably Ce_le-alkyl radical,
in particular a saturated Clo_ls-alkyl
radical, for example a saturated Clz_14-
alkyl radical,
R1' is a hydrogen atom or a Cl_4-alkyl
radical, optionally hydroxy- or amino-
substituted, e.g. a methyl, ethyl,
hydroxyethyl or aminopropyl radical,
R18 is the radical of one of the 20 natural
a-amino acids H2NCH (R18) COOH, and
' CA 02306376 2000-04-20
- 17 -
M"' is hydrogen, an alkali metal, an
alkaline earth metal or a protonated
alkanolamine, e.g. protonated mono-, di-
or triethanolamine.
Particularly preferred alkyl-substituted amino acids
are the aminopropionates according to formula (IVa),
R13-NH-CHzCHZCOOM' (IVa)
in which R13 and M' have the same meaning as in formula
(IV) .
Examples of alkyl-substituted amino acids are the
following compounds named in accordance with INCI:
Aminopropyl Laurylglutamine, Cocaminobutyric Acid,
Cocaminopropionic Acid, DEA-Lauraminopropionate,
Disodium Cocaminopropyl Iminodiacetate, Disodium
Dicarboxyethyl Cocopropylenediamine, Disodium
Lauriminodipropionate, Disodium Steariminodipropionate,
Disodium Tallowiminodipropionate, Lauraminopropionic
Acid, Lauryl Aminopropylglycine, Lauryl
Diethylenediaminoglycine, Myristaminopropionic Acid,
Sodium C12-15 Alkoxypropyl Iminodipropionate, Sodium
Cocaminopropionate, Sodium Lauraminopropionate, Sodium
Lauriminodipropionate, Sodium Lauroyl Methylamino-
propionate, TEA-Lauraminopropionate and TEA-
Myristaminopropionate.
Acylated amino acids
Acylated amino acids are amino acids, in particular the
20 natural a-amino acids, which carry, on the amino
nitrogen atom, the acyl radical R19C0 of a saturated or
unsaturated fatty acid R19COOH, where Rl9 is a saturated
or unsaturated C6_2~-alkyl radical, preferably Ce_le-alkyl
radical, in particular a saturated. Clo-ls-alkyl radical,
for example a saturated Clz_14-alkyl radical. The
acylated amino acids can also be used as alkali metal
salt, alkaline earth metal salt or alkanolammonium
' CA 02306376 2000-04-20
- 18 -
salt, e.g. mono-, di- or triethanolammonium salt.
Examples of acylated amino acids are the acyl
derivatives listed in accordance with INCI under Amino
Acids, e.g. Sodium Cocoyl Glutamate, Lauroyl Glutamic
Acid, Capryloyl Glycine or Myristoyl Methylalanine.
Preferably, the amphoter=c surfactants, in particular
alkylamidobetaines, are used in amounts of from 0.1 to
14.9% by weight, in particular from 1 to 10% by weight,
most preferably from 1.5 to 8% by weight, for example 2
to 7% by weight.
Nonionic surfactants
For the purposes of the invention, nonionic surfactants
can be alkoxylates, such as polyglycol ethers, fatty
alcohol polyglycol ethers, alkylphenol polyglycol
ethers, terminally capped polyglycol ethers, mixed
ethers and hydroxy mixed ethers and fatty acid
polyglycol esters. It is also possible to use ethylene
oxide, propylene oxide, block polymers and fatty acid
alkanolamides and fatty acid polyglycol ethers. An
important class of nonionic surfactants which can be
used according to the invention are the polyoh
surfactants, particularly the glycosurfactants, such as
alkyl polyglycosides and fatty acid glucamides.
Particular preference is given to alkyl polyglycosides,
in particular the alkyl polyglucosides.
Alkyl polyglycosides are surfactants which can be
obtained by reacting sugars and alcohols according to
appropriate processes of preparative organic chemistry,
a mixture of monoalkylated, oligomeric or polymeric
sugars resulting depending on the nature of the
preparation. Preferred alkyl polyglycosides are the
alkyl polyglucosides, where the alcohol is particularly
preferably a long-chain fatty alcohol or a mixture of
long-chain fatty alcohols having branched or unbranched
Ce- to C18-alkyl chains, and the degree of
oligomerization (DP) of the sugars is between 1 and 10,
v CA 02306376 2000-04-20
- 19 -
preferably 1 to 6, in particular 1.1 to 3, most
preferably 1.1 to 1.7.
Preferably, one or more nonionic surfactants, in
particular alkyl polyglycosides, are used in amounts of
from 0.1 to 14.9% by weight, in particular 1 to 10% by
weight and most preferably 1.5 to 5%. by weight, for
example 2 to 3% by weight.
In a preferred embodiment of the invention the hand
dishwashing detergent comprises
(a) 0.2 to 49.8% by weight, preferably 5 to 45% by
weight, particularly preferably 8 to 40% by
weight, of anionic surfactants, in particular
fatty alcohol ether sulfates,
(b) 0.1 to 14.9% by weight, preferably 1 to 10% by
weight, of amphoteric surfactants, in particular
alkylamidobetaines, and
(c) 0.1 to 14.9% by weight, preferably 1 to 10% by
weight, of nonionic surfactants, in particular
alkyl polyglucosides.
Microcapsules
The microcapsules which can be used are any of the
surfactant-stable capsules and capsule materials or
spheres and sphere materials offered on the market,
such as, for example, Hallcrest microcapsules (capsule
material: gelatin, gum arabic) from Hallcrest, Inc.
(US), Coletica thalaspheres (capsule material: maritime
collagen) from Coletica (FR), Lipotec millicapsules
(capsule material: alginic acid, agar agar) from
Lipotec S.A. (ES), Induchem unispheres (capsule
material: lactose, microcrystalline cellulose,
hydroxypropylmethylcellulose) and Unicerin C30 (capsule
material: lactose, microcrystalline cellulose,
hydroxypropylmethylcellulose) from Induchem AG (CH),
Kobo glycospheres (capsule material: modified starch,
fatty acid esters, phospholipids) and soft spheres
(capsule material: modified agar agar) from Kobo (US),
CA 02306376 2000-04-20
- 20 -
and Kuhs Probiol nanospheres (capsule material:
phospholipids) from Kuhs (DE) and others.
The microcapsules can have any desired form within the
framework defined by the preparation, but are
preferably egg-shaped or ellipsoid or, more accurately,
spherical. The diameter along their greatest spatial
extension can be between 100 nm (not visually
recognizable as capsules) and 10 mm, depending on the
active ingredient and application. The preferred
diameter is in the range between 0.1 mm and 7 mm,
particular preference being given to microcapsules
having a diameter between 0.4 mm and 5 mm.
For the purposes of the invention, active ingredients
are, inter alia, dermatologically effective substances,
such as vitamin A, vitamin B2 , vitamin H12 , vitamin C,
vitamin E, D-panthenol, sericin, collagen partial
hydrolysate, various vegetable protein partial
hydrolysates, protein hydrolysate fatty acid
condensates, liposomes, cholesterol, vegetable and
animal oils, such as, for example, lecithin, soya oil,
etc., plant extracts, such as, for example, Aloe Vera,
azulene, hamamelis extracts, algae extracts, etc.,
allantoin, A.H.A. complexes. For the purposes of the
invention, active ingredients are additionally
antibacterial active ingredients, such as, for example,
benzoic acid, lactic acid, salicylic acid, sorbic acid
or mixtures thereof or salts thereof. For the purposes
of the invention, active ingredients are also essential
oils, such as, for example, perfumes, limonene,
geraniol, nerol, and additives for improving the ware
shine, such as, for example, vinegar. To improve the
appearance, dyes, colored pigments or pearlizing
components are mixed in.
Accordingly, in a preferred embodiment, the hand
dishwashing detergent according to the invention
comprises microcapsules in which one or more
~
CA 02306376 2000-04-20
- 21 -
representatives from the group consisting of
dermatologically active substances, antibacterial
active ingredients, essential oils and additives for
improving the ware shine and the appearance are
included.
The active ingredient can be released from the
microcapsules either as a result of the microcapsules
rubbing together during the cleaning process, or else
as a result of rupture using a suitable dosing device .
It is also conceivable that the active ingredient is
released by changing the temperature (introduction into
warm wash liquor), by shifting the pH, or by-changing
the electrolyte content, etc.
The content of microcapsules is customarily from 0.01
to 10% by weight, preferably from 0.1 to 5% by weight,
in particular from 0.2 to 3% by weight and most
preferably from 0.3 to 2% by weight, where the
composition according to the invention can comprise
exclusively microcapsules of the same type, or else
mixtures of different types of microcapsules.
Viscosity
The viscosity which is favorable for the compositions
according to the invention is, at 20°C and a shear rate
of 10 s-l, between 300 and 20,000 mPa~s, preferably
between 700 and 15,000 mPa~s, particularly preferably
between 1000 and 10,000 mPa~s, or, at 20°C and a shear
rate of 30 s-1, between 500 and 18,000 mPa~s, preferably
between 700 and 13,000 mPa~s, particularly preferably
between 900 and 10,000 mPa~s, in particular between
1100 and 8000 mPa~s, most preferably between 1300 and
6500 mPa-s, for example between 1000 and 4000 mPa-s.
Zero shear viscosity r~o values preferred for favorable
storage properties are between .100 and 5000 Pa~s,
preferably between 200 and 3000 Pa-s.
CA 02306376 2000-04-20
- 22 -
Many of the mixtures investigated according to the
invention exhibit a viscosity profile which changes
with time. This is particularly desirable since during
the production process, a low-viscosity mass is
preferred, but with regard to storage stability and use
comfort importance is placed on products of higher
viscosity.
The viscosity of the compositions according to the
invention can be adjusted by the polymer.. The required
amounts can be different from polymer to polymer. The
surfactant composition used likewise plays a role in
the choice of quantity, as does the presence of
solubilizers.
Solubilizers
The solubilizers, for example for dyes and perfume
oils, can, for example, be alkanolamines, polyols, such
as ethylene glycol, 1,2-propylene glycol, glycerol and
other mono- and polyhydric alcohols, and alkylbenzene-
sulfonates having from 1 to 3 carbon atoms in the alkyl
radical.
To stabilize the hand dishwashing detergent according
to the invention, particularly if the surfactant
content is high, it is possible to add one or more
dicarboxylic acids and/or salts thereof, alone or in a
mixture, in particular a composition of Na salts of
adipic, succinic and glutaric acid in admixture, as is
available, for example, under the trade name Sokalan~
DSC. They are advantageously used in amounts of from
0.1 to 8% by weight, preferably 0.5 to 7% by weight, in
particular 1.3 to 6% by weight and particularly
preferably 2 to 4% by weight.
A change in the dicarboxylic acid .(salt) content can -
in particular in amounts above. 2% by weight -
contribute to a clear solution of the ingredients.
Likewise, within certain limits, it is possible to
~
CA 02306376 2000-04-20
- 23 -
influence the viscosity of the mixture by virtue of
this agent. Furthermore, this component influences the
solubility of the mixture. This component is
particularly preferably used at high surfactant
contents, in particular at surfactant contents above
30% by weight.
Instead of or in addition to the dicarboxylic acids
and/or salts thereof, it is possible, to regulate the
viscosity, to also use other organic acids or salts
thereof, such as, for example, sodium formate, sodium
acetate, sodium citrate and sodium tartrate, and
inorganic salts, such as, for example, sodium chloride,
magnesium chloride and magnesium sulfate, and also
salts of the abovementioned anions with other alkali
metals or alkaline earth metals individually or in
mixtures.
Solvents
A further advantageous component of the compositions
according to the invention are solvents, in particular
lower alcohols, preferably ethanol, n-propanol or
isopropanol, particularly preferably ethanol. They
contribute to the incorporation of perfume and dye,
prevent the formation of liquid-crystalline phases and
participate in the formation of clear products. The
viscosity can be reduced by increasing the amount of
solvent. However, too much solvent brings about too
great a decrease in the viscosity. For this reason,
according to the invention, one or more solvents are
customarily present in amounts of from 0.1 to 12% by
weight, preferably 1 to 10% by weight, particularly
preferably 3 to 8% by weight, for example 5 to 6% by
weight.
Auxiliaries and additives
A further improved cleaning performance, particularly
in the case of baked on soil, is achieved using
abrasive substances, preferably water-soluble abrasive
~
CA 02306376 2000-04-20
- 24 -
substances, in particular alkali metal bicarbonate,
alkali metal sulfate.
In addition, it is also possible for further
auxiliaries and additives customary in hand dishwashing
detergents, in particular W stabilizers, perfume
substances, pearlizing agents (INCI opacifying agents;
for example glycol distearate, e.g. Cutina~ AGS from
Henkel KGaA, or mixtures containing this, e.g. the
Euperlane~ from Henkel KGaA), dyes, corrosion
inhibitors and/or preservatives, in amounts usually not
exceeding 5~ by weight to be present.
The pH of the compositions according to the invention
can be adjusted by means of customary pH regulators,
for example citric acid or NaOH, where - essentially
because of the required tolerability by the hands - a
range from 5 to 8, preferably 5.5 to 7.5, in particular
5.7 to 7 is preferred.
Preparation
The hand dishwashing detergents according to the
invention can be prepared by stirring together the
individual constituents in any order. The charging
order is unimportant for the preparation of the
composition.
In this respect, water, surfactants and optionally
further ingredients from those mentioned above are
preferably stirred together. If perfume and/or dye are
used, then these are added to the resulting solution.
Finally, the polymer is added, optionally in the form
of an aqueous solution in order to facilitate its
homogeneous dissolution. The pH is then adjusted as
described above and, finally, the microcapsules are
mixed in.
CA 02306376 2000-04-20
- 25 -
Embodiments of the Invention are further described by reference to
the following:
Examples
The compositions E1 to E16 according to the invention
were prepared as described above, and their pH,
viscosity and storage stability were determined.
The compositions of the compositions E1 to E16
according to the invention in % by weight, and the
properties determined are shown in Tables 1 to 3. In
addition, a number of compositions E1 to E16 according
to the invention comprise traces of dye . The pH of the
compositions E1 to E16 according to the invention was
adjusted to values between 5.5 and 7 using citric acid.
The viscosity of the compositions El to E16 according
to the invention was determined at 20°C in accordance
with Brookfield (Brookfield LV DV II+ viscometer;
spindle 25; rate of rotation 30 min-1) .
The stability of the compositions was tested by
assessing the compositions visually after storage in
each case for four weeks at room temperature of 20°C,
at elevated temperature of 40°C, and in the cold at a
temperature of 5°C. Irrespective of the storage
temperature, none of the compositions exhibited a
change which was visually detectable after 4 weeks, and
in particular no change in the shape of the capsules or
in their spatial distribution within the composition
was observed.
CA 02306376 2000-04-20
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CA 02306376 2000-04-20
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CA 02306376 2000-04-20
28
Table 3 B15 S16
Clzm4-alcohol ether sulfate(2E0) - -
Na salt
C12i14-alcohol ether sulfate(1.3E0) salt 31.5 35.0
Na
Clzils-alkyl polyglucoside, 1.5 7.5
DP = 1.4
Cocoamidopropylbetaine 7.0 7.5
Dicarboxylic acid mixture 2.0 3.3
(Sokalan~ DCS Na)
Ethanol 5.0 6.0
Perfume 0.7 0.8
Polymer (Aculyn~ 33) 4.0 2.0
Microspheres (Unispheres 508) - 1.5
RE
Microcapsules (Lipotec TypeII 1~ 0.8 -
211)
Water ad 100 100
pH 6.5 6.5
Viscosity at 20C [mPa-s] 8000 5000
Detergency on grease soil 4 g/10 [%] 109 -
I 1
Detergency on grease soil 4 g/l0 [%] 116 -
II 1
Detergency on mixed soil 4 g/10 [%] 117 -
1
The microcapsules used were readily visible with the
naked eye from a distance of about 0.5 m. The diameter
of the microcapsules was 0.8 ~ 0.4 mm in formulation
El, 2 ~ 0.5 mm in formulations E2, E7, E10 and E15, and
4 ~ 0.5 mm in formulations E5, E8, E11 and E14.
The detergency of the formulations according to the
invention was for the most part likewise determined -
except for E9, E10 and E16. The determination was
carried out in a semiautomatic plate test apparatus
using two different pure grease soilings I and II or a
greasy mixed soiling in a use concentration of 4 and/or
8 g/10 1. For this, at a constant temperature of 40 or
45°C respectively in 5 1 of water having a hardness of
16°, plates soiled_with the test soil were washed under
standard conditions, compared with a high-value classic
hand dishwashing detergent as laboratory standard,
until the foam - formed before the start of the
experiment - had disintegrated and the plates were no
CA 02306376 2000-04-20
- 29 -
longer clean. The concentration of the composition was
4 or 8 g respectively per liter of water. The number of
washed plates is given in Tables 1 to 3 as a percentage
relative to a commercially available high-performance
hand detergent composition set as 100%, as detergency
on the soil in question at the concentration given in
each case.
In particular, the compositions E3 to E7 and E15
demonstrate, as a result of their high detergency, the
superiority of the hand dishwashing detergents
according to the invention.
