Note: Descriptions are shown in the official language in which they were submitted.
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CLEAR LIQUID FABRIC SOFTENING COMPOSITIONS
15 Technical field of the invention
The present invention relates to fabric softening composition useful for
softening
fabrics. It especially relates to fabric softening compositions suitable for
use in
the rinse cycle of a textile laundering operation. The compositions of the
invention are translucent or clear liquid softening compositions.
Background of the invention
Fabric softening compositions, in particular clear liquid fabric softening
compositions are known. in the art as is their formulation. Hence, WO 97/03169
describes the formulation of liquid fabric softening compositions using
specific
solvents. The compositions of WO 97/03169 are said to provide excellent fabric-
softening/static-controb benefits, reduced staining of fabric, excellent water
dispersibility, rewettability, and/or storage and viscosity stability at sub-
normal
temperatures, i.e., temperatures below normal room temperature, e.g.,
25°C.
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However, it has been found that upon slight level variations of the solvents
or
even temperature change, the clarity and stability of the resulting
compositions
was often impaired.
In addition to this, a problem encountered with the use of these solvents is
their
undesirable odour which at high levels is even more perceptible. Still another
problem with these solvents is their relative cost and their low supply
capacity.
Accordingly, the formulator of softening compositions is faced with the dual
challenge of formulating a clear or tranluscent composition without being
detrimental to the stability and clarity of the liquid softening compositions.
One solution to these problem is to use a high level of organic acid as
provided in
EP-A-0,404,471. However, this still does not provide complete satisfaction
over
temperature or level variations.
The Applicant has now found that the use of a specific nonionic surfactant in
a
softening composition comprising a fabric softener and the specific solvents
of
WO 97!03169 fulfills this need.
Still another advantage of the invention is that the use of this nonionic
surfactant
enables a reduction in the solvent level in the softening composition whilst
not
impairing the performance of the softening compositions.
A further advantage of the invention is that the use of this nonionic
surfactant
enables the use of wide range of solvents. Indeed, typical solvent for use in
clear
formulations have a Clog P between 0.15 to 0.64. It has now been found that
the
level reduction of solvent by use of the nonionic surfactant is also
applicable to
solvents having a higher Clog P.
Still a further advantage of the invention is that the softening composition
of the
invention also provides similar benefit to those of WO 97/03169, i.e. fabric-
softening/static-control benefits, reduced staining of fabric, excellent water
dispersibility, rewettability, and/or storage and viscosity stability at sub-
normal
temperatures, i.e., temperatures below normal room temperature, e.g.,
25°C.
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Summary of the invention
The present invention relates to a clear fabric softening composition
comprising a
fabric softening compound, a principal solvent having a CIogP of from 0.15 to
1.0
and a nonionic alkoxylated surfactant, wherein said nonionic surfactant is
selected from:
i)- alkyl or alkylphenol alkoxylated with less than 9 alkoxy moieties;
ii)- alkyl amine alkoxylated with at least 5 alkoxy moieties; and
- iii)- block co-polymers obtained by copolymerisation of ethylene oxide and
propylene oxide; and
iv)- mixtures thereof.
Detailed description of the invention
I-Nonionic alkoxvlated surfactant
A nonionic alkoxylated surfactant is an essential component of the invention.
Not
to be bound by theory, it is believed that the nonionic alkoxyiated
surfactants
help to achieve clear products at low solvents levels by helping to maintain a
flexible, yet stable interface with zero curvature. The nonionic surfactants
will
reduce the interfacial tension at the hydrophobic-water interface, thus
promoting
flexibility, while enhancing packing efficiency at the interface and therefore
promoting interfacial stability. Due to the tendency of the nonionic
surfactant
head group to become highly hydrated, the surfactant will help to get to net
zero
curvature by filling void spaces in the pallisade layer.
By "pallisade layer", it is meant the area between hydrophilic groups and the
first
few carbon atoms in the hydrophobic layer (M.J Rosen, Surfactants and
interfacial phenomena, Second Edition, page 172).
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Typical levels of incorporation of the nonionic alkoxylated surfactant in the
softening compositions are of less than 10% by weight, preferably from 0.1 %
to
7% by weight, more preferably from 2% to 5% by weight of the composition.
The nonionic alkoxylated compounds described herein differ from the principal
solvents described hereinafter by their surfactancy properties. Of course, for
the
purpose of the present invention, these nonionic alkoxylated compounds are not
principal solvent as defined herein.
By "surfactant", it is meant a substance which, when present at low
- concentrations in a system, has the property of adsorbing onto surfaces or
interfaces of the system and of altering to a marked degree the surface or
interfacial free energies of those surfaces or interfaces. (M.J Rosen,
Surfactants
and interfacial phenomena, Second Edition, page 1 ).
Preferably, for the purpose of the invention, the nonionic alkoxylated
surfactants
have a critical micelle concentration (CMC) of less than 10-2M. The CMC being
defined in M.J ROSEN, Surfactants and interfacial phenomena, 1988, p.215.
The nonionic alkoxyiated surfactant for use herein is selected from:
i)- alkyl or alkylphenoi alkoxylated with less than 9 alkoxy moieties;
ii)- alkyl amine alkoxylated with at least 5 alkoxy moieties; and
iii)- block co-polymers obtained by copolymerisation of ethylene oxide and
propylene oxide; and
iv)- mixtures thereof.
i)-Suitable alkyl phenol alkoxylated with less than 9 alkoxy moieties are the
polyethylene oxide condensates of alkyl phenols, e.g., the condensation
products
of alkyl phenols having an alkyt or alkenyl group containing from 6 to 20
carbon
atoms in a primary, secondary or branched chain configuration, preferably from
8
to 12 carbon atoms, with ethylene oxide, the said ethylene oxide being
preferably
present in amounts equal to 3 to less than 9 moles of ethylene oxide per mole
of
alkyl phenol. The alkyl substituent in such compounds may be derived from
polymerized propylene, diisobutylene, octane, and nonane. Examples of this
type
of nonionic surfactants include Triton N-57~ a nonyi phenol ethoxylate (5E0)
from Rohm 8 Haas, Dowfax~ 9N5 from Dow and Lutensol~ AP6 from BASF.
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Still other suitable nonionic alkoxylated surfactants are the alcohols
alkoxylated
with less than 9 aikoxy moieties. Typical of this class are the aliphatic
aicohols
having from 6 to 22 carbon atoms alkoxylated with less than 9 alkoxy moieties.
5 The aliphatic alcohols for use herein have from 6 to 22 carbon atoms, and
are in
either straight chain or branched chain configuration, preferably from 8 to 18
carbon atoms, with less than 9 moles of ethylene oxide, preferably from 2 to
7,
and more preferably is from 3 to 6 on the average.
Preferably, the condensation product of aliphatic alcohols compounds of this
class are surfactants of the general formula:
R2 _ Y _ (C2H4p)Z _ H
wherein R2 is selected from the group consisting of primary, secondary and
branched chain alkyl and/or acyl hydrocarbyl groups; primary, secondary and
branched chain alkenyl hydrocarbyl groups; said hydrocarbyl groups preferably
having a hydrocarbyl chain length of from 6 to 20, preferably from 8 to 18
carbon
atoms. More preferably the hydrocarbyl chain length is from 10 to 15 carbon
atoms. In the general formula for the ethoxylated nonionic surfactants herein,
Y
is -O-, -C(O)O-, and z is less than 9, preferably from 2 to 7, and more
preferably
is 3 to 6 on the average.
Examples of nonionic surfactants of this class follow. In the examples, the
integer
defines the number of ethoxy (EO) groups in the molecule.
a. Straight-Chain. Primay Alcohol Alkoxvlates
The tri-, penta-, hepta-ethoxyiates of dodecanol, and tetradecanol are useful
surfactants in the' context of this invention. The ethoxylates of mixed
natural or
synthetic alcohois in the "coco" chain length range are also useful herein.
Commercially available straight-chain, primary alcohol alkoxylates for use
herein
are available under the tradename Marlipal~ 24/70 from Huls, and Genapol~ C-
050 from Hoechst.
b. Strai4ht-Chain. Secondary/ Alcohol Alkoxvlates
The tri-, yenta-, hepta-ethoxyiates of 3-hexadecanol, 2-octadecanol, 4-
eicosanol,
and 5-eicosanol are useful surfactants in the context of this invention.
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A commercially available straight-chain seconaary alcohol ethoxyiate for use
herein is the material marketed under the tradename Tergitol 15-S-7 from Union
Carbide, which comprises a mixture of secondary a~cohois having an average
hydrocarbyl chain length of 11 to 15 carbon atoms concensed with an average 7
moles of ethylene oxide per mole equivalent of alcohol.
c. Olefinic Alkoxvlates
The alkenyl alcohols, both primary and secondary, and alkenyl phenols
corresponding to those disclosed immediately hereinabove can ~e ethoxyiated
and used as surfactants.
Commercially available olefinic alkoxylates for use herein are available under
the
tradename Genapol O-050 from Hoechst.
d. Branched Chain Alkoxylates
Branched chain primary and secondary alcohols which may be available from the
well-known "OXO" process or modification thereof can be ethoxylated.
Particularly preferred among these ethoxylates of the primary OXO alcohols are
the surfactants marketed under the name Lutensol by BASF or Dobanol by the
Shell Chemicals, U.K., LTD. The preferred Dobanols are primary alcohols with
hydrocarbyl groups of 9 to 15 carbon atoms, with the majority having a
hydrocarbyl group of 13 carbon atoms. Particularly preferred are Dobanols with
an average degree of ethoxylation of 3 to less than 9, and preferably 5 on the
average.
An example of this type of material is an aliphatic alcohol ethylene oxide
condensate having from 3 to less than 9 moles of ethylene oxide per mole of
aliphatic alcohol, the aliphatic alcohol fraction having from 9 to 14 carbon
atoms.
Other examples of this type of nonionic surfactants include certain of the
commercially available Dobanol~, Neodol~ marketed by Shell or Lutensol~ from
BASF. For example Dobanol~ 23.5 (C 12-C 13 EOS), Dobanof~ 91.5 (C9-C 11 EO
5) and and Neodol 45 E5.
ii)- Other suitable nonionic alkoxylated surfactants are alkyl amines
alkoxylated
with at least 5 alkoxy moieties. Typical of this class of compounds are the
surfactants derived from the condensation of ethylene oxide with an
hydrophobic
alkyl amine product, Preferably the hydrophobic alkyl group, has from 6 to 22
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carbon atoms. Preferably, the alkyl amine is alkoxylated with 10 to 40, and
more
preferably 20 to 30 alkoxy moieties.
Example of this type of nonionic surfactants are the alkyl amine ethoxylate
commercially available under the tradename Genamin from Hoechst. Suitable
example for use herein are Genamin C-100, Genamin 0-150, and Genamin S-
200.
Still other suitable type of nonionic surfactant among this class are the
N,N',N'-
polyoxyethylene (12)-N-tallow 1,3 diaminopropane commercialised under the
tradename Ethoduomeen T22 from Akzo, and Synprolam from ICI.
(iii)- The block co-polymers obtained by copoiymerisation of ethylene oxide
and
propylene oxide is another suitable class of nonionic alkoxylated surfactants
suitable for use in the present invention. Typical compounds among this class
are the condensation products of ethylene oxide with a hydrophobic base formed
by the condensation of propylene oxide with propylene glycol. The hydrophobic
portion of these compounds will preferably have a molecular weight of from
1500
to 1800 and will exhibit water insolubility. The addition of polyoxyethylene
moieties to this hydrophobic portion tends to increase the water solubility of
the
molecule as a whole, and the liquid character of the product is retained up to
the
point where the polyoxyethylene content is 50% of the total weight of the
condensation product, which corresponds to condensation with up to 40 moles of
ethylene oxide. Examples of compounds of this type include certain of the
commercially available PluronicTM surfactants, marketed by BASF. For example
Pluronic PE 4300.
The above ethoxylated nonionic surfactants are useful in the present process
invention alone or in combination, and the term "nonionic surfactant"
encompasses mixed nonionic surface active agents.
A preferred class of compound for the purpose of the invention is that of
_ condensation product of aliphatic alcohol defined under i), in particular
the sub-
- class of branched chain alkoxylates. Indeed, this particular sub-class of
compound has been found more efficient for reducing the level of solvent.
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In term of principal solvent reduction, with the invention compositions, a
reduction
of at least 30% can be made without impairing the performance of the
composition compared to compositions without the nonionic alkoxylated
surfactant hereinbefore described. Using the preferred sub-class, a reduction
of
more than 50% was obtained.
II- Fabric softening compound
The composition of the invention also comprise a fabric softening compound as
an essential component.
. Typical levels of incorporation of the softening compound in the softening
composition are of from 1 % to 80% by weight, preferably from 5% to 75%, more
preferably from 15% to 70%, and even more preferably from 19% to 85%, by
weight of the composition.
The fabric softener compound is preferably selected from a cationic, nonionic,
amphoteric or anionic fabric softening component.
Typical of the cationic softening components are the quaternary ammonium
compounds or amine precursors thereof as defined hereinafter.
A)-Quaternary Ammonium Fabric Softening Active Compound
(1) Preferred quaternary ammonium fabric softening active compound have the
formula
(R ~ N (CH2~-Q-R~ X
m
(1)
or the formula:
T
(R)a.f" N (~"~,.~, - ~ - CH, - Q - R~ ?C
m
Q - R~ (2)
wherein Q is a carbonyl unit having the formula:
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-O-C- . -0-O- , -O-C-O- , R2 0 O R2
-N-C- , -C-N-
each R unit is independently hydrogen, C1-Cg alkyl, C1-Cg hydroxyalkyl, and
mixtures thereof, preferably methyl or hydroxy alkyl; each R1 unit is
independently linear or branched C11-C22 alkyl, linear or branched C11-C22
alkenyl, and mixtures thereof, R2 is hydrogen, C1-C4 alkyl, C1-C4
hydroxyalkyl,
and mixtures thereof; X is an anion which is compatible with fabric softener
actives and adjunct ingredients; the index m is from 1 to 4, preferably 2; the
index n is from 1 to 4, preferably 2.
1Q
An example of a preferred fabric softener active is a mixture of quatemized
amines having the formula:
+ O
R2-N (CH2~-O-C-R~ X -
2
wherein R is preferably methyl; R1 is a linear or branched alkyl or alkenyl
chain
comprising at least 11 atoms, preferably at least 15 atoms. In the above
fabric
softener example, the unit -02CR1 represents a fatty aryl unit which is
typically
derived from a triglyceride source. The triglyceride source is preferably
derived
from tallow, partially hydrogenated tallow, lard, partially hydrogenated lard,
vegetable oils and/or partially hydrogenated vegetable oils, such as, canola
oil,
safflower oil, peanut oil, sunflower oil, com oil, soybean oil, tall oil, rice
bran oil,
etc. and mixtures of these oils.
The preferred fabric softening actives of the present invention ace the
Diester
and/or Diamide Quaternary Ammonium (DEQA) compounds, the diesters and
diamides having the formula:
~+
(R m N (CH2)n-Q-R~ X'
m
wherein R, R 1, X, and n are the same as defined herein above for formulas ( 1
)
and (2), and D has the formula:
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H O
-N-C
These preferred fabric softening actives are formed from the reaction of an
amine
with a fatty acyl unit to form an amine intermediate having the formula:
5
R-N (CH2}n-Z
2
wherein R is preferably methyl, Z is -OH, -NH2, or mixtures thereof; followed
by
quaternization to the final softener active.
10 Non-limiting examples of preferred amines which are used to form the DEQA
fabric softening actives according to the present invention include methyl
bis(2-
hydroxyethyl)amine having the formula:
CH3
HON OOH
methyl bis(2-hydroxypropyl)amine having the formula:
C H3
N
HO OH
methyl (3-aminopropyl) (2-hydroxyethyl)amine having the formula:
CH3
HO~N~NH2
methyl bis(2-aminoethyl)amine having the formula:
CH3
HEN ~ N ~N H
triethanol amine having the formula:
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~OH
HON OOH
di(2-aminoethyl) ethanolamine having the formula:
~OH
H2N~N~NHa
The counterion, X(-) above, can be any softener-compatible anion, preferably
the anion of a strong acid, for example, chloride, bromide, methyisulfate,
ethylsulfate, sulfate, nitrate and the like, more preferably chloride or
methyl
sulfate. The anion can also, but less preferably, carry a double charge in
which
case X(-) represents half a group.
Tallow and canola oil are convenient and inexpensive sources of fatty acyl
units
which are suitable for use in the present invention as R1 units. The following
are
non-limiting examples of quaternary ammonium compounds suitable for use in
the compositions of the present invention. The term "tallowyl" as used herein
below indicates the R~ unit is derived from a tallow triglyceride source and
is a
mixture of fatty aryl units. Likewise, the use of the term canolyl refers to a
mixture of fatty acyi units derived from canola oil.
Table II
Fabric Softener Actives
N,N-di(tallowyl-oxy-ethyIrN,N-dimethyl ammonium chloride;
N,N-di(canolyl-oxy-ethyl)-N,N-dimethyl ammonium chloride;
N,N-di(tallowyl-oxy-ethyl)-N-methyl, N-(2-hydroxyethyl) ammonium
chloride;
N,N-di(canolyl-oxy-ethyl)-N-methyl, N-(2-hydroxyethyl) ammonium
chloride;
~N,N-di(2-tallowyloxy-2-oxo-ethyl)-N,N-dimethyl ammonium chloride;
N,N-di(2-canolyloxy-2-oxo-ethyl)-N,N-dimethyl ammonium chloride
N,N-di(2-tallowyloxyethyfcarbonyloxyethyl)-N,N-dimethyl ammonium
chloride;
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N,N-di(2-canolyloxyethylcarbonyloxyethyl)-N,N-dimethyl ammonium
chloride;
N-(2-tallowoyloxy-2-ethyl)-N-(2-tallowyloxy-2-oxo-ethyt)-N,N-dimethyt
ammonium chloride;
N-(2-canolyloxy-2-ethyl)-N-(2-canolyloxy-2-oxo-ethyl)-N,N-dimethyl
ammonium chloride;
N,N,N-tri(tallowyl-oxy-ethyl)-N-methyl ammonium chloride;
N,N,N-tricanolyl-oxy-ethyl)-N-methyl ammonium chloride;
N-(2-tallowyloxy-2-oxoethyl)-N-(tallowyl)-N,N-dimethyl ammonium
chloride;
N-(2-canoiyloxy-2-oxoethyl)-N-(canolyl)-N, N-dimethyl ammonium chloride;
1,2-ditaltowytoxy-3-N,N.N-trimethylammoniopropane chloride; and
1,2-dicanolyloxy-3-N,N,N-trimethylammoniopropane chloride;
and mixtures of the above actives.
Other examptes of quaternay ammoniun softening compounds are
methytbis(tallowamidoethyl)(2-hydroxyethyl)ammonium methylsulfate and
methylbis(hydrogenated tatlowamidoethyl)(2-hydroxyethyl)ammonium
methylsulfate; these materials are available from Witco Chemical Company
under the trade names Varisoft~ 222 and Varisoft~ 110, respectively.
Particularly preferred are N,N-di(canotyl-oxy-ethyl)-N,N-dimethyl ammonium
chloride and N,N-di(canolyl-oxy-ethyl)-N-methyl, N-(2-hydroxyethyl) ammonium
methyl sulfate.
The level of unsaturation contained within the tallow, canola, or other fatty
acyl
unit chain can be measured by the Iodine Value (IV) of the corresponding fatty
acid, which in the present case should preferably be in the range of from 5 to
100
with two categories of compounds being distinguished, having a IV below or
above 25.
Indeed, for compounds having the formula:
(R)4-m N (CH2~-Q-R~ X'
m
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derived from tallow fatty acids, when the Iodine Value is from 5 to 25,
preferably
15 to 20, it has been found that a cis/trans isomer weight ratio greater than
about
30/70, preferably greater than about 50/50 and more preferably greater than
about 70/30 provides optimal concentrability.
For compounds of this type made from tallow fatty acids having a Iodine Value
of
above 25, the ratio of cis to traps isomers has been found to be less critical
unless very high concentrations are needed.
Other suitable examples of fabric softener actives are derived from fatty acyi
groups wherein the terms "tallowyl" and canolyl" in the above examples are
replaced by the terms "cocoyl, palmyl, lauryl, oleyl, ricinoleyl, stearyl,
palmityl,"
- which correspond to the triglyceride source from which the fatty acyl units
are
derived. These alternative fatty acyl sources can comprise either fully
saturated,
~or preferably at least partly unsaturated chains.
As described herein before, R units are preferably methyl, however, suitable
fabric softener actives are described by replacing the term "methyl" in the
above
examples in Table II with the units "ethyl, ethoxy, propyl, propoxy,
isopropyl,
butyl, isobutyi and t-butyl.
The counter ion, X, in the examples of Table II can be suitably replaced by
bromide, methylsulfate, formate, sulfate, nitrate, and mixtures thereof. In
fact,
the anion, X, is merely present as a counterion of the positively charged
quaternary ammonium compounds. The scope of this invention is not considered
limited to any particular anion.
For the preceding ester fabric softening agents, the pH of the compositions
herein is an important parameter of the present invention. Indeed, it
influences
the stability of the quaternary ammonium or amine precursors compounds,
especially in prolonged storage conditions.
The pH, as defined in the present context, is measured in the neat
compositions
at 20 °C. While these compositions are operable at pH of less than
about 6.0, for
optimum hydrolytic stability of these compositions, the neat pH, measured in
the
above-mentioned conditions, must preferably be in the range of from about 2.0
to
about 5, preferably in the range of 2.5 to 4.5, preferably about 2.5 to about
3.5.
The pH of these compositions herein can be regulated by the addition of a
Bronsted acid.
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Examples of suitable acids include the inorganic mineral acids, carboxylic
acids,
in particular the low molecular weight (C1-C5) carboxylic acids, and
alkylsulfonic
acids. Suitable inorganic acids include HCI, H2S04, HN03 and H3P04.
Suitable organic acids include formic, acetic, citric, methylsulfonic and
ethylsulfonic acid. Preferred acids are citric, hydrochloric, phosphoric,
formic,
methylsulfonic acid, and benzoic acids.
As used herein, when the diester is specified, it will include the monoester
that is
normally present in manufacture. For softening, under no/low detergent
carry-over laundry conditions the percentage of monoester should be as low as
possible, preferably no more than about 2.5%. However, under high detergent
- carry-over conditions, some monoester is preferred. The overall ratios of
diester
to monoester are from about 100:1 to about 2:1, preferably from about 50:1 to
about 5:1, more preferably from about 13:1 to about 8:1. Under high detergent
carry-over conditions, the di/monoester ratio is preferably about 11:1. The
level
of monoester present can be controlled in the manufacturing of the softener
compound.
One preferred fabric softening compound for use in the present invention is a
compound derived from the reaction product of (partly) unsaturated fatty acid
with Triethanolamine, di-Me sulfate quaternised (as described in co-pending
application PCT/US97I09130 incorporated herein by reference).
Branched chain fatty acids that can be used in the preparation of the DEQA
fabric softening compounds herein and examples of their synthesis are
described
in copending U.S. Patent Application, Serial Number 08/679,694, of Errol H.
Wahl, Toan Trinh, Eugene P. Gosselink, and Mark R. Sivik, filed July 11, 1996
for FABRIC SOFTENING COMPOUND/COMPOSJTIONS, equivalent to
PCTIUS97/03374, said applications being incorporated herein by reference.
DEQA fabric softening compounds as described herein before and their
synthesis are described in WO 97/03169 incorporated herein by reference.
Other DEQA fabric softening compounds described herein that can be used in
the preparation of the fabric softening composition herein and having
desirable
levels of unsaturation, and their syntheses, are described in copending U.S.
Patent Application, Serial Number 08/620,775, of Errol H. Wahl, Helen B.
Tordil,
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Toan Trinh, and Eugene R. Carr, filed March 22, 1996 for CONCENTRATED
FABRIC SOFTENING COMPOSITION WITH GOOD FREEZE/THAW
RECOVERY AND UNSATURATED FABRIC SOFTENER COMPOUND
THEREFOR, equivalent to PCT/US97/05097 said applications being
5 incorporated herein by reference.
Mixtures of actives of formula ( 1 ) and (2) may also be prepared.
2)-Still other suitable quaternary ammonium fabric softening compounds for use
10 herein are cationic nitrogenous salts having two or more long chain acyclic
- aliphatic Cg-C22 hydrocarbon groups or one said group and an arylalkyl group
which can be used either alone or as part of a mixture are selected from the
group consisting of:
15 (i) acyclic quaternary ammonium salts having the formula:
R4 +
R8-N-RS A'
~s
wherein R4 is an acyctic aliphatic Cg-C22 hydrocarbon group, R5 is a C1-
C4 saturated alkyl or hydroxyalkyl group. R8 is selected from the group
consisting of R4 and R5 groups, and A- is an anion defined as above;
(ii) diamino alkoxylated quaternary ammonium salts having the formula:
+
O Rs O
II I II
R~-C-NH-R2-N-R2-NH-C-R~ A
I
(CH~CH~O~H
wherein n is equal to 1 to about 5, and R1, R2, R5 and A- are as defined
above;
(iii) mixtures thereof.
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Examples of the above class cationic nitrogenous salts are the well-9cnown
dialkyldi methyiammonium salts such as ditallowdimethylammonium chloride,
ditallowdimethylammonium methylsulfate,
di(hydrogenatedtallow)dimethylammonium chloride, distearyldimethylammonium
chloride, dibehenyldimethylammonium chloride. Di(hydrogenatedtallow)di
methylammonium chloride and ditallowdimethylammonium chloride are preferred.
Examples of commercially available dialkyldimethyl ammonium salts usable in
the present invention are di(hydrogenatedtallow)dimethylammonium chloride
(trade name Adogen~ 442}, ditallowdimethylammonium chloride (trade name
Adogen~ 470, Praepagen~ 3445), distearyl dimethylammonium chloride (trade
- name Arosurf~ TA-100), all available from Witco Chemical Company.
Dibehenyldimethylammonium chloride is sold under the trade name Kemamine
Q-2802C by Humko Chemical Division of Witco Chemical Corporation.
Dimethylstearylbenzyl ammonium chloride is sold under the trade names Varisoft
~ SDC by Witco Chemical Company and Ammonyx~ 490 by Onyx Chemical
Company.
B)-Amine Fabric SoftenindActive Compound
Suitable amine fabric softening compounds for use herein, which may be in
amine form or cationic form are selected from:
(i)- Reaction products of higher fatty acids with a polyamine selected from
the
group consisting of hydroxyalkylalkyienediamines and dialkylenetriamines and
mixtures thereof. These reaction products are mixtures of several compounds in
view of the multi-functional structure of the polyamines.
The preferred Component (i) is a nitrogenous compound selected from the group
consisting of the reaction product mixtures or some selected components of the
mixtures.
One preferred Component (i) are reaction products of substantially unsaturated
and/or branched chain higher fatty acids with diaikylenetriamines in, e.g., a
molecular ratio of about 2:1, said reaction products containing compounds of
the
formula:
3 5 R 1--C (O}-N H-R~-N H-R~--N H-C(O~.-R 1 f .
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17
wherein each R1 and R2 are defined as above, and subsequently neutralized
with an acid having the anion X-.
An example of Component (i) is reaction products of oleic acids with
diethylenetriamine in a molecular ratio of about 2:1, said reaction product
mixture
containing N,N"-dioleoyldiethylenetriamine with the formula:
R1-C(O)-NH-CH2CH2-NH-CH2CH2-NH-C(O)-R1
wherein R1-C(O) is oleoyl group of a commercially available oleic acid derived
from a vegetable or animal source, such as Emersol~ 223LL or Emersol~ 7021,
available from Henkel Corporation, and R2 and R3 are divalent ethylene groups.
Another preferred component (i) is a compound of formula:
[R1-C(O}-NR-RZ--NRH-R~-NR--C(O)--R1J+ A-
wherein each R, R1, R2, and A- are defined as above.
An example of Compound (i) is a difatty amidoamine based softener having the
formula:
[R1-C(O)-NH-CH2CH2-NH(CH2CH20H)-CH2CH2-NH-C(O)-R1)+ Ch
wherein R1-C(O) is oleoyi group.
Still another preferred component (i) is a compound selected from the group
consisting of substituted imidazoline compounds having the formula:
N
R~--~
N
I
R8-NH-C-R7
I I
~
wherein R7 is an acyclic aliphatic C15-C21 hydrocarbon group and R8 is a
divalent C1-Cg alkylene group.
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18
Component (i) materials are commercially available as: Mazamide~ 6, sold by
Mater Chemicals, or Ceranine~ HC, sold by Sandoz Colors 8 Chemicals; stearic
hydroxyethyl imidazoiine sold under the trade names of Alkazine~ ST by Alkaril
Chemicals, inc., or Schercozoline~ S by Scher Chemicals, Inc.; N,N"-
ditallowalkoyldiethylenetriamine; 1-tallowamidoethyl-2-tallowimidazoiine
(wherein
in the preceding structure R1 is an aliphatic C15-C17 hydrocarbon group and R8
is a divalent ethylene group).
Certain of the Components (i) can also be first dispersed in a Bronsted acid
dispersing aid having a pKa value of not greater than about 4; provided that
the
- pH of the final composition is not greater than about 6. Some preferred
dispersing aids are hydrochloric acid, phosphoric acid, or methyisulfonic
acid.
Both N,N"-ditailowalkoyldiethylenetriamine and 1-tallow(amidoethyl)-2-
tallowimidazoline are reaction products of tallow fatty acids and
diethylenetriamine, and are precursors of the cationic fabric softening agent
methyl-1-tallowamidoethyl-2-tallowimidazolinium methylsulfate (see "Cationic
Surface Active Agents as Fabric Softeners," R. R. Egan. Journal of the
American
Oil Chemicals' Society, January 1978, pages 118-121). N,N"-ditallow
alkoyldiethylenetriamine and 1-tallowamidoethyl-2-tallowimidazoline can be
obtained from Witco Chemical Company as experimental chemicals. Methyl-1-
tallowamidoethyl-2-tallowimidazolinium methylsulfate is sold by Witco Chemical
Company under the tradename Varisoft~ 475.
(ii)-softener having the formula:
N ~..p
R~
C
O
N CZ-Q ?C~
Rs
R~ C G R2
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19
wherein each R2 is a C1-g alkylene group, preferably an ethylene group; and G
is an oxygen atom or an -NR- group; and each R, R1, Rr2 and R5 have the
definitions given above and A- has the definitions given above for X'.
An example of Compound (ii) is 1-oleylamidoethyl-2-oleylimidazolinium chloride
wherein R1 is an acyclic aliphatic C15-C17 hydrocarbon group, R2 is an
ethylene
group, G is a NH group, R5 is a methyl group and A- is a chloride anion.
(iii)- the reaction product of substantially unsaturated and/or branched chain
higher fatty acid with triethanolamine, and subsequently neutralized with an
acid
having the anion A-.
An example of Compound (iii) is reaction products of oleic acids with N-2-
hydroxyethylethylenediamine in a molecular ratio of about 2:1, said reaction
product mixture containing a compound of the formula:
R1-C(O)-NH-CH2CH2-N(CH2CH20H)-C(O)-R1
wherein R 1-C(O) is oleoyl group of a commercially available oleic acid
derived
from a vegetable or animal source, such as Emersol~ 223LL or Emersol~ 7021,
available from Henkel Corporation.
(iv) softener having the formula:
H H
\N-Rz-N
N~ IV 2A~
Ri Ri
wherein R, R1, R2, and A- are defined as above.
An example of Compound (iv) is the compound having the formula:
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~O+
H H
N CH~CH~ N I C1
N~ ~N
R' R~
wherein R1 is derived from oleic acid.
Additional fabric softening agents useful herein are described in U.S. Pat.
No.
5 4,661,269, issued April 28, 1987, in the names of Toan Trinh, Errol H. Wahl,
Donald M. Swartfey, and Ronald L. Hemingway; U.S. Pat. No. 4,439,335, Bums,
- issued March 27, 1984; and in U.S. Pat. Nos.: 3,861,870, Edwards and Diehl;
4,308,151, Cambre; 3,886,075, Bemardino; 4,233,164, Davis; 4,401,578,
Verbruggen; 3,974,076, Wiersema and Rieke; 4,237,016, Rudkin, Clint, and
10 Young; and European Patent Application publication No. 472,178, by Yamamura
et al., all of said documents being incorporated herein by reference.
Of course, the term "softening active" can also encompass mixed softening
active agents.
15 Preferred among the classes of softener compounds disclosed herein before
are
the diester or diamido quaternary ammonium fabric softening active compound
(DEQA).
The fabric softener actives herein described are employed in clear or
translucent
20 formulations.
III-Principal solvent
A principal soivent is another essential ingredient for use in the present
composition invention. The principal solvent is typically used at a level of
less
than 40% by weight, preferably from 5% to 25%, more preferably from 6% to
12%, by weight of the composition. An advantage of the present invention is
that
the use of the specific nonionic enables the use of a lower level of solvents,
that
is of less than 15% by weight of the composition, which is preferred for
odour,
safety and economy reasons. Furthermore, it has been found that in the absence
of the nonionic as defined hereinbefore, this low level of principal solvent
is
insufficient to provide good clarity of the composition. In contrast, when the
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21
nonionic is used in addition to this low level of principal solvent, a
composition
with good clarity is obtained. In preferred compositions, the level of
principal
solvent is insufficient to provide the required degree of clarity andlor
stability and
the addition of the nonionic surfactant provides the desired
clarity/stability.
The principal solvent is selected to minimize solvent odor impact in the
composition and to provide a low viscosity to the final composition. For
example,
isopropyl alcohol is not very effective and has a strong odor. n-Propyi
alcohol is
more effective, but also has a distinct odor. Several butyl alcohols also have
odors but can be used for effective claritylstability, especially when used as
part
of a principal solvent system to minimize their odor. The alcohols are also
selected for optimum low temperature stability, that is they are able to form
compositions that are liquid with acceptable low viscosities and translucent.
preferably clear, down to 40°F (4.4°C)~ and are able to recover
after storage down
to 20°F (6.7°C).
The suitability of any principal solvent for the formulation of the liquid,
preferably
clear, fabric softener compositions herein with the requisite stability is
surprisingly
selective. Suitable solvents can be selected based upon their octanol/water
partition coefficient (P). Octanol/water partition coefficient of a principal
solvent is
the ratio between its equilibrium concentration in octanof and in water. The
partition coefficients of the principal solvent ingredients of this invention
are
conveniently given in the form of their logarithm to the base 10, IogP.
The IogP of many ingredients has been reported; for example, the Pomona92
database, available from Daylight Chemical Information Systems, Inc. (Daylight
CIS), Irvine, California, contains many, along with citations to the original
literature. However, the IogP vatues are most conveniently calculated by the
"CLOGP" program, also available from Daylight CIS. This program also lists
experimental IogP values when they are available in the Pomona92 database.
The "calculated IogP" (CIogP) is determined by the fragment approach of Hansch
and Leo (cf., A. Leo, in Comprehensive Medicinal Chemistry, Vol. 4, C. Hansch,
P. G. Sammens, J. B. Taylor and C. A. Ramsden, Eds., p. 295, Pergamon Press,
1990,. incorporated herein by reference). The fragment approach is based on
the
chemical structure of each ingredient, and takes into account the numbers and
types of atoms, the atom connectivity, and chemical bonding. These CIogP
values, which are the most reliable and widely used estimates for this
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22
physicochemical property, are preferably used instead of the experimental IogP
values in the selection of the principal solvent ingredients which are useful
in the
present invention. Other methods that can be used to compute CIogP include,
e.g., Crippen's fragmentation method as disclosed in J. Chem. Inf. Comput.
Sci.,
27, 21 (1987); Viswanadhan's fragmentation method as disclose in J. Chem. Inf.
Comput. Sci., 29, 163 (1989); and Broto's method as disclosed in Eur. J. Med.
Chem. - Chim. Theor., 19, 71 (1984). The principal solvents herein are
selected
from those having a CIogP of from 0.15 to 1.0, preferably from 0.15 to 0.64,
more
preferably from 0.25 to 0.62, and most preferably from 0.40 to 0.60, said
principal
solvent preferably being at least somewhat asymmetric, and preferably having a
- melting, or solidification, point that allows it to be liquid at, or near
room
temperature. Solvents that have a low molecular weight and are biodegradable
are also desirable for some purposes. The more assymetric solvents appear to
be very desirable, whereas the highly symmetrical solvents such as 1,7
heptanediol, or 1,4-bis(hydroxymethyl) cyclohexane, which have a center of
symmetry, appear to be unable to provide the essential clear compositions when
used alone, even though their CIogP values fall in the preferred range.
The most preferred principal solvents can be identified by the appearance of
the
softener vesicles, as observed via cryogenic electron microscopy of the
compositions that have been diluted to the concentration used in the rinse.
These dilute compositions appear to have dispersions of fabric softener that
exhibit a more , unilamellar appearance than conventional fabric softener
compositions. The closer to uni-lamellar the appearance, the better the
compositions seem to perform. These compositions provide surprisingly good
fabric softening as compared to similar compositions prepared in the
conventional way with the same fabric softener active.
Operable principal solvents are disclosed and listed below which have CIogP
values which fall within the requisite range. These include mono-ols, C6
diols, C7
diols, octanediol isomers, butanediol derivatives, trimethylpentanediol
isomers,
ethylmethylpentanediol isomers, propyl pentanediol isomers, dimethylhexanediol
isomers, ethylhexanediol isomers, methyiheptanediol isomers, octanediol
isomers, nonanediol isomers, alkyl glyceryl ethers, di(hydroxy alkyl) ethers,
and
aryl glyceryl ethers, aromatic glyceryl ethers, alicyclic diois and
derivatives, C3C7
diol alkoxylated derivatives, aromatic diols, and unsaturated diols. These
principal solvents are all disclosed in WO 97/03169 having the title
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23
"CONCENTRATED, STABLE, PREFERABLY CLEAR, FABRIC SOFTENING
COMPOSITION" incorporated herein by reference.
Particularly preferred principal solvents include hexanediols such as 1,2-
hexanediol; and C8 diols such as 2-ethyl-1,3-hexanedioi and 2,2,4-trimethyl-
1,3-
pentanediot, ethoxylates of 2,2,4-trimethyl-1,3-pentanediol and ethoxyiates of
2-
ethyl-1,3-hexanediof; phenoxyethanol and 1,2 cyclohexanedimethanol. Most
preferred principal solvents for use herein are selected from 2,2,4-trimethyl-
1,3-
pentanediol, ethoxyiates of 2,2,4-trimethyl-1,3-pentanediol, 1,2 hexanediol, 2-
ethyl-1,3-hexanediol, phenoxyethanol, butyl carbitol and mixtures thereof.
Even
most preferred principal solvents for use herein are selected from 2,2,4-
trimethyl-
1,3-pentanediol, ethoxylates of 2,2,4-trimethyl-1,3-pentanediol, 1,2
hexanediol,
' 2-ethyl-1, 3-hexanediol, phenoxyethanol, and mixtures thereof. Mixtures of
principal solvents can also be used for the purpose of the present invention.
The principal solvents are desirably kept to the lowest levels that are
feasible in
the present compositions for obtaining translucency or clarity. The presence
of
water exerts an important effect on the need for the principal solvents to
achieve
clarity of these compositions. The higher the water content, the higher the
principal solvent level (relative to the softener level) is needed to attain
product
clarity. Inversely, the less the water content, the less principal solvent
(relative to
the softener) is needed. Thus, at low water levels of from 5% to 15%, the
softener active-to-principal solvent weight ratio is preferably from 55:45 to
95:5,
more preferably from 60:40 to 90:10. At water levels of from 15% to 70%, the
softener active-to-principal solvent weight ratio is preferably from 45:55 to
90:10,
more preferably from 55:45 to 85:15. But at high water levels of from 70% to
80%, the softener active-to-principal solvent weight ratio is preferably from
30:70
to 80:20, more preferably from 35:65 to 75:25. At even higher water levels,
the
softener to principal solvent ratios should also be even higher.
The compositions can also inherently provide improved perfume deposition of
certain perfume components, especially for those that are pooriy fabric
substantive as compared to conventional fabric softening compositions,
especially when the perfume is added to the compositions at, or near, room
temperature
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24
More preferred for use herein is a combination of principal solvents. Most
preferred combinations are 2,2,4-trimethyl-1,3-pentanediol (TMPD) in
combination with 1,2 hexanediol or 2- ethyl 7 ,3 hexanediol. With the above
preferred combinations, lower total levels of solvents can be achieved thereby
further reducing the overall cost of the formulation. By the present principal
solvent combinations, it has been found that the resulting products have
increased phase stability and fully recover from free2ing down to 0°F (-
18°C).
The resulting products have also been surprisingly found to have excellent
water
dispersibility.
When in such clear or transluscent liquid forms, it has been found most
- preferred, in order to improve the stability of the softening composition
according
to the invention, that the softening compositions have a pH of from 2 to 5,
preferably 2.5 to 4.
Fully formulated fabric softening compositions may contain, in addition to the
hereinbefore described components, one or more of the following ingredients.
IV-Optional ingredients
(A)- Low molecular weight water soluble solvents
Low molecular weight water soluble solvents can also be used at levels of from
0% to 12%, preferably from 1 % to 10%, more preferably from 2% to 8% by
weight. The water soluble solvents cannot provide a clear product at the same
low levels of the principal solvents described hereinbefore but can provide
clear
product when the principal solvent is not sufficient to provide completely
clear
product. The presence of these water soluble solvents is therefore highly
desirable. Such solvents include: ethanol; isopropanol; propylene gfycoi;1,2-
propanediol; 1,3-propanediol; propylene carbonate; 1.4 cyclohexanedimethanol;
etc. but do not include any of the principal solvents (A). These water soluble
solvents have a greater affinity for water in the presence of hydrophobic
materials like the softener compound than the principal solvents.
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Among the above described co-solvent to be used in combination with the
principal solvent, 1,4 cyclohexanedimethanol and/or ethanol are preferred co-
solvents.
5 !81-Brighteners
The compositions herein can also optionally contain from 0.005% to 5% by
weight of certain types of hydrophilic optical brighteners which also provide
a dye
transfer inhibition action. If used, the compositions herein will preferably
comprise from 0.001 % to 1 % by weight of such optical brighteners.
10 The hydrophilic optical brighteners useful in the present invention are
those
having the structural formula:
R~ R2
N H H N
N ~~-N O C C O
H H
R2 S03M S~3M Ri
wherein R1 is selected from anilino, N-2-bis-hydroxyethyl and NH-2-
hydroxyethyl;
15 R2 is selected from N-2-bis-hydroxyethyl, N-2-hydroxyethyl-N-methylamino,
morphilino, chloro and amino; and M is a salt-forming ration such as sodium or
potassium.
When in the above formula, R1 is anilino, R2 is N-2-bis-hydroxyethyl and M is
a
ration such as sodium, the brightener is 4,4',-bis[(4-anilino-6-(N-2-bis
20 hydroxyethyl)-s-triazine-2-yl)amino]-2,2'-stilbenedisulfonic acid and
disodium salt.
This particular brightener species is commercially marketed under the
tradename
Tinopal-UNPA-GX~ by Ciba-Geigy Corporation. Tinopal-UNPA-GX is the
preferred hydrophilic optical brightener useful in the rinse added
compositions
herein.
25 When in the above formula, R1 is anilino, R2 is N-2-hydroxyethyl-N-2-
methylamino and M is a ration such as sodium, the brightener is 4,4'-bis[(4-
anilino-6-(N-2-hydroxyethyl-N-methylamino)-s-triazine-2-yl)amino]2,2'-
stilbenedisulfonic acid disodium salt. This particular brightener species is
commercially marketed under the tradename Tinopal 5BM-GX~ by Ciba-Geigy
Corporation.
When in the above formula, R1 is anilino, R2 is morphilino and M is a ration
such
as sodium, _ . the brightener is 4,4'-bis[(4-anilino-6-morphilino-s-triazine-2-
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2s
yl)aminoJ2,2'-stilbenedisulfonic acid, sodium salt. This particular brightener
species is commercially marketed under the tradename Tinopal AMS-GX~ by
Ciba Geigy Corporation.
(C)-Dis ersibility Aids
Relatively concentrated compositions containing both saturated and unsaturated
diester quaternary ammonium compounds can be prepared that are stable
without the addition of concentration aids. However., the compositions of the
present invention may require organic andlor inorganic concentration aids to
go
to even higher concentrations andlor to meet higher stability standards
depending on the other ingredients. These concentration aids which typically
can be viscosity modifiers may be needed, or preferred, for ensuring stability
under extreme conditions when particular softener active levels are used. The
surfactant concentration aids are typically selected from the group consisting
of
(1) single long chain alkyl cationic surfactants; (2) nonionic surfactants;
(3) amine
oxides; (4) fatty acids; and (5) mixtures thereof. These aids are described in
P8~G Copending Application Serial No. 08/461,207, filed June 5, 1995, Wahl et
al., specifically on page 14, line 12 to page 20, line 12, which is herein
incorporated by reference.
When said dispersibility aids are present , the total level is from 2% to 25%,
preferably from 3% to 17%, more preferably from 4% to 15%, and even more
preferably from 5% to 13% by weight of the composition. These materials can
either be added as part of the active softener raw material, (I), e.g., the
mono-
long chain alkyl cationic surfactant andlor the fatty acid which are reactants
used
to form the biodegradable fabric softener active as discussed hereinbefore, or
added as a separate component. The total level of dispersibility aid includes
any
amount that may be present as part of component (I).
(1 ) Mono-Alkyl Cationic Quaternary Ammonium Compound
When the mono-alkyl cationic quaternary ammonium compound is present, it is
typically present at a level of from 2% to 25%, preferably from 3% to 17%,
more
preferably from 4% to 15%, and even more preferably from 5% to 13% by weight
of the composition, the total mono-alkyl cationic quaternary ammonium
compound being at least at an effective level.
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27
Such mono-alkyl cationic quaternary ammonium compounds useful in the
present invention are, preferably, quaternary ammonium salts of the general
formula:
~R4N+(R5)31 X_
wherein
R4 is Cg-C22 alkyl or alkenyl group, preferably C10-C1g alkyl or afkenyl
group;
more preferably C 10-C 14 or C 1 g-C 1 g alkyl or alkenyl group;
each R5 is a C1-Cg alkyl or substituted alkyl group (e.g., hydroxy alkyl),
preferably C1-C3 alkyl group, e.g., methyl (most preferred), ethyl, propyl,
and the
like, a benzyl group, hydrogen, a polyethoxylated chain with from 2 to 20
oxyethylene units, preferably from 2.5 to 13 oxyethylene units, more
preferably
from 3 to 10 oxyethylene units, and mixtures thereof; and
X- is as defined hereinbefore for (Formula (I)).
Especially preferred dispersibility aids are monolauryl trimethyl ammonium
chloride and monotallow trimethyl ammonium chloride available from Witco under
the trade names Adogen~ 412 and Adogen~ 471, monooleyi or monocanola
trimethyl ammonium chloride available from Witco under the tradename Adogen
~ 417, monococonut trimethyl ammonium chloride available from Witco under
the trade name Adogen~ 4fi1, and monosoya trimethyl ammonium chloride
available from Witco under the trade name Adogen~ 415.
The R4 group can also be attached to the cationic nitrogen atom through a
group
containing one, or more, ester, amide, ether, amine, etc., linking groups
which
can be desirable for increased concentratability of component (I), etc. Such
linking groups are preferably within from one to three carbon atoms of the
nitrogen atom.
Mono-alkyl cationic quaternary ammonium compounds also include C8-C22 alkyl
choline esters. The preferred dispersibility aids of this type have the
formula:
R1C(O)-O-CH2CH2N+(R)3 X-
wherein R1, R and X- are as defined previously.
Highly preferred dispersibility aids include C12-C14 coco choiine ester and
C16-
C1g tallow choline ester.
Suitable biodegradable single-long-chain alkyl dispersibility aids containing
an
ester linkage in the long chains are described in U.S. Pat. No. 4,840,738,
Hardy
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28
and Walley, issued June 20, 1989, said patent being incorporated herein by
reference.
When the dispersibility aid comprises alkyl choline esters, preferably the
compositions also contain a small amount, preferably from 2% to 5% by weight
of
the composition, of organic acid. Organic acids are described in European
Patent Application No. 404,471, Machin et al., published on Dec. 27, 1990,
supra, which is herein incorporated by reference. Preferably the organic acid
is
selected from the group consisting of glycolic acid, acetic acid, citric acid,
and
mixtures thereof.
Ethoxylated quaternary ammonium compounds which can serve as the
- dispersibility aid include ethylbis(polyethoxy ethanol)alkylammonium ethyl-
sulfate
with 17 moles of ethylene oxide, available under the trade name Variquat~ 66
from Witco Corporation; polyethylene glycol (15) oleammonium chloride,
available under the trade name Ethoquad~ 0/25 from Akzo; and polyethylene
glycol (15) cocomonium chloride, available under the trade name Ethoquad~
C/25 from Akzo.
Quaternary compounds having only a single long alkyl chain, can protect the
cationic softener from interacting with anionic surfactants and/or detergent
builders that are carried over into the rinse from the wash solution.
(2) Nonionic Surfactant (Alkoxylated Materials)
Suitable nonionic surfactants to serve as the viscosityldispersibility
modifier
include addition products of ethylene oxide and, optionally, propylene oxide,
with
fatty alcohols, fatty acids, fatty amines, etc. They are referred to herein as
ethoxylated fatty atcohols, ethoxyiated fatty acids, and ethoxylated fatty
amines.
Any of the alkoxylated materials of the particular type described hereinafter
can
be used as the nonionic surfactant. In general terms, the nonionics herein,
when
used alone, in liquid compositions are at a level of from 0% to 5%, preferably
from 0.1 % to 5%, more preferably from 0.2% to 3%. Suitable compounds are
substantially water-soluble surfactants of the general formula:
R2 - Y - (C2H40)Z - C2H40H
wherein R2 for both solid and liquid compositions is selected from the group
consisting of primary, secondary and branched chain alkyl andlor acyl
hydrocarbyl groups; primary, secondary and branched chain alkenyl hydrocarbyl
groups; and primary, secondary and branched chain alkyl- and
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29
alkenyi-substituted phenolic hydrocarbyl groups; said hydrocarbyl groups
having
a hydrocarbyl chain length of from 8 to 20, preferably from 10 to 18 carbon
atoms. More preferably the hydrocarbyl chain length for liquid compositions is
from 16 to 18 carbon atoms and for solid compositions from 10 to 14 carbon
atoms. In the general formula for the ethoxylated nonionic surfactants herein,
Y
is typically -O-, -C(O)O-, preferably -O-, and in which R2, when present, have
the meanings given hereinbefore, and z is at least 8, preferably at least 10-
11.
Performance and, usually, stability of the softener composition decrease when
fewer ethoxylate groups are present.
The nonionic surfactants herein are characterized by an HLB
(hydrophilic-lipophilic balance) of from 7 to 20, preferably from 8 to 15. Of
course, by defining R2 and the number of ethoxylate groups, the HL8 of the
surfactant is, in general, determined. However, it is to be noted that the
nonionic
ethoxylated surfactants useful herein, for concentrated liquid compositions,
contain relatively long chain R2 groups and are relatively highly ethoxylated.
While shorter alkyl chain surfactants having short ethoxylated groups can
possess the requisite HLB, they are not as effective herein.
Nonionic surfactants as the viscosity/dispersibility modifiers are preferred
over
the other modifiers disclosed herein for compositions with higher levels of
perfume.
(3) Amine Oxides
Suitable amine oxides include those with one alkyl or hydroxyalkyi moiety of 8
to
22 carbon atoms, preferably from 10 to 18 carbon atoms, more preferably from 8
to 14 carbon atoms, and two alkyl moieties selected from the group consisting
of
alkyl groups and hydroxyalkyl groups with 1 to 3 carbon atoms.
Examples include dimethyloctylamine oxide, diethyidecytamine oxide, bis-(2-
hydroxyethyi)dodecyl-amine oxide, dimethyldodecylamine oxide, dipropyl-
tetradecylamine oxide, methylethylhexadecylamine oxide, dimethyl-2-
hydroxyoctadecylamine oxide, and coconut fatty alkyl dimethylamine oxide.
(D)-Stabilizers
Stabilizers can be present in the compositions of the present invention. The
term
"stabilizer," as used herein, includes antioxidants and reductive agents.
These
agents are present at a level of from 0% to 2%, preferably from 0.01% to 0.2%.
more preferably from 0.035% to 0.1 % for antioxidants, and more preferably
from
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0.01 % to 0.2% for reductive agents. These assure good odor stability under
long
term storage conditions. Antioxidants and reductive agent stabilizers are
especially critical for unscented or low scent products (no or low perfume).
Examples of antioxidants that can be added to the compositions of this
invention
5 include a mixture of ascorbic acid, ascorbic palmitate, propyl gallate,
available
from Eastman Chemical Products, Inc., under the trade names Tenox~ PG and
Tenox~ S-1; a mixture of BHT (butylated hydroxytoluene), BHA (butylated
hydroxyanisole), propyl gallate, and citric acid, available from Eastman
Chemical
Products, Inc., under the trade name Tenox~l-6; butylated hydroxytoluene,
avail-
10 able from UOP Process Division under the trade name Sustane~ BHT; tertiary
- butylhydroquinone, Eastman Chemical Products, Inc., as Tenox~ TBHQ; natural
tocopherois, Eastman Chemical Products, Inc., as Tenox~ GT-1/GT-2; and
butylated hydroxyanisole, Eastman Chemical Products, Inc., as BHA; long chain
esters (C8-C22) of gallic acid, e.g., dodecyl gallate; trganox~ 1010; Irganox~
15 1035; Irganox~ B 1171; Irganox~ 1425; Irganoxx~l 3114; Irganox~ 3125; and
mixtures thereof; preferably Irganox~ 3125, Irganox~ 1425, Irganox~ 3114, and
mixtures thereof; more preferably Irganox~ 3125 alone or mixed with citric
acid
and/or other chelators such as isopropyl citrate, Dequest~ 2010, available
from
Monsanto with a chemical name of 1-hydroxyethylidene-1, 1-diphosphonic acid
20 (etidronic acid), and Tiron~, available from Kodak with a chemical name of
4,5-
dihydroxy-m-benzene-sulfonic acidlsodium salt, and DTPA~, available from
Aldrich with a chemical name of diethylenetriaminepentaacetic acid.
(E)-Soil Release Aaent
25 In the present invent'ron, an optional soil release agent can be added. The
addition of the soil release agent can occur in combination with the premix,
in
combination with the acid/water seat, before or after electrolyte addition, or
after
the final composition is made. The softening composition prepared by the
process of the present invention herein can contain from 0% to 10%, preferably
30 from 0.2% to 5%, of a soil release agent. Preferably, such a soil release
agent is
a polymer. Polymeric soil release agents useful in the present invention
include
copolymeric blocks of terephthalate and polyethylene oxide or polypropylene
oxide, 'and the like.
A preferred soil release agent is a copolymer having blocks of terephthalate
and
polyethylene oxide: More specifically, these polymers are comprised of
repeating units of ethylene terephthalate and polyethylene oxide terephthalate
at
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31
a molar ratio of ethylene terephthalate units to polyethylene oxide
terephthaiate
units of from 25:75 to 35:65, said polyethylene oxide terephthalate containing
polyethylene oxide blocks having molecular weights of from 300 to 2000. The
molecular weight of this polymeric soil release agent is in the range of from
5,000
to 55,000.
Another preferred polymeric soil release agent is a crystallizable polyester
with
repeat units of ethylene terephthalate units containing from 10% to 15% by
weight of ethylene terephthalate units together with from 10% to 50% by weight
of polyoxyethylene terephthalate units, derived from a polyoxyethylene glycol
of
average molecular weight of from 300 to 6,000, and the molar ratio of ethylene
terephthalate units to polyoxyethylene terephthalate units in the
crystallizable
polymeric compound is between 2:1 and 6:1. Examples of this polymer include
the commercially available materials Zelcon 4780~ (from Dupont) and Milease T
~ (from ICI). .
Highly preferred soil release agents are polymers of the generic formula:
O
X- OCH CH O-O-R14 C ~-OR15 O 14
( 2 2)p( )u(O-C-R -OC-0)(CH2CH20-)n-X
in which each X can be a suitable capping group, with each X typically being
selected from the group consisting of H, and alkyl or acyl groups containing
from
1 to 4 carbon atoms. p is selected for water solubility and generally is from
6 to
113, preferably from 20 to 50. a is critical to formulation in a liquid
composition
having a relatively high ionic strength. There should be very little material
in
which a is greater than 10. Furthermore, there should be at least 20%,
preferably at least 40%, of material in which a ranges from 3 to 5.
The R14 moieties are essentially 1,4-phenylene moieties. As used herein, the
term "the R14 moieties are essentially 1,4-phenylene moieties" refers to
compounds where the R14 moieties consist entirely of 1,4-phenylene moieties,
or are ~ partially substituted with other arylene or alkarylene moieties,
alkylene
moieties, alkenylene moieties, or mixtures thereof. Arylene and alkarylene
moieties which can be partially substituted for 1,4-phenylene include 1,3-
phenytene, 1,2-phenylene, 1,8-naphthylene. 1,4-naphthylene, 2,2-biphenylene,
4,4-biphenylene, and mixtures thereof. Alkylene and alkenylene moieties which
can be partially substituted include 1,2-propylene, 1,4-butylene, 1,5-
pentyiene,
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32
1,6-hexamethylene, 1,7-heptamethyiene, 1, 8-octamethylene, 1,4-cyclohexylene,
and mixtures thereof.
For the R14 moieties, the degree of partial substitution with moieties other
than
1,4-phenylene should be such that the soil release properties of the compound
are not adversely affected to any great extent. Generally the degree of
partial
substitution which can be tolerated will depend upon the backbone length of
the
compound, i.e., longer backbones can have greater partial substitution for 1,4-
phenylene moieties. Usually, compounds where the R14 comprise from 50% to
100% 1,4-phenylene moieties (from 0% to 50% moieties other than 1,4-
phenylene) have adequate soil release activity. For example, polyesters made
according to the present invention with a 40:60 mole ratio of isophthalic (1,3-
phenylene) to terephthalic (1,4-phenytene) acid have adequate soil release
activity. However, because most polyesters used in fiber making comprise
ethylene terephthalate units, it is usually desirable to minimize the degree
of
partial substitution with moieties other than 1,4-phenylene for best soit
release
activity. Preferably, the R14 moieties consist entirely of (i.e., comprise
100%)
1,4-phenylene moieties, i.e., each R14 moiety is 1,4-phenylene.
For the R15 moieties, suitable ethylene or substituted ethylene moieties
include
ethylene, 1,2-propylene, 1,2-butylene, 1,2-hexylene, 3-methoxy-1,2-propylene,
and mixtures thereof. Preferably, the R15 moieties are essentially ethylene
moieties, 1,2-propylene moieties, or mixtures thereof. Inclusion of a greater
percentage of ethylene moieties tends to improve the soil release activity of
compounds. Surprisingly, inclusion of a greater percentage of 1,2-propylene
moieties tends to improve the water solubility of compounds.
Therefore, the use of 1,2-propylene moieties or a similar branched equivalent
is
desirable for incorporation of any substantial part of the soil release
component
in the liquid fabric softener compositions. Preferably, from 75% to 100%, are
1,2-
propylene moieties.
The value for each p is at least 6, and preferably is at least 10. The value
for
each n usually ranges from 12 to 113. Typically the value for each p is in the
range of from 12 to 43.
A more complete disclosure of soil release agents is contained in U.S. Pat.
Nos.:
4,661,267; 4,711,730; 4,749,596; 4,818,569; 4,877,896; 4,956,447; and
4,976,879, all of said patents being incorporated herein by reference.
These soil release agents can also act as scum dispersants.
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33
(F)-Scum Disaersant
In the present invention, the premix can be combined with an optional scum
dispersant, other than the soil release agent, and heated to a temperature at
or
above the melting points) of the components.
The preferred scum dispersants herein are formed by highly ethoxylating
hydrophobic materials. The hydrophobic material can be a fatty alcohol, fatty
acid, fatty amine, fatty acid amide, amine oxide, quaternary ammonium
compound, or the hydrophobic moieties used to form soil release polymers. The
preferred scum dispersants are highly ethoxylated, e.g., more than 17,
preferably
more than 25, more preferably more than 40, moles of ethylene oxide per
molecule on the average, with the polyethylene oxide portion being from 76% to
97%, preferably from 81 % to 94%, of the total molecular weight.
The level of scum dispersant is sufficient to keep the scum at an acceptable,
preferably unnoticeable to the consumer, level under the conditions of use,
but
not enough to adversely affect softening. For some purposes it is desirable
that
the scum is nonexistent. Depending on the amount of anionic or nonionic
detergent, etc., used in the wash cycle of a typical laundering process, the
efficiency of the rinsing steps prior to the introduction of the compositions
herein,
and the water hardness, the amount of anionic or nonionic detergent surfactant
and detergency builder (especially phosphates and zeolites) entrapped in the
fabric (laundry) will vary. Normally, the minimum amount of scum dispersant
should be used to avoid adversely affecting softening properties. Typically
scum
dispersion requires at least 2%, preferably at least 4% (at least 6% and
preferably at least 10% for maximum scum avoidance) based upon the level of
softener active. However, at levels of 10% (relative to the softener material)
or
more, one risks loss of softening efficacy of the product especially when the
fabrics contain high proportions of nonionic surfactant which has been
absorbed
during the washing operation.
Preferred scum dispersants are: Brij 700~; Varonic U-250~; Genapol T-500~,
Genapol T-800~; Plurafac A-79~; and Neodol 25-50~.
(G)-Bactericides
Examples of bactericides used in the compositions of this invention include
glutaraldehyde, formaldehyde, 2-bromo-2-vitro-propane-1,3-diol sold by Inolex
Chemicals, located in Philadelphia, Pennsylvania, under the trade name
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34
Bronopol~, and a mixture of 5-chloro-2-methyl-4-isothiazoline-3-one and 2-
methyl-4-isothiazoline-3-one sold by Rohm and Haas Company under the trade
name Kathon 1 to 1,000 ppm by weight of the agent.
(H)-Perfume
The present invention can contain any softener compatible perfume. Suitable
perfumes are disclosed in U.S. Pat. 5,500,138, said patent being incorporated
herein by reference.
As used herein, perfume includes fragrant substance or mixture of substances
including natural (i.e., obtained by extraction of flowers, herbs, leaves,
roots,
barks, wood, blossoms or plants), artificial (i.e., a mixture of different
nature oils
or oil constituents) and synthetic (i.e., synthetically produced) odoriferous
substances. Such materials are often accompanied by auxiliary materials, such
as fixatives, extenders, stabilizers and solvents. These auxiliaries are also
included within the meaning of "perfume", as used herein. Typically, perfumes
are complex mixtures of a plurality of organic compounds.
Examples of perfume ingredients useful in the perfumes of the present
invention
compositions include, but are not limited to, hexyl cinnamic aldehyde: amyl
cinnamic aldehyde; amyl salicylate; hexyl salicylate; terpineol; 3,7-dimethyl-
cis-
2,6-octadien-1-ol; 2,6-dimethyl-2-octanol; 2,6-dimethyl-7-octen-2-ol; 3,7-
dimethyl-
3-octanol; 3,7-dimethyl-traps-2,6-octadien-1-ol; 3,7-dimethyl-6-octen-1-ol;
3,7-
dimethyl-1-octanol; 2-methyl-3-(para-tert-butylphenyl)-propionaldehyde; 4-(4-
hydroxy-4-methyipentyl)-3-cyclohexene-1-carboxaldehyde; tricyciodecenyl
propionate; tricyctodecenyl acetate; anisaldehyde; 2-methyl-2-(para-iso-
propylphenyl)-propionaldehyde; ethyl-3-methyl-3-phenyl glycidate; 4-(para-
hydroxyphenyl)-butan-2-one; 1-(2,6,6-trimethyl-2-cyctohexen-1-yl)-2-buten-1-
one;
para-methoxyacetophenone; pare-methoxy-alpha-phenylpropene; methyl-2-n-
hexyl-3-oxo-cyclopentane carboxyfate; undecalactone gamma.
Additional examples of fragrance materials include, but are not limited to,
orange
oil; lemon oil; grapefruit oil; bergamot oil; clove oil; dodecalactone gamma;
methyl-2-(2-pentyl-3-oxo-cyciopentyl) acetate; beta-naphthol methylether;
methyl-beta-naphthylketone; coumarin; decylaldehyde; benzaldehyde; 4-tert
butylcyclohexyl acetate; alpha,alpha-dimethylphenethyl acetate;
methylphenyicarbinyl acetate; Schiffs base of 4-(4-hydroxy-4-methylpentyl)-3
cyclohexene-1-carboxaldehyde and methyl anthranilate; cyclic ethylenegfycol
diester of tridecandioic acid; 3,7-dimethyl-2,6-octadiene-1-nitrite; ionone
gamma
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methyl; ionone alpha; ionone beta; petitgrain; methyl cedrylone; 7-acetyf-
1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethyl-naphthalene; ionone methyl;
methyl-1,6,10-trimethyl-2,5,9-cyclododecatrien-1-yl ketone; 7-acetyl-
1,1,3,4,4,6-
hexamethyl tetraiin; 4-acetyl-6-tert-butyl-1,1-dimethyl indane; benzophenone:
6-
5 acetyl-1,1,2,3,3,5-hexamethyl indane; 5-acetyl-3-isopropyl-1,1,2,6-
tetramethyl
indane; 1-dodecanal; 7-hydroxy-3,7-dimethyl octanal; 10-undecen-1-al; iso-
hexenyl cyclohexyl carboxaldehyde; formyl tricyclodecan; cyclopentadecanolide;
16-hydroxy-9-hexadecenoic acid lactone; 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-
hexamethylcyclopenta-gamma-2-benzopyrane; ambroxane; dodecahydro-
10 3a,6,6,9a-tetramethylnaphtho-[2,1b]furan; cedrol; 5-(2,2,3-
trimethylcyclopent-3-
enyl)-3-methylpentan-2-ol; 2-ethyl-4-(2,2,3-trimethyl-3-cycfopenten-1-yl)-2-
buten-
1-0l; caryophyllene alcohol; cedryl acetate; para-tert-butylcyclohexyl
acetate;
patchouli; olibanum resinoid; labdanum; vetivert; copaiba balsam; fir batsam;
and
condensation products of: hydroxycitronellal and methyl anthranitate;
15 hydroxycitronellai and indol; phenyl acetaldehyde and indol; 4-(4-hydroxy-4-
.
methyl pentyl)-3-cyclohexene-1-carboxaldehyde and methyl anthranilate.
More examples of perfume components are geraniol; geranyl acetate; linalool;
linalyl acetate; tetrahydrolinalool; citronellol; citronellyl acetate;
dihydromyrcenol;
dihydromyrcenyl acetate; tetrahydromyrcenol; terpinyi acetate; nopol; nopyi
. 20 acetate; 2-phenylethanol; 2-phenylethyl acetate; benzyl alcohol; benzyi
acetate;
benzyl salicylate; benzyl benzoate; styrallyl acetate; dimethylbenzylcarbinol;
trichloromethyiphenylcarbinyl methylphenylcarbinyl acetate; isononyi acetate;
vetiveryl acetate; vetiverol; 2-methyl-3-(p-tert-butylphenyl)-propanal; 2-
methyl-3-
(p-isopropylphenylrpropanal; 3-(p-tert-butylphenyl)-propanal; 4-(4-methyl-3-
25 pentenyl~3-cyclohexenecarbaldehyde; 4-acetoxy-3-pentyltetrahydropyran;
methyl dihydrojasmonate; 2-n-heptyicyclopentanone; 3-methyl-2-pentyl-
cyciopentanone; n-decanal; n-dodecanal; 9-decenol-1; phenoxyethyl isobutyrate;
phenylacetaldehyde dimethylacetal; phenyiacetaldehyde diethylacetal;
geranonitrile; citronellonitrile; cedryl acetal; 3-isocamphylcyclohexanol;
cedryl
30 methylether; isolongifolanone; aubepine nitrite; aubepine; heliotropine;
eugenol;
vanillin; Biphenyl oxide; hydroxycitroneilal ionones; methyl ionones;
isomethyl
ionomes; irones; cis-3-hexenol and esters thereof; indane musk fragrances;
tetraiin musk fragrances; isochroman musk fragrances; macrocyclic ketones;
macrolactone musk fragrances; ethylene brassylate.
35 The perfumes useful in the present invention compositions are substantially
free
of haiogenated materials and nitromusks.
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36
Suitable solvents, diluents or carriers for perfumes ingredients mentioned
above
are for examples, ethanol, isopropanol, diethylene glycol, monoethyl ether,
dipropyiene glycol, diethyl phthalate, triethyl citrate, etc. The amount of
such
solvents, diluents or carriers incorporated in the perfumes is preferably kept
to
the minimum needed to provide a homogeneous perfume solution.
Perfume can be present at a level of from 0~~ to 10%, preferably from 0.1 % to
5%, and more preferably from 0.2% to 3%, by weight of the finished
composition.
Fabric softener compositions of the present invention provide improved fabric
perfume deposition.
(I)-Chelatina A
The compositions and processes herein can optionally employ one or more
copper and/or nickel chelating agents ("chelators"). Such water-soluble
chelating
agents can be selected from the group consisting of amino carboxylates, amino
phosphonates, polyfunctionally-substituted aromatic chelating agents and
mixtures thereof, all as hereinafter defined. The whiteness and/or brightness
of
fabrics are substantially improved or restored by such chelating agents and
the
stability of the materials in the compositions are improved.
Amino carboxylates useful as chelating agents herein . include ethylenedi
aminetetraacetates (EDTA), N-hydroxyethylethyienediaminetriacetates,
nitrilotri
acetates (NTA), ethylenediamine tetraproprionates, ethyienediamine-N,N'
diglutamates, 2-hyroxypropylenediamine-N,N'-disuccinates,
triethyienetetraaminehexacetates, diethylenetriaminepentaacetates (DETPA),
and ethanoldigiycines, including their water-soluble salts such as the alkali
metal,
ammonium, and substituted ammonium salts thereof and mixtures thereof.
Amino phosphonates are also suitable for use as chelating agents in the
compositions of the invention when at least low levels of total phosphorus are
permitted in detergent compositions, and include ethylenediaminetetrakis
(methylenephosphonates), diethylenetriamine-N,N,N',N",N"-pentakis(methane
phosphonate) (DETMP) and 1-hydroxyethane-1,1-diphosphonate (HEDP).
Preferably, these amino phosphonates to not contain alkyl or alkenyl groups
with
more than 6 carbon atoms.
The chelating agents are typically used in the present rinse process at levels
from 2 ppm to 25 ppm, for periods from 1 minute up to several hours' soaking.
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37
The preferred EDDS chelator used herein (also known as ethylenediamine-N,N'-
disuccinate) is the material described in U.S. Patent 4,704,233, cited
hereinabove, and has the formula (shown in free acid form):
H-N-CHI-CHI-N-H
I ' - I
CH, CH CH CH,
COOH COOH COOH COOH
As disclosed in the patent, EDDS can be prepared using malefic anhydride and
ethylenediamine. The preferred biodegradable [S,S] isomer of EDDS can be
prepared by reacting L-aspartic acid with 1,2-dibromoethane. The EDDS has
advantages over other chelators in that it is effective for chelating both
copper
and nickel cations, is available in a biodegradable form, and does not contain
phosphorus. The EDDS employed herein as a chelator is typically in its salt
form, i.e., wherein one or more of the four acidic hydrogens are replaced by a
water-soluble cation M, such as sodium, potassium, ammonium,
triethanolammonium, and the like. As noted before, the EDDS chelator is also
typically used in the present rinse process at levels from 2 ppm to 25 ppm for
periods from 1 minute up to several hours' soaking. At certain pH's the EDDS
is
preferably used in combination with zinc rations.
As can be seen from the foregoing, a wide variety of chelators can be used
herein. tndeed, simple polycarboxylates such as citrate, oxydisuccinate, and
the
like, can also be used, although such chelators are not as effective as the
amino
carboxylates and phosphonates, on a weight basis. Accordingly, usage levels
may be adjusted to take into account differing degrees of chelating
effectiveness.
The chelators herein will preferably have a stability constant (of the fully
ionized
chelator) for copper ions of at least 5, preferably at least 7. Typically, the
chelators will comprise from 0.5% to 10%, more preferably from 0.75% to 5%, by
weight of the compositions herein. Preferred chelators include DETMP, DETPA,
NTA, EDDS and mixtures thereof.
(J)-Enzyme
The compositions and processes herein can optionally employ one or more
enzymes such as lipases, proteases, cellulase, amylases and peroxidases. A
preferred enzyme for use herein is a cellulase enzyme. Indeed, this type of
enzyme will further provide a color care benefit to the treated fabric.
Cellulases
usable herein include both bacterial and fungal types, preferably having a pH
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38
optimum between 5 and 9.5. U.S. 4,435,307 discloses suitable fungal cellulases
from Humicola insolens or Humicola strain DSM1800 or a cellulase 212-
producing fungus belonging to the genus Aeromonas, and cellulase extracted
from the hepatopancreas of a marine mollusk, Dolabella Auricula Solander.
Suitable celtulases are also disclosed in GB-A-2.075.028; GB-A-2.095.275 and
DE-OS-2.247.832. CAREZYME~ and CELLUZYME~ (Novo) are especially
useful. Other suitable cellulases are also disclosed in WO 91117243 to Novo,
WO 96/34092, WO 96/34945 and EP-A-0,739,982. In practical terms for current
commercial preparations, typical amounts are up to 5 mg by weight, more
typically 0.01 mg to 3 mg, of active enzyme per gram of the detergent
composition. Stated otherwise, the compositions herein wilt typically comprise
- from 0.001 % to 5%, preferably 0.01 %-1 % by weight of a commercial enzyme
' preparation. In the particular cases where activity of the enzyme
preparation can
be defined otherwise such as with cellulases, corresponding . activity units
are
preferred (e.g. CEVU or cellulase Equivalent Viscosity Units). For instance,
the
compositions of the present invention can contain cellulase enzymes at a level
equivalent to an activity from 0.5 to 1000 CEVU/gram of composition. Cellulase
enzyme preparations used for the purpose of formulating the compositions of
this
invention typically have an activity comprised between 1,000 and 10,000
CEVU/gram in liquid form, around 1,000 CEVU/gram in solid form.
(K)-Other Optional Ingredients
The present invention can include optional components conventionally used in
textile treatment compositions, for example: colorants; preservatives;
surfactants;
anti-shrinkage agents; fabric crisping agents; spotting agents; germicides;
fungicides; anti-oxidants such as butylated hydroxy toluene, anti-corrosion
agents, and the like.
The present invention can also include other compatible ingredients, including
those as disclosed in copending applications Serial Nos.: 08/372,068, filed
January 12, 1995, Rusche, et al.; 08/372,490, filed January 12, 1995, Shaw, et
al.; and 08/277,558, filed July 19, 1994, Hartman, et al., incorporated herein
by
reference.
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Fabric Softener Processing
Processing of the softening composition of the invention is made
conventionally.
A typical example for processing said softening composition can be found in WO
97/03169 incorporated herein by reference.
The synthesis of the mixtures of biodegradable fabric softening actives is
described in pending application PCT US 97/03374 and WO 97103169
incorporated herein by reference.
All percentages, weights, and ratios herein are by weight unless otherwise
specified, and all numerical limits and numbers have the normal
accuracy/variability associated with such numbers. All references herein are
incorporated herein by reference, to the extent that they are relevant.
The following are non-limiting examples of the present invention:
Abbreviations used in the Examples
In the softening compositions, the abreviated component identification have
the
following meanings:
TMPD : 2,2,4-trimethyl-1,3-pentanediol
TEA DiEsterQuat : reaction product of (partly) unsaturated fatty acid with
Triethanolamine, di-Me sulfate quatemised (as described
in co-pending application PCT/US97109130, page 41
synthesis Example 3)
DEA DiEsterQuat : reaction product of (partly) unsaturated fatty acid with
Methyl di-Ethanolamine, MeCI quaternised (as described
in W097/03169 at page 108-109 under DEQAa)
Praepagen 3445 : DTallowDimethyl Ammonium Chloride, 72% solution in
water and Isopropanol, supplied by Hoechst
Lutensoi T05 : C13E05 commercially available from BASF
Lutensol A05 : C13C15E05 commercially available from BASF
Dowfax 9N5 : nonylphenol 5E0 commercially availabte from Dow
Genamin C200 : coco amine ethoxylated with 20 EO commercially
available from Hoechst
Genamin O-050 :. oleyl alcohol ethoxylated with 5 EO commercially
available from Hoechst
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Synthesis example of TEA DiEsterQuat
1 )-Esterification:
571 grams of Canola fatty acid with an IV of about 100 and an Acid Value of
5 about 196 as made according to Fatty Acid Compound Synthesis Example G is
added into the reactor, the reactor is flushed with N2 and 149 grams of
triethanolamine is added under agitation. The molar ratio of fatty acid to
methanol
amine is of 2.0:1. The mixture is heated above 150 C and the pressure is
reduced to remove the water of condensation. The reaction is prolonged until
an
10 Acid Value of 3 is reached.
- 2)-Quatemization:
To the 698 grammes of the product of condensation 122 grams of
dimethylsulfate is added under continuous agitation. The reaction mixture is
kept
15 above 50 C and the reaction is followed by verifying the residual amine
value.
820 grams of softener compound of the invention is obtained.
The quaternized material is optionally diluted with e.g. 15% of a 50:50
ethanol/
hexyleneglycol mixture which lower the melting point of the material thereby
20 providing a better ease in the handling of the material.
30
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41
Example 1
The following compositions are in accordance with the invention.
1 2 3 4 5 6
TEA DiEsterQuat 26% 26% 26% 26% 26% 26%
(100% active)
Ethanol 2.5% 2.5% 2.5% 2.5% 2.5% 4.5%
He lene i col 2.5% 2.5% 2.5% 2.5% 2.5% 2.5%
TMPD 8% 8% 6% 8% 5% -
2-ethyl l,3 hexanediol- - - _ _ 10%
Lutensol T05 3% - - _ _ 4%
flowfax 9N5 - 4% - - _ _
Genamin C200 - - 2% _ _ _
Genapol0-050 - - - 4% _ _
Lutensol A05 - - . _ 3% _
Perfume 2% 2% 2% 2% 2% 2%
demin water Balance Balance BalanceBalance Balance Balance
Example 2
The following compositions are in accordance with the invention.
7 8 9 10
TEA DiEsterQuat 2fi% 8% - -
( 100% active)
DEA DiEsterQuat - - - 26%
( 100% active)
Praepagen 3445 (72% - - 36% -
act'rve)
Ethanol 2.5% 0.6% - 2.5%
He lene cot - 0.6% - 2.5%
Diprop lene lycol 3% - - -
Butyl carbitol 10% - _ _
TMPD - - 8% 8%
1,2 hexanediol - 9% -.
Lutensol T05 3% 2% 4% 3%
Perfume ~ 2% 0.7 % 2% 2%
demin water Balance Balance Balance Balance
