Note: Descriptions are shown in the official language in which they were submitted.
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The-~resent invention relates to fabric softener compositions
adapted for the use in the rinse cycle of a laundering process and
in particular to concentrated aqueous fabric softener compositions
which are stable at both low and high ambient temperatures, i.e.
such compositions do not form a gel, and which are easily dispers-
ed in water when used.
Compositions containing quaternary ammonium salts having at
least one long chain hydrocarbyl group are commonly used to pro-
vide fabric softening benefits when employed in a laundry rinse
operation; for example, see United States Patents 3,349,033; 3,644,203;
3,946,115; 3,997,453; 4,073,735 and 4,119,545.
~or most aqueous softener compositions containing cationic
quaternary ammonium compounds as active ingredients, the concen-
tration of such cationics has, in general, been limited to the
range of about 3 to 6% by weight (see United States Patent 3,904,533 and
United S~ates Patent 3,920,565~. Such a low concentration is generally
necessitated by the fact that cationics form gels in water systems
at concentrations at above about ~%, and while the use of elec-
trolytes to lower ~he viscosity of such compositions is known (see
in particular United States Patent 4,199,545), such electrolytes are far
from satisfactory. From a functional point of view, the
electrolytes often do not perform as required particularly at con-
centrations of the cationics in the neighbourhood of about 12-15%.
~urther, while the performance of the electrolytes may mitigate
some of the gelling problem, their use is far from satisfactory
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in providing a highly concentrated aqueous system of cationics
which does not gel or severely change in viscosity wi-thin the
usual range of temperatures encountered in the handling thereof,
for example 0 F (about -18 C) up to about 140F (about 60C). In
U.S. Patent 3,681,241 a concentrated fabric softening emulsion
is described which consists essentially of 3.5 to 6. 5 parts by
weight of a compound represen-tecl for example by distearyl dimethyl
ammonium chloride,from 3.5 to 6.5 parts by weight of an alkyl
amido imidazolinium alkylsulfate,and from 0 to 3 parts by weight
of a different but similar fatty amido imidazolinium alkylsulfate,
the latter alleged]y providing low temperature stability f`or the
composi-tion. The total actives contemplated range from about 8
to 13%.
In British application 2053249A published February 4, 1981,
there are disclosed ca-tionic fabric softening compositions con-
taining ] 5 to 60% by weight of cationic softener, 25 to 75% by
weight of an aqueous medium, and 0. 5 to 40% by weight of a
specified water soluble polymer.
In U.S. Patent 3,97LI,076 there are disclosed quaternary
ammonium-containing softening COmposition of conventional cationic
concentrations, i.e. about 3% to about 6%. These compositions are
characterized by the very small par-ticle size of the substantially
water-insoluble quaternary ammonium softening compound, i.e. 90~
by weight of the quaternary ammonium compounds exist as particles
which will pass through a 1. 2 micron filter. The compositions are
described as a combination of the cationic softener, a C8 to C20
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alkyl alcohol with Erom about 0.1% to about 2.0% of a non-ionie
surfactant having a HLB of from about 8 to about 15, and
preferably from about 10 -to about 14. The preferred non-ionics
have a llpophilic hydrocarbyl moiety equivalent of 9 to 15
carbon atoms with 7 to 13 ethylene oxide hydrophilic moie-ties.
This patent does not relate to -the problem of stability of
concentrated aqueous cationic softening compositions but ra-ther
to improving the level and uniforrnity of softening using
conventional concentrations.
The present invention provides low and high tempera-
ture stable, concentrated, aqueous softener compositions based
upon quaternary ammonium softening compounds and a minor amount
of both a nonionic surfactant and an electrolyte. The present
invention also provides a method by which highly concentrated
fabric softening compositions are produced.
Thus, according to the present invention, there is
provided a stable, aqueous, concentrated fabric softening
composition comprising about (A) 12 to 20% by weight of a
cationie softener of the formula:
\ N < X
wherein R1, R2, R3 and R4 are alipha-tlc radials of C1 to C30
with at least two being alkyl of C14 to C30 and X is a water-
solubilizing anion; (B) 1 to 5% by weight of a non-ionie sur-
factant having an HLB value of 16.5-1.0; and (C) 0.5 to about
5% by weight of an electrolyte.
In another aspect, the invention provides a method
of preparing a composition as defined above, which comprises
first preparing an aqueous solu-tion of the non-ionie surfactan-t
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in warm water at a temperature up to about 80C thereaf-ter
adding cationic softener in melted form to form a gel, cooling
said gel to below 40C, and then adding electrolyte to break
the gel.
The compositions of the present invention are stable
aqueous compositions which con-tain a high concentration of
the cationic fabric softener which is a water dispersible
quaternary ammonium compounds as hereinafter described, non-
ionic surfactant and electrolyte.
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The aqueous compositions of this invention contain at least
about 12% cationic softener up to about 20% -thereof, said
cationic softener having the general formula I
R -~
R -R Y
wherein the R groups are selected from Cl to C30 aliphatic, pre-
ferably alkyl or alkenyl, aryl (e.g. phenyl, tolyl, cumyl, etc.);
aralkyl (e.g. benzyl, phenethyl, etc.); and the halo, amide,
hydroxyl, and carboxy substituents thereof; with the proviso that
e R is C14 to C30 and preferablY C14 to C18 and the
others are lower alkyl,and more preferably at leas-t two R's are
C14 to Clg and the others are lower alkyl of Cl to C4 (and most
preferably methyl or ethyl),and Y is a water-solubili~ing anion
such as chloride,bromide, iodide,fluoride, sulfate, me-thosulfate,
nitrite, nitrate, phosphate and carboxylate (i.e. acetate, adipate,
propionate, phthalate, benzoate, oleate, e-tc.). Typical cationics
of formula I include the following:
distearyl dimethyl ammonium chloride
ditallow dimethyl ammonium chloride
dihexadecyl dimethyl ammonium chloride
distearyl dimethyl ammonium bromide
di(hydrogenated tallow) dimethyl ammonium bromide
distearyl, di(isopropyl) ammonium chloride
distearyl dimethyl ammonium methosulfate
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The non-ionic component of the present compositions com-
prises from about 1 to about 5% by weight of the composition and
generally may vary with the cationic softener in a weight ratio
of cationic to nonionic of from about 20:1 to about 3:1 and
preferably from about 10:1 to about 5:1. The non-ionic compounds
are ethylene oxide condensates of C12 to C20 aliphatic alcohols
and alkyl phenols characterized by an HLB (hydrophilic-lipophilic
balance) of 16.5 _ 1Ø A complete discussion of the HLB system
can be found in "The HLB System" (1976 Edition 16 pages) pub-
lished by ICI United States, Inc. Generally the non-ionics as
herein contemplated are hydrophilic in nature with a large and
strong hydrophilic group. In the present invention this group
is an oxyethyl chain generally of at least about 15 terminal oxy-
ethyl groups (i.e. the oxyethyl groups are contiguous and termin-
ate in an hydroxyl group).
Particularly suitable non-ionic surfactants include a
C13 15 aliphatic alcohol containing 20 moles of condensed ethyl-
ene oxide and available as Synperonic A20; an e-thoxylated octyl
phenol with 16 moles of ethylene oxide available as Triton
X-165 and an ethoxylated nonyl phenol with 30 moles of ethylene
oxide available as Dowfax* NP30.
A third preferred ingredient is an electrolyte (ionic)
material in an amount of from about 0.1 to about 1.5~ by weight.
The use of an electrolyte acts not only to control viscosity but
also assists in stabilizing the system against gelling and phase
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inversion at high temperatures e.g. above about 40C.
Particularly suitable electrolytes include sodium chloride
and calcium chloride. Other useful electrolytes include sodium
formate, sodium nitrite, sodium nitrate, sodium ace-ta-te among
others as well as water-soluble salts of other cations such as
potassium,lithium, magnesium ammonium and the like.
Minor amounts of lower alkanols may be used particularly
where it is desired to further modify the viscosity. In general,
alcohols tend to lower the viscosity at ambient temperatures,
although moderate amounts may effect a lowering of the phase
inversion temperature. The preferred compositions of this inven-
tion exhibit phase inversion temperatures above about 80C and
preferably above abou-t 90 C with amounts of alcohol in the range
of about 1 to about 10~ by weight. Particularly suitable alcohols
are ethyl and isopropyl alcohol.
In addi-tion to the foregoing components of the sof-tening
compositions of this invention, there may also be included numerous
conventional, sup-plemental, and optional ingredients which do not
adversely affect the stability and/or functional characteristics
of the instan-t compositions. Thus, for example, there may be
present -the ubiquitous perfumes, dyes, pigments, opacifiers,
germicides, optical brigh-teners, anti-corrosion agents (e.g.
sodium silicate) water-soluble polymers, an-ti-static agents and
the like. Where used, each may comprise from 0.01~ to about 5
by weight of the composition.
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It is, of course, recognized and understood that mos-t
available chemical materials and particularly those containing
an hydrocarbyl moiety are generally mixtures of closely rela-ted
moieties. Thus, -the long chain alkyl substituents (R) in the
cationics used in -this invention may not only be a single carbon
length chain but more probably a mixture. In this regard a
particularly useful quaternary set wherein the alkyl groups are
derived from tallow may contain about 35% C16 and 60% Cl8 and
minor amounts of C14 and even others. Similarly, the aliphate
alcohol percursors for the non-ionics used herein may be of a
single carbon chain length but more likely, again, it will and can
be a mixture in any propor-tion of the operable chain length
compounds.
The fabric softening compositions of this invention must have
in addition to viscosity and phase stability, the requisite vis-
cosity (i.e. for pourability) and water-dispersibility in the
rinse cycle (or any other form of dilution prior to use) which
the consumers have come to accept and demand from -their use of
the less concentrated products. Thus the products contemplated
herein may have viscosities ranging from about 30 cps -to about
250 cps and preferably from about 40 cps to about 120 cps.
The general procedures for preparing the compositions herein
are several in number, -the final produce varying somewhat in
stability. The procedures differ in -the order of material
addition as well as processing conditions.
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A preferred procedure (A) involves adding -the non-ionic
materials and coloring to the formula weight of water which is at
about 70C. To this solution slowly add the cationic sof-tener in
melted form. Usually a gel wi:Ll f`orm. The mixture is cooled to
about 40 C and then the electrolyte is added to break the gel.
The composition is then cooled to room temperature with stirring.
A modification o~ procedure (A) involves adjus-ting the pH to about
12 before adding the melted cationic. In this case no gel forms.
After cooling to about 40 C, the pH is readjusted to 5 to 6, cooled
with stirring to room temperature and then electrolyte is used to
adJust the viscosity (Procedure B). Still another procedure (C)
involves adding the non-ionics to at least 80~ of warm water
(not above about 40C), then the electrolyte, and finally the
melted ca-tionic. The rest, if any, of the water is then added,
and the composition is then cooled with agita-tion to room termpera-
ture.
The following examples will serve to illustrate the present
invention without being deemed limitative thereof. Parts are by
weight unless o-therwise indicated.
Example 1
Eollowing Procedure (A) described above, 2 parts of an
ethoxylated nonyl phenol (containing 16 moles of ethylene oxide)
are dissolved in about 75 parts of water at a temperature of
about 70C. To this solution are slowly added 20 parts of
distearyl dimethyl ammonium chloride (75% active and containing
385~
about 10% isopropanol and the balance water) in melted ~orm
(Temperature = 55C) with stirring. A gel is formed. The gel is
cooled down to about 40C and -then 0.5 parts of calcium chloride
dehydrate are added. The mixture is cooled to room temperature
(about 20C) with stirring. A stable produc-t resul-ts with a
viscosity of about 100 cps.
Example 2
The procedure o~ Example 1 is repeated utilizing the
follo~ing parts o~ (A) cationic (active), (B) surfactant, and
(C) electrolyte
(a) A - 12; B = 1.0; C = 0.5
(b) A = 1ll; B = 1.5; C = 0.5
(c) A = 16; B = 1.8; C = 0.7
(d) A = 18; B = 2.5; C = 1.0
Example 3
Examples 1 and 2 are repeated utilizing in place o~ distearyl
dimethyl ammonium chloride the following:
(a) ditallow dimethyl ammonium chloride
(b) distearyl dimethyl ammonium methosulfate
(c) di(hydrogenated tallow) dimethyl ammonium bromide
(d) di-hexadecyl dimethyl ammonium chloride
(e) distearyl diethyl ammonium chloride
Example ll
Examples 1, 2 and 3 are repeated adding in all instances 1
part of polyethylene glycol (MWI~OO) with the non-ionic in the
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first step of the process of the preparation.
Polyethylene glycol (MW400) is illus-trative of
low molecular weight. water-soluble polymers which may be
used if desired in the softening compositions of this invention.
Among other useful polymers reference is made to Bri-tish pub-
lished application 2053249A described above. The compositions
of this invention may include any and all oE such polymers
and other water-soluble polymers as well. In the composi-tions
of this invention one may use from 0.1% to 20% by weight of
the total composition of these materials.
Example 5
Each of the foregoing examples l to 4 is repeated
using as the electrolyte the following:
(a) sodium chloride
(b) sodium nitrate
(c) sodium Eorma-te
(d) ammonium bromide
(e) potassium chloride
(f) calcium ni-trate
(g) lithium acetate
(h) magnesium chloride
Example 6
Each of Examples l to 5 is repeated, composition-
wise, but following the Procedure (B) for making -the composi-
tions. In this procedure the change in -the processing
described in Ex~mple l involves adjusting -the pH to 12 with
sodium hydroxide after dissolution of -the non-ionic (and
polyethylene glycol where used), and readjusting -the pH -to
5-6 wi-th hydroch:Loric acid after the
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addition of the cationic. At this point no gel forms as in
Procedure (A). The electrolyte is added after the mixture has
been cooled to room temperature.
Examp:le 7
Each of Examples 1 -to 5 is repeated again, composition-wise
but folJowing Procedure (C) to prepare the cornpositions.
In this procedure the non~-ionic (and the water soluble
polye-thylene glycol where used) is dissolved in 80% of the
formula weight of water at a temperature of 35-40C. The
electrolyte is then added, followed by -the melted cationic. The
remaining formula weight of water is then added and thereaf-ter
the mixture is cooled to room temperature with stirring.
The aqueous softening composi-tions of -this invention are
generally applicable as other such compositions, particularly
useful in the rinse cycle of an automatic laundry machine. In
such operations as well as in any other desired method of treating
clothes, the compositions are usually employed to provide
generally an actives concentration of from about 0.005% to 0.3%
based on the weigh-t of clothes treated preferably 0.007% to about
0.2% and most preferably from abou-t 0.01~ to about 0.15%.
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