Note: Descriptions are shown in the official language in which they were submitted.
Sue
-- 1 --
This invention relates to solid particulate
laundry softener-antistatic compositions formed when
water solutions or dispersions of certain surface
active sulfate or sulfonate salts are mixed with
water solutions or dispersions of certain surface
active qua ternary ammonium salts, and the resulting
electrically neutral water insoluble and non dispersible
undissociated organic salts are isolated in a form
substantially free from other components. These come
positions give surprising substantivity to fabrics when added to the laundry wash cycle, producing sub-
staunchly softening and antistatic effects which are
unexpected from an uncharged molecule since the prior
art teaches that a net cat ionic charge is necessary to
impart substantivity to softener-antistatic compost-
lions.
The quality of softness of laundered fabric
as used herein is well defined in the art and refers
to the quality of a treated fabric whereby its texture
is smooth, pliable, and fluffy. The use of modern
heavy duty laundry detergents tends to leave laundered
clothes with an undesirable harshness due partly to
the deposition of Cay and My carbonates, phosphates,
etc., on the clothes. It is an object of this invent-
ion to provide a composition that will restore a soft pliable texture to laundered clothes.
Another problem encountered in laundering
clothes, particularly if a mechanical dryer is used,
is that of static cling, which is defined in the art
as the tendency of laundered and dried fabric, especial-
lye synthetic fabric such as nylon and polyester, to
cling to itself and to the walls of the dryer due to
the build-up of static electrical charges. When the
fabric possesses static electrical charges it tends to
attract lint and dust and furthermore is uncomfortable
to wear. It is an object of this invention to provide
1;;:3Z8~9
-- 2 --
a composition which will dissipate the static charge
on laundered and dried fabric.
Qua ternary ammonium salts containing fatty
alkyd groups have traditionally been used in household
laundry softeners because they are substantive to the
laundered fabric and provide both softening and control
of static cling. However, they are incompatible with
anionic detergents which severely restricts their use
in the wash cycle. They are also incompatible with
optical brighteners and proteolytic enzymes which are
commonly incorporated into detergents and detergency
boosters used in the wash cycle. The use of qua ternary
ammonium salts in the rinse cycle necessitates an extra
trip to the washing machine to add the softener at the
appropriate time. It is a further object of this
invention to provide a variety of products with soften-
in and antistatic activity, including liquid or
powdered detergents; dry bleaching products containing
perorates, dry chlorine compounds, per carbonates, or
peroxyacids; products for boosting detergency contain-
in sodium tetraborate, surfactants, enzymes, optical
brighteners, and the like; and wash cycle softener-
antistatic compositions which can be added at the
beginning of the wash cycle, thus eliminating the
inconvenience of adding softener in the rinse cycle.
Many methods have been used to render
qua ternary ammonium softener compositions compatible
with detergents containing anionic surfactants in the
laundry wash cycle.
US. Patent 4,184,970 discloses a wash cycle
laundry softener composition in which particles or
pills containing a qua ternary ammonium salt are
sprayed with a solution of an 'anionic completing
component , which can be an anionic synthetic sun-
fact ant including water soluble salts of organic
sulfuric acid reaction products. Optionally, the
~Z328~9
-- 3 --
particles or pills and the completing component can
be admixed as solids and sprayed with water. This
procedure, however, only partially complexes the
qua ternary ammonium salt, and the presence of the
counter-ions from the two components causes the
particles to disperse to an undesirable extent in
the wash water. Also, since these pills are not
homogeneous, their effectiveness depends on maintain-
in the physical integrity of the particle throughout
the wash cycle. It is a further object of this in-
mention to provide a homogeneous composition which
because of its homogeneity does not depend on
maintaining a layered structure in the original
particles to be effective.
US. Patent 3,703,480 discloses the use of
aminopolyureylene resins mixed with qua ternary ammonium
salts to form a detergent compatible softener. US.
Patent 3,626,891 discloses certain mixtures of qua ternary
ammonium salts which are detergent compatible. Sun-
fact ant sulfates and sulfonates and qua ternary ammonium
salts have been combined in various ways in laundry
softener compositions. US. Patent 4,184,970 has been
described above. US. Patent 4,058,489 concerns
softener qua ternary ammonium compounds and anionic
surfactants combined in molar ratios of anionic sun-
fact ant to qua ternary ammonium salt of 0.6 to 1 to
0.95 to 1 and kept dispersed with a non ionic or an
amphoteric surfactant. US. Patent 3,644,203 concerns
combinations of a fatty alcohol-fatty alcohol sulfate
complex with softener qua ternary ammonium salts. The
resulting softener compositions must be used in non-
ionic detergents or in rinse cycle softeners. US.
Patent 4,000,077 concerns combination of softener
qua ternary ammonium salts and fatty alcohol sulfates
in weight ratios of 10 to 1 to 2 to 1, useful as rinse
cycle softeners. US. Patent 4,173,539 relates to
~2819
-- 4 --
fatty monoalkyl qua ternary ammonium salts and anionic
detergents in aqueous suspension used as rinse cycle
softeners. US. Patent 4,255,294 concerns "complexes"
of qua ternary ammonium salts and anionic detergents
as wash cycle softeners. The molar ratio of anionic
detergents to qua ternary ammonium salt is from 1.2
to 1 to 12 to 1, and a non ionic detergent is included
as a dispersant. Canadian Patent 818,419 discloses
the formation of an "electro-neutral complex" formed
by combining a cat ionic textile softening agent with
an anionic surfactant in the presence of a non ionic-
cat ionic dispersing agent. The softening activity of
this electro-neutral complex depends on a cat ionic
environment, and thus is not operable with all deter-
gent systems, especially those based on anionic sun-
fact ants. Further, the "electro-neutral complex"
cannot be isolated in a form substantially free from
other components which could be sold as an article of
commerce, or admixed with other products to add soft-
eying and antistatic activity. US. Patents 3,431,265
and 3,535,039 describe compositions formed by mixing a
biologically active qua ternary ammonium compound with
a surfactant sulfate or sulfonate which contains a
glycerol moiety or a polyether moiety. These mixtures
result in compositions which are water dispersible and
possess no textile softening activity. All of these
softener compositions depend for their softening and
antistatic activity on their being effectively dispel-
sod, either through the use of an excess of one of the
charged components, i.e. the softener qua ternary
ammonium salt or the anionic detergent or surfactant,
or through the use of a non ionic surfactant or an
amphoteric surfactant as a dispersant. Further those
which are proposed as wash cycle products depend for
their effectiveness as detergents on a very careful
selection of detergent surfactant which will be
1~3Z~319
-- 5 --
compatible with the dispersed softeners. An object of
this invention is to provide a softener antistatic
composition that remains a separate, solid phase
during the wash cycle and the rinse cycle, and spreads
on the clothes to provide softening and static protect-
ion as the clothes are dried in a mechanical dryer.
It is a further object to provide a composition that,
because it is a separate, solid phase, does not inter-
act with the detergent surfactants and thus is
compatible with all surfactant systems and detergent
components, thus eliminating or easing most of the
prior restriction on formulating products with softeners
to be used in the wash cycle. It is a further object
to provide a softener-antistatic composition which is
a single chemical compound and is effective in a pure
form without a requirement for dispersants, dispersion
inhibitors, specially formulated detergents and the
like.
We have discovered that by forming a solid,
particulate, water insoluble organic salt of a surface
active sulfate or sulfonate anion and a surface active
qua ternary ammonium cation by methods herein described
there results a composition which is a superior laundry
softener and antistatic agent which is compatible with
all detergent surfactant systems. These compositions
are not complexes, nor are they mixtures of cat ionic
salts and anionic surfactant salts, but are distinct
chemical compounds which are neither anionic nor
cat ionic in nature. They are undissociated organic
salts, or "ion pairs" with no water soluble component.
They are distinguished from qua ternary ammonium halides,
sulfates, phosphates, acetates, and the like in that
the compounds of this invention do not dissociate at
all in water. They are distinguished from the systems
of the prior art in that they are preformed and is-
fated as pure compounds, dried, and put into particles
1~3~8~9
-- 6
of the desired size. By doing this the insoluble
organic salt, which also forms in the systems of
the prior art, becomes surprisingly much more
effective as a softener-antistatic agent, and also
becomes inert to the other components of the
detergent or other laundry product with which it is
used. Without being held to theory, we believe that
we have modified the size, hardness, and the surface
properties of the particles of the softener so that
they both remain intact and undispersed in the wash
liquor throughout the wash cycle and also tend to
attach themselves to the fabric in the wash in a
manner unaffected by the surfactants present.
This invention relates to particles of an
undissociated organic salt which results when a sun-
face active water soluble or dispersible sulfate or
sulfonate salt is chemically combined with a surface
active water soluble or dispersible qua ternary
ammonium salt in exact stoichiometric ratio and under
conditions of intimate mixing, preferably in a water
medium, and the organic phase which forms is separated
from the water phase in dry particulate form sub-
staunchly free from other ingredients. Thus we have
discovered that by isolating this water insoluble
organic phase under conditions such that the counter-
ions of the sulfate or sulfonate surfactant and the
qua ternary ammonium surfactant are removed in the
water phase and then purifying, drying, and grinding
the insoluble phase, homogeneous water insoluble and
under normal laundry conditions non dispersible come
positions, which are undissociated organic salts of
the sulfate or sulfonate anions and the qua ternary
ammonium cations, result. Since the non dispersibility
of the particles of this invention is vital to their
function, we define non dispersibility in a functional
way as being able to recover essentially unchanged in
7 ~2328l9
size and shape the particles of softener after the
wash liquor containing detergent and softener has been
agitated in a simulated wash cycle to which no fabric
is added. This can be accomplished with standard
sieves and examination of the isolated particles with
a magnifying glass. These compositions, when added
to the laundry wash cycle as small particles are
effective softener antistatic agents when the clothes
are subsequently dried in a mechanical dryer.
The compositions of this invention are
chemical compounds in the classical sense in that they
have a precise weight ratio of components. They are
water insoluble and non dispersible undissociated ion
pairs of a surface active qua ternary ammonium cation
and a surface active sulfate or sulfonate anion of the
structure:
i. R1R2R3R4N OS02(0)x 5
wherein
Al is an alkyd, alkenyl, alkoxyalkyl or
acylamidoalkyl group containing about 12 to 22 carbon
atoms with the alkyd radical of the acylamidoalkyl
being ethyl or propel,
R2 is Al, hydroxyethyl, hydroxypropyl, ethyl,
or methyl,
R3 and R4 are methyl, ethyl, propel, hydroxy-
ethyl, hydroxypropyl or bouncily
R5 is an alkyd, alkenyl, alkaryl or moo-
hydroxyalkyl group containing about 14 to 22 carbon
atoms, and
x is 0 or 1, and
N +
R7 OS02(0)xR5
N 0
2 2 7
- 8 _ 1232~
wherein
R6 is methyl or ethyl,
R7 is alkyd or alkenyl containing about 14
to 22 carbon atoms, and
R5 and x are as defined above.
The anionic portion of the ion pair is
derived from surfactant sulfate or sulfonate salts
included in the group consisting of
R - S04
wherein R is an alkyd or alkenyl group containing 14
to 22 carbon atoms, and is preferably an alkyd group
containing about 14 to 20 carbon atoms, and is most
preferably a straight chain alkyd group containing
about 16 to 20 carbon atoms, and
R'- S03
wherein R' is an alkyd, alkenyl, alkyd aureole, or
hydroxyalkyl group containing about 14 to 22 carbon
atoms.
Since the ion pair product no longer contains
the original cation associated with the sulfate or
sulfonate anion except as a minor impurity, its choice
is one of convenience. It must, however, dissociate
from the sulfate or sulfonate anion to a substantial
extent in water. Suitable cations include No , K ,
H+, Ho ethanol ammonium, diethanol ammonium,
triethanol ammonium, and other water soluble amine.
Less suitable are My and Cay which usually do not
dissociate sufficiently.
Suitable surfactant alcohol sulfate salts
include sodium stroll sulfate, sodium Seattle sulfate,
sodium myristyl sulfate, sodium oilily sulfate, sodium
lonelily sulfate, and sodium tallow sulfate, and the
corresponding ammonium and potassium salts. These
products are well known in the art and are readily
available from many sources. Especially preferred
alcohol sulfates are those of alcohols derived from
1232~19
g
hydrogenated tallow or hydrogenated vegetable oil.
Sulfonates useful in this invention include
those which result from the reaction of olefins
containing 14 to 22 carbon atoms with sulfur trioxides
The product of this reaction is a mixture of isomers
of alkenyl sulfonates and hydroxyalkyl sulfonates of
the structures
RICH = CH-CH2SO3H
RICH -CH-CH2SO H
OH
in which R" is alkyd containing 11 to 19 carbon atoms:
which are neutralized with alkali metal hydroxides to
the corresponding alkali metal sulfonate salts.
Also included are alkylaryl sulfonates
resulting from the reaction of C8 to C18 alkyd benzenes
and naphthalenes with sulfur trioxides of the structure
R''' - Y - SUE
wherein R"' is alkyd containing 8 to 18 carbon atoms
and Y is phenol or naphthyl, which are neutralized
with alkali metal hydroxides to the corresponding
alkali metal sulfonate salts.
Paraffin sulfonates of the structure
Ho SHEA ) mCI Ho SHEA ) n
SUE
wherein m and n are integers from O to 22 and m + n is
14 to 22; made by the sulfoxidation of n-paraffins are
also included.
The cat ionic portion of the ion pair is
derived from qua ternary ammonium salts whose cat ionic
portions are of the structure
i . RlR2R3R4N
wherein
Al is an alkyd, alkenyl, alkoxyalkyl or
acylamidoalkyl group containing about 12 to 22 carbon
- 10 - I 9
atoms with the alkyd radical of the acylamidoalkyl
being ethyl or propel,
R2 is Al, hydroxyethyl, hydroxypropyl,
ethyl, or methyl,
R3 and R4 are methyl, ethyl, propel,
hydroxyethyl, hydroxypropyl or bouncily, and
ii. R6
I
C R7
No 1l
2 2 7
wherein
R6 is methyl or ethyl, and
R7 is alkyd or alkenyl containing about 14 to
22 carbon atoms.
Cations of the first structure are preferred,
and are most preferred when Al and R2 are C16 to C20
alkyd and R3 and R4 are methyl or ethyl.
Since the ion pair product no longer contains
the original anion associated with the qua ternary
ammonium cation except as a minor impurity, its choice
is one of convenience. It must, however, dissociate
from the qua ternary ammonium cation to a substantial
extent in water. Suitable anions include Of , By , I ,
methosulfate, ethosulfate, S04 , N03 , acetate and other
anions which dissociate in water.
Suitable qua ternary ammonium salts include
distearyl-dimethyl ammonium chloride, cetyltrimethyl
ammonium chloride, disallow dim ethyl ammonium
methosulfate, dicocodimethyl ammonium chloride,
stearamidopropyl trim ethyl ammonium chloride, alkyd
(C12 16) dimethylbenzyl ammonium chloride, tridecyloxy-
propel trim ethyl ammonium chloride, stroll Dow-
hydroxyethyl methyl ammonium chloride, dihydrogenatedtallow ethyl imidazolinium ethosulfate, dihydrogenated
~232~9
-- 11 --
tallow dim ethyl ammonium chloride, tallow di-2-hydroxy-
propel methyl ammonium chloride, stroll trim ethyl
ammonium chloride, and distearamidoethyl dim ethyl
ammonium chloride.
Another aspect of this invention is to the
process for preparing a laundry softener-antistatic
composition which is a water insoluble organic salt of
a surface active sulfate or sulfonate anion and a
surface active qua ternary ammonium cation. This pro-
cuss consists essentially of
- (i) intimately mixing, in any order from about
40 to 90 parts of water, preferably from about 50 to
80 parts of water with about 10 to 60 parts, prefer-
ably about 20 to 50 parts of the combination of
(a) a salt of the sulfate or sulfonate anion and
a counter ion which is substantially ionized
in water, and
(b) a salt of the qua ternary ammonium cation and
a counter ion which is substantially ionized
in water, the molar ratio of a to b being
from about 0.8 to 1 to 1.2 to 1 and prefer-
ably being about 1 to 1;
(ii) allowing the mixture to stand at a sufficient
temperature for a sufficient period of time such that
the water insoluble organic salt of the sulfate or
sulfonate anion and the qua ternary ammonium cation
separates from the water phase in a form such that
it is no more than about 60% water by weight, and is
preferably less than about 40% water, and contains no
more than about 0.25 moles of the salt of the counter-
ions per mole of the ion pair of the sulfonate or
sulfate anion and the qua ternary ammonium cation, and
preferably contains less than about 0.1 mole of
counter ion salt per mole of product organic salt;
(iii) evaporating the trapped water from the
sulfate or sulfonate-quaternary ammonium organic
123~
- 12 -
salt until it contains less than about 25% water by
weight, and preferably contains less than about 10%
water by weight, and
(iv) grinding, spray congealing, or otherwise
putting the composition in the form of small particles
of less than about 500 microns, and preferably from
about 50 to 400 microns in diameter.
Drying can be effected by any of a number of
methods common in the art. Examples of suitable methods
include the use of a Sandvik belt dryer and the use of a
Mizzen soap dryer. Products which are non-tacky solids
can be simultaneously dried and ground in a ribbon
blender. A preferred method is spray-congealing, whereby
the molten compounds are sprayed counter currently through
air to give small, discrete particles, the size of which
can be controlled.
The dried product is put into a powder form
suitable for adding to the laundry wash cycle by methods
known in the art. Hard, non-tacky solids are readily
ground to particles less than about 500 microns, and
preferably from about 50 microns to 400 microns in
diameter, or they may be melted and spray-congealed
into pills of this size. Preferred products have
sistering points from about 35 to 120C, and more
preferred products have sistering points from about
55 to 100C.
The compositions of this invention effect
good static protection and softening with all types
of laundry detergents in common use. They are
effective in built powders based on polyphosphates,
ETA, sodium carbonate, or zealots, and containing
non ionic, anionic, and amphoteric surfactants. They
can either be incorporated into the powder or added
separately to the washing machine. They are also
effective when added with built or unbolt liquid
detergent containing non ionic, anionic, or amphoteric
13 I 9
surfactants.
Since these compositions are uncharged and
furthermore do not dissolve or disperse in the wash
liquor, they do not interfere with the activity of
proteolytic enzymes and optical brighteners, and thus
can be used in detergents and detergency boosters
containing these components.
It will be recognized that these compositions
can be used in the rinse cycle of the laundry operation.
They can be added as powders or less preferably can be
dispersed by methods standard in the art and added as
dispersions or emulsions. They can also be applied in
the dryer, where they have the advantage of being non-
corrosive. For dryer application melting point modifiers,
substrates and other modifications common in the art may
be used.
It is understood that other adjutants commonly
added to laundry softener compositions, such as perfumes,
dyes, and the like, can be incorporated into the come
positions of this invention.
Our invention is further illustrated by the following examples.
Example 1
Standard ethylene blue titrations were used
to determine the equivalent weights of a 45% paste of
sodium tallow alcohol sulfate (Avirol T-45, trademark
of Continental Oil Companioned a 75~ alcohol dispersion
of di(hydrogenated tallow) dim ethyl ammonium chloride
(Adogen 442, trademark of Shrieks Chemicals). The equip
valet weight per surface active sulfate group of the
as is paste of Avirol T-45 was 1100; the equivalent weight
per surface active ammonium group of the as is dispersion
of Adogen 442 was 766.
55 g of Avirol T-45 (0.05 moles) was mixed
35 with 38.4 g of Adogen 442 (0.05 moles) and 100 g of
water was added. The mixture was heated to 60C, then
... I.
1232819
-- 14
stirred for 30 minutes at 60-70C. A water phase
separated from an emulsion phase when agitation
stopped, on standing about 2 hours at 70C the
emulsion broke and the organic phase was nearly
clear. The composition was cooled to room tempera-
lure, at which temperature the organic phase was very
hard and the water phase could be decanted readily.
The organic phase weighed 62.7 g and contained 21.5%
water by weight. It was broken into small lumps and
spread in a thin layer to evaporate the remaining
water. When it contained less than 5% water it was
ground to a fine, non-tacky powder in a Waring Blender
and screened through a 40 mesh sieve. To show that
the composition of this example had neither cat ionic
nor anionic character, 0.1 g of the dried powder was
dissolved and 10 ml of trichloroethylene, and 5 ml of
1 N H2SO4 and 5 ml of ethylene blue indicator solution
were added. The mixture was shaken vigorously and the
layers were allowed to separate. The ethylene blue
was the same intensity in both layers. If an excess
of qua ternary ammonium salt were present the ethylene
blue would have all remained in the water phase; if an
excess of tallow sulfate were present, the ethylene
blue would have been in the ethylene chloride only.
Therefore the composition of this example has no net
cat ionic or anionic functionality.
The product was tested as a wash cycle
softener-antistat by the following method: 8 lobs. of
mixed soiled clothes containing about equal portions
of synthetic fabric (nylon, polyester and acrylic),
permanent press fabrics (cotton-polyester blends) and
cotton fabrics were placed in a 20 gal capacity auto-
matte washer and the washer was filled with 100 Pam
hard water at 40C. 100 g of a powdered detergent
containing 6.1% phosphorus and non ionic and anionic
surfactants, and the stated quantity of the softener-
1 ;~3281~
- 15 -
anti stat of this example were added as the washer
started agitating. The washer completed its cycle
of a 10 minute wash, spin, room temperature rinse,
and final spin to about 50% moisture pickup. The
clothes were dried in an electric hot air dryer
using a 40 minute heat cycle plus a 5 minute cool-
down cycle. Static was evaluated visually by a
trained observer and was rated 0 if no static could
be detected, + if static was just detectable, ++ if
static was present but judged to be less than that
produced by using the detergent alone, and +++ if
there was no reduction from the detergent alone. A
rating of + is acceptable, a rating of 0 is of course
preferred.
Hand was evaluated on a cotton terry cloth
towel and was rated on a scale of 1 to 4, in which a
ranking of 1 is the equivalent of using a qua ternary
ammonium softener in the rinse cycle, and 4 is the
equivalent of the detergent alone. A ranking of about0 2.5 is acceptable, lower rankings being preferred.
Results from testing the composition of
Example 1 are shown in Table 1. At 4.5 g per 8 lb. of
laundry, static was eliminated and the hand was
excellent. At 3 g per 8 lb. of laundry the static was5 just detectable and the hand was still very good.
Table 1
Softening and antistatic activity of the composition
of Example 1.
Quantity of composition of
30 Example 1 added to 8 lb. of
laundry, q Static Hand
4.5 0
3 + 2
1~3Z819
- 16 -
Example 2
Compositions were prepared by the procedure
of Example 1, except that the molar ratio of sodium
tallow alcohol sulfate to dihydrogenated tallow dim ethyl
ammonium chloride was varied.
Composition A: 55 g of Avirol T-45 (0.05
moles) was mixed with 28.7 g of Adogen 442 (0.0375
moles) and 100 g of water. The water phase which
separated was cloudy, and contained about 4% of the
added sodium tallow alcohol sulfate. The dried product
was a non-tacky powder.
Composition B: 55 g of Avirol T-45 (0.05
moles) was mixed with 52.5 g of Adogen 442 (0.069
moles) and 100 g of water. A clear water phase that
contained no surfactant separated. The dried product
was a non-tacky powder.
Compositions A and B were tested by the method
described in Example 1. The results are shown in Table
2. Composition A, with excess sodium tallow alcohol
sulfate had both unacceptable static and softening at
US g per 8 lb. of laundry. Composition B eliminated
static but was less effective as a softener than was
the mole/mole product of Example 1.
Table 2
25 Softener added to 8 lb. of laundry Static Hand
4.5 g of Composition A ++ 3
4.5 g of Composition B 0 2
Example 3
The organic salts listed below were prepared
by the method of Example 1, and were tested as laundry
wash cycle softeners. All were effective as softeners
and all showed antistatic activity.
A. di(hydrogenated tallow) dim ethyl ammonium
cetyl-stearyl sulfate
~32~19
- 17 -
B. di(hydrogenated tallow) dim ethyl ammonium C12 15
Al Kane sulfonate
C. di(stearamidoethyl) dim ethyl ammonium C16 18
olefin sulfonate
D. tallow trim ethyl ammonium C12_14 olefin
sulfonate
E, disallow methyl imidazolinium dodecyl Bunsen
sulfonate.
Example
To show that the softener-antistat obtained in
a particulate form substantially free from other in-
gradients is superior to a composition formed in situ
in the wash liquor, the following detergents were
prepared:
15 Ingredient Composition A Composition B
(parts by weight)
Sodium tripolyphosphate 40 40
Soda ash 41.4 41.4
Sodium silicate pentahydrate 5 5
20 Sodium tetraborate pentahydrate
Sodium carboxymethyl cellulose
Linear alcohol ethoxylate 7 7
Sodium alkylbenzene sulfonate
(90%) 1.5
25 Di(hydrogenated tallow) dim ethyl
ammonium chloride (75%) 3
Composition of Example 1 3.6
To show the difference in the physical nature
of the compositions 0.6 g of detergent was added to
300 g of tap water at 49C stirring with a slight vortex.
After 90 seconds the detergent solutions were poured
through a 9 cm circle of black percale in a Buchner
funnel, and particles trapped on the fabric were noted.
Composition A left very few large particles that were
undissolved qua ternary ammonium salt. Composition B
left many small uniform particles. When viewed at lox
1 Z3Z8~9
- 18 -
magnification, they appeared to be no different in size
and shape from the softener powder added to the deter-
gent. The softening end antistatic activity of the
two compositions was tested by the procedure of Example
1. Static produced on synthetic fabrics in the dryer
was measured with an electrostatic voltmeter. The
average charge from the load washed with Composition A
was 4.1 TV; that of the load washed with Composition B
was 3.7 TV. The hand of the cotton terry towels from
Composition A was rated 3.7, those from Composition B
rated 3.2.
Liquid detergency boosters designed to be
added with a detergent to the laundry wash cycle possess-
in softening and antistatic activity can be prepared by
mixing suitable surfactants, optical brighteners,
enzymes, builder salts, polymers, and the particulate
softener-antistatic compositions herein described.
Such compositions can contain from about 5% to 50% of
one or more non ionic, anionic, or amphoteric surfactants;
from 0 to about 1% optical brighteners, from 0 to about
12% enzymes: from 0 to about 20% builder salts such as
sodium tripolyphosphate, tetrapotassium pyrophosphate,
sodium carbonate, sodium citrate, borax, and the like:
from 0 to about 5% of a polymeric anti redeposition
agent such as carboxymethyl cellulose, sodium polyp
acrylate, polyvinylpyrrolidone, and the like; and from
about 2% to 35% of one or more particulate softener-
antistatic agents herein described, the balance being
water. In these compositions the softener-antistatic
agent is present as particles.
Example 5
A product to be used with laundry detergents
as a detergency booster-softener-antistat combination
was prepared by mixing 15.4 g of tallowoyl isethionate
35 (67%), 5 g of a 10% solution of polyvinylpyrrolidone,
4 g of a 5.25% solution of optical brightener in 25%
1232~
-- 19 --
ethanol, 160 g of water, and 15.8 g of the compost-
lion of Example 1. The same composition was pro-
pared without the softener-antistatic composition
of Example 1. Both products were tested by the
procedure in Example 1, using 57 g (1/4 cup) of
the detergency booster product with 100 g of a
powdered non-phosphate anionic detergent. Static
charge in the synthetic fabrics was measured with
an electrostatic voltmeter, and was found to be
reduced by 1/2 by adding the softener-antistat
(first composition above) from that of the compost-
lion without the softener-antistat. The hand was
also substantially improved by adding the softener-
; anti stat. After the composition had stood for 16
months a sample was screened through a 200 mesh sieve, and particles of the added softener-antistat
were still present.
Powdered detergency boosters designed to be
added with a detergent to the laundry wash cycle
possessing softening and antistatic activity can be
prepared by mixing suitable surfactants, bleaches,
enzymes, optical brighteners, builder salts, polymers,
and other adjutants, and the particulate softener-
antistatic compositions herein described. Such combo-
sessions may contain from 0 to about 80% of one or more
non ionic, anionic, or amphoteric surfactants; from 0
to about 30% of a powdered bleach such as sodium
perorate, sodium per carbonate, proxy organic acids,
dry chlorine containing compounds, and the like; from
0 to about 12% enzymes; from 0 to about 1% optical
brighteners; from 20 to about 98% builder salts such
as condensed phosphates, borax, sodium carbonate,
zealots, trisodium nitrilotriacetate, and the like;
from 0 to about 5% of an anti redeposition polymer such
as sodium carboxymethyl cellulose, sodium polyacrylateand other polycarboxylates, and the like, and from
- 20 _ 1~32~9
about 2% to 50% of one or more of the particulate
softener-antistatic compositions herein described.
Example 6
To prepare a detergency booster-softener-
anti stat product in a powdered form, 12 g of dinonyl-
phenol condensed with 150 moles of ethylene oxide
(mop. 60C) was warmed to 65C, and 6 g of the come
position of Example 1 was mixed in thoroughly. The
mixture, containing particles of the softener-antistat
in the molten non ionic surfactant, was allowed to cool
to room temperature and was ground in a Waring blender
and screened through a 20 mesh sieve. Using the same
quantities of softener-antistat and non ionic surfactant
another composition was prepared and heated to 95C
at which temperature the softener-antistat was also
molten, so that the particles were destroyed and the
product was dispersed in the non ionic surfactant. It
was mixed, cooled, and ground in the same way as the
previous composition. To test, 13.5 g (6 g of non-
ionic and 4.5 g of softener-antistat) of the products
were added with 100 g of a non-phosphate anionic
powdered detergent to the wash cycle. The first come
position, in which the softener particles remained
intact, showed a large reduction in static from the
detergent alone, and the hand effect was rated 2.5.
The second composition in which the softener was
melted into the non ionic surfactant showed a marginal
reduction in static and a hand effect rated 3.8. This
demonstrates that to obtain softening and antistatic
effects from the compositions of this invention it is
necessary for the particles of softener to remain
intact in the laundering process.
Example 7
The composition of Example 1 was mixed with
sodium tetraborate decahydrate (borax) at a ratio of
3.5 parts of softener to 96.5 parts of borax, to
- 21 ~23Z~319
prepare a detergency booster with softening and anti-
static activity. It was tested by the procedure of
Example 1 for ten cycles. Static was rated 0 for
each of the 10 cycles. There was no yellowing of
white fabrics in the load as evidenced by no change
in the reflectance measured with a Gardener reflect-
meter.
Example 8
The particles of this invention can be sup-
penned in liquid laundry detergents to obtain detergent-
- softener-antistat compositions. The following deter-
gents were prepared:
Ingredient Composition A Composition B
(parts by weight)
15 Linear alcohol ethoxylate 25 25
Composition of Example 1 5
Avirol T-45 (see Example 1) 5.2
Adogen 442 (see Example 1) 3.6
Water 70 66.2
The "black cloth test" of Example 4 was used
to show that the softener particles in Composition A
remained intact in the wash liquor, and that no part-
ales were present in the wash liquor from Composition
B. The two compositions were tested as detergent-
softeners by the procedure of Example I Static
generated on synthetic fabrics in the dryer was
measured with an electrostatic voltmeter. The average
charge in the load washed with Composition A was 2.4
TV; the average charge from Composition B was 3.8 TV.
The hand of the terry towels washed with Composition A
was rated marginally superior to that of the towels
washed with Composition B. The detergency of Compost-
lion A can be improved by the incorporation of a
proteolytic enzyme. Since the softener particles are
uncharged, and furthermore remain intact throughout the
wash cycle, the softener does not interfere with the
activity of the enzyme.
Jo ,
