Note: Descriptions are shown in the official language in which they were submitted.
-BACKGROUND OF THE INVENTION
The present invention relates to articles and methods
for supplying~conditioning benefits to fabrics in an
automatic clothes washer and dryer. The articles comprise a
receptacle releasably containing a fabric conditioning
composition.
The home laundering operation can provide an opportunity
to treat fabrics being laundered with a variety of materials
which impart some desirable benefit or quality to the fabrics
during laundering. At each stage of the laundering operation
(presoaking, washing, rinsing, drying) fabrics are, to varying
degrees, found in contact with water which can provide the
medium for delivery of fabric conditioning agents.
1100260
Delivery of fabric conditioning agents to fabrics during
the laundering operation is not, however, accomplished without
certain difficulties. Surfactants are generally employed during
the presoaking and washing steps for the purpose of removing
materials Isoil) fro~ the fabrics. Simultaneous deposition onto
fabrics of fabric conditioning agents can, therefore, prove
troublesome. While some of these problems can be overcome by
conditioning fabrics in the automatic dryer (see, for example,
Gaiser; U.S. Patent 3,442,692, issued May 6, 1969), it is never-
theless exceptionally difficult to achieve efficient depositionin the dryer of all fabric conditioning agents. For example, it
is difficult for dryer added fabric softener/antistat composi-
tions to match the softening performance of rinse added softeners.
Attempts have been made to improve the efficiency of condi-
tioning agent fabric deposition during the laundering process.
Some of the attempts are found in the prior art references listed
subsequently herein. Included in such previous attempts are
articles/compositions which rely on a film insolubilization/
solubilization technique to control the release of fabric con-
ditioning agents. Such executions are, however, not free fromproblems.
One problem discovered with fabric conditioning articles
which rely on the insolubilization/solubilization technique is
that the fabric conditioning agents are oftentimes poorly re-
leased to the fabrics. This has been found to be due in part to
high concentrations of insolubilization agent being present
around certain parts of the film which envelopes the fabric
conditioner. It has been found that this problem can be over-
come by physically separating the insolubilization agent from
the film coated particles.
It has been discovered by the present inventor that even
with the above-described separation, fabric softener/antistat
~ -2-
~ 1100260
compositions do not deliver optimum performance. In the present
invention it has been surprisingly found that improved perfor-
mance can be achieved by placing uncoated fabric antistat parti-
cles in with the coated fabric softener/antistat. The uncoated
fabric antistat particles are formulated so that they can survive
the washing and rinsing cycles and be carried into the dryer to
melt. This allows the coated fabric softener/antistat to be for-
mulated to deliver maximum softening performance. Further the
antistat particles may deliver substantive perfumes to the fabrics
being dried.
Accordingly, it is an o~ject of the present invention to
provide articles which can be added to a clothes washer to con-
dition fabrics in a superior manner concurrently with a washer
and dryer operation. The articles are structured in a manner
which overcc~es m~ny of the p~oblems present in the prior art executions.
It is a further object herein to provide methods for
conditioning fabrics during the home laundering process.
Th~se and other objects will become obvious from the
following disclosure.
DESCRIPTION OF THE PRIOR ART
.
U. S~ Patent 3,822,145, Liebowitz et al., FABRIC SOFTENING,
issued July 2, 1974, relates to the use of spherical materials
as fabric softening agents. U. S. Patents 3,743,534, Zamora et
al., PROCESS FOR SOFTENING FABRICS IN A DRYER, issued July 3,
1973; 3,698,095, Grand et al., FIBER CONDITIONING ARTICLE,
issued October 17, 1972; 3,686,025, Morton, TEXTILE SOFTENING
AGENTS IMPREGNATED INTO ABSORBENT MATERIALS, issued August 22,
1972; 3,676,199, Hewitt et al., FABRIC CONDITIONING ARTICLE AND
USE THEREOF, issued July 11, 1972; 3,633,538, Hoeflin,
SPHERICAL DEVICE FOR CONDITIONING FABRICS IN DRYER, issued
January 11, 1972; 3,624,947, Furgal, COATING APPARATUS, issued
.
-3-
llOOZ60
January 18, 1972; 3,632,396, Zamora, DRYER-ADDED FABRIC-
SOFTENING COMPOSITIONS, issued January 4, 1972; 3,442,692, Gaiser,
METHOD OF CONDITIONIN5 FABRICS, issued May 6, 1969; and 3,947,g71,
Bauer, FABRIC SOFTENER AND DISPENSER, issued April 6, 1976, each
relate to articles and methods for conditioning fabrics in auto-
matic dryers. U.S. Patent 3,594,212, Ditsch, TREATMENT OF FIBROUS
MATERIALS WITH MONTMORILLONITE CLAYS AND POLYAMINES AND POLY-
QUATERNARY AMMONIUM COMPOUNDS relates to the treatment of fibrous
materials with clays and amine or ammonium compounds.
Granular detergent compositions containing fabric condition-
ing materials are disclosed in U.S. Patent 3,862,058, Nirschl
et al., DETERGENT COMPOSITIONS CONTAINING A SMECTITE-TYPE CLAY
AND SOFTENING AGENT, issued January 21, 1975; U.S. Patent 3,861,870,
Edwards et al., FABRIC SOFTENING COMPOSITIONS CONTAINING WATER
INSOLUBLE PARTICULATE, issued January 21, 1975; and Japanese
Publication Number 1924/77, Washing Assistants, published
January 19, 1977.
SUMMARY OF THB INVENTION
The instant invention is based on the discovery that
superior fabric conditioning articles can be prepared by
releasably placing an effective amount of fabric softener/
antistat particles which have as a coating a film which has
its solubility controlled by pH or electrolyte level within a
receptacle having at least a part of one wall made of a water
insoluble, porous material. Also enclosed within said recep-
tacle is an amount of a pH control agent or electrolyte
sufficient to insolubilize said film. Further, the film coated
particles are separated from the insolubilizing agent in said
receptacles by forming separate parts by sealing one part of
the receptacle off from the other; coating the film coated
particles with a water-soluble film which is not a~fected by
.' ~ .
--4--
llOOZ60
the level of electrolyte-pH control agent used in the article; or
by separating the receptacle into two parts by means of a wall
which may be water-insoluble/indispersible and permeable or im-
permeable or water-soluble and not affected as described above
for the film. The water soluble materials should not completely
dissolve until the pH control agent/electrolyte has dissolved
in the wash water. Further, in addition to the coated fabric
softener/antistat particles the present articles contain uncoated
particles of a fabric antistat agent.
In its process aspect, this invention encompasses a process
for conditioning fabrics comprising combining an article of the
type disclosed above with a load of fabrics in a clothes washer
and leaving the article with the fabrics through the wash/rinse
cycle of the washer and the drying cycle of an automatic clothes
dryer.
DETAILED DESCRIPTION OF THE INVENTION
The articles herein comprise multiple components each of
which is described, in turn, below.
Receptacle
The receptacle which contains the coated particles, uncoated
antistat particles and the pH control agent and/or electrolyte
in the present invention is a closed article wherein at least a
part of one wall is constructed of a material which is water-
insoluble and indispersible and is sufficiently porous to allow
for the release of the pH control agent and/or electrolyte during
the wash cycle and the fabric softener/antistat composition during
the rinse cycle and in the dryer. The uncoated fabric antistat
particles are retained in the receptacle when the latter is
placed into a dryer; the dryer heat causes the particles to melt
thereby delivering the agent to the fabrics. The remainder of
~ .
--5--
)Z60
the receptacle can then be any water-insoluble/indispersible
porous or nonporous material.
Since it is desirable to make the articles herein as
aesthetically pleasing as possible and inasmuch as the articles
are to be used in a clothes washer and an automatic clothes
dryer, it is preferred that the porous wall of the receptacle
be both water-insoluble and heat resistant. Therefore, the
receptacle herein can be made of any materials meeting these
requirements. The wall can be made, for example, of porous
materials such as open weave cotton, polyester, and the like,
cloth or foams.
In a preferred receptacle herein, the porous wall or walls
is an elastic, open cell foam or elastic nonwoven material.
The open cell f ~ s are distinguished from closed cell foams in that the
closed cell structure substantially isolates the individual
cells while the open cell structure does not. Regardless of
what material is used, it should not inhibit the release of the
coated fabric softener/antistat composition.
Open cell foams can be made from polystyrene, polyurethane,
polyethylene, polyvinyl chloride cellulose acetate, phenolformal-
dehyde and other materials such as cellular rubber. Many of
these materials and their method of manufacture are disclosed
in standard references such as Encyclopedia of Polymer Science
and Technology, Interscience Publishers, John Wiley & Sons, Inc.
(1965~.
The preferred nonwoven cloth materials used herein can
generally be defined as adhesively bonded fibrous or filamentous
products having a web or carded fiber structure (where the fiber
strength is suitable to allow carding), or comprising fibrous mats
in which the fibers or filaments are distributed haphazardly or
in random array (i.e., an array of fibers in a carded web wherein
partial orientation of the fibers is frequently present, as well
~OOZ60
as a completely haphazard distributional orientation), or
substantially aligned. The fibers or filaments can be natural
(e.g., wool, silk, jute, hemp, cotton, linen, sisal, or ramie)
or synthetic (e.g., rayon, cellulose ester, polyvinyl derivatives,
poly-olefins, polyamides, or polyesters). Preferred materials
` include polyesters, polyamides, poly-olefins and polyvinyl deriva-
tives and mixtures of these with rayon or cotton to achieve the
- desired elasticity.
Methods of making nonwoven cloths are not a part of this
invention and, being well known in the art, are not described
in detail herein. Generally, however, such cloths are made by
air- or water-laying processes in which the fibers or filaments
are first cut to desired lengths from long strands, passed into
a water or air stream, and then deposited onto a screen through
which the fiber-laden air or water is passed. The deposited
` fibers or filaments are then adhesively bonded together, dried,
cured, and otherwise treated as desired to form the nonwoven
cloth. Nonwoven cloths made of polyesters, polyamides, vinyl
resins, and other thermoplastic fibers can be spun-bonded, i.e.,
the fibers are spun out onto a flat surface and bonded (melted)
: together by heat or by chemical reactions.
Especially preferred materials for preparing the above-
described wall of the article herein are open pore polyurethane
foams and spun-bonded nonwoven cloths, especially those made
from polyesters. The polyurethane foams preferably have a density
of from about 0.02 g/cm3 to about 0.04 g/cm3 while the polyester
has a basis weight of about 10 g/sq.yd. to 90 g/sq.yd. The
thickness of this wall can vary depending on the aesthetic pro-
perties desired by the manufacturer, but will preferably be from
about 0.2 cm to about 4 cm for polyurethane and from about 0.01
cm to about 6 cm for polyester. The air permeability of the por-
ous wall need only provide sufficient porosity to allow for the
~100260
release of the fabric softener/antistat composition but is
preferably in the range of 700 to 1400 cubic feet per minute per
square foot of surface. The air permeability is measured
according to ASTM Method D737-69, "Standard Method of Test for
Air Permeability of Textile Fabrics."
It is also within the scope of the present invention to
provide articles wherein the receptacle is made of more than one
layer of the above-described materials. For example, two layers
of non-woven polyester may be selected to provide articles having
an appearance which connotes optimum fabric conditioning.
pH Con-trol Agent and/or Electrolyte
.
Achieving the superior fabric conditioning performance
described hereinbefore is in part dependent on the fabric
softener/antistat composition not being released until the rinse
cycle of the clothes washer and during the drying cycle of the
clothes dryer. As a result of this release pattern, the consumer
can have the convenience of putting the article in with the
fabrics to be washed at the start of the wash cycle while obtain-
ing, for example, softening/antistatic performance which issuperior to that delivered by rinse cycle or dryer added softeners/
antistats.
The insolubility of the particle coating in the present
articles during the wash cycle is achieved by maintaining a
sufficiently high electrolyte level and/or proper pH in wash
solution. The electrolyte level and/or pH are critical since,
looking at the former first, the electrolyte either through a
chemical reaction or salting out mechanism may cause the
particle coating material to gel or precipitate (hereinafter
both referred to as "gel") and, hence, be water-insoluble.
Once the electrolyte level drops below the gelling level (i.e.,
when the wash water containing the electrolyte is removed and
--8
llOQ26o
replaced with clean rinse water), the particle coating can begin
to dissolve/disperse, thereby releasing the fabric softener/anti-
- stat composition which it surrounds. The obtaining of efficient
gelling in many instances is dependent on the electrolyte resid-
ing in an environment having a pH within a certain range. The
pH allows the electrolyte to complex with the coating material
;n the most efficient manner. This is especially true where the
electrolyte has an anion which can be protonated within a pH range
encountered by the articles herein. If protonation occurs gela-
tion is hindered. Therefore it is necessary in such instances
to maintain the pH of the wash solution above the pKA of the anion.
- Many materials are insolubilized solely as the result of pH
control. The critical pH is generally thought to be around the
isoelectric point and can be achieved through the use of pH con-
trol agents. Examples of such agents will be discussed herein
later.
: The materials which can serve as electrolytes in the present
invention are any of those materials which are solid and can
; sufficiently complex or salt out the coating material to cause
it to gel or precipitate. Examples of suitable agents include
but are not limited to sodium borate, sodium metaborate,
ammonium sulfate, sodium sulfate, potassium sulfate, zinc sulfate,
cupric sulfate, ferrous sulfate, magnesium sulfate, aluminum
sulfate, potassium aluminum sulfate, ammonium nitrate, sodium
- nitrate, potassium nitrate, aluminum nitrate, sodium chloride,
potassium chloride, sodium phosphate, potassium chromate, potas-
sium citrate and mixtures thereof.
The amount of electrolyte employed herein is an amount
sufficient to gel the particle coatings. This can be determined
by dispersing/dissolving a small amount, for example, about 0.5
grams, of the coating material in a known quantity of about 32 C
wash solution and then adding the electrolyte until reversible
_g_
ll~Q260
gelation occurs. This amount can then be increased to maintain
the molar concentration of the electrolyte in the wash water
at the gelation level for the total amount of water present in
washers. For most washers a water volume of 64 to 83 liters,
or on average about 70 liters, is present during the wash cycle.
Therefore, the amount of electrolyte to be used in the articles
herein should be sufficient to maintain the concentration at
the gelation level in 70 liters of water. Thus, if one liter of
water is used to determine gelation, the amount of electrolyte
for use in the article would be 70 times that amount. The wash
bath solutions in which the articles herein are used will contain
detergent compositions and these will affect the solubility of
the particle coatings. Therefore, to the liter of water should
be added a detergent composition at a concentration equivalent
to normal wash conditions. Since there are two basic types of
laundr~ detergents, liquids and granules, two tests should be
conducted. In one test about 0.9 ml. of a liquid detergent
should be dissolved in the water prior to electrolyte addition
and in the other test about ~.5 ml. of a granule detergent
should be dissolved. These amounts correspond to 1/4 cup of
liquid detergent per wash load and 1 1/4 cup of granules. The
amount of electrolyte/pH control agent used in the articles
herein is the greater of the two amounts determined to be re-
quired for gelation. This amount insures that the article is
operable in all types of wash solutions. Of course, it is to be
appreciated that the critical factor is the electrolyte
concentration in the wash solution and not how it is achieved.
(i.e., If more than one article is used the total amount of
electrolyte used must be enough to insolubilize or make indis-
persible the particle coatings). All of the electrolyte can be
present in one article or split between the articles as
explained hereinafter.
, x~ --10--
)260
As is true with the electrolyte component of the present
invention, the pH control agent can be any of a wide variety of
solid acids, bases and general buffering systems. Included
among such materials are citric acid, glycolic acid, tartaric
acid, maleic acid, gluconic acid, boric acid, glutamic acid,
;sophthalic acid, sodium bisulfate, potassium bisulfate, sodium
hydroxide, potassium hydroxide and alkali metal and ammonium
phosphates, carbonates, borates, bicarbonates and metaborates.
A preferred electrolyte/pH control agent is sodium borate and/or
sodium metaborate. It is to be appreciated that waters of
hydration may be present on any of the agents which are hydrat-
able (e.g., borax).
The amount of pH control agent used herein is an amount
sufficient to insure the insolubility/indispersibility of the
particle coating. This will vary with the particular material
selected but can easily be determined in the manner described
above for the electrolyte.
It is oftentimes advantageous to coat the electrolyte/pH
control agent with a material to reduce the dustiness which such
agents may possess when in powder form. Materials which are
suitable for this use include water-soluble nonionics such as
- ethoxylated alcohols.
Fabric Softener/Antistat Particle Coating
The particle coating, as explained herein previously, serves
to prevent the fabric softener/antistat composition from being
released to the fabrics until preferably the rinse cycle of the
washer and the drying cycl~ of the dryer. The coating material
must therefore be water-soluble or dispersible but be insolubilized/
made indispersible during the wash cycle by the maintenance of a
sufficient electrolyte level and/or the appropriate pH. Materials
which satisfy this requirement are many and will be discussed
hereinbelow.
:
--1 1--
260
The materials which can be used for the particle coating herein
include polyvinyl alcohol, gelatins and other proteins, polyvi~yl
pyrrolidone, polyethylene oxide, methyl cellulose, hydroxypropyl
methyl cellulose, polyfructose, and polysaccharides such as guar
gum, among many ot~ers including derivatives and mixtues of these
materials. The coating can have a broad range of molecular
weights and amount to varying weight percentages of the total
particle weight. However, it is preferred that the former be
from about 2,000 to about 200,000 and the latter be from about 0.1%
to about 50~. These limitations provide for particle coatings
which can most effectively dissolve/disperse to release the fabric
conditioning composition.
The materials listed above can be grouped by the type of agent
required to make the mater al insoluble and indispersible.
Those which are controlled by electrolyte level include polyvinyl
alcohol, polyethylene oxide, methyl cellulose, guar gum, and
hydroxypropyl methyl cellulose. Those which are controlled by pH
include gelatin and other proteins, polyvinyl pyrrolidone and
polyfructose.
The preferred materials for use as the particle coating are
polyvinyl alcohol and gelatins. The polyvinyl alcohol preferably
has a degree of hydrolysis of from about 73% to about 100% more
preferably about 88%, and a molecular weight of about 2,000 to
130,000, preferably about 90,000. The gelatin materials can be
either Type A, isoelectric point of pH 7-9, or Type B, isoelectric
point of pH 4.7 - 5. The gelation of gelatin takes place near
the isoelectric point. A detailed discussion of polyvinyl al-
cohol can be found in C. A. Finch (Editor), Polyvinyl Alcohcl -
Properties and Applications, John Wiley & Sons, New York, 1973.
Detailed discussions of proteins can be found in H. R. Mahler &
E. H. Cordes, Biological Chemistry, Harper and Row, New York,
1971, and A. H. Lehninger, Biochemistry, Worth Pub., Inc., New
~ -12-
. .
260
York, 1975. Discussions of the previously mentioned cellulose
derivatives, polyvinyl pyrrolidone and ethylene oxide are found
in R.L. Davidson & M. Sittig (Editors), Water-Soluble Resins,
Van Nostrand Reinhold Company, New York, 1968. A discussion
of polysaccharides is found in R. L. Whistler (Editor),
Industrial Gums - Polvsaccharides and Their Derivatives, American
,, ~ -.
Press, New York, 1973.
' .
-13-
~' ~
11~0260
Softener/Antistat Composition
The fabric softener/antistat agents employed herein are most
generally any of the wide variety of water-insoluble nonionic and
cationic materials known to supply these benefits. These materials
are substantive, and have a melting point within the range of from
about 20C to about 115C, preferably within the range of from
about 30C to about 60C.
The most common type of cationic softener/antistat materials
are the cationic nitrogen-containing compounds such as quaternary
ammonium compounds and amines having one or two straight-chain
organic groups of at least eight carbon atoms. Preferably, they
have one or two such groups of from 12 to 22 carbon atGms. Pre-
- ferred cation-active softener compounds include the quaternary
ammonium softener/antistat compounds corresponding to the
formula
.
-14-
,
~lOQZ60
_ _
Rl R3
N X
/ \
R~
.
: '' ' .
,
' '
1l . - .
.
,' .
.~ ~
'i '
.
~' ~' ' '
' .
:~
.
:~ '`~ "
.
'
.~ .
~10(~260
wherein Rl is hydrogen or an aliphatic group of from 1 to 22
carbon atoms; R2 is an aliphatic group having from 12 to 22
carbon atoms; R3 and R4 are eachalkyl groups of from 1 to 3
carbon atoms; and X is an anion selected from halogen, acetate,
phosphate, nitrate and methyl sulfate radicals.
Because of their excellent softening efficacy and ready
availability, preferred cationic softener/antistat compounds
of the invention are the dialkyl d methyl ammonium salts wherein
the alkyl groups have from 12 to 22 carbon atoms and are derived
from long-chain fatty acids, such as hydrogenated tallow. As
employed herein, alkyl is intended as including unsaturated com-
pounds such as are present in alkyl groups derived from naturally
occurring fatty oils. The term "tallow" refers to fatty alkyl
groups derived from tallow fatty acids. Such fatty acids give
rise to quaternary softener compounds wherein Rl and R2 have pre-
dominantly from 16 to 18 carbon atnms. The term "coconut" refers
to fatty acid groups from coconut oil fatty acids. The coconut-
alkyl Rl and R2 groups have from about 8 to about 18 carbon atoms
and predominate in C12 to C14 alkyl groups. Representative
examples of quaternary softeners of the invention include tallow
trimethyl ammonium chloride; ditallow dimethyl ammonium chloride;
ditallow dimethyl ammonium methyl sulfate; dihexadecyl dimethyl
ammonium chloride; di(hydrogenated tallow)dimethyl ammonium
chloride; dioctadecyl dimethyl ammonium chloride; dieicosyl
dimethyl ammonium chloride; didocosyl dimethyl ammonium chloride;
di(hydrogenated tallow) dimethyl ammonium methyl sulfate;
dihexadecyl diethyl ammonium chloride; dihexadecyl dimethyl
ammonium acetate; ditallow dipropyl ammonium phosphate; di-
tallow dimethyl ammonium nitrate; di(coconut-alkyl) dimethyl
ammonium chloride.
; ~ -16-
~ 1100260
An especially preferred class of quaternary ammonium
softener/antistats of the invention correspond to the formula
llOQ260
Rl +
CH3 N C~I3 X
.
`"` '
~ ~ L
.
,
'
. ~ .
.::
.
. `
.
.
~10~260
wherein Rl and R2 are each straight chain aliphatic groups of
from 12 to 22 carbon atoms and X is halogen, e.g., chloride
or methyl sulfate. Especially preferred are ditallow dimethyl
ammonium methyl sulfate ~or chlGride) and di(hydrogenated
tallow-alkyl~ dimethyl ammonium methyl sulfate (or chloride)
and di(coconut-alkyl) dimethyl ammonium methyl sulfate (or
chloride), these compounds being preferred from the standpoint
of excellent softening properties and ready availability.
Suitable cation-active amine softener/antistat compounds
are the primary, secondary and tertiary amine compounds having
at least one straight-chain organic group of from 12 to 22
carbon atoms and 1,3-propylene diamine compounds having a
straight-chain organic group of from 12 to 22 carbon atoms.
Examples of such softener actives include primary tallow amine;
primary hydrogenated-tallow amine; tallow 1,3-propylene diamine;
oleyl 1,3-propylene diamine; coconut 1,3-propylene diamine; soya
1,3-propylene diamine and the like.
Other suitable cation-active softener/antistat compounds
herein are the quaternary imidazolinium salts. Preferred
salts are those conforming to the formula
~ -19-
I` ~ t'-
~1~0260
.H I
.; H - C C -- H O
~: N~ ~N~ C2H4 1 C R7 X
P~8
~ . . ,
. ~'.- ', ' .
.. _ . ... _ ... ... ~ . . . . . . ... . , .... , , _ _ _ _ _ _ _ _
` '
. . .
.' - '
'" ' ' " ,
.
,
'
:
1~0~260
wherein R6 is an alkyl containing from 1 to 4, preferably
from 1 to 2 carbon atoms, R5 is an alkyl containing from 1
to 4 carbon atoms or a hydrogen radical, R8 is an alkyl
containing from 1 to 22, preferably at least 15 carbon atoms or
a hydrogen radical, R7 is an alkyl containing from 8 to 22, pre-
ferably at least 15 carbon atoms, and X is an anion, preferably
methylsulfate or chloride ions. Other suitable anions include
those disclosed with reference to the cationic quaternary ammoni-
um fabric softener/antistats described hereinbefore. Particularly
preferred are those imidazolinium compounds in which both R7 and
R8 are alkyls of from 12 to 22 carbon atoms, e.g., l-methyl-l-
I(stearoylamide)ethyl]-2-heptadecyl-4,5-dihydroimidazolinium
methyl sulfate; l-methyl-l-[(palmitoylamide)ethyl]-2-octadecyl-4,5-
dihydroimidazo'inium chloride and l-methyl-l-[(tallowamide) ethyl]~
2-tallow-imidazolinium methyl sulfate.
~. -~1-
11~(1 260
Other cationic quaternary ammonium fabric softener/antistats
which are useful herein include, for example, alkyl (C12 to C22)-
pyridinium chloridesr alkyl (C12 to C22)-alkyl (C1 to C3)-morpho-
linium chlorides, and quaternary derivatives of amino acids and
amino esters.
Nonionic fabric softener/antistat materials include a wide
variety of materials including sorbitan esters, fatty alcohols
and their derivatives, diamine compounds and the like. One pre-
ferred type of nonionic fabric antistat/softener material com-
prises the esterified cyclic dehydration products of sorbitol,
i~e., sorbitan ester. Sorbitol, itself prepared by catalytic
hydrogenation of glucose, can be dehydrated in well-known fashion
to form mixtures of cyclic 1,4- and 1,5-sorbitol anhydrides and
small amounts of isosorbides. (See Brown; U.S. Patent 2,322,821;
issued June 29, 1943) The resulting complex mixtures of cyclic
anhydrides of sorbitol are collectively referred to herein as
"sorbitan". It will be recognized that this "sorbitan" mixture
will also contain some free uncyclized sorbitol.
Sorbitan ester fabric softener/antistat materils useful
herein are prepared by esterifying the "sorbitan" mixture with
a fatty acyl group in standard fashion, e.g., by reaction with
a fatty (C10-C24) acid or fatty acid halide. The esterification
reaction can occur at any of the available hydroxyl groups, and
various mono-, di-, etc., esters can be prepared. In fact,
complex mixtures of mon-, di-, tri-, and tetra-esters almost
always result from such reactions, and the stGichiometric ratios
of the reactants can simply be adjusted to favor the desired
reaction product.
The foregoing complex mixtures of esterified cyclic
dehydration products of sorbitol (and small amounts of esterified
sorbitol~ are collectively referred to herein as "sorbitan esters".
Sorbitan mono- and di-esters of lauric, myristic, palmitic,
~ -22-
260
stearic and behenic acids are particularly useful herein for
conditioning the fabrics being treated. Mixed sorbitan esters,
e.g., mixtures of the foregoing esters, and mixtures prepared by
esterifying sorbitan with fatty acid mixtures such as the mixed
tallow and hydrogenated palm oil fatty acids, are useful herein
and are economically attractive. Unsaturated C10-Cl8 sorbitan
esters, e.g., sorbitan mono-oleate, usually are present in such
mixtures. It is to be recognized that all sorbitan esters, and
mixtures thereof, which are essentially water-insoluble and
which have fat~y hydrocarbyl 'Itails''~ are useful fabric softener/
antistat materials in the context of the present invention.
- The preferred alkyl sorbitan ester fabric softener/antistat
materials herein comprise sorbitan monolaurate, sorbitan mono-
myristate, sorbitan monopalmitate, sorbitan monostearate, sorbi-
tan monobehenate, sorbitan dilaurate, sorbitan dimyristate,
sorbitan dipalmitate, sorbitan distearate, sorbitan dibehenate,
and mixtures thereof, the mixed coconutalkyl sorbitan mono-
and di-esters and the mixed tallowalkyl sorbitan mono- and di-
esters. Thé tri- and tetra-esters of sorbitan with lauric,
myristic, palmitic, stearic and behenic acids, and mixtures
thereof, are also useful herein.
Another useful type of nonionic fabric softener/antistat
material encompasses the substantially water-insoluble compounds
chemically classified as fatty alcohols. Mono-ols, di-ols,
and poly-ols havins the requisite melting points and water-
insolubility properties set forth above are useful herein. Such
alcohol-type fabric conditioning materials also include the mono-
and di-fatty glycerides which contain at least one "free" OH
group.
-23-
Z60
All manner of water-insoluble, high melting alcohols
(including mono- and di-glycerides), are useful herein,
inasmuch as all such materials are fabric sustantive. Of
course, it is desirable to use those materials which are
colorless, so as not to alter the color of the fabrics being
treated. Toxicologically acceptable materials which are
safe for use in contact with skin should be chosen.
A preferred type of unesterified alcohol useful herein
includes the higher melting members of the so-called fatty
alcohol class. Although once limited to alcohols obtained
from natural fats and oils, the term "fatty alcohols" has
come to mean those alcohols which correspond to the alcohols
obtainable from fats and oils, and all such alcohols can be
made by synthetic processes. Fatty alcohols prepared by the mild
oxidation of petroleum products are useful herein.
Another type of material which can be classified as an
alcohol and which can be employed as the fabric softener/
antistat material in the instant invention encompasses
various esters of polyhydric alcohols. Such "ester-alcohol"
materials which have a melting point within the range recited
herein and which are substantially water-insoluble can bè
employed herein when they contain at least one free hydroxyl
sroup, i.e., when they can be classified chemically as
alcohols.
The alcoholic di-esters of glycerol useful herein include
both the 1,3-di-glycerides and the 1,2-di-glycerides.
In particular, di-glycerides containing two C8-C20, preferably
C10-Cl8, alkyl groups in the molecule are useful fabric condi-
tioning agents.
Non-limitlng examples of ester-alcohols useful herein include:
.
t~ ` --24--
l~OQ260
glycerol-1,2-dilaurate; glycerol-1,3-dilaurate; glycerol-1,2-
dimyristate; glycerol-1,3-dimyristate; glycerol-1,2-dipalmitate;
glycerol-1,3-dipalmitate; glycerol-1,2-disteara~e and glycerol-
1,3-distearate. Mixed glycerides available from mixed tallow-
alkyl fatty acids, i.e., 1,2-ditallowalkyl g'ycerol and 1,3-
ditallow--alkyl glycerol, are economically attractive for use
herein. The foregoing ester-alcohols are preferred for use
herein due to their ready availability from natural fats and oils.
~ - 2
26o
Mono- and di-ether alcohols, especially the C10- C18
di-ether alcohols having at least one free -OH group, also
fall within the definition of alcohols useful as fabric
softener/antistat materials herein. The ether-alcohols can
be prepared by the classic Williamson ether synthesis. As with
the ester-alcohols, the reaction conditions are chosen such
that at least one free, unetherified -OH group remains in the
molecule.
Ether-alcohols useful herein include glycerol-1,2-
dilauryl ether; glycerol-1,3-distearyl ether; and butane
tetra-ol-1,2,3-trioctanyl ether.
Yet another type of nonionic fabric softener/antistat
agent useful herein encompasses the substantially water-
insolu~le (or dispersible) diamine compounds and diamine deriva-
tives. The diamine fabric conditioning agents are selected from
the group consisting of particular alkylated or acylated
- diamine compounds.
Useful diamine compounds have the general formula
-26-
. ,~ .
lll)OZ60
1 2 1 3
R~ (CH;2 ) n 4
:~ ~' '` ~ . .
s
.
.
)Z60
wherein Rl is an alkyl or acyl group containing from about 12
to 20 carbon atoms; R2 and R3 are hydrogen or alkyl o. from
ahout 1 to 20 carbon atoms and R4 is hydrogen, Cl 20 alkyl or
C12 20 acyl. At least two of R2, R3 and R4 are hydrogen or
alkyl containing 1 to 3 carbon atoms, and n is from 2 to 6.
Non-limiting examples of such alkylated diamine compounds
include:
15H31 N(CH3) (CH2)3-N(CH3)2
18H37 N(CH3)-(CH2)2-N(C2H5)2
C12H25-N(CH3)-~cH2)3 HN C12 25
12H25 N (C2H5)--(CH2) 3--N (C3H7) 2
RTallow NH~(CH2)3 N(C2H5)2
20 41 N(CH3)-(CH2)2-N(CH3)2
C15H31 ~ (C2H5)--(CH2) 3--NH2
C18H 7-NH-~CH ) -HN-CH
C16H33-NH-(CH2)3 HN C16 33
Tallow N(CH3)-(CH2)3-N(C2H
16H33N(CIL3)-(CH2)5-N(C2H5)2
12 25N(c2Hs)-(cH2)2-N(c3H7)2 and
14 29N(CH3) ~CH2)3-(CH3)N-C8H17
wherein in the above formulas RTallow is th~ alkyl ~roup
derived from tallow fatty acids.
~ -28-
260
Other examples of suitable aklyated diamine compounds
include N-tetradecyl, N'-propyl-1,3-propane-diamine,
N~e cosyl,N,N',N'-triethyl-1,2-ethane-diamine and N-octadecyl,
N,N',N'-tripropyl-1,3-propane-diamine.
Examples of suitable acylated diamine fabric softener/
antistat materials include C13 20 amido amine derivatives.
The fabric softener/antistats mentioned above can be used
singly or in combination in the practice of the present
invention.
Preferred materials for use herein are ditallowdimethyl-
ammonium methylsulfate, l-methyl-l [(tallowamide)ethyl3-2-tallow
imidazalonium methyl sulfate and mixtures of either of these with
sorbitan tristearate in a ratio of from about 50:50 to about
100:0, more preferably 80:20 to 100:0, cationic material to the
sorbitan compound.
~ -29-
11C~026U
Optional Components for Fabric
Softener!Antistat Composition
In addition to the softener/antistat agents the particles
herein can also optionally contain minor proportions (i.e., 0.01%
to about 15% by weight of the total particle composition) of various
other ingredients which provide additional fabric conditioning
benefits. Such optional ingredients include perfumes, fumigants,
bactericides, fungicides, optical brighteners and the like. Spe-
cific examples of typical solid, water-soluble additives useful
herein can be found in any current Year Book of the American
Association of Textile Chemists and Colorists. Such additional
components can be selected from those compounds which are known
to be compatible with the softener/antistat agents employed
herein.
A preferred optional ingredient is a fabric substantive
perfume material. Included among such perfume materials are
musk ambrette, musk ketone, musk xylol, ethyl vanillin, musk
tibetine, coumarin, aurantiol and mixtures thereof. The above
perfumes are preferably used in an amount of from about 0.1% to
about 5% by weight of the total particle composition.
The water-soluble silicate materials recognized in the
art as corrosion inhibitors can be employed in the present
compositions at levels of about 5% by weight.
-30-
260
Separation of Eleatrolyte/pH Control Agent
from Film'Coated Fabric Softener/Anti'stat Particles
The articles of the present invention require that the
electrolyte/pH control agent (insolubilizing agent) be separated
from the film coated fabric softener/antistat particles. Such
separation is necessary to reduce the tendency of the film to
become very insoluble due to occlusion of the insolubilizing agent
by the film. The separation can take many forms with the only
requirement being that the separation allow the insolubilizing
agent to be released to the wash water and dissolved before it
makes contact with the film coating the fabric softener/antistat
particles. Several methods of separation are given below.
The first method is to simply put the electrolyte/pH
control agent into a separate recPptacle from the one containing
the fabric conditioning agent. With this execution the two
receptacles form a kit with both receptacles being used simul-
taneously in the wash bath. The receptacle containing the
electrolyte/pH control agent is constructed in the same manner
and from the same materials described hereinbefore for the
receptacle holding both the electrolyte/pH control agent and
the fabric conditioning particles. Further, the receptacle may
be constructed of any water-soluble material which is not
affected by the level of electrolyte/pH control agent present
in the receptacle. Such materials include but are not limited
to polyethylene oxide, polyvinyl pyrrolidone, and cellulose
derivatives among many others.
The preferred separation of the actives in the present
invention involves having a single receptacle with the
separating barrier being provided within the receptacle. The
separation can be obtained by sealing one part of the receptacle
off from the other by means of: (1) sewing, sonic sealing,
~ -31-
)260
gluing or some other similar means; the materials used for gluing
or sewing may be water-insoluble or water soluble and dissolve
after the insolubilizing agent has escaped; (2) inserting an
additional wall within the receptacle, which wall is constructed
of a water-insoluble material which is impermeable or permeable
and having a porosity of less than 300 cubic feet per minute per
square foot of surface area (cfm), or a water-soluble material; or
~3) placing a coating of a water-soluble material around the film
coated fabric conditioning particles. The water-insoluble
impermeable or permeable material can be any of these mentioned
hereinbefore for the walls of the receptacle. The impermeable
nature can be o~tained by a simple selection of materials.
The same is true of the material having a permeability of less
than 300 cfm. This degree of permeability allows for the elec-
trolyte/pH control agent to escape from the receptacle before
coming into contact with the fabric conditioning particles. The
fabric conditioner is, however, able to move through the wall and
utilize all of the porous surface of the receptacle to escape
into the rinse water of the washer.
The water-soluble material which can be used to construct
the additional wall can be any of a wide variety of materials
whïch are not affected by the level of electrolyte/pH control
agent present in the article. Such materials include polyvinyl-
pyrrolidone, polyethylene oxide, carboxymethyl cellulose and
other cellulose derivatives. Additionally the wall may be construct-
;~ ed of a water insoluble web which has its openings filled with a
material such as polyethylene glycol.
These same materials can be used to form a coating around
the film coated particles. This coating takes the place of the 30 wall and like the wall will dissolve after the electrolyte/pH
control agent has escaped from the receptacle into the wash water.
The coating can be accomplished as described hereinafter.
^ /i -32-
.
- ~\
llO~)Z60
The water~soluble materials can ha~e molecular weights in
the range indicated hereinbefore for the film which is insolubi-
lized by the pH control agent/electrolyte (i.e. 2,000 to about
200,000). When in the form of a wall the thickness is preferably
from about 0.1 mil. to about 5 mil. When used as a coating the
material preferably amounts of from about 0.1% to about 50%,
more preferably 3% to about 10%, by weight of the coated fabric
so~tener/antistat particle.
~ ~32a-
260
Fabric Antistat Particles
The other factor important in the present invention's arti-
cles' ability to deliver superior fabric softening and static
reduction is the presence of fabric antistat particles. These
particles are not coated with the film which coats the fabric
softener/antistat particles. The coating is not necessary due to
the formulation of the antistat particles and their physical nature.
Additionally, the antistat particles need not be separated from
the insolubilizing agent and may be placed in with the insolubiliz-
;ng agent, the coated fabric softener/antistat particle or both.
The antistat particles are comprised of a mixture of cationic
antistat agents and a solid organic dispersion inhibitor. The
cationic antistat agents can be any of those mentioned previously
herein for the coated softener/antistat particles. Preferred
- agents include ditallowdimethyl ammonium methylsulfate and l-methyl-
l-[(tallowamide)ethyl3-2-tallow imidazolinium methylsulfate.
The dispersion inhibitor functions as described in U.S. Patent
3,936,537, February 3, 1976, to Baskerville, Jr., et al. The
materials which function as a dispersion inhibitor are generally
those solid organic materials having a softening point of 35 -
95C, a water-solubility not greater than 50 parts per million
(ppm) and is selected from the group consisting of paraffinic
waxes, cyclic and acylic mono- and polyhydric alcohols, substituted
and unsubstituted aliphatic carboxylic acids, esters of the fore-
going alcohols and acids, C3-C4 alkylene oxide condensates of
any of the foregoing materials and mixtures thereof. Preferred
for use herein are the aliphatic fatty alcohols described
previously, saturated fatty acids having 12 to 24 carbon atoms
in the alkyl chain, such as lauric, myristic, palmitic, stearic
and behenic; and the sorbitan esters described previously. Most
30 preferred for use as the dispersion inhibitor are the sorbitan
esters, particularly sorbitan tristearate.
~ -33-
ll~Q260
The antistat agent and the dispersion inhibitor are present
in the antistat particles herein in a ratio of from about 90:10
to about lO:90, preferably from about 50:50 to about 20:80. A
preferred combination of materials is sorbitan tristearate and
dimethylditallowammonium methylsulfate.
The fabric antistat particles, preferably have a particle
size of from about 200 to about lO,000 microns, most preferably
of from about 500 to about 5,000 microns. Particles of such size
can conveniently be made by forming a melt of the antistat agent(s)
and the dispersion inhibitor, dropping droplets of the melt into
cold water to harden and recovering the hardened droplets.
A desirable additive for the fabric antistat particles is a
fabric substantive perfume. Examples of such materials are given
herein previously as optional components with the coated fabric
softener/antistat particles. The amount of perfume used is from
about 0.1% to about 10% of the weight of the fabric antistat
particles.
-34-
` - ,
260
Prep`aration and Usage
The articles of the present invention are prepared by
fashioning a receptacle of the type hereinbefore described and
enclosing therein an effective amount of the film coated fabric
softener/antistat particles. By an "effective amount" of the
fabric softener/antistat particles herein is meant an amount
sufficient to condition an average load of fabrics in an auto-
matic washer/dryer. Of course, the actual amount of the fabric
softener/antistat particles employed will depend on the fabric
load and the particular agents selected for use in the article.
For example, when an average 5 lbs. to 8 lbs. load of fabrics is
being treated, from about 1 gram to 12, preferably 1 to 6, grams
of any of the foregoing softener/antistat agents provide good
fabric conditioning. The lower level is acceptable for use
herein due to the ability of the articles of this invention to
protect the conditioning agent from being lost during the washing
process. The particles may be formed in any convenient manner.
- A preferred method is to form prills by spraying a melt of the
actives into a cooled, closed tower.
The amount of fabric antistat particles used with loads of
the above size is generally from about 0.1 to about 5 grams,
preferably 0.5 to about 1.5 grams. Since these particles do not
escape from the article in the wash, the lower levels provide
excellent static reduction.
The fabric softener/antistat particles are coated with the
film capable of being insolubilized/made indispersible by pH or
electrolyte level. This coating can be applied to individual
particles or preferably agglomerates of particles by techniques
which are well known in the art. For example, with the preferred
polyvinyl alcohol coating material the particles can be sprayed
with an aqueous polyvinyl alcohol coating in a closed coating
cannister in which the coating agent is sprayed onto a fluid bed
of the fabric softener/antistat particles.
~ -35-
110~260
Agglomeration is a weIl-known granule formation technique
and can be undertaken in any convenient, conventional manner.
Generally, an aqueous slurry, solution or melt of an agglomerat-
ing medium is prepared and sprayed into an agitated dry mixture
of the softener/antistat agent. Other solvents such as ethanol
may also be used. Any suitable spraying device can be used and
the agglomerating medium can be the same agent that is used to
coat the agglomerate. The agglomerating/coating materials may
contain plasticizers such as glycerol to make them more flexible.
Since it is desirable to retain the coated particles or ag-
glomerates within the receptacle until the rinse cycle or the
dryer cycle, the size of particles should be selected such that
the particles in coated form are larger than the openings in
the receptacle walls (generally from about 200 to about 1500
microns~. The particles/agglomerates, once the coating is re-
moved, should be small enough to pass through the porous walls
or capable of easily breaking into smaller particles which can
pass through the porous portion of the receptacle (generally
from about 40 to about 120 microns).
The receptacle herein can be provided in a variety of sizes
and shapes and the particular configuration of the receptacle
is not critical to the practice of this invention. For example,
the receptacle herein can be provided wherein only one wall, or
a portion of one wall, comprises the materials described previously
herein. Preferably the whole of the receptacles comprise the
described materials.
In its simplest and preferred aspect, the article herein
is prepared in theshape of a pouch. The receptacle in the
preferred articles comprises a nonwoven polyester cloth having
an air permeability of from about 700 to about 1400 cubic feet
per minute per square foot. In one preferred execution the
receptacle is formed by sealing three edges of the material by
-~ -36-
1100260
heat, glue, sewing or sonic sealing, leaving an opening along
one edge. The fabric softener/antistat particles in this pre-
ferred embodiment are coated with polyvinyl alcohol and subse-
quently coated with a thin coating of polyethylene glycol or
polyethylene oxide. The coated particles are added to the re-
ceptacle along with an eIectrolyte, preferably a mixture of
sodium metaborate/sodium borate, and the fabric antistat parti-
cles. The fourth edge is then sealed.
- In another preferred embodiment herein the above-described
pouch is split into two parts by sonic sealing or conventional
sewing. The coated particles, again preferably coated with poly-
vinyl alcohol, are placed into one half of the pouch and the
electrolyte is placed into the other half. The fabric antistat
particles are preferably split between the parts although they
may be put entirely in one part or the other. The pouch is then
completely sealed.
In yet another preferred embodiment herein the pouch, rather
~ than being split as described above, has an additional wall
; placed within it to split the pouch. This additional wall is
preferably made of polyester and possesses an air permeability
- of less than 300 cfm. Into one half ar0 placed the fabric
softener/antistat particles while the electrolyte/pH control
agent is placed into the other half. The fabric antistat parti-
cles are split between the sides.
As was noted hereinbefore, the size of the present articles
is not criticai and can be whatever the manufacturer desires.
For ease of handling, however, it is preferred that the receptacle
be from about 2 inches x 3 inches to about 4 inches x 6 inches.
The preferred pH control agent/electrolyte for use with the
polyvinyl alcohol coated particles is a sodium borate or sodium
borate/metaborate system sufficient to provide a molar boron
- concentration of from about 1 x 10 3 to about 2 x 10 2 and a pH
greater than 8.5, preferably 9.0-9.5 in the wash water.
~ -37-
Z60
Usage
The articles of the present invention can be utilized in a
variety of ways depending on the desires of the user. In a pre-
ferred process, an article prepared as described herein is placed
;n with a load of fabrics at the start of the wash cycle in a
standard clothes washer and left with the fabrics through the
entire wash, rinse and spin drying cycles. The temperature of
the wash and rinse waters can be any temperatures desired by the
user, but generally are in the range of from about 4C to about
60C. The article then remains with the damp fabrics when they
are placed in the drum of an automatic clothes dryer. The dryer
i6 operated in standard fashion to dry the fabrics, usually at a
temperature from about 50C to about 80C for a period of from
about lO to about 60 minutes.
The detergent composition which can be used to wash the
fabrics during the above-described wash cycle can be any convention-
al detergent compositlon. Such a composition generally contains
from about 1% to about 50% of a detersive surfactant. The
detergents may be liquid or solid and contain other components
such as a detergency builder, bleaches, enzymes, among other
detergency adjuvants. The surfactants which may be used include
any of the common anionic, nonionic, ampholytic and zwitterionic
detersive agents well known in the detergency arts. Mixtures of
surfactants may also be used. Examples of surfactants are given
in U.S. Patents 3,717,630, Booth, February 20, 1973, and 3,443,880,
Kessler et al., July 25, 1967.
The detergency builder salts which are oftentimes utilized
in detergent compositions include both inorganic, as well as
organic, water-soluble builder salts and the various water-
insoluble and so-called "seeded" builders. Typical laundry
detergent compositions are designed to provide a concentration of
builder salt of from about 50 ppm to about 1000 ppm and a concen-
tration of detersive surfactant in the range of 50 ppm to about
-38-
.
Z60
1000 ppm. These concentrations are generally met in the average
aqueous solutions used to wash fabrics (5-25 gallons). The amount
of detergent composition utilized per wash load is familiar to
users of laundry products and ranges from about 1/4 cup to 1 1/4
cup .
- The performance delivered by the receptacles herein when used
as described above is equivalent to a rinse added liquid softener
in terms of softness and a dryer added sheet in terms of static
control.
- 10 All percentages and ratios used herein are by weight unless
otherwise designated.
The invention will be further illustrated by the following
nonlimiting examples:
-39-
Z60
Example I
An article of the present invention in the form of a pouch
is made in the following manner:
A. One hundred parts of a particulate fabric softener/
antistat composition comprising 20% sorbitan tristearate
and 80% ditallowdimethylammonium methylsulfate is
agglomerated with one part of polyvinyl alcohol, 88%
hydrolyzed, medium viscosity and plasticized with 0.1
part glycerol, and subsequently coated with 2 parts of
the same polyvinyl alcohol which is plasticized with
0.2 parts of glycerol. Polyvinyl alcohol at a level
of 8% and 0.8% glycerol are dissolved in 50% ethyl
alcohol and 41.2% water for this application. The
fa~ric softener/antistat particles are formed by spraying
a melt of the softener/antistat composition into a
cooled tower to form prills. These prills are sprayed
with the polyvinyl alcohol solution in an agglomerating/
coating cannister.
B. A pouch measuring 3 inches x 4 1/2 inches is formed
with walls having two polyester layers, one layer having
a basis weight of 20 grams/sq. yd. and the other being
air laid and having a basis weight of 45 grams/sq. yd.
C. The pouch of (B) is bonded on three edges, two long
edges and one short, using an ultrasonic sewing machine.
D. To the sealed pouch of (C) is added 10 grams of sodium
tetraborate decahydrate and 15 grams of sodium metaborate
octahydrate.
E. The part of the pouch of (D) containing the borate/
metaborate salts is sealed using a thread stitching.
F. Six grams of the coated fabric softener/antistat
composition of (A) is added to the pouch of (E).
-40-
)260
G. One gram of fabric antistat particles made of 6 parts
of sorbitan tristearate and 2 parts of ditallowdimethyl-
ammonium methylsulfate are added to the side of the
pouch containing the fabric softener composition. The
unsealed end of the pouch is then sealed using an ultra-
sonic sewing machine.
The fabric antistat particles are made by melting the
materials and dropping droplets of the melt into a water trough
carrying water (~20C). Hard particles having an average parti-
cle size of ~2000 microns are recovered and used as described
in (G).
A similar article to that described above is made but the
fabric antistat particles are not added.
EXAMPLE II
The pouches of Example I are added to separate automatic
washers along with a 5.5 lb. bundle of unsoiled fabrics and 96
grams o an anionic detergent. The washers are operated for
14 minutes using 32C temperature water. After the completion
of the wash cycle, the rinse cycle using 32C water and the spin
dry cycles are completed. The two fabric loads along with the
pouches are placed into separate dryers which are operated for
a period of 50 minutes at a normal temperature setting. Three
additional treatments identical to those described above are also
conducted.
The results of all treatments show that the articles of the
present invention in which the fabric antistat particles are
present deliver superior static control as determined by visual
observation.
-EXAMPLE III
An article of the present invention in the form of a pouch
is made as described in Example I. However, in this instance
-41-
' ` ' '
260
the fabric antistat particles are made of 6 parts of sorbitan
tristearate, 1 part of ditallowdimethylammonium methylsulfate
and 1 part of 1-methyl-1-[(tallowamide)ethyl]-2-tallowimidazo-
linium methylsulfate. Additionally, 1/2 gram of the fabric
antistat particles are added to the pouch half containing the
coated fabric softener/antistat particles and 1/2 gram to the
pouch half containing the borate/metaborate salts.
When the above-described article is tested as described in
Example II, it delivers static control superior to that delivered
by the pouch having no fabric antistat particles.
In the above examples equivalent results are obtained by
using one or more of the following in place of the fabric
softener/antistats used: sorbitan monostearate, l-methyl-l-
[(tallowamide)ethyl]-2-tallowimidazolinium methylsulfate, other
sorbitan esters and other quaternary ammonium compounds.
Similarly, in the fabric antistat particles, the sorbitan
esters may be replaced by tallow alcohol, "Castorwax"
triglycerides and parrafinic waxes with equivalent results
obtained.
.
*Trademark for hydrogenated castor oil
. .
. . ~ .
