Note: Descriptions are shown in the official language in which they were submitted.
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CLEANING METHOD FOR TEXTILE FABRICS
The present invention relates to a method of removing
spots and stains from textile fabrics.
Some stains are not always effectively removed by
conventional laundry cleaning processes, for example in
a washing machine. Such stains may be more effectively
removed by pre-treatment, which herein means a cleaning
treatment carried out before the conventional laundry
cleaning process; and/or by post-treatment, which herein
means a cleaning treatment carried out after the
conventional laundry cleaning process. The present
invention is concerned with a post-treatment cleaning
method.
EP200807, published on 12th November 1986, discloses an
iron intended for cleaning clothes during ironing, i.e.
a post-treatment. To achieve this objective the housing
of the iron can be adapted with a recess to receive a
brush (page 3, line 22 to page 4, line 1). The iron is
also provided with vacuum cleaning means. There is no
suggestion that cleaning compositions could be used to
~nh~nce the cleaning method.
US3748268, published on 24th July 1973, discloses spot
and stain removing detergent compositions. The
compositions are intended primarily for cleaning
carpets, although textile fabrics are also mentioned The
patent suggests that a pre-treatment cleaning method
comprising gentle rubbing action may be used to help
work the detergent composition into the stain, followed
by stain removal using a dry absorbent cloth. Water is
then applied to complete the cleaning operation,
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optionally using an absorbent material to remove the
soil and composition remnants.
Many textile fabrics, however, especially those made
from silk or wool, are much more delicate than carpets.
What may be considered as a gentle rubbing action when
applied to a carpet could be considered as a harsh
rubbing action when applied to a textile fabric. The
very gentle treatment that i6 acceptable for delicate
fabrics, however, may result in incomplete ~el..vval of
stains.
DE-A-43 03 454, published on 11th August 1994, describes
a process for stain ~c...~v~l and a stain removal set. The
process comprises the steps of applying a stain remover
to a stain which is then activated and washed out with
hot water. The hot water is applied by means of heating
water in a sponge using a hot iron. This cl~n; ng
process results in water being applied to a large area
of the ~abric, i.e. and area corresponding at least to
the area of the sponge, which can result in fresh,
greasy stains being spread over the ~abric rather than
being ellloved. Furthermore, the presence of the sponge
between the fabric and the iron prevents the heat from
effectively reaching the region of the spot or stain.
Simply applying more heat from the iron results in
scorching or melting the sponge.
The object o~ the present invention is to provide a more
e~fective method of treating a spot or stain on a
textile ~abric comprising the steps of: applying a
detergent composition to the spot or stain; placin~ an
absorbent layer adiacent to one side of the textile
~abric in the region of the spot or stain; and applying
heat, pressure, or heat and pressure so that some or all
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of the spot or stain is absorbed into the absorbent
layer.
It is a further object of the present invention that the
textile fabric should be dry and ready to wear at the
end of the cleaning method.
Summary of the Invention
The ob~ect of the invention is achieved by applying the
heat and/or pressure to the opposing side of the textile
fabric in the region o~ the spot or stain preferably in
the presence of a hydrophilic solvent or water. Without
wishing to be bound by theory it is believed that the
application o~ heat and/or pressure improves the
cleaning efficiency by modi~ying the physical
characteristics, such as viscosity, which promotes
better penetration of the detergent composition into the
stain, thereby improving cle~n; ng ef~iciency.
Furthermore the application of heat evaporates any -
residual water leaving the textile fabric dry.
In a preferred embodiment of the invention a method of
treating a spot or stain on a textile ~abric is provided
comprising the steps of:
(a) applying a detergent composition to the spot or
stain and placing an absorbent layer ad~acent to the
textile ~abric in the region of the spot or stain and a
first means for transferring some or all of the spot or
stain into the absorbent layer; and subsequently
(b) applying a hydrophilic solvent, or water, to the
textile fabric in the region of the spot or stain and
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placing an absorbent layer adjacent to the textile
fabric in the region of the spot or stain and a second
means for trans~erring some or all of the spot or stain
into the absorbent layer.
The second means for tranqferring the stain to the
absorbent layer is preferably by applying heat, more
preferably by using a hand-held domestic iron. The first
means for transferring some or all of the spot or stain,
preferably comprises the step of rubbing, pressing or
brushing the spot or stain.
Brief Description of the Drawings
Fig 1 shows the top and longitll~; n~l view of a
container
with a foam pad secured to its cap. The cap has
a
small central opening through which the liquid
can
pass.
Fig 2 shows the top and longitl~;n~l view of a
container
with a brush secured to its cap. The cap has a
small central opening through which the li~uid
can
pass.
Fig 3 shows the top and longitudinal view of a
cont~; n~
with a convex shaped polypropylene porous pad.
The
pad has pore size ranging from 300 to 700
micrometers.
Fig 4 shows the top and longitudinal view of a
container
with a convex shaped polypropylene porous pad
and a
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supporting plate which has a plurality of holes
which restricts the amount of liquid that passes
through the porous material. The pad has pore
size
ranging from 300 to 700 micrometers.
Fig 5 shows the top and longitll~; nA l view of a
container
with a roll-on type extremity.
Fig 6 shows the top and longitll~;nAl view of a
container
with a piston-type extremity. Upon pressing of
the
tip of the piston against a fabric surface, a
liquid is released from within the container
onto
the fabric.
Fig 7 shows the longitll~; nA 1 view of a conventional
container with an elongated extremity, used to
apply liquid on surfaces.
Fig 8 shows a hand-operated device having sponge-type
first and second treatment members.
Fig 9 shows a hand-operated device having a brietled
protuberances comprising the ~irst treatment
member
and a disposable sponge as a second treatment
member.
Fig lO shows a hand-operated device with the first and
second treatment members comprising looped
protuberances.
Detailed Description of the Invention
A most preferred cleaning method comprises the steps o~:
~a~ applying a detergent composition to a spot or stain
and placing an absorbent layer adjacent to the textile
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~abric in the region of the spot or stain and a ~irst
means ~or transferring some or all o~ the spot or stain
into the absorbent layer; and subsequently
(b) applying a hydrophilic solvent, or water, to the
textile ~abric in the region of the spot or stain and
placing an absorbent layer adjacent to the textile
fabric in the region of the spot or stain and the step
of applying heat to the textile fabric in the region o~
the spot or stain. The application of heat or pressure,
or both, may be achieved by any means, but i~ most
preferably achieved by a hand-held device such as an
iron. A conventional iron having a hot-plate ~ixed to a
body is a highly pre~erred hand held device. The hot-
plate is heated most co~monly by electrical means, and
may have a means for controlling the temperature. A
supply o~ water or steam may also be provided by the
iron. Most pre~erably the absorbent layer is placed on a
flat sur~ace, such as an ironing board, and the stained
or soiled textile ~abric is laid ~lat on top o~, and in
contact with, the absorbent layer. The iron can then be
easily applied to the textile ~abric in the region o~
the stain or spot in order to ensure complete, or
substantially complete, trans~er o~ the stain or spot
into the absorbent layer. The iron is pre~erably
operated at a temperature o~ from 40~C to 180~C.
An alternative device for applying heat or pressure is a
heated roller or any other heated applicator. The roller
or applicator may also be pro~ided with a supply o~ the
detergent composition.
Suitable applicators include a steam iron with suction
brush attachment, such as that disclosed in EP-A-0 493
348, and a thermoelectric applicator, such as that
disclosed in EP-A-0 552 397. Also suitable is a steam
iron with atomiser, such as that disclose in EP-A-0 629
736 wherein the detergent composition may optionally be
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stored in the iron and delivered directly onto the
textile fabrics by means of the atomiser.
Without wishing to be bound by theory it is believed
that hydrophobic stains are first rendered hydrophilic
0 by applying a detergent composition, optionally with a
gentle rubbing action; water i~ then applied to the
stain, again, optionally with a gentle rubbing action.
The stain is removed by laying the stained fabric
adjacent to an absorbent layer. The stain, which has
been rendered more hydrophilic by the treatment, is
transferred to the absorbent layer.
Textile fabrics are any materials made from cloth,
including garments such as shirts, blouses, socks,
skirts, trousers, jackets, underwear etc, and also
including tablecloths, towels, curtains etc. The
definition of textile fabrics as used herein does not
include carpets and similar ~loor coverings.
Textile fabrics which are to be used in the present
invention are commonly made by weaving or knitting. Many
different ~ibres may be used to produce woven, knitted
or other types of textile fabric including synthetic
fibres (such as polyester, polyamide, etc.) and natural
~ibres from plants (such as cotton, hemp) and from
~n;m~l S (8uch as wool, angora, silk). Blends of
different fibres are also commonly used.
Preferred components of the detergent composition will
~ now be described in more detail.
A highly preferred component of the detergent
composition for use herein is a solvent. More preferred
solvents are defined in terms of Hansen parameters. A
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hydrophobic solvent as defined herein is considered to
be a solvent having Hansen hydrogen bonding cohe~ion
parame~er dH below 18 (Joule/cm3)0 5 . Preferred
hydrophobic solvents ha~e a Hansen hydrogen bonding
cohesion parameter dH below 12 (Joule/cm3)~ 5 and a
Hansen polar parameter dP below 8 (Joule/cm3)0-5 .
Preferred ~olvents for use comprise mixtures of
hydrocarbons with a flash point no lower than 70~C, an
initial boiling point no lower than 130~C and a
solidification point not above 20~C and aliphatic fatty
acid esters. More preferred solvents would be Al k~n~s or
alkenes with a chain length above C7, and particularly
alkanes and alkenes with an average of C8 to C20 atoms.
Particularly pre~erred hydrophobic solvents are
deodorised kerosine; solvent naphta; chlorinated
hydrocarbons; and terpenes. Even more pre~erred are
paraffins; isoparaffins; naphthenes; aromatics; olefins;
1,1,1-trichloroethane perchloroethylene; methylene
chloride; Shellsol SS~ mixture (C8-Cll isoparaffin t 5
aliphatic C7 ester); and D-T~i mo~ene ~ Solvents are used
in the detergent compositions of the present invention
preferably at a level of ~rom 3% to 90~, more preferably
from 4~ to 45~, and most pre~erably from 5~ to 25~ by
weight o~ the detergent composition.
Other solvents having a Hansen parameter of dH less than
18 ~oule/cm3)0 5 include glycol ethers, more
preferably glycol ethers based upon ethylene oxide,
propylene oxide, or mixtures thereof. Particularly
preferred are ethylene glycol monoethyl ether; Propylene
glycol monomethyl ether; 2-butoxy ethanol; butyl
diethylene glycol ether ethanol; butoxytriglycol;
butylene glycol; hexylene glycol; and propyl propanol.
Such solvents may, and preferably are, used in
combination with either short chain surfactants, long
chain surfactants, or mixtures thereof.
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g
In one embodiment of the invention the hydrophobic
solvents defined above are used in combination with
mixtures of short chain and long chain surfactants
having preferably an overall HLB value of from 2 to 16,
and more preferably from 8 to 14. Preferred molar ratio
of short-chain to long chain ratios are from 1:10 to
10:1, more preferably between 1:3 and 3:1, most
preferably about 1:1.
Surfactants are preferably present at a level of from 1
to 50~, more preferably 10 to 40~ and most preferably 15
to 30~ by weight of the detergent composition.
Short chain surfactants are surfactants which comprise a
C6-C10 alkyl chain as their hydrophobic portion.
Preferred short-chain surfactants for use are the C4-C8
fatty alcohol polyglycol ethers with 2-~ E0. C6-C8 alkyl
sulphonates, C6-C8 alkyl sulphates, C6-C8 alkyl ethoxy
sulphates, C6-C10 betaines or C6-C10 amine oxides could
also be useful.
Long-chain surfactants useful in the detergent
compositions of the present invention include the
following.
Water-soluble salts o~ the higher fatty acids, i.e.,
'isoaps", are use~ul anionic sur~actants in the
compositions herein. This includes alkali metal soaps
such as the sodium, potassium, ethanolamine, ammonium,
and alkyl~mmo~;um salts o~ higher ~atty acids containing
from about 8 to about 24 carbon atoms, and preferably
from about 12 to about 18 carbon atoms. Soaps can be
made by direct saponification of fats and oils or by the
neutralization of ~ree ~atty acids. Particularly useful
are the ethanolamine, sodium and potassium salts o~ the
mixtures of fatty acids derived from coconut oil and
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tallow, i.e., monoethanolamine, sodium or potassium
tallow and coconut soap.
Useful anionic surfactants also include the water-
soluble salts, preferably the alkali metal,
ethanolamine, ammonium and alkylolammonium salts, of
organic sulfuric reaction products having in their
molecular structure an alkyl group cont~;n;ng from about
lO to about 20 carbon atoms and a sulfonic acid or
sulfuric acid ester group. (Included in the term "alkyl"
is the alkyl portion of acyl groups.) ~xamples of this
group of synthetic surfactant~ are the alkyl sul~ates,
especially those obtained by sulfating the higher
alcohols (C8-Clg carbon atoms) such as those produced by
reducing the glycerides of tallow or coconut oil; and
the a-kyl benzene sulfonates in which the alkyl group
contains from about 9 to about l~ carbon atoms, in
straight or branched chain configuration, e.g., those of
the type described in U.S. Pat. Nos. 2,220,099 and
2,477,383; and methyl ester sulphonates. Especially
valuable are l; n~ straight chain alkyl benzene
sulfonates in which the average number of carbon atoms
in the alkyl group is from about ll to 13, abbreviated
as Cll-C13 LAS.
Other anionic surfactants herein are the alkyl glyceryl
ether sulfonates, especially those ethers of higher
alcohols derived from tallow and coconut oil; coconut
oil fatty acid monoglyceride sulfonates and sulfates;
salts of alkyl phenol ethylene oxide ether sulfates
containing from about l to about lO units of ethylene
oxide per molecule and wherein the alkyl groups contain
from about 8 to about 12 carbon atoms; and salts of
alkyl ethylene oxide ether sulfates cont~;n;ng from
about l to about lO units of ethylene oxide per molecule
and wherein the alkyl group contains from about lO to
about 20 carbon atoms.
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11
other useful anionic surfactants herein include the
wat~r-soluble salts of esters of alpha-sulfonated fatty
acids containing from about 6 to 20 carbon atoms in the
fatty acid group and from about 1 to 10 carbon atoms in
the ester group; water-soluble salts of 2-acyloxy-
alkane-1-sulfonic acids cont~;n;ng from about 2 to 9
carbon atoms in the acyl group and from about 9 to about
23 carbon atoms in the alkane moiety; alkyl ether
sulfates containing from about 10 to 20 carbon atoms in
the alkyl group and from about 1 to 30 moles of ethylene
oxide; watersoluble salt~ of olefin sul~onates
cont~;n;ng from about 12 to 24 carbon atoms; and beta-
alkyloxy alkane sulfonates cont~;n;ng from about 1 to 3
carbon atoms in the alkyl group and from about 8 to
about 20 carbon atoms in the alkane moiety.
Water-soluble nonionic surfactants are also useful as
surfactants in the compositions of the invention.
Indeed, preferred processes use anionic/nonionic blends.
Such nonionic materials include compounds produced by
the con~n~tion of alkylene oxide groups (hydrophilic
in nature) with an organic hydrophobic compound, which
may be aliphatic or alkyl aromatic in nature. The
length of the polyoxyalkylene group which is condensed
with any particular hydrophobic group can be readily
adjusted to yield a water-soluble compound having the
desired degree of balance between hydrophilic and
hydrophobic elements.
Suitable nonionic surfactants include the polyethylene
oxide ~o~n~ates of alkyl phenols, e.g., the
con~n~ation products o~ alkyl phenols having an alkyl
group cont~;n;ng from about 6 to 16 carbon atoms, in
either a straight chain or branched chain configuration,
with from about 4 to 25 moles of ethylene oxide per mole
of alkyl phenol.
-
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12
.
Pre~erred nonionics are the water-soluble condensation
products of aliphatic alcohols containing from 8 to 22
carbon atoms, in either straight chain or branched
con~iguration, with from 1 to 25 moles of ethylene oxide
per mole of alcohol, especially 2 to 7 moles of ethylene
oxide per mole of alcohol. Particularly preferred are
the condensation products of alcohols having an alkyl
group cont~;ning from about 9 to 15 carbon atoms; and
con~n~ation products of propylene glycol with ethylene
oxide.
Other preferred nonionics are polyhydroxy fatty acid
amides which may be prepared by reacting a fatty acid
ester and an N-alkyl polyhydroxy amine. The pre~erred
amine for use in the present invention is N-(Rl)-
CH2 (CH20H) 4-CH2-OH and the preferred ester is a C12-C20
fatty acid methyl ester. Most preferred is the reaction
product of N-methyl glucamine ~which may be derived from
glucose) with C12-C20 fatty acid methyl ester.
Methods of manufacturing polyhydroxy fatty acid amides
have been described in WO 9206073, published on 16th
April, 1992. Thi~ application describes the preparation
of polyhydroxy fatty acid amides in the presence o~
solvents. In a highly preferred embodiment of the
invention N-methyl glucamine is reacted with a C12-C20
methyl ester.
Semi-polar nonionic sur~actants include water-soluble
amine oxides cont~;n;ng one alkyl moiety of from about
10 to 18 carbon atoms and 2 moieties selected from the
group consisting of alkyl groups and hydroxyalkyl groups
containing from 1 to about 3 carbon atoms; water-soluble
phosphine oxides containing one alkyl moiety of about 10
to 18 carbon atoms and 2 moieties selected from the
group consisting o~ alkyl groups and hydroxyalkyl groups
.;
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13
containing from about 1 to 3 carbon atoms; and water-
soluble sulfoxides containing one alkyl moiety of from
about 10 to 18 carbon atoms and a moiety selected from
the group consisting of alkyl and hydroxyalkyl moieties
o~ from about 1 to 3 carbon atoms.
Ampholytic surfactants include derivatives of aliphatic
or aliphatic derivatives of heterocyclic secondary and
tertiary amines in which the aliphatic moiety can be
either straight or branched chain and wherein one of the
aliphatic substituents contains from about 8 to 18
carbon atoms and at least one aliphatic substituent
contains an anionic water-solubilizing group.
Zwitterionic surfactants include derivatives of
aliphatic quaternary ammonium phosphonium, and sulfonium
compounds in which one of the aliphatic substituents
contains from about 8 to 18 carbon atoms.
Useful cationic surfactants include water-soluble
quaternary ammonium compounds of the form R4RsR6R7N+X~,
wherein R4 is alkyl having from 10 to 20, preferably
from 12-18 carbon atoms, and Rs, R6 and R7 are each C
to C7 alkyl preferably methyl; X~ is an anion, e.g.
chloride. Examples of such trimethyl ~mmo~; um compounds
include C12_14 alkyl trimethyl ~mmon; um chloride and
cocalkyl trimethyl ~mmon; um methosulfate.
Other surfactants that may be used in the compositions
o~ the present invention include C10-Cl8 glycerol
ethers, C10-18 alkyl polyglycoside and their
corresponding sulphated polyglycosides, alkyl ester
sulphonates, and oleoyl sarcosinate.
Enzymes can also be incorporated into the composition of
the present invention.
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14
The composition of the present invention can contain
neutral or alkaline salts which have a pH in solution of
~even or greater, and can be either organic or inorganic
in nature. While some of the salts are inert, many o~
them also function as detergency builder materials in
the laundering solution.
Examples of neutral water-soluble salts include the
alkali metal, ethanolamine, ammonium or substituted
Am~o~;um chlorides, fluorides and sulfates. The sodium,
ethanolamine and Ammon; um salts of the above are
preferred. Citric acid and, in general, any other
organic or inorganic acid may be incorporated into the
present invention.
Other useful water-soluble salts include the compounds
commonly known as detergent builder materials. Builders
are generally selected from the various water-soluble,
alkali metal, ethanolamine, ~mmo~; um or substituted
Ammon; um phosphates, polyphosphates, phosphonates,
polyphosphonates, carbonates, silicates, borates, and
polyhydroxysulfonates. Preferred are the sodium,
ethanolamine and ~m~n; um salts of the above.
Specific examples of inorganic phosphate builders are
sodium and potassium tripolyphosphate, pyrophosphate,
polymeric metaphosphate having a degree of
polymerization of from about 6 to 21, and
orthophosphate. Examples of polyphosphonate builders
are the salts of ethylene diphosphonic acid, the salts
of ethane 1-hydroxy-1,1-diphosphonic acid and the salts
of ethane, 1,1,2-triphosphonic acid. Other phosphorus
builder compounds are disclosed in U.S. Pat. Nos.
3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176
and 3,400,148, incorporated herein by reference. In
general, however, phosphates are preferably avoided for
environmental reasons.
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Example~ of nonphosphorus, inorganic builders are sodium
and potassium carbonate, bicarbonate, ses~uicarbonate,
tetraborate decahydrate, and silicate having a molar
ratio
of SiO2 to alkali metal oxide of from about 0.5 to about
4.0, preferably from about l.0 to about 2.4.
It is preferred that the detergent composition used ,
herein is in li~uid form, comprising active components
selected from those described above, the balance of the
detergent composition, typically from 5~ to 92~ by
weight, consisting of water. The preferred viscosity of
the detergent composition is from l to lO000 mPa.s, more
preferably from l to 4000 mPa.s, and most preferably
from l to 300 mPa.s.
Hydrophilic solvents for use herein are considered to be
those solvents having a Hansen parameter of either dH
more than 18 (Joule/cm3)0 5 , or dP more than 8
(Joule/cm3)0 5
Preferred hydrophilic solvents are: water (including
aqueous solutions); alcohol ~ethanol, IPA); glycol
ethers including diethylene glycol, triethylene glycol
and ethylene glycol; ethylene cyanohydrin; ethanol amine
and triethanolamine.
Bleaching agents may also be useful in the method of the
present invention for treating bleachable stains. The
bleaching agents may be incorporated into the
compositions described above, or may be added as
separate bleaching compositions. Peroxide bleaching
agents are most preferred.
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16
A~sorbent layers
As used herein, the term "absorbent layers~ refers
to ma~erials which absorb and contain fluids.
The absorbent layer may be any absorbent means which is
generally compressible, conformable, and capable of
absorbing and retaining liquids. The absorbent pad may
be manufactured in a wide variety of sizes and shapes
(e.g., rectangular, round, asymmetric, etc.). Examples
of suitable absorbent materials include co~m;nllted wood
pulp, creped cellulose wadding; meltblown polymers;
chemically stiffened, modified or cross-linked
cellulosic fibers; tissue including tissue wraps and
tissue laminates; absorbent foams; absorbent sponges;
superabsorbent polymers; absorbent gelling materials; or
any equivalent material or combinations of materials.
The configuration and construction of the absorbent pad
may also be varied (e.g., the absorbent pad may have
varying caliper zones, a hydrophilic gradient, a
superabsorbent gradient, or lower average density and
lower average basis weight acquisition zones; or may
comprise one or more layers or structures). Further, the
size and absorbent capacity of the absorbent pad may be
varied.
- Optionally, the absorbent layer can include a backsheet
which can be either liquid permeable (poly film) or not
(e.g. non-woven, too).If the backsheet is a poly film,
the following applies: The poly backsheet is positioned
on the bottom surface of the absorbent pad and is
preferably joined thereto by attachment means such as
those well known from the manufacture of disposable
articles. For example, the backsheet may be secured to
the absorbent pad by a uniform continuous layer of
adhesive, a patterned layer of adhesive, or an array of
separate lines, spirals, or spots of adhesive.
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17
Adhesives which have been found to be satisfactory are
manufactured by H. B. Fuller Company of St. Paul,
Minnesota and marketed as HL-1258. The attachment means
will preferably comprise an open pattern network of
filaments of adhesive as is disclosed in U.S. Patent
4,573,986 entltled "Disposable Waste-Cont~inm~nt
Garment", which issued to Minetola et al. on March 4,
1986, more preferably several lines of adhesive
filaments swirled into a spiral pattern such as i8
illustrated by the apparatus and methods shown in U.S.
Patent 3,911,173 issued to Sprague, Jr. on October 7,
~975; ~.S. Patent 4,785,996 issued to Ziecker, et al. on
November 22, 1978; and U.S. Patent 4,842,666 issued to
Werenicz on June 27, 1989. Alternatively, the attac~m~nt
means may comprise heat bonds, pressure bonds,
ultrasonic bonds, dynamic mechanical bonds, or any other
suitable attachment means or combinations of these
attachment means as are known in the art.
The backsheet is impervious to liquids and is
preferably manufactured from a thin, heat resistant,
plastic film, although other flexible liquid impervious
materials may also be used. The backsheet prevents the
liquids absorbed and contained in the absorbent pad from
wetting underlying materials. The backsheet may thus
comprise a woven or nonwoven material, polymeric films
such as thermoplastic films of polyethylene or
polypropylene, or composite materials ~uch as a ~ilm-
coated nonwoven material.
Optionally, the ab60rbent layer may include a topsheet
or outer, protective layer. The topsheet is liquid
pervious permitting liquids to readily penetrate through
- its thickness. Preferably, the characteristics of this
outer protective layer includes :
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18
- that it be of appropriate design to substantially
- prevent 1088 or transfer of fibers of the inner sorbent
material outwardly there through,
- that it preferably possesses sufficient heat transfer
or heat sink characteristics, to inhibit transfer of
sufficient heat through to the inner sorbent material to
cause substantial melting thereof; and,
- that it be relatively stable to heat from contact with
a hot domestic iron or the like
A suitable topsheet may be manufactured from a wide
range of materials, such as porous foams; reticulated
foams; apertured plastic films; or woven or nonwoven
webs of natural fibers (e.g., wood or cotton fibers),
synthetic fibers (e.g., polyester or polypropylene
fibers3, or a combination of natural and synthetic
fibers. There are a number of manufacturing techniques
which may be used to manufacture this topsheet. For
example, it may be a nonwoven web of fibers spunbonded,
carded, wet-laid, meltblown, hydroentangled,
combinations of the above, or the like. A preferred
topsheet is carded and thermally bonded by means well
known to those skilled in the fabrics art. A preferred
topsheet comprises a web of staple length polypropylene
fibers such as is manufactured by Veratec, Inc., a
Division of International Paper Company, of Walpole,
~as~h--~etts under the designatiion P-8.
Another usable non woven material is manufactured from
Crown ~ellerbach of Camas, under the trade name
Celestra.
.
The absorbent structure is located between the topsheet
and the backsheet, and mig~t comprise these two as in
integral element. It can be produced from a wide
CA 02238497 l998-0~-2~
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19
variety of liquid-absorbent materials, such as also
commonly used in disposable hygienic articles, such as
diapers, catamenials or Adult incontinence articles.
Exemplary absorbent structures for use as absorbent
layer as used in the disposable industry are described
in U.S. Patent 4,610,678 entitled "High-Density
A~sorbent Structures" issued to Weisman et al. on
September 9, 1986; U. S. Patent 4,673,402 entitled
"Absorbent Articles With Dual-Layered Cores~' issued to
Weisman et al. on June 16, 1987; U. S . Patent 4,888,231
entitled "Absorbent Core Ha~ing A Dusting Layer" issued
to Angstadt on December 19, 1939; and U.S. Patent
4,834,735, entitled "High Density Absorbent Members
Having Lower Density and Lower Basis Weight Acquisition
Zones~, issued to Alemany et al. on May 30, 1989. Other
absorbent pad designs are described in European Patent
Application No.'s 93305150.0 alld 93309614.1.
Exemplary designs comprise the use of fibrous (e.g.
cellulosic) materials in combination with
"Superabsorbent materials", essentially hydrogel forming
materials. Absorbent gelling materials are extensively
used in absorbent hygiene articles such as diapers or
sanitary napkins, due to their high absorption capacity
~or liquids, which may typically range from 15 g per
gram to about 50 g/g. The gelling material is most
often applied in particulate form in particle sizes
ranging from 20 to 2000 micrometers.
EP-A-O 407 838 discloses a gel-forming material for use
in foodstuf f S, which comprises a mixture of a
crosslinked polymer and a non-crosslinked polymer for
lump-free solution in water.
EP-A-O 278 601 discloses a mixture of an absorbent
gelling polymer, such as formed from water-soluble,
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ethylenically unsaturated monomers or crosslinked
products thereof, including acrylic acid or a salt of
acrylic acid as the main component, and inorganic
material such as aluminia, or silica. The polymers in
the mixture may be comprised of any combination o~ two
or more chemically different types. The disclosed
absorbent mixture is suited to absorb both low-viscosity
and high-viscosity liquids.
Wo 91/12029 discloses an odor control composition
comprising aggregated absorbent gelling material
particles and zeolite material. The absorbent gelling
material i8 made o~ hydrolized acrylonitrile grafted
starch, acrylic acid gra~ted starch, polyacrylates,
malice anhydride-ba~ed copolymers and combinations
thereof.
US patent No 4,333,464 discloses a sanitary napkin
having water absorbent polymer which may comprise a
mixture of two types of absorbent gelling material from
the group consisting of starch, ~-hydroxyethylacrylate,
acrylonitrile, acrylic acid and acrylamide,
carboxymethylcellulose, hydrophilic copolymers o~
acrylates, copolymers of a vinyl ester and an
ethylenically unsaturated carboxylic acid and their
saponification products, polyvinyl alcohol, and its
derivatives.
US patent no 4,902,544 discloses a flexible tubular
casing comprising a crosslinked hydrocolloid and
naturally occurring cellulose such as saw dust, crushed
corncobs, cottonlinters, wood pulp and the like, ion-
~ch~nge resins or clay minerals.
GB-B-1 544 002 discloses a mixture of a salt of an
acrylic acid polymer and either guar gum, alginates or
xanthan gum to provide an absorbent material with good
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21
absorbent properties, irrespective of the presence of an
electrolyte in the liquid to be absorbed. P~lyvalent
ions may be incorporated in the absorbent composite.
.
US patent no 4,411,660 discloses in an absorbent product
two layers of absorbent material of different types,
such that the upper layer gels slower than the first
layer.
European Patent Specification EP-B-0 401 189 discloses
that favourable properties of absorbent products can be
achieved by using two different types of absorbent
gelling material in separate layers, rather than as a
mixture of the two absorbent gelling materials in a
single layer.
The hydrogel-forming absorbent polymers useful in the
present invention include a variety of substantially
water-insoluble, but water-swellable polymers capable of
absorbing large ~uantities of liquids. Such polymers
materials are also commonly referred to as
"hydrocolloids", or ~'superabsorbent" materials. These
hydrogel-forming absorbent polymers preferably have a
multiplicity of anionic, functional groups, such as
sulfonic acid, and more typically carboxy, groups.
Examples of polymers suitable for use herein include
those which are prepared from polymerizable,
unsaturated, acid-cont~;n;ng monomers. Thus, such
monomers include the olefinically unsaturated acids and
anhydrides that contain at least one carbon to carbon
olefinic double bond. More specifically, these monomers
can be selected from olefinically unsaturated carboxylic
acids and acid anhydrides, olefinically unsaturated
sulfonic acids, and mixtures thereof.
Some non-acid monomers can also be included, usually
in minor amounts, in preparing the hydrogel-forming
absorbent polymers herein. Such non-acid monomers can
-
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W097l20099 PCT~S96/19171
22
include, ~or example, the water-soluble or water-
dispersible esters of the acid-containing monomers, as
well as monomers that contain no carboxylic or sulfonic
acid group~ at all. Optional non-acid monomers can thus
include monomers cont~'n;ng the following types o~
functional groups: carboxylic acid or sulfonic acid
esters, hydroxyl groups, amide-groups, amino groups,
nitrile groups and guaternary ammonium salt groups.
These non-acid monomers are well-known materials and are
described in greater detail, for example, in U.S. Patent
4,076,663 IMasuda et al), issued February 28, 1978, and
in U.S. Patent 4,062,817 (Westerman), issued December
13, 1977, both of which are incorporated by re~erence.
Olefinically unsaturated carboxylic acid and
carboxylic acid anhydride monomers include the acrylic
acids typified by acrylic acid itself, methacrylic acid,
ethacrylic acid, -chloroacrylic acid, a-cyanoacrylic
acid, -methylacrylic acid (crotonic acid), -
phenylacrylic acid, -acryloxypropionic acid, sorbic
acid, -chlorosorbic acid, angelic acid, c; nn~; C acid,
p-chloroc; nn~m; C acid, -sterylacrylic acid, itaconic
acid, citroconic acid, mesaconic acid, glutaconic acid,
aconitic acid, maleic acid, fumaric acid,
tricarboxyethylene and maleic acid anhydride.
Olefinically unsaturated sul~onic acid monomers
include aliphatic or aromatic vinyl sulfonic acids such
as vinylsulfonic acid, alkyl sulfonic acid, vinyl
toluene sulfonic acid and styrene sulfonic acid; acrylic
and methacrylic sulfonic acid such as sulfoethyl
acrylate, sulfoethyl methacrylate, sulfopropyl acrylate,
sulfopropyl methacrylate, 2-hydroxy-3-methacryloxypropyl
sul~onic acid and 2-acrylamide-2-methylpropane sulfonic
acid.
Preferred hydrogel-forming absorbent polymers ~or
- use in the present invention contain carboxy groups.
These polymers include hydrolyzed starch-acrylonitrile
graft copolymers, partially neutralized starch-
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23
acrylonitrile graft copolymers, starch-acrylic acid
graft copolymers, partially neutralized starch-acrylic
acid graft copolymers, saponified vinyl acetate-acrylic
ester copolymers, hydrolyzed acrylonitrile or acrylamide
copolymers, slightly network crosslinked polymers of any
of the foregoing copolymers, partially neutralized
polyacrylic acid, and slightly network crosslinked
polymers of partially neutralized polyacrylic acid.
These polymers can be used either solely or in the form
of a mixture of two or more different polymers.
Examples of these polymer materials are disclosed in
U.S. Patent 3,661,875, U. S . Patent 4,076,663, U. S .
Patent 4,093,776, U. S . Patent 4,666,983, and U.S. Patent
4,734,478.
Most preferred polymer materials for use in making
hydrogel-forming particles are slightly network
crosslinked polymers of partially neutralized
polyacrylic acids and starch derivatives thereof. Most
pre~erably, the hydrogel-forming particles comprise from
about 50 to about 95~, preferably about 75~,
neutralized, slightly network crosslinked, polyacrylic
acid (i.e. poly (sodium acrylate/acrylic acid)).
As described above, the hydrogel-forming absorbent
polymers are preferably slightly network crosslinked.
Network crosslinking serves to render the polymer
substantially water-insoluble and, in part, determines
the absorptive capacity and extractable polymer content
characteristics of the precursor particles and the
resultant macrostructures. Processes for network
crosslinking the polymers and typical network
crosslinking agents are described in greater detail in
the hereinbefore-referenced U.S. Patent 4,076,663, and
in DE-A-4020780 (Dahmen).
Although the hydrogel-forming absorbent polymers can
have a size varying over a wide range, specific particle
size distributions and sizes are preferred. For
purposes of the present invention, particle size is
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24
defined for hydrogel-~orming absorbent polymers that do
not have a large greatest dimension/smallest dimension
ratio such as fibers (e.g., granules, flakes, or
pulverulents) as the ~;m~n~ion of a precursor particle
that is determined by sieve size analysis. Thus, for
example, a hydrogel-forming absorbent polymer particle
that is retained on a standard #30 sieve with 600 ~icron
openings is considered to have a particle size greater
than 600 microns, a hydrogel-forming absorbent polymer
particle that passes through the #30 sieve with 600
micron openings and is retained on a st~n~A~d #35 sieve
with 500 micron openings is considered to have a
particle size between 500 and 600 microns, and a
hydrogel-forming absorbent polymer particle that passes
through a #35 sieve with 500 micron openings is
considered to have a particle size less than 500
microns. For preferred hydrogel-forming absorbent
polymers useful in the present invention, the particles
will generally range in size from about l micron to
about 2000 microns, more pre~erably from about 20
microns to about lO00 microns.
Further, for purposes of this invention, the mas~
median particle size of the hydrogel-forming absorbent
polymers is important in determining the characteristics
and properties of the resultant particles. The mass
m~ n particle size of a given sample of hydrogel-
forming absorbent polymer particles is defined as the
particle size that divides a sample in half on a mass
basis. Instead of the mass median particle size, the
mass average particle size could be specified as a
measure for the ~;m~n~ion of the particles, wherein the
mass average particle size is the average particle size
of the sample on a mass basis. A method for determ; n; ng
the mass median particle size of a sample is described
hereinafter in the Test Methods section. The mass
median particle size of the hydrogel-forming absorbent
polymer particles will generally be from about 20
-
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microns to about 1500 microns, more preferably from
about 50 microns to about 1000 microns. For preferred
hydrogel-forming absorbent polymers useful in the
present invention, the particles have a mass median
particle size less than about 1000 microns, more
preferably less than about 600 microns, most preferably
less than about 500 microns.
The particle size of materials having a large
greatest dimension/smallest ~;m~n~ion such as fibers is
typically defined by their largest ~;m~nqion. For
example, if hydrogel-forming absorbent polymeric fibers
are used in the present invention, the length o~ the
fibers iB used to define the "particle size." (The
denier and/or the diameter of the fibers can also be
specified.) For exemplary embodiments of hydrogel-
forming absorbent polymers useful in the present
invention, the fibers have a length greater than about 5
mm, preferably between about 10 mm and about 100 mm,
more preferably between about 10 mm and about 50 mm.
Pre~erred hydrogel-forming absorbent polymer
particles of the present invention are those which
exhibit a high absorptive capacity or Teabag Centrifuge
Capacity value. Absorptive capacity, or Teabag
Centrifuge Capacity, re~ers to the capacity of a given
polymer to absorb liquids with which it comes into
contact under free-swelling conditions. TCC can vary
significantly with the nature o~ the liquid being
absorbed and with the mAnn~ in which the liquid
contacts the polymer material. For purposes of the
present invention, Teabag Centrifuge Capacity iq defined
in terms of the amount of 0.9 ~ saline solution absorbed
by any given polymer in terms of grams o~ saline
solution per gram of polymer material in a Tea bag
Centrifuge Capacity test procedure hereinafter defined
in the Test Methods section. Preferred hydrogel-forming
absorbent polymer particles of the present invention are
those which have Teabag Centrifuge Capacity values of at
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26
least about 20 grams, more preferably at least about 25
grams, of saline solution per gram o~ polymer material.
Typically, the hydrogel-forming absorbent polymer
particles use~ul herein have Teabag Centrifuge Capacity
values of from about 20 grams to about 70 grams o~
saline solution per gram of polymer. Mixtures of
hydrogel-forming absorbent polymers particles having
this relatively high absorptive capacity characteristic
are especially useful in the present invention since the
resultant absorbent member formed from such particles
can, by definition, hold desirably high amounts of
fluid.
Other Absorbent structures for current absorbent pads
can use of particulate Superabsorbent materials as
described above, but forming a coherent structure ~rom
these. Such "Porous, absorbent polymeric macrostructures
and methods of making same" are described in US patent
5,124,188 /WO 91/15362 assigned to Roe et al.
Alternatively, Superab~orbent highly absorbent foam
materials suitable for use in current invention are
described in US patent 5.328.935 and 5.338.766, assigned
to Trokhan and Phan.
Alternatively, ~Absorbent Foam Materials for aqueous
body fluids and absorbent articles cont~;n;ng such
materials" as described in US patent 5.268.224 assigned
to DesMarais et al. are suitable for current
application, too
Optionally, the absorbent structure may include some
specialized materials developed to absorb oils and
greases. One example o~ this is T-151 oil sorbent, a 3M
product, ~Minnesota Mining and Manufacturing, ST. Paul,
~;~ne~ota3~ T-151 absorbent and s;m;lA~ absorbent
materials are typically non-woven polymeric fiber webs
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and include certain polyolefin polymers such as
polypropylene, polyethylene, poly-4-methylpentene,
arylene, styrene, and copolymers thereof, as well as
polyesters, polyamides, and polycarbonates.
Met~ods
Teabaq Centrifuge Ca~acity Test
The Teabag Centrifuge Capacity test measures the Teabag
Centri~uge Capacity values, which are a measure of the
retention of liquids in the gelling material at
hydrostatic pressure
The superabsorbent material is placed within a
"teabag", immersed in a 0.9 % by weight sodium chloride
solution for 20 minutes, and then centrifuged for 3
minutes. The ratio of the retained li~uid weight to the
initial weight o~ the dry superabsorbent material is the
absorptive capacity of the superabsorbent material.
21 of O.g~ by weight sodium chloride in distilled
water is poured into a tray having ~;m~n~ions 24cm x 30
cm x 5cm. The liquid ~illing height should be about
3cm.
The teabag pouch has ~;m~n~ions 6.5cm x 6.5cm and
is available ~rom a company called Tee~anne in
Dusseldorf, Germany. The pouch is heat sealable with a
g~n~d kitchen plastic bag sealing device (e.g.
VACUPACK2 PLUS from Krups, Germany).
The teabag i8 opened by carefully cutting it
partially, and is then weighed. A 0.200g +/- 0.005g
sample of the superabsorbent material is placed in the
teabag. The teabag is then closed with a heat sealer.
This is called the sample teabag.
An empty teabag is sealed and used as a blank.
Each teabag is then held horizontally, and the
sample teabag i6 shaken so as to distribute the
superabsorbent material evenly throughout the bag. The
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sample teabag and the blank teabag are then laid on the
surface o~ the saline solution, and submerged for about
~econds using a spatular to allow complete wetting
(the teabags will ~10at on the surface o~ the saline
solution but are completely wetted). The timer is
started immediately.
After 20 minutes soaking time the sample teabag and
the blank teabag are removed ~rom the saline solution,
and placed in a Bauknecht WS130, Bosch 772 NZK096 or
equivalent centrifuge ~230 mm diameter), so that each
bag sticks to the outer wall of the centrifuge basket.
The centrifuge lid is closed, the centrifuge is started,
and the speed increased quickly to 1,40Orpm. Once the
centrifuge has been stabilised at 1,400rpm the timer is
started. After 3 minutes, the centrifuge is 6topped.
The sample teabag and the blank teabag are removed
and weighed separately.
The Teabag Centrifuge Capacity (TCC) for the sample
of superabsorbent hydrogel-~orming material ' i6
calculated as follows:
TCC = [(sample teabag weight after
centrifuging) - (blank teabag weight after
centrifuging) - (dry superabsorbent hydrogel-
forming material weight)J . (dry
superabsorbent material weight).
Mass median particle size determination
The particle size distribution of superabsorbent
material is determined by placing a known weight of a
sample in a Retsch mechanical ~ieving device, and
shaking for a specified period of time under defined
conditions. Sample sections that are retained on each
sieve and the bottom pan are weighed and reported as
percentages of the original sample weight.
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29
lOOg +/- 0.5g of dry superabsorbent polymeric
material is weighed into a sample 8up which is then
closed by a lid.
Four sieves are nested from bottom to top as
follows: stainless steel bottom pan, No. 325, No. 100,
No. 50 and No. 20; these being numbers of the U.S. sieve
series (ASTM-E-11-61~. The sample is transferred to the
upper most of the series of sieves, and the powder is
distributed evenly around the screen. A stainless steel
cover is places on the No. 20 sieve.
The nested sieves are placed in position on a
Retsch testing sieve shaker Vibotronic Type VBl with
timer. It is ensured that the Retsch lid fits a ~
tightly as possible against the top of the shaker. The
timer is set for 10 minutes, and started to begin the
test. When the shaker has stopped, the nest of sieves i8
removed from the shaker.
~ ach of the sieve fractions ret~; n~ by the sieve
is then weighed, for example by different measurements,
to the nearest O.Og.
I-t is important to work ~uickly in this test to
avoid moisture pickup by the superabsorbent material.
The mass median particle size of a given sample of
hydrogel-forming absorbent polymer particles is defined
as the particle size that divides the sample in half on
a mass basis, i.e., one-half of the sample by weight
will have a particle size less than the ma~s median size
and one-half of the sample will have a particle size
greater than the mass median size. A standard particle-
size plotting method (wherein the cumulative weight
percent of the particle sample retained on or passed
through a given sieve size opening is plotted versus
sieve size opening on probability paper) is typically
- used to determine mass median particle size when the 50
mass value does not correspond to the size opening of a
U.S.A. Standard Testing Sieve. These methods for
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wo s7nooss
determining particle sizes o~ the hydrogel-forming
absorbent polymer particles are ~urther described in
U.S. Patent 5,061,259 (Goldman et. al), issued October
29, 1991, which is incorporated by re~erence.
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31
Examples
In the examples, all compositions are expressed as ~ by
weight (unless otherwise stated).
Examples l to 78
CompositionsEx. l Ex. 2 Ex. 3 Ex. 4
Limonene 18.3 36 23.5
Shellsol ~ 23.5
Monoethanol Amine 3 5.8 5.8
HLAS l6.5
Butyl carbitol lo 18 ll.7 ll.7
Oleic Acid 9 6 6
Alkyl sulphate C8AS lO 7.8 7.8
Water Balance Balance Balance Balance
CompositionsEx. 5 Ex. 6 Ex. 7 Ex. 8
Shellsol ~ 20 60 25
Ethylene glycol lS 7
monobutyl ether
Trichloroethylene 5
Sodium lauryl 15 5
sulphate
Alkyl sulphate C8AS 4
Dehydol C8E04 ~ 3 5
- Dobanol 25C3 ~ 3 lO
Water Balance Balance Balance Balance
In Table l, Shellsol ~ is a mixture of C8-Cll
isoparaffins with 5~ aliphatic C7 ester. Dehydol ~ is a
fatty alcohol polyglycol ether octyl 4E0, supplied by
- Henkel. Dobanol is a ethoxylated primary alcohol 3E0
supplied by Shell.
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A set of polycotton swatches (50mm square) were soiled
with make-up, chocolate sauce and tomato sauce. The
stain was left to age for a day, in the dark, at normal
room temperature ~c.a. 20~C, 60~RH). Each soiled swatch
was cleaned by the following method:
1. The stained area was placed directly upon a strip of
absorbent paper (the paper used was the absorbent core
of a diaper).
2. 1 ml of the composition of Example 1 was dripped on
to the stained area.
3. The stained area was brushed with a conventional
electrical toothbrush for 10 seconds (the toothbrush
used, a Braun~ dental d3, was one normally intended for
daily oral care).
4. The steps 2. and 3. were repeated one more time.
5. 1 ml of distilled water was dripped on to the s~Aine~
area, and pressure and heat were applied using an iron
set at a temperature of 120~C for 10 seconds. A typical
ironing pressure, a~ normally used for removing wrinkles
in ~abrics, was used.
6. Step 5. was repeated with a further 2ml of distilled
water.
7. The swatch was dried and smoothed.
The method of cleaning was repeated on stained swatches
using the compositions of Examples 2 to 78 in place of
the composition of Example 1.
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Ingredient Ex. 9 Ex. lO Ex. ll Ex. 12 Ex. 13
Perchlorethylene 99.693 95.8 95 84.25 59.23
MEA-LAS1 0.3 40
Sodium Dodecyl sulphate 0.03 0.0047
Sodium Dioctyl 3.2
sul~osuccinate
Nonyl Phenol ethoxylate 4.97 0.7455
8 EO
Isopropanol 0.005
Ethylene glycol 0.5
monobutyl ether
Brightener 0.0002 0.02
Water RA1 AnC R~1 ~nCe
e
lMonoethanol amine salt of linear alkyl benzene
sulphonic acid
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34
Ingredient Ex. 14 Ex. 15 Ex. Ex. Ex. 18
16 17
Perchlorethylene 40 20
Stoddard solvent 95
Ethylene glycol 5 5 25
monobutyl ether
Octyl phenol 50 lO
ethoxylate EO 7-8
Nonyl phenol 5
ethoxylate EO 6
Isopropyl 5 50
dodecylbenzene
Sl~l ph~n~te
Coconut diethanolamide
Isopropyl alcohol 5 25
Mineral spirits 69
Mineral Oil 24
Optical bright~n~r
Per~ume O.l O.l
Water R~1 AnCe RA1 ;~n~
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Ingredient Ex. l9
Butoxy propoxy propanol 7
l,2 octanediol 0 5
Pemulen TR-l (emulsifier from Goodrich) 0.15
KOH 0.08
Perfume 0 75
Water Balance
pH=6.5
Ingredient Ex. 20 Ex. 2l
Shellsol SS 33 lO
Cl2-Cl5 alkyl ethoxylate E03 16 6
Cl2-Cl5 alkyl ethoxylate E09 16 6
Isopropyl alcohol 13 13
Oleic fatty acid 6 2
Triethano~ ~m; ne 3 l.O5
Sodium xylene sulfonate 2.4
Water Balance Balance
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36
Ingredient Ex. 22Ex. 23 Ex. 24 Ex. 25 Ex. 26
Sodium dodecyl sulphate 15
Sodium Hexadecyl 15
sulphate
Nonyl phenol ethoxylate 40
EO 9
Octyl phenol ethoxylate 40
EO 6
Octyl phenol ethoxylate 15
EO 3
Pentanol 55 50 40 40 55
Water BalanceR~7 Ance,RA1 Ant~e RA1 Anr~e RA1 AnC~e
Ingredient EX. 27 Ex. 28 Ex. 29
Shellsol SS 25
High flash ~phtA* 50 l0
Xerosene 30
Sodium dodecyl sulphate 16
Ammonium t7~ AnoYy-polyethlenoxy 36 40
ethyl sufate
mono-butyl ether of ethylene glycol20 2.5
Perfume 0.2 0.2 0.2
WaterRA1 Ant~e RA1 ~nce RA7 AnCe
* Hi-flash Naphta, a mixture of saturated hydrocarbon
from Amsco Company
Ingredient Ex. 30 Ex. 31 Ex. 32
Cyclo~Y~nol 7 6 5
isopropanol 2 2.5
toluene 20 20 15
1,2 dichloroethane 18 20 6
-
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37
1,1,1 trichloroethane 45 40 65
Water Balance Balance Balance
Ingredient Ex. 33 Ex. 34 Ex. 35 Ex. 36
Citric acid 5 5 16.1 3.57
NaOH 3.1 3.1 10 2.21
Sodium dioctyl 6 6 1.6 4.28
sulphosuccinate
Nonylnonoxylnol-7 phosphate 2 1.6 1.42
Isopar Kl 20 20 16 42.85
Sorbitan ester (monooleate) 0.6 0.48 0.42
Polyethylene sorbitan ester 1.4 1.12
(monooleate)
T.;mr n~ne 1 1 1 0.71
Water R~l ~nc R~l ~n~ R~1 ~nc R~l ~n~
e e e e
C10-C12 isoparaffinic hydrocarbon, from Rxxon
Ingredient Ex. 37 Ex. 38 Ex. 39 Ex. 40 Ex. 41
LAS 0.32
Coconut alkyl sulphate 5.28
C12-C14 alkyl ethoxylate 6.32
EO7
C13-C15 alkyl ethoxylate 7.84 7.47 35.88 23
EO7
Fatty acid ~ 6.2 0.16
Citric acid 1.03
- IPA
Paraffin C9-C12 40 47.24
Water R~1 ~nce Balance RA 1 ~nr~ R~ l~n~e Balance
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38
Ingredient Ex. 42 Ex. 43Ex. 44Ex. 45 Ex. 46
Cl3-Cl5 alkyl ethoxylate 12
E03
Cl3-Cl5 alkyl ethoxylate 3 5
E07
C8 alkyl sulphate lO 14 14
C8 alkyl sulphonate 9 20
C7-C9 alkyl ethoxylate 5
E06
C8 alkyl ethoxylate E04
C8-ClO alkyl ethoxylate 20 9
E05
C8-ClO alkyl ethoxylate 20 20
E06
Cl2-Cl3 alkyl ethoxylate 8 8
E03
Cl3-Cl5 alkyl ethoxylate 6 5
EO30
Citric acid 6 3 12 12
Monoe~hAnolamine
Triethanolamine 3
Diethylene Glycol 6 30
:- -hntyl ether
Potassiu~ ~ ~h~n~ te 4 4
Palm Kernel Fatty acid l.2
2-Butyl octanol
Water and minors R~l ~n~e Balance R~l ~n~e R~l ~n~e R~l ~nce
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Ingredient 3x. 47 Ex. 48 Ex. 49 Ex. 50
Cl0 alkyl sulphate l.2
Cl2-Cl4 alkyl sulphate 0.5
Cl3-Cl5 EO 30 0.75
Cl2-Cl3 EO 6.5 o,g
Cl2-Cl3 EO 3
Cl4-Cl5 EO 7
C9-Cll EO l0 l.6 2.6
Phosphonate 0.18 0.3
PVP 0.2
H~lo~ Peroxide 6.8 7 6
Ghlorine 5
Sulphuric Acid 0.013 0.013
NaOH l.4
~ Na2CO3 1.25
Na2SiO3 0.5
Iso~ol 12 0.49
2 Hexyl ~n~l 0 3
MA/A~.l 1
Isopropyl alcohol 5
Optical bright~n~r 0.04 0.06
Dye 0.0006 0.0006
Pe~LI 0.25
Water R~l ~nr~e R;~ n-~e R;~l ~n~e Rs~7 ;~nce
pH 4
lMA/AA = Acrylic maleic based copolymers, MW of 70000,
the ratio o~ acrylate to maleate segments vary from 10:1
to 2:1. Sokalan CP5 from BASF
Ingredient Ex. 5I Ex. s2 Ex. 53
Cl2 dimethyl amine oxide . l l l.8
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C8 alkyl sulphate 4 8
polyacrylate (polygel DK), 1.5
thickener
C12 fatty acid (thickener) 0.8
Sodium benzoate 0.5
NaOE up to pH 12-13 12-13 12-13
Water Balance Balance Balance
Ingredient Ex. 54 Ex. 55 Ex. 56
C14-C17 alkyl sulphonate 27 20 35
C12-C15 alkyl ether sulphate (EO 3) 4 5 8.5
C9-C11 alkyl ethoxylate EO 8 5.4 11
C8-C18 alkyl sulphate 4 }.85
Water R~l~nc Balanc Balanc
e e e
Ingredient Ex. 57 Ex. 58 Ex. 59
3-(N-dodecyl-N-N-dimethyl)-2~ 2 10
hydroxy-propane-l sul~onate
C9-Cll alkyl ethoxylate EO 2.5 1.1 5
C9-C11 alkyl ethoxylate EO 6 2.9 15
C9-C11 alkyl ethoxylate EO 8 3
Butoxy Propoxy Propanol 5 25
Oxydisuccinic acid 10 10
Sodium cumene sulfonate 4.2 20
Maleic acid 20
Water RA1 ~nC Ba~anc RA1 AnC
e e e
pH,1
Ingredient Ex. 60 Ex. 61
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41
Cl2-Cl3 EO 6.5 2.5 25
Dipropylene Glycol Monbutyl Ether 3 30
Monoethanolamine 0.5 5
Sodium Dodecyl~enzene sulfonate 0.5 3
Coconut Fatty acid 0.03 3
Water Balance Balance
Ingredi~nt Ex. 62 Ex. 63
Sodium Lauryl Sulphate 12.6 12.6
Isopropanol 3 16.5
Propylene Glycol Methyl Ether 2
Amyl Acetate 0.25 0.3
Monopotassium Phosphate O.9 0.9
Methylene chloride 5
Sodium EDTA 0.05
Water Balance Balance
IngredientEx. 64 Ex. 65 Ex. Ex. Ex.
66 67 68
~ne 67
Decane 25 32.5
Dodecane 2.5 lO
Cl2-Cls alkyl ethoxylate EO 9 20
Cl4-Cl5 alkyl ethoxylate EO 8 20
Cl2-Cl3 alkyl ethoxylate EO 35
5.5
Cl6-Cl8 alkyl ethoxylate EO 9 12.5 40
Ethylene glycol 55 13 81 47.5
Glycerol 4 2.5
PEG 300 32.5
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42
Ingredient Ex. 69 Ex. 70 Ex. 71
Sodium 2, 6, 9 trioxa- 12 6 . 4
hexyleicosyl sulphate
Sodium dodecylbenzene ll.7 ll.7
sulphonoate
Butanol 4.l 7.3 7.3
NaCl 4.4 2 . 9 2 . 9
Kerosene 8.5
isoparaf~inic hydrocarbon 6.2
pine oil 8.5
Water Balance Balance Balance
. .
CA 02238497 l998-05-25
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43
Ingredient Ex. 72 Ex. 73
Cl4-Cl5 alkyl ethoxylate EO 2.25 sulphate 18 9
Cl2-Cl3 alkyl ethoxylate EO 6.5 2
Cl2-Cl4 N-methylglucamide 6 3
Citric acid 4 2
Cl2-Cl4 fatty acid 2
Ethanol 4 2
l,2 prop~n~Ai ol 7 3.5
Monoethnol ~mi n~ 1 0 . 5
optical brightener 0.l
Soil release polymerl 0.3 0.15
Boric acid 2.5 l.25
Protease l.4 0.7
Lipase 0.18 o.og
Polyethylene glycol tMW 4000) 1.5 0.75
Polyaspartic acid (MW l0,000) 0.5 0.25
NaOH up to up to
pH=l0 pH=l0
Water R~l Anc Balanc
e e
lEthoxylated copolymer o~ polyethylene-polypropylene
terephtalate polysul~onic acid
Ingredient Ex. 74 Ex. 75 Ex. 76 Ex. 77 Ex. 78
Alkyl sulphate 16.75 1.6 4.48
Alkyl ethoxy sulphate 2 0.2 13.58
LAS 7,57
Cl2-Cl5 alkyl 5.5 0.55 l0 5.61
ethoxylate EO7
Cl2-Cl8 N- 5.5 0.55
methylglucamide
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44
Citric acid 1 0.1 16.8 0.63 1.56
Fatty acid 10.5 1.05 2.9 13.67
Carbonate 1.2
PropAn~;ol 11.5 1.15 6.97
Ethanol 1.4 0.14 5.08
PEG 200-300 35
Glycerine 4,54
MEA 7.8 0.78
NaOH 1.2 0.12
Phosphonate 1 0.01 0.5 0.21
Zeolite 28.01
Ethoxylated 0.25 0.025
tetraethylenp~ntAmine
Soil release polymer 0.15 0.015
CMC
Protease 0.5 0.05 0.5
Lipolase 0.07 0.007
Amylase 0.15 0.015 0.18
Cellula~e 0.03 0.003
CaCl2 0.02 0.002
Boric acid 3-5 0~35
Silicone oil 0.2
Dispersant 0.02
Silica 0.013
Propyl 0.02
trime~hoxysilane
Optical brightener 0.15 0.0147
Dye 0.001
PB1 13
PB4 2
Water R;~1 ~qnCe RA1 :~ncl9 Balance R5~ nCe R~1 Anre
pH=8.5
Example 79
CA 02238497 1998-0~-2~
WO 97/20099 PCT/US96/19171
A set of wool, polycotton and cotton swatches (50mm
square) were soiled with honey, salad dressing and
tomato sauce. The stain was left to age for a day, in
the dark, at normal room temperature (c.a. 20~C, 60%R~)
Each soiled swatch was cleaned by the ~ollowing method.
1. The stained area was placed directly upon a strip of
absorbent paper (the paper used was the absorbent core
o~ a diaper).
2. 1 ml of the composition of Example 74 was applied on
to the stained area by means of an applicator of design
indicated in fig 1. This applicator comprised a bottle,
a cap with a pad of polyurethane ~oam attached to it.
The cap has a small central opening through which the
liquid can pass.
A~ter application of the detergent composition, the
stain was massaged with the outer surface of the pad to
loosen it.
3. 1 ml of distilled water was sprayed on the stained
area, and pressure and heat were applied using an iron
set at a temperature o~ 80~C ~or lS seconds. A typical
ironing pressure, as normally used ~or removing wrinkles
in fabrics, was used.
4. Step 3. was repeated with a further 2ml of distilled
water.
5. The swatch was then dried and smoothed.
The method o~ cl~n; ng was repeated on stained swatches
using the applicator of ~igures 2 to 7 in place of the
applicator o~ figure 1.
CA 02238497 1998-0~-2~
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46
The method of cleaning was repeated on polycotton
swatches stained with dirty motor oil using the
applicator of ~igure 4 in place of the applicator of
~igure 1 and the cleaning composition of example 5 in
place of the composition of example 74.
Examples 80 to 93
A set of cotton swatches (50mm square) were soiled with
lipstick and clay. The stain was left to age ~or a day,
in the dark, at normal room temperature (c.a. 20~C,
60~RH). Each soiled swatch was cleaned ~y the following
method.
1. The stained area was placed directly upon a strip of
absorbent paper (the paper used was the absorbent core
of a diaper).
2. 1 ml o~ the composition of Example 6 was applied on
to the stained area by means o~ an applicator of a
design indicated in fig 7. After application of the
detergent composition, the stain was massaged with the
tip of the cleansing bottle to loosen it.
3. 1 ml of the composition of Example 80 was sprayed on
the stained area, and pressure and heat were applied
using an iron set at a temperature of lQ0~C for 15
seconds. A typical ironing pressure, as normally used
for removing wrinkles in fabrics, was used.
4. Step 3 was repeated with a further 2ml of distilled
water.
5. The swatch was then dried and smoothed.
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47
The method of cleaning was repeated on stained swatches
using the applicator of examples 81 to 93 in place o~
the composition of example 80.
.
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48
Ingredient Ex. 80 Ex. 81
Isopropyl alcohol 18 10
C8 Alkyl phenol ethoxylate E07-8 0.5
C8-C18 alkyl ethoxylate E0 7-8 0.5
Citric acid 3
Amonium Hydroxide 2
Mazawet DF wetting agent (~rom 0.2
Mazer)
Masil 1066c emulsion1 0.2
Coconut amine 0.4
Water Balance Balance
1Specialty silicone ~luid from Mazer
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49
Ingredient Ex. 82 Ex. 83 Ex. 84 Ex. 85 Ex. 86
Isopropyl alcohol 15 5 50 35 8
methanol 47
Diethylene glycol 7,5
m~no,m~thylether
Ethylene glycol n- l
butyl ether
C12-15 alkyl 0.1
ethoxylate EO 6.5
Nonyl phenol 0,5
ethoxylate EO 9
Ammon; um . 0.15
ethoxysulphate
(Nedodol 25-3a)
Triton Qs-3ol 0.5
Caprylo~mrho~;~cetate 0.3
Ammonium hydroxide 0.15
Water RA1 ~nC Balanc R~1 ~nC R~1 ~nC R~1 ~nC
e e e e e
1Phosphate ester
2Wetting agent
Ingredient Ex. 87 Ex. 88 Ex. 89 Ex. 90
Octyl phenol ethoxylate EO5 20 5
Octyl phenol ethoxylate E9- 2.5
Octyl phenol ethoxylate 5 5
EO12-13
C12-C14 alkyl sulphate 10
Triton H661 7.5 7.5 2
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Dipropylene glycol methyl 4 4 6
ether
Phosphonate 2
Citric acid 15 3
Pine oil 0.25
Water Balanc R~l AnC R~l ~nc Balanc
e e e e
Potassium phosphate ester from Rohm and Haas
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51
Ingredient Ex. 9l Ex. 92 Ex. 93
ClO alkyl sulphate l.2
Cl2-Cl4 alkyl sulphate 0,5
Cl3-Cl5 EO 3Q 0.75
Cl2-Cl3 EO 6.5 0.9
Cl2-Cl3 EO 3
Cl4-Cl5 EO 7
C9-Cll EO lO 1.6 2.6
Phosphonate 0.18 0.3
PVP 0.2
Isofol 12 0.49
2 Hexyl decanol 0.3
MA/AAl
Isopropyl alcohol 5
Water and minors Balance Balance Balance
lMA/AA = Acrylic maleic based copolymers, MW o~ 70000,
the ratio of acrylate to maleate segments vary ~rom lO:l
to 2:l. Sokalan CP5 ~rom BASF
CA 02238497 1998-0~-2~
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52
Example 94
A set o~ silk and wool swatches (50mm s~uare~ were
soiled with make-up and tomato sauce. The stain was le~t
to age for a day, in the dark, at normal room
temperature (c.a. 20~C, 60~H). Each soiled swatch was
cleaned by the following method.
1. The stained area was placed directly upon a strip of
absorbent paper (the paper used was the absorbent core
of a diaper).
2. A non-linting sheet is prepared using a non-woven,
two-ply fabric stock comprising polyester fibres,
calliper 0.25 to 0.34 mm, basis weight 84g/m2. The
fabric is cut into a 1OOcm2 sheet, lOcm on a side. 10 g
of the composition of example 19 are applied by dipping
the composition onto the substrate, followed by
squeezing with a roller.
This sheet is placed on top of the soiled area. The area
o~ overlap between the paper and the 80il i8 brushed
with a toothbrush for lO seconds. A typical pre~sure as
normally used to clean teeth was used. After brushing
the paper i~ discarded.
3. 1 ml of water was sprayed on the stained area, and
pressure and heat were applied using an iron set at a
temperature of 40~C for 15 seconds. A typical ironing
pressure, as normally used for removing wrinkles in
fabrics, was used.
4. Step 3. was repeated with a further 2ml of water.
5. The swatch was then dried and smoothed.
_
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53
In an alternate mode, the soiled area was pretreated by
pressing or rubbing with a sheet prepared according to
the instructions given here above. After pretreatment
with the cleaning sheet, the stained area was cleaned
with the iron in the manner described in steps 3, 4 and
herein. In this mode of application, during the
rubbing stage, the stain is pushed through the fabric
onto the underlying absorbent paper.
Example 95
A set of silk and wool swatches (50mm square) were
soiled with make-up and tomato sauce. The stain was le~t
to age for a day, in the dark, at normal room
temperature ~c.a. 20~C, 60~RH). Each soiled swatch was
cleaned by the following method.
1. The stained area was placed directly upon a strip of
absorbent paper (the paper used was a sheet of kitchen
paper towel).
2. A non-linting sheet is prepared using a non-woven,
two-ply fabric stock comprising polyester fibres,
calliper 0.25 to 0.34 mm, basis weight 84g/m2. The
fabric is cut into a lOOcm2 sheet, lOcm on a side. 10 g
of the composition of example 19 are applied by dipping
the composition onto the substrate, followed by
squeezing with a roller.
This sheet is placed on top of the soiled area. The
soiled area sandwiched between the paper towel and the
cleaning sheet was inserted between the clips of the
device of a design given in fig 8. The body of the
device is made of plastic, a pad of polyurethane foam is
attached on each side o~ the clip.
CA 02238497 l998-0~-2~
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54
A~ter insertion o~ the sheet/~oil/absorbent paper
assembly within the clips. The gap between the sponges
is closed by applying pressure to the connecting means
as indicated by the arrow, thereby causing the sponges
to contact with the cleaning sheet and the paper towel.
The tool thus designed allows pushing of the stain
through the fabric onto the underlying absorbent paper
without any damage to the fabric.
3. 1 ml o~ water was sprayed on the stained area, and
pressure and heat were applied using an iron set at a
temperature of 40~C for 15 seconds. A typical ironing
pressure, as normally used for removing wrinkles in
fabrics, was used.
4. Step 3. was repeated with a further 2ml of water.
5. The swatch was then dried and smoothed.
The method o~ cleaning was repeated on stained swatches
using the spot cleaning device of Fig. 9 in place of the
spot cleaning device o~ Fig. 8.
Example 96
A set o~ polycotton swatches (50mm square) were soiled
with make-up, chocolate sauce and tomato sauce. The
- stain was left to age for a day, in the dark, at normal
room temperature (c.a. 20~C, 60~RH). Each soiled swatch
was cleaned by the ~ollowing method:
1. The stained area was placed directly upon a strip of
absorbent paper (the paper used was the absorbent core
of a diaper).
CA 02238497 1998-0~-2~
W097/20099 PCT~S96/19171 -
2. 1 ml of the composition o~ Example 1 was dripped on
to the stained area.
3. The stained area was brushed with a dual-temperature
cordless massager ~rom Ultratherm~, model TM2000.
4. The step~ 2. and 3. were repeated one more time.
5. 1 ml of distilled water was dripped on to the stained
area, and pressure and heat were applied using an iron
set at a temperature o~ 120~C for 10 seconds. A typical
ironing pressure, as normally used for removing wrinkles
in ~abrics, was used.
6. Step 5. was repeated with a further 2ml of distilled
water.
7. The swatch was dried and smoothed.
The method o~ cleaning was repeated on stained swatche~
using the compositions o~ Examples 2 to 5, and 19 in
place o~ the composition o~ Example 1.
Example 97
A set of polycotton swatches (50mm square) were soiled
with make-up, chocolate sauce and tomato sauce. The
stain was le~t to age for a day, in the dark, at normal
room temperature (c.a. 20~C, 60~RH). ~ach soiled swatch
was cleaned by the ~ollowing method:
CA 02238497 1998-0~-2~
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56
1. The stained area was placed directly upon a strip of
absorbent paper (the paper used was the ab~orbent core
of a diaper).
2. 1 ml of composition of example 19 was dripped on to
the stained area, and pressure and heat were applied
using an iron (Braun~ Saphir 7000~ set at a temperature
of 100~C for 10 seconds. A typical ironing pressure, as
- normally used for removing wrinkles in fabrics, was
used.
3. The steps 2. and 3. were repeated one more time.
4. 1 ml of distilled water was dripped on to the stained
area, and pressure and heat were applied using an iron
set at a temperature of 120~C for 10 seconds. A typical
ironing pressure, as normally used for removing wrinkles
in fabrics; was used.
5. Step 4. was repeated with a further 2ml of distilled
water.
6. The swatch was dried and smoothed.
The method of cle~n i ng was repeated on stained swatches
using the compositions of Examples 1 to 8, and in place
of the composition of Example 19.
Example 98
A set of silk and wool swatches (50mm s~uare) were
soiled with make-up, chocolate sauce and tomato sauce.
The stain was left to age for a day, in the dark, at
CA 02238497 1998-0~-2~
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57
normal room temperature (c.a. 20~C, 60~RH). Each soiled
swatch was cleaned by the following method:
l. The stained area was placed directly upon a strip of
absor~ent paper (the paper used was the absorbent core
of a diaper).
2. The water tank of a Rowenta Steam Brush DA55 was
filled with the composition of Example l9. The appliance
was placed over the stained area, and l ml of the
detergent composition was steamed on to it.
3. lml of the detergent composition was steamed over the
soiled area. At the same time, the soiled area was
brushed with the cloth brush attached to the head of the
appliance.
4. The steps 2. and 3. were repeated one more time.
5. l ml of distilled water was dripped on to the stained
area, and pressure and heat were applied using an iron
set at a temperature o~ 120~C ~or lO seconds. A typica}
ironing pressure, as normally used for l~l.,oving wrinkles
in ~abrics, was used.
6. Step 5. was repeated with a further 2ml o~ distilled
water.
7. The swatch was dried and smoothed.
In an alternate mode, a~ter the pretreament with the
detergent composition indicated in steps 2, 3 and 4
herein . The water tank was emptied of the detergent
composition and filled with distilled water. lml o~
distilled water was then dripped on to the stained area,
CA 02238497 1998-0~-2~
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58
and pressure and heat were applied using the Rowenta~
Steam Brush DA55.
Example 99
A set of silk and wool swatches (50mm square3 were
soiled with make-up and tomato sauce. The stain was
left to age for a day, in the dark, at normal room
temperature (c.a. 20~C, 60~RH). ~ach soiled swatch was
cleaned by the following method.
1. A non-linting sheet is prepared using a non-woven,
two-ply fabric stock comprising polyester ~ibres,
calliper 0.25 to 0.34 mm, basis weight 84g/m2. The
fabric is cut into a 100 cm2 sheet, 10 cm on a side. 10
g of the composition of example 19 are applied by
dipping the composition onto the substrate, followed by
squeezing with a roller.
A hand-held spot removal device as shown in Figure 10 is
prepared using conventional plastic injection molding
techniques and apparatus. The arms which comprise the
connecting means are fashioned $rom polypropylene, about
(O.48 cm) in thickness. The connecting means may each
have a uniform width of about (1.9 cm), or can be shaped
to provide a more aesthetically pleasing aspect by
gently narrowing the connecting means to a width of
about (1.27cm) at the bend shown in the Figure. The
overall length of the device is about (13.34 cm).
The diameter of the base of each treatment member is
about (3.33 cm) and the diameter of the region of the
looped protrusions extending outwardly from each
- treatment member is about (2.86 cm).
Due to the angle of the bend between the arms o~ the
connecting means and the resiliency of the
polypropylene, the gap between the first and second
CA 02238497 1998-0~-2~
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59
treatment members is about (1.59 cm) when the device is
at rest. When squeezed by hand pressure, the gap is
easily closed such that the protrusions which extend
from each treatment members are brought into contact
with opposite sides of the stains on the fabrics being
treated.
With respect to the multiple protusions which comprise
the first and second treatment member, in this device
the protrusions comprise stiff, looped monofilament
fibers which extend from the face of each treatment
member for a distance of about 2.0 mm.
The soiled area is moistened with cleaning composition
by gently dabbing it with a sheet article of the
foregoing type. Once moist, a device of the type shown
in Figure 10 is placed at the stained area, with the
treatment members on either side of the fabric area of
staining. The device is squeezed 10-30 times, slowly,
to bring the illustrated looped protuberances into close
contact with the fabric, thereby loosening the stain
without damaging the fabric surface. The area is then
again padded with the sheet article.
2. The stained area was then placed directly upon a slip
of absorbent paper (the paper used was a sheet of
kitchen paper towel).
3. 1 ml of water was sprayed on the stained area, and
pressure and heat were applied using an iron set at a
temperature of 40~C ~or 15 ~econds. A typical ironing
pressure, as normally used for ,e...oving wrinkles in
fabrics, was used.
4. Step 3 was repeated with a further 2 ml of water.
5. The swatch was then dried and smoothed.
CA 02238497 1998-05-25
W097/20099 PCT~S96/19171 -
The method o~ cleaning was repeated on stained swatches
using the spot cleaning device of Figure 8 to 9 in place
of the spot c~eaning device of Figure 10.
