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Sommaire du brevet 1039142 

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  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Brevet: (11) CA 1039142
(21) Numéro de la demande: 1039142
(54) Titre français: DETERSIF A MOUSSE CONTROLEE
(54) Titre anglais: CONTROLLED-SUDSING DETERGENT COMPOSITIONS
Statut: Durée expirée - au-delà du délai suivant l'octroi
Données bibliographiques
Abrégés

Abrégé anglais


ABSTRACT OF THE DISCLOSURE
Granular built laundry detergent compositions are
disclosed which contain a suds-suppressing mixture of a water-
insoluble wax and a silicone in a water soluble or water
dispersible carrier.

Revendications

Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.


The embodiments of the invention in which an
exclusive property or privilege is claimed are defined as
follows:
1. A granular, built detergent composition that
comprises:
(a) from 2% to 40% by weight of an organic, syn-
thetic nonionic, zwitterionic or anionic surfactant, or a
mixture of any of these;
(b) from 10% to 90% by weight of one or more in-
organic or organic detergency-building salts;
(c) from 0.02% to 5% by weight of a substantially
water-insoluble wax or mixture of waxes, said wax or mixture
having a melting point of from 35°C to 125°C and a saponifica-
tion value less than 100; and
(d) a stable suds-controlling component comprising
a silicone suds-controlling agent releasably incorporated in
a water-soluble or water-dispersible, substantially non-
surface-active, detergent-impermeable carrier, said silicone
suds-controlling agent being selected from the group consist-
ing of
(i) a siloxane having the general structure
<IMG>
wherein x is from about 20 to about 2,000 and R and
R' are each alkyl or aryl groups,
(ii) an alkylated siloxane of (i) above combined with
solid silica wherein the silica has a particle size
of not more than 100 millimicrons and the surface
area thereof exceeds 50 m2/g,
19

(iii) an alkylated siloxane of (i) above combined with
hydrophobic silica wherein the silica has a particle
size of not more than 100 millimicrons and the
surface area thereof exceeds 50 m2/g,
(iv) a siloxane of (i) above sorbed onto and into a solid
wherein the weight ratio of siloxane to solid is
from 20:1 to about 1:20,
(v) a mixture of (i) above, alkylated silicone resin and
silica xerogels and xerogels having a particle size
of not more than 100 millimicrons and a surface area
exceeding 50 m2/g, and
(vi) mixtures thereof wherein the ratio of wax to said
suds-controlling component is from 20:1 to 1:10 by
weight;
said wax component being in an intimate mixture with some or all
of said organic surfactant or surfactants.
2. A composition according to claim i, which
contains from 10% to 70% by weight of component (b), and
wherein said wax or mixture of waxes has a melting point in
the range 35°C to 115°C.
3. A composition according to claim 1 or 2, which
contains from 0.004% to 1% by weight of the silicone suds-
controlling agent.
4. A composition according to claim 1 or 2, which
contains from 0.04 to 0.1% by weight of the silicone suds-
controlling agent.
5. A composition according to claim 1 or 2, wherein
the suds-controlling component (d) contains from 1% to 50%
by weight of silicone suds-controlling agent.

6. A composition according to claim 1 or 2, wherein
the suds-controlling component (d) contains from 4% to 10%
by weight of silicone suds-controlling agent.
7. A composition according to claim 1 or 2, which
contains from 0.25 to 3% by weight of the microcrystalline
wax.
21

Description

Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.


The present invention relates to granular built
laundry detergent compositions which have controlled sudsing
properties.
Especially when washing is performed in front-loading
automatic washing machines, excessive sudsing in the washing
step is undesirable. Not only does it interfere with the action
of the wash liquor upon the fabrics, but also the foam may reach
unintended parts of the washing machine and, in particular, it
may not be properly swept out of the machine before the rinse
liquor is added. The last problem can considerably increase the
amount of foaming in the rinse, and correspondingly increase the
difficulty of suppressing this foaming.
Copending, commonly assigned Canadian patent applica-
tion 217,689 filed January 10, 1975 discloses that certain waxes,
when used in granular, built detergent compositions, are capable
of suppressing the suds in the rinse; such waxes can also be
~' ~

~3~ Z
used either to cause little or no suds depression in the washing
step, or, if desired, to cause a controllable degree of suds
suppression in the washing step. In particular, the invention
of the said application provides a granular, built detergent
composition which comprises:
(a) from about 2% to about 40% by weight of an organic syn-
thetic detergent selected from the group consisting of
nonionic, zwitterionic, and anionic detergents and mixtures
thereof;
0 (b) from about 0.02% to about 5% by weight of a substantially
water-insoluble microcrystalline wax having a melting
point in the range from 35C to 115C and saponification
value less than 100 or mixtures thereof; and
(c) from about 10% to about 90% by weight of a detergency
building salt or mixtures thereof;
said wax being in intimate admixture with the said organic
detergent.
It is also disclosed, in our copending Canadian Patent
Application 117,771, filed July 31, 1973, that certain sili-
cone suds-suppressing agents, suitably isolated from premature
contact with the surface-active agents, are very effective for
controlling sudsing during the wash.
It is now found that a combination of the above-men-
tioned wax and silicone suds-suppressing agents has a synergistic
effect, so that a lower level of the combination can be used
to give effective suds control in the wash and in the rinse than
would be required if either were used alone. The advantage can
best be made clear by an illustration. A built, granular
detergent composition containing a nonionic organic surface-
active agent oversudsed severely in a drum automatic washingmachine. The sudsing in the wash could be adequately controlled

1~?39J.4Z
by addition of 2% by weight of a prilled silicone/silanated
silica suds-depressing component (containing about 8% silicone/
silanated silica in a non-surface-active carrier); the rinse
sudsing was not very well controlled. Higher l~evels of this
type of suds-depressant were found to cause excessive,'defoamant
action in the wash and had some undesirable side effects, for
instance upon cleaning performance. Alternatively, adequate
control in the wash and in the rinse could be obtained by use ''
of 3% of microcrystalline wax. However, a combination of only
1/2% each of the wax and of the silicone/silanated silica prills
was quite satisfactory for control of suds in both the wash
and the rinse.
The present invention thus provides a granular, built
detergent composition that comprises:
(a) from 2% to 40%, preferably 10% to 30%, by weight of an
organic, synthetic nonionic, zwitterionic or anionic
surfactant, or a mixture of any of these;
(b) from 10% to 90%, preferably 10~ to 70%, by weight of one
or more inorganic or organic detergency-building salts;
(c) from 0.02% to 5% by weight of a substantially water-
insoluble microcrystalline wax having a melting point
of from 35C to 125C and a saponification value less
than 100, or a mixture of such waxes; and
(d) a stable suds-controlling component comprising a silicone
suds-controlling agent releasably incorporated in a water-
soluble or water-dispersible, substantially non-surface-active,
detergent-impermeable carrier, said silicone suds-controlling
agent being selected from the group consisting of
(i) a silioxane having the general structure
R
~SiOtX
R'

1~)3914Z
wherein x is from about 20 to about 2,000 and R and R'
are each alkyl or aryl groups,
(ii) an alkylated siloxane of (i) above combined with solid
silica wherein the silica has a particle size of not more
than 100 millimicrons and the surface area thereof exceeds
50 m /g,
(iii) an alkylated siloxane of (i) above combined with hydro-
phobic silica wherein the silica has a particle size of not
more than 100 millimicrons and the surface area thereof
exceeds 50 m2/g,
(iv) a siloxane o~ (i) above sorbed onto and into a solid
wherein the weight ratio of siloxane to solid is from
20:1 to about 1:20,
(v) a mixture of (i) above, alkylated silicone resin and
silica xerogels and xerogels having a particle size of not
more than 100 millimicrons and a surface area exceeding
50 m /g, and
(vi) mixtures thereof wherein the ratio of wax to said suds-
controlling component is from 20:1 to 1:10 by weight;
said wax or waxes being in an intimate mixture with some or all
of said organic surfactant or surfactants.
Polyethoxy nonionic surfactants and mixtures thereof
with zwitterionic surfactants are preferred. Other suitable
organic, synthetic surfactants as well as suitable detergency-
building salts are disclosed in Canadian patent application
217,689 discussed above.
The waxes suitable for the present invention are any of
those suitable for the invention of Canadian patent application
217,689, particularly those described therein as suitable where
suds depression in the wash is required. Particularly preferred
are microcrystalline petrolatum waxes known as "Be Square 175" *,
* Trademark
-- 4 --

lQ3~4Z
sold by the Bareco division, Petrolite Corporation, Tulsa,
Oklahoma; "Mobilwax 2305"**, sold by the Mobil Oil Company Limited,
Wallasey Bridge Road, Birkenhead, Cheshire, England; and Shell
"MicrowaX 185/190"***.
In preparing the compositions it is important that
the wax be intimately associated with the surfactant. Methods of
achieving this by mixing the wax with the liquid or pasty
surfactant during the preparation of the product are described
in Canadian patent application 217,689.
The suds-controlling component (d) of the present com-
positions comprises a silicone suds-controlling agent which is
incorporated in a water-soluble or water-dispersible, sub-
stantially non-surface-active, detergent-impermeable carrier
material. The carrier material contains within its interior
substantially all of the silicone suds-controlling agent and
effectively isolates it from, i.e. keeps it out of contact with,
the detergent component of the compositions. The carrier material
is selected such that, upon admixture to water, the carrier matrix
dissolves or disperses to release the silicone material in-
corporated therein to perform its suds-controlling function.
The silicone materials employed as the suds-controlling
agents herein can be alkylated polysiloxane materials of several
types, either singly or in combination with various solid
materials such as silica aerogels and xerogels and hydrophobic
silicas of various types. In industrial practice, the term
"silicone" has become a generic term which emcompasses a variety
of relatively high-molecular-weight polymers containing siloxane
units and hydrocarbyl groups of various types. Generally, the
silicone suds-controllers can be described as siloxanes having
** Trademark
*** Trademark

J~)39~4Z
the general structure:
R
~siotX
~'
wherein x is from about 20 to about 2,000, and R and R' (which
may be alike or different) are each an alkyl or aryl group,
especially methyl, ethyl, propyl, butyl and phenyl. The
polydimethylsiloxanes (R and R' are methyl) having a molecular
weight within the range of from about 200 to about 200,000, and
higher, are all useful as suds-controlling agents. Suitable
silicone fluids of this type are commercially available from the
Dow Corning Corporation under the trademark "silicone 200 Fluids".
Additionally, other silicone materials wherein the
side chain groups R and R' are alkyl, aryl or mixed alkyl and
aryl hydrocarbyl groups exhibit useful suds-controlling pro-
perties. These materials are readily prepared by the hydrolysis
of the appropriate alkyl, aryl or mixed alkylaryl silicone
dichlorides with water in the manner well known in the art. As
specific examples of such silicone suds-controlling agents use-
ful herein there can be mentioned, for example, diethyl poly-
siloxanes; dipropyl polysiloxanes; dibutyl polysiloxanes; methyl-
ethyl polysiloxanes; phenylmethyl polysiloxanes; and the like.
The dimethyl polysiloxanes are particularly useful herein owing
to their low cost and ready availability.
A second type of silicone suds-controlling agent useful
in the compositions herein comprises a mixture of an alkylated
siloxane of the type hereinabove disclosed and solid silica.
Such mixtures of silicone and silica can be prepared by affixing
the silicone to the surface of silica (SiO2), for example by
means of the catalytic reaction disclosed in U.S. Patent
3,235,509. Suds-controlling agents comprising mixtures of

~Q3~ Z
silicone and silica prepared in; this manner preferably comprise
silicone and silica in a silicone:silica weight ratio of from
19:1 to 1:2, preferably 10:1 to 1:1. The silica can be
chemically and/or physically bound to the silicone in an amount
which is preferably about 10% to 15~ by weight, based on the
silicone. The particle size of the silica employed in such
silica/silicone suds controlling agents should preferably be not
more than 100 millimicrons, preferably from 10 millimicrons to
20 millimicrons, and the specific surface area of the silica
should exceed about 50 m2/g.
Alternatively, suds-controlling agents comprising
silicone and silica can be prepared by admixing a silicone fluid
of the type hereinabove disclosed with a hydrophobic silica having
a particle size and surface area in the range disclosed above.
Any of several known methods may be used for making a hydro-
phobic silica which can be employed herein in combination with
a silicone as the suds-controlling agent. For example, a fumed
silica can be reacted with a trialkyl chlorosilane (i.e.
"silanated") to affix hydrophobic trialkylsilane groups on the
surface of the silica. In a preferred and well known process,
fumed silica is contacted with trimethylchlorosilane and a
preferred hydrophobic silanated silica useful in the present
compositions is secured.
In an alternative procedure, a hydrophobic silica use-
ful in the present compositions and processes is obtained by
contacting silica with any of the following compounds: metal,
ammonium and substituted ammonium salts of long-chain fatty
acids, such as sodium stearate, aluminium stearate, and the
like; silylhalides, such as ethyltrichlorosilane, butyl-
trichlorosilane, tricyclohexylchlorosilane, and the like;and long-chain alkyl amines or ammonium salts, such as cetyl

~C~3~4Z
trimethyl amine, cetyl trimethyl ammonium chloride, and the like.
A preferred suds-controlling agent herein comprises a
hydrophobic silanated (most preferably trimethylsilanated)
silica having a particle size in the range from about lO
millimicrons to 20 millimicrons and a specific surface area
above about 50 m /g intimately admixed with a dimethyl silicone
fluid having a molecular weight in the range of from about 500
to about 200,000, at a weight ratio of silicone to silanated
silica of from about l9:1 to about 1:2. Such suds-controlling
agents preferably comprise silicone and the silanated silica
in a weight ratio of silicone:silanated silica of from lO:1
to l:l. The mixed hydrophobic silanated tespecially trimethyl-
silanated) silica-silicone suds-controlling agents provide suds
control over a broad range of temperatures, presumably due to
the controlled release of the silicone from the surface of the
silanated silica.
Another type of suds control agent herein comprises a
silicone material of the type hereinabove disclosed sorbed
onto and into a solid. Such suds controlling agents comprise
the silicone and solid in a silicone: solid ratio of from
20:1 to about 1:20, preferably about 5:1 to anout 1:1. Examples
of suitable solid sorbents for the silicones herein include
sodium carbonate, sodium tripolyphosphate, any of the sodium
silicates, c~ay, starch, kieselguhr, Fuller's earth, and the
like. The alkalinity of the solid sorbents is of no consequence
to the compositions herein, inasmuch as it has been discovered
that the silicones are stable when admixed therewith. As
disclosed hereinabove, the sorbent-plus-silicone suds controlling
agent must be coated or otherwise incorporated into a carrier
material of the type hereinafter disclosed to effectively
isolate the silicone from the detergent component of the
present compositions.
-- 8

1039~2
Yet another type of silicone suds-controlling agent
hereincomprises a silicone fluid, a silicone resin and silica.
The silicone fluids useful in such suds-controlling mixtures
are any of the types hereinabove disclosed, but are preferably
dimethyl silicones. The silicone "resins" used in such compo-
sitions can be any alkylated silicone resins, but are usually
those prepared from methylsilanes. Silicone resins are commonly
described as "three-dimentional" polymers arising from the
hydrolysis of alkyl trichlorosilanes, whereas the silicone fluids
are "two-dimensional" polymers prepared from the hydrolysis of
dichlorosilanes. The silica components of such compositions are
the micro-porous materials such as the fumed silica aerogels and
xerogels having the particle sizes and surface areas herein-
above disclosed.
The mixed silicone fluid/silicone resin/silica materials
useful in the present compositions can be prepared in the
manner disclosed in U.S. Patent 3,455,839. These mixed
materials are commercially available from the Dow Corning
Corporation. According to U.S. Patent 3,455,839, such materials
can be described as mixtures consisting essentially of:
(a) fromlabout 10 parts to about 100 parts by weight of a
polydimethylsiloxane fluid having a viscosity in the
range of from 20 cs. to 1500 cs. at 25C;
(b) 5 to 50 parts by weight of a siloxane resin composed of
(CH3)3SiOl/2 units and SiO2 units in which the ratio of
the (CH3)3SiOl/~ units to the SiO2 units is within the
range of from 0.6:1 to 1.2:1; and
(c) 1 to 10 parts by weight of a silica aerogel.
Such mixtures can also be sorbed onto and into a water-soluble
solid as disclosed above.
Again, such mixed silicone resin/silica suds-controlling

4Z
agents must be combined with a detergent-impermeable carrier
material to be useful in the compositions herein.
The silicone suds-controlling agents of the afore-
mentioned type must be incorporated within (i.e. coated, en-
capsulated, covered by, internalized, or otherwise substantially
contained within) a water-soluble or water-dispersible carrier
material which must be impermeable to detergents and which,
itself, must be substantially non-surface active. By sub-
stantially non-surface active is meant that the carrier material,
itself, does not interact with the silicone material in such
fashion that it is emulsified or otherwise excessively dis-
persed throughout an aqueous medium, rather than at the air/water
interface.
Of course, when preparing a dry powder or granulated
detergent composition it is preferable that the silicone suds
controlling component thereof also be substantially dry and
non-tacky at ambient temperatures. Accordingly, it is pre-
ferred herein to use as the carrier material or vehicle plastic,
organic compounds which can be conveniently melted, admixed with
the silicone suds-controlling agent, and thereafter cooled to
form solid powders, granules or prills. There are a wide variety
of such carrier materials useful herein. Since the silicone
suds-controlling- agent is to be releasably incorporated in
the carrier, such that the silicone is released into the aqueous
bath upon admixture of the composition therewith, it is preferred
that the carrier material be water-soluble. However, water-dis-
persible materials are also useful, inasmuch as they will also
release the silicone upon addition to an aqueous bath.
A wide variety of carrier materials having the re-
quisite solubility/dispersibility characteristics and theessential features of being non-surface active and detergent-
-- 10 --

iQ39~l42
impermeable are known. For example, the high-molecular-weight
"Carbowax"*-es which have substantially no surface-active
characteristics are useful herein. Examples of this type of
material include the polyethyleneglycols having a molecular
weight of from about 1,500 to about 10,000, especially about
4,000. Surprisingly, highly ethoxylated fatty alcohols such as
tallow alcohol condensed with about 25 molar proportions of
ethylene oxide are useful herein. Other alcohol condensates
containing extremely high ethoxylate proportions (ca. 25 and
above) are also useful herein. Such high ethoxylates apparently
lack sufficient surface-active characteristics to interact or
otherwise interfere with the desired suds-control properties
of the silicone agents herein. A particularly preferred ethoxyl-
ated carrier material herein is tallowalcohol condensed with
about 25 molar proportions of ethylene oxide, and abbreviated
TAE25.
A variety of other materials useful as the carrier
agents herein may also be mentioned: gelatin; agar; gum arabic;
and various algae-derived gels.
The silicone suds controlling component of the present
invention can be conveniently prepared by admixing or spraying
the silicone suds-controlling agent with a carrier material
to form a granular product. Conveniently, a melt of carrier
material and silicone suds-controlling agent is prepared and
sprayed in a cooling tower to form droplets comprising the
carrier material with the silicone suds-controlling agent
releasably incorporated therein. When this procedure is used,
the silicone suds-controlling agent is contained within the
carrier material so effectively that when this material is
* "Carbowax" is a trademark of Union Carbide Corporation for a
series of polyethylene glycols. They have characteristics as
described in The Merck Index, 9th Ed. (1976) pp. 983-384.
-- 11 --

iO391~2
eventually admixed with or incorporated into a detergent
composition, the silicone does not substantially come into
contact with the detergent surfactant ingredient.
In order to provide a granular, non-tacky suds controll-
ing component useful in dry granular detergent compositions, the
composite of the silicone suds controlling agent and carrier
material should be substantially solidified. This can be
achieved by use of long drying towers or rapid refrigeration
processes which quickly cool the droplets such that the carrier
melt is hardened. However, such procedures are not preferred
in an industrial process because of extra plant requirements.
It has been discovered that a rapid and effective way
for solidifying a carrier melt containing the silicone suds-con-
trolling agent is by spray-drying the carrier melt into and
onto a fluidized bed of a solid, preferably water-soluble
material to form coated granules. The resulting coated granules
of suds-controlling component are crisp and free-flowing, and
are especially adapted for use in detergent compositions.
Any type of powdered material is useful to form a
fluidized bed suitable for cooling and coating the spray-dried
melts therein. Of course, it is particularly suitable to choose
dry powders which are useful per se in detergent compositions
for their builder, soil-suspending, softening, and the like
properties. Specific examples of suitable powdered coating
materials useful in the flùidized bed processes herein include,
for example, sodium tripolyphosphate tSTPP)~ sodium carbonate,
sodium carboxymethyl-cellulose, granulated starch, clay, sodium
citrate, sodium acetate, sodium sulfate, and the like. The
particle size of such coating materials is in no way limited
but must be such that a fluidized bed can be conveniently secured.
In general, particle size range will be from about 0.1 micron to
- 12 -

~3~3~l4Z
about 100 microns.
It is recognized that the amount of carrier used to
isolate the silicone suds-controlling agent herein from the
detergent component of the compositions herein is not critical.
It is only necessary that enough carrier be used to provide
sufficient volume that substantially all the silicone can be
incorporated therein. Likewise, it is preferred to have
sufficient carrier material to provide for sufficient strength
of the resultant granule to resist prematuxe breakage.
Likewise, the amount of solid powder material which
optionally coats the carrier-plus-silicone granule is not
critical. For most purposes, sufficient powder is employed to
substantially coat the mixture of carrier having the silicone
incorporated therein with one or two layers of the powder. In
addition to cooling and solidifying the carrier, the particulate
coating material provides additional protection from the
detergent component of the compositions, but it is not essential
for this purpose.
It is usually preferred, however, that the suds-con-
trolling component (d) should contain about 1 to 50% especiallyabout 2 to 20% and in particular about 4 to 10~ of the silicone
suds controlling agent by weight.
The size of the particles of the suds-controlling
component td) in the present compositions is not critical to
their use and performance characteristics. In general, spray-
drying processes result in particles in a size of from about
1 micron to about 1000 microns in diameter.
The amount of microcrystalline wax and of silicone
suds-suppressing component required in a particular detergent
composition depends upon many factors, such as the degree of
suds suppression required, the nature of the detergent composition,

~ 3~ Z
the kind of washing machine, and so on. Generally, as indicated
above, less of each is required than would be needed if it were
used alone. Thus usually the amount of silicone suds-suppressing
agent (.e.g silicones and silanated silica) is from 0.004 to 1%
by weight of the composition, preferably from 0.01 to 0.2%
and especially from 0.04 to 0.1%. Preferably, the level of
wax component is from 0.25 to 3%, especially from 0.3 to about
2%. The ratio of wax to silicone suds-suppressing component
(e.g. prills) is generally from 20:1 to 1:10, usually from
2:1 to 1:3, and especially about 1:1~
The compositions may, of course, contain other com-
ponents usual in laundry detergent compositions; such adjuvants
are mentioned in the complete specification of Canadian Patent
Application 217,689, filed January 10, 1975.
The present invention is illustrated in and by the
following Examples.
Example 1
Granular detergent compositions were prepared having
the compositions given below. In these compositions "Dobanol
45-E-7" (trademark) is a mixture of primary alcohols having
14-15 carbon atoms condensed with 7 molar proportions of
ethylene oxide; the silicone/silanated silica prills consisted
essentially of 5% silicone, 5% silanated silica, about 50%
sodium tripolyphosphate and about 40% tallow alcohols condensed
with 25 molar proportions of ethylene oxide; the wax is
"Mobilwax 2305" (trademark), a microcrystalline petroleum wax
of melting point 170F. The wax was predissolved in the
"Dobanol 45-E-7" before mixing with the other components (except
the silicone/silanated silica prills and perborate) for spray
drying. The silicone/silanated silica prills and the perborate
were dry mixed with the spray-dried granules constituting the
remainder of the composition.
- 14 -

~ 3~l4Z
Composi*ion 1 2 3 4 5 6 7 8 9 10
"Dobanol 45-E-7" 12 1212 1212 12 12 1212 12
Sodium tripolyphos-
phate 36 3636 3636 36 36 3636 36
Sodium silicate 7 7 7 7 7 7 7 7 7 7
Sodium sulphate 5.5 4.5 4.5 4.5 4 4 4 3.5 3.5 3.5
Sodium perborate 25 25 25 25 25 25 25 25 25 25
Water 12 12 12 12 12 12 12 12 12 12
Miscellaneous minor
components 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5
Silicone/silanated
silica prills - - 0.5 1.0 0 0.5 1.5 0 1.5 2.0
Wax - 1 0.5 - 1.5 1.0 0 2 0.5 0
These compositions were tested according to the method
described in Example 2 of Canadian Patent Application 217,689.
Composition 1, with no suds-suppressant, oversudsed
severely in the wash and was unsuitable for use in the washing
machine. Results obtained for the other compositions are given
below.
Suds height in the window of the "Hoover"* machine
during the wash and coverage (%) of the window of the Indesit
machine after pumping out the indicated liquors were as follows:
Suds % coverage
Composition Height (ins.) Wash Rinse 1- 2 3 4 5
2 3.4 100 75 ~0 10 0 0
3 1.4 100 50 10 0 0 0
4 2.5 100 100 50 10 0 0
2.8 100 75 25 10 0 0
6 0 100 50 10 0 0 0
7 2.0 100 100 50 10 0 0
8 1.6 100 50 25 10 0 0
9 0 100 50 10 0 0 0
2.5 100 75 25 10 0 0
* Trademark
- 15 -

1~3~L4.Z
Suds coverage (~) of surface the container after the
indicated liquids had been pumped into it were as follows:
Composition WashRinse 1 2 3 4 5
2 100 100 100 10 0 0
3 100 100 50 10 0 0
4 100 100 100 5025 0
100 100 75 10 0 0
6 100 100 50 10 0 0
7 100 100 100 5025 0
8 100 100 50 10 0 0
9 100 100 50 10 0 0
100 100 100 25 0 0
Example 2
The effect of the synergistic suds depressant com-
binations of the invention upon the suds profile of the products
listed below was evaluated using a Minidrum (miniature drum-type
washing machine). The products were used at 0.5% by weight
concentration in 18H (258 ppm as CaCO3) hard water to wash
realistically soiled loads consisting of 2 cotton terry towels
and one cotton tea towel. This gave a cloth to liquor ratio
of about 1:10 by weight.
The wash water, with the load in it, was heated with
intermittent agitation from about 25C to 90C during 45
minutes, and the suds height was measured in the window of
the machine at intervals of 20C.
The products tested were as follows:
- 16 -

1~3~l4A~
Test Product 1 2 3 4 5 6 7 8 9
"Dobanol 45-E-7" 12 1212 12 12 12 12 12 12
Sodium linear dodecyl
benzene sulphonate
Sodium tripoly-
phosphate 36 3636 36 36 36 36 36 36
Sodium silicate 7 7 7 7 7 7 7 7 7
Sodium perborate25 2525 25 25 25 25 25 25
Sodium sulphate 5 5 5 5 5 5 5 5 5
Water 10 1010 10 10 10 10 10 10
Minor components3 3 3 3 3 3 3 3 3
*Silicone depressant 1 - 0.5 - 0.5 - 0.5 - 0.5
"Mobilwax 2305" - 10.5 - - - - - -
Shell "Microwax 185/190"- - - 10,5
Paraffin Wax (M.Pt.
120-125F) - - - - - 1 0.5
Beeswax - - - - - - - 1 0.5
* Prills containing 4% by weight of a 9:1 mixture of silicone-
silanated silica.
1 2 3 4 5 6 7 8 9
Suds heights (ins.) at
30C 1 1 ~ 6 2
50C 3 - 1~~ ~ 0 1 ~ 62 42
70C 6 12 ~ 0 6 4 12 52
90C 1 7 0 4 0 12 3 12 2~
This table shows excellent performance of mixtures with
microcrystalline waxes and limited effectiveness with paraffin
wax and beeswax.
Example 3
Naturally soiled clothes were washed in the "boil-wash"
cycle of a Miele 421S washing machine, and the suds levels in
the window of the machine were measured at stated temperatures
during the heat up stage of the main wash. Washing conditions
- 17 -

1(~3~Z
were: cold water fill; 18H (258 ppm as CaCO3, Ca:Mg ratio
10:1 by weight); 70 g product in prewash, 140 g in main wash.
22 cms suds height corresponded to a full window. The com-
positions compared and the suds heights are given in the
following table.
Composition 1 2 3 4 5
"Dobanol 45-E-7" 8 8 8 8 8
C14.g alkyl dimethyl-
ammoniopropane sulphonate 4 4 4 4 4
Sodium tripolyphosphate32 32 32 32 32
Sodium silicate 6 6 6 6 6
Sodium sulphate 9 6.5 4.0 8 6.7
Sodium perborate 23 23 23 23 23
Moisture and miscellaneous
minors 17 17 17 17 17
Shell "Microwax 185/190"1 1 1 2 2
Silicone depressant
(As employed in Example2) - 2.5 5.0 - 1.25
Suds heights, cms, at 1 2 3 4 5
40C 17 trace trace trace trace
60C 18 4 trace 4trace
80C 20 8 trace 13trace
95C oversudsed 9 trace 17 2 "
-- 18 --

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2024-08-01 : Dans le cadre de la transition vers les Brevets de nouvelle génération (BNG), la base de données sur les brevets canadiens (BDBC) contient désormais un Historique d'événement plus détaillé, qui reproduit le Journal des événements de notre nouvelle solution interne.

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Inactive : CIB de MCD 2006-03-11
Inactive : CIB de MCD 2006-03-11
Inactive : Périmé (brevet sous l'ancienne loi) date de péremption possible la plus tardive 1995-09-26
Accordé par délivrance 1978-09-26

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Page couverture 1994-05-18 1 14
Abrégé 1994-05-18 1 7
Revendications 1994-05-18 3 67
Dessins 1994-05-18 1 5
Description 1994-05-18 18 617