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Sommaire du brevet 1228521 

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  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Brevet: (11) CA 1228521
(21) Numéro de la demande: 1228521
(54) Titre français: DETERGENTS LIQUIDES
(54) Titre anglais: LIQUID DETERGENT COMPOSITIONS
Statut: Durée expirée - après l'octroi
Données bibliographiques
(51) Classification internationale des brevets (CIB):
  • C11D 01/831 (2006.01)
  • C11D 01/14 (2006.01)
  • C11D 01/22 (2006.01)
  • C11D 01/29 (2006.01)
  • C11D 01/52 (2006.01)
  • C11D 01/72 (2006.01)
  • C11D 01/83 (2006.01)
(72) Inventeurs :
  • ATKINSON, RONALD E. (Royaume-Uni)
  • WILMSHURST, STEPHEN J. (Royaume-Uni)
  • LAWSON, JOHN R. (Royaume-Uni)
(73) Titulaires :
  • THE PROCTER & GAMBLE COMPANY
(71) Demandeurs :
  • THE PROCTER & GAMBLE COMPANY (Etats-Unis d'Amérique)
(74) Agent: GOWLING WLG (CANADA) LLP
(74) Co-agent:
(45) Délivré: 1987-10-27
(22) Date de dépôt: 1984-05-11
Licence disponible: S.O.
Cédé au domaine public: S.O.
(25) Langue des documents déposés: Anglais

Traité de coopération en matière de brevets (PCT): Non

(30) Données de priorité de la demande:
Numéro de la demande Pays / territoire Date
8313348 (Royaume-Uni) 1983-05-14

Abrégés

Abrégé anglais


LIQUID DETERGENT COMPOSITIONS
ABSTRACT
Stable liquid dishwashing detergent compositions are
provided incorporating an alkyl benzene sulphonate and/or
alkyl sulphate, an alkyl ethoxy sulphate and an ethoxylated
C9-C13 alcohol containing an average of from 3 to 12
moles of ethylene oxide and wherein the ethoxylated alcohol
contains no more than 1% by weight of unethoxylated alcohol.

Revendications

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


C L A I M S
1. A physically stable liquid detergent composition consisting essentially of:
(a) from about 20% to about 50% by weight of an anionic surfactant system consisting essentially of (1) a surfactant selected from the group
consisting of a C10-C16 alkyl benzene sulfonate salt, a C10-C16
primary alkyl sulfate salt, and mixtures thereof; and (ii)
a C10-C16 primary alkyl ethoxy sulfate salt containing an
average of not more than about 6 ethylene oxide groups per
alkyl group in the alkyl ether sulfate,
(b) from about 1% to about 5% by weight of an ethoxylated C9-C11
aliphatic alcohol containing an average of from about 6 to about 10
moles of ethylene oxide per mole of alcohol, said ethoxylated alcohol
containing not more than about 1% by weight of unethoxylated alcohol;
(c) from about 3% to about 10% by weight of a hydrotrope selected from
the group consisting of C1-C3 aliphatic alcohols, urea, a lower alkyl
benzene sulfonate, and mixtures thereof; and
(d) the balance being water; said composition being free of paraffin
sulfonate surfactant.
2. A liquid detergent composition according to Claim 1 wherein the ethoxy-
lated alcohol contains less than 0.7% by weight of unethoxylated alcohol.
3. A liquid detergent composition according to Claim 1 wherein the alcohol
ethoxylate is a primary alcohol ethoxylate.
4. A liquid detergent composition according to Claims 1, 2 or 3 wherein the
level of monoethoxylated alcohol in the alcohol ethoxylate is no more than
5% by weight of the alcohol ethoxylate.
26

5. A liquid detergent composition according to Claim 2 wherein the
ethoxylated alcohol contains less than 0. 5% by weight of unethoxylated
alcohol.
6. A liquid detergent composition according to Claim 5 which further includes
from about 2% to about 8% by weight of a suds promoting agent selected
from the group consisting of C10-C16 mono-and di-C2-C3 alkanolamides,
C8-C18 alkyl di C1-C3 alkyl amine oxides, and mixtures thereof.
27

Description

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


AL
LIQUID DETERGENT COMPOSITIONS
R E Atkinson
S J Wilmshurst
J R Lawson
Field of the Invention
This invention relates to aqueous liquid detergent
compositions and particularly to dishwasing compositions
incorporating a mixture of anionic and ethoxylated
non ionic surfactant~.
Background of the Invention
Liquid detergent compositions intended for use as
dish washing products conventionally take the form of
cleat aqueous solution containing a mixture of one or
more sulfite and sulphonate anionic surfactants
together with a suds stabilizing agent. Where cellophane-
ate surfactants are used in such mixtures they may be
of the olefin sulphonate, paraffin sulphonata or most
usually alkyd Bunsen sulphonate type whilst alkyd
sulfites and alkyd ether sulpha~es form the sulfite
species commonly employed. Recently there has been a
trend towards the use of magnesium cations for at least
.. ,

Al 35~
-- 2
part of the anionic surfactants present and thy
disclosures of British patent Specifications Nos.
1,524,441 and 1,551,074, British published Patent
Application No. 2,010,893 A and European Patent
Application Publication No. 0039110; published November
4, 1981, are representative of the state of the art.
'rho art teaches that these formulations have enhance
performance, particularly when used in water of low
mineral hardness. Nevertheless, the pressure to improve
the cost-effectiveness of liquid detergent compositions
has meant that the search has continued for compositions
having improve economy, performance and in-use kirk-
teristics. In particular, intensive effort has been
expended in increasing the concentration of dish washing
liquid detergent compositions and in reducing the level
of diluer.ts such as water and solubilising hydrotropes
without sacrificing the storage stability of the
compositions.
In most liquid dish washing detergent compositions
based primarily on anionic surfactants the use of
anionic surfactant levels above about 30~ my weight of
the composition the precise value being dependent on
the surfactants employed) demands an increase in hydra-
trove level. An exception Jo this general pattern ox
'I'
,. I,

I
-- 3 --
behavior is, however, provided by paraffin su~phonates,
commercial sources of which contain disulphonate
components which are believed to provide some hydra-
trouping characteristics. These components make
compositions containing paraffin sulphonates more
tolerant towards otherwise poorly soluble ingredients
such as inorganic salts and certain suds stabilizers
such as alkanolamides. In the absence of a significant
level twig. 5%) of paraffin sulphonates, the addition
of suds stabilizers such as alkanolamides and amine
oxides require additional hydrotrope in order Jo main-
lain the phase stability of the composition on storage.
Ethoxylated non ionic surfactants constitute a class
of materials capable of solubilisin~ other components in
aqueous media but this capability is strongly dependent
on their average degree of ethoxylation (E 3. Highly
a
ethoxylated non ionic surfactant~ e, sly), axe
a
very hydrophilic in nature and thus tend to reduce the
oily soil removal capability of liquid douching
detergent formulations which is undesirable why no oil
and grease is an imprint criterion of consumer
acceptance. on the other hand, non ionic surfactant~
having low levels of ethoxylation (i.e. E I art too
a
hydrophobic and do not have adequate water volubility.

I
-- 4
A feature shared by all exulted non ionic
surfactants is the presence of a level of unethoxylated
material, the magnitude of which depends on the degree
of ethoxylation, but which can constitute up to 15% my
weight of the non ionic surfactant. Unethoxylated
Cg-Cl5 aliphatic primary alcohols are odorous materials
having a low water volubility, but the comparatively low
level of the unethoxylated fraction in an ethoxylated
Cg-Cl5 alcohol surfactant makes such characteristics
used in laundry detergent proxy particularly
granular products for use in automatic washing machines.
However, consumers tend to be very aware of the physical
characteristics ox liquid detergent compositions,
particularly those used for dish washing, because of the
manual nature of the task and the greater degree of
exposure of the consumer to the hot wash liquor.
Accordingly, the odor and phase stability corrugators-
tics of liquid detergents formulated with ethoxylated
non ionic surfactants have been considered to be less
than optimum.
In dish washing liquid detergent formulations in
which a paraffin sulphonate is the, or the principal,
sulphonate species present, the inclusion of ethoxylated
non ionic surfactants having E in the rang 2-6 has been
a
-

-- 5 --
judged to be acceptable anesthetically by consumers.
Nevertheless, for surfact~nt mixtures not containing
paraffin sulphonate, the adverse influence ox unethox
slated components in the non ionic surfactant has been
judged to be unacceptable.
In particular, liquid do hashing detergent combo-
sweetness containing alkyd sulfites and/or alkyd Bunsen
sulphonates have been found to be subject to odor and
storage stability problems when formulated with ethos-
slated non ionic surfactants containing the normal spread of ethoxylated species, and this effect is more
pronounced when the composition also contains magnesium
ions. However, it has now been found that certain
alcohol ethoxylates, from which the unethoxyla~ed, and
preferably at least part of the mono-ethoxylated,
species have been removed, can be incorporated in alkyd
Bunsen sulphonate or alkyd sulphat~-containing liquid
dish washing compositions without adverse effect on the
storage stability of the latter.
so
According to tile present invention therefore there
it provided a physically stable liquid detergent combo-
session comprising from 20-50~ of an anionic surfactant
I;

-- 6
system consisting essentially of a C -C alkyd
16
Bunsen sulphonate salt and/or a C -C primary alkyd
16
sulfite salt together with a C -C primary alkyd
16
ethics sulfite salt containing an average of not more
than 6 ethylene oxide groups per alkyd group in the
alkyd ether sulfite, and optionally including a suds
stabilizing agent wherein the composition also includes
from 1-5% of an ethoxylated C -C aliphatic alcohol
13
containing an average of 3-12 moles of ethylene oxide
lo per mole of alcohol, said ethoxylated alcohol containing
less than 1% by weight of unethoxylated alcohol.
In preferred compositions in accordance with the
invention thy ethoxylated C -C aliphatic alcohol
g 13
contains an average of from 6 to 10 Miss of ethylene
oxide per mole ox alcohol.
Preferably, the ethoxylated alcohol contains less
than 0.7%, most preferably lo than 0.5~ or unethox-
fated material, and in highly preferred compositions
the level of mono-ethoxylated alcohol it no more than
I by weight of the non ionic surfactant.
Preferred liquid detergent compositions, in
accordance with the invention, incorporate an alkyd
sulfite surfactant and magnesium ions in a molar amount
corresponding to at least half ox the molar mount of
I,

the alkyd ~ulphate present and contain from 2-4% by
weight of the ethox~lated alcohol.
One preferred group of compositions incorporates a
three component anionic surfactant system, comprising
8-12~ by weight of the composition of C -C primary
alkyd sulfite, 9-11% of a C -C primary alkyd
16
ethoxysulphate containing an average of from 1.5 to 3
ethics groups per alkyd group, and 13-17~ of a C -C
alkyd Bunsen sulphonate. The cations in this system
are a mixture of ammonium and magnesium ion the level
of magnesium corresponding to approximately one half
of the molar amount of alkyd sulfite present.
Another preferred group of compositions employs a
two component anionic surfaetant system comprising from
4-8% C -C primary alkyd sulfite and from 20~25
16
C -C alkyd ethics sulfite containing from 0.5 to 2.0
I 16
epoxy groups per alkyd group
Preferably also compositions in accordance with
the invention contain 2~-8%, most preferably 3~-4~ by
weight of a suds booster selected from C -C moo and
lo 16
disc alkanolamidef and C -C alkyd at Cluck alkyd
amine oxides
or

-- 8 --
Dot l the I~e~ti~r
Detergent compositions in accordance with the
present invention comprise a mixture of anionic sun
fact ants of defined constitution, an amount of from 20
to 50~ by weight ox the composition, together with an
ethoxylated non ionic surfactant having a low content of
unethoxylated material.
All compositions in accordance with the invention
incorporate an alkyd sulfite and/or an alkyd Bunsen
sulphonate component in combination with an alkyd ethics
sulfite.
The alkyd sulfite component it a primary alkyd
sulfite in which the alkyd group contains 10-16 carbon
atoms, more preferably an avexase of 12-14 carbon atoms
preferably in a linear chain. C -C alcohols, derived
16
from natural fats or Ziegler olefin build up or OX
synthesis, form suitable source for the alkyd group.
Examples of synthetically derived material include
"Dobanol 23" (RUM) sold by Shell Chemicals US Ltd.,
"Ethyl 24" *sold by the ethyl Corporation, a lend of
C -C alcohols in the ratio 67% C , 33~ C sold
13 15 13 15
under the trademark "lu~ensol" by BASS Smb~l and
and Synperonic RUM by ICY Ltd., and "Hal swilled
by Liquichimica Italian. Example of naturally
* Trademark
** Trademark
or

- 9 -
occurring materials from which the alcohols cay be
derived are coconut oil and palm kernel oil and the
corresponding fatty acids.
When present in compositions in accordance with the
invention, the level of the alkyd sulfite component
lies in the range of from 4% to 20% by weight of the
composition, more generally from 4% to 16% by weight.
In one preferred compositional aspect of the invention
in which alkyd Bunsen sulphonate is also incorporated,
the usage level lies in the range prom 8% to 12% by
weight, most preferably in the range from 8% to 11~ by
weight. In another compositional aspect of the invent
lion in which a sulphonate component is not present,
the alkyd sulfite level lies in the range from 12~ to
20~, more preferably Roy 14~ to 18% by weigh.
For the purposes of the present invention any
alkali metal, alkali earth metal ammonium or subset
tuned ammonium cation can he used in association with
the alkyd sulfite. However, in highly preferred
compositions in accordance with the invention the alkyd
sulfite is associated with a source of magnesium ions
which, as will be described hereinafter, can either ye
introduced as the oxide or hydroxide to neutralize the
,. w .

~2~5~
-- 10 --
acid or can be added to the composition as a water
soluble salt. The addition of appreciable levels of
magnesium salts to the dish washing compositions of the
invention raises the temperature at which inorganic salt
crystals form in the compositions on cooling and is
therefore less preferable.
In composition comprising a mixture of alkyd
Bunsen sulphonate, alkyd sulfite and alkyd ether
sulfite, the molar amount of magnesium ion in the
compositions is controlled to correspond to 0.20-0.70X,
preferably 0.45-0.55X where X is the number of moles of
C -C alkyd sulfite present. Most preferably the
16
magnesium ion content is adjusted to provide the
stoichiometric equivalent of the alkyd sulfite present
In practice the magnesium ion will be present at a level
of from abut Owe to about 0.70% by weight, preferably
from 0.35~ to 0.55~ by weight of the composition.
By contrast, compositions containing only alkyd
sulfite and alkyd ether sulphatP as the anionic
surfactants will preferably contain up Jo about 0.90% by
weight of the composition of magnesium ion, and part of
the allele ether sulfite will also be neutralized by
magnesium ion.
Al
.

a
Alkyd Bunsen sulphonates useful in compositions ox
the present invention are those in which the alkyd group,
which is substantially linear, contains 10~16 carbon
atoms, preferably 11-13 carbon atoms, a material with an
average carbon chain length of 11.8 being most preferred.
The phenol isomer distribution, i.e. the point of
attachment ox the alkyd chain to the Bunsen nucleus, is
not critical but alkyd benzenes having a high phenol
isomer content are preferred. When employed in
compositions in accordance with the present invention,
an alkylbenzene s~lphonate content ox from 10~ to 28~
by weight of the composition is required generally from
12% to 26% by weight. In a preferred aspect of thy
invention an al~ylbenzene sulphonate content of prom
13~ to 17% by weight is used and highly preferred
compositions in accordance with this aspect of the
invention have from 14% to 17% of C alkyd Bunsen
11.8
sulphonate.
The alkyd ethics sulfite ~urfactant component
comprises a primary alkyd ethics sulfite derived from
the condensation product of a C10~ alcohol with an
average of up to 6 ethylene oxide groups The C10-Clb
alcohol itself can be obtained from any of the sources
previously described or the alkyd sulfite component.
It has, however, been

35~
- 12 -
found preferable to use alkyd sulfite and alkyd ether
sulfite in which the carbon chain length distributions
are the same. C -C alkyd ether sulfites art pro-
12 13
furred and the level of alkyd ethics sulfite in the
composition lies between I and 25~ by weight of the
compositions, generally in the range from 10~ to 25%
by weight. In the preferred aspect of the invention
incorporating an alkyd Bunsen sulphonate surfactant,
the level lies in the range from 9% to 11% by weight
most preferably in the range from 9% to 15% by weight.
Conventional ethoxylation processes result in a
distribution of individual ethoxylates ranging from
1 Jo 10 ethics groups per mole of alcohol, so that the
desired average can be obtained in a variety of ways.
lo Blends can ye made of material having different degrees
of ethoxylation anger different ekhoxylate distributions
arising from the specific ethoxylatiQn techniques
employed and subsequent processing steps such as distill
lotion. For example, it has been found what equivalent
seducing and grease removal performance Jo that given by
a blend of alkyd sulfite and alkyd triethoxy ether
sulfite can be obtained by reducing the level of alkyd
sulfite and using an alkyd ether sulfite with an
average ox approximately two ethics groups per mole of
r
Jo .. .

~2~35~
- 13 -
alcohol. In preferred compositions in accordance with
the present invention the average degree of ethoxylation
is from 0.5 to 4, more preferably from 0~8 to 2Ø
The counter ion or the alkyd sulfite can be any
one of sodium, potassium, ammonium or alkanol-ammonium
or a mixture thereof. However, for the purposes of
obtaining the lowest possible chill point temperature
(the temperature at which inorganic salt crystals
separate), it is desirable that at least 30% of the
counter ions for the alkyd ethics sulfite should be
ammonium. In compositions containing an alkyd Bunsen
sulphonate component it is highly preferred that the
alkyd ethics sulfite is completely neutralized by
ammonium ions.
lo The counter ions in association with the alkyd
Bunsen sulphonate art independently selected in the
same manner as those for the alkyd ethics s~lphate,
there being preferably at least So of ammonium ions.
In order for compositions in accordance with the invent
lion to have a chill point of Cook, at least 70~ of the
neutralizing cations for the anionic surfactants should ammonium ions and Yost preferably ammonium constitutes
the only cation present other than magnesium

3L;~285~
- 14 -
The ethoxylated non ionic surfactant component of
the invention is a C -C aliphatic alcohol ethoxylate
9 13
containing an average of 3 12, preferably from 6 to 10
moles of ethylene oxide per mole of alcohol and not more
than 1% by weight of unethoxylated alcohol.
The starting alcohol is preferably a primary
alcohol which may be derived from natural or synthetic
sources. Thus natural fats or oils, or products of
Ziegler olefin build up reactions or OX synthesis
may all be used as the source of the hydrocarbon chain,
the structure of which may be linear or branched in type.
The preferred alcohol chain length range is from
C -C as it has been found that performance, viz.
g 11
seducing volume and mileage, are optimum for ethoxylates
made from such alcohols. The average degree of ethos-
ylat~on (E ) lies in the rang from 3 12 Poles per moleav
of alcohol, but is preferably in the range from 5-10
moles per mole of alcohol. A discussed with respect to
the alkyd ethics sulfite component, normal (base
catalyzed) ethoxylation process to produce an average
degree of ethoxylation of 6-10 results in a distribution
of ethoxylate species which ranges from 1 to 15 moles of
ethylene oxide per mole of alcohol. An increase in E
a

I
- 15 -
causes some ennui in this distribution, principally a
reduction in the level of unethoxylated material, but
an increase in E from 3 to 5 will still leave appear-
a
ximately 5-10~ of such material in the ethoxylated
product.
In the liquid dish washing detergent compositions of
the invention, this level of unethoxylated material will
give rise to phase stability/chill point problems and/or
will result in a product having a fatty alcohol odor
which is unacceptable to consumers and cannot be masked
by conventional detergent perfumes. It has been found
that the maximum level of unethoxylated alcohol that can
be tolerated in the ethoxylated alcohol component is 1
by weight. More preferably the une~hoxylated alcohol
level ill not more than 0.7~ and most preferably is less
than I by weight of the ethoxylated alcohol component.
Distillation under vacuum is employed to remove the
undesired material and this also removes a portion of the
monoethoxylate fraction, thereby increasing the E of
a
the remaining material. In preferred embodiments of the
invention the level of monoethoxylate is not more Han
s% by weight of toe ethoxylated alcohol.
The level ox usage of the ethoxylated alcohol
component in compositions of the invention is from 1 to
, .

1;;~28S~
- 16
I by weight, more preferably from I Jo I Betty.
Liquid dish washing detergent compositions in accordance
with the invention and incorporating from I to 4% by
weight of a C -C alcohol condensed with an average of
9 11
6 0.5 moles ethylene oxide per mole of alcohol, the
alcohol ethoxylate containing 0.5~ by weight of
unethoxylated alcohol, display chill points <0C and
enhanced seducing and mileage performance relative to
prior art compositions.
A highly preferred ingredient of the composition
according to the invention is a suds-promoting agent
present at a level of from 2% to I by weight of the
composition, preferably from 3% to 6% and most prefer-
ably 3%-4%-
lo The suds-promoting agent can ye any of C C
16
moo- and disc -C alkanolamide, and tertiary amine
oxides containing a C -C alkyd group.
Examples of the alkanolamides are coconut alkyd
monoethanolamide, coconut alkyd diethanolamides and
palm kernel and coconutalkyl moo and do isopropanol
Amadeus The palm kernel or coconut alkyd residue may
either ye Whole cut', including the C and C fractions
I 16
or may the so-called narrow cut' C -C reaction
12 14
Synthetic sources ox the C -C alkyd group can also be
, Jo
Jo .

8~2~L
- 17 -
used.
Amine oxides useful in the present invention have
one alkyd or hydroxyalkyl moiety of 8 to 18 carbon atoms,
preferably 8 to 16 carbon atoms, and two moieties
selected from alkyd groups and hydroxyalkyl groups con-
twining 1 to 3 carbon atoms. Examples of such materials
include dimethyloctyl~mine oxide, diethyldecylamine
oxide, bis-(2-hydroxyethyl~ dodecylamine oxide, methyl-
ethylhexadecylamine oxide, and dimethyl-~-hydroxyocta-
decylamine oxide.
A highly preread example of the tertiary amine
oxide is a C -C alkyd dim ethyl amine oxide in which
12 14
the C -C alkyd group is derived from coconut oil.
I 14
The balance of the formula comprises a hydrotrope-
water system in which the hydrotrope may be urea, a C -C3
aliphatic alcohol, or a lower alkyd Bunsen ~ulphonate ox
mixtures of any of these. Normally a snugly hydrotrope
will be adequate to provide the required phase stability,
but compositions in accordance with the present invention
I preferably employ a mixture such as urea-alcohol-water or
alcohol-lower alkyd Bunsen sulphonate-water in order to
achieve the desired viscosity, and to remain twill and
easily purl. For compositions having an organic
active concentration less than about I by weight, the

~22~3~i2~
- 18 -
preferred alcoholic hydrotrope is ethanol which is
employed at from I to 10~ by weight of the composition,
preferably at from 4% to 8%, usually in admixture with
urea. Mixtures ox hydrotropes can, of course, be
employed for cost effectiveness reasons irrespective of
any stability/viscosity considerations.
Optional ingredients of the liquid detergent
compositions of the invention include pacifiers such
as ethylene jackal distrait, thickeners such as guard
gum, antibacterial agents such as glutaraldehyde and
"Bronnpol" RUM anti tarnish agents such as bent-
oxytriazole, heavy metal chelating agents such as ETDAor ETDMP, perfumes an dyes. The pi of the compositions
may be anywhere within the range 6-7.5 but as m~nufac-
lured the compositions normally haze a pi in the range
of 6.6-7.3 and are subjected to a final pi trimming
operation to obtain the desired finished product phi
For colored products the pi preferably lies in the
range 6.5-6.9 in order to maintain color stability.
2 a The technique of manufacture of the compositions
is not thought to be critical and the composition can
be made in a number of ways.
-or
Jo

~L2~3S~
-- 19 --
Thus, individual anionic surfactants can be m de
as aqueous solutions of alkali metal ox ammonium salts
which are then mixed together with the suds booster and
with the hydrotype, following which any magnesium ion
can be introduced as water soluble salt such a the
chloride or sulfite. The ethoxylated non ionic surface
lent and any optional minor ingredients are then added
at the same time as the pi and viscosity are adjusted.
This method has the advantage ox utilizing conventional
techniques and equipment but does result in the intro-
diction of additional chloride or sulfite ions which
increase the chill point temperature (the temperature
at which inorganic salts precipitate as crystals in the
liquid).
An alternative method is to mix on alcohol and
alcohol ethoxylate together and carry out a single
sulphation and neutralization. For this, the alcohol
and alcohol ethoxylate should be mixed in a wright ratio
lying in the range 4~3 TV 1:6. Sulphation can wake place
by means of any of the conventional sulfating agents
such as e.g. Selfware trioxides or chlorosulphonic acid,
Neutralization of the alkyd ether sulfuric acid and the
alkyd sulfuric acid is curried out with the appropriate
alkali or with a magnesium oxide or hydroxide slurry
r

~%~
- 20 -
which avoids the addition ox chloride or sulfite ions.
In preferred executions of this technique in which
magnesium hydroxide slurry is employed, it is convenient
to use a mixture ox these acids, as the magnesium salt
of the alkyd ether sulfuric acid has relatively greater
aqueous volubility than the alkyd sulfuric acid coupon-
en. The suds booster is then dissolved in this heel
of alkyd sulfite and alkyd ether sulfite active.
The separately neutralized alkyd Bunsen sulphonate
salt, and the neutralized alkyd and alkyd ether sulfite
salts containing the suds booster and hydrotrope are then
added to the final mixing tank and the exulted
non ionic surfactant and any optional ingredients added
before the pi is adjusted as above.
Preferred compositions in accordance with the
invention-are clear simple phase liquids, but the
invention also embraces opaque products containing
dispersed phases provided that such products are
physically stable it do not separate) on storage.
The invention is illustrate in the following non-
limitative examples in which all parts and percentages
are by weight unless otherwise specified.
I,

SLY
- 21 -
EXAMPLE 1
The following compositions were prepared
A B C D E
Ammonium C linear
11.8
alkyd Bunsen sulphonate 14.2 14.214.2 14~2 14.2
Ammonia C alkyd
12-13
(HO) 6ulphate 10.4 10.410.4 10.410.4
Magnesium C C
12 13
alkyd sulfite I 8.68.6 I 8.6
Primary Alcohol - 3.51 3.52 3,53 3,54
ethoxylate
Coconut Monoethanolamide 4.0 4.0 4.0 4.0 4.0
Ethanol 9.1 9.1~.1 9.1 9~1
Water _ _ to loo
It Dobanol" RUM ale
predominately linear C C alcohol lend
9 11
containing an average of 5 ethylene oxide units per
mole of alcohol, supplied by Shell International Ltd.
and 'topped' to reduce the level of unethoxylated
C C alcohol Jo I by weight of the ethoxylate,
11
thereby increasing the average degree of ~thoxylation
to increasing the average degree of ethoxylat.ion to
approximately 6.
,. . .

- 22 - I
2 "Dobanol" (RUM) EYE 5
A predominantly linear Cg-Cll alcohol blend containing
an average of 2.5 ethylene oxide units per mole ox
alcohol.
3 "Dobanol" (RUM) EYE 5
A predominantly linear C12-C13 alcohol blend containing
an average ox 6.5 ethylene oxide units per mole of
alcohol.
4 "Dobanol" (RUM) EYE
A predominantly linear C14-C15 alcohol blend containing
an average of 7 ethylene oxide units per mole of
alcohol.
In the preparation of Composition A, a mix use of
alcohol and alcohol ethoxylate was sulfated using
Syria sulphation, and was then neutralized in an
alcoholic ammonium hydroxide solution to which magnesium
hydroxide had been added in an amount corresponding to
half the molar quantity of alkyd sulfite present A
separate sulphonation of the alkyd Bunsen was employed
to produce alkyd Bunsen .sulphonic acid which was added
to the alkaline 501ution of the other active and
Jo

~;~28~
- 23 -
neutralized with the excess ammonia to pal 7. The
monoethanolamide was then added before final pi trimming
to pi 6.8. The chill point of Composition A was -5C.
Compositions B-E were prepared in a similar manner
except that the ethoxylated non ionic surfactant was
added during the final pi trimming operation.
The chill point of the various compositions was
measured and each composition way assessed for solution
odor. A comparison of the suds mileage of the come
positions under identical test conditions was alto made using the mechanical seducing test method described below
under the following test conditions
Product Concentration 0.12%
Water Temperature 47~C
Water Hardness OH and 18H
Soil : Cake Mix Mixed free fatty acids OF
The Cake Mix is l'McDougall's Sponge Mix" (trademark)
The free fatty acids comprise 2 parts oLeic acid
2 parts linol0ic acid
1 part Starkey acid
2.5 parts palmetto acid
367 parts corn oil
to jive 2% MFFA mixture.
The method uses 4 cylinder of length 30 cm and

22~
- I -
diameter 10 cm fixed side by side, and rotatable at a
speed of 24 rum about a central axis. Each cylinder is
charted with 500 mls of product solution at a concern
traction of OWE% and a temperature of 45~C. The outer
two cylinders are used for one of the products being
compared and the inner two for the other product.
The cylinders are rotated for 2 minutes, stopped,
the initial suds are measured and a soil load is then
added. The grease soil comprises a mixture of fatty
acids in a cooking oil base and 1 ml of this mixture
(MFFA) is added to each cylinder. All of the paxticu-
late soil is also added at this stage. After 1 minute
the cylinders are restarted and allowed to rotate for 1
minute. The suds height is noted and 1 ml of the 2%
MFFA is added to each cylinder. After 1 minute the
cylinders are restarted. This process continues until
the suds height in the cylinder is lower than 0.5 cam
Product A is designated as the control and suds
mileage iguxes are calculated for the other product
versus the 'control' product on the following basis.
mileage of test product
= number of soil additions to test product solution
to reduce suds height to 0~5 cm x 100
r ox sardines to control product
reduce suds height to 0.5 cm
The results of the chill point measurements and
Jo

2~35~
- 25 -
odor assessments and the mileage comparisons using
Composition A as 100% were as follows:
Composition Mileage Chill Point Odor Type
2H 18H C
B 114 120 -5 Bland
C 113 100 ~24 Strong fatty
alcohol note
D 100 100 -1.5 Fatty alcohol
note
E 91 I -4 Fatty alcohol
note
It can be seen that only Composition B showed the
combination of a consistent mileage advantage in both
hard and soft water, an acceptable chill point and an
acceptable odor.
.,

Dessin représentatif

Désolé, le dessin représentatif concernant le document de brevet no 1228521 est introuvable.

États administratifs

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.

Veuillez noter que les événements débutant par « Inactive : » se réfèrent à des événements qui ne sont plus utilisés dans notre nouvelle solution interne.

Pour une meilleure compréhension de l'état de la demande ou brevet qui figure sur cette page, la rubrique Mise en garde , et les descriptions de Brevet , Historique d'événement , Taxes périodiques et Historique des paiements devraient être consultées.

Historique d'événement

Description Date
Inactive : CIB de MCD 2006-03-11
Inactive : CIB de MCD 2006-03-11
Inactive : CIB de MCD 2006-03-11
Inactive : CIB de MCD 2006-03-11
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 2004-10-27
Accordé par délivrance 1987-10-27

Historique d'abandonnement

Il n'y a pas d'historique d'abandonnement

Titulaires au dossier

Les titulaires actuels et antérieures au dossier sont affichés en ordre alphabétique.

Titulaires actuels au dossier
THE PROCTER & GAMBLE COMPANY
Titulaires antérieures au dossier
JOHN R. LAWSON
RONALD E. ATKINSON
STEPHEN J. WILMSHURST
Les propriétaires antérieurs qui ne figurent pas dans la liste des « Propriétaires au dossier » apparaîtront dans d'autres documents au dossier.
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Revendications 1993-09-26 2 43
Abrégé 1993-09-26 1 11
Dessins 1993-09-26 1 14
Description 1993-09-26 25 773