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Sommaire du brevet 1064360 

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L'apparition de différences dans le texte et l'image des Revendications et de l'Abrégé dépend du moment auquel le document est publié. Les textes des Revendications et de l'Abrégé sont affichés :

  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Brevet: (11) CA 1064360
(21) Numéro de la demande: 1064360
(54) Titre français: DETERSIF ET METHODE DE PRODUCTION
(54) Titre anglais: DETERGENT COMPOSITIONS AND THE PRODUCTION THEREOF
Statut: Durée expirée - au-delà du délai suivant l'octroi
Données bibliographiques
(51) Classification internationale des brevets (CIB):
  • C11D 1/72 (2006.01)
  • C11D 1/52 (2006.01)
  • C11D 3/06 (2006.01)
  • C11D 3/075 (2006.01)
  • C11D 10/04 (2006.01)
(72) Inventeurs :
  • BROUWER, HENDRIK W.
  • CLARKE, DAVID E.
  • NIEMANTSVERDRIET, ROBERT E.
  • TUNE, JOHN B.
(73) Titulaires :
  • UNILEVER LIMITED
(71) Demandeurs :
  • UNILEVER LIMITED (Royaume-Uni)
(74) Agent:
(74) Co-agent:
(45) Délivré: 1979-10-16
(22) Date de dépôt:
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: S.O.

Abrégés

Abrégé anglais


ABSTRACT
A heavy duty fabric washing powder having detergency
equivalent to products of higher phosphate content is
based on 5-50% of an ethoxylated alcohol as the
predominant detergent active compound, 10-30% by weight
of a water soluble soap and 10-40% by weight of sodium
tripolyphosphate. Particularly preferred components
contain C12-15 alcohols ethoxylated with from 4 to 12
moles of ethylene oxide per mole of alcohol, from about
20 to about 30% by weight of sodium tripolyphosphate
and from about 8 to 15% of soap. Processes for
making the powders are also described.

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 heavy duty fabric washing powder comprising a
non-soap detergent, a water-soluble soap and sodium
tripolyphosphate wherein
(a) the non-soap detergent consists essentially
of a nonionic surfactant formed by ethoxyla-
tion of a mixture of C12-15 primary alcohols
with from about 4 to about 12 moles of -
ethylene oxide per mole of alcohol and is
present in an amount of from about 5 to 50%
by weight
(b) the water soluble soap is present in an
amount of from about 10-30% by weight
and (c) the sodium tripolyphosphate is present in
an amount of from about 10-40% by weight
the balance being conventional components of fabric
washing powders.
2. A heavy duty fabric washing powder according to
Claim 1 wherein the water-soluble soap is present in
an amount of from about 15-25% by weight.
3. A heavy duty fabric washing powder according to
Claim 2 wherein the water-soluble soap is present in an
amount of from about 10-20% by weight.
27

4. A heavy duty fabric washing powder according to
Claim 3 wherein the water-soluble soap comprises a
mixture of tallow soap and coconut oil soap in the
ratio 3:1 to 1:2.
5. A heavy duty fabric washing powder according to
Claim 4 wherein the water-soluble soap comprises a
hardened rape seed oil soap.
6. A heavy duty fabric washing powder according to
Claim 5 wherein the water-soluble soap is a mixture
comprising
from about 45-60% by weight of tallow soap
from about 20-30% by weight of cocnut oil soap
from about 15-25% by weight of hardened rape seed
oil soap.
7. A heavy duty fabric washing powder according to
Claim 1 wherein the nonionic surfactant consists of a
mixture of long and short chain ethoxylates in which the
average degree of ethoxylation is from 6 to 9 moles of
ethylene oxide per mole of alcohol.
8. A heavy duty fabric washing powder comprising a non-
soap detergent, a water soluble soap and sodium tripoly-
phosphate wherein
28

(a) the non-soap detergent consists essentially of
a nonionic surfactant made by ethoxylation of a
mixture of C12-15 primary alcohols with from
about 6 to 9 moles of ethylene oxide per mole
of alcohol and is present in an amount of from
about 5 to 15% by weight
(b) the water soluble soap is a mixture comprising
from about 45-60% by weight of tallow soap
from about 20-30% by weight of coconut oil soap
from about 15-25% by weight of hardened rape
seed oil soap
and is present in an amount of about 15-20% by
weight
and (c) the sodium tripolyphosphate is present in an
amount of from about 20-25% by weight
the balance being conventional components of fabric
washing powders.
29

Description

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


C778
10643~0
The invention relates to detergent compositions which
are adapted for fabric washing, and in particular to such
compositions containing phosphate detergency builders.
The most commonly used detergency builders are the
condensed phosphates, especially sodium tripolyphosphate,
but it has been suggested that the use of these phosphate
detergency builders can contribute to eutrophication problemsO
There have been very many suggestions for alternative,
mainly organic, materials to be used as detergency builders
instead of the condensed phosphates, but most of these
materials tend to be unsatisfaotory for one reason or
another, for e~ample they are less e~ficient or biologically
unacceptable, or they may simply be too e~pensive.
,,.
- It has also been proposed to mitigate the problems of
eutrophication by using dec~eased levels of condensed
phosphate detergency builders, with or without the presence
oi other detergenoy builders, but ~ew oi these proposals
have been aoceptable. ~hus, when reduced levels oi sodlum
tripolyphosphate are used without supplemental builders,
there oan be oonsiderable problems when using the compositions
in hard water if there is insuf~icient phosphate to
! sequester all the caloium ions present, as this oauses
the precipitation of insoluble calcium phosphate salts
! which can accumulate on the washed fabrics. When a condensed
1 ., .
,
~ _ 2
L~, .. . . . , - . - . ~ .
- . , . . ~ - ~.

C778
1064360
phosphate builder is used with other types oi detergency
builders, then they tend to interact and o~ten the
iormer prevents the latter irom iunctioning efiectively,
especially in the case oi other detergency builders
which act by precipitating the calcium salt, ior example
sodi~m carbonate.
., :
We have now discovered that certain mixtures o~
- sodium tripolyphosphate and soap iunction as eiiicient
detergenoy builders and that these materials, when combined
with a nonionic suriactant, produce a heavy duty iabric
washing powd~r having good detergency and producing
pleasant aiter wash ieel characteristics.
''
According to the present invention there is provided
a heavy duty iabric washing powder comprising a non-soap
detergent, a water-soluble soap and sodium tripolyphosphate.
wherein
ta) the non-soap detergent consists essentially oi
an alkoxylated aloohol nonionic suriactant
,.~
which is present in an amount oi i~om 5 to S0~0
by weight
(b) the water-soluble soap is present in an amount
' oi irom 10_30% by weight, and
t (c) the sodium tripolyphosphate is present in an
amount oi irom 10_40% by weight,
.

C778
` ~064360
the balance being conventional components oi iabric
washing powders. By choosing the amounts oi the sodium
tripolyphosphate and soap to be in the ranges stated
it is possible to iormulate efiective detergent
compositions containing lower phosphorus levels than
conventional detergent compositions oi comparable
periormance. Insofar as these two materials iunction
normally in dii~erent ways, ie sodium tripolyphosphate
acting as a seque~trant detergency builder and the soap
iunctioning as a precipitant builder, it is somewhat
surprising that a mixture oi the materials iunctions ~o
eiiectively. In particular, the tendency ior sodium
tripolyphosphate to cause inorganic depositlo~ on washed
iabrics when it is used at low levels in detergent compositions
is aecreased in the presence of the soap. Moreover, the
sodium tripolyphosphate does not appear to inhibit the
detergency building action oi the ~oaps, as it does with
many other detergency builders, and any soap not preoipitated
; as the calcium salt, eg. when the compositions are used
; 20 in soit water or at higher product concentrations, can
function as a debergent active compound,so increasing the
detergency oi the compositionsO
The soaps used are the sodium, or less desirably
,,'! potassium~ salts oi C8-C22 iatty acids, especially
~"
, 4
.
.. ~ .: . . . . .
. , -
.

C778
1064360
natural fatty acids derived from nut oils, such as
; coconut oil or palm kernel oil, or tallow class fats,
such as beef and mùtton tallows, palm oil, lard, some
vegetable butters and castor oil. The tallow class
fats may be hardened, if desired, so as to decrease the
content oi unsaturated acids such as oleic acid and
linoleic acid, and this is particularly beneficial if
some more highly polyunsaturated oils such as soybean oil
are de~ired to be used as tallow cla~s fats at
~ 10 signiricant levels.
:~'. . .
It is preierred to use mixtures oi soaps derived
from tallow class iats (C14-C20, mainly C18 iatty acids) and
soaps from nut oils, which are 30aps oi predominantly
- C10-Cl4, mainly C12 iat$y acids, of which normally at
least about 75~ are saturated iatty acids; again the nut
oils may be hardened ii desired. Such mixtures tend
to have better solubilities than tallow soap alone,
ooupled with sufiiciently low caloium soap solubilities ior
satisfaotory detergenoy bullding, and suiiioiently low
oritioal mioelle oonoentrations approaching that oi tallow
~oap alone, to enable any exoess of the soap to iunction
as an extra detergent active component. ~he preierred
mixtures are irom about 9 1 to 1:9, for example about
5~1 to 1:5 and espeoially about 3:1 to 1:2 parts by weight
'~! 25 of tallow ola^ss soap to nut oil olass soap, respectively.
'' ' ' . ', : ' ,: , : ,, ' . .. ', ,: ~ ,

C778
1064360
In general, higher proportions oi tallow class soaps in
such mi~tures give better detergency building properties,
whilst higher proportions oi nut oil class soaps
give better solubility properties.
In addition to ~e tallow class soap, and any optional
nut oil soap, some soap oi longer carbon chain length
can be used ii desired, e~pecially C20-C24 ~oaps, eg.
rapeseed soaps, which are useiul ior lather-depressing
properties. A particularly preierred mixture oi soaps
is one comprising i~om 45-60% by weight oi soap oi tallow
class iats, irom 20-30% by weight of coconut oil soap
and irom 15_25~o by weight of hardened rape seed oil soap.
When incorporated into a powder at a level oi 15~ by
weight this has been iound to enable a powder having
desirable powder properties to be produced. Soaps
- oi synthetic iatty acids may also be used. In distinction
j from naturally-occurring or derived iatty acids which have
linear carbon chain lengths of even numbers, synthetic
iatty acids can have both odd and even numbers ard they
can be oi both linear and branched-ohain iorm. Synthetic
iatty acids oi carbon chain length predominantly C14-C~0,
which are preierably at least about 40~ saturated and at least
about 75~ linear, can be used in partial or iull replacement
~ oi natural tallow class soaps, and synthetic iatty acids
.
:~.
:: .: ,- i . .

C778
1064360
of carbon chain length predominantly C1O~C16, preferably
at least about 75~ saturated and at least about 50~ linear,
can be used in partial or iull replacement o~ natural nut
oil soaps. Ii any branched-chain ~atty acids are used they
are pre~erably c~ -alkyl, eg.~ -methyl branched, rather
than being more highly branched.
~ here have in the past been many suggestions ior
using sodium tripolypho3phate as a detergency builder
in detergent compositions comprising soap as a detergent
active material. For example in so-called ternary active
mi~tures ior use in low sudsing compositions, it is
usual to have pre 9 ent some 5 oap, at a low level o~ up to
about 8~ by weight together with very low levels o~
;' a~ionic and nonionic surfactantsO Normally such soaps
are tallow soaps or soaps o~ longer~chain length ~atty
acids. Also, detergent compositions based on soap have
contained low amounts o~ sodium tripolyphosphate. However,
to the Applioants' knowledge~ it has not been proposed
hitherto to u9e the speciiio detergenoy builder mi~tures
of sodium trlpolyphosphate and soap in the proportions as
set out above ~or use in iabrio washing detargent compositions
aocording to the present invention.
~,3,
The ratio o~ the sodium tripolyphsphate to the soap
. i .

C778
1()64360
in the detergent composition is generally ~rom about
4:1 about 1:3 parts by weight, preferably about 3:1 -
to about 1:3 parts by weight, and especially from about
2:1 to about 4:3 parts by weight. The total amount
o~ sodium tripolyphosphate plus soap is generally irom
about 20~o to about 70~0, preierably about 25% to about
60~, and especially about 25~ to about 45~, by weight
o~ the composition. Lower levels of sodium tripolyphosphate
and soap tend to be mare desirable ior compositions intended
for use either at higher product concentrations or in so~t
water.
.
- It will be appreciated that the amount oi sodium
tripolyphosphate is ohosen according to the overall
phosphate detergency builder level which is desired in the
.,
detergent compositions or according to the ma~imum
permitted phosphorus content. An amount of sodium
:~;
tripolyphosphate is normally used within the range
of from about 15~ to about 3Syo by weight of the composition.
However, ii the compositions of the invention are intended
to be used with decreased phosphate levels for
environmental reasons, then lower amounts o~ about 10%
to about 25%, or preierably about 10% to about 25%, or
preierably about 10~ to about 20~, are used. A level
o~ 20~ sodium tripolyphosphate by weight o~ composition
is equivalent to only about S~ by weight of phosphorus, and
- 8
. - ~ . ...... -. ... ., , , . ~ - -............ . ...... . -
:.- . , ~ : ........ . - . . . .. . .

C~78
106436~
it is a feature o~ the invention that detergent compositions
can be prepared with these low phosphate levels and yet
having particularly good detergent properties.
The minimum level of 30ap which should be present
is 10% by weight o$ the composition, and the maximum level ~-
is 40~ by weight, pre~erably les~ than about 25yo by
weight o* the composition, and especially about lO~o to about
20~ by weight.
The amounts o~ the sodium tripolyphosphate and soap
$or use in a particul'ar detergent composition are selected
according to ths expected washing conditions. We have
iound for example that amounts o$ 20yO and 15~o~ respectively,
give optimum per$ormance (at 5% phosphorus level) ~or
compositions intended for use at relatively high product
concentrations, ie. about 0.3yo~tO about 0.8% by weight,
as is common practice in Europe, especially in $ront-
loading automatic''''washing machines. But in oompositions
intended for use at relatively low product concentrations,
i.e. about 0.1~ to 0.3~, as is common practice under
North American washing conditions, espeoially in toploading
automatic washing machines, we have found that amounts
Or about 24yo sodium tripolyphosphate and about 15% soap give
optimum per$ormance at 6~ pho~phorus level, or as little
as 16yo sodium tripolyphosphate and as much as 30yo soap i~
;~ _ g _ ,
'
; ,
.
. : :, . -,
.

- C778
1064360
a lower 4~0 phosphorus level is required.
The detergent compositions o~ the invention necessarily
include an amount of a nonionic surfactant. Many such
detergent active compounds are commercially available and
are fully described in the literature, ~or example in
"Sur~ace Active Agents and Detergents", ~olumes I and II,
by Schwartz, Perry and Berch.
The nonionic sur~actant used in the compositions o~ this
invention will be alkoxylated alcohols.
The alcohols used can be primary or secondary alcohols
containing straight or branched carbon chains. The number
o~ carbon atoms will generally be ~rom about 7 to about 24,
preierably ~rom about 8 to 18 and most pre~erably from
about 12 to 15. These alcohols may ~be the so-called
synthetic alcohols made by the well known Ziegler or Oxo
processes7 or the so-called "natural alcohols~.
, , .
The alkoxylation reaction will be carried out by
conventional means, generally using ethylene oxide
or propylene oxide. The degree of ethoxylation can
vary widely both ~rom one hydrophobe to the other and
; even when using a single hydrophobe. Thus ethylene oxide
chains containing as few as 1 and more than 20 ethylene
; oxide units are quite o~ten ~ound in nonionic sur~actants
and will be applicable here.
The choice o~ carbon chain length o~ the hydrophobe
,., 10
1 , . . . . . . ' ' .. . , . . . - . ' ' . . ' ' .
.~ . .. . . .
- , . .
: . . - . ~ . ,
- , -: - ~ . . : .

C~78
1064360
~ ~.
alkoxy chain is largely determined by the detergent
properties required o~ the molecule. The relationship
between the chain length o~ the hydrophobic part o~
the molecule and that o~ the hydrophilic part can
be expressed numerically as the hydrophilic lipophilic
balance ~HLB). A rough and ready way oi determining t~e
HLB is to use the e~pres 9 ion
- - ~LB_wt percenta~e o~ ethylene oxide
Nonionic surfactants which are suitable for use
in heavy duty ~abric washing powders generally have
an HLB in the range 9 to 13, although HLBs outside
this range are not excluded.
.. . .
An additional iaGtor in the choice of nonionic
, surfactant is that alcohols containing both short carbon and
; 15 short ethoxylate chain lengths are relatively low boiling
and can volatilise under the conditions prevailing
in a spray drying tower. Hence aloohols containing
les9 than about 8 oarbon atoms will not normally be chosen
unless their ethoxy chains contain at least about 8
ethylene oxide units ~or ~ear o~ exceeding emission
regulations unless it is p~oposed to incorporats these
materials into the powder by a route other than spray-
drying.
. ..
,
,~ - 11 _
)!
: . .," ' '.: . '
; , ' ''. . :: . ~ ~ ' .

C778
1064360
Pre~erred alcohol ethoxylates for use in this
invention are derived from the following series~
Tergitols (Trade Mark) which are a series of
ethoxylates oi secondary alcohols sold by the Union
Carbide Corporation, especially Tergitol 15_S_7,
15_S_9, 15-S-12 and 15_S-15 which are ethoxylates of
a mi2ture oi Cli-15 alcohols and ~ergitols 45_S_7,
45_S-9, 45-S-12 and 45-S-15 which are ethoxylates oi a
,~ mi~ture oi C14 and C15 alcohols, the degree o~ ethoxylation
iO being shown by the postscript.
Ethoxylates of primary alcohols made by the Oxo
process and containing about 20% oi alpha branched material
sold by Shell Chemlcals Ltd. tDobanols Trade Mark) and
Shell Chemicals Inc. (Neodols ~rade Mark), especially Dobanol ard
.;,. . . .
and Neodol 25-7, 25-9, 25-12 a~d 25-15 which are ethoxylates
oi a mixture oi C12-C15 alcohols and Dobanol 45-7, 45_9,
25-12 and 25-15 which are ethoxylates of a mixture
oi C14_15 alcohols~
.
Lutensols (Trade Mark) which are a series of C13 15
alcohols oi ethoxylates prepared by the 'OX0' process ~rom
; an oleiine produced by the polymerisation of ethylene ,
manufactured by Badische Anilin und Soda Fabrik GmbH,
O .
.
; _ 12 - ~

C778
10~;4360
especially Lutensol A0 8 an~ 12.
Ukanils (Trade Mark) which are a series o~ ethoxylates
oi Oxo alcohols containing about 25% 0~ alpha methyl
branched and about 10~ oi ethyl branched material.
Acropols (~rade Mark) manuiactured by Ugine
Euhlma~ et Cie, especially Acropol 35-7, 35-9, 35-11,
and 35_15 which are derived ~rom a mixture oi C13-C15
alcohols~.
. . -
Synperonics (Trade Mark), a series o~ ethoxylates oi
aloohols containing 45-55~ oi alkyl branching, mostly
methyl branching, sold by Imperial Chemical Industries
Limited, especially those based on a C13 15 mixture oi
~ alcohols and etho*ylated to 7, 9, 11 and 15 units oi ethylene
't. oxide.
Ethoxylates oi primary Ziegler aloohols sold as
Aliols (Trade Mark) derived by oxidative polymerisation
, oi ethylene and manuiactured by Conooo-Condea,
^l especially Aliol 12/14-7, 12/14_9, 12/14-12, 12/14-15 and
Aliol 14112-7, 14/12-9, 14~12-12, 141i2-15 which are
~ 20 ethoxylates oi mixtures oi C12 and C14 alcohols.
.~ . .
Ethoxylates oi primary Oxo alcohols a~out SOo/o branched,
- 13
, ~
. '.' ' ' : ' ' ~ ' ' :' . :'
. . : . ' ' ': ' , ' ., , : ,, '.

C778
-
106436()
mainly ~ methyl sometimes called Lials (Trade Mark)
produced from olefins manufactured by Liquichemica.
The required HLB can be achieved not only by
selecting the carbon chain length of the hydrophobe and
the length of the ethylene chain in a single or
substantially single material (because of the nature
of their process of production, all nonionic surfactants
which are spoken of as if they were single substances
are in fact mixtures~. It can also be achieved by
deliberately taking two "substances" of widely differing
HLBs and mixing them. This approach is described in our
British Patent Application 16641/76, in Netherlands
Patent Application No. 7,413,522 and in Netherlands
Patent Application No. 7,4Q6,0Q3. It is also possible
to obtain the required HLB by "stripping" some chain
lengths from a nonionic surfactant mixture as described
in US Patent No. 3,682,849.
Nonionic detergent active compounds have been
found to exhibit good detergency particularly with higher
levels of sodium tripolyphosphate, ie over about 20% by
weight and they are useful in facilitating soap scum
dispersion and inhibiting its deposition on washing machine
~; parts.
f
. -- 14 --

C778
1064360
.
.
'`.: `- - . .
. ..
Amounts oi amphoteric or zwitterionic detergent
active compou~ds can also be used in the compositions
S of the invention but this is not normally desired due
to their relatively high costO Ii any amphoteric
or zwitterionic detergent active compounds are used
they will generally be present in only small amounts.
; Eowever, some such zwitterionic or amphoteric compounds,
especially sulphobetaines such as hexadecyldimethlammonio-
propane sulphonate, have useiul soap scum dispersion
properties.
.''
The amount oi the non-soap detergent active compound
; or compounds used i9 generally in the range oi irom about
; lS 5~ to about S0~0, preieerably about 70~ to about 2S~,
by weight oi the oompositions, depending on the desired
-propertieb. Some oi the soap added can also act as a
detergent active ¢ompound in so-called "overbuilt"
circumstances, ie. at higher product conoentrations
:!, 20 or when using soit water, but the soap is not included
in the a~ount oi non-soap detergent compound. The ratio
o~ the total detergent compounds to the total of the
. . .
.' ! ~ ~ 15
' ' .
. _ _, . . _, .
', ., : ~ - , ' ' ,' ,' ~. ' . :', ' .', .

C778
~ 064360
amount oi sodium tripolyphosphate and soap should
generally be in the range of ~rom about 10:1 to 1:10,
especially.about 3:1 to 1:5, parts by weight.
Apart ~rom the non-soap detergent and detergency
builders, a ~abric washing powder o~ the invention
can contain any o~ the conventional additives in the
amounts in which such additives are normally employed
in such compositions. Examples oi these additiYes
include lather boosters such as alkanolamides, particularly
the monoethanolamides derived irom palm kernel ~atty
acids and coconut iatty acids, powder flow aids such as
silicas and aluminosilicates, lather depressants such
as phosphate esters, particularly the C12 18 mono alkyl
esters, anti-redoposition agents such as sodium
.
carboxymethylce1lulose, oxygen-releasing bleaching agents
such as sodium perborate and sodium percarbonate,
- per-acid bleach precursors, chlorine-releasing bleaching
agents such as trichloroisocyanuric acid and alkali metal
salts oi dichloroisocyanuric acid, ~abric soitening agents
such as c1ays oi the smeotite and illite types anti-ashing
aids, starches, soap scum dispersants, inorganic salts
sucb as sodium sulphate higher levels o~ which lead to
; improved powder properties, and, usually present in very
minor amounts, iluorescent agents, periumes, en~ymes such
as proteases and amylases, germicides and colourants. In
_ 16
:,;
.- , , . ., .: . . - . . .. . . - . -

~ C778
1064360 -
addition, it may be desirable to add slurry stabilisers
such as copolyethylene-maleic anhydride and copolyvinyl-
methylether-maleic anhydride, usually in salt iorm.
It i9 also possible to include in ~e detergent
compositions of the invention minor amounts, e.g.
not more than 25~ by weight, oi other detergency builders,
which may be either so-called precipitant builders
or sequestrant builders. ~his may be of particular
beneiit where it is desired to increase detergency
iO whilst using particularly low levels of the sodium
tripolyphosphate, so as to achieve particularly low
phosphorus contents in the detergent compositions.
Examples of such other debergency builders are amine
carboxylates such as sodium nitrilotriacetate, sodium
1~ carbonate and alumino-silicate builders such as those
desoribed in German Patent Applioations--2,412,83~ and
2,422,655 It may also be noted that some minor
amounts of sodium pyrophosphate and 90dium orthopho~phate
are normally formed by hydrolysis of sodiu~ tripolyphosphate
during spray drying processes to make detergent powders,
90 low levels of these other phosphate builders may be
present in the detergent compositions.
.
~l It is possible to include in the compositions an
.~i ; .
~,,~,., ,~ .
17
.. .
- , . , . .,, - ..
- , - ~ . .
, . - . . ~ , ,

- C778
1064360
amount o~ an alkali metal silicate, particularly sodium
ortho_, meta- or preierably neutral or alkaline silicate.
The presence oi such alkali metal silicate at levels oi
ior example about 5~ to about 15% by weight, is usually
advantageous in decreasing the corrosion oi metal
parts in washing machines, besides giving procei~sing
benefits and generally improved powder properties.
- In addition, the amount oi silicate can he used to some
extent to control the pH of the compositions which should
generally be within the range o~ about 9 to about 11, ~ -
preierably about 9.5 to about lO S, in aqueous solution
o~ the compo3itions at the recommended concentrationsO
A high p~, i.e. over about pH 10.5, tends to be more
e~iicient as regards detergency but it may be less
lS desirable ~or domestic saiety.
.~ '
The compositions may be produced by any oi the
techniques commonly employed in the manufa¢ture oi fabric
was~ing compositions, including particularly slurry
making and spray drying processes ~or the manu~acture oi
detergent powders. However, it has been iound that the
presenoe of appreciable levels oi soap in the detergent
slurries tends to give rise to problems in spray drying,
notably the production oi powders o~ low bulk density and
with high proportions oi gmall particles (~ines).
... .
~5 In a iurther~aspect oi the invention, it has been
,

C778
1064360
found beneficial to produce the detergent compositions
- by a slurry making and spray drying process in which
either none or only a proportion of the soap, preferably
not more than about 8~ by weight, is added to the slurry
s and ~11 or the remainder of the soap is post-dosed
to the spray dried powder in particulate ~orm, egO as
noodles, granules, pellets, ribbons, threads,
- flakes, small spheres or marumes. It may be beneiicial
in this case to add minor ingredients, for example
periumes, to the detergent compositions in the post-do3ed
soap particles. Such soap particles can be made by the
usual processes depending on the final shape and size
desired, and it is preierable to mill the soap thoroughly
before making the par~icles, as this tends to improve
their solubility, especially for particles with a
higher content oi tallow 90ap.
. . .
Alternatively, it is possible to spray dry two
separate slurries, either in the same or different spray
;~ drying towers, and then mig them to iorm the final
composition. In this case, one slurry preferably has all
the major ingredients in it but not more than about 8
by weight of soap, and the other slurry has a major
proportion o~ soap with other minor ingredients. The
term 1~spray drying" is used above to include processes in
~: ,
1 g
.
.~ . . . . .

C778
1064360
which detergent slurries are sprayed into relatively
hot gas, normally air, either in counter-current or
co-current processes and processes in which hotter
slurries are sprayed into relatively cool air,ie.
in so-called spray coolingor flash drying processes.
Conventional slurry and drying gas temperatures are
used in such spray drying processes for produc~g
the detergent compositions according to the invention.
.
Furthermore, it is po~sible to manuiacture the
powders by a process which involves ~orming a
slurry containing part o~ the nonionic sur~actant
and spray drying it, and then post-dosing the remainder
oi the nonionic suriactant. Such a process is particularly
appropriate when a b~end oi two nonionic sur~actants
is being used in the ~ormulation, since it is then
possible to incorporate the component which is least
volatile into the slurry and, for example, to spray
the more valatile component (which will probably be
a liquid) onto the resulting spray-dried powder.
Alternatlvely, the volatile component can be incorporated
into an ad~unct, ior example a noodle or a granule
and post-dosed into the spray-dried portion o~ the powder.
Processes oi the general type described above are also
described in US Patent Nos. 3,838,072 and 3,886,098 and
1. ~
` _ 20
.
:~ , . .. . ,, . . . . -. - .. - . . .. . .. . - - - . - .. ., -
; , . :- .. ~ , . . . , . . . . . . , - - .. .

C778
~064360
in Netherlands Patent Application Nos. 7,504,264,and
7,50~,797,
The inventlon is illustrated by the following
Examples in which parts and percentages are by weight
except where otherwise indicated.
EXAMPLE 1
' . ' .
- A spray dried det-ergent composition was prepared
to the following formulation:~0 by wei~ht
of F
In~redient Parts Composition'
C14-C15 alcoh~l - 1~ E0 9.0 7.8
Sodium tripolyphosphate ~16.0 13.4
Sodium alkaline silicate10.0 8.7
, Sodium carbonate 20.0 17.5
~ Sodium sulphate 6.0 5.2
" -, Sodium carboxymethylcellulose 0.4 0.3
; Water and fluoresoent agents 8.6 7,5
, 70.0
, .
~his was then admi~ed with 45 parts by weight of a
separately spray dried composition having the following
~.~ 20 formulation: '
,J-,
;l:
~ - 21
,.. ,,., ~ . , ,, . - .. ~ , , ,, - -

C778
1064360
by weight
o~ ~inished
~n~redientParts compositi~^~
Sodium soap (tallow:coconut,
74:26) 29. 29.7 25.8
Coconut iatty ethanolamide ~.6 1.4
-Sodium alkaline silicate600 5.3
Sodium ethylenediamine
- tetraacetate 0.2 0.2
Fluorescent agent 0.4 0.3
Noisture 7 1 6.1
: 45.0
, .
The resultant compositions were, respectively, ~ound to ~ -
compare favourably ~or detergency properties with commercially
available nonionic~ and anionic- based detergent compositions
containing 33~ of sodium tripolyphosphateO
EXA~PLE 2
" ~he procedure of Example 1 was repeated except that
instead o~ the 45 parts o~ the soap based spray dried
. 20 composition, 30 parts oi potassi~m tallow soap in
.~ noodle ~orm were added to the spray dried base powderO
.
EXAMPLE 3
3-~
! A detergent composition was prepared to the following
. . .
22
.

C778
1064360
iormulation:
~n~redient
Linear C12 15 OXO-alcohol - 12 EO
condensate 8.0
Sodium tripolyphosphate 3100
Sodium tallow soap 8.0
Sodium coconut soap 4.0
Sodium hardened rapeseed soap 3.0
Sodium alkaline silicate 6.0
. 10 Sodium carbo~ymethylcellulose 0.8
Water and minor additives (fluorescent
agents ? perfume, preservatives,
enzyme, stabilisers, etc.) 12.2
. Sodium perborate 27.0
,~, ..
~ 15 lOO.o
:i ~
,,
. The composition was prepared by slurry making and spray
drying techniques, except that 5~ oi the nonionic
oomponent, ie. the linear Ci2 15 OXO-alcohol - i2 EO
condensate and the periume (0.2~) were sprayed onto
1 20 the powder aiter spray drying, and the perborate and
enzyme granules (0,5~) were dry-mixed with the powder.
This detergent oomposition was iound to have good
.'; detergenoy properties in comparison with commercially
.~ - available detergent compositions oi similar phosphate
2S content.
~ .
. _ 23
: .... :. ~ : . : ,. . .
- ; , - . . . -

C778
1064360
EXAMPLE_4
The procedure of E~ample 3 was repeated with the
- following modi~ications.
The linear C12 15 OXO-alcohol - i2 EO condensate
S wa~ replaced by an 8 EO condensate o~ the same alcohol.
:
Nonionic surfactant was entirely absent from the spray-
dried slurry. One half (4~ by weight o~ the iinished
composi~ia~)was sprayed onto the spray-dried powder
produced from the slurry and the second hal~ was added
as an adjunct. The adjunct was formed by mixing the nonionic
suriactant with sodium perborate monohydrate.
J'
~ he resultant powder was equivalent in detergency
performance to the powder of E~ample 3 and had satis~actory
. powder properties.
- .,
., .
- 15 EXAMPLE S
.'. '
?`
;' The procedure of Example 4 was repeated with the
~,, following modifications.
One quarter of the linear C12 lS OXO alcohol 8 EO
~, condensate (2~ by weight oi the finished çomposition)
~ was replaced by the 12 EO condensate of the same alcohol.
. .
~ : .
~ 24

C778
1064360
This 12 E0 condensate was incorporated into the slurry
as in Example 3 and spray_dried with the remainder
o~ the components. 2~ by weight o~ the iinished
composition oi the 8 E0 condensate was sprayed onto
S the spray-dried powder and the remainder was added as
an adjunct as in Example 4.
EXAMPLE_6
.. .
The procedure o~ Example 3 was repeated, e~cept that only
2~o (based on the weight of othar iini~hed components)
oi the alcohol_ethylene oxide condensate was incorporated
into the slurry, the remaining 6~ being ~ormed into
an adjunct with sodium perborate monohydrate and
dosed into the spray-dried powder as in Example 4.
The powders produced in Example~ 5 and 6 had
equi~alent performance and properties to the powder
of Example 4.
EXAMPLE 7
. _ .
~ by wei~ht
Luten901 A0 12 ta mixture of C13 15 aloohol9 with 8
less than 20~ branching, ethoxylated with
12 moles of ethylene oxide ^per mole of
alcohol).
Hardened Tallow soap 15
: . "`"' '
. _ 25
" ''' ' '-: ' ' . ' ' , ' ' '
. .
.. . ~ . . .

C778
1064360
~ by weight
.
Sodium tripolyphosphate 17
Trisodium orthophosphate ~ . 8
Alkaline sodium silicate 10
Sodium perborate tetrahydrate 27
Moisture and minor ingredientsto 100
:
EXAMPLE 8
. ' '
by weight
Linear C12 15 OX0 alcohol 8 F0 condensate 8
Eardened tallow soap 15
Sodium tripolyphosphate 23
~i, .
~ Alkaline sodium silicate 10
.'~ Sodium perborate tetrahydrate 27
.:;I Moisture and mi~or ingredientsto 100
. . .
.~ .
. ~ . . .
1; .
... .
.... .
.~ .
',1~. . '
. ,.
- 26

Dessin représentatif

Désolé, le dessin représentatif concernant le document de brevet no 1064360 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 : Périmé (brevet sous l'ancienne loi) date de péremption possible la plus tardive 1996-10-16
Accordé par délivrance 1979-10-16

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Titulaires au dossier

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

Titulaires actuels au dossier
UNILEVER LIMITED
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DAVID E. CLARKE
HENDRIK W. BROUWER
JOHN B. TUNE
ROBERT E. NIEMANTSVERDRIET
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Description du
Document 
Date
(aaaa-mm-jj) 
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Revendications 1994-04-27 3 94
Abrégé 1994-04-27 1 21
Dessins 1994-04-27 1 9
Description 1994-04-27 25 899