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Sommaire du brevet 1110516 

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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 1110516
(21) Numéro de la demande: 1110516
(54) Titre français: DETERGENTS
(54) Titre anglais: DETERGENT COMPOSITIONS
Statut: Durée expirée - après l'octroi
Données bibliographiques
(51) Classification internationale des brevets (CIB):
  • C11D 1/00 (2006.01)
  • C11D 3/06 (2006.01)
  • C11D 3/10 (2006.01)
(72) Inventeurs :
  • CLARKE, DAVID E. (Royaume-Uni)
  • DAVIES, JAMES F. (Royaume-Uni)
  • TUNE, JOHN B. (Royaume-Uni)
(73) Titulaires :
  • UNILEVER LIMITED
(71) Demandeurs :
  • UNILEVER LIMITED (Royaume-Uni)
(74) Agent: SMART & BIGGAR LP
(74) Co-agent:
(45) Délivré: 1981-10-13
(22) Date de dépôt: 1978-11-07
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
46841/77 (Royaume-Uni) 1977-11-10

Abrégés

Abrégé anglais


- 1 -
ABSTRACT OF THE DISCLOSURE
A particulate alkaline detergent composition is made
from over 15% to 50% of a partially neutralised alkali metal
orthophosphate salt, from over 20% to 50% of an alkali metal
carbonate salt and from 5% to 40% of a synthetic detergent
surfactant. The compositions have good detergency
properties in relation to the phosphorus content, especially
at low phosphorus levels with over 15% to 30% of orthophos-
phate salt, and the use of partially neutralised alkali metal
orthophosphate avoids excessively high alkalinity.

Revendications

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


- 21 -
THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A particulate alkaline detergent composition produced
from over about 15% to about 50% of a partially neutralized
alkali metal orthophosphate salt, from over about 20% to
about 50% of an alkali metal carbonate salt, and from about
5% to about 40% of a synthetic detergent surfactant, all
these percentages being by weight of the total detergent
composition.
2. A composition according to claim 1, wherein the
partially neutralised alkali metal orthophosphate salt is
disodium monohydrogen orthophosphate or a mixture thereof
with monosodium dihydrogen orthophosphate.
3. A composition according to claim 2, wherein the
partially neutralised alkali metal orthophosphate salt is a
mixture of disodium and monosodium hydrogen orthophosphates
in the molar ratio of about 1:3 to 2:3 parts, respectively.
4. A composition according to claim 1 comprising not more
than about 30% by weight of the partially neutralised
alkali metal orthophosphate salt.
5. A composition according to claim 4 comprising about 20%
to about 25% by weight of the orthophosphate salt.

- 22 -
6. A composition according to claim 1 comprising from about
30% to about 50% of the orthophosphate salt.
7. A composition according to claim 1, wherein the alkali
metal carbonate salt is sodium carbonate, sodium bicarbonate
or a mixture thereof.
8. A composition according to claim 1, wherein the amount
of alkali metal carbonate salt is from about 25% to about
45% by weight of the composition.
9. A composition according to claim 8 comprising from about
20% to about 30% of the alkali metal carbonate salt.
10. A composition according to claim 1 comprising from about
5% to about 25% of a nonionic detergent surfactant.
11. A composition according to claim 1 comprising from about
0. 5% to about 25% by weight of soap.
12. A composition according to claim 1 comprising from about
10% to about 40% by weight of sodium percarbonate.
13. A composition according to claim 1 comprising not more
than about 10% by weight of sodium silicate.

- 23 -
14. A composition according to claim 1 comprising from about
0.05% to about 5% by weight of an antideposition agent.
15. A composition according to claim 14, wherein the anti-
deposition agent is a polymeric aliphatic carboxylate.
16. A composition according to claim 15, wherein the
polymeric aliphatic carboxylate is an alkali metal or
ammonium salt of a homo- or co-polymer of acrylic acid or a
substituted acrylic acid.
17. A composition according to claim 1 comprising not more
than about 5% by weight of alkali metal tripolyphosphate or
pyrophosphate.
18. A composition according to claim 1 having a pH in 0.1%
aqueous solution of from about 9.25 to about 10.5.

Description

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


- 1 - cC.1016
.
DETERC~EN~ CO~IPOSITIONS
This invention relates to detergent compositions in
particula-te form which are adapted for fabric ~ashing, and in
particular -to such compositions containing a synthetic
detergent surfactant together ~ith a phosphate detergency builder.
The most co~monly used detergency builders are the
condensed phosphates, especially sodium tripolyphosphate, but
it has been suggcsted that the use of phosphate detergency
builders can contribute to eutrophication proble~s. 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 unsatisfac$ory for one reason or another, for example
they are less efficient or biologically unacceptable, or they
may simply be too expensive.
.
.
:
,

S~6
2 _ ~C.1016
I-t has also beerl proposed to mi-tigate the problems of
eutrophica-t-ion by using decreased Levels o:E condensed
phosphatc detergency buildcrs, with or witllout the presence
of o-ther dctergency builders, but few oi these proposals
have approactle~d commercial accept~lce. ~lhus, when reduced
leve]s of sodium -tripolyphosphate are used witllout supplemeIltal
buildcrs, the~e can be considerable problems when using the
compositions in hard water if there is insufficient phosphate
to sequester all the calcium ions present. This causes -the
precipitation of insoluble calcium phosphate salts which can
be deposited on the washed fabrics, besides giving decreased
detergency due to inadequate sof-tening of the wa-ter, sometimes
accompanied by precipitation of insoluble calcium sal-ts o:E
anionic detergent compounds.
On the other hand, when a condensed phosphate builder is
used with some non-phosphate detergency builders, the former
may prevent the latter from functioning effectively~
especially in the case of other detelgency builders which act
by precipitating the calcium salt, for example sodium
carbonate. Moreover, there are relatively few other
detergency builders which are completely acceptable environ-
mentally and which are good enough to be worth using7 even in
part replacement for a condensed phosphate builder.
In recent years a lot of e-ffort and expense has been
directed to solving these problems, with the synthesis and
evaluation of great numbers of new materials. ~owever~ it
would inevitably ta~e several years for any completely new
.
,
'' . ~.

S~
- 3 ~ cC.10~6
material -to be clcared for domestic use, and therefore most
recent in-tcrest has centered on known low and non-phosphate
materials which act as builders by either sequestration,
precipitation or ion-exchange and ~hich are known to be
ellvLro~llentally safe.
~ ccording to one aspect o~ the present invention we
have now found it possible to obtain effective detergency
propcrties at reduced phosphate builder levels by using a
partially neutralised alkali metal orthophosphate salt in
combination with an alkali metal carbonate sal-t in defined
proportions. As both of these materials are well known per
se, there are no problems concerning environmental sa~ety,
provided that the compositions do not give excessively
alkaline solu~ions in use. Moreover, although both of the
essential detergency building materials are so-called
precipi-tant builders, that is they inactivate calcium
hardness ions by forming insoluble calcium salts, the
precipitate can readily be prevented from depositing on
clothes at unacceptably high levels.
In a further aspect of the invention, particulate
detergent compositions are provided which contain higher
levels of partially neutralised alkali metal orthophosphate
salts together with alkali me$al carbonate salts, which can
be made with increased detergency building properties and yet
with decreased energy consumption compared with otherwise
similar compositions based on sodium tripolyphosphate.

...6
- ~ - cC.~16
The particlllate alkaline de-tergent co~npositions of the
invent-;or are produced from over about 15% -to about 50% oE a
partially neutraLised alkali metal orthophosphate salt" :Crom
over .ibollt 20% to about 500~b oL` an a]kali metal carbonat;e saLt
S antl :Crolll abou-t 5% to about ~U% of a synthetic detergent
sur:Eactant, all these percen-tages being by weight oE the
to-tal de-tergent composition. The degree of alkalini-ty of`
the detergent compositions should be such -that the p~ of a
0.1% aqueous solution of the composition is Erom 9 to 11.
It was proposed in our UK p~tent 1~4i2~40i to form
detergent compositions comprising from 5% to 15% of ortho-
phosphate salts and 20% to .450,b by weight oE al~aline salts,
Eor e~ample sodium carbonate, in order to give a pH of at ,~
least ~.2 in use. These compositions were of particularly
iS low phosphate content and also intended for use at low
product concentrations. However, it transpired that such
levels of phosphate were unnecessarily low for compliance
with the legislation now expected to be enacted in several
countries. In addition, at higher product concentra-tions,
as commonly used in many European countries, the composi-tions
of UK pa-tent 1,412,40i were less effective than desired in
comparison with other higher phosphate compositions based on
sodium tripolyphospha-te alone as a detergency builder. The
present invention provides compositions of higher, ie over
15%~ phospha-te content, which have more effective detergency
building properties.

~ ~ - cC.iO16
The partially neutralised alka]i metal orthophosphate
salt uscd is either a potassium or preferably a sodium ortho-
phosphate salt, as the latter are cheaper ~nd more readily
available. ~-t :is preferred to -use so~e or all disodium
S morlohydrogcn ortllopllosphate in the preparation o~ the oompo-
si-tions, a'Lthough a proportion may be neutralised during
powder pxocessing to form -the trialkali metal salt or some of
the la-t-ter may also be present initially provided the p~ is
not too high. ~lternatively, the mono- or mixed mono- and
di-alkali metal orthophosphate salts may be used if desired
to ~orm the compositions. Ii too much of the monosodium
dihydrogen salt is used the pH can drop substantially, in
which case some more alkaline material must also be added.
It may be advantageous to use as the source of the
alkali metal orthophosphate salts a mixture of disodium and
monosodium hydrogen orthophosphates in a molar ratio of about
1:3 to 2:3, especially about 1:2~ as such a mixture is
commercially available, being produced as a feedstock in the
manufacture of sodium tripolyphosphate, when it is known as
~'kiln-feed~'. This gives valuable cost savings because the
energy otherwise employed to convert the ki'ln-feed into
sodium tripolyphosphate is saved. The invention therefore
includes a process ~or preparing the compositions of the
invention in ~hich -the partially neutralised alkali metal
orthophosphate salt used is a mixture of the mono- and di-
sodium salts as described above.
,

5~6
_ 6 - cC.1016
The alkali metal orthophosphate salt used in the
preparatioII of the detergent composi-tions may be in -the form
O:e nnhyd:rous or hydrated salts, for e.Y~nple as disodium mono-
hydrogell ortllophosphate dodccahyd.rate. It will be
appreciated that hydr~tioll ox dehydration may also take place
during de-tergen-t processing~ but the alnounts of the ortho-
phosphate salts are calcu].a-ted in anhydro-us Iorm.
Whilst the ~nount of the alkali metal orthopbosphate
salt can be varied generally within the range of over about
15/S to about 50%~ it is preferred to have a maxi~um or-tho-
phosphate salt content of about 30% by weight, which corres-
ponds to a ma~imum phosphorus content in the compositions of
about 6% by weight. It is particularly preferred to have an
alk.ali metal orthophosphate content of about 20% to 25%~ ie
15 about .4% to 5% phosphorus in the compositions. It will be
appreciated that these levels of phosphorus are well below
those which are cus-tomary when using sodium tripolyphosphate
as the detergency builder, ie at levels which, until
recently, were generally in excess of 30% of the compositions.
When higher levels of the alkali metal orthophosphate
salts are used, especially within the range of about 30% to
50%, the compositions are particularly ~seful as so-called
soaker/prewash compositions, when they are used at relatively
low produc-t concentrations to aid in soil re~loval prior to
~5 normal washing. Otherwise they can be used as conventional
fabric washi}lg compositions themselves, where high ~ater
hardness levels are found and there are no phosphate eutro-
'

- 7 - cC.1016
phication prob:Lems. Use of the partially neutralised
alkali metal orthophosphate salts preven-ts excessively high
a].kal.:inity, especially wben higher levels o:E the orthophos~
phato 9 alt are prescnt.
The a.l.ka.l.i.llletal carbonate salt used is potassium or
p.referably sodium carbonate or a mi.xture -thereof. The
carbonate salt is preferably fully neutralised, but it may
contain sorne potassiwn or sodium bicarbonate or sesqui~
carbonate.
Although -the amoun-t of the alkali metal carbonate salt
can be varied between over about 20% to about 50% by weight
of the compositions~ it is preferred to.use an amount of
about 250,b to about 45C/o by l~eight depending on the type of ,.
composition to be produced. Lower levels of carbonate salt
within the range of over about 20% to about 30% are normally
used l~hen the higher levels of orthophosphate salt are
employed. The amount of the alkali metal carbonate is
determined on an anhydrous basis, although the carbonate
salts may be hydrated either before or when incorporated
20 into the detergent compositions.
. - :
The detergent compositions of the present invention
necessarily include from about 5% to about ~0%~ preferably
not more than about 257b, eg about 10% t 0 about 20% ~ by weigh-t
. of a syntheti.c anionic, nonionic, amphoteric or zwitterionic
detergent surfactant or a mixture thereof. It is particularly
preferred to use a nonionic de-tergent surfactant either alone
or in admixture with o-ther anionic detergent surfac-tants in

51~
- 8 - cC.1016
the case of low l~thering compositions. ~Iany suitable
detergellt surfact~lts are commercially available c~ld are
flllly descr-ibed ill the Literclture, for example in Sehwartz,
l'erry ~ Berch in "Surface ~etive ~ents and Detergents~,
VoLuules I ~nd :~:C.
The pre:f~xred nonionic detergent surfactants whicll m~y
be used include in particu]ar the reac-tion products of
eompounds having a hydrophobie group and a reactive hydrogen
atom, for exal~ple aliphatie alcohols 7 aeids, amides or alkyl
phenols with alkylene oYides, especially ethylene oxide
ei.ther alone or with propylene oxide. Speeifie nonionie
detergent surfaetants are alkyl (C6-C22) phenol-ethylene
oxide condensates, generally 5 to 25 EO, ie 5 to 25 units of
ethylene oxide per molecule; the condensa-tion produc-ts of
aliphatic (C6-C18) primary or secondary linear or branehed
aleohols with ethylene oside, generally 6 to 30 EO, and
products made by condensation of ethylene oxide with the
reaction produets of propylene oxide and ethylenediamine.
Other so~ealled nonionie detergent surfaetants include long
eh~in tertiary amine oxides, long ehain tertiary phosphine
oxides and dialkyl sulphoxidesO Mixtures of amine o~ides
with ethoxylated nonionie eompounds can also be used.
~ he anionic detergent surfactants which ean be used are
usually water-soluble alkali metal salts o~ organic sulphates
and sulphonates having alkyl radicals con~aining from about 8
to 22 carbon atoms, the term alkyl being used to include the
alkyl portion of higher acyl radieals. Examples of suitable

s~
- ~ - cC.lOi6
sy~ltllct.i.c ani.v:rl:ic detergcnt surIactants are sodium ancl
~ota.q.qi.llm allcyl. sulr)l~ates~ ospecial~Ly tlloso obtained by
slllpllatlTI~ h-i~llor (C~~C18) a:lcollol.s p:roduce(l :Eo:r e~ample lrom
tnl:Low or COCOllllt o:i.l.; so(l~ m an(l potass:Lutn a].lcy:l. (C8-C20)
l~oll~.otlo su:lpllorl;ltos, part:i.cularly HoclLum l:ln(~ar soconclary
allcy l. (c~ O a l ~ onPello sulpllonates; sodium a~l~yl glyceryl
other sulplllltes, ospoc:ial.:Ly thoso ethers o:E the higlter
alcol~o:l.s do:r:i.vecl :lirolll tallow or coconut oil and syn-the-tic
alcohols dorivetl from petroleu~; sodiuln COCollUt oil fatty
ac:i.d monoglyccr:ide sulphates and sulphonates; sodl~ and
potassi~ saltg O:e sulphuric acid esters o:~ higller (C8-C18~
I`atty a:Lcollol~a:lky:l.(3ne ox:icle, particularly e-thylene o~ide,
roacl;:i.on prodtLcts; the reaction products of fak-ty acids
s~ch as coconut :Latty acids esteri:eied with i.sethionic acic~
lS ~ncl nelltra:li.st~d with soclium hydrQx:Lde; sodium and potassillm
salts o:E fatty acid ~nides of uletllyl taurine; allcane luono-
sulphonates S~ICll as those derived by reacting alpha-oleEins
(C8-C20) with sodiuul bisulphite and those derived by reacting
p~aEfins with S02 and G12 and then hydrolysing with a base
to produce a rando~L sulphonate; and olefin sulphonates,
whiclt term is used -to describe tho material made by reacting
ole.-Eins, parti.cularly C8-C20 alpha-olefins, wi-th Sn3 and
then neutralising and hydrolysing~the reaction product. ~he
pre:Eerre~l anionic de-tergent surfactants ~re sodiulu (ClO~C15)
allcyl benY.ene sulphonates and sodium (Ci2-Ci8) all~yl sulp
~ mounts o:E ~llpho-teric or ~witterionic detergent
surt`actants mly also be used iIl the COIllpOSitiOIlS o:E the

- 1~ - cC.1016
inve:rltion but this is not normal].y desired due to their
rel.atively high cost. Il' any amphoteric or zwitter:ionic
doto.rgen-t surfac-t~nts are uscd it is gencrally in small
amoullts in colnpos:itions based on the Inuch mo.re co~ only used
syntllot:ic ~m:i.oll:io and/or nonioni.c de-tergent sur:Cac~ ts.
Solne soaps may also be used in thc compositions of the
invelltion, but not as the sole detergen-t surfactants. Soap
is particularly useful at low levels in binary and ternary
mi,Ytures together with nonionic or mixed synthetic anionic
and nonionic detergent surfactants, which have low sudsing
proper-ties. The soaps which are used are -the sodium, or
less desirably potassium, salts of C10-C2.4 fat y
is particlllarly preferred tllat the soaps should be bascd
~ainly on the longer chain fatty acids wi$hin this range,
that is with at least half of the soap having a carbon chai.n
length of 16 or over. This is most conveniently accomplished
by using soaps from natural sources such as tallow, palm oil
or rapeseed oil, which can be hardened if desired, with lesser
~nounts of other shorter chain soaps, prepared from nut oils
such as coconut oil or palm ~ernel oil. The amount of such
soaps can be varied between about 0. 5% and about 255b by
weight, with lower amounts of about 0. 5% to about 5% being
generally sufficien-t for lather control. ~mounts of soap
between about 2% and about 20%~ especially between about 50/b
~5 and about l50,b, are preferably used to give a beneficial
effect on detergency.
. ,
:
:
:

5~6
cC.1016
~ part rrom -tlle de-tergent surfactants ancl detergency
buildcrs, the detergent compositions O:r the invention c~n
contaill any oL the conventional additives in the c~mounts in
~YhlCIl SllCl~ mat~rials are norlllally employed :in l`abric washin~
detergetlt colnpositions. Ex~nples of thesc additives include
Lather boosters such as alkanola~nides, particularly the mono-
ethanolantides derived from palm kernel fatty acids and
coconut fatty acids, lather depressants such as alkyl
phosphates, w~xes and silicones, antiredeposition agents such
as sodium carboxymethylcellulose and polyvinyl pyrrolidone,
oxygen-based bleaching agents such as sodium perbora-te and
sodi~n percarbonate, per-acid bleach precursors, chlorine-
releasing bleaching agents such as ~trichloroisocyamlric acid
and alkali metal salts of dicllloroisocyanuric acid, fabric
softening agents, inorganic salts such as sodium sulphate
and magnesium silicate, and, usually present in very minor
amounts, fluorescent agents, perf-~es, enzymes such as
proteases and amylases, germicides and colourants.
I-t is particularly beneiicial to include in the
detergent compositions -an amount of sodium percarbona~e,
preferably be-tween about luok and about .40%~ for example about
15% to about 30%, by weight of the compositions. It has
been found that tha efficiency of sodium percarbonate is
increased in these compositions. Moreover, after the sodium
percarbonate has lost its oxygen in use, the residual sodium
carbonate call contribute to the reserve all~alinity of the
wash solution.
; `

- 12 - cC.1~
I-t is desiral~le to include one or more antideposition
a~en-ts in -the detergent compositions of the i.nvention, -to
dec:rease a tendellcy to forlll i.norganic deposi.ts on washed
:Cal)rics . rrhe mos t cffective antideposit:ion agents are
an:ionic polye lcc-trolytes, especially polyme:ric aliphatic
carboxylates whi.ch appoar to stabilise the suspensions of
insoluble calcium sal-ts and thereby inhibi.t their deposition
onto fabrics. The amount of any such antideposition agent .
is normally :Crom about 0.05~0 to about 50lh by ~eight, preferably
from about O.i% to about 2~ by weight of the compositions.
Speciïic preferred antideposition agents are the alkali
metal or amlllorliuill, preferably sodium salts of homo- and co-
polymers of acrylic acid or substituted acrylic acids, such
as sodium polyacrylate, the sodium sal-t of copolymethacryl-
amide/acrylic acid and sodilml poly-alpha-hydrogyacrylate,
salts OI copolymers of maleic anhydride wi-th ethylene, vinyl-
methylether or styrene, especially 1:1 copolymers, and
optionally with partial esterificati.on of the carboxyl
groups. Such copolymers generally have molecular ~eights
in the range of about 2,000 to 500,000. Other antideposition
agents include the sodium salts of polymaleic acid, polyita-
conic acid and polyaspartic acid, phosphate esters oï ethoYy-
la-ted alipha-tic alcohols, polyethylene glycol pllosphate
esters, and certain phosphonates such as sodium ethane~
hydroxy-1, 1-diphosphonat e, s odium ethy lenedi amine t etra-
niethylene phosphonate, and sodium 2-phosphonobutane
tricarboxylate. ~Iixtures of organic phosphonic acids or
, :
,

5~
~ 13 - cC.1016
substituted acrylic acids or their salts with protective
colloids such as gelatin as described in Netherlands
Appl-.i.cat:ion ~6020S2 may also be used. ~he most preferred
cmtidcpositiorl agent is sodium polyacrylate hnving a ~ of
out 10,000 to 5~,~00, ~or example about 20,0~0 ~o 30,000.
It is also poss:i~le to inc].ude in the deter~ent
composi.tions O:e the invention minor amounts of other
phosphate or non~phosphate detergency builders, which latter
may be ei-ther so-ca~led precipitant builders, sequestran-ts or
ion-exchange builders. Low levels of alkali metal tripoly-
phosphate or pyrophosphate may be present with the alkali
metal orthophosphate as impurities, for example c~t levels up
to about 5~ by weight, but it is preferred not to have them
present in thc compositions. The presence of other non-
phosphate det~rgency builders may be benefioial, when it isdesired to increase detergency whilst using relatively low
levels of the alkali me-tal orthophosphate and without using
excessively high alkali metal carbonate levels, because of
the high alkalinity this would otherwise cause. Exa~lples of
2~ such other detergency builders which could be used in these
circumstances are amine carboxylates such as sodium nitrilo-
triacetate, and sodium aluminosilicate ion-exchange materials,
eg ~eolites A and X. However, such other detergency builder
materials are not essential and it is a particular benefit of
.5 the compositions of -the invention that satisfactory
de-tergency building properties can be achieved with -the mixed
alkali metal orthophosphate and alkali metal carbonate
.

5~L6
~ cC.10~6
builder salts at lower pllosphate levels than hitll~r-to
considered necessary without other non-phosphate detergency
bui'lders.
I-t is ~lso generall~ desi.rable -to include in -tlle
clctox~cn-t compositions an amoun.t o:t' an all~ali metal
sl'.l.icate, particularly sodium or-tho-, meta- or preEerably
neutral or alkalille silicate. l'he more highly alkaline
ortho- and meta-silicates are normally only -used at lower
levels, in admixture l~i-th the neutral or alkaline silica-tes.
The presence of such alkali metal silicates, usually at
levels oI from about 50,b to about 15% by weight of the
compositions, is advantageous in decreasing the corrosion of
metal parts in washing machines, besides giving processing 1'
benefits and generally improved powder properties. Eowever,
the presence of the allcali metal silicates in the compositions
- of the invention can contribute to increased inorganic
deposits on washed fabrics, and it is therafore preferred to
use only low levels of.such silicates, if any, for eYample~not
- more than about 10% by weight of the compositions.
The compositions of the invention are required to be
al~aline, but not too strongly alkaline, as this could result
in fabric damage and also be hazardous for domestic usage. ~'
In practice the compositions should give a pH of from 9 to 11
- in use in aqueous wash solu-tion. It is preferred in
particular for domes-tic products to have a minimum pH of a-t
least about 9.25 a~d especially a pH of about 9.5 or over, as
. .
lower pHs tend to be less effective for optimuul detergency

- ~5 - cC.10~6
building, .~1d a m~im~n plI of about 10.5. ~he p~
should be measuJed ~-t the lowest normal usage concentration
ol 0.1~ w/v O:e thc product in wator of 12I-I (Ca) (French
per~ ont hardnoss, calcium only) at 50C, so -tllat a
s~ltisL~ctoxy do~rçc oE alka:Linity c~ be ass~rcd in use at
all norma:l procluct concentrations. ~he pH of the cletergent
colllposltions in use is controlled by the amount and type of
the par-tially neutralised alkali metal orthophosphate and
alkali metal carbonate used, and on the other alkaline salts
which may be present, silch as alkali me-tal silicate and
sodium perbora-te or sodium percarbonate. It will be
appreciated that because of the high a]kalinity of the
compositions of the invention the other ingredients in the
compositiolls should of course be chosen for their alkaline
i5 stability, especially for pH-sensitive materials such as
en~symes.
~ he detergcnt compositions of the present in~ention are
required to be in particulate form, which includes powders
and granules, and they may be made by conventional techniques.
for eYample by granulation or by slurry m~ing and spray
drying processes. Dry mi~ing of the ingredients can also be
used, especially for products to be sold in individual dose
packs such as sachets, but this is not recommended for
products sold in bulk for the consumer to dispense in use,
because of potential segregation problems and because of the
less uniform appearance of the products. I-t will be
appreciated that if production of the detergent composi-tions

- 16 - cC . 10~6
is conducted in the presence of moisture, the ingrediellts may
reac-t together, for example the partially neutralised a].kali
metal orthopllospllate salts may be f-urther neu-tralised by
other more alkali.ne ingredi.ents present.
B 'rhe .invcnt:ion is illus t.rated by the :Eollot~ing 13xalllples
in wllich parts and percent ages arc by ~,lci.ght, the amoullts o:E
the ingredients being eh~pressed on an anhydrous basis,
except where o-therwise indicated.
Examples 1 and 2
~ particulate detergent composition was prepared by
slurry malcing and sp:ray drying -to the following nominal
formulat iOll: '
~;_edient o/0
C12-C15 alcohol - 8 E0 lO . 0
Disodium orthophosphate 20. 0
Sodium c arbonat e 35 . 0
Sodium percarbonate2 25 . 0
Sodi-um carboxymethylcellulose :1. 5
Sodium polyacrylate .1. 0
Sodium alkyl pho.sphat e 0 . 5
Fluores cent agent 0 . 5
Water to 100. 0
4% of the nonionic detergent surfactant ~as included
in the spray dried powder and the remaining 6% was
sprayed onto the finished product.
2 ~dded after spray drying.
.'

,
- 17 - cC.1016
This comp~sition (Example 1) was tes~ted for detergency
at a product concelltra-tion oE o.~o/O in water of 25H
(c~ r~ ) a-t ~5C and showed equality with a
comlllerci.ll ~roduct contailling 3~% sodium tripoLyphos~phatc.
S 'rho po~der was also cx~ninecl for inorganic deposi-tlon aCter
mllltiple wash cycles. The latter tests were also done in an
alltolllatic (rotating clrum) washing luachine at a product
collcentration of 0.6% in 35H water (Ca~:Mg~ :1) at 95C
using natura]ly soiled wash loads wi-th test cloths. The
results after iO wash cycles showed an inorganic deposition
level of l.S%"ihich co~lpared favourably with that (2.2~ob)
for a col~parative commercially available sodi~ tripolypllos-
phate-built product. ~Iter 20 wash cycles the figures were,
respectively, 3.3% and 4.90,b~ which still showed a1uarked
benefit for -the composition of the invention despite its high
conten-t of precipitant builder salts. The same test cloths
were also examined for soil redeposition from the naturally
soiled clothes, by measuring the change in light reflectance
after both 10 and 20 wash cycles, when it was found that the
product of the invention gave significantly less redeposition
than the comparative commercially available product.
~ further powder (E~ample 2) was prepared with a similar
formulation but with the nonionic surfactant level decreased
from 10% to ~% and wi-th 6% sodium alkyl benzene sulphonate
added instead. I~ addition 3/0 of sodium tallow soap was
added and the amount of sodi-um percarbonate correspondin-gly
decreased to 22%. This composition was ~lso found to have

5~
- 18 - cC.10~.6
good :Cabric waslling and bleaching properties despi-te -the low
phosphate contcnt.
Both colllposi.ti.ons wele superior to the comltlerc:ial. sodilmi
-tr3.po:Lyphospllate_b~lilt product in blcaching tea-stn:i.1letl test
5 clotlls, the increuse in ligllt ro:Electance being 6.3 arld 8.2
units ~reater for Exalllples 1 and 2~ respec-tively.
~xamples 3 and .4
Two compositions were made by dry mixing the ingredients
to the sa~le formula as Example 1 except -that the amount of
disodiwll orthophosphate was increased to 25% ancl 30%~
. respectively, and the amount of sodium carbonate was
decreased -to 30,/0 and 25%~ respec-tively, in Examples 3 and ~.
The products were evaluated for fabric washing properties in
a Terg_0_Tolueter against the product o:E Example 1, a first
lS con-trol formulation containing only 10% of the disodium
or-thophospha-te and 450,h of the sodium carbona-te but otherwise
being the same as Examples 3 and .4, and a second control
formulation containing 30% sodium tripolyphospha~e as
detergency builder with 25//o sodium perborate, at .4 g/l in
water of 25H at 80-85C. The products of both E~amples 3
and 4 were found to have slightly better detergency
properties on artificially soiled test cloths compared with
Example 1, significantly better detergency than the first
control product and significantly improved bleaching
25 properties compared with the second control product.

5~6
- 19 - cC.lOi6
Ex~nples 5 to 7
The formu]ations of Examples 3 and 4 were varied by
fiIst:Ly changing the sodium percarbonatc of Ex~llple 3 for
sodi~ per~orate (Ex~nple 5), secondly by cllal1ging th0 10%
~5 nollio~lio sllr;l~lctclllt in Exa~ple 4 I`or 6% so~liuul alkyl benzene
stl:lpllonate a~ 1% 0~ tbe same nonionic detergent suriactc~t
(Exatllple 6), and thirdly by changing the 10% norlionic
surfactarlt in Ex~lple ~ for 10% of sodium alkyl benzene
sulphona-te and also challging the disodium orthophosphate and
sodium car~on~te levels to 15.5% and 400,b, respectively
~Ex~lple 7~. The products were evalua-ted for detergency and
bleaching properties in a Terg-0-Tometer c~nd again found to
give good results. Ilowever, the use of the perbor~te in
Ex~llple 5 was found -to give marginally less beneficial
~leaching on the test clo-th and the lowering of the nonionic
surfactant level in Exaulple 6 was found to give slightly
lo~er ~ut still good detergency results. ~he product o~
Example 7 was found to have very good detergency properties
despite its low phosphorus level, when evaluated against a
similar product con-taining 30/~o of sodium tripolyphosphate as
the de-tergency builder.
Examples 8 to 10
Three products ~ere made to the same formulations as
for Examp1es ~, 3 and 4, respectively, except that the
25 disodiwn orthophosphate was replaced by kiln-feed, ie mixed
disodium and monosodiwllllydrogen phospllates (ratio about 1:2).
Evaluation tests sho~ed the products of Ex~nples 8 to 10 gave
'
,

5~6
- 20 - cC.1016
wash solutions of lower p~I (0.3-0..4 units) compared with
Exalllples i, 3 cmd .4. ~part from thi.s there was a directional
benel`it but not a sigllil'ic~qn-t chaMge in detergency on US:illg
tho l~iln-:Ceod instead o:~ the d:isodiulll orthophosphate.
~x~tlp:Les ll to 13
~ detcrgent colllpositi.on (~AYample ll) was made by dry
mi.~ing to the same l`ormulati.on as E,~ample l, excep-t or the
omission of the sodiu~l polyac:rylate. To this COIupOSitiOll
was added either 1.0% of sodil~u copoly(i:l)vinylmethylether-
maleate (in Ex~uple 12) or 1.0% of sodium polyacrylate (~
~25,000) (in Example 13). The levsl of i.norganic deposi-ts
on COttO11 terry towelling was then determined in coJnparison
with the control formulaticn containing 30/O sodi~un tripoly-
phosphate and 25% sodiulu perborate with the Iollowing
15 results (product dosage 6 g/l în 35H water at 80-85C):
% deposits
Example 5 s~ashes l0 s~ashes 20 wash~s
ll 4.2 8.0 10.. 4
12 1.3 2.0 . 2.5
13 1.2 2.3 2.
Control 0.6 2.8 3.6
These results show the beneficial results of
incorporating an antideposition agent in the products
acGording to the invention.
**~

Dessin représentatif

Désolé, le dessin représentatif concernant le document de brevet no 1110516 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.

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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 : Périmé (brevet sous l'ancienne loi) date de péremption possible la plus tardive 1998-10-13
Accordé par délivrance 1981-10-13

Historique d'abandonnement

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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
JAMES F. DAVIES
JOHN B. TUNE
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Description du
Document 
Date
(aaaa-mm-jj) 
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Revendications 1994-03-29 3 72
Abrégé 1994-03-29 1 16
Page couverture 1994-03-29 1 15
Dessins 1994-03-29 1 10
Description 1994-03-29 20 731