Note: Descriptions are shown in the official language in which they were submitted.
~L8~2~
- 1 - C.1081
D _ RGENT CO~SPOSITIGNS
This invention relates to detergent compositions which
are particularly, but not essentially, adapted for fabric
washing, and more particularly to phosphate built detergent
compositions including a bleach system.
It is known to incorporate peracid bleaches such as
sodi~m perborate, together with peracid bleach precursors
or peroxy bleach activator in detergent compositions. Such
detergent compositions conventionally include, in addition
to a detergent active material, a phosphate detergency
builder such as sodium tripolyphosphate. In some
circ~mstances, it is thought that the use o~ phosphates in
QBZOlX
2~2~
- 2 - C.1081
detergent compositions can lead to environmental problems
in waste waters. There is therefore a desire to reduce the
level of phosphorus in detergent compositions.
Water-insoluble alumino-silicate ion exchange
materials have been suggested as alternative builders to
phosphates. (See for example GB 1 429 143 - Procter &
Gamble Co.) However, it has been found that in
alumino-silicate built compositions the performance of
this bleach system is significantly reduced.
It has also been found that, where a detergent
composition ls based on aluminosilicate as the only
builder, or on sodium tripolyphosphate as the only builder,
the bleach performance of the composition is reduced as the
final water hardness is increased. Thus, for a fixed
product dosage where the level of builder material in the
product is intentionally reduced, possibly as a cost saving
exercise, or where the product is used at a dosage which is
lower than that recommended, the bleach performance of the
product is reduced.
We have now surprisingly found however, that the
bleach per~ormance can be substantially maintained and that
the reduction in bleach performance with increasing water
hardness can be substantially overcome if only a specific
part of the tripolyphosphate is replaced by the
alumino-silicate and if the peroxy bleach and the activator
therefor are present in specific relative proporticns.
Thus, according to the invention there is provided a
particulate alkaline detergent composition comprising:
from about 5% to about 40% by weight of at least one
synthetic detergent active material;
liB~026
~ 3 - C.1081
from about 12.5~ to about 25% by weight of an alkali
metal tripolyphosphate calculated on an anhydrous
basis;
from about 7~0% to about 36% by weight of a water-
insoluble aluminosilicate detergency builder material
calculated on an anhydrous basis;
from about 5% to about 30% by weight of a peroxy
bleach; and
up to about 15% by weight of an activator for said
peroxy bleach,
the weight ratio of said peroxy bleach to said activator
being between about 2:1 and about 15:1.
It is particularly beneficial if the percentage
quantity of alkali metal tripolyphosphate (T) and the
percentage quantity of the aluminosilicate material (A) are
~elated to each other in such a manner that the sum
T ~ 0.5 A
lies between about 25 and about 37, preferably between
about 28 and about 34.
The detergent compositions of the invention
necessarily include from about 5% to about 40%, preferably
about 10~ to about 25% by weight of a synthetic anionic,
nonionic, amphoteric or zwitterionic detergent compound or
mixture thereof. Many suitable detergent active compounds
are commercially available and are fully described in the
literature, for example in "Surface Active Agents and
Detergents", Volumes I and II, by Schwartz, Perry and
Berch.
Generally, fabric washing detergent compositions also
- ~ - C.1081
contain fluorescent agents for improvin~ the brightening
activity of the compositions towards fabrics washed
therewith. The fluorescent agents co~monly used are
derivatives of 4/4'-di(sym-triazinylamino)-stilbene-
2,2'-disulphonic acid or salts thereof. Other fluorescent
agents that have also been used for example are,derivatives
of diphenyldistryryl compounds, such as 4,4'-di(3-
sulphostyryl)-diphenyl; derivatives of 4,4'-di(triazolyl)-
stilbene-2,2'-disulphonic acid and derivatives of diphenyl-
2~pyrazoline. Such fluorescent agents, however, whenincorporated in bleaching detergent compositions are liable
to decompose with consequent loss of fluorescent activity,
possibly owing to interaction with the bleaching system
therein.
We have now surprisingly found that the Eluorescer
stability can be substantially maintained if a major part
of the detergent active material is constituted by an
anionic material. Thus, it is preferred that the
detergent active material selected from anionic synthetic
detercJent active materials and mixtures thereof with a
les~er amount o~ one vr more non-anionic synthetic
detergent active materials.
The synthetic anionic detergent compounds are usually
water soluble alkali metal salts of crganic sulphates and
sulphonates having alkyl radicals containing from about 8
to about 22 carbon atoms, the,term alkyl being used to
`include the alkyl portion of higher aryl radicals.
Examples of suitable synthetic anionic detergent compounds
are sodium and potassium alkyl sulphates, especially those
obtained by sulphating higher (C8-C18) alcohols
produced for example from tallow or coconut oil; sodium and
potassium alkyl (C9-C20? benzene sulphonates,
particularly sodium linear secondary alkyl (C10-C15)
benzene sulphonates; sodium alkyl glyceryl ether sulphates,
- 5 - C.1081
especially those ethers of the higher alcohols derived from
tallow or coconut oil and synthetic alcohols derived from
petroleum; sodium coconut oil fatty acid monoglyceride
sulphates and sulphonates; sodium and potassium salts of
sulphuric acid esters of higher (Cg-Cl8) fatty
alcohol-alkylene oxidel particularly ethylene oxide,
reaction products; the reaction products of fatty acids
such as coconut fatty acids esterified with isethionic acid
and neutralised with sodium hydroxide; sodium and potassium
salts of fatty acid amides of methyl taurine; alkane
monosulphonates such as those derived by reacting alpha-
olefins (C8-C20) with sodium bisulphite and those
derived by reacting paraffins with SO2 and C12 and then
hydrolysing with a base to produce a random sulphonate; and
olefin sulphonates, which term is used to describe the
material made by reacting olefins, particularly C10-C20
alpha-olefins, with SO3 and then neutralising and
hydrolysing the reaction product. The preferred anionic
detergent compounds are sodium ~C~l-C15) alkyl benzene
sulphonates and sodium (C16-C18) alkyl sulphates-
Examples of suitable nonionic detergent compoundswhich may be used, preferably together with the anionic
detergent compounds include in particular the reaction
products of alkylene oxides, usually ethylene oxide, with
alkyl (C6-C22) phenols, generally 5 to 25 EO, ie 5 to
25 units of ethylene oxides per molecule; the condensation
products of aliphatic (C8-C18) primary or secondary
linear or branched alcohols with ethylene oxide/ generally
6 to 30 EO, and products made by condensation of ethylene
oxide with the reaction products of propylene oxide and
ethylenediamine. Other so-called nonionic detergent
compounds incl~de long chain tertiary amine oxides, long
chain tertiary phosphine oxides and dialkyl sulphoxides.
Mixtures of the anionic detergent compounds with, for
- 6 - C.1081
example, nonionic compounds may be used in the detergent
compositions, particularly to provide controlled low
sudsing properties. This is beneficial for compositions
intended for use in suds-intolerant automatic washing
machines. The presence of some nonionic detergent
compounds in the compositions may also help to improve the
solubility characteristics of the detergent powder. A
preferred anionic to nonionic ratio is at least about 2:1,
most preferably from about 3:1 to about 10:1.
Amounts of amphoteric or zwitterionic detergent
compounds can also be used in the compositions of the ,
invention but this is not normally desired due to their
relatively high cost. If any amphoteric or zwitterionic
detergent compounds are used it is generally in small
amounts in compositions based on the much more commonly
used synthetic anionic and nonionic detergent compounds.
Some soaps may also be used in the compositions of the
invention, but not as the sole detergent compounds. They
are particularly useful at low levels in binary
(soap/anionic~ or ternary mixtures together with nonionic
or mixed synthetic anionic and nonionic detergent
compounds, which have low sudsing properties. The soaps
which are used are preferably the sodium, or less desirably
potassium, salts of C10-C24 fatty acids. It is
particularly preferred that the soaps should be based
mainly on the longer-chain fatty acids within this range,
that is with at least half of the soap having a carbon
chain 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 amounts of other shorter-chain soaps,
prepared from nut oils such as coconut oil or palm kernel
oil. The amount of such soaps can be varied between about
0.5% and about 25% by weight, with lower amounts of about
512~
- 7 ~ C.1081
0.5% to about 5% beiny generally sufficient for lather
control. Amounts of soap between about 2% and about 20%r
especially between about 5% and about 15%, are preferably
used to give a beneficial effect on detergency. This is
particularly valuable in compositions used in hard water
when the soap acts as a supple~entary builder. In
addition, we have found that the addition of soap helps to
decrease the tendency of the compositions to form inorganic
deposits in the wash, for which purpose it is preferred to
use about 2~ to about 15~, especially about 2.5% to about
10~ by weight of soap in the composition. When soap is
present, it is preferred that the total level of detergent
actives, including the soap, lies between about 5~ and
about 40% by weight, most preferably between about 10% and
about 25% by weight. Further, when both the soap and a
nonionic detergent active material are present together
with a synthetic anionic detergent active material, it is
preferred that the weight ratio of the synthetic anionic
material and soap to the nonionic material is at least
ahout 2:1, most preferably about 3:1 to about 10:1.
The alkali tripolyphosphate is preferably sodium
tripolyphosphate, advantageously present in an amount of
from more than about 15~ to about 22% by weight. While it
is desirable that the only phosphate material present is
the tripolyphosphate, up to about 5% by weight of the
composition of other phosphate materials may also be added,
such as orthophosphate or pyrophosphate. Low levels of
these other phosphate materials , even over 5~ by weight of
the composition, may in any case be present in compositions
which have been prepared by spray drying, as a consequence
of the hydrolysis of sodium tripolypohosphate. Thus, for
example, a spray dried product nominally containing 25%
sodium tripolyphosphate (STP) may in fact contain up to
about 10% by weight of other phosphates derived from the
breakdown of the tripolyphosphate. The res~lting sodium
26
- 8 - C.1081
orthophosphate and sodium pyrophosphate both contribute to
fabric ashing and should be kept to a minimum.
Although careful control of processing conditions can
reduce this STP breakdown, it is preferred to prevent all
breakdown-in the spray drying tower by post dosing all the
STP. There may still be some ortho- and pyrophosphate in
the final, powder because t~e raw material STP may contain
about 5~ of them and some further breakdown may occur
during storage.
The aluminosilicate builder material is preferably
crystalline or amorphous material having the general
formula:
N~z (AlO2)z (SiO2)y x H2O
wherein Z and Y are i~tegers of at least 6, the molar ratio
of Z to Y is in the range from 1.0 to 0.5, and x is an
integer from 15 to 264 such that the moisture content is
rom'10% to 28% by weight. The prleferred range of
alum~nosilicate is from about 12% to about 30% on an
anhydrous basis. The alumino-silicate preferably has a
particle size of from 0.1 to 100 microns~ ideally between
0.1 and 10 microns and a calcium ion exchange capacity of
at least 200 mg.calcium carbona'te/g. In a preferred
embodiment, the water-insoluble'`aluminosilicate ion
exchange material has the formula
Nal2 (A12Si2 ) 12XH2
wherein x is an integer of from 20 to 30, preferably about
27. This material is available commercially as Zeolite A.
The bleach system used essentiaily comprises a peroxy
bleach compound which is an inorganic persalt, and an
0~6
- 9 - C.1081
activator therefor. The activator makes the bleaching
more effective at lower temperatures, ie in the range from
ambient temperature to about 60C, so that such bleach
systems are commonly known as low-temperature bleach
systems and are well known in the art. The inorganic
persalt such as sodium perborate, both the monohydrate and
the tetrahydrate, acts to release active oxygen in
solution, and the activat~r therefor is usually an organic
compound having one or more reactive acyl residues, which
cause the formation of peracids, the latter providing for
a more effective bleaching action at lower temperatures
than the peroxybleach compound~ The ratio by weight of
the peroxy bleach compound to the activator is about 15:1
to about 2:1, preferably about 10:1 to about 3.5:1~
Whilst the amount of the bleach system, i.e. peroxy bleach
compound and activator may be varied between about 5% and
about 35~ by weight of the detergent compositions, it is
preferred to use about 6% to about 30% of the ingredients
forming the bleach sy~tem. Thus, the preerred level of
thc peroxy bleach compound in the composition is between
about 5.5~ and about 27% by weight, while the preferred
.I@vel o~ the activator is between about 0.5% and about 10%,
most preerably between about 0.5~ and about 3.2% by
weight.
Typical examples of suitable peroxybleach compounds
are alkalimetal perborates, both tetrahydrates and
monohydrates, alkali metal percarbonates, persilicates and
perphosphates, of which sodium perborate is preferred. The
peroxybleach compound is normally added in separately to
the detergent base powder, and it is desirable to avoid
segregation by having the particles of both of generally
the same order.
Activators for peroxybleach compounds have been amply
described in the literature, including British patents
)2~1~
- 10 - C.1081
836,988, 855,735, 907,356, 907,358, 970,950, 1,003,310 and
1,246,339, US patents 3,332,882 and 4,128,494, Canadian
patent 844,481 and South African patent 68/6,344. Specific
suitable activators include:
(a) N~diacylated and N,N'-polyacylated amines, such as
N,N,N',N'-tetraacetyl methylene diamine and
N,N,N',N'-tetraacetyi ethylene diamine,
N,N-diacetylaniline, N,N-diacetyl-p-toluidine,
1,3-diacylated hydantoins such as, for example,
1,3-diacetyl-5,5-dimethyl hydantoin and
1,3-dipropionyl hydantoini~-acetoxy-(NN,N')-
polyacylmalonamide, for example~-acetoxy-(N,N')-
diacetylmalonamide;
~b) N-alkyl-N-sulphonyl carbonamides, for example the
compounds N-methyl-N-mesyl~acetamide, N-methyl-N-
mesyl-benzamide f N-methyl-N-mesyl-p-nitrobenzami.de
and N-methyl-N-~esyl-p-methoxybenzamide;
~c) N-acylated cyclic hydrazides, acylated triazones or
urazoles, for example monoacetylmaleic acid hydrazide;
(d) O,N,N-trisubstituted hydroxylamines, such as
O-benzoyl-N,N-succinyl hydroxylamine,
O-acetyl-N,N-succinyl hydroxylamine,
O-p-methoxybenzoyl-N,N-succinyl-hydroxylamine,
O-p-nitrobenzoyl-N,N-succinyl-hydroxylamine and
O,N,N-triacetyl hydroxylamine;
(e) N,N'-diacyl-sulphurylamides, for example N,N'-
dimethyl-N,N'-diacetyl-sulphurylamide and N,N'-
diethyl-NjN'-dipropionyl sulphurylamide;
(f) Triacylcyanurates, for example triacetyl cyanurate and
tribenzoyl cyanurate;
2~
~ C.1081
(g) Carboxylic acid anhydrides, such as benzoic anhydride,
m-chloro-benzoic anhydride, phthalic anydride,
4-chloro phthalic anhydride;
.
(h) Sugar esters~ for example glycose pentaacetate;
(i) 1,3-diacyl-4,5-diacyloxy-imidazolidine, for example
1,3-di~ormyl-4,5-diacetoxy-imidazolidine,
1,3-diacetyl-4,5-diacetoxy-imidazolidine,
l,3-diacetyl-4,5-dipropionyloxy-imidazoline;
(j) Tetraacetylglycoluril and tetrapropionylglycoluril;
(k) Diacylated 2,5-diketopiperazine, such as 1,4-diacetyl-
2,5-diketopiperazine, 1,4-dipropionyl-2,5-
diketopiperazine and 1,4-dipropionyl-3,6-dimetyl-
2,5-diketopiperazine;
(1) Acylation produc~.s of propylenédiurea or 2,2-dimethyl-
propylenediurea (2,4,6,8-tetraaza~bicyclo (3,3,1)-
nonane~3,7-dione or its 9,9-dimethyl derivative),
~pecially the tetraacetyl- or the tetrapropionyl-
prop~lenediurea or their dimethyl derivatives;
(m) Carbonic acid esters, for example the sodium salts of
p-~ethoxycarbonyloxy)-benzoic acid and p-(propoxy-
carbonyloxy)-benzenesulphonic acid.
(n) Acyloxy-(N,Nl)polyacyl malonamides, such as
~-acetoxy(N,Nl)diacetyl malonamide.
The N-diacylated and N,N'-polyacylatedamines mentioned
under (a) are of special interest, particularly N,N,N',N'-
tetra-acetyl-ethylenediamine ~TAED).
21~i
- 12 - C.1081
It is preferred to use the activator in granular form,
preferably wherein the activator is finely divided as
described in our Canadian patent No 1,153,162.
Specifically, it is preferred to have an activator of an
average particle size of less than lS0 micrometers, which
gives significant improvement in bleach efficiency. The
sedimentation losses, when using an activator with an
average par~icle size of less than 150 /um, are
substantially decreased. Even better bleach performance is
obtained if the average particle size of the activator is
less than 100 /~m. However, too small a particle size
gives increased decomposition, dust-formation and handling
problems, and although particle sizes below 100 /um
can provide for an improved bleaching efficiency, it is
desirable that the activator should not have more than 20%
by weight of particles with a size of less than 50 /um.
On the other hand, the activator may have a certain amount
of particles of a size greater than 150 /um, but it
should not contain more than 5% by weight of particles
greater than 300/um, and not more than 20% by weight of
partlcles greater than 200/umr preferably greater than
150/um. It is to be understood that these particle sizes
refer to the activator present in the granules, and not to
the granules themselves. The latler have a particle size,
the major part of it ranging from 100 to 2000/um,
preferably 250 to 1000/um. ~p to 5% by weight of
granules with a particle size of greater ~han 1700/um and
up to 10% by weight of granules less than 250/um is
tolerable. The granules incorporating the activator,
preferably in this finely-divided form, may be obtained by
granulating a suitable carrier material, such as sodium
tripolyphosphate and/or potassium tripolyphospate with
activator particles of the required size. Other
granulation methods, e.g. using organic and/or inorganic
granulation aids, can also be usefully applied. The
granules can be subsequently dried, if required.
2~
- 13 - C~1081
Basically, any granulatlon process is applicable, as long
as the granule contains the activator, and as long as the
other materials present in the granule do not negatively
affect the activator~
It is particularly preferred to include in the
detergent compositions a stabiliser for the bleach system
for example ethylene diamine tetramethylene phosphonate and
diethylene triamine pentamethylene phosphonate. These
activators can be used in acid or salts form, especially in
calcium, magnesium, zinc or aluminium salt form, as
described in our Canadian patent No. 1,135,589. The
stabiliser may be present at a level of up to about 1% by
weight, preferably between about OL1~ and about 0.5% by
weight.
Apart from the components already mentioned, the
detergent compositions of the invention can contain any of
the conventional additives in the amounts in which such
materials are normally employed in fabric washing detergent
compositions. P,xamples of these additives include lather
boosters such as alkanolamides, par~icularly the
monoethanolamides derived from palm kernel fatty acids and
coconut fatty acids, lather depressants such as alkyl
phosphates and silicates, anti-redeposition agents such as
sodium carboxymethylcellulose and alkyl or substituted
alkyl cellulose ethers other stabilisers such as
ethylenediamine tetraacetic acid, fabric softening agents~
inorganic salts such as sodium sulphate and sodium
carbonate, and, usually present in very minor amounts,
fluorescent agents, perfumes, enzymes such as proteases and
amylases, germicides and colourants. In parti~ular,
compositions according to the invention may include the
salt of an alkyl phosphoric acid as suds-suppressant and a
wax as hydrophobic material as disclosed in DOS 2 701 664.
- 14 - C.1081
The fl~orescen~ agents which can be used.in the
bleachin~ detergent compositions of the invention are well
known and many such fluorescent agents are available
commercially. Specific fluorescent agents which may be
mentioned by way of example are:
(a) 4,4'di(2"-anilino-4"-morphollnotriazin-6"-ylamino)-
stilbene-2,2'-disulphonic acid and its salts,
(b) 4,4'-di(2't-anilino-4"-N-methylethanolaminotriazin-
6"-ylamino)-stilbene-2,2'-disulphonic acid and its
salts,
(c) 4,4'-di(2"-anilino-4"-diethanolaminotriazin-6"-
ylamino)-stilbene~2,2'-disulphonic acid and its salts,
(d) 4,4-di(2"-anilino~4"-dimethylaminotriazin-~"
ylamino)-stilbene-2,2'-disulphonic acid and its salts,
~e) 4,4'-di(2"-anilino-4"-diethylaminotriazin-6"-
~lamino)-stilbene-2,2'-disulphonic acid and its salts,
(f) 4,4'-di(2"-anilino-4"-monoethanolaminotriazin-6"-
ylamino)-stilbene-2,2'-disulphonic acid and its salts,
(g) 4,4'-di(2"-anilino-4"-(1-methyl-2-hydroxy)ethyl-
aminotriazin~6"-ylamino)-stiIbene-2,2'-disulphonic
acid and its salts,
(h) 4,4'-di(2"-methylamino-4"-p-chloroanilinotriazin-
6"-ylamino)-stilbene-2,2'-disulphonic acid and its
salts,
(i) 4,4'-di(2"-dietholamine-4"-sulphanilinotriazin-
6"-ylamino)-stilbene-2,2'-disulphonic acid and its
salts,
- 15 - C.1081
(j) ~,4'-di(3-sulphostyryl)diphenyl and its salts,
(k) 4,4'-di(4 phenyl-1,2,3-triazol-2-yl)-stilbene-
2,2'-disulphonic acid and its salts,
(1) 1-(p-sulphonamidophenyl)-3-(p-chlorophenyl)- ~ 2_
pyrazoline.
The salt of the acid defined in (a) above, is referred to
below as "fluorescer X".
Usually these fluorescent agents are supplied and used
in detergent compositions in the form of their alkali metal
salts, for example, the sodium salts. In addition to these
fluorescent a~3ents, the detergent composition of the
invention may contain other types of fluorescent agents as
desired. The total amount of the fluorescent agent or
agents used in a detergent composition is generally from
0.02-2~ by weight.
It ls desirable to include one or more antideposition
ag~nts in the detergent compositions of the invention, to
decrease a tendency to form inorganic deposits on washed
fabrics. The amount of any such antideposition agent is
normally ~rom about 0.1% to about 5~ by weight, preferably
rom about 0.2~ to about 2.5~ by weight of the composition.
The preferred antideposition agents are anionic poly-
electrolytes, especially polymeric aliphatic carboxylates,
or organic phosphonates.
It may be desirable to include in the compositions an
amount of an alkali metal silicate, particularly sodium
ortho-, meta- or preferably neutral or alkaline silicate.
The presence of such alkali metal silicates at levels of at
least about 1%, and preferably from about 5% to about 15%
by weight of the compositions, is advantageous in
~ C.1081
decreasing the corrosion of metal parts in washing
machines, besides giving processing benefits and generally
improved powder properties. The more highly alkaline
ortho- and meta-silicates would normally only be used at
lower amounts within this range, in admixture with the
neutral or alkaline silicates.
The compositions of the invention are required to be
alkaline, 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 o
from about 8.5 to abc,ut 11 in use in aqueous wash solution.
It is preferred in particular for domestic products to have
a pH of from about 9.0 to about 10.5 as lower pHs tend to
be less effective for optimum detergency building, and more
h:iyhly alkaline products can be hazardous if misused. The
pH is measured at the lowest normal usage concentration of
0.1% w/v of the product in water of 12H (ca), (French
permanent hardness, calcium only) at 50~C so that a
sati~actory degree of alkalinity can be assured in use at
all normal product concentrations.
The detergent compositions of the invention should be
in free-flowing particulate, eg powdered or granular form,
and can be produced by any of the technique commonly
employed in the manufacture of such washing compositons,
but preferably by slurry making and spray drying processes
to form a detergent base powder to which the ingredients of
the bleach system, and optionally also the alkali metal
tripolyphosphate are added. It is preferred that the
process used to form the compositions should result in a
product having a moisture content of not more than about
12%, more preferably from about 4~ to about 10% by weight
as the lower moisture levels have been found to be
beneficial for stability of the bleach systems employed.
~8%~
- 17 - C.1081
The invention will now be illustrated by.the following
non-limi.ting examplesO
EXAMPLE 1
The followlng base powders were prepared by spray
drying a slurry containing the specified constituents:
Comparative
Ingredient Example 1 Example A
(parts by weight)
Anionic detergent act~ve 6.5 6.5
Nonionic detergent active 3.0 ~ 3.0
Soap 5~0 5~0
STP ~5.0 35.0
Zeolite (anhydrous) 1~.0
Sodium silicate 2.0 6.0
Trirnagnesiurn dequest* - 0.12
Fluorescer X 0.2 0.2
Sodium ulpha~e, water and
minor ingredients 21.39 20.27
76.09 76.0g
*Calculated as the equivalent amount of the acid form -
Dequest 2041.
To these base powders were post-dosed the following
ingredients:
,$
o~e~ f r~ rnarf~
- 18 - C.1081
Ingredlent_ __ Exam~le 1 Comparative Example A
(parts by weight)
TAED 2.0 2.0
Sodium perborate 15.54 15.54
Dequest 2041 0.3 0.2
Sodium sulphate 6.07 6.17
23.91 23.91
These powders were then tested using the following
procedure. A Miele W484 automatic washing machine was
used, set on its 60C main wash only programme. The load
used consisted of 4 kg of unsoiled cotton and 4 standard
soiled bleach sensitive tea-stained test pieces. lOOg of
the test powder was introduced using the machine's
dispenser. The machine's intake of water (hardness 15FH)
was 20 litres. Each powder was tested three tirnes.
During the wash/ samples of the wash liquor were taken
when the wash liquor first reached 40DC. The content of
p~racetic acid and active oxygen was determlned in each
sample using conventional analytical techniques. At the
end of each wash the bleaching performance on the standard
test pieces was determined by measuring the reflectance at
460 nm on a Zeiss Elrepho photometer using a 420 nm W
interEerence filter (R 460*). The mean relectance of the
samples before washing was 32.6 and the bleaching effect is
quoted as a change in fabric reflectance, ~ R460*.
,
The results obtained were as follows:
Example 1 Example A
Peracetic acid yield
(% theoretical) 72 71
Active oxygen yield
(% theoretical) 85 84
i~ R460* 17.6 17.8
- lg C.1081
This Example demonstrates that the performance of the
STP/zeolite product ls surprising similar to the
performance of the STP only product (Comparative.Example
A), despite the lower total-phosphorus level.
EXAMPLE 2
The experiments of Example 1 were repeated with
powders made ~p according to the following formulations:
Ingredient Example 2 Comparative Example B
(parts by weight)
Anionic detergent active 6.5 6.5
Nonionic detergent active 3.0 3.0
Soap 5.0 5~0
STP 18.0
Zeolite 21.0 40.0
Sodium sllicate 6.0 6.0
Fluorescer, X 0.2 0.2
Sodlum sulphate, water
and minor ingredients14.8 13.8
74.5 74.5
Post-dosed ingredients: .
TAED 2.0 2.0
Calcium dequest* 0.3 0.3
Sodium perborate 20.0 20.0
22 3 22.3
* Calculated as the equivalent amount of the acid form -
Dequest 2041.
The procedure of Example 1 was modified in that the
experiment was carried out in a Tergotometer with a heat-up
2~
- 20 - C.1081
from 16~C to 60~C in 34 minutes. A product dosage of 5 g/l
was usedO The water hardness was 40 FH.
The results obtained were as follows:
Example ~ Comparative Example B
-
A R450* 9.8 6.0
This example demonstrates that the bleaching
performance of the STP/zeolite product is substantially
better than the zeolite only product ~Comparative
Example B).
EXAMPLE 3
To the base powders given in Example 2 and in
comparative Example B there were post-dosed the following
ingredients:
Exampl_ 3 Comparative Example C
Base powder Ex.2 Ex.B
.
TAED 3,0 3.0
Calcium dequest
Sodium perboLate 6.0 6.0
Usiny the same procedure as in Example 2, modified
only in that the water hardness was 35 FH, the results
obtained were as follows:
Example 3 Co~parative Example C
A R 460* 4.7 2.2
~8;~6
- 21 - C.1081
EXAMPLE 4
To the base powders given in Example 2 and in
Comparative Example B, there were post-dosed ~he following
ingredients: . .
IngredientExam~le 4 Comparative Exa~ple D
Base powder Ex.2. Ex.B
TAED 2.0 2.0
Calcium dequest ~ -
Sodium perboFate 15.0 15.0
Using the same procedure as in Example 3, the
following results were obtained:
Example 4 Comparative Example D
R460* 8.2 6.6
EXAMPLES 5 AND 6
__
Detergent powders were prepared according to the
following approximate formulations and were found to give
excellent results when compa~ed with similar formulations
in which sodium tripolyphosphate (STP? was the only builder
material.
~%~
- 22 - C.1081
Example No 5 6
Ingredients (~ by weight)
Anionic detergent active 6 6
Nonionic detergent active 4
STP 18 18
Zeolite 17 22
Sodium perborate 20 20
TAED . 2.3 2.3
Suds-suppressant material 1.0 1.0
Sodium polyacrylate 0.9
Water, fluorescer and other --- balance ---
convention ingredients
The suds-suppressant material used was a 1:3 mixture
of a C16 alkyl phosphoric acid ester and petroleum jelly
with a drop melting point of 54C.
EXAMPLE 7
The experiments of Example 1 were repeated with
powders made up according to the following formulations
(parts by weight):
.
- 23 - C.1081
Ingredient Example Comparative Examples
_ 7 E F
Anionic detergent active6.5 6.5 6.5
Nonionic detergent active 3.0 3.0 3.0
Soap 5.0 5.0 5.0
STP (post-dosed) 18.0 32.0
Zeolite 2100 - 30.0
Sodium silicate 6.0 6.0 6.0
Fluorescer X 0.2 0.2 0.2
TAED ) post 2.0 2.0 2.0
CalciUm DeqUest ) dosed
-Sodium perborate) 15.0 15.0 15.0
Sodium sulphate, water and
minor ingredients --------balance to 100--------
* Calculated as the eyuivalent amount of the acid form -
~equest 2041.
The procedure of Example 1 was modified in that the
experiment was carried out in a Tergotometer with a heat-up
~o~ 16C to 55C in 30 minutes. With a further 30
minutes at 55C a product dosage of 5 g/l was used. Water
hardnesses o 35FH and 60FH were used.
The results obtained were as follows:
R460* Example Comparative Example
7 E F
.
35FH 16.5 18.2 18.8
60FH 18.4 17.6 15.8
This Example demonstrates that the bleaching
performance of the composition according to the invention
(Example 7) is improved. with increased water hardness,
- 24 - C.10~1
while the bleaching performance of the compositions based
on STP only and zeolite only (Comparative Examples E and F)
is reduced with increased water hardness.
EXAMPLE 8
The experiments of Example 1 were repeated with
powders made up according to the following formulations
(parts.by weight):
Ingredient . Example Comparative Example
_ _ 8 G __
Anionic detergent active 6.5 6.5
Nonionic detergent active 3.0 3.0
Soap 5.0 5.0
STP ~po~t~-dosed) 18.0 18.0
Zeoli.te . 21.0 ~1.0
Sodium silicate 6.0 6.0
Fluorescer X 0.2 0.2
TAED ) post- 2.0
Sodlum perborate) dosed15.0 15.0
Sodlum sulphate, water and
minor ingredlents ~--------balance to 100--------
The procedure of Example l~was modified in that the
experiment was carried out in a Tergotometer with a heat-up
from 16C to 55C in 60 minutes. A product dosage of 5
g/l was used. Water hardnesses of 35FH and 60FH were
used.
The results obtained were as follows:
R460* Example Comparative Example
8 G
~ r
35F 10.8 7.7
60F 16.0 7,0
- 25 - C.1081
This Example demonstrates that the bleaching
performance of the composition according to the invention
(Example 8) is improved with increased water hardness,
while the bleaching performance of the composition
containing perborate without TAED is reduced with reduced
water hardness.
EXAMPLE 9
The following formulation represents a further
exemplary detergent composition according to the invention.
Ingredient % by weiyht
Anionic detergent active 11.0
Nonionic detergent active 5.0
Soap 5.0
STP (post-dosed) 18.0
Zeolite 17.0
Sodlum perborate 12.0
TAED 2.0
C~lclum dequest (calculated as
the equivalent Dequest 2041~ 0.3
Fluorescer X 0.2
Sodium silicate 6.0
Sodium polyacrylate 0.9
Water 10.0
Sodium sulphate and other
conventional ingredients balance
In the above examples, the anionic detergent active
used was the sodium salt of alkyl (approx. C12) benzene
sulphonate and the nonionic used was a mixture of Dobanol
45-18 and Lutensol 12EO. The soap used was a mixture of
hardened tallow soap and hardened rapeseed soap. The
zeolite used was zeolite A (ex Degussa).
