Note: Descriptions are shown in the official language in which they were submitted.
3~
-- 1 --
DETERGENT COMPOSITION
BACKGROUND OF THE INVENTION
The present invention relates to a gelatinous
or pasty detergent composition contained in a container.
Hitherto, there are used various detergents in
various forms such as powder, liquid and the like.
A powdery detergent is usually bagged or boxed,
but it causes problems in handling due to its low
apparent specific gravity and it makes transportation
cost comparatively high.
With respect to a liquid detergent on the other
hand, the detergent components essentially include a
builder because of functional reason and the builder is
in a solid form. Accordingly the liquid detergent has to
be in a form of aqueous solution in which the
concentration of effective components is about 50 % or
less (% means ~ by weight in this specification unless
otherwise specified) so that a uniform composition is
obtalned, and due to such a restriction there are
problems in handling so far.
In the circumstances, there have been under
development a gelatinous or pasty detergent composition
which has detergent component concentration higher than
that of a liquid detergent composition and accordingly is
less voluminous and easier to handle than a liquid
detergent, and which is a detergent composition contained
in a container suitable for washing clothing or the like,
but none of such detergent compositions have yet been put
into practical use except for that of the present
invention.
An object of the present invention is to solve
the above-mentioned problem and to provide a detergent
composition which is unvoluminous and easy to handle and
which has a less tendency to change in quality with a
passage of time.
SUMMARY OF THE INVENTION
2~ 3~3
In accordance with the present invention, there
is provided a detergent composition contained in a tube
or a pumping container, which is a gelatinous or pasty
detergent composition including homogeneous or dispersed
S mixture of nonionic surface active agent having fluidity
at room temperature and at least one member selected from
a group consisting of organic sulfonic acid salts and
organic sulfuric ester salts.
BRIEF EXPLANATION OF THE DRAWINGS
Fig. 1 is a plan view of a tube used in the
present invention;
Fig. 2 is a plan view of another tube used in
the present invention; and
Fi~. 3 is a sectional view of a pumping
container used in the present invention.
DETAILED DESCRIPTION
A nonionic surface active agent having fluidity
at room temperature used in the present invention is a
nonionic surface active agent preferably having a
viscosity of about 50 to about 2000 poise at room
temperature (15 to 25C). As the above agent, any
fluidic nonionic surface active agent in accordance with
the purposed application and the like of the detergent
composition can be selected and used without any
limitation as far as it is commonly used for the purpose
of emulsification, dispersion, osmosis, washing,
solubilization or the like. Particularly, preferable
examples thereof are, for instance, adduct of alkylene
oxide such as ethylene oxide, propylene oxide and
butylene oxide to active hydrogen compound having 8 to 20
average carbon atoms such as alcohol, alkylphenol, fatty
acid and alkylamine; ester of sorbitan, sucrose or the
like with fatty acid having 8 or more carbon atoms; and
the like. With respect to the above-mentioned nonionic
surface active agent, any one kind may be used alone or
alternatively two or more kinds may be used together.
Z~
- 3
Preferable content of the nonionic surface
active agent in the detergent composition is 10 to 60 %
and more preferably 25 to 45 %. The content lower than
10 % increases the apparent viscosity of gelatinized
product and consequently tends to make it difficult to
squeeze the detergent composition out of a tube or a
pumping container. On the other hand the content higher
than 60 % tends to cause a separation at high
temperatures.
The organic sulfonic acid salt and/or organic
sulfuric ester salt is a component used as a main
component of the detergent agent. As the above salt, any
organic sulfonic acid salt and/or organic sulfuric ester
salt in accordance with the purposed application and the
like of the detergent composition can be selected and
used without any limitation as far as it is commonly used
in a detergent composition for clothes or the like.
Particularly preferable examples thereof are, for
instance, organic sulfonic acid salt such as
alkylbenzenesulfonic acid salt, dialkylbenzenesulfonic
acid salt, naphthalenesulfonic acid salt and ~-
olefinesulfonic acid salt; organic sulfuric ester salt
such as sulfuric ester salt of alcohol and sulfuric ester
salt of adduct of ethylene oxide to alcohol; and the
like. With respect to the above-mentioned salt, any one
kind may be used alone or alternatively two or more kinds
can be used together. A use of organic sulfonic acid
salt provides an advantageous feature that there can be
obtained a detergent composition having improved
detergency while a use of organic sulfuric ester salt
provides another advantageous feature that there can be
obtained a well biodegradable and highly safe detergent
composition.
Preferable content of the organic sulfonic acid
salt and/or the organic sulfuric ester salt in the
detergent composition is 10 to 60 % and more preferably
25 to 45 %. The content lower than 10 % tends to cause
insufficient detergency effect. On the other hand the
;~Q~
content higher than 60 % tends to provide excessively
high viscosity of gelatinized product and consequently it
tends to be difficult to obtain soft gel.
In addition to the nonionic surface active
agent and the organic sulfonic acid salt and/or the
organic sulfuric ester salt above-mentioned, the
detergent composition contained in a container in
accordance with the present invention may optionally
include as occasion demands other additives commonly used
as additives for a detergent composition such as surface
active agent other than the nonionic surface active
agent, the organic sulfonic acid salt or the organic
sulfuric ester salt (hereinafter referred to as other
surface active agent); builder; enzymes; fluorescent
material; peroxide; perfume: solvent; and the like.
Examples of the above-mentioned other surface
active agent are, for instance, soaps such as sodium
oleate, sodium laurate, potassium oleate and sodium
stearate; amphoteric surface active agent such as AMOGEN
K (alkylbetaine amphoteric surface active agent available
from DAI-ICHI KOGYO SEIYAKU CO., LTD.); and the like.
Preferable content thereof in the detergent composition
is normally 15 % or lower.
Examples of the builder are, for instance,
sodium tripolyphosphate, zeolite, soda ash, sodium
polyacrylate and the like. Preferable content thereof in
the detergent composition is normally 5 to 50 %.
With respect to the enzymes, enzymes which
exhibit their inherent enzyme activities in washing
process are preferably used. Examples thereof being
classified by enzyme reactivity are, for instance,
hydrolases, hydrases, oxidoreductases, desmolases,
transferases, isomerases and the like and any of them can
be employed in the present invention. Hydrases are
particularly preferable and detailed examples thereof are
protease, esterase, carbohydrase and nuclease.
Preferable amount of enzymes in the detergent composition
is normally 0.5 to 2.0 %.
Examples of the fluorescent material are, for
instance, 2-(stilphenyl) naphthothiazole derivative,
4,4'-bis(triazole-2-yl) stilbene derivative,
bis(triazinylamino) stilbene disulfonic acid derivative,
4,4'-bis(2-sulfostyryl) biphenyl salt, 4,4'-bis(4-chloro-
3-sulfostyryl) biphenyl salt and the like. Preferable
amount of the fluorescent material in the detergent
composition is normally 1.0 to 4.0 %.
Examples of the peroxide are, for instance,
sodium perca~bonate and the like. Preferable amount of
the peroxide in the detergent composition is normally 1.0
to 4.0 %.
Further components such as perfume, coloring
agent and the like may also be included in the detergent
composition and preferable amount thereof in the
detergent co~position is normally 1.0 to 4.0 %.
With respect to the solvent, for example there
can be used, as the occasion may demand, water,
glyceline, ethylene glycol, diethylene glycol monobutyl
ether and the like.
The detergent composition to be contained in a
tube or a pumping container in accordance with the
present invention is a gelatinous or pasty composition
including homogeneous or dispersed mixture of nonionic
surface active agent having fluidity at room temperature
and at least one member selected from a group consisting
- of organic sulfonic acid salts and organic sulfuric ester
salts.
The term homogeneous or dispersed mixture used
in this specification means a mixture wherein all
components are unformly mixed including a mixture wherein
all components are homogeneously dissolved or a mixture
wherein all components are uniformly dispersed.
The above-mentioned detergent composition used
in the present invention has a gelatinous or pasty
form. In the detergent composition, all components may
be homogeneously dissolved or may be uniformly
dispersed. Particularly, a composition wherein all
3Q;~
components are homogeneously dissolved is preferable
because it does not easily cause a separation.
With respect to a tube or a pumping container
to be filled with the detergent composition, there are no
particular limitations for material, structure or
configuration thereof and there can be used those
described below for example.
Material of the tube may be plastics, metal or
the like and there can be used a laminated tube having a
wall of plural-layer structure as well as a tube having a
wall of single-layer structure. The tube may have a
cylindrical configuration having a round or an elliptical
cross section for example, and the tube may be equipped
with a cap such as a screw cap or unscrew cap. For
example, there are preferably used the tube 1 and the
tube 2 respectively illustrated in Fig. 1 (plan view) and
Fig. 2 (plan view).
Preferable material of the pumping container
may be synthetic resin including polyolefine such as
polyethylene or polypropylene; polyethylene
terephthalate; and the like. However, under certain
circumstances there may also be employed metal or paper
suitably processed to prevent the gelatinous or pasty
composition from permeating. With respect to the
structure and the configuration, the pumping container
preferably has a tubular shape like one employed for
tooth paste container or the like, for example those
disclosed in Japanese Unexamined Utility Model
Publications No. 34641/1979, No. 38783/1981, No.
46572/1981, No. 100378/1981, No. 121677/1981, No.
44041/1982, No. 74168/1982, No. 164079/1982, Japanese
Unexamined Patent Publications No. 68367/1982, No.
68368/1982 and the like. For example, the pumping
container 3 illustrated in Fig. 3 is preferably used.
Next, there is explained a process for
preparing the detergent composition to be contained in a
container in accordance with the present invention.
~here are no particular limitations in
2~3~
-- 7
preparing process of the above-mentioned detergent
composition. A preferable preparing process involves a
step of neutralization of organic sulfonic acid and/or
organic sulfuric ester in the presence of nonionic
surface active agent (in this neutralizing step the
nonionic surface active agent exhibits liquid behavior),
and then there is prepared a homogeneous or dispersed
mixture of nonionic surface active agent having fluidity
at room temperature and at least one member selected from
a group consisting of organic sulfonic acid salts and
organic sulfuric ester salts. Thereafter, other optional
components are added as occasion demands in accordance
with a common procedure to the obtained mixture. This
process is preferable because a desired gelatinous or
pasty composition can be easily obtained.
Examples of the above-mentioned organic
sulfonic acid or organic fulfuric ester are acid
components which form the previously-mentioned organic
sulfonic acid salt or organic sulfuric ester salt.
Typical examples of the neutralizer used in the
above-mentioned neutralizing step are caustic soda,
caustic potash, lithium hydroxide, ammonia,
monoethanolamine, triethanolamine and the like.
Next there is explained a method of filling a
tube or a pumping container with the detergent
composition obtained in the above-mentioned manner.
There are no particular limitations in filling
a tube with the detergent composition. For example,
there can be employed a method like a common and known
method of filling a tube with tooth paste, wherein the
gelatinous or pasty detergent composition is put into a
filling device comprising a cylinder of a certain
capacity, then the composition is introduced into the
tube through the unsealed bottom end thereof, and finally
the tube bottom end is sealed in accordance with a
certain sealing method.
Also, there are no particular limitations in
filling a pumping container with the detergent
3~L~
composition. For example, there can be employed a method
like a common and known method of filling a pumping
container with tooth paste, wherein the gelatinous or
pasty detergent composition is put into a filling device
comprising a cylinder of a certain capacity, then the
composition is intro~uced into the pumping container
through the bottom opening thereof, and finally the
container bottom is sealed by means of a certain cover or
plug.
The detergent composition contained in a
container in accordance with the present invention is
advantageous because it is unvoluminous and easy to
handle and because it does not tend to become dry or to
cause deterioration of its detergency even in case that
it has been stored for a long period. Therefore, the
detergent composition of the present invention is
especially suitable for application as a pocket type
detergent, a detergent for washing small clothes in a
bath room or at a washstand, a detergent for partial
washing and the like.
The present invention is more specifically
described and explained by means of the following
Examples. However, it is to be understood that the
present invention is not limited to the Examples, and
various changes and modifications may be made in the
present invention without departing from the sprit and
scope thereof.
Examples 1 to 3
Each of examples having respective formulations
shown in Table 1 was prepared in the following manner.
Nonionic surface active agent was put into a mixing
vessel, then linear alkylbenzene sulfonic acid having
linear alkyl group having 8 to 13 carbon atoms and/or
linear alkylsulfuric ester having linear alkyl group
having 12 to 13 carbon atoms were added thereto, and a
uniform mixture was prepared by mixing sufficiently and
concurrent heating tO a temperature of 65 to 70C.
2~3~
g
Thereafter, solid caustic soda (in flaky shape and of 99
% or higher purity) in an amount counterbalancing the
acid number of the mixture was gradually added for
neutralization of the mixture. When pH of the mixture
was controlled to 10+0.5, there was obtained a llquid,
turbid in white, uniform mixture containing surface
active agent. Thereafter, other additive components than
those above-mentioned were added thereto in order
indicated in the Table 1, then the product was collected
from the vessel after sufficient uniform mixing. The
collected product was naturally cooled to a temperature
of 25 to 30C and there was obtained a long-term-stable
detergent composition in which all components were
uniformly dispersed.
Table 1
... ... _ _
Part~ by weight
Component
Ex. 1 Ex. 2 Ex. 3
.
Nonionic surface active agent 135 20 30
Linear alkylbenzene sulfonic 10 20 5
acid sodium salt 2
Linear alkylsulfuric ester 5
sodium salt 3
1 Soap*4 3.0 5.0 5.0
2 Sodium carbonate 20 22.0 22.0
3 Sodium silicate 7 8 8
4 Sodium aluminosilicate 10 15 15
- continued
-- 10
- continued - ~
_ _
Parts by weight
Component
Ex. 1 Ex. 2 Ex. 3
_ _ _ _
5 Sodium sulfate 6 6 6
6 Glyceline - - 5
7 Water 4 4 4
-
(Notes) *l : Polyoxyethylene nonylphenyl ether
(~.6 mol EO addition product)
*2 : Mixture having 8 to 13 carbon atoms in
linear alkyl group
*3 : Mixture having 12 to 13 carbon atoms in
linear alkyl group
*4 : Sodium salt of coconut oil fatty acid
1 to 7 indicate the order of addition.
Apparent specific gravity, solubility,
25 viscosity, stability in appearance, detergency and
squeezability (fluidity and controllability in squeezing
operation out of a tube) of the obtained pasty detergent
composition were evaluated respectively in accordance
with the following methods. The obtained results are
shown in Table 3.
(Apparent specific gravity)
Weight per fixed volume is measured with a
particular container specified in JIS K 3362.
(Solubility)
Several washing liquid mixture having detergent
concentration of 0.133 % are prepared using 30 ~ of water
3~01
(water from city water supply) at 5C, 10C, 15C or 20C
and 40 9 of the detergent composition in electric washing
machine (Hitachi, double sink type washing machine, model
PS-753, available from Hitachi Ltd.). Into the washing
liquid 3 kg of knit underwear is immersed, then the
washing machine is operated for 10 minutes in the mode of
the standard water stream. After the operation,
alkalinity of the washing liquid mixture ~free alkalinity
in accordance with ISO international standard 4314-1977)
is measured and solubility ratio defined by the following
formula is calculated.
Alkalinity of each washing
liquid mixture using water
at respective specified
temperature after 10 minutes
washing operation
Solubility ratio (%~ = - . x 100
Alkylinity of completely
dissolved reference washing
liquid mixture having
detergent concentration of
0.133
(Viscosity)
Measurement is conducted using HELIPATH
viscosity meter suitable for viscosity measurement for
gelatinous products such as tooth paste, gelatinous
shampoo and the like.
(Stability in appearance)
200 mQ of each gelatinous detergent composition
contained in a tube (a tube 1 shown in Fig. 1 or a tube Z
shown in Fiq. 2 each having internal volume of 200 m~ and
outlet diameter of 12.9 mm) is stored for 3 months at an
atmospheric temperature between -5C and 40C, and
thereafter occurrence of separation is inspected and
evaluated in accordance with the following criteria.
2~i~3Q~
- 12
Gr. A: No change observed
Gr. B: Separation observed to some extent
Gr. C: Separation observed
(Detergency)
1 ~ of aqueous detergent solution having
concentration of 0.1 % is prepared by adding the
detergent composition to water.
Separately, 12 pieces of arti~icially dirtied
cloths are prepared in advance in a manner wherein sample
cloths (cottom shirtings and No. 60 broad cloth
(cotton/polyester = 65/35) each having a size of 10 cm x
10 cm) are uniformly mixed with oil component comprising
cotton seed oil: 60 ~, cholesterol: 10 %, palmitic acid:
10 ~, liquid parafin: 5 % and solid parafin: 5 % and with
carbon black (THE JAPAN OIL CHEMISTS' SOCIETY) to make
the sample cloths dirty.
12 pieces of the artificially dirtied cloths
are put into the above-mentioned aqueous detergent
solution (1 Q) and additionally appropriate numbers of
clean cloths having the same size are also put thereinto
so that bath ratio becomes 1/60, then washing operation
is conducted using Terg-O-Tometar at 100 rpm. The
duration of the washing operation is 10 minutes, water
hardness is 8DH, water temperature is 15C and the
washing operation is followed by a 25 minute long rinsing
operation using water from city water supply.
Reflectances of sample cloths are measured by
self-recording colorimeter (available from Shimadzu
- Corporation) respectively before mixing with dirt, after
mixing with dirt before washing and after washing. Based
on the measured reflectances, each detergent efficiency
defined by the following formula is calculated and
subsequently an average detergent efficiency of 12 pieces
of sample cloths is calculated.
Z~3101
- 13
Detergent efficiency (%)
Reflectance after washing _ Reflectance
just before washing
_ ___ _ x 100
Reflectance before mixing with dirt
Squeezability)
100 sets of the tube contained detergent
composition are prepared using the tube 1 shown in Fig. 1
or the tube 2 shown in Fig. 2. Each of 10 woman
evaluators opens a tube outlet, and using the thumb and
the fifth finger of her left hand she presses the middle
portion of the tube to squeeze the gelatinous detergent
composition out of the tube outlet. Each of 10
evaluators tests 10 tubes and evaluates the squeezability
in accordance with the following criteria.
Gr. A: Squeezable by weak force
Gr. B: Slightly hard
Gr. C: Too hard to squeeze
Gr. D: Excessively soft and discharging amount is
uncontrollable.
Comparative Example 1
A comparative composition having the
formulation shown in Table 2 was prepared in the
following manner. Nonionic surface active agent was put
into a mixing vessel, then sodium salt of alkyl sulfuric
ester was added thereto, and a uniformly dispersed
mixture was prepared by sufficient mixing and concurrent
heating to a temperature of 65 to 70C. Thereafter,
other additive components were added in order indicated
in the Table 2 and concurrently mixing and dispersion are
performed by mixing, then the product was collected from
the vessel. The collected product was naturally cooled
to a temperature of 25 to 30C and there was obtained a
gelatinous detergent composition which was similar to the
compositions prepared in Examples 1 to 3 as far as its
.
3~L~
- 14
appearance was concerned.
The same measurements as employed in Examples 1
to 3 were conducted to evaluate the properties of tne
obtained detergent composition. The measurement results
are shown in Table 3.
Table 2
Parts by weight
Components
Com. Ex. 1
Nonionic surface active agent 5 70
Alkyl sulfuric ester salt 6 5
1 Sodium carbonate 10
2 Sodium silicate 2
3 Sodium alminosilicate 10
4 Water 3
0 (Notes) *5 : NOIGEN ET 135 ~name of product available
from DAI-ICHI KOGYO SEIYAKU CO., LTD.)
*6 : MONOGEN Y-500 ~name of product available
from DAI-ICHI KOGYO SEIYAKU CO., LTD.)
1 to 4 indicate the order of addition.
Comparative Example 2
A powdery detergent composition was prepared by
spray-drying the detergent composition prepared in
Example 1.
With respect to the powdery detergent
composition, average particle diameter was measured and
apparent specific gravity, solubility and detergency were
measured in the same manner as employed in Example 1.
The measurement results are shown in Table 3.
Comparative Example 3
100 parts by weight of the powdery detergent
- 15 ~
composition prepared in Comparative Example 2 was further
subjected to compaction into a circular column shape
having a diameter of 3 mm using Extruder (available from
Fuji Paudaru Kabushiki Kaisha). To 100 parts by weight
of the compacted powdery detergent composition there was
added 10 parts by weight of aluminosilicate salt having
an average particle diameter of 2.7 ~m, and concurrently
crushing and granulation were conducted using Fitzmill
(available from Fitzpatrick (U.S.A.)) equipped with a
screen having sieve opening size oE 1.5 mm.
With respect to the obtained detergent
composition, average particle diameter was measured and
apparent specific gravity, solubility and detergency were
measured in the same manner as employed in Example 1.
The measurement results are shown in Table 3.
3~
-- 16
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As demonstrated in Table 3, the detergent
composition contained in a container in accordance with
the present invention was unvoluminous and excellent in
solubility, detergency and stability, and has desirable
viscosity and an advantageous feature that squeeæing
operation out of a tube or a pumping container is easily
carried out.
As described hereinbefore, the detergent
composition contained in a container in accordance with
the present inYention is, compared with prior art
detergent composition, unvoluminous, easy to handle,
stable in quality against a long-term-storage and
satisfactory in detergency.
