Specification
FORM - 2
THE PATENTS ACT, 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See Section 10 and Rule 13)
A NON-TOWER DETERGENT COMPOSITION
HINDUSTAN UNILEVER LIMITED, a company incorporated under
the Indian Companies Act, 1913 and having its registered office
at 165/166, Backbay Reclamation, Mumbai -400 020, Maharashtra, India
The following specification particularly describes the invention and the manner in which it is to be performed.
FIELD OF INVENTION
The present invention relates to granular detergent compositions made by Non-Tower-Route (NTR).
BACKGROUND AND RELATED ART
Any discussion of the prior art throughout the specification should in no way be considered as an admission that such prior art is widely known or forms part of the common general knowledge in the field.
Generally, granular detergent compositions are made by spray-drying process, or by an agglomeration process. The agglomeration process is also known as "NTR" (Non-Tower Route) process. Such a process typically involves in-situ neutralization of a precursor of an anionic surfactant, for example, LABSA (Linear Alkylbenzene sulphonic acid) in the presence of an alkali (generally Sodium carbonate, also known as Soda Ash); followed by granulation in a high, or, a medium speed mixer or densifier; typically in the presence of co-surfactants and other ingredients. NTR process is suitable for making granular detergent compositions containing high levels of surfactants, and having Bulk Density (BD) in the range of 500 to 1200 kg/m3.
A known drawback of granular detergent compositions made by NTR process is that uniformity in distribution of the anionic surfactants (the most common is Sodium salt of linear Alkylbenzene Sulphonate, commonly abbreviated as Na-LAS) in the granules, across the range of particle sizes, i.e. £100 μm, 100 μm, 250 μm, and so on, is relatively lower. Yet another drawback is that, in-use, when the granules are dosed into water; the amount of anionic surfactants which is released in the wash-liquor in the first 30 to 120 seconds is relatively lower. In general, it has been observed that oversize particles carry higher amounts of surfactants.
When a granular detergent composition is dosed into a bucket of water, the kinetics of the initial dissolution of the granules; especially that of the anionic surfactants in the granules, plays an important role. Consumers expect higher foam and soapy-feel in the first 30 to 120 seconds. These attributes are directly proportional to the amount of anionic surfactants which is released in the wash-liquor. When the uniformity in the distribution of the anionic surfactants in the granules is relatively lower; then some granules contain higher amount of anionic surfactants, while some have very low or no anionic surfactant. In this event, the initial foam and soapy-feel is sub-optimal; as all particles may not contribute to the same extent towards foam and soapy-feel.
Thus, there is a need for granular detergent compositions, which are made by NTR process, in which the distribution of the anionic surfactant, particularly linear Alkylbenzene sulphonates across the granules of varying particle size ranges is relatively more uniform. There is also a need for granular detergent compositions that are made by NTR process, in which, a relatively higher percentage of the anionic surfactants, particularly linear Alkylbenzene sulphonates is released into the wash-liquor in the first 30 to 120 seconds.
One of the most common and obvious ways to achieve the benefits mentioned above, is to increase the content of the anionic surfactants in the formulation. While increased levels of anionic surfactants are known to provide some benefits in terms of cleaner and whiter fabrics; a known drawback of the same is that the higher surfactant levels lead to formation of higher levels of agglomerated granules, primarily due to non-uniform distribution of the anionic surfactants. Such agglomerated granules do not dissolve easily; therefore, the anionic surfactant contained within such granules does not get released quickly. It is desirable to reduce the amount of anionic surfactants in the compositions.
US2003/0060392 (Unilever) exemplifies granular detergent compositions containing a relatively high amount (>15 wt%) of anionic surfactant, such as Na-LAS, Sodium carbonate and Sodium sulphate, with a ratio of Sodium sulphate to Sodium carbonate in the range of 1:0.52 to 1:0.68. This publication describes the
use of non-surfactant acid salts formed in-situ, such as organic and inorganic acids, to lower the bulk density of the powders and to improve powder properties, such as better flow, less stickiness and smaller particle size. The present inventors have found that when the anionic surfactant content is relatively higher, such as in this publication, it leads to the formation of higher levels of agglomerated granules.
WO01/21757 A1 (Unilever PLC) describes detergent compositions which include a Calcium-tolerant anionic surfactant, such as Alpha-Olefin sulphonates, for improved flow properties and good detergency. In the exemplified powders, the ratio of Inorganic salt to Sodium carbonate is 1:0.53. The present inventors have found that when the ratio is relatively lower, the percentage of anionic surfactant that gets released into the wash-liquor remains relatively lower.
US2008/0287339 A1 (P&G) describes detergent additive extrudates containing alkyl benzene sulphonate having improved physical stability, dissolution property abd ease of processing. The extrudates contain water-soluble carboxylate containing polymers, a water-soluble inorganic salt and from 2-10 wt% moisture. This publication also describes powder detergent compositions that contain the extrudates.
Another method of achieving the above benefits involves admixtures of spray-dried detergent powders and NTR granules. One such process, and compositions obtained therefrom, has been disclosed in Procter & Gamble's Publication number WO9634084A1.
This approach relies upon the benefits of a spray-dried detergent powder to achieve faster dissolution, which inherently dissolve easily. However, the drawbacks of NTR powders remain un-addressed.
OBJECTS OF THE INVENTION
It is an object of the present invention to overcome or ameliorate at least one of the disadvantages of the prior art.
It is an object of the present invention to provide a granular NTR detergent composition, in which, distribution of the anionic surfactant, particularly linear Alkylbenzene sulphonate across the granules of varying particle size ranges is relatively more uniform.
It is an object of the present invention to provide a granular NTR detergent composition having a relatively lower amount of anionic surfactant, particularly linear Alkylbenzene sulphonate, in which, a relatively higher percentage of the anionic surfactant is released into the wash-liquor in the first 30 to 120 seconds.
Other objects of the present invention will become apparent to those skilled in the art by reference to the specification.
The present inventors have surprisingly found that the above objects may be met with a granular NTR detergent composition that includes a combination of an anionic surfactant, a halide or sulphate salt of an alkali metal, a carbonate builder, and a flow-aid with a particular ratio between the salt and the carbonate builder.
SUMMARY OF THE INVENTION
The present invention provides a granular NTR detergent composition comprising:
(i) 5 to 14 weight% anionic surfactant;
(ii) 40 to 50 weight% halide or sulphate salt of an alkali metal;
(iii) 24 to 55 weight% carbonate builder; and,
(iv) 0.1 to 15 weight% flow-aid whose Liquid Carrying Capacity is from 10 to
200 g non-ionic/100 g flow-aid, preferably from 35 to 75 g non-ionic/100 g
flow-aid, (v) wherein ratio of (ii) to (iii) is in the range of 1:0.6 to 1:1.1.
The term "comprising" is meant not to be limiting to any subsequently stated elements but rather to encompass non-specified elements of major or minor functional importance. In other words the listed steps, elements or options need not be exhaustive. Whenever the words "including" or "having" are used, these terms are meant to be equivalent to "comprising" as defined above.
Except in the operating and comparative examples, or where otherwise explicitly indicated, all numbers in this description indicating amounts of material ought to be understood as modified by the word "about".
It should be noted that in specifying any range of concentration or amount, any particular upper concentration can be associated with any particular lower concentration or amount.
For a more complete understanding of the above and other features and advantages of the invention, reference should be made to the following detailed description.
DETAILED DESCRIPTION
The term "weight%" wherever used in this specification means "percentage by weight".
The invention relates to a granular NTR detergent composition comprising:
(i) 5 to 14 weight% anionic surfactant;
680 18.0 7.0 13.0 10.0 10.0 11.0
500 17.0 7.0 11.0 6.0 8.0 9.0
250 11.0 4.0 8.0 8.0 6.0 5.0
150 8.0 4.0 8.0 7.0 6.0 8.0
<100 6.0 9.0 9.0 10.0 8.0 9.0
Range (approximate) 12.0 5.0 5.0 3.0 4.0 6.0
The data in the above table indicates a significantly lower difference between the maximum and minimum Na-LAS content in the various size fractions of the compositions according to the invention; when compared to that of Control-1. In other words, the distribution of Na-LAS across the granules of various particle size ranges is relatively more uniform.
EXAMPLE-3
Further compositions (Ex-5, Ex-6 and Ex-7) within the invention were made; final formulations of which were as per table-6 below.
Table-6
lngredients/weight% Control-2 Ex-5 Ex-6 Ex-7
Na-LAS 11.0 5.0 7.5 7.0
Alpha Olefin sulphonate - 2.5 - -
C-12-7EO (Non-ionic surfactant) - - - 0.7
Sodium carbonate 24.0 35.0 35.0 35.0
Sun dried Sodium chloride 14.0 46.0 47.0 47.0
Sodium chloride PVD 26.5 - - -
Dolomite 8.0 - - -
Microfine Dolomite 11.0 5.0 5.0 5.0
Colored Speckles 1.0 1.0 1.0 1.0
Fluoroescer 0.05 0.05 0.05 0.05
perfume, moisture NDOM, other minors to 100.0 100.0 100.0 100.0
Ratio 1:0.59 1:0.76 1:0.74 1:0.74
The data on percentage anionic surfactant released in the wash-liquor in 30 to 120 seconds is given in table-7 below.
Table-7
Time/seconds Control-2 Ex-5# Ex-6 Ex-7
Na-LAS in was h-liquor as % of total amount in the composition
30 30.0 78.0 72.0 88.0
60 51.0 83.0 82.0 95.0
90 67.0 86.0 85.0 100.0
120 78.0 89.0 87.0 100.0
Note:
# for Ex-5, the data indicates combined value for Na-LAS and Alpha Olefin
Sulphonate.
The data in the above table further establishes that a relatively higher percentage of anionic surfactant is released in the wash-solution in the case of compositions Ex-5, Ex-6 and Ex-7.
Experiments on cleaning efficacy
Standard WFK® 20D and AS-12® fabric swatches were washed with a 5 gpl (grams
per litre) solution of the compositions Ex-5, Ex-6 and Ex-7 of table-7, and the
detergency scores, in terms of reflectance value of the fabric, were recorded by following the standard Terg-O-tometer Method.
The principle involved in the above method is to wash a synthetically soiled fabric piece under a specific concentration of the detergent, and specific test conditions. The reflectance readings R460* (UV excluded) are then recorded for the un-washed, i.e. initial, and the post-wash fabrics. Detergency is then expressed as percentage of the soil that gets removed.
Requirements
1) Synthetically soiled fabric swatches
2) Terg-O-tometer
3) Reflectance Spectrophotometer
Test Conditions
(i) Wash Mode Terg-O-tometer
(ii) Temperature Ambient
(iii) Fabric: Liquor ratio 1:100
(iv) Wash time 10 minutes
(v) Detergent Concentration 5 gpl
(vi) Water hardness 24° FH - Ca+2: Mg+2 (2:1)
(vii) RPM of Terg-O-tometer 100
The test method involved the following steps:
(i) Soiled test pieces were cut into swatches of 7cm x 7cm. Five replicate
samples of swatches were taken for each formulation to be tested. (ii) The R460* value was then measured for each test piece using a
Reflectance Spectrophotometer. (iii) The required quantity of the detergent solution was then dosed into each
jar of the Terg-O-tometer to maintain a fabric: liquor ratio of 1:100. (iv) The five test swatches were then added, one-by-one, into each jar. (v) The Terg-O-tometer was then operated for 10 minutes at 100
strokes/minute.
(vi) The test swatches were then transferred into a large beaker, and rinsed three-times with 24 °FH water at fabric: liquor ratio of 1:10.
(vii) The swatches were then squeezed dry.
(viii) The reflectance (R460*) of the washed and dried swatches was then measured.
Calculation
The detergency value is calculated by the following equation:
% Detergency = Rw-Rs x 100 Ro-Rs
Where;
Rw = reflectance after washing
Rs = reflectance of soiled fabric
R0 = reflectance of clean unsoiled fabric
The results are presented in table-8 below. Tabfe-8
Detergency score for \NFK® 20D Detergency / score 1 orFS-12®data
Control-2 Ex-5 Ex-6 Ex-7 Control-2 Ex-5 Ex-6 Ex-7
80.71 86.43 79.73 86.02 45.66 41.56 43.75 44.70
79.85 84.08 84.61 85.10 44.70 44.57 46.24 48.27
80.92 87.34 83.71 83.95 42.47 46.44 46.18 49.93
82.24 85.84 82.24 83.54 41.17 45.22 48.92 44.72
83.05 83.90 81.63 85.26 38.33 43.52 41.18 55.51
81.36 85.52 82.38 84.77 42.47 44.26 45.26 48.62
Data in the above table indicates that the detergency scores for the compositions Ex-5, Ex-6 and Ex-7 were either comparable to, or were higher than Control-2. This was un-expected, as Control-2 composition had relatively higher anionic surfactant content.
Consumer Panel Study
The benefits of a detergent composition are best judged by a consumer.
Therefore, in order to ascertain reactions of the consumers to the benefits of the
compositions, a consumer-panel test which included trained volunteers, was set-up. They used the compositions in the usual manner in which hand-wash detergent powders are used. Each Panellist was also asked to use Control-2, after which the Panellists were asked to rate the compositions Ex-5, Ex-6 and Ex-7, as being "less", "at parity", or "more" on various product/functional attributes, when compared to the Control-2. A questionnaire was given to each panellist and their responses were collected. The averaged-out responses are presented in table-9 below.
Table-9
Attribute Ex-5 Ex-6 Ex-7
oversize" particles less less less
uniformity# more more more
softness# more more Parity
free-flow# more more more
tendency to form lumps* less less less
clings to hands* less parity Parity
density* less dense less dense less dense
perfume impact* parity parity Parity
transparency in solution more more more
un-dissolved granules* less less less
soapiness in solution more more more
speed of lather (slow/parity or fast) parity parity Slow
amount of lather* parity parity less
density of lather# parity parity less
soapy lather* more more more
un-dissolved fines after five minutes* less less less
speed of dirt removal* parity parity Parity
dirt in water after 30 minutes soak* parity parity Parity
soapiness on fabric* less less less
clean WFK® 10D fabric # Parity Parity Parity
clean WFK® 20D fabric # Parity Parity Parity
Note: For * parameters - "less" was preferable
For # parameters - "more" was preferable
Data in the above table indicates that the compositions Ex-5, Ex-6 and Ex-7 were either superior to, or at-par with the Control-2.
It will be appreciated that the illustrated examples provide a granular NTR detergent composition, in which the distribution of the anionic surfactant; particularly linear Alkylbenzene sulphonates, across the granules of varying particle size ranges, is relatively more uniform.
It will be appreciated that the illustrated examples provide a granular NTR detergent composition having a relatively lower amount of anionic surfactant, particularly linear Alkylbenzene sulphonates, and which is made by NTR process; in which a relatively higher percentage of the anionic surfactant is released into the wash-liquor in the first 30 to 120 seconds.
It should be understood that the specific forms of the invention herein illustrated and described are intended to be representative only as certain changes may be made therein without departing from the clear teachings of the disclosure.
We claim:
1. A granular non-tower detergent composition comprising:
(i) 5 to 14 weight% anionic surfactant;
(ii) 40 to 50 weight% halide or sulphate salt of an alkali metal;
(iii) 24 to 55 weight% carbonate builder; and,
(iv) 0.1 to 15 weight% flow-aid whose Liquid Carrying Capacity is
from 10 to 200 g non-ionic/100 g flow-aid, wherein ratio of (ii) to (iii) is from 1:0.6 to 1:1.1.
2. A granular non-tower detergent composition as claimed in claim 1 wherein said salt of alkali metal is Sodium chloride or Sodium sulphate.
3. A granular non-tower detergent composition as claimed in claim 2 wherein said Sodium chloride is sun-dried or partially vacuum-dried.
4. A granular non-tower detergent composition as claimed in claim 2 or 3 wherein particle size of Sodium chloride is in the range of 150 to 500 urn.
5. A granular non-tower detergent composition as claimed in any one of the preceding claims wherein said Liquid Carrying Capacity is from 35 to 75 g non-ionic/100 g flow-aid,
6. A granular non-tower detergent composition as claimed in any one of the preceding claims wherein said anionic surfactant is selected from Alkylbenzene sulphonates, Alkylarylbenzene sulphonates, Alpha-Olefin sulphonates, Secondary Alkane Sulphonates, Fatty Acid Ester Sulphonates, Primary Alkyl Sulphates, Fatty Alcohol Sulphates, Secondary Alcohol Sulphates, or Alkyl Ether Sulphates.
7. A granular non-tower detergent composition as claimed in any one of the preceding claims wherein said flow-aid is selected from Calcite, precipitated Calcite, Zeolite, precipitated Silica, talc or microfine Dolomite.
8. A granular non-tower detergent composition as claimed in any one of the preceding claims wherein said composition comprises 0.1 to 6 weight% neutral, alkaline or meta-silicates.
9. A granular non-tower detergent composition as claimed in any one of the preceding claims wherein its reserve alkalinity is in the range of 16 to 16.5 g of Sodium hydroxide per 100 g of the composition.