Title of Invention

SOLUBLE SPECKLE GRANULE

Abstract Use of a soluble speckle granule in a particulate laundry detergent composition, characterised in that the granule comprises a clay mineral carrier material and a mica pigment. Preferably the granule further comprises sodium tripolyphosphate and it may be provided with a water-soluble polymer coating.
Full Text C4427/C
FORM - 2
THE PATENTS ACT, 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See Section 10 and Rule 13)
SOLUBLE SPECKLE GRANULE
HINDUSTAN UNILEVER LIMITED, a company incorporated under the Indian Companies Act, 1913 and having its registered office at Hindustan Lever House, 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

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SOLUBLE SPECKLE GRANULE
The present invention relates to a soluble speckle granule for use in granular detergent compositions.

Particulate detergent compositions may contain coloured speckles. This may be achieved by adding coloured dyes. However, such dyes may cause stains on fabrics being washed. Speckles may alternatively contain pigments such as copper phthalocyanine. Although chosen for their poor fabric
substantivity, pigments may nevertheless stain some fabrics and may be environmentally unsound.
WO 00 61718 (Procter & Gamble) suggests that the problems associated with use of dyes, particularly aqueous dyes, can be overcome by use of a coating of particles that reflect light. Mica or titanium dioxide coated granules are described. The exemplified base granules may be sodium citrate dihydrate, sodium carbonate or sodium sulphate. The coated granule may be formed by dusting a particulate material with the light reflecting component and then optionally applying binding material to the dusted particle. It is stated that the alternative process of mixing the light reflecting material with the base ingredients is less preferred because then only a part of the light reflecting material will be at the surface of the particle.
WO 00 27980 (Procter & Gamble) discloses a cleaning composition speckle particle which comprises a solid material which is coloured with a colorant, the particle having a sparkle index of at least 5%, and a transparency

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index of at least 5%. The speckle particle preferably comprises a crystalline hydrated inorganic salt, a crystalline organic acid salt, a crystalline organic salt, a crystalline surfactant, a saccharide, or mixtures thereof. It is particularly preferred that the particle comprises
trisodium citrate dihydrate, most preferably coloured with a dye. Other ingredients commonly employed in detergent compositions that are crystalline materials, such as crystalline silicate, including crystalline layered silicate may also be useful, according to this disclosure.
According to the present invention there is provided a soluble speckle granule comprising at least one clay mineral carrier material coated in mica particles. This provides an attractive, different and robust speckle for use in
detergent compositions. Preferably, the granule comprises from 0.5 to 1.5 wt% mica.
The speckle granule preferably has an average particle size of from 0.8 mm to 3.0 mm. More preferably, it has an average particle size of from 1.0 mm to 2.0 mm.
To improve the speed of dispersion of the granule in wash liquor it is advantageous to include a soluble builder salt admixed with the clay in the granule. The preferred material is sodium tripolyphosphate (STP) and it is preferably mixed with the clay mineral in a ratio clay: STP from 1:2 to 5:1, most preferably about 1:1.

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The Clay Mineral
The clay mineral carrier is preferably one or more clays selected from bi-layer clays (e.g. china clay and halloysite) which may be dioctahedral clays (such as kaolin) or trioctahedral clays (such as antigorite and amesite); tri-layer clays such as smectite and hormite, bentonite, beidelite, nontronite, hectorite, attapulgite, pimelite, mica, muscovite and vermiculite as well as pyrophyllite/
talc, willemseite and minnesotaite clays. A preferred class of clays is the bentonites. It is highly desirable that the clay should be capable of providing a benefit in the wash. Preferably, the clay is chosen from the class of clays that will give a fabric softening benefit. The particle size of
the clay preferably lies in the range 1 to 2 mm. However, it is an aid to dispersion if lower swelling clay swelling is used, especially if the amount of STP is reduced or absent; a swelling of 20 ml or less is preferred in this case.

The Mica Particles
Finely divided mica pigment material may be used as the Mica Particles. Preferably, the mica is coated. More
preferably, it is coated with a very thin layer of titanium dioxide. Most preferably, it is coated with a mixture of titanium dioxide and iron oxide to give a gold lustre. Suitable titanium coated pigments are available from Merck as Timiron MP 115 and as IriodinĀ® 300 with the additional
iron oxide coating. Suitable pigments have a particle size of from 10 to 60 microns.

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The Sodium Tripolyphosphate
Anhydrous Sodium Tripolyphosphate is preferred. A standard grade of the usual particle size for detergent formulations is suitable.
The Polymeric Coating
Optionally the speckle granule may have a water-soluble polymeric coating. This may help to prevent the mica
pigment from leaving the clay, thereby reducing the speckle effect, during storage and handling. The coating may be polyvinyl alcohol or microcrystalline cellulose. We have found that microcrystalline cellulose is preferred for granules with low levels of STP or no STP and polyvinyl
alcohol is preferred when STP is used at the optimum amount. This selection gives the required combination of fast dispersion and good coating adhesion.
Without wishing to be bound by any particular theory, it is believed that the polymeric coating seeps into the pores of the clay carrier and anchors itself onto the surface of the speckle.
The Speckle Manufacturing Process
Although many processes could be used to make the speckle we have found that one process is particularly advantageous to get a high yield of dry and well coated particles of the required particle size, durability and dispersibility when the appropriate composition is used.

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In this process, the dry ingredients are preblended for about one minute. This includes the mica pigment, the bentonite clay, and the soluble STP builder salt. A double cone mixer with multiple spay heads has been found to be
ideal for the process. After pre-blending of the dry ingredients the optional coating material (or water) is sprayed at pressure onto the particles for about 25 minutes in a dilute solution and the mixture is then further mixed for a few minutes to obtain the speckle granules.

Detergent Ingredients
The speckle granule may be combined in any amount with any of the granular ingredients normally found in granular
laundry detergent cleaning compositions. Advantageously it is used at a level of 1 to 4 % by weight, preferably 1.5 to 3 % by weight in the detergent powder composition. This is particularly useful if the clay is a softening type of clay, so that it provides a benefit to the fabric.

The invention will now be further described with reference to the following non-limiting examples.

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EXAMPLES
The ingredients in the amounts detailed in Table 1 were added to a double cone mixer and manufactured into speckle granules using the process outlined below.
TABLE 1







1Bentonite in particulate form with particle sizes ranging
from 1.0 to 2.0 mm was obtained from Bentonit Uniao as
Pelben 10 (Examples 5 and 7) or Pelben 35. Pelben 10 has a
swelling of 10 ml whereas Pelben 35 has a swelling of 35 ml
plus.


2Mica with particle size 10 to 60 microns was obtained from Merck as Iriodin 300 and Timiron Starluster MP-115.

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The Bentonite, mica and, when used, STP were gently blended in the mixer for 1 minute. Then, the coating solution was sprayed into the mixer and mixing continued for 25 minutes. Two different types of coating solution were used: Coating A was microcrystalline cellulose and Coating B was polyvinyl alcohol. Their compositions are detailed in table 2.
TABLE 2

Ingredient Wt% of final Wt% of final
granule granule
Micro-crystalline 0.25 0.0
Cellulose
Polyvinyl alcohol 0.00 0.1
Water 9.75 9.9
The process is controlled so that the speckle granules produced have substantially the same particle size as the original Bentonite granules. However, as seen from table 1
the dispersal times for granules without STP are too long to be of practical use in some wash processes, especially after they have been coated so that the mica did not rub off the surface during subsequent manual handling. Since it is often necessary to use such a coating to avoid the coating
rubbing off and thereby rendering the granule indistinct and unsuitable for use as a speckle, it is clearly advantageous to use STP in the speckle granule.

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CLAIMS
1. Use of a soluble speckle granule in a particulate
laundry detergent composition, characterised in that
the granule comprises a clay mineral carrier material and mica.
2. Use of a speckle granule as claimed in claim 1 wherein
the granule further comprises sodium tripolyphosphate.

3. Use as claimed in claim 1 or claim 2, wherein the
granule has a water-soluble polymer coating.
4. Use as claimed in claim 3, wherein the polymer is a
polymeric alcohol.
5. Use as claimed in claim 3, wherein the polymer is
cellulose.
6. Use of a speckle granule as claimed in any preceding
claim, wherein the granule has an average particle size of from 0.8 mm to 3.0 mm.
7. Use of a speckle granule as claimed in claim 5, which
has an average particle size of from 1.0 mm to 2.0 mm.
8. Use of a speckle granule as claimed in any preceding
claim, which comprises from 0.5 to 1.5 wt% mica.

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9. Use of a speckle granule as claimed in any preceding claim, wherein the clay mineral comprises a softening clay.
10. Use of a speckle granule as claimed in claim 9, wherein the clay mineral comprises bentonite clay.
11. Use of a speckle granule as claimed in any preceding
claim, wherein the mica is coated, preferably with
titanium dioxide.
12. Use of a speckle granule as claimed in claim 11 in
which the mica is coated with titanium dioxide and iron
oxide.

13. Use of a speckle granule as claimed in any preceding
claim wherein the detergent composition comprises from
1 to 4 wt% of the speckle granule.
14. Use of a speckle granule as claimed in claim 13,
wherein the detergent composition comprises from 1.5 to 3 wt% of the speckle granule.

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AMENDED CLAIMS
received by the International Bureau on 08 September 2006 (08.09.2006)
1. Use of a soluble speckle granule in a particulate
laundry detergent composition, characterised in that
the granule comprises a bantonite clay mineral carrier material and mica.
2. Use of a speckle granule as claimed in. claim 1 wherein.
the granule further comprises sodium tripolyphosphate.

3. Use as claimed in claim 1 or claim 2, wherein the
granule has a water-soluble polymer coating.
4. Use as claimed in claim 3, wherein the polymer is a
polymeric alcohol.
5. Use aa claimed in claim 3, wherein the polymer ie
cellulose.
6. Use of a speckle granule as claimed In any preceding
claim, wherein, the granule has an average particle siza of from 0.8 mm to 3.0 mm.
7. Use of a speckle granule as claimed in claim 5, which has an average particle size of from 1.0 mm to 2.0 ram.
B. Use of a speckle granule as claimed in any preceding claim, which comprises from 0,5 to 1.5 wt% mica.
AMENDED SHEET (ARTICLE 19)

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9. Use of a speckle granule as claimed in any preceding claim/ wherein the clay mineral comprises a softening clay.
10. Use of a speckle granule as claimed in any preceding claim, wherein the mica is coated, preferably with titanium dioxide.
11. Use of a speckle granule as claimed in claim 10 in
which the mica is coated with titanium dioxide and iron oxide.
12. UsĀ© of a speakle granule as claimed in any preceding
claim wherein the detergent composition comprises from
1 to 4 wt% of the speckle granule,
13. Use of a speckle granule as claimed in claim 12,
wherein the detergent composition comprises from 1.5 to
3 wt% of the speckle granule.




AMENDED SHEET (ARTICLE 19)

Documents:

1405-mumnp-2007-cancelled pages(3-8-2009).pdf

1405-MUMNP-2007-CLAIMS(3-8-2009).pdf

1405-MUMNP-2007-CLAIMS(AMENDED)-(3-8-2009).pdf

1405-mumnp-2007-claims(complete)-(12-9-2007).pdf

1405-mumnp-2007-claims(granted)-(11-6-2010).pdf

1405-MUMNP-2007-CLAIMS(MARKED COPY)-(3-8-2009).pdf

1405-mumnp-2007-claims.pdf

1405-MUMNP-2007-CORRESPONDENCE 2-7-2008.pdf

1405-mumnp-2007-correspondence(16-1-2008).pdf

1405-MUMNP-2007-CORRESPONDENCE(30-10-2009).pdf

1405-MUMNP-2007-CORRESPONDENCE(4-1-2010).pdf

1405-MUMNP-2007-CORRESPONDENCE(8-2-2012).pdf

1405-mumnp-2007-correspondence(ipo)-(7-7-2010).pdf

1405-mumnp-2007-correspondence-others.pdf

1405-mumnp-2007-correspondence-received.pdf

1405-mumnp-2007-description(complete)-(12-9-2007).pdf

1405-mumnp-2007-description(granted)-(11-6-2010).pdf

1405-MUMNP-2007-FORM 1(3-8-2009).pdf

1405-mumnp-2007-form 18(16-1-2008).pdf

1405-mumnp-2007-form 2(complete)-(12-9-2007).pdf

1405-mumnp-2007-form 2(granted)-(11-6-2010).pdf

1405-MUMNP-2007-FORM 2(TITLE PAGE)-(3-8-2009).pdf

1405-mumnp-2007-form 2(title page)-(complete)-(12-9-2007).pdf

1405-mumnp-2007-form 2(title page)-(granted)-(11-6-2010).pdf

1405-MUMNP-2007-FORM 3(24-2-2010).pdf

1405-MUMNP-2007-FORM 3(4-8-2010).pdf

1405-MUMNP-2007-FORM 5(3-8-2009).pdf

1405-mumnp-2007-form-1.pdf

1405-mumnp-2007-form-3.pdf

1405-mumnp-2007-form-5.pdf

1405-mumnp-2007-form-pct-isa-237.pdf

1405-mumnp-2007-form-pct-separate sheet-237.pdf

1405-MUMNP-2007-GENERAL POWER OF ATTORNEY(3-8-2009).pdf

1405-MUMNP-2007-OTHER DOCUMENT(3-8-2009).pdf

1405-MUMNP-2007-PCT-ISA-210(3-8-2009).pdf

1405-mumnp-2007-pct-search report.pdf

1405-MUMNP-2007-REPLY TO EXAMINATION REPORT(3-8-2009).pdf

1405-mumnp-2007-wo international publication report(12-9-2007).pdf


Patent Number 240985
Indian Patent Application Number 1405/MUMNP/2007
PG Journal Number 25/2010
Publication Date 18-Jun-2010
Grant Date 11-Jun-2010
Date of Filing 12-Sep-2007
Name of Patentee HINDUSTAN UNILEVER LIMITED
Applicant Address HINDUSTAN LEVER HOUSE 165/166,BACKBAY RECLAMATION, MUMBAI 400 020,
Inventors:
# Inventor's Name Inventor's Address
1 ANDRADE PAULO CESAR PUELLE PASEO DE LOS TAMARINDOS 150, ARCOS NORTE D, COL. BOSQUES DE LAS LOMAS, DEL. CUAJIMALPA, MEXICO, D.F.
2 NUNZIO MARIO JOVELINO DEL MIXING QUIMICA INDUSTRIA E COMERCIO, IMPORTACAO E EXPORTACAO LTDA,ESTRADA SANTA BRANCA, KM 02, 12380-000, PARAIBUNA SP.
3 SANCHES ADREY MARCEL MARCHI UNILEVER BRAZIL LTDA, AV. MANOEL DOMINGOS PINTO, 481, 05120-000, SAO PAULO, SP.
4 SILVA ANDREA DE FREITAS UNILEVER BRAZIL LTDA, AV. MANOEL DOMINGOS PINTO, 481, 05120-000, SAO PAULO, SP.
5 STEEL ANDREW THOMAS UNILEVER R&D PORT SUNLIGHT, QUARRY ROAD, EAST, BEBINGTON, WIRRAL, MERSEYSIDE CH63 3JW.
PCT International Classification Number C11D3/12
PCT International Application Number PCT/EP2006/002302
PCT International Filing date 2006-03-13
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 0505778.1 2005-03-22 U.K.