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 WO 2006/099964 PCT/EP2006/002302 - 1 - 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 WO 2006/099964 PCT/EP2006/002302 - 2 - 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. WO 2006/099964 PCT/EP2006/002302 - 3 - 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 Iriodin® 300 with the additional iron oxide coating. Suitable pigments have a particle size of from 10 to 60 microns. WO 2006/099964 PCT/EP2006/002302 - 4 - 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. WO 2006/099964 PCT/EP2006/002302 - 5 - 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. WO 2006/099964 PCT/EP2006/002302 - 6 - 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. WO 2006/099964 PCT/EP2006/002302 - 7 - 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. WO 2006/099964 PCT/EP2006/002302 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. WO 2006/099964 PCT/EP2006/002302 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. WO 2006/099964 10 PCT/EP2006/002302 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) WO 2006/099964 11 PCT/EP2006/002302 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. Us© 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)

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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