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Publication numberUS20010055575 A1
Publication typeApplication
Application numberUS 09/854,371
Publication dateDec 27, 2001
Filing dateMay 11, 2001
Priority dateMay 12, 2000
Also published asEP1280503A2, US6419910, WO2001085118A2, WO2001085118A3
Publication number09854371, 854371, US 2001/0055575 A1, US 2001/055575 A1, US 20010055575 A1, US 20010055575A1, US 2001055575 A1, US 2001055575A1, US-A1-20010055575, US-A1-2001055575, US2001/0055575A1, US2001/055575A1, US20010055575 A1, US20010055575A1, US2001055575 A1, US2001055575A1
InventorsZhuning Ma, David Brewster, Anthony Scafidi
Original AssigneeUnilever Home & Personal Care Usa, Division Of Conopco, Inc.
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Preparation of antiperspirant gels which obviates the use of simple glycols
US 20010055575 A1
Abstract
A clear emulsion and gel-type composition, which is an antiperspirant or deodorant composition which is a water-in-oil emulsion which comprises:
a clear emulsion and gel-type cosmetic composition which is an antiperspirant and/or deodorant composition, which is a water-in-oil emulsion comprising:
a) about 65% to about 92% of an aqueous solution of an effective amount of antiperspirant active;
b) about 8% to about 35% of an oil phase consisting of silicones, emollients and a silicone emulsifying agent; and
c) a water soluble, non-glycol component that raises the refractive index of said aqueous solution.
wherein said composition is essentially free of simple glycols and low and middle chain alcohols;
is described.
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Claims(10)
What is claimed is:
1. A clear emulsion and gel-type cosmetic composition which is an antiperspirant and/or deodorant composition, which is a water-in-oil emulsion comprising:
a) about 65% to about 92% of an aqueous solution of an effective amount of antiperspirant active;
b) about 8% to about 35% of an oil phase consisting of silicones, emollients and a silicone emulsifying agent; and
c) a water soluble, non-glycol component that raises the refractive index of said aqueous solution.
wherein said composition is essentially free of simple glycols and low and middle chain alcohols.
2. A composition according to
claim 1
, wherein said non glycol compound is selected from the group consisting of glycine, alanine, d1-trytophan; monovalent, divalent, trivalent salts including sodium chloride, sodium sulfate, calcium chloride, calcium sulfate, magnesium chloride, aluminum salts and mixtures thereof; sodium lactate, aluminum lactate, zinc lactate, magnesium lactate, aluminum chloride, acetamide MEA and lactamide MEA; and urea and zinc glycinate.
3. A composition according to
claim 1
; wherein the refractive indices of said water phase and said oil phase are matched to within about 0.0008.
4. A composition according to
claim 4
, wherein the refractive indices of said water phase and said oil phase are matched to within about 0.0004.
5. A composition according to
claim 1
, which has a turbidity of about 50 NTU or less at about 21 C.
6. A composition according to
claim 1
, wherein the oil phase can range from about 30% to about 10%.
7. A composition according to
claim 1
, wherein the oil phase comprises a volatile silicone from about 1% to about 20%.
8. A composition according to
claim 1
, wherein the oil phase comprises a non-volatile silicone from about 9% to about 25%.
9. A composition according to
claim 1
wherein the final refractive index is about 1.3993 to about 1.4200.
10. A method for controlling or preventing odor or perspiration which comprises topically applying an effective amount of a composition according to
claim 1
to the underarm area.
Description
    BACKGROUND OF THE INVENTION
  • [0001]
    Cosmetic products can be in emulsion form. Antiperspirant and deodorant products which are in emulsion form are known in the art. These products may have an oil phase and a water phase. Moreover, these emulsions may be in gel form.
  • [0002]
    Is One can use such gel-type products, which can be antiperspirant and deodorants, by rubbing the underarm area of the body so as to apply an odor and/or perspiration reducing layer of the gel to the skin. Because such products are applied directly to the skin, such products should have certain aesthetic properties so that they will achieve consumer acceptance. Included in such aesthetic properties are non-tackiness during dry-down, non-tackiness when the user perspires after application of the product, smoothness, glide, a lack of oily or crumbly or scratchy feeling; and a product which leaves no white physical residue on skin or clothes after application.
  • [0003]
    Clarity is also an especially desired esthetic property in the eyes of the consumer.
  • [0004]
    It is an object of this invention to provide emulsion and gel-type cosmetic products especially an antiperspirant or deodorant product which has the above-recited aesthetic properties.
  • [0005]
    The following patent publications relate to this field of invention.
  • [0006]
    U.S. Pat. No. 5,587,153 discloses a clear gel-type cosmetic product which has a viscosity of at least about 50,000 cps at 21 C., and includes an emulsion with an oil phase and a water phase that includes an incorporated active ingredients. The refractive indices of the water and oil phases match to at least 0.0004, the refractive index of the product is about 1,4000, and the product clarity is better than thirty NTU.
  • [0007]
    U.S. Pat. No. 5,863,525 also discloses a clear gel-type cosmetic product which has a viscosity of at least about 50,000 cps at 21 C., and includes an emulsion with an oil phase and a water phase that includes an incorporated active ingredient. The refractived indices of the water and oil phases match to at least 0.0004 the refractive index of the product is about 1,4000, and the product clarity is better than thirty NTU.
  • [0008]
    U.S. Pat. No. 5,925,338 discloses a clear gel composition comprising a water-in-oil emulsion of specified viscosity, and specified amounts of water and oil, wherein the oil phase comprises a volatile cyclic silicone, an emulsifying agent, optionally a non-volatile oil, and a volatile linear silicone.
  • [0009]
    U.S. Pat. No. 5,393,518 discloses an optically clear antiperspirant product in the form of a stable water-in-oil emulsion with a specified viscosity which includes a stabilizing agent that has substantial solubility in each of the oil and water phases and which has long term stability over specified temperature ranges.
  • [0010]
    WO 92/05767 discloses a clear gel-type cosmetic product that has a viscosity of at least about 50,000 cps at 21 degrees C., and includes an emulsion with an oil phase and a water phase, wherein the refractive indices of the water and oil phases match to at least 0.0004, the refractive index of the product is about 1.4000 and the product clarity is better than 30 NTU.
  • SUMMARY OF THE INVENTION
  • [0011]
    The invention relates to a clear emulsion and gel-type cosmetic composition, and in particular to an antiperspirant and/or deodorant composition which comprises a water-in-oil emulsion comprising:
  • [0012]
    a) about 65% to about 92% of an aqueous solution of an effective amount of antiperspirant active;
  • [0013]
    b) about 8% to about 35% of an oil phase consisting of silicones, emollients and a silicone emulsifying agent; and
  • [0014]
    c) a water soluble, non-glycol component that raises the refractive index of said aqueous solution.
  • [0015]
    The water phase is essentially free of glycols and low and middle chain alcohols and incorporates inorganic salts, organic salts, amino acids or urea to raise the refractive index of the aqueous phase. Glycols are defined here as alkanes and alkoxyalkanes containing at least two hydroxy groups. Propylene glycol and dipropylene glycol are non-limiting examples of glycols. Low chain alcohols have from one to four carbon atoms. Middle chain alcohols have from 5 to 12 carbon atoms.
  • [0016]
    The invention also relates to a method for preventing and controlling perspiration wetness in humans which comprises applying to the underarm area an effective amount of a composition of the invention.
  • DETAILED DESCRIPTION OF THE INVENTION
  • [0017]
    As used herein, % means weight % of the entire composition, unless otherwise specified. As used herein “essentially free of simple glycols” means that the level of simple glycols present in the composition is in too low off amount to contribute to the tackiness or the stickiness or the wetness or the coolness of the product either during dry down or on perspiring after the product has been applied. This level is usually 0 to about 1% glycols or less. As used herein “simple glycols” means alkanes and alkoxyalkanes containing at least two hydroxy groups and three or less carbon atoms. Propylene glycol is a non-limiting examples of a simple glycol. “Essentially free of low or middle chain alcohols” means that the level of low or middle chain alcohols present is so low that those low or middle chain alcohols in too low off amount to contribute to the tackiness or the stickiness of the product either during dry down or on perspiring after the product has been applied. This level is usually about 0 to about 1% of low and/or middle chain alcohols.
  • [0018]
    All of the ingredients used to prepare compositions of the invention are known or can be prepared according to known methods. The compositions of the invention can be prepared by known methods or by methods analogous to known methods.
  • [0019]
    The invention relates to an emulsion and gel-type cosmetic composition, and in particular to an antiperspirant and/or deodorant composition which comprises a water-in-oil emulsion comprising:
  • [0020]
    The invention relates to a clear emulsion and gel-type cosmetic composition, and in particular to an antiperspirant and/or deodorant composition which comprises a water-in-oil emulsion comprising:
  • [0021]
    a) about 65% to about 92% of an aqueous solution of an effective amount of antiperspirant active;
  • [0022]
    b) about 8% to about 35% of an oil phase consisting of silicones, emollients and a silicone emulsifying agent; and
  • [0023]
    c) a water soluble, non-glycol component that raises the refractive index of said aqueous solution.
  • [0024]
    The water phase is essentially free of glycols and low and middle chain alcohols and incorporates inorganic salts, organic salts, amino acids or urea to raise the refractive index of the aqueous phase. Simple Glycols are as defined herein. Propylene glycol is a non-limiting example of a simple glycols. Low chain alcohols have from one to four carbon atoms. Middle chain alcohols have from 5 to 12 carbon atoms.
  • [0025]
    The invention also relates to a composition as described above wherein the refractive indices of the water phase and the oil phase are matched to within about 0.0008, or more preferably about 0.0004.
  • [0026]
    The invention also relates to optically clear compositions which have an NTU of 50 or lower. NTU means Nephelometric Turbidity Units.
  • [0027]
    The invention also relates to cosmetic compositions as described above which have decreased tackiness, stickiness, wetness and coolness measurements as ascertained by trained sensory panelists.
  • [0028]
    As noted above, the compositions of the invention can have an aqueous phase from about 65% to about 92%. More preferably, the composition of the invention can have an aqueous phase of about 70% to about 90%. The compositions of the invention can have an oil phase of about 8% to about 35%, more preferably about 10% to about 30%.
  • [0029]
    As noted just above, the compositions of the invention can have an optical clarity of 50 NTU or lower. More preferably, they can have an optical clarity of about 0 to about 30 NTU.
  • [0030]
    The invention also relates to a method for preventing and controlling perspiration wetness in humans which comprises applying to the underarm area an effective amount of a composition of the invention.
  • [0031]
    What follows now is a more detailed description of the ingredients which are included in the compositions of the invention.
  • [0032]
    As has been noted above, the compositions of the invention are essentially free of glycols and low to middle chain alcohols. However, glycols normally are used in gelled cosmetic compositions to raise the refractive index of the water phase and thereby match the refractive index of the water phase to the refractive index of the oil phase and thereby obtain a clear composition.
  • [0033]
    Without glycols, another means must be found to raise the refractive index of the water phase of the composition.
  • [0034]
    In the present invention, this is accomplished by using inclusions other than glycols in the water phase. More specifically, said deodorant or antiperspirant active can have this refractive index raised by combining it with a non-glycol compound that is water soluble, and raises the refractive index of the water phase and is not deleterious to the properties of the antiperspirant or deodorant active, or to the esthetics of the final composition. Such compounds may have a carboxylate group. Preferably such compounds can include an amino acid such as glycine, alanine or d1-trytophan. Alternatively other inorganic salts such as water soluble salts as or more preferably monovalent, divalent, trivalent salts including sodium chloride, sodium sulfate, calcium chloride, calcium sulfate, magnesium chloride, aluminum salts and mixtures thereof can be added to the water phase to raise the refractive index thereof. Other examples include salts of organic acids such as sodium lactate, acetamide MEA and lactamide MEA. Also urea and other salts of amino acids may be utilized such as zinc glycinate.
  • [0035]
    An advantage to using this method for matching refractive indices is that it achieves compositions that are not sticky or tacky during drydown or after the user has re-perspired. Another advantage is that this represents an inexpensive way to obtain clear compositions.
  • Deodorant or Antiperspirant Actives
  • [0036]
    Nonlimiting examples of said deodorant or antiperspirant actives which have been combined with the just above mentioned compounds are as follows: antiperspirant complexes using the antiperspirant salts which are known in the art. For example, U.S. Pat. No. 3,792,068 Luedders et al., herein incorporated by reference, discloses complexes of aluminum, zirconium and amino acids such as glycines. Complexes such as those disclosed in Luedders and other similar complexes are commonly known as ZAG (OR Zag). ZAG complexes are chemically analyzable for the presence of aluminum, activated ZAG compounds and chlorine. ZAG complexes useful herein are identified by the specification of both the molar ratio of aluminum to zirconium (the Al:Zr ratio) and the molar ratio of total metal to chlorine (metal:Cl) ZAG complexes useful herein have an Al:Zr ratio of from about 1.67 to about 12.5 and a metal:Cl ratio of about 0.73 to about 1.93.
  • [0037]
    Another patent which discloses ZAG compounds is U.S. Pat. No. 4,985,238 to Tanner et al. This just-mentioned patent is herein incorporated by reference. Preferred ZAG complexes are described in U.S. Pat. No. 4,985,238 to Tanner et al.
  • [0038]
    The active deodorant or antiperspirant is present in the aqueous phase at usually about 5% to about 50% of the total composition on an active basis.
  • Water
  • [0039]
    The water which is used in the aqueous phase of compositions of the invention can be deionized water. The water phase, and indeed the entire composition, is essentially free of simple glycols and low or middle chain length alcohols as described herein.
  • The Oil Phase
  • [0040]
    The oil phase of compositions of the invention can be a blend of liquids which include a polyorganosiloxane, such as DC9010, DC9040 or more preferably dimethicone or cyclomethicone, such as DC 245 or DC345. Dimethicone is available from Dow Corning under the name DC-225 and DC200 fluid and it has a refractive index of about 1.3995. Other non-silicone liquids which can be included in the oil phase of nonlimiting of compositions of the invention include, isopropyl myristate, isopropyl palmitate, and diisopropyl sebacate. These have refractive indices respectively of 1.4340, 1.4370, and 1.4320. Other non-limiting, non-silicone oils which can be included in the oil phase of the compositions of the invention include C12-15 alcohols benzoate, isostearyl isostearate, octyl dodecanol, octyl nonanoate and PPG-14 butyl ether.
  • [0041]
    The oil phase of the compositions of the invention can also include a silicone emulsifying agent at a level that is effective to form emulsions. Non-limiting examples of silicone emulsifying agents include Abil EM90, Abil EM97, DC9010 silicone elastomer, and most preferably a polyether substituted silicone of cyclomethicone and dimethicone copolyl which can be obtained form Dow Corning under the name DC-3225C and DC-5225C. This emulsifying agent is a dispersion of dimethicone copolyol, which is a silicone surfactant in cyclomethicone (Dow Coming 344 fluid). The dimethicone is present at about 10% of the dispersion, and the cyclomethicone is present at about 90% of the dispersion. Stable emulsions containing a large percentage of oil phase can be prepared using this emulsifying agent The oil phase of the compositions of the invention can also contain organic esters such as isostearyl stearate, Finsolv TN C12-C15 benzoates, ethers such as polyethylene glycols, PPG 14 Butyl Ether, hydrocarbons such as Silkflo 366 and 344 Permethyl 102A isostearyl cyclohexane and halo carbons such as chlorocarbons or fluorocarbons.
  • Optional Ingredients
  • [0042]
    Compositions of the invention can further comprise other cosmetic ingredients such as fragrances, colorants, emollients, preservatives, and thickeners.
  • Ingredients in Compositions of the Invention can Fall Within the Following Ranges
  • [0043]
    Compositions of the invention can comprise about 8% to about 35% of oil phase; more preferably about 10% to about 30% oil phase; most preferably 15% to about 30% oil phase.
  • [0044]
    Compositions of the invention can comprise about 65% to about 92% water phase, more preferably about 70 to about 85% water phase.
  • [0045]
    Optically clear compositions using ingredients described above can be achieved by matching the refractive index of the oil phase with the refractive index of the water phase. This is done by combining the ingredients of the oil phase and measuring the refractive index of the resulting oil phase, at about room temperature, which is about 21 C. Then the ingredients which comprise the aqueous phase are mixed and its refractive index is measured at room temperature, 21 C.
  • [0046]
    If necessary, in order to match the refractive index of the water phase to that of the oil phase, water can be added to the water phase (to lower total water phase refractive index) In order to raise water phase refractive index, the level of the water soluble salt, amino acid or other non-glycol, water soluble additive such as urea may be added for adjustment purposes.
  • [0047]
    Following this adjustment, the water phase is optically remeasured to determine whether its refractive index matches that of the oil phase. Thus, if the oil phase had a refractive index of 1.4000 and the initial refractive index of the water phase was 1.3980, additional non-glycol inclusions such as an inorganic salt are added to make its refractive index about 1.4000. In the compositions of the invention, the closer the match of the water and the oil phase, the more optically clear is the resulting emulsion.
  • [0048]
    The above oil phase and water phase refractive indices are measured by using refractometers which are known in the art. An example of such a refractometer is a Reichert-Jung, Abbe Mark II Refractometer Model 10480. And the refractive index is measured at a suitable temperature, usually, at about 21 C. which is room temperature.
  • [0049]
    The water phase is then added slowly to the oil phase (or vice versa), while the mixture is mixed at 10,000 RPM or higher as needed to form a stable emulsion. A sonolator is the preferred method of shearing the product to form a gel with a viscosity of 50.000-200,000 cps. at about 21 C. measured using a Brookfield Viscometer with a T-F bar @10 rpm/30 seconds. Preferably the emulsion has a viscosity between about 50,000 cps to about 100,000 cps measured as described above.
  • [0050]
    Within the oil phase there can be a volatile silicone. The volatile silicone can range from about 1% to about 5%, more preferably between about 2% to about 4%.
  • [0051]
    Within the oil phase there can be a non-volatile silicone. The non-volatile silicone can range from about 9% to about 25%, more preferably between about 15% to about 25%.
  • [0052]
    Within the oil phase there can be an emollient. The emollient can range from about 0.5% to about 5%, more preferably between about 2% to about 4%.
  • [0053]
    What follows is a non-limiting list of compounds and ingredients which can be included in the compositions of the invention. An upper limit in weight per cent is given for each compound and ingredient. This upper limit, refers only to the particular compound or ingredient that is in the same row as said compound or ingredient. Moreover, specific compositions of the invention can have higher amounts of a particular compound or ingredient than are set forth in the list. It is understood that any given composition of the invention will have an aqueous phase, an oil phase, and a non glycol compound as described elsewhere herein.
    Generic formulation
    Brand Name INCI Name Upper limit in wt %
    DC 245 Cyclopentasiloxane 20%
    DC silicone fluid Dimethicone 20%
    200 350 cst.
    DC silicone fluid Dimethicone 20%
    200 100 cst.
    DC 556 Phenyltrimethicone 15%
    DC 9040 Cyclomethicone & 15%
    dimethicone crosspolymer
    DC 9010 Ethoxylated cyclomethicone 15%
    and dimethicone cross
    polymer
    DC 5225C Dimethicone copolyol 15%
    Abil EM 90 Cetyl dimethicone copolyol  3%
    GE SF1555 Bis-phenylpropyl dimethicone 15%
    Silkoflo 366NF Hydrogenated polydecene 15%
    Finsolv TN C12-15 alkyl benzoate 15%
    Fragrance Fragrance  2%
    Water Soft water 30%
    Westchlor 41 45% Aluminum zirconium 60%
    aqueous solution tetrachlorohydrex-gly
    solution
    Rezal 67 aqueous Aluminum zirconium 60%
    solution pentachlorohydrate solution
    Urea Urea 15%
    Zinc Glycinate Zinc glycinate  5%
    Glycine Glycine 10%
    Sodium lactate Sodium lactate solution 20%
    60% solution
    Lactamide MEA Mixture of ethanolamides of 20%
    lactic acid
    Calcium chloride Calcium chloride hexahydrate 10%
    Magnesium Lactate Magnesium lactate  4%
    Carbowax 400 Polythylene glycol 8 or PEG 8 15%
  • [0054]
    Compositions of the invention can be made by known processes or by processes which are analogous to known processes. What follows are specific compositions of the invention which are clear gels and which have been made. These examples are illustrative and are not meant to limit the present invention.
    Ex- Ex- Ex- Ex- Ex- Ex-
    am- am- am- am- am- am-
    ple 1 ple 2 ple 3 ple 4 ple 5 ple 6
    % % % % % %
    Trade Name INCI Name (w) (w) (w) (w) (w) (w)
    DC 9010 Ethoxylated 6.70 9.47
    cyclomethicone
    and
    dimethicone
    crosspolymer
    DC 9040 Cyclo- 4.00 4.95 5.04
    methicone and
    dimethicone
    crosspolymer
    Abil EM 90 Cetyl di- 0.99 0.97
    methicone
    copolyol
    DC 245 cyclopenta- 18.55 12.55 16.35 15.72
    siloxane
    DC 5225C Cyclo- 7.40 7.40
    methicone and
    dimethicone
    copolyol
    GE SF1555 Bisphenyl 3.50
    trimethicone
    Dimethicone Dimethicone 2.64 12.10 1.13 5.99 5.25 15.80
    350 cst. 350 cst.
    DC 556 Phenyl 1.61 3.06 4.00
    trimethicone
    Finsolv TN C12-C15 alkyl 3.23 3.14 2.97
    benzoate
    Solkflo Hydrogenated 2.56 2.51
    366NF polydecene
    Glycine Glycine 3.83
    Magnesium Magnesium 2.27
    lactate lactate
    Carbowax Polyethylene 8.50 8.00
    400 oxide
    Urea Urea 7.15 0.50 5.75 4.95 2.00 0.50
    Fragrance Fragrance 0.66 0.80 1.15 0.99 1.00 0.80
    Deionized Deionized 9.67 7.20 12.57 5.83 8.88 7.50
    water water
    Westcholor Aluminum 56.00 56.00
    41 45% zirconium
    tetrachloro-
    hydrex-gly
    Reheis AZG Aluminum 56.98 55.81
    35% zirconium
    tetrachloro-
    hydrex-gly
    35%
    Reheis AZG Aluminum 47.23 47.90
    zirconium
    penta chloro-
    hydrex-gly
    40% solution
  • [0055]
    The general method of preparation is as follows:
  • [0056]
    A composition of the invention can be made by preparing the oil phase and the water phase in separate vessels and matching their respective refractive indices. The water phase is added gradually to the oil phase with rapid agitation using a lightning mixer. The resulting mixed solution is then placed in a homogenizer and mixed at 10,000 rpm or higher until it gels.
  • [0057]
    The above examples have optical clarifies and refractive indexes within the following ranges as noted just below.
  • [0058]
    Refractive indices from about 1.3993 to about 1.4200 at 21 C.
  • [0059]
    Optical clarities at about 50 NTU at 21 C., or less.
  • [0060]
    Viscosities from about 50,000 to about 100,000 cps at 21 C., using a Brookfield Viscometer with a T-F bar @10 rpm/30 seconds.
  • [0061]
    Moreover, the above compositions have reduced tackiness or stickiness, reduces wetness and coolness. This can be demonstrated by trained sensory panelists applying measured doses of the product to underarms and inner forearms and evaluating tackiness immediately after application, and again at 5,10 and 15 minute intervals. The panelists can also evaluate wetness and coolness.
  • [0062]
    While particular embodiments of the invention have been shown and described, various modifications will be apparent to those skilled in the art, and therefore it is not intended that the invention be limited to the disclosed embodiments or the details thereof, and departures may be made therefrom within the spirit and the scope of the inventions.
Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US20110110990 *May 12, 2011L'oreal, S.A.Cosmetic compositions comprising at least one dimethicone, at least one linear hydrocarbon wax and at least one compatibilizing agent
WO2015055199A3 *Sep 26, 2014Aug 6, 2015Henkel Ag & Co. KgaaAntiperspirant cosmetic agents having alpha-hydroxy acids
Classifications
U.S. Classification424/65, 424/401, 424/400
International ClassificationA61K8/58, A61Q15/00, A61K8/06, A61K8/894, A61K8/04
Cooperative ClassificationA61K8/06, A61K8/064, A61Q15/00, A61K8/894, A61K2800/262, A61K8/585, A61K8/042
European ClassificationA61K8/06B, A61K8/58C, A61K8/04A, A61K8/894, A61K8/06, A61Q15/00
Legal Events
DateCodeEventDescription
Jul 25, 2001ASAssignment
Owner name: UNILEVER HOME & PERSONAL CARE USA, DIVISION OF CON
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:MA, ZHUNING;BREWSTER, DAVID ALLEN;SCAFIDI, ANTHONY ALOYSIUS;REEL/FRAME:012033/0555;SIGNING DATES FROM 20010521 TO 20010523
Feb 1, 2006REMIMaintenance fee reminder mailed
Jul 17, 2006LAPSLapse for failure to pay maintenance fees
Sep 12, 2006FPExpired due to failure to pay maintenance fee
Effective date: 20060716