• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    manufacturing process of a conditioning gel phase and manufacturing a conditioning composition "manufacturing process of a conditioning gel phase comprising: forming an aqueous isotropic solution of cationic surfactant; mixing the aqueous isotropic solution of cationic surfactant with molten fatty alcohol , and the temperature during the mixture of fatty alcohol with the isotropic solution of cationic surfactant is maintained at 55ºc to 65ºc.
    公开号:BR112015001730B1
    申请号:R112015001730-4
    申请日:2013-07-24
    公开日:2020-02-18
    发明作者:Christia Casugbo；David Serridge；John Alan Hough；John Michael Naughton；Mark Flanagan
    申请人:Unilever N.V.；
    IPC主号:
    专利说明:

    “PROCESS OF MANUFACTURING A CONDITIONING GEL PHASE AND
    PROCESS OF MANUFACTURING A COMPOSITION
    CONDITIONER ”[001] The present invention relates to a process for manufacturing improved conditioner compositions.
    [002] Patent document WO 2010/136285 (Unilever) describes a process in which molten fatty alcohol and mineral oil are mixed in an aqueous composition comprising lactic acid, stearamidopropyl dimethyl amine and BTAC.
    [003] US patent document 2006/078527 (Sanjeev) and US patent document 4,726,945 (Patel) describe a multiphase personal treatment composition comprising stearamidopropyl dimethylamine glutamate and addition of fatty alcohol.
    [004] Despite the state of the art, there is still a need for improved conditioning compositions.
    [005] Correspondingly, and in a first aspect, a process for manufacturing a conditioning gel phase according to claim 1 is provided.
    [006] A conditioning composition made using a conditioning gel phase of the invention proved to be superior to compositions made by standard processes where the materials are mixed in water at around 70 ° C. The superior conditioning effect manifests itself in superior conditioning thickness (despite presenting lower levels of solids) and the next day benefits from a feeling of cleanliness and conditioning. These are surprising since it would be expected that superior conditioning products usually leave the hair shrunk and greasy and on the following day they allow the formation of excessive deposition of solids.
    Petition 870190111043, of 10/31/2019, p. 13/41
    2/11 [007] Preferably, the temperature of the mixture of the aqueous isotropic solution and fatty alcohol is maintained from 55 ° C to 65 ° C.
    [008] Preferably, the molten fatty alcohol is added to the aqueous isotropic solution of cationic surfactant.
    [009] In this process the temperature of the mixture is controlled by changing the temperature / rate of the fatty alcohol mixture and the cationic surfactant solution. The temperature needs to be carefully controlled in order to obtain the correct conditioning gel phase structure. The improvement, therefore, lies in the balance of thermal energy at the point of mixing fatty alcohol with the isotropic mixture.
    [010] After the formation of the gel phase, water and additional ingredients can also be added at once or it can be in stages. Preferably the gel phase is cooled before adding water.
    [011] The conditioning composition made by using such conditioning gel phase improved the conditioning capabilities.
    [012] Preferably, the temperature of the mixture of fatty alcohol and aqueous isotropic solution is maintained at 58 ° C to 62 ° C; most preferably at 60 ° C.
    [013] Preferably, before adding to the isotropic mixture, the fatty alcohol is kept at a temperature sufficient to maintain the fatty alcohol in a liquid phase. Preferably, the fatty alcohol is maintained at 80 ° C to 85 ° C.
    [014] Preferably, the resulting conditioning gel phase is mixed with a mixer with a rotor tip speed of 10-34, preferably 21-27 and especially preferably 24 ms -1 .
    [015] Preferably, the fatty alcohol comprises 8 to 22 carbon atoms, more preferably 16 to 22. Fatty alcohols are typically compounds containing straight chain alkyl groups. Examples of
    Petition 870190111043, of 10/31/2019, p. 14/41
    3/11
    Preferred fatty alcohols include cetyl alcohol, stearyl alcohol and mixtures thereof.
    [016] The level of fatty alcohol in the conditioner of the invention (not just the conditioning gel phase) generally ranges from 0.01 to 10%, preferably from 0.1% to 8%, more preferably from 0.2% to 7 %, most preferably 0.3% to 6% by weight of the composition. The weight ratio of cationic surfactant to fatty alcohol is suitably 1: 1 to 1:10, preferably 1: 1.5 to 1: 8, ideally 1: 2 to 1: 5. If the weight ratio of cationic surfactant to fatty alcohol is too high, it can lead to eye irritation due to the composition. If it is too short, it may produce a strident hair sensation for some consumers.
    [017] Suitable conditioning components include those selected from cationic surfactants, used alone or in mixture. Preferably, the cationic surfactants have an N + R 1 R 2 R 3 R4 formula in which R 1 , R 2 , R 3 and R 4 are independently alkyl (C 1 to C 30) or benzyl. Preferably, one, two or three of R 1 , R 2 , R 3 and R 4 are independently alkyl (C4 to C30) and the other group R 1 , R 2 , R 3 and R 4 or groups are alkyl (C1-C6 ) or benzyl. More preferably, one or two of R 1 , R 2 , R 3 and R 4 are independently alkyl (C 6 to C 30) and the other groups R 1 , R 2 , R 3 and R 4 are alkyl (C 1 -C 6) or benzyl groups. Optionally, the alkyl groups can comprise one or more ester (-OCO- or -COO-) and / or ether (-O-) bonds within the alkyl chain. Alkyl groups can optionally be substituted with one or more hydroxyl groups. Alkyl groups can be straight or branched and for alkyl groups with 3 or more carbon atoms, cyclic. The alkyl groups may be saturated or may contain one or more carbon-carbon double bonds (for example, oleyl). Alkyl groups are optionally ethoxylated on the alkyl chain with one or more ethyleneoxy groups.
    [018] Cationic surfactants suitable for use in
    Petition 870190111043, of 10/31/2019, p. 15/41
    4/11 invention include cetyltrimethylammonium chloride, behenyltrimethylammonium chloride, cetylpyridinium chloride, tetramethylammonium chloride, tetraethylammonium chloride, dodecyltrimethylmethyl chloride, dodecyltrimethylmethyl chloride, dichloramethylmethyl chloride of didodecyldimethylammonium, dioctadecyldimethylammonium chloride, sebotrimethylammonium chloride, dihirogenated tallow dimethyl ammonium chloride (eg, Akzo Nobel Arquad 2HT / 75), cocotrimethylammonium chloride, PEG-2-oleamonium chloride and the corresponding hydroxides. Other suitable cationic surfactants include those materials with the designations CTFA Quaternium-5, Quaternium-31 and Quaternium-18. Mixtures of any prior materials may also be suitable. A cationic surfactant particularly useful for use in conditioners according to the invention is cetylmethylammonium chloride, commercially available, for example, as GENAMIN CTAC, ex Hoechst Celanese. Another cationic surfactant particularly useful for use in conditioners according to the invention is behenyltrimethylammonium chloride, commercially available, for example, as GENAMIN KDMP, ex Clariant.
    [019] Preferably, the conditioning composition formed by the conditioning gel phase of the invention comprises from 0.1% by weight to 10% by weight of the total composition of quaternary ammonium surfactant of the formula N + R 1 R 2 R 3 R 4 as above described, more preferably from 0.2% by weight to 5% by weight.
    [020] Preferably the aqueous isotropic solution comprises from 1 to 5% by weight of quaternary ammonium surfactant.
    [021] Preferably, the aqueous isotropic solution comprises from 1 to 5% by weight of amidoamine surfactant.
    [022] Adequate cationic amidoamine surfactants are
    Petition 870190111043, of 10/31/2019, p. 16/41
    5/11 preferably of the general formula (I).
    (I) R 1 CONH (CH2) mN (R 2 ) R 3 in which R 1 is a hydrocarbyl chain with 10 or more carbon atoms, R 2 and R 3 are independently selected from hydrocarbyl chains of 1 to 10 carbon atoms , em is an integer from 1 to approximately 10; and as used herein, the term hydrocarbyl chain means an alkyl or alkenyl chain.
    [023] Preferred amidoamine compounds are those corresponding to formula (I) in which R 1 is a hydrocarbyl residue with approximately 11 to approximately 24 carbon atoms, R 2 and R 3 are independently hydrocarbyl residues, preferably alkyl groups, with 1 to approximately 4 carbon atoms, and m is an integer from 1 to approximately [024] Preferably, [025] Preferably, or propylene.
    [026] Stearamido-propildimethylamine amidoamines, stearamidoethyldiethylamine, palmitamidopropildimethylamine, palmitamidoethildiethylamine, behenamidopropildimethyl-amine
    4.
    R 2 and R 3 are methyl or ethyl groups.
    m is 2 or 3, that is, a useful preferred ethylene group includes stearamidopropylethylamine, stearamidoethyldimethylamine, palmitamidopropyl-diethylamine, palmitamidoethyldimethylamine, behenamidopropildietilmine, behenamidoethyldylethylamethylamethylamethylamethylamethylamethylamethylamethylamethylamethylamethylamine, aracid.
    [027] Particularly preferred amidoamines useful here are stearamidopropyldimethylamine, stearamidoethyldiethylamine, and mixtures thereof.
    [028] Commercially available amidoamines include here:
    Petition 870190111043, of 10/31/2019, p. 17/41
    6/11 stearamidopropyl dimethylamine with trade names LEXAMINE S-13 available from Inolex (Philadelphia Pennsylvania, USA) and AMIDOAMINE MSP available from Nikko (Tokyo, Japan), stearamido ethyl diethylamine with the brand name AMIDOAMINAS available from Nikko, behenamidopropyl dimethylamine with the trade name INCROMINE BB available from INCROMINE BB Croda (North Humberside, England), and several amidoamines with trade names SCHERCODINE series available from Scher (Clifton New Jersey, USA).
    [029] Preferably, the isotropic solution comprises neutralizer for any amidoamine present. Preferred neutralizers include acid. The acid can be any organic or mineral acid that is capable of protonating amidoamine in the conditioning composition. Suitable acids here include hydrochloric acid, acetic acid, tartaric acid, fumaric acid, lactic acid, malic acid, succinic acid and mixtures thereof. Preferably, the acid is selected from the group consisting of acetic acid, tartaric acid, hydrochloric acid, fumaric acid, lactic acid and mixtures thereof.
    [030] Particularly preferred is lactic acid.
    [031] The main role of the acid is to protonate amidoamine in the hair treatment composition thus forming a tertiary amine salt (TAS) in situ in the hair treatment composition. TAS is a non-permanent quaternary ammonium or pseudo-surfactant of quaternary and cationic ammonium.
    [032] Suitably, the acid is included in an amount sufficient to protonate more than 95 mole% (293 K) of the amidoamine present.
    [033] If an amidoamine of the type described here is present then the corresponding acid component will be present in the aqueous isotropic solution.
    Petition 870190111043, of 10/31/2019, p. 18/41
    7/11 [034] Preferably the composition comprises from 0.1% by weight to 10% by weight of the total protonated amidoamine composition as described above, more preferably from 0.2% by weight to 5% by weight.
    [035] In a preferred embodiment the weight ratio of protonated amidoamine to quaternary ammonium surfactant is 1: 2 to 2: 1.
    [036] In conditioning compositions of the invention (not merely the conditioning gel phase), the total level of cationic surfactant generally ranges from 0.01% to 10%, more preferably 0.05% to 7.5%, most preferably 0.1% to 5% by weight of the composition.
    [037] Preferably, the fused fatty alcohol is added to the aqueous cationic surfactant. More preferably, it is added gradually to the cationic surfactant.
    [038] In a second aspect, a process for manufacturing a conditioning composition is provided by forming a conditioning gel phase obtained by the first aspect and then adding any remaining ingredients. Typical remaining ingredients include fragrances, silicones, fiber actives or other beneficial agents.
    [039] Preferably, the conditioning composition is mixed with a rotor tip speed of 10-34, preferably 21-27 and especially preferably 24 ms -1 or more times after the remaining ingredients have been added.
    [040] Mixers suitable for use with the invention have indices of kw / kg preferably in the range of 2 to 30 kw / kg, more preferably 10 - 25 and even more preferably 15 -25.
    [041] Conditioning compositions of the invention or use of conditioning gel phase of the invention also deposit silicone better than conventionally made conditioning compositions.
    Petition 870190111043, of 10/31/2019, p. 19/41
    8/11 [042] Correspondingly, the compositions of the invention may contain emulsified droplets of a silicone conditioning agent to increase conditioning performance.
    [043] Suitable silicones include polydiorganosiloxanes, particularly polydimethylsiloxanes bearing the designation CTFA dimethicone. Also suitable for use are compositions of the invention (particularly shampoos and conditioners) are polydimethyl siloxanes with hydroxyl end groups that bear the designation CTFA dimethicone. Also suitable for use in compositions of the invention are silicone gums with a light degree of crosslinking as described, for example, in patent document WO 96/31188.
    [044] The viscosity of the emulsified silicone itself (without the emulsion or final hair conditioning composition) is typically at least 10,000 cst under 25 o C the viscosity of the silicone itself is preferably at least 60,000 cst, most preferably at least 500,000 cst, ideally at least 1,000,000 cst. Preferably the viscosity does not excedeu10 9 cst for ease of formulation.
    [045] Emulsified silicones for use in the shampoo compositions of the invention typically have an average silicone droplet size in the composition of less than 30, preferably less than 20, more preferably less than 10 microns, ideally 0.01 to 1 microns. Silicone emulsions with an average silicone droplet size of 0.15 microns are generally called microemulsions.
    [046] Emulsified silicones for use without conditioning compositions of the invention in general typically have a size in the composition of less than 30, preferably less than 20, more preferably less than 15. Preferably, the average silicone droplet is greater than 0.5
    Petition 870190111043, of 10/31/2019, p. 20/41
    9/11 microns, more preferably greater than 1 micron, ideally 2 to 8 microns.
    [047] Silicone particle size can be measured using a laser light scattering technique, for example, using a Malvern Instruments 2600D particle sizer.
    [048] Examples of suitable preformed emulsions include Xiameter MEM 1785 and microemulsion DC2-1865 available from Dow Corning. These are dimethiconol emulsions / microemulsions. Cross-linked silicone gums are also available in a pre-emulsified form that is advantageous for ease of formulation.
    [049] Another preferred class of silicones for inclusion in shampoos and conditioners of the invention are amino-functional silicones. "Amino-functional silicone" means a silicone containing at least one primary, secondary or tertiary amine group or a quaternary ammonium group. Examples of suitable amino-functional silicones include polysiloxanes with the CTFA designation "amodimethicone".
    [050] Specific examples of amino-functional silicones suitable for use in the invention are the aminosilicone oils DC28220, DC2-8177 and DC2-8566 (all ex Dow Corning).
    [051] Suitable quaternary silicone polymers are described in patent document EP-A-0 530 974. A preferred quaternary silicone polymer is K3474 ex Goldschmidt.
    [052] Emulsions of silicone oils with amino functionality with non-ionic and / or cationic surfactants are also suitable.
    [053] Preformed amino-emulsion silicone emulsions are also available from silicone oil suppliers such as Dow Corning and General Electric. Specific examples include cationic emulsion DC939 and nonionic emulsions DC2-7224, DC2-8467, DC2-8177 and
    Petition 870190111043, of 10/31/2019, p. 21/41
    11/10
    DC2-8154 (all ex Dow Corning).
    [054] The total amount of silicone is preferably 0.01% by weight to 10% by weight of the total composition, more preferably 0.1% by weight to 5% by weight, most preferably 0.5% by weight at 3% by weight is an adequate level.
    Example
    Material Active level THE 1 Stearylamidopropyl dimethylamine 100 1.25 1 Behentrimonium Chloride 70 1.25 1 Lactic acid 88 0.38 0.285 Cetearyl alcohol 100 5 4 perfume 100 0.6 0.6 Preservative 55 0.1 0.1 Disodium EDTA 100 0.1 0.1 Preservative 1.5 0.04 0.04 Potassium chloride 100 0.1 0.1 ChlorideDimethicone / amodimethicone / Cetrimony 70 3.57 3.57 Waterto 100 to 100
    [055] Formulation A is made through a standard process that involves mixing BTAC and fatty alcohol in water at around 70C. On the other hand, formulation 1 is made by adding cationic surfactants to water at 60 o C, maintaining the temperature by using external heating and stirring.
    [056] Gradually adding melted fatty alcohol (85 ° C) to this mixture, maintaining the temperature at 60 ° C by using external heating or cooling and stirring.
    [057] Cooling to room temperature by adding more water and other room temperature ingredients and using external cooling if necessary, and stirring.
    [058] The compositions feature different levels of conditioning conditioner to demonstrate improved conditioning performance
    Petition 870190111043, of 10/31/2019, p. 22/41
    11/11 of the composition made by the claimed process.
    Volunteer panel data THE 1 Conditioner attribute Conditioner thickness 63.19 B 74.61 A Modeling facility 70.79 bc 75.08 a Conditioning level 64.37 C 70.48 AB Global modeling 67.38 BC 72.64 A Following day ND feeling clean 61.96 D 69.74 AB ND conditioning 59.33 C 67.23 A
    [059] Data from a panel of volunteers with 40 members with dry damaged hair. Line scale analysis. (5 different products tested in total vs. control).
    [060] The data show that using a better process we will have a thicker product despite having less total solids (i.e. FA and BTAC). The ingredients are used more efficiently.
    [061] Furthermore, the product is both more conditioning than the control as it gives a feeling of much cleaner the next day - unusual, as there is usually a dilemma (more conditioning = heavier) again, despite presenting a lesser level of solids, ie, active conditioner. A composition that provided improved conditioning benefits immediately after application was expected to achieve this through increased deposition. However, if that were the case, the next day the benefit would be drastically reduced.
    权利要求:
    Claims (8)
    [1]
    1. GEL PHASE MANUFACTURING PROCESS
    CONDITIONER, characterized by understanding:
    (i) formation of an aqueous isotropic solution of cationic surfactant, in which the isotropic solution also comprises neutralizer when amidoamine is present;
    (ii) addition of fused fatty alcohol to the aqueous isotropic solution of cationic surfactant;
    where the temperature during mixing of the fatty alcohol with the isotropic solution of cationic surfactant is maintained at 55 ° C to 65 ° C and where the fatty alcohol has a straight chain alkyl group comprising 8 to 22 carbons and where the cationic surfactant comprises a cationic surfactant of the formula N + R1R 2 R 3 R 4 in which R 1 , R 2 , R 3 and R 4 are independently alkyl (C1-C30) or benzyl (iii) and subsequently the addition of any remaining ingredients .
    [2]
    2. PROCESS, according to claim 1, characterized by the isotropic solution of cationic surfactant comprising from 1 to 5% by weight of protonated amidoamine surfactant.
    [3]
    PROCESS according to any one of claims 1 to 2, characterized in that the composition comprises from 0.2 to 7% by weight of the total fatty acid composition.
    [4]
    4. PROCESS according to any one of claims 1 to 3, characterized in that the cationic surfactant comprises behenyltrimethylammonium chloride.
    [5]
    PROCESS according to any one of claims 1 to 4, characterized in that the fatty alcohol is a C16 to C22 alcohol.
    [6]
    6. PROCESS, according to any of the
    Petition 870190111043, of 10/31/2019, p. 24/41
    2/2 claims 1 to 5, characterized in that the resulting mixture is mixed with a mixer with a rotor tip speed of 10-34 ms -1 .
    [7]
    7. PROCESS FOR MANUFACTURING A CONDITIONING COMPOSITION, characterized by the addition of any remaining ingredients to a conditioning gel phase obtained as defined in any one of claims 1 to 6.
    [8]
    PROCESS according to claim 7, characterized in that it comprises mixing the composition with a mixer with a rotor tip speed of 10-30 ms -1 .
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    JP2021526514A|2018-06-07|2021-10-07|ユニリーバー・ナームローゼ・ベンノートシヤープ|Method|
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    法律状态:
    2018-03-06| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2018-03-13| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2018-03-20| B06I| Publication of requirement cancelled [chapter 6.9 patent gazette]|Free format text: ANULADA A PUBLICACAO CODIGO 6.6.1 NA RPI NO 2462 DE 13/03/2018 POR TER SIDO INDEVIDA. |
    2019-05-07| B06T| Formal requirements before examination [chapter 6.20 patent gazette]|
    2019-07-30| B15K| Others concerning applications: alteration of classification|Free format text: AS CLASSIFICACOES ANTERIORES ERAM: A61K 8/34 , A61K 8/41 , A61K 8/42 , A61Q 5/12 Ipc: A61K 8/04 (2006.01), A61K 8/34 (2006.01), A61K 8/4 |
    2019-08-06| B07A| Application suspended after technical examination (opinion) [chapter 7.1 patent gazette]|
    2020-01-28| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-02-18| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 24/07/2013, OBSERVADAS AS CONDICOES LEGAIS. |
    2021-02-09| B25A| Requested transfer of rights approved|Owner name: UNILEVER IP HOLDINGS B.V. (NL) |
    优先权:
    申请号 | 申请日 | 专利标题
    EP12178165.2|2012-07-27|
    EP12178165|2012-07-27|
    PCT/EP2013/065645|WO2014016351A2|2012-07-27|2013-07-24|Process|
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