CN103201373A - 洗衣用洗涤剂颗粒 - Google Patents
洗衣用洗涤剂颗粒 Download PDFInfo
- Publication number
- CN103201373A CN103201373A CN2011800496478A CN201180049647A CN103201373A CN 103201373 A CN103201373 A CN 103201373A CN 2011800496478 A CN2011800496478 A CN 2011800496478A CN 201180049647 A CN201180049647 A CN 201180049647A CN 103201373 A CN103201373 A CN 103201373A
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- Prior art keywords
- detergent particle
- coated detergent
- particle
- weight
- dyestuff
- Prior art date
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- SEACYXSIPDVVMV-UHFFFAOYSA-L eosin Y Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C1=C2C=C(Br)C(=O)C(Br)=C2OC2=C(Br)C([O-])=C(Br)C=C21 SEACYXSIPDVVMV-UHFFFAOYSA-L 0.000 description 1
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- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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- 108010020132 microbial serine proteinases Proteins 0.000 description 1
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- 108010087558 pectate lyase Proteins 0.000 description 1
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- HXITXNWTGFUOAU-UHFFFAOYSA-N phenylboronic acid Chemical compound OB(O)C1=CC=CC=C1 HXITXNWTGFUOAU-UHFFFAOYSA-N 0.000 description 1
- GVKCHTBDSMQENH-UHFFFAOYSA-L phloxine B Chemical compound [Na+].[Na+].[O-]C(=O)C1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1C1=C2C=C(Br)C(=O)C(Br)=C2OC2=C(Br)C([O-])=C(Br)C=C21 GVKCHTBDSMQENH-UHFFFAOYSA-L 0.000 description 1
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003219 pyrazolines Chemical class 0.000 description 1
- TVRGPOFMYCMNRB-UHFFFAOYSA-N quinizarine green ss Chemical compound C1=CC(C)=CC=C1NC(C=1C(=O)C2=CC=CC=C2C(=O)C=11)=CC=C1NC1=CC=C(C)C=C1 TVRGPOFMYCMNRB-UHFFFAOYSA-N 0.000 description 1
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- UWMZZSRDUVJJDP-UHFFFAOYSA-M sodium 2-[3-(2-methylanilino)-6-(2-methyl-4-sulfonatoanilino)xanthen-10-ium-9-yl]benzoate Chemical compound [Na+].Cc1ccccc1Nc1ccc2c(-c3ccccc3C([O-])=O)c3ccc(Nc4ccc(cc4C)S([O-])(=O)=O)cc3[o+]c2c1 UWMZZSRDUVJJDP-UHFFFAOYSA-M 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- DJDYMAHXZBQZKH-UHFFFAOYSA-M sodium;1-amino-4-(cyclohexylamino)-9,10-dioxoanthracene-2-sulfonate Chemical compound [Na+].C1=2C(=O)C3=CC=CC=C3C(=O)C=2C(N)=C(S([O-])(=O)=O)C=C1NC1CCCCC1 DJDYMAHXZBQZKH-UHFFFAOYSA-M 0.000 description 1
- GTKIEPUIFBBXJQ-UHFFFAOYSA-M sodium;2-[(4-hydroxy-9,10-dioxoanthracen-1-yl)amino]-5-methylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC(C)=CC=C1NC1=CC=C(O)C2=C1C(=O)C1=CC=CC=C1C2=O GTKIEPUIFBBXJQ-UHFFFAOYSA-M 0.000 description 1
- RBYJOOWYRXEJAM-UHFFFAOYSA-M sodium;5,9-dianilino-7-phenylbenzo[a]phenazin-7-ium-4,10-disulfonate Chemical compound [Na+].C=1C=CC=CC=1[N+]1=C2C=C(NC=3C=CC=CC=3)C(S(=O)(=O)[O-])=CC2=NC(C2=CC=CC(=C22)S([O-])(=O)=O)=C1C=C2NC1=CC=CC=C1 RBYJOOWYRXEJAM-UHFFFAOYSA-M 0.000 description 1
- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 230000019635 sulfation Effects 0.000 description 1
- 238000005670 sulfation reaction Methods 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- UJMBCXLDXJUMFB-GLCFPVLVSA-K tartrazine Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C1=NN(C=2C=CC(=CC=2)S([O-])(=O)=O)C(=O)C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 UJMBCXLDXJUMFB-GLCFPVLVSA-K 0.000 description 1
- 235000012756 tartrazine Nutrition 0.000 description 1
- 239000004149 tartrazine Substances 0.000 description 1
- GMMAPXRGRVJYJY-UHFFFAOYSA-J tetrasodium 4-acetamido-5-hydroxy-6-[[7-sulfonato-4-[(4-sulfonatophenyl)diazenyl]naphthalen-1-yl]diazenyl]naphthalene-1,7-disulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].OC1=C2C(NC(=O)C)=CC=C(S([O-])(=O)=O)C2=CC(S([O-])(=O)=O)=C1N=NC(C1=CC(=CC=C11)S([O-])(=O)=O)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 GMMAPXRGRVJYJY-UHFFFAOYSA-J 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
- ZNRSXPDDVNZGEN-UHFFFAOYSA-K trisodium;chloride;sulfate Chemical compound [Na+].[Na+].[Na+].[Cl-].[O-]S([O-])(=O)=O ZNRSXPDDVNZGEN-UHFFFAOYSA-K 0.000 description 1
- ABDKAPXRBAPSQN-UHFFFAOYSA-N veratrole Chemical compound COC1=CC=CC=C1OC ABDKAPXRBAPSQN-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/40—Dyes ; Pigments
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/08—Silicates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/10—Carbonates ; Bicarbonates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Detergent Compositions (AREA)
Abstract
本发明提供了一种扁豆状或圆盘状的涂覆洗涤剂颗粒,其具有正交尺寸x、y和z,所述颗粒包含:(i)40至90重量%的表面活性剂,其选自:阴离子型表面活性剂和非离子型表面活性剂;(ii)1至40重量%的水溶性无机盐;(iii)0.0001至0.1重量%的染料,其中所述染料选自:阴离子型染料和非离子型染料;和(iv)0至3重量%的香料,其中所述无机盐和染料在所述洗涤剂颗粒上作为涂层存在,而所述表面活性剂作为核存在。
Description
发明领域
本发明涉及大的洗衣用洗涤剂颗粒。
发明背景
WO 9932599描述了制造洗衣用洗涤剂颗粒的方法,所述方法是挤出法,在所述方法中,增效剂和表面活性剂(该表面活性剂包含硫酸盐或磺酸盐阴离子型表面活性剂作为主要组分)被送入在至少40℃、优选至少60℃温度下机械工作的挤出机中,并通过具有许多挤出孔的挤出头被挤出。在大多数实施例中,表面活性剂与增效剂一起以大于1份增效剂比2份表面活性剂的重量比供应给挤出机。挤出物明显需要进一步干燥。在实施例6中,PAS糊料被干燥和挤出。这种PAS条是现有技术中已知的。所述条通常是圆柱形形状,并且它们的长度超过它们的直径,如实施例2所述。
US 7,022,660公开了用于制备具有涂层的洗涤剂颗粒的方法。
发明概述
我们已经发现,可能具有一种提供减轻沾染(staining)的含染料的涂层。本发明还可以提高所述染料在产品储存时的光稳定性。
在一个方面,本发明提供一种正交尺寸为x、y和z的涂覆洗涤剂颗粒,其中x是从1至2mm、y是从2至8mm(优选3至8mm)、和z是从2至8mm(优选3至8mm),其中所述颗粒包含:
(i)40至90重量%、优选50至90重量%的表面活性剂,其选自:阴离子型表面活性剂;和非离子型表面活性剂;
(ii)1至40重量%、优选20至40重量%的水溶性无机盐;
(iii)0.0001至0.1重量%的染料,优选0.001至0.01重量%的染料,其中所述染料选自:阴离子型染料;和非离子型染料;
(iv)0至3重量%、优选0.001至3重量%的香料,并且,其中所述无机盐和染料在所述洗衣用洗涤剂颗粒上作为涂层存在,而所述表面活性剂作为核存在。
除非另有说明,所有重量%是指颗粒中以干重计的总百分比。
在另一个方面,本发明提供了一种涂覆洗涤剂颗粒,它是表面活性剂多于无机固体的浓缩制剂。只有通过使所述涂层包覆柔软的表面活性剂,才能产生这种洗涤所需的单位用量降低的颗粒状浓缩物。向所述核添加溶剂将导致将所述颗粒转变为液体制剂。另一方面,具有更高量的无机固体将产生较低浓缩的制剂;高的无机含量将使制剂返回到常规的低表面活性剂浓度的粒状粉末。本发明的涂覆洗涤剂颗粒介于这两种常规(液体和粒状)形式之间。
发明详述
形状
优选地,所述涂覆的洗衣用洗涤剂颗粒是曲面的。
涂覆的洗衣用洗涤剂颗粒可以是扁豆形的(形状像完整的干的小扁豆)、即扁椭球体,其中z和y是赤道直径,且x是极直径;优选y=z。
所述涂覆的洗衣用洗涤剂颗粒可以是圆盘形状。
优选地,涂覆的洗衣用洗涤剂颗粒没有孔;也就是说,所述涂覆的洗衣用洗涤剂颗粒没有贯穿过核的贯通通道,即所述涂覆的洗涤剂颗粒具有的拓扑亏格(topologic genus)为零。
核
表面活性剂
涂覆的洗衣用洗涤剂颗粒包含40至90重量%、优选50至90重量%的表面活性剂,最优选70至90重量%。一般而言,表面活性剂体系的非离子型和阴离子型表面活性剂可以选自下列文献描述的表面活性剂:Schwartz & Perry的″表面活性剂(Surface Active Agents)″第一卷,Interscience,1949年,和Schwartz、Perry & Berch的第二卷,Interscience,1958年;在Manufacturing Confectioners Company出版的现行版″McCutcheon的乳化剂和洗涤剂(McCutcheon′s Emulsifiers andDetergents)″中或在H.Stache的第二版,Carl Hauser Verlag,1981年的″Tenside-Taschenbuch″中。优选地,所使用的表面活性剂是饱和的。
阴离子型表面活性剂
可以使用的合适的阴离子型洗涤剂化合物通常是具有含约8至约22个碳原子的烷基的有机硫酸和磺酸的水溶性碱金属盐,所用的术语烷基包括较高级酰基的烷基部分。合适的合成的阴离子型洗涤剂化合物的例子是烷基硫酸钠和烷基硫酸钾,尤其是通过将从例如牛脂或椰子油产生的C8至C18的高级醇硫酸化而得到的那些;烷基C9至C20苯磺酸钠和钾,特别是直链仲烷基C10至C15苯磺酸钠;和烷基甘油基醚硫酸钠,尤其是从牛脂或椰子油衍生的较高级醇和从石油衍生的合成醇的那些醚。最优选的阴离子型表面活性剂是月桂基醚硫酸钠(SLES),特别优选具有1至3个乙氧基,C10至C15的烷基苯磺酸钠和C12至C18的烷基硫酸钠。适用的表面活性剂还有例如EP-A-328 177(Unilever)中描述的那些(其显示出耐盐析性),EP-A-070 074中描述的烷基多聚糖苷,和烷基单糖苷。所述表面活性剂的链可以是支链的或直链的。
皂也可以存在。使用的脂肪酸皂优选含有约16至约22个碳原子,优选为直链构型。皂的阴离子贡献优选是总阴离子的0至30重量%。
优选地,至少50重量%的阴离子型表面活性剂选自:C11至C15的烷基苯磺酸钠;和C12至C18的烷基硫酸钠。甚至更优选地,所述阴离子型表面活性剂是C11至C15的烷基苯磺酸钠。
优选地,所述涂覆的洗衣用洗涤剂颗粒中存在的阴离子型表面活性剂的水平是总表面活性剂的15至85重量%,更优选50至80重量%。
非离子型表面活性剂
可以使用的合适的非离子型洗涤剂化合物特别包括,具有疏水基和反应性氢原子的化合物(例如脂族醇、酸、酰胺或烷基酚)与环氧烷(尤其是单独的环氧乙烷或其与环氧丙烷一起)的反应产物。优选的非离子型洗涤剂化合物是C6至C22的烷基酚-环氧乙烷缩合物,通常为5-25EO、即每分子中含5至25个环氧乙烷单元,以及直链或支链的脂族C8至C18伯或仲醇与环氧乙烷的缩合产物,通常5-50EO。优选地,所述非离子型化合物是10-50EO,更优选20-35EO。特别优选烷基乙氧基化物。
优选非离子型表面活性剂在所述涂覆的洗衣用洗涤剂颗粒中存在的水平是总表面活性剂的5至75重量%,更优选为总表面活性剂的10至40重量%。
阳离子型表面活性剂可以作为次要成分存在,其水平优选是总表面活性剂的0至5重量%。
优选地,在干燥之前将所有表面活性剂混合在一起。可以使用常规的混合设备。可以通过挤出或碾压形成洗衣用洗涤剂颗粒的表面活性剂核,随后用无机盐涂覆。
耐钙的表面活性剂体系
在另一个方面,所使用的表面活性剂体系是耐钙的,因为这减少了对增效剂的需要,所以是优选的方案。
优选不需要存在增效剂就能在硬水中有效洗涤的表面活性剂混合物。如果它们通过了下文中提出的测试的话,这样的混合物就被称为耐钙的表面活性剂混合物。然而,本发明也可以用于软水洗涤,所述软水是天然存在的或利用软水剂制成的。在这种情况下,耐钙性不再重要,并且可以使用并非耐钙的那些混合物。
如下测试表面活性剂混合物的耐钙性:
所讨论的表面活性剂混合物制成每升水0.7g表面活性剂固体的浓度,所述水含有足够的钙离子以产生40的French硬度(4x 10-3摩尔Ca2+)。向所述溶液添加其他不含硬度离子的电解质,例如氯化钠、硫酸钠和氢氧化钠,以将离子强度调节到0.05M和将pH调节到10。在样品制备之后15分钟测量波长540nm的光通过4mm样品的吸收。做十次测量并计算平均值。给出小于0.08的吸收值的样品被认为是耐钙的。
满足上述耐钙性测试的表面活性剂混合物的例子包括下述的那些:其具有LAS表面活性剂(本身不是耐钙的)作为主要部分与一种或多种耐钙的其他表面活性剂(助表面活性剂)混合,产生充分耐钙以致可在很少或没有增效剂下使用并通过所给定的测试的混合物。合适的耐钙的助表面活性剂包括SLES 1-7EO,和烷基-乙氧基化物非离子型表面活性剂,特别是熔点低于40℃的那些。
LAS/SLES表面活性剂混合物具有优于LAS非离子型表面活性剂混合物的泡沫特性,因此是需要高水平泡沫的手洗制剂中优选的。SLES可以使用的水平最多为表面活性剂混合物的30重量%。
水溶性无机盐
水溶性无机盐优选选自碳酸钠、氯化钠、硅酸钠和硫酸钠、或其混合物,最优选总水溶性无机盐的70至100重量%是碳酸钠。水溶性无机盐在颗粒上作为涂层存在。水溶性无机盐优选以将所述洗衣用洗涤剂颗粒的粘度降低至一个值的水平存在,在该值下所述颗粒是自由流动的。
本领域技术人员将理解,虽然可以施加具有相同或不同涂层材料的多个涂层,但为操作简单和使涂覆的厚度最大化,优选单层涂覆。为了使洗涤剂颗粒的抗结块性能的结果最好,涂覆的量应该是所述颗粒的1至40重量%、优选20至40重量%、更优选25至35重量%。
所述涂层优选通过从水溶性无机盐的水溶液沉积而施加于表面活性剂核的表面上。或者,可以使用浆料进行涂覆。所述水溶液优选含有大于50g/L、更优选200g/L的所述盐。已经发现,所述涂覆溶液在流化床中的水性喷雾给出良好的结果,并还可以在所述流化过程期间对洗涤剂颗粒产生轻微的圆滑作用。可能需要干燥和/或冷却来完成所述过程。
优选的耐钙的涂覆洗衣用洗涤剂颗粒中的表面活性剂包含15至100重量%的阴离子型表面活性剂,表面活性剂的20至30重量%是月桂基醚硫酸钠。
染料
染料描述于K.Hunger编辑的Industrial Dyes,2003,Wiley-VCH ISBN3-527-30426-6中。
用于本发明中的染料选自阴离子型和非离子型染料。阴离子型染料在pH 7的水性介质中是带负电的。阴离子型染料的实例参见颜色索引(Colour Index)(Society of Dyers and Colourists和American Associationof Textile Chemists and Colorists 2002)中的酸性和直接染料类别。阴离子型染料优选含有至少一个磺酸盐或羧酸盐基团。非离子型染料在pH 7的水性介质中是不带电的,实例发现于颜色索引(Colour Index)中的分散染料类别中。
染料可以烷氧基化。烷氧基化染料优选具有以下的通式:染料-NR1R2。NR1R2基团连接到染料的芳香环。R1和R2独立地选自具有2个或更多个重复单元的聚氧化烯链,并且优选具有2-20个重复单元。聚氧化烯链的实例包括环氧乙烷、环氧丙烷、缩水甘油醚(glycidoloxide)、氧化丁烯及其混合物。
优选的聚氧化烯链是[(CH2CR3HO)x(CH2CR4HO)yR5),其中x+y≤5,其中y≥1,并且z=0-5,R3选自:H、CH3、CH2O(CH2CH2O)zH及其混合物;R4选自:H、CH2O(CH2CH2O)zH及其混合物;以及R5选自:H、和CH3。
用于本发明中的优选烷氧基化染料是:
优选地,染料选自酸性染料、分散染料和烷氧基化染料。
最优选地,染料是非离子型染料。
优选地,染料选自具有蒽醌、单偶氮、双偶氮、呫吨(xanthene)、酞菁、和吩嗪发色团的那些。更优选地,染料选自具有蒽醌和单偶氮发色团的那些。
所述染料加入涂层浆料中并搅拌,之后施涂于颗粒的核上。施涂可以通过任何合适的方法,优选喷雾到如以上详述的核颗粒上。
染料可以是任何颜色的,优选染料是蓝色、紫色、绿色或红色。最优选,染料是蓝色或紫色。
优选地,染料选自:酸性蓝80、酸性蓝62、酸性紫43、酸性绿25、直接蓝86、酸性蓝59、酸性蓝98、直接紫9、直接紫99、直接紫35、直接紫51、酸性紫50、酸性黄3、酸性红94、酸性红51、酸性红95、酸性红92、酸性红98、酸性红87、酸性黄73、酸性红50、酸性紫9、酸性红52、食品黑1、食品黑2、酸性红163、酸性黑1、酸性橙24、酸性黄23、酸性黄40、酸性黄11、酸性红180、酸性红155、酸性红1、酸性红33、酸性红41、酸性红19、酸性橙10、酸性红27、酸性红26、酸性橙20、酸性橙6、磺酸化的Al和Zn酞菁、溶剂紫13、分散紫26、分散紫28、溶剂绿3、溶剂蓝63、分散蓝56、分散紫27、溶剂黄33、分散蓝79:1。
染料优选是为洗衣织物赋予洁白感的遮蔽染料(shading dye)。优选酸性紫50、溶剂紫13、分散紫27、分散紫28、烷氧基化噻吩,或阳离子吩嗪,如WO 2009/141172和WO 2009/141173中所述。存在遮蔽染料时,优选存在另外的绿色染料,以将颗粒的颜色从紫色转变成蓝-绿色。
染料可以共价结合到聚合物上。
可以使用染料组合。
涂覆的洗衣用洗涤剂颗粒
优选地,所述涂覆的洗衣用洗涤剂颗粒占包装中洗衣用洗涤剂制剂的10至100重量%、更优选50至100重量%、甚至更优选80至100重量%、最优选90至100重量%。
所述包装是用于向公众销售的商业制剂的包装,优选在0.01kg至5kg、优选0.02kg至2kg、最优选0.5kg至2kg的范围内。
优选地,所述涂覆的洗衣用洗涤剂颗粒使得至少90至100%的涂覆洗衣用洗涤剂颗粒中最大与最小的涂覆洗衣用洗涤剂颗粒在x、y和z尺寸上的变化在20%以内、优选10%以内。
含水量
在293K和50%相对湿度下,所述颗粒优选包含0到15重量%的水,更优选0到10重量%,最优选1到5重量%的水。这促进了所述颗粒的储存稳定性和它的机械性质。
其他助剂
所述涂层或核中可以存在如下所述的助剂。它们可以存在于核或涂层中。
荧光剂
涂覆的洗衣用洗涤剂颗粒优选包含荧光剂(荧光增白剂)。荧光剂是公知的,并且许多这样的荧光剂是市售的。通常,这些荧光剂以它们的碱金属盐例如钠盐的形式供应和使用。所述组合物中使用的一种或多种荧光剂的总量通常为0.005到2重量%,更优选0.01到0.1重量%。适合用于本发明的荧光剂描述在K.Hunger编著的《工业染料》(IndustrialDyes)第7章(2003年,Wiley-VCH ISBN 3-527-30426-6)中。
优选的荧光剂选自以下类别:二苯乙烯联苯、三嗪基氨基均二苯代乙烯、二(1,2,3-***-2-基)均二苯代乙烯、二(苯并[b]呋喃-2-基)联苯、1,3-二苯基-2-吡唑啉和香豆素。所述荧光剂优选是磺化的。
优选的荧光剂类别是:二-苯乙烯联苯化合物,例如Tinopal(商标)CBS-X,二-胺均二苯代乙烯二磺酸化合物,例如Tinopal DMS pureXtra和Blankophor(商标)HRH,和吡唑啉化合物,例如Blankophor SN。优选的荧光剂是:2(4-苯乙烯基-3-磺苯基)-2H-萘酚[1,2-d]***钠,4,4′-二{[4-苯胺基-6-(N-甲基-N-2-羟乙基)氨基-1,3,5-三嗪-2-基)]氨基}均二苯代乙烯-2-2′二磺酸二钠,4,4′-二{[4-苯胺基-6-吗啉基-1,3,5-三嗪-2-基)]氨基}均二苯代乙烯-2-2′二磺酸二钠,和4,4′-二(2-磺基苯乙烯基)联苯二钠。
TinopalDMS是4,4′-二{[4-苯胺基-6-吗啉基-1,3,5-三嗪-2-基)]氨基}均二苯代乙烯-2-2′二磺酸二钠的二钠盐。TinopalCBS是4,4′-二(2-磺基苯乙烯基)联苯二钠的二钠盐。
香料
优选所述组合物包含香料。所述香料优选为0.001到3重量%、最优选0.1到1重量%。许多合适的香料实例提供在CFTA Publications出版的CTFA(化妆品及盥洗用品、香水协会(Cosmetic,Toiletry andFragrance Association))1992年国际买家指南(1992 International BuyersGuide),和Schnell Publishing Co.出版的OPD 1993年化学品买家目录80周年版(Chemicals Buyers Directory 80th Annual Edition)中。
制剂中存在多种香料组份是很寻常的。在本发明的组合物中,可有四种或更多种、优选五种或更多种、更优选六种或更多种或甚至七种或更多种不同的香料组份。
在香料混合物中,优选15到25重量%是头香。头香由Poucher定义(Journal of the Society of Cosmetic Chemists 6(2):80[1955])。优选的头香选自柑橘油、里哪醇、乙酸里哪酯、熏衣草、二氢月桂烯醇、玫瑰醚和顺式-3-己醇。
所述香料起到分散染料以使所述染料更直观的作用。
优选所述涂覆的洗衣用洗涤剂颗粒不含过氧漂白剂,例如过碳酸钠、过硼酸钠和过酸。
聚合物
所述组合物可以包含一种或多种其它的聚合物。实例是羧甲基纤维素、聚(乙二醇)、聚(乙烯醇)、聚乙烯亚胺、乙氧基化聚乙烯亚胺、水溶性聚酯聚合物、聚羧酸酯例如聚丙烯酸酯、马来酸/丙烯酸共聚物和甲基丙烯酸月桂酯/丙烯酸共聚物。
酶
本发明的组合物中优选存在一种或多种酶。
优选每种酶的水平是基于产品计0.0001重量%至0.5重量%蛋白质。
特别可使用的酶包括蛋白酶、α-淀粉酶、纤维素酶、脂肪酶、过氧化物酶/氧化酶、果胶酸裂解酶、和甘露聚糖酶,或其混合物。
适合的脂肪酶包括细菌或真菌来源的那些脂肪酶。包括化学修饰或蛋白质工程的突变体。有用的脂肪酶的实例包括源自腐质霉属(Humicola)(同义词嗜热真菌属(Thermomyces))的脂肪酶,例如源自EP258068和EP 305216中所述的疏棉状腐质霉(H.lanuginosa)(细毛嗜热霉(T.lanuginosus))或出自WO 96/13580中所述的特异腐质霉(H.insolens);假单胞菌属(Pseudomonas)脂肪酶,例如源自产碱假单胞菌属(P.alcaligenes)或类产碱假单胞菌(P.pseudoalcaligenes)(EP 218272)、洋葱假单胞菌(P.cepacia)(EP 331 376)、斯氏假单胞菌(P.stutzeri)(GB 1,372,034)、荧光假单胞菌(P.fluorescens)、假单胞菌属菌株SD 705(WO 95/06720和WO 96/27002),威斯康星假单胞菌(P.wisconsinensis )(WO 96/12012);芽孢杆菌属(Bacillus)脂肪酶,例如源自枯草芽孢杆菌(B.subtilis)(Dartois等(1993),Biochemica etBiophysica Acta,1131,253-360)、嗜热脂肪芽胞杆菌(B.stearothermophilus)(JP 64/744992)或短小芽孢杆菌(B.pumilus)(WO91/16422)。
其他实例有脂肪酶变体,例如下列文献中描述的那些:WO92/05249、WO 94/01541、EP 407 225、EP 260 105、WO 95/35381、WO96/00292、WO 95/30744、WO 94/25578、WO 95/14783、WO 95/22615、WO 97/04079、WO 97/07202、WO 00/60063、WO 09/107091和WO09/111258。
优选的可商购的脂肪酶包括LipolaseTM和Lipolase UltraTM,LipexTM(Novozymes A/S)和LipocleanTM。
本发明的方法可以在归类为EC 3.1.1.4和/或EC 3.1.1.32的磷脂酶存在下进行。在本文中使用时,术语磷脂酶是指对磷脂有活性的酶。
磷脂,例如卵磷脂或磷脂酰胆碱,由甘油的外部(sn-1)和中部(sn-2)位置被两个脂肪酸酯化并且其第三个位置被磷酸酯化而构成;所述磷酸进而可以被酯化为氨基醇。磷脂酶是参与磷脂水解的酶。可以区别几种类型的磷脂酶活性,包括水解一个脂酰基(分别在sn-1和sn-2位置)形成溶血磷脂的磷脂酶A1和A2;和可以水解溶血磷脂中剩余脂肪酰基的溶血磷脂酶(或磷脂酶B)。磷脂酶C和磷脂酶D(磷酸二脂酶)分别释放二酰基甘油或磷脂酸。
合适的蛋白酶包括动物、植物或微生物来源的蛋白酶。优选微生物来源的。包括化学修饰或蛋白质工程的突变体。所述蛋白酶可以是丝氨酸蛋白酶或金属基蛋白酶,优选碱性微生物蛋白酶或类胰蛋白酶。优选的市售蛋白酶包括AlcalaseTM、SavinaseTM、PrimaseTM、DuralaseTM、DyrazymTM、EsperaseTM、EverlaseTM、PolarzymeTM和KannaseTM(Novozymes A/S)、MaxataseTM、MaxacalTM、MaxapemTM、ProperaseTM、PurafectTM、Purafect OxPTM、FN2TM、和FN3TM(GenencorInternational Inc.)。
本发明的方法可以在归类为EC 3.1.1.74的角质酶存在下进行。本发明使用的角质酶可以是任何来源的。优选的角质酶是微生物来源的,特别是细菌、真菌或酵母来源的。
合适的淀粉酶(α和/或β)包括细菌或真菌来源的淀粉酶。包括化学修饰或蛋白质工程的突变体。淀粉酶包括例如如下来源的α-淀粉酶:芽孢杆菌属、例如在GB 1,296,839中有更详细描述的地衣形芽胞杆菌(B.licheniformis)特殊菌株、或WO 95/026397或WO 00/060060中公开的芽孢杆菌菌株。市售的淀粉酶是DuramylTM、TermamylTM、TermamylUltraTM、NatalaseTM、StainzymeTM、FungamylTM和BANTM(NovozymesA/S)、RapidaseTM和PurastarTM(来自Genencor International Inc.)。
合适的纤维素酶包括细菌或真菌来源的那些纤维素酶。包括化学修饰或蛋白质工程的突变体。合适的纤维素酶包括源自芽孢杆菌属、假单胞菌属、腐质霉菌属、镰刀菌属(Fusarium)、梭孢壳属(Thielavia)、枝顶孢属(Acremonium)的纤维素酶,例如US 4,435,307、US 5,648,263、US 5,691,178、US 5,776,757、WO 89/09259、WO 96/029397和WO98/012307中公开的由特异腐质霉(Humicola insolens)、土生梭孢霉(Thielavia terrestris)、嗜热毁丝霉(Myceliophthora thermophila)和尖孢镰刀菌(Fusarium oxysporum)产生的真菌纤维素酶。可商购的纤维素酶包括CelluzymeTM、CarezymeTM、EndolaseTM、RenozymeTM(Novozymes A/S)、ClazinaseTM和Puradax HATM(Genencor InternationalInc.)、和KAC-500(B)TM(Kao Corporation)。
合适的过氧化物酶/氧化酶包括植物、细菌或真菌来源的那些。包括化学修饰或蛋白质工程的突变体。有用的过氧化物酶的例子包括出自鬼伞属(Coprinus)、例如出自灰盖鬼伞(C.cinereus)的过氧化物酶,及其变体,如WO 93/24618、WO 95/10602和WO 98/15257中描述的那些。市售的过氧化物酶包括GuardzymeTM和NovozymTM 51004(NovozymesA/S)。
适用的其它酶公开在WO2009/087524,WO2009/090576、WO2009/148983和WO2008/007318中。
酶稳定剂
组合物中存在的任何酶可以利用常规的稳定剂稳定,所述稳定剂例如,多元醇(如丙二醇或甘油)、糖或糖醇、乳酸、硼酸、或硼酸衍生物例如芳族硼酸酯、或苯基硼酸衍生物例如4-甲酰基苯基硼酸,并且所述组合物可以按照例如WO 92/19709和WO 92/19708中的描述配制。
在烷基长得足以形成分支链或环状链时,所述烷基包含支链、环状和直链的烷基链。烷基优选是直链或支链的,最优选直链的。
除非另有说明,“一”或“一个”和相应的“所述”在本文中使用时是指至少一个、或一个或多个。除非另作说明,该单数形式包括复数。
所述涂覆的洗衣用洗涤剂颗粒中可以存在螯合剂。
优选所述涂覆的洗涤剂颗粒的核壳比为3至1∶1,最优选2.5至1.5∶1;最佳核壳比是2∶1。
试验
LAS指直链烷基苯磺酸盐。PAS是指伯烷基硫酸盐。NI是指具有平均30个乙氧基化单元和C12-14烷基链的乙氧基化醇非离子型表面活性剂。具体使用如下物质:LAS-来自Unger的UFASAN 65,PAS-来自Stepan的Stepanol CFAS70,和NI-来自BASF的Leutensol AO 30。
实施例1:(颗粒制造)
两种涂覆洗衣用洗涤剂颗粒颜色通过含有酸性紫50产生,使得:
颗粒1在核中含有酸性紫50(参照)
颗粒2在碳酸盐涂层中含有酸性紫50
所述颗粒是扁椭球体,其具有以下尺寸:x=1.1mm,y=4.0mm,z=5.0mm。
所述颗粒每个重~0.013g。
颗粒1看起来呈现紫色,颗粒2看起来呈现灰白色。
制备颗粒1的核
1962.5g干燥、磨细的表面活性剂混合物(LAS/PAS/NI以重量计68/17/15)与37.38g香料油和0.124g酸性紫50染料充分混合。然后利用ThermoFisher 24HC双螺杆挤出机以8kg/hr的速率运行,挤出所述混合物。挤出机的入口温度设置在20℃,在马上要到模具板之前上升至40℃。使用的模具板钻有6个直径5mm的圆形孔。
挤出的制品在模具板之后利用设置成产生~1.1mm厚度的颗粒的高速切割器进行切割。
颗粒1的涂层
764g上述的挤出物被装载到Strea 1实验室流化床式干燥机(Aeromatic-Fielder AG)的流化室,并利用顶喷配置,使用1069g在748.3g水中含有320.7g碳酸钠的溶液进行喷涂。
将所述涂层溶液通过蠕动泵(Watson-Marlow 101U/R型)进料至Strea 1的喷嘴,进料的初始速度为3.3g/min,在所述涂覆试验的过程中上升到9.1g/min。
流化床涂布机运行时,初始进气口空气温度为55℃,在所述涂覆试验过程中增加到90℃,同时出口温度在整个涂层过程中始终保持在45-50℃的范围。
制备颗粒2的核
1962.9g干燥、磨细的表面活性剂混合物(LAS/PAS/NI以重量计68/17/15)与37.38g香料油混合,并利用ThermoFisher 24HC双螺杆挤出机以8kg/hr速率运行挤出所述混合物。挤出机的入口温度设置在20℃,在马上要到模具板之前上升至40℃。使用的模具板钻有6个直径5mm的圆形孔。
挤出的制品在模具板之后利用设置成产生~1.1mm厚度的颗粒的高速切割器进行切割。
颗粒2的涂层
715g上述挤出物被装载到Strea 1实验室流化床式干燥机(Aeromatic-Fielder AG)的流化室,并利用顶喷配置,使用1000g在0.09g酸性紫50和669.91水中含有300g碳酸钠的溶液进行喷涂。
将所述涂层溶液通过蠕动泵(Watson-Marlow 101U/R型)进料至Strea 1的喷雾嘴,进料的初始速度为2.7g/min,在所述涂覆试验的过程中上升到25g/min。
流化床涂布机运行时,初始进气口空气温度为60℃,在所述涂覆试验过程中增加到75℃,同时出口温度在整个涂覆过程中始终保持在47-52℃的范围。
实施例2:(液体的颜色)
2.04g颗粒2和2.25g颗粒1分别溶解在100mL软化水中。溶液以11000RPM离心15分钟,在UV-VIS吸收分光计上测量液体的颜色。这两种液体看起来都呈紫色。
UV-VIS光谱为这两种溶液给出了酸性紫50的光谱,最大吸收在570nm。光密度在下表中给出:
光密度(5cm),570nm下 | |
颗粒1:染料在核中(参照) | 0.175 |
颗粒2:染料在涂层中 | 0.155 |
这两种颗粒都将酸性紫50有效传递给溶液。
实施例3:(沾染)
每种颗粒25个分散在20×20cm的白色棉织物片上,所述棉织物片浸在500mL软化水中,使得所述布被2cm水覆盖。所述颗粒静置40分钟,然后将布洗涤、漂洗和干燥。计数每块布上污斑的数量,并计算%沾染。%沾染是产生污斑的颗粒的分数:
%沾染=100x(污斑数)/(颗粒数)
结果在下表中给出:
%沾染 | |
颗粒1:染料在核中(参照) | 12 |
颗粒2:染料在涂层中 | 4 |
染料在涂层中的颗粒意外地显示出最少的沾染。
实施例4:(颗粒制造)
两种涂覆洗衣用洗涤剂颗粒颜色通过含有酸性紫50产生,使得:
颗粒3在核中含有酸性紫50(参照)
颗粒4在碳酸盐涂层中含有酸性紫50
所述颗粒是扁椭球体,具有以下尺寸x=1.1mm,y=4.0mm,z=5.0mm。
所述颗粒每个重~0.013g。
制备颗粒3的核(参照)
2000g干燥、磨细的表面活性剂混合物(LAS/PAS/NI以重量计68/17/15)与0.124g酸性紫50染料充分混合。然后利用ThermoFisher24HC双螺杆挤出机以8kg/hr的速率运行,挤出所述混合物。挤出机的入口温度设置在20℃,在马上要到模具板之前上升至40℃。使用的模具板钻有6个直径5mm的圆形孔。
挤出的产品在模板之后利用设置成产生~1.1mm厚度的颗粒的高速切割器进行切割。
颗粒3的涂层(参照)
764g上述的挤出物被装载到Strea 1实验室流化床式干燥机(Aeromatic-Fielder AG)的流化室,并利用顶喷配置,使用1069g在748.3g水中含有320.7g碳酸钠的溶液进行喷涂。
将所述涂层溶液通过蠕动泵(Watson-Marlow 101U/R型)进料给Strea1的喷雾嘴,进料初始速度为3.3g/min,在所述涂覆试验的过程中上升到9.1g/min。
流化床涂布机运行时,初始进气口空气温度为55℃,在所述涂覆试验过程中增加到90℃,同时出口温度在整个涂覆过程中始终保持在45-50℃的范围。
制备颗粒4的核
2000g干燥、磨细的表面活性剂混合物(LAS/PAS/NI以重量计68/17/15)利用以8kg/hr速率运行的ThermoFisher 24HC双螺杆挤出机挤出。挤出机的入口温度设置在20℃,在马上要到模具板之前上升至40℃。使用的模具板钻有6个直径5mm的圆形孔。
挤出的制品在模具板之后利用设置成产生~1.1mm厚度的颗粒的高速切割器进行切割。
颗粒4的涂层
715g上述挤出物被装载到Strea 1实验室流化床式干燥机(Aeromatic-Fielder AG)的流化室,并利用顶喷配置,使用1000g在0.09g酸性紫50和669.91g水中含有300g碳酸钠的溶液进行喷涂。
将所述涂层溶液通过蠕动泵(Watson-Marlow 101U/R型)进料给Strea 1的喷雾嘴,进料初始速度为2.7g/min,在所述涂覆试验的过程中上升到25g/min。
流化床涂布机运行时,初始进气口空气温度为60℃,在所述涂覆试验过程中增加到75℃,同时出口温度在整个涂覆过程中保持在47-52℃的范围。
实施例5:(液体的颜色)
2.04g颗粒3和2.04g颗粒4分别溶解在100mL软化水中。溶液以11000RPM离心15分钟,在UV-VIS吸收分光计上测量液体的颜色。这两种液体看起来都呈紫色。
UV-VIS光谱为这两种溶液给出酸性紫50的光谱,最大吸收在570nm。光密度在下表中给出:
光密度(5cm),570nm下 | |
颗粒3:染料在核中(参照) | 0.15 |
颗粒4:染料在涂层中 | 0.18 |
这两种颗粒均将酸性紫50有效传递给溶液。
实施例6:(染斑)
将每种颗粒25个分散在20*20cm的白色棉织物片上,所述棉织物片浸在500mL软化水中,使得所述布被2cm水覆盖。所述颗粒静置40分钟,然后将布洗涤、漂洗和干燥。计数每块布上的斑点数量并计算%染斑。%染斑是产生斑点的颗粒的分数:
%染斑=100x(斑点数)/(颗粒数)
结果在下表中给出:
%染斑 | |
颗粒3:染料在核中(参照) | 12 |
颗粒4:染料在涂层中 | 0 |
染料在涂层中的颗粒意外地显示出最少的染斑。
所述颗粒不含香料。
Claims (22)
1.一种涂覆洗涤剂颗粒,其具有正交尺寸x、y和z,其中x为1至2mm、y为2至8mm、和z为2至8mm,其中所述颗粒包含:
(i)40至90重量%的表面活性剂,其选自阴离子型表面活性剂和非离子型表面活性剂;
(ii)1至40重量%的水溶性无机盐;
(iii)0.0001至0.1重量%的染料,其中所述染料选自:阴离子型染料和非离子型染料;和
(iv)0至3重量%的香料,
其中所述无机盐和染料在所述洗涤剂颗粒上作为涂层存在,而所述表面活性剂作为核存在。
2.权利要求1的涂覆洗涤剂颗粒,其中所述染料选自酸性染料、分散性染料和烷氧基化染料。
3.权利要求1或2的涂覆洗涤剂颗粒,其中所述染料选自具有蒽醌、单偶氮、双偶氮、呫吨、酞菁、和吩嗪发色团的那些染料。
4.权利要求3的涂覆洗涤剂颗粒,其中所述染料选自具有蒽醌和单偶氮发色团的那些染料。
5.权利要求1的涂覆洗涤剂颗粒,其中所述染料选自非离子型染料。
6.前述权利要求任一项的涂覆洗涤剂颗粒,其中所述无机盐充当增效剂。
7.权利要求6的涂覆洗涤剂颗粒,其中所述无机盐包括碳酸钠。
8.前述权利要求任一项的涂覆洗涤剂颗粒,其中所述涂覆洗涤剂颗粒的总表面活性剂包含15到85重量%的阴离子型表面活性剂和5到75重量%的非离子型表面活性剂。
9.权利要求1-7任一项的涂覆洗涤剂颗粒,其中所述涂覆洗涤剂颗粒的总表面活性剂包含15到100重量%的阴离子型表面活性剂,其中20到30重量%是月桂基醚硫酸钠。
10.前述权利要求任一项的涂覆洗涤剂颗粒,其中所述阴离子型表面活性剂选自烷基苯磺酸盐、烷基醚硫酸盐、烷基硫酸盐。
11.权利要求10的涂覆洗涤剂颗粒,其中所述阴离子型表面活性剂选自具有1至3个乙氧基的月桂基醚硫酸钠、C10至C15烷基苯磺酸钠和C12至C18烷基硫酸钠。
12.前述权利要求任一项的涂覆洗涤剂颗粒,其中所述非离子型表面活性剂是10至50EO的非离子型表面活性剂。
13.权利要求12的涂覆洗涤剂颗粒,其中所述非离子型表面活性剂是直链或分支的脂族C8至C18伯或仲醇与20至35个环氧乙烷基团的缩合产物。
14.前述权利要求任一项的涂覆洗涤剂颗粒,其中所述涂覆洗涤剂颗粒总计包含20至40重量%的无机盐增效剂作为涂层。
15.权利要求14的涂覆洗涤剂颗粒,其中所述涂覆洗涤剂颗粒包含25至35重量%的无机盐增效剂作为涂层。
16.前述权利要求任一项的涂覆洗涤剂颗粒,其中所述颗粒包含0至15重量%的水。
17.权利要求16的涂覆洗涤剂颗粒,其中所述颗粒包含1至5重量%的水。
18.前述权利要求任一项的涂覆洗涤剂颗粒,其中所述涂覆洗涤剂颗粒占包装中洗涤剂制剂的10至100重量%。
19.权利要求18的涂覆洗涤剂颗粒,其中所述涂覆洗涤剂颗粒占包装中洗涤剂制剂的50至100重量%。
20.权利要求19的涂覆洗涤剂颗粒,其中所述涂覆洗涤剂颗粒占包装中洗涤剂制剂的80至100重量%。
21.权利要求20的涂覆洗涤剂颗粒,其中所述涂覆洗涤剂颗粒占包装中洗涤剂制剂的90至100重量%。
22.前述权利要求任一项的涂覆洗涤剂颗粒,其中至少90至100%的涂覆洗涤剂颗粒中,最大与最小的涂覆洗涤剂颗粒在x、y和z尺寸上的变化在20%以内。
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BR (1) | BR112013009130B1 (zh) |
CA (1) | CA2813789C (zh) |
CL (1) | CL2013001026A1 (zh) |
ES (1) | ES2613702T3 (zh) |
IN (1) | IN2013MN00616A (zh) |
MX (1) | MX2013003972A (zh) |
MY (1) | MY164216A (zh) |
PL (1) | PL2627757T3 (zh) |
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ZA (1) | ZA201302295B (zh) |
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CN110785481A (zh) * | 2017-06-20 | 2020-02-11 | 荷兰联合利华有限公司 | 包含香料的颗粒洗涤剂组合物 |
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AU2013242985B2 (en) * | 2012-04-03 | 2015-01-29 | Unilever Plc | Laundry detergent particles |
WO2013149753A1 (en) * | 2012-04-03 | 2013-10-10 | Unilever Plc | Laundry detergent particles |
MY167809A (en) * | 2012-04-03 | 2018-09-26 | Unilever Plc | Laundry Detergent Particle |
EP3190167B1 (en) | 2016-01-07 | 2018-06-06 | Unilever PLC | Bitter pill |
WO2018113643A1 (en) * | 2016-12-22 | 2018-06-28 | The Procter & Gamble Company | Laundry detergent composition |
EP3559194A4 (en) * | 2016-12-22 | 2020-05-20 | The Procter and Gamble Company | LAUNDRY DETERGENT COMPOSITION |
WO2018113644A1 (en) * | 2016-12-22 | 2018-06-28 | The Procter & Gamble Company | Laundry detergent composition |
WO2018113646A1 (en) * | 2016-12-22 | 2018-06-28 | The Procter & Gamble Company | Laundry detergent composition |
WO2020109227A1 (en) | 2018-11-28 | 2020-06-04 | Unilever N.V. | Large particles |
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- 2011-09-01 MX MX2013003972A patent/MX2013003972A/es not_active Application Discontinuation
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CN110785481A (zh) * | 2017-06-20 | 2020-02-11 | 荷兰联合利华有限公司 | 包含香料的颗粒洗涤剂组合物 |
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Also Published As
Publication number | Publication date |
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EP2627757A1 (en) | 2013-08-21 |
CA2813789C (en) | 2020-07-21 |
CL2013001026A1 (es) | 2013-12-20 |
CA2813789A1 (en) | 2012-04-19 |
BR112013009130A2 (pt) | 2016-07-19 |
EP2627757B1 (en) | 2016-11-02 |
PL2627757T3 (pl) | 2017-08-31 |
AU2011315790B2 (en) | 2014-03-06 |
AU2011315790A1 (en) | 2013-04-11 |
US20130281348A1 (en) | 2013-10-24 |
WO2012048947A1 (en) | 2012-04-19 |
AR083404A1 (es) | 2013-02-21 |
IN2013MN00616A (zh) | 2015-05-29 |
MX2013003972A (es) | 2013-05-14 |
US9290723B2 (en) | 2016-03-22 |
CN103201373B (zh) | 2016-06-08 |
ES2613702T3 (es) | 2017-05-25 |
ZA201302295B (en) | 2014-06-25 |
BR112013009130B1 (pt) | 2021-10-26 |
MY164216A (en) | 2017-11-30 |
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