CN103797104A - 储存稳定的酶颗粒 - Google Patents
储存稳定的酶颗粒 Download PDFInfo
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- CN103797104A CN103797104A CN201280044386.5A CN201280044386A CN103797104A CN 103797104 A CN103797104 A CN 103797104A CN 201280044386 A CN201280044386 A CN 201280044386A CN 103797104 A CN103797104 A CN 103797104A
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- enzyme
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- polyamine
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- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- OHOTVSOGTVKXEL-UHFFFAOYSA-K trisodium;2-[bis(carboxylatomethyl)amino]propanoate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C(C)N(CC([O-])=O)CC([O-])=O OHOTVSOGTVKXEL-UHFFFAOYSA-K 0.000 description 1
- WGIWBXUNRXCYRA-UHFFFAOYSA-H trizinc;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O WGIWBXUNRXCYRA-UHFFFAOYSA-H 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- 239000012588 trypsin Substances 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
- 229940030186 xpect Drugs 0.000 description 1
- 239000011746 zinc citrate Substances 0.000 description 1
- 235000006076 zinc citrate Nutrition 0.000 description 1
- 229940068475 zinc citrate Drugs 0.000 description 1
- RZLVQBNCHSJZPX-UHFFFAOYSA-L zinc sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Zn+2].[O-]S([O-])(=O)=O RZLVQBNCHSJZPX-UHFFFAOYSA-L 0.000 description 1
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Abstract
用于去污剂的酶颗粒的储存稳定性可以通过加入这样的聚胺来改善，所述聚胺的分子含至少10%w/w的氮，其中至少50%的氮原子作为胺存在。
Description
发明领域
本发明涉及酶颗粒。更具体地，本发明涉及这样的酶颗粒，它们在单独储存过程中或者作为颗粒去污剂的一部分储存的过程中的储存稳定性提高。
发明背景
呈颗粒形式的酶在颗粒(粉末)去污剂中普遍使用，且在酶颗粒单独储存和作为颗粒去污剂的成分储存的过程中，储存稳定性都是一个主要的关注因素。
用于去污剂的酶颗粒的储存稳定性的改善在现有技术中已经受到许多关注，且人们已经提出了多种添加剂来改善储存稳定性。
EP0674002A1,DE4422609A1,US2010/078381A1,WO94/16064A1,WO98/17768A1和US6872297A1公开了多种酶颗粒的配方。
发明内容
本发明人已经发现，通过掺入聚胺可以改善单独的酶颗粒或去污剂中的酶颗粒的储存稳定性。
相应地，本发明提供一种颗粒，其具有包含均匀(homogenous)混合物的核心，所述混合物包含可溶形式的酶以及聚胺。所述聚胺分子含有至少10%w/w的氮，且至少50%的N原子作为胺存在。本发明进一步提供制备所述颗粒的方法、以及包含所述酶颗粒的颗粒去污剂组合物。
发明详细说明
聚胺
所述聚胺通常具有三个或更多个伯胺或仲胺基团(NH2或NH)。聚胺分子含有至少10%w/w的氮；其可以含有至少15%w/w的氮，具体地是至少20%、至少25%或至少30%。聚胺分子中至少60%的N原子可以作为胺(伯胺、仲胺和叔胺)存在，具体地是至少70%、至少80%或至少90%。至少50%的N原子可以作为伯胺或仲胺存在，具体地是至少55%、至少60%、至少65%或至少70%。
有用的聚胺的一个例子是基于乙烯亚胺(ethylene imine)、尤其是聚乙烯亚胺的阳离子聚合物。有用的聚胺还包括：聚赖氨酸、聚烷基胺；聚烯丙基胺(polyallylamines)、聚乙烯胺(polyvinylamines)；聚(1-氨基丁二烯)[poly(l-aminobutadiene)]、胺封端的超支化聚脲[amine-terminatedhyperbranched polyurea]；聚(氨基乙基甲基丙烯酸酯)[poly(aminoethylmethacrylate)]；和氨基乙基化的丙烯酸类聚合物(aminoethylated acrylicpolymers)；胺封端的丁二烯丙烯腈共聚物[amine terminatedpoly(butadiene-co-acrylonitrile)]；多氨基取代的单糖、二糖、寡糖、多糖；包含一个或多个胺部分的树状分子；聚氨基酸、氨基官能化的聚二烷基硅氧烷(amino functionalized polydialkylsiloxane)、多氨基烷基(polyaminoalkyls)及它们的混合物。
聚胺的平均分子量(重均)可高于800Da，尤其是高于1200Da，高于1500Da或高于2000Da。平均分子量可低于2,000,000Da，尤其是低于1,000,000Da,低于100,000Da,低于20,000或低于10,000Da。所述聚胺可以以按所述混合物(未包被的核心)的重量计0.1-10%、或0.2-5%的量，尤其是0.5-2%的量存在。
聚乙烯亚胺
聚乙烯亚胺(PEI)是一种阳离子聚合物，可以是直链的或者是支链的。直链PEI由以-NH-CH2-CH2-作为重复单元的聚合链构成，基本上所有的N原子均作为仲胺存在。支链PEI可以通过乙烯亚胺(又称氮丙啶(azeridine))的聚合来制备。支链PEI中仲胺对伯胺的比例可高于0.7，尤其是高于0.9或高于1.1；所述比例可低于2，尤其是低于1.5、低于1.25或低于1。支链PEI中叔胺对伯胺的比例可高于0.4,尤其是高于0.5,高于0.6,或高于0.7；所述比例可低于1,尤其是低于0.8或低于0.6。
任选的多价阳离子的盐
为了改善储存稳定性，颗粒核心中的所述混合物可还包含多价阳离子的盐，尤其是二价阳离子的盐。在25℃，所述盐在水中的溶解度高于0.01g/100ml，尤其是高于0.1g/100ml，高于1g/100ml，或高于1.0g/100ml。
所述阳离子可以是Zn++,Mg++,Cu++或Mn++。所述可溶盐的阴离子可以是有机的或无机的，例如硫酸根、乙酸根、硝酸根、磷酸根、柠檬酸根、甲酸根、氯(chloride)、或亚硫酸根。所述盐可以是无水的，或者是水合物的形式。具体的例子是MgSO4·7H2O,ZnSO4·7H2O,以及乙酸锌、乙酸镁(Mg-acetate)、,MgCl2,ZnCl2,Mg(NO3)2,Zn(NO3)2,ZnSO3,柠檬酸镁(Mg-citrate)、柠檬酸锌(Zn-citrate)。
所述混合物可以以按重量计0.01-90%、更具体地是0.05-50%、更优选的是0.1-20%、或0.1-10%的量(以无水形式计算)包含盐或盐的组合。所述混合物典型地以0.005-5%、更优选0.01-2%的量包含所述阳离子(例如Zn和/或Mg)。
酶
所述酶可以是水解酶(酶命名法EC3)、脂肪酶、角质酶、蛋白酶、淀粉酶、纤维素酶、甘露聚糖酶、裂合酶或果胶酸裂合酶。
脂肪酶和角质酶
合适的脂肪酶和角质酶包括细菌或真菌来源的那些。包括化学修饰的或蛋白质工程化的变体。例子包括来自嗜热丝孢菌属(Thermomyces)，例如如EP258068和EP305216中描述的来自疏棉状嗜热丝孢菌(T.lanuginosus)(原先名为疏棉状腐质霉(Humicola lanuginosa)的脂肪酶，来自腐质霉属(Humicola)的角质酶，例如WO96/13580中描述的来自特异腐质霉(H.insolens)的角质酶；假单胞菌属(Pseudomonas)脂肪酶，例如来自产碱假单胞菌(P.alcaligenes)或假产碱假单胞菌(P.pseudoalcaligenes)(EP218272)、洋葱假单胞菌(P.cepacia)(EP331376)、斯氏假单胞菌(P.stutzeri)(GB1,372,034)、荧光假单胞菌(P.fluorescens)、假单胞菌菌株SD705(WO95/06720和WO96/27002)、威斯康星假单胞菌(P.wisconsinensis)(WO96/12012)、芽孢杆菌属(Bacillus)脂肪酶，例如来自枯草芽孢杆菌(B.subtilis)(Dartois et al.,1993,Biochemica et Biophysica Acta,1131:253-360)、嗜热脂肪芽孢杆菌(B.stearothermophilus)(JP64/744992)或细小芽孢杆菌(B.pumilus)(WO91/16422)。
其他例子是如WO92/05249,WO94/01541,EP407225,EP260105,WO95/35381,WO96/00292,WO95/30744,WO94/25578,WO95/14783,WO95/22615,WO97/04079,WO97/07202,WO00/060063,WO2007/087508和WO2009/109500中描述的脂肪酶变体。
优选的可商购脂肪酶包括LipolaseTM,Lipolase UltraTM,and LipexTM；LecitaseTM,LipolexTM;LipocleanTM,LipoprimeTM(Novozymes A/S)。其他可商购的脂肪酶包括Lumafast(Genencor Int Inc)；Lipomax(Gist-Brocades/Genencor Int Inc)和来自Solvay的芽孢杆菌属脂肪酶。
蛋白酶
合适的蛋白酶包括动物、植物或微生物来源的那些。优选微生物来源。蛋白酶可以是丝氨酸蛋白酶或金属蛋白酶，优选碱性微生物蛋白酶或胰蛋白酶样蛋白酶。碱性蛋白酶的例子有枯草杆菌蛋白酶，尤其是源自芽孢杆菌属的那些，例如枯草杆菌蛋白酶Novo、枯草杆菌蛋白酶Carlsberg、枯草杆菌蛋白酶309、枯草杆菌蛋白酶147和枯草杆菌蛋白酶168(描述于WO89/06279)。胰蛋白酶样蛋白酶的实例为胰蛋白酶(例如，猪或牛来源的)，和描述于WO89/06270和WO94/25583的镰孢属(Fusarium)蛋白酶。
可用的蛋白酶的实例为描述于WO92/19729、WO98/20115、WO98/20116和WO98/34946的变体，特别是在下述位置中一个或多个具有取代的变体：27、36、57、76、87、97、101、104、120、123、167、170、194、206、218、222、224、235和274。
优选的商业上可获得的蛋白酶包括AlcalaseTM，SavinaseTM，PrimaseTM，DuralaseTM，EsperaseTM，和KannaseTM(Novozymes A/S)，MaxataseTM，MaxacalTM，MaxapemTM，ProperaseTM，PurafectTM，Purafect oxpTM，Fn2TM，和Fn3TM(Genencor International Inc.)。
淀粉酶：
合适的淀粉酶(α和/或β)包括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。淀粉酶包括，例如从芽孢杆菌属获得的α-淀粉酶，例如，从一种详述于GB1,296,839中的特殊地衣芽孢杆菌菌株获得的α-淀粉酶。
可用的淀粉酶的实例为描述于WO94/02597、WO94/18314、WO96/23873和WO97/43424的变体，特别是在下述位置中一个或多个具有取代的变体：15、23、105、106、124、128、133、154、156、181、188、190、197、202、208、209、243、264、304、305、391、408和444。
商业上可获得的淀粉酶为Stainzyme；Stainzyme Plus，DuramylTM，TermamylTM，Termamyl Ultra；Natalase，FungamylTM和BanTM(Novozymes A/S)，RapidaseTM和PurastarTM(来自Genencor International Inc.)。
裂合酶
裂合酶可以是源自芽孢杆菌属，尤其是地衣芽孢杆菌或B.agaradhaerens的果胶酸裂合酶，或者衍生自其中任一者的变体，例如如US6,124,127,WO1999/027083,WO1999/027084,WO2002/006442,WO2002/092741,WO2003/095638中所述的，一种可商购的果胶酸裂合酶是XPect;Pectawash和Pectaway(Novozymes A/S)。
甘露聚糖酶
所述甘露聚糖酶可以是家族5或26的碱性甘露聚糖酶。其可以是来自芽孢杆菌属或腐质霉属，尤其是B.agaradhaerens,地衣芽孢杆菌,耐碱芽孢杆菌(B.halodurans),克劳氏芽孢杆菌(B.clausii),或特异腐质霉。合适的甘露聚糖描述于WO1999/064619中。一种可商购的甘露聚糖酶是Mannaway(Novozymes A/S)。
纤维素酶
合适的纤维素酶包括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。它可以是来自特异腐质霉(US4,435,307)或来自木霉属(Trichoderma)，例如里氏木霉(T.reesei)或绿色木霉(T.viride)的真菌纤维素酶。纤维素酶的例子描述于EP0495257。可商购的纤维素酶包括CarezymeTM、CelluzymeTM、CellucleanTM、CelluclastTM、和EndolaseTM；Renozyme；Whitezyme(Novozymes A/S)Puradax,Puradax HA,和Puradax EG(可获自Genencor)。
酶核心
所述包含酶和聚胺的均匀混合物(酶核心)以当在水中或洗涤液中稀释时会溶解的形式含有所述酶。溶解度可以通过例如本说明书后文中描述的溶解测试来加以测定。
所述酶基本上没有对所述聚胺的共价连接(covalent links)。因此，颗粒中存在的该酶的分子量与单独的该酶多肽的分子量没有实质差异，例如，颗粒中存在的酶的平均分子量是该酶多肽的+/-500Da以内。优选的是该组合物中没有添加胺交联剂，例如本领域中已知的戊二醛或亚氨酸酯，以避免酶通过共价反应(例如与添加的聚胺)被固定化，以及多胺与配方中的不溶粒子共价反应。
制备颗粒的方法可见于Handbook of Powder Technology;Particle sizeenlargement，C.E.Capes著；Volume1;1980;Elsevier。制备方法包括已知的饲料和颗粒制剂技术，即：
a)喷雾干燥产物，其中在喷雾干燥塔中雾化液体含酶溶液以形成小液滴，在它们在沿干燥塔下降的过程中干燥形成含有酶的颗粒状物质。该方法可产生非常小的颗粒(Michael S.Showell(编);Powdered detergents;SurfactantScience Series;1998;第71卷，140-142页;Marcel Dekker)。
b)成层的(layered)产物，其中酶作为层包被在预成型的惰性核心颗粒周围，其中将含有酶的溶液雾化，通常流化床设备中(其中预形成的核心粒子被流化)雾化，含有酶的溶液粘附于核心粒子并干燥，在核心颗粒的表面上留下干燥酶的层。如果能找到具有期望尺寸的有用的核心粒子，则该方法可获得具有期望尺寸的颗粒。这种类型的产品描述于例如WO97/23606中。
c)吸收的(absorbed)粒子，其中不是将酶包被为核心周围的层，而是使酶被吸收到核心的表面上和/或表面中。这样的方法描述于WO97/39116中。
d)挤出或丸粒化(pelletized)的产品，其中将含有酶的糊料压成丸粒(pellets)或在压力下通过小的开口挤出并切割为粒子，随后干燥该粒子。这样的粒子通常具有相当大的尺寸，因为开有挤出开口的材料(通常是具有钻孔的板)限制了挤出口上的容许压降。此外，当使用小的开口时，非常高的挤出压力可增加酶糊料的产热，这对酶是有害的(Michael S.Showell(编);Powdereddetergents;Surfactant Science Series;1998;第71卷，140-142页;MarcelDekker)。
e)喷射造粒产物，其中将酶粉末悬浮于熔化的蜡中，并将悬浮液喷射(例如通过转盘喷雾器)到冷却室中，在此冷却室中液滴快速地固化(Michael S.Showell(编辑);Powdered detergents;Surfactant Science Series;1998;第71卷，140-142页;Marcel Dekker)。所获产物中酶均匀分布于惰性材料中而不是集中在其表面上。US4,016,040和US4,713,245也是涉及此技术的文献。
f)混合器造粒产物，其中将含酶液体添加于常规造粒组分的干燥粉末组合物。将液体和粉末以合适的比例混合，并且随着液体的水分为干燥粉末所吸收，干燥粉末的组分开始粘着并团聚，粒子变大，形成包含酶的微粒(granulates)。这样的方法描述于US4,106,991和有关的文献EP170360、EP304332、EP304331、WO90/09440和WO90/09428中。在该方法的一种具体产品中，其中可以用各种高剪切混合器作为造粒机，将由作为活性化合物的酶、填充剂和粘合剂等组成的微粒与纤维素纤维混合以强化粒子，而得到所谓的T-微粒(T-granulate)。经强化的粒子更加坚固，酶粉尘释放更少。
g)粉碎(size reduction)，其中通过磨碎或压碎含有酶的较大的粒子、丸粒、片体(tablet)、坯块(briquettes)等而产生核心。通过将磨碎或压碎的产物过筛来获得所需要的核心粒子级分。尺寸过大和尺寸过小的粒子可循环利用。粉碎描述于(Martin Rhodes(编辑);Principles of Powder Technology;1990;Chapter10;John Wiley&Sons)中。
h)流化床造粒。流化床造粒包括将细粒(particulate)悬浮于空气流中并经喷嘴喷射液体到流化的粒子上。被喷射的液滴击中的粒子湿润并发粘。粘性的粒子与其它粒子碰撞并粘附于其上而形成颗粒。
i)可对核心进行干燥，如在流化床干燥器中干燥。本领域技术人员可以使用饲料或酶工业中其它已知的用于干燥颗粒的方法。所述干燥优选在25-90℃的产品温度进行。对于某些酶，包含酶的核心在用盐包被之前含水量低是重要的。如果在除去过量水之前就用盐包被水敏感性酶，则水分会被截留在核心中并可能给酶的活性造成不利的影响。在干燥之后，所述核心优选含有0.1-10%w/w的水。
任选的包衣
盐包衣
所述颗粒包含核心，该核心可以是无包衣的，或者可以被至少一个包衣所包围。包衣可包含按重量计至少60%w/w的盐，例如按重量计至少65%,至少70%,至少75%,至少80%,至少85%,至少90%,至少95%或至少99%w/w的盐。
包衣可以以核心重量的至少5%，例如至少10%或15%的量施加。所述量可为至多70%、50%、40%或30%。
为了提供可接受的保护，盐包衣优选为至少1μm厚，尤其是至少2μmm、至少4μmm、或至少8μmm厚。包衣越厚，产生颗粒就越耗时、越昂贵。在一个具体的实施方案中，盐包衣的厚度低于100μm。在一个更具体的实施方案中，盐包衣的厚度低于60μm。在一个甚至更具体的实施方案中，盐包衣的总厚度低于40μm。
包衣应通过形成基本上连续的层来包被核心单元。基本上连续的层应理解为极少有孔或无孔的包衣，从而使得它所包裹/封装的核心单元极少有或没有未包被区域。层或包衣特别应在厚度上是均匀的。盐可以从完全溶解有该盐的盐溶液、或从其中细粒子小于50μm、例如小于10μm或小于5μm的盐悬液加入。优选的是所述盐作为包衣层中的连续相存在。
盐包衣可以进一步含有如本领域已知的其他材料，例如填充剂、防粘剂、色素、染料、增塑剂和/或粘合剂，例如二氧化钛、高岭土、碳酸钙或滑石。
优选的是包衣层的连续部分(相对于离散的填充粒子(filler particles))占包衣的至少50%w/w，更优选多于60%,75%,90%或95%。
盐
盐包衣可以包含单一盐或两种或多种盐的混合物。盐可以是水溶性的，特别具有在20℃在100g水中至少5克，优选每100g水至少10g的溶解度。
盐可以是无机盐。这些盐中的阳离子的离子是铵、钠、钾和镁。阴离子的例子包括氯(chloride)、硫酸根、磷酸根、柠檬酸根。具体实例包括NaH2PO4、Na2HPO4、Na3PO4、(NH4)H2PO4、K2HPO4、KH2PO4、Na2SO4、K2SO4、KHSO4、MgSO4、Mg(NO3)2、(NH4)2SO4和柠檬酸钠。
盐可以是无水形式，或它可以是水合盐，即具有结合的结晶水的结晶盐水合物。具体例子包括无水硫酸钠(Na2SO4)、无水硫酸镁(MgSO4)、七水硫酸镁(MgSO4(7H2O))、七水磷酸氢二钠(Na2HPO4(7H2O))、六水硝酸镁(Mg(NO3)2(6H2O))、二水柠檬酸钠和四水乙酸镁。
优选地，将所述盐作为该盐的溶液涂施，例如使用流化床。
任选的额外包衣
所述颗粒可以包括一个或多个额外的包衣，例如用来进一步改进储存稳定性或降低粉尘形成(dust formation)。合适的包衣材料的例子有聚乙二醇(PEG)、甲基羟丙基纤维素(MHPC)、和聚乙烯醇(PVA)。
测试方法
溶解测试
下述溶解测试可以用来确定颗粒的核心中的酶是否为可溶形式。该测试用来区分可溶形式的酶和固定化的酶。
将水或去污剂溶液(经30min搅拌并通过一层丝网过滤)调整到20℃±2℃并放置在一台调节到600rpm±10rpm的4叶螺旋桨式搅拌器(4-bladedpropeller stirrer)之下。在T0加入75mg含酶粒子(75mg enzyme containingparticle)/l去污剂溶液。添加含酶粒子之后，在最先的60秒内每15秒从去污剂溶液中抽取样品并过滤来测量释放到去污剂溶液中的酶的浓度。然后每30秒取出样品直到120秒，再每60秒取出样品直到1100秒。分别计算从含酶颗粒释放50%和90%的酶的时间。如果90%释放的时间小于10分钟，尤其是小于5分钟或小于3分钟，或者如果50%释放的时间小于5分钟，尤其是小于2.5分钟或1.5分钟，则认为核心中的酶是可溶形式。
抽出的样品中的酶活性可以通过合适的分析方法来测量，例如对于脂肪酶，使用包含合成底物，如对硝基苯基丁酸酯或对硝基苯基棕榈酸酯的测定法。或者，作为测定酶活性的替代，可以通过测定去污剂溶液或水中酶蛋白的量来求出酶释放。
去污剂组合物
所述颗粒特别适合掺入包含表面活性剂的颗粒去污剂中。依照本发明的酶颗粒当掺入到去污剂中，即使是包含有攻击性(aggressive)的组分如漂白体系的去污剂中时，导致该酶的储存稳定性改善。
所述去污剂组合物可以例如配制为用于手洗或机洗的洗衣去污剂组合物，该组合物包含适于预处理沾污织物的清洁添加剂组合物，或织物软化组合物，或用于一般家用硬表面清洁操作的去污剂组合物，或用于手动或机器餐具洗涤操作的组合物。
本发明的去污剂组合可以是任何方便的干燥形式，例如条、片、粉末、微粒或糊料。其也可以是液体去污剂，或者是水性液体去污剂或非水性去污剂。
表面活性剂
所述去污剂组合物包含一种或多种表面活性剂，表面活性剂可以是非离子型(包括半极性)和/或阴离子型和/或阳离子型和/或两性离子型。表面活性剂典型地以按重量计0.1至60%的水平存在。
当包含在其中时，去污剂通常将含有约1%至约40%的阴离子型表面活性剂，例如直链烷基苯磺酸盐(linear alkylbenzenesulfonate)、α-烯烃磺酸盐(alpha-olefinsulfonate)、烷基硫酸盐(alkyl sulfate)(脂肪醇硫酸盐(fattyalcoholsulfate))、醇乙氧基硫酸盐(alcohol ethoxysulfate)、仲烷基磺酸盐(secondaryalkanesulfonate)、α-磺基脂肪酸甲酯(alpha-sulfo fatty acid methyl ester)、烷基或烯基琥珀酸(alkyl-or alkenylsuccinic acid)或肥皂(soap)。
当包含在其中时，去污剂通常会含有约0.2%-约40%的非离子表面活性剂，如醇乙氧基化物(alcohol ethoxylate)、壬基酚乙氧基化物(nonylphenolethoxylate)、烷基多糖苷(alkylpolyglycoside)、烷基二甲胺氧化物(alkyldimethylamineoxide)、乙氧基化脂肪酸单乙醇酸胺(ethoxylated fatty acidmonoethanolamide)、脂肪酸单乙醇酸胺(fatty acid monoethanolamide)、多羟基烷基脂肪酸酰胺(polyhydroxy alkyl fatty acid amide)、或葡糖胺的N-酰基N-烷基衍生物(N-acyl N-alkyl derivatives of glucosamine)(“葡糖酸胺”(glucamides))。
所述去污剂组合物可包含一种或多种表面活性剂，表面活性剂可以是阴离子型和/或阳离子型和/或非离子型和/或半极性型和/或两性离子型，或者是它们的混合物。在一个具体的实施方案中，所述去污剂组合物包含一种或多种非离子型表面活性剂和与一种或多种阴离子表面活性剂的混合物。表面活性剂典型地以按重量计大约0.1%至60%、例如约1%至约40%、或约3%至约20%、或约3%至约10%的水平存在。
当包含在其中时，所述去污剂通常将会含有按重量计约1%至约40%，例如约5%至约30%，包括约5%至约15%，或约20%至约25%的阴离子型表面活性剂。阴离子型表面活性剂的非限制性实例包括硫酸盐(sulfates)和磺酸盐(sulfonates)，尤其是直链烷基苯磺酸盐(LAS)、支链烷基苯磺酸盐(BABS)、苯基链烷磺酸盐、α-烯烃磺酸盐(AOS)、烯烃磺酸盐、链烯烃磺酸盐、链烷-2，3-二基双(硫酸盐)、羟基链烷磺酸盐和二磺酸盐、烷基硫酸盐(AS)例如十二烷基硫酸钠(SDS)、脂肪醇硫酸盐(FAS)、伯醇硫酸盐(PAS)、醇醚硫酸盐(AES或AEOS或FES，也称为醇乙氧基硫酸盐或脂肪醇醚硫酸盐)、仲链烷磺酸盐(SAS)、石蜡磺酸盐(PS)、磺酸酯、磺化脂肪酸甘油酯、α-磺基脂肪酸甲酯(α-SFMe或SES)包括甲酯磺酸盐(MES)、烷基或烯基琥珀酸、十二烯/十四烯琥珀酸(DTSA)、氨基酸的脂肪酸衍生物、磺基-琥珀酸的二酯和单酯或肥皂、及其组合。
阳离子型表面活性剂的非限制性例子包括烷基二甲基乙醇胺季铵化合物(ADMEAQ)、十六烷基三甲基溴化铵(CTAB)、二甲基双十八烷基氯化铵(DSDMAC)和烷基苯甲基二甲铵、及其组合。
当包括在其中时，去污剂通常会含有按重量计约0.2%-约40%，例如约0.5%-约30%，特别是约1%-约20%、约3%-约10%，例如约3%-约5%、或约8%-约12%的非离子型表面活性剂。非离子型表面活性剂的非限制性例子包括醇乙氧基化物(AE或ΑΕO)、醇丙氧基化物、丙氧基化脂肪醇(PFA)、烷氧基化脂肪酸烷基酯,例如乙氧基化和/或丙氧基化脂肪酸烷基酯、烷基酚乙氧基化物(ΑΡΕ)、壬基酚乙氧基化物(NPE)、烷基多糖苷(APG)、烷氧基化胺、脂肪酸单乙醇酰胺(FAM)、脂肪酸二乙醇酰胺(FADA)、乙氧基化脂肪酸单乙醇酰胺(EFAM)、丙氧基化脂肪酸单乙醇酰胺(PFAM)、多羟基烷基脂肪酰胺、或葡糖胺的N-酰基N-烷基衍生物(葡糖酰胺，GA，或脂肪酸葡糖酰胺，FAGA)，以及可以通过商品名SPAN和TWEEN获得的产品，及其组合。
半极性型表面活性剂的非限制性例子包括氧化胺(AO)例如烷基二甲基氧化胺、N-(椰油烷基)-N,N-二甲基氧化胺和N-(牛脂-烷基)-N,N-双(2-羟乙基)氧化胺、脂肪酸链烷醇酰胺和乙氧基化脂肪酸链烷醇酰胺、及其组合。
两性离子型表面活性剂的非限制性例子包括甜菜碱、烷基二甲基甜菜碱、和磺基甜菜碱、及其组合。
增洁剂或络合剂
去污剂可以含有0-65%的去污剂增洁剂(detergent builder)或络合剂，例如沸石、二磷酸盐、三磷酸盐、膦酸盐、碳酸盐、柠檬酸盐、次氮基三乙酸、乙二胺四乙酸、二乙烯三胺五乙酸、烷基或烯基琥珀酸、可溶性硅酸盐或层状硅酸盐(例如来自Hoechst的SKS-6)。
在餐具洗涤去污剂中，增洁剂的水平一般为40-65%，特别是50-65%。增洁剂和/或共增洁剂(co-builder)可以特别是与Ca和Mg形成水溶性络合物的螯合剂。增洁剂的非限制性例子包括沸石、二磷酸盐(焦磷酸盐)、三磷酸盐例如三磷酸钠(STP或STPP)、碳酸盐例如碳酸钠、可溶性硅酸盐例如偏硅酸钠、层状硅酸盐(例如来自Hoechst的SKS-6)、乙醇胺例如2-氨基乙-1-醇(MEA)、亚氨基二乙醇(DEA)和2,2’,2”,-次氮基三乙醇(TEA)、和羧甲基菊粉(CMI)、及其组合。
去污剂组合物可以包括单独的共增洁剂、或与如沸石增洁剂等增洁剂组合的共增洁剂。共增洁剂的非限制性例子包括聚丙烯酸盐的同聚物或其共聚物，例如聚(丙烯酸)(PAA)或共聚(丙烯酸/马来酸)(PAA/PMA)。进一步的非限制性例子包括柠檬酸盐、螯合剂例如氨基羧酸盐、氨基多羧酸盐和膦酸盐、和烷基或烯基琥珀酸。另外的特定例子包括2,2’,2”-次氮基三乙酸(NTA)、乙二胺四乙酸(EDTA)、二乙烯三胺五乙酸(DTPA)、亚氨基二琥珀酸(IDS)、乙二胺-N,N’-二琥珀酸(EDDS)、甲基甘氨酸二乙酸(MGDA)、谷氨酸-N,N-二乙酸(GLDA)、1-羟基乙烷-1,1-二基双(膦酸)(HEDP)、乙二胺四(甲叉)四(膦酸)(EDTMPA)、二乙烯三胺五(甲叉)五(膦酸)(DTPMPA)、N-(2-羟乙基)亚氨基二乙酸(EDG)、天冬氨酸-N-单乙酸(ASMA)、天冬氨酸-N,N-二乙酸(ASDA)、天冬氨酸-N-单丙酸(ASMP)、亚氨基二琥珀酸(IDA)、N-(2-磺甲基)天冬氨酸(SMAS)、N-(2-磺乙基)天冬氨酸(SEAS)、N-(2-磺甲基)谷氨酸(SMGL)、N-(2-磺乙基)谷氨酸(SEGL)、N-甲基亚氨基二乙酸(MIDA)、α-丙氨酸-N,N-二乙酸(α-ALDA)、丝氨酸-N,N-二乙酸(SEDA)、异丝氨酸-N,N-二乙酸(ISDA)、苯丙氨酸-N,N-二乙酸(PHDA)、邻氨基苯甲酸-N,N-二乙酸(ANDA)、磺胺酸-N,N-二乙酸(SLDA)、牛磺酸-N,N-二乙酸(TUDA)和磺甲基-N,N-二乙酸(SMDA)、N-(羟乙基)-乙二胺三乙酸盐(N-(hydroxyetheyl)-ethylidenediaminetriacetate)(HEDTA)、二乙醇甘氨酸(DEG)、二亚乙基三胺五(甲叉膦酸)(DTPMP)、氨基三(甲叉膦酸)(ATMP)、及其组合和盐。进一步的示例性增洁剂和/或共增洁剂在例如WO09/102854、US5977053中描述。
聚合物
去污剂可以包含一种或多种聚合物。例子有羧甲基纤维素、聚(乙烯吡咯烷酮)、聚(乙二醇)、聚(乙烯醇)、聚(乙烯吡啶-N-氧化物)、聚(乙烯咪唑)、聚羧酸盐/酯例如聚丙烯酸盐/酯、马来酸/丙烯酸共聚物和月桂基甲基丙烯酸/丙烯酸共聚物。
漂白体系
所述去污剂可以含有漂白体系，其可以包含H2O2来源例如过硼酸盐或过碳酸盐，其可以与过酸形成性漂白活化剂(例如四乙酰乙二胺或壬酰氧苯磺酸盐)组合。可替代地，漂白体系可以包含过酸，例如酰胺、亚胺或砜类型的过酸。
合适的漂白体系组分包括漂白催化剂、光漂白剂、漂白活化剂、过氧化氢来源例如过碳酸钠和过硼酸钠、预形成的过酸及其混合物。合适的预形成的过酸包括但不限于过氧羧酸和盐、过碳酸和盐、过亚胺酸和盐、过一硫酸和盐例如臭氧(R)、及其混合物。漂白体系的非限制性例子包括与过酸形成漂白活化剂组合的基于过氧化物的漂白体系，其可以包含例如无机盐，包括碱金属盐例如过硼酸盐的钠盐(通常为单或四水合物)、过碳酸盐、过硫酸盐、过磷酸盐、过硅酸盐。合适的光漂白剂可以例如是磺化锌酞菁。合适的漂白活化剂包括4-(十二烷酰氧基)苯磺酸盐(LOBS)、4-(癸酰氧基)苯磺酸盐、4-(癸酰氧基)苯甲酸盐(DOBS)、4-(3,5,5-三甲基己酰氧基)苯磺酸盐(ISONOBS)、四乙酰基乙二胺(TAED)和4-(壬酰氧基)苯磺酸盐(NOBS)和/或公开于WO98/17767中的那些。可替代地，漂白体系可以包含例如酰胺、亚胺或砜类型的过酸。漂白体系还可以包含过酸例如6-(邻苯二甲酰氨基)过己酸(PAP)。漂白体系还可以包括漂白催化剂。在一些实施方案中，漂白组分可以是选自具有下式的有机催化剂的有机催化剂：
(iii)及其混合物；其中每个R1独立地是含有9–24个碳的支链烷基或含有11–24个碳的直链烷基，优选地，每个R1独立地是含有9–18个碳的支链烷基或含有11–18个碳的直链烷基，更优选地，每个R1独立地选自2-丙基庚基、2-丁基辛基、2-戊基壬基、2-己基癸基、正十二烷基、正十四烷基、正十六烷基、正十八烷基、异壬基、异癸基、异十三烷基和异十五烷基。其他示例性漂白体系例如在WO2007/087258、WO2007/087244、WO2007/087259、WO2007/087242中描述。
助水溶物(hydrotrope)
助水溶物是溶解水溶液中的疏水化合物(或相反地，非极性环境中的极性物质)的化合物。一般地，助水溶物具有亲水和疏水两种特征(如由表面活性剂已知的所谓的两亲性质)；然而，助水溶物的分子结构一般不利于自发性自聚集，参见例如通过Hodgdon和Kaler(2007)，Current Opinion in Colloid &Interface Science 12：121-128的综述。助水溶物不显示如表面活性剂和脂质形成性微团、薄层或其他熟知的中间相中可见的临界浓度(超过该浓度即发生自聚集)。相反，许多助水溶物显示连续类型的聚集过程，其中聚集物的大小随着浓度增加而增长。然而，许多助水溶物可改变含有具备极性和非极性特征的物质的体系的相行为、稳定性和胶体性质，包括水、油、表面活性剂和聚合物的混合物。助水溶物常规地在从药学(pharma)、个人护理、食品到技术应用的各个产业中使用。助水溶物在去污剂组合物中的使用允许例如更浓的表面活性剂配方(如在通过去除水来压缩液体去污剂的工艺中)，而不诱发不希望有的现象，例如相分离或高粘度。
去污剂可以含有按重量计0-5%、例如约0.5-约5%或约3%-约5%的助水溶物。助水溶物的非限制性例子包括苯磺酸钠、对甲苯磺酸钠(STS)、二甲苯磺酸钠(SXS)、异丙苯磺酸钠(SCS)、伞花烃磺酸钠、氧化胺、醇和聚乙二醇醚、羟基萘甲酸钠、羟基萘磺酸钠、乙基己基硫酸钠及其组合。
织物固色剂(Fabric hueing agents)
本发明的去污剂组合物还可以包括织物固色剂例如染料或色素，当配制在去污剂组合物中时，当所述织物与包含所述去污剂组合物的洗液接触时，所述织物固色剂可以沉积到织物上，从而通过可见光的吸收/反射改变所述织物的色调。荧光增白剂发出至少某些可见光。相比之下，当织物固色剂吸收至少部分可见光谱时，它们改变表面的色调。合适的织物固色剂包括染料和染料-粘土缀合物，并且还可以包括色素。合适的染料包括小分子染料和聚合染料。合适的小分子染料包括选自下述的小分子染料：属于Direct Blue、DirectRed、Direct Violet、Acid Blue、Acid Red、Acid Violet、Basic Blue、Basic Violet和Basic Red的颜色指数(C.I.)分类的染料，或其混合物，例如如WO2005/03274、WO2005/03275、WO2005/03276和EP1876226(在此引入作为参考)中所述的。去污剂组合物优选包含约0.00003重量%-约0.2重量%、约0.00008重量%-约0.05重量%、或甚至约0.0001重量%-约0.04重量%织物固色剂。该组合物可以包含0.0001重量%-0.2重量%织物固色剂，当该组合物是单位剂量小袋的形式时，这可以是尤其优选的。合适的固色剂还公开于例如WO2007/087257、WO2007/087243中。
去污剂配方
酶颗粒可以包括在如WO09/092699、EP1705241、EP1382668、WO07/001262、US6472364、WO04/074419或WO09/102854中所述配方的颗粒状去污剂中。其他有用的去污剂配方在下述中描述：WO09/124162,WO09/124163,WO09/117340,WO09/117341,WO09/117342,WO09/072069,WO09/063355,WO09/132870,WO09/121757,WO09/112296,WO09/112298,WO09/103822,WO09/087033,WO09/050026,WO09/047125,WO09/047126,WO09/047127,WO09/047128,WO09/021784,WO09/010375,WO09/000605,WO09/122125,WO09/095645,WO09/040544,WO09/040545,WO09/024780,WO09/004295,WO09/004294,WO09/121725,WO09/115391,WO09/115392,WO09/074398,WO09/074403,WO09/068501,WO09/065770,WO09/021813,WO09/030632,WO09/015951,WO2011025615,WO2011016958,WO2011005803,WO2011005623,WO2011005730,WO2011005844,WO2011005904,WO2011005630,WO2011005830,WO2011005912,WO2011005905,WO2011005910,WO2011005813,WO2010135238,WO2010120863,WO2010108002,WO2010111365,WO2010108000,WO2010107635,WO2010090915,WO2010033976,WO2010033746,WO2010033747,WO2010033897,WO2010033979,WO2010030540,WO2010030541,WO2010030539,WO2010024467,WO2010024469,WO2010024470,WO2010025161,WO2010014395,WO2010044905,WO2010145887,WO2010142503,WO2010122051,WO2010102861,WO2010099997,WO2010084039,WO2010076292,WO2010069742,WO2010069718,WO2010069957,WO2010057784,WO2010054986,WO2010018043,WO2010003783,WO2010003792,WO2011023716,WO2010142539,WO2010118959,WO2010115813,WO2010105942,WO2010105961,WO2010105962,WO2010094356,WO2010084203,WO2010078979,WO2010072456,WO2010069905,WO2010076165,WO2010072603,WO2010066486,WO2010066631,WO2010066632,WO2010063689,WO2010060821,WO2010049187,WO2010031607,或WO2010000636。
实施例
实施例1：
一种典型的配方是例如WO03/000456的实施例1中产生的高剪切T微粒(high-shear T-granulate)(含有酶、硫酸钠(Na-sulfate)、纤维素纤维和粘合剂例如蔗糖或糊精)，其中在核心中有如下配方(按未包衣的干微粒的重量%)：
·按重量计4%的七水硫酸锌
按重量计1%的50%聚胺溶液(例如聚乙烯亚胺)这些稳定剂优选在制粒前加入含水酶浓缩物中。
在制粒和干燥之后在相对湿润的条件下(在流出空气中RH按重量计约50%)在流化床中施加按重量计40%(按未包被的干微粒的重量%)的硫酸钠包衣(例如如WO03/000456的实施例4所产生的)。在包被过程中所施加的硫酸钠溶液保持高于32℃。在涂料混合器中进一步施加一层装饰性的、减少粉尘的外层薄膜(2.5%PEG4000:TiO21:1w/w)。
实施例2：
制备具有下述组成的脂肪酶微粒。给出的各个量是相对粗(未包被的)微粒而言的。通过高剪切制粒制备微粒，通过流化床包被然后在涂料混合器中进行聚合物包被来加以包被。所述聚胺是支链型改性聚乙烯亚胺(PEI,LupasolPO100,BASF的产品)。其平均分子量为5000，并以1%w/w的量添加PEI含量为50%的产品。
实施例3：
通过如下表所示混合酶和稳定剂并在混合器中造粒，制备了多种酶微粒。如标示地施加了盐包衣和薄膜包衣。然后将每种微粒加入颗粒漂白去污剂或颗粒非漂白去污剂，并在37℃、70%相对湿度，或35℃、55%相对湿度下储存。各个量是相对于核心重量的重量%给出的。盐包衣以按核心的重量计40%的量施加。所述聚胺是与实施例2中相同的聚乙烯亚胺(作为50%溶液的量给出)。
结果表明了添加聚胺、多价阳离子和施加盐包衣的效果。因此，微粒A和B的结果的比较显示了添加多价阳离子的效果；微粒B和C的结果的比较显示了添加多胺的效果；微粒C和D(或E和F)的结果的比较显示了施加盐包衣的效果；微粒C和E的结果的比较显示了替代阳离子的一般性的稳定化效果。
实施例4：
通过如下表所示混合酶和稳定剂并在混合器中造粒，制备了两种酶微粒。然后将每种微粒加入颗粒漂白去污剂或颗粒非漂白去污剂，并在37℃、70%相对湿度，或35℃、55%相对湿度下储存。各个量是相对于核心重量的重量%给出的。所述聚胺是与实施例2中相同的聚乙烯亚胺。
结果证明了添加聚胺的稳定化效果。因此，微粒G和H的结果的比较显示了添加聚胺的效果。实施例3和实施例4中的结果证明添加聚胺的稳定化效果是一般性的效果，因为它可稳定化不同的酶。
实施例5：
制备了具有下述组成的纤维素酶微粒。给出的各个量是相对粗(未包被的)微粒而言的。通过高剪切制粒制备颗粒，通过流化床包被然后在涂料混合器中进行聚合物包被来加以包被。
使用的聚胺为Lupasol(聚乙烯亚胺含量为50%w/w，以1%w/w的量添加)。它是一种支链同聚聚乙烯亚胺，Mw≈5000。伯:仲:叔胺的比例大约为1:1.05:0.76。
实施例6
通过如下表所示混合酶和稳定剂并在混合器中造粒，制备了多种酶微粒。如标示地施加了盐包衣和薄膜包衣。然后将每种微粒加入颗粒漂白去污剂或颗粒非漂白去污剂，并在37℃、70%相对湿度下储存。盐包衣以相对于核心重量的40重量%的量施加。PEG(聚乙二醇)蜡包衣是在混合器中制备的。
这些结果证明了添加聚胺、多价阳离子、柠檬酸缓冲剂以及施加盐包衣的效果。因此，微粒A和B的结果的比较显示了添加多价阳离子和施加包衣的效果；微粒B和C的结果的比较显示了进一步添加聚胺的效果；微粒C和D的结果的比较显示了施加柠檬酸缓冲剂的效果。
实施例7：
制备了在核心中含有不同聚胺作为添加剂的酶微粒并添加到粉末去污剂中：
Lupasol产品可获自BASF，Germany。Epomin P-1050是Nippon ShokubaiJapan的产品。Aldrich产品可获自Sigma-Aldrich Co.LLC。
Claims (14)
1.一种颗粒，其具有包含均匀混合物的核心，该混合物包含可溶形式的酶和聚胺，所述聚胺的分子具有至少10%w/w的氮，其中至少50%的N原子作为胺存在。
2.权利要求1的颗粒，其中所述聚胺是聚乙烯亚胺。
3.权利要求1或2的颗粒，其中所述聚胺的平均分子量高于800Da。
4.前述权利要求中任一项的颗粒，其中所述聚胺的平均分子量低于2,000,000Da。
5.前述权利要求中任一项的颗粒，其中所述聚胺以所述核心中的混合物的重量的0.1-10%、尤其是0.2-5或0.5-2%的量存在。
6.前述权利要求中任一项的颗粒，其中所述核心中的混合物还包含多价阳离子的可溶盐，尤其是二价阳离子的可溶盐。
7.前述权利要求中任一项的颗粒，其中所述阳离子是Zn、Mg、Cu或Mn。
8.前述权利要求中任一项的颗粒，其中所述可溶盐是硫酸盐或乙酸盐。
9.前述权利要求中任一项的颗粒，其中所述可溶性盐以按无水形式重量计0.1-20%，尤其是0.5-10%或1-5%的量存在。
10.前述权利要求中任一项的颗粒，其中所述颗粒包含按所述核心的重量计1-5%的量的乙酸锌。
11.前述权利要求中任一项的颗粒，其中所述酶是脂肪酶、角质酶、淀粉酶、糖酶、纤维素酶、果胶酶、果胶酸裂合酶、甘露聚糖酶、阿拉伯糖酶、半乳聚糖酶、木聚糖酶、氧化酶、漆酶、或过氧化物酶。
12.前述权利要求中任一项的颗粒，其中所述核心具有包含盐的包衣，具体是相对于未包被的颗粒以重量计占5-70%的包衣，更具体是包含以重量计60%w/w的所述盐的包衣，最具体地是包含在20℃具有至少60%的恒定湿度的盐的包衣。
13.制备前述权利要求中任一项的颗粒的方法，其包括用包含所述酶和所述聚胺的水溶液制粒。
14.一种颗粒去污剂组合物，其包含表面活性剂和权利要求1-12中任一项的酶颗粒。
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| EP11173592.4 | 2011-07-12 | ||
| EP11173592 | 2011-07-12 | ||
| PCT/EP2012/063131 WO2013007594A1 (en) | 2011-07-12 | 2012-07-05 | Storage-stable enzyme granules |
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| CN201710881623.8A Division CN107523441A (zh) | 2011-07-12 | 2012-07-05 | 储存稳定的酶颗粒 |
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- 2012-07-05 WO PCT/EP2012/063131 patent/WO2013007594A1/en active Application Filing
- 2012-07-05 US US14/232,076 patent/US10711262B2/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111448302A (zh) * | 2017-10-16 | 2020-07-24 | 诺维信公司 | 低粉化颗粒 |
| CN111542589A (zh) * | 2017-10-16 | 2020-08-14 | 诺维信公司 | 低粉化颗粒 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107523441A (zh) | 2017-12-29 |
| US10711262B2 (en) | 2020-07-14 |
| WO2013007594A1 (en) | 2013-01-17 |
| US20140256610A1 (en) | 2014-09-11 |
| EP2732018B1 (en) | 2017-01-04 |
| EP2732018A1 (en) | 2014-05-21 |
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