CN103459442B - 作为洗涤和清洁产品的阻垢添加剂且包含羧酸基团、磺基和聚氧化烯基团的共聚物 - Google Patents
作为洗涤和清洁产品的阻垢添加剂且包含羧酸基团、磺基和聚氧化烯基团的共聚物 Download PDFInfo
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- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- BWSZXUOMATYHHI-UHFFFAOYSA-N tert-butyl octaneperoxoate Chemical compound CCCCCCCC(=O)OOC(C)(C)C BWSZXUOMATYHHI-UHFFFAOYSA-N 0.000 description 1
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- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
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- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F216/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F216/12—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
- C08F216/14—Monomers containing only one unsaturated aliphatic radical
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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Abstract
本发明涉及共聚物,其通过共聚引入有:a1)30-90重量%至少一种单烯属不饱和C3-C8羧酸或其酸酐或盐;a2)3-60重量%至少一种含磺基的单体;a3)3-60重量%至少一种式(I)H2C=C(R1)(CH2)xO[R2-O]o-R3(I)的非离子单体,其中R1为氢或甲基,R2相同或不同且为可呈嵌段或无规排列的直链或支化C2-C6亚烷基,R3为氢或直链或支化C1-C4烷基,x为0、1或2且o为3-50的自然数;a4)0-30重量%一种或多种可与a1)、a2)和a3)聚合的其他烯属不饱和单体;其中a1)、a2)、a3)和a4)之和等于100重量%。
Description
本发明涉及包含羧酸基团、磺基和聚氧化烯基团的共聚物,及其作为洗涤和清洁产品,尤其是用于机器洗碗的含磷酸盐和不含磷酸盐的洗涤剂配制剂的阻垢添加剂的用途。
机器洗碗应在无残留物的干净条件下以无瑕疵的闪亮表面提供经洗涤的碗碟,对此通常必须使用洗涤剂、漂洗助剂和用于水软化的再生盐。2001年市场上出现了“3合1”型洗碗机洗涤剂,其兼具洗涤剂、漂洗助剂和再生盐的功能于一种产品中。除了用于移除器皿上的污渍的洗涤剂组分之外,其包含整合的漂洗助剂表面活性剂,其能确保在漂洗和干燥周期中,水从所述器皿的整个区域流走,从而防止污垢和水斑。此外,其包含用于结合产生硬度的钙和镁离子的组分。因此,消费者无需在洗碗机中再添加漂洗助剂和盐。引入其他功能(例如保护玻璃以免腐蚀以及保护银以免失去光泽)导致开发出x合1型(其中x=6或9)或“全合1”型产品。
多年来,由含羧基和含磺基的单体构成的共聚物已成为含磷酸盐和不含磷酸盐的机器洗碗洗涤剂的重要部分。然而,其对洗涤剂和漂洗性能的贡献,尤其是对防止器皿上的污垢的贡献仍需改进。
EP-A0778340描述了烯丙醇乙氧基化物和丙烯酸的共聚物在无磷酸盐洗碗机洗涤剂组合物中的应用。
WO05/08527公开了含磺基的共聚物、所述共聚物的制备及其作为洗涤、清洁和漂洗助剂产品的添加剂的用途。所述共聚物包含:(a)70-100mol%至少两种不同单烯属不饱和羧酸单体和(b)0-30mol%一种或多种非离子单体。磺基通过用氨基-C1-C2-链烷烃磺酸酰胺化而引入。
WO2005/042684描述了丙烯酸、甲基丙烯酸和丙烯酸烷氧基化物的特定共聚物作为机器洗碗中的阻垢添加剂的用途。
DE10225794描述了含磺基的共聚物作为洗涤和清洁产品的阻垢添加剂的用途,所述共聚物由30-95mol%单烯属不饱和羧酸、3-35mol%至少一种含磺基的单体和2-35mol%(甲基)丙烯酸烷氧基化物形成。在实施例中,使用由(甲基)丙烯酸、甲氧基聚乙二醇甲基丙烯酸酯和磺乙基甲基丙烯酸钠盐形成的共聚物。在另一实施例中,使用由丙烯酸和2-丙烯酰胺基-2-甲基丙磺酸形成的二元共聚物。
WO2008/132131描述了含磺基的共聚物作为洗碗机洗涤剂的阻垢添加剂以防止形成磷酸钙沉积物的用途,所述共聚物由30-95mol%丙烯酸和/或甲基丙烯酸、3-35mol%含磺基的单体和2-35mol%下式的非离子单体形成:
H2C=C(R2)-COO-R3-[-R4-O-]n-R5
WO2010/024468描述了由含羧酸根的单体、含磺酸根的聚合物和烯丙基醚或具有1-5个氧化乙烯基团的烯丙醇乙氧基化物形成的共聚物作为洗涤和清洁产品添加剂的用途。优选的含磺酸根的单体为2-羟基-3-烯丙氧基丙磺酸。
本发明的目的是提供其特征在于具有有利的应用性能,尤其是其阻垢作用和在机器洗碗领域中于含磷酸盐和不含磷酸盐的洗碗机洗涤剂中的很宽适用性的共聚物。
本发明的另一目的是提供改进的用于机器洗碗的含磷酸盐和不含磷酸盐的洗涤剂配制剂,其能提供改善的洗涤效果。本发明的特定目的是提供该配制剂,其能在不使用其他漂洗助剂下获得无条纹、无沉积物且无滴流的碗碟。
所述目的通过如下共聚物实现,其包含呈共聚形式的如下物质:
a1)30-90重量%至少一种单烯属不饱和C3-C8羧酸或其酸酐或盐;
a2)3-60重量%至少一种含磺基的单体;
a3)3-60重量%至少一种式(I)的非离子单体:
H2C=C(R1)(CH2)xO[R2-O]o-R3 (I)
其中R1为氢或甲基,R2相同或不同且为可呈嵌段或无规排列的直链或支化C2-C6亚烷基,R3为氢或直链或支化C1-C4烷基,x为0、1或2且o为3-50的数;
a4)0-30重量%一种或多种可与a1)、a2)和a3)聚合的其他烯属不饱和单体;其中a1)、a2)、a3)和a4)之和总计为100重量%。
所述目的还通过所述共聚物作为洗涤和清洁产品,尤其是不含磷酸盐或含磷酸盐的机器洗碗用洗涤剂配制剂的阻垢添加剂的用途实现。
已发现通过将包含羧酸基团、磺基和聚氧化烯基团的本发明共聚物添加至含磷酸盐和不含磷酸盐的洗碗机洗涤剂中,可获得优异的清洁和助洗性能以及就无机和有机沉积物而言的优异阻垢性能。
此外,所述目的通过一种用于机器洗碗的洗涤剂配制剂实现,其包含作为组分的如下物质:
a)1-20重量%至少一种共聚物,其包含呈共聚形式的如下物质:
a1)30-90重量%至少一种单烯属不饱和C3-C8羧酸或其酸酐或盐;
a2)3-60重量%含磺基的单体;
a3)3-60重量%至少一种式(I)的非离子单体:
H2C=C(R1)(CH2)xO[R2-O]o-R3 (I)
其中R1为氢或甲基,R2相同或不同且为可呈嵌段或无规排列的直链或支化C2-C6亚烷基,R3为氢或直链或支化C1-C4烷基,x为0、1或2且o为3-50的数;
a4)0-30重量%一种或多种可与a1)、a2)和a3)聚合的烯属不饱和单体;
其中a1)、a2)、a3)和a4)之和总计为100重量%;
b)0-20重量%不同于组分a)的聚羧酸盐;
c)0-50重量%络合剂;
d)0-70重量%磷酸盐;
e)0-60重量%其他助洗剂和共助洗剂;
f)0.1-20重量%非离子表面活性剂;
g)0-30重量%漂白剂和任选的漂白活化剂和漂白催化剂;
h)0-8重量%酶;
i)0-50重量%一种或多种其他添加剂,如阴离子或两性离子表面活性剂、碱性载体、腐蚀抑制剂、消泡剂、染料、香料、填料、有机溶剂、成片助剂(tabletting aid)、崩解剂、增稠剂、加溶剂和水;
其中组分a)至i)之和总计为100重量%。
作为组分a1),所述共聚物包含30-90重量%至少一种单烯属不饱和C3-C8羧酸或其酸酐或盐。
合适的不饱和C3-C8羧酸尤其为丙烯酸、甲基丙烯酸、乙基丙烯酸、乙烯基乙酸、烯丙基乙酸、巴豆酸、马来酸、富马酸、中康酸和衣康酸及其水溶性盐。当所述不饱和C3-C8羧酸可形成酸酐时,后者也适于作为单体a1),例如马来酸酐、衣康酸酐和甲基丙烯酸酐。
优选的单烯属不饱和C3-C8羧酸为丙烯酸和甲基丙烯酸及其水溶性盐。水溶性盐尤其为所述酸的钠盐和钾盐。
作为单体a2),所述共聚物包含3-60重量%至少一种含磺基的单体。
所述含磺基的单体优选为式(IIa)和(IIb)的那些:
H2C=CH-X-SO3H (IIa)
H2C=C(CH3)-X-SO3H (IIb)
其中X为任选存在的间隔基团,其可选自-(CH2)n-(其中n=0-4)、-C6H4-、-CH2-O-C6H4-、-C(O)-NH-C(CH3)2-、-C(O)-NH-CH(CH2CH3)-、-C(O)NH-CH(CH3)CH2-、-C(O)NH-C(CH3)2CH2-、-C(O)NH-CH2CH(OH)CH2-、-C(O)NHCH2-、-C(O)NH-CH2CH2-和-C(O)NH-CH2CH2CH2-。
特别优选的含磺基单体为1-丙烯酰胺基-1-丙磺酸(在式IIa中,X=-C(O)NH-CH(CH2CH3)-)、2-丙烯酰胺基-2-丙磺酸(在式IIa中,X=-C(O)NH-CH(CH3)CH2-)、2-丙烯酰胺基-2-甲基丙磺酸(AMPS,在式IIa中,X=-C(O)NH-C(CH3)2CH2-)、2-甲基丙烯酰胺基-2-甲基丙磺酸(在式IIb中,X=-C(O)NH-C(CH3)2CH2-)、3-甲基丙烯酰胺基-2-羟基丙磺酸(在式IIb中,X=-C(O)NH-CH2CH(OH)CH2-)、烯丙基磺酸(在式IIa中,X=CH2)、甲基烯丙基磺酸(在式IIb中,X=CH2)、烯丙氧基苯磺酸(在式IIa中,X=-CH2-O-C6H4-)、甲基烯丙氧基苯磺酸(X=-CH2-O-C6H4-)、2-羟基-3-(2-丙烯氧基)丙磺酸、2-甲基-2-丙烯-1-磺酸(在式IIb中,X=CH2)、苯乙烯磺酸(在式IIa中,X=C6H4)、乙烯基磺酸(在式IIa中,X不存在)、丙烯酸3-磺丙基酯(在式IIa中,X=-C(O)O-CH2CH2CH2-)、甲基丙烯酸2-磺乙基酯(在式IIb中,X=-C(O)O-CH2CH2-)、甲基丙烯酸3-磺丙基酯(在式IIb中,X=-C(O)O-CH2CH2CH2-)、磺基甲基丙烯酰胺(在式IIb中,X=-C(O)NH-)、磺甲基甲基丙烯酰胺(在式IIb中,X=-C(O)NH-CH2-),以及所述盐酸的盐。合适的盐通常为所述酸的水溶性盐,优选为钠盐、钾盐和铵盐。
尤其优选1-丙烯酰胺基丙磺酸、2-丙烯酰胺基-2-丙磺酸、2-丙烯酰胺基-2-甲基丙磺酸(AMPS)、2-甲基丙烯酰胺基-2-甲基丙磺酸、3-甲基丙烯酰胺基-2-羟基丙磺酸、2-羟基-3-(2-丙烯氧基)丙磺酸、甲基丙烯酸2-磺乙基酯、苯乙烯磺酸、乙烯基磺酸、烯丙基磺酸(ALS)和甲基烯丙基磺酸,以及所述酸的盐。
非常特别优选的含磺基单体为2-丙烯酰胺基-2-甲基丙磺酸(AMPS)和烯丙基磺酸及其水溶性盐,尤其是其钠盐、钾盐和铵盐。
作为组分a3),所述共聚物包含3-60重量%至少一种式(I)的非离子单体:
H2C=C(R1)(CH2)xO[R2-O]o-R3 (I)
其中R1为氢或甲基,R2相同或不同且为可呈嵌段或无规排列的直链或支化C2-C6亚烷基,R3为氢或直链或支化C1-C4烷基,x为0、1或2且o为3-50的数。
所述亚烷基也可呈嵌段或无规排列,即以相同氧化烯基团的一个或多个嵌段形式排列以及额外地,以两种或更多种不同氧化烯基团的一个或多个嵌段形式无规排列。这也被措辞“呈嵌段或无规排列”所涵盖。
优选的非离子单体a3)为基于烯丙醇(R1=H;x=1)和异戊烯醇(R1=甲基;x=2)的那些。
所述非离子单体a3)优选包含平均8-40个,更优选10-30个,尤其是10-25个氧化烯单元。式(I)中的指数o基于氧化烯单元的平均数。
优选的氧化烯单元R2-O为氧化乙烯、1,2-氧化丙烯和1,2-氧化丁烯,特别优选氧化乙烯和1,2-氧化丙烯。
在一个具体实施方案中,非离子单体a3)仅包含氧化乙烯单元。在另一具体实施方案中,非离子单体a3)包含氧化乙烯和1,2-氧化丙烯单元,其可可呈嵌段或无规排列。
R3优选为氢或甲基。
作为组分a4),所述共聚物可包含0-30重量%一种或多种可与a1)、a2)和a3)聚合的其他烯属不饱和单体。
可用的其他烯属不饱和单体a4)包括例如丙烯酰胺、叔丁基丙烯酰胺、乙酸乙烯酯、乙烯基甲基醚、羟丁基乙烯基醚、1-乙烯基吡咯烷酮、1-乙烯基己内酰胺、1-乙烯基咪唑、2-乙烯基吡啶、4-乙烯基吡啶、甲基丙烯酸甲酯、丙烯酸乙酯、异丁烯、二异丁烯、异戊烯醇、1-链烯烃如1-辛烯、N,N-二甲基丙烯酰胺和苯乙烯。
共聚单体a1),尤其是共聚的丙烯酸、甲基丙烯酸或这些酸的水溶性盐的比例优选为40-90重量%,更优选为45-85重量%,尤其优选为50-85重量%。共聚单体a2),尤其是共聚的2-丙烯酰胺基-2-甲基丙磺酸的比例优选为4-40重量%,更优选为6-35重量%,尤其优选为8-32重量%。式(I)单体单元a3)的比例优选为4-40重量%,更优选为6-35重量%,尤其为8-32重量%。
如果本发明的共聚物中存在单体a4),则其比例优选为至多20重量%,更优选至多15重量%,尤其是至多10重量%。
本发明共聚物a)的平均分子量Mw通常为2000-200000g/mol,优选为3000-100000g/mol,更优选为10000-50000g/mol,借助凝胶渗透色谱法在室温下使用水作为洗脱液对聚丙烯酸酯标样测定。
其K值为15-100,优选为20-80,更优选为30-50,根据H.Fikentscher,Cellulose-Chemie第13卷,第58-64页和第71-74页(1932)在pH7下于25°C的1重量%水溶液中测定。
本发明共聚物可通过单体的自由基聚合制备。其可通过任何已知的自由基聚合方法进行。除本体聚合法之外,还尤其应提及溶液聚合法和乳液聚合法,其中优选溶液聚合法。
所述聚合优选在作为溶剂的水中进行。然而,也可在醇类溶剂,尤其是在C1-C4醇如甲醇、乙醇和异丙醇或这些溶剂与水的混合物中进行。
合适的聚合引发剂为热分解、通过氧化还原机理分解或光化学(光敏引发剂)分解以形成自由基的化合物。
在可热活化的聚合引发剂中,优选分解温度为20-180°C,尤其是50-90°C的引发剂。合适的热引发剂实例为无机过氧化合物,如过硫酸盐(过硫酸铵,优选过硫酸钠)、过硫酸盐、过碳酸盐和过氧化氢;有机过氧化合物,如过氧化二乙酰、过氧化二叔丁基、过氧化二戊基、过氧化二辛酰、过氧化二癸酰、过氧化二月桂酰、过氧化二苯甲酰、过氧化二(邻甲苯基)、过氧化丁二酰、过新癸酸叔丁酯、过苯甲酸叔丁酯、过异丁酸叔丁酯、过新戊酸叔丁酯、过辛酸叔丁酯、过新癸酸叔丁酯、过苯甲酸叔丁酯、过氧化叔丁基、氢过氧化叔丁基、氢过氧化枯烯、过氧化2-乙基己酸叔丁酯和过氧基二氨基甲酸二异丙酯;偶氮化合物,如2,2’-偶氮二异丁腈、2,2’-偶氮双(2-甲基丁腈)和偶氮双(2-酰胺基丙烷)二盐酸盐。
这些引发剂可与还原性化合物组合使用以作为引发剂/调节剂体系。该还原性化合物的实例包括磷化合物如亚磷酸、次磷酸盐和次膦酸盐,硫化合物如亚硫酸氢钠、亚硫酸钠和甲醛次硫酸钠和肼。
还常用的有由过氧化合物、金属盐和还原剂构成的氧化还原引发剂体系。合适的过氧化合物实例为过氧化氢、过硫酸盐(如铵盐、钠盐或钾盐)、过硫酸盐,和有机过氧化合物如氢过氧化叔丁基、氢过氧化枯烯或过氧化二苯甲酰。合适的金属盐尤其为铁(II)盐如七水硫酸铁(II)。合适的还原剂为亚硫酸钠、2-羟基-2-亚磺酸基乙酸的二钠盐、2-羟基-2-磺酸基乙酸的二钠盐、羟甲基亚磺酸钠、抗坏血酸、异抗坏血酸或其混合物。
合适的光敏引发剂实例为二苯甲酮、苯乙酮、苄基二烷基酮及其衍生物。
优选使用热引发剂,其中优选无机过氧化合物,尤其为过硫酸钠。所述过氧化合物尤其有利地与含硫还原剂,尤其是亚硫酸氢钠组合使用以作为氧化还原引发剂体系。在使用该引发剂/调节剂体系的情况下,获得包含-SO3 -Na+和/或-SO4 -Na+作为端基的共聚物,其特征在于优异的洗净力和阻垢作用。
或者,还可使用含磷引发剂/调节剂体系,如次磷酸盐/次膦酸盐。
光敏引发剂和引发剂/调节剂体系的量应与每种情况下所用的物质匹配。例如,如果使用优选的过硫酸盐/亚硫酸氢盐体系,则通常使用2-6重量%,优选3-5重量%的过硫酸盐和通常为5-30重量%,优选为5-10重量%的亚硫酸氢盐,在每种情况下基于单体a1)、a2)、a3)和任选的a4)。
需要的话,还可使用聚合调节剂。合适的实例为硫化合物如巯基乙醇、硫基乙醇酸2-乙基己酯、硫基乙醇酸和十二烷基硫醇。当使用聚合调节剂时,其用量通常为0.1-15重量%,优选为0.1-5重量%,更优选为0.1-2.5重量%,基于单体a1)、a2)、a3)和任选的a4)。
聚合温度通常为20-200°C,优选为20-150°C,更优选为20-120°C。
所述聚合反应可在大气压下进行,但优选在密闭系统中在其自生压力下进行。
所述共聚物可以以酸性状态获得,但如果出于应用需要的话,则其也可早在聚合期间或聚合结束后,通过添加碱,尤其是氢氧化钠溶液而中和或部分中和。所述共聚物水溶液的优选pH值为3-8.5。
本发明所用的共聚物可以以在借助于水中溶剂聚合的制备过程中所得的水溶液形式直接使用,或者以干燥形式(例如通过喷雾干燥、喷雾造粒、流化喷雾干燥、滚筒干燥或冷冻干燥)使用。
除组分a)之外,本发明的洗涤剂配制剂还可包含不同于组分a)的0-20重量%聚羧酸盐作为组分b)。这些可为亲水或疏水改性的。
如果存在不同于组分a)的聚羧酸盐,则其通常以0.1-20重量%的量存在。
合适的实例为丙烯酸或甲基丙烯酸的均聚物和共聚物的碱金属盐。适于共聚的有单烯属不饱和二羧酸如马来酸、富马酸、马来酸酐、衣康酸和柠康酸。合适的聚合物尤其为优选具有2000-40000g/mol摩尔质量的聚丙烯酸。由于其优异的溶解性,该类聚合物优选可为具有2000-10000g/mol,尤其是3000-8000g/mol摩尔质量的短链聚丙烯酸。此外,合适的还有共聚聚羧酸盐,尤其是丙烯酸与甲基丙烯酸的那些和丙烯酸或甲基丙烯酸与马来酸和/或富马酸的那些。
还可使用至少一种选自单烯属不饱和C3-C10单羧酸或二羧酸或其酸酐的单体(如马来酸、马来酸酐、丙烯酸、甲基丙烯酸、富马酸、衣康酸和柠康酸)与至少一种如下文所列举的亲水或疏水改性单体的共聚物。
合适的疏水单体例如为异丁烯,二异丁烯,丁烯,戊烯,己烯和苯乙烯,具有10个或更多个碳原子的烯烃或其混合物如1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯、1-十八碳烯、1-二十碳烯、1-二十二碳烯、1-二十四碳烯和1-二十六碳烯,C22α烯烃,以及C20-C24α烯烃与平均具有12-100个碳原子的聚异丁烯的混合物。
合适的亲水单体为具有磺酸根或磷酸根的单体以及具有羟基官能团或氧化烯基团的非离子单体。实例包括:烯丙醇、异戊烯醇、甲氧基聚乙二醇(甲基)丙烯酸酯、甲氧基聚丙二醇(甲基)丙烯酸酯、甲氧基聚丁二醇(甲基)丙烯酸酯、甲氧基聚(氧化丙烯-共聚-氧化乙烯)(甲基)丙烯酸酯、乙氧基聚乙二醇(甲基)丙烯酸酯、乙氧基聚丙二醇(甲基)丙烯酸酯、乙氧基聚丁二醇(甲基)丙烯酸酯和乙氧基聚(氧化丙烯-共聚-氧化乙烯)(甲基)丙烯酸酯。聚亚烷基二醇包含3-50个,尤其是5-40个,特别是10-30个氧化烯单元。
特别优选的含磺基单体为1-丙烯酰胺基-1-丙磺酸、2-丙烯酰胺基-2-丙磺酸、2-丙烯酰胺基-2-甲基丙磺酸、2-甲基丙烯酰胺基-2-甲基丙磺酸、3-甲基丙烯酰胺基-2-羟基丙磺酸、烯丙基磺酸、甲基烯丙基磺酸、烯丙氧基苯磺酸、甲基烯丙氧基苯磺酸、2-羟基-3-(2-丙烯氧基)丙磺酸、2-甲基-2-丙烯-1-磺酸、苯乙烯磺酸、乙烯基磺酸、丙烯酸3-磺丙基酯、甲基丙烯酸2-磺乙基酯、甲基丙烯酸3-磺丙基酯、磺基甲基丙烯酰胺、磺甲基甲基丙烯酰胺和所述酸的盐,如其钠盐、钾盐和铵盐。
特别优选的含膦酸根的单体为乙烯基膦酸及其盐。
此外,还可额外使用两性聚合物和阳离子聚合物。
作为组分c),本发明的洗涤剂配制剂可包含0-50重量%一种或多种络合剂。如果存在络合剂,则其以0.1-50重量%,优选1-45重量%,更优选1-40重量%的量存在。优选的络合剂选自次氮基三乙酸、乙二胺四乙酸、二亚乙基三胺五乙酸、羟乙基乙二胺三乙酸和甲基甘氨酸二乙酸、谷氨酸-二乙酸、亚氨基二琥珀酸、羟基亚氨基二琥珀酸、乙二胺二琥珀酸、天冬氨酸-二乙酸及其盐。特别优选的络合剂c)为甲基甘氨酸二乙酸及其盐。
作为组分d),本发明洗涤剂可包含0-70重量%磷酸盐。当所述洗涤剂包含磷酸盐时,其通常以1-70重量%,优选5-60重量%,更优选20-55重量%的量包含磷酸盐。
在多种市售磷酸盐中,碱金属磷酸盐,特别优选三聚磷酸五钠或三聚磷酸五钾(三聚磷酸钠或三聚磷酸钾)在洗涤和清洁产品工业中最为重要。
适用于洗碗组合物的磷酸盐尤其为碱金属磷酸盐和聚合碱金属磷酸盐,其可以以其碱性、中性或酸性钠盐或钾盐形式存在。该类磷酸盐的实例为磷酸三钠、二磷酸四钠、二磷酸二氢二钠、三聚磷酸五钠(称为六偏磷酸钠)、低聚度为5-1000,优选5-50的低聚磷酸三钠和相应的钾盐,或六偏磷酸钠与相应钾盐的混合物,或钠盐与钾盐的混合物。尤其优选三聚磷酸盐。
作为组分e),本发明洗涤剂可包含0-60重量%助洗剂和共助洗剂。当所述洗涤剂包含助洗剂和共助洗剂时,其通常以0.1-60重量%的量包含助洗剂和共助洗剂。助洗剂和共助洗剂为水溶性或水不溶性物质,其主要任务是结合钙和镁离子。
这些可为低分子量羧酸及其盐如碱金属柠檬酸盐,尤其是无水柠檬酸三钠或柠檬酸三钠二水合物;碱金属琥珀酸盐;碱金属丙二酸盐;脂肪酸磺酸盐;氧基二琥珀酸盐(oxydisuccinat);烷基或烯基琥珀酸盐;葡糖酸;氧杂二乙酸盐(oxadiacetate);羧甲基氧基琥珀酸盐;酒石酸单琥珀酸盐;酒石酸二琥珀酸盐;酒石酸单乙酸盐、酒石酸二乙酸盐和α-羟基丙酸。
可存在于本发明洗涤剂中且具有共助洗剂性质的其他物质类别为膦酸盐。这些尤其为羟基链烷烃膦酸盐或氨基链烷烃膦酸盐。在羟基链烷烃膦酸盐中,1-羟基乙烷-1,1-二膦酸盐(HEDP)作为共助洗剂特别重要。其优选以钠盐、中性二钠盐和碱性四钠盐(pH值为9)形式使用。可用的氨基链烷烃膦酸盐优选包括乙二胺四亚甲基膦酸盐(EDTMP)、二亚乙基三胺五亚甲基膦酸盐(DTPMP)或其更高级同系物。其优选以中性钠盐,例如EDTMP的六钠盐或DTPMP的七钠盐和八钠盐形式使用。选自膦酸盐的所用助洗剂优选为HEDP。此外,氨基链烷烃膦酸盐具有显著的重金属结合能力。因此,尤其当所述组合物还包含漂白剂时,可优选使用氨基链烷烃膦酸盐,尤其是DTPMP,或者使用所述膦酸盐的混合物。
助洗剂体系中的另一类物质为硅酸盐。可存在具有通式NaMSixO2x+1yH2O的结晶层状硅酸盐,其中M为钠或氢,x为1.9-22,优选为1.9-4,特别优选x的值为2、3或4,且y为0-33,优选0-20。此外,可使用SiO2:Na2O之比为1-3.5,优选1.6-3,尤其为2-2.8的无定形硅酸钠。
此外,使用碳酸盐和碳酸氢盐,其中优选碱金属盐,尤其是钠盐。
作为组分f),本发明的洗涤剂配制剂包含0.1-20重量%非离子表面活性剂,通常为弱起泡或低起泡非离子表面活性剂。这些优选以0.1-15重量%,更优选0.25-10重量%的比例存在。
合适的非离子表面活性剂包括通式(III)的表面活性剂:
R18-O-(CH2CH2O)p-(CHR17CH2O)m-R19 (III)
其中
R18为具有8-22个碳原子的直链或支化烷基,
R17和R19各自独立地为氢或具有1-10个碳原子的直链或支化烷基或H,其中R17优选为甲基,
p和m各自独立地为0-300。优选地,p=1-100且m=0-30。
式(III)的表面活性剂可为无规共聚物或嵌段共聚物,优选为嵌段共聚物。
此外,可使用由氧化乙烯和氧化丙烯形成的二嵌段共聚物和多嵌段共聚物,其可例如以(BASF SE)或(BASF Corporation)名称商购获得。此外,可使用由脱水山梨醇酯与氧化乙烯和/或氧化丙烯形成的反应产物。同样合适的是氧化胺或烷基糖苷。合适的非离子表面活性剂的综述由EP-A851023和DE-A19819187给出。
还可存在若干种不同非离子表面活性剂的混合物。
作为组分g),本发明的洗涤剂配制剂可包含0-30重量%漂白剂,任选的漂白活化剂和任选的漂白催化剂。如果所述洗涤剂配制剂包含漂白剂、漂白活化剂或漂白催化剂,则其以总计为0.1-30重量%,优选1-30重量%,更优选5-30重量%的量包含后者。
漂白剂分为氧漂白剂或氯漂白剂。所用的氧漂白剂包括碱金属过硼酸盐及其水合物和碱金属过碳酸盐。就此而言,优选的漂白剂为呈一水合物或四水合物形式的过硼酸钠,过碳酸钠或过碳酸钠的水合物。
同样可用作氧漂白剂的有过硫酸盐和过氧化氢。
典型的氧漂白剂还有有机过酸如过苯甲酸、过氧化α-萘甲酸、过氧化月桂酸、过氧化硬脂酸、邻苯二甲酰亚氨基过氧己酸、1,12-二过氧基十二烷二酸、1,9-二过氧基壬二酸、二过氧间苯二甲酸或2-癸基二过氧基丁烷-1,4-二酸。
此外,如下氧漂白剂也可用于所述洗涤剂配制剂中:专利申请US5,422,028、US5,294,362和US5,292,447中所述的阳离子过氧酸和专利申请US5,039,447中所述的磺酰基过氧酸。
同样可使用氯漂白剂以及氯漂白剂与过氧漂白剂的组合。已知的氯漂白剂例如为1,3-二氯-5,5-二甲基乙内酰脲、N-氯磺酰胺、氯胺T、二氯胺T、氯胺B、N,N′-二氯苯甲酰脲、二氯对甲苯磺酰胺或三氯乙胺。优选的氯漂白剂为次氯酸钠、次氯酸钙、次氯酸钾、次氯酸镁、二氯异氰脲酸钾或二氯异氰脲酸钠。
氯漂白剂通常以基于全部洗涤剂配制剂为0.1-20重量%,优选0.2-10重量%,更优选0.3-8重量%的量使用。
此外,可添加少量漂白稳定剂如膦酸盐、硼酸盐、偏硼酸盐、偏硅酸盐或镁盐。
漂白活化剂为在过氧化氢解条件(perhydrolysebedingungen)下形成优选具有1-10个碳原子,尤其是2-4个碳原子的脂族过氧羧酸和/或取代的过苯甲酸的化合物。合适的化合物为包含一个或多个N-或O-酰基和/或任选取代的苯甲酰基的那些,例如选自酐、酯、酰亚胺、酰基化咪唑或肟的物质。实例为四乙酰基乙二胺(TAED)、四乙酰基亚甲基二胺(TAMD)、四乙酰基甘脲(TAGU)、四乙酰基己二胺(TAHD)、N-酰基亚胺如N-壬酰基琥珀酰亚胺(NOSI)、酰基化的苯酚磺酸盐如正壬酰基-或异壬酰基氧基苯磺酸盐(正或异NOBS)、五乙酰基葡萄糖(PAG)、1,5-二乙酰基-2,2-二氧六氢-1,3,5-三嗪(DADHT)或靛红酸酐(ISA)。适于作为漂白活化剂同样还有腈季铵盐(nitrilquat),例如N-甲基吗啉基乙腈盐(MMA盐)或三甲基铵乙腈盐(TMAQ盐)。
优选合适的漂白活化剂为选自多酰基化的亚烷基二胺的那些,更优选TAED、N-酰基亚胺,更优选NOSI,酰基化的苯酚磺酸盐,更优选正或异NOBS、MMA和TMAQ。
漂白活化剂以基于全部洗涤剂配制剂通常为0.1-10重量%,优选1-9重量%,更优选1.5-8重量%的量使用。
除常规漂白活化剂或其替代物之外,还可存在所谓的漂白催化剂。这些物质为漂白增强过渡金属盐或过渡金属配合物如锰-、铁-、钴-、钌-或钼-salen配合物或-羰基配合物。可用的漂白催化剂还有锰、铁、钴、钌、钼、钛、钒和铜与含氮三脚架配体的配合物以及钴-、铁-、铜-和钌-胺配合物。
作为组分h),本发明的洗涤剂配制剂可包含0-8重量%酶。如果所述洗涤剂配制剂包含酶,则其通常以0.1-8重量%的量包含后者。可将酶添加至所述洗涤剂中以提高所述洗涤剂的性能或确保在更温和的条件下达到相同的清洁性能品质。最常用的酶包括脂肪酶、淀粉酶、纤维素酶和蛋白酶。此外,也可使用例如酯酶、果胶酶、乳糖酶和过氧化物酶。
此外,本发明洗涤剂可包含0-50重量%一种或多种其他添加剂作为组分i),例如阴离子表面活性剂或两性离子表面活性剂、碱性载体、腐蚀抑制剂、消泡剂、染料、香料、填料、有机溶剂、成片助剂、崩解剂、增稠剂、加溶剂和水。如果所述洗涤剂配制剂包含其他添加剂,则其通常以0.1-50重量%的量存在。
所述配制剂可包含阴离子表面活性剂或两性离子表面活性剂,优选呈与非离子表面活性剂的混合物形式。合适的阴离子表面活性剂或两性离子表面活性剂描述于EP-A851023和DE-A19819187中。
作为所述洗涤剂配制剂的其他成分,可存在碱性载体。除已对所述助洗剂物质提及的碳酸铵或碱金属碳酸盐、碳酸氢铵或碱金属碳酸氢盐和倍半碳酸铵或碱金属倍半碳酸盐之外,所用的碱性载体也可为氢氧化铵或碱金属氢氧化物、硅酸铵或碱金属硅酸盐和偏硅酸铵或碱金属偏硅酸盐,以及上述物质的混合物。
所用的腐蚀抑制剂可为选自三唑类、苯并三唑类、二苯并三唑类、氨基三唑类、烷基氨基三唑类和过渡金属盐或配合物的银防腐蚀剂。
为了防止玻璃腐蚀(其体现为玻璃上的发雾、虹彩、条纹和线),使用玻璃腐蚀抑制剂。优选的玻璃腐蚀抑制剂选自镁、锌和铋盐以及配合物。
可任选将石蜡油和硅油用作消泡剂以保护塑料和金属表面。消泡剂通常以0.001-5重量%的比例使用。此外,可在本发明的洗涤剂配制剂中添加染料如专利蓝、防腐剂如Kathon CG、香料和其他芳香物质。
合适的填料实例为硫酸钠。
本发明的洗涤剂配制剂可以以液态或固体形式、在一个或多个相中、作为片剂或其他剂量单位形式、包装形式或未包装形式提供。
通过下文实施例对本发明进行详细阐述。
实施例
在所有情况下,分子量借助凝胶渗透色谱法(GPC)测定。这使用2柱(Suprema Linear M)和预置柱(Suprema precolumn)(全部为获自PolymerStandard Service(Mainz,德国)的Suprema-Gel牌(HEMA))在35°C下以0.8ml/分钟的流速进行。洗脱液为用TRIS缓冲的pH值为7水溶液,其中已添加有0.15M NaCl和0.01M NaN3。标定使用Na-PAA标样进行,其积分分子量分布曲线通过耦合SEC-激光散射根据M.J.R.Cantow等的标定法(J.Polym.Sci.,A-1,5(1967)1391-1394)测定,但不使用其中提出的浓度校准。用50%氢氧化钠溶液将所有试样调节至pH7,使用软化水将一部分该溶液稀释至固含量为1.5mg/ml,并将所述混合物搅拌12小时。随后过滤所述试样。在每种情况下,借助Sartorius Minisart RC25(0.2μm)注入100μl。
对照实施例C1
首先在反应器中装入503.9g软化水和2.36g50重量%亚磷酸水溶液。随后,在氮气气氛下将所述混合物加热至内部温度为100°C。在该温度下,在搅拌下同时分开且平行计量加入58.9g10.0重量%过硫酸钠水溶液、39.2g40重量%亚硫酸氢钠水溶液和394.0g由10.9重量%经蒸馏的丙烯酸、11.2重量%甲氧基聚乙二醇甲基丙烯酸酯(Mw=1086g/mol)、11.9重量%经蒸馏的甲基丙烯酸、4.5重量%2-磺乙基甲基丙烯酸钠盐和61.5%软化水构成的混合物。在5小时内计量加入所述单体混合物,在5.25小时内计量加入过硫酸钠,并在5小时内计量加入亚硫酸氢钠。此后,在100°C下再继续聚合2小时。随后,将所述混合物冷却至室温,然后使用90.0g50重量%氢氧化钠水溶液以获得7.4的pH值。测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
对照实施例C2
首先在反应器装入904.6g软化水和2.36g50重量%亚磷酸水溶液。随后,在氮气气氛下将所述混合物加热至内部温度为100°C。在该温度下,在搅拌下同时分开且平行计量加入117.8g10.2重量%过硫酸钠水溶液、78.4g40重量%亚硫酸氢钠水溶液和752.8g由11.4重量%经蒸馏的丙烯酸、11.8重量%甲氧基聚乙二醇甲基丙烯酸酯(Mw=1086g/mol)、12.5重量%经蒸馏的甲基丙烯酸和64.3%软化水以及140.8g25重量%乙烯基磺酸钠溶液构成的混合物。在5小时内计量加入所述单体混合物,在5.25小时内计量加入过硫酸钠,并在5小时内计量加入亚硫酸氢钠。此后,在100°C下再继续聚合2小时。随后,将所述混合物冷却至室温,然后使用1g50重量%氢氧化钠水溶液以获得7.2的pH值。测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
实施例1
首先在反应器装入225.0g软化水和225.0g式CH2=CHCH2O-(EO4.1)(EO12.3PO5.5)-H的烯丙醇烷氧基化物。随后,在氮气气氛下将所述混合物加热至内部温度为90°C。在该温度下,在搅拌下同时分开且平行计量加入107.1g7重量%过硫酸钠水溶液、46.9g40重量%亚硫酸氢钠水溶液和994.8g由30.1重量%经蒸馏的丙烯酸、22.9重量%2-丙烯酰胺基-2-甲基丙磺酸、0.006重量%4-甲氧基苯酚溶液、4.4重量%氢氧化钠溶液和42.6重量%软化水构成的混合物。在3小时内计量加入所述单体混合物,在4.5小时内计量加入过硫酸钠,并在2.75小时内计量加入亚硫酸氢钠。在所述单体加料结束后,在内部温度90°C下于1.5小时内添加110.0g50重量%氢氧化钠水溶液。此后,在90°C下再继续聚合1小时。随后,添加382.7g软化水,其将所述聚合物溶液冷却至室温。测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
实施例2
首先在反应器装入300.0g软化水和120.0g式CH2=CHCH2O-(EO4.1)(EO12.3PO5.5)-H的烯丙醇烷氧基化物。随后,在氮气气氛下将所述混合物加热至内部温度为90°C。在该温度下,在搅拌下同时分开且平行计量加入85.7g7重量%过硫酸钠水溶液、45.0g40重量%亚硫酸氢钠水溶液和880.5g由40.9重量%经蒸馏的丙烯酸、13.8重量%2-丙烯酰胺基-2-甲基丙磺酸、0.003重量%4-甲氧基苯酚溶液、5.3重量%氢氧化钠溶液和40.0重量%软化水构成的混合物。在3小时内计量加入所述单体混合物,在4.5小时内计量加入过硫酸钠,并在2.75小时内计量加入亚硫酸氢钠。在所述单体加料结束后,在内部温度90°C下于1.5小时内添加148.9g50重量%氢氧化钠水溶液。此后,在90°C下再继续聚合1小时。随后,添加132.7g软化水,其将所述聚合物溶液冷却至室温。测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
实施例3
首先在反应器装入300.0g软化水和60.0g式CH2=CHCH2O-(EO4.1)(EO12.3PO5.5)-H的烯丙醇烷氧基化物。随后,在氮气气氛下将所述混合物加热至内部温度为90°C。在该温度下,在搅拌下同时分开且平行计量加入85.7g7重量%过硫酸钠水溶液、75.0g40重量%亚硫酸氢钠水溶液和915.3g由52.4重量%经蒸馏的丙烯酸、6.6重量%2-丙烯酰胺基-2-甲基丙磺酸、0.002重量%4-甲氧基苯酚溶液、2.5重量%氢氧化钠溶液和38.5重量%软化水构成的混合物。在3小时内计量加入所述单体混合物,在4.5小时内计量加入过硫酸钠,并在2.75小时内计量加入亚硫酸氢钠。在所述单体加料结束后,在内部温度90°C下于1.5小时内添加148.9g50重量%氢氧化钠水溶液。此后,在90°C下再继续聚合1小时。随后,添加132.7g软化水,其将所述聚合物溶液冷却至室温。测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
实施例4
首先在反应器装入225.0g软化水和225.0g式CH2=CHCH2O-(EO4.1)(EO12.3PO5.5)-H的烯丙醇烷氧基化物。随后,在氮气气氛下将所述混合物加热至内部温度为90°C。在该温度下,在搅拌下同时分开且平行计量加入112.0g7重量%过硫酸钠水溶液、103.1g40重量%亚硫酸氢钠水溶液和931.4g由48.3重量%经蒸馏的丙烯酸、8.1重量%2-丙烯酰胺基-2-甲基丙磺酸、0.002重量%4-甲氧基苯酚溶液、3.1重量%氢氧化钠溶液和40.5重量%软化水构成的混合物。在3小时内计量加入所述单体混合物,在4.5小时内计量加入过硫酸钠,并在2.75小时内计量加入亚硫酸氢钠。在所述单体加料结束后,在内部温度90°C下于1.5小时内添加188.7g50重量%氢氧化钠水溶液。此后,在90°C下再继续聚合1小时。随后,添加350.0g软化水,其将所述聚合物溶液冷却至室温。测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
实施例5
首先在反应器装入150.0g软化水和50.0g式CH2=CHCH2O-(EO16)-H的烯丙醇烷氧基化物。随后,在氮气气氛下将所述混合物加热至内部温度为90°C。在该温度下,在搅拌下同时分开且平行计量加入214.0g7重量%过硫酸钠水溶液、50.0g40重量%亚硫酸氢钠水溶液和818.7g由36.7重量%经蒸馏的丙烯酸、18.5重量%2-丙烯酰胺基-2-甲基丙磺酸、0.001重量%4-甲氧基苯酚溶液、7.5重量%氢氧化钠溶液和37.7重量%软化水构成的混合物。在3小时内计量加入所述单体混合物,在4.5小时内计量加入过硫酸钠,并在2.75小时内计量加入亚硫酸氢钠。在所述单体加料结束后,在内部温度90°C下于1.5小时内添加162.2g50重量%氢氧化钠水溶液。此后,在90°C下再继续聚合1小时。随后,将所述聚合物溶液冷却至室温。测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
实施例6
首先在反应器装入250.0g软化水和50.0g式(CH2=CHCH2O-(EO7.7PO3.0)-H的烯丙醇烷氧基化物。随后,在氮气气氛下将所述混合物加热至内部温度为90°C。在该温度下,在搅拌下同时分开且平行计量加入75.0g7重量%过硫酸钠水溶液、50.0g30.7重量%次磷酸钠水溶液和760.4g由39.5重量%经蒸馏的丙烯酸、20.0重量%2-丙烯酰胺基-2-甲基丙磺酸、0.002重量%4-甲氧基苯酚溶液、7.6重量%氢氧化钠溶液和32.9重量%软化水构成的混合物。在3小时内计量加入所述单体混合物,在4.5小时内计量加入过硫酸钠,并在2.75小时内计量加入亚硫酸氢钠。在所述单体加料结束后,在内部温度90°C下于1.5小时内添加120.0g50重量%氢氧化钠水溶液。此后,在90°C下再继续聚合1小时。随后,添加75.0g软化水以将所述聚合物溶液冷却至室温。测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
实施例7
首先在反应器装入250.0g软化水和50.0g式CH2=CHCH2O-(EO6)(EO5.1PO3.6)-H的烯丙醇烷氧基化物。随后,在氮气气氛下将所述混合物加热至内部温度为90°C。在该温度下,在搅拌下同时分开且平行计量加入75.0g7重量%过硫酸钠水溶液、50.0g40重量%亚硫酸氢钠水溶液和760.4g由39.4重量%经蒸馏的丙烯酸、19.9重量%2-丙烯酰胺基-2-甲基丙磺酸、0.002重量%4-甲氧基苯酚溶液、7.6重量%氢氧化钠溶液和33.1重量%软化水构成的混合物。在3小时内计量加入所述单体混合物,在4.5小时内计量加入过硫酸钠,并在2.75小时内计量加入亚硫酸氢钠。在所述单体加料结束后,在内部温度90°C下于1.5小时内添加132.0g50重量%氢氧化钠水溶液。此后,在90°C下再继续聚合1小时。随后,添加50.0g软化水以将所述聚合物溶液冷却至室温。测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
实施例8
首先在配备有搅拌器、温度计、pH电极和数个进料装置的玻璃反应器中装入30g去离子水、59g烯丙基磺酸钠水溶液(35重量%烯丙基磺酸钠)和0.01g七水硫酸铁(II),将其调节至20°C的聚合引发温度(初始进料)。在独立的进料容器中,将72g丙烯酸与72g去离子水均匀混合(溶液A)。在另一独立的进料容器中,将式10.5g式CH2=C(CH3)CH2CH2-(EO11.3)-H的异戊烯醇聚乙二醇与10.5g去离子水均匀混合(溶液B)。混合后,将0.75g2-巯基乙醇添加至溶液B中。平行制备处于45g水中的5g羟甲基亚磺酸钠(获自Brüggemann GmbH的Brüggolit SFS)的第三溶液。
在制备溶液A、B和C后,将6g过氧化氢(30重量%,于水中)添加至所述初始进料混合物中。同时,开始将溶液A、溶液B和溶液C添加至所述搅拌的初始进料中。
溶液A以144g/h的添加速率经60分钟添加。
溶液B以21.75g/h的添加速率经所述60分钟平行添加。
溶液C以10g/h的添加速率经所述60分钟平行添加。随后,将溶液C的添加速率提高至50g/h并在搅拌下经10分钟将其泵入所述初始进料混合物中。在溶液A、B和C添加结束后,所述反应容器中没有发现过氧化物。
随后,用约2.8g50重量%氢氧化钠溶液将所得聚合物溶液调节至pH2.6。
以固含量为37.0%的无色溶液获得了所得共聚物。所述共聚物的平均分子量Mw为18000g/mol。
测定pH和K值、分子量Mn和Mw以及固含量,并视觉评估产物混合物。
所述聚合物的组成示于表1中。
表1
实施例 | 共聚物的单体组成 | 单体比例[重量%] |
C1 | AS/MAS/SEMA/MPEGMA(1000) | 28.3:31.0:29.2:11.6 |
C2 | AS/MAS/VS/MPEGMA(1000) | 28.3:31.0:29.2:11.6 |
1 | AS/AMPS/CH2=CHCH2O-(EO4.1)(EO12.3PO5.5)-H | 40:30:30 |
2 | AS/AMPS/CH2=CHCH2O-(EO4.1)(EO12.3PO5.5)-H | 60:20:20 |
3 | AS/AMPS/CH2=CHCH2O-(EO4.1)(EO12.3PO5.5)-H | 80:10:10 |
4 | AS/AMPS/CH2=CHCH2O-(EO4.1)(EO12.3PO5.5)-H | 60:10:30 |
5 | AS/AMPS/CH2=CHCH2O-(EO16)-H | 60:30:10 |
6 | AS/AMPS/CH2=CHCH2O-(EO7.7PO3.0)-H | 60:30:10 |
7 | AS/AMPS/CH2=CHCH2O-(EO6.0)(EO5.1PO3.6)-H | 60:30:10 |
8 | AS/IPEG500/ALS | 60:20:20 |
AS=丙烯酸
MAS=甲基丙烯酸
AMPS=2-丙烯酰胺基-2-甲基丙磺酸
IPEG500=平均具有11.3个氧化乙烯单元的异戊烯醇聚乙二醇
所述聚合物的分析数据示于表2中。
表2:实施例的分析数据
a)ISO3251(0.25g,150°C,2h)
b)通过Fikentscher法使用1%软化水溶液测定
c)通过凝胶渗透色谱法测定
在下述不含磷酸盐的配制剂PF1和PF2以及磷酸盐基配制剂P1中对所述聚合物进行测试。所述测试配制剂的组成示于表3中(数据以重量%计)
表3
PF1 | PF2 | P1 | |
蛋白酶 | 1 | 2 | 2 |
淀粉酶 | 0.2 | 0.5 | 0.5 |
表面活性剂 | 5 | 5 | 4.5 |
聚合物 | 10 | 14 | 6.5 |
过碳酸钠 | 10.5 | 12.5 | 12.5 |
四乙酰基乙二胺 | 4 | 4 | 4 |
二硅酸钠 | 2 | 5 | 4 |
三聚磷酸钠 | 40 | ||
重苏打 | 18.8 | 25 | 25 |
二水柠檬酸钠 | 33 | 25 | |
柠檬酸 | 5 | ||
甲基甘氨酸二乙酸 | 15 | 0 | |
羟基乙烷-(11-二膦酸) | 0.5 | 2 | 1 |
观察到如下测试条件:
洗碗机:Miele G1222SCL
程序:65°C(具有预洗)
器皿:3把刀(WMF Berlin餐刀,整体)3个Amsterdam饮用玻璃杯,0.2L3块“OCEAN BLAU”早餐台(蜜胺)3块瓷板:平边板,19cm
排列:刀位于餐具抽屉中,玻璃位于上部篮子中,板归类于下部篮子中
洗碗机洗涤剂:21g
添加污垢:预洗后将50g熔融基础污物(Ballastschmutze)与配制剂一起计量加入,参见下文组合物
漂洗温度:65°C
水硬度:21°dH(Ca/Mg):HCO3(3:1):1.35
漂洗周期:15;每个周期之间暂停1小时(开门10分钟,关门50分钟)
评估:15个漂洗周期后视觉评估
在15个周期后,于暗室中在光下于孔板后使用10(非常好)至1(非常差)评分标准对所述器皿进行评估。对斑点(非常多的密集斑点=1至没有斑点=10)和污垢(1=非常高的污垢,10=没有污垢)给予1-10的评分。
基础污物组成:
淀粉:0.5%马铃薯淀粉,2.5%肉汁
脂肪:10.2%人造奶油
蛋白质:5.1%蛋黄,5.1%牛奶
其他:2.5%番茄酱,2.5%芥末,0.1%苯甲酸,71.4%水
结果:
与对照实施例相比,本发明共聚物尤其在玻璃和刀上显示出改善的效果。
下表列出了对刀和饮用玻璃杯上的污垢形成和斑点所给的评分。
不含磷酸盐的配制剂PF1
聚合物 | 刀(S+B) | 玻璃(S+B) | 总计(最大值40) |
C1 | 12 | 12 | 24 |
C2 | 11 | 11 | 22 |
2 | 14 | 15 | 29 |
3 | 16 | 16 | 32 |
4 | 16 | 11 | 27 |
5 | 14 | 16 | 30 |
6 | 12 | 14 | 26 |
7 | 13 | 14 | 27 |
8 | 14 | 14 | 28 |
S=斑点
B=污垢
含磷酸盐的配制剂P1
聚合物 | 刀(S+B) | 玻璃(S+B) | 总计(最大值40) |
C1 | 19 | 12 | 31 |
C2 | 18 | 13 | 31 |
1 | 18 | 15 | 33 |
2 | 19 | 13 | 32 |
也在配制剂PF2中对本发明聚合物进行了测试。在使用配制剂PF2下,本发明共聚物也优于对照聚合物。
Claims (19)
1.一种用于机器洗碗的洗涤剂配制剂,其包含如下物质作为组分:
a)1-20重量%至少一种共聚物,其包含呈共聚形式的如下物质:
a1)30-90重量%至少一种选自丙烯酸、甲基丙烯酸及其盐的单体;
a2)3-60重量%至少一种含磺基的单体,其选自烯丙基磺酸和2-丙烯酰胺基-2-甲基丙磺酸;
a3)3-60重量%至少一种式(I)的非离子单体:
H2C=C(R1)(CH2)xO[R2-O]o-R3 (I)
其中R1为氢或甲基,R2相同或不同且为呈嵌段或无规排列的直链或支化C2-C6亚烷基,R3为氢或直链或支化C1-C4烷基,x为0、1或2且o为>5至50的自然数;
a4)0-30重量%一种或多种可与a1)、a2)和a3)聚合的其他烯属不饱和单体;
其中a1)、a2)、a3)和a4)之和总计为100重量%;
b)0-20重量%不同于组分a)的聚羧酸盐;
c)0-50重量%络合剂;
d)0-70重量%磷酸盐;
e)0-60重量%其他助洗剂和共助洗剂;
f)0.1-20重量%非离子表面活性剂;
g)0-30重量%漂白剂和任选的漂白活化剂和漂白催化剂;
h)0-8重量%酶;
i)0-50重量%一种或多种其他添加剂;
其中组分a)至i)之和总计为100重量%。
2.根据权利要求1的洗涤剂配制剂,其中式(I)中的x为1。
3.根据权利要求2的洗涤剂配制剂,其中式(I)中的R1为H。
4.根据权利要求1的洗涤剂配制剂,其中式(I)中的x为2。
5.根据权利要求4的洗涤剂配制剂,其中式(I)中的R1为甲基。
6.根据权利要求1的洗涤剂配制剂,其中式(I)的非离子单体包含嵌段和/或无规共聚的氧化乙烯和/或氧化丙烯。
7.根据权利要求1的洗涤剂配制剂,其中式(I)的非离子单体包含呈共聚形式的平均为8-40个的氧化烯单元。
8.根据权利要求1的洗涤剂配制剂,其中共聚物a)包含40-90重量%单体a1)、4-40重量%单体a2)和4-40重量%单体a3)。
9.根据权利要求8的洗涤剂配制剂,其中共聚物a)包含45-85重量%单体a1)、6-35重量%单体a2)和6-35重量%单体a3)。
10.根据权利要求1的洗涤剂配制剂,其中所述其他添加剂选自阴离子或两性离子表面活性剂、碱性载体、腐蚀抑制剂、消泡剂、染料、香料、填料、有机溶剂、成片助剂、崩解剂、增稠剂、加溶剂和水。
11.根据权利要求1-10中任一项所定义的共聚物a)作为机器洗碗用的不含磷酸盐或含磷酸盐的洗涤剂配制剂中的阻垢添加剂的用途。
12.一种共聚物,其包含呈共聚形式的如下物质:
a1)30-90重量%至少一种选自丙烯酸、甲基丙烯酸及其盐的单体;
a2)3-60重量%至少一种含磺基的单体,其选自烯丙基磺酸和2-丙烯酰胺基-2-甲基丙磺酸;
a3)3-60重量%至少一种式(I)的非离子单体:
H2C=C(R1)(CH2)xO[R2-O]o-R3 (I)
其中R1为氢或甲基,R2相同或不同且为呈嵌段或无规排列的直链或支化C2-C6亚烷基,R3为氢或直链或支化C1-C4烷基,x为0、1或2且o为>5至50的自然数;其中式(I)的非离子单体包含嵌段和/或无规共聚的氧化乙烯和/或氧化丙烯;
a4)0-30重量%一种或多种可与a1)、a2)和a3)聚合的其他烯属不饱和单体;其中a1)、a2)、a3)和a4)之和总计为100重量%。
13.根据权利要求12的共聚物,其中式(I)中的o>5。
14.根据权利要求12的共聚物,其中式(I)的非离子单体包含呈共聚形式的平均为8-40个的氧化烯单元。
15.根据权利要求12-14中任一项的共聚物作为机器洗碗用的不含磷酸盐或含磷酸盐的洗涤剂配制剂中的阻垢添加剂的用途。
16.一种共聚物,其包含呈共聚形式的如下物质:
a1)30-90重量%至少一种选自丙烯酸、甲基丙烯酸及其盐的单体;
a2)3-60重量%至少一种含磺基的单体,其选自烯丙基磺酸和2-丙烯酰胺基-2-甲基丙磺酸;
a3)3-60重量%至少一种式(I)的非离子单体:
H2C=C(R1)(CH2)xO[R2-O]o-R3 (I)
其中R1为氢或甲基,R2相同或不同且为呈嵌段或无规排列的直链或支化C2-C6亚烷基,R3为氢或直链或支化C1-C4烷基,x为2且o为3-50的自然数;
a4)0-30重量%一种或多种可与a1)、a2)和a3)聚合的其他烯属不饱和单体;其中a1)、a2)、a3)和a4)之和总计为100重量%。
17.根据权利要求16的共聚物,其中式(I)中的o>5。
18.根据权利要求16的共聚物,其中式(I)中的R1为甲基。
19.根据权利要求16-18中任一项的共聚物作为机器洗碗用的不含磷酸盐或含磷酸盐的洗涤剂配制剂中的阻垢添加剂的用途。
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CN1190408A (zh) * | 1995-05-12 | 1998-08-12 | 施托克豪森公司 | 水溶性共聚物及其生产方法和应用 |
EP0798320A2 (en) * | 1996-03-26 | 1997-10-01 | Nof Corporation | Ternary copolymer |
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MX2013005750A (es) | 2013-08-01 |
CN103459442A (zh) | 2013-12-18 |
BR112013012623B1 (pt) | 2020-06-16 |
WO2012069365A1 (de) | 2012-05-31 |
PL2643370T3 (pl) | 2019-12-31 |
MX366238B (es) | 2019-07-03 |
JP2014500903A (ja) | 2014-01-16 |
BR112013012623A2 (pt) | 2017-03-28 |
EP2643370B1 (de) | 2019-07-03 |
CA2817174A1 (en) | 2012-05-31 |
JP5952825B2 (ja) | 2016-07-13 |
CA2817174C (en) | 2019-01-15 |
RU2013128414A (ru) | 2015-01-10 |
ES2746919T3 (es) | 2020-03-09 |
KR20140001219A (ko) | 2014-01-06 |
KR101859789B1 (ko) | 2018-05-18 |
EP2643370A1 (de) | 2013-10-02 |
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