CN100557121C - 分散剂混合物 - Google Patents

分散剂混合物 Download PDF

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CN100557121C
CN100557121C CNB2004800364977A CN200480036497A CN100557121C CN 100557121 C CN100557121 C CN 100557121C CN B2004800364977 A CNB2004800364977 A CN B2004800364977A CN 200480036497 A CN200480036497 A CN 200480036497A CN 100557121 C CN100557121 C CN 100557121C
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CN1890427A (zh
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B·S·老贝利
B·O·格里芬
B·W·莱昂斯
M·韦伯
B·萨雷托
H·施林曼
G·马勒
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BASF Schweiz AG
Ciba SC Holding AG
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Abstract

本发明涉及一种至少两种不同分散剂的混合物，含有选自苯并三唑、苯并三嗪和二苯酮的紫外线吸收剂和至少两种不同的分散剂的混合物的水分散体，以及用于在静电染色工艺中降低压差的方法。

Description

分散剂混合物
本发明涉及一种至少两种不同分散剂的混合物，含有选自苯并三唑、苯并三嗪和二苯酮的紫外线吸收剂(UVA)和至少两种不同的分散剂的混合物的水分散体，以及用于在静电染色工艺中降低压差的方法。
在静电染色中，压差经常由紫外线吸收剂制剂、某些染料或染液的其它组分的掺杂引起。这些含苯并三唑、取代的苯并三唑、苯并三嗪或二苯酮作为活性剂的制剂，用于保护纺织物免受紫外线的破坏。
它们经常与分散染料联合使用。在很多情况下，在用于静电染色设备时，这种染浴组合造成额外的压差，所述的静电染色设备包括但不限于package-染色机、散纤染色机、经轴染色机等。
压差是染色机泵在正常循环条件下，在加入染料和化学试剂之前产生的压力与将染料和化学试剂加入染色机后产生的压力相比之间的差。
当染料和化学试剂转移进入纤维本身时，染浴温度的升高导致压差增加，直到达到尽染温度。压力的增加导致了不均匀的循环，使得染料和化学试剂不规则地沉淀到整个被染物，导致不合格的或不均匀的染色。当纤维的纤细度增加时，和/或在要被染色的底布密度增加时，该间题变得更加严重。对于这种条件，已知一些染料和化学试剂是有麻烦的，其包括但不限于分散染料、苯并三唑紫外线吸收剂、取代的苯并三唑紫外线吸收剂、苯并三嗪紫外线吸收剂、一些二苯酮紫外线吸收剂，以及某些类型的通常用于合成纤维的分散剂和染料或化学试剂。
目前已出乎意料地发现，当至少两种不同的分散剂的特殊混合物与苯并三唑、苯并三嗪和二苯酮类紫外线吸收剂一起使用时，所述的压差可以显著降低乃至消除的。
因此，本发明涉及一种组合物，包括
(A)75-95重量％的式(1)化合物
Figure C20048003649700061
其中R1、R2、R3和R4彼此独立地表示氢、C1-C12烷基、C5-C24-芳基或C6-C36芳烷基、Y表示亚乙基或亚丙基，n是4-50的数，X表示氢、C1-C12烷基、无机含氧酸的酸基或有机酸的酸基，和
(B)5-25重量％的由芳基磺酸和甲醛制备的甲醛缩合产物，组分(A)+(B)的总量为100重量％。
如上所述的组分(A)和(B)在织物染色领域是公知的分散剂和/或表面活性剂。
C1-C12烷基作为R1至R4和X包括例如甲基、乙基、丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、戊基、特戊基(1，1-二甲丙基)、正戊基、新戊基和正己基。
C5-C24芳基的例子是苯基、甲苯基、2，4，6-三甲苯基、isityl、二甲苯基、萘基、蒽基和菲基。
作为R1的C6-C36芳烷基包括例如苄基、2-苯基乙基、二苯基甲基、萘基甲基和2-萘基乙基。
酸基X例如衍生自低分子量二羧酸，例如马来酸、琥珀酸或磺基琥珀酸，并且通过酯桥连接到分子的亚烷基氧基部分。然而，优选X衍生自无机多元酸，如硫酸，特别是正磷酸。酸基X可以游离酸或盐的形式存在，即，例如作为碱金属盐、碱土金属盐、铵盐或胺盐。这类盐的例子是锂、钠、钾、镁、钙、钡、铵、三甲基胺、二乙基胺、乙醇胺、二乙醇胺和三乙醇胺的盐。单和二乙醇胺的盐可另外被1-25个亚乙基氧基单元醚化。
根据本发明的组合物优选含有作为成分(A)的式(1)化合物，其中R1是C4-C12烷基、苯基、甲苯基、苯基-C1-C3烷基或甲苯基-C1-C3烷基，R2和R3彼此独立地是氢、C4-C12烷基、苯基、甲苯基、苯基-C1-C3烷基或甲苯基-C1-C3烷基，R4是氢、X是衍生自硫酸或正磷酸的酸基，Y表示亚乙基，n是4-40的数。
作为成分(A)特别优选式(1)化合物，其中R1是1-苯乙基、R2和R3彼此独立地是氢或1-苯基乙基，R4是氢，Y表示亚乙基，n是12-30的数。
非常特别优选一种混合物的乙醇胺、二乙醇胺、三乙醇胺、铵、钾或钠盐，所述的混合物是12-18摩尔的环氧乙烷与1到3摩尔的苯乙烯和1摩尔苯酚的加合物的聚加合物的磷酸单酯和二酯的混合物。
例如在美国专利No.5,009,669中描述了式(1)化合物。
在美国专利No.5,009,669中还描述了合适的组分(B)。
优选组分(B)是甲醛与磺化的萘(sulfonated naphthalene)、C1-C4烷基萘、联苯、二苯醚、二甲苯醚、苯酚、甲苯、二甲苯或1，3，5-三甲基苯的缩合产物。
特别优选甲醛与磺化的二甲苯醚的缩合产物和甲醛与磺化的二(2-萘基)甲烷的缩合产物。
在另一个优选的实施方案中，根据本发明的组合物还含有(C)0.1到10重量％的、2-80摩尔烯化氧与8到22个碳原子的不饱和或饱和一元醇、脂肪酸、脂肪族胺或脂肪酰胺的聚加合物；组分(A)+(B)+(C)的总量为100重量％。
成分(C)优选是3-30摩尔的环氧乙烷或环氧丙烷与1摩尔1224个碳原子的脂肪醇的聚加合物。
作为成分(C)尤其优选20-30摩尔的环氧乙烷与1摩尔硬脂醇的聚加合物。
组分(A)、(B)和(C)的相对量可以在宽范围内变化。
优选根据本发明的组合物含有76-84重量％、特别是77-82重量％的成分(A)，14-22重量％、特别是16-21重量％的成分(B)和2-6重量％、特别是3-5重量％的成分(C)。
如上所述，根据本发明的分散剂混合物可有利地与苯并三唑、苯并三嗪或二苯酮紫外线吸收剂一起使用，这些紫外线吸收剂往往在静电染色工艺中导致压差。
因此，本发明的另一个目的是一种水分散体，含以总的组合物为基础计5-40重量％的选自苯并三唑、苯并三嗪和二苯酮的紫外线吸收剂和以总的组合物为基础计5-30重量％的上述分散剂组合物。
优选，根据本发明的水分散体含有式(2)的苯并三唑化合物紫外线吸收剂，
其中R1是卤素、C1-C12烷基或C1-C12烷氧基和R2和R3彼此独立地是氢、卤素、C1-C12烷基或C1-C12烷氧基。
合适的式(2)化合物例如是在美国专利No.5,009,669中描述的。
式(2a)的化合物是特别优选的，
Figure C20048003649700082
除了紫外线吸收剂和分散剂混合物以外，根据本发明的水分散体有利地另外含有以总的组合物为基础计1-10重量％的稳定剂或增稠剂。
这类添加剂用来调节分散体系的粘度。
合适稳定剂或增稠剂尤其是含羧基的聚合物。
基于溶液或分散体，这些以0.5-10％水溶液或分散体的形式使用。
这些聚合物有利地是3-5个碳原子的烯基不饱和单羧酸或二羧酸聚合物，例如聚丙烯酸或甲基丙烯酸、巴豆酸、衣康酸、芸康酸、马来酸、富马酸、柠康酸或甲基富马酸的聚合物；烯烃共聚物，例如乙烯或丙烯、双烯酮、丙烯酸酯、异丁烯酸酯或丙烯酰胺和上述的单体(包括丙烯酸)的共聚物；或丙烯酸与甲基丙烯酸、甲基丙烯腈或乙烯基单体(例如乙烯基膦酸)的共聚物；马来酸和苯乙烯、马来酸和乙烯基酯(例如醋酸乙烯酯)的共聚物。
增稠的含羧基聚合物可具有0.5-6百万的分子量。
其它的增稠剂是多糖，例如羧甲基纤维素、甲基纤维素、甲基羟基乙基纤维素、槐豆氟醚(locust bean fluor ether)、淀粉醚、藻酸盐、聚乙二醇、聚乙烯吡咯烷酮、聚乙烯醇或细分散的二氧化硅(优选具有50-380平方米/克的比表面积)，以及层状硅酸盐，例如膨润土、有机皂土、蒙脱石和蒙脱土。
特别有用的增稠剂是丙烯酸聚合物。如聚丙烯酸和丙烯酸和丙烯酰胺的共聚物，其中相应的分子量可以在0.5-6百万范围内变化。
另一种特别有用的增稠剂是由单糖葡萄糖和甘露糖和葡糖醛酸形成的杂多糖，例如，黄原胶。
根据本发明的水分散体可含有其它常用辅料，包括例如其它阴离子的或非离子的分散剂或表面活性剂、多价螯合剂、渗透促进剂、抗冻剂、消泡剂、防腐剂和杀菌剂。
根据本发明的分散体有利地通过在搅拌机中将紫外线吸收剂、分散剂混合物和水打浆，然后加入任何需要的其它组分，例如多价螯合剂、抗冻剂、消泡剂、防腐剂和杀菌剂，分散1-30小时，优选1-10小时。所述的分散有利地通过高剪切力的作用完成，例如通过在球磨机、砂磨机或玻璃珠研磨机中研磨。研磨后，可加入稳定剂或增稠剂的水溶液，如果需要可再加入水，然后搅拌直至均匀地分散。
根据本发明的分散体以优秀的运输和储藏稳定性著称。当用于染液时，其尤其在直到130摄氏度的高温都非常稳定。
根据本发明的分散体的使用取决于在含合成纤维、特别是聚酯纤维的纺织品染色中的染料。染色法以常规的方式进行。根据本发明的分散体缓慢地加入到搅拌的含水浴中，加入染料，然后溶液准备用于染色。
本发明因此还提供一种用于纺织品染色的方法，其包括在含有紫外线吸收剂和如上所述分散剂组合物的水分散体存在下将材料染色。
根据本发明的助剂分散体加入到染液中的量，基于纤维的重量，在0.5-10重量％范围内变化，优选1-5重量％。
可在新的光稳定剂助剂混合物存在下染色的所述纤维材料，特别是纺织品包括例如纤维素酯纤维、芳族聚酰胺纤维和聚酯纤维。
染色有利地通过吸尽法在水性液体中进行。
因此液比可以在宽范围内选择，例如1∶3到1∶100，优选1∶7到1∶50。进行染色或增白的温度优选至少70摄氏度，通常不高于140摄氏度。优选在80-135摄氏度范围内。
优选含染料、助剂混合物和任何其它添加剂并已经调节到pH4.5-5.5的染浴在60-80摄氏度循环通过纤维材料5分钟，然后在15到35分钟内将温度提高至110-135摄氏度，染色液保持在该温度15到90分钟。
通过将染色液冷却到60-80摄氏度，用水漂洗染色，然后，如果必要，在碱性介质中以常规方式还原固定染色，完成染色。然后再一次漂洗染色并且干燥。这在合成纤维材料、特别是线型聚酯纤维上产生了深且均匀的染色，此外，所述的染色以优秀的耐光性和耐磨度著称。
往往与紫外线吸收剂和某些染料有关的在静电染色设备中的压差被根据本发明的特殊分散体显著降低了。
因此，本发明还涉及一种通过使用分散染料和含紫外线吸收剂和如上所述分散剂组合物的水分散体降低静电染色工艺中压差的方法。
以下实施例用来举例说明本发明；份数和百分数基于重量，除非另有说明。
实施例1
水分散体F1通过混合下述组分制备：
54.22g软化水
12.5g 2-(2’-羟基-3’-叔丁基-5’-甲基苯基)-5-氯苯并三唑
2g磺化的二甲苯基醚甲醛缩合物(B1)
0.5g C16-18烷基醇和25mole环氧乙烷的加成物
4.0g另外的市场上可买到的分散剂
1.0g市场上可买到的消泡剂
混合物在砂磨机或玻珠研磨机中研磨直至颗粒尺寸小于2.5μm。在分离了砂或玻璃珠后，加入
0.4g黄原胶基的增稠剂，
0.38g市场上可买到的杀真菌剂(Proxel GXL)，
25.0g软化水。
得到的分散体具有250mPas的粘度和优良的储藏稳定性。
实施例2
水分散体F2通过混合以下组分制备：
54.22g软化水
12.5g 2-(2’-羟基-3’-叔丁基-5’-甲基苯基)-5-氯苯并三唑
7.7g三(1-苯乙基)苯酚和16摩尔的环氧乙烷的加成物
2.1g磺化的二甲苯基醚甲醛缩合物
0.7g C16-18基醇和25mole环氧乙烷的加成物
1.0g市场上可买到的消泡剂
混合物在砂磨机或玻珠研磨机中研磨直至颗粒尺寸小于2.5μm。在分离了砂或玻璃珠后，加入
0.4g黄原胶基的增稠剂，
0.38g市场上可买到的杀真菌剂(Proxel GXL)，
25.0g软化水。
得到的分散体具有250mPas的粘度和优良的储藏稳定性。
实施例3
水分散体F3通过混合以下组分制备：
54.22g软化水
12.5g 2-(2′-羟基-3′-叔丁基-5′-甲基苯基)-5-氯苯并三唑
7.7g三(1-苯乙基)苯酚和16摩尔的环氧乙烷的加成物
2.1g磺化烷基萘甲醛缩合物(B2)
0.7g C16-18烷基醇和25mole环氧乙烷的加成物
1.0g市场上可买到的消泡剂
混合物在砂磨机或玻珠研磨机中研磨直至颗粒尺寸小于2.5μm。在分离了砂或玻璃珠后，加入
0.4g黄原胶基的增稠剂，
0.38g市场上可买到的杀真菌剂(Proxel GXL)，
25.0g软化水。
得到的分散体具有200mPas的粘度和优良的储藏稳定性。
实施例4
水分散体F4通过混合以下组分制备：
3g的根据实施例1制备的分散体和
1.2g分散剂组合物，分散剂钮合物含77重量％的三(1-苯乙基)苯酚和16摩尔的环氧乙烷的加成物、21重量％磺化二甲苯基醚甲醛缩合物和2重量％C16-18烷基醇和25mole环氧乙烷的加成物。
得到稳定的分散体。
实施例5
水分散体F5通过混合以下组分制备：
3g的根据实施例1制备的分散体和
1.2g分散剂组合物，分散剂组合物含77重量％的三(1-苯乙基)苯酚和16摩尔的环氧乙烷的加成物、21重量％磺化烷基萘甲醛缩合物和2重量％C16-18烷基醇和25mole环氧乙烷的加成物。
得到的分散体稳定。
实施例6
通过在配备压差和流率测量装置的循环染色装置中处理一个40g聚酯细纱纺锤测试上述分散体F1-F5的关于降低压差的性能。
测试参数为：
-泵的输出量：0.5l/min
-泵方向：内部-外部
-pH值：4.5-5.0；用乙酸调节
-温度：60摄氏度-130摄氏度，2-4摄氏度/分钟；在130摄氏度10分钟；冷却。观察到的最大压差峰值列于下表1中：
  ％UV   ％A   ％B   ％C   另外的分散剂   ΔP[巴]
  F1   12.5   -   2   0.5   4   1.4
  F2   12.5   7.7   2.1(B1)   0.7   -   0.32
  F3   12.5   7.7   2.1(B2)   0.7   -   0.28
  F4   9   21.9   6.0(B1)   0.6   -   0.11
  F5   9   21.9   6.0(B2)   0.6   -   0.13

Claims (16)

1.一种用于在静电染色工艺中降低压差的组合物，含有(A)75-95重量％的式(1)化合物
Figure C2004800364970002C1
其中R1、R2、R3和R4彼此独立地表示氢、C1-C12烷基、C5-C24-芳基或C6-C36芳烷基，Y表示亚乙基或亚丙基，n是4-50的数，和X表示氢、C1-C12烷基，无机含氧酸的酸基或有机酸的酸基，和
(B)5-25重量％由芳族磺酸和甲醛制备的甲醛缩合产物，组分(A)+(B)的总量为100重量％。
2.根据权利要求1的组合物，含作为成分(A)的式(1)化合物，
其中
R1是C4-C12烷基、苯基、甲苯基、苯基-C1-C3烷基或甲苯基-C1-C3烷基，R2和R3彼此独立地是氢、C4-C12烷基、苯基、甲苯基、苯基-C1-C3烷基或甲苯基-C1-C3烷基，
R4是氢，
X是衍生自硫酸或正磷酸的酸基，
Y表示亚乙基和
n是4-40的数。
3.根据权利要求1的组合物，含有式(1)化合物作为成分(A)，其中R1是1-苯基乙基，R2和R3彼此独立地是氢或1-苯基乙基，R4是氢，Y表示亚乙基，和n是12-30的数。
4.根据权利要求1的组合物，含作为成分(B)的甲醛与磺化的萘、C1-C4烷基萘、联苯、二苯醚、二甲苯基醚、苯酚、甲苯、二甲苯或1，3，5-三甲基苯的缩合产物。
5.根据权利要求1的组合物，含作为成分(B)的甲醛与磺化的二甲苯基醚的缩合产物或甲醛与磺化的二(2-萘基)甲烷的缩合产物。
6.根据权利要求1的组合物，还含有
(C)0.1到10重量％的、2-80摩尔烯化氧与8到22个碳原子的不饱和或饱和一元醇、脂肪酸、脂肪族胺或脂肪酰胺的聚加合物；
组分(A)+(B)+(C)的总量为100重量％。
7.根据权利要求6的组合物，含作为成分(C)的3-30摩尔的环氧乙烷或环氧丙烷与1摩尔12-24个碳原子的脂肪醇的聚加合物。
8.根据权利要求6的组合物，含作为成分(C)的20-30摩尔的环氧乙烷与1摩尔的硬脂醇的聚加合物。
9.根据权利要求6的组合物，含76-84重量％的成分(A)、14-22重量％的成分(B)和2-6重量％的成分(C)。
10.一种用于在静电染色工艺中降低压差的水分散体，含基于总的组合物5-40重量％的选自苯并三唑、苯并三嗪和二苯酮的紫外线吸收剂和基于总的组合物计5-30重量％的根据权利要求1的组合物。
11.根据权利要求10的水分散体，含作为紫外线吸收剂的式(2)苯并三唑化合物，
Figure C2004800364970003C1
其中R1是卤素、C1-C12烷基或C1-C12烷氧基和R2和R3彼此独立地是氢、卤素、C1-C12烷基或C1-C12烷氧基。
12.根据权利要求10的水分散体，含作为紫外线吸收剂的式(2a)苯并三唑化合物
Figure C2004800364970003C2
13.根据权利要求10的水分散体，另外含以总的组合物计1-10重量％的稳定剂或增稠剂。
14.根据权利要求13的水分散体，含由单糖葡萄糖和甘露糖和葡糖醛酸形成的杂多糖作为增稠剂。
15.用于纺织品染色的方法，其包括在根据权利要求10的水分散体存在下将所述材料染色。
16.在静电染色工艺中降低压差的方法，通过使用分散染料和根据权利要求10的水分散体。
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