CN103966855A - 用于纤维材料的防油和/或防水整理的组合物 - Google Patents
用于纤维材料的防油和/或防水整理的组合物 Download PDFInfo
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Abstract
本发明公开了用于纤维材料的防油和/或防水整理的组合物。本发明描述了可用于处理纺织材料以给予其防油和/或防水性质的8种含水组合物。所述组合物尤其含有包含全氟烷基(RF基团)的聚合物，其中55-100％的RF基团含有6个碳原子。
Description
本申请是以下申请的分案申请：申请日2010年9月22日，申请号201080043192.4，发明名称“用于纤维材料的防油和/或防水整理的组合物”。
技术领域
本发明涉及含水组合物，其对处理由纤维材料组成的纺织织物(比如，例如，织造物、针织物或者纤维非织造网(非织造物))非常有用。本发明更进一步涉及用于处理织物的方法。
背景技术
已知用含有具有结构CF3-(CF2)x-CF2-的全氟烷基(RF基团)的聚合物处理由纤维材料组成的纺织织物。当所述式中x为6或以上，即当RF基团含有8个或更多个碳原子时，这些RF基团为它们惯常的链长度。这样的聚合物可用来给予纤维材料防油和/或防水性质。在现有技术的组合物中，含有RF基团的聚合物常具体化为含有以下结构单元的聚(甲基)丙烯酸酯：
这样的聚合物作为用于纺织材料的防油/防水整理(finishing)的制剂的成分特别有用。
含有RF基团的聚丙烯酸酯用于处理纺织品的用途从EP314 944 A2显而易见。类似地，WO03/14180A1描述了用含有RF基团的聚合物处理纤维材料。
用含有RF基团的聚合物处理纺织材料也由EP1 632 542A1已知。
从生态上讲，期望使用RF基团较短的链长度，即RF链中少于8个碳原子。然而，测试已显示较短的链长度导致较差的防油/防水值(参见"Macromolecules2005，38，5699-5705"Takahara等人)。
EP1493 761A1描述了组合物，其中聚合物的RF基团的链长度总计3或4个碳原子。根据该参考文献，织物整理中可获得的防油值和防水值与使用RF基团链长度为8个碳原子的含氟聚合物时得到的值大致在相同的水平。然而，不管生态上的优势，用该EP的组合物获得的防油和防水效果并非完全令人满意。
WO2008/022985A1的组合物同样描述了含有全氟烷基的聚合物，其中RF基团含有不到8个碳原子。此处牵涉具体的聚合物，其制备使用可热交联的或者反应性异氰酸酯作为单体构造单元。类似地，该参考文献的组合物未能提供对整理的纺织品最佳的防油和/或防水性质。
发明内容
本发明的目的是提供一种组合物，其提供相对于已知组合物的生态学及成本优势，其中含有全氟烷基的所述聚合物的RF基团包含8个或更多个碳原子，且提供至少这些已知组合物的效果水平(就涉及整理的纺织材料的防油和防水性质而言)。
我们发现这个目的通过至少含有组分A，B和C的含水组合物实现，其中
组分A是至少含有组分A1-A3的混合物，其中
组分A1是石蜡，
组分A2是具有12-22个碳原子的醇，醚化的(优选季铵化的)多羟甲基三聚氰胺以及任选另外的多官能乙醇胺的缩合产物，该缩合产物可含有按重量计0.05％-1.5％的酸，优选为乙酸，
组分A3是水，
或者其中
组分A是至少含有组分A4-A6的混合物，其中
组分A4是聚硅氧烷，所述聚硅氧烷除连接于硅原子的烷基外，另外含有连接于硅原子的氢原子，即烷基-氢-聚硅氧烷，
组分A5是水而且
组分A6是分散剂，优选为乙氧基化醇或者乙氧基化醇的混合物，其中优选使用具有8-20个碳原子的乙氧基化直链或支化的醇，
其中组分B是至少含有组分B1-B3的混合物，其中组分B1是含有异氰酸酯基团的聚氨酯，且其异氰酸酯基团是被封端的，优选用脂肪族酮肟封端，其中所述聚氨酯优选由芳香族或者脂肪族(优选芳香族)二异氰酸酯构成，其中该二异氰酸酯优选与具有2-6个碳原子的二醇、三羟基(trivlanet)脂肪醇和N-烷基化二乙醇胺或者三乙醇胺反应，
其中组分B2是分散剂或者分散剂混合物并且含有乙氧基化醇与任选的二羟基脂肪醇及任选的无机酸，
其中组分B3是水，
其中组分C是含有全氟烷基(RF基团)的聚合物，其中55-100％的所有存在的RF基团含有6个碳原子，
其中
该组合物任选还含有作为组分D的锆盐，优选为乙酸锆。
具体实施方式
一般说来缩短RF基团的链长度时观察到由纤维处理制剂给予的防油和防水效果变差。这种不期望的变差可以在某种程度上通过将含有RF基团的聚合物的组合物与称为增量剂的其它产品混合来补偿。用这种方法，EP1 493 761A1的组合物近似获得RF基团中8个碳原子的链长度产生的效果水平，虽然该EP的组合物中链长度仅等于3或者4个碳原子。另一方面，较短的链长度相对于C8提供生态上的优势。
所提到的发现似乎暗示本发明的组合物将对整理的纺织品产生与使用一方面3或4个碳原子和另一方面8个碳原子的链长度的结果在大致相同水平的防油和防水效果。出人意料地，情况不是这样。这是因为发现(对于本领域专业人员而言相当意外)，和使用含有RF基团的聚合物(其中RF基团中碳原子的平均数为3-4，或者8)相比，根据本发明的组合物对整理的纺织材料提供明显改善的防油和/或防水性质。这适用于相同的纤维附加物(add-on)，因此和已知制剂的情况相比，纺织品上较低(lower)的产品附加物和根据本发明的组合物一起使用，以便可实现相同的效果水平。可以理解，这带来成本优势。
本发明的组合物的决定性的一点是RF基团的链长度。链长度分布的最大值应该处于6个碳原子，即所有存在的RF基团数的55-100％，优选70-100％必须具有6个碳原子。当所有存在的RF基团100％含有6个碳原子时得到特别良好的结果。然而，一些RF基团(即0-45％)可具有不同于6的链长度。但是，当约100％的RF基团含有6个碳原子时得到最佳结果。因此优选RF链的70-100％含有6个碳原子。不含有6个碳原子的RF基团大都具有4或8个碳原子的链长度。
具有全氟烷基(RF基团)的聚合物(＝根据本发明的组合物的组分C)优选为聚丙烯酸酯或者聚甲基丙烯酸酯，其中醇组分含有RF基团。所讨论的聚合物优选包含下式单元
此外，所述聚合物可更进一步含有由可共聚单体衍生的单元。其实例为：氯乙烯、偏二氯乙烯、苯乙烯、N-羟甲基丙烯酰胺和无氟相对长链(甲基)丙烯酸酯比如硬脂醇丙烯酸酯及其羟基衍生物。
可用作组分C的聚合物可用已知的方法通过使(甲基)丙烯酸或其酯与含有RF基团的醇反应，然后进行自由基聚合(任选在其它可聚合单体存在下)而获得。含有RF基团的醇在RF基团中大都具有6个碳原子，即所有RF基团的55-100％含有6个碳原子。所述RF基团优选具有下式
其中在大多数RF基团中a为4。
合适的(甲基)丙烯酸酯的结构及其制备描述于WO2009/000370 A1、EP234 724A1以及FR2 213 333A中。类似于这些参考文献，可获得可用作根据本发明的组合物的组分C的聚合物，除了必须注意RF基团的链长度。
除了优选的(甲基)丙烯酸酯以外，组分C也可使用其它含有RF基团的聚合物，例如具有RF基团的聚氨酯。
根据本发明的组合物中组分A是混合物，至少含有组分A1-A3的混合物，或者至少含有组分A4-A6的混合物。
同样适用于本发明组合物的是含有组分A的所述供选两者的混合物(即不但含有组分A1-A3而且含有组分A4-A6的混合物)，或者含有组分A1-A3，A4和A6(组分A5可忽略因为它相当于组分A3)的混合物。
组分A1是石蜡。这样的蜡市售可得且由CAS号8002-74-2和64742-43-4描述。优选使用熔化范围为50℃-80℃的蜡。
组分A2是缩合产物，其可通过使具有12-22个碳原子的醇(优选为直链单羟基醇)，一方面与多羟甲基三聚氰胺(其被醚化且优选季铵化)，且另一方面与任选另外的多官能乙醇胺反应而获得。用甲醇醚化和用烷基硫酸酯季铵化的六羟甲基三聚氰胺特别有用。该缩合产物在相对长链的醇同时与三聚氰胺和多官能乙醇胺反应时形成。二乙醇胺和三乙醇胺是非常合适的乙醇胺。组分A2可另外含有较少量的酸(例如乙酸)，例如按重量计0.05-1.5％。
组分A3是水。
根据本发明的组合物中组分B是至少含有组分B1-B3的混合物。
组分B1是含有封端的异氰酸酯基团(所有异氰酸酯基团的至少90％被封端)的聚氨酯。从文献已知的产品可用作封端剂。脂肪族酮肟(例如丁酮肟)用作封端剂特别有利。优选的聚氨酯优选由脂肪族(或优选芳香族)二异氰酸酯与三羟基脂肪醇(例如1，1，1-三羟甲基丙烷)和N-烷基化二乙醇胺或三乙醇胺优选反应而构成。可用作组分B1的聚氨酯例如从Huntsman Textile Effects(Germany)GmbH市售可得。
可用作组分B1的聚氨酯及其制备描述于EP872 503A1。
组分B2是分散剂或者分散剂的混合物。组分B2含有一种或多种乙氧基化醇(基于相对长链(优选为直链)的单羟基醇)，和任选另外的二羟基脂肪醇以及任选少量的无机酸，例如盐酸。所述乙氧基化醇的单羟基源醇的链长度的优选范围是8-22个碳原子。任选的二羟基醇优选具有2-6个碳原子。乙二醇和1，2-丙二醇非常有用。
组分B3是水。
在一个有利的实施方案中，根据本发明的组合物另外含有作为组分D的锆盐，对于所述锆盐乙酸锆特别有用。
根据本发明的组合物仍可含有其它产品，例如褐煤蜡酸(CAS No.68476-03-9)，特别是当乙酸锆存在时，或者除组分A已存在的石蜡之外，仍可含有其它石蜡。另一任选的产品是乙氧基化脂肪酸衍生物(CAS No.61791-12-6)。此外，可以存在其它分散剂，特别是阳离子表面活性剂。
由于分散剂的存在，根据本发明的组合物通常是含水分散体。它们可用已知的方法例如通过将单独的组分在室温下或者必要时在升高的温度下混合并且随后机械均化而获得。
但是，优选首先制备含有组分A和B而不含组分C的混合物。这种混合物具有良好的储存稳定性。用这种方式，组分C仅正好在使用本发明的组合物之前加入。
优选地，根据本发明的组合物含有相对于彼此的以下量的组分A-D：
35-120重量份，优选45-90重量份，更优选50-75重量份的组分A
1-60重量份，优选5-50重量份，更优选8-20重量份的组分B
1-60重量份，优选1-45重量份，更优选2-20重量份的组分C
0-30重量份，优选0-15重量份，更优选1.5-8重量份的组分D。
优选的实施方案的特征还在于组分A不含有组分A4-A6而含有以下量的组分A1和A2，
A1：10-30重量％，优选12-25重量％
A2：5-15重量％，优选6-12重量％，
其中组分A的余部由水(组分A3)及任选由少量的乙酸形成，
或者其特征在于组分A不含有组分A1-A3且特征在于它含有以下量的组分A4-A6：
A4：25-45重量％，优选30-40重量％
A5：50-70重量％，优选55-65重量％
A6：1-5重量％，优选3-5重量％。
当根据本发明的组合物含有A1-A6所有组分时，优选相对于彼此的如下量：
A1：8-30重量份，优选10-20重量份
A2：3-20重量份，优选4-12重量份
A4：1-15重量份，优选2-10重量份
A6：0.05-3重量份，优选0.1-2重量份
其中组分A的余部由水(组分A3和A5)形成。
组分B优选包含以下量的组分B1和B2：
B1：8-40重量％，优选12-30重量％
B2：2-20重量％，优选3-15重量％，
其中组分B的余部由水(组分B3)形成。
本发明的组合物对处理由纤维材料组成的纺织织物非常有用，原因在于结果为这些纺织织物给予了优良的防油和/或防水性质。此处织物通常为织造物、针织物或者纤维非织造网(非织造物)。它们尤其可以用于制造以下最终使用物品：防水衣和工作服。优选地，纺织品由聚酰胺、聚酯或者聚酯-棉共混物组成。
用本发明的组合物处理纺织织物可通过已知方法实现，例如通过轧车(pad-mangle)操作，在这种情况下将已涂敷所述组合物的织物干燥并且通常在进一步升高的温度下固化。
如已提到的，当根据本发明的组合物通过以下生产时是有利的：首先只将组分A和B相互混合并任选机械均化，而组分C仅在正好将组合物用于纺织品处理之前加入。处理液随后调节到通常使用的浓度。
以下实施例说明本发明。
实施例1(本发明)：
制备含有68g/l组分A，32g/l组分B及18.5g/l组分C(＝来自Huntsman Textile Effects(Germany)GmbH的CP-S)的含水液体F1。此处组分C是在醇组分中具有RF基团的聚丙烯酸酯，其中大约100％的所有RF基团含有6个碳原子。所使用的组分A含有一组分A1，一组分A2及一组分A3。
实施例2(非本发明，比较实施例)：
重复实施例1，除了使用不同的组分C(S)，量为14.5g/l。该组分C同样包含具有RF基团的聚丙烯酸酯。但是，这些RF基团大都含有8个碳原子。
这样得到的液体在下文中称为F2。
实施例3(本发明)：
制备含有34g/l组分A，26g/l组分B及9.5g/l与实施例1相同的组分C的液体F3。此处使用的组分A含有一组分A1，一组分A2，一组分A3，一组分A4以及一组分A6。
实施例4(非本发明，比较实施例)：
重复实施例3，除了与实施例2相同的丙烯酸酯用作组分C，量为7.5g/l。这样得到的液体在下文称为液体F4。
液体F1-F4各自另外含有1g/l60％的乙酸。
将液体F1-F4每一种通过轧染(padding)涂敷于由65％聚酯/35％棉组成的织造织物，然后挤压到大约60重量％的湿物品(wet pickup)，在110℃下干燥并且在150℃下固化5分钟。
这样得到的织物样品进行以下测试：
a)防油性按照AATCC Test Method118-2002
b)水滴测试按照AATCC Test Method193-2005
c)喷雾试验防水性按照AATCC Test Method22-2005
所有测试不但在原织物样品上而且在样品30次洗涤(60℃用加入的洗衣清洁剂)后进行。所述洗涤按照DIN EN ISO6330，洗涤法2A进行并翻滚干燥。
结果显示在下表中：
较大的数字表示较好的防油或者防水性。
清楚地证明用本发明的液体F1和F3处理的织物比用液体F2和F4处理的那些具有更好的性质。
Claims (15)
1.一种至少含有组分A，B和C的含水组合物，其中
组分A是至少含有组分A4-A6的混合物，其中
组分A4是聚硅氧烷，所述聚硅氧烷除连接于硅原子的烷基外，另外含有连接于硅原子的氢原子，即烷基-氢-聚硅氧烷，
组分A5是水而且
组分A6是分散剂，
组分B是至少含有组分B1-B3的混合物，其中
组分B1是含有异氰酸酯基团的聚氨酯，且其异氰酸酯基团是被封端的，
组分B2是分散剂或者分散剂混合物并且含有乙氧基化醇与任选的二羟基脂肪族醇及任选的无机酸，
组分B3是水，
组分C是含有全氟烷基基团的聚合物，其中55-100%的所有存在的全氟烷基基团含有6个碳原子，
其中该组合物任选还含有作为组分D的锆盐。
2.根据权利要求1的组合物，其中所述作为组分A6的分散剂为乙氧基化醇或者乙氧基化醇的混合物。
3. 根据权利要求2的组合物，其中所述乙氧基化醇为具有8-20个碳原子的乙氧基化直链或支化的醇。
4. 根据权利要求1的组合物，其中所述异氰酸酯基团是被脂肪族酮肟封端的。
5. 根据权利要求1的组合物，其中所述聚氨酯由芳香族或者脂肪族二异氰酸酯构成。
6. 根据权利要求5的组合物，其中所述二异氰酸酯与具有2-6个碳原子的二醇、三羟基脂肪族醇和N-烷基化二乙醇胺或者三乙醇胺反应。
7. 根据权利要求5的组合物，其中所述聚氨酯由芳香族二异氰酸酯构成。
8. 根据权利要求1的组合物，其中所述锆盐为乙酸锆。
9. 根据权利要求1－8任意一项的组合物，其特征在于所述组分C是在醇组分中含有全氟烷基基团的聚丙烯酸酯或者聚甲基丙烯酸酯。
10. 根据权利要求1－8任意一项的组合物，其特征在于它含有以下量的组分A-D：
35-120重量份的组分A；
1-60重量份的组分B；
1-60重量份的组分C；
0-30重量份的组分D。
11. 根据权利要求1－8任意一项的组合物，其特征在于组分A含有以下量的组分A4-A6：
A4：25-45重量%，
A5：50-70重量%，
A6：1-5重量%。
12. 根据权利要求1－8任意一项的组合物，其特征在于组分B含有以下量的组分B1和B2：
B1：8-40重量%，
B2：2-20重量%，
其中组分B的余部由组分B3形成。
13. 一种用于处理由纤维材料组成的纺织织物的方法，其中该织物用根据权利要求1-12任意一项的组合物处理并且随后干燥。
14. 根据权利要求13的方法，其特征在于所述纤维材料由聚酰胺、聚酯或聚酯/棉共混物组成。
15. 根据权利要求13或14的方法，其特征在于组分C仅正好在处理所述纤维材料之前与组分A和B混合。
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| WO2013083110A1 (de) * | 2011-12-05 | 2013-06-13 | Guido Radde | Imprägnierflüssigkeit zum wasserabweisendmachen von papierartigem material und textilen flächengebilde und die verwendung desselben |
| CN102965925A (zh) * | 2012-11-20 | 2013-03-13 | 吴江市新丝源纺织有限公司 | 一种防水涂层面料 |
| DE102013209170A1 (de) * | 2013-05-17 | 2013-09-12 | Cht R. Beitlich Gmbh | Wasserabweisende Effekte auf textilen Oberflächen |
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- 2010-09-22 EP EP10812849.7A patent/EP2480713B1/en active Active
- 2010-09-22 ES ES10812849.7T patent/ES2438166T3/es active Active
- 2010-09-22 CN CN201410207027.8A patent/CN103966855B/zh active Active
- 2010-09-22 JP JP2012530166A patent/JP6030957B2/ja active Active
- 2010-09-22 MX MX2012002194A patent/MX2012002194A/es active IP Right Grant
- 2010-09-22 BR BR112012006454A patent/BR112012006454B1/pt active IP Right Grant
- 2010-09-22 US US13/394,354 patent/US8840964B2/en active Active
- 2010-09-22 IN IN465DEN2012 patent/IN2012DN00465A/en unknown
- 2010-09-22 WO PCT/EP2010/005812 patent/WO2011035906A2/en not_active Ceased
- 2010-09-22 CN CN201080043192.4A patent/CN102549212B/zh active Active
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| CN107407047B (zh) * | 2015-02-13 | 2020-10-27 | 3M创新有限公司 | 使用包括含有异氰酸酯衍生的(甲基)丙烯酸酯聚合化合物的不含氟组合物处理纤维基材的方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| KR101761096B1 (ko) | 2017-07-25 |
| KR20120092557A (ko) | 2012-08-21 |
| BR112012006454A2 (pt) | 2016-04-26 |
| ES2438166T3 (es) | 2014-01-16 |
| US8993067B2 (en) | 2015-03-31 |
| EP2480713B1 (en) | 2013-10-30 |
| EP2480713A2 (en) | 2012-08-01 |
| WO2011035906A2 (en) | 2011-03-31 |
| MX2012002194A (es) | 2012-03-16 |
| US20140356541A1 (en) | 2014-12-04 |
| JP2013506055A (ja) | 2013-02-21 |
| BR112012006454B1 (pt) | 2019-12-17 |
| WO2011035906A3 (en) | 2011-05-26 |
| WO2011035906A8 (en) | 2011-08-11 |
| IN2012DN00465A (zh) | 2015-06-05 |
| JP6030957B2 (ja) | 2016-11-24 |
| US20120177832A1 (en) | 2012-07-12 |
| US8840964B2 (en) | 2014-09-23 |
| CN102549212B (zh) | 2014-10-29 |
| CN103966855B (zh) | 2016-08-17 |
| CN102549212A (zh) | 2012-07-04 |
| EP2302130A1 (de) | 2011-03-30 |
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