CN1147281A - 减少溶纺纤维素纤维织物原纤化倾向的处理方法 - Google Patents

减少溶纺纤维素纤维织物原纤化倾向的处理方法 Download PDF

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CN1147281A
CN1147281A CN95192877A CN95192877A CN1147281A CN 1147281 A CN1147281 A CN 1147281A CN 95192877 A CN95192877 A CN 95192877A CN 95192877 A CN95192877 A CN 95192877A CN 1147281 A CN1147281 A CN 1147281A
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C·D·波特
J·M·泰勒
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Abstract

在酸催化剂存在时，用一种交联剂处理溶纺纤维素纤维织物，可以减小溶纺纤维素纤维织物的原纤化倾向及减小已原纤化的溶纺纤维素纤维织物的原纤化程度。当所使用的催化剂与选用的交联剂重量比至少在0.5∶1时，可获得良好的结果，当固着在该织物上的交联剂的量为织物重量的0.5-1.5％(重量)时，也可获得良好的结果。

Description

减少溶纺纤维素纤维织物原纤化倾向的处理方法
发明领域
本发明涉及一种减少溶纺纤维素织物原纤化倾向及减少发生原纤的溶纺纤维素纤维织物原纤化程度的方法。
众所周知，纤维素纤维可通过把纤维素溶于适当溶剂中的溶液挤出于一纺丝凝固浴而制得。上述方法被称为“溶液纺”，所纺得的纤维素纤维被称为“溶液纺”纤维素纤维或溶纺纤维素纤维(lyocell fibre)。溶纺纤维素纤维应区别于由其它已知方法所制得的纤维素纤维，这些已知方法依赖于形成可溶的纤维素衍生物以及随后的分解，再生出纤维素的过程，例如，粘胶法。溶液纺方法的一个例子记载于美国专利号US-A-4,246,221的专利文献上，本发明参照使用了其中所述的内容。将纤维素溶于例如一种叔胺N-氧化物的水溶液中，例如，溶于N-甲基吗啉N-氧化物的水溶液中。然后将形成的溶液通过一合适的模子挤压入一水浴，以制得纤维长丝束该纤维长丝束经水洗去除溶剂，然后进行干燥。
此处所使用的，“溶纺纤维素纤维”一词指，由有机溶剂纺丝方法所制得的纤维素纤维，其中，所述的有机溶剂基本上由一有机化合物和水的混合物组成，所述的溶液纺丝包括：将纤维素溶于该有机溶剂中，以形成溶液，该溶液在不必形成纤维素衍生物的情况下纺成纤维。此处所使用的，“溶纺纤维素织物”一词指，由其中至少某些纱线为溶纺纤维素纤维的纱线经针织或机织而制得的织物。
纤维会显示出原纤化的倾向，特别是在湿的状态下经受机械应力时。当纤维结构在径向断裂时，就会发生原纤化，即有细小的原纤从纤维上部分地脱离下来，使该纤维或含有该纤维的织物，例如机织物或针织物，产生毛茸状外观。含有该原纤化纤维的染色织物易产生一种“霜花”般外观，这从美学上来说是不希望的。据认为，这种原纤化是由于纤维在处于湿的状态或溶胀的状态下受到机械摩擦而引起的。湿的加工方法，例如，染色工序，将不可避免地会使纤维受到机械的摩擦。而高温、长时间的处理通常使原纤化程度加剧。溶纺纤维素纤维比起通常其它的纤维素纤维来，其对于所述的摩擦特别敏感，因此常更易原纤化。特别是，棉纤维织物具有固有的很低的原纤化倾向。背景技术
多年来，人们已知用一交联剂处理纤维素织物，以改善织物的抗皱性，如在Kirk-Othmer的《化学技术百科全书》Wiley-Interscience第三版，第22卷(1983)769-790页上题为“纺织(整理工艺)”一文中所描述的，及H.Petersen在《ReV.Prog.Coloration》第17卷(1987)，第7-22页上所描述的方法。交联剂有时被称为其它一些名称，如交联树脂，化学整理剂及树脂整理剂。交联剂为一种含有多个可与纤维素中的羟基反应、形成交联的官能团的小分子。在一种通常的整理过程中，首先是用一种交联剂，例如用浸轧浴处理纤维素纤维织物，然后干燥，加热固化树脂，引发交联(浸轧-干燥-固化)。已知，抗皱整理处理导致纤维素纤维织物的脆化，其耐磨性能、抗拉强度及撕破强度也同时丧失。在选择整理系统时成本是一个重要的因素。
一类已知的交联剂包括N-羟甲基树脂，即包括含有二个或二个以上的N-羟甲基或N-烷氧基甲基，特别是N-烷氧基甲基基团的小分子。N-羟甲基树脂通常与酸催化剂一起使用用来改善交联性能，在一个典型的方法中，含有约5-9％(重量)的N-羟甲基树脂交联剂和0.4-3.5％(重量)的酸催化剂的溶液浸轧于干燥纤维素纤维织物上，以获得60-100％(重量)的加重率，然后干燥和加热该潮湿的织物，以固化和固定交联剂。一典型的可有约70-75％(重量)的交联剂固着在织物上。酸催化剂与交联剂的比例应选择尽可能与其有效反应相一致地低。酸催化剂的使用量大，增加了处理的成本，并可能导致交联树脂的破裂和酸对纤维素纤维的损伤。酸损伤导致织物强力的降低。更为典型的是，催化剂和交联剂的重量比在约1∶4至1∶20的范围。
发明简述
本发明提供了一种减少溶纺纤维素纤维织物原纤化倾向的方法，所述方法包括以下步骤：
(a)使织物与一种含有酸催化剂及附加交联剂的水溶液接触，及
(b)加热该织物，
其特征在于，所述的酸催化剂和附加交联剂的重量比至少为约0.5∶1。
本发明提供了一种减少已原纤化的溶纺纤维素纤维织物原纤化程度的方法，所述方法包括以下步骤：
(a)使织物与一种含有酸催化剂及附加交联剂的水溶液接触，及
(b)加热该织物，
其特征在于，所述的酸催化剂和附加交联剂的重量比至少为约0.5∶1。
本发明还提供了一种减少溶纺纤维素纤维织物原纤化倾向方法，所述方法包括以下步骤：
(a)使织物与一种含有酸催化剂和交联剂的水溶液接触，及
(b)加热该织物以固化交联剂，
其特征在于，固着在织物上的交联剂的量为织物重量的0.5-1.5％(重量)。
本发明进一步提供了一种减小发生了原纤化的溶纺纤维素纤维织物原纤化程度的方法，所述方法包括以下步骤：
(a)使织物与一种含有酸催化剂和交联剂的水溶液接触，及
(b)加热该织物以固化交联剂，
其特征在于，固着在织物上的交联剂的量为织物重量的0.5-1.5％(重量)。
已知，通常的交联剂处理可以减小溶纺纤维素纤维织物原纤化的倾向。现在已明显地发现，即使所述的处理液体丝毫不含交联剂，或交联剂含量相当地低，也可得到类似的效果。
上述的酸催化剂可以是铵盐催化剂，例如硫酸铵；但最好是一种路易斯酸类的金属盐催化剂。较好的催化剂包括氯化镁，氯化锌，氟硼酸锌，硝酸锌及其混合物。所述的酸催化剂也可以是一种水溶性有机酸，如被取代的羧酸，优选的是脂肪酸。其优点是在所述的加热条件下是非挥发性的。合适的有机酸包括酒石酸，特别是柠檬酸。也可以使用酸催化剂的混合物。
处理液中酸催化剂的浓度在一定程度上取决于所用的酸催化剂的性质。酸催化剂的浓度不应过高，以避免在加热过程中在织物上形成显著的酸损伤。高活性酸催化剂的浓度可比低活性酸催化剂的低些。高活性的金属盐催化剂的浓度一般可在从约2至约20g/l的范围，通常在约5-10g/l的范围。低活性催化剂，例如胺类盐催化剂的浓度可以高至约40g/l。有机酸催化剂的浓度一般在1-10g/1的范围。柠檬酸较好的浓度为4-6g/l。
所述水溶液的pH通常为弱酸性。
所述的水溶液可由通常用于纤维素纤维织物的整理的方法，例如浸轧浴，施加至织物上。
施加了水溶液之后，最好在加热之前干燥织物。所述的干燥工序可作为加热步骤中的预处理来进行。
一般来说，加热处理可在类似于通常的交联处理中用于固化交联树脂的条件下进行，例如在125-180℃的温度下处理30秒至5分钟。一般来说，处理温度较高，则处理时间较短。应对加热条件加以选择，以尽量减小对织物可能造成的酸损伤。
可选用的交联剂可以是任何在本领域已知的纤维素纤维纺织品的整理中所用的交联剂。
当水溶液包含附加交联剂时，要使得：交联剂在织物上的固着量为纤维素纤维的织物重量的0.5-1.5％(重量)。这种量比通常在抗皱处理中所用的交联剂的用量低得多。在抗皱处理中，固着的交联剂量通常为织物重量的约3％。可以选择使用的交联剂最好是低甲醛类，例如N-羟甲基树脂，或零甲醛类交联剂。
人们知道，纤维素酶处理可以除去发生原纤化的溶解纤维素纤维的织物上的原纤。本发明提供了一种经济、快速且简便地去除这类原纤的方法。尽管本发明的应用一般也导致织物拉伸性能的降低，但这种降低程度总的来说，与通常纤维素纤维批量生产时有时发生的拉伸性能的降低相差无几。
以上所描述或所使用的“原纤化”一词意指长的原纤或纤毛从纤维上部分地脱离下来，由此含有该纤维的织物显示出了不希望有的绒毛外观，而含有该纤维的染色织物显示出霜花般外观。这类原纤化现象也可称作初级原纤化。“原纤化”也可用于描述另一种现象，该原纤化现象可称为二次原纤化。在二次原纤化中，短原纤从织物中的纤维上部分地脱离，但是仍大量地留在织物结构中。这种现象给织物增添了一种所希望的桃皮状外观。再有，初级原纤化现象一般发生于织物的局部处，而二次原纤化现象的分布则一般来说更为均匀。在纤维和二次原纤化之间存在的染色性的任何不同之处并未导致如桃皮织物上的霜外观等不理想的视觉效果。因此，只要能避免初级原纤化则二次原纤化可产生一种理想的效果。可以理解，以上所提到的、与本发明有关的原纤化是初级原纤化。进一步发现，本发明的方法可理想地用来引起二次原纤的发生。
以下，用下述试验方法1评价各种材料的原纤化程度。试验方法1(原纤化的测试)
对于原纤化的测试，尚无一个普遍为人们可接受的标准方法。下述方法用于测试原纤化指数(F.I.)。将许多试样按原纤化程度的大小排成系列。测得各试样纤维的标准长度，然后计数该标准长度的纤维上原纤(伸出该纤维主体的细毛绒)的根数。再测得每根原纤的长度，然后将原纤数目乘以原纤的平均长度得出一人为的数值。显示最高乘积值的纤维被认定为原纤化最大的纤维，并规定其原纤化指数为10。完全未原纤化的纤维的原纤化指数规定为0，其余的纤维根据显微镜测量并计算的该数值，则排在0-10之间。
然后，将上述测得的纤维构成一标准级别。为测定任何其它的纤维试样，在显微镜下将5-10根纤维与标准级别的纤维进行目测比较。接着，将对各纤维作目测所测得的数取平均值，以得出试样的原纤化指数。可以看到，目测测量和取平均值的过程数倍地快于实际的测量，而且发现，一个熟练的纤维技术人员在对纤维进行这种测定等级方面，结果是稳定的。
织物的原纤化指数可由抽拉出织物表面的纤维根数测定。F.I.指数为约2或更大的机织及针织织物通常显示了不佳的外观。
下面以实施例来说明本发明。在所有的例子中，所使用的溶纺纤维素织物仅由溶纺纤维素纤维组成。溶纺纤维素纤维可从考特沃兹纤维(控股)有限公司购得，商品名为TENCEL。实施例1
将染过色的机织溶纺纤维素纤维的织物进行洗涤，以引发原纤化(F.I.＝5.5)。将该织物在含有各种量的Condensol FB(BASF AG的商标名)水溶液中进行浸轧。然后在各种条件下加热。Condensol FB是一种氟硼酸锌和氯化镁的酸催化剂。进一步洗涤该织物，测定其对原纤化的影响。结果示于表1。
                   表1
Condensol FB
浓度              加热                F.I.
g/l        时间，分  温度℃        1w/t    5w/t
O(对照)       -        -           5.8     5.4
10            3       140          2.7     0.4
              5       140          3.4     0.2
              3       160          2.9     0.9
             1.5      160          2.4     0.6
             0.5      180          3.7     0.6
20            3       140          1.6     0.0
              5       140          1.5     0.2
              3       160          1.8     0.1*
             1.5      160          1.0     0.0*
             0.5      180          1.4     0 2*
在上表中，“W/t”表示洗涤翻动循环数。(*)表示织物的强度明显减少。如果使用高浓度的Condensol FB(50g/l或100g/l)，则织物明显损伤。实施例2
重复实施例1，不同之处在于在所有的例子中，Condensol FB的浓度都为10g/l。结果如表2所示：
                      表2
       加热                   F.I.
时间，分  温度℃    10w/t    15w/t    20w/t
   3       140       1.6      0.6      3.2
   5       140       0.8      0.6      2.4
   6       160       0.5      0.4      0.0
  1.5      160       0.3      0.0      0.0
  0.5      180       1.1      0.3      0.0实施例3
用含有10g/lCondensol FB的水溶液浸轧机织溶纺纤维素纤维织物的试样，干燥后在160℃下加热1.5分钟。用标准测试方法测得该试样的物理性能。结果示于表3：
                      表3
试验                        对照    处理
拉伸强力(扯边纱条试样)
经纱B.L.N                    648     647
经纱伸长％                  18.2    15.7
纬纱B.L.N                    540     509
纬纱伸长％                  17.5    18.5
埃尔门多夫撕破强力CN
经纱                        1068    1149
纬纱                         999     816
起球(11000转)                2-3     4-5
马丁代尔试验仪
磨损(9kpa)                 10250    9500
(B.L.＝断裂载荷)
上述经处理的织物与对照试样的性能非常相似，只是其抗起球性能得到改善。实施例4
重复实施例1，不同之处在于，使用氟硼酸锌作酸催化剂，试样为针织溶纺纤维素纤维织物。结果如表4所示：
                         表4
                            机织织物        针织织物浓  度        加  热            F.I.            F.I.
g/l    时间，分  温度℃     1w/t   5w/t     1w/t   5w/tO(对照)     -        -        4.1    6.1      5.2    5.7
 4        3       140       4.3    4.9      1.3    1.8
          5       140       3.4    1.9      2.7    2.9
          3       160       1.4    2.7      0.8    1.3
         1.5      160       2.2    0.9      1.8    1.9*
 6        3       140       2.2    1.6      2.5    1.5
          5       140       2.1    0.0      1.6    0.6*
          3       160       0.9    0.0      1.3    1.3*
         1.5      160       1.3    0.0      1.5    1.0
星号表示该织物强度有所下降。Condensol FB浓度为10g/l时，织物明显损伤。实施例5
重复实施例1，不同之处在于，使用硫酸铵作为酸催化剂。结果如表4所示：
                          表5
酸催化剂           加热               F.I.
浓度g/l    时间，分    温度℃      1w/t    5w/t
20            0.5       180        2.6     4.8
40             3        140        3.6     3.4
40             5        140        4.1     4.4
40             3        160        3.7     5.9
40            1.5       160        3.9     4.2
40            0.5       180        2.6     5.9
当使用80g/l的硫酸铵时，则织物强度降低。实施例6
绳状伤痕为织物上白色的褶皱状伤痕，该伤痕是由于织物在湿加工过程中，不改变位置而经受了连续的摩擦所至。这种伤痕代表了高度原纤化的区域。尽管人们知道，纤维素酶的处理可有效地用于从原纤化的溶纺纤维素织物上除去原纤绒毛，但是这样的处理并不能除去这种绳状伤痕。
一块溶纺纤维素纤维织物的试样本身的F.I.指数为1.4，而织物上绳状伤痕的F.I.指数为4.1。用含有10g/l各种酸催化剂的水溶液浸轧该织物的试样，干燥后在160℃下加热3分钟。原纤化结果列于表6：
                     表6
酸催化剂       绳状痕迹       主体织物
             1w/t    5w/t   1w/t    5w/t
无(对照)      3.7     4.7    4.3     5.2
Condensol FB  2.3     2.2    1.5     2.6
硝酸锌        0.8     0.4    0.7     0.8
氯化锌        1.8     0.8    1.1     1.0
洗涤后，使用Condensol FB的试样显示了浅淡的绳状伤痕及原纤化现象。对照试样则显示了全面的原纤化，这种原纤化掩盖了所述的绳状伤痕。使用了硝酸锌和氯化锌的试样的外观都很清洁，但是，在织物本体上再看不出绳状伤痕了。实施例7
用含有交联剂和酸催化剂的水溶液浸轧机织的溶纺纤维素纤维织物，干燥后在180℃下加热30秒以固化交联剂。结果如表7所示：
                             表7                  F.I.
处    理            基于织物计的固着树脂％    1w/t  5w/t  10w/t对照(无交联剂和催化剂)              -             2.0   7.4   4.117g/l Arkofix NG conc             1.1            1.3   0.3   1.815g/l Condensol FB17g/l Arkofix NG conc             1.2            0.7   1.0   0.420g/l Condensol FB50g/l Arkofix NG conc             3.1            0.8   0.4   0.715g/L Condensol FB
其中，Arkoix NG Conc(Hoechst AG的商标名)是一种4，5-二羟基-1，3-二甲氧基亚乙基脲(DHDMEU)的低甲醛交联剂。
显见，固着有1.1％的树脂的试样在10w/t的循环后出现了原纤化现象，而其它的试样则显示了清洁的外观。所有的织物对60℃的洗涤皆具有优良的稳定性。
可以看到，固着有1.1％及1.2％的树脂、催化剂和树脂的比例为0.9∶1和1.2∶1的试样可获得良好的结果，固着有3.1％的树脂、催化剂/树脂的比例为0.3∶1的对照试样也获得良好的结果。实施例8
使用普施安海军蓝(Procion Navy)HER150(Procion为ICI plc的商标名)对机织溶纺纤维素纤维织物进行染色，洗涤，使其发生原纤化现象(F.I.＝7.0)。用含有15g/l的硝酸锌的水溶液浸轧，110℃下烘干。然后将上述试样的一半在150℃下加热处理1分钟。所有的织物试样经十个洗烫循环。该织物的未经加热处理的部分表面比起对照试样具有较清洁的外观，而该织物的经加热处理的部分表面肉眼观察清洁，无原纤化的现象。显微检查表明，在洗烫后织物的纤维上有原纤的短丝束存在。实施例9
按实施例8的方法对溶纺纤维素纤维织物进行染色和洗涤。染色织物的试样浸轧以含有15g/l硝酸锌但不同pH(4.0，6.0，8.0或10.0)的水溶液，110℃下烘干，在150℃下加热处理1分钟。在pH10.0时金属盐从溶液中析出。织物试样然后经十个洗烫循环。该织物的外观随pH的减小而改善，在pH4.0时处理的织物外观肉眼看来非常干净。如同实施例8，显微检查表明在洗烫后织物的纤维上有原纤的短丝束存在。实施例10
重复实施例8，不同之处在于，使用了柠檬酸(4g/l)水溶液以取代硝酸锌水溶液。经十个洗烫循环的加热处理织物的表面显得干净，显示出一种引人注目的桃皮状外观。显微检查结果类似于实施例8。

Claims (10)

1.一种减少溶纺纤维素纤维织物原纤化倾向的方法，所述方法包括以下步骤：
(a)使织物与一种含有酸催化剂和附加的交联剂的水溶液接触，及
(b)加热该织物，
其特征在于，所述的酸催化剂和该可附加的交联剂的重量比至少为约0.5∶1。
2.一种减少已原纤化的溶纺纤维素纤维织物原纤化程度的方法，所述方法包括以下步骤：
(a)使织物与一种含有酸催化剂及附加交联剂的水溶液接触，及
(b)加热该织物，
其特征在于，所述的酸催化剂和附加的交联剂的重量比至少为约0.5∶1。
3.如权利要求1或2所述的方法，其特征在于，所述的水溶液不含有交联剂。
4.一种减少溶纺纤维素纤维织物原纤化倾向的方法，所述方法包括以下步骤：
(a)使织物与一种含有酸催化剂和交联剂的水溶液接触，及
(b)加热该织物以固化所述的交联剂，
其特征在于，固着在织物上的交联剂的量为织物重量的0.5-1.5％(重量)。
5.一种减少已原纤化的溶纺纤维素纤维织物原纤化程度的方法，所述方法包括以下步骤：
(a)使织物与一种含有酸催化剂和交联剂的水溶液接触，及
(b)加热该织物以固化交联剂，
其特征在于，固着在织物上的交联剂的量为织物重量的0.5-1.5％(重量)。
6.如上述任一权利要求所述的方法，其特征在于，所述的酸催化剂为一种路易斯酸类的金属盐催化剂。
7.如权利要求6所述的方法，其特征在于，所述的金属盐催化剂的浓度为约2-20g/l的范围。
8.如权利要求1-5所述的方法，其特征在于，所述的酸催化剂是一种水溶性有机酸。
9.如权利要求8所述的方法，其特征在于，所述的酸催化剂为柠檬酸。
10.如权利要求1，2或4-9中之任一项所述的方法，其特征在于，所述的交联剂选自含N-甲氧基树脂和零甲醛树脂。
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CN1329583C (zh) * 2003-03-04 2007-08-01 莱恩真纤维有限公司 经过染色和整理的莱奥塞尔织物的生产方法
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CN105040427A (zh) * 2008-06-27 2015-11-11 连津格股份公司 纤维素纤维及其制备方法
CN111893749A (zh) * 2020-08-14 2020-11-06 亚太森博（山东）浆纸有限公司 交联剂及莱赛尔纤维的抗原纤化处理方法
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US5759210A (en) 1998-06-02
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