CN1083913C - 纺织品的阻燃和织物柔软处理 - Google Patents

纺织品的阻燃和织物柔软处理 Download PDF

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CN1083913C
CN1083913C CN95120388A CN95120388A CN1083913C CN 1083913 C CN1083913 C CN 1083913C CN 95120388 A CN95120388 A CN 95120388A CN 95120388 A CN95120388 A CN 95120388A CN 1083913 C CN1083913 C CN 1083913C
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M·扎基克哈尼
X·P·雷
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Solvay Solutions UK Ltd
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    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/44—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen containing nitrogen and phosphorus

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Abstract

一种复合组合物能使纺织品具有阻燃性和织物柔软性，它含有IHP+盐，有机氮化合物(例如尿素)和具有12或更多碳原子的羟基活性的有机化合物。这种化合物的优选的例子包括(C12胺，C18胺和牛脂胺(即C16/C18/C20胺的混合物)。

Description

纺织品的阻燃和织物柔软处理
本发明涉及一种适用于使纺织品具有阻燃性和织物柔软性的组合物，生产所述组合物的方法及使用所述组合物处理织物的方法。
已知的对织物包括纤维素纤维(例如，棉纤维)的阻燃性处理工艺包括将织物在聚(羟有机)鏻化物水溶液中浸渍，例如四羟有机鏻盐(tetrakis(hydroxy-organo)phosphonium(THP+)salt)。可选择地，聚(羟有机)鏻化合物可同含氮化合物，例如尿素缩聚。浸渍之后，将织物干燥并用氨交联，以使交联的、不溶于水的聚合物机械地固着在织物的纤维间。交联之后，将聚合物氧化，使三价磷转化为五价磷，再将织物洗涤并干燥。依据上述工艺处理的织物及使用如此处理的织物制成的衣服Albright & Wilson Limited以注册商标PROBAN出售。
我们的英国专利说明书No.GB-A-2271787公开了向浸渍溶液中加入一种或多种质子化的和中和了的胺(例如醋酸胺)。这种添加可提高鏻化合物在纤维中的固着效果，并能增加鏻化合物在此系统中的均匀分布，而且我们接着发现它能增加阻燃性和防水性。
我们的英国专利说明书No.GB-A-2040299公开了在与尿素缩聚之前，向THP+化合物中加入无机碱或C1-C4叔胺碱。但是，上述专利GB-A-2040299没有涉及用此产物处理纺织品时，纺织品的柔软性(悬垂性)问题。
我们相同的申请No.GB 9412484.9公开了一种增加THP+化合物在织物上添加率的方法，它能导致织物阻燃性的增加。
现在我们发现，在配料反应产生THP+盐和有机氮化合物的缩聚物之前，向THP+盐和有机氮化合物的水混合物中加入具有12个或更多碳原子的伯或仲脂肪族胺，可导致产生一种组合物，当使用它按前述PROBAN工艺处理纺织品时，它不仅可使纺织品具有阻燃性而且能提高织物柔软性。
本发明提供了一种适用于使纺织品具有阻燃性和织物柔软性的组合物，其中所述组合物包括由下列反应所得的产物的稳定的60％含水溶液：
(a)四羟有机鏻盐(THP+)；
(b)选自尿素或硫脲的有机氮化合物；和
(c)选自正-十二烷胺(C12H25NH2)、正-十八烷胺(C18H37NH2)、和含有正-十六烷胺(C16H33NH2)、正-十八烷胺(C18H37NH2)和正-二十烷胺(C20H41NH2)的牛脂胺的具有12～20个碳原子的脂肪胺，
并且THP+盐(a)与有机氮化合物(b)和胺(c)的和的摩尔比为a∶(b+c)的范围为4∶1～1.5∶1。
优选，a∶b∶c的摩尔比范围为4～1.5∶0.95～0.75∶0.25～0.05。
本发明也提供了一种制造上述组合物的方法，所述方法包括下列步骤：
(i)将THP+盐(a)放入反应釜中，使用无机碱将其pH值调至6.0；
(ii)将选自尿素或硫脲的有机氮化合物(b)溶于THP+盐/碱溶液；
(iii)向混合物[(a)+(b)]中加入选自正-十二烷胺(C12H25NH2)、正-十八烷胺(C18H37NH2)、和含有正-十六烷胺(C16H33NH2)、正-十八烷胺(C18H37NH2)和正-二十烷胺(C20H41NH2)的牛脂胺的具有12～20个碳原子的脂肪胺(c)；
(iv)将混合物[(a)+(b)+(c)]在回流的温度保持3至4小时直到全部的胺溶解，使之形成(a)和(b)的缩合产物；
(v)冷却产物；和
(vi)向产物中加入足够的水制成所述产物的稳定的60％含水溶液。
本发明提供了一种适用于使纺织品具有阻燃性和织物柔软性的组合物，在所述组合物中含有下述反应的产物：
(a)一种四(羟有机)鏻(THP+)盐；
(b)一种有机氮化合物；及
(c)具有12或更多的碳原子的脂肪族，羟基活性的化合物。
本发明还提供了一种由前一段描述的组合物处理的纺织品。
本发明还提供了生产前述组合物的方法，该方法包括下述步骤：
(i)将THP+盐(a)放入容器中，使用无机碱将其pH值调至约6.0；
(ii)将有机氮化合物(b)溶于THP+盐/碱溶液中；
(iii)向混合物[(a)+(b)]中加入化合物(c)；
(iv)在适当的温度将混合物[(a)+(b)+(c)]保持足够的时间，使之形成(a)和(b)的缩聚物；
(v)冷却产物；且
(vi)向产物中加入足够的水制成所述产物的稳定溶液。
本发明进一步提供了按前一段描述的方法制成的组合物。
THP+盐(a)优选四(羟烷基)鏻盐，例如氯化四羟甲基鏻(THPC)或硫酸化四羟甲基鏻(THPS)。
有机氮化合物(b)优选酰胺，例如尿素或硫脲。
化合物(c)可以是，例如下列的一种或几种(每种至少含有一个具有12个碳或更多的碳原子的烷基基团)：
(i)伯胺
(ii)仲胺
(iii)叔胺
(iv)二元胺
(v)季铵盐
(vi)乙氧基化胺
(vii)乙氧基化二元胺
(viii)胺氧化物
(ix)烷基氨基取代的羧酸
(x)酰胺
(xi)乙氧基化酰胺
(xii)酰胺-咪唑啉
(xiii)硅氧烷衍生物
(xiv)硅烷衍生物
其中化合物(c)是胺，它可以是，基本上由正-十二烷胺(C12H25NH2)或正-十八烷胺(C18H37NH2)组成。
可选择地，化合物(c)可以是牛脂胺，确信其组成含有正-十六烷胺(C16H33NH2)，正-十八烷胺(C18H37NH2)和正-二十烷胺(C20H42NH2)。
特别地，THP+盐(a)与有机氮化合物(b)和化合物(c)的和的摩尔比，即：a∶(b+c)的范围为4∶1～1.5∶1，优选2.5∶1～3∶1。
例如，a∶b∶c的摩尔比可以是下列任一个：
      4      ∶    0.95    ∶    0.05
      3.5    ∶    0.95    ∶    0.05
      3      ∶    0.95    ∶    0.05
      2.5    ∶    0.95    ∶    0.05
      2.5    ∶    0.9     ∶    0.1
      2.5    ∶    0.75    ∶    0.25
      2.0    ∶    0.95    ∶    0.05
      2      ∶    0.9     ∶    0.1
或    1.5    ∶    0.95    ∶    0.05
纺织品基本上由100％的纤维素纤维(如棉花，亚麻，黄麻，粗麻布或再生纤维素材料)构成。
可选择地，纺织品可由纤维素纤维和非纤维素纤维构成。非纤维素纤维可以是，例如，羊毛或丝纤维或它含有合成纤维如聚酯，聚酰胺，丙烯酸或芳族聚酰胺纤维。
纺织品最好是一种有纤维素纤维(例如，棉花)或可以含有棉纤维和聚酯纤维，例如，60％棉纤维和40％聚酯纤维。
在本发明的方法中，在第(i)步使用的无机碱可以是，例如，氢氧化钠或氢氧化钾。
在本方法的第(iv)步，混合物可以，例如，在回流温度下保持3-4小时。这一步可在大气压或高于大气压，例如，约1.25bar条件下进行。
在本方法的第(vi)步，足够的水可以是加入水至使产物成为60％的稳定溶液。
尽管本发明没有指出所依据的特定的理论，但可以确信，将THP+盐的pH值调至约6.0可使其对有机氮化合物有更高的活性。而且还可以相信，被处理的纺织品的柔软控制(悬垂度)可被证明部分地是由交联度的降低引起的，这种交联度的降低是由于THP+盐/化合物(c)缩聚到材料上和/或由于在链中存在化合物(c)引起的。而且，进一步可以相信，依照本发明处理纺织品可导致其撕裂强度和耐磨性增加。
下列实施例将具体说明本发明：
实施例1：
向一装有冷凝器的2升树脂釜中加入1400g氯化四羟甲基鏻(THPC)。加入75g 50％氢氧化钾溶液将pH值调到约为6。向树脂釜中加入132g尿素，并搅拌使之溶解。向釜中加入38g正-十八烷胺(可从ARMEEN*HTD获得)，并升高温度使其回流。将混合物在回流温度保持3-4小时，直到所有胺全部消失。停止加热，加入水制成60％的溶液。
THPC∶尿素∶正-十八烷胺的摩尔比为2.5∶0.95∶0.05。
将一重量为280g/m2的100％棉织物用上述液体浸轧，轧液率为40％PROBAN*，操作依据已知的PROBAN*工艺。整理后织物有干添加率为18.5％缩聚产物。
经过上述液体处理的织物，通过德国(a)，法国(b)和英国(c)FR试验，在93℃条件下经过40次循环洗涤，织物在洗涤前后均含有2.75％的P和2.38％的N。
实施例1注解：
*：ARMEEN和PROBAN是注册商标。
(a)西德工业标准D IN 66083 s-b
(b)NFG 07-184
(c)BS 6249
实施例2-6
按实施例1重复操作，用量和结果列于下面的表1：
表1
实施例号 (a)THPC(g) 50％KOH(g) (b)尿素(g) (c)胺(g)     摩尔比(a∶b∶c) 干添加率(％) 试验织物含量
  P(％)     N(％)
    23456  11901428119014281190     60756075101  108171108162108 48*36*48*72*18.5+  2.5∶0.75∶0.252.0∶0.95∶0.252.5∶0.9∶0.12∶0.9∶0.12.5∶0.9∶0.1   17.61917.619-   2.62.772.62.62.96     2.252.552.252.442.52
*：正-十八烷胺
+：正-十二烷胺
实施例2-6都经过列于实施例1中的阻燃性试验。
实施例7-10
重复操作实施例1的过程，但这些实施例只涉及制备这些阻燃的组合物而不将它们用于纺织品。用量列于下面的表2中：
表2
实施例号 (a)THPC(g) 50％KOH(g) (b)尿素(g) (c)胺(g)     摩尔比(a∶b∶c) 注解
  78910  1190119011901074     60606060   957181.4171   20151736   3∶0.95∶0.054∶0.95∶0.053.5∶0.95∶0.051.5∶0.95∶0.05 形成了聚凝胶
使用实施例1-6(上述)产物处理的织物与按前述GB-A-2040299中所描述的处理的织物相比，其手感和悬垂性有了很大提高。
实施例11-15
重复操作实施例1的过程，但摩尔比THPC∶尿素∶胺为3∶0.95∶0.05，其压力，温度和时间列于下面的表3：表3
  实施例 温度(℃) 压力Bar(巴) 时间(分钟)
    11     105-108   Atmospheric     180
    12     110     0.5     150
    13     130     1.25     20
    14     130     1.25     20
    15     130     1.25     20
将重量为280g/m2的100％棉织物用上述产品处理。经测试发现处理过的织物中磷和氮的含量分别为3％和2.5％，并在93℃洗涤40次后通过了德国，法国，英国和新欧洲PrEN 533的阻燃性测试。
实施例16-20
重复实施例11，并使用下列表4中所列的织物：
表4
实施例   织物组成％棉    PET*     结构   织物重量g/m2
    16  100    0   斜纹布     280
    17  100    0   平纹布     155
    18  100    0(印有颜色的)   平纹布     185
    19  75     25   斜纹布     255
    20  65     25   斜纹布     280
所处理的织物在经过耐洗性洗涤后通过了德国，法国，英国和新欧洲PrEN 533的阻燃性标准。
*-PET＝聚对苯二甲酸乙二(醇)酯
下面表5列出了织物在经过耐洗试验前后P和N的含量结果：
表5
实施例 P&N％含量(未洗涤的)P％    N％    P&N％含量(经过洗涤)P％     N％
    1617181920     3.054.552.983.023.49     2.463.652.452.462.81     2.84-2.103.012.97     2.26- *1.632.242.42
而且，织物显示出优秀的手感和悬垂性。另外，处理过的织物是防水的。*实施例17中，使织物与氧化剂在无洗涤剂下一起在74℃洗涤200次。在经过洗涤后，织物中磷含量为2.80％且氮含量为2.21％，且它能通过BS 5867第二部分的B型试验。

Claims (5)

1.一种适用于使纺织品具有阻燃性和织物柔软性的组合物，其特征在于所述组合物包括由下列反应所得的产物的稳定的60％含水溶液：
(a)四羟有机鏻盐(THP+)；
(b)选自尿素或硫脲的有机氮化合物；和
(c)选自正-十二烷胺(C12H25NH2)、正-十八烷胺(C18H37NH2)、和含有正-十六烷胺(C16H33NH2)、正-十八烷胺(C18H37NH2)和正-二十烷胺(C20H41NH2)的牛脂胺的具有12～20个碳原子的脂肪胺，
其特征还在于THP+盐(a)与有机氮化合物(b)和胺(c)的和的摩尔比为a∶(b+c)的范围为4∶1～1.5∶1。
2.权利要求1的组合物，其特征在于THP+盐(a)是氯化四羟甲基鏻(THPC)或硫酸化四羟甲基鏻(THPS)。
3.权利要求1的组合物，其特征在于a∶b∶c的摩尔比范围为4～1.5∶0.95～0.75∶0.25～0.05。
4.一种制造权利要求1组合物的方法，其特征在于所述方法包括下列步骤：
(i)将THP+盐(a)放入反应釜中，使用无机碱将其pH值调至6.0；
(ii)将选自尿素或硫脲的有机氮化合物(b)溶于THP+盐/碱溶液；
(iii)向混合物[(a)+(b)]中加入选自正-十二烷胺(C12H25NH2)、正-十八烷胺(C18H37NH2)、和含有正-十六烷胺(C16H33NH2)、正-十八烷胺(C18H37NH2)和正-二十烷胺(C20H41NH2)的牛脂胺的具有12～20个碳原子的脂肪胺(c)；
(iv)将混合物[(a)+(b)+(c)]在回流的温度保持3至4小时直到全部的胺溶解，使之形成(a)和(b)的缩合产物；
(v)冷却产物；和
(vi)向产物中加入足够的水制成所述产物的稳定的60％含水溶液。
5.权利要求4的方法，其特征在于在(i)步骤中所用的无机碱是氢氧化钠或氢氧化钾。
CN95120388A 1994-10-25 1995-10-25 纺织品的阻燃和织物柔软处理 Expired - Lifetime CN1083913C (zh)

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