CN1064092C - 阻燃纤维和非织造织物 - Google Patents

阻燃纤维和非织造织物 Download PDF

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CN1064092C
CN1064092C CN95107713A CN95107713A CN1064092C CN 1064092 C CN1064092 C CN 1064092C CN 95107713 A CN95107713 A CN 95107713A CN 95107713 A CN95107713 A CN 95107713A CN 1064092 C CN1064092 C CN 1064092C
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中嶌裕司
谷口雅彦
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Abstract

本发明提供了一种氧化或燃烧时不产生二英相关的化合物的热塑性树脂纤维，并且即使用较低的阻燃剂时，其阻燃性也极为优异。这种阻燃纤维含有5-15%重量的具有下列通式(1)的阻燃剂：
通式(1)中R1至R5和R1′至R5′独立表示Br或Cl，比例Br/Cl为100/0至40/60，n为整数2至16，2-8%重量的作为阻燃促进剂的氧化锑，以及0.02至1%重量的烷基部分具有12至18个碳原子的沉积在纤维表面上的烷基磷酸盐。

Description

阻燃纤维和非织造织物
本发明一般涉及阻燃纤维和由这种纤维形成的非织造织物，更特别涉及燃烧时不形成二噁英相关化合物的阻燃纤维及由这种纤维制备的非织造织物、机织织物和形成的产品。
合成纤维，诸如由尼龙、聚酯、聚丙烯等形成的，因其优异的物理和化学性质，目前发现广泛应用于形成布、窗帘、地毯和其它材料。然而，这些纤维是可燃的；所以当用作车内和房屋装璜等时，需要具有阻燃性。
使纤维具有阻燃性一般是通过将阻燃剂加入原料聚合物中或用阻燃剂后处理纤维来实现的。
在其中加有阻燃剂的聚合物的典型例子，如日本专利特开昭58(1983)-156019公开的，是与微细颗粒状阻燃剂混合的聚烯烃复合纤维，其中阻燃剂的分解温度至少高于纺丝温度100℃。
公开日本专利特开昭54(1979)-134120的另一基于聚酯的典型复合纤维，包括含磷和／或卤素的聚酯组分和形成纤维的聚酯组分。
在已知的可加入原料聚合物的阻燃剂中，存在一种具有用很小量就可使聚合物充分阻燃优点的十溴联苯醚。这样得到的纤维具有聚合物本身的性质，但存在的缺点是燃烧时形成与二噁英相关的化合物。由已知与二噁英相关的化合物具有致癌作用，因此预料在不久的将来，将禁止使用十溴联苯醚。
为使聚合物充分阻燃，其它具有防止生成二噁英相关物质结构的阻燃剂(例如：磷酸三(甲苯酯)、磷酸铵和氢氧化铝)必须大剂量加入原料聚合物中。所以，这些阻燃剂，如果不加入足够量，就会具有使聚合物纤维物理性质变差的缺点，这样费用显然将有所增加。
对于用阻燃剂后处理纤维，可将用水或有机溶剂稀释的阻燃剂通过浸渍或喷洒沉积于纤维或织物上。例如，日本专利特开昭48(1973)-13696公开了用含磷的有机卤素型阻燃剂喷洒的热塑性树脂纤维。用这种方法，使纤维或织物阻燃相当容易。然而，这种方法的问题是阻燃剂以粉末状从纤维表面分离出来，或洗涤时容易从纤维中分离。
因此，本发明的目的是提供价廉物美的纤维，这种纤维即使燃烧时也不形成二噁英相关的化合物，并且即使使用少量的阻燃剂时也可保持所需的阻燃性。
通过为达到上述目的进行的广泛深入研究，已发现通过使用下面的阻燃剂有可能获得需要的阻燃纤维。
本发明的一个方面涉及含基于纤维总重量的5-15％(重量)的作为阻燃剂的具有下列通式(1)的化合物和2-8％(重量)的作为阻燃促进剂的氧化锑：
通式(1)：
Figure 9510771300051
其中R1至R5和R′1至R′5独立为Br或Cl，比例Br／Cl为100／0至40／60，n为2-16的整数。
本发明的第一方面在下面将详细解释。
对于本发明中用于阻燃纤维的热塑性树脂，涉及到α-烯烃均聚物的例子如聚丙烯，聚乙烯，聚丁烯-1和聚-4-甲基戊烯-1，丙烯与其它α-烯烃二元共聚物和三元共聚物，聚对苯二甲酸乙二醇酯及乙烯-醋酸乙烯酯共聚物，在这些聚合物中，考虑到用来纺丝和承受梳理等的能力，优选使用熔点约115℃或更高并且为结晶性的聚烯烃树脂。
本发明中用作阻燃剂的具有上述通式(1)的化合物的熔点约为345℃，分解温度约为360℃。这种化合物，因其分子中无醚键，燃烧时不生成二噁英相关的化合物。同时，此化合物，因其含溴量高于已知的阻燃剂，可减少用量使纤维具有较高阻燃性能。在通式(1)中，需要n为2至16，优选2至5，原因是n=1的化合物结构不稳定。在此化合物中，比例Br／Cl优选为100／0至70／30，因为比例小于40／60时，取得的阻燃性效果较差。
本发明中，加入纤维中的阻燃剂的量为基于纤维总重量的5-15％(重量)。应注意加入纤维中阻燃剂量的上限依纤维的纤度而变化。对于纤度的约1至20d／f的纤维，阻燃剂的优选用量为约5．0至8％(重量)，对于纤度为约21至100d／f的纤维，阻燃剂用量为约5．0至12％，对于纤度为约100至5000d／f的纤维，阻燃剂用量为约5至15％。
阻燃促进剂为三氧化锑或五氧化锑，在纤维中的加入量为纤维总重量的2-8％，或通常为阻燃剂量的一半。
在其中加有阻燃剂和阻燃促进剂的热塑性树脂可用已知的熔融纺丝技术制成纤维，然后进行拉伸和折皱。这种熔融纺丝技术，例如包括单或复合纺丝法，纺粘法和熔体喷射法。对阻燃纤维的纤度无特别限制，即：它们的纤度依据其使用的目的进行选取，例如，纤度为约0．5至1，000d／f的纤维用于形成短纤维或多纤维丝，纤度为约50至5，000d／f的用于形成单纤丝。
本发明的阻燃纤维可以为复合纤维形式如皮芯型、并列型、天星型和多分裂型纤维。皮芯型纤维可同时在外皮和芯线部分中含相同量或不同量的阻燃剂和阻燃促进剂。此外，皮芯和芯线部分都可以含已知的改性剂如消光剂、抗静电剂、导电剂、颜料或其它聚合物。
本发明的另一方面涉及在上述本发明第一方面中的阻燃纤维中加入0．02至1％(重量)的表面处理剂得到的阻燃纤维，其中表面处理剂为具有12至18碳原子的烷基的烷基磷酸盐。这种烷基磷酸盐的例子有十二烷基磷酸钾、十四烷基磷酸钾、十六烷基磷酸钾和十八烷基磷酸钾或其钠盐。用这种表面处理剂沉积其上的纤维具有抵抗因气体引起的褪色的极佳性能。当沉积在纤维上的表面处理剂的量低于0．01％(重量)时，对于抵抗因气体引起的褪色无充分改进，而当沉积在纤维上的量超过1％(重量)时，会造成纤维具有粘性，换言之，沉积量超出0．02％至1％(重量)范围不是优选的。
本发明的再一方面涉及通过使用聚烯烃作为原料聚合物得到的阻燃纤维，由这种阻燃纤维形成的非织造织物，由这种阻燃纤维形成的机织织物和由这种阻燃纤维形成的产品。
本发明的实施方式将用一些优选实施例进行解释。其中涉及到的物理或其它性质用如下方式进行测试：
阻燃性：
切割一基重为300g／m2的非织造织物的2．5cm×30cm测试片，将其固定呈30°角，在较底端用火柴点10秒钟。完全着火后，测量试片连续燃烧多长时间。燃烧时间为6秒或更短的试片被认为阻燃性能可接受。如果样品经过20次燃烧试验后得到超过80％的试验其阻燃性可接受，就认为可接受。
因气体引起的褪色：
切割一基重为300g／m2的针刺非织造织物的40cmm×40cm试片，并将其悬挂在交通拥挤的路边的货栈的屋檐上。经过150天时间间隔后，此非织造织物的褪色情况根据JIS-L0805测量污染的灰度，灰度为1至5分表示严重至轻度污染。
存在或无二噁英相关的化合物：
使用气相色谱和质谱连用，可检测出在阻燃试验过程中产生的燃烧气体内是否存在二噁英及其相关的化合物。
实施例1-3
按表1中的重量比将十溴联苯乙烷和三氧化锑加入聚丙烯粉末中，其中聚丙烯粉末在230℃时测量，10分钟内的熔体流动速率为21，熔点为163℃，得到混合物的总重量为100％，然后将混合物用单螺杆挤出机进行造粒。
将得到的各种颗粒在260℃温度下，通过一具有60个直径为1．5mm喷丝孔的喷丝板进行熔融纺丝制得54d／f的纤维。将此短纤维在90℃下以拉伸比3．0进行拉伸，用折皱机制得每25mm具有12皱缩，并用切断机切成具有单丝纤度为18．0d／f和纤维长度为64mm的纤维丝。在实施例1和2中，将0．3％(重量)的作为表面处理剂的十二烷基磷酸钾沉积在每种纤维丝上，在实施例3中，将作为表面处理剂的十二烷基磷酸钾沉积在纤维丝上。
用梳理机将每种纤维丝梳理成梳理纤维网，将此纤维网依次进行针刺获得具有重量为300g／m2的地毯。测量此地毯的阻燃性、因气体引起的褪色和在燃烧气体中是否存在二噁英相关的混合物。得到的结果列于表1中。
实施例4
将与实施1中相同的阻燃剂和阻燃促进剂按与实施例1相同的量加入高密度聚乙烯粉末中，并造粒得到用作复合纤维的第一组分，其中高密度聚乙烯粉末在190℃测量，10分钟内的熔体流动速度为22，熔点为134℃。本实施例中的第二组分为其中加有实施例2使用的阻燃剂的聚丙烯。
使用一具有100个直径为0．8mm纺丝孔的皮芯型复合纺丝板，在上述第一和第二组分在复合物重量比为1∶1和相同的纺丝温度260℃同时将第一和第二组分分别置于外和芯线面上条件下进行熔融纺丝。即得纤度为18d／f的皮芯型复合纤维丝。将0．3％(重量)的用作表面处理剂的十二烷基磷酸钾沉积在这种丝上。将这种短丝在90℃温度下，以拉伸比3进行拉伸，并用折皱器使每25mm上具14个皱缩，然后用切断机切成单纤维纤度为6．0d／f，纤维长度为64mm的阻燃纤维丝。用梳理机将这种纤维丝梳理成梳理纤维网，将此纤维网依次进行针刺得到重量为300gm2的地毯。然后将得到的地毯在145℃下用热空气干燥机热处理4分钟制得在纤维交叉点热熔化相连接的地毯。发现这种地毯在80％或更多试验中显示可接受的阻燃性，同时抵抗因气体引起的褪色的灰度为4。
最后得到的地毯可铺在车内或房间里，其背面可有或无聚乙烯或发泡聚氨酯叠层。这种地毯也可以经加热后模压，这样可使其较好的适应模的轮廓。
这些地毯的性能如表1所示。发现实施1和2中得到的产品具有可接受的足够的阻燃性，无二噁英生成。发现用0．3％(重量)表面处理剂沉积其上而得的产品具有可接受的抵抗因气体引起的褪色(实施例1和2)。
然而，用0．01％(重量)表面处理剂沉积其上的产品，虽然其阻燃性可接受并不会产生二噁英，但对于抵抗因气体引起的褪色稍差。
对比例1-3
按照实施例1制备聚丙烯混合物，不同的是用亚乙基双四溴苯邻二甲酰亚胺(对比例1)、十溴联苯醚(对比例2)和磷酸铵及三嗪衍生物(对比例3)作为阻燃剂。
与实施例1一样，将这些混合物进行熔融纺丝、沉积表面处理剂、针刺和其它加工方法得到地毯，并测其物理性质，估算结果如表1所示。
对比例1和2中的纤维其阻燃性和抵抗因气体引起的褪色性都可接受，但发现燃烧时产生二噁英。
对比例3的纤维阻燃性差，因此必须含有更多阻燃剂以达到充分阻燃，但抵抗因气体引起的褪色性较差。用0．30％(重量)的实施例1中表面处理剂沉积在此纤维上。但在气体褪色试验中变成粉红。据信这是由于加入的阻燃剂与表面处理剂反应的结果。
表1
Figure 9510771300111
①十溴联苯乙烷
②亚乙基双四溴苯邻二甲酰亚胺
③十溴联苯醚
④磷酸铵／三嗪衍生物
从表1可证明，本发明的阻燃剂的纤维，阻燃性优异并且当燃烧时不会产生二噁英相关的化合物。表面处理沉积还改进了抵抗因气体引起的褪色性。
所以，本发明的阻燃纤维可进行针刺、栽绒、织造和其它加工；因而它们可用作安全的汽车装饰材料、地毯、窗帘和其它用于房间和建筑物的材料。

Claims (5)

1．一种阻燃纤维，包括5-15％重量的具有下列通式(1)的阻燃剂：
Figure 9510771300021
其中(1)中R1至R5和R′1至R′5独立为Br或Cl，比例Br／Cl为100／0至40／60，n为2-16的整数；
2至8％重量的作为阻燃促进剂的氧化锑；以及
0．02至1％重量的烷基部分具有12至18个碳原子的沉积在纤维表面上的烷基磷酸盐。
2．根据权利要求1的纤维，其中包括聚烯烃纤维。
3．由根据权利要求1至2任何一项的阻燃纤维制备的非织造织物。
4．由根据权利要求1至2任何一项的阻燃纤维制备的机织织物。
5．由根据权利要求1至2任何一项的阻燃纤维制备的模塑产品。
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