CN1289377A - 发光纤维及其制造方法和应用 - Google Patents

发光纤维及其制造方法和应用 Download PDF

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CN1289377A
CN1289377A CN99802369A CN99802369A CN1289377A CN 1289377 A CN1289377 A CN 1289377A CN 99802369 A CN99802369 A CN 99802369A CN 99802369 A CN99802369 A CN 99802369A CN 1289377 A CN1289377 A CN 1289377A
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pigment
inorganic light
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A·西格尔
T·波特拉瓦
H·朗海姆
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Honeywell Specialty Chemicals Seelze GmbH
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Abstract

包含至少一种成纤材料的发光纤维,该成纤材料中分散有至少一种无机发光颜料,所述无机发光颜料的平均粒度为1—30微米。

Description

发光纤维及其制造方法和应用
本发明涉及含至少一种成纤材料的发光纤维。该成纤材料中分散有至少一种无机发光颜料。
由于用可溶有机紫外活性染料染色而发光的纤维是已知的。这些聚酰胺或粘胶纤维例如用于有价证券，以证实其真实性。视所用的染料或染料混合物而异，这些纤维在紫外辐射激发下发出绿色、黄色、红色或兰色的光。然而，这些有机染色纤维的缺点是耐光牢度低，而且有机紫外活性染料既不能发出红外光也不能发出磷光，所以这些纤维不能用作有机证券的安全标志。
DE-A-19539315描述了含有平均粒度小于1微米(较好为0.5-0.7微米)的0.01-5％(重量)无机发光体的发光再生纤维素纤维。这些无机发光体都是掺有锰、锑、锡、铅、铜、银或稀土元素的碱土金属、过渡元素或稀土元素的磷酸盐、钨酸盐、氧化物、硅酸盐和铝酸盐，碱金属或碱土金属的卤化物。这些发光体的耐光性优于有机染料，但也不能产生磷光和红外发光效应，且只能产生低的发光强度。这可能会导致某些不确定的结果，例如在检验用这些发光体标志的有价证券时。
本发明的目的是提供特别适用于有价证券的发光纤维。这些发光纤维产生荧光或磷光作用，具有高的耐光牢度，且在可见和/或不可见光谱范围内具有强的发光效应。
这个目的可由本发明的发光纤维达到。本发明的发光纤维包含至少一种成纤材料，该成纤材料中分散有至少一种无机发光颜料，该无机发光颜料的平均粒度为1-30微米。
由于DE-A-19539315清楚地表明无机发光体的平均粒度宜小于1微米，且在背景技术讨论中引证日本专利公开87-327866时指出当将硫氧化钇发光体颜料研至粒度为1微米以下时，会失去其发光效应，所以通过选择发光颜料的特定平均粒度能增强发光度是令人惊奇的。
本发明中成纤材料的选择不受任何特定的限制，只要它能与要求粒度的发光颜料混和。本发明发光纤维中的成纤材料较好是粘胶，因为由其制成的发光纤维能与常规纤维素基纸原料高度相容，且可用各种印刷方法(如平版印刷法)印刷，从而使用这种纤维没有造纸(特别是有价证券)方面的问题。本发明的纤维也可用于纺织品领域，以隐蔽或公开标志高级品牌产品。强的发光体和高的耐光性使得本发明的纤维特别适用于标志各种含纤维的制品，如纺织品、纸，特别是有价证券。
本发明中所用的无机发光颜料的平均粒度较好为2-30微米，更好为4-20微米，最好为5-20微米。本发明发光纤维中发光颜料的用量可以在宽的范围内变化，按无水纤维总量计较好为0.01-50％(重量)，更好为5-50％(重量)。按无水纤维总量计，优选的百分数为7-40％(重量)，特别好为10-20％(重量)。
特别适用于本发明中的无机发光颜料在可见或紫外辐射的激发下产生磷光效应。为了让发光颜料能产生磷光效应，它们的发光必然涉及能量储存过程，从而在激发结束后至少仍有部分发光。磷光作用的优点是一种确保机器可读性和允许激发位置和测试位置可分开的简单方法。即使用白光也可激发磷光效应，从而足以在黑暗的环境中进行目测。这样有利于核对产品(如纺织品)的安全编码和核对有价证券。
本发明宜使用的无机发光颜料在波长为200-680纳米的可见或紫外辐射激发后可产生波长为380-680纳米的可见光。
较好使用掺有一种或多种过渡金属元素或镧系元素的硫化锌、硫化锌镉、碱土金属铝酸盐、碱土金属硫化物或碱土金属硅酸盐。例如，掺铜的硫化锌产生绿色的磷光，掺镧系元素的碱土金属铝酸盐、碱土金属硫化物或碱土金属硅酸盐产生绿色、兰色或红色的磷光，掺铜的硫化锌镉视含镉量的不同产生黄色、橙色或红色磷光。
优选的是掺有铕的碱土金属铝酸盐和除铕外还含有另一个稀土元素共活化剂(特别是镝)的碱土金属铝酸盐。上述特别有用的碱土金属铝酸盐描述于EP-A-0622440和US 5376303中。这两个专利全部参考引用于本发明中。
另一组可用于本发明的无机发光颜料在紫外辐射激发时产生磷光效应。这些颜料在紫外辐射激发时产生绿色、黄色或兰色的光线。用简单的市售紫外光源可证实是否存在紫外活化的发光材料。这在使用时可能构成一个优点，但在其它情况下(如有价证券)可能产生缺点，因为未经授权的人员也可知道是否存在安全装置。
较好的一组发光颜料在波长为200-680纳米的紫外辐射激发时产生波长为380-680纳米的可见光。特别好的一组发光颜料为均掺有一种或多种过渡金属元素或镧系元素的硫化锌、氧化锌、硫氧化锌、硅酸锌或铝酸锌。例如，掺铜的硫化锌产生绿色的荧光，掺银的硫化锌产生兰色的荧光，掺有过渡金属或镧系元素的氧化锌、硫氧化锌、硅酸锌或铝酸锌产生绿色、兰色或红色的荧光。
本发明所用的另一组优选的发光颜料是一组红外活化的发光颜料，即含有红外活化发光体的颜料，其发光过程包括至少部分波长在680纳米以上的长波、红外辐射。这些颜料不仅包括在波长为680纳米以上的红外辐射激发时产生波长为680纳米以下的短波发光辐射的反斯托克斯发光体，还包括在波长为680纳米以下的较短波长辐射的激发时产生波长为680纳米以上的红外辐射的斯托克斯发光体。这些反斯托克斯发光体具体描述WO98/39392及其引用的现有技术。该专利同样全部参考引用于本发明中。这组发光颜料也包括在红外辐射激发时产生不同波长红外辐射的红外-红外转换发光体。
本发明发光纤维的制造方法是简单的，只需将掺有活化剂的无机发光颜料加入成纤材料或其溶液，然后由其纺成纤维。例如将掺杂的颜料加入粘胶原液中，然后用粘胶纺丝法将粘胶原液纺成纤维。同样可将掺杂的颜料加入纤维素溶液中，然后例如按铜氨法、溶纺纤维素(lyocell)法或按低取代纤维素醚的方法将其纺成纤维。有用溶剂的一个实例是氧化N-甲基吗啉/水。
与合适的激发源相结合，这种粘胶纤维可用于产品的安全标志，从广义上说可用于鉴定和控制纺织品、有价证券、安全纸的自动识别。这方面，必须使用难于伪造且与其它安全装置结合也难以生产出的材料和安全装置。也需要具有任何人都可目测的简单方法，如有必要且视安全等级不同，安全装置仅由熟练分析人员才可检测。与用常规安全印刷技术均匀涂布相应的发光颜料相比，发光纤维可以有局部的高信号强度和更好的信噪比。制造安全装置的长期目的是在科学技术上超过伪造者，从而由于安全装置的复杂性而减少伪造的动机。
本发明的纤维提供了很多应用优点，如简单、快速、非接触和经济的检测方法、机器可读性、与其它效果的相容性、被不同的波长特定激发和在不同波长激发时产生不同的发光颜色。本发明的材料可用于制造不能复制的纺织品、有价证券和安全纸，且与纤维素基原料高度相容，可用各种印刷方法(如浮凸印刷法、平版印刷法)印刷，可与安全印刷油墨或其它安全装置相组合。
与合适的激发源相结合，产生磷光作用的本发明发光粘胶纤维例如可用于产品的公开安全标志及其鉴别。由于用天然或人工白光就能激发磷光效应，且可在暗处通过目测验证安全装置，本发明的磷光作用纤维为任何人提供了简单、快速、非接触和经济验证的使用优点。另外，使用光检测器也提供了简便的机器可读性，这时磷光效应允许激发位置与验证位置在空间上相互分离。
产生荧光效应而不产生磷光效应的本发明纤维同样可被任何人检测，但检测所需的紫外激发足以增加检测的难度，由此产生了更高的安全等级。
使用红外活性的发光体标记和防伪有价证券，产生了更高级别的安全性。其中，红外活性发光颜料的低信号强度大大提高了激发和验证所需的分析难度，因此对检测是否存在安全装置也很困难。
实施例1
室温下将含9重量份纤维素的纺丝溶液与发光颜料的分散体混合。上述分散体的制备方法是将100重量份平均粒度为5微米和掺有400ppm铜的硫化锌搅拌入聚乙烯醇、水和Orotan润湿剂的溶液，形成含22重量份单分散性发光颜料、2.8重量份聚乙烯醇和0.05重量份Orotan的分散体。用筛目大小为40微米的市售筛子过滤上述分散体，与10000重量份纺丝溶液混合，并在生产条件下将其纺入酸性纺丝浴。干燥时所得的纤维在紫外辐射激发时具有绿色的荧光。
实施例2
通过将100重量份平均粒度为5微米和掺有400ppm铜的硫化锌直接与10000重量份纺丝溶液混合，用筛目大小为40微米的市售筛子过滤，并在生产条件下将其纺入酸性纺丝浴，重复实施例1。干燥时所得的纤维在紫外辐射激发时具有绿色的荧光。
实施例3
通过将225重量份平均粒度为5微米和掺有400ppm铜的硫化锌与10000重量份纺丝溶液混合形成分散体，并在生产条件下将其纺入酸性纺丝浴，重复实施例1。干燥时所得的纤维在紫外辐射激发时具有绿色的荧光，其光强度高于实施例1。
实施例4
通过将100重量份平均粒度为20微米和掺有80ppm铜和5ppm钴的硫化锌与10000重量份纺丝溶液混合形成分散体，并在生产条件下将其纺入酸性纺丝浴，重复实施例1。干燥时所得的纤维在紫外辐射激发时具有绿色的荧光，在白光激发时产生绿色的磷光。
实施例5
通过将100重量份平均粒度为10微米和掺有12％镱和8％铕的硫氧化钇与10000重量份纺丝溶液混合形成分散体，并在通常生产条件下将其纺入酸性纺丝浴。重复实施例1。干燥时，所得的纤维在红外辐射激发时具有绿色的荧光。

Claims (11)

1．发光纤维，它包含至少一种成纤材料，该成纤材料中分散有至少一种无机发光颜料，其特征在于所述无机发光颜料的平均粒度为1-30微米。
2．如权利要求1所述的发光纤维，其特征在于所述无机发光颜料的平均粒度为4-20微米，较好为5-20微米。
3．如权利要求1或2所述的发光纤维，其特征在于按无水纤维总量计，所述无机发光颜料的含量为5-50％重量，较好为7-40％重量，最好为10-20％重量。
4．如权利要求1-3中任一项所述的发光纤维，其特征在于所述成纤材料是粘胶。
5．如权利要求1-4中任一项所述的发光纤维，其特征在于在可见或紫外辐射激发时，所述的无机发光颜料产生至少一部分磷光效应。
6．如权利要求5所述的发光纤维，其特征在于所述的发光颜料包括掺有一种或多种过渡金属元素或镧系元素的硫化锌、硫化锌镉、碱土金属铝酸盐、碱土金属硫化物或碱土金属硅酸盐。
7．如权利要求1-4中任一项所述的发光纤维，其特征在于在紫外辐射激发时，所述的无机发光颜料产生至少一部分荧光效应。
8．如权利要求7所述的发光纤维，其特征在于所述的发光颜料包括掺有一种或多种过渡金属元素或镧系元素的硫化锌、氧化锌、硫氧化锌、硅酸锌或铝酸锌。
9．如权利要求1-4中任一项所述的发光纤维，其特征在于所述的有机发光颜料至少部分可被红外辐射激发。
10．一种制备如权利要求1-9中任一项所述的发光纤维的方法，其特征在于在成纤材料或其溶液中加入无机发光颜料，然后将其纺成纤维。
11．含有如权利要求1-9中任一项所述的发光纤维的含纤维制品，较好是纺织品、有价证券或纸。
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