CN1277644A - 非织造材料的制造方法 - Google Patents

非织造材料的制造方法 Download PDF

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CN1277644A
CN1277644A CN98810503A CN98810503A CN1277644A CN 1277644 A CN1277644 A CN 1277644A CN 98810503 A CN98810503 A CN 98810503A CN 98810503 A CN98810503 A CN 98810503A CN 1277644 A CN1277644 A CN 1277644A
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B·约翰森
L·芬格尔
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Abstract

通过水刺缠结纤维混合物制造非织造材料的方法,该纤维混合物含例如熔喷和/或纺粘纤维的连续长丝以及天然纤维和/或合成短纤维。该方法的特征在于,形成天然纤维和/或合成短纤维的泡沫化纤维网(14)并经水刺缠结使该泡沫化纤维分散体与连续长丝(11)缠结在一起而形成复合材料,其中连续长丝与剩余的纤维被很好地整体化。

Description

非织造材料的制造方法
发明背景
本发明涉及一种通过水剌缠结纤维混合物而制造非织造材料的方法，该纤维混合物含连续长丝以及天然纤维和/或合成短纤维。
水刺缠结法或射流喷网法(spunlace)是1970年代引入的技术，参见例如加拿大专利CA 841938。该方法包括用于法成网或者湿法成网形成纤维网，然后依靠高压下非常细的喷射水流使该纤维缠结。将几排喷射水流直对支撑在可移动金属丝网(wire)上的纤维网。然后干燥缠结的纤维网。在该材料中使用的纤维可为合成或再生短纤维，例如聚酯、聚酰胺、聚丙烯、粘胶等，浆粕纤维或浆粕纤维与短纤维的混合物。射流成网材料能够以高质量及趋于合理的成本制造，并且吸收容量高。它们可例如用作家庭或工业用的擦拭材料，用作医疗中的以及供卫生用途等的用可弃材料。
在WO96/02701中公开了泡沫化纤维网的水刺缠结法。纤维网中所包含的纤维可为浆粕纤维和其它天然纤维以及合成纤维。
由例如EP-B-0333211和EP-B-0333228已知，纤维组分之一为熔喷纤维的纤维混合物的水刺缠结法。基材即受水刺缠结的纤维状材料，要么由至少两层预制纤维层组成，其中一层由熔喷纤维构成；要么由“共成形(coform)材料”组成，其中实质上均质的熔喷纤维和其它纤维的混合物在金属丝网上被气流成网并接着进行水刺缠结。
由EP-A-0308320已知，将连续长丝网与含浆粕纤维和短纤维的湿法成网纤维材料合并在一起，并使各自成形的纤维网经水刺缠结在一起形成叠层。这样的材料中，因为水刺缠结期间纤维相互粘连且仅有非常有限的可移动性，从而不同纤维网中的纤维相互间将不能整体化。发明目的及最重要特征
本发明的目的是提供由纤维混合物制造水剌非织造材料的方法，该纤维混合物是例如熔喷和/或纺粘纤维形式的连续长丝与天然纤维和/或合成短纤维的混合物，其中纤维的选择有很大自由并且其中连续长丝与剩余的纤维被很好地整体化。按照本发明，通过使天然纤维和/或合成短纤维的纤维网泡沫化并使泡沫化纤维分散体与连续长丝水刺缠结到一起形成复合材料实现了这一点，其中连续长丝与剩余的纤维被很好的整体化。
经泡沫化，改善了天然纤维和/或合成纤维与合成长丝的混合，所述混合效果经水刺缠结得到加强，以致得到其中所有类型纤维实质上被相互均质混合的复合材料。和此特征一起的其它特征表现为，该材料非常高的强度性能以及宽的孔体积分布。附图描述
以下将参考附图所示的一些实施方案，对本发明进行更清楚的描述。
图1~5图示了装置的一些不同实施方案，该装置用于按本发明制造水刺非织造材料。
图6和7显示了作为参照材料的泡沫化射流喷网材料形式和仅由熔喷纤维组成的射流喷网材料形式的孔体积分布。
图8显示了本发明复合材料的孔体积分布。
图9以条形图形式显示了，复合材料及其中包括的两种基材料在干和湿条件下以及在表面活性剂溶液中的拉伸强度。
图10显示了按本发明所制非织造材料的电子显微镜照片。部分实施方案描述
图1图示了按本发明制造水刺缠结复合材料的装置。用熔喷设备10按照常规的熔喷技术形成熔喷纤维的气体流，例如用美国专利US 3,849,241或者US 4,048,364中已知的那种。简言之，该方法包括将熔融聚合物通过喷嘴以极细流挤出，并且将会聚的空气流指向聚合物流以使它们被牵伸而出，成为直径很小的连续长丝。该纤维依据它们的尺寸可以是微细纤维或大纤维。微细纤维的直径至多20微米，但通常其直径介于2和12微米之间。大纤维的直径在20微米以上，例如介于20~100微米之间。
原则上，所有的热塑性聚合物能用于制造熔喷纤维。可用聚合物的例子是聚烯烃例如聚乙烯和聚丙烯、聚酰胺、聚酯和聚交酯。当然也可以使用这些聚合物的共聚物以及具有热塑性的天然聚合物。
纺粘纤维用略有不同的方法制造，即挤出熔融聚合物，将其冷却并牵伸至适当的直径。这种纤维的直径通常在10微米以上。例如介于10和100微米之间。
以下将描述如熔喷纤维的连续长丝，但应理解为也可使用其它类的连续长丝，例如纺粘纤维。
按照图1所示的实施方案，熔喷纤维11被直接置于金属丝网12上，在此使它们形成比较疏松、开放的网结构，其中纤维相互间相对自由。实现这一点或是通过相对增大熔喷喷嘴和金属丝网之间的距离，以便长丝在它们落到金属丝网12上之前冷却下来，在12上它们的粘性降低；或是在它们落到该金属丝网上之前用一些其它方法使熔喷纤维冷却，例如通过喷淋液体。所形成熔喷层的单位面积重量(basis weight)应当介于2和100克/米2之间，且松密度介于5和15厘米3/克。
从高位流料箱15出来的泡沫化纤维网14被置于熔喷层的顶端。泡沫化是指由含水和表面活性剂泡沫液体中的纤维分散体形成纤维网。例如在GB 1,329,409、US 4,443,297和在WO96/02701中描述了此泡沫化技术。泡沫化纤维网具有非常均匀的纤维构造。为了更详细地描述泡沫化技术，引用上述文献作为参考。通过强化的泡沫效果，在此阶段将已经发生熔喷纤维和泡沫化纤维分散体的混合。离开高位流料箱15的强紊乱泡沫中生出的空气泡将向下渗透到可移动的熔喷纤维之间并推动这些纤维使其分开，以致更粗糙几分的泡沫化纤维将与熔喷纤维整体化。因此，在此步骤后，存在的将主要是整体化的纤维网而不再有不同纤维网的多层。
许多不同种类并且以不同比例混合的纤维可用于制造泡沫化纤维网。因此可以使用浆粕纤维或者浆粕纤维与例如聚酯、聚丙烯、粘胶、莱塞尔(Lyocell)等合成纤维的混合物。作为合成纤维的替代物，可以使用纤维长度长，例如12毫米以上的天然纤维，例如，种子纤维如棉、木棉和马利筋属植物(milkweed)；叶纤维如剑麻、马尼拉麻、菠萝、新西兰麻(hamp)，或者韧皮纤维如亚麻、***、苎麻、黄麻、kenaf。可以使用不同的纤维长度，并且依靠泡沫化技术，能够使用比常规纤维网湿法成网中可用纤维更长的纤维。水刺缠结中长纤维，大约18~30毫米，是有利的，因为它们提高了材料在干以及湿条件下的强度。泡沫化带来的进一步好处是，和湿法成网能够制造的材料相比，能够制造单位面积重量更低的材料。其它纤维长度短的天然纤维可用来作为浆粕纤维的替代物，例如细茎针茅草、五色草和农作物种子产生的麦管。
依靠排布在金属丝网下面的抽吸箱(未示出)，经过金属丝网12抽吸泡沫，并且该泡沫向下通过置于该金属丝网上的熔喷纤维网。当熔喷纤维和其它纤维的整体化纤维网仍被金属丝网12支撑时进行水刺缠结，并且用此方法形成复合材料24。有可能在水刺缠结之前将该纤维网转移到特殊的缠结金属丝网上，使其有可能被赋予图案，从而形成图案化的非织造材料。缠结装置16可包括数排喷嘴，在非常高的压力下非常细的喷射水流从这里直对纤维网刺去，使纤维缠结。
用例如加拿大专利CA 841938作为参考，以便进一步描述水刺缠结或者也被称为射流喷网的技术。
熔喷纤维将因此在水刺缠结之前已与泡沫效果所致泡沫化纤维网中的纤维混合并整体化。在随后的水刺缠结中，将使不同类型的纤维缠结，并获得其中所有类型的纤维大体上均质混合且相互整体化的复合材料。容易地将微细可移动熔喷纤维与其它纤维缠绕和缠结，将得到很高强度的材料。此水刺缠结所需的能量供应相对低，即此材料将易于缠结。水刺缠结中的能量供应大约在50~300千瓦时/吨。
图2所示实施方案与前一方案的区别在于，使用了预制薄纱(tissue)层或射流喷网材料17，即水刺非织造材料，在其上搁置熔喷纤维11，然后将泡沫化的纤维网15置于该熔喷纤维的顶端。这三层纤维层因泡沫效果而混合，并在水刺缠结装置15处水刺缠结形成复合材料24。
按照图3所示的实施方案，从第一高位流料箱19出来的第一泡沫化纤维网18被置于金属丝网12上，在该纤维网的顶端，搁置熔喷纤维11，最后是第二高位流料箱21出来的第二泡沫化纤维网20。相互位于顶端形成的纤维网18，11和20因泡沫效果而混合，然后当它们仍受金属丝网12支撑时使它们水刺缠结。当然也可能仅有第一泡沫化纤维网18和熔喷纤维11并将这两层水刺缠结在一起。
按照图4的实施方案与前面的区别在于，将熔喷纤维11置于单独的金属丝网22上，并且将预制的熔喷网23喂入两泡沫化装置18和20之间。当然在图1和2所示的装置中，也能用相应的预制熔喷网23(图1和2中未示出，译者注)，其中仅从熔喷网23的上侧进行泡沫化。
按照图5所示的实施方案，将熔喷纤维层11直接置于第一金属丝网12a上，此后将第一泡沫化纤维网18置于该熔喷层的顶端。然后将该纤维网传送到第二金属丝网12b上并翻转，此后，将第二泡沫化纤维网20从面对“熔喷侧”的一边置于“熔喷侧”上。将该纤维网传送到缠结金属丝网12c，并进行水刺缠结。为了简单起见，图5中未示出介于构造-和缠结装置之间沿着传送部件的纤维网。
按照进一步选择性的实施方案(未示出)，早于或者与其形成相联系地将熔喷纤维直接喂入泡沫化纤维分散体中。例如，熔喷纤维的掺混可在高位流料箱中进行。
优选以公知的方式从纤维状材料的两侧进行水刺缠结，以此方式获得更均质的等面(equilateral)材料。
水刺缠结之后，干燥并卷取材料24。然后以公知方法将此材料转换为合适的规格并进行包装。实施例1
将含50％化学牛皮纸浆浆粕纤维与50％聚酯纤维(1.7分特，19毫米)混合物的泡沫化纤维分散体以单位面积重量42.8克/米2置于熔喷纤维(聚酯，5~8微米)的网上，并随即将其水刺缠结在一起，以此方法获得单位面积重量为85.9克/米2的复合材料。水刺缠结时的能量供应为78千瓦时/吨。从双侧对此材料进行水刺缠结。测定此材料干和湿条件下的抗张强度，伸长率以及吸收容量，结果示于下表。水刺缠结作为参照材料的泡沫化纤维网(参照物1)和熔喷纤维网(参照物2)，其与制造此复合材料所用的那些一致。在下列表1中列出了这些参照材料独立以及放置在一起构成双层材料的测试结果。表1
  复合材料   参照物1   参照物2   参照物1+2分别拉   参照物1+2一起拉
  单位面积重量(g/m2)   85.9   43.6   42.8   86.4   86.4
  厚度(μm)   564   373   372   745   745
  松密度(cm3/g)   6.6   8.6   8.7   8.6   8.6
  抗张刚度指数   102.5   22.2   8.8   -   -
  抗张强度干，MD(N/m)   1155   540   282   822   644
  抗张强度 干，CD(N/m)   643   136   318   454   438
  抗张指数，干(Nm/g)   10   6.2   7   7.1   6.1
  伸长率MD，％   40   26   75   -   -
  伸长率CD，％   68   116   103   -   -
  √MD.CD   52   55   88   -   -
  断裂功MD(J/m2)   375   163   175   -   -
  断裂功CD(J/m2)   341   99   256   -   -
  断裂指数(J/g)   4.2   2.9   4.9   -   -
  抗张强度，湿，MD(N/m)   878   372   299   671   -
  抗张强度，湿，CD(N/m)   538   45   285   330   -
  抗张指数 湿(Nm/g)   8   3   6.8   5.4   -
  抗张强度 表面活性剂，MD(N/m)   605   116   281   397   -
  抗张强度 表面活性剂CD，(N/m)   503   22   326   348   -
  抗张指数 表面活性剂(Nm/g)   6.4   1.2   7.1   4.3   -
  能量供给(kWh/ton)   78   61   77   -   -
  总吸收(g/g)   4.5   6.1   0.2   -   -
正如从上述测试结果所看出的那样，在干以及在湿条件下和在表面活性剂溶液中，复合材料比结合的参照材料抗张强度高了很多。这说明在熔喷纤维和其余纤维之间存在良好的混合，其导致材料强度增加。
在图9中，以条形图的形式示出了干和湿条件下以及在表面活性剂溶液中不同材料的抗张指数。
复合材料的总吸收几乎和参照材料1的一样好，即和未混合熔喷纤维的射流喷网材料相当。另一方面，此吸收比参照材料2，即纯熔喷材料的高了许多。
在图6(原文为7，译者注)中，图示了泡沫化参照材料——参照物1的孔体积分布，单位毫米3/微米·克，以及归一化累积孔体积，单位％。可以看出，材料中大部分孔为60~70微米的。在图7中，图示了熔喷材料——参照物2的相应孔体积分布。此材料中的大部分孔是50微米以下的。从显示如上复合材料孔体积分布的图8中可以看出，此材料的孔体积分布比两种参照材料的宽了许多。这说明在此复合材料中存在有效的纤维混合。纤维结构中的宽孔体积分布提高了此材料的吸收-和液体分配性能，因此是有利的。
还可以从图10，按上述实施例制造的复合材料的电子显微镜照片中看出，纤维相互间被很好地整体化和混合。实施例2
制造纤维组份不同的许多水刺非织造材料，并就干和湿条件下抗张强度，断裂功以及伸长率进行测试。材料1：
将含100％化学牛皮纸浆的浆粕纤维，单位面积重量为20克/米2的泡沫化纤维分散体置于非常轻微热粘合，轻微压缩的1.21分特、单位面积重量为40克/米2聚丙烯(PP)纺粘纤维层的双面上，并随即被水刺缠结在一起。PP纤维的抗张强度为20厘牛/特，E-模量为201厘牛/特并且伸长率为160％。从双侧对此材料进行水刺缠结。水刺缠结时的能量供应为57千瓦时/吨。材料2：
将化学浆粕纤维的薄棉纸层置于和上述材料1(原文为A，译者注)中同样的纺粘材料的双面上，从双侧对此材料进行水刺缠结。水刺缠结时的能量供应为55千瓦时/吨。材料3：
将含100％化学牛皮纸浆的浆粕纤维，单位面积重量为20克/米2的泡沫化纤维分散体置于非常轻微热粘合，轻微压缩的1.45分特、单位面积重量为40克/米2聚酯(PET)纺粘纤维层的双面上，并随即被水刺缠结在一起。PET纤维的抗张强度为22厘牛/特，E-模量为235厘牛/特并且伸长率为76％。从双侧对此材料进行水刺缠结。水刺缠结时的能量供应为59千瓦时/吨。材料4：
将浆粕纤维(85％化学浆粕和15％CTMP)的薄棉纸层，以单位面积重量为26克/米2置于和上述材料1(原文为A，译者注)中同样的纺粘材料的双面上。从双侧对此材料进行水刺缠结。水刺缠结时的能量供应为57千瓦时/吨。材料5：
对湿法成网的含50％聚酯(PET)纤维(1.7分特，19毫米)和50％化学浆粕浆粕纤维的纤维网，采用71千瓦时/吨的能量供应进行水刺缠结。此材料的单位面积重量为87克/米2。PET纤维的抗张强度为55厘牛/特，E-模量为284厘牛/特，并且伸长率为34％。材料6：
除了用高了许多的能量供应——301千瓦时/吨进行水刺缠结之外，和上述材料5相同。此材料的单位面积重量为82.6克/米2。
材料1和3为按照本发明的复合材料，而材料2和4为本发明以外的叠层材料且将被视为参照材料。材料5和6为常规水刺缠结材料且也应当被视为参照材料。材料5水刺缠结时的能量供应与材料1~4水刺缠结时所用的为相同数量级，而材料6水刺缠结时的能量供应相当高。
测量结果示于下表2。表2
   材料1    材料2    材料3    材料4    材料5    材料6
  单位面积重量(g/m2)    86.7     93.3     83.6     90.7     87     82.6
  厚度2kPa(μm)    520     498     415     470     550     463
  松密度2kPa(cm3/g)    6.0     5.3     5.0     5.2     6.3     5.6
  抗张刚度MD(N/m)    18310     18290     20740     20690     10340     12590
  抗张刚度CD(N/m)    3250     3531     6546     4688     1756     1709
  抗张刚度指数(Nm/g)    89     86     139     109     49     56.2
  抗张强度干MD，(N/m)    4024     3746     4192     3893     2885     4674
  抗张强度干CD，(N/m)    1785     1460     2255     1619     998     1476
  抗张指数干(Nm/g)    31     25     37     28     19.5     31.8
  伸长率MD(％)    73     84     80     83     32     34.4
  伸长率CD(％)    129     123     100     98     90     87.6
  伸长率√MDCD(％)    97     102     89     90     54     55
  断裂功MD(J/m2)    2152     2618     2318     2370     600     906
  断裂功CD(J/m2)    1444     1216     1425     1084     484     695
  断裂功指数(J/g)    20.3     19.1     21.7     17.7     6.2     9.6
  抗张强度MD，湿(N/m)    4401     2603     4028     3574     2360     4275
  抗张强度CD，湿(N/m)    1849     1850     1940     1365     729     1363
  抗张指数，湿(Nm/g)    32.9     23.5     33.4     24.4     15.1     29.2
  相对强度水(％)    106     94     91     88     77     92
  抗张强度MD表面活性剂(N/m)    3987     1489     3554     2879     874     3258
  抗张强度CD表面活性剂(N/m)    1729     1083     1684     1214     234     985
  抗张指数 表面活性剂(Nm/g)    30.3     13.6     29.3     20.6     5.2     21.7
  相对强度 表面活性剂(％)    98     54     80     74     27     68
结果显示，和相应的叠层材料(材料2和4)比较、以及和已经用等价能量供应进行缠结的湿法成网参照材料(材料5)比较，本发明的复合材料(材料1和3)强度值都更高。尤其是湿、干以及表面活性剂中的抗张强度值，本发明的复合材料要比参照材料高许多。高强度值证实，人们得到了纤维整体化非常好的复合材料。
对于缠结所用能量供应比复合材料的高许多(大约高5倍)的材料6而言，干燥条件下的抗张强度与复合材料的处于同一水平上。湿-和表面活性剂中相对强度以及断裂功指数仍显著低于复合材料的。
作为进一步对照，水刺缠结两层在以上测试中用到的纺粘材料。这些材料表示为材料7和8(原文为6和7)。材料7：
PP纺粘物两层，1.21分特，单位面积重量各为40克/米2，以66千瓦时/吨的能量供应进行水刺缠结。材料8：
PET纺粘物两层，1.45分特，单位面积重量各为40克/米2，以65千瓦时/吨的能量供应进行水刺缠结。
这些材料的测量结果示于下表3。表3
   材料7    材料8
  单位面积重量(g/m2)     78.2     78.4
  厚度2kPa(μm)     865     762
  松密度21kPa(cm3/g)     11.1     9.7
  抗张刚度MD(N/m)     8314     9792
  抗张刚度CD(N/m)     507     897
  抗张刚度指数(Nm/g)     26     38
  抗张强度MD干(N/m)     642     798
  抗张强度CD干(N/m)     183     558
  抗张指数 干(Nm/g)     4     9
  伸长率MD(％)     9     32
  伸长率CD(％)     112     105
  伸长率√MDCD(％)     32     58
  断裂功MD(J/m2)     313     604
  断裂功CD(J/m2)     253     508
  断裂功指数(J/g)     3.6     7.1
  抗张强度MD湿(N/m)     210     965
  抗张强度CD湿(N/m)     217     659
  抗张指数 湿(Nm/g)     2.7     10.2
  相对强度 湿(％)     62     120
  抗张强度MD表面活性剂(N/m)     840     713
  抗张强度CD表面活性剂(N/m)     178     292
  抗张指数 表面活性剂(Nm/g)     4.9     5.8
  相对强度 表面活性剂(％)     113     68
正如所看到的那样，和按照本发明的复合材料相比，这些材料在所有方面强度值都低许多。
按照本发明的复合材料在缠结时能量供给非常低的情况下，具有非常高的强度值。其原因是已经创造出的均质纤维混合物，在其中合成纤维和浆粕纤维在纤维网络中协作，以致非同寻常地获得受欢迎的协同效果。伸长率和断裂功的高数值证实，存在整体化非常好的纤维复合材料并且它们协作使得该材料能承受非常大的变形而不断裂。
本发明当然不限于附图所示的实施方案以及上面的描述，并且可在权利要求的范围内改变。

Claims (9)

1.通过水刺缠结含连续长丝与天然纤维和/或合成短纤维的纤维混合物制造非织造材料的方法，其特征在于，使天然纤维和/或合成短纤维的纤维网(14；18，20)泡沫化，并经水刺将该泡沫化纤维分散体与连续长丝(11；23)缠结在一起以形成复合材料(24)，其中该连续长丝与剩余的纤维被很好地整体化。
2.如权利要求1中所述的方法，其特征在于，该泡沫化直接发生在连续长丝层(11；23)上，并且贯穿该长丝层发生该泡沫化纤维网(14)的排液。
3.如权利要求1中所述的方法，其特征在于，将连续长丝层(11)直接置于泡沫化纤维分散体(18)的顶端，接着是所述泡沫化纤维分散体的排液。
4.如权利要求1中所述的方法，其特征在于，将连续长丝层(11；23)置于两泡沫化纤维分散体(18，20)之间，接着是所述泡沫化纤维分散体的排液。
5.如前述权利要求中任何一项所述的方法，其特征在于，该连续长丝(11；23)置于薄纱或非织造物预制层(17)之上。
6.如权利要求1中所述的方法，其特征在于，在形成所述泡沫化纤维分散体的构造过程之前或者随同该过程，将该连续长丝直接喂入泡沫化纤维分散体中。
7.如前述权利要求中任何一项所述的方法，其特征在于，该泡沫化纤维分散体中存在浆粕纤维。
8.如前述权利要求中任何一项所述的方法，其特征在于，以其中纤维基本上相互自由的比较疏松、开放的网状纤维结构形式提供该连续长丝(11；23)，以致它们能容易地相互释放并与该泡沫化纤维分散体中的纤维整体化。
9.如前述权利要求中任何一项所述的方法，其特征在于，该连续长丝是熔喷纤维和/或纺粘纤维。
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CN112760826A (zh) * 2020-12-28 2021-05-07 杭州鹏图化纤有限公司 一种斜网成形在线熔喷的水刺复合无纺布及其制备方法
CN112746394B (zh) * 2020-12-28 2022-03-25 杭州鹏图化纤有限公司 一种斜网成形在线纺粘的水刺复合无纺布及其制备方法
CN112746394A (zh) * 2020-12-28 2021-05-04 杭州鹏图化纤有限公司 一种斜网成形在线纺粘的水刺复合无纺布及其制备方法
CN112746395A (zh) * 2020-12-28 2021-05-04 杭州鹏图化纤有限公司 一种长网成形在线纺粘的水刺复合无纺布及其制备方法
CN113737398A (zh) * 2021-09-09 2021-12-03 东纶科技实业有限公司 水刺绣花布的加工装置及方法

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CA2308784A1 (en) 1999-05-06
ATE211193T1 (de) 2002-01-15
US6163943A (en) 2000-12-26
KR20010031362A (ko) 2001-04-16
EP0938601B1 (en) 2001-12-19
SK5502000A3 (en) 2001-04-09
CN1107753C (zh) 2003-05-07
BR9813271B1 (pt) 2009-01-13
TR200001120T2 (tr) 2000-09-21
SE9703886L (sv) 1999-04-25
PL187958B1 (pl) 2004-11-30
RU2215835C2 (ru) 2003-11-10
DE69803035D1 (de) 2002-01-31
SE9703886D0 (sv) 1997-10-24
WO1999022059A1 (en) 1999-05-06
ES2170531T3 (es) 2002-08-01
AU734656B2 (en) 2001-06-21
DE69803035T2 (de) 2002-08-29
JP2001521075A (ja) 2001-11-06
EP0938601A1 (en) 1999-09-01
HUP0004252A2 (hu) 2001-04-28
PL340215A1 (en) 2001-01-15
BR9813271A (pt) 2000-08-22

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