CN1181246C - 用作补强剂和助滤剂的阳离子淀粉/阳离子半乳甘露聚糖胶共混料 - Google Patents
用作补强剂和助滤剂的阳离子淀粉/阳离子半乳甘露聚糖胶共混料 Download PDFInfo
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Abstract
一种在造纸中用作补强剂和助滤剂的组合物,其包括:阳离子淀粉、阳离子半乳甘露聚糖胶(例如瓜耳胶、刺槐豆胶、胡芦巴胶)和酸。
Description
技术领域
本发明涉及在造纸中用作补强剂和助滤剂的阳离子淀粉与阳离子半乳甘露聚糖胶例如瓜耳胶、刺槐豆胶、胡芦巴胶等的共混料。
背景技术
阳离子淀粉和阳离子瓜耳胶被造纸工业有效地用作补强剂和助滤剂。通常地,仅有一种这些产物被加入至造纸机的湿部。阳离子淀粉是更常用的。然而,也有报道,将这些产物在不同的部位分别地加入至纸机中。在造纸工艺中通常较早地加入阳离子淀粉而提供强度。而稍后将阳离子瓜耳胶加入至纸机中以提供滤水性和保证纤维留着率。
通常可将最高为18.144千克(40磅)的阳离子淀粉加入以得到所需的强度增强。阳离子瓜耳胶的添加量通常为453.6-3628.8克(1-8磅)。将两种产物以粉末状形式添加至纸机中。通常将阳离子淀粉制成固含量为10-15%的水悬浮体,然后置于高温下,并在加入至纸机之前稀释。高含量的淀粉可能在造纸工艺中产生问题,例如增加了生物需氧量和淀粉聚集,并降低了淀粉的有效性。阳离子瓜耳胶必须使用喷射器进行分散,并以低固含量溶解在水中,通常低于1%。随着纸机逐步排干其中的水体系,则制备瓜耳胶溶液所需的大量清水变得更难于得到。与瓜耳胶粉末产生的粉尘也是安全隐患,其可能导致事故和引发呼吸疾病。与阳离子淀粉胶的成本和加工性能限制了它在纸张干强度方面的用途。
Larsson在US4755259中公开了,将阳离子淀粉、阳离子瓜耳胶和胶态二氧化硅分别加入至造纸机中。Larsson并未公开,将阳离子淀粉和阳离子瓜耳胶的共混料添加至造纸机中。
Rushmere在US4927498中公开了,将阳离子聚合物,例如阳离子淀粉或阳离子瓜耳胶或阳离子聚丙烯酰胺和阴离子聚硅酸盐微凝胶添加至纸机中。这些阳离子聚合物可互换使用而不以共混料的形式一起加入。
“新型树胶在提高强度和生产率方面的应用”(K.E.Burnfield,TAPPI出版社,1995年4月26日)公开了,为了提高含淀粉体系的脱水性,将阳离子瓜耳胶添加至含有阳离子淀粉的造纸体系中。将阳离子瓜耳胶和阳离子淀粉分别地加入至造纸体系中而不以共混料的形式加入。
在发现本发明之前,熟悉淀粉和瓜耳胶化学性质的人员认为,是难于或几乎不可能将干阳离子淀粉和干瓜耳胶通过常规技术例如通过淀粉蒸煮器进行共混而达到将它们添加至纸机中的目的。
发明内容
本发明提供了一种粉末组合物,其包括(a)阳离子淀粉,(b)阳离子半乳甘露聚糖胶,和(c)颗粒状的水溶性酸,其为富马酸、柠檬酸、抗坏血酸、羟基乙酸或乳酸,其中所述阳离子半乳甘露聚糖胶与所述阳离子淀粉的比率是1∶1至1∶20,所述酸的含量是使得所述组合物的水溶液pH是7-10。
本发明还提供了一种于提高纸制品干强度和/或滤水性的方法,其包括:一种用于提高纸制品干强度和/或滤水性的方法,其包括:
(1)制备上述粉末组合物的水悬浮液,
(2)将所述水悬浮液在足够的温度下加热足够长的时间以溶解所述组合物,
(3)将所溶解的组合物添加至纸浆水悬浮液中
(4)过滤纸浆水悬浮液以制成纸幅,且
(5)干燥所述纸幅而制成纸制品。
具体实施方式
本发明是一种阳离子淀粉、阳离子半乳甘露聚糖胶(如含硼瓜耳胶)和酸的共混料。作为粉末形式的该产物可使用常规淀粉制备***在造纸厂中现场加工并制成溶液。本发明省去了制备阳离子瓜耳胶溶液的步骤,因为该步骤是危险的且需要水。本发明将一种共混有阳离子瓜耳胶和阳离子淀粉的溶液添加至纸机中。出乎意料地,相比于只添加阳离子瓜耳胶或阳离子淀粉,或将阳离子淀粉和阳离子瓜耳胶在不同的部位添加至纸机中的情况,添加共混料可使纸张强度进一步提高。
阳离子瓜耳胶是本发明中最优选使用的阳离子半乳甘露聚糖胶。本发明在一些情况下具体针对瓜耳胶或阳离子瓜耳胶,然而本领域的一般技术人员将意识到,这些教示通常也可应用于半乳甘露聚糖胶或阳离子半乳甘露聚糖胶。
现有技术公知的是,当阳离子瓜耳胶和阳离子淀粉以溶液的形式在造纸工艺中单独地添加入,它们均提高了纸张的滤水性和强度。相比于只添加阳离子淀粉或阳离子瓜耳胶,在造纸工艺中共同添加阳离子淀粉和阳离子瓜耳胶将有望也增加强度和滤水性。本发明意外地发现,将阳离子瓜耳胶和阳离子淀粉在添加至纸机之前进行预共混,可以比不经预混分别添加的情况提高纸张强度20%以上。本发明的另一个重要特征是,添加共混料可达到由分别添加阳离子淀粉和阳离子瓜耳胶所能达到的滤水性改进值。而且,已发现,可以配制出含有所需比率的阳离子淀粉和阳离子瓜耳胶的干制品,以使得共混料在添加至纸机之前,可按等同于淀粉的方法进行加工。在发现本发明之前,在制备阳离子淀粉/阳离子瓜耳胶共混料期间产生的粘度高得难于加工,所以导致昂贵的设备磨损和无法接受的需水量。
阳离子半乳甘露聚糖胶可为阳离子瓜耳胶、刺槐豆胶或胡芦巴胶,阳离子半乳甘露聚糖胶优选为阳离子瓜耳胶或阳离子刺槐豆胶,且最优选为阳离子瓜耳胶。
阳离子瓜耳胶可以是由瓜耳胶与N-(3-氯代-2-羟丙基)三甲基氯化铵(例如可购自密执安州米德兰的陶氏化学公司的Quatl 88)反应制成的羟丙基三甲基氯化铵瓜耳胶衍生物。阳离子瓜耳胶可以是纯化的阳离子瓜耳胶如GalactasolSP 813D,或者是阳离子/阴离子瓜耳胶产物的共混料例如可购自赫尔克里士公司的AQU D-3376D或AQUD-3373D。羟丙基三甲基氯化铵单元与瓜耳胶糖类单元的比率可以是0.03-0.2,但优选为0.07-0.15。本反应可在水和氢氧化钠存在下进行。可将硼,其为硼酸钠、硼酸、硼砂或其它水溶性含硼化合物的形式,在反应之后或之前,或在瓜耳胶产物干燥之前加入。
在本发明中使用的阳离子淀粉是季铵盐改性的淀粉。所述淀粉可以是蜡质种玉米、土豆、玉米、小麦或木薯淀粉,例如国家淀粉和化学公司的Cato232,A.E.Staley加工公司的STAoLOK400,粮食加工公司的ChargemasterR430。阳离子淀粉优选是阳离子玉米、土豆或蜡质种玉米淀粉,且其最优选是阳离子玉米淀粉。在配方中阳离子瓜耳胶与阳离子淀粉的比率可以至少是约1∶1,优选至少是约1∶4和最优选至少是约1∶10。这个比率可以最高为约1∶20,优选最高为约1∶15 。
所述酸可以是能够将最终的阳离子瓜耳胶/阳离子淀粉溶液的pH值降低至约7的任意酸。为了便于使用,所述酸优选应为干态且颗粒状。所述酸可以具有任意粒径且其优选能够通过4目的筛网,最优选能通过100目筛网。优选的酸为有机酸,例如富马酸、柠檬酸或其它水溶性粉末状酸例如抗坏血酸、羟基乙酸和乳酸。酸的添加量应使阳离子淀粉、阳离子瓜耳胶和酸的溶液的pH值至少为约7,优选至少为约8.5。酸的含量可使溶液的pH最高为约10,优选最高为约9.5。
本发明的组合物可通过将干态阳离子淀粉、阳离子瓜耳胶和酸分别添加至共混机中并混合而制得。而且,可先添加任意两种组分并共混,然后在加入第三者。干共混是优选的,因为其十分有利于本发明的加工。然后将干态共混料按造纸商目前使用淀粉的相同样式和浓度制成水悬浮液,由此消除了与制造瓜耳胶溶液相关的问题。该悬浮液可以是在100℃分批蒸煮20分钟或在高于100℃的温度下及在压力下连续蒸煮(喷射蒸煮器)。蒸煮步骤可以等同于由阳离子淀粉制造商建议用于他们的淀粉的蒸煮步骤。所得的溶液将是易于添加至纸机中,然而,实际上在添加之前通常将其稀释10倍之多。
由蒸煮步骤制得的阳离子淀粉溶液,以及阳离子瓜耳胶溶液在添加至纸浆中之前可按上述比率(基于干重)混合在一起。
蒸煮后的最终溶液的粘度是相同的,而与制备该溶液的步骤无关。所得的最终纸张性能也是可比较的。
本发明所要求保护的范围并不意欲通过下列实施例限制,这些实施例仅用于说明的目的。除非另外提及,所有份数和百分比均是基于重量。
实施例1
将100克Galactosol SP 813D阳离子瓜耳胶和900克ChargemasterR430阳离子玉米淀粉放在一掺混机中且共混形成均匀的浓度。将干粉状富马酸逐步添加直至上述10%固含量的共混料的水悬浮液达到pH9.5。将该10%固含量的悬浮液在50℃保持7小时,而显示粘度没有明显增长。将悬浮液加热至100℃保持20分钟。发现粘度明显地增长。
实施例2
重复实施例1,并添加额外的富马酸以降低pH至8.5。发现结果没有明显的改变。
实施例3
重复实施例1,并进一步添加富马酸以降低pH至7.5。在50℃保持期间,发现粘度明显增长。这个粘度增长是相关于瓜耳胶在体系中的稳定性并受淀粉的标准蒸煮步骤的影响。
实施例4
重复实施例1,但不添加富马酸。所得溶液的粘度明显低于实施例1,2和3,表明阳离子瓜耳胶没有溶解至溶液中。添加富马酸以将pH值降低至6.0。粘度等于或高于实施例1,2和3中所观察到的值。
实施例5
使用真空辅助滤水装置进行滤水研究。滤水装置是配备有541硬化无灰滤纸的Whatman 12.5厘米3单元过滤漏斗。在将滤纸放置在漏斗中之前,将滤纸进行干燥和洗涤。将漏斗放置到一连接有真空泵和真空表的真空烧瓶上。制备Chargemaster R430阳离子玉米淀粉和Galactasol SP 813S阳离子瓜耳胶的溶液并按实施例1中的相同比率掺混在一起。将预掺混的阳离子淀粉和阳离子瓜耳胶溶液以对干纸浆基重有1.1%固含量的量添加至500毫升0.2%牛皮纸浆悬浮液中。将纸浆悬浮液与阳离子淀粉和阳离子瓜耳胶的溶液混合15秒。在添加纸浆悬浮液之前对漏斗进行抽真空。将纸浆悬浮液添加至漏斗中。记录纸浆悬浮液通过过滤器滤水所需的时间。滤水结果列于表1中。使用分别添加阳离子淀粉和/或阳离子瓜耳胶而重复上述试验。
实施例6
重复实施例5,只是用按实施例4中制备的STAoLOK400阳离子土豆淀粉/Galactasol SP 813D阳离子瓜耳胶溶液替代ChargemasterR430/Galactasol SP 813S共混溶液。
实施例7
重复实施例6,并且将共混料中的淀粉降低25%且添加基于纸浆为0.5%的共混固体。
实施例8
重复实施例5,将阳离子瓜耳胶的含量增加至为共混料的20%并添加基于纸浆为1.25%的共混固体。
实施例9
用中性的亚硫酸盐半化学浆替换牛皮浆,重复实施例5。
实施例10
用旧瓦楞纸箱浆(回用纸板盒制得的纸浆)替换牛皮浆,重复实施例5。
实施例11
用STAoLOK 400阳离子土豆淀粉替换Chargemaster R430阳离子玉米淀粉,重复实施例10。
实施例12
使用实施例11中所述的阳离子瓜耳胶/阳离子淀粉共混料制成手抄纸而进行强度研究。使用造纸化学实验室有限公司(纽约,Carmel)的动态手抄纸模具并按其操作手册上介绍的方法制备手抄纸。相应地,在113.55升(30加仑)的箱槽中将牛皮纸浆稀释成0.18%浓度。对每个手抄纸而言,从上述113.55升(30加仑)的箱槽中取出2毫升纸浆并放在一个搅拌器上。将阳离子瓜耳胶/阳离子淀粉共混料以基于纸浆干重为1.1%固含量的量添加入。将所述纸浆添加至手抄纸模具中并用推进式混合器进行搅拌。搅拌以1500转/分钟进行5秒钟。将搅拌器降低至1000秒/分钟下再进行5分钟。在将搅拌器叶片提起离造纸网1″并打开排水阀之前,将搅拌器进一步降低至400转/分钟。然后在70目网上制成手抄纸。
对手抄纸进行抽真空。所用的技术是在打开阀门制备手抄纸之前,将体系抽成508毫米汞柱(20英寸汞柱)的真空。打开阀门,而从纸页中除去多余的水分。当真空降低至254毫米汞柱(10英寸汞柱)时,关闭阀门。将湿的手抄纸进行称重并从筛网上移除。将该手抄纸放置在吸水纸之间并压制至453.6千克(1000磅)。将纸页在鼓式干燥器上于250℃干燥并放置在一个防潮器中。将纸页切成1.27厘米(半英寸)纸条并在25℃和50%相对湿度下进行Instron抗张强度。抗张强度列于表2中。
实施例13
将阳离子瓜耳胶的量提高至共混料的20%并添加基于纸浆干重的1.25%的共混固体,重复实施例12。
实施例14
用未漂白牛皮纸浆替代牛皮纸浆,重复实施例12。
实施例15
用旧瓦楞纸盒纸浆替代牛皮纸浆,重复实施例12。
实施例16
用Chargemaster R430阳离子玉米淀粉替换STAoLOK400阳离子土豆淀粉,重复实施例15。
表1滤水的滤水率(秒)
实施例 | 5 | 6 | 7 | 8 | 9 | 10 | 11 |
对照 | 38 | 42 | 32 | 38 | 101 | 63 | 63 |
阳离子瓜耳胶 | 18 | 16 | 15 | 19 | 24 | 19 | 19 |
阳离子淀粉 | 26 | 17 | 21 | 26 | 76 | 33 | 14 |
瓜耳胶和淀粉 | 20 | 19 | 23 | 15 | 14 | ||
瓜耳胶/淀粉共混料 | 19 | 12 | 15 | 19 | 19 | 18 | 17 |
表2断裂抗张强度(Kg/cm2)(括号内数据为以磅/平方英寸为单位)
实施例 | 12 | 13 | 14 | 15 | 16 |
对照 | 1.218(17.4) | 1.218(17.4) | 0.56(8.0) | 0.567(8.1) | 0.567(8.1) |
阳离子瓜耳胶 | 1.225(17.5) | 1.176(16.8) | 0.56(8.0) | 0.595(8.5) | 0.595(8.5) |
阳离子淀粉 | 1.274(18.2) | 1.274(18.2) | 0.56(8.0) | 0.644(9.2) | 0.581(8.3) |
瓜耳胶和淀粉 | 1.288(18.4) | 1.379(19.7) | 0.644(9.2) | 0.679(9.7) | 0.672(9.6) |
瓜耳胶/淀粉共混料 | 1.428(20.4) | 1.498(21.4) | 0.721(10.3) | 0.770(11.0) | 0.798(11.4) |
*1磅/平方英寸等于0.07kg/cm2
Claims (7)
1、一种粉末组合物,其包括(a)阳离子淀粉,(b)阳离子半乳甘露聚糖胶,和(c)颗粒状的水溶性酸,其为富马酸、柠檬酸、抗坏血酸、羟基乙酸或乳酸,其中所述阳离子半乳甘露聚糖胶与所述阳离子淀粉的比率是1∶1至1∶20,所述酸的含量是使得所述组合物的水溶液pH是7-10。
2、如权利要求1所述的组合物,其中所述阳离子淀粉为蜡质种玉米、土豆、玉米、小麦或木薯淀粉。
3、如权利要求1所述的组合物,其中所述半乳甘露聚糖胶为瓜耳胶、刺槐豆胶或胡芦巴胶。
4、如权利要求1所述的组合物,其中所述阳离子半乳甘露聚糖胶与所述阳离子淀粉的比率是1∶4至1∶15。
5、如权利要求1所述的组合物,其中酸的含量是使所述组合物的水溶液pH是8.5-9.5。
6、如权利要求1所述的组合物,其中所述酸是富马酸。
7、一种用于提高纸制品干强度和/或滤水性的方法,其包括:
(1)制备权利要求1的粉末组合物的水悬浮液,
(2)将所述水悬浮液在足够的温度下加热足够长的时间以溶解所述组合物,
(3)将所溶解的组合物添加至纸浆水悬浮液中
(4)过滤纸浆水悬浮液以制成纸幅,且
(5)干燥所述纸幅而制成纸制品。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/207,895 US6217709B1 (en) | 1998-11-23 | 1998-11-23 | Cationic starch/cationic galactomannan gum blends as strength and drainage aids |
US09/207,895 | 1998-11-23 |
Publications (2)
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CN1289381A CN1289381A (zh) | 2001-03-28 |
CN1181246C true CN1181246C (zh) | 2004-12-22 |
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CNB998023736A Expired - Fee Related CN1181246C (zh) | 1998-11-23 | 1999-11-04 | 用作补强剂和助滤剂的阳离子淀粉/阳离子半乳甘露聚糖胶共混料 |
Country Status (17)
Country | Link |
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US (1) | US6217709B1 (zh) |
EP (1) | EP1049832B1 (zh) |
JP (1) | JP2002530549A (zh) |
KR (1) | KR20010034322A (zh) |
CN (1) | CN1181246C (zh) |
AT (1) | ATE219808T1 (zh) |
AU (1) | AU1812000A (zh) |
BR (1) | BR9907220A (zh) |
CA (1) | CA2319163A1 (zh) |
CO (1) | CO5210991A1 (zh) |
DE (1) | DE69901935T2 (zh) |
DK (1) | DK1049832T3 (zh) |
ES (1) | ES2179692T3 (zh) |
NO (1) | NO20003760L (zh) |
PL (1) | PL342013A1 (zh) |
RU (1) | RU2215079C2 (zh) |
WO (1) | WO2000031339A1 (zh) |
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KR100406758B1 (ko) * | 2001-02-23 | 2003-11-21 | 변유량 | 양이온성 혼합폴리머, 그 제조방법 및 이를 포함하는제지용 첨가제 |
US7074845B2 (en) * | 2002-04-09 | 2006-07-11 | Pulp And Paper Research Institute Of Canada | Swollen starch-latex compositions for use in papermaking |
TW200503762A (en) * | 2003-05-09 | 2005-02-01 | Toho Chem Ind Co Ltd | Cation-modified galactomannan polysaccharide and cosmetic composition containing the same |
FR2992967B1 (fr) * | 2012-07-06 | 2016-01-22 | Roquette Freres | Melanges de polyvinylamines et de compositions de matieres amylacees cationiques liquides comme agents ameliorant la resistance a sec des papiers et des cartons |
WO2014191408A1 (en) * | 2013-05-27 | 2014-12-04 | Dupont Nutrition Biosciences Aps | Cationic modified polysaccharides and uses thereof in papermaking |
CN105090295B (zh) * | 2014-05-19 | 2018-07-06 | 三菱电机株式会社 | 电磁制动装置及使用该电磁制动装置的电梯装置 |
CN105839451A (zh) * | 2015-11-04 | 2016-08-10 | 山东太阳生活用纸有限公司 | 造纸助剂、造纸方法及纸巾 |
RU2742433C1 (ru) * | 2020-04-21 | 2021-02-05 | Ирина Амировна Четвертнева | Композиция для безглинистых биополимерных буровых растворов |
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US3471362A (en) | 1967-04-28 | 1969-10-07 | Hodag Chem Corp | Starch and gum additive compositions and use thereof in papermaking processes |
US4385961A (en) | 1981-02-26 | 1983-05-31 | Eka Aktiebolag | Papermaking |
SE432951B (sv) | 1980-05-28 | 1984-04-30 | Eka Ab | Pappersprodukt innehallande cellulosafibrer och ett bindemedelssystem som omfattar kolloidal kiselsyra och katjonisk sterkelse samt forfarande for framstellning av pappersprodukten |
SE8107078L (sv) | 1981-11-27 | 1983-05-28 | Eka Ab | Forfarande for papperstillverkning |
GB8311152D0 (en) | 1983-04-25 | 1983-06-02 | Rheocal Bucks Ltd | Paper and board manufacture |
SE8403062L (sv) | 1984-06-07 | 1985-12-08 | Eka Ab | Forfarande vid papperstillverkning |
US4927498A (en) * | 1988-01-13 | 1990-05-22 | E. I. Du Pont De Nemours And Company | Retention and drainage aid for papermaking |
US5104487A (en) | 1988-09-02 | 1992-04-14 | Betz Paper Chem., Inc. | Papermaking using cationic starch and naturally anionic polysacchride gums |
US4954220A (en) | 1988-09-16 | 1990-09-04 | E. I. Du Pont De Nemours And Company | Polysilicate microgels as retention/drainage aids in papermaking |
US5338406A (en) | 1988-10-03 | 1994-08-16 | Hercules Incorporated | Dry strength additive for paper |
SE9003954L (sv) | 1990-12-11 | 1992-06-12 | Eka Nobel Ab | Saett foer framstaellning av ark- eller banformiga cellulosafiberinnehaallande produkter |
US5318669A (en) | 1991-12-23 | 1994-06-07 | Hercules Incorporated | Enhancement of paper dry strength by anionic and cationic polymer combination |
US5338407A (en) | 1991-12-23 | 1994-08-16 | Hercules Incorporated | Enhancement of paper dry strength by anionic and cationic guar combination |
US5620510A (en) | 1995-06-23 | 1997-04-15 | Cpc International Inc. | Swollen starches as papermaking additives |
US5723023A (en) | 1996-09-27 | 1998-03-03 | National Starch And Chemical Investment Holding Corporation | Method of papermaking using modified cationic starch |
US5859128A (en) | 1997-10-30 | 1999-01-12 | E. I. Du Pont De Nemours And Company | Modified cationic starch composition for removing particles from aqueous dispersions |
-
1998
- 1998-11-23 US US09/207,895 patent/US6217709B1/en not_active Expired - Lifetime
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1999
- 1999-11-04 JP JP2000584139A patent/JP2002530549A/ja active Pending
- 1999-11-04 AU AU18120/00A patent/AU1812000A/en not_active Abandoned
- 1999-11-04 ES ES99961571T patent/ES2179692T3/es not_active Expired - Lifetime
- 1999-11-04 DE DE69901935T patent/DE69901935T2/de not_active Expired - Fee Related
- 1999-11-04 CN CNB998023736A patent/CN1181246C/zh not_active Expired - Fee Related
- 1999-11-04 RU RU2000120950/12A patent/RU2215079C2/ru not_active IP Right Cessation
- 1999-11-04 AT AT99961571T patent/ATE219808T1/de not_active IP Right Cessation
- 1999-11-04 KR KR1020007008045A patent/KR20010034322A/ko active IP Right Grant
- 1999-11-04 PL PL99342013A patent/PL342013A1/xx not_active Application Discontinuation
- 1999-11-04 CA CA002319163A patent/CA2319163A1/en not_active Abandoned
- 1999-11-04 BR BR9907220-3A patent/BR9907220A/pt not_active Application Discontinuation
- 1999-11-04 DK DK99961571T patent/DK1049832T3/da active
- 1999-11-04 WO PCT/US1999/025916 patent/WO2000031339A1/en active IP Right Grant
- 1999-11-04 EP EP99961571A patent/EP1049832B1/en not_active Expired - Lifetime
- 1999-11-22 CO CO99073356A patent/CO5210991A1/es not_active Application Discontinuation
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Also Published As
Publication number | Publication date |
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RU2215079C2 (ru) | 2003-10-27 |
EP1049832B1 (en) | 2002-06-26 |
CN1289381A (zh) | 2001-03-28 |
DK1049832T3 (da) | 2002-10-14 |
JP2002530549A (ja) | 2002-09-17 |
ES2179692T3 (es) | 2003-01-16 |
DE69901935T2 (de) | 2003-01-23 |
EP1049832A1 (en) | 2000-11-08 |
KR20010034322A (ko) | 2001-04-25 |
WO2000031339A1 (en) | 2000-06-02 |
NO20003760D0 (no) | 2000-07-21 |
CO5210991A1 (es) | 2002-10-30 |
US6217709B1 (en) | 2001-04-17 |
CA2319163A1 (en) | 2000-06-02 |
NO20003760L (no) | 2000-09-08 |
ATE219808T1 (de) | 2002-07-15 |
DE69901935D1 (de) | 2002-08-01 |
PL342013A1 (en) | 2001-05-07 |
BR9907220A (pt) | 2000-10-24 |
AU1812000A (en) | 2000-06-13 |
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