CN1361717A - 多层反应器和它的用途以及制备过氧化氢的方法 - Google Patents
多层反应器和它的用途以及制备过氧化氢的方法 Download PDFInfo
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- CN1361717A CN1361717A CN00810400A CN00810400A CN1361717A CN 1361717 A CN1361717 A CN 1361717A CN 00810400 A CN00810400 A CN 00810400A CN 00810400 A CN00810400 A CN 00810400A CN 1361717 A CN1361717 A CN 1361717A
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Abstract
本发明涉及一种包括圆柱形立式搅拌反应器(V)的装置,该反应器上安装了沿单一的纵向搅拌轴排列的离心涡轮(a),及其在实施若干气体组分在悬浮于液相中的固体的存在下发生反应的任何方法中的用途。该装置特别适用于直接制备过氧化氢。
Description
本发明涉及一种其中的气体组分在悬浮于液相中的固体的存在下发生反应的方法。本发明还涉及实施该方法的装置。更具体地说,本发明涉及利用悬浮于液相中的催化剂由氧气和氢气直接制备过氧化氢的装置和方法。
国际专利申请WO 96/05138和WO 92/04277披露,氢气和氧气可以在管状反应器中发生反应,其中存在高速循环的含水反应介质,包括悬浮的催化剂。这样,氢气和氧气以超过氢气可燃性极限的比例,即氢气对氧气的摩尔浓度比大于0.0416的比例分散在反应介质中(Enclopédie des Gaz[气体百科全书]-Air Liquide,909页)。只要氢气和氧气保持小气泡的形式,这种方法就是安全的。另外,为了获得合理的气体反应物转化,管状反应器的长度必须相当长,而且不得不包括很多弯管。在这些条件下,确保不形成气囊是困难的。此外,含水反应介质循环的任何中断都会导致***性的连续的气相出现。
欧洲专利申请EP 579109公开了氢气和氧气可以在“喷淋床(tricklebed)”式反应器中进行反应,该反应器中装填了催化剂固体颗粒,通过该催化剂,可以使含水反应介质与包含氢气和氧气的气相同向流动。然而还是难于确保这类方法是安全的,因为部分喷淋床可能有干透的危险,而且分散该反应所产生的大量的热是困难的。
此外,US 4009252,US 4279883,US 4681751和US 4772458公开了直接制备过氧化氢的方法,其中氢气和氧气在悬浮于含水反应介质中的催化剂的存在下于搅拌反应器中进行反应。但是,使用搅拌反应器的缺点在于导致低的转化率或不合适的产率。
文献一般性地指出,绝对的操作安全需要牺牲产率,反之,增加过氧化氢的产率就要以安全为代价。
因此,本发明的主题是提供一种方法,包括使气体组分在悬浮于液相中的固体的存在下发生反应的步骤,特别是在绝对安全的情况下以最佳产率直接制备过氧化氢的方法,以及实施上述方法的装置。
本发明的装置包括圆柱形立式搅拌反应器,其底部安装了注入气体反应物的设备,其顶部安装了移除气体反应物的排放设备,而且安装了沿单一纵向搅拌轴排列的,优选规则地排列的离心涡轮。该纵向轴一般由齿轮连接的电动机单元来驱动,所述的电动机单元经常位于反应器的上面或下面。依据轴的长度,可以由一个或多个轴承来支撑。
反应器上还可以安装反向挡板和/或热交换器。
完整的搅拌反应器是由单一空间组成的,不存在任何固定的水平隔板。反应器的高度通常为其直径的1.5~10倍,优选为其直径的2~4倍。反应器的底部还安装了盖子,该盖子可以是扁平状的或半球形的。
图1为本发明具体装置的简图。
该装置包括安装了离心涡轮(a)的搅拌反应器(V),所述的离心涡轮(a)沿马达(M)驱动的搅拌轴排列。所述的反应器还安装了反向挡板(c)和热交换器(R)。注入气体反应物的设备(1,2)安装在反应器的底部,而排放设备(3)位于反应器的顶部,用来排出气体反应物。
根据图1,能够将液体、气泡和悬浮的固体的混合物拉向反应器的中心轴,而且能够在水平面上沿径向抛出该混合物,以循环液体、气泡和悬浮的固体的混合物的任何离心涡轮均适用于本发明。
优选具有1个或2个中央开口的凸缘径流式涡轮。特别优选类似于抽吸孔向下的离心水泵中所使用的凸缘涡轮。
涡轮上可以装有径向排列或以一定角度排列或形成螺旋状的叶片。
涡轮的数目取决于反应器高度与反应器直径的比例,并且通常为2~20个,优选3~8个。
两个涡轮之间的距离优选为涡轮外径的0.5~1.5倍;后者优选为反应器直径的0.2~0.5倍。
涡轮的厚度优选为涡轮直径的0.07~0.25倍。该厚度是指涡轮的两个凸缘之间的距离。
本发明的装置还可以包括安装于反应器内部或外部的过滤器。
在运行中,反应器的下部被包含悬浮的固体催化剂和很多气相反应物的小气泡的液相所占据,而上部则为连续的气相所占据。连续的气相所占据的体积为反应器总体积的10~30%,优选为20~25%。
涡轮沿搅拌轴排列,以便搅拌停止时它们浸没在液相中,优选完全浸没液相中。
涡轮的旋转速度如此选择,以便每单位体积液相的可能气泡数目最大化和气泡直径最小化。
为了防止整个液相旋转,反应器装有反向档板,优选由排列于涡轮四周的纵向矩形板组成。该反向挡板通常位于反应器的圆柱形器壁与涡轮之间。
这些金属板的高度一般接近于反应器的圆柱形部分的高度。其宽度通常为反应器直径的0.05~0.2倍。
所选择的反向挡板的数目为其宽度的函数,并且一般为3~24个,优选为4~8个。
反向挡板(c)优选距离反应器器壁(p)1~10mm纵向排列,并且朝向来自反应器中心的半径轴,如图2所示,该图2是装有特定涡轮的反应器的横截面图,其中(O)代表涡轮的吸孔,(f)代表涡轮的凸缘,而(u)代表涡轮的叶片。
一些或全部的反向挡板可以被热交换器替代。热交换器优选由一束立式的圆柱形管子组成,其高度接近或等于反应器的圆柱形部分的高度。
这些管子(t)通常按图2那样纵向排列于涡轮的周围。
这些管子的数目和直径按这样的方式确定,即保持液相温度在所需的范围之内。管子的数目通常为8~64。
尽管本发明的装置可用以实施大气压下的反应,但更经常地优选在压力下操作。优选10~80bar级的高压,以便提高反应速度。
反应器、搅拌设备和热交换器可以由化工领域中常用的任何材料如不锈钢(304L或316L)等制成。
在反应器的所有内表面以及搅拌设备和热交换器的外表面上,可以涂敷聚合物保护涂层,如PVDF(聚1,1-二氟乙烯)、PTFE(聚四氟乙烯)、PFA(C2F4与全氟化乙烯基醚的共聚物)或FEP(C2F4与C3F6的共聚物)。也可以将涂层限定于某些磨损部件,如涡轮上。
该装置特别适用于直接制备过氧化氢,氢气和氧气以直径低于3mm优选0.5~2mm的小气泡形式注入含水的液相中,优选摩尔流速使得氢气的摩尔流速与氧气的摩尔流速之比大于0.0416,同时保持连续气相中氢气的含量低于可燃烧极限。
常用的催化剂为US 4772458中所描述的那些。这些催化剂是以钯和/或铂为基础的固体催化剂,任选地载在二氧化硅、氧化铝、碳或铝硅酸盐上。
除悬浮的催化剂之外,通过加入无机酸酸化的水相还可以包括过氧化氢稳定剂和分解抑制剂,如卤化物。溴化物是特别优选的,并且可以方便地与游离溴(Br2)组合使用。
本发明还提供一种方法,包括使气体组分在悬浮于液相中的固体存在下进行反应的步骤。该方法包括在反应器的底部以单独的或混合物的方式引入气体组分(两种或多种)。当气体混合物的组分是相容的且满足安全性需要时,优选以混合物的形式引入。这种情况下,反应物的进料可以通过嵌入搅拌轴中的管道,然后再借助于一组位于反应器底部的涡轮中央的小孔来进行,按这种方式可以在涡轮喷出的液体流中产生大量的小气泡。
当该方法需要以产生着火或***危险的比例供给气体组分时,气体反应物单独引入反应器,或者通过位于涡轮最低吸入孔上游的分立管道,或者通过刚好位于最低涡轮下方的分立的烧结管道。
本发明的装置可以连续或半连续地操作。
在半连续的方式中,气体反应物在规定的时间连续地引入到反应器的下部分,该部分被包含悬浮的固体催化剂的液相所占据。
到达反应器的连续气相的过量气体反应物,一般通过保持反应器内部的不变的主压力而连续地排出。在规定的时间结束时,使反应器出料,以回收反应产物。
当连续操作时,气体反应物和反应溶液连续地引入到反应器中,先装填悬浮于构成液相的反应溶液中的固体催化剂。过量的气体反应物连续地排出,并且借助于一个或多个过滤器,通过连续取出液相而将反应产物转移至其它容器,按这种方式可以保持固体催化剂悬浮于反应器的内部。
所述的过滤器可以是由烧结的金属或陶瓷材料制成的烛形过滤器,该过滤器优选与纵向的冷却管或反向挡板并排地放置在反应器中。
该过滤器也可以放置在反应器的外部,这种情况下,过滤器优选由金属或陶瓷材料制成的中空的多孔管组成,在其内部来自反应器的包括悬浮催化剂的液相进行闭路的循环。图3说明了包括反应器外部过滤器的装置。所述的中空管(g)纵向排列,并在其底部供给反应器底部取出的液相,并使在该中空管顶部收集的液相返回反应器的上部。这种连续循环可以通过泵或通过反应器的旋转涡轮所产生的局部压力增加实现。
根据图3所代表的本发明的优选装置,除去催化剂之后的澄清液体收集于位于多孔中空管周围的夹套中,然后通过控制阀(6)排出,按这种方式,可以保持反应器中液相的水平恒定。反应溶液以计算的流速连续地泵入反应器,以使溶解于液相中的反应产物的浓度保持选定的值。有利的是,一些反应溶液可以借助于管道7逐步地注入到夹套(h)中,以解除过滤器的堵塞。反应溶液也可以以高压喷射,用来连续地清洁反应器中的连续的气相。
气体反应物通过途径1和2连续地引入到反应器的底部(b),而那些尚未反应的气体反应物则可以通过途径4来循环。
直接合成过氧化氢时,选定流速的氢气通过(1)注入到底部涡轮(b)之下的液相中。选定流速的包含低比例氢气的氧气从反应器中的连续气相中取出(4),并通过(2)进入底部涡轮(b)之下的液相。一定流量的新鲜氧气(5)注入到反应器中的连续气相中,以补偿消耗的氧气,并保持连续地气相在可燃性极限之外。压力调节器(放气阀)允许过量的气体反应物(3)和新鲜氧气中可能存在的惰性气体如氮气从反应器中的连续气相中排出。
本发明的装置在发生搅拌偶然停止时的优点在于,它使气体反应物的所有气泡上升,并只在重力作用下独自直接到达连续的气相。
实验部分(实施例)
直接合成过氧化氢水溶液的装置
容积1500cm3的反应器,包括高200mm直径98mm的圆柱形容器。
底和盖子是扁平形的。
可拆卸的厚度1.5mm的PTFE套筒置于反应器的内部。
搅拌通过长180mm直径8mm的纵向不锈钢轴来提供,该轴由置于反应器盖子上的磁耦合来驱动。
可以将一个、两个或三个外径45mm厚度9mm(两个凸缘之间)的带有凸缘的涡轮以不同的选定高度固定在搅拌轴上,该涡轮上带有直径12.7mm的向下的吸孔,并且带有8个宽度9mm长度15mm厚度1.5mm的扁平的放射状叶片,按这种方式,可以将液相分成基本上相等的体积。
底下的涡轮距底部32mm,第二涡轮距底部78mm,而第三涡轮距底部125mm。
四个反向挡板的高度为190mm,宽度为10mm,厚度为1mm,纵向放置于容器中,并垂直于反应器的内壁,而且通过两个定心环与该壁保持1mm的距离。
通过8个直径6.35mm长度150mm排列于距容器轴35mm的环中的纵向管道提供冷却或加热。
恒温的水流流经该盘管。
氢气和氧气通过两个分立的直径1.58mm的不锈钢管注入液相中,将该气体导入底下涡轮的中央。气体反应物注入含水的介质中,以及氧气注入连续的气相中,均借助于质量流量计来控制。在某些进行的实验中,用不同比例的氧气和氮气混合物代替氧气。
反应器内部的主压力通过放气阀保持恒定。
用串联的气相色谱测定氢气量、氧气量以及任选的构成反应器排放气流的氮气量。
催化剂的制备
所使用的催化剂包含0.7%重量的钯金属和0.03%重量的铂,载于微孔的二氧化硅上。
所述催化剂是通过用包含PdCl2和H2PtCl6水溶液浸渍具有下列特性的二氧化硅(Aldrich Ref.28,851-9):
-平均粒度 5~15μm
-BET表面积 500m2/g
-孔隙体积 0.75cm3/g
-平均孔径 60然后干燥,最后在300℃的氢气下热处理3小时而制备的。
然后将催化剂(10g/l)悬浮于包含60mg NaBr、5mg Br2和12g H3PO4的溶液中,将该溶液在40℃加热5小时,然后滤出催化剂、用软化水洗涤并干燥。
含水反应介质
通过将12g H3PO4、58mg NaBr和5mg Br2加到1000cm3的软化水中制备含水溶液。
一般的操作规程
将选定体积的含水反应介质加到高压釜中,然后加入计算量的催化剂。通过以选定的流量将氧气注入连续的气相使高压釜增压。由于压力调节器该压力保持恒定。通过冷却管束内的控温循环水,使液体介质达到选定的温度。
控制搅拌为900rpm,并将氢气和氧气以选定的流速注入到底下涡轮的中央。
测量来自压力调节器的气体混合物的流量及其中的氢气含量。
反应1小时之后,关闭氢气和氧气到含水反应介质的流入,并保持氧气到连续气相的注入,直到氧气中的氢气全部消失为止。然后关闭氧气的流入,并使反应器减压,最后回收过氧化氢的水溶液。
一旦回收了过氧化氢水溶液,立即将其称重,然后通过在Milliporer过滤器上过滤分离出催化剂。
然后通过碘量法分析所得到的溶液,由此可以计算出过氧化氢的浓度。该合成的选择性定义为所形成的过氧化氢摩尔数除以所消耗的氢气摩尔数时所得到的百分数。
转化率定义为所消耗的氢气的体积除以引入的氢气的体积时所得到的百分数。
不同实验过程中的操作条件及所得到的结果示于下面的表中。
例如实施例2、3、7、8、9和14的操作是用两个底下涡轮完成的。
表(反应1小时)
实施例 | 反应器中的涡轮数目 | 催化剂量(g) | 含水溶液的初始体积(cm3) | 注入底涡轮的H2流量(Nl/h) | 注入底涡轮的O2流量(Nl/h) | 与O2一起注入底涡轮的N2流量(Nl/h) | 注入连续气相的O2流量(Nl/h) | 反应器中的压力(bar) | 反应器中的温度(℃) | 反应器中连续气相中的H2浓度(%) | 所得水溶液中H2O2的浓度(%) | 氢气转化率(%) | 基于氢气的反应选择性(%) |
1 | 1 | 6 | 430 | 120 | 240 | 0 | 2640 | 50 | 40 | 2.5 | 12.5 | 36 | 91 |
2 | 2 | 6 | 700 | 120 | 240 | 0 | 2640 | 50 | 41 | 1.4 | 12.2 | 60 | 90 |
3 | 2 | 9 | 700 | 120 | 240 | 0 | 2640 | 50 | 41 | 1.4 | 12.2 | 60.8 | 89 |
4 | 3 | 8.5 | 1000 | 120 | 240 | 0 | 2640 | 50 | 40 | 0.95 | 10.6 | 73 | 90 |
5 | 3 | 8.5 | 1000 | 120 | 240 | 0 | 2640 | 60 | 40 | 0.87 | 10.8 | 76 | 89 |
6 | 3 | 8.5 | 1000 | 120 | 240 | 0 | 2640 | 60 | 60 | 0.5 | 11.0 | 82 | 84 |
7 | 2 | 6 | 700 | 25 | 335 | 0 | 265 | 50 | 39 | 2.1 | 2.3 | 45 | 97 |
8 | 2 | 6 | 700 | 80 | 280 | 0 | 1640 | 50 | 40 | 1.8 | 8.1 | 53 | 96 |
9 | 2 | 6 | 700 | 100 | 260 | 0 | 2140 | 50 | 40 | 1.6 | 10.2 | 57 | 92 |
10 | 3 | 8.5 | 1000 | 120 | 216 | 24 | 2640 | 50 | 40 | 0.95 | 10.5 | 73 | 89 |
11 | 3 | 8.5 | 1000 | 120 | 240 | 60 | 2580 | 50 | 40 | 1.13 | 10.0 | 68 | 90 |
12 | 3 | 8.5 | 1000 | 120 | 120 | 480 | 1980 | 50 | 40 | 1.83 | 6.3 | 55 | 70 |
13 | 3 | 8.5 | 1000 | 100 | 130 | 520 | 1400 | 50 | 40 | 2.07 | 5.7 | 50.4 | 80 |
14 | 2 | 6 | 700 | 140 | 220 | 0 | 3140 | 50 | 40 | 1.43 | 13.8 | 61 | 87 |
15 | 3 | 8.5 | 1000 | 140 | 220 | 0 | 3140 | 50 | 40 | 0.82 | 12.2 | 74 | 89 |
实施例1、2、3和4表明,在相同的温度、压力以及H2/O2比例下,增加辐射状涡轮的数目使转化率增加,就象将多个反应器串联起来一样有效。
这是因为,如果τ1代表一级(带有1个涡轮的反应器)转化率,τ2代表具有2个涡轮的反应器的总转化率,而τ3代表具有3个涡轮的反应器的转化率,那么实际上适用于计算串联安装的搅拌反应器中的转化率的规则如下:
(1-τ2)=(1-τ1)(1-τ1)和
(1-τ3)=(1-τ1)(1-τ1)(1-τ1)
利用这种关系可以外推出实现本发明的高转化率所需要的涡轮数。
实施例7、8和9表明,对于同一反应器和相同的反应条件,向液相引入浓的氢气气体混合物时,反应1小时之后的转化率和溶液中H2O2的含量显著增加。
实施例5和6表明,用本发明的反应器可以只用3个涡轮就获得80%的转化率,每1立方米反应器每小时超过100kg H2O2的产量,以及非常高的选择性。
实施例10和11表明,利用本发明的反应器,使用氧气与氮气(10%至20%)的混合物代替纯氧气,可以获得高的转化率和浓的H2O2。
使用空气(实施例12和13)也给出令人感兴趣的结果。
同时,H2/O2比例不同的实施例14和15表明,从2个涡轮变成3个涡轮使得氢气的转化率增加和反应器的连续气相中H2的浓度下降。
Claims (16)
1.一种包括圆柱形立式搅拌反应器的装置,其底部安装了注入气体反应物的设备,顶部安装了气体排放设备,以及任选地安装反向挡板和/或热交换器,其特征在于,所述的反应器安装了离心涡轮,所述的涡轮优选沿单一纵向搅拌轴规则地排列。
2.权利要求1的装置,其特征在于该反应器的高度为直径的1.5~10倍,优选为直径的2~4倍。
3.权利要求1或2的装置,其特征在于所述的涡轮为辐射状的。
4.权利要求3的装置,其特征在于该涡轮是带有凸缘的。
5.权利要求4的装置,其特征在于该涡轮具有一个或两个中央开口。
6.权利要求1至5中任一项的装置,其特征在于所述涡轮数目为2~20,优选为3~8。
7.权利要求1至6中任一项的装置,其特征在于该涡轮的外径为反应器直径的0.2~0.5倍。
8.权利要求1至7中任一项的装置,其特征在于该涡轮的厚度为其直径的0.07~0.25倍。
9.权利要求1至8中任一项的装置,其特征在于该涡轮安装了形成螺旋的或者以一定角度或辐射状排列的叶片。
10.权利要求1至9中任一项的装置,其特征在于,运行期间,包含悬浮固体催化剂和很多气体反应物小气泡的液相占据该反应器的下部,而连续的气相占据反应器的上部。
11.权利要求10的装置,其特征在于所述的连续的气相占据反应器体积的10~30%,优选为20~25%。
12.权利要求10或11的装置,其特征在于该涡轮在搅拌停止时浸没于,优选完全浸没于所述的液相之中。
13.权利要求1至12中任一项的装置,其特征在于该反应器装有一个或多个过滤器。
14.权利要求13的装置,其特征在于该过滤器位于反应器的内部或外部。
15.一种包括用气体反应物在悬浮于液相中的固体存在下发生反应的方法,其特征在于该气体反应物到达权利要求1至14中任一项的装置的反应器底部。
16.一种由氢气和氧气制备过氧化氢水溶液的方法,其特征在于使用权利要求1至14中任一项的装置。
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FR99/09260 | 1999-07-16 | ||
FR9909260A FR2796311B1 (fr) | 1999-07-16 | 1999-07-16 | Reacteur multietage, ses applications et procede de fabrication du peroxyde d'hydrogene |
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CNB2005100739688A Expired - Fee Related CN100490969C (zh) | 1999-07-16 | 2000-06-07 | 载体金属催化剂、其制备方法和其在直接制备过氧化氢中的用途 |
CNB2006100943646A Expired - Fee Related CN100460316C (zh) | 1999-07-16 | 2000-06-07 | 从氢和氧直接制备过氧化氢的方法 |
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CNB2006100943646A Expired - Fee Related CN100460316C (zh) | 1999-07-16 | 2000-06-07 | 从氢和氧直接制备过氧化氢的方法 |
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US (1) | US20060198771A1 (zh) |
EP (1) | EP1204471A1 (zh) |
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CN102358760A (zh) * | 2011-07-22 | 2012-02-22 | 浙江大学 | 一种搅拌釜反应器 |
CN105960277A (zh) * | 2014-02-10 | 2016-09-21 | 霍尼韦尔国际公司 | 用于液相氟化的反应器设计 |
CN111282531A (zh) * | 2018-12-06 | 2020-06-16 | 张存续 | 微波处理装置 |
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US8957254B2 (en) | 2009-07-06 | 2015-02-17 | Solvay Sa | Process for chemical synthesis from an alkenone made from a halogenated precursor |
US20120020847A1 (en) * | 2010-07-20 | 2012-01-26 | Lurgi, Inc. | Retention Of Solid Powder Catalyst By In-Situ Cross Flow Filtration In Continuous Stirred Reactors |
KR20140053186A (ko) | 2011-07-15 | 2014-05-07 | 솔베이(소시에떼아노님) | 과산화수소를 수득하는 방법, 및 상기 방법을 위한 촉매 담지체 |
EP2607343A1 (en) | 2011-12-22 | 2013-06-26 | Solvay Sa | Process for the manufacture of halogenated precursors of alkenones and of alkenones |
WO2018016359A1 (ja) * | 2016-07-19 | 2018-01-25 | 三菱瓦斯化学株式会社 | 過酸化水素製造用貴金属触媒および過酸化水素の製造方法 |
SI25590A (sl) | 2018-01-15 | 2019-07-31 | Univerza V Ljubljani | Postopek priprave izotopsko označenega vodikovega peroksida |
CN113828206B (zh) * | 2021-07-13 | 2024-03-22 | 重庆大学 | 一种提高流体混合效果的喷气式射流搅拌桨 |
CN115739202B (zh) * | 2022-11-22 | 2024-02-23 | 太仓斯迪克新材料科技有限公司 | 催化剂浸渍设备 |
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1999
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- 2000-06-07 CN CNB2005100739688A patent/CN100490969C/zh not_active Expired - Fee Related
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102358760A (zh) * | 2011-07-22 | 2012-02-22 | 浙江大学 | 一种搅拌釜反应器 |
CN105960277A (zh) * | 2014-02-10 | 2016-09-21 | 霍尼韦尔国际公司 | 用于液相氟化的反应器设计 |
CN107913646A (zh) * | 2014-02-10 | 2018-04-17 | 霍尼韦尔国际公司 | 用于液相氟化的反应器设计 |
CN111282531A (zh) * | 2018-12-06 | 2020-06-16 | 张存续 | 微波处理装置 |
Also Published As
Publication number | Publication date |
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KR100436790B1 (ko) | 2004-06-24 |
TR200200074T2 (tr) | 2002-06-21 |
NZ515748A (en) | 2003-05-30 |
FR2796311B1 (fr) | 2001-09-14 |
NO325226B1 (no) | 2008-02-25 |
CN1739851A (zh) | 2006-03-01 |
EA200200171A1 (ru) | 2002-06-27 |
NO20016239L (no) | 2001-12-19 |
NO20016239D0 (no) | 2001-12-19 |
AU759296B2 (en) | 2003-04-10 |
CN1880215A (zh) | 2006-12-20 |
EP1204471A1 (fr) | 2002-05-15 |
PL352482A1 (en) | 2003-08-25 |
US20060198771A1 (en) | 2006-09-07 |
EA003039B1 (ru) | 2002-12-26 |
CN1170627C (zh) | 2004-10-13 |
KR20020023411A (ko) | 2002-03-28 |
WO2001005498A1 (fr) | 2001-01-25 |
CA2377127A1 (fr) | 2001-01-25 |
CA2377127C (fr) | 2006-07-25 |
JP2003504193A (ja) | 2003-02-04 |
BR0012261A (pt) | 2002-03-12 |
FR2796311A1 (fr) | 2001-01-19 |
AU4931100A (en) | 2001-02-05 |
UA74340C2 (uk) | 2005-12-15 |
CN100460316C (zh) | 2009-02-11 |
CN100490969C (zh) | 2009-05-27 |
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