CN1195194C - 用蒸馏器低温蒸馏制氮的方法和装置 - Google Patents
用蒸馏器低温蒸馏制氮的方法和装置 Download PDFInfo
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Abstract
一个单体塔(109)用于通过分离清洁的压缩空气(100)来制氮(117)。一个精馏器(111)用于纯化来自塔顶部的氮(116)。来自塔底的富氧液流(110)在一洗馏器(112)中洗提分馏。洗提后的气流(115)被再循环至馈入空气(100)。从洗馏器出来的是废气(143)。精馏器(111)和洗馏器(112)热连接。
Description
本发明涉及一种方法和装置,用以通过低温蒸馏制备氮气。
以低温蒸馏制氮为公知技术,并记载于多个专利公开中(例如:
J53-122861; US.5,144,809; US.4,867,773; US.5,385,024;
US.4,927,441; US.4,848,996; US.4,883,519; US.4,872,893;
US.4,869,742; US.5,711,167; US.5,611,218; US.5,582,034;
US.5,402,647; US.4,883,519; US.5,385,025; WO/PCT/IB96/
00323),并且公开于:“Production of Medium Pressure Nitrogen
by Cryogenic Air Seperation”Gas Separation&Purification,1991
Vol.5,December,pp.203-209。
过去数年中,人们作了很多努力以改进生产技术,降低氮的成本,其主要包括动力消耗以及设备成本。一般来说,一种高效工艺往往要求增加设备的复杂性,从而导致成本上升。因此,总是需要一个高效而简单的工艺,以保证在动力消耗及设备成本之间取得好的平衡。
下面叙述的新发明应用分馏技术在工艺循环的次级区将蒸馏塔与换热器结合成简单紧凑的板翅式热交换设备。这样得到了明显的成本降低,同时可维持整个工艺的良好效率。
分馏被用于促进同时的热、质传递,所以可在一单一换热器内同时进行热交换及蒸馏效应。回流冷凝是分馏的一个应用,其中,由精馏分离的一气相混合物与由换热蒸发的一流体束同时进行热交换,并因此使被精馏的流体冷凝,产生一反向回流。与之类似,洗提再沸是分馏的另一特征,其中,换热器内部的一向下流动液体与另一流束进行热交换,产生部分蒸发并形成上升蒸汽,这一上升蒸汽与所述向下流动的液体直接接触,产生洗提效应。
数种低温分馏的工艺方法公开在如下先有专利及教科书中:
U.S.2,861,432;U.S.2,963,872;U.S.5,592,832;U.S.5,694,790;
U.S.5,030,339; U.S.5,144,809; U.S.5,207,065; U.S.5,410,855;
U.S.5,438,836; U.S.5,592,832; U.S.5,596,883;
“The Physical Principles of Gas Liquefaction and LowTemperature Rectification”by Mansel Davies published 1949 pp.137-139,
“Zerlegung der Luft”by H.Hausen published 1957 p.164 and“Separation of Gases”by Ruheman,2nd Edition,pp.70,174,279-831 291,292.
上述出版物指出了分馏在制备O2、N2、H2、He中的应用。
氮气广泛地应用于隋性气体工业,覆盖,氨气生产以及电子工业中。对氮纯度的要求,大多数应用中一般在ppm氧含量量级,对电子工业则要达到亚ppb量级。在某些情况,可使用低纯度氮(1%-2%O2或99%-98%N2)。
基本的制氮方法示于图1,这一方法也称为经典方法。
空气由一主空压机1压缩,之后在3中被净化,除去水和CO2。其在换热器5中被冷却并被送入塔9,在那里,它被分离成富氧底部部分12以及富氮顶部部分。部分富氮部分作为液流19从塔顶部引出。富氮气体在冷凝器11中被冷凝,它是通过与来自塔底的膨胀富氧液12(富集液)进行热交换而冷凝的。蒸发的富集液15在换热器中加温,经透平7膨胀,为工艺提供冷量并进一步升温后排出。气态氮17从塔顶引出,并在换热器中加温。
US.5,199,809公开了一种制氮方法,其中塔和换热器结合为一个单体的板翅式换热器。部分中间空气流经过分馏,制成中等纯度的氮气(99-98%)。这一方法提供了低成本的设备,但是只限于应用在纯度要求不高的情况,它的功耗相对较高。
US.4,867,773以及US.4,966,002公开了一种类似于经典方法的工艺。不同的是,部分蒸发的富集液从塔底抽出,并再次压缩,再送回塔中或送回到馈入塔中的空气流。这种安排相比经典方法而言在功耗方面产生了某些改进。
US.4,848,996在US.4,867,773/4,966,002的富集液蒸发器上方增加了一个短塔,以产生一股气体流,其组成与空气(合成空气)相似。所述气体流之后再循环返到一空压机中间级处的空气流,节省了一台另外的循环压缩机。
US.4,883,519叙述了一种对US.4,867,773/4,966,002的改进,其部分地蒸发富集液,再循环产生的气体流,并且在另一换热器中膨胀至低压并蒸发。
US.4,927,441说明了一种对US.4,883,519的改进,其中增加了一个短蒸馏塔,其使高压塔的底部富集液蒸馏为低压的气体流,(其具有与空气类似的组成)以及一束第二液流。所述新的气体“空气”流再循环至主空压机的中间级并与馈入蒸馏塔的主空气流再次汇合。所述蒸馏塔将馈入空气分离为顶部氮产品流及底部富集液(富O2)。所述第二液流膨胀为低压并接着蒸发,产生废氮气流。塔顶部的部分气态氮流被分成二束:第一束在位于短塔底部的换热器中冷凝,为塔提供必要的再沸腾;第二束在另一换热器中冷凝,为第二液流的蒸发提供条件。
如上对工艺流程发展所作的证明中可以看出,工艺方法在效率上的一种改进会导致增加工艺流程上的复杂性并因此而导致成本的增加。
本发明提供了一种低温蒸馏制氮方法,其包括:
a)压缩并净化馈入空气,除去污物,其在低温冷却下被冻结去除;
b)冷却的压缩空气被引入一蒸馏塔,在塔中空气被分离为富氧流体和富氮流体;
c)一第一束富氧液流从塔底引出,膨胀并送入一洗提分馏器;
d)从所述洗提分馏器引出一第二束富氧液流以及一第三束流;
e)至少部分所述第二束液流在一蒸发器中至少部分地蒸发,以产生另一气流;
f)将上述富氮流体从上述塔送入一精馏分馏器,以生产一产品氮和一液体,所述精馏分馏器与所述洗提分馏器进行热交换;以及
g)将至少部分上述液体作为回流送入上述塔。
根据本发明的进一步特点,其工艺方法可选择地包括:
—将至少部分所述第三流回送至塔;
—将所述第三流与馈入空气混合;
—在所述净化步骤的上游混合所述第三流及馈入空气;
—将所述第二液流送入一分离器并将至少部分该第二液流的组份从所述分离器送入所述蒸发器;
—从所述蒸发器送流体至所述分离器;以及
—从所述分离器引出气体并膨胀该气体。
所述蒸发器,精馏分馏器以及洗提分馏器可以结合成一个单体的板翅式换热器。
根据本发明的进一步特点,提供了一种低温蒸馏制氮方法,其包括:
a)压缩并净化馈入空气,除去污物,其在低温冷却下被冻结去除;
b)冷却的压缩空气被引入一蒸馏塔,在塔中空气被分离为富氧流体和富氮流体;
c)一第一束富氧液流从塔底引出,膨胀并送入一洗提分馏器;
d)从所述洗提分馏器引出一第二束富氧液流以及一第三束流;
e)至少部分所述第二束液流在一蒸发器中至少部分地蒸发,以产生另一气流;
f)将上述富氮流体从上述塔送入一冷凝器,以生产一产品氮和一液体,所述冷凝器与所述洗提分馏器进行热交换;以及
g)将至少部分上述液体作为回流送入上述塔。
本发明的其它可选择特性包括:
—将至少部分所述第三流回送至塔;
—将所述第三流与馈入空气混合;
—在所述净化步骤的上游混合所述第三流及馈入空气;
—将所述第二液流送入一分离器并将至少部分该第二液流的组份从所述分离器送入所述蒸发器;
—从所述蒸发器送流体至所述分离器;以及
—从所述分离器引出气体并膨胀该气体。
所述冷凝器,洗提分馏器以及蒸发器可结合成一个单体的板翅式换热器。
所述第二液流可于蒸发前膨胀,或者,所述第二液流于蒸发前不膨胀,这时,分离器与洗提分馏器处于相同的压力。
根据本发明进一步的特点,提供了一种低温蒸馏制氮装置,其包括:
a)一蒸馏塔;
b)一换热器;
c)一压缩机构,其用于压缩馈入空气并将其送入所述换热器,之后送入所述塔;
d)用于将一第一富氧液流从塔底引出的机构;
e)一洗提分馏器;
f)一精馏分馏器,与所述洗提分馏器热连接;
g)一蒸发器,与所述冷凝器热连接;
h)用于将所述第一液流送入所述洗提分馏器的机构;
i)用于将一第二富氧液流以及一第三气流从所述洗提分馏器引出的机构;
j)用于将至少部分所述第二富氧液流送入所述蒸发器的机构;
k)用于从所述蒸发器引出一流体的机构;
l)用于将一富氮气流送入所述精馏分馏器的机构;以及
m)一机构,用于将一液体从所述精馏分馏器送入所述塔,以及,一机构,用于将富氮产品气从所述精馏分馏器引出。
根据本发明的另一特点,提供了一种低温蒸馏制氮装置,其包括:
a)一蒸馏塔;
b)一换热器;
c)一压缩机构,其用于压缩馈入空气并将其送入所述换热器,之后送入所述塔;
d)用于将一第一富氧液流从塔底引出的机构;
e)一洗提分馏器;
f)一冷凝器,与所述洗提分馏器热连接;
g)一蒸发器,与所述冷凝器热连接;
h)一机构,用于将所述第一液流送入所述洗提分馏器;
i)一机构,用于将一第二富氧液流以及一第三气流从所述洗提分馏器引出;
j)一机构,用于将至少部分所述第二富氧液流送入所述蒸发器;
k)一机构,用于从所述蒸发器引出一流体;
l)一机构,用于将一富氮气送入所述冷凝器;以及
m)一机构,用于将一液体从所述冷凝器送入所述塔,以及,一机构,用于将富氮产品气从所述冷凝器引出。
新的发明提供了一套较简单的设备装置,并且维持循环的热力效率。一个双分馏器(即精馏分馏器及洗提分馏器)或一个筒单的分馏器可被使用来替代经典循环中蒸馏塔的顶部冷凝器。
图1是现有技术制氮方法的示意图;
图2,3和4示出本发明的三种制氮方法及装置。
图2中,周围空气100在空气主压缩机101中被压缩,并且与流程中抽出的再循环流115混合。这一混合最好控制在前端净化器103之前或之后,在净化器103中,空气中的水份和CO2被去除,以避免它们在下游的低温设备中冻结。再循环流的压缩最好控制在一个单独的压缩机121中,或者是在主压缩机101的某部分中(如图中虚线所示)。对后者,再循环流于主压缩机的级间被混合。
图2示出如下工艺方法:压缩的空气流在热交换器105中冷却并被送入蒸馏塔109中,以便在塔顶产生富氮流,在塔底产生富氧第一液流110。该第一液流然后经阀119膨胀为低压进入洗提分馏器(洗馏器)112,其含有三个理论分馏盘,与塔109顶部的冷凝氮热连通。
在洗馏器112中,下流的液体与精馏器111中的富氮流进行热交换,产生上升蒸气,该上升蒸气接着洗提下流液体,并产生第三富氮顶流115。一个第二液流118(比第一液流110更富氧)生成于洗馏器底部。该第二液流接着膨胀至低压进入一个分离器或接收器131。该接收器的液体141通过与精馏器111热交换,在废料蒸发器113中至少部分地蒸发,产生气体流123,其与液流118混合,被送入分离器131,并且作为废气流143排出。
再循环富氮流115最好在压缩机121中进一步压缩,并与馈入塔109的空气流混合。这一压缩可在环境温度下完成,也可在低温下(例如在下游的热交换器105中)完成。
图2的实施例还示出一个冷凝侧的精馏器。这种设置有时称为双分馏器,其中,洗提侧与精馏侧热连通。蒸馏塔109顶部的富氮气116进入精馏器,与废料蒸发器的蒸发富液进行热交换,洗提侧产生一冷凝液流,与上升的富氮流反向下流。这一下流的冷凝液精馏了上升的富氮流并在精馏器111顶部产生更富含氮的气流,并在其底部产生液体回流。至少一部分液体回流最好返回蒸馏塔,作为蒸馏的逆向回流(为简明也标为116)。所述富氮气流更好地回收为产品氮。所述精馏器最好含有三个理论分馏盘。
微量组份例如Ne,He和H(也称为不可冷凝物)存在于馈入空气中并在富氮气流中浓缩。如果高浓度的不可冷凝物是不希望的,则氮产品可从蒸馏塔的顶部或接近顶部抽出,并且该富氮气流变为不可冷凝气流。这一气流通常随废气流143一同排出。
所述废气流143最好经一膨胀机107膨胀,以供给工艺所需的冷量。该膨胀机可与压缩机121配套使用。或者,也可代之以液体致冷或与膨胀机配合使用。
图2的实施例中,废料蒸发器113,精馏器111以及洗馏器112结合成一个单体的板翅式换热器。
图2中各股流体的总结示于表1。气流100的组成为干燥且不含CO2。
表1
流束 | 压力 | 流量 | 组成(摩尔%) | ||
序号 | (bar) | (Nm3/h) | N2 | Ar | O2 |
100 | 1.01 | 1000 | 78.1 1 | 0.93 | 20.96 |
115 | 4.14 | 752.8 | 71.75 | 1.76 | 26.49 |
110 | 8.89 | 1069.2 | 59.65 | 2.10 | 38.25 |
117 | 8.70 | 683.6 | 99.98 | 0.02 | 3vpm |
143 | 3.36 | 316.4 | 30.85 | 2.90 | 66.25 |
图1和图2工艺流程的比较示于表2
表2
图2 | 图1 | |
净馈入流量(Nm3/h) | 1000 | 1750 |
馈入压力(bar) | 9.04 | 9.04 |
再循环流量(Nm3/h) | 752.8 | 0 |
再循环压力(bar) | 4.14 | n/a |
再循环出口压力(bar) 9.04 n/a | ||
氮流量(Nm3/h) | 684 | 684 |
氮纯度 | 3ppm氧 | 3ppm氧 |
塔内理论分馏盘 | 40 | 40 |
氮压力(bar) | 8.55 | 8.55 |
相对功率 | 72.7 | 100 |
图2所示方法的功率收益约为27%。
图3所示方法表明的情形是,冷凝氮侧不是精馏器。冷凝侧是一个氮冷凝器211。洗馏器212带有三块理论分馏盘,与冷凝氮热交换,并且在氮侧不发生分馏。在这一实施例中生产的氮比图2例中的氮纯度低,这里由于氮流出蒸馏塔后没经过精馏。
气态氮从塔109顶部流出,分为流217和216。流216被送入氮冷凝器211顶部并且冷凝氮226作为回流被送回塔109。
图3中,氮冷凝器211,废料蒸发器213以及洗馏器212结合为一个单体的板翅式换热器。
如果高浓度不可冷凝物是我们不希望的,则产品氮最好从蒸馏塔顶部或接近顶部提取,并且富氮气体流变为不可冷凝流,其一般地经管道230排出或与气态废料一起排出。或者是,也可应用液体协助制冷。
图4中,使用了一个双分馏器,并且第二富集液以大致相同于洗馏器的压力被送入分离器/接收器131:被蒸发的废气流也就以大致相同的压力作为再循环流出现。当然,这一特点也可应用于图3实施例的安排中。
虽然上述公开只说明了使用板翅式换热器作为分馏器,本发明应理解为包含所有这类方法和设备,它们可利用任何装置,其能促进内部流体的汽相和液相之间同时的热、质传递,并因此使流体产生洗馏或精馏效果。至少另一股流体将热量传入正在分馏的流体或从其传走,所述另一股流体或是经受分馏(双分馏情况)的或者简单的就是加热流或冷却流。
除了上述几股流(洗馏、精馏、加热或冷却)之外,一个分馏器还可以包含其它的工艺流束。
本工艺可生产中等纯度、高纯度、或超高纯度的氮。在一些其它变型中,人们可以不必使再循环流115与空气流混合,而代之以将该流束直接引入塔109的不同于主空气流位置的一个馈入盘。
当然,如果有足够的冷量,图2,3和4的方法和设备也可用于生产液体氮。
尽管图2,3和4示出,废料蒸发器首先与精馏器热连通,但也可安排这套设备使精馏器首先与洗馏器热交换,然后与废料蒸发器热交换。
可选择地,离开洗馏器的第二富氧液流在经膨胀阀膨胀进入上述接收器131之前,可被送入另一辅助接收器(未示出)。在这种情况下,可简单地通过调节辅助接受器的液面来控制该膨胀液体。如果不想设另外的容器,则板翅式洗馏器的液体收集器头可用作辅助接收器。
人们也可选择不使废料蒸发器与分馏器相结合。这时的废料蒸发器是一个分开的热交换器,其中废气流的蒸发是通过从塔顶或接近塔顶抽出的氮气的冷凝进行热交换完成的。
所述塔可含有任何标准填充材料,例如分馏盘,结构填料。
尽管以上说明是针对各种实施例的,但本发明应视为决不限制于上述具体例子。本领域中的技术人员将会承认,在所附权利要求的范围内本发明还有许多其它实施例。
Claims (22)
1.一种低温蒸馏制氮方法,包括:
a)压缩并净化馈入空气,除去污物,其在低温冷却下被冻结去除;
b)冷却的压缩空气被引入一蒸馏塔,在塔中空气被分离为富氧流体和富氮流体;
c)一第一束富氧液流从塔底引出,膨胀并送入一洗提分馏器;
d)从所述洗提分馏器引出一第二束富氧液流以及一第三束流;
e)至少部分所述第二束液流在一蒸发器中至少部分地蒸发,以产生一废气流;
f)将上述富氮流体从上述塔送入一精馏分馏器,以生产一产品氮和一液体,所述精馏分馏器与所述洗提分馏器进行热交换;以及
g)将至少部分上述液体作为回流送入上述塔。
2.根据权利要求1的方法,其特征在于,包括将至少部分所述第三束流送回上述塔。
3.根据权利要求2的方法,其特征在于,包括将所述第三束流与馈入空气混合。
4.根据权利要求3的方法,其特征在于,包括将所述第三束流与馈入空气在其净化步骤的上游混合。
5.根据权利要求1的方法,其特征在于,所述蒸发器,所述精馏分馏器以及所述洗提分馏器被结合为一个单体的板翅式换热器。
6.根据权利要求1的方法,其特征在于,所述第二束液流在蒸发之前膨胀。
7.根据权利要求1的方法,其特征在于,所述第二束液流在蒸发之前不膨胀。
8.根据权利要求1的方法,其特征在于,包括将所述第二束液流送到一分离器以及将液体从所述分离器送到所述蒸发器。
9.根据权利要求8的方法,其特征在于,包括从所述蒸发器送流体至所述分离器。
10.根据权利要求8的方法,其特征在于,包括从所述分离器引出气体并膨胀该气体。
11.一种低温蒸馏制氮方法,包括:
a)压缩并净化馈入空气,除去污物,其在低温冷却下被冻结去除;
b)冷却的压缩空气被引入一蒸馏塔,在塔中空气被分离为富氧流体和富氮流体;
c)一第一束富氧液流从塔底引出,膨胀并送入一洗提分馏器;
d)从所述洗提分馏器引出一第二束富氧液流以及一第三束流;
e)至少部分所述第二束液流在一蒸发器中至少部分地蒸发,以产生一废气流;
f)将上述富氮流体从上述塔送入一冷凝器,以生产一产品氮和一液体,所述冷凝器与所述洗提分馏器进行热交换;以及
g)将至少部分上述液体作为回流送入上述塔。
12.根据权利要求11的方法,其特征在于,包括将至少部分所述第三束流送回上述塔。
13.根据权利要求11的方法,其特征在于,包括将所述第三束流与馈入空气混合。
14.根据权利要求13的方法,其特征在于,包括将所述第三束流与馈入空气在其净化步骤的上游混合。
15.根据权利要求11的方法,其特征在于,所述冷凝器,所述洗提分馏器以及所述蒸发器被结合为一个单体的板翅式换热器。
16.根据权利要求11的方法,其特征在于,所述第二束液流在蒸发之前膨胀。
17.根据权利要求11的方法,其特征在于,所述第二束液流在蒸发之前不膨胀。
18.根据权利要求11的方法,其特征在于,包括将所述第二束液流送到一分离器以及将液体从所述分离器送到所述蒸发器。
19.根据权利要求18的方法,其特征在于,包括从所述蒸发器送流体至所述分离器。
20.根据权利要求18的方法,其特征在于,包括从所述分离器引出气体并膨胀该气体。
21.一种低温蒸馏制氮装置,包括:
a)一蒸馏塔,具有一塔底;
b)一换热器;
c)一压缩机构,其用于压缩馈入空气并将其送入所述换热器,之后送入所述蒸馏塔;
d)一管道,用于从所述塔底引出一第一富氧液流;
e)一洗提分馏器;
f)一精馏分馏器,与所述洗提分馏器热连接;
g)一蒸发器,与所述精馏分馏器热连接;
h)一管道,用于将所述第一液流送入所述洗提分馏器;
i)一管道,用于将一第二富氧液流以及一第三气流从所述洗提分馏器引出;
j)一管道,用于将至少部分所述第二富氧液流送入所述蒸发器;
k)一管道,用于从所述蒸发器引出一流体;
l)一管道,用于将一富氮气送入所述精馏分馏器;以及
m)一管道,用于将一液体从所述精馏分馏器送入所述塔,以及,一管道,用于将富氮产品气从所述精馏分馏器引出。
22.一种低温蒸馏制氮装置,包括:
a)一蒸馏塔;
b)一换热器;
c)一压缩机构,其用于压缩馈入空气并将其送入所述换热器,之后送入所述塔;
d)一洗提分馏器;
f)一冷凝器,与所述洗提分馏器热连接;
g)一蒸发器,与所述冷凝器热连接;
h)一管道,用于将所述第一液流送入所述洗提分馏器;
i)一管道,用于将一第二富氧液流以及一第三气流从所述洗提分馏器引出;
j)一管道,用于将至少部分所述第二富氧液流送入所述蒸发器;
k)一管道,用于从所述蒸发器引出一流体;
l)一管道,用于将一富氮气送入所述冷凝器;以及
m)一管道,用于将一液体从所述冷凝器送入所述塔,以及,一管道,用于将富氮产品气从所述冷凝器引出。
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US1932903A (en) * | 1927-11-17 | 1933-10-31 | Ralph H Mckee | Process of and apparatus for liquefying gases |
GB1271797A (en) * | 1968-07-04 | 1972-04-26 | Geoffrey Gordon Haselden | Improvements in or relating to low temperature separation of gas mixtures |
US4525187A (en) * | 1984-07-12 | 1985-06-25 | Air Products And Chemicals, Inc. | Dual dephlegmator process to separate and purify syngas mixtures |
US4872893A (en) * | 1988-10-06 | 1989-10-10 | Air Products And Chemicals, Inc. | Process for the production of high pressure nitrogen |
FR2665755B1 (fr) * | 1990-08-07 | 1993-06-18 | Air Liquide | Appareil de production d'azote. |
US5257505A (en) * | 1991-04-09 | 1993-11-02 | Butts Rayburn C | High efficiency nitrogen rejection unit |
US5410885A (en) * | 1993-08-09 | 1995-05-02 | Smolarek; James | Cryogenic rectification system for lower pressure operation |
US5442925A (en) * | 1994-06-13 | 1995-08-22 | Air Products And Chemicals, Inc. | Process for the cryogenic distillation of an air feed to produce a low to medium purity oxygen product using a single distillation column system |
JP2875206B2 (ja) * | 1996-05-29 | 1999-03-31 | 日本エア・リキード株式会社 | 高純度窒素製造装置及び方法 |
US5669236A (en) * | 1996-08-05 | 1997-09-23 | Praxair Technology, Inc. | Cryogenic rectification system for producing low purity oxygen and high purity oxygen |
-
1998
- 1998-05-22 US US09/083,570 patent/US5899093A/en not_active Expired - Fee Related
-
1999
- 1999-05-14 TW TW088107895A patent/TW431904B/zh not_active IP Right Cessation
- 1999-05-17 AU AU40686/99A patent/AU4068699A/en not_active Abandoned
- 1999-05-17 JP JP2000551208A patent/JP4308432B2/ja not_active Expired - Fee Related
- 1999-05-17 CN CNB998065145A patent/CN1195194C/zh not_active Expired - Fee Related
- 1999-05-17 DE DE69910569T patent/DE69910569T2/de not_active Expired - Fee Related
- 1999-05-17 CA CA002344503A patent/CA2344503C/en not_active Expired - Fee Related
- 1999-05-17 WO PCT/US1999/007050 patent/WO1999061854A1/en active IP Right Grant
- 1999-05-17 EP EP99924106A patent/EP1086345B1/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
DE69910569T2 (de) | 2004-06-17 |
CA2344503A1 (en) | 1999-12-02 |
AU4068699A (en) | 1999-12-13 |
TW431904B (en) | 2001-05-01 |
US5899093A (en) | 1999-05-04 |
EP1086345B1 (en) | 2003-08-20 |
WO1999061854A1 (en) | 1999-12-02 |
CA2344503C (en) | 2008-09-16 |
DE69910569D1 (de) | 2003-09-25 |
JP4308432B2 (ja) | 2009-08-05 |
CN1302369A (zh) | 2001-07-04 |
EP1086345A1 (en) | 2001-03-28 |
JP2002516980A (ja) | 2002-06-11 |
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