CN1729087A - 用于预发泡热塑塑料微球的方法与装置 - Google Patents
用于预发泡热塑塑料微球的方法与装置 Download PDFInfo
- Publication number
- CN1729087A CN1729087A CN200380106874.5A CN200380106874A CN1729087A CN 1729087 A CN1729087 A CN 1729087A CN 200380106874 A CN200380106874 A CN 200380106874A CN 1729087 A CN1729087 A CN 1729087A
- Authority
- CN
- China
- Prior art keywords
- foaming machine
- microballoon
- scrapers
- ducted body
- feed arrangement
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/3461—Making or treating expandable particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/3415—Heating or cooling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/3442—Mixing, kneading or conveying the foamable material
- B29C44/3446—Feeding the blowing agent
- B29C44/3449—Feeding the blowing agent through the screw
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/36—Feeding the material to be shaped
- B29C44/38—Feeding the material to be shaped into a closed space, i.e. to make articles of definite length
- B29C44/44—Feeding the material to be shaped into a closed space, i.e. to make articles of definite length in solid form
- B29C44/445—Feeding the material to be shaped into a closed space, i.e. to make articles of definite length in solid form in the form of expandable granules, particles or beads
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
本发明涉及一种制备发泡热塑塑料微球的方法,所述方法包括将可热发泡微球填充到一发泡设备(6)中,所述发泡设备(6)包括被一中空体包围的旋转进给装置(8),和一个或多个刮刀(9)。所述发明还涉及一种用于发泡热塑塑料微球的发泡设备。
Description
技术领域
本发明涉及一种制备发泡热塑塑料微球的方法和一种发泡设备。
背景技术
可热发泡微球在现有技术中是已知的,并已在US3615972,EP486080,EP566367和EP1067151中详细描述,这些文件在此结合以作参考。在这种微球壳体中,推进剂以胶囊形式包裹在热塑壳体中。一旦加热,推进剂蒸发产生内部压力,同时随着壳体软化,导致微孔有效发泡,通常直径增大约2至5倍。
作为未发泡或预发泡的热塑塑料微球能够用于各种应用中。已发泡微球的应用例子对于干球而言是以树脂为基础的溶剂,如聚酯,对于湿球而言是以涂敷体系为基础的水,如颜料。
热塑塑料微球的完全发泡由于完全发泡所需的高温从而会导致因发泡引起的与薄热塑壳体结合而结块的问题。这需要提供一种用于制备发泡热塑塑料微球的方法和一种发泡设备,其中发泡程度能够被控制,以便有可能提供不同密度的发泡微球。还需要提供一种用于制备发泡热塑塑料微球的方法和一种发泡设备,它们简单且仅需要较小空间,相对便宜,并易于被最终用户使用,且由于已发泡微球就地被使用,从而节省了运输空间和成本。
EP0348372公开了一种制备发泡热塑塑料微球的工艺,其中发泡发生于传送带上。所述工艺运行良好,但占用较大空间且较为昂贵。
US4,722,943和US5,342,689描述了用于发泡微球的方法,其中微球混合有表面阻挡涂层以防止在干燥步骤中结块。但是,加工助剂,如滑石量非常高,而这影响了急冷的可能性。这也在控制微球发泡程度上产生困难。
发明内容
本发明的一个目的是提供一种制备热塑塑料微球的方法,所述方法能在小型设备上运行,所述方法提供最小的灰尘问题,提供最小的结块问题,且其中微球的发泡程度也比以前的方法能更容易地控制,所述方法还提供一种连续生产具有狭窄密度分布的发泡微球产品的可能性。本发明的另一目的是提供了一种用于制备适合于上述方法的发泡热塑塑料微球的发泡设备。
根据本发明,人们惊奇地发现通过制备发泡热塑塑料微球的方法和一种发泡设备而获得了上述目的。根据本发明的方法包括将可热发泡微球填充到一发泡设备中,所述发泡设备包括被一中空体包围的旋转进给装置,和一个或多个刮刀,其中刮刀防止微球层在发泡设备中的积聚,在提高微球的温度以进行发泡的同时将微球移过发泡设备,并排出微球。所述一个或多个刮刀适当地设置在进给装置的外径与中空体的内表面之间。所得到的发泡设备内的进给方向大体适当地与进给装置的旋转方向运动。
本发明还涉及一种制备发泡微球的发泡设备,所述设备包括被一中空体包围的旋转进给装置,一个或多个设置在进给装置的外径与中空体的内表面之间的刮刀。
所述方法与所述发泡设备允许连续生产发泡热塑塑料微球。
所述一个或多个刮刀,或所述一个或多个刮刀的表面层由合适的聚合材料制成,最好由耐热聚合材料制成。所述聚合材料最好是氟塑料材料,诸如PTFE,PVDF,PFA或FEP。如果聚合材料是热塑塑料,所述聚合材料的熔点适于高于约200℃,最好高于250℃。
所述一个或多个刮刀最好至少与中空体的内表面部分接触。所述一个或多个刮刀适当地具有某种挠性,于是当其压靠所述中空体的内表面时,所述一个或多个刮刀将在所述一个或多个刮刀与中空体的内表面间提供一种紧密接触。
所述中空体适当地设置有一个或多个加热器。所述加热器是合适的水套加热器。进给装置本身也适当设置有一个或多个加热器。
通过使用一装有加热器的螺旋供料器将所述可热发泡微球适当送入发泡设备的入口中。
所述可热发泡微球在进入发泡设备前被与防止微球结块的填料适当预混合。所述填料为合适的细颗粒形式,所述颗粒具有从约1·10-9到约1·10-3m,,最好从约1·10-8到约3·10-5m的颗粒直径范围。填料的例子是无机化合物,如铝粉、碳酸镁、磷酸镁、氢氧化镁、白云石、碳酸钙、磷酸钙、硫酸钙、滑石、高岭土、二氧化硅、氧化铁、氧化钛、氧化铝和氢氧化物、氧化锌、水滑石、云母、重晶石、玻璃球、飞尘、细砂、矿物纤维和普通加强纤维,硅灰石、长石、硅藻土、珍珠岩、蛭石、中空石英和陶瓷球。也可以使用有机化合物,特别是具有足够高软化温度的聚合物,纤维素、木粉、炭黑、碳纤维和石墨纤维。最好所述填料是诸如二氧化硅的氧化硅。所述填料可以以其不搀杂形式使用,或可以不同形式进行表面处理,以便提高防结块效果。对填料进行表面处理的一种方式是使其疏水。填料加入微球的重量比取决于所使用的填料,但是合适地是从约1∶1000到约5∶1,较好是从约1∶500到约1∶1,更好是从约1∶100到约1∶3,最好是从约1∶25到约1∶5。
根据本发明的方法和发泡设备能够用于已知的各种可发泡热塑塑料微球,如那些以Expancel商标销售的微球。相应的微球可以具有由聚合物或共聚物制成的热塑壳体,所述聚合物或共聚物通过聚合各种烯烃不饱合单体而获得,所述不饱合单体可以是包含如下单体的腈,如丙烯腈、甲基丙烯腈、α-氯代丙烯腈、α-乙氧基丙烯腈、富马腈(fumaro nitrile)、巴豆腈(croto nitrile)、诸如丙烯酸甲酯或丙烯酸乙酯的丙烯酸酯、诸如甲基丙烯酸甲酯、异冰片基甲基丙烯酸酯,或甲基丙烯酸乙酯的甲基丙烯酸酯,诸如氯乙烯的乙烯基卤化物,诸如偏二氯乙烯、乙烯基吡啶的偏二卤乙烯、诸如醋酸乙烯酯的乙烯酯类、诸如苯乙烯、卤化的苯乙烯、或α-甲基苯乙烯的苯乙烯类,或诸如丁二烯,异戊二烯和氯丁二烯的二烯烃。上述单体的任意混合都可以使用。有时希望用于聚合物壳体的单体能够包括交联的多功能单体,诸如二乙烯基苯、二(甲基)丙烯酸乙二醇酯、二(甲基)丙烯酸二甘醇酯、三甘醇二(甲基)丙烯酸酯、二(甲基)丙烯酸丙二醇酯、二(甲基)丙烯酸1,4-丁二醇酯、二(甲基)丙烯酸1,6-己二醇酯、二(甲基)丙烯酸丙三醇酯、二(甲基)丙烯酸1,3-丁二醇酯、二(甲基)丙烯酸新戊二醇酯、二(甲基)丙烯酸1,10-癸二酰酯、三(甲基)丙烯酸季戊四醇酯、四(甲基)丙烯酸季戊四醇酯、六(甲基)丙烯酸季戊四醇酯、二羟(甲基)三环十二烷二(甲基)丙烯酸酯、三烯丙基缩甲醛三(甲基)丙烯酸酯、甲基丙烯酸烯丙基酯、三羟甲基丙烷三(甲基)丙烯酸酯、三羟甲基丙烷三丙烯酸酯、二(甲基)丙烯酸三丁二醇酯、PEG#200二(甲基)丙烯酸酯、PEG#400二(甲基)丙烯酸酯、PEG#600二(甲基)丙烯酸酯、3-丙烯酰氧乙二醇一丙烯酸酯、三丙烯缩甲醛或三烯丙基异氰酸酯、三烯丙基异氰脲酸酯等中的一个或多个。就目前而言,这种交联单体最好由约0.1至约1重量百分比(wt%)构成,且最好由用于聚合物壳体的单体总量的约0.2至约0.5重量百分比(wt%)构成。聚合物壳体最好由全部微球的约60至约95重量百分比(wt%),且更好由约75至约85重量百分比(wt%)构成。
微球内的推进剂通常是沸点温度不高于热塑聚合物壳体的软化温度的液体。也称发泡剂或起泡剂的所述推进剂,可以是诸如n-戊烷、异戊烷、新戊烷、丁烷、异丁烷、己烷、异己烷、新己烷、庚烷、异庚烷、辛烷、异辛烷或其混合物构成的碳氢化合物。当然,其它类型的碳氢化合物也可以使用,诸如石油醚、含氯或含氟的碳氢化合物,诸如甲基氯化物、亚甲基氯化物、二氯乙烷、二氯乙烯、三氯乙烷、三氯乙烯、三氯氟甲烷等。所述推进剂适当地由微球的约5至约40重量百分比wt%构成。
微球的起始发泡温度称作Tstart,而所达到的最大发泡温度称作Tmax,它们都是以每分钟20℃的温度增长率确定的。本发明中所使用的可热发泡微球适当地具有从约20至约200℃的Tstart,最好具有从约40至约180℃的Tstart,更好具有从约60至约150℃的Tstart。本发明中所使用的可热发泡微球适当地具有从约50至约300℃,最好从约100至约250℃,更好具有从约140至约200℃的Tmax。
根据本发明,所述可热发泡微球容重的平均颗粒尺寸适当地从约1至约500μm,较好是从约3至约100μm,最好是从约5至约50μm。通过加热至超过Tstart的温度,通常可能将微球直径膨胀2至7倍,最好膨胀4至7倍。
所排出微球的密度通过选择合适的加热温度和/或微球在发泡设备中存在的时间长度而进行控制。在发泡设备中的温度适宜高于Tstart,较好是高于Tstart5至150℃,最好是高于Tstart20至50℃。微球在发泡设备内的平均停留时间为约5至约200秒,较好是约10至100秒,最好是约30至约90秒。
湿和干可热发泡微球都可以用于根据本发明的方法。然而,根据本发明的方法特别适用于具有较低含湿量的可热发泡微球。相应地,所述可热发泡微球具有超过约50重量百分比,较好超过约80重量百分比,最好超过约97重量百分比的干固体含量。
进给装置的转速适当地为约1至约100转/分,较好为约5至约90转/分,最好为约40至约80转/分。
所述一个或多个刮刀适于安装在进给装置上,并适于朝着中空体的内表面径向延伸到进给装置的外径以外。此外,所述一个或多个刮刀适于沿进给方向纵向延伸。所述一个或多个刮刀适当安装,于是所述刮刀单独或相结合实现对中空体的内表面纵向长度的从约1至约100%的刮削,较好是从约10至约100%,最好是从约20至约95%。刮刀可以具有不同的个体长度。例如可以是一个或多个长刮刀和一个或多个短刮刀的结合。最好,实现对中空体的内表面纵向长度约70至约100%的刮削的一个或两个刮刀连同1至5,最好是2至4个实现中空体的内表面纵向长度约10至约40%刮削的刮刀一起使用。如果使用太多长刮刀,就有使微球阻塞在螺杆内的危险,特别是在螺距较小情况下。相应地,刮刀的长度依据其它工艺参数,如发泡设备的尺寸、转速、微球类型、填料含量等可以调整到最合适状况。
在一些情况下,例如加入微球中的填料的重量比在约1∶100至1∶10时,刮刀实现中空体的内表面纵向长度的约20至约60%的刮削。在其它情况下,例如加入微球中的填料的重量比在约1∶10至约1∶3时,刮刀实现中空体的内表面纵向长度的约50至约100%的刮削。
安装在进给装置上的刮刀的数量合适的是1至6个,最好是2至4个。
刮削运动能够在中空体的内表面的任何部位上进行。相应地,所述一个或多个刮刀在发泡设备入口侧开始安装在进给装置上,即未发泡微球被添加的位置并从此处延伸。
在本发明的一个最佳实施例中,进给装置是螺杆形式。所述螺杆具有合适的从约0.05至约1.5、最好从0.15至约0.5的螺距与直径比。所述螺杆的螺距在螺杆的开始处,即靠近入口处要小于螺杆端部处。所述螺距是沿着螺杆逐渐增加的。可选择地,所述螺距可以是以不连续的阶段增加的,于是螺杆的一部分较之螺杆的其它部分具有不同的螺距。
在本发明的另一最佳实施例中,进给装置是一个或多个从柱心伸出的浆板(paddle)形式。所述浆板被适当布置,于是其投影角(α)相对进给方向为0<α<90°,最好为约10°至约60°。
根据本发明的方法及发泡设备,可热发泡微球的一种更容易的发泡方法被提供,所述方法要求较小的设备,并减少已发泡微球的运输成本。微球的发泡程度较之以前也更易于控制。
附图说明
图1显示了本发明的一个实施例,其中进给装置是螺杆。图2显示进给装置是螺杆形式,图3显示进给装置是浆板形式。
具体实施方式
图1显示了方法实施例,其中未发泡的热塑塑料微球从贮槽1被泵至料仓2,并经过滤器3过滤。此后,微球送入第一螺旋输送机4并送至发泡设备6的入口5,所述发泡设备6包括加热装置7,装有刮刀9的螺杆8。入口5设置有一振动器10,且螺杆被适当连接到一马达11。已发泡微球适于经出口12排出,出口12设置有一振动器13,并适于将微球泵出。
图2显示装有刮刀9,具有直径d的螺杆8。螺杆的一部分A具有螺距p1,螺杆的另一部分B具有不同的螺距p2。
图3显示进给装置是从柱心15伸出的浆板14形式的实施例。所述浆板装有刮刀16。每个浆板相对进给方向具有角度α。不同的浆板具有不同的角度α。图3所描述的进给装置可以替代图1中的螺杆。
本发明的优点将结合下文实施例进一步描述,但是所述实施例不应被理解为对本发明范围的限定。
实施例
例1:
根据本发明的包括一中空体的一种发泡设备,其具有一用作进给装置的螺杆,所述发泡设备用于热塑可发泡微球的发泡。所述螺杆长2200mm,直径为205mm。所述螺杆从入口处开始被分成相等长度的三段,每段具有不同的螺距,分别为40,50和60mm。所述螺杆上安装有4个刮刀,其中一个具有相应中空体的内表面长度的90%的长度,另三个刮刀每个具有中空体的内表面长度的25%的长度。螺杆的转速是54转/分。Expancel461DU型微球具有由容重测出的12μm的平均颗粒尺寸,且Tstart=99℃,Tmax=140℃,所述微球与相应其85份重量的疏水二氧化硅,15份重量的二氧化硅预混合。随后微球混合物送入发泡设备。微球在发泡设备内的停留时间为60秒。
平均密度为14kg/h的已发泡微球被排出。螺杆内微球没有严重的结块现象。
Claims (16)
1.一种制备发泡热塑塑料微球的方法,所述方法包括将可热发泡微球填充到一发泡设备(6)中,所述发泡设备(6)包括被一中空体包围的旋转进给装置(8),和一个或多个刮刀(9),其中刮刀防止微球层在发泡设备中的积聚,在提高微球的温度以进行发泡的同时将微球移过发泡设备,并排出微球。
2.一种制备发泡热塑塑料微球的发泡设备,所述设备包括被一中空体包围的旋转进给装置(8),一个或多个设置在进给装置的外径与中空体的内表面之间的刮刀(9)。
3.如权利要求1所述的方法,其特征在于,所述一个或多个刮刀设置在进给装置的外径与中空体的内表面之间。
4.如权利要求1或3中任一个所述的方法,或如权利要求2所述的发泡设备,其特征在于,所述一个或多个刮刀安装在进给装置上,并朝着中空体的内表面径向延伸到进给装置的外径以外。
5.如权利要求1或3-4中任一个所述的方法,或如权利要求2或4中任一个所述的发泡设备,其特征在于,所述一个或多个刮刀单独或相结合实现对中空体的内表面纵向长度的从约20至约95%的刮削。
6.如权利要求1或3-5中任一个所述的方法,或如权利要求2或4-5中任一个所述的发泡设备,其特征在于,所述一个或两个刮刀实现对中空体的内表面纵向长度约70至约100%的刮削,2至4刮刀实现中空体的内表面纵向长度约10至约40%的刮削。
7.如权利要求1或3-6中任一个所述的方法,或如权利要求2或4-6中任一个所述的发泡设备,其特征在于,所述一个或多个刮刀在发泡设备入口侧开始安装在进给装置上,并从此处延伸。
8.如权利要求1或3-7中任一个所述的方法,或如权利要求2或4-7中任一个所述的发泡设备,其特征在于,所述一个或多个刮刀,或所述一个或多个刮刀的表面层由氟塑料材料制成。
9.如权利要求1或3-8中任一个所述的方法,或如权利要求2或4-8中任一个所述的发泡设备,其特征在于,所述中空体装有一个或多个加热器(7)。
10.如权利要求1或3-9中任一个所述的方法,或如权利要求2或4-9中任一个所述的发泡设备,其特征在于,所述进给装置装有一个或多个加热器(7)。
11.如权利要求1或3-10中任一个所述的方法,其特征在于,所述可热发泡微球在进入发泡设备(6)之前,与防止微球结块的填料预混合。
12.如权利要求11所述的方法,其特征在于,所述填料是二氧化硅。
13.如权利要求11-12中任一个所述的方法,其特征在于,所填加填料与微球的重量比在约1∶100至约1∶3之间。
14.如权利要求1或3-13中任一个所述的方法,其特征在于,所述可热发泡微球具有超过约97重量百分比的干固体内容物。
15.如权利要求1或3-14中任一个所述的方法,或如权利要求2或4-10中任一个所述的发泡设备,其特征在于,进给装置是螺杆(8)的形式。
16.如权利要求1或3-14中任一个所述的方法,或如权利要求2或4-10中任一个所述的发泡设备,其特征在于,进给装置是从柱心(15)向外伸出的一个或多个浆板(14)的形式。
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CN (1) | CN100429061C (zh) |
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BR (1) | BRPI0317486B1 (zh) |
CA (1) | CA2510024C (zh) |
DE (1) | DE60332955D1 (zh) |
DK (1) | DK1572432T3 (zh) |
EC (1) | ECSP055882A (zh) |
ES (1) | ES2347143T3 (zh) |
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NO (1) | NO20053527L (zh) |
PL (1) | PL207926B1 (zh) |
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SI (1) | SI1572432T1 (zh) |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104582925A (zh) * | 2012-09-07 | 2015-04-29 | 阿克佐诺贝尔化学国际公司 | 用于制备膨胀热塑性微球的方法和装置 |
CN104582925B (zh) * | 2012-09-07 | 2017-08-01 | 阿克佐诺贝尔化学国际公司 | 用于制备膨胀热塑性微球的方法和装置 |
CN110198821A (zh) * | 2016-11-11 | 2019-09-03 | 生活实验公司 | 使可膨胀性聚合物微球膨胀的方法 |
CN110715538A (zh) * | 2019-11-15 | 2020-01-21 | 快思瑞科技(上海)有限公司 | 可膨胀微球干燥系统和方法 |
CN110860260A (zh) * | 2019-12-23 | 2020-03-06 | 快思瑞科技(上海)有限公司 | 超轻质材料连续制备系统和方法 |
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NO20053527L (no) | 2005-09-20 |
KR20050086905A (ko) | 2005-08-30 |
WO2004056549A1 (en) | 2004-07-08 |
KR100764379B1 (ko) | 2007-10-08 |
ZA200504161B (en) | 2006-08-30 |
DK1572432T3 (da) | 2010-10-11 |
JP4474285B2 (ja) | 2010-06-02 |
PL207926B1 (pl) | 2011-02-28 |
PL375898A1 (en) | 2005-12-12 |
SI1572432T1 (sl) | 2010-10-29 |
EP1572432B1 (en) | 2010-06-09 |
PT1572432E (pt) | 2010-09-03 |
EP1572432A1 (en) | 2005-09-14 |
ECSP055882A (es) | 2005-09-20 |
MXPA05005875A (es) | 2005-08-29 |
AU2003288874A1 (en) | 2004-07-14 |
BR0317486A (pt) | 2005-11-16 |
CN100429061C (zh) | 2008-10-29 |
BRPI0317486B1 (pt) | 2016-08-23 |
JP2006511360A (ja) | 2006-04-06 |
CA2510024A1 (en) | 2004-07-08 |
ATE470549T1 (de) | 2010-06-15 |
AU2003288874B2 (en) | 2006-09-14 |
UA78636C2 (en) | 2007-04-10 |
NO20053527D0 (no) | 2005-07-18 |
DE60332955D1 (de) | 2010-07-22 |
RU2301739C2 (ru) | 2007-06-27 |
CA2510024C (en) | 2008-12-02 |
ES2347143T3 (es) | 2010-10-26 |
RU2005122926A (ru) | 2006-02-27 |
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