TW201343994A - 具有可相容之支撐長絲的複合膜 - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
過濾膜具有包括長絲之支撐結構且係經塗布料塗覆以產生聚合物膜層。一些或所有該等長絲包括在該塗布料之溶劑中可溶或可膨脹之第二聚合物。該支撐結構可以紗線編織。一或多根紗線可包括包含該第二聚合物之長絲。在一實例中,經編織管狀支撐物係經基於存於NMP中之PVDF之塗布料塗覆。該編織物之一些或所有該等紗線係由雙組份芯-鞘PET-PVDF長絲製造。在該編織物中有少至4%之該等紗線由雙組份長絲製造時,該膜之剝離強度及拉力相對於全部由PET紗線製造之編織物有所改良。在實驗實例中,產生不可剝離之複合膜。可將該膜用於(例如)水或廢水過濾應用。
Description
本說明書係關於過濾膜。
下列論述不承認下文所論述之任何內容係熟習此項技術者之一般常識或背景知識。
頒予Mahendran等人之美國專利第5,472,607號闡述包括經編織管狀支撐物之中空纖維膜,在該管狀支撐物之外表面上塗覆有不對稱半滲透聚合物薄膜。經編織支撐物中之孔隙足夠小以抑制成膜塗布料之大量滲透。聚合物薄膜在上方延伸超過編織物橫截面積之外側部分33%以下。在一實例中,玻璃纖維之管狀編織物係經存於N-甲基-2-吡咯啶酮(NMP)中之聚偏二氟乙烯(PVDF)塗布料塗覆。編織物具有1.0 mm之內徑及1.5 mm之外徑。完整微濾(MF)膜具有1.58 mm之外徑。
頒予Mahendran等人之美國專利第6,354,444號闡述支撐於管狀編織物上之微濾(MF)膜或超濾(UF)膜。闡述較佳編織物之多個物理特徵。編織物可係自(例如)聚酯或耐綸(nylon)製造。在比較測試中發現,當用於曝氣、浸漬式微濾模組中時,由塗覆至聚酯編織物上之存於NMP中之PVDF塗布料製造之膜比具有玻璃纖維編織物之膜破裂頻率低。
通常如美國專利第6,354,444號中所闡述之膜用於由GE Water and
Process Technologies出售之ZeeWeed膜模組中。該等最初由Zenon Environmental公司研發之模組可能係已製造之最成功的用於膜生物皮應器(MBR)中之浸漬式膜產品。然而,儘管該等膜不破裂,但當膜塗層在苛刻操作條件下自經編織支撐物剝離時,該等膜仍偶然發生失效。該等脫層失效尤其發生在膜進入樹脂灌封塊之高應力點處。儘管纖維不破裂,但脫層使膜之排斥能力遭到破壞。
在美國專利第7,807,221號中,Shinada等人嘗試藉由在兩個單獨塗覆層中施加膜材料來增加膜材料與支撐編織物之間之黏著。在美國專利第7,909,177號中,Lee等人嘗試藉由在編織物中使用細長絲且將穩定劑添加至膜塗布料中以避免在膜與編織物之界面附近形成大型大孔隙孔來增加剝離強度。
以下說明意欲向讀者詳細說明且不限制或界定任何所主張之發明。
本說明書闡述過濾膜之替代支撐結構。該支撐結構包括長絲。該支撐結構係經聚合物膜層塗覆以產生經支撐膜。聚合物膜層不完全滲透穿過支撐結構。支撐結構之一些或所有長絲包括在用於製造膜澆注聚合物溶液(或者稱作塗布料)之膜層聚合物之溶劑中可溶或可膨脹之聚合物。膜可用於任何過濾應用中,包含(例如)飲用水過濾、三級過濾或膜生物反應器中之混合液過濾。
膜可支撐於經編織或織造支撐物上,該支撐物具有第一支撐聚合物及一或多個包括具有第二支撐聚合物之長絲之載體或紗線。第二支撐聚合物在膜塗布料之溶劑中可溶或可膨脹。第二支撐聚合物較佳亦對成膜聚合物具有高親和力。第二支撐聚合物可視情況與成膜聚合物相同。一或多個載體或紗線可視情況基本上全部由包括第二支撐聚合物之長絲組成。包括第二支撐聚合物之長絲可係第二支撐聚合物與
第一支撐聚合物或第三支撐聚合物之雙組份長絲。支撐物並未完全包埋於膜聚合物層中。
詳細說明闡述作為實例之編織物支撐之中空纖維膜。聚酯(PET)因其高拉伸強度而用於製造經編織支撐物。聚偏二氟乙烯(PVDF)因其極佳耐化學性而用於膜層。膜層係藉由用基於存於N-甲基-2-吡咯啶酮(NMP)中之PVDF之塗布料塗覆編織物來產生。然而,PVDF對聚酯具有低黏著且編織物並未完全包埋於膜層中。當用由包括PVDF之長絲製造之紗線取代PET紗線時,可改良膜之剝離強度。編織物大於一半之橫截面積係由PET製造且因此膜保留有足夠拉伸強度。然而,用PET/PVDF芯-鞘長絲之紗線替代編織物中少至4%之紗線即可提供不可剝離之膜。
不意欲受限於任何具體理論,剝離強度之改良似乎係基於兩種機制。第一,PVDF長絲對基於PVDF之塗布料具有高親和力,此促進塗布料沿具有包括PVDF之長絲之紗線或進入該紗線滲透至編織物中。第二,PVDF長絲當暴露於NMP時部分或全部溶解,此使滲透塗布料錨定至支撐結構中。
10‧‧‧經支撐膜
12‧‧‧支撐結構
14‧‧‧聚合物膜層
16‧‧‧上方區域
18‧‧‧滲透區域
226‧‧‧外表面
227‧‧‧內表面
228‧‧‧長絲
228a‧‧‧PET長絲
228b‧‧‧PET-PVDF-鞘長絲
230‧‧‧紗線
230a‧‧‧第一紗線
230b‧‧‧第二紗線
234‧‧‧自結皮
235‧‧‧支撐區域
236‧‧‧大孔隙
310‧‧‧塗覆噴嘴
312‧‧‧內筒
313‧‧‧內鏜孔
314‧‧‧軸向鏜孔
315‧‧‧螺紋接管
320‧‧‧外筒構件
321‧‧‧埠
322‧‧‧內部軸向室
325‧‧‧圓柱形基底
400‧‧‧雙組份紗線/第二紗線
402‧‧‧PVDF鞘
404‧‧‧PET芯
406‧‧‧PET-PVDF-鞘長絲
408‧‧‧PET長絲
410‧‧‧第一紗線
圖1係膜剖面之示意圖。
圖2係圖1膜之一部分之放大圖。
圖3係沿用於產生中空纖維膜之塗覆噴嘴之縱向軸之剖視圖。
圖4係由PET-PVDF芯-鞘長絲製造之紗線之一部分之剖面之掃描顯微照片。
圖5至圖10係經編織支撐物之示意圖,其中一些或所有紗線已經一或多根由PET-PVDF芯-鞘長絲製造之紗線取代。
圖11係塗覆在具有PET紗線及PET-PVDF紗線摻合物之管狀編織物上之中空纖維膜之一部分之掃描顯微照片。
圖1顯示經支撐膜10之剖面示意圖。膜10具有支撐結構12及聚合物膜層14。膜層14包含通常位於支撐結構12頂部之上方區域16。膜層14視情況亦可具有位於支撐結構12內之滲透區域18。滲透區域18(若存在)可延伸穿過支撐結構12之整個厚度但較佳延伸穿過支撐結構之一半或更小厚度。圖1中之膜10係中空纖維膜,通常具有約3 mm或更小之外徑。其他膜10可呈扁平薄片或管形式,該等管通常具有約5 mm或更大之直徑。
圖2顯示膜10之剖面之一部分之放大圖。支撐結構12界定外表面226及內表面227。該兩個表面226、227皆不規則且破裂有開口通往穿過支撐結構12之孔或通道。支撐物12可介於約0.1 mm厚與0.5 mm厚之間。膜10之上方區域16可介於約50微米厚與230微米厚之間。在中空纖維膜之情形中,內表面227可界定膜10之腔或鏜孔,該腔或鏜孔可具有介於約0.25 mm與2.3 mm之間之標稱直徑,且支撐結構12之外徑可介於約0.6 mm與約2.5 mm之間。
支撐結構12係由長絲228構成。該等長絲可視情況集合在一起形成紗線230。紗線230可藉由(例如)編織集合在一起形成薄片或管。如本文所使用,術語「經編織」及相關術語包含針織及織造結構及其相關術語。另一選擇為,支撐結構12可係由長絲228直接構成,如(例如)非織基材(例如針刺、紡黏或熔噴基材)形式。在中空纖維膜之情形中,經編織管可係自在每英吋約5根與100根緯紗之間編織約16根至96根紗線或經紗來製造。
在支撐結構12之外表面226上,在毗鄰或交叉長絲228之間或在紗線230之間(若將長絲228配置於紗線230中)存在空間或孔隙。孔隙可具有與直徑介於約10微米與100微米之間之環狀開口面積相似之中值或平均面積。可調節此範圍以適應膜塗布料。然而,大小小於10微
米之孔隙可干擾穿過膜之滲透通量。大小大於100微米之孔隙可允許過量塗布料滲透,此可導致膜腔阻塞或膜層14變厚。厚膜層14消耗過量膜塗布料且亦可引起通量減少。大孔隙往往亦與存在較少長絲228一致,此可降低支撐結構12與膜層14之間之黏著。
在圖2中,膜層14係不對稱的,其在支撐區域235上方具有自結皮234。皮234係緻密或具有界定膜10之過濾範圍之小孔之薄層。標稱孔徑之大小可(例如)介於約10 nm與1微米之間,且一些孔大於及小於標稱大小。支撐區域可含有大孔隙236。製造其之適宜膜層及方法闡述於(例如)國際公開案第WO 2010/062454 A1號中,該公開案以引用方式併入本文中。亦可使用其他膜結構。
膜10係藉由將一或多種膜塗布料澆注於支撐結構12上來產生。塗布料通常包括形成薄膜之聚合物及用於該聚合物之溶劑以及視情況其他添加劑,例如非溶劑、弱非溶劑及親水添加劑。形成薄膜之聚合物離開其與溶劑之溶液後形成膜層14。
適宜的形成薄膜之聚合物包含(例如)聚碸、聚醚碸、聚醚醚酮、聚氯乙烯(PVC)、聚偏二氯乙烯(PVDC)、氯化聚氯乙烯(CPVC)、聚偏二氟乙烯(PVDF)、聚氟乙烯(PVF)、其他含氟聚合物或共聚物、乙酸纖維素、硝酸纖維素、三乙酸纖維素、丁酸纖維素、聚丙烯腈、磺化聚醚醚酮、磺化聚碸、磺化聚醚碸、聚醯亞胺、聚醯胺、聚甲基丙烯酸甲酯、聚苯乙烯或上述之摻合物或共聚物。
膜塗布料中最常使用之溶劑包含戊烷、己烷、環己烷、乙酸乙酯、二氯乙烷、氯仿、二甲基甲醯胺(DMF)、二甲基乙醯胺(DMAc)、N-甲基-2-吡咯啶酮(NMP)、N-乙基吡咯啶酮(NET)、甲醯胺、磷酸三乙酯(TEP)、γ-丁內酯、ε-己內醯胺、二甲基亞碸(DMSO)、四氫呋喃(THF)、丙酮、六氫吡啶、咪唑及硫酸。
概言之,塗布料係在與支撐結構相對於澆注裝置之速度相關聯
之流速下引入澆注裝置(例如塗覆噴嘴、澆注冒口或澆注刀)中。塗布料流速係經選擇以提供膜層14之合意厚度。
例如,圖3顯示可用於在管狀編織物上形成聚合物膜薄膜以產生中空纖維膜之塗覆噴嘴310之剖視圖。噴嘴310包括具有內鏜孔313之內筒312,管狀支撐物穿過內鏜孔313進入螺紋接管315之軸向鏜孔314中。螺紋接管315可與筒312整合或可固定在單獨筒312末端。鏜孔314提供圓形孔口以幫助管狀支撐物在其經塗布料塗覆之前獲得環狀橫截面。圓形孔口之直徑可係在小於管狀編織物之標稱直徑約1%至10%之範圍內。將筒312插入具有圓柱形基底325之外筒構件320中。外筒320提供有內部軸向室322。引入噴嘴310之埠321中之塗布料流入室322中且然後沿牽引編織物穿過鏜孔314之方向行進。當管狀編織物前進離開鏜孔314時,其經塗布料塗覆。使經塗布料塗覆之編織物進入凝聚浴槽中。在凝聚浴槽中,藉由(例如)非溶劑致相分離法(NIPS)或熱致相分離法(TIPS)將塗布料溶劑驅逐出塗布料。在凝聚浴槽中,將形成薄膜之聚合物轉化成膜層14。
在支撐結構12中,一些長絲228包括第一聚合物且一些或所有長絲228包括第二聚合物。一些長絲228可係雙組份長絲,例如芯-鞘長絲。雙組份長絲可包括第一聚合物及第二聚合物。另一選擇為,雙組份長絲可包括第二聚合物及第三聚合物。在雙組份長絲228中,應使第二聚合物暴露於長絲228之至少部分且較佳全部外表面上。
選擇第一聚合物主要係由於其機械性質(例如強度、延展性或撓性)或諸如成本等其他因素。第二聚合物係經選擇以在膜塗布料之溶劑(例如NMP)中可溶或可膨脹。第二支撐聚合物較佳亦對塗布料之形成薄膜之聚合物具有高親和力。第二聚合物可視情況與膜塗布料中之形成薄膜之聚合物相同。可選擇第三聚合物(若存在)係由於其機械性質、諸如成本等其他因素或其在雙組份長絲中與第二聚合物之相容
性。
第一聚合物可係(例如)聚酯(PET)或聚酯之共聚物(coPET)。其他可能的第一聚合物包含(例如)聚烯烴、聚氯乙烯(PVC)、聚醯胺(PA)、聚丙烯(PP)、聚碸、聚酯碸、聚苯基碸、聚丙烯腈、纖維素及其衍生物。第二聚合物可係PVDF。其他可能的第二聚合物包含(例如)聚偏氯乙烯、聚丙烯腈(PAN)及其共聚物、聚碸、聚醚碸、聚苯基碸及其衍生物。所列示既可作為第一聚合物亦可作為第二聚合物之聚合物可適合與另一第一聚合物之其他長絲組合用作勻質長絲。
在經編織支撐物結構12中,長絲228集合在一起形成紗線230。包括第二聚合物之長絲228可以全部由包括第二聚合物之雙組份長絲構成之紗線230或以第二聚合物之勻質長絲之紗線來提供。另一選擇為,雙組份或第二聚合物長絲228可與一或多根紗線230中之第一聚合物之長絲混合。然而,本說明書在書寫時並未明確含有包括第二聚合物之長絲與第一聚合物之長絲之混合物之紗線230是否可提供與全部由第二聚合物之長絲製造之紗線230(包括第二聚合物之長絲之數目相同)相同程度之剝離強度改良。因此,當前支撐結構12較佳具有一或多根有50%或更多或所有長絲228係包括第二聚合物之長絲之紗線230。
儘管可選,但雙組份長絲228可具有減少支撐結構中在給定第二聚合物表面積中第二聚合物之總量之優點。此可因第二聚合物具有較差機械性質或因其他原因(例如其成本)而合意。介於1%與100%之間之長絲228或紗線230可係包括第二聚合物之長絲或紗線。然而,至少50%之支撐物橫截面積較佳係由第一聚合物製造。藉由使用雙組份纖維,即使所有長絲228皆包括第二聚合物,支撐結構12中之50%或更多亦可由第一聚合物製造。
在實驗實例中,製造編織物支撐之中空纖維膜,其中一些或所
有紗線經由雙組份纖維製造之紗線取代。聚酯(PET)因其高拉伸強度而被用作第一聚合物。在參照膜中,編織物係自PET長絲之紗線製造。PVDF因其極佳耐化學性而被選擇用於膜層。膜塗布料中之主要溶劑係NMP。儘管已按此方式成功製造了商業膜,但PVDF對聚酯具有低黏著且在實際應用中已出現一些膜剝離或脫層失效。如下文將更詳細地論述,當一或多根PET紗線經由包括PVDF之長絲製造之紗線取代時,可改良膜之剝離強度。編織物小於一半之橫截面積係由PVDF製造且因此膜保留有足夠拉伸強度。用PET-PVDF芯-鞘長絲替代編織物中少至4%之紗線即可提供不可剝離之膜。
實驗中之每一膜皆係支撐在以具有24個載體之規則編織物圖案(一根紗線浮在兩根毗鄰紗線上方)製造之管狀編織物上。編織物具有36-40根緯線/英吋。使用400 dtex f96及460 dtex f96聚酯(PET)扁平紗線製造兩種參照膜。如圖5中所指示,使用多個尺寸不同之兩種類型之編織物。在實驗膜中,製造新支撐結構,其中一或多根聚酯紗線在編織機上經由芯-鞘PET-PVDF雙組份長絲構成之紗線取代。雙組份長絲係由經PVDF塗覆之PET製造,且芯直徑為21 μm且外徑為26 μm。經取代之紗線係由雙組份長絲構成之467 dtex f72(由72根長絲製造之420丹尼紗線)。雙組份紗線400之一部分之剖面顯示於圖4中。在所顯示之雙組份紗線400中,長絲406各自具有PET芯404及PVDF鞘402。
在不同實驗中,24個載體中之1個、2個、6個、12個及24個載體經雙組份長絲替代,從而獲得4%、8%、25%、50%及100%之替代率。編織機具有兩個對旋載體系統。當在單載體系統中有兩個或更多個載體經替代時,經替代載體圍繞載體系統均勻間隔且產生一組平行螺旋。當6個及12個載體經替代時,每一載體系統上定位一半經替代載體,以產生雙組份紗線與PET紗線之間之交叉圖案。所得編織物結構示意性顯示於圖5至圖10中。在該等圖中,黑色紗線係編織物前側
上之PET-PVDF雙組份紗線。顯示帶有黑色邊框之紗線係編織物背側上之雙組份紗線。在兩個載體經雙組份紗線替代(8%取代率)之情形中,在一情形中,雙組份紗線(兩個經替代載體)位於一個載體系統上以產生雙平行螺旋配置,而在另一情形中,每一載體系統上有一個載體經替代以產生交叉螺旋配置(圖6及圖7)。
使用基於存於NMP中之PVDF之塗布料在編織物樣品上澆注膜層以產生鬆散超濾膜或緻密微濾膜。膜層不可自任何具有經改良編織物之膜剝離,該經改良編織物具有至少一種雙組份長絲之紗線。具體而言,由於使用標準測試設備無法將膜層自支撐結構移除,因此無法實施標準剝離強度測試。
在將膜樣品灌封至聚胺基甲酸酯之固體塊中後實施「拉脫」測試以獲得數值數據。樹脂塊中之膜長度係30 mm。由於聚胺基甲酸酯對膜之黏著高於膜層對支撐結構之黏著,因此當向膜施加足夠大的力時膜層與支撐結構之間之邊界處發生脫層。此使得可藉由量測將膜拉脫樹脂塊所需要之力來量化膜層與支撐結構之間之黏著。膜之性質概述於表1中。
如表1中所指示,甚至一根雙組份長絲之紗線亦可顯著提高拉脫強度。拉脫強度隨雙組份長絲之紗線增加而持續提高。膜品質在低取代率下通常不變,但滲透率在取代率超過25%時開始下降。然而,具有50%類型1圖案之雙組份紗線之膜之滲透率仍優於具有類型2圖案之PET編織物之膜。
不意欲受限於任何具體理論,剝離強度之改良似乎係基於兩種機制。第一,PVDF長絲對PVDF塗布料具有高親和力,此促進塗布料沿PVDF長絲滲透至編織物中。第二,PVDF長絲在暴露於NMP時部分或全部溶解,此使滲透塗布料錨定至支撐結構中。圖11顯示,儘管完成膜之膜層14對由PET長絲408、228a製造之第一紗線410、230a具有有限黏著,但其潤濕、圍繞且包埋由PET-PVDF芯-鞘長絲406、228b製造之第二紗線230b、400之相鄰外側部分。
儘管如上文所闡述之膜可用於多種應用中,但其增加的機械強度尤其可用於浸漬式膜生物反應器(MBR)中。在MBR中,膜經常經劇
烈曝氣以沖刷膜,且在灌封頭之間安裝過長膜以促使其在曝氣時擺動。此抑制積垢,但倘若膜末端固定於灌封頭中則亦會產生應力。預期增加的剝離強度可降低用於MBR及其他苛刻操作環境中之浸漬膜模組之脫層失效率。本文所闡述之膜可用於浸漬式、抽吸驅動式超濾或微濾膜模組中,例如由GE Water and Process Technologies製造之ZeeWeedTM 500系列模組。
10‧‧‧經支撐膜
12‧‧‧支撐結構
14‧‧‧聚合物膜層
16‧‧‧上方區域
18‧‧‧滲透區域
Claims (20)
- 一種形成膜之方法,其包括以下步驟,a)將複數根紗線編織成支撐結構;b)用包括形成薄膜之聚合物及溶劑之塗布料塗覆該支撐結構;及,c)使該塗布料凝聚以在該支撐結構上形成膜層,其中,d)該支撐結構包括第一聚合物;且e)一或多根該等紗線包括包含在該溶劑中可溶或可膨脹之第二聚合物之長絲。
- 如請求項1之方法,其中該第二聚合物係與該形成薄膜之聚合物相同之聚合物。
- 如請求項1之方法,其中在一或多根該等紗線中之50%或更多之該等長絲包括該第二聚合物。
- 如請求項3之方法,其中在一或多根該等紗線中基本上全部該等長絲皆包括該第二聚合物。
- 如請求項1之方法,其中該支撐結構之50%或更多係由該第一聚合物或該第一聚合物及第三聚合物構成。
- 如請求項5之方法,其中介於1%與100%之間之該等紗線包括包含該第二聚合物之長絲。
- 如請求項1之方法,其中該等包括該第二聚合物之長絲係雙組份長絲。
- 如請求項7之方法,其中在該支撐結構中介於1%與100%之間之該等紗線基本上係由雙組份長絲組成。
- 如請求項1之方法,其中該第二聚合物係與該形成薄膜之聚合物 相同之材料。
- 如請求項9之方法,其中該第二聚合物係PVDF。
- 如請求項10之方法,其中該第一聚合物係PET。
- 一種過濾膜,其包括,a)包括長絲之支撐結構;及,b)該支撐結構上之包括膜聚合物之膜層;其中,c)該支撐結構並未完全包埋於該膜層中;d)該支撐結構包括第一支撐聚合物及一或多種具有第二支撐聚合物之長絲;且,e)該第二支撐聚合物在該膜聚合物之溶劑中可溶或可膨脹。
- 如請求項12之過濾膜,其中該第二支撐聚合物係與該膜層聚合物相同之聚合物。
- 如請求項12之過濾膜,其中該支撐結構包括該第一聚合物之紗線及包括該第二聚合物之長絲之紗線。
- 如請求項14之過濾膜,其中包括該第二支撐聚合物之該等長絲係該第二支撐聚合物之雙組份長絲。
- 一種浸漬式膜模組,其包括編織物支撐之中空纖維膜,該等膜包括經編織支撐層及膜層,該膜層包括PVDF,該支撐層包括由包括PVDF之長絲製造之紗線。
- 如請求項16之浸漬式膜模組,其中該支撐層進一步包括聚酯紗線。
- 如請求項16之浸漬式膜模組,其中包括PVDF之該等長絲係具有PVDF鞘之雙組份長絲。
- 如請求項18之浸漬式膜模組,其中該等雙組份長絲具有聚酯核心。
- 如請求項16之浸漬式膜模組,其中包括PVDF之該等長絲基本上全部係由PVDF構成。
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-
2012
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- 2013-02-07 WO PCT/US2013/025110 patent/WO2013133926A1/en active Application Filing
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- 2013-02-07 EP EP13705345.0A patent/EP2822675B1/en active Active
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US9022229B2 (en) | 2015-05-05 |
CN107174961B (zh) | 2021-04-20 |
KR102031395B1 (ko) | 2019-10-11 |
WO2013133926A1 (en) | 2013-09-12 |
CN104168987A (zh) | 2014-11-26 |
EP2822675B1 (en) | 2017-05-31 |
KR20140143781A (ko) | 2014-12-17 |
ES2634032T3 (es) | 2017-09-26 |
HUE035636T2 (en) | 2018-05-28 |
CN107174961A (zh) | 2017-09-19 |
US20130233788A1 (en) | 2013-09-12 |
EP2822675A1 (en) | 2015-01-14 |
TWI597396B (zh) | 2017-09-01 |
CN104168987B (zh) | 2017-06-20 |
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