TW202103788A - 具殺生物性塗料之顆粒 - Google Patents
具殺生物性塗料之顆粒 Download PDFInfo
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- TW202103788A TW202103788A TW109108544A TW109108544A TW202103788A TW 202103788 A TW202103788 A TW 202103788A TW 109108544 A TW109108544 A TW 109108544A TW 109108544 A TW109108544 A TW 109108544A TW 202103788 A TW202103788 A TW 202103788A
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- polymer
- water
- particles
- polyamine
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Classifications
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Abstract
製備具抗菌性塗料顆粒之方法,其包括以下步驟:(a)在一混合器中於小於或等於10°C之溫度下提供一水性懸浮液,其包含一聚胺、一交聯劑及一呈顆粒形式之多孔有機或無機載體材料,使該聚胺塗覆該無機載體材料;(b)在該無機載體材料孔洞中使該有機聚合物交聯同時除去水。
Description
本發明係關於製備用於去除重金屬、較高氧化態酸或較低氧化態酸(elementic or elementous acids)之陰離子以及水溶液中特定微污染物及細菌之吸附樹脂,其中一方法包括商購離子交換體之單純外部塗覆或以含氨基聚合物完全塗覆之多孔聚合物顆粒隨後用官能化配體改變該聚合物。
根據世界經濟論壇報告(2015),水危機被定義為將影響整個全球人口之頭號全球風險。
世界衛生組織(WHO)及聯合國兒童基金會(UNICEF)也強調世界上目前有6.63億人無法獲得乾淨之飲水,有24億人使用品質不佳之水源(截至2015年)。
總體情況有多種原因,其中可提到人口之持續增長,由於氣候變遷及全球暖化導致水資源減少及被工業廢棄物污染之水資源污染加劇。因此,提高飲水品質及減少水污染至關重要。
飲水源可能被各種污染物污染。此等包括化學物質、細菌、微污染物及重金屬。出於健康原因,必須在飲用前將此等污染物從水中去除。
為了獲得安全、乾淨之飲水,有幾種去除污染物之可能方法。最普遍技術係機械過濾,其使用不同技術及方法來實現。必須借助具有較污染物小之限定孔徑之過濾器、膜等來過濾污染物。
此等過濾方法之一為逆滲透,其中大多數待過濾水被當作廢棄物丟棄(約90%),且營運成本較高(例如電力需求)。有鑑於當今世界之水資源枯竭,開發可應用於過濾飲水之符合成本效益且節水之技術非常重要。
現在很明顯地在市場上可獲得之任一技術都無法涵蓋所有可能污染物範圍。此亦適用於instrAction GmbH供應之樹脂,例如不能從水中去除「氯」。結果,需要一種有智慧及新穎之組合,其組合已知淨化技術(例如用於「氯」之活性炭)與創新之吸附樹脂(去除重金屬、較高氧化態(elementic)酸及較低氧化態(elementous)酸之陰離子、微量污染物及細菌)。
在給定污染物情況及所需消耗速率下,生產率基本上取決於在吸附樹脂床中之必要停留時間。例如,因為污染物擴散路徑短故而以小顆粒為佳,但另一方面此會以非所願方式增加反壓。較大顆粒需要較大之床,而小床難以穩定地承裝大顆粒;另一方面,由於擴散路徑較長,其很可能需要更長之停留時間。
關於市場上可取得之競爭技術,逆滲透(RO)為使用最廣泛之技術。根據Grand View Research(市場研究報告及諮詢)於2017年進行之市場研究,其在家庭飲水處理領域中約有44%市佔率。2016年全球銷量總計為2.1億單元。
逆滲透模組之嚴重缺點為產率很差。僅引入水之10-20%實際上經淨化可供客戶使用。另一缺點為需要泵及水質而必須使用電力:RO系統提供之淨水不含必要鹽類,故一定要另行添加(例如鈣及鎂)。
在蒸餾方法中常見耗能極高之缺點。此外,如同在逆滲透下,還去除掉能促進健康之元素,結果形成不適合長期使用之蒸餾水,且必須於後續步驟中再添加重要成分(如鎂鹽)。
將多種過濾技術結合在單獨之單元/濾芯(cartridges)中之淨水機需要帶有相應之閥門或連接器之複雜管道(piping),但是此等閥門或連接器易出現故障且可能導致洩漏等。此外,由於流動環境對於細菌等而言連接器正是具特佳生長機會之位置。
於市場上已知在使用之過濾介質例如有活性炭,用作為具線性通流濾芯中之顆粒填充床或用作具徑向通流之壓製中空圓筒。
同樣能與重金屬結合之離子交換樹脂會與鈣及鎂競爭因而不可靠,或者在該離子交換體總容量耗盡前就會從該樹脂中小量洗出濃縮形式之重金屬。同時,特別在有硬水存在時,會非常快地達到耗盡狀態。從那時起,再也無法去除重金屬。而在該離子交換體上無法移動之重金屬離子會以相對較小之體積被洗脫,因為該等重金屬離子會被存在之過量鹼土金屬置換。同時,鈉離子會藉由該離子交換體被釋放到水中:人們越來越懷疑飲水中高鈉含量與嬰兒食品及心血管疾病有關。除重金屬外,較高氧化態(elementic)酸及較低氧化態(elementous)酸(如硒化物、硒酸鹽、砷化物及砷酸鹽)之陰離子被懷疑與消費者及用水者之健康狀況有關。
由此產生之目的係製備用於重金屬及較高氧化態(elementic)酸及較低氧化態(elementous)酸之陰離子之穩定廉價吸附材料,其能夠可靠地、高產量地淨化水同時仍能去除細菌。
本發明目的係藉由一種製備具抗菌性塗料顆粒之方法來實現,其中該方法包括以下步驟:
(a) 在一混合器中在小於或等於10°C之溫度下提供一水性懸浮液,該水性懸浮液包含一聚胺、一交聯劑及一呈顆粒形式之多孔有機或無機載體材料,其係用於使該聚胺塗覆該無機載體材料;
(b) 在該無機載體材料孔洞中使該有機聚合物交聯同時除去水。
在本發明意義內較佳為至少重複一次步驟a)及b)。
根據該方法之一較佳具體實施例,該交聯步驟係在攪拌反應器中進行。
已證明對於以非脫鹽狀態使用之該聚胺有利。
該有機載體聚合物較佳為聚苯乙烯。
根據另一具體實施例,該有機載體聚合物係一強陰離子交換體或一弱陰離子交換體,該有機載體聚合物僅在其外表面上塗覆聚合物。那些具有磺酸基團之有機聚合物被稱為強陰離子交換體。弱陰離子交換體係具有羧酸基團之聚合物。
根據本發明一其他具體實施例,該有機聚合物係選自於聚苯乙烯、聚甲基丙烯酸酯及聚丙烯酸酯。
該聚合物也可為一無機聚合物,其係選自於矽膠及羥磷石灰。
此外,較佳為該聚胺係聚乙烯胺。
本發明一其他主題係殺生物性多孔顆粒,較佳為一交聯之聚胺,其可根據上述方法獲得或製備。
本發明又一主題為吸收重金屬之多孔顆粒,其係根據上述方法製備。
本發明一其他主題為吸附性多孔顆粒,其吸附該較高氧化態(elementic)酸及較低氧化態(elementous)酸(如亞硒酸鹽(selenides)、硒酸鹽(selenates)、砷化物(arsenides)及砷酸鹽(arsenates))之陰離子,其中該顆粒可根據上述方法獲得或製備。
帶有四個氧原子之元素週期表第15及16族(以前為第5及6主族)化合物被稱為較高氧化態(elementic)酸或較高氧化態酸之陰離子,例如H3
AsO4
或AsO4 3-
、H3
SeO4
或SeO4 3-
。
帶有三個氧原子之元素週期表第15及16族化合物被稱為較低氧化態(elementous)酸或該較低氧化態酸之陰離子,例如H3
AsO3
或AsO3 3-
、H3
SeO3
或SeO3 3-
。
如同活性炭,離子交換體也會受微生物污染並在其表面形成生物膜。因此,最終他們認為即使微生物污染程度低之飲水在所謂「淨化」後也會含有更多細菌。
由此而生之目的係提供諸如在飲水軟化中所使用之具抗菌性表面之離子交換體,而不會顯著降低離子交換體能力。
同時,潛在性有毒之微污染物正逐漸成為公共利益及專家所關注之焦點。
此尤其適用於全氟表面活性劑(perfluorinated surfactants)(如全氟辛酸、全氟辛烷磺酸),其無法或很難被生物降解因而具有極高之耐久性(„Sachstandsbericht ADONA und perfluorierte Substanzen” [“Assessment report ADONA and perfluorinated substances”],來源:Bavarian State Office for Health and Food Safety)。
有一系列非常低效且昂貴之用於從飲水中去除全氟表面活性劑之方法存在,諸如通過活性炭過濾(對此類型污染物僅有很低之能力)、或膜處理法(儘管其提供清潔飲水但同時產生包含濃縮形式全氟表面活性劑之大量廢水)。此外,必須以一定之成本對其進行處理(通常焚化)否則其將再次進入廢水中。據吾人所知,目前還沒有高效能全氟表面活性劑之選擇性吸附劑。
由此而生之目的係修改及進一步開發已知樹脂,使得其可從飲水中去除重金屬及細菌外還可從飲水中去除全氟表面活性劑。
已知樹脂可從飲水中去除重金屬(WO2015EP01754、 WO2016EP78787)及細菌(DE102017007273.6)。於此氨基聚合物被固定在相應載體上,與雙官能交聯劑反應以形成穩定三維網絡。因此該樹脂既適合作為飲水淨化設備之重金屬過濾器,又適合於在正交法(orthogonal methods)淨化級聯(cascade)終端用於去除重金屬之「保衛過濾(police filters)」之過濾器。
在製備樹脂之第一步,所需之塗料聚合物,聚乙烯甲醯胺在類聚合物反應中藉氫氧化鈉溶液生產及水解以形成聚乙烯胺(PVAm)。然後,藉耗時且高成本之錯流過濾(crossflow filtration)去除試劑及分離產物。該脫鹽聚合物溶液現在用於第二步中用以塗覆該載體材料。
由環境問題(減少能源耗費及廢水量)及飲水淨化系統市場需求導致之目的為簡化製備過程,使其更便宜且更節約資源。
到目前為止,僅已知所謂MetCap®顆粒可成功地從溶液中去除細菌(DE102017007273.6),其係以矽膠為基礎或無需載體即可使用。在DE102017007273.6中揭露製備方式及活性檢測。其描述用非脫鹽聚合物塗覆之矽膠顆粒(作為模板)及隨後該無機載體之溶解及其抗菌性活性。
對於以有機載體(例如聚苯乙烯)為基礎之顆粒,到目前為止還沒有相應之活性。現在可以驚奇地在根據新方法製備之聚苯乙烯系樹脂上建立該活性。此觀點令人驚訝,因為聚苯乙烯通常傾向於形成顯著生物膜,當然不能去除細菌。顯然地,該新穎塗料可以確保細菌不在聚苯乙烯表面上生長,而是迫使細菌離開基質(於此為飲水)。
出於指定原因而導致一系列目的在於開發及進一步開發已知樹脂,其目標如下:簡化現用於生產instrAction MetCap及BacCap樹脂之製備方法,減少廢物流,藉由結合離子交換體軟化性能與已知金屬或細菌結合性能擴大產品範圍以及用於結合全氟表面活性劑之吸附樹脂之製備(此代表飲水處理中一日益嚴重之問題)。此外,將產品範圍擴展到有機載體(例如聚苯乙烯)將具有很大優勢,因為可以廉價地獲得不同規格(顆粒尺寸及孔徑)。聚苯乙烯具有良好之機械性能,且在市場上已經很成熟。
藉由省去該聚合物水解產物之脫鹽步驟以及進一步之處理改變可簡化使用聚苯乙烯系樹脂之製備過程,其特別涉及於添加及乾燥該載體聚合物以形成該聚合物溶液。
出乎意料地,可藉由固定在多孔聚苯乙烯顆粒上而無需對該聚合物溶液進行預先脫鹽之情況下製備MetCap®及BacCap®樹脂。此更令人驚訝,因為在較早研究中發現該聚合物在多孔載體上之沉積或固定速率顯然取決於該聚合物水解產物之鹽含量。
藉由調整塗覆方法(例如多重塗覆、在Lödige犁刀式混合機中乾燥、引入新洗滌策略),可以省去該聚合物水解產物脫鹽複雜昂貴之方法步驟,而不必接受產品效率限制。
總而言之,可以說改變製備方法(特別為藉由膜過濾省去脫鹽步驟)及擴展為有機載體材料帶來決定性優勢。
該聚合物含量現在由該聚合作用中之批次計算確定。令作者驚訝地,該塗覆及在Lödige真空鏟式乾燥機(shovel dryer)中與乙二醇二環氧丙基醚(ethylene glycol diglycidyl ether)之預交聯與不含鹽PVAm聚合物溶液作用完全相同。然後在製備用於後交聯之懸浮液時,將所含鹽類部分溶出。在藉助氫氧化鈉溶液將載體之矽膠溶解後,將所有鹽類(矽酸鹽(silicates)、甲酸鹽(formates)、氯化物(chlorides)等)從經交聯之單純有機模板材料中沖洗掉。如此獲得之BacCap®T或MetCap®T材料具有與根據使用脫鹽PVA聚合物方法製備之吸附樹脂相同性能。此為該方法之第一個改良,其為很大之驚喜,因為迄今為止普遍假設(文獻資料也證實)該聚合物溶液中高濃度鹽數量要求將僅由於其尺寸而阻止有效完全地將聚合物填充到顆粒中。
第二種方法涉及具抗菌性PVA聚合物殼之商購強或弱離子交換體塗料。
商購離子交換體,尤其為於此所使用之陽離子交換體,通常有共價結合到該聚合物載體 (例如聚苯乙烯、丙烯酸酯等)上之酸性基團。在弱離子交換體情況下該酸性基團為羧酸或羧酸鹽,而在強離子交換體情況下該酸性基團為磺酸或磺酸鹽。兩種類型都用於軟化飲水。
為了使此等離子交換體具有抗菌性同時又不會顯著降低其軟化能力,只尋求該顆粒之外部塗覆而不改變該顆粒孔洞中之酸性基團,大部分承載能力酸性基團都位於此。
藉由使用相應聚合物來實現此目標,該聚合物由於其尺寸及流體動力學半徑而不能滲透到該離子交換體顆粒之孔洞中。在商購離子交換體之情況下,孔徑在20 nm至100 nm範圍內。對於尺寸為10,000-20,000 g/mol之聚合物而言,此等孔洞無法滲透。
在該方法中,在一較佳具體實施例中,僅塗覆在該顆粒半徑處測量之該顆粒外部之2-25%。更佳地,僅塗覆在該顆粒半徑處之該顆粒外部之2-10%。最佳地,僅塗覆在於半徑觸測量之該顆粒外部之2-5%。
到目前為止,大多數能進行離子交換之基團仍然可以用此方式軟化水。
相應尺寸之該非脫鹽聚合物也可以用於此目的,但此並非強制前提。也可能為含脫鹽聚合物之塗料,也可使用非脫鹽聚合物。
用氫氧化鈉溶液水解聚乙烯胺之醯胺基團然後用鹽酸中和,該聚合物含有呈甲酸鈉及氯化鈉形式之大約15-25 wt%之鹽。在該非脫鹽聚合物之情況下,該水溶液中該聚合物之含量相當於9-13重量%。
在迄今為止之方法中,藉逆滲透以複雜方式去除鹽,並使用鹽含量小於2.5重量%之該聚合物。該新方法可以省去這一複雜而昂貴之脫鹽步驟。因此,在新方法中,較佳使用鹽含量為2.5-15重量%之部分脫鹽聚合物。更佳為使用鹽含量為10-15重量%之部分脫鹽聚合物。最佳為使用鹽含量為15-25重量%之非脫鹽聚合物。實施例 1
1712 g 濕載體材料,Lewatit S1567 離子交換體,被直接輸送到VT5犁刀式混合機(Lödige)中。然後於80°C乾燥該離子交換體60 min。秤量乾燥離子交換體以確定水分損失。已去除掉380 g水。將乾燥機中之產品溫度調整為10°C。以每分鐘180轉之速度運行該混合機。一旦混合桶中之產品溫度達到10°C就加入225 g離子交換體,非脫鹽聚乙烯胺溶液批次: PC 18007 (聚合物含量10%)降溫至10°C,秤量1 g 乙二醇二環氧丙基醚 (EGDGE) [2224-15-9]至容器中,加入去離子水直至總體積達到350 ml。在10分鐘內將該混合物放入該混合機中,並在10℃下混合1 h。然後,在80°C及50 mbar減壓下交聯該聚合物被吸附物2 h。然後將該塗覆聚合物之離子交換體冷卻至室溫。
然後將該顆粒轉移到合適之吸濾器中,並用以下溶劑(BV=床體積)洗滌:3 BV 0.1 M NaOH,3 BV去離子水,3 BV 0.2 M HCl,3 BV水,6 BV 0.1 M NaOH,6 BV去離子水。獲得為水濕顆粒之BacCap產品。實施例 2
在孔隙率3玻璃料(frit)上用15 l去離子水洗滌3 l Lewatit S 8227(Lanxess)。秤量 2270 g 濕離子交換體放入VT 5真空鏟式乾燥機(Lödige)中。在80°C夾套溫度30 mbar壓力及57 rpm轉速下乾燥該離子交換體2小時。在乾燥後,將915 g乾燥之離子交換體倒回至該VT 5真空鏟式乾燥機中。將夾套溫度調節到4°C,當產品溫度低於20°C時,在15分鐘內通過蠕動泵將600 ml去離子水輸送到以180 rpm轉速運行之該混合機中。對於該塗料,227 g 聚乙烯胺溶液(聚合物含量10%)批次:秤量PC 18007及227 g 去離子水至容器中。作為交聯劑,9.20 g 乙二醇二環氧丙基醚 (EGDGE) [2224-15-9]被秤量至另一容器中。將該交聯劑加入至該聚合物溶液中充分混合。然後使用蠕動泵在5 min內將該混合物輸送到Lödige混合機中。將該混合機旋轉速度調節至240 rpm,並將夾套溫度保持在4℃。加入後,以240 rpm繼續混合15分鐘。然後將該乾燥機夾套溫度調節至80°C,並將轉速控制在120 rpm以下。
然後,將該顆粒再次降溫至室溫然後轉移到合適之吸濾器中,並用以下溶劑洗滌:3 BV 0.1 M NaOH,3 BV 去離子水,3 BV 0.1 M HCl,6 BV水。獲得為水濕顆粒之BacCap產品。實施例 3
500 g 載體材料,具有1.35 ml/g吸附能力之磺化聚苯乙烯PRC 15035 (平均孔徑450 Å,平均顆粒大小500 μm),被直接吸入VT5犁刀式混合機(Lödige)。將乾燥機中之產品溫度調整為10°C。該混合機以每分鐘180轉之速度運轉。一旦混合桶中之產品溫度達到10°C,225 g非脫鹽聚乙烯胺溶液批次:將 PC 16012 (聚合物含量12%)降溫至10°C,秤量20 g 乙二醇二環氧丙基醚 (EGDGE) CAS No. [2224-15-9]及430 g 去離子水放入容器中。將混合物在10 min內放入混合機中,並在10℃下混合1 h。然後,在65°C下交聯該聚合物被吸附物。然後使該產品降溫至室溫。然後將顆粒轉移到合適之吸濾器中並用以下溶劑洗滌:3 BV 1 M NaOH, 3 BV 去離子水,3 BV 2 M HCl,3 BV水,6 BV 1 M NaOH,6 BV 去離子水。獲得1297 g水濕顆粒產品。陰離子容量(AIC): 471 μmol/g。實施例 4
製備顆粒徑為100μm之交聯聚合物之多孔顆粒之說明(批次: BV 18007): 1st
製備聚合物被吸附物:750 g 載體材料,矽膠 (AGC Si-Tech Co. M.S Gel D-200-100批號: 164M00711),被直接輸送到到VT5犁刀式混合機(Lödige)中。產品溫度被調整為10°C。該混合機以每分鐘180轉之速度運轉。一旦混合桶中產品溫度達到10°C,1125 g 非脫鹽聚乙烯胺溶液批次:PC 18007 (聚合物含量10%),降溫至10°C,被秤量放入容器中並加入23.2 g 乙二醇二環氧丙基醚 (EGDGE) CAS No. [2224-15-9]。將混合物在10 min內放入混合機中並在10℃下混合1 h。然後,在80°C及50 mbar乾燥該聚合物被吸附物(approx. 2 h)。然後使該塗覆之矽膠降溫至10°C。對於2nd
塗覆,降溫至10°C之750 g 聚合物溶液PC 18007 (聚合物含量10%)被秤量放入容器中並加入15 g 乙二醇二環氧丙基醚 (EGDGE) CAS No. [2224-15-9]。在5 min內將該聚合物溶液倒入至該混合桶中。在10°C混合該聚合物被吸附物30 min。然後,Lödige混合機之溫度再次升高至65°C經1 h。將3 l 去離子水加入至該聚合物被吸附物中。該懸浮液係被用於交聯。將懸浮在水中該經塗覆之矽膠轉移至10-l 具自動溫度控制之玻璃反應器中。將該懸浮液攪拌並加熱至80℃。然後,在20 min內將317 g 環氧氯丙烷CAS No. [106-89-8]加入,結果反應器中溫度不超過85℃。然後在20 min內將211 g 1,2-乙二胺 [107-15-3] 逐滴加入。然後在20 min內第二次添加317 g環氧氯丙烷CAS No. [106-89-8],接著再次加入211 g 1,2-乙二胺 CAS No. [107-15-3]。最後,最終加入317 g 環氧氯丙烷CAS No. [106-89-8]並於85°C攪拌該反應1 h。然後將該反應混合物降溫至25℃,加入1500ml 50%NaOH並攪拌反應混合物12 h。然後將模板顆粒轉移到合適之吸濾器中,並用以下溶劑洗滌:3 BV 1 M NaOH,3 BV 去離子水,3 BV 2 M HCl,3 BV水,6 BV 1 M NaOH及6 BV 去離子水。
獲得之產物為濕濾餅。實施例 5
根據實施例1、實施例3或實施例4製備之一吸附樹脂被懸浮在溶劑(例如DMF)中。然後,將 110 mol%之2,2,3,3,4,4,5,5-八氟戊基環氧丙基醚(glycidyl-2,2,3,3,4,4,5,5-octafluoropentyl ether)(基於起始樹脂之氨基基團,圖2)加入至該經攪拌之樹脂懸浮液中於70°C攪拌12 h。然後,用注射器及以下溶劑沖洗懸浮液:3 BV DMF,3 BV n-庚烷,3 BV 1 M於DMF中之HCl,3 BV於DMF 中之1 M NaOH及 3 BV DMF。再次製備DMF中之50% 懸浮液。在第二個反應步驟中,再次將110 mol%之2,2,3,3,4,4,5,5-八氟戊基環氧丙基醚(glycidyl-2,2,3,3,4,4,5,5-octafluoropentyl ether)加入至此懸浮液中。然後將反應混合物在70℃下攪拌12h。然後,用以下溶劑洗滌該吸附樹脂:3 BV DMF,3 BV n-庚烷,3 BV 1 M於DMF中之HCl,3 BV於DMF中之1 M NaOH及3 BV MeOH。然後在真空中乾燥該吸附樹脂至恆重。
該吸附樹脂的結構如圖1所示。實施例 6
將實施例5中製備之吸附樹脂、活性炭(100Å,45μm)及商購C-18 層析凝膠(Kromasil,C18,100Å,10μm)分別倒入33.5 x 4 mm尺寸之HPLC管柱中,將層析管柱密封,然後對其進行正面分析(frontal analysis)。為此,要製備100 ppm全氟辛酸水溶液,並泵送通過層析管柱直到容量用盡。在205 nm下之UV光譜法測量突破(breakthrough)。
下表(表1)列出在三種吸附物上測得之全氟辛酸吸附物容量:
表1全氟表面活性劑選擇性instrAction凝膠ND 150201與商購吸附劑之全氟辛酸容量
ME 15036 | |||
管柱 | PV 150778 | PV 150775 | PV 150772 |
樹脂批號 | EP 14433 | EP 15010 | ND 150201 |
全氟辛酸 | Kromasil C18 | 活性炭 | 改良之instrAction樹脂 |
吸附[mg/ml相] | 0 | 64 | 220 |
如表1所示,全氟辛酸在instrAction相(批號ND 150201)上之吸附容量約比活性炭大3-4倍。商購RP18凝膠顯示未吸附全氟辛酸。
正面分析突破曲線如圖3所示。實施例 7
製備instrAction樹脂(按實施例3製備BV 18009)在水中之懸浮液,並以軸向通流方式倒入濾芯中,以使床體積約為100毫升(床尺寸:平均約6.3 x 9 cm)。
然後,以每小時100-500 ml/min(60-300 BV/h)流速分階段增加地將大腸桿菌(104
-105
CFU/l)懸浮液泵入濾芯中。在每個流速階段3-5分鐘後收集流出液,然後使用標準程序檢查殘留細菌。
調查結果如圖5所示:在整個調查範圍內,流出液中均未檢測到細菌。此意指細菌會以與飲水相關濃度被完全清除。實施例 8
如下研究在實施例3中製備之InstrAction樹脂對綠膿桿菌(P. aeruginosa)之活性:將500g用自來水洗滌之樹脂在反應容器中與106
CFU之綠膿桿菌在10ml自來水中懸浮液一起溫育。在3、6、12及24小時後取樣,並使用標準程序檢查綠膿桿菌。結果如圖6所示:溫育僅三個小時後細菌就不再被檢測到。實施例 9
濾水壺(jugs)
將來自Brita及BWT行業慣用濾水壺裝滿根據實施例1或2及實施例3所製備之本發明instrAction樹脂與活性炭比例為1:1之混合物,並與加入銀原始濾芯進行比較,比較細菌生長。
為此,首先將1 l之8.3 x 105
cfu/l大腸桿菌懸浮液添加到濾芯中,將其儲存並研究3週後洗脫細菌。
調查結果如圖7所示。
不出所料,由於BWT及Brita中添加有銀之原始濾芯沖洗介質中沒有檢測到細菌因為濾芯中添加之銀被部分洗脫,從而阻止細菌在濾液中生長。含有於此請求專利之樹脂及活性炭混合物之濾芯,同樣也不會檢測到細菌或僅檢測到與輸入量相比被強烈減少至接近檢測極限之少數細菌。
因此證明本申請案請求專利之樹脂之抑菌作用。因此,在濾芯中不需要添加之銀係多餘。
與添加銀之商業濾芯相比,填充有本案請求之樹脂及活性炭混合物之濾芯之過濾速度(對於應用而言很重要)係在相同範圍內。
圖1:2,2,3,3,4,4,5,5-八氟戊基環氧丙基醚(Glycidyl-2,2,3,3,4,4,5,5-octafluoropentyl ether)。
圖2:全氟表面活性劑吸收劑兩種結構異構體之一(R = 聚合物)。
圖3: PV 150772之層析突破外廓 (instrAction樹脂批次:批次no. ND 150201);直到大約900 min或每毫升樹脂220 mg全氟辛酸之後,才能達到突破。
圖4:研究BacCap樹脂降低細菌之實驗裝置:1.帶有細菌(E. coli)懸浮液(104
Cfu/l)之儲存容器,2. 泵,3. 帶有instrAction BacCap樹脂之管柱/濾芯,4. 分次)。
圖5:僅在外部塗覆離子交換體上動態除菌結果。
圖6:在靜態條件下,存在instrAction BacCap樹脂情況下綠膿桿菌濃度隨時間變化。
圖7:抑菌效果。
Claims (13)
- 一種具抗菌性塗料顆粒之製備方法,其中該方法包括以下步驟: (a) 在一混合器中在小於或等於10°C之溫度下提供一水性懸浮液,該水性懸浮液包含一聚胺、一交聯劑及一呈顆粒形式之多孔有機或無機載體材料,其係用於使該聚胺塗覆該無機載體材料; (b) 在該無機載體材料孔洞中使該有機聚合物交聯同時除去水。
- 如請求項1所述之方法,其中步驟a)及b)被重覆至少一次。
- 如請求項1或2中任一項所述之方法,其中該交聯步驟係在攪拌反應器中進行。
- 如請求項1至3中任一項所述之方法,其中該聚胺係在非脫鹽狀態下使用。
- 如請求項1至4所述之方法,其中該有機聚合物係一聚苯乙烯。
- 如請求項1至4所述之方法,其中該有機聚合物係強或弱陰離子交換體,僅其外表層經以該聚合物塗覆。
- 如請求項1至4所述之方法,其中該有機聚合物係選自於聚苯乙烯(polystyrene)、聚甲基丙烯酸酯(polymethacrylate)及聚丙烯酸酯(polyacrylate)。
- 如請求項1至4所述之方法,其中該聚合物係一無機聚合物,其係選自於矽膠(silica gel)及羥磷石灰(hydroxyapatite)。
- 如請求項1至7中任一項所述之方法,其中該聚胺係一聚乙烯胺(polyvinylamine)。
- 一種多孔顆粒,其係根據請求項1至9中任一項所述之方法製備。
- 一種如請求項10所述之多孔顆粒之用途,其用於去除水、飲水或其他水溶液中細菌。
- 一種如請求項10所述之多孔顆粒之用途,其用於去除水、飲水或其他水溶液中重金屬。
- 一種如請求項10所述之多孔顆粒之用途,其用於去除較高氧化態酸(elementic acids)陰離子及較低氧化態酸(elementous acids)陰離子。
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DE102005021221A1 (de) * | 2005-05-07 | 2006-11-09 | Geohumus International Gmbh & Co. Kg | Superabsorber mit anorganischen und organischen Ballast- und Zusatzstoffen |
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