TW201534395A - 奈米膠體粒子載持體之製造方法及其載持體 - Google Patents
奈米膠體粒子載持體之製造方法及其載持體 Download PDFInfo
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Abstract
本發明提供一種可獲得下述奈米膠體粒子載持體之製造方法,該奈米膠體粒子載持體可抑制奈米膠體粒子間之凝聚而使膠體溶液可高濃度化,且長期儲存下仍可保持粒子大小,亦容易再分散。前述製造方法具有以下步驟:獲得已在界面活性劑溶液中溶解或潤脹的多醣類系高分子之步驟;及,將該已溶解或潤脹的多醣類系高分子與使奈米膠體粒子分散於分散介質中而成的奈米膠體液混合之步驟;藉由前述製造方法即獲得使奈米膠體粒子受載於多醣類系高分子之載持體。
Description
本發明係有關於奈米膠體粒子載持體之製造方法、及以該製法獲得之奈米膠體粒子載持體。
奈米膠體粒子在使用於如燃料電池及廢氣淨化用的催化劑時,係以陶瓷及高分子等基材浸漬於金屬奈米膠體溶液中,以進行吸附。其中,在奈米膠體粒子的比表面積越大時越可提高催化劑作用,因此膠體溶液中的奈米膠體粒子須要高濃度化。然而另一方面,在粒子高濃度化時則易產生由於粒子間凝聚的粗大化,因此此種凝聚有加以抑制之須要。
由於要滿足此種相反之要求,必須添加在一個分子內含疏水基及親水基的分散劑及保護劑,經由吸附在奈米膠體粒子表面、包覆在粒子中,而抑制奈米膠體粒子間凝聚,增加分散性,獲得高濃度奈米膠體粒子分散液(如專利文獻1)。
然而,在此種奈米膠體粒子以分散劑包覆之情形時,又會有奈米膠體粒子所期望之催化劑作用等受分散劑
所阻礙的問題。
此外,專利文獻2中,曾揭示在聚氯化乙烯等乙烯系高分子之表面利用還原劑使金微粒附著所獲得之高分子材料。同時,專利文獻3中,則揭示在主成分為纖維素之纖維上載持含白金族元素之催化劑的固體催化劑,該固體催化劑,係以如在含催化劑的溶液中將上述纖維浸泡之後再加以乾燥所得。然而,該專利文獻2、3所載之方法中,均有不易獲得高濃度載持體的問題。
另外,專利文獻4中,曾揭示在纖維素奈米纖維的表面載持金屬奈米粒子之複合物。其中記載該製法,係在表面含羧基或羧酸基的纖維素奈米纖維之此等基之上鍵結金屬化合物之後,再以添加還原劑等,使鍵結在上述羧基等之上的金屬化合物還原成金屬奈米粒子。然而,該奈米膠體粒子載持體,亦有在高濃度下在調製時所載持的奈米膠體粒子會粗大化等,使粒徑之控制不易的問題。
進而,專利文獻5中,曾揭示一種使金屬銀膠體載持於纖維化之纖維素的消臭紙,並記載其係將水溶性銀化合物在陽離子性界面活性劑及複合金屬氫化物(還原劑)存在下還原而得。然而,該方法中,金屬膠體粒子被大量使用之界面活性劑包含,因此無法使用在催化劑等其他領域中。
專利文獻1:日本專利特許第4865772號公報
專利文獻2:日本專利特許第5114008號公報
專利文獻3:日本專利特開2011-98280號公報
專利文獻4:國際公開WO 2010/095574號公報
專利文獻5:日本專利特開2006-261709號公報
鑑於上述情況,本發明之目的便在於提供一種使奈米膠體粒子載持於載持體並解決上述問題的奈米膠體粒子載持體及其製造方法。亦即,目的在於提供下述奈米膠體粒子載持體以及可以簡便方式獲得該載持體之製造方法:該載持體不會在奈米膠體粒子間發生凝聚而使膠體溶液可高濃度化,在長期儲存下仍可保持粒子大小,且奈米膠體粒子表面幾乎未經界面活性劑包覆,亦容易再分散。
為解決上述問題,本發明之奈米膠體粒子載持體之製造方法,設定為具有以下步驟:獲得已在界面活性劑溶液中溶解或潤脹的多醣類系高分子之步驟;及,將該已溶解或潤脹的多醣類系高分子與使奈米膠體粒子分散於分散介質中而成的奈米膠體液混合之步驟;且,獲得使奈米膠體粒子受載於上述多醣類系高分子的載持體。
上述方法中,奈米膠體粒子可使用選自金、銀、鉑、鈀、釕、銠、鋨、銥、及銅中之1種或2種以上金屬及/或上述1種或2種以上金屬之合金粒子。
又,界面活性劑可使用選自4級銨鹽及羧酸鹽中
之1種或2種以上。
上述界面活性劑的用量宜相對於奈米膠體粒子100質量份在1至10質量份之範圍內。
上述多醣類系高分子可使用選自纖維素、幾丁質、及幾丁聚醣中之1種或2種以上。
上述多醣類系高分子之平均纖維口徑在20至1000nm之範圍內為佳。
本發明之奈米膠體粒子載持體係以上述本發明之製造方法製造,形成奈米膠體粒子經由上述界面活性劑受載於上述多醣類系高分子者。
上述奈米膠體粒子的載持量宜相對於上述多醣類系高分子100質量份在1至15質量份之範圍內。
依據本發明之製造方法,可製得下述奈米膠體粒子載持體:可抑制奈米膠體粒子間凝聚而粗大化(二次凝聚),且即使在經長期保存而沉澱時,仍可藉由將容器輕輕振盪等簡便之操作而再分散。
上述奈米膠體粒子載持體中,雖認為經由所添加之界面活性劑使奈米膠體粒子吸附在多醣類系高分子上,但該奈米膠體粒子並未被界面活性劑所包含,除上述吸附部分之外幾乎粒子的表面部分均露出,因此亦可發揮使奈米膠體粒子原本所有之催化劑作用等幾乎不減低的效果。
而且,本發明中所使用之上述多醣類系高分子,種類並無特別之限定,藉由添加界面活性劑,可提高奈米
膠體粒子受載於多醣類系高分子之比例,並且,在保存時,與未使用界面活性劑者相比,還可發揮粒徑長期穩定之效果。
加之,不同於同時進行奈米膠體粒子之形成及奈米膠體粒子載持體之形成的先前技術,分為形成奈米膠體粒子之步驟(奈米膠體液調配步驟)、及使所調配之奈米膠體液與纖維素奈米纖維分散液混合以形成奈米膠體粒子載持體之步驟,由於可如所述以獨立之製程調製奈米膠體粒子,因此可更自由地控制載持之奈米膠體粒子的組成。例如對習知之使用還原劑使高分子表面析出金屬奈米膠體粒子的方法而言,要使固溶體(solid solution)及混晶(mixed crystal)之奈米膠體粒子載持於纖維素奈米纖維甚是困難,但本發明亦可達成。
並且,由於如上述為獨立之製程,故可簡便且大量地合成奈米膠體粒子,進而可在常溫、常壓下以環境負荷少之製程大量地製造奈米膠體粒子載持體。
以下,再對本發明之實施形態加以說明,惟本發明並不限定於此。
本發明之奈米膠體粒子載持體,如上所述,係使奈米膠體粒子受載於多醣類系高分子者,並可以包含下述
步驟之製造方法製得:將已和界面活性劑溶液混合而溶解或潤脹的多醣類系高分子,與使奈米膠體粒子分散於分散介質中而成的奈米膠體液混合。
本發明中所使用之奈米膠體粒子,為平均粒徑1至100nm的粒子,可舉例如金、銀、銅及鉑、鈀、釕、銠、鋨、銥等鉑族等之金屬粒子。而且,亦可為含此類金屬之1種或2種以上的合金之粒子。奈米膠體液即為使此類奈米膠體粒子分散於分散介質中而成的液體。
分散介質可舉例如水、異丙醇(IPA)、N-甲基吡咯啶酮(NMP)、甲醇、乙醇、甲苯等,但並不限定於此。但,由容易分散此點而言以水較佳。
奈米膠體液可藉由將上述奈米膠體粒子以一般已知之方法分散於上述分散介質中來製造,亦可適當利用市售之商品。其製造方法並無特別之限定,例如可藉由令金奈米膠體為四氯金(Ⅲ)酸(H[AuCl4])、令銀奈米膠體為硝酸銀並各在液體中以還原劑予以還原的方法來製得。還原劑方面,可使用氫化硼鈉及檸檬酸鈉、抗壞血酸鈉等。
其次,本發明中作為載持體使用之多醣類系高分子,係由單醣分子100單元以上鍵結而成之高分子。多醣類系高分子形成纖維狀且比表面積大,因此在此類多醣類系高分子的表面載持奈米膠體粒子,可使奈米膠體粒子高濃度化。
多醣類系高分子的分散介質方面,只要是水或IPA、NMP、甲醇、乙醇、甲苯等只要可經有機溶劑溶解或
潤脹者即無特別限定,但就基材為親水性而容易分散等而言,以水較佳。
多醣類系高分子之例,可舉如:纖維素、乙醯基纖維素、羧甲基纖維素、幾丁質、幾丁聚醣、直鏈澱粉、糊精、肝醣、瓊脂醣、鹿角菜膠等,亦可使用2種以上之混合物。
其中,天然纖維素、幾丁質、幾丁聚醣,在親水性、分散介質可使用水之點上較佳。而且,在價廉且調製容易之點上亦佳。
多醣類系高分子以微粉末為佳,平均纖維口徑以20至1000nm為佳,20至200nm更佳。使用此類微細粒子,可使比表面積更大,因此可載持大量的奈米膠體粒子。
其次本發明中所使用之界面活性劑並無特別之限定,可使用任意陰離子系、陽離子系、非離子系。陰離子系界面活性劑之例,可舉如:單烷基硫酸鹽、烷基聚環氧乙烷硫酸鹽、烷基苯磺酸鹽、單烷基磷酸鹽、羧酸鹽等。陽離子系界面活性劑之例,可舉如:烷基三甲基銨鹽、二烷基二甲基銨鹽、烷基苯甲基二甲基銨鹽等4級銨鹽。非離子系界面活性劑之例,可舉如:聚環氧乙烷烷基醚、脂酸山梨醇酐酯、烷基聚醣苷、脂酸二乙醇醯胺、烷基單甘油基醚等非離子系活性劑等。由於奈米膠體粒子之吸附效率高之點,以上述4級銨鹽或羧酸鹽較佳。只要不違背本發明目的之範圍,亦可併用2種以上界面活性劑。
界面活性劑宜預先溶於溶劑中做成界面活性劑
溶液,再與上述多醣類系高分子混合。但是,亦可採取預先將多醣類系高分子在溶劑中溶解或潤脹之後再於其中加入界面活性劑的方法,或可採取將多醣類系高分子及界面活性劑同時加入溶劑中混合而使多醣類系高分子溶解或潤脹之方法。
其中可使用的溶劑之例,可舉如:水或IPA、NMP、甲醇、乙醇、甲苯等,由界面活性劑溶解容易而言,以水較佳。
界面活性劑的用量雖與其種類亦有關,但宜以換算為固體成分計相對於奈米膠體粒子100質量份為1至10質量份,且1至5質量份更佳。只要在1質量份以上,就易於進行本發明目標之奈米膠體粒子的高濃度化。另一方面認為,只要在10質量份以下,則界面活性劑基本上只使用在使奈米膠體粒子吸附在多醣類系高分子上,且不吸附在上述多醣類系高分子上而游離在溶液中的量成可忽略之程度,奈米膠體粒子之表面幾乎未經界面活性劑包覆而形成露出狀態。
令多醣類系高分子溶解在上述界面活性劑溶液中、或令其以界面活性劑溶液潤脹,再將該含多醣類系高分子及界面活性劑的溶液,與使上述奈米膠體粒子分散於分散介質中而成的奈米膠體液混合,藉此即可獲得使奈米膠體粒子受載於多醣類系高分子的載持體。亦可獲得令奈米膠體粒子之載持量在一般用途上相對於多醣類系高分子100質量份為1質量份以上、視需要為15質量份以上的高
濃度載持體。
形成載持體的具體操作及條件並無特別限定,可在上述之混合後,譬如在室溫下混合來立即形成奈米膠體粒子載持體。所得之載持體再經過離心分離機,將以上清液分離的分散介質去除即可高濃度化,該已高濃度化之載持體經加水並輕輕振盪,即可輕易地再分散。
以下所示為本發明之實施例,惟本發明並不限定於以下的實施例。再者,以下之配合比例等,除非特別限定係質量基準(質量份、質量%)。
[實施例1]
(1)奈米膠體粒子分散液之調製
先在1L玻璃燒杯中加入5℃之蒸餾水868.5g,在將該燒杯冷卻保持液溫為5℃之下,加入40mM氫化硼鈉水溶液22.5mL,並使用磁攪拌粒以800至900rpm攪拌15分鐘。其次,再以將10mM之硝酸銀水溶液,以16至20秒/1滴的滴入速度合計滴入9mL可製得銀奈米膠體粒子分散液。滴入終了後並再靜置1日。
(2)纖維素-水分散液之調製
在於纖維素奈米纖維-水分散液(Sugino機械公司製造,BiNFi-s,工業用短纖維,2wt%)5.0g中加入蒸餾水95.0g並以玻璃棒預備分散之後,再以超音波處理進行本分散。在該所得之分散液至回復為常溫為止加以靜置之後,再以於以1wt%氯化硬脂基三甲基銨(STMAC)水溶液以合計量
10μL滴入之後,於室溫下,使用磁攪拌粒以150至350rpm攪拌1小時,即可製得纖維素-水分散液(分散液1)。
(3)奈米膠體粒子載持體分散液之調製
之後將上述(1)中獲得之銀奈米膠體粒子分散液92.7g移至玻璃燒杯中,並使用磁攪拌粒以350rpm預攪拌,然後加入上述(2)中獲得之纖維素-水分散液22mL,攪拌10分鐘即可製得奈米膠體粒子載持體分散液。然後由燒杯取出攪拌粒,並於室溫下靜置1日。同時為確定長期穩定性而在室溫下靜置1000小時。
然後由上述靜置後之奈米膠體粒子載持體分散液去除上清液,再經過轉速2000rpm離心分離3分鐘,並以傾斜法將液相去除,即可製得奈米膠體粒子載持體水分散體之濃縮物。
[實施例2、3、比較例3]
先如上述實施例1同樣操作製得銀奈米膠體粒子分散液,並在滴入終了之後再靜置1日。
除以1wt%氯化硬脂基三甲基銨(STMAC)水溶液以合計量50μL滴入以外,在與上述實施例1相同之方法之下,可得纖維素-水分散液2。同時,除以STMAC水溶液以合計量100μL滴入以外,在與上述實施例1相同之方法之下,可得纖維素-水分散液3。同時,除不使用STMAC水溶液以外,在與上述實施例1相同之方法之下,可得纖維素-水分散液4。
之後於所得之多醣類系高分子分散液中,除各使
用如表2所示之物以外與實施例1同樣地操作,可各調製奈米膠體粒子載持體分散液,在室溫下靜置1日及1000小時之後,如實施例1同樣操作去除液相即可得奈米膠體粒子載持體水分散體的濃縮物。
[實施例4]
(1)奈米膠體粒子分散液之調製
先在1L玻璃燒杯中加入5℃之蒸餾水787.5g,在將該燒杯冷卻保持液溫為5℃之下,加入40mM氫化硼鈉水溶液22.5mL,並使用磁攪拌粒以800至900rpm攪拌15分鐘。其次,再將1mM之四氯金(Ⅲ)酸(H[AuCl4])水溶液,以16至20秒/1滴的滴入速度合計滴入90mL可製得金奈米膠體粒子分散液。滴入終了後並再靜置1日。
(2)纖維素-水分散液之調製
除以1wt%氯化硬脂基三甲基銨(STMAC)水溶液以合計量50μL滴入以外,在與上述實施例1相同之方法之下,可得纖維素-水分散液2。
(3)奈米膠體粒子載持體分散液之調製
除以上述(1)中獲得之金奈米膠體粒子分散液50.8g及上述(2)中獲得之纖維素-水分散液(分散液2)以外與上述實施例1同樣地操作可調製奈米膠體粒子載持體分散液,並在室溫下靜置1日及1000小時之後,如實施例1同樣操作去除液相即可得奈米膠體粒子載持體水分散體的濃縮物。
[實施例5]
(1)奈米膠體粒子分散液之調製
先在1L玻璃燒杯中加入5℃之蒸餾水859.5g,在將該燒杯冷卻保持液溫為5℃之下,加入40mM氫化硼鈉水溶液22.5mL,並使用磁攪拌粒以800至900rpm攪拌15分鐘。其次,再將5mM之氯化鈀水溶液,以16至20秒/1滴的滴入速度合計滴入18mL可製得鈀奈米膠體粒子分散液。滴入終了後並再靜置1日。
(2)纖維素-水分散液之調製
除以1wt%氯化硬脂基三甲基銨(STMAC)水溶液以合計量100μL滴入以外,在與上述實施例1相同之方法之下,可得纖維素-水分散液3。
(3)奈米膠體粒子載持體分散液之調製
除以上述(1)中獲得之鈀奈米膠體粒子分散液94.0g及上述(2)中獲得之纖維素-水分散液(分散液3)以外與上述實施例1同樣地操作可調製奈米膠體粒子載持體分散液,並在室溫下靜置1日及1000小時之後,如實施例1同樣操作去除液相即可得奈米膠體粒子載持體水分散體的濃縮物。
[比較例1]
先在1L玻璃燒杯中加入5℃之蒸餾水868.5g,在將該燒杯冷卻保持液溫為5℃之下,加入40mM氫化硼鈉水溶液22.5mL,並使用磁攪拌粒以800至900rpm攪拌15分鐘。其次,再將10mM之硝酸銀水溶液,以16至20秒/1滴的滴入速度合計滴入9mL可製得奈米膠體粒子分散液,並於滴入終了後再靜置1日。靜置後該奈米膠體粒子分散液雖然穩定,但銀濃度為約10ppm。
[比較例2]
先在1L玻璃燒杯中加入5℃之蒸餾水868.5g,在將該燒杯冷卻保持液溫為5℃之下,加入40mM氫化硼鈉水溶液225mL,並使用磁攪拌粒以800至900rpm攪拌15分鐘。其次,再將10mM之硝酸銀水溶液,以16至20秒/1滴的滴入速度合計滴入90mL。剛開始滴入時雖然銀奈米膠體粒子在分散液中穩定存在,若持續滴入時,奈米膠體粒子即會粗大化,即刻成為懸浮液。
之後對上述實施例及比較例中所得之奈米膠體粒子載持體及比較之試樣,如下換算求出濃度,同時進行光譜解析測定膠體粒徑。其結果如表2所示。
<換算濃度>
實施例3之奈米膠體粒子載持體的容積,係以定量量筒等器具測量,在假定在相同離心條件下每單位重量之纖維素奈米纖維壓縮率並不變化之下,以實施例3之體積為基準,求出對應纖維素奈米纖維投入重量之濃度。
<光譜解析>
係使用紫外線-可見光分光光度計(島津製作所公司製造,UV-2600,使用積分球ISR-2600),以以下之條件測定吸光度光譜。同時,以膠體粒徑與吸收波長成立線性關係為前提,試樣間差異的解析,係以標定吸光度波強度比較調平之光譜形狀進行比較。本解析方法係使用在具有接近高斯分布形狀之吸光度光譜中,具體地,係以吸光度波波長λp、半值全寬(FWHM)或者半值半寬(HWHM)的數值資料值求出,以解析原料奈米膠體粒子分散液與調平之吸光度波、半值全寬或者半值半寬之差異。解析之前,先選出數種參考試樣進行稀釋操作,確定在吸光度0.3至3的範圍下標定可使波在基本上一致。
比色管:polystyrol/Polystyrene REF 67.754 10×10×45mm SARSTEDT AG & Co.製造
波長範圍:350至800mm
掃描速度:中速
自動取樣間隔:ON
光柵寬:1.0mm
S/R轉換:標準
累計時間:1.0秒
由表2所示之結果可知,像是比較例1、2未載持於高分子之情況下並無法獲得高濃度且穩定之奈米膠體粒子分散液,又如比較例3未使用界面活性劑之情況下,則無法形成載持體、抑或是可形成載持體卻難以高濃度化。
因此本發明之奈米膠體粒子載持體可利用於催化劑等。
Claims (8)
- 一種奈米膠體粒子載持體之製造方法,其特徵在於具有以下步驟:獲得已在界面活性劑溶液中溶解或潤脹的多醣類系高分子之步驟;及將該已溶解或潤脹的多醣類系高分子與使奈米膠體粒子分散於分散介質中而成的奈米膠體液混合之步驟;且,獲得已使前述奈米膠體粒子受載於前述多醣類系高分子之載持體。
- 如請求項1之奈米膠體粒子載持體之製造方法,其中前述奈米膠體粒子係選自金、銀、鉑、鈀、釕、銠、鐵、銥、及銅中之1種或2種以上金屬及/或前述1種或2種以上金屬之合金粒子。
- 如請求項1或2之奈米膠體粒子載持體之製造方法,其中前述界面活性劑係選自4級銨鹽及羧酸鹽中之1種或2種以上。
- 如請求項1或2之奈米膠體粒子載持體之製造方法,其中前述界面活性劑的用量係相對於前述奈米膠體粒子100質量份在1至10質量份之範圍內。
- 如請求項1或2之奈米膠體粒子載持體之製造方法,其中前述多醣類系高分子係選自纖維素、幾丁質、及幾丁聚醣中之1種或2種以上。
- 如請求項5之奈米膠體粒子載持體之製造方法,其中前述多醣類系高分子具有在20至1000nm之範圍內的平均纖維口徑。
- 一種奈米膠體粒子載持體,其係以如請求項1或2之製造方法製造,且前述奈米膠體粒子受載於前述多醣類系高分子。
- 如請求項7之奈米膠體粒子載持體,其中前述奈米膠體粒子的載持量係相對於前述多醣類系高分子100質量份在1至15質量份之範圍內。
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