TW201714945A - 一種含奈米銀粒子之高分子乳膠顆粒組成物 - Google Patents
一種含奈米銀粒子之高分子乳膠顆粒組成物 Download PDFInfo
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Abstract
本發明係有關於一種含奈米銀粒子之高分子乳膠顆粒組成物,係包括高分子乳膠顆粒及分散塗覆於高分子乳膠顆粒表面之奈米銀粒子,具有抗菌功能。
Description
本發明係有關於一種含奈米銀粒子之高分子乳膠(polymer latex)顆粒組成物,尤其係指藉由特定條件製備得到的高分子乳膠顆粒組成物,其表面均勻且牢固地塗覆有一層奈米銀。藉此,本發明之乳膠顆粒具有良好的抗菌活性,不僅可以取代化妝品中防腐劑之添加,亦可解決微小的奈米銀穿過皮膚進入人體細胞之問題,並且可使該銀粒子達到奈米級分散,增進其抗菌功效。
近年來,化妝保養品已成為愛美人士每天不可或缺的生活必需品之一,業者為延長化妝保養品的使用期限,必需在化妝保養品中添加化學抗菌劑或防腐劑以提高保存年限。最常添加在化妝保養品的防腐劑例如對羥基苯甲酸酯(Paraben)、苯氧乙醇(Phenoxyethanol)、安息香酸(苯甲酸,Benzoic acid)、山梨酸(Sorbic acid)等有機化學物,且具有良好的抗菌效果,但經過長期使用而累積超過一定劑量時,仍然有造成肌膚過敏和毒性的疑慮。
除了化學合成的有機抗菌劑或防腐劑之外,目前最廣為人知的無機類抗菌劑為奈米銀粒子,其具有極佳的除臭及殺菌效果,且可耐高溫。除此之外,奈米銀粒子亦可避免使用二氧化鈦光觸媒抗菌時需接觸紫外光之缺失。據此,目前已有多項發明係藉由將奈米粒子結合到不同的基材上,使基材具備附加的抗菌功能。
舉例而言,中華民國專利公告第I455778號「含基材表面結合金屬奈米粒子的製造方法」,即揭示一種基材表面結合金屬奈米粒子的製造方法,包含下列步驟:將一預定材質的基材浸入一含有預定濃度之金屬離子的鹽類溶液,使該鹽類溶液中的金屬離子附著到該基材上,再將該基材取出,並將一含有一預定還原劑的反應液添加至該基材上,及提供一能量作用於該基材,使附著在該基材上的金屬離子被還原為金屬奈米粒子,最後,以一預定方法使該基材乾燥,製得結合金屬奈米粒子的基材製品,藉此所製出的製品不易殘留對人體有害的化學成分,而不需再以複雜的分離程序處理;中華民國專利公告第I495481 號「聚矽氧複合粒子及其製造方法、以及化妝料」,即揭示一種可添加於體香劑化妝料的聚矽氧複合粒子,其特徵在於100質量份的聚矽氧彈性體球狀粒子塗覆有0.5~25質量份的聚矽氧樹脂,其中該聚矽氧彈性體球狀粒子的平均粒徑為0.1~100 μm,以及該聚矽氧樹脂係具有有機矽倍半氧烷單位作為主成分,且含有平均粒徑為100 nm以下之無機微粒子;以及中華民國專利公告第I455718號「用於抗菌之奈米銀粒子/黏土複合物及其製造方法」,揭示一種可應用於生物、醫藥、化學、化工、材料等領域(例如抗菌及燒燙傷醫療)的奈米銀粒子/黏土複合物,其係為一粉體,包括金屬粒子及片狀無機黏土,其中該片狀無機黏土之長寬比為100~1000,並作為該金屬粒子之載體,以使該金屬粒子達到奈米級之分散,該抗菌之奈米金屬粒子/無機黏土複合物之大小為5~100nm;其中該片狀無機黏土為皂土或奈米矽片,且該片狀無機黏土為皂土時,奈米金屬粒子與黏土重量比為1:100~1:13.83或1:6.944~100:1;該片狀無機黏土為奈米矽片時,奈米金屬粒子與黏土重量比為1:13.43~100:1;該金屬係選自銀所組成之群組。
根據文獻搜尋結果可知,將奈米銀粒子結合到不同基材上之運用雖然很多,但如何達到使奈米銀粒子均勻結合於基材上,仍須視不同的製備方式而定。爰此,如何研發製作出更佳的含奈米銀粒子聚苯乙烯乳膠顆粒作為抗菌劑,乃為相關領域發明人亟需突破之方向。
本發明主要目的為提供一種藉由特定條件製備得到的乳膠顆粒,其表面係均勻且牢固的黏著、分布有奈米銀。藉此,本發明製得之乳膠顆粒具有良好的抗菌活性,可用以當作防腐劑添加於化妝品。
為了達到上述實施目的,本發明一種含奈米銀粒子之高分子乳膠顆粒組成物,其係包括高分子乳膠顆粒及分散塗覆於高分子乳膠顆粒表面之奈米銀粒子,其中高分子乳膠顆粒之直徑為大於50 nm,奈米銀粒子之直徑為1~500 nm,且高分子乳膠顆粒與奈米銀粒子重量百分比為1000:1至1:1。
於本發明之一實施例中,高分子乳膠顆粒可例如為聚苯乙烯(polystyrene)乳膠顆粒、聚甲基丙烯酸甲酯(polymethylmethacrylate)乳膠顆粒、苯乙烯與甲基丙烯酸甲酯共聚物之乳膠顆粒、苯乙烯與甲基丙烯酸丁酯共聚物之乳膠顆粒、甲基丙烯酸甲酯與甲基丙烯酸丁酯共聚物之乳膠顆粒。
於本發明之一實施例中,含奈米銀粒子之高分子乳膠顆粒組成物係具有球狀結構或橢圓形結構;若高分子乳膠顆粒為聚苯乙烯乳膠顆粒,則組成物之製備方法可例如為:將含聚苯乙烯乳膠顆粒懸浮液與硝酸銀(AgNO3
)水溶液均勻混合以形成一混合溶液,並於溫度90℃作用1小時;以及將混合溶液降溫至80℃,再加入檸檬酸鈉水溶液於混合溶液中作用0.5小時,以得到表面塗覆有奈米銀粒子之聚苯乙烯乳膠顆粒;其中含聚苯乙烯乳膠顆粒懸浮液係由3.8 wt%聚苯乙烯乳膠顆粒及剩餘重量百分比的水所組成。
於本發明之一實施例中,含奈米銀粒子之高分子乳膠顆粒組成物可用於抑制革蘭氏陽性菌、革蘭氏陰性菌及真菌之生長;藉此,含奈米銀粒子之高分子乳膠顆粒組成物可用於化妝材料組成物及醫藥組成物,作為抑菌劑或防腐劑。
本發明之目的及其結構功能上的優點,將依據以下圖面所示之結構,配合具體實施例予以說明,俾使審查委員能對本發明有更深入且具體之瞭解。
本發明一種含奈米銀粒子之高分子乳膠顆粒組成物,其係包括高分子乳膠顆粒及分散塗覆於高分子乳膠顆粒表面之奈米銀粒子,其中高分子乳膠顆粒之直徑為大於50 nm,奈米銀粒子之直徑為1~500 nm,且高分子乳膠顆粒與奈米銀粒子重量百分比為1000:1至1:1。
上述含奈米銀粒子之高分子乳膠顆粒組成物為球狀結構或橢圓形結構;高分子乳膠顆粒為聚苯乙烯(polystyrene)乳膠顆粒、聚甲基丙烯酸甲酯(polymethylmethacrylate)乳膠顆粒或聚甲基丙烯酸丁酯(poly-n-butyl methacrylate)乳膠顆粒、苯乙烯與甲基丙烯酸甲酯共聚物之乳膠顆粒、苯乙烯與甲基丙烯酸丁酯共聚物之乳膠顆粒、甲基丙烯酸甲酯與甲基丙烯酸丁酯共聚物之乳膠顆粒…等;若高分子乳膠顆粒為聚苯乙烯乳膠顆粒,則組成物可例如以下述方法製備而得:將含聚苯乙烯乳膠顆粒懸浮液(可例如由3.8 wt%聚苯乙烯乳膠顆粒及剩餘重量百分比的水所組成)與硝酸銀(AgNO3
)水溶液均勻混合以形成一混合溶液,並於溫度90℃作用1小時;以及將混合溶液降溫至80℃,再加入檸檬酸鈉水溶液於混合溶液中作用0.5小時,以得到表面塗覆有奈米銀粒子之聚苯乙烯乳膠顆粒,係具有抑制細菌(如革蘭氏陽性菌與革蘭氏陰性菌)及真菌生長的能力,因此可添加於化妝材料組成物及醫藥組成物。
在此值得注意的是,本案發明人於同日申請有另一申請案『一種含奈米銀粒子高分子乳膠顆粒之製備方法』,在此不詳細說明,特將其所有內容包含於此作為參考。
此外,藉由下述具體實施例,可進一步證明本發明可實際應用之範圍,但不意欲以任何形式限制本發明之範圍。
實施例一:製備聚苯乙烯乳膠顆粒
聚苯乙烯乳膠顆粒合成步驟為(1)先將1.9 g聚醚醯亞胺(polyethylenimine, PEI)、30 g甲醇及1 g去離子水混合均勻,再置入反應槽(低速攪拌);(2)取0.3 g起始劑AIBN (Azobisisobutyronitrile)溶於15 g甲醇以配製成AIBN甲醇溶液;(3)秤取10 g苯乙烯(styrene)加入反應槽中與步驟(1)溶液一同攪拌,並加溫至70℃約15分鐘;(4)將步驟(2)均勻溶解的AIBN甲醇溶液快速倒入反應槽中,維持溫度70℃作用8小時,以得到含聚苯乙烯乳膠顆粒的乳狀溶液(PS latex emulsion);以及(5)以離心方式純化聚苯乙烯乳膠顆粒,其平均粒徑大於100 nm (約為100~2000 nm)。
實施例二
請參閱表一,本實施例含奈米銀粒子聚苯乙烯乳膠顆粒合成步驟為(1)取實施例一製得之1 g聚苯乙烯乳膠顆粒(PS乳膠顆粒)與25 克去離子水混合均勻,以形成聚苯乙烯乳膠顆粒懸浮液;(2)將混合均勻的聚苯乙烯乳膠顆粒懸浮液置入反應槽,在不接冷凝管及通氮氣下,將溫度升至90℃並持續攪拌;(3) 將0.1 g硝酸銀(AgNO3
)與5 g去離子水混合以製得硝酸銀水溶液;(4) 於溫度90℃,將硝酸銀水溶液加入反應槽中(此時反應槽溶液會逐漸變成鵝黃色溶液),以形成一混合溶液,並作用1小時;(5)將混合溶液降溫至85℃之後,再加入檸檬酸鈉水溶液(1.94克檸檬酸鈉溶於10克去離子水),繼續反應10分鐘使溶液慢慢變成黑色狀態,即得到表面塗覆有奈米銀粒子之聚苯乙烯乳膠顆粒,其中聚苯乙烯乳膠顆粒之平均粒徑為390~990 nm,奈米銀粒子之平均粒徑為5~100 nm。利用穿透式電子顯微鏡(Transmission Electron Microscopy;TEM)觀察的結果請參閱第一圖,因為加入檸檬酸鈉後,只反應10分鐘,反應的時間太短,使得所合成的銀顆粒數量太少,且銀顆粒來不及吸附在PS乳膠顆粒上,所以無法佈滿整個PS乳膠顆粒的表面,有些PS乳膠顆粒的表面呈現裸露的現象。
表一
實施例三
請參閱表二,本實施例含奈米銀粒子聚苯乙烯乳膠顆粒合成步驟為(1)取實施例一製得之1 g聚苯乙烯乳膠顆粒(PS乳膠顆粒)與25 克去離子水混合均勻,以形成聚苯乙烯乳膠顆粒懸浮液;(2)將混合均勻的聚苯乙烯乳膠顆粒懸浮液置入反應槽,在不接冷凝管及通氮氣下,將溫度升至90℃~95℃並持續攪拌;(3) 將0.1 g硝酸銀(AgNO3
)與5 g去離子水混合以製得硝酸銀水溶液;(4) 於溫度90℃~95℃,將硝酸銀水溶液加入反應槽中(此時反應槽溶液會逐漸變成鵝黃色溶液),以形成一混合溶液,並作用1小時;(5)將混合溶液降溫至80℃之後,再加入檸檬酸鈉水溶液(1.94克檸檬酸鈉溶於10克去離子水),繼續反應20分鐘使溶液慢慢變成黑色狀態,即得到表面塗覆有奈米銀粒子之聚苯乙烯乳膠顆粒,其中聚苯乙烯乳膠顆粒之平均粒徑為390~990 nm,奈米銀粒子之平均粒徑為5~100 nm。利用穿透式電子顯微鏡(TEM)觀察的結果請參閱第二圖,因為加入檸檬酸鈉後,只反應20分鐘,反應的時間太短,使得所合成的銀顆粒數量太少;另一方面,因反應溫度太高,所以銀顆粒迅速形成,使得銀顆粒來不及吸附在PS乳膠顆粒上,所以無法佈滿整個PS乳膠顆粒的表面,有些PS乳膠顆粒的表面呈現裸露的現象。進一步經過測試,若將步驟(5)加入檸檬酸鈉後的反應時間拉長為30分鐘,亦得到類似的結果(圖中未顯示)。因此,有必要再測試不同的條件。
表二
實施例四
請參閱表三,本實施例含奈米銀粒子聚苯乙烯乳膠顆粒合成步驟為(1)取實施例一製得之1 g聚苯乙烯乳膠顆粒(PS乳膠顆粒)與25 克去離子水混合均勻,以形成聚苯乙烯乳膠顆粒懸浮液;(2)將混合均勻的聚苯乙烯乳膠顆粒懸浮液置入反應槽,在不接冷凝管及通氮氣下,將溫度升至90℃並持續攪拌;(3) 將0.3 g硝酸銀(AgNO3
)與15 g去離子水混合以製得硝酸銀水溶液;(4) 於溫度90℃,將硝酸銀水溶液加入反應槽中(此時反應槽溶液會逐漸變成鵝黃色溶液),以形成一混合溶液,並作用1.5小時;(5)將混合溶液降溫至80℃之後,再加入檸檬酸鈉水溶液(5.82克檸檬酸鈉溶於30克去離子水),繼續反應30分鐘使溶液慢慢變成黑色狀態,即得到表面塗覆有奈米銀粒子之聚苯乙烯乳膠顆粒。利用穿透式電子顯微鏡(TEM)觀察的結果請參閱第三圖,由於硝酸銀和檸檬酸鈉的量加入過多,且加入硝酸銀後反應1.5小時,反應的時間較久,因此反應所產生的銀過多,以至於許多銀都聚集在一起。
表三
實施例五
請參閱表四,本實施例含奈米銀粒子聚苯乙烯乳膠顆粒合成步驟為(1)取實施例一製得之1 g聚苯乙烯乳膠顆粒(PS乳膠顆粒)與25 克去離子水混合均勻,以形成聚苯乙烯乳膠顆粒懸浮液;(2)將混合均勻的聚苯乙烯乳膠顆粒懸浮液置入反應槽,在不接冷凝管及通氮氣下,將溫度升至90℃並持續攪拌;(3) 將0.3 g硝酸銀(AgNO3
)與15 g去離子水混合以製得硝酸銀水溶液;(4) 於溫度90℃,將硝酸銀水溶液加入反應槽中(此時反應槽溶液會逐漸變成鵝黃色溶液),以形成一混合溶液,並作用1小時;(5)將混合溶液降溫至80℃之後,再加入檸檬酸鈉水溶液(5.82克檸檬酸鈉溶於30克去離子水),繼續反應30分鐘使溶液慢慢變成黑色狀態,即得到表面塗覆有奈米銀粒子之聚苯乙烯乳膠顆粒。利用穿透式電子顯微鏡(TEM)觀察的結果請參閱第四圖,由於硝酸銀和檸檬酸鈉的量加入過多,因此反應所產生的銀過多,以至於許多銀都聚集在一起。
表四
實施例六
請參閱表五,本實施例含奈米銀粒子聚苯乙烯乳膠顆粒合成步驟為(1)取實施例一製得之1 g聚苯乙烯乳膠顆粒(PS乳膠顆粒)與25 克去離子水混合均勻,以形成聚苯乙烯乳膠顆粒懸浮液;(2)將混合均勻的聚苯乙烯乳膠顆粒懸浮液置入反應槽,在不接冷凝管及通氮氣下,將溫度升至90℃並持續攪拌;(3) 將0.1 g硝酸銀(AgNO3
)與5 g去離子水混合以製得硝酸銀水溶液;(4) 於溫度95℃,將硝酸銀水溶液加入反應槽中(此時反應槽溶液會逐漸變成鵝黃色溶液),以形成一混合溶液,並作用1小時;(5)將混合溶液降溫至85℃之後,再加入檸檬酸鈉水溶液(1.94克檸檬酸鈉溶於10克去離子水),繼續反應30分鐘使溶液慢慢變成黑色狀態,即得到表面塗覆有奈米銀粒子之聚苯乙烯乳膠顆粒,其中聚苯乙烯乳膠顆粒之平均粒徑為390~990 nm,奈米銀粒子之平均粒徑為5~100 nm。利用穿透式電子顯微鏡(TEM)觀察的結果請參閱第五圖,因為進行合成時,加入適當含量的硝酸銀,且反應的時間長短適當,所以形成適當數量的銀,而且因為反應時間較久,所以銀顆粒可以有足夠的時間吸附在PS乳膠顆粒上,使得所產生的PS乳膠顆粒的表面上均勻的佈滿銀顆粒。
表五
實施例七:最低抑菌濃度(MIC)試驗
取實施例六製得之含奈米銀粒子聚苯乙烯乳膠顆粒進行抑菌測試,以得知含奈米銀粒子聚苯乙烯乳膠顆粒的最低抑菌濃度(minimum inhibitory concentration,簡稱MIC)。所謂「最低抑菌濃度」即為測定能夠抑制90%培養基內的定量試驗菌株生長的最低樣品濃度值,MIC值越低代表樣品抑菌效果越佳。本實施例取革蘭氏陽性菌-金黃色葡萄球菌(Staphylococcus aureus
)與革蘭氏陰性菌-大腸桿菌(Escherichia coli
)進行實驗。於無菌養菌管中分別加入不同濃度(0~0.020%)之抗菌樣品(含奈米銀粒子聚苯乙烯乳膠顆粒),再加入1 c.c.之Nutrient broth或TSB培養液和已知菌種之菌液混合均勻;然後,將其置於37℃的培養箱中震盪培養一天。取培養後較為澄清養菌管之懸浮液,用連續十倍稀釋法,取適量滴於洋菜膠平板培養基上塗佈均勻,依其適當生長條件培養後,觀察並計算菌落產生之數量來決定MIC值。
結果請參閱第六圖,實施例六製得之含奈米銀粒子聚苯乙烯乳膠顆粒確實具有抑菌作用,對於金黃色葡萄球菌與大腸桿菌的最低抑菌濃度分別為0.0075%和0.011%。
由於本發明製得之聚苯乙烯乳膠顆粒具有銀粒子均勻地塗覆於聚苯乙烯乳膠顆粒表面,因此具有良好的抑菌效果,且由於該等銀粒子係牢固地附著於聚苯乙烯乳膠顆粒表面,不會任意脫離。因此,將含奈米銀粒子聚苯乙烯乳膠顆粒添加至化妝品中,不僅可以取代傳統防腐劑之添加,亦可解決微小的奈米銀穿過皮膚進入人體細胞之問題,並且可使該銀粒子達到奈米級分散,增進其抗菌功效。
綜上所述,本發明之含奈米銀粒子之高分子乳膠顆粒組成物,的確能藉由上述所揭露之實施例,達到所預期之使用功效,且本發明亦未曾公開於申請前,誠已完全符合專利法之規定與要求。爰依法提出發明專利之申請,懇請惠予審查,並賜准專利,則實感德便。
惟,上述所揭之圖示及說明,僅為本發明之較佳實施例,非為限定本發明之保護範圍;大凡熟悉該項技藝之人士,其所依本發明之特徵範疇,所作之其它等效變化或修飾,皆應視為不脫離本發明之設計範疇。
無
第一圖:本發明其一具體實施例所製得含奈米銀粒子聚苯乙烯乳膠顆粒之外觀型態圖。
第二圖:本發明其二具體實施例所製得含奈米銀粒子聚苯乙烯乳膠顆粒之外觀型態圖。
第三圖:本發明其三具體實施例所製得含奈米銀粒子聚苯乙烯乳膠顆粒之外觀型態圖。
第四圖:本發明其四具體實施例所製得含奈米銀粒子聚苯乙烯乳膠顆粒之外觀型態圖。
第五圖:本發明其五具體實施例所製得含奈米銀粒子聚苯乙烯乳膠顆粒之外觀型態圖。
第六圖:本發明含奈米銀粒子聚苯乙烯乳膠顆粒之抑菌濃度分析圖。
Claims (7)
- 一種含奈米銀粒子之高分子乳膠顆粒組成物,係包括高分子乳膠顆粒及分散塗覆於該高分子乳膠顆粒表面之奈米銀粒子,其中該高分子乳膠顆粒之直徑為大於50 nm,該奈米銀粒子之直徑為1~500 nm,且該高分子乳膠顆粒與該奈米銀粒子重量百分比為1000:1至1:1。
- 如申請專利範圍第1項所述之含奈米銀粒子之高分子乳膠顆粒組成物,其中該組成物具有球狀結構或橢圓形結構。
- 如申請專利範圍第1項所述之含奈米銀粒子之高分子乳膠顆粒組成物,其中該組成物係用於抑制革蘭氏陽性菌、革蘭氏陰性菌及真菌之生長。
- 如申請專利範圍第1項所述之含奈米銀粒子之高分子乳膠顆粒組成物,其中該高分子乳膠顆粒為聚苯乙烯(polystyrene)乳膠顆粒、聚甲基丙烯酸甲酯(polymethylmethacrylate)乳膠顆粒、聚甲基丙烯酸丁酯(poly-n-butyl methacrylate)乳膠顆粒、苯乙烯與甲基丙烯酸甲酯共聚物之乳膠顆粒、苯乙烯與甲基丙烯酸丁酯共聚物之乳膠顆粒,或甲基丙烯酸甲酯與甲基丙烯酸丁酯共聚物之乳膠顆粒。
- 如申請專利範圍第4項所述之含奈米銀粒子之高分子乳膠顆粒組成物,其中該高分子乳膠顆粒為聚苯乙烯乳膠顆粒,且該組成物之製備方法包括:將含聚苯乙烯乳膠顆粒懸浮液與硝酸銀(AgNO3 )水溶液均勻混合以形成一混合溶液,並於溫度90℃作用1小時;以及將該混合溶液降溫至80℃,再加入檸檬酸鈉水溶液於該混合溶液中作用0.5小時,以得到表面塗覆有奈米銀粒子之聚苯乙烯乳膠顆粒。
- 如申請專利範圍第5項所述之含奈米銀粒子之高分子乳膠顆粒組成物,其中該含聚苯乙烯乳膠顆粒懸浮液係由3.8 wt%聚苯乙烯乳膠顆粒及剩餘重量百分比的水所組成。
- 如申請專利範圍第1項所述之含奈米銀粒子之高分子乳膠顆粒組成物,係用於化妝材料組成物及醫藥組成物。
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