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研究生: 黃威廸
Wei-di Huang
論文名稱: 製備具高表面電位之奈米球
Fabricate nanosphere with high-level electric potential
指導教授: 陳暉
Hui Chen
口試委員:
學位類別: 碩士
Master
系所名稱: 工學院 - 化學工程與材料工程學系
Department of Chemical & Materials Engineering
畢業學年度: 100
語文別: 中文
論文頁數: 163
中文關鍵詞: 表面電位穩定乳液奈米高分子球無乳化劑乳化聚合微乳化聚合
外文關鍵詞: Zeta potential, microemulsion, emulsion stabilization, nanosphere, soap-free emulsion
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  • 本研究乃使用無乳化劑乳化聚合法與微乳化聚合法,以苯乙烯(St)為主要單體,離子型共單體對-苯乙烯磺酸鈉鹽﹙NaSS﹚為共單體,製備出具高表面電位的奈米尺寸高分子球,另外在反應溶液中加入架橋劑二乙烯苯﹙DVB﹚或乙二醇二甲基丙烯酸酯(EGDMA),製備出具高表面電位之架橋奈米尺寸高分子球。並以動態粒徑分析儀(DLS)來探討在各種製備條件下對製備出的奈米高分子球其粒徑分佈、粒徑大小與表面電位的影響。
    無乳化劑乳化聚合法使用沸騰法,將其反應溫度提升至沸騰狀態,加快反應時間,並利用不同的單體比例、一步驟合成法、兩步驟合成法與使用架橋劑等變數製備奈米高分子球與架橋高分子球。由實驗結果顯示加入水溶性離子單體的確可以使高分子球的粒徑更小,達到奈米尺寸的程度,且其表面電位也比-40.0 mV小。其中,以兩步驟合成法可得到更小粒徑與粒徑分佈較窄的奈米球,在第一階段轉化率50%時添加二階段單體,可合成出數目平均粒徑為21.7nm且其表面電位可達到 -51.4 mV的奈米球。
    微乳化聚合法是使用十二烷基硫酸鈉﹙SDS﹚為乳化劑,在不同比例的單體比例搭配架橋劑,製備奈米高分子球或架橋高分子球。實驗結果顯示,添加NaSS可使反應的乳化劑添加量由3%降為1%,且數平均粒徑由19.7 nm降為7.7 nm。同時所製備之奈米架橋高分子,雖然架橋劑的存在,亦可得到9.9 nm大小數平均粒徑。


    Preparations of nanospheres with high-level zeta potential by soap-free emulsion polymerization and microemulsion polymerization have been developed. These nanospheres were prepared by using styrene (St) as the main monomer, ionic co-monomer styrene sulfonate salt (NaSS) as comonomer. On the other hand, the crosslinked nanospheres were prepared by further adding crosslinking agent DVB or EGDMA. The size distribution, particle size and Zeta potential of nanospheres were measured by Dynamic particle size analysis (DLS).
    The soap-free emulsion polymerization was reacted at the boiling state to increase the reaction rate. The results showed that increasing the weight fraction of NaSS from 0 to 6 wt.%, the size of nanosphere was decreased from 300 to 20 nm. The Zeta potential of nanosphere was smaller than -40.0 mV when the weight fraction of Nass was more than 1 wt.%. Nanospheres prepared by two step, adding Nass during a period of reaction time, the particle size and particle size distribution of nanospheres were decreased. However, the particle size and particle size distribution of crosslinked nanospheres were larger than those of nanospheres.
    In microemulsion polymerization, nanosphere was prepared by adding NaSS to reduce the amount of emulsifier, sodium dodecyl sulfate (SDS). The results showed that increasing the weight fraction of SDS from 0 to 3 wt.%, the size of nanosphere was decreased from 300 to 20 nm. But when the SDS was 1%, increasing the weight fraction of NaSS from 0 to 4 wt.%, the size of nanosphere was decreased from 30 to 7.7 nm. adding NaSS can reduce emulsifier amount 3% to 1%, and the number average particle size reduced from 19.7 nm to 7.7 nm. The crosslink-nanosphere can also get the average particle size of 9.9 nm, the size of the number

    摘要 I Abstract III 誌 謝 V 目錄 VI 表目錄 VIII 圖目錄 X 第一章 緒論 1 1-1 不同粒徑高分子球製備方法 2 1-2 無乳化劑乳化聚合法 3 1-3 微乳化聚合法之簡介 5 1-4 乳液的穩定性 6 1-5 研究動機及目的 8 第二章 實驗 9 2-1 實驗藥品 9 2-2 實驗儀器 10 2-3 實驗方法 11 2-3-1 單體精製 11 2-3-2 以無乳化劑乳化聚合法製備奈米球 11 2-3-3 以微乳化聚合法製備奈米球 15 2-4 乳液純化 17 2-4-1 透析 17 2-5 儀器分析 17 2-5-1 掃描式電子顯微鏡(SEM)測試條件 17 2-5-2 動態粒徑分析儀(DLS)測試條件 17 第三章 結果與討論 18 3-1 以無乳化劑乳化聚合法製備具電位的奈米球 19 3-2-1 不同比例的單體對-苯乙烯磺酸鈉鹽(NaSS)對奈米球的影響 19 3-2 二步驟添加法製備奈米球 27 3-2-1 反應時間對奈米球之影響 27 3-2-2 第一階段不同轉化率添加二階段單體對奈米球之影響(第一階段NaSS 4%含量) 36 3-2-3 第一階段單體NaSS含量對奈米球之影響(添加轉化率為50%) 59 3-3 比較一步驟合成法與二步驟合成法之間的關係 80 3-4 添加不同含量、種類的架橋劑對奈米球之影響 83 3-4-1 添加10wt%乙二醇二甲基丙烯酸酯(EGDMA)對奈米球之影響 83 3-4-2 添加20wt% EGDMA對奈米球之影響 90 3-4-3 添加20wt%二乙烯苯(DVB)對奈米球之影響 97 3-4-4 比較添加不同含量、種類架橋劑對奈米球之間的關係 104 3-5 以微乳化聚合法製備奈米球 106 3-5-1 添加不同含量乳化劑SDS對奈米球之影響 106 3-5-2不同比例的單體對-苯乙烯磺酸鈉鹽(NaSS)對奈米球的影響 113 3-5-3添加不同架橋劑對奈米球的影響 120 3-5-4 比較以乳化聚合法在不同製備條件下之高分子球之間的關係 133 第四章 結論 135 文獻回顧 137

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