連續微流道反應器中進行防污聚合物篩選

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黃聖迪(Sheng-Ti Huang) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

連續微流道反應器中進行防污聚合物篩選
(Antifouling Polymer screening in Continuous Flow Microreactor)

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至系統瀏覽論文 (2028-7-31以後開放)

摘要(中)

連續式聚合提供了一些明顯的優勢，包括均勻混合、易於控制停留時間、高重現性和高安全性。除此之外，流動反應器系統，只需用數個小時即可得到高轉化率的產物，通過適當選擇反應參數，可快速確定最佳反應條件，而此最佳條件可以透過微流道系統應用於大規模生產。相較於批式反應器需要大容量存儲空間亦耗時，並花費大量生產成本，連續式聚合可增加生產效率。
在此實驗中，採用了一個簡單和低成本的管狀連續式反應器，而管線與停留時間可以隨時調整，因此單體的完全轉化將成為目標，以避免任何純化步驟，除此之外，此管狀連續式反應器用來方便地擴大規模和降低合成成本，還可以用高通量的方法來篩選共聚物組成。從而快速合成一個廣泛的聚合物。鑑於此，我們透過傳統的自由基聚合反應合成不同條件下的共聚物，並利用浸塗處理將共聚物以物理吸附至組織培養聚苯乙烯(TCPS)進行表面修飾。此共聚物以2-羥乙基甲基丙烯酸乙酯 (HEMA) -甲基丙烯酸月桂酯 (DMA)為基礎，其一，HEMA其擁有高生物相容性、親水性，其二，DMA能夠使共聚高分子物理吸附於TCPS，共聚物利用核磁共振氫譜 (1H NMR) 鑑定結構和轉化率，再透過凝膠滲透層析儀 (GPC) 確認不同條件下之分子量;使用水接觸角測量儀確認塗層的親水性；X射線光電子能譜儀 (XPS)及衰減全反射傅立葉轉換紅外光譜儀 (ATR-FTIR) 驗證塗層表面組成;運用橢圓偏光儀 (Ellipsometer) 分析修飾厚度;細菌及蛋白質貼附測試檢測平板的抗污特性。
本實驗中，藉由調整反應時間、反應溫度、單體濃度、單體對起始劑比例去檢驗最佳反應條件，得知塗層之最佳親水性、抗汙性，由於可快速篩選的特性，此流動式反應器系統有望高產量製造有益的表面修飾材料應用於醫療器材。

摘要(英)

Continuous polymerization offers several advantages, including uniform mixing, easy control of residence time, high reproducibility, and high safety. In addition, a flow reactor system can produce high conversion rates in just a few hours, and by appropriately selecting reaction parameters, the optimal reaction conditions can be quickly determined, which can be applied to large-scale production through microchannel systems. Compared to batch reactors, which require large storage spaces and are time-consuming and expensive, continuous polymerization can increase production efficiency.
In this experiment, a simple and low-cost tubular continuous reactor was used. The pipeline and residence time can be adjusted at any time, so the complete conversion of the monomer will be the goal to avoid any purification steps. In addition, this tubular continuous reactor is used to conveniently scale up, and high-throughput methods can be used to screen copolymer compositions, thereby quickly synthesizing a wide range of polymers library. In this view, we synthesized copolymers under different conditions via free radical polymerization and the copolymer was physically adsorbed onto tissue-cultured polystyrene (TCPS) through a dip coating process to perform surface modification and used dip coating to physically adsorb the copolymers for surface modification. The copolymer is based on 2-hydroxyethyl methacrylate (HEMA)-ran-Dodecyl methacrylate (DMA). First HEMA is known as a hydrophilic and biocompatible monomer. Second DMA for physical absorption of polymers on TCPS. The copolymer structure and conversion rate were determined by 1H nuclear magnetic resonance (1H NMR), and the molecular weight under different conditions was confirmed by gel permeation chromatography (GPC). The hydrophilicity of the coating was confirmed using a water contact angle goniometer, and the surface composition of the coating was verified using attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR).
In this experiment, the optimal hydrophilicity and antifouling properties of the coating were examined by adjusting reaction time, reaction temperature, monomer concentration, and monomer-to-initiator ratio. Due to its rapid screening capabilities, this flow reactor system is expected to produce high-yield beneficial surface modification materials for use in medical devices.

關鍵字(中)

★ 連續式反應器
★ 流動化學
★ 醫療塗層
★ 非特異性吸附
★ 高通量
★ 雙親性高分子

關鍵字(英)

★ continuous reactor
★ flow chemistry
★ medical coatings
★ non-specific adsorption
★ high throughput
★ amphiphilic copolymers

論文目次

中文摘要 I
ABSTRACT II
致謝 III
目錄 IV
圖目錄 VII
表目錄 IX
化學品名詞簡稱 X
共聚物名詞簡稱 X
一、文獻回顧 1
1-1 批次反應器合成高分子之應用與困境 1
1-2連續式反應器 2
1-2-1連續式反應器之優勢 2
1-2-2晶片型微流道反應器 (Microchip Reactor) 3
1-2-3線圈管式微流道反應器 (Coiled Tube Microreactor) 4
1-3高通量(HIGH THROUGHPUT)實驗方法 5
1-3-1高通量實驗 5
1-3-2 一次一因子實驗 (One Factor At a Time Experimentation,OFAT) 5
1-3-3 一次一因子實驗(OFAT)缺點 6
1-3-4 實驗設計 (Design of Experiments) 7
1-4 抗吸附材料 8
1-4-1 2-甲基丙烯酸羥乙酯(2-Hydroxyethyl Methacrylate,HEMA) 8
1-4-2 2-甲基丙烯醯氧乙基磷醯膽鹼 (2-Methacryloyloxy ethyl phosphorylcholine,MPC) 9
1-4-3 2-(甲基丙烯醯氧基)乙基]三甲基銨(2-(Methacryloyloxy) ethyltrimethylammonium chloride,TMAEMA) 10
1-4-4 聚乙二醇(poly(ethylene glycol), PEG) 10
1-5 表面改質基板 11
1-5-1金屬生物材料 11
1-5-2高分子生物材料 11
二、研究目的 13
三、實驗藥品與實驗方法 15
3-1實驗藥品與設備 15
3-1-1 藥品清單 15
3-1-2 儀器設備清單 16
3-1-3 微流道設計 16
3-2材料製備 19
3-2-1 合成Poly(HEMA-ran-DMA) 19
3-2-2 合成Poly(MPC-DMA) 19
3-2-3 合成Poly(TMAEMA-DMA) 19
3-2-4 合成Poly(PEGMA-DMA) 19
3-2-5 矽晶圓(silicon wafer ) 基材製備 20
3-2-6 組織培養聚苯乙烯(TCPS)基材準備 20
3-3 實驗方法 21
3-3-1 液態核磁共振氫譜 (1H NMR) 21
3-3-2 凝膠滲透層析儀 (Gel Permeation Chromatogragh ,GPC) 21
3-3-3 P(HEMA-ran-DMA)TCPS平板修飾 21
3-3-4 衰減全反射式傅立葉轉換紅外光譜儀 (Attenuated Total Reflectance-Fourier-Transform Infrared Sepectroscopy,ATR-FTIR) 21
3-3-5 X射線光電子能譜儀 (X-ray Photoelectron Spectroscopy,XPS) 22
3-3-6 水接觸角測量 (Water Contact Angle Measurement) 22
3-3-7 薄膜厚度之量測 (Ellipsometry) 22
3-3-8 細菌貼附測試 (Bacteria Adhesion Test) 22
3-3-9 蛋白質吸附測試 (Protein Adsorption Test) 23
四、結果討論 24
4-1 高通量合成 24
4-1-1 反應時間與單體比例對轉化率影響 25
4-1-2 Poly(2-Hydroxyethyl methacrylate-ran-dodecyl methacrylate), P(HEMA-ran-DMA)鑑定 (1H NMR) 26
4-1-3反應時間與單體比例對分子量影響 27
4-1-4 反應溫度與單體濃度對轉化率影響 28
4-1-5 反應溫度與單體濃度對分子量影響 30
4-1-6 單體對起始劑比例對轉化率影響 31
4-1-7 單體對起始劑比例對分子量影響 32
4-2塗層表面特性檢測 34
4-2-1 平板表面官能基測定 (ATR-FTIR) 34
4-2-2 表面元素測定 (XPS) 35
4-3 塗層表面功能性分析 37
4-3-1反應時間對薄膜膜度影響 37
4-3-2 反應溫度與單體濃度對薄膜厚度影響 38
4-3-3單體對起始劑比例對薄膜厚度影響 39
4-3-4反應時間與DMA/HEMA 比例對水接觸角影響 40
4-3-5 反應溫度與單體濃度對水接觸角影響 41
4-3-6 單體對起始劑比例對水接觸角影響 42
4-4浸塗表面抗吸附測試 43
4-4-1細菌貼附測試 43
4-4-2 蛋白質吸附試驗 49
4-5 不同單體鑑定 52
4-5-1不同單體性質測試 52
4-5-2不同單體塗層表面元素分析 55
4-5-3不同單體塗層表面功能性分析 61
4-5-4不同單體浸塗表面抗吸附測試 62
五、結論 66
六、未來展望 67
七、參考文獻 68

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指導教授

黃俊仁(Chun-Jen Huang)

審核日期

2023-7-26

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