Preparation and Characterization of Deltamethrin/Syndiotactic Polypropylene Solid Dispersion Based Filaments

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姓名

蔡雅鈞(Ya-chen Tsai) 查詢紙本館藏

畢業系所

化學工程與材料工程學系

論文名稱

(Preparation and Characterization of Deltamethrin/Syndiotactic Polypropylene Solid Dispersion Based Filaments)

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摘要(中)

本篇論文的研究主旨在於探討以固體分散體理論為基礎製備出的含有溴氰菊酯的聚丙烯纖維的製備方法以及對於其物性上的鑑定結果。
在本篇研究中，我們模擬溼式紡絲法，將含有溴氰菊酯與聚丙烯的混合溶液利用針筒注入凝固浴中形成纖維狀的溴氰菊酯與聚丙烯的混合物。為了挑選適合的溶劑來製備含藥纖維，我們對溴氰菊酯進行了初步溶劑篩選。對於溴氰菊酯來說，一共有二十一個良好溶劑(溶解度 5mg/mL)，和兩個不良溶劑(溶解度 5mg/mL)；藉由初步溶劑篩選的結果，我們建立了溴氰菊酯的form space，接著利用form space，我們可以準確的挑選出適當的溶劑來進行模擬溼式紡絲法。
我們使用了多種分析儀器來針對樣品的各種性質做了鑑定。藉由低溫示差掃描熱分析儀測量溴氰菊酯與聚丙烯固態分散薄膜及纖維的熔點和玻璃轉化溫度；利用傅立葉轉換紅外線光譜儀來鑑定聚丙烯在薄膜及纖維狀下的形態以及測試溴氰菊酯與聚丙烯固態分散薄膜中兩者之間是否有分子間作用力的存在；含有溴氰菊酯的聚丙烯纖維的晶粒尺寸可以透過X光繞射圖譜計算獲得；附有加熱裝置的偏光顯微鏡可以透過加熱過程中的相變化來判斷溴氰菊酯與聚丙烯熔融後混合介面中的成分；最後我們進行溶離試驗來比較不同比例的含有溴氰菊酯的聚丙烯纖維間的溶離速率。
經過一連串的實驗結果，我們發現在所有比例中溴氰菊酯與聚丙烯之間都是不互溶的；並且兩者分子之間並沒有任何分子作用力的存在。而在不同比例的溴氰菊酯/聚丙烯的纖維中，重量比例為10/90的含藥纖維所測量出來溴氰菊酯晶粒尺寸為6.9奈米；比例20/80的是13.4奈米；比例30/70的是18.9奈米；而比例100/0的是47.1奈米，其溶離速率的快慢為10/90 > 20/80 > 30/70 > 100/0。接著使用Korsemeyer-Peppas model 對溶離速率曲線作迴歸，所有得到的n值(release exponent)皆小於5，這代表溴氰菊酯是從多孔隙的纖維釋放出來的。
綜合X光繞射圖譜與溶離速率曲線的結果，我們推測奈米化的溴氰菊酯晶粒增加了其表面面積，而增加的表面面積也代表病媒蚊與藥物的接觸面積增加，因此病媒蚊的死亡率也可以相對的提升，進而達到更好的瘧疾防護效率。不僅如此，模擬溼式紡絲法提供了與現有的長效型蚊帳傳統生產方法不一樣的好處，例如：對於熔融紡絲法而言，如果紡絲品是較高熔點的高分子，模擬濕式紡絲法可以避免了低熔點藥物的裂解，並且其相較於熔融紡絲法較低溫度的製程可以節省能源。

摘要(英)

The aim of this thesis is to prepare and characterization solid dispersion based deltamethrin/syndiotactic polypropylene(sPP) filaments by the solvent method. We use the imitative wet spinning (needle injection) method to prepare deltamethrin/sPP filaments. Initial solvent screening was used to establish the form space of deltamethrin. There were 21 good solvents and two bad solvents for deltamethrin. From the form space of deltamethrin, we chose the suitable solvent which could be used to imitative wet spinning process. The melting points and glass transition temperatures of solid dispersions samples could be determined by LTDSC. FT-IR was used to observe the polymorphic form of sPP and interaction between deltamethrin and sPP. XRD was used to determine the crystallite sizes of deltamethrin in deltamethrin/sPP filaments. HSPOM was used to observe the melting and crystallization behaviors of samples. The dissolution tests were used to compare the dissolution rates in different ratios of deltamethrin/sPP filaments. Deltamethrin and sPP were immiscible in all the ratios of solid dispersions samples. The FTIR spectra did not show any peak shift which indicated that was no interaction between deltamethrin and sPP. The deltamethrin/sPP filaments with weight ratios of 10/90, 20/80, 30/70, and 100/0 gave the deltamethrin crystallite sizes of 6.9, 13.4, 18.9 and 47.1 nm, respectively. The dissolution rates of deltamethrin/sPP filaments were arranged in the descending order according to the weight ratios of 10/90 > 20/80 > 30/70 > 100/0. The Korsemeyer-Peppas model was used to fit the dissolution profiles. All n values were < 0.5 which meant that the drug was released from a porous system. From XRD patterns and dissolution profiles, we believed that the nanosized deltamethrin crystallites within the solid dispersion based filaments increased the surface area of deltamethrin which could increase the mortality of anopheles by increasing the contact area between anopheles and the insecticide.

關鍵字(中)

★ 含藥型蚊帳
★ 固態分散體

關鍵字(英)

論文目次

摘要 ........................ I
Abstract ....................III
Acknowledgement ............. V
Table of contents ........... VI
List of Figures ............. X
List of Tables .................XIV
Chapter 1 Executive Summary .................. 1
1.1 Introduction ............................ 1
1.2 Brief Introduction of Deltamethrin ............... 4
1.3 Brief Introduction of Syndiotactic Polypropylene................................... 6
1.4 Conceptual Framework................... 10
1.5 References ....................... 12
Chapter 2 Analytical Instruments ........................ 19
2.1 Introduction ....................................... 19
2.2 Spectroscopy Analysis Methods ................. 22
2.2.1 Fourier Transform Infrared (FT-IR) Spectroscop......... 22
2.2.2 Ultraviolet-Visible Molecular Absorption Spectrometer (UV/Vis) ................. 24
2.3 Thermal Analysis Method .................................. 27
2.3.1 Thermogravimetric Analysis (TGA) ............................ 27
2.3.2 Low Temperature Differential Scanning Calorimetry (LT-DSC) .................... 28
2.4 Crystallographic Analysis Method ....................................... 32
2.4.1 Powder X-ray Diffractometry (PXRD) ........................................................... 32
2.5 Microscopic Methods ................................. 36
2.5.1 Hot Stage Polarized Optical Microscopy (HSPOM) ............. 36
2.6 Conclusions ................................... 39
2.7 References ................................... 40
Chapter 3 Preparation and Characterize of Deltamethrin/Syndiotactic Polypropylene Solid Dispersions ................................................. 43
3.1 Introduction ................... 43
3.1.1 Insecticide-treated Nets .............. 43
3.1.2 Solid dispersions ................................. 45
3.2 Materials ...................................... 51
3.2.1 Chemicals ........................................ 51
3.2.2 Solvents ................................. 51
3.3 Experimental Procedures ......................... 55
3.3.1 Initial solvent screening of deltamethrin ......................................................... 55
3.3.2 Preparation of deltamethrin/sPP solid dispersions .......................................... 55
3.3.3 Preparation of deltamethrin/sPP filaments ............................................... 55
3.3.4 Miscibility test ....................... 56
3.3.5 Crystallization Behavior ......................... 56
3.3.6 Dissolution studies ........................... 56
3.3.7 Analytical Measurements ...................... 57
3.4 Results and Discussions .......................... 61
3.4.1 Characterization of Deltamethrin and sPP................ 61
3.4.2 Form Space of Deltamethrin.................. 66
3.4.3 DSC Studies ......................... 69
3.4.4 Miscibility Studies ................ 74
3.4.4 FT-IR studies ............................... 75
3.4.5 X-Ray Diffractometry Studies ............ 76
3.4.6 Crystallization Behavior ........ 78
3.4.7 Dissolution Studies .............................. 80
3.5 Conclusions ........................... 82
3.6 Reference .......................................... 83
Chapter 4 Conclusions and Future Work ................. 89
4.1 Initial solvent screening ............. 89
4.2 Deltamethrin/sPP solid dispersions films and filaments ................................... 90
4.3 Other applications for solid dispersions filaments .................................. 90
4.4 References .................................. 91

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Chapter 4
1 Mahakittikun, V.; Boitano, J. J.; Komoltri, C.; Ninsanit, P.;& Wangapai, T. Anti-mite Covers: Potential Criteria for Materials Used Against Dust Mites. Text. Res. J. 2009, 79(5), 436-443.
2 Shi, H.; Xin, J. H. Cosmetic Textiles: concepts, application and prospects. In Proceeding in the 9th Asia Textile Conference.D01-14, TaiChun, Taiwan, June 28-30, 2007

指導教授

李度(Tu Lee)

審核日期

2013-7-22

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