A Study of Crosslinked Poly(butylenes succinate) Nanocomposites 交聯型聚琥珀酸丁酯奈米複合材料 Chaoyang University of Technology Applied Chemistry 朝陽科技大學 應用化學系 Adviser: Professor 石燕鳳 Student : 游雅淳 Date : December 10, 2011

Outline Introduction Experiment Results and discussion Conclusions Materials Preparation of samples Measurement Results and discussion Conclusions

Introduction Since the last century, plastic industry has developed so fast that plastic products have gained universal application in many fields. However, most of the plastic products are not biodegradable, and this causes serious environmental pollution. Among aliphatic polyesters, poly(butylene succinate) (PBS) has relatively higher melting temperature and other excellent properties. However, the insufficient mechanical properties of PBS have prevented it from being used in diverse applications. Crosslinking is another effective method to improve the properties of PBS.

Experiment Materials (1/2) Poly(butylene succinate) (聚琥珀酸丁酯，PBS) Montmorillonite (奈米蒙脫土，MMT) (HT：hydrogenated Tallow)

Experiment Materials (2/2) Dicumyl Peroxide (過氧化二異丙苯，DCP) Triallyl isocyanurate (三烯丙基異三聚氰酸酯，TAIC)

Experiment Preparation of samples 1. Modification of Montmorillonite

PBS Mechanism

Table 1 The composition and code of samples Experiment Table 1 The composition and code of samples Name PBS (g) TFC (g) TAIC (g) DCP (g) PBS 100 1PBS 97 3 0.2 0.25 2PBS 0.5 3PBS 1.0 4PBS 5PBS 6PBS

Experiment Measurement Thermal Gravimetric Analyzer (熱重分析儀，TGA) Differential Scanning Calorimeter(微差掃描式熱分析儀， DSC) Polarizing Optical Microscope (偏光顯微鏡，POM) Gel fraction of crosslinked PBS (交聯程度測試) Biodegradability (生物分解性實驗) Water absorption  (吸水性實驗)

Results and discussion(1/7) TGA analysis Fig 1. TGA curves of MMT and TFC

Results and discussion(2/7) Table 2 The samples of gel fraction Gel fraction of crosslinked PBS Name Gel fraction(%) 1PBS 61.14 2PBS 73.37 3PBS 80.85 4PBS 89.92 5PBS 93.77 6PBS 93.57

Results and discussion(3/7) TGA analysis Fig 2 . TGA curves of PBS with different concentrations of DCP

Results and discussion(4/7) DSC analysis Fig 3. DSC curves of of PBS with different concentrations of DCP

Results and discussion(5/7) POM observation (A) (B) (C) (D) Fig 4. POM photographs of PBS

Results and discussion(5/7) POM observation 4PBS 5PBS 6PBS Fig 5. POM photographs of PBS with different concentrations of DCP

Results and discussion(6/7) Biodegradation of crosslinked PBS Fig 6. Weight loss of original and crosslinked PBS in biodegradation

Results and discussion(7/7) Water absorption test Fig 7. Water absorption of original and crosslinked PBS

Conclusions(1/2) 1.The modified montmorillonite can enhance the thermal stability of PBS. 2.Gel fraction increased with increasing content of the crosslinking agent. 3. As crosslinked happened, Tc shifted to higher temperatures, and the degree of crystallinity decreased slightly.

Conclusions(2/2) 4. The degradation rate of PBS was decreased with the introduction of crosslinked structure. 5. In water absorption testing, the results reveal that PBS is a hydrophobic material and the montmorillonite-containing sample tends to be a hydrophilic material.

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Gel fraction 利用索氏萃取(Soxhlet extraction)裝置，取適量交聯後之 PBS樣品，並秤其重量We使用氯仿為溶劑，於80℃下，萃 取24小時，將樣品中未交聯之分子洗去，再將交聯之樣品 烘乾之後秤重Wf，即可計算其交聯度(Gel fraction)。

Biodegradation 先將試片，各別秤重記錄初始重量Wa，放入樣品瓶 中，加入含有酵素之緩衝溶液中，於往復式震盪恆溫 水槽中，於50℃下，轉速175rpm下震盪。每48小時將 樣品取出，秤重記錄重量Wb，計算重量損失Wloss。

Water absorption 先將樣品精秤至小數點下第四位Wc，將秤重好的樣品浸入 水中，於室溫下靜置48小時，將樣品取出，利用擦拭紙將 樣品表面的水吸乾，記錄其重量Wd，計算其吸水性Wl， 再將樣品放回樣品瓶，計算其吸水性。