聚合物有機(jī)硅阻燃復(fù)合材料的制備和性能研究

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摘 要
多面體低聚倍半硅氧烷(Polyhedral Oligomeric Silsesquioxane,簡(jiǎn)稱POSS)是一種具有籠狀結(jié)構(gòu)的有機(jī)/無(wú)機(jī)雜化分子。與蒙脫土、二氧化硅等傳統(tǒng)的納米填料不同，POSS具有規(guī)整的籠狀結(jié)構(gòu)、納米尺度以及與聚合物良好的相容性，POSS能與聚合物形成真正意義上的分子級(jí)復(fù)合，提高了聚合物的熱穩(wěn)定性，機(jī)械強(qiáng)度，阻燃性，抗氧化，抗老化等性能。
本文首先合成了一種POSS單體(四甲基銨硅氧烷)，并用核磁共振(NMR)，X射線衍射測(cè)試(XRD)，熱重分析（TGA）等對(duì)POSS的結(jié)構(gòu)進(jìn)行了表征。隨后以這種POSS為基礎(chǔ)，制備了PP/IFR/POSS納米復(fù)合材料，并對(duì)其做了錐形量熱儀實(shí)驗(yàn)測(cè)試，得到了PP/IFR/POSS納米復(fù)合材料的熱釋放速率(HRR)、質(zhì)量損失（MLR）、生煙速率（SPR），通過(guò)分析了解它們的阻燃性能。本文具體以三章展開(kāi)：
第一章是前言。描述了POSS的發(fā)展和應(yīng)用等，并詳述了目前POSS合成的研究現(xiàn)狀，對(duì)許多POSS化合物的制備進(jìn)行了歸納總結(jié)。
第二章是四甲基銨硅氧烷和PP/IFR/POSS納米復(fù)合材料的合成。用四甲基氫氧化銨、正硅酸乙酯為原料，采用溶膠-凝膠法制備的八(四甲基銨)籠形倍半硅氧烷(OctaT MA_POSS)。制備足夠的POSS后，進(jìn)一步制備PP/IFR/POSS納米復(fù)合材料。
第三章是四甲基銨硅氧烷和PP/IFR/POSS納米復(fù)合材料的表征與分析。對(duì)POSS單體進(jìn)行了核磁共振、X射線衍射、熱重分析等測(cè)試；對(duì)PP/IFR/POSS納米復(fù)合材料進(jìn)行了錐形量熱儀測(cè)試。

關(guān)鍵詞： 多面體低聚倍半硅氧烷；雜化材料；納米材料；聚丙烯；PP/IFR/POSS納米復(fù)合材料；阻燃性能

ABSTRACT

Polyhedral Oligomeric Silsesquioxane (POSS) is a cage-like organic/inorganic hybrid molecular. Unlike clay and silica, POSS has a well-defined and nanoscale cage-like structure, it is also compatible with polymers. POSS can composite with polymer at molecular level. POSS modified polymers have enhanced properties. It can improved the performance of polymer which is thermal stability, mechanical strength, flame retardant, antioxidant, anti-aging, etc. it is very significant to prepare novel polymer/POSS nanohybrids.
This paper synthesized a kind of POSS monomers (tetramethyl ammonium siloxane), and nuclear magnetic resonance (NMR), X-ray diffraction (XRD) test, thermogravimetric analysis (TGA) had been used to characterize the structure of POSS. Then, on the basis of POSS, PP/IFR/POSS nanocomposites were prepared by means of melt blending, and heat release rate (HRR), mass loss (MLR) provision and smoke generation rate (SPR) were tested by cone calorimeter, which reveal the flame retardant performance of PP/IFR/POSS nanocomposites. The frame structure can be divided into three parts. The first part is an introduction, and the second part is focused on the synthesis of POSS and PP/IFR/POSS nanocomposites. The details of this paper as follows:
Chapter 1 is the preface, which describes the origin, development and application of POSS. Most important, the current research of POSS was described and the preparation of many POSS compounds was summarized.
Chapter 2 is the synthesis of tetramethyl ammonium silicone and PP/IFR/POSS nanocomposites synthesis. Octa(tetramethylammonium) polyhedral oligomeric silsesqioxanes were synthesized by the sol-gel method, using tetramethylammonium hydroxide and tetraethoxysilane as raw material. After synthesizing enough POSS, further production of PP/IFR/POSS nanocomposites.
Chapter 3 is the characterization and analysis of Octa(tetramethylammonium) polyhedral oligomeric silsesqioxanes and PP/IFR/POSS nanocomposites. Taken nuclear magnetic resonance (NMR), X-ray diffraction (XRD),thermogravimetric analysis (TGA) and other test for POSS, Taken cone calorimeter test for PP / IFR / POSS nanocomposite.

KEY WORDS： Polyhedral Oligomeric Silsesquioxane; Hybrid materials; Nanomaterials ; Polypropylene ; PP/IFR/POSS nanocomposites; Flame retardant performance

目 錄
第一章 緒論 1
1.1 引言 1
1.2 常用聚合物阻燃方法 1
1.3 無(wú)鹵阻燃的研究進(jìn)展 2
1.3.1 磷系阻燃劑 2
1.3.2 氫氧化物阻燃劑 3
1.3.3 硅系阻燃劑 4
1.3.4 膨脹性阻燃劑 5
1.4 POSS制備及POSS/聚合物納米復(fù)合材料的阻燃性能研究 6
1.4.1 POSS的結(jié)構(gòu)特點(diǎn) 7
1.4.2 POSS單體的制備 7
1.4.3 POSS/聚合物納米復(fù)合材料的制備 8
1.4.4 POSS/聚合物納米復(fù)合材料的阻燃性能研究 10
1.5 研究思路及內(nèi)容 12
第二章 POSS及PP/IFR/POSS復(fù)合材料的合成與表征 14
2.1 實(shí)驗(yàn)試劑及儀器 14
2.1.1 化學(xué)試劑及規(guī)格 14
2.1.2 所用儀器及生產(chǎn)廠家 14
2.2 四甲基銨籠型硅酸鹽的合成 15
2.3 PP/IFR/POSS納米復(fù)合材料的制備 16
2.4 POSS和PP/IFR/POSS納米復(fù)合材料的表征與測(cè)試 19
2.4.1 核磁共振 19
2.4.2 X射線衍射測(cè)試(XRD) 19
2.4.3 熱重分析 19
2.4.4 掃描電鏡 20
2.4.5 透射電鏡 20
2.4.6 錐型量熱儀實(shí)驗(yàn)測(cè)試 20
第三章 POSS及聚丙烯/POSS復(fù)合材料的結(jié)構(gòu)、性能分析 21
3.1 引言 21
3.2 四甲基銨硅氧烷（POSS）的結(jié)構(gòu)表征 21
3.2.1 核磁共振 21
3.2.2 XRD圖譜分析 22
3.2.3 熱重分析 23
3.2.4 掃描電鏡和透射電鏡 23
3.3 PP/IFR/POSS復(fù)合材料的性能表征 24
3.3.1 PP/IFR/POSS復(fù)合材料的熱釋放速率 25
3.3.2 PP/IFR/POSS復(fù)合材料的質(zhì)量損失 25
3.3.3 POSS/IFR/POSS復(fù)合材料的生煙速率 26
本文總結(jié)及進(jìn)一步工..