【摘要】：采用實(shí)驗(yàn)室自制的籠型八苯基硅倍半氧烷(OPS)和一種新型阻燃劑含磷籠型低聚硅倍半氧烷(DOPO-POSS),通過(guò)雙螺桿擠出機(jī)加工的方式與聚碳酸酯(PC)共混制得質(zhì)量分?jǐn)?shù)4%DOPO-POSS和6%OPS的阻燃復(fù)合物。利用裂解-氣相色譜/質(zhì)譜聯(lián)用儀(Py-GC/MS)對(duì)復(fù)合物的裂解產(chǎn)物進(jìn)行了分析;通過(guò)傅里葉變換紅外光譜儀(FT-IR)和掃描電子顯微鏡-X射線能譜儀(SEM-EDS)分別對(duì)殘?zhí)康哪巯嘟Y(jié)構(gòu)與元素組分進(jìn)行分析。Py-GC/MS分析結(jié)果表明,總的質(zhì)譜圖顯示PC/DOPO-POSS和PC/OPS復(fù)合物在熱解過(guò)程中釋放出大量小分子氣體產(chǎn)物,有效地促進(jìn)了炭層的膨脹;OPS在氣相裂解中釋放出大量的苯和氣態(tài)Si O2,并有少量CO2氣體釋放;DOPO-POSS裂解過(guò)程中釋放出多種小分子氣體,其中DOPO含量最高,達(dá)到26%。FT-IR對(duì)凝聚相炭層結(jié)構(gòu)測(cè)試表明,PC/OPS和PC/DOPO-POSS復(fù)合物的內(nèi)部炭層結(jié)構(gòu)相似,由無(wú)機(jī)炭結(jié)構(gòu)組成;在外部炭層結(jié)構(gòu)中,PC/OPS復(fù)合物含有大量-O-Si-O-結(jié)構(gòu),并伴隨有少量的芳香烴炭結(jié)構(gòu)和Si-C結(jié)構(gòu);PC/DOPO-POSS復(fù)合物主要由-P(=O)-O-Si-結(jié)構(gòu)和少量Si-O結(jié)構(gòu)組成。SEM-EDS測(cè)試結(jié)果表明,PC/DOPO-POSS復(fù)合物炭層成分中C元素含量最高,O元素含量次之,Si和P元素含量最少;PC/OPS復(fù)合物炭層成分中,Si和O元素含量最大,占到92.5%,C元素含量最低。
[Abstract]:The caged octylsilyl hemioxane (OPS) and a new flame retardant containing phosphorus-containing cage polysilysilyl hemioxane (DOPO-POSS) were used in this paper. The flame retardant composites of 4%DOPO-POSS and 6%OPS were prepared by blending polycarbonate (PC) with twin-screw extruder. The pyrolysis products were analyzed by pyrolysis-gas chromatography-mass spectrometry (Py-GC/MS). The condensed phase structure and elemental composition of carbon residue were analyzed by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy X-ray energy spectrometer (SEM-EDS) respectively. The results of Py-GC/MS analysis showed that, The mass spectra show that the PC/DOPO-POSS and PC/OPS complexes release a large number of small molecular gas products during the pyrolysis process, which can effectively promote the expansion of the carbon layer. OPS releases a large amount of benzene and gaseous Si O _ 2 in gas phase cracking, and a small amount of CO2 gas is released. During the cracking of DOPO-POSS, a variety of small molecular gases were released, among which the content of DOPO was the highest, and the structure of condensed carbon layer was tested by 26%.FT-IR. The results showed that the structure of carbon layer in PC/OPS and PC/DOPO-POSS complex was similar. It is composed of inorganic carbon structure. In the outer carbon layer structure, PC/OPS complex contains a lot of O-Si-O- structure, accompanied by a small amount of aromatic carbon structure and Si-C structure. The PC/DOPO-POSS complex is mainly composed of -P (= O) -O-Si-structure and a small amount of Si-O structure. The results of SEM-EDS test show that the content of C element in the carbon layer of PC/DOPO-POSS complex is the highest, and the content of O element is the second. The contents of Si and P were the least; The content of Si and O is the highest in the carbon layer of PC/OPS complex, accounting for 92.5% of C element.
【作者單位】： 北京理工大學(xué)材料學(xué)院國(guó)家阻燃材料工程技術(shù)研究中心;
【基金】：國(guó)家自然科學(xué)基金青年基金資助項(xiàng)目(51303011) 北京理工大學(xué)基礎(chǔ)研究基金(20130942002)
【分類號(hào)】：TQ317;TB332

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