聚碳酸酯与硅倍半氧烷复合物气相热裂解和凝聚相产物对比

发布时间：2019-01-23 20:20

【摘要】：采用实验室自制的笼型八苯基硅倍半氧烷(OPS)和一种新型阻燃剂含磷笼型低聚硅倍半氧烷(DOPO-POSS),通过双螺杆挤出机加工的方式与聚碳酸酯(PC)共混制得质量分数4%DOPO-POSS和6%OPS的阻燃复合物。利用裂解-气相色谱/质谱联用仪(Py-GC/MS)对复合物的裂解产物进行了分析;通过傅里叶变换红外光谱仪(FT-IR)和扫描电子显微镜-X射线能谱仪(SEM-EDS)分别对残炭的凝聚相结构与元素组分进行分析。Py-GC/MS分析结果表明,总的质谱图显示PC/DOPO-POSS和PC/OPS复合物在热解过程中释放出大量小分子气体产物,有效地促进了炭层的膨胀;OPS在气相裂解中释放出大量的苯和气态Si O2,并有少量CO2气体释放;DOPO-POSS裂解过程中释放出多种小分子气体,其中DOPO含量最高,达到26%。FT-IR对凝聚相炭层结构测试表明,PC/OPS和PC/DOPO-POSS复合物的内部炭层结构相似,由无机炭结构组成;在外部炭层结构中,PC/OPS复合物含有大量-O-Si-O-结构,并伴随有少量的芳香烃炭结构和Si-C结构;PC/DOPO-POSS复合物主要由-P(=O)-O-Si-结构和少量Si-O结构组成。SEM-EDS测试结果表明,PC/DOPO-POSS复合物炭层成分中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复合物炭层成分中,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.
【作者单位】：北京理工大学材料学院国家阻燃材料工程技术研究中心;
【基金】：国家自然科学基金青年基金资助项目(51303011) 北京理工大学基础研究基金(20130942002)
【分类号】：TQ317;TB332

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