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多孔硅橡胶材料的制备及性能研究
论文作者:童鞋论文网  论文来源:www.txlunwenw.com  发布时间:2019/9/6 7:51:17  

摘要:硅橡胶是使用较为广泛的硅基有机弹性体,具有独特的结构与性能。硅橡胶具有更好的热稳定性、耐氧化性和耐电磁辐射性,是优异的耐高温材料和绝缘材料。多孔结构是一种特殊的表面结构,孔隙的引入大大增加了材料的比表面积和孔隙率,提高了材料的可组装性、渗透性和吸附性等性能。将硅橡胶制备成多孔材料可以使所制材料兼具二者的优势而获得特殊功能性。本文首先制备高交联密度加成型硅橡胶,对硅橡胶的结构与性能进行研究;并利用悬浮聚合法制备多孔硅橡胶微球,探究实验条件对多孔硅橡胶微球结构与性能的影响;在此基础上,利用呼吸图法制备多孔硅橡胶膜,并深入研究制备条件对孔径及孔隙率的影响。

分别以不同乙烯基含量的聚二甲基硅氧烷(VS-PDMS)为基胶制备出一系列高交联密度加成型硅橡胶。通过傅立叶变换红外光谱、电子万能试验机、溶胀实验、透光率/雾度测试、热重分析、动态力学分析等对样品进行表征。结果表明:当两种基胶(VS5000/VS200)复配比例为1:0.5时,拉伸强度可达0.79 MPa;在此基础上添加高乙烯基硅油(GS5210),当加入量为10 wt%时,拉伸强度达1.46 MPa。溶胀实验结果表明,交联密度随乙烯基含量增加而增大,交联网络结构由分散交联向集中交联转变。热失重和动态力学分析结果表明,所制备的高交联度硅橡胶材料具有较好的热稳定性和耐低温性,玻璃化转变温度为-113 ℃。

利用悬浮聚合法以乙烯基封端聚二甲基硅氧烷(VS-PDMS)为基胶,聚甲基丙烯酸甲酯(PMMA)微球为致孔剂,乙酸乙酯为溶剂,制备出一系列多孔硅橡胶微球。利用傅立叶变换红外光谱、激光粒度分布仪、热重分析、偏光显微镜、扫描电子显微镜、透光率/雾度测定等对多孔硅橡胶微球的结构、形貌和性能进行表征。结果表明:随着致孔剂用量的增加,多孔微球的粒径先增大后减小,表面孔径分布均匀;随着搅拌速率增加,多孔微球粒径降低;在搅拌速率为800 r/min、PMMA微球用量为1.5 g、溶剂用量为12.5 g的条件下,多孔硅橡胶微球的孔径分布均匀且孔洞较深,具有较好的热稳定性,且可以用于提高PMMA膜材的雾度。

以乙烯基封端聚二甲基硅氧烷(VS-PDMS)和含氢硅油(XL-1341)为主要原料,利用呼吸图法制备出尺寸均匀,形貌规整的多孔硅橡胶膜。通过傅立叶变换红外光谱、热重分析、偏光显微镜、扫描电子显微镜和接触角测试进行表征,最后利用数学分析定量讨论了不同实验条件下多孔膜的表面形貌、孔径分布及孔隙排布情况。实验结果表明:增加硅橡胶的亲水性可以改善多孔膜的成孔性,尤其是亲水性硅胶共混法可以高效实现硅橡胶的本体亲水改性;滴注的铸膜方式可以实现简易条件下的高湿环境铸膜;助溶剂的加入使得孔隙形状更为圆润规整;纳米级SiO2小球可对孔隙形状起到一定的修复作用。此外,孔径会随温度的降低,溶剂沸点的升高及聚合物分子量的增加而增大;随溶剂用量的增加先减小后增大。综上,当VS500:亲水支化硅胶:交联剂Si-H1341:二氯甲烷:乙醇 = 1:0.5:0.67:25.5:3 (质量比)时,硅橡胶微孔膜的成孔性最佳。

Silicone rubber is the most widely used silicone-based organic elastomer with unique structure and properties. In the short-range structure, the bond energy of -Si-O- (368 kJ/mol) is greater than the bond energy of -C-C-bond (347 kJ/mol), which makes silicone rubber have better thermal stability, oxidation resistance and electromagnetic radiation resistance. It is an excellent high temperature resistant material and insulating material. In the long-range structure, the silicone rubber molecules have a small single-link rotation steric hindrance, good molecular chain flexibility, and excellent low temperature resistance.The porous structure is a special surface structure. The introduction of pores greatly increases the specific surface area and porosity of the material, and improves the assemblability, permeability and adsorption properties of the material. Due to the unique characteristics of silicone rubber and porous materials, the preparation of silicone rubber into a porous material can make the materials have both advantages. In this paper, the transparent cross-linked silicone rubber with high crosslink density was first prepared to study the structure and properties of silicone rubber. The porous silicone rubber microspheres were prepared by suspension polymerization method, and the effects of experimental conditions on the structure and properties of porous silicone rubber microspheres were investigated. On this basis, the porous silicone rubber membrane was prepared by the breath figure method, and the effects of prepartion conditions and mechanism on the pore size and porosity were investigated.

A series of the transparent cross-linked silicone rubber with high crosslink density were prepared by different vinyl content polydimethylsiloxane (PDMS) and hydrogen silicone oil (XL-1341). The samples were characterized by Fourier transform infrared spectroscopy, universal tensile tester, swelling test, light transmittance/haze test, thermogravimetric analysis, dynamic mechanical analysisand so on. The results showed that when the ratio of the two base rubbers (VS5000/VS200) is 1:0.5, the tensile strength can reach 0.79 MPa; on this basis, a high vinyl silicone oil (GS5210) was added, and when the amount was 10 wt%, the tensile strength was 1.46 MPa.The results of swelling experiments showed that the crosslink density increased with the increase of vinyl content, and the crosslinked network structure changed from "disperse cross-linking" to "central cross-linking". The results of thermogravimetric analysis and dynamic mechanical analysis showed thatthe prepared highly cross-linked silicone rubber material has good thermal stability and a glass transition temperature of -113 ℃.

Using suspension polymerization method, vinyl terminated polydimethylsiloxane (PDMS) as the base rubber, polymethyl methacrylate (PMMA) microspheres as porogen and ethyl acetate as solvent to prepare a series of porous silicone rubber microspheres. The structure and properties of porous silicone rubber microspheres were characterized by Fourier transform infrared spectroscopy, laser particle size distribution analyzer, thermogravimetric analysis, polarized light microscope, scanning electron microscope and transmittance haze meter. The results showed that with the increase of the amount of porogen, the particle size of the microspheres first increased and then decreased, and the pore size distribution of the microspheres was uniform; as the stirring rate increased, the particle size of the microspheres decreased. Under the conditions of stirring rate of 800 r/min, PMMA microspheres of 1.5 g and solvent dosage of 12.5 g, the porous silicone rubber microspheres have uniform pore size distribution and deep pores, which have good thermal stability and can be used to improve the haze of PMMA film.

关键词:聚硅氧烷;悬浮聚合;呼吸图法;多孔材料

Polysiloxane; Suspension Polymerization; Breath Figure method(BFs); Porous Material

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