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胶体五氧化二锑的制备和性质及对涤纶阻燃增效作用研究
吴建国
Subtype博士
Thesis Advisor柯家骏
1991-06-30
Degree Grantor中国科学院研究生院
Abstract本文主要研制一种新的胶体五氧化二锑体系,研究其成胶过程、胶体性能及在涤纶织物中的阻燃增效作用,开展有关的应用和应用基础工作。本文首次在单一使用少量无机物磷酸的稀溶液中,采用H_2O_2氧化Sb_2O_3方法制备出颗粒小于200A的高度分散的CP-Sb_2O_5溶胶。该新方法具有操作简单和成本降低的特点。通过研究CP-Sb_2O_5氧化成胶过程和分析各影响因素,提出了随着磷酸用量的增加反应体系通过氧化-络合-聚合的途径转化形成CP-Sb_2O_5溶胶的机理。结合XRD、IR和Raman光谱分析的结果,表明氧化产物与磷酸之间存在着相互作用。实验结果还指出,溶液中存在的电解质对CP-Sb_2O_5溶胶的氧化成胶过程、胶体稳定性及颗粒大小均有影响。CP-Sb_2O_5溶胶在甲醇、乙醇、乙二醇极性有机溶剂中能够均匀分散和稳定存在。在胶凝作用下,CP-Sb_2O_5溶胶逐渐转变成凝胶,但增加磷酸用量则可以获得较长期的高浓度的CP-Sb_2O_5溶胶。CP-Sb_2O_5的热稳定性显示出其能满足作为阻燃增效剂的要求。通过对H_2O_2氧化法制备的TEA-Sb_2O_5胶体溶液的氧化成胶了三乙醇胺在胶体溶液中的作用。三乙醇胺在体系中对氧化产物有一定的缔合作用,并对缔合解出的胶体颗粒具有分散稳定作用。分别测定了电解质和有机溶剂对TEA-Sb_2O_5胶体溶液稳定性的影响,并考察了TEA-Sb_2O_5胶体溶液稳定性与放置时间的关系。CP-Sb_2O_5溶胶与四溴双酚A阻燃剂在乙醇溶剂中均匀混合,具有良好的相容许。将组成的溴-锑系复合阻燃液直接对纬编针织涤纶进行阻燃整理。氧指数和垂直燃烧法测试结果表明,整理后的涤纶织物阻燃性能明显提高。CP-Sb_2O_5溶胶不仅显示出明显的阻燃增效作用,而且还可使四溴双酚A阻燃剂的用量适当减少。本文还探索了在硫酸介质中用过硫酸铵将三氧化二锑氧化制备固体水合五氧化二锑的一种新方法。结果指出,在硫酸介质中,过硫酸铵可将三氧化二锑氧化成固体水合五氧化二锑,自身则被还原成硫酸铵进入溶液。
Other AbstractThe main objects of this work are to prepare a new kind of colloidal sol of antimony pentoxide and to investigate the formation process and properties of colloidal sol as well as flame retardant synergism of the colloid in polyester fiber. A colloidal sol of CP-Sb_2O_5 with high dispersion and fine particle size less than 200 A is firstly prepared by the oxidation of antimony trioxide with hydrogen peroxide in aqueous solution only containing small amounts of inorganic phosphoric acid. It is characterized by simple operation and lower cost in the producing procedure. Based on the studies of the oxidation and formation process of CP-Sb_2O_5 sol and the analyses of various influential factors, it is proposed that the formation of CP-Sb_2O_5 sol occur through the paths of oxidation-complexation-aggregation as the concentration of phosphoric acid in reaction system increases. The chemical interaction between the oxidation product and phosphoric acid is confirmed by XRD, IR and Raman spectra. Experimental results further indicate that electrolytes in solution have influences on the conversion process, stability and particle size of CP-Sb_2O_5 sol. The CP-Sb_2O_5 sol proves to be well and stably dispersed in some polar organic solvents such as methanol, ethanol and glycol. Owing to gelation, CP-Sb_2O_5 sol will be slowly converted into a gel. But higher concentration of stable CP-Sb_2O_5 sol can be obtained with adding more amounts of phosphoric acid into the dispersion system. The thermal stability of CP-Sb_2O_5 is satisfactory to the requirement of flame retardant synergist. Analysis and discussion on the function of triethanolamine in the colloidal solution are given from the investigation results on the conversion of reaction system into colloidal solution of TEA-Sb_2O_5 and the spectral determinations of the colloidal product. It is proposed that triethanolamine can be associated with the oxidation product in the dispersion system and have the function to disperse and stabilize the colloidal particles. The experiments on the stability of colloidal solution of TEA-Sb_2O_5 are also carried out. The mixture of CP-Sb_2O_5 sol with organic bromide of tetrabromo bisphenol A is rather stable in the alcohol solvent. Polyester fiber is directly treated with the bromo-antimony flame retardant solution. The measurement results of oxygen index and vertical combustion show that the flame retardance of the treated polyester fiber is obviously improved. The colloidal particles of CP-Sb_2O_5 can increase the flame retardant synergism and reduce the amounts of tetrabromo bisphenol A during the treatment of polyester fiber. A method has been developed to prepare hydrous antimony pentoxide by the oxidation of antimony trioxide with ammonium persulfate in aqueous medium of sulfuric acid. In terms of experimental results, ammonium persulfate oxidizes antimony trioxide into hydrous antimony pentoxide and is reduced it self into ammonium sulfate in aqueous medium of sulfuric acid.
Pages131
Language中文
Document Type学位论文
Identifierhttp://ir.ipe.ac.cn/handle/122111/5813
Collection研究所(批量导入)
Recommended Citation
GB/T 7714
吴建国. 胶体五氧化二锑的制备和性质及对涤纶阻燃增效作用研究[D]. 中国科学院研究生院,1991.
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