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主管单位 中华人民共和国
工业和信息化部
主办单位 中国材料研究学会
哈尔滨工业大学
主编 苑世剑 国际刊号ISSN 1005-0299 国内刊号CN 23-1345/TB

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引用本文:杜兆芳,李继丰,董丹丹.超声场醇盐水解三氧化二锑颗粒的制备与表征[J].材料科学与工艺,2019,27(2):77-83.DOI:10.11951/j.issn.1005-0299.20170239.
DU Zhaofang,LI Jifeng,DONG Dandan.Preparation and characterization of Sb2O3 particles by hydrolysis of alkoxides in ultrasonic[J].Materials Science and Technology,2019,27(2):77-83.DOI:10.11951/j.issn.1005-0299.20170239.
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超声场醇盐水解三氧化二锑颗粒的制备与表征
杜兆芳,李继丰,董丹丹
(安徽农业大学 轻纺工程与艺术学院,合肥 230036)
摘要:
为减少协效阻燃剂中Sb2O3用量,降低其作为阻燃剂对材料性能的损伤.试验用SbCl3通过超声场醇盐水解法制备Sb2O3粒子,探究阳离子和非离子表面活性剂对颗粒制备的粒径影响,再以正交试验考察氨水量、超声波处理时间及温度对Sb2O3颗粒生成时尺寸大小的影响,并得出最优制备工艺.通过扫描电子显微镜(SEM)、X射线衍射仪(XRD)对Sb2O3粒子微观结构进行了观察.结果表明:影响制备的试验条件为氨水与水体积比>超声处理温度>超声时间,且当氨水与水体积比为50∶0、超声处理20 min、45 ℃时,制得颗粒粒径为1.17 μm;晶体类型为斜方晶型,结晶度高、晶粒度较大;在干燥时粒子进行了二次生长,大多数Sb2O3粒子呈长方体结构,轮廓尖锐,粒径0.5~2.0 μm.为验证复合阻燃性,将其制备成介层多孔核-壳型Sb2O3@SiO2阻燃颗粒,复合阻燃颗粒与聚合物基体相容性较好,颗粒分布均匀,材料阻燃效果明显.较于纳米型Sb2O3颗粒,复合颗粒表现出协同阻燃效果,并降低了软质塑料阻燃成本.
关键词:  超声醇盐水解  Sb2O3晶体  正交试验  微观形貌  阻燃性能
DOI:10.11951/j.issn.1005-0299.20170239
分类号:TB321
文献标识码:A
基金项目:安徽省教育厅2013年全省高校省学术技术带头人及后备人选培养资助项目.
Preparation and characterization of Sb2O3 particles by hydrolysis of alkoxides in ultrasonic
DU Zhaofang, LI Jifeng, DONG Dandan
(College of Light-textile Engineering and Art, Anhui Agricultural University, Hefei 230036, China)
Abstract:
This study aims to decrease the amount of Sb2O3 in synergistic flame retardants and reduce its damage as flame retardant additive to the mechanical properties of materials. The Sb2O3 particles used in this experiment were prepared by the hydrolysis of SbCl3. Effects of cationic and nonionic surfactants on the particle size of the prepared particles were investigated. The effect of ammonia concentration, ultrasonic treatment time, and temperature on Sb2O3 particle size was studied by orthogonal experiment, and the optimum process was obtained. The microstructure, crystal structure, and morphology of the Sb2O3 were characterized by SEM and XRD. Results show that the conditions and factors affecting the preparation of particles are: ammonia/water rate>ultrasonic treatment temperature>ultrasonic time. For example, when ammonia/water rate was 50∶0, ultrasonic time was 20 min, and ultrasonic temperature was 45 ℃, the Sb2O3 particle size was 1.17 μm. X-ray powder diffraction characterization of the crystal type was orthorhombic with high crystallinity and large grain size. SEM and laser particle size analyzer showed that most Sb2O3 particles had a rectangular parallelepiped structure with a sharp particle profile ranging from 0.5 to 2.0 μm. The nanosized Sb2O3 crystal particles prepared during the drying process experienced secondary growth. The particles were further prepared into porous core-shell Sb2O3 @ SiO2 flame retardant particles to achieve the synergistic flame retardant effect and reduce the cost of flame retardants as soft plastic. Compared with nano-Sb2O3, the trace addition is more compatible with the polymer matrix, the distribution is more uniform, and the material flame retardant effect is more obvious with lower cost.
Key words:  hydrolysis of alkoxides in ultrasonic field  Sb2O3 crystals  orthogonal experiment  microstructure  flame retardant

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