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沉淀法超细纳米白炭黑的制备
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摘要
以水玻璃(Na_2SiO_3·nH_2O)为原料,十二烷基苯磺酸钠(LAS)为分散剂,NaCl为絮凝剂,滴加H_2SO_4调节体系pH值,控制硅酸的聚合得到白炭黑沉淀。通过TEM、SEM、BET、吸油值测试等表征方法考察了反应温度、絮凝剂NaCl加入量、水玻璃浓度、体系pH值等条件对产物结构和形貌的影响。结果表明:通过调节NaCl加入量、温度、水玻璃浓度、反应体系pH可实现对白炭黑形貌的有效控制;白炭黑产品一次和二次平均粒径分别为25.37nm、130.6nm,吸油值2.3 mL/g,为球形粒子;BET比表面积为136.0 m~2/g,并且具备微孔、介孔和大孔等较为完整的孔体系,为非晶结构。
By means of the dropwise addition of H_2SO_4 to adjust the pH of the system,nano-silica particles have been successfully prepared through the hydrolysis and condensation of sodium silicate(NaC2SiO_3 ·nH_2O),using NaCl as a flocculant,and sodium dodecyl benzene sulfonate(LAS) as a dispersing agent.The effects of varying the flocculation dosage,substrate concentration,temperature,and pH value of the system have been studied.Laser particle size analysis,nitrogen adsorption measurements,oil adsorption tests,X-ray diffractometry(XRD),trans-mission electron microscopy(TEM),and scanning electron microscopy(SEM) were carried out in order tocharac-terize the structure and morphology of then ano-silica particles.The results show that when the temperature was 70℃,the salt concentration was 0.26 mol/L,the substrate concentration was 0.56 mol/L,and the pH value was 10.65,nano-silica particles with a good dispersion ability can be prepared.Then ano-silica particles exhibit a spherical morphology and amorphous state,with a DBP of 2.3 mL/g,a primary particle size of25.37 nm and a secondary particle size of 130.6 nm.Nano-silica particles have a specific surface area of136.0 m~2/g with ahierar-chical pore system including micropores,mesopores and macropores.
引文

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