Large-scale synthesis of paratacamite nanoparticles with controlled size and morphology
Large-scale synthesis of paratacamite nanoparticles with controlled size and morphology
复制标题
尺寸和形态可控的副氯铜矿纳米颗粒的大规模合成
DOI：
10.1049/mnl.2011.0401
复制
发表时间：
2011-10-01
影响因子：
1.3
通讯作者：
Cui, Hongtao
中科院分区：
文献类型：
--
作者：
Liu, Yan;Ren, Wanzhong;Cui, Hongtao
采用环氧化合物为沉淀剂，一步合成法在室温下制备了尺寸和形貌可控的副氯铜矿（γ-Cu-2（OH）（3）Cl）纳米粒子。单次反应的最大生产能力高达约80 g，这仅受实验室所用设备体积的限制。在制备过程中，通过环氧化物的氧质子化开环反应，促进了金属离子水溶液配合物的水解。由于水溶液中Cu 2+配合物的酸度较低，它们的部分水解发生而没有进一步缩合生成的氢氧化物中间体，导致形成沉淀而不是溶胶或凝胶。这导致Cl-离子插入中间体，形成γ-Cu-2（OH）（3）Cl结构。由反应产生的氯代醇化合物使颗粒的表面官能化，导致所得粉末在水和乙醇中的高重现性。表征结果表明，随着Cu ~（2+）浓度的增加和反应时间的延长，产物的粒径逐渐增大。另一方面，通过改变沉淀剂的种类，可以将环氧丙烷沉淀下的立方体形貌转变为环氧环己烷沉淀下的由团聚的小颗粒组成的球形形貌。
A facile one-step procedure using epoxide as precipitation agent was applied to prepare paratacamite (gamma-Cu-2(OH)(3)Cl) nanoparticles with well-controlled size and morphology on a large scale at room temperature. The maximum production capacity in single reaction is as much as about 80 g, which is only limited by the volume of the facilities used in the laboratory. During the preparation, the hydrolysis of aquo complexes of metal ions was promoted by the ring opening reaction of epoxide through protonation of its oxygen. Owing to the low acidity of aquo Cu2+ complexes in solution, their partial hydrolysis occurred without further condensation of the generated hydroxide intermediate, resulting in the formation of precipitate instead of sol or gel. This induced the interposition of Cl- ions into intermediate to form the structure of gamma-Cu-2(OH)(3)Cl. The chlorinated alcohol compound, resulting from the reaction, functionalised the surface of particles, leading to the high re-dispersibility of obtained powder in water and ethanol. As confirmed by the characterisation results, the particle size increased with the increasing of Cu2+ concentration and reaction time. On the other hand, by changing the precipitation agent, the morphology of the particle was transformed from cubic shape under using propylene oxide to the spherical shape that was composed of agglomerated small nanoparticles by using cyclohexene oxide.