纳米磷酸锌的可控合成

doi:10.11962/1006-4990.2018-0524

摘要/Abstract

摘要：

在氧化锌、磷酸固-液反应体系中,以研磨反应代替搅拌反应,辅助表面活性剂对磷酸锌的颗粒尺寸进行可控合成,考察了研磨介质、磨球比例、球料比、固液比、表面活性剂等工艺条件对磷酸锌粒径分布、形貌及团聚状况的影响,并采用SEM、XRD、粒度分布和TEM对纳米磷酸锌做了表征。结果表明,表面活性剂CTAB浓度为9×10^-4 mol/L、研磨时间为3 h、锆球为研磨介质、球料质量比为150:1、Φ10 mm与Φ6 mm磨球质量比为1:4、转速为200 r/min、固液比[氧化锌和（磷酸+表面活性剂）的质量比]为1:1时,可以制备粒径分布为59~79 nm、平均粒径为68 nm、无团聚的粒状纳米磷酸锌。

关键词: 磷酸锌, 纳米颗粒, 可控合成

Abstract:

Particle size of zinc phosphate was controlled-synthetized by grinding reaction instead of stirring reaction and assisted surfactant in the solid-liquid reaction system between zinc oxide and phosphoric acid.The effects of grinding medium,grinding ball ratio,ball-to-material ratio,solid-liquid ratio and surfactant on the particle size distribution,morphology and agglomeration of zinc phosphate were investigated.Nano zinc phosphate was characterized by SEM,XRD,particle size distribution and TEM.Results showed that the non-aggregation granular nanometer zinc phosphate with particle size distribution between 59~79 nm and average particle size of 68 nm could be prepared under the technological conditions as follows:c（CTAB）=9×10^-4mol/L,grinding time was 3 h,zirconium ball as grinding medium,mass ratio of ball to material was 150:1,grinding ball mass ratio of Φ10 mm and Φ6 mm was 1:4,rotating speed was 200 r/min and solid-liquid ratio[mass ratio of zinc oxide to（phosphoric acid+surfactant）] was 1:1.

Key words: zinc phosphate, nano-particle, controlled-synthesis

中图分类号:

TQ126.35

陈心怡,黄云龙,袁爱群,黄增尉,韦冬萍,马少妹. 纳米磷酸锌的可控合成[J]. 无机盐工业, 2019, 51(8): 20-24.

Chen Xinyi,Huang Yunlong,Yuan Aiqun,Huang Zengwei,Wei Dongping,Ma Shaomei. Controlled-synthesis of nanometer zinc phosphate[J]. Inorganic Chemicals Industry, 2019, 51(8): 20-24.

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参考文献 17

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磨球类型	粒度分布	平均粒径	形貌,团聚程度
玛瑙球	142~712 nm, 4.8~6.4 μm	1.5 μm	块状+粒状,无团聚
锆球	531 nm~1.1 μm	728 nm	粒状,无团聚

磨球类型	粒度分布	平均粒径	形貌,团聚程度
玛瑙球	396 nm~1.7μm,3.1~6.4 μm	1.4 μm	块状+粒状,微团聚
锆球	59~79 nm	68 nm	粒状,微团聚

磨球质量比	粒度分布	平均粒径	形貌,团聚程度
1:2	915 nm~1.5 μm	1.15 μm	块状+粒状,团聚明显
1:4	59 ~79 nm	68 nm	粒状,无团聚
1:6	531~825 nm	642 nm	块状+粒状,团聚明显
1:0.5:0.5	615 nm~1.1 μm	883 nm	块状+粒状,微团聚
1:1:1	295~459 nm	376 nm	块状+粒状,团聚明显
1:2:4	459~712 nm	578 nm	块状+粒状,团聚明显

球料质量比	粒度分布/nm	平均粒径/nm	形貌,团聚程度
50:1	68~106, 531~1 100	803	块状+粒状,微团聚
100:1	459~712	565	块状+粒状,微团聚
150:1	59~79	68	粒状,无团聚
300:1	122~220	159	粒状,微团聚

固液比	粒度分布/nm	平均粒径/nm	形貌,团聚程度
1:0.5	531~1 010	681	粒状+块状,微团聚
1:1	59~79	68	粒状,无团聚
1:1.5	615~1 100	754	粒状+块状,团聚

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