反应条件对磷酸铁粒度分布的影响

doi:10.6040/j.issn.1672-3961.0.2014.196

山东大学学报(工学版) ›› 2015, Vol. 45 ›› Issue (1): 82-87.doi: 10.6040/j.issn.1672-3961.0.2014.196

反应条件对磷酸铁粒度分布的影响

骆艳华^1,2, 佘世杰², 曹卫国¹, 潘峰^1,3

1. 南京理工大学化工学院, 江苏南京 210094;
2. 中钢集团安徽天源科技股份有限公司, 安徽马鞍山 243000;
3. 国家民用爆破器材质量监督检验中心, 江苏南京 210094

收稿日期:2014-07-17 修回日期:2015-01-08 发布日期:2014-07-17
通讯作者: 潘峰(1971-),男,江苏南京人,副教授,博士,主要研究方向为电纺丝,超级电容器和锂电池等方面的研究与开发.E-mail:panfengiem@163.com E-mail:panfengiem@163.com
作者简介:骆艳华(1977-),女,河北衡水人,博士研究生,主要研究方向为无机材料研究与开发.E-mail:masbaowei@163.com
基金资助:
国家自然科学基金资助项目(51372117);江苏省公安基础研究基金资助项目(201201004TJ)

Effects of reaction conditions on the size distribution of iron phosphate

LUO Yanhua^1,2, SHE Shijie², CAO Weiguo¹, PAN Feng^1,3

1. School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, Jiangsu, China;
2. Anhui Tianyuan Technology Co. Ltd, Sinosteel Corporation, Maanshan 243000, Anhui, China;
3. National Quality Supervision and Inspection Center for Industrial Explosive Materials, Nanjing 210094, Jiangsu, China

Received:2014-07-17 Revised:2015-01-08 Published:2014-07-17

摘要/Abstract

摘要： 采用正交实验方法对乙醇体系中制备磷酸铁的工艺参数进行了优化分析,研究结果表明影响磷酸铁粒度分布的工艺参数主次顺序依次为乙醇的加入速度、反应温度和搅拌速度,且乙醇的加入速度是影响磷酸铁粒度分布的关键因素。当乙醇的加入速度为40 L/min,反应温度为90 ℃,搅拌速度为60 r/min时,制备磷酸铁的d₅₀为0.73 μm；当乙醇的加入速度为10 L/min,反应温度为50 ℃,搅拌速度为120 r/min时,制备的磷酸铁的d₅₀为2.10 μm。通过对磷酸铁进行SEM、BET和XRF分析,当d₅₀为0.73 μm时,比表面积大于60 m²/g;当d₅₀为2.10 μm时,比表面积约为45 m²/g,两种磷酸铁的磷铁物质的量比近似为1:1,当磷酸铁的粒度较细时,其杂质硫含量相对较高。

关键词: 乙醇, 硫含量, 磷酸铁, 正交实验, 粒径

Abstract: The process parameters of preparing iron phosphate in ethanol system were optimized by the method of orthogonal experiment. The results showed that the influencing order of the parameters affecting the particle size distribution of iron phosphate was ethanol addition rate, reaction temperature and stirring speed. The ethanol adding speed was the key factor to influence the size distribution of iron phosphate. When the addition of ethanol was 40 L/min, the reaction temperature was 90 ℃ and the stirring speed was 60 r/min, the d₅₀ of iron phosphate was 0.73 μm. When the addition of ethanol was 10 L/min, the reaction temperature was 50 ℃ and the stirring speed was 120 r/min, the d₅₀ of iron phosphate was 2.10 μm. The physical-chemical indicators of iron phosphate were charaterized by SEM, BET and XRF. When d₅₀ was 0.73 μm, the BET of iron phosphate was larger than 60 m²/g. When d₅₀ was 2.10 μm, the BET of iron phosphate was approximately 45 m²/g. The molar ratio of P and Fe of two kinds of iron phosphate was about 1:1. The content of sulfur was relatively high, when the particle size of iron phosphate was smaller.

Key words: ethanol, iron phosphate, orthogonal experiment, particle size, sulfur content

中图分类号:

O614.81

骆艳华, 佘世杰, 曹卫国, 潘峰. 反应条件对磷酸铁粒度分布的影响[J]. 山东大学学报(工学版), 2015, 45(1): 82-87.

LUO Yanhua, SHE Shijie, CAO Weiguo, PAN Feng. Effects of reaction conditions on the size distribution of iron phosphate[J]. JOURNAL OF SHANDONG UNIVERSITY (ENGINEERING SCIENCE), 2015, 45(1): 82-87.

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反应条件对磷酸铁粒度分布的影响

Effects of reaction conditions on the size distribution of iron phosphate

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