反应条件对磷酸铁粒度分布的影响

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。

Effects of reaction conditions on the size distribution of iron phosphate

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.