湿法炼锌赤铁矿渣制备透明氧化铁颜料的研究
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摘要
湿法炼锌赤铁矿渣的综合利用既能作为二次资源再次利用,又能减少湿法炼锌赤铁矿渣对环境所造成的污染。利用湿法炼锌赤铁矿渣制备得到的化学纯级别的绿矾来制备性能优良的透明氧化铁颜料,这对于湿法炼锌赤铁矿渣的综合利用开辟了一种新的途径。
本研究以湿法炼锌赤铁矿渣为原料,先通过热酸浸出、净化、还原、结晶等工艺步骤,制得化学纯级别的绿矾,然后以此为原料,用空气氧化法,成功制备出基本满足质量要求的透明氧化铁颜料。与传统的空气氧化法不同的是,本研究只用一次氧化直接得到透明氧化铁产品,而不需要制备晶种和二次氧化。因此反应所需的设备和工艺都得到了简化,易于工业实践,降低了成本。
以赤铁矿渣为原料来制备绿矾关键在热酸浸出和净化两个过程。在热酸浸出阶段,通过各种主要金属(Fe、Zn、Pb)的电位-pH图来确定酸浸的条件;在净化阶段,通过各种离子(Fe、Zn、Mn、Mg、Cu)沉淀的pH不同,来除去杂质,以得到纯净的绿矾。结果表明,最佳的浸出条件为:酸浸温度:80℃、酸浸时间:2.5h、硫酸过量系数:1.20。净化阶段,控制溶液pH为4.1可以将Fe~(3+)沉淀,与其他离子分离。
透明氧化铁黄的制备的关键分为沉铁和氧化两部分。在沉铁阶段,研究了以NaOH为沉淀剂,同时鼓入氮气,生成Fe(OH)_2,并探讨了Fe~(2+)初始浓度、碱比、添加剂用量、温度等对最终产品的影响;在氧化阶段,鼓入空气进行氧化,并探讨了氧化温度、氧化时间、搅拌速度等条件对产品的影响。实验结果表明最佳工艺条件为:Fe~(2+)初始浓度C_2 mol/L、碱比R=1.5、分散剂Y_B用量为七水合硫酸亚铁用量的0.16%;沉铁:温度22～25℃、搅拌速度250r/min、FeSO_4溶液向NaOH溶液的滴加速度为3.3ml/min;氧化:氧化温度28～30℃、搅拌速度750r/min、空气鼓入速度为3.5L/min、氧化时间为1.5h;表面处理:表面活性剂A用量为料浆中铁黄颜料量的20～30%、温度为常温、处理时间1h。
透明氧化铁黄在350℃煅烧得到透明氧化铁红。
本研究所制得的透明氧化铁黄产品形貌为纺锤形,长轴约95nm,短轴约26nm,轴比为3.7,基本达到透明氧化铁颜料的质量要求。
The comprehensive utilization of hydrometallurgy zinc hematite residues can not only reclaim the resources but also control the cinders pollution. Transparent iron oxide pigments have been made from high quality FeSO_4·7H_2O . This can open up a new way of the comprehensive utilization of hydrometallurgy zinc hematite residues.
In this study, hydrometallurgy zinc hematite residues is used as raw materials, FeSO_2·7H_2O is made through the process of sulfuric acid pickling, purifying, reduction and crystallizing. Transparent iron oxide pigments which have been made by air oxidation method achieve the quality requirements. In this study use the direct oxidation to get transparent iron oxide, without the need for preparation of the seed and secondary oxidation,which is different from traditional methods. Therefore, the necessary equipment and processes have been simplified, easy to be applied in industry, and the cost has been reduced.
The key two parts of the preparation of copperas from hydrometallurgy zinc hematite residues are sulfuric acid pickling and purifying. In sulfuric acid pickling stage, use the E-pH diagram of major metals (Fe, Zn, Pb) to determine the conditions of sulfuric acid pickling. In purifying stage, use the difference of precipitation pH of the metals (Fe, Zn, Mn, Mg, Cu) to remove the impurities, so as to obtain copperas. The results show that the optimum conditions are as follows: sulfuric acid pickling stage,reaction temperature: 80℃、reaction time: 2.5h、vitriol excess coefficient: 1.20; purifying stage, keeping the pH at 4.1 can make Fe~(3+) precipitate out, and separated from other ions.
The key of preparation of transparent yellow iron oxide is divided into two parts, iron precipitation and oxidation. In the stage of iron precipitation, studied NaOH as the precipitant,at the same time, blowned nitrogen to prepare Fe(OH)_2,and explored the effects of Fe~(2+) initial concentration, alkali ratio, the amount of additives and temperature on the products. In the oxidation stage, explored the effects of oxidation temperature and oxidation time, mixing speed on the products. The results show that,the optimum conditions are:initial concentration of Fe is C_2 mol/L, alkali ratio is 1.5, the quantity of dispersant Y_B is 0.16% of FeSO_4.7H_2O amount;iron precipitation stage: temperature 22-25℃, stirring speed 250r/min, FeSO_4 solution dropping to NaOH solution at the speed of 3.3ml/min; oxidation stage: temperature 28-30℃, stirring speed 750r/min, flow velocity of oxygen 3.5L/min, oxidation time 1.5h ;surface treatment stage: quantity of A is 20%-30% of transparent iron oxide pigments amount, at room temperature for the temperature, reaction time 1h.
Transparent yellow iron oxide calcined at 350℃can get transparent red iron oxide.
The pigment in this research is the shape of the spindle, major axis is about 95nm, minor axis is about 26nm, axis ratio is about 3.7, which achieve the quality requirements.
本研究以湿法炼锌赤铁矿渣为原料,先通过热酸浸出、净化、还原、结晶等工艺步骤,制得化学纯级别的绿矾,然后以此为原料,用空气氧化法,成功制备出基本满足质量要求的透明氧化铁颜料。与传统的空气氧化法不同的是,本研究只用一次氧化直接得到透明氧化铁产品,而不需要制备晶种和二次氧化。因此反应所需的设备和工艺都得到了简化,易于工业实践,降低了成本。
以赤铁矿渣为原料来制备绿矾关键在热酸浸出和净化两个过程。在热酸浸出阶段,通过各种主要金属(Fe、Zn、Pb)的电位-pH图来确定酸浸的条件;在净化阶段,通过各种离子(Fe、Zn、Mn、Mg、Cu)沉淀的pH不同,来除去杂质,以得到纯净的绿矾。结果表明,最佳的浸出条件为:酸浸温度:80℃、酸浸时间:2.5h、硫酸过量系数:1.20。净化阶段,控制溶液pH为4.1可以将Fe~(3+)沉淀,与其他离子分离。
透明氧化铁黄的制备的关键分为沉铁和氧化两部分。在沉铁阶段,研究了以NaOH为沉淀剂,同时鼓入氮气,生成Fe(OH)_2,并探讨了Fe~(2+)初始浓度、碱比、添加剂用量、温度等对最终产品的影响;在氧化阶段,鼓入空气进行氧化,并探讨了氧化温度、氧化时间、搅拌速度等条件对产品的影响。实验结果表明最佳工艺条件为:Fe~(2+)初始浓度C_2 mol/L、碱比R=1.5、分散剂Y_B用量为七水合硫酸亚铁用量的0.16%;沉铁:温度22～25℃、搅拌速度250r/min、FeSO_4溶液向NaOH溶液的滴加速度为3.3ml/min;氧化:氧化温度28～30℃、搅拌速度750r/min、空气鼓入速度为3.5L/min、氧化时间为1.5h;表面处理:表面活性剂A用量为料浆中铁黄颜料量的20～30%、温度为常温、处理时间1h。
透明氧化铁黄在350℃煅烧得到透明氧化铁红。
本研究所制得的透明氧化铁黄产品形貌为纺锤形,长轴约95nm,短轴约26nm,轴比为3.7,基本达到透明氧化铁颜料的质量要求。
The comprehensive utilization of hydrometallurgy zinc hematite residues can not only reclaim the resources but also control the cinders pollution. Transparent iron oxide pigments have been made from high quality FeSO_4·7H_2O . This can open up a new way of the comprehensive utilization of hydrometallurgy zinc hematite residues.
In this study, hydrometallurgy zinc hematite residues is used as raw materials, FeSO_2·7H_2O is made through the process of sulfuric acid pickling, purifying, reduction and crystallizing. Transparent iron oxide pigments which have been made by air oxidation method achieve the quality requirements. In this study use the direct oxidation to get transparent iron oxide, without the need for preparation of the seed and secondary oxidation,which is different from traditional methods. Therefore, the necessary equipment and processes have been simplified, easy to be applied in industry, and the cost has been reduced.
The key two parts of the preparation of copperas from hydrometallurgy zinc hematite residues are sulfuric acid pickling and purifying. In sulfuric acid pickling stage, use the E-pH diagram of major metals (Fe, Zn, Pb) to determine the conditions of sulfuric acid pickling. In purifying stage, use the difference of precipitation pH of the metals (Fe, Zn, Mn, Mg, Cu) to remove the impurities, so as to obtain copperas. The results show that the optimum conditions are as follows: sulfuric acid pickling stage,reaction temperature: 80℃、reaction time: 2.5h、vitriol excess coefficient: 1.20; purifying stage, keeping the pH at 4.1 can make Fe~(3+) precipitate out, and separated from other ions.
The key of preparation of transparent yellow iron oxide is divided into two parts, iron precipitation and oxidation. In the stage of iron precipitation, studied NaOH as the precipitant,at the same time, blowned nitrogen to prepare Fe(OH)_2,and explored the effects of Fe~(2+) initial concentration, alkali ratio, the amount of additives and temperature on the products. In the oxidation stage, explored the effects of oxidation temperature and oxidation time, mixing speed on the products. The results show that,the optimum conditions are:initial concentration of Fe is C_2 mol/L, alkali ratio is 1.5, the quantity of dispersant Y_B is 0.16% of FeSO_4.7H_2O amount;iron precipitation stage: temperature 22-25℃, stirring speed 250r/min, FeSO_4 solution dropping to NaOH solution at the speed of 3.3ml/min; oxidation stage: temperature 28-30℃, stirring speed 750r/min, flow velocity of oxygen 3.5L/min, oxidation time 1.5h ;surface treatment stage: quantity of A is 20%-30% of transparent iron oxide pigments amount, at room temperature for the temperature, reaction time 1h.
Transparent yellow iron oxide calcined at 350℃can get transparent red iron oxide.
The pigment in this research is the shape of the spindle, major axis is about 95nm, minor axis is about 26nm, axis ratio is about 3.7, which achieve the quality requirements.
引文
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