铬渣解毒与氧化铬清洁制备工艺的研究
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摘要
铬盐是无机盐行业主要产品之一,在国民经济中具有重要作用。铬盐广泛应用于电镀、鞣革、印染、医药、颜料、催化剂、氧化剂及金属缓蚀剂等方面。而铬盐工业也是一个重污染行业,其污染主要源于固体危险废物,主要固体危险废物有铬渣和含Cr(Ⅵ)硫酸盐。铬渣是铬盐生产中的熟料经水浸出所得到的高碱残渣,是铬盐工业第一大公害；含Cr(Ⅵ)硫酸盐是铬盐制备过程中所产生的硫酸钠和硫酸氢钠,是铬盐工业的第二大公害。
铬盐的生产是从铬铁矿的焙烧开始的。铬铁矿的焙烧主要有钙焙烧法和无钙焙烧法两种。有钙焙烧法的主要缺点是铬渣量多,且难以解毒或利用,而无钙焙烧法可以避免上述缺点。虽然我国铬盐生产未来发展方向是无钙焙烧法,但历年留下大量的待处理的铬渣,对环境构成严重污染。
目前,工业上生产氧化铬的方法主要有两种：重铬酸钠与硫酸铵热分解法和铬酸酐热分解法,主要存在硫酸消耗高、含Cr(Ⅵ)硫酸盐污染等问题。
因此,针对上述有钙铬渣和传统氧化铬工业所产生的含Cr(Ⅵ)硫酸盐污染问题,本文围绕铬渣解毒和氧化铬清洁制备工艺两大主题,对淀粉水热法解毒铬渣、制革污泥干法解毒铬渣、含氟废水湿法解毒铬渣和淀粉水热法、干法制备氧化铬的相关基础理论和技术进行了系统的研究。研究表明：
含Cr(Ⅵ)针状钙矾石的生成是导致含硫物质常温湿法解毒铬渣不彻底的主要原因。本文在硫酸浸出铬渣热力学分析过程中发现,温度的升高能有效抑制钙矾石的生成,并在实验中得到了验证。在所确定的实验条件下,淀粉水热法解毒后的铬渣达到了进入生活垃圾填埋场的标准。
在温度超过400℃时,制革污泥中的油脂和蛋白质等有机物会分解成一氧化碳和烃类有机物,能将铬渣中的Cr(Ⅵ)还原为Cr(Ⅲ),从而实现铬渣的解毒。在适宜的条件下,制革污泥干法解毒后的处理渣达到了进入生活垃圾填埋场的标准。
对氢氟酸浸出铬渣过程热力学、动力学和含氟废水解毒铬渣工艺进行分析和研究,发现氢氟酸和含氟废水也能够有效破坏铬渣中含Cr(Ⅵ)矿物和其它矿物的结构,将其中的Cr(Ⅵ)释放出来；铬渣中酸溶性Cr(Ⅵ)的浸出过程动力学可以用粒径不变的收缩未反应核模型来描述,其浸出过程为内扩散控制；柱浸和槽浸结果非常相似。用含氟废水浸出30d后,其浸出渣达到了进入一般工业垃圾填埋场标准。用硫酸亚铁溶液作还原剂,继续柱浸1d经含氟废水浸出60d后的柱浸渣,其还原渣达到了进入生活垃圾填埋场的标准。用硫酸亚铁作还原剂、氢氧化钙作沉淀剂处理含氟废水浸出液,处理后的废水Cr(Ⅵ)达到了国家污水排放标准。
对淀粉水热还原Cr(Ⅵ)过程动力学和水热法制备氧化铬进行了研究,表明淀粉水热还原Cr(Ⅵ)的动力学模型可以用等温、恒容、不可逆反应动力学模型来描述,且属化学反应控制；在所确定的实验条件下,Cr(Ⅵ)还原率达到98%以上,得到660-880nrn、粒度均匀的氧化铬粉体；通过添加表面活性剂,可以制得110-130nm的粒度均匀的球形的超细氧化铬粉体。
对淀粉干法还原Cr(Ⅵ)过程热力学和干法还原制备氧化铬进行分析和研究,发现干法还原Cr(Ⅵ)的还原产物因铬酸盐种类和温度的不同而不同。淀粉干法还原铬酸钠的还原产物为亚铬酸钠,而重铬酸钠的还原产物与温度有关。在温度低于550℃时,重铬酸钠的还原产物主要为氧化铬,随着反应温度的升高,还原产物由氧化铬逐渐过渡到亚铬酸钠,亦即,高温会导致氧化铬向亚铬酸钠转变。在所确定的实验条件下,Cr(Ⅵ)还原率达到98%以上,得到418-438nm形状不规则的超细氧化铬粉体。
Chromates, as one of the main products of inorganic chemicals, are widely used in many aspects such as electroplating, tannage, printing and dyeing, medicine, paint, catalyst, oxidant and metal inhibitor, playing a very important role in the national economy. However, the chromate industry produces a large amount of solid hazardous wastes mainly including chromite ore processing residue (COPR) and sulphates containing hexavalent chromium (Cr(Ⅵ)), which are the first and second hazard in the process, respectively.
Chromates production is beginned with the roasting process of chromite ore. There are two main processes for extracting chromate from chromite ore. One is the high lime roasting process characterised by large amount of COPR produced, and the other is the non-lime roasting process with less amount of COPR. The trends of chromates production is the non-lime roasting process in the future in China, but there is plenty of COPR to be treated in the past several decades.
There are also two processes for producing chromium oxide (Cr2O3): one is the pyrolysis of sodium dichromate and ammonium sulphate, and the other is pyrolysis of chromic anhydride (CrO3). Both processes have the problem of high consumption of sulphuric acid and produce hazardous material of suphates containing Cr(VI).
So this dissertation mainly focused on the theory and technology of COPR remediation with starch by hydrothermal process, with tannage sludge by pyrolysis process and with wastewater containing hydrofluoric acid. The theory and technology of clean production of Cr2O3was also investigated with starch by hydrothermal process and dry reduction process. The main argumentations and original conclusions were made as follows:
The formation of acicular ettringite bearing Cr(Ⅵ) was the main reason of incomplete remediation of COPR with sulphur-containing reductants in aqueous solution at the ambient temperature. The thermodynamic calculation showed that increasing temperature could effectively suppress ettringite formation, which was further verified by experimental results, subsequently. The COPR treated with starch by hydrothermal process could meet the standard of entering the landfill yard of household garbage under the optimized conditions.
Carbon monoxide and hydrocarbon organic compounds released from the decomposition of grease and protein of tannage sludge could reduce Cr(Ⅵ) in COPR to trivalent chromium (Cr(Ⅲ)) for the remediation of COPR at temperature of over400℃. And COPR treated with tannage sludge by pyrolysis process also met the standard of entering the landfill yard of household garbage.
Thermodynamic calculation and kinetic study of the leaching of COPR with hydrofluoric acid as well as the remediation technology of COPR with wastewater containing hydrofluoric acid were investigated in this work. Results showed that hydrofluoric acid and wastewater containing hydrofluoric acid could also destroy the structures of minerals containing Cr(Ⅵ), leading to release Cr(Ⅵ) in COPR. And the leaching kinetics of acidic Cr(Ⅵ) from COPR followed the shrinking unreacted core model and was controlled by inner diffusion. Results also showed that the remediation effect of column leaching was very close to that of the pond leaching. The COPR treated with wastewater containing hydrofluoric acid for30days met the standard of entering the landfill yard of general industrial wastes. And the COPR treated with wastewater containing hydrofluoric acid for60days by column leaching, further column leached by ferrous sulphate solution for1day, could meet the standard of entering the landfill yard of household garbage. In addition, the Cr(Ⅵ) content of the leachate treated with ferrous sulphate solution and calcium hydroxide reached the national sewage discharge standard.
The kinetics and technology of preparation of Cr2O3by hydrothermal process of Cr(Ⅵ) with starch as the reductant were also conducted. Results showed that the kinetics could be described by the kinetic model of isothermal irreversible reaction with constant volume, and the hydrothermal reduction was controlled by the chemical reaction. Homogeneously distributed Cr2O3powder with particle size of660-880nm was obtained with Cr(Ⅵ) reduction rate of more than98%by hydrothermal process. Furthermore, ultra-fine near-spherical or spherical Cr2O3powder with uniform size of110-130nm could be prepared by the application of surfactant in the hydrothermal process.
The thermodynamics and technology of preparation of Cr2O3by dry-process of Cr(Ⅵ) with starch were carried out. Results indicated that the reduction product varied with the kind of chromates and the reduction temperature. The reduction product of sodium chromate was sodium chromate(Ⅲ)(NaCrO2), while the reduction product of sodium dichromate depended on the temperature. Cr2O3was obtained with the reduction temperature of lower than550℃, and Cr2O3gradually tranformed to NaCrO2with increasing the reduction temperature. Irregular Cr2O3powder with the particle size of418-438nm was produced with the Cr(Ⅵ) reduction rate of above98%under the optimal conditions.
铬盐的生产是从铬铁矿的焙烧开始的。铬铁矿的焙烧主要有钙焙烧法和无钙焙烧法两种。有钙焙烧法的主要缺点是铬渣量多,且难以解毒或利用,而无钙焙烧法可以避免上述缺点。虽然我国铬盐生产未来发展方向是无钙焙烧法,但历年留下大量的待处理的铬渣,对环境构成严重污染。
目前,工业上生产氧化铬的方法主要有两种：重铬酸钠与硫酸铵热分解法和铬酸酐热分解法,主要存在硫酸消耗高、含Cr(Ⅵ)硫酸盐污染等问题。
因此,针对上述有钙铬渣和传统氧化铬工业所产生的含Cr(Ⅵ)硫酸盐污染问题,本文围绕铬渣解毒和氧化铬清洁制备工艺两大主题,对淀粉水热法解毒铬渣、制革污泥干法解毒铬渣、含氟废水湿法解毒铬渣和淀粉水热法、干法制备氧化铬的相关基础理论和技术进行了系统的研究。研究表明：
含Cr(Ⅵ)针状钙矾石的生成是导致含硫物质常温湿法解毒铬渣不彻底的主要原因。本文在硫酸浸出铬渣热力学分析过程中发现,温度的升高能有效抑制钙矾石的生成,并在实验中得到了验证。在所确定的实验条件下,淀粉水热法解毒后的铬渣达到了进入生活垃圾填埋场的标准。
在温度超过400℃时,制革污泥中的油脂和蛋白质等有机物会分解成一氧化碳和烃类有机物,能将铬渣中的Cr(Ⅵ)还原为Cr(Ⅲ),从而实现铬渣的解毒。在适宜的条件下,制革污泥干法解毒后的处理渣达到了进入生活垃圾填埋场的标准。
对氢氟酸浸出铬渣过程热力学、动力学和含氟废水解毒铬渣工艺进行分析和研究,发现氢氟酸和含氟废水也能够有效破坏铬渣中含Cr(Ⅵ)矿物和其它矿物的结构,将其中的Cr(Ⅵ)释放出来；铬渣中酸溶性Cr(Ⅵ)的浸出过程动力学可以用粒径不变的收缩未反应核模型来描述,其浸出过程为内扩散控制；柱浸和槽浸结果非常相似。用含氟废水浸出30d后,其浸出渣达到了进入一般工业垃圾填埋场标准。用硫酸亚铁溶液作还原剂,继续柱浸1d经含氟废水浸出60d后的柱浸渣,其还原渣达到了进入生活垃圾填埋场的标准。用硫酸亚铁作还原剂、氢氧化钙作沉淀剂处理含氟废水浸出液,处理后的废水Cr(Ⅵ)达到了国家污水排放标准。
对淀粉水热还原Cr(Ⅵ)过程动力学和水热法制备氧化铬进行了研究,表明淀粉水热还原Cr(Ⅵ)的动力学模型可以用等温、恒容、不可逆反应动力学模型来描述,且属化学反应控制；在所确定的实验条件下,Cr(Ⅵ)还原率达到98%以上,得到660-880nrn、粒度均匀的氧化铬粉体；通过添加表面活性剂,可以制得110-130nm的粒度均匀的球形的超细氧化铬粉体。
对淀粉干法还原Cr(Ⅵ)过程热力学和干法还原制备氧化铬进行分析和研究,发现干法还原Cr(Ⅵ)的还原产物因铬酸盐种类和温度的不同而不同。淀粉干法还原铬酸钠的还原产物为亚铬酸钠,而重铬酸钠的还原产物与温度有关。在温度低于550℃时,重铬酸钠的还原产物主要为氧化铬,随着反应温度的升高,还原产物由氧化铬逐渐过渡到亚铬酸钠,亦即,高温会导致氧化铬向亚铬酸钠转变。在所确定的实验条件下,Cr(Ⅵ)还原率达到98%以上,得到418-438nm形状不规则的超细氧化铬粉体。
Chromates, as one of the main products of inorganic chemicals, are widely used in many aspects such as electroplating, tannage, printing and dyeing, medicine, paint, catalyst, oxidant and metal inhibitor, playing a very important role in the national economy. However, the chromate industry produces a large amount of solid hazardous wastes mainly including chromite ore processing residue (COPR) and sulphates containing hexavalent chromium (Cr(Ⅵ)), which are the first and second hazard in the process, respectively.
Chromates production is beginned with the roasting process of chromite ore. There are two main processes for extracting chromate from chromite ore. One is the high lime roasting process characterised by large amount of COPR produced, and the other is the non-lime roasting process with less amount of COPR. The trends of chromates production is the non-lime roasting process in the future in China, but there is plenty of COPR to be treated in the past several decades.
There are also two processes for producing chromium oxide (Cr2O3): one is the pyrolysis of sodium dichromate and ammonium sulphate, and the other is pyrolysis of chromic anhydride (CrO3). Both processes have the problem of high consumption of sulphuric acid and produce hazardous material of suphates containing Cr(VI).
So this dissertation mainly focused on the theory and technology of COPR remediation with starch by hydrothermal process, with tannage sludge by pyrolysis process and with wastewater containing hydrofluoric acid. The theory and technology of clean production of Cr2O3was also investigated with starch by hydrothermal process and dry reduction process. The main argumentations and original conclusions were made as follows:
The formation of acicular ettringite bearing Cr(Ⅵ) was the main reason of incomplete remediation of COPR with sulphur-containing reductants in aqueous solution at the ambient temperature. The thermodynamic calculation showed that increasing temperature could effectively suppress ettringite formation, which was further verified by experimental results, subsequently. The COPR treated with starch by hydrothermal process could meet the standard of entering the landfill yard of household garbage under the optimized conditions.
Carbon monoxide and hydrocarbon organic compounds released from the decomposition of grease and protein of tannage sludge could reduce Cr(Ⅵ) in COPR to trivalent chromium (Cr(Ⅲ)) for the remediation of COPR at temperature of over400℃. And COPR treated with tannage sludge by pyrolysis process also met the standard of entering the landfill yard of household garbage.
Thermodynamic calculation and kinetic study of the leaching of COPR with hydrofluoric acid as well as the remediation technology of COPR with wastewater containing hydrofluoric acid were investigated in this work. Results showed that hydrofluoric acid and wastewater containing hydrofluoric acid could also destroy the structures of minerals containing Cr(Ⅵ), leading to release Cr(Ⅵ) in COPR. And the leaching kinetics of acidic Cr(Ⅵ) from COPR followed the shrinking unreacted core model and was controlled by inner diffusion. Results also showed that the remediation effect of column leaching was very close to that of the pond leaching. The COPR treated with wastewater containing hydrofluoric acid for30days met the standard of entering the landfill yard of general industrial wastes. And the COPR treated with wastewater containing hydrofluoric acid for60days by column leaching, further column leached by ferrous sulphate solution for1day, could meet the standard of entering the landfill yard of household garbage. In addition, the Cr(Ⅵ) content of the leachate treated with ferrous sulphate solution and calcium hydroxide reached the national sewage discharge standard.
The kinetics and technology of preparation of Cr2O3by hydrothermal process of Cr(Ⅵ) with starch as the reductant were also conducted. Results showed that the kinetics could be described by the kinetic model of isothermal irreversible reaction with constant volume, and the hydrothermal reduction was controlled by the chemical reaction. Homogeneously distributed Cr2O3powder with particle size of660-880nm was obtained with Cr(Ⅵ) reduction rate of more than98%by hydrothermal process. Furthermore, ultra-fine near-spherical or spherical Cr2O3powder with uniform size of110-130nm could be prepared by the application of surfactant in the hydrothermal process.
The thermodynamics and technology of preparation of Cr2O3by dry-process of Cr(Ⅵ) with starch were carried out. Results indicated that the reduction product varied with the kind of chromates and the reduction temperature. The reduction product of sodium chromate was sodium chromate(Ⅲ)(NaCrO2), while the reduction product of sodium dichromate depended on the temperature. Cr2O3was obtained with the reduction temperature of lower than550℃, and Cr2O3gradually tranformed to NaCrO2with increasing the reduction temperature. Irregular Cr2O3powder with the particle size of418-438nm was produced with the Cr(Ⅵ) reduction rate of above98%under the optimal conditions.
引文
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