在三相流化床中NO_x全循环催化氧化预处理氰化尾渣的试验研究
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摘要
随着易处理金矿资源的日益消耗,难浸金矿和氰化尾渣的开发利用引起世界范围内的广泛关注。据统计,世界上80%的黄金冶炼企业采用氰化法提金,由此产生了大量的氰化尾渣,该尾渣含有可回收的金、银、铜、铅、锌、铁等有价金属元素。氰化尾渣的资源化,尤其是金、银、铁等元素的综合回收利用,不仅能消除氰化尾渣带来的环境污染,而且又能给炼金企业带来巨大经济效益,所以开发利用此类黄金资源具有十分重要的现实意义和长远意义。利用此类黄金资源最核心的内容是预处理方法的选择和运用,这将直接关系到不同元素的回收率,生产费用和环保等因素。
在查阅大量文献资料和本课题组原有研究的基础上,提出采用在三相流化床中NO_x全循环催化氧化预处理氰化尾渣。本研究以产自中原黄金冶炼厂的氰化尾渣为物料,以NO_x为氧化剂,考察了深度预处理过程中影响铁浸出率的主要因素,研究得出最佳的预处理条件为反应温度为75℃,反应时间为3.5小时,硝酸质量浓度分数为15%,硫酸质量浓度分数为5%,气速为0.5m~3/h,分布板孔径为1mm-2mm,孔与孔之间距离为4mm-7mm。试验结果表明,在此条件下,氰化尾渣中铁的浸出率达到97.92%,失重率达到58.73%,氧化效果非常明显。在同等条件下预处理难浸金矿,铁的浸出率达到95.29%,失重率达到72.68%,表明该方法也是预处理难浸金矿的有效方法。并对其氧化机理进行初步分析。
采用X射线衍射仪,LV扫描电子显微镜和X射线能谱仪对氰化尾渣和最佳工艺条件下预处理后的氧化渣分别进行X射线衍射,X射线线扫描和X射线面扫描微区分析和对比,得出该预处理方法能有效氧化黄铁矿,使包裹的金裸露出来,提高尾渣氰化提金率。把氰化尾渣和氧化渣在液固比5:1、PH=9-10、NaCN用量:2.0-3.0g/L、氰化时间为24h的条件下进行氰化提金,提金率从66.44%提高到99.39%。可见该预处理方法能够有效提高氰化提金率。
最后比较了NO_x循环利用和不循环对预处理氰化尾渣的影响,研究结果表明NO_x循环利用能节约大量硝酸,缓解液体中硝酸浓度下降,提高反应速率,缩短氧化时间。实现了低温常压下NO_x自循环。在此基础上进行了扩大三相流化床催化氧化实验,研究表明,间隔一定时间只补充少量的硝酸就能维持氧化反应连续进行,铁的浸出率持续提高。
本文所研究的预处理方法,预处理效果好,有效提高了氰化提金率,而且反应过程中实现NO_x全循环,减少了污染,符合环保节能减排的要求。但反应装置和材质需要进一步的研究和改进。
With increasingly exhausting of easily leachable gold ores,Developments of refractory gold ores and cyanide tailings have attracted extensive attention around the world.According to statistics,80%of the world's gold smelting enterprises to adopt cyaniding,resulting in a large number of cyanide tailings,the tailings contain recoverable gold,silver,copper,lead,zinc,iron and other valuable metal elements.These cyanide tailings are resourced,especially gold,silver, iron and other elements of a comprehensive recycling,it can eliminate the environmental pollution caused by cyanide tailings,but can bring tremendous economic benefits to the alchemical enterprise.It is practically Meaningful to explore better methods to utilize the refractory gold ores and cyanide tailings at present and in the future of china.Most important thing of developing this type of mineral is the choice and application of pretreatment method.This will directly relate to the recovery levels of different elements,cost,environmental protection and so on.
According to in checking a large number of documents and the original study of our research group,the innovation of retreating cyanide tailings by the way of the catalytic oxidation system that in a three-phase circulating fluidized-bed with NO_x-wide circulation.In this paper,the cyanide tailings from Zhongyuan Gold Smelter used as the test materials,and NO_x reagent as the oxidant,The factors affecting the pretreatment process were examined,the optimum condition was obtained by study under conditions:Pretreatment temperature is 75℃,oxygenation time is 3.5h, initial concentration of nitric acid is 15%,initial concentration of Sulfuric acid is 5%,gas velocity is 0.5m~3/h,aperture of distribution plate is 1mm-2mm,the distance between the hole and the hole for 4mm-7mm.The results show,on this condition,the leaching rate of Fe reached 94.25%and weight loss reached 55.82%,oxidation effect is very obvious.Under the same conditions, pretreatment of refractory gold,the leaching rate of Fe reached 95.29%and weight loss reached 72.68%,indicating that the method of pretreatment of refractory gold is an effective way.The oxidation mechanism of the reaction was analyzed preliminarily.
The X-ray diffraction(XRD),LV scanning electron microscopy(SEM) and Energy Dispersive Spectrometer(EDS) adapted to the cyanide tailings before and after the pretreatment respectively.Through analysis and comparison,this method of pretreatment is effective oxidation of pyrite,so that parcels out of gold exposed to enhance the rate of cyanide gold extraction.The cyanide tailings and oxide slag are cyanided gold under the conditions of the liquid-solid ratio 5:1, PH=9-10,NaCN dosage:2.0-3.0g/L,cyanide time for 24h,gold extraction rate from 66.44%to 99.39%.Can be seen that the pretreatment method to effectively improve the rate of cyanide gold extraction.
Finally,Comparison of NO_x recycling and does not cycle on the effects of pretreatment cyanide tailings,the results show that recycling can save a lot NO_x nitric acid,nitric acid concentration in the liquid down to ease and improve the reaction rate and shorten the oxidation time.NO_x is achieved with a self-loop at low temperature and Normal pressure.On this basis,the catalytic oxidation experiments have been enlarged scale in three-phase fluidized bed.The results show that would only add a small amount of nitric acid oxidation reaction can be to maintain continuous in a certain time interval,and the iron leaching rate continued to improve.
The pretreatment method studied in this paper,pretreatment effect is good,and effectively raise the rate of cyanide gold extraction.And the NO_x-wide circulation is achieved in reaction process;reduce pollution,environmentally friendly energy-saving emission reduction requirements.It is necessary to further study and improves the response equipment and the materials of equipment.
在查阅大量文献资料和本课题组原有研究的基础上,提出采用在三相流化床中NO_x全循环催化氧化预处理氰化尾渣。本研究以产自中原黄金冶炼厂的氰化尾渣为物料,以NO_x为氧化剂,考察了深度预处理过程中影响铁浸出率的主要因素,研究得出最佳的预处理条件为反应温度为75℃,反应时间为3.5小时,硝酸质量浓度分数为15%,硫酸质量浓度分数为5%,气速为0.5m~3/h,分布板孔径为1mm-2mm,孔与孔之间距离为4mm-7mm。试验结果表明,在此条件下,氰化尾渣中铁的浸出率达到97.92%,失重率达到58.73%,氧化效果非常明显。在同等条件下预处理难浸金矿,铁的浸出率达到95.29%,失重率达到72.68%,表明该方法也是预处理难浸金矿的有效方法。并对其氧化机理进行初步分析。
采用X射线衍射仪,LV扫描电子显微镜和X射线能谱仪对氰化尾渣和最佳工艺条件下预处理后的氧化渣分别进行X射线衍射,X射线线扫描和X射线面扫描微区分析和对比,得出该预处理方法能有效氧化黄铁矿,使包裹的金裸露出来,提高尾渣氰化提金率。把氰化尾渣和氧化渣在液固比5:1、PH=9-10、NaCN用量:2.0-3.0g/L、氰化时间为24h的条件下进行氰化提金,提金率从66.44%提高到99.39%。可见该预处理方法能够有效提高氰化提金率。
最后比较了NO_x循环利用和不循环对预处理氰化尾渣的影响,研究结果表明NO_x循环利用能节约大量硝酸,缓解液体中硝酸浓度下降,提高反应速率,缩短氧化时间。实现了低温常压下NO_x自循环。在此基础上进行了扩大三相流化床催化氧化实验,研究表明,间隔一定时间只补充少量的硝酸就能维持氧化反应连续进行,铁的浸出率持续提高。
本文所研究的预处理方法,预处理效果好,有效提高了氰化提金率,而且反应过程中实现NO_x全循环,减少了污染,符合环保节能减排的要求。但反应装置和材质需要进一步的研究和改进。
With increasingly exhausting of easily leachable gold ores,Developments of refractory gold ores and cyanide tailings have attracted extensive attention around the world.According to statistics,80%of the world's gold smelting enterprises to adopt cyaniding,resulting in a large number of cyanide tailings,the tailings contain recoverable gold,silver,copper,lead,zinc,iron and other valuable metal elements.These cyanide tailings are resourced,especially gold,silver, iron and other elements of a comprehensive recycling,it can eliminate the environmental pollution caused by cyanide tailings,but can bring tremendous economic benefits to the alchemical enterprise.It is practically Meaningful to explore better methods to utilize the refractory gold ores and cyanide tailings at present and in the future of china.Most important thing of developing this type of mineral is the choice and application of pretreatment method.This will directly relate to the recovery levels of different elements,cost,environmental protection and so on.
According to in checking a large number of documents and the original study of our research group,the innovation of retreating cyanide tailings by the way of the catalytic oxidation system that in a three-phase circulating fluidized-bed with NO_x-wide circulation.In this paper,the cyanide tailings from Zhongyuan Gold Smelter used as the test materials,and NO_x reagent as the oxidant,The factors affecting the pretreatment process were examined,the optimum condition was obtained by study under conditions:Pretreatment temperature is 75℃,oxygenation time is 3.5h, initial concentration of nitric acid is 15%,initial concentration of Sulfuric acid is 5%,gas velocity is 0.5m~3/h,aperture of distribution plate is 1mm-2mm,the distance between the hole and the hole for 4mm-7mm.The results show,on this condition,the leaching rate of Fe reached 94.25%and weight loss reached 55.82%,oxidation effect is very obvious.Under the same conditions, pretreatment of refractory gold,the leaching rate of Fe reached 95.29%and weight loss reached 72.68%,indicating that the method of pretreatment of refractory gold is an effective way.The oxidation mechanism of the reaction was analyzed preliminarily.
The X-ray diffraction(XRD),LV scanning electron microscopy(SEM) and Energy Dispersive Spectrometer(EDS) adapted to the cyanide tailings before and after the pretreatment respectively.Through analysis and comparison,this method of pretreatment is effective oxidation of pyrite,so that parcels out of gold exposed to enhance the rate of cyanide gold extraction.The cyanide tailings and oxide slag are cyanided gold under the conditions of the liquid-solid ratio 5:1, PH=9-10,NaCN dosage:2.0-3.0g/L,cyanide time for 24h,gold extraction rate from 66.44%to 99.39%.Can be seen that the pretreatment method to effectively improve the rate of cyanide gold extraction.
Finally,Comparison of NO_x recycling and does not cycle on the effects of pretreatment cyanide tailings,the results show that recycling can save a lot NO_x nitric acid,nitric acid concentration in the liquid down to ease and improve the reaction rate and shorten the oxidation time.NO_x is achieved with a self-loop at low temperature and Normal pressure.On this basis,the catalytic oxidation experiments have been enlarged scale in three-phase fluidized bed.The results show that would only add a small amount of nitric acid oxidation reaction can be to maintain continuous in a certain time interval,and the iron leaching rate continued to improve.
The pretreatment method studied in this paper,pretreatment effect is good,and effectively raise the rate of cyanide gold extraction.And the NO_x-wide circulation is achieved in reaction process;reduce pollution,environmentally friendly energy-saving emission reduction requirements.It is necessary to further study and improves the response equipment and the materials of equipment.
引文
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