从镍钼矿冶炼渣中回收制备镍化合物的研究
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摘要
镍钼矿冶炼渣是镍钼矿提取钼的过程中产生的渣,含有镍等重金属以及稀有金属,具有一定的回收价值。其可以作为提取镍的原料。
本文研究的内容是采用“还原焙烧-硫酸浸出-净化-溶剂萃取”的工艺从镍钼矿冶炼渣中回收镍,对还原焙烧、硫酸浸出以及萃取回收镍的机理以及各种影响因素进行了研究。此外,还对制备氧化亚镍进行了研究。
研究数据表明：活性炭较粉煤、石墨对镍钼矿冶炼渣的还原性好。当还原焙烧的温度为850℃、焙烧时间为2h,活性炭的加入量为m活性炭：m干渣=1：2.5以及硫酸浸出时硫酸的浓度为4.5 mol/L,液固比为6：1,浸出时间为5h,浸出温度为80℃,双氧水(30%H2O2)的添加量为每克干渣0.6 ml时,镍的浸出率达到90.5%。浸出液经过氧化中和水解、硫化物沉淀、氟化物沉淀的方法除去铁、铜、钙、镁,以及PC-88A萃取除锌后,得到纯净的硫酸镍溶液。最佳的萃取和反萃条件是：有机相中PC-88A的添加量为30%(体积分数),萃取时料液的pH值为6.7,有机相与水相的相比O/A=1：3,萃取时间为3 min,萃取温度30℃；反萃时盐酸浓度为2 mol/L,有机相与水相的相比O/A=3：1,反萃时间为3 min,在此适宜条件下二级错流萃取镍的萃取率可达99.6%,一级反萃镍的反萃率可达99.3%。
本研究采用新的工艺来处理镍钼矿冶炼渣,使镍的浸出率以及回收率有了很大提高。为回收镍钼矿冶炼渣中的镍提供了一条新的途径。
Residue of metalliferous black shale was a residue of extracting molybdenum from metalliferous black shale. The residue contained many heavy metals and rare metals can be used as a raw material for extraction of nickel.
In this paper, extracting nickel from molybdenum leach residue of metalliferous black shale by the process of "reduction roasting-sulfuric acid leaching-purification-solvent extraction" was investigated. Moreover, the mechanism and parameters of reduction roasting, sulfuric acid leaching and solvent extraction on nickel recovery were studied. In addition, the method of preparation of high-purity nickel monoxide was also studied.
The results show that activated carbon was the most effective reductive agent for reduction roasting of the residue among activated carbon, pulverized coal and graphite. When the temperature of reduction roasting is 850℃; the time of reduction roasting is 2 h; the activated carbon dosage is mactivated carbon:mdry residue=1:2.5; as well as sulfuric acid leaching; when the concentration of sulfuric acid is 4.5 mol/L; liquid-solid ratio of 6:1; leaching time of 5 h; leaching temperature:80℃; adding amount 30% H2O20.6mi for 1g dry residue; the leaching rate of nickel is up to 90.5%. Oxidation and hydrolysis was used to reject iron; sulfide precipitation was chosen to remove copper; fluoride precipitation was adopted to remove calcium and magnesium and solvent extraction was used to remove zinc from leach liquor. Then, purged liquor was obtained. Optimum parameters of extraction and stripping were established as follows:adding PC-88A of 30%(Vpc-88A:Vorganic phase); pH value of feed solution of 6.7; organic phase to aqueous phase ratio of 1:3; phase contact time:3 min; extraction temperature:30℃; hydrochloric acid concentration:2 mol/L, organic phase to aqueous phase ratio of 3:1; phase contact time:3 min; under these experimental conditions, nickel extraction rate of is up to 99.6% under two step cross-current extraction and the extent of nickel stripping is up to 99.3% under one step stripping.
A new process was carried out to deal with the residue, so that the leaching rate of nickel and the recovery rate of nickel had been significantly improved. The process shows a new way of recovery nickel from the residue.
本文研究的内容是采用“还原焙烧-硫酸浸出-净化-溶剂萃取”的工艺从镍钼矿冶炼渣中回收镍,对还原焙烧、硫酸浸出以及萃取回收镍的机理以及各种影响因素进行了研究。此外,还对制备氧化亚镍进行了研究。
研究数据表明：活性炭较粉煤、石墨对镍钼矿冶炼渣的还原性好。当还原焙烧的温度为850℃、焙烧时间为2h,活性炭的加入量为m活性炭：m干渣=1：2.5以及硫酸浸出时硫酸的浓度为4.5 mol/L,液固比为6：1,浸出时间为5h,浸出温度为80℃,双氧水(30%H2O2)的添加量为每克干渣0.6 ml时,镍的浸出率达到90.5%。浸出液经过氧化中和水解、硫化物沉淀、氟化物沉淀的方法除去铁、铜、钙、镁,以及PC-88A萃取除锌后,得到纯净的硫酸镍溶液。最佳的萃取和反萃条件是：有机相中PC-88A的添加量为30%(体积分数),萃取时料液的pH值为6.7,有机相与水相的相比O/A=1：3,萃取时间为3 min,萃取温度30℃；反萃时盐酸浓度为2 mol/L,有机相与水相的相比O/A=3：1,反萃时间为3 min,在此适宜条件下二级错流萃取镍的萃取率可达99.6%,一级反萃镍的反萃率可达99.3%。
本研究采用新的工艺来处理镍钼矿冶炼渣,使镍的浸出率以及回收率有了很大提高。为回收镍钼矿冶炼渣中的镍提供了一条新的途径。
Residue of metalliferous black shale was a residue of extracting molybdenum from metalliferous black shale. The residue contained many heavy metals and rare metals can be used as a raw material for extraction of nickel.
In this paper, extracting nickel from molybdenum leach residue of metalliferous black shale by the process of "reduction roasting-sulfuric acid leaching-purification-solvent extraction" was investigated. Moreover, the mechanism and parameters of reduction roasting, sulfuric acid leaching and solvent extraction on nickel recovery were studied. In addition, the method of preparation of high-purity nickel monoxide was also studied.
The results show that activated carbon was the most effective reductive agent for reduction roasting of the residue among activated carbon, pulverized coal and graphite. When the temperature of reduction roasting is 850℃; the time of reduction roasting is 2 h; the activated carbon dosage is mactivated carbon:mdry residue=1:2.5; as well as sulfuric acid leaching; when the concentration of sulfuric acid is 4.5 mol/L; liquid-solid ratio of 6:1; leaching time of 5 h; leaching temperature:80℃; adding amount 30% H2O20.6mi for 1g dry residue; the leaching rate of nickel is up to 90.5%. Oxidation and hydrolysis was used to reject iron; sulfide precipitation was chosen to remove copper; fluoride precipitation was adopted to remove calcium and magnesium and solvent extraction was used to remove zinc from leach liquor. Then, purged liquor was obtained. Optimum parameters of extraction and stripping were established as follows:adding PC-88A of 30%(Vpc-88A:Vorganic phase); pH value of feed solution of 6.7; organic phase to aqueous phase ratio of 1:3; phase contact time:3 min; extraction temperature:30℃; hydrochloric acid concentration:2 mol/L, organic phase to aqueous phase ratio of 3:1; phase contact time:3 min; under these experimental conditions, nickel extraction rate of is up to 99.6% under two step cross-current extraction and the extent of nickel stripping is up to 99.3% under one step stripping.
A new process was carried out to deal with the residue, so that the leaching rate of nickel and the recovery rate of nickel had been significantly improved. The process shows a new way of recovery nickel from the residue.
引文
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