黝铜矿型铜铅锌硫化矿浮选新药剂及其综合回收新工艺研究
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摘要
呷村铜铅锌多金属硫化矿富含黝铜矿,生产实践表明其分选困难。为提高该类资源的综合回收水平,本文首先对其矿石性质进行了工艺矿物学和密度泛函理论研究。工艺矿物学研究表明,由于呷村多金属硫化矿中各目的矿物呈微细粒状相互紧密镶嵌,导致其矿物单体解离较困难。密度泛函理论研究表明,相较黄铜矿铜的主要矿物-黝铜矿与方铅矿之间可浮性更接近,尤其是含铁杂质的黝铜矿与方铅矿之间很难浮选分离。可见针对该黝铜矿型铜铅锌硫化矿应用常规的浮选药剂和采用传统的全优先、部分混浮工艺很难取得令人满意的浮选分离效果,因此有必要展开新型高选择性捕收剂和浮选新工艺乃至选冶联合综合回收工艺的研究。
然后就呷村实际矿石进行了铜、铅浮选的捕收剂筛选,发现新型捕收齐EICTU(N-乙基-N’-异丙氧羰基硫脲)、BITCM(S-苄基-N-乙氧羰基硫氮酯)分别对呷村铜、铅矿物的捕收能力和选择性均相对最优。并在与矿物金属离子的络合作用和对单矿物的捕收性能及其在单矿物表面的吸附行为方面比较了新型捕收剂和常规药剂的浮选性能,进一步证实了EICTU、BITCM分别对铜、铅硫化矿物具有很强的捕收能力和最优的选择性。再采用密度泛函方法对各捕收剂分子的构效关系及EICTU、BTITCM在矿物表面的吸附机理进行了研究。构效关系方面通过分析各捕收剂分子的羰基硫原子共价键键长和Mulliken布居及捕收剂分子与矿物晶体之间的前线轨道能量匹配情况,同样可知EICTU、BITCM分别对铜、铅硫化矿物具有很强捕收能力和最优的选择性。吸附机理方面通过对EICTU、BITCM在矿物表面的吸附进行分子模拟,发现EICTU在黝铜矿、黄铜矿表面吸附BITCM在方铅矿表面吸附时,捕收剂分子的羰基S、羰基O分别与相应铜原子或铅原子分别生成正配键、反馈键而与之发生反应,由于反馈键作用相对较弱,正配键起主导作用；黝铜矿表面的锌、砷、银杂质缺陷对EICTU吸附的影响较小,而铁杂质缺陷明显不利于EICTU的吸附。
针对呷村黝铜矿型铜铅锌多金属硫化矿对各浮选工艺进行研究、比较发现,全优先浮选工艺有利于降低精矿互含,部分混合浮选工艺有利于银的回收,且这两种工艺结合EICTU和BITCM后,其浮选综合回收率均得到明显提升；以铜为主的铜铅等可浮选新工艺能在降低精矿互含损失的同时提高银的回收率,其与EICTU、BITCM相结合能最大限度地提高呷村多金属硫化矿的浮选综合回收率；在应用EICTU和BITCM的等可浮选闭路实验中,铜、铅、锌、银回收率分别为77.82%、71.83%、84.42%、79.11%,相较选厂现行药剂制度和流程下的浮选闭路实验结果,铜、铅、锌、银回收率分别提高了5.79%、7.91%、1.06%、8.34%,但该工艺的铜精矿和铅精矿1的互含损失仍然严重,因此有必要针对等可浮选铜铅混合精矿采用冶炼方法替代浮选进行分离。
对等可浮选铜铅混合精矿进行两段逆流氧压酸浸工艺的研究发现,该工艺的Cu、Zn浸出率分别高达96.30%、97.37%,杂质元素Fe、As、Sb浸出率分别低至15.23%、6.20%、0.50%,且Pb、Ag基本上不被浸出,铜、锌与铅银分离较彻底。等可浮选-氧压酸浸综合回收新工艺的铜、铅、锌、银综合回收率分别高达82.94%、80.05%、90.40%、79.11%,相较应用EICTU、BITCM的单一的等可浮选工艺,铜、铅、锌回收率分别提高5.12%、8.22%、5.98%,银回收率不受影响。该工艺的资源综合回收率较高,且具有冶炼规模小、流程短等优点,故本文针对黝铜矿型铜铅锌多金属硫化矿最终推荐采用结合应用EICTU、BITCM的等可浮选与铜铅混合精矿氧压酸浸的选冶联合综合回收新工艺。图107幅,表53个,参考文献158篇
Gacun Cu-Pb-Zn polymetallic sulfide ore is rich in tetrahedrite, and productive practice has shown that its flotation separation is very difficult. In order to improve the comprehensive recovery of this kind of resource, the studies of process mineralogy and density functional theory were done first to understand the ore property in this thesis. The research result of the process mineralogy showed that mineral liberation of the ore is difficult because its minerals inlay closely each other and furthermore their particle sizes are so fine. And the research result of the density functional theory showed that the flotation separation between tetrahedrite, which is the primary Cu mineral in Gacun mine, and galena is more difficult than the separation between chalcopyrite and galena, and the floatability of impure tetrahedrite bearing iron is especially close to galena. It is thus clear that the flotation separation indexes of this tetrahedrite type Cu-Pb-Zn sulfide ore will be unsatisfactory if only routine flotation reagents and conventional processes such as differential flotation or partial bulk flotation are applied, so that the studies of new collectors, new flotation process and even beneficiation-metallurgy combination process are necessary.
Afterward, the screening experiments of Cu collectors and Lead collectors with the Gacun raw ore were done, and experiment results showed that both of collecting capabilities and selectivities of the two new-type collectors named EICTU (N-ethyl-N'-isopropoxycarbonyl thiourea) and BITCM (S-benzyl-N-ethoxycarbonyl dithiocarbamate) are respectively optimal for Cu and Pb. It was confirmed by the comparison of collectors'complexations with metal ions, collection performances with pure natural minerals and adsorption behaviors on the surfaces of the pure minerals that the selectivities of EICUT for copper and BITCM for lead are both superior to routine collectors, and furthermore the collecting capabilities of the two new-type collectors are also excellent. And then the researches of structure-activity relationships of collectors and the microscopic mechanisms on atomic level how EICTU and BITCM absorb on mineral surfaces were done with density functional method. On the aspect of structure-activity relationship, the analysises of bond lengths of carbonyl S atoms and Mulliken populations of collector molecules and the energy matching of frontier molecular orbitals between collector molecules and mineral crystals have been done, and the results showed again that both of selectivities and collecting capabilities of EICUT and BITCM are separately excellent for Cu and Pb. On the aspect of adsorption mechanism, the adsorptions of EICTU and BITCM molecules on mineral crystal surfaces were simulated, and the research results showed that when an EICTU molecule adsorbs on the surface of tetrahedrite or chalcopyrite or when a BITCM molecule adsorbs on galena surface, carbonyl S and carbonyl O of the collector react with corresponding Cu atoms or Pb atoms and yield respectively normal covalent bonding and back donating bonding and furthermore normal covalent bonding take leading role, and the effects of Zn, As, Ag impurities in tetrahedrite surface on EICTU's adsorption are negligible but Fe impurity is obvious disadvantage for the adsorption.
Three kinds of flotation processes were studied contrastively with Gacun Cu-Pb-Zn polymetallic sulfide ore, and the result showed that differential flotation is beneficial to decrease dirtpercentages of concentrate products whilst partial bulk flotation is helpful to recover silver, and the performaces of the both two prossces were improved distinctly after their combination with EICTU and BITCM, while the new process, Cu-Pb iso-flotation emphasizing on Cu, is able to decrease dirtpercentages of concentrates and increase the Ag recovery simultaneously. The iso-flotation combined with EICTU and BITCM is able to improve furthest the flotation comprehensive recovery of Gacun polymetallic sulfide ore. The percent recoveries of Cu, Pb, Zn and Ag were respectively77.82%,71.83%,84.42%and79.11%in the closed-circuit test of this new process combined with the two new-type collectors, and the recoveries of these metals were raised separately5.79%,7.91%,1.06%and8.34%than the result of the closed-circuit test whose reagent regime and process flow were exactly the same as Gacun dressing plant. But the flotation separation indexes of Cu-Pb bulk concentrate of iso-flotation were still unsatisfactory, so that it is necessary that the flotation is substituted by certain a befitting metallurgical method for a more thorough separation of the bulk concentrate.
The experimental investigation of two stage oxygen pressure acid leaching of iso-flotation Cu-Pb bulk concentrate showed that the extraction ratios of Cu and Zn were as high as96.30%and97.37%, while the extraction ratios of impurities such as Fe, As and Sb were as low as15.23%,6.20%and0.50%, and furthermore Pb and Ag weren't extracted basically, so Cu and Zn can be separated with Pb and Ag relatively thoroughly by this process. The comprehensive recoveries of Cu, Pb, Zn and Ag of the iso-flotation-oxygen pressure acid leaching process were respectively as high as82.94%,80.05%,90.40%and79.11%, and the recoveries of Cu, Pb and Zn were raised separately5.12%,8.22%and5.98%whilst Ag recovery stayed the same compared with the single iso-flotation. The benefication-metallurgy combination new process combining iso-flotation and oxygen pressure acid leaching was recommended in the end for the tetrahedrite type Cu-Pb-Zn polymetallic sulfide ore, because that the comprehensive recoveries of this process are high whilst its metallurgical scale is small and process flow is short.
然后就呷村实际矿石进行了铜、铅浮选的捕收剂筛选,发现新型捕收齐EICTU(N-乙基-N’-异丙氧羰基硫脲)、BITCM(S-苄基-N-乙氧羰基硫氮酯)分别对呷村铜、铅矿物的捕收能力和选择性均相对最优。并在与矿物金属离子的络合作用和对单矿物的捕收性能及其在单矿物表面的吸附行为方面比较了新型捕收剂和常规药剂的浮选性能,进一步证实了EICTU、BITCM分别对铜、铅硫化矿物具有很强的捕收能力和最优的选择性。再采用密度泛函方法对各捕收剂分子的构效关系及EICTU、BTITCM在矿物表面的吸附机理进行了研究。构效关系方面通过分析各捕收剂分子的羰基硫原子共价键键长和Mulliken布居及捕收剂分子与矿物晶体之间的前线轨道能量匹配情况,同样可知EICTU、BITCM分别对铜、铅硫化矿物具有很强捕收能力和最优的选择性。吸附机理方面通过对EICTU、BITCM在矿物表面的吸附进行分子模拟,发现EICTU在黝铜矿、黄铜矿表面吸附BITCM在方铅矿表面吸附时,捕收剂分子的羰基S、羰基O分别与相应铜原子或铅原子分别生成正配键、反馈键而与之发生反应,由于反馈键作用相对较弱,正配键起主导作用；黝铜矿表面的锌、砷、银杂质缺陷对EICTU吸附的影响较小,而铁杂质缺陷明显不利于EICTU的吸附。
针对呷村黝铜矿型铜铅锌多金属硫化矿对各浮选工艺进行研究、比较发现,全优先浮选工艺有利于降低精矿互含,部分混合浮选工艺有利于银的回收,且这两种工艺结合EICTU和BITCM后,其浮选综合回收率均得到明显提升；以铜为主的铜铅等可浮选新工艺能在降低精矿互含损失的同时提高银的回收率,其与EICTU、BITCM相结合能最大限度地提高呷村多金属硫化矿的浮选综合回收率；在应用EICTU和BITCM的等可浮选闭路实验中,铜、铅、锌、银回收率分别为77.82%、71.83%、84.42%、79.11%,相较选厂现行药剂制度和流程下的浮选闭路实验结果,铜、铅、锌、银回收率分别提高了5.79%、7.91%、1.06%、8.34%,但该工艺的铜精矿和铅精矿1的互含损失仍然严重,因此有必要针对等可浮选铜铅混合精矿采用冶炼方法替代浮选进行分离。
对等可浮选铜铅混合精矿进行两段逆流氧压酸浸工艺的研究发现,该工艺的Cu、Zn浸出率分别高达96.30%、97.37%,杂质元素Fe、As、Sb浸出率分别低至15.23%、6.20%、0.50%,且Pb、Ag基本上不被浸出,铜、锌与铅银分离较彻底。等可浮选-氧压酸浸综合回收新工艺的铜、铅、锌、银综合回收率分别高达82.94%、80.05%、90.40%、79.11%,相较应用EICTU、BITCM的单一的等可浮选工艺,铜、铅、锌回收率分别提高5.12%、8.22%、5.98%,银回收率不受影响。该工艺的资源综合回收率较高,且具有冶炼规模小、流程短等优点,故本文针对黝铜矿型铜铅锌多金属硫化矿最终推荐采用结合应用EICTU、BITCM的等可浮选与铜铅混合精矿氧压酸浸的选冶联合综合回收新工艺。图107幅,表53个,参考文献158篇
Gacun Cu-Pb-Zn polymetallic sulfide ore is rich in tetrahedrite, and productive practice has shown that its flotation separation is very difficult. In order to improve the comprehensive recovery of this kind of resource, the studies of process mineralogy and density functional theory were done first to understand the ore property in this thesis. The research result of the process mineralogy showed that mineral liberation of the ore is difficult because its minerals inlay closely each other and furthermore their particle sizes are so fine. And the research result of the density functional theory showed that the flotation separation between tetrahedrite, which is the primary Cu mineral in Gacun mine, and galena is more difficult than the separation between chalcopyrite and galena, and the floatability of impure tetrahedrite bearing iron is especially close to galena. It is thus clear that the flotation separation indexes of this tetrahedrite type Cu-Pb-Zn sulfide ore will be unsatisfactory if only routine flotation reagents and conventional processes such as differential flotation or partial bulk flotation are applied, so that the studies of new collectors, new flotation process and even beneficiation-metallurgy combination process are necessary.
Afterward, the screening experiments of Cu collectors and Lead collectors with the Gacun raw ore were done, and experiment results showed that both of collecting capabilities and selectivities of the two new-type collectors named EICTU (N-ethyl-N'-isopropoxycarbonyl thiourea) and BITCM (S-benzyl-N-ethoxycarbonyl dithiocarbamate) are respectively optimal for Cu and Pb. It was confirmed by the comparison of collectors'complexations with metal ions, collection performances with pure natural minerals and adsorption behaviors on the surfaces of the pure minerals that the selectivities of EICUT for copper and BITCM for lead are both superior to routine collectors, and furthermore the collecting capabilities of the two new-type collectors are also excellent. And then the researches of structure-activity relationships of collectors and the microscopic mechanisms on atomic level how EICTU and BITCM absorb on mineral surfaces were done with density functional method. On the aspect of structure-activity relationship, the analysises of bond lengths of carbonyl S atoms and Mulliken populations of collector molecules and the energy matching of frontier molecular orbitals between collector molecules and mineral crystals have been done, and the results showed again that both of selectivities and collecting capabilities of EICUT and BITCM are separately excellent for Cu and Pb. On the aspect of adsorption mechanism, the adsorptions of EICTU and BITCM molecules on mineral crystal surfaces were simulated, and the research results showed that when an EICTU molecule adsorbs on the surface of tetrahedrite or chalcopyrite or when a BITCM molecule adsorbs on galena surface, carbonyl S and carbonyl O of the collector react with corresponding Cu atoms or Pb atoms and yield respectively normal covalent bonding and back donating bonding and furthermore normal covalent bonding take leading role, and the effects of Zn, As, Ag impurities in tetrahedrite surface on EICTU's adsorption are negligible but Fe impurity is obvious disadvantage for the adsorption.
Three kinds of flotation processes were studied contrastively with Gacun Cu-Pb-Zn polymetallic sulfide ore, and the result showed that differential flotation is beneficial to decrease dirtpercentages of concentrate products whilst partial bulk flotation is helpful to recover silver, and the performaces of the both two prossces were improved distinctly after their combination with EICTU and BITCM, while the new process, Cu-Pb iso-flotation emphasizing on Cu, is able to decrease dirtpercentages of concentrates and increase the Ag recovery simultaneously. The iso-flotation combined with EICTU and BITCM is able to improve furthest the flotation comprehensive recovery of Gacun polymetallic sulfide ore. The percent recoveries of Cu, Pb, Zn and Ag were respectively77.82%,71.83%,84.42%and79.11%in the closed-circuit test of this new process combined with the two new-type collectors, and the recoveries of these metals were raised separately5.79%,7.91%,1.06%and8.34%than the result of the closed-circuit test whose reagent regime and process flow were exactly the same as Gacun dressing plant. But the flotation separation indexes of Cu-Pb bulk concentrate of iso-flotation were still unsatisfactory, so that it is necessary that the flotation is substituted by certain a befitting metallurgical method for a more thorough separation of the bulk concentrate.
The experimental investigation of two stage oxygen pressure acid leaching of iso-flotation Cu-Pb bulk concentrate showed that the extraction ratios of Cu and Zn were as high as96.30%and97.37%, while the extraction ratios of impurities such as Fe, As and Sb were as low as15.23%,6.20%and0.50%, and furthermore Pb and Ag weren't extracted basically, so Cu and Zn can be separated with Pb and Ag relatively thoroughly by this process. The comprehensive recoveries of Cu, Pb, Zn and Ag of the iso-flotation-oxygen pressure acid leaching process were respectively as high as82.94%,80.05%,90.40%and79.11%, and the recoveries of Cu, Pb and Zn were raised separately5.12%,8.22%and5.98%whilst Ag recovery stayed the same compared with the single iso-flotation. The benefication-metallurgy combination new process combining iso-flotation and oxygen pressure acid leaching was recommended in the end for the tetrahedrite type Cu-Pb-Zn polymetallic sulfide ore, because that the comprehensive recoveries of this process are high whilst its metallurgical scale is small and process flow is short.
引文
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