锌电解阳极泥锰铅银分离的技术与理论研究
摘要
电解锌阳极泥是生产电解锌过程中产生的渣泥,是一种富含锰、铅、银等金属的二次资源。电解锌阳极泥作为氧化剂返回浸出作业可以实现锰资源的综合利用,但目前对于其中的铅银资源尚无行之有效的回收技术。本文在研究电解锌阳极泥物理化学性质的基础上,开发了“浮选-磁选-重选”联合选矿技术,实现了锰铅银矿物的分离富集与综合回收。通过对该矿浆体系进行系统深入的热力学分析,明确了锌阳极泥矿浆体系的电化学性质、组成元素的赋存状态及浮选剂的存在形式,并结合红外光谱分析、量子化学计算等研究手段,探讨了该矿浆体系中巯基捕收剂与矿物表面的作用机制。论文的主要研究内容与创新成果如下：
(1)锌阳极泥的物理化学性质与锰铅银矿物综合回收技术
锌阳极泥中含锰铅银等主要有价元素,其中锰主要以隐钾锰矿(KMn8O16)存在,铅以铅矾(PbSO4)存在,银以氯银矿(AgCl)、氧化银(Ag203)和一硝代八氧化七银(Ag7NO11)存在,锌阳极泥的矿浆为pH值低于5的酸性矿浆,矿浆中Mn2+的浓度为5.8×10-2mol.L-1。
巯基捕收剂对银矿物具有良好的选择性捕收作用,硫化浮选法无法实现锌阳极泥中的铅矾的富集。采用“浮选-磁选-重选”联合流程方案,可以实现电解锌阳极泥中锰铅银矿物的分离与富集。对于锰、铅、银品位分别为37.48%、21.54%和1628g/t的电解锌阳极泥,采用该技术,获得了含银48515g/t的浮选银精矿,含铅60.89%的铅精矿和含锰50.17%的锰精矿,铅在铅精矿和银精矿中的总回收率为84.78%,银在铅精矿和银精矿中的总回收率为74.71%,锰回收率达到91.86%。
(2)锌阳极泥矿浆体系的热力学分析
根据热力学数据计算绘制了各种体系的Eh-pH图,以此作为基础讨论锌阳极泥的背景矿浆电位及其对铅、银矿物赋存状态、巯基捕收剂存在形式、硫化-黄药浮选铅矾等的影响。热力学研究结果表明,锌阳极泥矿浆的电位受MnO2、Mn2+离子浓度和矿浆pH的控制,形成强氧化电位。在锌阳极泥背景矿浆电位下,铅的热力学稳定存在化合物为硫酸铅,银的热力学稳定存在化合物为单质Ag、Ag2O和AgCl等；矿浆中硫的热力学稳定产物不是S2-和SH-组分,而是S042-组分,因此,硫化钠和硫氢化钠会被氧化成S042-组分,不能实现对硫酸铅矿物表面的硫化改性；黄药、黑药、乙硫氮的热力学稳定产物分别为双黄药、双黑药和双乙硫氮,加入到锌阳极泥矿浆中的巯基捕收剂会被氧化为相应的二聚物。
(3)锌阳极泥矿浆中铅银矿物的浮选行为
硫酸铅与氯化银纯矿物浮选试验表明,以黄药和黑药为捕收剂,在pH3-7范围内,氯化银、硫酸铅可浮性良好,有二氧化锰存在体系氯化银仍保持较好的可浮性,但硫酸铅的浮选受到抑制。
双黄药和双黑药对氯化银有较强的捕收能力,而对硫酸铅捕收能力较差。红外光谱分析表明,在用硫酸调浆的pH=4的酸条件下,戊基双黄药和戊基双黑药在氯化银矿物表面发生明显吸附,而难以在硫酸铅表面吸附。
(4)锌阳极泥矿浆中含银矿物表面选择性吸附巯基捕收剂二聚氧化物的机理研究
根据元素的离子化势能和电子亲和能数据和半经验量子力学方法中的PM6计算了Mn4+、Pb2+、Ag+及巯基捕收剂二聚氧化物的前线轨道HOMO和LUMO的能量。比较Mn4+、Pb2+、Ag+电子空隙的最低未占分子轨道LUMO的能量与巯基捕收剂二聚氧化物的最高占据分子轨道HOMO的能量发现,巯基捕收剂二聚氧化物的HOMO的能量与Ag+的LUMO的能量非常接近,表明巯基捕收剂二聚氧化物与Ag+之间容易发生共价性配位健化学吸附。
采用Materials Studio软件的Adsorption Locater模块计算了氯化银、氧化银、硫酸铅、隐钾锰矿等四种矿物晶体吸附质与双黄药、双黑药、双乙硫氮分子、水分子、氢氧根离子、氯离子、硫酸根离子等吸附剂的作用能变化,结果表明,双黄药、双黑药、双乙硫氮分子等巯基捕收剂二聚氧化物无法吸附在隐钾锰矿表面,可以吸附在硫酸铅、氯化银、氧化银矿物表面,但在有硫酸根存在的条件下,上述巯基捕收剂二聚氧化物在氯化银、氧化银矿物表面仍然能发生吸附,而硫酸铅矿物表面对硫酸根离子的吸附比对上述巯基捕收剂二聚物的吸附强得多,表明双黄药、双黑药、双乙硫氮等巯基捕收剂二聚氧化物对含银矿物存在选择性吸附作用。
Zinc anode slime, a kind of residue produced in the process of zinc electrowinning, is a secondary resource abundant in manganese, lead and silver etc. The present method treating this residue in zinc ectrowinning plants is to return it to the leaching operation as an oxidant. It works well in reuse of manganese by not changing Mn(IV) to Mn(II), but fails to recycle lead and silver efficiently as early as possible. And there is no feasible and efficient technology till now which has done well in both of these two aspects. In this thesis, a combined beneficiation technology, including flotation, magnetic separation and gravity separation, to realize the separation of manganese, lead and silver, was developed based on the physicochemical property research. The electrochemical atmosphere background produced by Mn(IV) and Mn2+in the acidic pulp of this residue and its influence on the occurrence of lead, silver as well as thiol collectors were determined with a themodynamic method. The interaction mechanism of the of thiol collectors with lead and silver minerals in the pulp was investigated by means of infrared spectroscopic analysis, quantum chemical calculation and other research methods. The main research contents and innovations are as follows:
(1) Physicochemical properties of zinc anode slime and technology for comprehensive recovery of manganese, lead and silver minerals.
Zinc anode slime contains such major valuable elements as manganese, lead and silver, of which the main existing forms of metalliferous minerals are cryptomelane (KMn8O16) for Mn, anglesite (PbSO4) for Pb, and kerargyrite (AgCl), silver oxide (Ag2O3) and silver oxy-salt of nitrate (Ag7NO11) for Ag. The pulp of zinc anode slime is weakly acid, with pH below5, and the concentration of Mn2+is5.8×10-2mol.L-1.
Thiol collectors could only recover silver minerals from zinc anode slime. Flotation by xanthate after sulfidation could not recover anglesite from zinc anode slime. The combined flowsheet of "flotation-magnetic separation-gravity separation" performed very well to separate minerals of manganese, lead and silver respectively. By applying this technology, a silver concentrate with high silver grade,48515g/t, an anglesite concentrate containing lead60.89%, and a manganese concentrate with50.17%manganese could be obtained from zinc anode slime with grade of manganese, lead and silver being37.48%,21.54%and1628g/t, respectively. The total recovery of lead and silver in the lead and silver concentrates reached84.78%and74.71%respectively, and the manganese recovery is91.86%.
(2)Thermodynamic analysis of the pulp system of zinc anode mud
The Eh-pH diagrams for different systems have been drawn according to the themodynamically calculated data, based on which the background pulp potential of zinc anode slime and its influence on the occurrence of lead and silver components, the existing state of thiol collectors as well as the flotation of anglesite by xanthate after sulfidation, have been discussed. The results indicate that the pulp potential of zinc anode slime is mainly controlled by the MnO2, the concentration of Mn2+and the pH in the pulp, thus forming a strong oxidation atmosphere which called the background pulp potential of zinc anode slime. In this strong oxidation background pulp potential, lead mainly occurred as anglesite, silver can occurred as Ag, Ag2O, AgCl, AgO, Ag2O3, etc. The themodynamically stable products of sulfur in the pulp is not S2-, HS-, or S0, but SO42-, demonstrating that the sulfidation of anglesite by Na2S or NaHS cannot be achieved; The thermodynamically stable products of thiol collectors in zinc anode slime pulp are their corresponding oxidized dipolymers.
(3) The flotation behavior of lead and silver minerals in the pulp of zinc anode slime
Microflotation tests for pure minerals of anglesite and kerargyrite indicated that these two minerals have good floatability with thiol collectors such as xanthate and aerofloat, on the pH range of3-7. In the presence of MnO2, the floatability of kerargyrite maintains well but that of anglesite turns worse. Dixanthogen and bis-aerofloat have strong collecting ability to kerargyrite comparing with worse collecting ability to anglesite in the presence of SO42-. The infrared spectrum tests verified the selective adsorption of dixanthogen and bis-aerofloat on the surface of kerargyrite in the presence of SO42-.
(4) Mechanism of the selective adsorption of thiol collector oxidized dipolymers on the surface of silver containing minerals in zinc anode slime.
The highest occupied molecular orbit (HOMO) energy and the lowest unoccupied molecular orbit (LUMO) energy of Mn4+、Pb2+、Ag+have been calculated according to the ionization potential and electron affinity of element. The HOMO and LUMO energy of thiol collector oxidized dipolymers have been also calculated according to PM6in semiempirical quantum mechanics method. It's clearly shown by comparing the LUMO energy of Mn4+、Pb2+、Ag+with the HOMO energy of thiol collector oxidized dipolymers that the latter was close to the LUMO energy of Ag+, indicating that the covalent coordinated chemisorption of those thiol collector oxidized dipolymers on Ag+is prone to happen.
The changes of interaction energy between four kinds of mineral crystals (kerargyrite, silver oxide, anglesite and cryptomelane) and a variety of adsorbents (dixanthogen, bis-aerofloat, bis-diethyl dithiocarbamate, H2O, OH-, Cl-, SO42-) have been calculated by Material Studio(Adsorption Locater module). The results indicate that thiol collector oxidized dipolymers could not be adsorbed on the surface of cryptomelane. These thiol collector oxidized dipolymers could be adsorbed on the surface of anglesite, kerargyrite and silver oxide in the absence of SO42-. With the existence of SO42-, these collectors could only be adsorbed on the surface of silver minerals, due to the competive adsorption of SO42-on the surface of anglesite.
(1)锌阳极泥的物理化学性质与锰铅银矿物综合回收技术
锌阳极泥中含锰铅银等主要有价元素,其中锰主要以隐钾锰矿(KMn8O16)存在,铅以铅矾(PbSO4)存在,银以氯银矿(AgCl)、氧化银(Ag203)和一硝代八氧化七银(Ag7NO11)存在,锌阳极泥的矿浆为pH值低于5的酸性矿浆,矿浆中Mn2+的浓度为5.8×10-2mol.L-1。
巯基捕收剂对银矿物具有良好的选择性捕收作用,硫化浮选法无法实现锌阳极泥中的铅矾的富集。采用“浮选-磁选-重选”联合流程方案,可以实现电解锌阳极泥中锰铅银矿物的分离与富集。对于锰、铅、银品位分别为37.48%、21.54%和1628g/t的电解锌阳极泥,采用该技术,获得了含银48515g/t的浮选银精矿,含铅60.89%的铅精矿和含锰50.17%的锰精矿,铅在铅精矿和银精矿中的总回收率为84.78%,银在铅精矿和银精矿中的总回收率为74.71%,锰回收率达到91.86%。
(2)锌阳极泥矿浆体系的热力学分析
根据热力学数据计算绘制了各种体系的Eh-pH图,以此作为基础讨论锌阳极泥的背景矿浆电位及其对铅、银矿物赋存状态、巯基捕收剂存在形式、硫化-黄药浮选铅矾等的影响。热力学研究结果表明,锌阳极泥矿浆的电位受MnO2、Mn2+离子浓度和矿浆pH的控制,形成强氧化电位。在锌阳极泥背景矿浆电位下,铅的热力学稳定存在化合物为硫酸铅,银的热力学稳定存在化合物为单质Ag、Ag2O和AgCl等；矿浆中硫的热力学稳定产物不是S2-和SH-组分,而是S042-组分,因此,硫化钠和硫氢化钠会被氧化成S042-组分,不能实现对硫酸铅矿物表面的硫化改性；黄药、黑药、乙硫氮的热力学稳定产物分别为双黄药、双黑药和双乙硫氮,加入到锌阳极泥矿浆中的巯基捕收剂会被氧化为相应的二聚物。
(3)锌阳极泥矿浆中铅银矿物的浮选行为
硫酸铅与氯化银纯矿物浮选试验表明,以黄药和黑药为捕收剂,在pH3-7范围内,氯化银、硫酸铅可浮性良好,有二氧化锰存在体系氯化银仍保持较好的可浮性,但硫酸铅的浮选受到抑制。
双黄药和双黑药对氯化银有较强的捕收能力,而对硫酸铅捕收能力较差。红外光谱分析表明,在用硫酸调浆的pH=4的酸条件下,戊基双黄药和戊基双黑药在氯化银矿物表面发生明显吸附,而难以在硫酸铅表面吸附。
(4)锌阳极泥矿浆中含银矿物表面选择性吸附巯基捕收剂二聚氧化物的机理研究
根据元素的离子化势能和电子亲和能数据和半经验量子力学方法中的PM6计算了Mn4+、Pb2+、Ag+及巯基捕收剂二聚氧化物的前线轨道HOMO和LUMO的能量。比较Mn4+、Pb2+、Ag+电子空隙的最低未占分子轨道LUMO的能量与巯基捕收剂二聚氧化物的最高占据分子轨道HOMO的能量发现,巯基捕收剂二聚氧化物的HOMO的能量与Ag+的LUMO的能量非常接近,表明巯基捕收剂二聚氧化物与Ag+之间容易发生共价性配位健化学吸附。
采用Materials Studio软件的Adsorption Locater模块计算了氯化银、氧化银、硫酸铅、隐钾锰矿等四种矿物晶体吸附质与双黄药、双黑药、双乙硫氮分子、水分子、氢氧根离子、氯离子、硫酸根离子等吸附剂的作用能变化,结果表明,双黄药、双黑药、双乙硫氮分子等巯基捕收剂二聚氧化物无法吸附在隐钾锰矿表面,可以吸附在硫酸铅、氯化银、氧化银矿物表面,但在有硫酸根存在的条件下,上述巯基捕收剂二聚氧化物在氯化银、氧化银矿物表面仍然能发生吸附,而硫酸铅矿物表面对硫酸根离子的吸附比对上述巯基捕收剂二聚物的吸附强得多,表明双黄药、双黑药、双乙硫氮等巯基捕收剂二聚氧化物对含银矿物存在选择性吸附作用。
Zinc anode slime, a kind of residue produced in the process of zinc electrowinning, is a secondary resource abundant in manganese, lead and silver etc. The present method treating this residue in zinc ectrowinning plants is to return it to the leaching operation as an oxidant. It works well in reuse of manganese by not changing Mn(IV) to Mn(II), but fails to recycle lead and silver efficiently as early as possible. And there is no feasible and efficient technology till now which has done well in both of these two aspects. In this thesis, a combined beneficiation technology, including flotation, magnetic separation and gravity separation, to realize the separation of manganese, lead and silver, was developed based on the physicochemical property research. The electrochemical atmosphere background produced by Mn(IV) and Mn2+in the acidic pulp of this residue and its influence on the occurrence of lead, silver as well as thiol collectors were determined with a themodynamic method. The interaction mechanism of the of thiol collectors with lead and silver minerals in the pulp was investigated by means of infrared spectroscopic analysis, quantum chemical calculation and other research methods. The main research contents and innovations are as follows:
(1) Physicochemical properties of zinc anode slime and technology for comprehensive recovery of manganese, lead and silver minerals.
Zinc anode slime contains such major valuable elements as manganese, lead and silver, of which the main existing forms of metalliferous minerals are cryptomelane (KMn8O16) for Mn, anglesite (PbSO4) for Pb, and kerargyrite (AgCl), silver oxide (Ag2O3) and silver oxy-salt of nitrate (Ag7NO11) for Ag. The pulp of zinc anode slime is weakly acid, with pH below5, and the concentration of Mn2+is5.8×10-2mol.L-1.
Thiol collectors could only recover silver minerals from zinc anode slime. Flotation by xanthate after sulfidation could not recover anglesite from zinc anode slime. The combined flowsheet of "flotation-magnetic separation-gravity separation" performed very well to separate minerals of manganese, lead and silver respectively. By applying this technology, a silver concentrate with high silver grade,48515g/t, an anglesite concentrate containing lead60.89%, and a manganese concentrate with50.17%manganese could be obtained from zinc anode slime with grade of manganese, lead and silver being37.48%,21.54%and1628g/t, respectively. The total recovery of lead and silver in the lead and silver concentrates reached84.78%and74.71%respectively, and the manganese recovery is91.86%.
(2)Thermodynamic analysis of the pulp system of zinc anode mud
The Eh-pH diagrams for different systems have been drawn according to the themodynamically calculated data, based on which the background pulp potential of zinc anode slime and its influence on the occurrence of lead and silver components, the existing state of thiol collectors as well as the flotation of anglesite by xanthate after sulfidation, have been discussed. The results indicate that the pulp potential of zinc anode slime is mainly controlled by the MnO2, the concentration of Mn2+and the pH in the pulp, thus forming a strong oxidation atmosphere which called the background pulp potential of zinc anode slime. In this strong oxidation background pulp potential, lead mainly occurred as anglesite, silver can occurred as Ag, Ag2O, AgCl, AgO, Ag2O3, etc. The themodynamically stable products of sulfur in the pulp is not S2-, HS-, or S0, but SO42-, demonstrating that the sulfidation of anglesite by Na2S or NaHS cannot be achieved; The thermodynamically stable products of thiol collectors in zinc anode slime pulp are their corresponding oxidized dipolymers.
(3) The flotation behavior of lead and silver minerals in the pulp of zinc anode slime
Microflotation tests for pure minerals of anglesite and kerargyrite indicated that these two minerals have good floatability with thiol collectors such as xanthate and aerofloat, on the pH range of3-7. In the presence of MnO2, the floatability of kerargyrite maintains well but that of anglesite turns worse. Dixanthogen and bis-aerofloat have strong collecting ability to kerargyrite comparing with worse collecting ability to anglesite in the presence of SO42-. The infrared spectrum tests verified the selective adsorption of dixanthogen and bis-aerofloat on the surface of kerargyrite in the presence of SO42-.
(4) Mechanism of the selective adsorption of thiol collector oxidized dipolymers on the surface of silver containing minerals in zinc anode slime.
The highest occupied molecular orbit (HOMO) energy and the lowest unoccupied molecular orbit (LUMO) energy of Mn4+、Pb2+、Ag+have been calculated according to the ionization potential and electron affinity of element. The HOMO and LUMO energy of thiol collector oxidized dipolymers have been also calculated according to PM6in semiempirical quantum mechanics method. It's clearly shown by comparing the LUMO energy of Mn4+、Pb2+、Ag+with the HOMO energy of thiol collector oxidized dipolymers that the latter was close to the LUMO energy of Ag+, indicating that the covalent coordinated chemisorption of those thiol collector oxidized dipolymers on Ag+is prone to happen.
The changes of interaction energy between four kinds of mineral crystals (kerargyrite, silver oxide, anglesite and cryptomelane) and a variety of adsorbents (dixanthogen, bis-aerofloat, bis-diethyl dithiocarbamate, H2O, OH-, Cl-, SO42-) have been calculated by Material Studio(Adsorption Locater module). The results indicate that thiol collector oxidized dipolymers could not be adsorbed on the surface of cryptomelane. These thiol collector oxidized dipolymers could be adsorbed on the surface of anglesite, kerargyrite and silver oxide in the absence of SO42-. With the existence of SO42-, these collectors could only be adsorbed on the surface of silver minerals, due to the competive adsorption of SO42-on the surface of anglesite.
引文
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