含铁回收料球团金属化烧结新工艺研究
摘要
摘要：钢厂含锌粉尘和化工厂硫酸渣具有排量大、含有多种有价金属元素和有害元素及含碳量高等特点,导致难以利用。该类含铁回收料的大量堆存不仅造成二次污染,而且浪费资源。因此,研究该类含铁回收料高效利用新技术,制备出优质高炉炉料,实现其综合利用,将具有重要的现实意义。
本文以三种含铅锌粉尘和一种高砷硫酸渣为对象,系统研究了其物理化学性质及工艺矿物学特征。研究了铁氧化物还原和锌、铅氧化物及FeAsO4还原挥发热力学行为；阐明了焙烧过程中锌、铅、砷还原挥发脱除行为,分析了金属化烧结过程脱除锌、铅、砷的可行性。在此基础上开发了“含铁回收料球团金属化烧结新工艺”,研究了烧结料层中锌、铅、砷的迁移规律及其脱除行为,揭示了预还原烧结矿的固结机理。
研究所用原料瓦斯灰、干法灰、转炉污泥和硫酸渣的铁品位分别为33.45%、26.40%、56.30%和46.02%；碳含量分别为33.80%、26.50%、0.57%和0.35%；锌含量分别为0.66%、5.77%、2.27%和0.25%；铅含量分别为0.15%、2.25%、0.49%和0.11%。硫酸渣中的砷含量为0.17%。三种含锌粉尘中的锌和铅主要以氧化锌和氧化铅的形式存在,它们主要以游离态吸附在铁氧化物颗粒表面。硫酸渣中的锌和铅主要以硫化物的形式存在,砷主要以FeAsO4的形式存在。因此,采用常规选矿工艺均难以有效脱除原料中的锌、铅和砷。
热力学研究表明：当固体碳还原ZnO时,随着温度的升高,ZnO还原对CO含量的要求逐渐降低。当体系温度低于1085℃时,FeO比ZnO更容易还原,当还原温度高于1085℃时,ZnO比FeO更容易还原。PbO极易被还原,在还原温度为800℃时,还原反应所需要的CO/(CO+CO2)比值仅为0.52%。当还原温度为1000℃,只有在弱还原性气氛时,FeAsO4才能还原成As406挥发。若体系中CO/(CO+CO2)比值大于9.39%时,FeAsO4被还原为金属砷挥发。在球团金属化烧结过程中,由于料层中燃烧和预还原带为还原性气氛,最高温度高于1300℃,能够实现铁氧化物的金属化和锌、铅、砷的还原挥发。
铁氧化物、氧化锌和氧化铅的还原动力学表明：铁氧化物还原和氧化锌还原挥发的限制环节为界面化学反应控制,其表观活化能分别为43.88KJ.mol-1和7.33KJ.mol-1。氧化铅还原挥发的限制环节为气体扩散控制,其表观活化能为18.22KJ.mol-1。高温快速还原的动力学条件,保证了铁的金属化率及锌、铅、砷的还原挥发。
球团金属化烧结新工艺研究表明：在内配无烟煤,生球水分18%,造球时间13min的条件下,得到的生球落下强度、抗压强度和爆裂温度分别为7.4次/0.5m,15N/个和461℃。在总C/Fe为0.5、外配烟煤(内外还原剂按碳量分加比例为50：50)、烧结料层高度400mm及风速0.4m/s的条件下进行鼓风烧结,可得到成品率85.62%、利用系数0.471t·m-2·h-1、转鼓强度81.31%及固体燃耗309.67kg·t-1的良好指标。金属化烧结矿中全铁含量60.53%,金属化率45.23%；Zn、Pb、As含量分别为0.18%、0.015%和0.025%,Zn、Pb、As的脱除率分别为92.78%、96.37%和62.45%。金属化烧结矿总还原度为80.69%,还原粉化指数RDI+3.15为96.45%,是一种优质的高炉炉料。烟气冷凝后得到的粉尘ZnO、PbO和As205含量分别为51.49%、3.15%和1.45%。
球团金属化烧结过程中锌、铅、砷迁移规律及还原挥发行为表明：烧结料层可划分为五个反应带：原始料带、过湿带、干燥预热带、燃烧和预还原带和成品矿带。在成品矿带,由于再氧化,球团周围的金属铁被氧化成浮氏体。在燃烧和预还原带,还原剂剧烈燃烧,料层温度迅速升高,最高温度大于1300℃,高温(大于1250℃)保持时间大于5mmin,料层气氛为还原性气氛,烟气中C02含量为12-15%,CO含量为10-13%,02含量为2-5%。球团内为强还原性气氛(球团内C/Fe为0.33),铁氧化物在该带还原成金属铁,ZnO、PbO和FeAsO4在该带还原成金属而挥发。在干燥预热带,料层温度急剧降低,料层气氛为氧化性气氛,金属锌、铅、砷在挥发过程中氧化,其氧化物在该带冷凝聚集,沉积在干燥预热球团表面。随着烧结过程的推进,冷凝在干燥预热球团表面的锌、铅、砷的氧化物经历再还原、再挥发氧化、再冷凝,如此不断反复循环,直至烧结过程结束而转入烟气。
金属化烧结矿的固结机理研究表明：金属化烧结矿的宏观结构是呈葡萄状结构,球团被液相粘结在一起。微观结构是球团内部主要以金属铁形成的金属键相互连接,金属铁含量为39.82%；球团之间粘结相主要以液相粘结为主,主要粘结相为浮氏体、铁橄榄石和钙镁橄榄石,其中浮氏体含量为31.95%,渣相含量为24.29%。金属化烧结矿同时以金属键和液相粘结两种形态实现固结。
球团金属化烧结新工艺一步实现了铁与铅、锌、砷等有色金属的分离,得到满足高炉炉料要求的预还原产品。新上艺因利用系数较高、对设备要求简单、生产成本低和对原料适应性强,具有良好的工业应用前景。本研究为大规模高效利用含锌粉尘和硫酸渣开辟了一条新的途径。图111幅,表41个,参考文献216篇
Abstract:Zinc-bearing dust and pyrite cinder discharged from steel companies and chemical companies,have the characteristics of the large amount and containing many valuable metals and detrimental elements, resulting in huge waste of resources and serious environment pollution. Therefore,it has the considerable realistic significance to develop a new technology of utilizing these dusts to obtain the high quality burden for blast furnace.
Three kinds of zinc-bearing dust and one kind of pyrite cinder were used in this thesis.The physical and chemical properties and mineralogy characters are systematically studied.The thermodynamic behaviors of iron oxides, ZnO, PbO and FeAsO4during the reduction roasting process are also analyzed. The results show that the metallized sintering process is a feasible process to remove Zn, Pb and As.On this basis, a new process of metallized sintering process to separate iron from Zn, Pb and As is developed,and the migrating behaviors of Zn, Pb and As,and the consolidation mechanism of pre-reduced sinter in the sintering process are also revealed.
The iron content of gas ash, dry tpyed dust, converter sludge and pyrite cinder are33.45%,26.40%,56.30%and46.02%, respectively. The carbon content are33.80%,26.50%,0.57%and0.35%, respectively. The Zn content are0.66%,5.77%,2.27%and0.25%, respectively. The Pb content are0.15%,2.25%,0.49%and0.11%, respectively. The As content of pyrite cinder is0.17%. The mineralogy of raw material shows that most Zn and Pb absorb in the form of ZnO and PbO in the surface of iron oxides in the zinc-bearing dust. Zn and Pb exist in the form of sulfide in the pyrite cinder, and As exists in the form of FeAsO4in the pyrite cinder. Therefore,the Zn, Pb and As cannot be removed effectively from zinc-bearing dust and pyrite cinder by conventional beneficiation processes.
Thermodynamics investigations show that when ZnO is reduced by carbon,the CO content requirement decreases sharply as the temperature increases.ZnO is harded than FeO to be reducd at the temperature lower than1085℃.However, ZnO is easier than FeO to be reduced at the temperature higher than1085℃. PbO is reduced to Pb easily, and the CO/(CO+CO2) requirement is only0.52%at the temperature of800℃. FeAsO4can be reduced to As4O6at the week reducing atmosphere, and FeAsO4is reduced to As at the CO/(CO+CO2) higher than9.39%at the temperature of1000℃. The Zn、Pb、As can be removed in the metallized sintering process because of the reducing atmosphere and high temperature in the burning and pre-reducing zone.
The results of dynamics of iron oxides,ZnO and PbO reductions show that the reactions are controlled by chemical reaction,and the calculated activation energier are43.88and72.33KJ.mol-1, respectively, for the reductions of iron oxides and ZnO. The calculated activation energy of18.22KJ.mol-1is characteristic for gas diffusion controlled process in the PbO reducing reaction.The dynamic conditions of high temperature and rapid reduction meet requirements for the reductions of iron oxides,ZnO and PbO.
The results of new process of metallized sintering show that the drop numbers, compressive strength and shock temperature of green balls are7.4times/0.5m,15N and461℃under the conditions of balling at18%moisture for13min.The green balls are used to conduct the metallized sintering process under conditions of C/Fe of0.5,the carbon ratio of inside to outside pellets of50:50, the bed height of400mm and the air speed of0.4m/s.The pre-reduced product, assaying60.53%Fe with the metallization degree of45.23%,and the Zn,Pb and As content of0.18%,0.015%and0.025%, was obtained at the yield of85.62%, productivity of0.471tm-2h-1, tumble index of81.31%,the solid fuel consumption of309.67kg·t-1,respectively. The reducibility index and reduction disintegration index (RDI+3.15)of pre-reduced product are80.69%and96.45%,which show the pre-reduced product is the high quality burden for blast furnace.The ZnO、PbO and As2O5content of condensation dust are51.49%,3.15%and1.45%,respectively.
The reducing and removing behaviors of Zn,Pb and As during the metallized sintering show that the bed can be devided five zones, including original material zone,wetting materials zone, drying and preheating zone,burning and pre-reducing zone and product zone.During the product zone,metallic iron outside the pellets is reoxided into wustite. During the burning and pre-reducing zone,the maximum temperature of bed is higher than1300℃,and the duration (temperature higher than1250℃) is longer than5min.The bed atmosphere is reducing atmosphere, and the content of CO2, CO and O2in the exhausted gas are12-15%,10～13%, and2～5%,respectively. The atmosphere inside the pellets is strong reducing atmosphere (C/Fe of pellets is0.33),and iron oxides are reduced into metallic iron.ZnO and PbO are reduced and volatilized in this zone, and FeAsO4is reduced to As.During the drying and preheating zone, the temperature of bed decreases sharply and the oxidized atmosphere strengthens.Zn,Pb and As are oxidized and condensed in the surface of dried and preheated pellets.As the running of sintering process, the ZnO, PbO and As2O5of the drying and preheating zone are re-reduced, re-volatilized, re-oxidized and re-condensed until the end of sintering process to the condensation dust.
The pre-reduced product presents in the form of grape structure, and the pellets adhere together with liquid phase. The microstructures show that metallic iron is the major bonding connection inside the pellets, and the metallic iron content is39.82%.The liquid phase, such as wustite, FeSiO4and CaMgSiO4are the major bonding connections between pellets, and the wustite and slag content are31.95%and24.29%, respectively. The pre-reducing sinter possesses the metallic iron and luquid phase boding connections to achieve the consolidation.
The new process is an effective one step process to separate iron from Zn, Pb and As,and the high quality burden for blast furnace is achieved.The new process possesses the characters of high productivity, simple equipments,low cost and material adaptability, which has the bright prospect in the industrial application.The study has opened a new way to utilize the zinc-bearing dust and pyrite cinder large scaly and efficiently.
本文以三种含铅锌粉尘和一种高砷硫酸渣为对象,系统研究了其物理化学性质及工艺矿物学特征。研究了铁氧化物还原和锌、铅氧化物及FeAsO4还原挥发热力学行为；阐明了焙烧过程中锌、铅、砷还原挥发脱除行为,分析了金属化烧结过程脱除锌、铅、砷的可行性。在此基础上开发了“含铁回收料球团金属化烧结新工艺”,研究了烧结料层中锌、铅、砷的迁移规律及其脱除行为,揭示了预还原烧结矿的固结机理。
研究所用原料瓦斯灰、干法灰、转炉污泥和硫酸渣的铁品位分别为33.45%、26.40%、56.30%和46.02%；碳含量分别为33.80%、26.50%、0.57%和0.35%；锌含量分别为0.66%、5.77%、2.27%和0.25%；铅含量分别为0.15%、2.25%、0.49%和0.11%。硫酸渣中的砷含量为0.17%。三种含锌粉尘中的锌和铅主要以氧化锌和氧化铅的形式存在,它们主要以游离态吸附在铁氧化物颗粒表面。硫酸渣中的锌和铅主要以硫化物的形式存在,砷主要以FeAsO4的形式存在。因此,采用常规选矿工艺均难以有效脱除原料中的锌、铅和砷。
热力学研究表明：当固体碳还原ZnO时,随着温度的升高,ZnO还原对CO含量的要求逐渐降低。当体系温度低于1085℃时,FeO比ZnO更容易还原,当还原温度高于1085℃时,ZnO比FeO更容易还原。PbO极易被还原,在还原温度为800℃时,还原反应所需要的CO/(CO+CO2)比值仅为0.52%。当还原温度为1000℃,只有在弱还原性气氛时,FeAsO4才能还原成As406挥发。若体系中CO/(CO+CO2)比值大于9.39%时,FeAsO4被还原为金属砷挥发。在球团金属化烧结过程中,由于料层中燃烧和预还原带为还原性气氛,最高温度高于1300℃,能够实现铁氧化物的金属化和锌、铅、砷的还原挥发。
铁氧化物、氧化锌和氧化铅的还原动力学表明：铁氧化物还原和氧化锌还原挥发的限制环节为界面化学反应控制,其表观活化能分别为43.88KJ.mol-1和7.33KJ.mol-1。氧化铅还原挥发的限制环节为气体扩散控制,其表观活化能为18.22KJ.mol-1。高温快速还原的动力学条件,保证了铁的金属化率及锌、铅、砷的还原挥发。
球团金属化烧结新工艺研究表明：在内配无烟煤,生球水分18%,造球时间13min的条件下,得到的生球落下强度、抗压强度和爆裂温度分别为7.4次/0.5m,15N/个和461℃。在总C/Fe为0.5、外配烟煤(内外还原剂按碳量分加比例为50：50)、烧结料层高度400mm及风速0.4m/s的条件下进行鼓风烧结,可得到成品率85.62%、利用系数0.471t·m-2·h-1、转鼓强度81.31%及固体燃耗309.67kg·t-1的良好指标。金属化烧结矿中全铁含量60.53%,金属化率45.23%；Zn、Pb、As含量分别为0.18%、0.015%和0.025%,Zn、Pb、As的脱除率分别为92.78%、96.37%和62.45%。金属化烧结矿总还原度为80.69%,还原粉化指数RDI+3.15为96.45%,是一种优质的高炉炉料。烟气冷凝后得到的粉尘ZnO、PbO和As205含量分别为51.49%、3.15%和1.45%。
球团金属化烧结过程中锌、铅、砷迁移规律及还原挥发行为表明：烧结料层可划分为五个反应带：原始料带、过湿带、干燥预热带、燃烧和预还原带和成品矿带。在成品矿带,由于再氧化,球团周围的金属铁被氧化成浮氏体。在燃烧和预还原带,还原剂剧烈燃烧,料层温度迅速升高,最高温度大于1300℃,高温(大于1250℃)保持时间大于5mmin,料层气氛为还原性气氛,烟气中C02含量为12-15%,CO含量为10-13%,02含量为2-5%。球团内为强还原性气氛(球团内C/Fe为0.33),铁氧化物在该带还原成金属铁,ZnO、PbO和FeAsO4在该带还原成金属而挥发。在干燥预热带,料层温度急剧降低,料层气氛为氧化性气氛,金属锌、铅、砷在挥发过程中氧化,其氧化物在该带冷凝聚集,沉积在干燥预热球团表面。随着烧结过程的推进,冷凝在干燥预热球团表面的锌、铅、砷的氧化物经历再还原、再挥发氧化、再冷凝,如此不断反复循环,直至烧结过程结束而转入烟气。
金属化烧结矿的固结机理研究表明：金属化烧结矿的宏观结构是呈葡萄状结构,球团被液相粘结在一起。微观结构是球团内部主要以金属铁形成的金属键相互连接,金属铁含量为39.82%；球团之间粘结相主要以液相粘结为主,主要粘结相为浮氏体、铁橄榄石和钙镁橄榄石,其中浮氏体含量为31.95%,渣相含量为24.29%。金属化烧结矿同时以金属键和液相粘结两种形态实现固结。
球团金属化烧结新工艺一步实现了铁与铅、锌、砷等有色金属的分离,得到满足高炉炉料要求的预还原产品。新上艺因利用系数较高、对设备要求简单、生产成本低和对原料适应性强,具有良好的工业应用前景。本研究为大规模高效利用含锌粉尘和硫酸渣开辟了一条新的途径。图111幅,表41个,参考文献216篇
Abstract:Zinc-bearing dust and pyrite cinder discharged from steel companies and chemical companies,have the characteristics of the large amount and containing many valuable metals and detrimental elements, resulting in huge waste of resources and serious environment pollution. Therefore,it has the considerable realistic significance to develop a new technology of utilizing these dusts to obtain the high quality burden for blast furnace.
Three kinds of zinc-bearing dust and one kind of pyrite cinder were used in this thesis.The physical and chemical properties and mineralogy characters are systematically studied.The thermodynamic behaviors of iron oxides, ZnO, PbO and FeAsO4during the reduction roasting process are also analyzed. The results show that the metallized sintering process is a feasible process to remove Zn, Pb and As.On this basis, a new process of metallized sintering process to separate iron from Zn, Pb and As is developed,and the migrating behaviors of Zn, Pb and As,and the consolidation mechanism of pre-reduced sinter in the sintering process are also revealed.
The iron content of gas ash, dry tpyed dust, converter sludge and pyrite cinder are33.45%,26.40%,56.30%and46.02%, respectively. The carbon content are33.80%,26.50%,0.57%and0.35%, respectively. The Zn content are0.66%,5.77%,2.27%and0.25%, respectively. The Pb content are0.15%,2.25%,0.49%and0.11%, respectively. The As content of pyrite cinder is0.17%. The mineralogy of raw material shows that most Zn and Pb absorb in the form of ZnO and PbO in the surface of iron oxides in the zinc-bearing dust. Zn and Pb exist in the form of sulfide in the pyrite cinder, and As exists in the form of FeAsO4in the pyrite cinder. Therefore,the Zn, Pb and As cannot be removed effectively from zinc-bearing dust and pyrite cinder by conventional beneficiation processes.
Thermodynamics investigations show that when ZnO is reduced by carbon,the CO content requirement decreases sharply as the temperature increases.ZnO is harded than FeO to be reducd at the temperature lower than1085℃.However, ZnO is easier than FeO to be reduced at the temperature higher than1085℃. PbO is reduced to Pb easily, and the CO/(CO+CO2) requirement is only0.52%at the temperature of800℃. FeAsO4can be reduced to As4O6at the week reducing atmosphere, and FeAsO4is reduced to As at the CO/(CO+CO2) higher than9.39%at the temperature of1000℃. The Zn、Pb、As can be removed in the metallized sintering process because of the reducing atmosphere and high temperature in the burning and pre-reducing zone.
The results of dynamics of iron oxides,ZnO and PbO reductions show that the reactions are controlled by chemical reaction,and the calculated activation energier are43.88and72.33KJ.mol-1, respectively, for the reductions of iron oxides and ZnO. The calculated activation energy of18.22KJ.mol-1is characteristic for gas diffusion controlled process in the PbO reducing reaction.The dynamic conditions of high temperature and rapid reduction meet requirements for the reductions of iron oxides,ZnO and PbO.
The results of new process of metallized sintering show that the drop numbers, compressive strength and shock temperature of green balls are7.4times/0.5m,15N and461℃under the conditions of balling at18%moisture for13min.The green balls are used to conduct the metallized sintering process under conditions of C/Fe of0.5,the carbon ratio of inside to outside pellets of50:50, the bed height of400mm and the air speed of0.4m/s.The pre-reduced product, assaying60.53%Fe with the metallization degree of45.23%,and the Zn,Pb and As content of0.18%,0.015%and0.025%, was obtained at the yield of85.62%, productivity of0.471tm-2h-1, tumble index of81.31%,the solid fuel consumption of309.67kg·t-1,respectively. The reducibility index and reduction disintegration index (RDI+3.15)of pre-reduced product are80.69%and96.45%,which show the pre-reduced product is the high quality burden for blast furnace.The ZnO、PbO and As2O5content of condensation dust are51.49%,3.15%and1.45%,respectively.
The reducing and removing behaviors of Zn,Pb and As during the metallized sintering show that the bed can be devided five zones, including original material zone,wetting materials zone, drying and preheating zone,burning and pre-reducing zone and product zone.During the product zone,metallic iron outside the pellets is reoxided into wustite. During the burning and pre-reducing zone,the maximum temperature of bed is higher than1300℃,and the duration (temperature higher than1250℃) is longer than5min.The bed atmosphere is reducing atmosphere, and the content of CO2, CO and O2in the exhausted gas are12-15%,10～13%, and2～5%,respectively. The atmosphere inside the pellets is strong reducing atmosphere (C/Fe of pellets is0.33),and iron oxides are reduced into metallic iron.ZnO and PbO are reduced and volatilized in this zone, and FeAsO4is reduced to As.During the drying and preheating zone, the temperature of bed decreases sharply and the oxidized atmosphere strengthens.Zn,Pb and As are oxidized and condensed in the surface of dried and preheated pellets.As the running of sintering process, the ZnO, PbO and As2O5of the drying and preheating zone are re-reduced, re-volatilized, re-oxidized and re-condensed until the end of sintering process to the condensation dust.
The pre-reduced product presents in the form of grape structure, and the pellets adhere together with liquid phase. The microstructures show that metallic iron is the major bonding connection inside the pellets, and the metallic iron content is39.82%.The liquid phase, such as wustite, FeSiO4and CaMgSiO4are the major bonding connections between pellets, and the wustite and slag content are31.95%and24.29%, respectively. The pre-reducing sinter possesses the metallic iron and luquid phase boding connections to achieve the consolidation.
The new process is an effective one step process to separate iron from Zn, Pb and As,and the high quality burden for blast furnace is achieved.The new process possesses the characters of high productivity, simple equipments,low cost and material adaptability, which has the bright prospect in the industrial application.The study has opened a new way to utilize the zinc-bearing dust and pyrite cinder large scaly and efficiently.
引文
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