Níquel laterítico compõe 70% das reservas disponíveis do metal. A produção de níquel a partir dessas reservas representa 40%, dos quais é possível extrair também cobre e cobalto. Isso ocorre devido ao alto teor de impurezas, principalmente ferro. Com a crescente demanda desses metais, o uso das reservas de lateritas de níquel passou a ser mais profundamente investigado, assim como o desenvolvimento de processos hidrometalúrgicos. Nesse caso, o íon férrico prejudica a recuperação do níquel e do cobalto, uma vez que em trocas iônicas esse metal compete na ocupação dos sítios catiônicos. Em processos de extração por solvente um efeito semelhante é observado. Além disso, durante a eventual precipitação do ferro ocorre a coprecipitação. Assim, para a troca iônica, o íon ferroso pode ser menos prejudicial do que o férrico. O presente trabalho teve por objetivo o estudo do processo de redução do íon férrico em solução aquosa, e também a posterior obtenção de cobalto e níquel por meio de resinas quelantes. Estudou-se o processo de redução do íon férrico e o efeito na adsorção de metais por troca iônica. Os ensaios de redução química do íon férrico em solução foram estudados utilizando ditionito de sódio, metabissulfito de sódio e sulfito de sódio. Os ensaios com os agentes redutores ditionito e metabissulfito de sódio foram feitos em São Paulo, e os ensaios com o sulfito de sódio foram feitos na The University of British Columbia. Os agentes redutores foram adicionados na solução monoelementar de ferro para redução do potencial redox. As variáveis potencial redox, entre 860mV e 240mV; pH, entre 0,5 e 3,5; temperatura, entre 25°C e 60°C; e tempo, entre 30min e 96 horas, foram estudadas em frascos erlenmeyer sob agitação constante. Analisou-se, então, a redução do íon férrico em solução multielementar de níquel laterítico. Nos ensaios de troca iônica, realizados em batelada e em coluna, utilizou-se a resina quelante Lewatit TP 207, de grupo funcional iminodiacetato, e a resina Lewatit TP220, de grupo funcional bis-picolilamina. Três soluções foram estudadas: uma preparada com Fe(III), outra com Fe(II) e a terceira com Fe(III) após o processo de pré-redução. Os ensaios em batelada foram realizados com a utilização de frascos erlenmeyer, sob agitação constante, com 100mL de solução para 1mL de resina. Estudou-se o efeito do pH, entre 0,5 e 3,5; tempo, entre 30min e 480min; e temperatura, entre 25°C e 60°C. Nos ensaios em sistema contínuo, as três soluções foram alimentadas em colunas de vidro preenchidas com resina. A solução foi alimentada com bombas peristálticas a vazão constante. Para eluição das colunas, ácido sulfúrico 1mol.L-1 foi alimentado na coluna com utilização de bomba peristáltica. A segunda parte do trabalho, realizado na The University of British Columbia, foi o estudo do uso de sulfito de sódio no processo de pré-redução. Foram estudadas duas resinas: a Lewatit TP 207, seletiva para cobre; e a Lewatit TP 220, seletiva para níquel e cobalto. O sulfito de sódio foi adicionado na solução para redução do potencial, em frascos, e colocado sob agitação constante. Após reação, as soluções foram colocadas em contato com a resina quelante, e ficaram em agitação. Os ensaios em batelada foram realizados e o efeito do pH estudado entre 0,5 e 3,5. No processo em coluna, a Coluna 1, preenchida com a resina Lewatit TP 207, foi utilizada para remoção do cobre; e a solução de saída foi alimentada na Coluna 2, preenchida com a resina Lewatit TP 220. Para a eluição, foram estudados os ácidos clorídricos e sulfúricos em duas diferentes concentrações, 1mol.L-1 e 2mol.L-1. Hidróxido de sódio foi utilizado para remover o ferro na solução obtida na saída da Coluna 2. A separação do cobalto da solução foi feita utilizando a técnica de extração por solventes (Cyanex 272 20%), estudando o efeito do pH, 4,0 e 5,0, e da temperatura, 25°C e 65°C. Os resultados mostraram que a redução do íon férrico utilizando ditionito de sódio foi de 100% na solução monoelementar e de 70% na multielementar contendo os outros metais. Nos ensaios de troca iônica em batelada, utilizando a resina TP 207, 62% do cobre foi adsorvido na solução após processo de pré-redução. Para solução com Fe(II), a adsorção de cobre foi de 61%; e para solução com Fe(III), 49%. Nos ensaios de troca iônica após pré-redução do ferro com sulfito de sódio, a adsorção do cobre foi de 69% em pH 2,0 pela resina TP 207. A resina TP 220 foi mais seletiva para níquel e cobalto em pH 2,0, em que as adsorções destes metais foram 32,5% e 69%, respectivamente. Nos ensaios em coluna, a Coluna 1 foi utilizada para remoção de cobre, porém houve perda de 17% de níquel e 7% de cobalto. Na alimentação da Coluna 2, verificou-se que 98% do níquel e 84% do cobalto foram adsorvidos. A solução obtida da Coluna 2 teve concentração de 618mg.L-1 de ferro, 13231mg.L-1 de níquel e 179mg.L-1 de cobalto. A remoção de 100% do ferro foi possível em pH 4,0. Para separação do cobalto da solução rica em níquel, utilizou-se a extração por solventes com o Cyanex 272 20% em querosene, no qual 99% do cobalto foi separado da solução a 65°C e pH 5,0, sem perda de níquel. Para estudos futuros, a remoção do cobre no início do processo pode ser explorada com a utilização de outras técnicas, a fim de se evitarem perdas de níquel e cobalto. Outro ponto que pode vir a ser explorado é a máxima utilização das colunas de troca iônica nas mesmas condições deste trabalho - solução com Fe(III), com Fe(II) e após processo de pré-redução - sobretudo em escala piloto, para estudar o efeito do estado de oxidação do ferro em um possível envenenamento da resina. / Nickel laterite ores represent 70% of the available metal reserves. The nickel production from these reserves represents 40%, where it is also possible extract copper and cobalt. It occurs due to the high impurities content, mainly iron. With the growing demand of these metals, the use of nickel laterite reserves became more deeply investigated, as well as hydrometallurgical process development. In this case, the ferric iron difficult the nickel and cobalt recovery, once in ion exchange processes this metal competes in the occupation of the cationic sites. In solvent extraction processes the same effect is observed. Besides that, during the eventual iron precipitation there is a co-precipitation. Therefore, for ion exchange, ferrous iron may be less damaging than ferric iron. The aim of this work was to study the reducing process of ferric iron in aqueous solution, and also the subsequent obtaining of cobalt and nickel through chelating resins. It was studied the reducing process of ferric iron and the effect of it in metals adsorption by ion exchange. Experiments of chemical reduction of ferric iron in solution were studied using sodium dithionite, sodium metabisulfite and sodium sulfite. Experiments with reducing agents sodium dithionite and metabisulfite were performed in São Paulo, and experiments with sodium sulfite were performed in The University of British Columbia. Reducing agents were added in ferric iron mono-elementary solution to decrease the redox potential. The variables potential redox, between 860mV and 240mV; pH, between 0,5 and 3,5; temperature, between 25°C e 60°C; and time, between 30min and 96 hours were studied in erlenmeyer flasks under constant stirring. Then, analyzed ferric iron reduction in multielementary solution of nickel laterite. In ion exchange experiments, performed in batch and column, it was used chelating resin Lewatit TP 207, with iminodiacetate functional group, and resin Lewatit TP 220, with bis-picolylamine functional group. Three solutions were studied: prepared with Fe(III), other with Fe(III) and the third with Fe(III) after pre-reducing process. Experiments in batch system were performed using erlenmeyer flasks, under constant stirring, with 100mL of solution to 1mL of resin. It was studied the effect of pH, between 0,5 and 3,5, time, between 30min and 480min, and temperature, between 25°C e 60°C. In experiments in continuous system, the three solutions were fed in glass columns filled with resin. The solution was fed using peristaltic pumps at constant flow rate. For column elution, sulfuric acid 1mol.L-1 was fed to the column using peristaltic pumps. The second part of this work, performed at The University of British Columbia, was the study of sodium sulfite application at prereducing process. It was studied two resins: Lewatit TP 207, selective for copper, and Lewatit TP 220, selective for nickel and cobalt. Sodium sulfite was added to the solution to decrease the potential, in flasks and it was placed under constant stirring. After reaction, the solution was placed in contact to the chelating resin, which was placed under stirring. Batch experiments were performed, and the effect of pH was studied between 0,5 and 3,5. In column process, the Column 1, filled with Lewatit TP 207, was used for copper removal, and output solution was feed in Column 2, filled with Lewatit TP 220. For the elution, it was studied sulfuric and hydrochloric acids in two different concentrations, 1mol.L-1 e 2mol.L-1. Sodium hydroxide was used for iron removal from solution obtained in Column 2 output. Cobalt separation was performed using solvent extraction technique (Cyanex 272 20%), studying the effect of pH, 4,0 and 5,0, and temperature, 25°C e 65°C. Results shows that ferric iron reduction using sodium dithionite was 100% in mono-elementary solution and 70% in multi-elementary solution with other metals. In ion exchange experiments performed in batch using resin TP 207, 62% of copper was adsorbed by the resin after pre-reducing process. For solution with Fe(II), the copper adsorption was 61%, and for solution with Fe(III), 49%. In ion exchange experiments after pre-reducing process using sodium sulfite, the copper adsorption was 69% at pH 2,0 by the resin TP 207. The resin TP 220 was more selective for nickel and cobalt at pH 2,0, where these metals adsorptions were 32,5% and 69%, respectively. In experiments performed in column, the Column 1 was used for copper removal, however there were losses of nickel (17%) and cobalt (7%). In the feeding of Column 2, it was found that 98% of nickel and 84% of cobalt were adsorbed. Solution obtained in Column 2 had concentration of iron 618mg.L-1, nickel was 13231mg.L-1 and cobalt 179mg.L-1. The iron removal was 100% at pH 4,0. For cobalt separation in nickel-rich solution, it was used the solvent extraction with Cyanex 272 20% with kerosene, where 99% of cobalt was separated from solution at 65°C and pH 5,0, without nickel loss. For future studies, the copper removal in the beginning of the process can be explored using other techniques, in order to avoid nickel and cobalt losses. Another point that can be explored is the maximum use of ion exchange columns in the same conditions of this work - solution with Fe(III), with Fe(II) and after the pre-reducing process - mostly on a pilot scale, to study the effect of iron oxidation state on possible resin poisoning.

Algumas indicações morfológicas sugerem que as superfícies de paisagem tropicais onde encontram-se os duricrusts ferruginosos, podem apresentar idades que variam desde o Quaternário até o Cretáceo, e que a laterização sobre estas superfícies pode ter sido iniciada simultaneamente ou não, estabelecendo-se uma sequência cronológica de formação escalonada de acordo com a elevação, em função da evolução geomorfológica das superfícies. Sabendo-se que no Planalto de Diamantina na Serra do Espinhaço Meridional (SdEM) são reconhecidos três níveis geomorfológicos correlatos aos ciclos de aplainamento da plataforma Sul-americana, o objetivo deste trabalho foi estudar as variações mineralógicas, geoquímicas e morfológicas de duricrusts ferruginosos da Serra do Espinhaço Meridional buscando entender os processos genéticos envolvidos e as implicações disto sobre a distribuição e evolução da paisagem regional e suas relações com os ciclos de aplainamento do continente Sul-americano. Para atingir estes objetivos, foram realizadas análises de difratometria de raios X, suscetibilidade magnética, microscopia eletrônica de varredura com sistema de energia dispersiva acoplado e análise elementar a partir da dissolução total dos minerais constituintes. Os resultados mostraram que no Planalto de Diamantina na SdEM coexistem níveis de ferricretes e lateritas na superfície correspondente ao ciclo erosivo Pós-Gondwanico. As superfícies lateríticas são provavelmente as formações supérgenas mais antigas da paisagem regional, originadas durante os processos denudacionais que ocorreram ao longo do ciclo erosivo Pós-Gondwanico. A erosão parcial de seu perfil laterítico constituíram o material fonte de Fe e Al para a gênese dos ferricretes distribuídos em superfícies elevadas (> 1200 m), especialmente aqueles em superfícies em torno de 1400 m de altitude. As variações paleoclimáticas do ciclo Pós-Gondwanico também proporcionaram ciclos erosivos alternados que resultaram no subescalonamento desta superfície, criando condições geomorfológicas favoráveis à gênese de ferricretes mais recentes (1200 - 1400 m). Além disso, os duricrusts ferruginosos do Planalto Diamantina (SdEM) sob influência do maciço quartzítico do Supergrupo Espinhaço e situados superfícies erosivas elevadas (> 1200 m), além de policíclicos, também podem apresentar características poligenéticas. / Some morphological indications suggest that the tropical landscape surfaces where the iron-rich duricrust are present may have ages varying from the Quaternary to the Cretaceous, and that the laterization on these surfaces may have been initiated simultaneously or not, establishing a sequence chronological formation according to the elevation, according to the geomorphological evolution of the surfaces. Three geomorphological levels correlated to the South American platform planing cycles are known on the Diamantina Plateau, for this the objective of this work was to study the mineralogical, geochemical and morphological variations of the iron-rich duricrust of the SdEM, trying to understand the genetic processes involved and the implications of this on the distribution and evolution of the regional landscape and its relations with the planning cycles of the South American continent. In order to reach these objectives, X-ray diffraction, magnetic susceptibility, scanning electron microscopy with dispersive energy system coupled and elemental analysis carried out from the total dissolution of the constituent minerals. The results showed that in the Diamantina Plateau at the SdEM, coexist levels of ferricretes and laterites on the surface corresponding to the Post-Gondwanic erosive cycle. The laterite surfaces are probably the oldest surviving formations of the regional landscape, originated during the denudation processes that occurred along the Post-Gondwanic erosive cycle. Partial erosion of its lateritic profile was source material of Fe and Al for the genesis of ferricretes distributed on high surfaces (> 1200 m), especially those on surfaces at 1400 m of altitude. The paleoclimatic variations of the Post-Gondwanic cycle also provided alternating erosive cycles that resulted in sub-scaling of this surface, creating geomorphological conditions favorable for genesis of earlier ferricretes (1200 - 1400 m). In addition, the ferricretes of the Diamantina Plateau (SdEM) under influence of the Quartzite massif of the Espinhaço Supergroup and located in elevated erosive surfaces (> 1200 m), besides polycyclics, may also present polygenetic characteristics.

Níquel laterítico compõe 70% das reservas disponíveis do metal. A produção de níquel a partir dessas reservas representa 40%, dos quais é possível extrair também cobre e cobalto. Isso ocorre devido ao alto teor de impurezas, principalmente ferro. Com a crescente demanda desses metais, o uso das reservas de lateritas de níquel passou a ser mais profundamente investigado, assim como o desenvolvimento de processos hidrometalúrgicos. Nesse caso, o íon férrico prejudica a recuperação do níquel e do cobalto, uma vez que em trocas iônicas esse metal compete na ocupação dos sítios catiônicos. Em processos de extração por solvente um efeito semelhante é observado. Além disso, durante a eventual precipitação do ferro ocorre a coprecipitação. Assim, para a troca iônica, o íon ferroso pode ser menos prejudicial do que o férrico. O presente trabalho teve por objetivo o estudo do processo de redução do íon férrico em solução aquosa, e também a posterior obtenção de cobalto e níquel por meio de resinas quelantes. Estudou-se o processo de redução do íon férrico e o efeito na adsorção de metais por troca iônica. Os ensaios de redução química do íon férrico em solução foram estudados utilizando ditionito de sódio, metabissulfito de sódio e sulfito de sódio. Os ensaios com os agentes redutores ditionito e metabissulfito de sódio foram feitos em São Paulo, e os ensaios com o sulfito de sódio foram feitos na The University of British Columbia. Os agentes redutores foram adicionados na solução monoelementar de ferro para redução do potencial redox. As variáveis potencial redox, entre 860mV e 240mV; pH, entre 0,5 e 3,5; temperatura, entre 25°C e 60°C; e tempo, entre 30min e 96 horas, foram estudadas em frascos erlenmeyer sob agitação constante. Analisou-se, então, a redução do íon férrico em solução multielementar de níquel laterítico. Nos ensaios de troca iônica, realizados em batelada e em coluna, utilizou-se a resina quelante Lewatit TP 207, de grupo funcional iminodiacetato, e a resina Lewatit TP220, de grupo funcional bis-picolilamina. Três soluções foram estudadas: uma preparada com Fe(III), outra com Fe(II) e a terceira com Fe(III) após o processo de pré-redução. Os ensaios em batelada foram realizados com a utilização de frascos erlenmeyer, sob agitação constante, com 100mL de solução para 1mL de resina. Estudou-se o efeito do pH, entre 0,5 e 3,5; tempo, entre 30min e 480min; e temperatura, entre 25°C e 60°C. Nos ensaios em sistema contínuo, as três soluções foram alimentadas em colunas de vidro preenchidas com resina. A solução foi alimentada com bombas peristálticas a vazão constante. Para eluição das colunas, ácido sulfúrico 1mol.L-1 foi alimentado na coluna com utilização de bomba peristáltica. A segunda parte do trabalho, realizado na The University of British Columbia, foi o estudo do uso de sulfito de sódio no processo de pré-redução. Foram estudadas duas resinas: a Lewatit TP 207, seletiva para cobre; e a Lewatit TP 220, seletiva para níquel e cobalto. O sulfito de sódio foi adicionado na solução para redução do potencial, em frascos, e colocado sob agitação constante. Após reação, as soluções foram colocadas em contato com a resina quelante, e ficaram em agitação. Os ensaios em batelada foram realizados e o efeito do pH estudado entre 0,5 e 3,5. No processo em coluna, a Coluna 1, preenchida com a resina Lewatit TP 207, foi utilizada para remoção do cobre; e a solução de saída foi alimentada na Coluna 2, preenchida com a resina Lewatit TP 220. Para a eluição, foram estudados os ácidos clorídricos e sulfúricos em duas diferentes concentrações, 1mol.L-1 e 2mol.L-1. Hidróxido de sódio foi utilizado para remover o ferro na solução obtida na saída da Coluna 2. A separação do cobalto da solução foi feita utilizando a técnica de extração por solventes (Cyanex 272 20%), estudando o efeito do pH, 4,0 e 5,0, e da temperatura, 25°C e 65°C. Os resultados mostraram que a redução do íon férrico utilizando ditionito de sódio foi de 100% na solução monoelementar e de 70% na multielementar contendo os outros metais. Nos ensaios de troca iônica em batelada, utilizando a resina TP 207, 62% do cobre foi adsorvido na solução após processo de pré-redução. Para solução com Fe(II), a adsorção de cobre foi de 61%; e para solução com Fe(III), 49%. Nos ensaios de troca iônica após pré-redução do ferro com sulfito de sódio, a adsorção do cobre foi de 69% em pH 2,0 pela resina TP 207. A resina TP 220 foi mais seletiva para níquel e cobalto em pH 2,0, em que as adsorções destes metais foram 32,5% e 69%, respectivamente. Nos ensaios em coluna, a Coluna 1 foi utilizada para remoção de cobre, porém houve perda de 17% de níquel e 7% de cobalto. Na alimentação da Coluna 2, verificou-se que 98% do níquel e 84% do cobalto foram adsorvidos. A solução obtida da Coluna 2 teve concentração de 618mg.L-1 de ferro, 13231mg.L-1 de níquel e 179mg.L-1 de cobalto. A remoção de 100% do ferro foi possível em pH 4,0. Para separação do cobalto da solução rica em níquel, utilizou-se a extração por solventes com o Cyanex 272 20% em querosene, no qual 99% do cobalto foi separado da solução a 65°C e pH 5,0, sem perda de níquel. Para estudos futuros, a remoção do cobre no início do processo pode ser explorada com a utilização de outras técnicas, a fim de se evitarem perdas de níquel e cobalto. Outro ponto que pode vir a ser explorado é a máxima utilização das colunas de troca iônica nas mesmas condições deste trabalho - solução com Fe(III), com Fe(II) e após processo de pré-redução - sobretudo em escala piloto, para estudar o efeito do estado de oxidação do ferro em um possível envenenamento da resina. / Nickel laterite ores represent 70% of the available metal reserves. The nickel production from these reserves represents 40%, where it is also possible extract copper and cobalt. It occurs due to the high impurities content, mainly iron. With the growing demand of these metals, the use of nickel laterite reserves became more deeply investigated, as well as hydrometallurgical process development. In this case, the ferric iron difficult the nickel and cobalt recovery, once in ion exchange processes this metal competes in the occupation of the cationic sites. In solvent extraction processes the same effect is observed. Besides that, during the eventual iron precipitation there is a co-precipitation. Therefore, for ion exchange, ferrous iron may be less damaging than ferric iron. The aim of this work was to study the reducing process of ferric iron in aqueous solution, and also the subsequent obtaining of cobalt and nickel through chelating resins. It was studied the reducing process of ferric iron and the effect of it in metals adsorption by ion exchange. Experiments of chemical reduction of ferric iron in solution were studied using sodium dithionite, sodium metabisulfite and sodium sulfite. Experiments with reducing agents sodium dithionite and metabisulfite were performed in São Paulo, and experiments with sodium sulfite were performed in The University of British Columbia. Reducing agents were added in ferric iron mono-elementary solution to decrease the redox potential. The variables potential redox, between 860mV and 240mV; pH, between 0,5 and 3,5; temperature, between 25°C e 60°C; and time, between 30min and 96 hours were studied in erlenmeyer flasks under constant stirring. Then, analyzed ferric iron reduction in multielementary solution of nickel laterite. In ion exchange experiments, performed in batch and column, it was used chelating resin Lewatit TP 207, with iminodiacetate functional group, and resin Lewatit TP 220, with bis-picolylamine functional group. Three solutions were studied: prepared with Fe(III), other with Fe(III) and the third with Fe(III) after pre-reducing process. Experiments in batch system were performed using erlenmeyer flasks, under constant stirring, with 100mL of solution to 1mL of resin. It was studied the effect of pH, between 0,5 and 3,5, time, between 30min and 480min, and temperature, between 25°C e 60°C. In experiments in continuous system, the three solutions were fed in glass columns filled with resin. The solution was fed using peristaltic pumps at constant flow rate. For column elution, sulfuric acid 1mol.L-1 was fed to the column using peristaltic pumps. The second part of this work, performed at The University of British Columbia, was the study of sodium sulfite application at prereducing process. It was studied two resins: Lewatit TP 207, selective for copper, and Lewatit TP 220, selective for nickel and cobalt. Sodium sulfite was added to the solution to decrease the potential, in flasks and it was placed under constant stirring. After reaction, the solution was placed in contact to the chelating resin, which was placed under stirring. Batch experiments were performed, and the effect of pH was studied between 0,5 and 3,5. In column process, the Column 1, filled with Lewatit TP 207, was used for copper removal, and output solution was feed in Column 2, filled with Lewatit TP 220. For the elution, it was studied sulfuric and hydrochloric acids in two different concentrations, 1mol.L-1 e 2mol.L-1. Sodium hydroxide was used for iron removal from solution obtained in Column 2 output. Cobalt separation was performed using solvent extraction technique (Cyanex 272 20%), studying the effect of pH, 4,0 and 5,0, and temperature, 25°C e 65°C. Results shows that ferric iron reduction using sodium dithionite was 100% in mono-elementary solution and 70% in multi-elementary solution with other metals. In ion exchange experiments performed in batch using resin TP 207, 62% of copper was adsorbed by the resin after pre-reducing process. For solution with Fe(II), the copper adsorption was 61%, and for solution with Fe(III), 49%. In ion exchange experiments after pre-reducing process using sodium sulfite, the copper adsorption was 69% at pH 2,0 by the resin TP 207. The resin TP 220 was more selective for nickel and cobalt at pH 2,0, where these metals adsorptions were 32,5% and 69%, respectively. In experiments performed in column, the Column 1 was used for copper removal, however there were losses of nickel (17%) and cobalt (7%). In the feeding of Column 2, it was found that 98% of nickel and 84% of cobalt were adsorbed. Solution obtained in Column 2 had concentration of iron 618mg.L-1, nickel was 13231mg.L-1 and cobalt 179mg.L-1. The iron removal was 100% at pH 4,0. For cobalt separation in nickel-rich solution, it was used the solvent extraction with Cyanex 272 20% with kerosene, where 99% of cobalt was separated from solution at 65°C and pH 5,0, without nickel loss. For future studies, the copper removal in the beginning of the process can be explored using other techniques, in order to avoid nickel and cobalt losses. Another point that can be explored is the maximum use of ion exchange columns in the same conditions of this work - solution with Fe(III), with Fe(II) and after the pre-reducing process - mostly on a pilot scale, to study the effect of iron oxidation state on possible resin poisoning.

Algumas indicações morfológicas sugerem que as superfícies de paisagem tropicais onde encontram-se os duricrusts ferruginosos, podem apresentar idades que variam desde o Quaternário até o Cretáceo, e que a laterização sobre estas superfícies pode ter sido iniciada simultaneamente ou não, estabelecendo-se uma sequência cronológica de formação escalonada de acordo com a elevação, em função da evolução geomorfológica das superfícies. Sabendo-se que no Planalto de Diamantina na Serra do Espinhaço Meridional (SdEM) são reconhecidos três níveis geomorfológicos correlatos aos ciclos de aplainamento da plataforma Sul-americana, o objetivo deste trabalho foi estudar as variações mineralógicas, geoquímicas e morfológicas de duricrusts ferruginosos da Serra do Espinhaço Meridional buscando entender os processos genéticos envolvidos e as implicações disto sobre a distribuição e evolução da paisagem regional e suas relações com os ciclos de aplainamento do continente Sul-americano. Para atingir estes objetivos, foram realizadas análises de difratometria de raios X, suscetibilidade magnética, microscopia eletrônica de varredura com sistema de energia dispersiva acoplado e análise elementar a partir da dissolução total dos minerais constituintes. Os resultados mostraram que no Planalto de Diamantina na SdEM coexistem níveis de ferricretes e lateritas na superfície correspondente ao ciclo erosivo Pós-Gondwanico. As superfícies lateríticas são provavelmente as formações supérgenas mais antigas da paisagem regional, originadas durante os processos denudacionais que ocorreram ao longo do ciclo erosivo Pós-Gondwanico. A erosão parcial de seu perfil laterítico constituíram o material fonte de Fe e Al para a gênese dos ferricretes distribuídos em superfícies elevadas (> 1200 m), especialmente aqueles em superfícies em torno de 1400 m de altitude. As variações paleoclimáticas do ciclo Pós-Gondwanico também proporcionaram ciclos erosivos alternados que resultaram no subescalonamento desta superfície, criando condições geomorfológicas favoráveis à gênese de ferricretes mais recentes (1200 - 1400 m). Além disso, os duricrusts ferruginosos do Planalto Diamantina (SdEM) sob influência do maciço quartzítico do Supergrupo Espinhaço e situados superfícies erosivas elevadas (> 1200 m), além de policíclicos, também podem apresentar características poligenéticas. / Some morphological indications suggest that the tropical landscape surfaces where the iron-rich duricrust are present may have ages varying from the Quaternary to the Cretaceous, and that the laterization on these surfaces may have been initiated simultaneously or not, establishing a sequence chronological formation according to the elevation, according to the geomorphological evolution of the surfaces. Three geomorphological levels correlated to the South American platform planing cycles are known on the Diamantina Plateau, for this the objective of this work was to study the mineralogical, geochemical and morphological variations of the iron-rich duricrust of the SdEM, trying to understand the genetic processes involved and the implications of this on the distribution and evolution of the regional landscape and its relations with the planning cycles of the South American continent. In order to reach these objectives, X-ray diffraction, magnetic susceptibility, scanning electron microscopy with dispersive energy system coupled and elemental analysis carried out from the total dissolution of the constituent minerals. The results showed that in the Diamantina Plateau at the SdEM, coexist levels of ferricretes and laterites on the surface corresponding to the Post-Gondwanic erosive cycle. The laterite surfaces are probably the oldest surviving formations of the regional landscape, originated during the denudation processes that occurred along the Post-Gondwanic erosive cycle. Partial erosion of its lateritic profile was source material of Fe and Al for the genesis of ferricretes distributed on high surfaces (> 1200 m), especially those on surfaces at 1400 m of altitude. The paleoclimatic variations of the Post-Gondwanic cycle also provided alternating erosive cycles that resulted in sub-scaling of this surface, creating geomorphological conditions favorable for genesis of earlier ferricretes (1200 - 1400 m). In addition, the ferricretes of the Diamantina Plateau (SdEM) under influence of the Quartzite massif of the Espinhaço Supergroup and located in elevated erosive surfaces (> 1200 m), besides polycyclics, may also present polygenetic characteristics.

Les latérites couvrent plus de 30% des surfaces émergées. Comprendre leur évolution future est essentiel pour prédire les changements qui affecteront le fonctionnement de la Zone Critique dans les siècles à venir. La littérature a pu montrer que les horizons indurés de ces sols comportaient plusieurs générations de minéraux secondaires qui pouvaient être reliées à différents événements paléoclimatiques. Des études isotopiques ont montré que les horizons non indurés de ces sols pouvaient aussi posséder des générations distinctes de minéraux secondaires. La datation par Résonance Paramagnétique Électronique, a été appliquée sur des kaolinites de latérites dans le but d’identifier si ce minéral possède bien plusieurs générations au sein d’un même profil et si ces dernières étaient corrélables avec des événements paléoclimatiques globaux ou régionaux. Au cours de cette thèse, deux régolithes du Plateau du Karnataka (Inde), quatre du bassin du Rio Négro (Brésil) et un de la région de Syerstone (Australie) ont été étudiés. Les résultats de ces datations ont permis de distinguer différentes générations de kaolinites au sein de chacun des profils étudiés. Ces dernières sont par ailleurs toutes corrélables avec des périodes de fortes précipitations liées aux évolutions climatiques régionales et/ou globales. Ces résultats confirment aussi l’existence du phénomène de rajeunissement profils latéritiques au cours des temps géologiques. Le travail de cette thèse corrobore l’hypothèse de l’évolution épisodique de ces sols tropicaux et souligne leur importante stabilité dans les temps géologiques. / Laterites are covering a third of the continental surfaces. Understanding their evolution through the ongoing climate change is critical to predict the future Critical Zone transformation. Laterite duricrusts can contain several generations of secondary minerals that can be correlated with distinct paleoclimatic events. Isotopic studies showed that loose laterites may also be formed by several generations of secondary minerals. The objective of this PhD was to confirm that loose laterites contain several generations of kaolinites and that they formed during regional and/or global paleoclimatic events. With this aim in view, a recent dating methodology, the Electron Paramagnetic Resonance dating of kaolinites, was used on tropical regolith profiles from three continents with distinct geodynamic histories: India (Karnataka plateau), South America (Rio Negro basin, Brazil) and Australia (Syerstone region, New South Wale). The data set of this PhD confirms that a regolith contains several generations of kaolinites. All the identified generations of the present study can be correlated with regional paleoclimatic events or with tropical weathering favourable periods initiated by global paleoclimatic trends. Kaolinite generations formed preferentially during high precipitations periods and result from the rejuvenation of laterite profiles. The results of this PhD confirm that laterites have an episodic evolution.

The aim of this study was to extract nickel and cobalt from the lateritic nickel ores of G&ouml / rdes region by hydrometallurgical methods under the optimum conditions. Limonitic and nontronitic types of G&ouml / rdes lateritic nickel ores were used during experiments. Agitative and column leaching experiments at atmospheric pressure were conducted with various parameters / these were duration, temperature and initial sulfuric acid concentration of leach solution. It was shown that in agitative leaching, under the optimum conditions that were determined as 24 hours of leaching at 95&deg / C with initial sulfuric acid concentration of 192.1 g/L for nontronite and 240.1 g/L for limonite, nickel and cobalt extractions were 96.0% and 63.4% for nontronite / 93.1% and 75.0% for limonite, respectively. Overall acid consumptions of ores were calculated as 669 kg H2SO4/ton dry ore for nontronitic type nickel ore and 714 kg H2SO4/ton dry ore for limonitic type nickel ore. Column leaching experiments also showed that nickel and cobalt could be extracted from both ore types by heap leaching. Nontronite type of laterite was found to be more suitable for column leaching by sulfuric acid. In column leaching, the calculated nickel and cobalt extractions were 83.9% and 55.2% for nontronite after 122 days of leaching with 100 g/L sulfuric acid concentration. Acid consumption of nontronite was found to be 462 kg H2SO4/ton dry ore.

ABSTRACT HIGH PRESSURE ACID LEACHING OF TURKISH LATERITES Kaya, Serif M.Sc., Department of Metallurgical and Materials Engineering Supervisor: Prof. Dr. Yavuz A. Topkaya January 2011, 91 pages The aim of this thesis study was to investigate and find the most cost effective way of extracting nickel and cobalt into the pregnant leach solution (PLS) from G&ouml / rdes lateritic nickel and cobalt ore by means of sulphuric acid leaching under high temperature and high pressure conditions.The high pressure acid leach (HPAL) experiments were conducted with nontronitic and limonitic types of G&ouml / rdes lateritic nickel ore, respectively. Leaching experiments of nontronite ore have shown that almost all of the nickel and cobalt contained in the nontronitic ore were easily extracted into the (PLS). Therefore, the rest of the experiments were concentrated on difficult to leach limonitic sample when compared with the nontronitic one, and higher nickel and cobalt extractions were aimed to be obtained. By taking economic and technical considerations into account, the basic (HPAL) process parameters for the limonitic sample were optimized as / leaching at 255 &deg / C with a particle size of 100% -850 &mu / with 0.30 sulphuric acid to ore weight ratio in 1 hour of leaching duration. The experiments were conducted with 30% solids ratio and it was found that 87.3% of nickel and 88.8% of cobalt present in the limonitic ore could be extracted into the pregnant leach solution. Nevertheless, these results were found to be below the desired values. Therefore, the possible reasons of this behavior were investigated and the presence of hematite mineral in the limonitic ore was found to be the most probable one. Therefore, in order to dissolve the nickel and cobalt present in the hematite mineral, the additions of HCl, ferrous ions, cuprous ions and sulphur were tried, respectively and they were found to be beneficial in order to increase the degree of nickel and cobalt extractions.

The aim of this thesis study was to extract nickel and cobalt from Sivrihisar limonitic nickel laterite ore by high pressure acid leaching (HPAL) method under most economical operating parameters. Optimizing the conditions to yield a saleable quality mixed hydroxide product from the pregnant leach solution (PLS) was also investigated. To extract high amounts of nickel and cobalt from the laterite matrix / leaching duration, leaching temperature and sulfuric acid/ore ratio were studied at fixed conditions of -850 &micro / limonitic ore particle size and 40% solids concentration. The Sivrihisar limonitic nickel laterite ore was found to be readily leachable. It was found that 95.4% of Ni and 91.5% of Co were extracted at the optimized conditions of 235oC, 0.23 acid/ore ratio in 60 minutes. The real pregnant leach solution produced at the optimized conditions of HPAL was purified in two iron removal stages under the determined optimum conditions. Nearly all of the Al and Cr were removed from the PLS in the two stages of iron removal. Then, nickel and cobalt were taken out from the PLS in the form of mixed hydroxide precipitates (MHP) in two stages. A MHP 1 product containing 33.41 wt.% Ni, 2.93 wt.% Co was obtained with a Mn contamination of 3.69 wt.% at the optimized conditions of pH=7, 50oC and 60 minutes. The MHP 1 product was also contaminated with Fe (2.83 wt.%) since it could not be completely removed from the PLS without the critical losses of nickel and cobalt during the two iron removal stages.

Thesis (Ph.D.)--University of Western Australia, 2005.

Thèse (D.R.M.)--Université du Québec à Chicoutimi, 1997. / Document électronique également accessible en format PDF. CaQCU