Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercrítico

Detalhes bibliográficos
Autor(a) principal: Reisdörfer, Gustavo
Data de Publicação: 2019
Tipo de documento: Tese
Idioma: por
Título da fonte: Manancial - Repositório Digital da UFSM
Texto Completo: http://repositorio.ufsm.br/handle/1/20730
Resumo: Technological innovation has brought with it a number of electro-electronic equipment, but its disposal has been faster, making these wastes a concern, as to their destination and the supply of raw materials. These equipments contain several materials with potential added value that can be recycled and reused. This is the case of neodymium (Nd), present in Hard Disk Drivers (HDDs), which is a rare earth, and makes up the list of critical and risky raw materials. The objective of this work was to study the recovery of Nd from permanent neodymium ironboron (NdFeB) magnets obtained from discarded HDDs using leaching organic acids. Leaches were performed under atmospheric pressure conditions and with the use of supercritical CO2 extraction. In addition, the behavior of NdFeB powders, roasted and unroasted (heat treatment) was evaluated to verify the potential of neodymium selectivity in relation to iron. In the initial stage, the HDDs were manually disassembled and the magnets removed from it. The magnet demagnetization tests were performed at high temperatures (300, 350 and 400 °C) varying the time (15, 30, 45 and 60 min). After this step, the magnets were comminuted in a ball mill to obtain particles smaller than 400 µm. Roasting (heat treatment) was performed at a temperature of 900 °C for 480 min. Atmospheric leaches were conducted to assess the influence of temperature (30, 50, 70 and 90 °C), acid concentration (0.2 to 1.2 M), solid: liquid ratio (1:10, 1:20, 1:30 and 1:50) and the best leaching time (10, 20, 30, 60, 120, 180, 360, 720 and 900 min). Extraction with supercritical CO2 was performed using different pressures (80, 100, 120 and 150 bar), temperatures (60, 70, 80 and 90 °C) and extraction times (5 to 120 minutes). The results showed that the best conditions found for atmospheric leaching for both malic acid and citric acid were 90 °C, 1.0 M and 1:20. Regarding the reaction time, for the roasting NdFeB powder 100% Nd recovery was achieved with 360 min of malic acid leaching. Citric acid leaching showed good efficiency up to 30 minutes of experiment, reaching 72.8% Nd recovery. In the supercritical CO2 extraction for the unroasted NdFeB powder at 90 °C and 120 bar, Nd recovery of 99.4% and 50.5% after 30 min was observed using malic acid and citric acid, respectively. For roasted NdFeB powder the efficiencies were 99.5% and 30.6% after 120 min using malic and citric acid at 90 °C and 100 bar respectively. Thus, the use of supercritical CO2 is highly effective for recovering Nd from the unroasted powder with malic acid, allowing a significant reduction in extraction time compared to atmospheric leaching from 360 to 30 min.
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spelling Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercríticoRecovery of neodimium from secondary sources using organic acids and CO2 supercriticalFluido supercríticoReciclagemLixiviaçãoNeodímioTerras rarasÁcidos orgânicosHard disk drivesSupercritical fluidRecyclingLeachingNeodymiumRare earthOrganic acidsCNPQ::ENGENHARIAS::ENGENHARIA QUIMICATechnological innovation has brought with it a number of electro-electronic equipment, but its disposal has been faster, making these wastes a concern, as to their destination and the supply of raw materials. These equipments contain several materials with potential added value that can be recycled and reused. This is the case of neodymium (Nd), present in Hard Disk Drivers (HDDs), which is a rare earth, and makes up the list of critical and risky raw materials. The objective of this work was to study the recovery of Nd from permanent neodymium ironboron (NdFeB) magnets obtained from discarded HDDs using leaching organic acids. Leaches were performed under atmospheric pressure conditions and with the use of supercritical CO2 extraction. In addition, the behavior of NdFeB powders, roasted and unroasted (heat treatment) was evaluated to verify the potential of neodymium selectivity in relation to iron. In the initial stage, the HDDs were manually disassembled and the magnets removed from it. The magnet demagnetization tests were performed at high temperatures (300, 350 and 400 °C) varying the time (15, 30, 45 and 60 min). After this step, the magnets were comminuted in a ball mill to obtain particles smaller than 400 µm. Roasting (heat treatment) was performed at a temperature of 900 °C for 480 min. Atmospheric leaches were conducted to assess the influence of temperature (30, 50, 70 and 90 °C), acid concentration (0.2 to 1.2 M), solid: liquid ratio (1:10, 1:20, 1:30 and 1:50) and the best leaching time (10, 20, 30, 60, 120, 180, 360, 720 and 900 min). Extraction with supercritical CO2 was performed using different pressures (80, 100, 120 and 150 bar), temperatures (60, 70, 80 and 90 °C) and extraction times (5 to 120 minutes). The results showed that the best conditions found for atmospheric leaching for both malic acid and citric acid were 90 °C, 1.0 M and 1:20. Regarding the reaction time, for the roasting NdFeB powder 100% Nd recovery was achieved with 360 min of malic acid leaching. Citric acid leaching showed good efficiency up to 30 minutes of experiment, reaching 72.8% Nd recovery. In the supercritical CO2 extraction for the unroasted NdFeB powder at 90 °C and 120 bar, Nd recovery of 99.4% and 50.5% after 30 min was observed using malic acid and citric acid, respectively. For roasted NdFeB powder the efficiencies were 99.5% and 30.6% after 120 min using malic and citric acid at 90 °C and 100 bar respectively. Thus, the use of supercritical CO2 is highly effective for recovering Nd from the unroasted powder with malic acid, allowing a significant reduction in extraction time compared to atmospheric leaching from 360 to 30 min.A inovação tecnológica trouxe consigo inúmeros equipamentos eletroeletrônicos, porém seu descarte tem sido cada vez mais rápido, tornando estes resíduos uma preocupação, quanto à sua destinação e o próprio fornecimento de matérias-primas. Estes equipamentos contêm diversos materiais, com potencial valor agregado e que podem ser reciclados e reaproveitados. É o caso de neodímio (Nd), presente nos Hard Disk Drivers (HDDs), que é uma terra rara, e compõe a lista de matérias-primas críticas e com risco de fornecimento. O objetivo deste trabalho foi estudar a recuperação de Nd a partir de imãs permanentes de neodímio-ferro-boro (NdFeB) obtidos de HDDs descartados, utilizando ácidos orgânicos na lixiviação. As lixiviações foram realizadas em condições de pressão atmosférica e com o uso da extração com CO2 supercrítico. Além disso, o comportamento dos pós de NdFeB com e sem roasting (tratamento térmico) foram avaliados para verificar o potencial de seletividade do neodímio em relação ao ferro. Na etapa inicial, os HDDs foram desmontados manualmente e os imãs retirados do mesmo. Os testes para desmagnetização dos imãs foram realizados a altas temperaturas (300, 350 e 400 °C) variando o tempo (15, 30, 45 e 60 min). Após esta etapa, os imãs foram cominuídos em um moinho de bolas para obter partículas menores que 400 µm. O roasting (tratamento térmico) foi realizado a uma temperatura de 900 °C durante 480 min. As lixiviações atmosféricas foram conduzidas de modo a se avaliar a influência da temperatura (30, 50, 70 e 90 °C), da concentração do ácido (0,2 a 1,2 M), razão sólido:líquido (1:10, 1:20, 1:30 e 1:50) e o melhor tempo de lixiviação (10, 20, 30, 60, 120, 180, 360, 720 e 900 min). A extração com CO2 supercrítico foi realizada utilizando diferentes pressões (80, 100, 120 e 150 bar), temperaturas (60, 70, 80 e 90 °C) e tempos de extração (5 a 120 minutos). Os resultados mostraram que as melhores condições encontradas para as lixiviações atmosféricas, tanto para o ácido málico como para o ácido cítrico, foram 90 °C, 1,0 M e 1:20. Em relação ao tempo de reação, para o pó de NdFeB sem roasting chegou-se a 100% de recuperação de Nd com 360 min de lixiviação com ácido málico. A lixiviação com ácido cítrico apresentou boa eficiência até 30 minutos de experimento, chegando a 72,8% de recuperação de Nd. Na extração com CO2 supercrítico para o pó de NdFeB sem roasting, a 90 °C e 120 bar, observou-se uma recuperação de Nd de 99,4% e 50,5% após 30 min, utilizando ácido málico e ácido cítrico, respectivamente. Para o pó de NdFeB com roasting, as eficiências foram de 99,5% e 30,6% após 120 min, utilizando ácido málico e cítrico, respectivamente, a 90 °C e 100 bar. Assim, o uso de CO2 supercrítico mostra-se altamente eficaz para a recuperação de Nd do pó sem roasting com ácido málico, permitindo uma redução significativa do tempo de extração, quando comparado à lixiviação atmosférica, de 360 para 30 min.Universidade Federal de Santa MariaBrasilEngenharia QuímicaUFSMPrograma de Pós-Graduação em Engenharia QuímicaCentro de TecnologiaTanabe, Eduardo Hiromitsuhttp://lattes.cnpq.br/9778700143605069Bertuol, Daniel AssumpçãoCancelier, AdrianoSilveira, Christian Luiz daBorba, Fernando HenriqueSouza, Ricson Rocha deReisdörfer, Gustavo2021-04-29T18:51:52Z2021-04-29T18:51:52Z2019-11-28info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfhttp://repositorio.ufsm.br/handle/1/20730porAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2021-04-30T06:03:14Zoai:repositorio.ufsm.br:1/20730Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2021-04-30T06:03:14Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.none.fl_str_mv Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercrítico
Recovery of neodimium from secondary sources using organic acids and CO2 supercritical
title Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercrítico
spellingShingle Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercrítico
Reisdörfer, Gustavo
Fluido supercrítico
Reciclagem
Lixiviação
Neodímio
Terras raras
Ácidos orgânicos
Hard disk drives
Supercritical fluid
Recycling
Leaching
Neodymium
Rare earth
Organic acids
CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA
title_short Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercrítico
title_full Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercrítico
title_fullStr Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercrítico
title_full_unstemmed Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercrítico
title_sort Recuperação de neodímio a partir de fontes secundárias utilizando ácidos orgânicos e CO2 supercrítico
author Reisdörfer, Gustavo
author_facet Reisdörfer, Gustavo
author_role author
dc.contributor.none.fl_str_mv Tanabe, Eduardo Hiromitsu
http://lattes.cnpq.br/9778700143605069
Bertuol, Daniel Assumpção
Cancelier, Adriano
Silveira, Christian Luiz da
Borba, Fernando Henrique
Souza, Ricson Rocha de
dc.contributor.author.fl_str_mv Reisdörfer, Gustavo
dc.subject.por.fl_str_mv Fluido supercrítico
Reciclagem
Lixiviação
Neodímio
Terras raras
Ácidos orgânicos
Hard disk drives
Supercritical fluid
Recycling
Leaching
Neodymium
Rare earth
Organic acids
CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA
topic Fluido supercrítico
Reciclagem
Lixiviação
Neodímio
Terras raras
Ácidos orgânicos
Hard disk drives
Supercritical fluid
Recycling
Leaching
Neodymium
Rare earth
Organic acids
CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA
description Technological innovation has brought with it a number of electro-electronic equipment, but its disposal has been faster, making these wastes a concern, as to their destination and the supply of raw materials. These equipments contain several materials with potential added value that can be recycled and reused. This is the case of neodymium (Nd), present in Hard Disk Drivers (HDDs), which is a rare earth, and makes up the list of critical and risky raw materials. The objective of this work was to study the recovery of Nd from permanent neodymium ironboron (NdFeB) magnets obtained from discarded HDDs using leaching organic acids. Leaches were performed under atmospheric pressure conditions and with the use of supercritical CO2 extraction. In addition, the behavior of NdFeB powders, roasted and unroasted (heat treatment) was evaluated to verify the potential of neodymium selectivity in relation to iron. In the initial stage, the HDDs were manually disassembled and the magnets removed from it. The magnet demagnetization tests were performed at high temperatures (300, 350 and 400 °C) varying the time (15, 30, 45 and 60 min). After this step, the magnets were comminuted in a ball mill to obtain particles smaller than 400 µm. Roasting (heat treatment) was performed at a temperature of 900 °C for 480 min. Atmospheric leaches were conducted to assess the influence of temperature (30, 50, 70 and 90 °C), acid concentration (0.2 to 1.2 M), solid: liquid ratio (1:10, 1:20, 1:30 and 1:50) and the best leaching time (10, 20, 30, 60, 120, 180, 360, 720 and 900 min). Extraction with supercritical CO2 was performed using different pressures (80, 100, 120 and 150 bar), temperatures (60, 70, 80 and 90 °C) and extraction times (5 to 120 minutes). The results showed that the best conditions found for atmospheric leaching for both malic acid and citric acid were 90 °C, 1.0 M and 1:20. Regarding the reaction time, for the roasting NdFeB powder 100% Nd recovery was achieved with 360 min of malic acid leaching. Citric acid leaching showed good efficiency up to 30 minutes of experiment, reaching 72.8% Nd recovery. In the supercritical CO2 extraction for the unroasted NdFeB powder at 90 °C and 120 bar, Nd recovery of 99.4% and 50.5% after 30 min was observed using malic acid and citric acid, respectively. For roasted NdFeB powder the efficiencies were 99.5% and 30.6% after 120 min using malic and citric acid at 90 °C and 100 bar respectively. Thus, the use of supercritical CO2 is highly effective for recovering Nd from the unroasted powder with malic acid, allowing a significant reduction in extraction time compared to atmospheric leaching from 360 to 30 min.
publishDate 2019
dc.date.none.fl_str_mv 2019-11-28
2021-04-29T18:51:52Z
2021-04-29T18:51:52Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/doctoralThesis
format doctoralThesis
status_str publishedVersion
dc.identifier.uri.fl_str_mv http://repositorio.ufsm.br/handle/1/20730
url http://repositorio.ufsm.br/handle/1/20730
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
info:eu-repo/semantics/openAccess
rights_invalid_str_mv Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Universidade Federal de Santa Maria
Brasil
Engenharia Química
UFSM
Programa de Pós-Graduação em Engenharia Química
Centro de Tecnologia
publisher.none.fl_str_mv Universidade Federal de Santa Maria
Brasil
Engenharia Química
UFSM
Programa de Pós-Graduação em Engenharia Química
Centro de Tecnologia
dc.source.none.fl_str_mv reponame:Manancial - Repositório Digital da UFSM
instname:Universidade Federal de Santa Maria (UFSM)
instacron:UFSM
instname_str Universidade Federal de Santa Maria (UFSM)
instacron_str UFSM
institution UFSM
reponame_str Manancial - Repositório Digital da UFSM
collection Manancial - Repositório Digital da UFSM
repository.name.fl_str_mv Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)
repository.mail.fl_str_mv atendimento.sib@ufsm.br||tedebc@gmail.com
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