Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume

Detalhes bibliográficos
Autor(a) principal: Cunha, Graziele da Costa
Data de Publicação: 2014
Tipo de documento: Tese
Idioma: por
Título da fonte: Repositório Institucional da UFS
Texto Completo: https://ri.ufs.br/handle/riufs/3474
Resumo: Alumina nanoparticles are among the most important materials in the ceramic industry due to their variety of potential applications. Currently, there is a search for more economic, eco friendly and efficient routes. In this way, the present work proposes the use of complexing capacity of water rich in Natural Organic Matter (NOM) (24mg L -1 COD) to synthesize nanostructured pigment, based on doped alumina with chrome ions obtained from reagents with high degree of purity of from solid and liquid residues from the tannery industry. In the synthesis process, many parameters were controlled, such as the pH of the precursor solution. It was observed that this parameter played a significant role on the production of particles with small sizes. Using pH 4,0 undoped alfa-alumina was obtained after calcination at 1000ºC/4h. This temperature is at least 200ºC lower than those reported for the production of alumina using sol-gel or Pechini routes. For doped alumina, the calcination conditions were 1100°C/4h, showing that doping had an influence over the phase transition temperature. The XRF data revealed that Cl, Si, Zn, S and Cu are the main impurities in the pure sample, as well as in the sample doped with chrome salts with high purity. On the other hand, the samples doped with recycled chrome contained compounds of calcium and sodium chloride, depending on the type of residue used (solid or liquid). Data from XANES proved that the valence of Cr in the alumina structure is influenced by the degree of purity of the dopant. Micrographs suggest the obtention of structures with spherical morphology, with particle sizes varying from 45 nm to 56 nm, showing that the origin of NOM, its molecular size, water storage conditions and the purity of the dopant has not significantly influenced the morphology or the average size of the particles. The PL and XEOL emission spectra chrome high purity doped alumina revealed a main band near 700 nm, and a dependency on the concentration of chromophore ion, as expected. However, for synthesized samples using recycled chrome ions, neither emission was observed. The physico-chemical and bacteriologic characterization of the recycled water showed that it attends to the standards required from the Brazilian health ministry. Furthermore, during the leaching tests the total chrome concentration was below the equipment detection limits.
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spelling Cunha, Graziele da CostaMacedo, Zélia Soareshttp://lattes.cnpq.br/29777645002817852017-09-26T11:53:11Z2017-09-26T11:53:11Z2014-08-01CUNHA, Graziele da Costa. Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume. 2014. 167 f. Tese (Doutorado em Engenharia de Materiais) - Universidade Federal de Sergipe, São Cristóvão, 2014.https://ri.ufs.br/handle/riufs/3474Alumina nanoparticles are among the most important materials in the ceramic industry due to their variety of potential applications. Currently, there is a search for more economic, eco friendly and efficient routes. In this way, the present work proposes the use of complexing capacity of water rich in Natural Organic Matter (NOM) (24mg L -1 COD) to synthesize nanostructured pigment, based on doped alumina with chrome ions obtained from reagents with high degree of purity of from solid and liquid residues from the tannery industry. In the synthesis process, many parameters were controlled, such as the pH of the precursor solution. It was observed that this parameter played a significant role on the production of particles with small sizes. Using pH 4,0 undoped alfa-alumina was obtained after calcination at 1000ºC/4h. This temperature is at least 200ºC lower than those reported for the production of alumina using sol-gel or Pechini routes. For doped alumina, the calcination conditions were 1100°C/4h, showing that doping had an influence over the phase transition temperature. The XRF data revealed that Cl, Si, Zn, S and Cu are the main impurities in the pure sample, as well as in the sample doped with chrome salts with high purity. On the other hand, the samples doped with recycled chrome contained compounds of calcium and sodium chloride, depending on the type of residue used (solid or liquid). Data from XANES proved that the valence of Cr in the alumina structure is influenced by the degree of purity of the dopant. Micrographs suggest the obtention of structures with spherical morphology, with particle sizes varying from 45 nm to 56 nm, showing that the origin of NOM, its molecular size, water storage conditions and the purity of the dopant has not significantly influenced the morphology or the average size of the particles. The PL and XEOL emission spectra chrome high purity doped alumina revealed a main band near 700 nm, and a dependency on the concentration of chromophore ion, as expected. However, for synthesized samples using recycled chrome ions, neither emission was observed. The physico-chemical and bacteriologic characterization of the recycled water showed that it attends to the standards required from the Brazilian health ministry. Furthermore, during the leaching tests the total chrome concentration was below the equipment detection limits.As nanopartículas de alumina estão entre os materiais mais importantes na indústria cerâmica por conta de suas diversas aplicações. Atualmente há uma busca por rotas mais econômicas, eco-amigáveis e eficientes. Assim, o presente trabalho propõe o uso da capacidade complexante da água rica em Matéria Orgânica Natural (MON) (24 mg L-1 carbono orgânico dissolvido) para sintetizar pigmento nanoestruturado a base de alumina dopada com íons cromo de elevado grau de pureza (P.A) e com íons obtidos a partir dos resíduos sólidos e líquidos provenientes da industria de curtume. No processo de síntese, avaliou-se vários parâmetros, porém o controle do pH da solução inicial foi o que mais influenciou a obtenção da alfa-alumina nanoestruturada. Os resultados de DRX comprovam a obtenção da fase única alfa-alumina para as amostras obtidas no pH 4,0 e calcinadas 1000°C/4h para alumina não dopada, essa temperatura é pelo menos 200°C inferior à empregada nas principais rotas tradicionais (sol-gel e Pechini). Para a alumina dopada, essa temperatura foi 1100°C/4h. Os dados de XRF revelaram que as principais impurezas presentes na alumina não dopada e dopada com ions cromo P.A são os sequintes: Cl, Si, S e Zn. Enquanto, que para as amostras dopadas com íons cromo reciclados, as pricipais impurezas foram: os compostos de cálcio para as amostras obtidas empregando o residuo liquido e cloreto de sódio para o residuo sólido. O resíduo sólido apresentou características melhores para utilização em pigmentos cerâmicos. Os dados de XANES comprovam a presença de Cr(VI), porém é possivel obter Al2O3:Cr livre dessa valência. As micrografias sugerem a obtenção de estruturas com morfologia esférica, com tamanho das particulas em torno de 56 nm. Os espectros de emissão PL e XEOL da alumina dopada com cromo P.A revelam uma banda principal de emissão em aproximadamente 700 nm, sendo que a eficiencia fotoluminescente e radioliminescente mostrou-se dependente da concentração do ion cromoforo. Porém, para as amostras sintetizadas usando os ions de cromo reciclados verificou-se a supressão dessas propriedades. A caracterização físico-química e bacteriológica da água reciclada mostra que a mesma atende aos padrões de potabilidade exigidos pela Portaria 2914. Ademais, os testes de lixiviação demostraram que não houve liberação do cromo incorporado na matriz da alumina.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de SergipePós-Graduação em Ciência e Engenharia de MateriaisUFSBRAlfa-aluminaMONReciclagemNanopigmento cerâmicoMateriaisCourosMateriais nanoestruturadosReaproveitamento (Sobras, refugos, etc.)CromoÓxido de alumínioLuminescênciaAlpha-aluminaRecycleChromiumCeramic pigmentCNPQ::ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICASíntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtumeinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSTEXTGRAZIELE_COSTA_CUNHA.pdf.txtGRAZIELE_COSTA_CUNHA.pdf.txtExtracted texttext/plain302815https://ri.ufs.br/jspui/bitstream/riufs/3474/2/GRAZIELE_COSTA_CUNHA.pdf.txt6b790f6eb0a849bd76941eafda9cdf9fMD52THUMBNAILGRAZIELE_COSTA_CUNHA.pdf.jpgGRAZIELE_COSTA_CUNHA.pdf.jpgGenerated Thumbnailimage/jpeg1337https://ri.ufs.br/jspui/bitstream/riufs/3474/3/GRAZIELE_COSTA_CUNHA.pdf.jpg4d3201cb1cb33a587dd082ce58fb2a3fMD53ORIGINALGRAZIELE_COSTA_CUNHA.pdfapplication/pdf5212940https://ri.ufs.br/jspui/bitstream/riufs/3474/1/GRAZIELE_COSTA_CUNHA.pdfab86beffbe746b8aa9ff5cba69dabc9eMD51riufs/34742017-11-27 21:31:19.808oai:ufs.br:riufs/3474Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2017-11-28T00:31:19Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false
dc.title.por.fl_str_mv Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume
title Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume
spellingShingle Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume
Cunha, Graziele da Costa
Alfa-alumina
MON
Reciclagem
Nanopigmento cerâmico
Materiais
Couros
Materiais nanoestruturados
Reaproveitamento (Sobras, refugos, etc.)
Cromo
Óxido de alumínio
Luminescência
Alpha-alumina
Recycle
Chromium
Ceramic pigment
CNPQ::ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
title_short Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume
title_full Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume
title_fullStr Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume
title_full_unstemmed Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume
title_sort Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume
author Cunha, Graziele da Costa
author_facet Cunha, Graziele da Costa
author_role author
dc.contributor.author.fl_str_mv Cunha, Graziele da Costa
dc.contributor.advisor1.fl_str_mv Macedo, Zélia Soares
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/2977764500281785
contributor_str_mv Macedo, Zélia Soares
dc.subject.por.fl_str_mv Alfa-alumina
MON
Reciclagem
Nanopigmento cerâmico
Materiais
Couros
Materiais nanoestruturados
Reaproveitamento (Sobras, refugos, etc.)
Cromo
Óxido de alumínio
Luminescência
topic Alfa-alumina
MON
Reciclagem
Nanopigmento cerâmico
Materiais
Couros
Materiais nanoestruturados
Reaproveitamento (Sobras, refugos, etc.)
Cromo
Óxido de alumínio
Luminescência
Alpha-alumina
Recycle
Chromium
Ceramic pigment
CNPQ::ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
dc.subject.eng.fl_str_mv Alpha-alumina
Recycle
Chromium
Ceramic pigment
dc.subject.cnpq.fl_str_mv CNPQ::ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
description Alumina nanoparticles are among the most important materials in the ceramic industry due to their variety of potential applications. Currently, there is a search for more economic, eco friendly and efficient routes. In this way, the present work proposes the use of complexing capacity of water rich in Natural Organic Matter (NOM) (24mg L -1 COD) to synthesize nanostructured pigment, based on doped alumina with chrome ions obtained from reagents with high degree of purity of from solid and liquid residues from the tannery industry. In the synthesis process, many parameters were controlled, such as the pH of the precursor solution. It was observed that this parameter played a significant role on the production of particles with small sizes. Using pH 4,0 undoped alfa-alumina was obtained after calcination at 1000ºC/4h. This temperature is at least 200ºC lower than those reported for the production of alumina using sol-gel or Pechini routes. For doped alumina, the calcination conditions were 1100°C/4h, showing that doping had an influence over the phase transition temperature. The XRF data revealed that Cl, Si, Zn, S and Cu are the main impurities in the pure sample, as well as in the sample doped with chrome salts with high purity. On the other hand, the samples doped with recycled chrome contained compounds of calcium and sodium chloride, depending on the type of residue used (solid or liquid). Data from XANES proved that the valence of Cr in the alumina structure is influenced by the degree of purity of the dopant. Micrographs suggest the obtention of structures with spherical morphology, with particle sizes varying from 45 nm to 56 nm, showing that the origin of NOM, its molecular size, water storage conditions and the purity of the dopant has not significantly influenced the morphology or the average size of the particles. The PL and XEOL emission spectra chrome high purity doped alumina revealed a main band near 700 nm, and a dependency on the concentration of chromophore ion, as expected. However, for synthesized samples using recycled chrome ions, neither emission was observed. The physico-chemical and bacteriologic characterization of the recycled water showed that it attends to the standards required from the Brazilian health ministry. Furthermore, during the leaching tests the total chrome concentration was below the equipment detection limits.
publishDate 2014
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identifier_str_mv CUNHA, Graziele da Costa. Síntese de alfa-alumina nanoestruturada não dopada e dopada com cromo a partir da matéria orgânica natural e resíduos da indústria de curtume. 2014. 167 f. Tese (Doutorado em Engenharia de Materiais) - Universidade Federal de Sergipe, São Cristóvão, 2014.
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