Thesis (Ph. D.)--Institute of Paper Science and Technology, Georgia Institute of Technology, 2003. / Includes bibliography.

Thesis (Ph. D.)--Institute of Paper Science and Technology, Georgia Institute of Technology, 2005. / Includes bibliography.

Thesis (MSc)--Stellenbosch University, 2015. / ENGLISH ABSTRACT: Lignocellulosic material is composed of three major macromolecule components i.e., cellulose, hemicelluloses and lignin. These components are chemically associated and directly linked to each other through covalent bonding which is scientifically denoted as lignin-carbohydrate complexes (LCCs) and their interaction is fundamentally important as to understand wood formation and reactivity during chemical and biological processing e.g. pulping and enzymatic hydrolysis. The association of lignin with polysaccharides (covalent linkages) has been surrounded by contradictions and controversy in several wood chemistry studies. These linkages exist in lignocellulosic materials from wood to herbaceous plants. In woody plants, they consist of ester and ether linkages through sugar hydroxyl to α-carbonyl of phenyl-propane unit on lignin. However, in herbaceous plants ferulic and p-coumaric acids are esterified to hemicelluloses and lignin respectively. In recent studies, the existence of the bonds has been shown by applying indirect analysis strategies which resulted to low yields and contaminations. The general aim of the current study was to isolate and fractionate LCCs from raw lignocellulosic materials (E. grandis and sugarcane bagasse) and corresponding processed materials (chemical pulps and water-insoluble residues (WIS)) in order to determine the chemical structure of the residual lignin associated with polysaccharides and how they affected industrial processing. The objective of the study is to compile a document that when the development of pulping and bio-ethanol bio-refinery will greatly depends on the detailed wood chemistry on how the components interact with each before and after hemicelluloses pre-extraction prior to pulping and steam explosion pre-treatment prior to enzymatic hydrolysis. The current study was focusing on understanding the effect LCCs isolated from two different industrial processing methods, i.e. pulping and enzymatic hydrolysis (EH). There were two lignocelluloses feedstocks used for pulping, i.e. Eucalyptus grandis and sugarcane bagasse whereas sugarcane bagasse was the only feedstock used for enzymatic hydrolysis. Hemicelluloses pre-extracted (mild alkali or dilute acid and autohydrolysis for sugarcane bagasse) pulps of Kraft or soda AQ from E. grandis and sugarcane bagasse were used to understand the effect of xylan pre-extraction prior to pulping on lignin-carbohydrate complexes has not been reported to the best knowledge of the primary author. Also prior to EH the material was subjected to two different treatment methods, i.e. steam explosion and ionic liquid fractionation in varying conditions. The study illustrated the types of extracted and fractionated LCCs from hemicelluloses pre-extracted pulps and WIS in comparison to the non-extracted pulps and reports from the literature. Lignin-carbohydrate complexes (LCCs) were isolated and fractionated by an inorganic method which yielded reasonable quantification quantities and no contamination and low yields for the hardwood compared to reports of using an enzymatic method. To the best knowledge of the authors, no work has been done on WIS material. The lignocelluloses were subjected to ball milling which was followed by a sequence of inorganic solvents swelling and dissolution into 2 fractions i.e. glucan-lignin and xylan-lignin-glucan. Characterisation of the isolated LCCs was made using a variety of analytical tools such as FTIR-PCA, HPLC, GPC and GC-MS. LCCs were evident when FTIR and HPLC studies were conducted. Residual lignin isolated from the lignocelluloses was assumed to be chemically bonded to carbohydrates and mostly to xylan. Approximately 60% and 30% of the lignin was linked to xylan while for the second and first fractions respectively. It is reported that lignin associated with xylan is more resistant and reduce the delignification process than when linked to glucan that is easily hydrolysable. With the FTIR and GPC analyses of LCC fractions, it was evident that the ester bonds of LCCs were destroyed through pre-extraction and pre-treatment, where this resulted to more cellulose being more accessible to alkaline pulping and enzymatic hydrolysis respectively. The linkages were either partially broken down or completely destroyed leading to significant changes of chemical structures. The polydispersity of the LCCs assisted in determining the structure of lignin, either existing as monolignols on the surfaces of fibres or a as complex two or three-dimensional structure that is linked to carbohydrates as the Mw increased or decreased. In general, these findings may have an important implication for the overall efficiency on bio-refinery. The molecular weights (Mw) of the extracted LCCs were measured by gel permeation chromatography. From the chromatograms, it was observed that the materials that were subjected to pre-processing prior to further processing, the Mw shifted to lower Mws regions. It was found that LCCs isolated from mild alkali pre-extracted pulps had high lignin syringyl to guaiacyl lignin contents than LCCs isolated from dilute acid pre-extracted pulps. High syringyl/guaiacyl ratio (S/G ratio) was an indication of low lignin content as a result of processing which will result to high product yields after downstream processing. The 5 average S/G ratio for the pulps from E. grandis and sugarcane bagasse was ranging between 1.1 to 19.01 and 1.4 to 18.16 respectively, while for the WIS-material generated from ionic liquid fractionated and steam exploded materials ranged from 3.29 to 9.27 and 3.5 to 13.3 respectively. The S/G ratios of the LCCs extracted from E. grandis and sugarcane bagasse pulps ranged from 0.42 to 2.39 and 0.041 to 0.31 was respectively while for the LCCs extracted from water-insoluble-solids (WIS) material generated from steam exploded material was from 4.87 to 10.40. The determination of S/G ratio is recommended for the LCC extraction and characterisation study as an evaluation of residual lignin in processed materials such as pulps and WIS. The obtained saccharifications were low, possibly due to the severity of the steam explosion pre-treatment and ionic liquid fractionation conditions which resulted on high accumulation of acetic acid and increased in cellulose crystallinity respectively. From quantitative analysis of the LCCs perspective it could be concluded that free lignin was present in mild alkali pre-extracted pulps than for the dilute acid pre-extracted pulps. / AFRIKAANSE OPSOMMING: Cellulose materiaal is saamgestel uit drie groot makromolekule komponente naamlik, sellulose, hemisellulose en lignien. Hierdie komponente is chemies verwante en direk met mekaar verbind deur kovalente binding wat wetenskaplik aangedui as lignien-koolhidraat komplekse (LCCs) en hul interaksie is fundamenteel belangrik as hout vorming en reaktiwiteit tydens chemiese en biologiese verwerking bv om te verstaan verpulping en ensiematiese hidrolise. Die vereniging van lignien met polisakkariede (kovalente verbindings) is omring deur teenstrydighede en omstredenheid in verskeie hout chemie studies. Hierdie skakeling bestaan in cellulose materiaal uit hout te kruidagtige plante. In houtagtige plante, hulle bestaan uit ester en eter bindings deur suiker hidroksiel te α-karboniel van feniel-propaan eenheid op lignien. Maar in kruidagtige plante ferulic en p-coumaric sure veresterd te hemisellulose en lignien onderskeidelik. In onlangse studies, het die bestaan van die bande is getoon deur die toepassing van indirekte analise strategieë wat gelei tot lae opbrengste en kontaminasie. Die algemene doel van die huidige studie was om te isoleer en fraksioneer LCCs van rou cellulose materiaal (E. grandis en suikerriet bagasse) en die ooreenstemmende verwerkte materiaal (chemiese pulp en water-oplosbare residue (WIS)) ten einde die chemiese struktuur van die te bepaal oorblywende lignien wat verband hou met polisakkariede en hoe hulle geaffekteerde industriële verwerking. Die doel van die studie is 'n dokument op te stel dat wanneer die ontwikkeling van verpulping en bio-etanol bio-raffinadery sal grootliks afhang van die gedetailleerde hout chemie oor hoe om die komponente met mekaar voor en na hemisellulose pre-onttrekking voor verpulping en stoom ontploffing pre-behandeling voor ensiematiese hidrolise. Die huidige studie was die fokus op die begrip van die effek LCCs geïsoleerd van twee verskillende industriële verwerking, maw verpulping en ensiematiese hidrolise (EH). Daar was twee lignocelluloses voerstowwe gebruik vir verpulping, dws Eucalyptus grandis en suikerriet bagasse terwyl suikerriet bagasse was die enigste grondstof gebruik vir ensiematiese hidrolise. Hemisellulose pre-onttrek (ligte alkali of verdunde suur en autohydrolysis vir suikerriet bagasse) pulp van Kraft of soda AQ van E. grandis en suikerriet bagasse is gebruik om die effek van Xylan pre-onttrekking te voor verstaan verpulping op lignien-koolhidraat komplekse het nie aan die berig is beste kennis van die primêre outeur. Ook voor EH die materiaal is onderworpe aan twee verskillende behandeling metodes, naamlik stoom ontploffing en ioniese vloeistof fraksionering in wisselende toestande. Die studie geïllustreer die tipes onttrek en gefractioneerd LCCs van hemisellulose pre-onttrek pulp en WIS in vergelyking met die nie-onttrek pulp en verslae van die literatuur. Lignien-koolhidraat komplekse (LCCs) is geïsoleer en gefraksioneer deur 'n anorganiese metode wat redelike kwantifisering hoeveelhede en geen besoedeling en lae opbrengste opgelewer vir die hardehout vergelyking met verslae van die gebruik van 'n ensiematiese metode. Na die beste kennis van die skrywers, het geen werk op WIS materiaal gedoen. Die lignocelluloses is onderworpe aan die bal maal wat gevolg is deur 'n reeks van anorganiese oplosmiddels swelling en ontbinding in 2 breuke dws glucan-lignien en Xylan-lignien-glucan. Karakterisering van die geïsoleerde LCCs is gemaak met behulp van 'n verskeidenheid van analitiese gereedskap soos FTIR-PCA, HPLC, GPC en GC-MS. LCCs was duidelik wanneer FTIR en HPLC studies is uitgevoer. Residuele lignien geïsoleerd van die lignocelluloses is aanvaar moet word chemies gebind aan koolhidrate en meestal te xylan. Ongeveer 60% en 30% van die lignien is gekoppel aan xylan terwyl dit vir die tweede en eerste breuke onderskeidelik. Dit is gerapporteer dat lignien wat verband hou met Xylan is meer bestand en die delignification proses as wanneer gekoppel aan glucane wat maklik hidroliseerbare verminder. Met die FTIR en GPC ontledings van LCC breuke, was dit duidelik dat die ester bande van LCCs is deur pre-ontginning en pre-behandeling, waar dit gelei tot meer sellulose om meer toeganklik te alkaliese verpulping en ensiematiese hidrolise onderskeidelik vernietig. Die skakeling is óf gedeeltelik afgebreek of heeltemal vernietig lei tot beduidende veranderinge van chemiese strukture. Die polydispersity van die LCCs bygestaan in die bepaling van die struktuur van lignien, hetsy bestaande as monolignols op die oppervlak van die vesel of 'n as komplekse twee of drie-dimensionele struktuur wat gekoppel is aan koolhidrate as die Mw vermeerder of verminder. In die algemeen, kan hierdie bevindinge het 'n belangrike implikasie vir die algehele doeltreffendheid op bio-raffinadery. Die molekulêre gewigte (Mw) die onttrek LCCs gemeet deur gelpermeasie- chromatografie. Van die chromatograms, was dit opgemerk dat die materiaal wat blootgestel is aan die pre-verwerking voor verdere verwerking, die Mw verskuif MWS streke te verlaag. Daar is gevind dat LCCs geïsoleerd van ligte alkali pre-onttrek pulp het hoë lignien syringyl lignien inhoud as LCCs geïsoleerd van verdunde suur vooraf onttrek pulp te guaiacyl. Hoë syringyl / guaiacyl verhouding (S/G-verhouding) was 'n aanduiding van 'n lae lignien inhoud as 'n resultaat van verwerking wat sal lei tot 'n hoë produk opbrengste ná stroomaf verwerking. Die gemiddelde S/G-verhouding vir die pulp van E. grandis en suikerriet bagasse was wat wissel tussen 1,1-19,01 en 1,4-18,16 onderskeidelik, terwyl dit vir die WIS-materiaal gegenereer uit ioniese vloeistof gefraksioneer en stoom ontplof materiaal het gewissel 3,29-9,27 en 3.5 13,3 onderskeidelik. Die S/G verhoudings van die LCCs onttrek uit E. grandis en suikerriet bagasse pulp gewissel 0,42-2,39 en ,041-,31 was onderskeidelik terwyl dit vir die LCCs onttrek uit water-oplosbare-vastestowwe (WIS) materiaal gegenereer uit stoom ontplof materiaal was van 4,87-10,40. Die bepaling van S/G-verhouding word aanbeveel vir die LCC ontginning en karakterisering studie as 'n evaluering van die oorblywende lignien in verwerkte materiaal soos pulp en WIS. Die verkry saccharifications was laag, moontlik as gevolg van die erns van die stoom ontploffing pre-behandeling en ioniese vloeistof fraksionering voorwaardes wat gelei op 'n hoë opeenhoping van asynsuur en vermeerder in sellulose kristalliniteit.

Orientadores: José Vicente Hallak d'Angelo, Marcelo Cardoso / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Química / Made available in DSpace on 2018-08-16T11:11:44Z (GMT). No. of bitstreams: 1 Emunds_RonaldLaauser_M.pdf: 1808008 bytes, checksum: cc469195b9e12b310096a07506d0138c (MD5) Previous issue date: 2010 / Resumo: Elementos não processáveis são definidos como sendo elementos cujos compostos não participam ativamente das diversas etapas do processo, porém seu acúmulo traz como conseqüência inúmeros distúrbios operacionais, tendo em vista a formação de compostos indesejáveis. O aumento das pressões ambientais sobre a indústria de um modo geral, fez com que a mesma iniciasse esforços no sentido de promover a diminuição das emissões de seus efluentes hídricos e gasosos, bem como a diminuição da captação de água, o que acarretou em acúmulo de elementos não processáveis. Este trabalho tem como objetivo estabelecer um balanço dos principais elementos não processáveis de uma fábrica de celulose avaliando o impacto dos resultados no processo. Análises para determinação da concentração dos elementos foram realizadas, além da validação do balanço elaborado mediante a comparação do mesmo com dados operacionais de processo. Verifica-se que a madeira utilizada na fabricação de celulose é a maior fonte destes elementos ao processo / Abstract: Non process elements are defined as the elements bonded to chemical compounds that do not actively participate on pulp production process steps, but the increasing concentration of these elements can cause many operational problems due to the formation of undesirable chemical compounds. The environmental stress from the society has forced industries to make efforts in order to close their process, minimizing effluent discharge and water consumption, causing the non process elements concentration to build up. The main objective of this work is to make a non process elements mass balance on a pulp Mill evaluating the extension of the non process elements concentration build up on the process. Chemical analysis were done to determine the non process elements concentrations in different points of the process done and mass balance data were confirmed with data taken from the process. The results have shown that wood is the main source of non process elements / Mestrado / Sistemas de Processos Quimicos e Informatica / Mestre em Engenharia Química

A biopolpação consiste no biotratamento de madeira por fungos degradadores de lignina como etapa prévia à produção de polpa celulósica. De uma forma geral, as madeiras biotratadas facilitam os processos posteriores de polpação. Entretanto, ensaios anteriores que avaliaram a biopolpação em escala piloto mostraram que é difícil estabelecer os cultivos de basidiomicetos de interesse livre de bolores contaminantes, já que não é fácil controlar perfeitamente a assepsia durante a inoculação. Para contribuir com o avanço do processo de biopolpação, este trabalho avaliou os cultivos mistos de Ceriporiopsis subvermispora e Phanerochaete chrysosporium sobre madeira de Eucalyptus grandis e Eucalyptus urograndis em regimes de incubação em temperaturas variáveis e em condições não assépticas. A estratégia de iniciar os cultivos em temperatura mais elevada (37°C) e depois manter as culturas em temperaturas variáveis de 27°C e 37°C se mostrou eficiente para inibir o crescimento de contaminantes indesejáveis tanto nos cultivos mistos como nos individuais de cada espécie avaliada. Para avaliar o efeito do biotratamento da madeira numa etapa subsequente de polpação quimiotermomecânica (CTMP) foi feito um estudo preliminar de ajuste de variáveis de polpação por refinamento mecânico de cavacos pré-digeridos com licor alcalino contendo sulfito de sódio. Os dados mostraram que é possível simular o rendimento e as características fisico-mecânicas de polpas industriais empregando uma etapa de pré-digestão dos cavacos com 6% de Na2SO3 e 3% de NaOH a 120°C por 2 h, seguida de desfibramento e refino em refinador de discos. As curvas de refino nesse processo CTMP mostraram que os cavacos biotratados deram origem a polpas com 300 mL de Freeness (CSF) consumindo menos energia do que o observado para o refino da madeira controle. As economias de energia chegaram a 60% em alguns casos, porém não foram maximizadas pelo efeito sinérgico do cultivo misto dos dois basidiomicetos em questão. Experimentos adicionais foram desenvolvidos empregando as espécies fúngicas Pycnoporus sanguineus e Trametes versicolor que foram eficientes para competir com contaminantes mesmo a 27oC. Neste caso, as economias de energia no processo CTMP subsequente somente foram obtidas com tempos mais longos de biotratamento (30 dias) e ainda assim os valores obtidos foram inferiores àqueles obtidos com as madeiras biotratadas por C. subvermispora e P. chrysosporium. Também a combinação das espécies C. subvermispora e Pleurotus ostreatus foi avaliada. Neste caso havia informação prévia da literatura indicando um efeito sinérgico da ação das duas espécies no que diz respeito a secreção da enzima manganês-peroxidase (MnP) e na degradação de lignina. Os resultados corroboraram que os cultivos mistos de C. subvermispora e P.ostreatus proporcionam maior produção de MnP do que os cultivos individuais de cada espécie. Por outro lado, P. ostreatus foi ineficiente para promover a redução do consumo de energia no processo CTMP subsequente. Os cultivos mistos também não proporcionaram efeito superior àquele observado com o cultivo individual de C. subvermispora. / Biopulping involves the wood biotreatment by selected white-rot fungi as a pretreatment step of conventional pulping processes. In general, the biotreated wood facilitates the subsequent pulping processes. However, previous studies on pilot scale showed that the process is susceptible to contamination by molds when the inoculation and biodegradation steps are carried out under non-aseptic conditions. To contribute with the biopulping progress this study evaluated the use of mixed cultures of Ceriporiopsis subvermispora and Phanerochaete chrysosporium acting on Eucalyptus grandis and Eucalyptus urograndis wood under non aseptic conditions where incubation was performed at varied temperatures. The simple strategy of initiating the incubation at 37°C for 3 days followed by a non-controlled step where the temperature could oscillate in the range of 27°C to 37°C proved to be efficient to inhibit the growth of contaminants. To evaluate the wood biotreatment effect in a subsequent step of chemithermomechanical pulping (CTMP), a preliminary study to adjust pulping variables was performed. Wood chips were predigested with alkaline-sulfite liquor, fibrillated and refined in a disk refiner. It was possible to simulate the yield and physico-mechanical properties of industrial CTMP pulps using a pre-digestion stage with 6% of Na2SO3 and 3% of NaOH at 120°C for 2 h. The refing curves in the CTMP process showed that the biotreated chips required less energy to reach 300 mL of Freeness (CSF) in the pulps than energy required to refine the control wood chips. Energy savings reached 60% in some cases, but were not maximized by the eventual synergic effect of the mixed cultures of the two basidiomycetes. Additional experiments were developed using the fungal species Trametes versicolor and Pycnoporus sanguineus that were efficient to compete with contaminants even at 27°C. In this case, the energy savings in the subsequent CTMP process were obtained only after long biotreatment times (30 days) and these values were lower than those obtained with the biotreated wood by C. subvermispora and P. chrysosporium. The combination C. subvermispora and Pleurotus ostreatus was also evaluated. In this case, previous literature information indicated some synergic effect of the two species regarding secretion of manganese peroxidase (MnP) and lignin degradation. The results corroborated that the mixed cultures of C. subvermispora and P.ostreatus provided an increased production of MnP compared to the individual cultivation of each species. On the other hand, P.ostreatus was not efficient to promote energy savings in the subsequent CTMP process. The mixed cultures did not provide increased energy savings as compared with the individual biotreatment with C. subvermispora.

A utilização de cana-de-açúcar para geração de açúcar, energia e etanol é uma das atividades mais importantes do Brasil. Esta intensa produção gera grandes quantidades de bagaço que podem ser utilizadas para aumentar a produção de etanol. Neste sentido, é de grande interesse técnico-científico o estudo de pré-tratamentos desta matéria prima, dentre os quais se inserem os processos de polpação. No presente trabalho buscou-se estudar a utilização da polpação hidrotrópica do bagaço de cana-de-açúcar para separação de seus principais componentes macromoleculares. Para tanto foram utilizados dois hidrótropos distintos, o benzoato de sódio e xilenossulfonato de sódio. Como referência, realizaram-se também polpações apenas com água, com soluções etanol/água e com soluções de hidróxido de sódio.O estudo foi realizado a partir de planejamento fatorial de experimentos, utilizando-se a influência das variáveis temperatura e tempo de reação. As respostas consideradas foram o rendimento de polpa e a quantidade de lignina residual. Este estudo exploratório revelou que o xilenossulfonato de sódio foi mais efetivo que o benzoato de sódio. Entretanto, o uso dos agentes hidrotrópicos foram menos eficiente quando comparado aos sistemas etanol/água e hidróxido de sódio. As ligninas extraídas nos processos de polpação hidrotrópica foram analisadas por diversas técnicas de caracterização. As ligninas extraídas na polpação com benzoato de sódio apresentaram menores massas molares quando comparado ao uso de xilenossulfonato de sódio. A análise das polpas obtidas nos diferentes processos revelou que as condições de maiores tempos e temperaturas produziram polpas com maiores índices de cristalinidade. / The production of sugar, energy and ethanol from sugar cane is one of the most important activities of Brazil and generates a enormous quantity of bagasse which can be used to increase the ethanol production. In this sense, the study of sugarcane bagasse is a very important task, in both technical and scientific approaches. Thus, the pre-treatment of sugar cane bagasse by using pulping/delignification processes constitutes a important step to recovery the main macromolecular components of the vegetal tissues of this raw material. In the present work it was studied the utilization of hydrotropic agents to promote the delignification of sugarcane bagasse. The study was carried out by using two different hydrotropes: sodium benzoate and sodium xylenosulfonate. As standard for comparison, it was also studied the pulping of sugarcane bagasse by using only water and ethanol/water and sodium hydroxide solutions. The pulping processes were carried out from factorial planning experiments employing two different levels (and a central point) for reaction time and temperature. As response it was determined the correspondents pulping yield and residual lignin contents. The results indicated that sodium xylenosulfonate was more effective than benzoate sodium in the promotion of the delignification. However, the utilization of hydrotropic systems were less efficient to promote the delignification, when compared with ethanol/water or sodium hydroxide aqueous solution. The lignins extracted in the pulping with sodium benzoate presented lower molar masses when compared with the use of sodium xylenesulfonate. The analysis of the pulps showed that the higher temperatures and reaction times produced pulps with higher crystallinity.

A indústria de papel e celulose convive com questões de adequação da oferta à demanda que influenciam na tomada de decisão em vários elos da cadeia produtiva. A pressão por baixos custos requer novos investimentos em tecnologia, normalmente associados ao processo e ao produto. Neste cenário, o objetivo do presente trabalho envolve o estudo da influência de variáveis de processo sobre a composição química da polpa e do licor preto, bem como sobre a formação de ácidos hexenurônicos, na polpação Kraft industrial de Eucalyptus. A metodologia proposta contemplou a realização de 36 polpações (em duplicata), sendo 3 níveis de álcali ativo (14, 17 e 19%), 2 níveis de sulfidez (20 e 30%) e 3 níveis de temperatura (150, 160 e 170oC). As polpas obtidas foram analisadas quanto à composição química, alvura e viscosidade. Os licores gerados no processo foram analisados quanto à composição química e por espectroscopia no infravermelho. Os resultados obtidos indicaram que uma maior sulfidez gera um menor teor de ácidos hexenurônicos na polpa independentemente da carga de álcali empregada. A temperatura exerce forte influência na geração destes ácidos, sendo que a 160°C foram geradas as maiores concentrações de ácidos hexenurônicos na polpa. Ainda com relação à temperatura, observou-se que o número kappa da polpa é reduzido quando a temperatura é elevada. A carga de álcali ativo leva a um aumento na quantidade de ácidos hexenurônicos gerados na polpa e a uma redução do número kappa. A alvura da polpa foi mais elevada para menores teores de ácidos hexenurônicos. A utilização da técnica de espectroscopia no infravermelho não se mostrou aplicável para a determinação dos teores de lignina nos licores de cozimento. / The pulp and paper industries have to manage issues concerning the offer of their products and the needs of different markets. To get this goal several important aspects of the productive chain has to be considered. The achievement of low costs of production requires investments in technologies for both processes and products. In this context, the aim of the present work involves the study of the influence that process parameters exerts in the chemical composition of the pulps and liquors, as well as hexenuronic acids generated in the industrial kraft pulping of Eucalyptus. The experimental work consisted in a factorial planning designed pulping reactions. 36 cookings were performed (in duplicate) with 3 levels of active alkali (14, 17 e 19%), 2 levels of sulfidity (20 e 30%) and 3 levels of temperature (150, 160 e 170oC). The obtained pulps were analyzed in relation to their chemical composition, brightness and viscosity. The black liquors were also analyzed by infrared spectroscopy. The results indicated that the higher sulfidity produced pulps with the lower content of hexenuronic acids, independently of the charge of active alkali employed in the process. The temperature of the pulping process exerted a strong influence in the production of hexenuronic acids, mainly at 160°C. Still considering the temperature, it was observed that occurs a reduction of the kappa number at higher temperatures. The active alkali charge produced an increase in the amount of hexenuronic acids and a decrease in the kappa number of the pulps. It was also observed an increase in the brightness for the pulps with lower amount of hexenuronic acids. Infrared spectroscopy showed not feasible results considering the determination of lignin content in the pulping liquors.

A crucial parameter in the production of mechanical pulp through refining is energy consumption. Although low consistency (LC) refining has been shown to be more energy efficient than conventional high consistency refining, the degradation of mechanical properties of the end-product paper due to fiber cutting has limited the widespread adoption of LC refining. In conventional control strategies, the onset of fiber cutting is determined by post-refining measurement of pulp properties which does not enable rapid in-process adjustment of refiner operation in response to the onset of fiber cutting. In this dissertation, we exploit a piezoelectric force sensor to detect the onset of fiber cutting in real time. Detection of the onset of fiber cutting is potentially beneficial in low consistency refining as part of a control system to reduce fiber cutting and increase energy efficiency. The sensor has a probe which replaces a short length of a refiner bar, enabling measurement of normal and shear forces applied to pulp fibers by the refiner bars. The custom-designed sensors are installed in an AIKAWA pilot-scale 16-in. single-disc refiner at the Pulp and Paper Centre at the University of British Columbia. Trials were run using different pulp furnishes and refiner plate patterns at differing rotational speeds and a wide range of plate gaps. Pulp samples were collected at regular intervals and the pulp and paper properties were measured. We observe distinct transitions in the parameters that characterize the distributions of peak normal and shear forces which consistently correspond to the onset of fiber cutting. In addition, the analysis of the power spectrum of the sensor data shows that the magnitude of the dominant frequency can be used as an indicator of fiber cutting. The power of the time domain signal of the normal force is shown to be the most reliable and consistent indication of the onset of fiber cutting. This parameter consistently identifies the onset of fiber cutting, as determined by fiber length data, for all tested pulp furnishes and plate patterns. In addition, we investigate the effect of pulp furnish and plate pattern on bar forces in LC refining. For tested pulp furnishes and at all plate gaps, the plate with higher bar edge length (which has smaller bar width and groove width) results in lower mean peak normal and shear forces but higher mean coefficient of friction. Moreover, at the onset of fiber cutting, the mean peak normal force of softwood pulp is higher than that for hardwood pulp. Our results also show that the mean coefficient of friction at the onset of fiber cutting is a function of plate gap, pulp furnish, and plate pattern. / Graduate / 2019-01-09

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