The depletion of fossil fuels and the need to deal with climate change lead to an increasing interest in renewable resources. Lignocellulosic biomass in general, and agricultural residues in particular, could serve as an excellent starting material for the production of cellulose, basic chemicals, lignin and bioethanol in a biorefinery framework as they are abundant, do not compete with food production and are distributed worldwide. Two factors considerably influence the composition and properties of biorefinery products: biomass feedstock and pretreatment process. Their influence on the separability of raw material into a carbohydrate and lignin fraction as well as the composition and properties of these products are objectives of this study. Hereby, the focus is on lignin, as its structure is particularly dependent on the aforementioned factors complicating its further utilisation. Different agricultural biomass namely barley straw, coconut shell powder, hemp shives, horse manure, maize straw, miscanthus, oat husk, pretreated alfalfa, rape straw, sunflower stalks, tomato stalks and wheat straw were investigated regarding their suitability for lignocellulose separation using alkaline soda pulping. Best separation into a carbohydrate and lignin fraction was achieved for pretreated alfalfa, miscanthus, wheat and barley straw. The purity of the obtained lignin fractions varied in the wide range of 57% klason-lignin content for sunflower stalks and 81% for pretreated alfalfa prior to further purification by dialysis. Lignin fractions were characterised by means of FTIR spectroscopy, elementary analysis, thioacidolysis, size-exclusion-chromatography, thermodesorption, differential scanning calorimetry and different wet chemical methods for determination of functional groups. Lignins could be classified into groups, within which they show similar characteristics: (A) horse manure, rape straw, (B) sunflower stalks, tomato stalks, (C) barley-, maize- and wheat straw and (D) hemp shives, miscanthus. In addition, promising lignin candidates were found for several applications. Thus, by screening different agricultural residues, it is possible to choose a specific raw material, in order to produce lignin with desired properties and functionalities. The effect of the pretreatment process was studied based on wheat straw. It was subjected to conventional alkaline pulping, microwave-assisted alkaline pulping and organosolv pulping using formic acid and hydrogen peroxide. Pulping parameters were varied in order to attain best possible separation into a carbohydrate and lignin fraction. Of the varied parameters the concentration of both sodium hydroxide and formic acid has the highest impact on yield and purity of the products for alkaline and organosolv pulping, respectively. It additionally influences the content of functional groups of the lignin fraction and is hence, an important parameter for lignin customisation for subsequent utilisation. Furthermore, the possibility of reducing pulping time by using microwave-assisted pulping instead of conventional alkaline pulping is promising, as the obtained carbohydrate fraction has a low intrinsic viscosity, which may enhance enzymatic hydrolysis.

The control of batch pulp digesters is hampered by insufficient measurements as well as nonlinearity and weak correlation between consecutive cooks. This makes a model-based approach to control attractive. Due to the age of the industry, many legacy controllers are in place on digesters around the world. The theoretical variance obtained by Monte Carlo modelling of a new controller is used as a benchmark for performance comparison between an old control system (S-factor) and a new model based controller developed by the University of Pretoria (the UP controller). This study covers the development of the controller, Monte Carlo modelling of the old and new controllers and in-situ testing of the UP controller on an operating digester. During Monte Carlo simulation, the UP controller outperformed the legacy controller, obtaining a theoretical overall variance of 3,07 (which will be used as the baseline for performance measurement) while also showing larger responses to tuning factors. The S-factor performed at 6,8 times the theoretical optimum variance during in situ testing, while the UP controller performed at 3,9 times the theoretical optimum (43% better than the S-factor controller). An average error 90% lower than that of the S-factor controller was obtained when using the UP controller. Additional benefits of the new controller include easy inclusion of new measurements and clear relations between the tuning parameters used and the conditions in the digester. / Dissertation (MEng (Control))--University of Pretoria, 2003. / Chemical Engineering / unrestricted

Thesis (PhD)--Stellenbosch University, 2013. / ENGLISH ABSTRACT: The extraction of hemicelluloses prior to pulping that would have been dissolved in black liquor during pulping process, is an attractive alternative for pulp and paper mills as they, in addition to their core products, can increase their revenue by producing biofuels, biopolymers, paper additives and other chemicals. However, the amount of hemicelluloses extracted will be limited by the requirement to maintain pulp yield and pulp quality in comparison to existing pulping processes. In the present study, mild alkaline (NaOH) and dilute sulphuric acid conditions were used to extract hemicelluloses from Eucalyptus grandis, giant bamboo (Bambusa balcooa) and sugarcane (Saccharum officinarum) bagasse (SCB) prior to kraft or sodaAQ pulping processes. The effects of catalyst concentration, temperature and reaction time on hemicelluloses pre-extraction were studied, using a statistical experimental design to investigate conditions under which hemicelluloses could be extracted prior to alkaline pulping with minimal interference on cellulose (glucan) content. Subsequently, selected pre-extracted materials were subjected to kraft or sodaAQ pulping to evaluate the effect of the hemicelluloses pre-extraction on cooking chemicals, pulp yield and properties. This study also included evaluation of hot water hemicelluloses pre-extraction of SCB as it was part of a dilute sulphuric acid experimental design. The pulp yield, cooking chemicals and handsheet strength properties were compared with those obtained from kraft or sodaAQ pulping of non extracted raw materials. The results showed that alkaline pre-extraction options investigated preserves the pulp yield with minimal effect on handsheet strength properties depending on the choice of the subsequent pulping method while a fraction of xylan was extracted in polymeric form. In addition, less active alkali was required to delignify the xylan extracted materials. The integration of hemicelluloses pre-extraction by alkaline methods into a kraft pulping process was preferred for giant bamboo and E. grandis since it maintained pulp yields at desired industrial levels of 50%, and pulps within a bleachable kappa number range. Another advantage observed was the reduction in total cooking active alkali required to delignify alkaline extracted giant bamboo or E. grandis by 8or 3 percentage points respectively. However, the compromise to maintain the pulp yield was obtained when only 13.6% or 12.4% polymeric xylan was solubilised from giant bamboo or E. grandis respectively. Slight improvement in burst index of the handsheet was observed for extracted giant bamboo. On the other hand, pulp viscosity was increased by 13% due to the removal of low molecular weight hemicelluloses, while the breaking strength of the handsheet was also increased by 8.9% for pulps produced from extracted E. grandis. In the case of sugarcane bagasse, hemicelluloses pre-extraction by alkaline methods integrated well with the sodaAQ pulping process. It enabled a xylan recovery of 69.1%, while providing pulp with higher screened pulp yield (45.0%), with an advantageous decrease in kappa number (15.5). The handsheet tear index was superior without reduction in viscosity compared to pulp produced from non extracted SCB. On the contrary, results obtained from optimised dilute sulphuric acid pre-extraction of all the tested feedstocks were found to negatively impact subsequent kraft or sodaAQ pulping processes resulting in lower pulp yields and poorer strengths properties. Nonetheless, the differences were better when sodaAQ pulping was used compared to kraft pulping. SodaAQ protects the carbohydrates against the peeling reaction under alkaline medium. Conversely, pre-extraction of SCB with hot water resulted in low concentration of xylooligomers (5.7%), while the subsequent sodaAQ pulping resulted in no pulp yield reduction. The tear index and optical brightness of the handsheet papers produced from hot water extracted SCB were slightly improved while the breaking length, tensile and burst indexes were similar to those of pulps produced from non extracted SCB fibres. Of equal importance were the observed higher tear and burst indexes of handsheets produced from giant bamboo compared to E. grandis for both extracted and non extracted materials prepared under similar pulping processes. The advantage of bamboo was due to the larger fibre length and different morphological properties to those of hardwoods. However, the pulps produced from giant bamboo showed higher kappa numbers than those pulps produced from E. grandis due to the high condensation behaviour of bamboo lignins under alkaline conditions. Higher kappa numbers explained the higher demand for subsequent bleaching chemicals. In conclusion, the pulp mill biorefinery concept through hemicelluloses pre-extraction with NaOH can be achieved with modified kraft pulping or the sodaAQ pulping processes, but it depends on the type of raw material, extraction method and quality and performance requirements of a particular paper. The low pulping chemicals demand, comparable pulp yields and the improvement in some physico-chemical properties of the pulps from preextracted materials were observed. Furthermore, owing to xylan pre-extraction a larger amount of (extracted) material could be loaded into the digester as when non-extracted materials were used. / AFRIKAANSE OPSOMMING: Ekstraksie van hemiselluloses wat tydens verpulping in die swartloog opgelos word, bied ‘n aantreklike alternatief aan pulp- en papiermeulens om, addisioneel tot hul hoofprodukte, hul inkomste deur die vervaardiging van biobrandstowwe, biopolimere, papierbymiddels en ander chemikalië, daardeur te kan verhoog. Die hoeveelheid hemiselluloses wat ge-ekstraheer kan word, sal egter beperk word deur die vereiste dat pulpopbrengs en –kwaliteit tydens bestaande verpulpingsprosesse gehandhaaf moet word. In hierdie ondersoek is matige alkaliese (NaOH) en verdunde swawelsuurtoestande gebruik om hemiselluloses vóór kraft- of natriumantrakinoonverpulping uit Eucalyptus grandis, reuse bamboes (Bambusa balcooa) en suikerriet (Saccharum officinarum) bagasse, mee te ekstraheer. Die invloed van katalisatorkonsentrasie, temperatuur en reaksietyd is mbv ‘n statistiese, eksperimentele ontwerp ondersoek om die toestande te bepaal waaronder hemiselluloses, met minimale effek op die sellulose (glukaan) –inhoud, vóór alkaliese verpulping ge-ekstraheer kan word. Die pre-ge-ekstraheerde materiale, met hoë glukaan- en voldoende hemisellulosesinhoud, is vervolgens aan kraft- en natriumantrakinoonverpulping onderwerp om die invloed van pre-ekstraksie van hemiselluloses op die verpulpingsreagense, pulpopbrengs en - eienskappe vas te stel. Hierdie studie het ook die evualering van warmwater hemisellulosespre-ekstraksie van suikerrietbagasse, wat deel is van ‘n verdunde swawelsuur eksperimentele uitleg, ingesluit. Pulpopbrengs, die hoeveelheid verpulpingsreagense en handveleienskappe van dieselfde materiale wat nie vooraf ge-ekstraheer is nie, is vergelyk. Die resultate toon dat alkaliese pre-ekstraksie metodes wat ondersoek is die pulpopbrengs met minimale effek op handvel sterkte-eienskappe afhangende van die keuse van daaropvolgende pulpmetode kon handhaaf terwyl ‘n fraksie van xilaan in polimeriese vorm ge-ekstraheer is. Addisioneel, is minder aktiewe alkali benodig om die xilaan ge-ekstraheerde materiale te delignifiseer. Die integrasie van hemisellulosespre-ekstraksie dmv alkaliese metodes tydens ‘n kraft verpulpingsproses is vir reuse bamboes en E. grandis verkies omdat pulpopbrengste op ideale industriële vlakke van 50% gehandhaaf en is en pulp in ‘n bleikbare kappa nommergebied interval kon lewer. ‘n Verdere voordeel wat waargeneem is was die vermindering in die totale gekookte aktiewe alkali benodig vir reuse bamboes of E. grandis met 8 of 3 persentasiepunte onderskeidelik. Die kompromie om die pulpopbrengs te handhaaf is verkry toe slegs 13.6% of 12.4% polimeriese xilaan opgelos is vanuit reuse bamboes of E. grandis onderskeidelik. ‘n Effense verbetering in bars-indeks van die handvelle is waargeneem vir ge-ekstraheerde reuse bamboes. Pulpviskositeit het met 13% gestyg agv die verwydering van die lae molekulêre massa hemiselluloses, terwyl breeksterkte van handvelle ook met 8.9% toegeneem het vir pulp verkry uit pre-gekstraheerde E. grandis. NaOH pre-ekstraksie van 69.1% xilaan (droë massa) uit suikerriet bagasse (SCB) het ‘n hoër natriumantrakinoon, gesifte pulpopbrengs gelewer (45.0%) met ‘n verbeterde afname in kappa-getal (15.5) en uitstekende skeursterkte sonder verlaging in viskositeit, soos vergelyk met nie-ge-ekstraheerde suikkerrietbagasse. Daarteenoor het die resultate verkry met die geoptimeerde verdunde swawelsuur preekstraksie van al die getoetste rumateriale getoon om‘n negatiewe effek te gehad het op die daaropvolgende kraft- of natriumantrakinoonverpulping dws het laer pulpopbrengste en swakker sterkte-eienskappe opgelewer. Die verskille was nietemin kleiner toe natriumantrakinoonverpulping ipv kraftverpulping gebruik is. Antrakinoon beskerm die koolhidrate teen die afskilreaksie in alkaliese medium. Daarteenoor het pre-ekstraksie van suikerrierbagasse met warm water tot 'n lae hoeveelheid (5.7%) xilaanoligomere gelei, terwyl die daaropvolgende natriumantrakinoonverpulping geen verlaging in pulpopbrengs veroorsaak het nie. Skeursterkte en optiese helderheid van handvelle wat uit warm water ge-ekstraheerde suikerrietbagasse vervaardig is, het ietwat verbeter terwyl breek-, trek- en barssterkte dieselfde was as van suikerrietbagasse pulp wat nie ge-ekstraheer is nie. Net so belangrik was die waargenome hoër skeur- en barsindekse van handvelle vervaardig van reuse bamboes in vergelyking met E. grandis van beide geekstraheerde en nie ge-ekstraheerde materiale voorberei onder dieselfde verpulpings toestande. Bamboes se sterker eienskappe was as gevolg van die hoër vesellengte en ander morfologiese eienskappe as diévan loofhout. Pulp wat vervaardig is van reuse bamboes het ‘n hoër kappanommer getoon as pulp van E. grandis as gevolg van die hoë kondensasiegedrag van bamboeslignien onder alkaliese toestande. Hoër kappanommers kon die gepaardgaande hoër aanvraag vir bleikchemikalieë verklaar. Ten slotte, die pulpmeul bio-raffinaderykonsep nl. deur hemisellulosesekstraksie met NaOH gekombineer met óf ‘n gemodifiseerde kraft verpulping óf ‘n gemodifiseerde natriumantrakinoon verpulping, is wel uitvoerbaar. Dit word egter sterk beïnvloed deur die tipe ru-materiaal en die ekstraksie-metode gebruik, asook deur die kwaliteits- en gebruiksvereistes van verskillende tipes papier. ‘n Lae aanvraag vir verpulpingschemikalieë, vergelykbare pulpopbrengste en die verbetering in fisies-chemiese eienskappe van pulp vanaf pre-ge-ekstraheerde materiale is waargeneem. Verder kon, as gevolg van xilaan ekstraksie, meer ge-ekstraheerde materiaal in die verteerder gelaai word as wanneer nie-ge-ekstraheerde materiaal gebruik is.

Os plantios do gênero Pinus nas regiões do Brasil são mais restritos em comparação ao Eucalyptus, principalmente pela adaptação climática de cada espécie. As espécies de pinus plantadas se destacam na região Sul e em parte da região Sudeste, enquanto nas outras regiões os plantios são pouco significativos. Assim, são necessárias pesquisas de novos materiais genéticos e inovações nas técnicas de cozimento para que o gênero Pinus se torne mais competitivo se consolide no mercado florestal. No presente estudo as árvores das espécies Pinus maximinoi e Pinus taeda (parâmetro de comparação) foram cortadas aos 7 anos de idade com o objetivo de avaliar as características anatômicas, físicas e químicas da madeira dessas espécies visando a produção de polpa celulósica kraft. Para a avaliação tecnológica dos materiais seguiram-se as principais análises: (1) Anatômica - os materiais foram descritos macro e microscopicamente e foram medidas as dimensões dos traqueídes e calculadas relações como coeficiente de flexibilidade, fração parede e índice de Runkel; (2) Física - foi determinada a densidade básica dos discos e cavacos, além da densidade aparente do lenho por densitometria de raios X; (3) Química - foram determinados o teor de extrativos, lignina, holocelulose e cinzas. Para as polpas obtidas pelo processo de polpação Lo-Solids® sendo determinado ao final de cada cozimento os rendimentos bruto, depurado e o teor de rejeitos. As condições de cozimento foram ajustadas visando a obtenção de polpa com número kappa 28±5%. Em relação às características anatômicas, a espécie P. maximinoi apresentou lenho tardio menos expressivo que P. taeda. As dimensões dos traqueídes tiveram diferenças significativas entre as duas espécies. Os valores médios para o comprimento, largura e diâmetro do lume dos traqueídes axiais foram superiores para a espécie P. taeda (3,8 mm, 62,6µm, e 54,8 µm, respectivamente) em relação à P. maximinoi (3,2 mm, 53,9 µm, e 44,0 µm). A densidade básica média ponderada foi de 0,361 g.cm-3 para P. maximinoi, não havendo diferença em comparação à espécie de P. taeda que apresentou densidade básica de 0,379 g.cm-3. A composição química das espécies não apresentou diferença estatística entre os resultados. P. maximinoi apresentou 3,98% de extrativos totais, enquanto P. taeda apresentou 4,51%, já o teor de lignina total foi de 31,81% e 32,16%, respectivamente. Sendo assim, as duas espécies apresentaram características tecnológicas muito semelhantes, o que propiciou um comportamento análogo frente ao processo de polpação Lo-Solids®, com algumas vantagens para espécie de P. maximinoi, que apresentou maior rendimento depurado (47,2%) - 1 ponto percentual a mais comparado à P. taeda (46,1%). E ainda por razões referentes às características silviculturais, o incremento médio anual em celulose (IMACEL) foi de 5,526 tsa.ha-1.ano-1 para P. maximinoi e de 4,101 tsa.ha-1.ano-1 para P. taeda. / Pinus plantations in the Brazilian regions are more restricted compared to Eucalyptus, mainly due to the climatic adaptation of each species. The planted pine species contrast in the South and part of the Southeast region of Brazil, while in other regions plantations are not significant. Therefore, research with new genetic materials and innovations in pulp processes are necessary to make pine species more competitive and consolidate in the forest sector. This study aimed to analyze the wood characteristics of 7-year-old Pinus maximinoi and Pinus taeda wood species for kraft pulp production. It were analyzed three wood characteristics: (i) Wood anatomy: macro and microscopical description and measurement of wood tracheids. (ii) Wood basic density (from wood discs and chips) and apparent density by X-ray densitometry technique; (iii) wood chemical characterization, including extractives, lignin, holocellulose and ash contents. Lo-Solids® pulping processes were carried out aiming pulps with kappa number of 28 ± 5%. The wood anatomy analysis showed that P. maximinoi presented latewood less distinct than P. taeda wood. The tracheids of P. taeda wood had greater length, width and lumen diameter (3.8 mm, 62.6 µm and 54.8 µm, respectively) than P. maximinoi tracheids. The basic density of P. maximinoi wood was 0.361 g.cm-3, slightly similar to P. taeda (0.379 g.cm-3). P. maximinoi and P. taeda chemical wood analysis resulted in 3.98% and 4.51% of total extractives content and 31.81 and 32.16% of total lignin content, respectively. The pulping processes resulted for P. maximinoi screened yield 1% higher than P. taeda pulp (47.2% and 46.1%). In addition, the forestry characteristics presents an advantage for P. maximinoi species, which resulted in 5.526 tsa.ha-1 year-1 of average annual increase in cellulose (IMACEL) compared to 4.101 tsa.ha-1 year-1 for P. taeda species.

Nas indústrias de celulose, o processo dominante é a polpação Kraft. A polpação ou o cozimento de madeira em digestores constitui a operação central da produção de celulose, onde se processam as reações de deslignificação dos cavacos de madeira. Em geral, aí os modelos são empíricos e baseados em experimentos em escala de laboratório, e o \"scale-up\" para nível de digestores industriais torna-se tedioso e às vezes impraticável, pelo número de experimentos necessários e pela dificuldade de reprodução de todas as condições operacionais. Propõe-se neste trabalho um modelo matemático de polpação Kraft de eucalipto. O modelo consiste num sistema de equações diferenciais parciais que descrevem os efeitos combinados da cinética de polpação e da difusão de reagentes, como um reator de mistura perfeita com fases heterogêneas. Apresentam-se as previsões das simulações, comparam-se seus valores com dados experimentais. Este modelo é heterogêneo e difere dos modelos homogêneos usualmente propostos para a polpação. O primeiros permite uma abordagem das influências da espessura, massa específica e porosidade de cavacos, e também da difusão de reagentes nos cavacos durante a polpação. O presente trabalho dá ainda alguns exemplos de aplicação e tece comentários quanto ao modelo. / Kraft pulping is the dominant process f the pulp industry. The pulping of wood in digesters is the central operation of the pulp production, which consists of the delignification of the wood chips. Usually, the models of the delignification are empiricals and derived from laboratory scale experiments . The scale-up for industrial applications is tedious and sometimes impracticable, requiring a large number of experiments and presenting difficulty in reproducing all the operational condictions. The present work suggests a mathematical model for the Kraft pulping of the eucalyptus. This model consists of a system of partial differential equations describing the combined effects of the pulping kinetics and the diffusion of reactants, in form of continuous stirred tank reactor with heterogeneous phases. The prediction of the values given by simulation and their comparison with experimental data are presented. Differing from the homogeneous model, the heterogeneous allows an approach to estimate the influence of the chip thickness, density, porosity and that of the diffusion of the reactants in the chips, during pulping. The present work gives further some examples of application and comments on the model.

Nas indústrias de celulose, o processo dominante é a polpação Kraft. A polpação ou o cozimento de madeira em digestores constitui a operação central da produção de celulose, onde se processam as reações de deslignificação dos cavacos de madeira. Em geral, aí os modelos são empíricos e baseados em experimentos em escala de laboratório, e o \"scale-up\" para nível de digestores industriais torna-se tedioso e às vezes impraticável, pelo número de experimentos necessários e pela dificuldade de reprodução de todas as condições operacionais. Propõe-se neste trabalho um modelo matemático de polpação Kraft de eucalipto. O modelo consiste num sistema de equações diferenciais parciais que descrevem os efeitos combinados da cinética de polpação e da difusão de reagentes, como um reator de mistura perfeita com fases heterogêneas. Apresentam-se as previsões das simulações, comparam-se seus valores com dados experimentais. Este modelo é heterogêneo e difere dos modelos homogêneos usualmente propostos para a polpação. O primeiros permite uma abordagem das influências da espessura, massa específica e porosidade de cavacos, e também da difusão de reagentes nos cavacos durante a polpação. O presente trabalho dá ainda alguns exemplos de aplicação e tece comentários quanto ao modelo. / Kraft pulping is the dominant process f the pulp industry. The pulping of wood in digesters is the central operation of the pulp production, which consists of the delignification of the wood chips. Usually, the models of the delignification are empiricals and derived from laboratory scale experiments . The scale-up for industrial applications is tedious and sometimes impracticable, requiring a large number of experiments and presenting difficulty in reproducing all the operational condictions. The present work suggests a mathematical model for the Kraft pulping of the eucalyptus. This model consists of a system of partial differential equations describing the combined effects of the pulping kinetics and the diffusion of reactants, in form of continuous stirred tank reactor with heterogeneous phases. The prediction of the values given by simulation and their comparison with experimental data are presented. Differing from the homogeneous model, the heterogeneous allows an approach to estimate the influence of the chip thickness, density, porosity and that of the diffusion of the reactants in the chips, during pulping. The present work gives further some examples of application and comments on the model.

A baixa porcentagem de plantios com árvores do gênero Pinus no Brasil e a crescente demanda por polpa celulósica de fibra longa no país evidenciam a necessidade de estudos de espécies de pinus tropicais que se desenvolvam em regiões além do sul brasileiro. Os objetivos deste trabalho foram caracterizar tecnologicamente a madeira de Pinus maximinoi e avaliar o desempenho desta matéria-prima para produção de polpa celulósica, a partir do processo de polpação modificado do tipo Lo-Solids®. Utilizou-se como referência tecnológica a madeira de Pinus taeda, espécie mais empregada no país para produção de polpa celulósica de fibra longa. Foram analisadas 5 árvores de P. maximinoi e 5 árvores de P. taeda, com 14 anos de idade e plantadas nas mesmas condições edafoclimáticas. As madeiras das duas espécies foram caracterizadas tecnologicamente quanto a densidade básica da madeira, composição química e morfologia dos traqueídes. Posteriormente, foram realizados cozimentos de caracterização, utilizando-se o processo de polpação kraft convencional com diferentes níveis de cargas alcalinas, com o intuito de avaliar o desempenho da madeira de P. maximinoi frente ao processo de polpação e ajustar modelos matemáticos para estimar parâmetros de interesse . Foram obtidas polpas branqueáveis com número kappa = 28±5% a partir do processo de polpação modificado do tipo Lo-Solids®, com fator H 2295, sulfidez de 30% e relação licor madeira de 4L/kg. Os resultados de caracterização da madeira de P. maximinoi demonstraram que esta possui densidade básica equivalente a 0,417 g/cm3, teores de 64,49 % de holocelulose, 31,06% de lignina total, 4,45% de extrativos totais e 0,16% de cinzas e traqueídes com 4,19 mm de comprimento, 56,95 μm de largura, 44,11 μm de diâmetro de lúme e 6,42 μm de espessura da parede. Os resultados dos cozimentos Lo-Solids® mostraram que a madeira de P. maximinoi demandou álcali ativo de 24,4% (base NaOH) e resultou em polpas com rendimento depurado de 47,5%, teor de rejeitos de 0,43% e viscosidade de 713 cm3/g. O consumo específico da madeira de P. maximinoi foi de 5,868 m3/tsa e incremento médio anual em celulose de 6,575 tsa/ha/ano. O teor de sólidos gerados por tonelada de celulose produzida para a madeira de P. maximinoi foi de 1,451 t/tsa. Os resultados obtidos neste estudo permitem concluir que a madeira de P. maximinoi representa uma alternativa interessante para produção de polpa celulósica de fibra longa, tendo em vista que possui características tecnológicas muito semelhantes à madeira de P. taeda, além do menor consumo específico da madeira e maior incremento médio anual em celulose. / The low percentage of plantation of pine genus in Brazil and the growing demand for long fiber pulp demonstrates the necessity of studies with tropical pine species that develop in regions beyond the south of Brazil. The main objectives of this study were to characterize the wood of the specie Pinus maximinoi and to evaluate the performance of this material for pulp kraft production, using the modified pulping process Lo-Solids®. Pinus taeda wood was used as technologinal reference since it is the most used pine specie in Brazil for softwood pulp production. Samples from 5 Pinus maximinoi trees and 5 Pinus taeda trees were analysed both with 14 years old, planted in the same conditions. Both of the materials were technollogicaly characterized by wood basic density analysis, wood chemistry and tracheids morphology. After that, were realized characterization pulping processes, using the conventional kraft pulping process, with different alkali charges, in order to study the behavior of Pinus maximinoi wood throughout the process and ajust mathematical models to estimate parameters of interest. Then, it was produced bleached pulps with kappa number of 28±5% using the modified pulping process Lo-Solids®, with H factor 2295, 30% of sulfidity and liquor to wood ratio = 4L/kg. The results from the wood characterization shows that Pinus maximinoi wood has basic wood density equivalent to 0,417 g/cm3, 64,49% content of holocellulose, 31,06% content of total lignin, 4,45% content of total extractives and 0,16% content of ash; the tracheids morphology showed that the tracheids has lenght 4,19 mm, 56,95 μm of width, 44,11 μm of lumen width and 6,42 μm of wall thickness. The results of the Lo-Solids® pulping process showed that Pinus maximinoi wood has demanded alkali charge of 24,4% (NaOH) and resulted in pulps with screened yield of 47,5%, rejects contents of 0,43% and viscosity pulp of 713 cm3/g. The specific wood consumption was 5,868 m3/tsa and the IMACEL 6,575 tsa/ha/ano. The solids content generated per ton of cellulose was 1,451 t/tsa for Pinus maximinoi wood. The results obtained in this study showed that the Pinus maximinoi wood represents an interesting alternative for softwood pulp production given that the technological characteristics were very similar between the P. taeda wood, beyond the higher forestry production, the lower wood specific consumption observed and higher IMACEL.

Este trabalho teve como objetivo avaliar o efeito de atributos físicos e químicos do solo na qualidade da madeira, estabelecendo correlações com as variáveis do processo de polpação celulósica. Para tanto, foram selecionadas cinco áreas no planalto ocidental do Estado de São Paulo, plantadas com um mesmo clone de Eucalyptus grandis Hill Ex Maiden (Coff´s Harbour), com idades variando entre 6,5 e 7,0 anos de idade, pertencentes à Suzano Papel e Celulose. Foram coletadas amostras de solo deformadas para fins de análises físicas e químicas. Amostras não deformadas foram utilizadas para análises físico-hídricas. Em cada uma das cinco áreas, foram demarcadas, aleatoriamente, 3 parcelas com 100 plantas cada. Em cada parcela, foram medidos os diâmetros à altura de 1,3 m (DAP) e a altura de todas as árvores. Os dados foram classificados em quatro classes de DAP e obtidos os DAPs médios de cada classe. Foi coletada uma árvore de cada classe e de cada parcela, mensuradas e estimadas as massas de lenho, casca, folha e galhos. Os troncos de cada árvore foram picados, individualmente, em picador industrial. Uma amostra dos cavacos foi utilizada para a análise de extrativos e componentes da madeira, de acordo com os métodos estabelecidos pela TAPPI e ABTCP. As condições de polpação foram estabelecidas, fixando-se o número kappa em 17 ± 0,5, a temperatura de cozimento em 165 °C, o tempo de elevação da temperatura em 90 minutos, o tempo à máxima temperatura em 60 minutos e a sulfidez do licor de cozimento em 24%. A carga de álcali foi variável e necessária para se atingir o número kappa desejado. Buscou-se descrever as relações entre os atributos do solo, a produtividade e a qualidade da madeira. Os resultados mostraram que os atributos físicos do solo, sobretudo o teor de argila, diretamente relacionado à quantidade de água disponível, foram os que mais afetaram a produtividade e a qualidade da madeira. A densidade básica da madeira não se alterou nas diferentes classes de solo. Por outro lado, aumentou exponencialmente com o volume das árvores, independentemente do solo em que cresceram. O teor de lignina total diminuiu e o de holocelulose aumentou exponencialmente, com o aumento do teor de argila do solo (até cerca de 35 a 40% de argila). O teor de extrativos não foi afetado pelos atributos do solo. Atribuiu-se à compensação entre o aumento do teor de holocelulose e a diminuição do teor de lignina total a não-variação da densidade básica da madeira nos diferentes solos. O rendimento de celulose depurada relacionou-se exponencialmente com o teor de argila do solo. No solo com textura muito argilosa (LVd2), o rendimento foi 6% maior do que no solo de textura arenosa (RQ). / The objective of this work was to evaluate the effect of soil physical and chemical attributes on timber quality, and to establish correlations with cellulose pulping process variables. To achieve this, five areas were selected at the Western Plateau of the State of São Paulo, planted with the same Eucalyptus grandis Hill Ex Maiden (Coff´s Harbour) clone, with ages ranging between 6.5 and 7.0 years, owned by Cia. Suzano Papel e Celulose. Deformed soil samples were collected for physical and chemical analysis purposes. Non-deformed samples were used in the physical and moisture analyses. Three plots containing 100 plants each were demarcated at random in each of the five areas. The diameters at a 1.3 m height (DBH) and heights of all trees were measured for each plot. The data were classified into four DBH classes and the mean DAP values for each class were obtained. One tree was collected from each class and each plot, and its wood, bark, leaf, and branch masses were measured and estimated. The trunks of each tree were individually chopped in a tree chopper. A sample from the chips was used in the analysis of wood extractives and components, according to methods established by TAPPI and ABTCP. The pulping conditions were established by fixing the Kappa number at 17 ± 0.5, cooking temperature at 165 °C, temperature ramp time at 90 minutes, time at maximum temperature at 60 minutes, and cooking liquor sulfidity at 24%. The alkali load was variable and adjusted as needed to reach the desired Kappa number. We sought to describe the relations between soil attributes and wood productivity and quality. The results showed that the soil physical attributes, especially clay content, which is directly related to the amount of available water, affected wood productivity and quality the most. Basic wood density did not change for different soil classes. On the other hand, it increased exponentially with tree volume, regardless of the soil where they were grown. Total lignin content decreased, and holocellulose content exponentially increased as soil clay content increased (until about 35 to 40% clay). The extractives content was not affected by soil attributes. The compensation between the increase in holocellulose content and the decrease in total lignin content was attributed to the lack of basic wood density variation in different soils. Screened cellulose yield exponentially increased with soil clay content. In the very clayey-textured soil (LVd2), yield was 6% higher than in the sandy-textured soil (RQ).

Este estudo teve como objetivo verificar os efeitos de misturas de madeiras de Eucalyptus grandis x Eucalyptus urophylla, Eucalyptus globulus e Pinus taeda na eficiência do processo Lo-Solids® e características das polpas celulósicas visando a diferenciação das propriedades dos papéis resultantes. Foram avaliados os comportamentos das madeiras, quanto aos parâmetros: densidade básica, composição química, polpação Lo-solids®, características químicas das polpas celulósicas, características das fibras das polpas celulósicas e testes físicos. Os mesmos parâmetros foram avaliados nas misturas entre as espécies, realizadas da seguinte forma: Eucalyptus grandis x Eucalyptus urophylla e Pinus taeda nas proporções de 10 a 50% de Pinus taeda, Eucalyptus globulus e Pinus taeda nas proporções de 10 a 50% de Pinus taeda e Eucalyptus grandis x Eucalyptus urophylla e Eucalyptus globulus nas proporções de 10 a 50% de Eucalyptus globulus. Para as misturas entre os Eucalyptus e o Pinus taeda, o número kappa das polpas celulósicas aumentou gradativamente, conforme a proporção de Pinus taeda aumentava na mistura, sendo que os números kappa variaram entre 17,9 e 22,1. Para atingir os números kappa desejados no trabalho, foi necessário ajustar a carga alcalina (álcali efetivo entre 19,3 e 21,3 % expresso como NaOH) e o fator H (entre 970 a 1420). Os resultados das análises indicaram uma tendência de queda dos rendimentos bruto e depurado e da viscosidade da polpa celulósica, dos teores de ácidos hexenurônicos, da solubilidade em NaOH 5%, do número de fibras por grama, da drenabilidade e do índice de tração e estouro, com o aumento da participação de Pinus taeda nas misturas. Em contrapartida, foram observadas tendências de aumento dos teores de lignina total na polpa, do comprimento e da largura das fibras, do coarseness, do índice de rasgo e do consumo específico de madeira à medida que a participação de Pinus taeda aumenta nas misturas. Nas misturas entre o Eucalyptus grandis x Eucalyptus urophylla e o Eucalyptus globulus, os números kappa variaram entre 17,9 e 18,6 e foram observadas tendências de queda dos rendimentos bruto e depurado, da viscosidade da polpa celulósica, do teor de lignina total e do coarseness, com a adição de Eucalyptus globulus ao Eucalyptus grandis x Eucalyptus urophylla. Para os parâmetros solubilidade em NaOH 5%, número de fibras por grama, drenabilidade, índices de tração, alongamento e estouro foram verificadas tendências de aumento com o aumento da proporção de Eucalyptus globulus nas misturas. Com base nos resultados obtidos, a adição de até 10% de fibra de Pinus taeda aos Eucalyptus pode melhorar a qualidade da polpa para os parâmetros índice de rasgo e drenabilidade. Essas características permitem maiores velocidades de operação das máquinas secadoras de polpa celulósica e máquinas de papel e consequentemente conduzem a uma maior produção. Plantas produtoras que desejam a produção de um tipo de celulose diferenciada, com elevada resistência ao rasgo, incremento da produção, ou ainda a produção de papéis especiais, de baixa gramatura, devem considerar a adição de pequenas proporções de Pinus taeda aos Eucalyptus. / The objective of this study was to evaluate the possibility of cooking mixtures between the species Eucalyptus grandis x Eucalyptus urophylla, Eucalyptus globulus and Pinus taedafor the production of kraft pulp with specific characteristics. The three species were analyzed for their wood density, chemical composition, Lo-solids® pulping, the chemical characteristics of the pulp, characteristics of its fibers and physical tests. The same parameters were evaluated in the mixtures between the species that were made up as: Eucalyptus grandis x Eucalyptus urophylla and Pinus taeda in the proportion of 10 to 50% of Pinus taeda, Eucalyptus globulus and Pinus taeda in the proportion of 10 to 50% of Pinus taeda and Eucalyptus grandis x Eucalyptus urophylla and Eucalyptus globulus in the proportion of 10 to 50% of Eucalyptus globulus. For the mixtures between the Eucalyptus and the Pinus taeda, the pulp kappa numbers increased as the proportion of Pinus taeda increased in the pulps, varying from 17.9 to 22.1. In order to reach the target kappa number it was necessary to adjust the alkali charge applied (from 19.3 to 21.3 %NaOH as effective alkali) and the H factor (between 970 and 1420). The results indicated a downward trend in total yield and screened yield values, in pulp viscosity, in the hexenuronic acid content, in solubility in NaOH 5%, in the number of fibers per gram of pulp, in the drainability and strength and burst indices, with the increasing proportion of Pinus taeda in the pulps. As the proportion of Pinus taeda increased in the pulps an increase was noticed for the parameters total lignin content in the pulp, length and width of the fibers, coarseness and tear indices. In the mixtures between Eucalyptus grandis x Eucalyptus urophylla and Eucalyptus globulus the kappa number varied from 17.9 to 18.6. Eucalyptus grandis x Eucalyptus urophylla performed performed better in pulping as it needed a lower alkali charge and had a higher pulp yield and pulp viscosity. Hence, in the Eucalyptus mixtures a downward trend was noticed in the values for pulp yield and pulp viscosity with an increasing proportion of Eucalyptus globulus. Falls in total lignin content in the pulp and in the coarseness were also observed as the proportion of Eucalyptus globulus increased. For the parameters solubility in NaOH 5%, number of fibers per gram of pulp, drainability, strength and burst indices an increase was noticed as the proportion of Eucalyptus globulus increased in the pulps. In conclusion, the addition of up to 10% of Pinus taeda to Eucalyptus can increase pulp quality for the tear index and drainability parameters, making pulp and paper mills faster at drying pulp, or speeding up the paper machines, resulting in higher productivity. These mixtures also allow the production of tailor-made pulp and special papers.

The mechanical pulping industry has been developing throughout the years, due to competitive prices in the electricity market and good accessibility of wood. This has made it possible for such and “expensive” process to further develop. Today, with increasing electricity prizes, it is of great interest to reduce electrical consumption in mechanical pulping industry, since the process consumes large amounts of electricity. Braviken paper mill is starting up a new thermomechanical pulping line, scheduled for start-up in August 2008, which aims to reduce electrical consumption. The new line will include chip pre-treatment equipment such as an impregnator, an Andrtiz Impressafiner (Screw press), a high intensity primary stage refines double disc (DD), and a new low consistency refiner (LC), significantly bigger than those earlier available on the market. This master´s thesis is one out of three Master´s thesis made at Braviken paper mill during spring 2008. They all are connected, and are investigating the possibility to reduce electric energy consumption within TMP production. Master´s thesis concerning high consistency refining was done by Dino Muhic, “High consistency refining of mechanical pulps during varying refining conditions”, and low consistency refining written by Fredrik Johansson “Increased energy efficiency in low consistency refining”. Chip pre-treatment is to be used to reduce electrical consumption. Mechanical pre-treatment, such as using an Andrtiz Impressafiner demolishes the chips while also making it possible to impregnate the chips with chemicals, the later giving additional possibilities to reduce electricity consumption. Chemical chip pre-treatment decreases the lignin softening temperature, which benefits the refining process, yielding longer and less damaged fibers that will create a fibrous pulp with reduced electrical energy input.The goal for this study was to investigate the effect of alkaline-peroxide on chip pre-treatment by using a design of experiment method, in terms of electric energy consumption for the process, strength properties, opacity and ISO-brightness within the pulp/sheets. The trials were built up as a factorial experiment, with two factors, alkaline and peroxide, with two levels each (high and low). The high level for alkaline was 15 kg/t and 10 kg/t for the low level, and the high level for peroxide was 10 kg/t and 5 kg/t for the low level. This resulted in four trials with two zero-points, and two reference pulps, one normal TMP, thermomechanical pulp, and the other TMP with pressafiner and water. The trials showed that adding alkaline-peroxide clearly had an impact on pulp properties, such as increased strength properties, fiber length improvements and less shives could be found in the alkaline-peroxide treated pulps. The yield was highest for the normal TMP, about 99% and it decreased with increasing alkaline addition, the lowest value was achieved for the pulps containing the highest dose of alkaline, about 95%. The optical properties were more or less as expected. Opacity had the highest value for the pulps that had been made from chips with the highest total alkaline level. The ISO brightness was highest for pulps containing low level of alkaline. It could not be decided if the electricity demand had been reduced for the chemically treated pulps; it actually had the opposite effect as expected. The chemically treated pulps demanded a higher SEC, specific energy consumption, compared to the reference pulps. This result could have depended on the small pilot plant high consistency refiners at CTP, Centre technique du papier, Grenoble, France, due to the plate size and what kind of plats that were used. To do trials like this and to be able to draw correct conclusions relevant for a full scale plant, bigger refiners might give a more comparable result. It was clear that the fiber properties had improved, which could be the key to reduce electricity when LE- (low-energy) plates are used in the HC-refiner. A higher intensity could be used and electricity energy could be saved.