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The aim is to investigate models that predicts the potential of pulp and evaluate the relevance of the zero-span tensile index within these. Two chemical pulps made from softwood and eucalyptus were refined in a Voith-beater with different energy input in order to study the change of fiber morphology signals and other pulp and paper properties. Chemical, THP pulp from Södra Värö is also used as an initial analysis for morphological connections to Zero-span tensile index. The L&W Fiber Tester Plus is used in order to study the pulps fiber morphology and Pulmac 2000 for zero span. Handsheets are made for mechanical tests such as tensile properties, ZD-strength and optical properties. Many of the given signals change according to clear patterns with increasing refining energy. Using least square methods, formulas describing the development with high adaptation could be formulated. Many of the measured aspects changes over already known patterns. These are then applied in the models. Three possible models is tested: linear regression, Shear-Lag and Page. Of the three, only the two first ones where able to produce reliable models, whereas the third required data that was difficult to acquire at the same time as the adaptation was very low. The only model that use exclusively morphology data is linear regression.

Polysaccharides are now popularly used in paper technology since they are able to improve mechanical properties of the paper. Xylan and pectin are two natural polymers that have a wide range of applications nowadays. These two polysaccharides can be used in their native forms as well as derivatives. In this study, xylan and pectin were modified to obtain cationic derivatives before adding into the paper for enhancement. The work was motivated by the fact that xylan and pectin share the same negative surface properties as cellulose. This leads to a slight repulsion effect between them once they are close. Their cationic derivatives, therefore, are believed to strengthen the paper due to electrostatic interactions between two oppositely charged objects beside hydrogen bonds. To fulfil the purposes, oat spelt xylan and apple pectin were chemically modified using different modification methods, including oxidation, amidation, and a combination of these two methods. A quantitative method to determine the adsorbed amount and relative retention capacity of xylan onto paper using high performance liquid chromatography was also developed. The results show that oat spelt and apple pectin, as well as their modified derivatives, can improve the paper mechanical properties. The oat spelt xylan significantly enhances the tensile strength, however, this contribution has a saturation level in correlation with the relative retention capacity of the xylan onto cellulose. The best retention capacity is achieved when 5% of xylan is added. This finding provides a practical approach to the application of xylan as a paper additive in consideration of economic issues. Although the application of apple pectin and its amidated derivatives in paper is rather rare, some interesting points have been discovered in this work. Among the apple pectin samples used, only the ones with low degree of esterification give a slight enhancement in tensile index at 5% dosage. The results also suggest that the dosage of the pectin added into the paper should not exceed 5% due to its viscous property at high concentrations.

Polysaccharides are now popularly used in paper technology since they are able to improve mechanical properties of the paper. Xylan and pectin are two natural polymers that have a wide range of applications nowadays. These two polysaccharides can be used in their native forms as well as derivatives. In this study, xylan and pectin were modified to obtain cationic derivatives before adding into the paper for enhancement. The work was motivated by the fact that xylan and pectin share the same negative surface properties as cellulose. This leads to a slight repulsion effect between them once they are close. Their cationic derivatives, therefore, are believed to strengthen the paper due to electrostatic interactions between two oppositely charged objects beside hydrogen bonds. To fulfil the purposes, oat spelt xylan and apple pectin were chemically modified using different modification methods, including oxidation, amidation, and a combination of these two methods. A quantitative method to determine the adsorbed amount and relative retention capacity of xylan onto paper using high performance liquid chromatography was also developed. The results show that oat spelt and apple pectin, as well as their modified derivatives, can improve the paper mechanical properties. The oat spelt xylan significantly enhances the tensile strength, however, this contribution has a saturation level in correlation with the relative retention capacity of the xylan onto cellulose. The best retention capacity is achieved when 5% of xylan is added. This finding provides a practical approach to the application of xylan as a paper additive in consideration of economic issues. Although the application of apple pectin and its amidated derivatives in paper is rather rare, some interesting points have been discovered in this work. Among the apple pectin samples used, only the ones with low degree of esterification give a slight enhancement in tensile index at 5% dosage. The results also suggest that the dosage of the pectin added into the paper should not exceed 5% due to its viscous property at high concentrations.

Submitted by Ana Paula Almeida Ferraz (ana.almeida.ferraz@gmail.com) on 2018-04-16T15:45:49Z No. of bitstreams: 1 Ana Paula Almeida Ferraz.pdf: 1528848 bytes, checksum: efac2d5c50a3b2eb9d3d5b0b7e2e6a11 (MD5) / Approved for entry into archive by Pamella Benevides Gonçalves null (pamella@feg.unesp.br) on 2018-04-16T19:14:08Z (GMT) No. of bitstreams: 1 ferraz_apa_me_guara.pdf: 1528848 bytes, checksum: efac2d5c50a3b2eb9d3d5b0b7e2e6a11 (MD5) / Made available in DSpace on 2018-04-16T19:14:08Z (GMT). No. of bitstreams: 1 ferraz_apa_me_guara.pdf: 1528848 bytes, checksum: efac2d5c50a3b2eb9d3d5b0b7e2e6a11 (MD5) Previous issue date: 2018-02-27 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / O presente estudo tem por objetivo elucidar sobre a correlação entre a viscosidade e as propriedades mecânicas da polpa. O material utilizado foi uma amostra de Eucalyptus grandis x Eucalyptus urophylla. Os cavacos foram submetidos a cozimentos com tempos de polpação de 90 e 120 minutos. Para as polpas produzidas com tempo de 90 minutos, realizou-se a deslignificação com oxigênio com temperatura de 95°C e para as polpas produzidas com o tempo de 120 minutos, a temperatura do estágio de deslignificação com oxigênio foi de 115°C, objetivando uma maior diferença de viscosidade entre as amostras. Ambas as polpas foram branqueadas a partir das sequências ECF OD(E+P)DD, OAHTD(E+P)DP e OD(E+P)(PO). Posteriormente as polpas foram refinadas em moinho PFI e avaliadas quanto ao índice de rasgo, tração e arrebentamento, segundo as normas da TAPPI (Technical Association of the Pulp and Paper Industry). Os resultados indicam que o aumento do tempo de cozimento em 30 minutos e aumento da temperatura da deslignificação com oxigênio de 95°C para 115°C afetam significativamente a viscosidade da polpa. O refino foi afetado pela diminuição da viscosidade das sequências produzidas com deslignificação com oxigênio à temperatura de 115°C. O índice de rasgo apresentou decréscimo quanto menor a viscosidade da polpa em todas as sequências de branqueamento deste estudo. Os índices de tração e arrebentamento apresentaram decréscimo de acordo com a diminuição da viscosidade em uma mesma sequência, entretanto, quando a comparação foi feita entre diferentes sequências de branqueamento, não houve relação entre os índices de tração e de arrebentamento com a viscosidade da polpa. / This study aims to elucidate the correlation between the viscosity and the mechanical properties of the pulp. The material used was a sample of Eucalyptus grandisx Eucalyptus urophylla. The chips were cooked with cooking times of 90 and 120 minutes. For the pulps produced in 90 minutes, the delignification with oxygen at temperature of 95ºC was performed and for the pulps produced in 120 minutes, the temperature of the oxygen delignification stage was 115ºC, aiming a greater difference of viscosity between the samples. Both pulps were bleached from the sequences ECF OD(E+P)DD, OD(E+P)(PO) and OAHTD(E+P)DP. Later, the pulps were refined in PFI mill and assessed for the tear, tensile and burst indexes, according to the TAPPI (Technical Association of the Pulp and Paper Industry) standards. The results indicate that the increase of cooking time in 30 minutes and the increase of temperature in oxygen delignification from 95°C to 115°C affect significantly the pulp viscosity. The refining was affected by the viscosity reduction of the sequences produced with delignification with oxygen at temperature of 115ºC. Tear index decreased as the pulp viscosity was lower, in all the bleaching sequences. Tensile and burst indexes presented decrease with the decrease of the viscosity in the same sequence, however, when comparing different bleaching sequences, there was no relation between the tensile and burst indexes with the pulp viscosity.

Modification of softwood kraft pulp by the addition of either polysulfide (PS) or sodium borohydride (NaBH4) has been shown to increase the pulp yield due to a higher retention of glucomannan.  The pulps with higher yield gave a paper with higher tensile index than reference pulp, especially at lower degrees of refining. The higher yield pulps also showed a greater porosity of the fibre wall, indicating an increase in the swelling potential of the fibres. This can lead to increased fibre flexibility and increased joint strength between the fibres and to the higher handsheet tensile index. However, the swelling increase associated with the higher hemicellulose content could also make dewatering more challenging because of the higher water retention of the pulp. The results of this study show however that the positive influence of the increase in yield (fewer fibres and a more open sheet structure) dominates over the negative influence of the higher hemicellulose content on the dewatering properties, especially at lower refining energy levels. Studies simulating full-scale tissue machine dewatering conditions showed that pulps with a higher yield and a higher hemicellulose content had a higher tensile index at the same dryness. Moreover, the same dryness level was achieved in a shorter dwell-time. A given tensile index was also achieved with less refining energy. Increasing the yield and hemicellulose content by the addition of either an oxidizing or a reducing agent in the softwood kraft pulping process thus has a potential for giving high quality fibres for tissue paper production with less refining energy and lower drying energy costs. / <p>Vid tidpunkten för framläggningen av avhandlingen var följande delarbeten opublicerade: delarbete 2 inskickat.</p><p>At the time of the defence the following papers were unpublished: paper 2 submitted.</p>

<p>Converting wood into paper is a complex process involving many different stages, one of which is pulping. Pulping involves liberating the wood fibres from each other, which can be done either chemically or mechanically. This thesis focuses on the most common chemical pulping method, the kraft cooking process, and especially on a recently developed improvement of the impregnation phase, which is the first part of a kraft cook.</p><p>Extended impregnation kraft cooking (EIC) technique is demonstrated to be an improvement of the kraft pulping process and provides a way to utilize softwood to a higher degree, at higher pulp yield. We demonstrate that it is possible to produce softwood (<em>Picea abies</em>) kraft pulp using a new cooking technique, resulting in a pulp that can be defibrated without inline refining at as high lignin content as 8% on wood, measured as kappa numbers above 90. Lignin is the wood constituent that holds the wood fibres together in the wood matrix. The new cooking technique uses the differences in reaction rate between the diffusion and consumption of hydroxide ions; it is used to ensure a homogenous impregnation of wood chips at lower impregnation temperatures and longer impregnation times than are generally used in the industry. The applied cooking temperatures are also substantially lower than those used in conventional kraft pulping systems, promoting uniform delignification. This results in a narrower kappa number distribution than in lab-cooked conventional kraft pulp.</p><p>High-kappa-number pulps were investigated for pulp sheet properties such as tensile strength, tensile stiffness, and compression strength. It was demonstrated that an EIC pulp of kappa number 95 has strength properties comparable to those of a conventional pulp of kappa number 82. Comparing the effects of starch multilayers on conventional and EIC pulps reveals similar effects. The use of the starch multilayer treatment increased the tensile index and decreased the tensile stiffness and short-span compression test (SCT) indices.</p><p>The EIC technique has also been used to produce a series of bleachable-grade pulps. The results indicate the possibility of increasing the lignin content of the pulp entering the oxygen delignification stage, since the reject content of gently defibered pulp is lower than 0.1% at kappa number 49.</p><p>In this thesis, we recommend that wood chips be impregnated for 2 h at 110 °C to neutralize acidic compounds in the wood and impregnate the chips with cooking chemicals, and that the ensuing cook be performed at 135–140 °C, depending on the target kappa number. We also recommend increasing the available amounts of cooking chemicals in the impregnation stage by using a higher liquor-to-wood ratio and keeping the alkali profile fairly high in the ensuing cook. This concept will reduce the amount of reject material, increase the pulping uniformity, and increase the selectivity towards lignin degradation in the kraft cook.</p> / <p>Omvandling av ved till papper är en komplicerad process som består av många olika steg där ett är massaframställningen (eng. <em>pulping</em>). Massaframställning medför att vedfibrerna frigörs från varandra på kemisk eller mekanisk väg. Denna avhandling fokuserar på den vanligaste kemiska metoden, sulfatkokning och speciellt den nyligen utvecklade förbättringen av impregnerings fasen, som är den första delen av ett sulfatkok. <em></em></p><p>Här visas att<em> Extended Impregnation kraft Cooking </em>(EIC) innebär en förbättring av sulfatkokningen och ett sätt att uppnå högre vedutnyttjande vid högre utbyte för barrved. Vi visar att det är möjligt att producera barrvedsmassa med en ny kokningsprincip som resulterar i en massa som är defibrerbar utan inline-raffinering vid så högt lignin innehåll som 8% (på ved), mätt som kappatal över 90. Lignin är den vedkomponent som håller ihop vedfibrerna i vedmatrisen. Kokningsprincipen utnyttjar skillnaderna i reaktionshastighet mellan diffusion och konsumtion av hydroxidjoner och nyttjas till att skapa en homogen impregnering av vedflisen vid lägre impregneringstemperatur och under längre tid än vad som vanligen används i industrin. De använda koktemperaturerna är också betydligt lägre än vid konventionell sulfatkokning vilket gynnar jämn delignifiering. Detta resulterar i en smalare kappatalsfördelning jämfört med laboratoriekokade konventionella massor.</p><p>Massor med höga kappatal undersöktes med avseende på egenskaper hos handark, såsom dragstyrka, dragstyvhet och kompressionsstyrka Det visades att handark från EIC massa vid kappatal 95 hade jämförbara styrkeegenskaper med konventionell massa vid kappatal 82. Vid jämförelse av effekten av stärkelse multilager på konventionella och EIC massor avslöjar liknande effekter. Användningen av stärkelsemultilager ökade dragindex och minskade dragstyvhets- och kompressions index (SCT, short-compression test).</p><p>Kokprincipen har även använts för att ta fram en serie blekbara massor. Resultaten visar på möjligheten att öka lignininnehållet i massan in till i syrgasdelignifierings-steget eftersom spetinnehållet för milt defibrerad massa var lägre än 0,1% vid kappatal 49.</p><p>I den här avhandlingen rekommenderar vi att vedflis impregneras i 2 timmar vid 110 °C för att neutralisera sura komponenter i veden och impregnera flisen med kokkemikalier, samt att utföra det efterföljande koket vid 135–140 °C beroende på önskat kappatal. Vi rekommenderar även att öka den tillgängliga mängden kokkemikalier i impregneringssteget genom att använda högre vätske-ved förhållande och att hålla alkali profilen relativt hög i det efterföljande koket. Detta koncept reducerar spetmängden, ger jämnare kokning och ökar selektiviteten för nedbrytning av lignin i sulfatkoket.</p>

Converting wood into paper is a complex process involving many different stages, one of which is pulping. Pulping involves liberating the wood fibres from each other, which can be done either chemically or mechanically. This thesis focuses on the most common chemical pulping method, the kraft cooking process, and especially on a recently developed improvement of the impregnation phase, which is the first part of a kraft cook. Extended impregnation kraft cooking (EIC) technique is demonstrated to be an improvement of the kraft pulping process and provides a way to utilize softwood to a higher degree, at higher pulp yield. We demonstrate that it is possible to produce softwood (Picea abies) kraft pulp using a new cooking technique, resulting in a pulp that can be defibrated without inline refining at as high lignin content as 8% on wood, measured as kappa numbers above 90. Lignin is the wood constituent that holds the wood fibres together in the wood matrix. The new cooking technique uses the differences in reaction rate between the diffusion and consumption of hydroxide ions; it is used to ensure a homogenous impregnation of wood chips at lower impregnation temperatures and longer impregnation times than are generally used in the industry. The applied cooking temperatures are also substantially lower than those used in conventional kraft pulping systems, promoting uniform delignification. This results in a narrower kappa number distribution than in lab-cooked conventional kraft pulp. High-kappa-number pulps were investigated for pulp sheet properties such as tensile strength, tensile stiffness, and compression strength. It was demonstrated that an EIC pulp of kappa number 95 has strength properties comparable to those of a conventional pulp of kappa number 82. Comparing the effects of starch multilayers on conventional and EIC pulps reveals similar effects. The use of the starch multilayer treatment increased the tensile index and decreased the tensile stiffness and short-span compression test (SCT) indices. The EIC technique has also been used to produce a series of bleachable-grade pulps. The results indicate the possibility of increasing the lignin content of the pulp entering the oxygen delignification stage, since the reject content of gently defibered pulp is lower than 0.1% at kappa number 49. In this thesis, we recommend that wood chips be impregnated for 2 h at 110 °C to neutralize acidic compounds in the wood and impregnate the chips with cooking chemicals, and that the ensuing cook be performed at 135–140 °C, depending on the target kappa number. We also recommend increasing the available amounts of cooking chemicals in the impregnation stage by using a higher liquor-to-wood ratio and keeping the alkali profile fairly high in the ensuing cook. This concept will reduce the amount of reject material, increase the pulping uniformity, and increase the selectivity towards lignin degradation in the kraft cook. / Omvandling av ved till papper är en komplicerad process som består av många olika steg där ett är massaframställningen (eng. pulping). Massaframställning medför att vedfibrerna frigörs från varandra på kemisk eller mekanisk väg. Denna avhandling fokuserar på den vanligaste kemiska metoden, sulfatkokning och speciellt den nyligen utvecklade förbättringen av impregnerings fasen, som är den första delen av ett sulfatkok. Här visas att Extended Impregnation kraft Cooking (EIC) innebär en förbättring av sulfatkokningen och ett sätt att uppnå högre vedutnyttjande vid högre utbyte för barrved. Vi visar att det är möjligt att producera barrvedsmassa med en ny kokningsprincip som resulterar i en massa som är defibrerbar utan inline-raffinering vid så högt lignin innehåll som 8% (på ved), mätt som kappatal över 90. Lignin är den vedkomponent som håller ihop vedfibrerna i vedmatrisen. Kokningsprincipen utnyttjar skillnaderna i reaktionshastighet mellan diffusion och konsumtion av hydroxidjoner och nyttjas till att skapa en homogen impregnering av vedflisen vid lägre impregneringstemperatur och under längre tid än vad som vanligen används i industrin. De använda koktemperaturerna är också betydligt lägre än vid konventionell sulfatkokning vilket gynnar jämn delignifiering. Detta resulterar i en smalare kappatalsfördelning jämfört med laboratoriekokade konventionella massor. Massor med höga kappatal undersöktes med avseende på egenskaper hos handark, såsom dragstyrka, dragstyvhet och kompressionsstyrka Det visades att handark från EIC massa vid kappatal 95 hade jämförbara styrkeegenskaper med konventionell massa vid kappatal 82. Vid jämförelse av effekten av stärkelse multilager på konventionella och EIC massor avslöjar liknande effekter. Användningen av stärkelsemultilager ökade dragindex och minskade dragstyvhets- och kompressions index (SCT, short-compression test). Kokprincipen har även använts för att ta fram en serie blekbara massor. Resultaten visar på möjligheten att öka lignininnehållet i massan in till i syrgasdelignifierings-steget eftersom spetinnehållet för milt defibrerad massa var lägre än 0,1% vid kappatal 49. I den här avhandlingen rekommenderar vi att vedflis impregneras i 2 timmar vid 110 °C för att neutralisera sura komponenter i veden och impregnera flisen med kokkemikalier, samt att utföra det efterföljande koket vid 135–140 °C beroende på önskat kappatal. Vi rekommenderar även att öka den tillgängliga mängden kokkemikalier i impregneringssteget genom att använda högre vätske-ved förhållande och att hålla alkali profilen relativt hög i det efterföljande koket. Detta koncept reducerar spetmängden, ger jämnare kokning och ökar selektiviteten för nedbrytning av lignin i sulfatkoket. / QC 20120216