Nesta pesquisa avaliou-se a influência da temperatura, da carga alcalina e dos aditivos antraquinona e etanol na deslignificação com oxigênio para polpa kraft de Eucalyptus grandis x Eucalyptus urophylla com alto número kappa e rejeitos, buscando a partir do desempenho do processo, definir as melhores condições para cada parâmetro estudado. Para produção da polpa celulósica foi utilizado o cozimento kraft convencional com carga alcalina de 13% e fator H de 580. Para redução do teor de rejeitos a polpa foi submetida, após o cozimento, a duas passagens por moinho desfibrador. A deslignificação com oxigênio foi feita em média consistência (10%), com pressão de oxigênio de 5 kgf.cm-2, em quatro cargas alcalinas (15, 30, 45 e 60 kg.t-1) e em quatro temperaturas (80, 100, 120 e 140ºC). Para avaliar o efeito dos aditivos foi feita a aplicação de 0,05% de antraquinona e etanol separadamente, bem como tratamentos sem aditivo como testemunhas. O número kappa da polpa produzida, a ser deslignificada, foi de 63,9 com 8,7% de rejeitos. A comparação entre os fatores carga alcalina e temperatura mostra que o primeiro é mais influente no processo de deslignificação com oxigênio, porém através da temperatura é possível reduzir o kappa com maior controle na seletividade, além disso, a temperatura serve de agente ativador das reações do processo, pois para qualquer carga aplicada a concentração de álcali residual diminui com o aumento da temperatura. O rendimento não apresentou queda com os aumentos da carga e da temperatura, pois, simultaneamente, a transformação dos rejeitos em polpa garante a manutenção do rendimento. A antraquinona não concedeu ganhos no rendimento e na eficiência da deslignificação, no entanto tornou o processo mais seletivo. A adição de etanol mostrou resultados positivos em termos de redução de número kappa, redução de rejeitos e também no rendimento. O total de sólidos gerados não sofreu influência significativa da ação dos aditivos. O teor de ácidos hexenurônicos foi baixo e não sofreu influência significativa de nenhum fator operacional. / This research evaluated the influence of temperature, alkali charge and the additives anthraquinone and ethanol at oxygen delignification for kraft pulp of Eucalyptus grandis x Eucalyptus urophylla with high kappa number and rejects, seeking, from the process performance, define the bests the conditions for each parameter studied. For the pulp production was used the conventional kraft cooking under soft conditions, alkali charge of 13% and H factor of 580. To reduce the rejects content the pulp was subjected, after cooking, for two passages by grinder mill. Oxygen delignification was done at medium consistency (10%), with oxygen pressure of 5 kgf.cm-², on four alkaline charges (15, 30 , 45 and 60kg.t-1) and four temperatures (80, 100, 120 and 140°C). To evaluate the actions of the additives they was applied 0,05 % of anthraquinone and ethanol separately and without additive, as well as witnesses treatments. The kappa number of the produced pulp, to be delignified, was 63,9% with 8,7% of rejects content. The comparison between the alkaline charge and temperature shows that the first one is more influential in the process, but through the temperature can reduce the kappa number with greater selectivity control, in addition the temperature is the activating agent of the process reactions, because for any alkaline charge applied the residual active alkali decreases with increasing temperature. The yield did not decreased with the increase of alkaline charge and temperature, because, simultaneously, processing the rejects into pulp ensures the yeld performance. The anthraquinone did not given earnings to the yield and efficiency of delignification, however anthraquinone increased the process selectivity. The addition of ethanol showed positive results in terms of kappa number reduction, rejects reduction and also at the yield improvement. The total solids generated was not affected by the action of additives, but the process as a whole, cooking and oxygen delignification, produced high content of solids generated. The hexenuronic acid content was low and was not affected by any operational factor.

Nesta pesquisa avaliou-se a influência da temperatura, da carga alcalina e dos aditivos antraquinona e etanol na deslignificação com oxigênio para polpa kraft de Eucalyptus grandis x Eucalyptus urophylla com alto número kappa e rejeitos, buscando a partir do desempenho do processo, definir as melhores condições para cada parâmetro estudado. Para produção da polpa celulósica foi utilizado o cozimento kraft convencional com carga alcalina de 13% e fator H de 580. Para redução do teor de rejeitos a polpa foi submetida, após o cozimento, a duas passagens por moinho desfibrador. A deslignificação com oxigênio foi feita em média consistência (10%), com pressão de oxigênio de 5 kgf.cm-2, em quatro cargas alcalinas (15, 30, 45 e 60 kg.t-1) e em quatro temperaturas (80, 100, 120 e 140ºC). Para avaliar o efeito dos aditivos foi feita a aplicação de 0,05% de antraquinona e etanol separadamente, bem como tratamentos sem aditivo como testemunhas. O número kappa da polpa produzida, a ser deslignificada, foi de 63,9 com 8,7% de rejeitos. A comparação entre os fatores carga alcalina e temperatura mostra que o primeiro é mais influente no processo de deslignificação com oxigênio, porém através da temperatura é possível reduzir o kappa com maior controle na seletividade, além disso, a temperatura serve de agente ativador das reações do processo, pois para qualquer carga aplicada a concentração de álcali residual diminui com o aumento da temperatura. O rendimento não apresentou queda com os aumentos da carga e da temperatura, pois, simultaneamente, a transformação dos rejeitos em polpa garante a manutenção do rendimento. A antraquinona não concedeu ganhos no rendimento e na eficiência da deslignificação, no entanto tornou o processo mais seletivo. A adição de etanol mostrou resultados positivos em termos de redução de número kappa, redução de rejeitos e também no rendimento. O total de sólidos gerados não sofreu influência significativa da ação dos aditivos. O teor de ácidos hexenurônicos foi baixo e não sofreu influência significativa de nenhum fator operacional. / This research evaluated the influence of temperature, alkali charge and the additives anthraquinone and ethanol at oxygen delignification for kraft pulp of Eucalyptus grandis x Eucalyptus urophylla with high kappa number and rejects, seeking, from the process performance, define the bests the conditions for each parameter studied. For the pulp production was used the conventional kraft cooking under soft conditions, alkali charge of 13% and H factor of 580. To reduce the rejects content the pulp was subjected, after cooking, for two passages by grinder mill. Oxygen delignification was done at medium consistency (10%), with oxygen pressure of 5 kgf.cm-², on four alkaline charges (15, 30 , 45 and 60kg.t-1) and four temperatures (80, 100, 120 and 140°C). To evaluate the actions of the additives they was applied 0,05 % of anthraquinone and ethanol separately and without additive, as well as witnesses treatments. The kappa number of the produced pulp, to be delignified, was 63,9% with 8,7% of rejects content. The comparison between the alkaline charge and temperature shows that the first one is more influential in the process, but through the temperature can reduce the kappa number with greater selectivity control, in addition the temperature is the activating agent of the process reactions, because for any alkaline charge applied the residual active alkali decreases with increasing temperature. The yield did not decreased with the increase of alkaline charge and temperature, because, simultaneously, processing the rejects into pulp ensures the yeld performance. The anthraquinone did not given earnings to the yield and efficiency of delignification, however anthraquinone increased the process selectivity. The addition of ethanol showed positive results in terms of kappa number reduction, rejects reduction and also at the yield improvement. The total solids generated was not affected by the action of additives, but the process as a whole, cooking and oxygen delignification, produced high content of solids generated. The hexenuronic acid content was low and was not affected by any operational factor.

The long-term trend regarding wood is an increase in price. Because wood contributes to a large part of production costs, the efficient utilisation of wood is greatly desired to reduce production costs for kraft pulp producers. During the 1990s, the development of improved modified kraft cooking began, which led to higher yields. There was also a trend of terminating kraft cooking at a higher kappa number to maximise the overall yield. For hardwood, the defibration point became a critical setback in allowing this termination at a high kappa number. This thesis discusses how this issue has been tackled in the laboratory by using improved modified kraft cooking combined with extended impregnation to enable a decrease in reject content and shift the defibration point towards a higher kappa number for hardwood. This lab concept is referred to as extended impregnation kraft cooking (EIC), and this thesis reveals that EIC cooking efficiently reduces the reject content for both birch and eucalypt. By using EIC cooking, the defibration point was shifted to a kappa number of ca. 30 from ca. 20 using conventional kraft cooking. This study demonstrates the great potential for achieving a higher overall yield for eucalypt by terminating the EIC cooking at a high kappa number, but with the conditions used in this thesis, no improvement in yield was observed for birch.   An important issue is that the termination of kraft cooking at high kappa number increases the demand for extended oxygen delignification to reach a similar kappa number into bleaching, i.e., due to cost and environmental reasons. Extended oxygen delignification was shown to be possible for both birch and eucalypt EIC pulps (i.e., from kappa number 27 to 10) with an acceptable pulp viscosity number.   The other part of this thesis addresses aspects regarding the limitations in oxygen delignification. It has previously been shown in the literature that a high xylan yield of kraft cooking could negatively affect the efficiency of subsequent oxygen delignification. In this work, the increased xylan content in eucalypt kraft pulp within the range of 8–18% had only a marginally negative impact on the oxygen delignification efficiency after correcting for the HexA contribution to the kappa number. It is also desired to extend the oxygen delignification towards lower kappa number, i.e., below kappa number 10 to decrease the bleaching chemical requirement. In this study, the hypothesis that the reduced efficiency of oxygen delignification at low kappa numbers could partly be due to the formation of oxidisable carbohydrate-related structures (i.e., HexA and/or other non-lignin structures) was also tested. No formation was established. On the other hand, a final oxygen delignification stage in the bleaching could be an attractive alternative for reducing yellowing and enhancing brightness; in fact, this has led to the development of a patent (SE 528066). / Ved står för en stor del av produktionskostnaderna vid framställning av sulfatmassa. Då vedpriserna har ökat genom åren är ett effektivt utnyttjande av veden önskvärt för att kunna sänka produktionskostnaderna. Under 1990-talet förbättrades den modifierade sulfatkokningen vilket innebar möjlighet till högre massautbyte. För att maximera massautbytet styrdes kokningsprocessen mot ett högre kappatal. Detta har visat sig vara svårare för lövved än för barrved, eftersom defibrerbarhetspunkten utgör ett kritiskt hinder. I denna avhandling har laborationsstudier utförts där förbättrad modifierad sulfatkokning kombinerats med förlängd impregnering för att kunna sänka spethalten och därmed förskjuta defibrerbarhetspunkten mot ett högre kappatal. Detta koncept kallas för extended impregnation kraft cooking (EIC). EIC-kokning visade sig vara en effektiv metod för att minska spethalten hos björk och eukalyptus. Med EIC-kokning kunde defibrerbarhetspunkten höjas från cirka 20 till cirka 30. I denna avhandling klarläggs att det finns stora möjligheter att öka massautbytet för eukalyptus genom att avsluta sulfatkoket vid ett högre kappatal. För björk kunde ingen ökning av massutbytet uppnås genom ovanstående metod.   Vid ett högre kappatal efter sulfatkoket ställs även krav på förlängd syrgasdelignifiering, för att kunna behålla samma kappatal in till blekeriet. Det visade sig vara fullt möjligt att förlänga syrgasdelignifieringen för de EIC-kokade björk- och eukalyptusmassorna (d.v.s. från kappatal 27 till 10) med accepterad massaviskositet.   Den andra delen av avhandlingen tar upp aspekter på syrgasdelignifieringens begränsningar. Tidigare studier har visat att ett högre utbyte av xylan vid sulfatkokning kan vara negativt för syrgasdelignifieringens effektivitet.  I denna studie har det påvisats att en ökad xylanhalt i intervallet 8–18 procent i eukalyptusmassa endast har en marginell negativ inverkan på syrgasdelignifieringens effektivitet efter att kappatalet korrigerats för HexA. Det är önskvärt att förlänga syrgasdelignifieringen till ett lägre kappatal än 10 för att minska förbrukningen av blekkemikalier. I den här studien prövades hypotesen att syrgasdelignifieringens begränsningar vid låga kappatal, under 10, delvis skulle kunna bero på bildning av oxiderbara kolhydratrelaterade strukturer (d.v.s. HexA och/eller andra okända ”non-lignin”-strukturer). Ingen bildning kunde dock observeras. Däremot indikerades att ett syrgassteg i slutet av bleksekvensen skulle kunna vara ett eftersträvansvärt alternativ för minskad eftergulning och ökad ljushet, vilket ledde till ett patent (SE 528066). / QC 20120507

Abstract Quality and economical requirements have raised evident need and interest in the industry to further develop continuous kraft cooking. A Kappa number, representing the cooking degree, is one of the few quality measures of cooking, and usually the only one measured on-line. Cooking degree is mainly controlled by temperature, chemical charge, and cooking time. Cooking conditions strongly depend on the packing degree of a chip column in the digester. At the same time, the packing of a chip column is affected by the cooking degree of chips. A typical problem is that the conditions and cooking degree in the process are not known. To achieve better control, more information about the cooking process is required. The aim of this thesis has been to more accurately describe the cooking conditions and phenomena in the digester scale. Conventional and Downflow Lo-Solids™ continuous cooking processes, producing both softwood and hardwood pulp, were investigated. Information achieved from measurements, and physical and chemical models describing chip scale phenomena, were utilised. Kappa number modelling was based on the use of an optimised and on-line adapted Gustafson's model. Modelling over grade change situations was accomplished by smoothly adjusting the model parameters as a function of temperature change profiles. Real-time profiles of cooking chemicals, temperature, and lignin and carbohydrates contents of chips within the processes were modelled. These real-time profiles were utilised in the modelling of the chip column's packing degree in the conventional process. Based on the developed models, blow-line Kappa numbers of both processes were predicted. By exploiting the prediction results, a new control strategy for the Kappa number was developed. In the strategy, set points for chemical charge and cooking temperature are iteratively solved by using only the developed prediction models of the blow-line Kappa number. It was shown that the modelled profiles of wood components and cooking chemicals can give new information regarding the continuous cooking processes. The modelling results are feasible in control purposes, and they also can support the operators' work. In the new control strategy, compared to the widely used H-factor based control, chemical concentrations can be more precisely taken into account.

To decrease the environmental footprint, the textile industry needs to become more circular. One company that is trying to close the textile lifecycle loop is the Swedish company Renewcell. In the Renewcell process, discarded clothes and other textile waste are turned into a dissolving pulp that can be used for production of new textiles. For this to work, it is important to generate a non-colored dissolved pulp. Therefore, it is of great interest to be able to optimize the bleaching process and evaluate different starting materials. Today, there are different methods that have been used for quantification of specific dyes and for identification of raw materials in textiles. However, there is no complete method that can be used for all types of dyes and raw materials. This master thesis will therefore investigate the bleaching step and the raw materials used in Renewcell’s recycling process. The aim with this project is to develop a method, to be able to analyse the presence of dyes qualitatively and quantitatively in the dissolved pulp from the recycled cotton-based textiles. To do so, different chemical analysing methods were used. These include kappa number measurements, UV-VIS and FTIR. Nine different types of jeans, one yarn, three raw materials (cotton, PET and elastane), and two pure dyes (indigo and black sulfur dye) were selected for this project. The result from the kappa number measurements shows that only the blue jeans, blue yarn and black jeans could be bleached and measured by using the original kappa number method at 25 degrees C. But when the same procedure was done manually and the temperature was increased to 70 degrees C, almost all materials could be bleached and measured. Therefore, the conclusion is that this method can be a successful quantification method. However, the temperature correction equation needs to be developed further to be able to quantify the exact amount of dyes. The kappa number was also compared with the absorbance factor, i.e. the k-value from the UV-VIS results. A correlation could be seen for the blue jeans, blue yarn, and black jeans. So, the UV-VIS method could also be a possible method for quantification of dyes in textiles. For the qualitative analyses, FTIR was used. The results showed that the raw materials could be identified by comparing the resulting FTIR spectra with a reference spectrum. For the jeans and yarn materials, indigo dye was identified for the blue jeans, blue yarn, and black jeans. However, for the other materials, the amount of dyes was too low to be able to draw conclusions about the chemical structure. With further development, these methods could be used as successful qualitative and quantitative methods for analysing dyes in textiles. This would generate positive consequences in several ways. The usage of bleaching chemicals could be optimized, and the quality of the final textile material could be improved. This would benefit both the manufacturer of these recycled textiles (economically) and the consumer who will buy the final product (quality). Indirectly, this would help to decrease the environmental footprint from the textile industry.

After cooking, kraft pulps always contain not only residual lignin but also significant amounts of hexenuronic acid and other non-lignin structures oxidizable by permanganate under the standard kappa number determination conditions. These here referred to as false lignin. Like ordinary lignin, the false lignin also consumes bleaching chemicals, thus increasing both the production costs and the environmental impact of bleach plant effluents. The false lignin also has an effect on pulp properties such as brightness stability. This necessitates the development of efficient experimental routines for the determination of false lignin in different types of unbleached and bleached kraft pulps, together with studies of its formation, chemical behaviour, and ultimate fate. The main aim of this work has been to establish a method for the quantification of various types of oxidizable structures in bleached kraft pulps and to study their impact on pulp quality, particularly, on the brightness stability of pulps bleached in elemental-chlorine-free (ECF) and a totally-chlorine-free (TCF) processes. Part of this research deals with the relationship between the kappa number and the lignin content in the case of partly oxidized lignins. Spruce and birch kraft pulps processed according to the ODEQP and OQ(OP)Q(PO) bleaching sequences, respectively, have been analyzed. It has been found that the oxidation equivalent of the residual lignin decreases with increasing degree of oxidation along each bleaching sequence. This finding has been further supported by experiments with a number of model compounds. The Ox-Dem kappa number method has been shown to be an accurate means of determining the residual lignin content and of monitoring the efficiency of lignin removal along different bleaching sequences. It has been demonstrated that the kappa number can always be fractioned into partial contributions, the first of which comes from the residual lignin and is measured by the Ox-Dem kappa number, and the second from the false lignin and is given by the difference between the standard kappa number and the Ox-Dem kappa number. The effect of false lignin on the pulp kappa number is most pronounced in unbleached and oxygen-delignified kraft pulps. The extractability of residual and false lignin in different solvents has been investigated. The changes that occurred in the kappa number following different extraction steps have been compared with corresponding changes in the chemical composition and the conclusion has been drawn that the hemicellulose component of a kraft pulp is a major sourse of non-lignin structures contributing to the kappa number. The influence on the brightness stability of various oxidizable structures, viz.: residual lignin, hexenuronic acid and other non-lignin structures, in spruce, birch and eucalyptus kraft pulps bleached in ECF and TCF type processes was studied. It was demonstrated that the selective removal of all false lignin structures significantly improves the brightness stability. The degree of yellowing was found to be proportional to the content of HexA groups in pulps. It has been shown that 2-furancarboxylic acid, 5-formyl-2furancarboxylic acid and reductic acid are formed during the course of thermal yellowing. The influence of two bleaching sequences, D0(EP)D1 (ECF-type) and Q1(OP)Q2(PO) (TCF)-type, on the content of different oxidizable structures in eucalyptus kraft pulp was studied in relation to the brightness stability of the pulp. It was shown by kappa number fractionation that pulp bleached to full brightness with ECF- and TCF-type sequences contains different amounts of HexA. The most significant discoloration was observed in the case of TCF-bleached pulp having an especially high content of HexA. The mechanism of the moist (8 % moisture) thermal yellowing of fully bleached kraft pulps was further studied using dissolving pulp impregnated with a set of model compounds representing the most likely HexA degradation products, viz. as 2-furancarboxylic acid (FA), 5-formyl-2-furancarboxylic acid (FFA) and reductic acid (RA), either alone or in combination with Fe(II) or Fe(III) ions. It was found that the latter two acids take part in reactions leading to colour formation whereas 2-furancarboxylic acid does not. The effect of iron ions on the colour formation appears to vary with their oxidation state. The brightness loss caused by either FFA or RA, present in an amounts similar to the content of HexA in industrial pulps, was of the same order of magnitude as that observed in industrial pulps aged under the same conditions. Based on these findings, it is suggested that the overall mechanism of moist thermal yellowing involves several stages, including the degradation of hexenuronic acid and the formation of reactive precursors, such as 5-formyl-2-furancarboxylic acid and reductic acid. The presence of ferrous ions further enhances the discoloration. / QC 20101005

No description available.

Chemical components in wood contain multiple anionic groups, including carboxyl groups and hydroxyl groups. During kraft cooking and bleaching, such structures are also formed, degraded or modified by the action of reactions both deliberate and unwanted. It has previously been found by Laine that anionic groups with pKa values of 3.3 and 5.5 can explain the observed anionic charge on chemical fibres, corresponding to carboxylic acids on hemicelluloses as well as oxidized lignin structures, respectively. It has further been found that most of the fibre charge can be accounted for through the contribution from methylglucuronic acids as well as hexenuronic acids. This study aimed to provide additional information regarding the charge component unaffiliated with either of the aforementioned uronic acids by studying kraft pulps procured from an industrial kraft mill corresponding to unit operations through a fibreline using the ODHot(EOP)D1D2 bleaching sequence. Each sample had its total charge determined by means of conductometric titration, its content of methylglucuronic acid determined by means of methanolysis followed by GC, and its content of hexenuronic acids determined by means of the HUT-method for the determination of hexenuronic acids, followed by either UV absorbance measurements or calculations based on the reduction in kappa number during the selective acid hydrolysis. The lignin content was determined by means of kappa number analysis as well as by calculations based on the kappa number after selective acid hydrolysis, which was assumed to be characteristic of the kappa number addition from the lignin content of the samples. The hexenuronic acid content was successfully determined according to the HUT-method. A difference in content was observed when results for the unbleached and oxygen delignified samples that was obtained from UV measurements were compared with the observed difference in kappa number prior and after selective acid hydrolysis for said samples. In both cases, the results based on the difference in kappa number was higher. No correlation between remaining charge and lignin content could be made. It was instead observed that individual bleaching steps had binary effects on each of the analysed components of the fibre charge. A significant increase in charge unaffiliated with methylglucuronic acid or hexenuronic acid was observed during the EOP step, indicating an oxidation of chemical structures in the pulp: this effect could not be correlated to lignin content. / Kemisk massa kan ses som ett kompositmaterial bestående av cellulosa, hemicellulosa och lignin. Dessa beståndsdelar, liksom separata lågmolekylära föreningar, innehåller anjoniska kemiska grupper som bidrar till att ge träfibrer en anjonisk laddning. Ytterligare sådana grupper kan bildas under reaktioner vid kokning och blekning, tillika kan sådana grupper modifieras eller brytas ner. Laine har tidigare visat att fiberladdningen kan förklaras genom två skilda kategorier av kemiska grupper med pKa värden på 3,3 samt 5,5, vilka kan kopplas till karboxylsyragrupper på hemicellulosor respektive till lignin. Man har därtill funnit att stora delar av fiberladdningen kan förklaras genom tillskott från de två uronsyrorna metylglukuronsyra och hexenuronsyra. Denna studie syftar till att undersöka det laddningstillskott som inte kan länkas till någon av dessa två uronsyror. Detta har gjorts genom att studera kemiska massor från industrin, tagna från de olika stegen i en bleksekvens av typen ODHot(EOP)D1D2. Massornas totalladdning mättes medelst konduktometrisk titrering, emedan metylglukuronsyrahalten mättes via methanolysis följt av GC och hexenuronsyrahalten mättes via selektiv syrahydrolys per HUT-metoden följt av UV-karakterisering respektive beräkningar baserade på differensen i kappa tal före och efter sagda hydrolys. Ligninhalten i samtliga prov mättes via kappatalsmätningar samt genom beräkningar baserade på kappatalet efter selektiv syrahydrolys, vilket anses vara kappatalsbidraget från ligninföreningarna. Hexenuronsyrahalterna uppmätta medelst UV-karakterisering respektive kappatalsdifferens jämfördes mot varandra och fanns ge olika resultat för de oblekta och syrgasdelignifierade massorna. I bägge fallen gav mätningen baserade på kappatalsdifferens högre utslag. Ingen korrelation mellan kvarvarande laddning - totalladdning minus tillskottet från uronsyrorna - och ligninhalt kunde observeras. Istället observerades binära effekter för varje uppmätt komponent under vardera blekningssteg. Under EOP-steget observerades ett tillskott till den kvarvarande laddningen, vilket skulle kunna förklaras genom oxidation av trästrukturer. Dock kan ej heller detta relateras till ligninhalten i proverna.

<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