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Fenton Pre-treatment of a Birch Kraft Pulp for MFC preparationHellström, Pia January 2015 (has links)
The potential to use acidic hydrogen peroxide in the presence of ferrous ions (Fenton’s reagent) as a pre-treatment when producing microfibrillar cellulose (MFC) from a fully bleached birch (Betula verucosa) kraft pulp was investigated and the properties of the produced MFC was compared to the properties of a MFC produced with enzymatic pre-treatment with a monocomponent endoglucanase (FiberCare® R). The mechanical treatment to MFC was performed in a laboratory colloid mill or in a pilot high-pressure homogeniser and the pre-treated pulps as well as the produced MFCs were chemically and morphologically characterised. Additionally, the MFCs produced in the colloid mill were evaluated as strength enhancers in test sheets representing the middle ply of paperboard. From the chemical characterisation, it was concluded that the Fenton pre-treatment caused a decrease in the degree of polymerisation (DP) and an increase in both carboxyl- and carbonyl groups. The increase in carbonyl groups could not be explained by the formation of new reducing end groups due to depolymerisation which indicates that carbonyl groups are introduced along the cellulose chain. The enzymatic pre-treatment as performed in this study caused less impact on the cellulosic material, i.e. resulted in a pulp with a higher DP and a much lower amount of carbonyl- and carboxylic groups compared with the Fenton pre-treated pulps. In the subsequent mechanical treatment in a colloid mill, the Fenton pre-treated pulps were easier to process mechanically i.e. reached a higher specific surface area and a higher surface charge at a given mechanical treatment time compared to enzymatic pre-treated pulps and pulps not subjected to any pre-treatment. These findings were confirmed when MFCs were produced by homogenisation at high pressure in multiple passes; the birch kraft pulp was either pre-treated with Fenton’s reagent or the combined mechanic and enzymatic pre-treatment methodology used at the Centre Technique du Papier (CTP, France). By size fractionation, rheological measurements and scanning electron microscopy, it was revealed that Fenton pre-treatment resulted in MFC suspension containing a significantly higher proportion of small sized material (< 0.2 mm). When the MFCs were evaluated as strength enhancers in test sheets produced from a furnish consisting of a spruce (Picea abies) chemithermomechanical pulp, MFC and a retention system containing cationic starch and an anionic silica sol, Fenton pre-treated MFCs increased the strength properties more than the enzymatic pre-treated MFCs. Addition of 5 wt% Fenton pre-treated MFC resulted in an increase in z-directional strength of about 50%, an increase in tensile stiffness index of about 25% and an increase in tensile index of 35% compared to test sheets prepared without MFC addition. / The potential to use acidic hydrogen peroxide in the presence of ferrous ions (Fenton’s reagent) as a pre-treatment when producing microfibrillar cellulose (MFC) from a bleached birch kraft pulp was investigated and the properties of the produced MFC was compared to the properties of a MFC produced with enzymatic pre-treatment. Additionally, the MFCs evaluated as strength enhancers in test sheets representing the middle ply of paperboard. From the chemical characterisation, it was concluded that the Fenton pre-treatment caused a decrease in the degree of polymerisation (DP) and an increase in both carboxyl- and carbonyl groups. In the subsequent mechanical treatment in a colloid mill, the Fenton pre-treated pulps were easier to process mechanically indicating a potential to lower the energy consumption. When the MFCs were evaluated as strength enhancers in test sheets, Fenton pre-treated MFCs increased the strength properties more than the enzymatic pre-treated MFCs at a given mechanical treatment time. Addition of 5 wt% Fenton pre-treated MFC resulted in an increase in z-directional strength of about 50%, an increase in tensile stiffness index of about 25% and an increase in tensile index of 35% compared to test sheets prepared without MFC addition.
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The origin of fibre charge in chemical pulp / Fiberladdningars ursprung i kemisk massaLindén, Pär January 2013 (has links)
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.
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