Ron Janzon

Upgrading of paper-grade pulps to dissolving pulps by nitren extraction : Optimisation of extraction parameters and application to different pulps

Abstract Xylans were selectively removed from paper-grade pulps by nitren extraction to produce dissolving pulps. Extraction parameters were optimised for a birch kraft pulp regarding time, temperature, liquor/pulp ratio, and total nitren charge. Furthermore, the applicability of the method was investigated for two other kraft pulps obtained from eucalyptus and mixed softwood, and for one beech sulfite pulp. Extracted pulps were characterised regarding their carbohydrate content and Cuen viscosity. The nitren charge was a decisive factor for xylan removal and pulp purity. The combination of a high nitren concentration and low liquor/pulp ratio was most effective for xylan removal. However, a high liquor/pulp ratio with a lower nitren concentration proved to be more selective and minimised cellulose degradation as well. Glucomannans were almost insoluble under the extraction conditions investigated. Therefore, softwood pulps were not suitable for the upgrading of chemical pulps to dissolving pulps by nitren extraction. On the other hand, hardwood pulps obtained by kraft and sulfite processes contained 96–97% cellulose after nitren extraction.

Effects of cationic xylan from annual plants on the mechanical properties of paper.

Xylan from oat spelt and wheat was used as an additive to enhance the dry strength of paper. The absorption of xylan by the cellulose fibers was increased by cationization to different degrees of substitution. Paper hand sheets with different doses of xylan and industrial cationic starch were produced, and the mechanical properties were determined. Absorption measurements of cationic oat spelt xylan on pulp fibers explained the differing influences of low and high cationized xylan addition on paper strength. The addition of cationic oat spelt xylan with a degree of substitution of 0.1 at a 4% dose provided the largest improvement in the tensile-index (67%), burst-index (105%) and tear-index (77%). Compared to cationic starch, cationic oat spelt xylan additives led to similar paper strength values, excepting the tear strength. The structural differences and protein impurities made the wheat xylan unsuitable as a strength additive for paper pulp.

Hot water extraction of Norway spruce (Picea abies [Karst.]) bark: analyses of the influence of bark aging and process parameters on the extract composition

Abstract The hot water (HW) extraction of Norway spruce (Picea abies [Karst.]) delivers condensed tannins and considerable amounts of other compounds. Yield and composition of the HW extracts were investigated as a function of natural weathering for up to 15 months. Total phenol monomers and oligomers were detected by Folin-Ciocaltau assay after fractionation by solid phase extraction (SPE). Procyanidins (PC) were determined by HPLC-UV after acid thiolysis and carbohydrates by HPLC combined with acid hydrolysis. Topochemistry of the bark before and after extraction was investigated by UV-microspectrometry (UMSP) and non-extractable PC analyzed by direct thiolysis on the bark. The influence of the parameters on the yield and composition of the extracts were evaluated, such as the extraction temperature, time and the addition of sodium sulfate and urea. Prolonged weathering resulted in a considerable decrease of the total extraction yield, partly because of leaching of phenolic monomers, mono- and oligosaccharides. The yield of phenolic oligomers also decreased at a moderate rate, while the yield of polysaccharides (pectins) was almost stable. Non-extractable and non-leachable compounds deposited in the cell lumens represent the majority of the phenolic extractives in spruce bark. Sequential extractions performed at increasing temperature proved to be a suitable method for the recovery of tannin-rich extracts.

Steam pretreatment of spruce forest residues: optimal conditions for biogas production and enzymatic hydrolysis.

Steam refining of non-debarked spruce forest residues was investigated as pretreatment for enzymatic hydrolysis as well as for biogas production. Pretreatment conditions were varied in the range of 190-220 °C, 5-10 min and 0-3.7% SO₂ according to a statistical design. For both applications highest product yields were predicted at 220 °C and 2.4% SO₂, whereas the reaction time had only a minor influence. The conformity of the model results allows the conclusion that enzymatic hydrolysis is a suitable test method to evaluate the degradability of lignocellulosic biomass in the biogas process. In control experiments under optimal conditions the results of the model were verified. The yield of total monomeric carbohydrates after enzymatic hydrolysis was equivalent to 55% of all theoretically available polysaccharides. The corresponding biogas yield from the pretreated wood amounted to 304 mL/gODM. Furthermore, furans produced under optimal process conditions showed no inhibitory effect on biogas production. It can be concluded that steam refining opens the structure of wood, thus improving the enzymatic hydrolysis of the polysaccharides to fermentable monomeric sugars and subsequently enabling a higher and faster production of biogas. Anaerobic fermentation of pretreated wood is a serious alternative to alcoholic fermentation especially when low quality wood grades and residues are used. Anaerobic digestion should be further investigated in order to diversify the biorefinery options for lignocellulosic materials.

Steam pretreatment for enzymatic hydrolysis of poplar wood: comparison of optimal conditions with and without SO2 impregnation

Abstract Steam refining of non-debarked poplar wood with SO2 impregnation prior to steaming was investigated as pretreatment for enzymatic hydrolysis. Pretreatment conditions were varied in the range of 170°C–220°C, 3–30 min and 0.7–2.5% SO2 according to a factorial design. Predicted steaming conditions for highest carbohydrate yields after enzymatic hydrolysis were at 200°C, 15 min, and 2.5% SO2. The yield of glucose and xylose from control tests under these conditions was 43% representing an increase of 9% compared to results of former experiments without SO2 impregnation. Investigations on lignin extracted from the fibers revealed no distinct differences between pretreatment with and without SO2. No sulfonation occurred by the impregnation with SO2. Topochemical analyses of the fibers by cellular UV microspectrophotometry (UMSP) showed an inhomogeneous lignin distribution within the S2 of fibers after pretreatment without SO2 and local depositions of high UV-absorbing substances in the lumina of fibers and parenchyma cells. The lignin distribution of fiber cell walls after pretreatment with SO2 was more homogeneous with a preserved fiber network and only little amounts of deposited phenolic compounds in the lumina. Therefore, it might be concluded that the expulsion of lignin hinders the enzymes in accessing the cellulose.

Anaerobic digestion of fines from recovered paper processing – Influence of fiber source, lignin and ash content on biogas potential

Fines concentration harms paper machine runability and output quality in recovered paper processing, hence, their extraction would be fundamentally beneficial. In this study, separated fines from an industrial recycled fiber pulp (RFP) were characterized and evaluated for their potential biogas yields with a focus on understanding the role of varying lignin and ash contents. Further, these results were compared with biogas yields from conventional chemical and mechanical pulps. Overall, methane yields of fines from mechanical pulps (21-28mL/gVS) and RFP (127mL/gVS) are relatively low compared to the high methane yields of 375mL/gVS from the chemical pulp fines. However, it was shown that the high ash content in RFP fines (up to 50%) did not negatively influence overall yield, rather, it was the presence of slowly biodegrading lignin-rich fiber fines.

Enzymatic treatment of deinking sludge – effect on fibre and drainage properties

ABSTRACT This work focused on the enzymatic treatment of deinking sludge (DS), a waste stream arising from German deinked pulp mills. Three industrial DS samples were characterised with respect to chemical composition and fibre morphology. In this study, four cellulase enzyme preparations were tested under neutral pH conditions and one cellulase was identified as suitable for DS conditioning with no need of pH adjustment. Additionally, our approach shows that inorganic particles contained in the DS samples do not negatively affect cellulase activity, as illustrated by respectable hydrolysis yields of up to 61%. Enzymatic treatment of DS led to fibre shortening and fibre fines generation with increasing enzyme dose and incubation time. The dewaterability of enzyme-treated DS samples was tested and the results showed that high amounts of fibre fines enhanced filter cake consolidation during dewatering, resulting in higher cake solids. A 10–14 percentage point increase in cake solids was obtained depending upon the enzyme dose applied, the origin of the DS sample, and the exposure period. Through the enzymatic treatment the annually generated amount of DS in Germany could be reduced by up to 20%, which would mean considerable disposal cost savings.

Determination of uronic acids and neutral carbohydrates in pulp and biomass by hydrolysis, reductive amination and HPAEC-UV

Abstract The exact quantification of all carbohydrate constituents in wood and pulp is a challenge because of the various glycosidic linkages of the polysaccharides with different stabilities. The individual detector responses for the compounds in the hydrolysates additionally complicate the quantification as pure standards for 4-O-methyl-α-D-glucuronic acid (meGlcA) and related oligosaccharides are not commercially available for calibration. In the present paper, a new analytical procedure is presented, based on the reductive amination of the carbohydrates obtained via acidic and enzymatic hydrolysis of the polysaccharides before quantification by means of high performance anion exchange chromatography (HPAEC) and UV-detection. This approach was suitable for the analysis of neutral carbohydrates and uronic acids obtained via enzymatic hydrolysis from bleached pulps. In the case of unbleached pulps, the enzymatic hydrolysis was not complete and unhydrolyzed nano-scaled and micro-scaled particles remained in the hydrolysates as detected by dynamic light scattering (DLS) measurements. The new HPAEC-UV methodology was also applied to kraft pulps and a sulfite pulp; six different kinds of wood as well as wheat straw and bagasse. All relevant monosaccharides and the dimer of meGlcA and xylose could be detected in the hydrolysates. Accordingly, significantly higher yields of meGlcA were found compared to literature data.