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Yang, J., Zasadowski, D., Edlund, H. & Norgren, M. (2019). Biorefining of Spruce TMP Process Water: Selective Fractionation of Lipophilic Extractives with Induced Air Flotation and Surface Active Additive. BioResources, 14(2), 4124-4135
Open this publication in new window or tab >>Biorefining of Spruce TMP Process Water: Selective Fractionation of Lipophilic Extractives with Induced Air Flotation and Surface Active Additive
2019 (English)In: BioResources, ISSN 1930-2126, E-ISSN 1930-2126, Vol. 14, no 2, p. 4124-4135Article in journal (Refereed) Published
Abstract [en]

Lignocellulose biomass plays an important role in reducing thedependency on fossil fuels and ameliorating the dire consequences ofclimate change. It is therefore important that all the components oflignocellulose biomass are exploited. These components includehemicelluloses and extractives that are liberated and sterically stabilizedduring the thermomechanical pulping and that form the dissolved andcolloidal substance (DCS) in the process water. Biorefining of this processwater can extract these substances, which have a number of promisingapplications and can contribute to the full exploitation of lignocellulosebiomass. This paper presents a simple treatment of unbleached Norwayspruce (Picea abies) process water from TMP (thermomechanical pulping)production using induced air flotation (IAF) and cationic surfactant,dodecyl trimethylammonium chloride (DoTAC) to refine the extractivesand prepare the waters so that hemicellulose could be easily harvested ata later stage. By applying 80 ppm of DoTAC at a pH of 3.5 and 50 °Cbefore induced air flotation, 94% of the lipophilic extractives wererecovered from process water. Dissolved hemicellulose polysaccharideswere cleansed and left in the treated process water. The process enabledefficient biorefining of lipophilic extractives and purification of the processwater to enable more selective harvesting of hemicelluloses in subsequentsteps.

Keywords
Biorefining; Lipophilic extractives; Thermomechanical pulping; Induced air flotation
National Category
Chemical Engineering
Identifiers
urn:nbn:se:miun:diva-35955 (URN)10.15376/biores.14.2.4124-4135 (DOI)000466449000115 ()2-s2.0-85071077339 (Scopus ID)
Projects
EU Reginal fund 2
Funder
European Regional Development Fund (ERDF)
Available from: 2019-04-05 Created: 2019-04-05 Last updated: 2019-09-03Bibliographically approved
Zasadowski, D., Yang, J., Edlund, H. & Norgren, M. (2014). Antisolvent precipitation of water-soluble hemicelluloses from TMP process water. Carbohydrate Polymers, 113, 411-419
Open this publication in new window or tab >>Antisolvent precipitation of water-soluble hemicelluloses from TMP process water
2014 (English)In: Carbohydrate Polymers, ISSN 0144-8617, E-ISSN 1879-1344, Vol. 113, p. 411-419Article in journal (Refereed) Published
Abstract [en]

During the thermomechanical pulping (TMP) of spruce, hemicelluloses (mainly galactoglucomannans, GGMs) are released into the process water at relatively low concentrations that are currently impossible to efficiently recover. This paper examines the recovery of hemicelluloses precipitated from TMP process water via solubility reduction by adding antisolvents such as methanol, ethanol, and acetone. The phase separation was monitored by turbidity measurements. Gravimetric analysis, FTIR, GC–MS, UV spectroscopy, and ICP-OES were used to determine the yield, purity, and composition of the precipitates. Gel permeation chromatography and pulsed field-gradient self-diffusion NMR were used to measure the molecular mass distribution of the precipitates. Acetone was found to be the most efficient antisolvent, giving the highest yield at the lowest addition. The contents of lipophilic extractives and lignin impurities were below 0.5% and 1.6%, respectively, and the metal content was approximately 2% in the precipitates obtained with acetone.

Keywords
Antisolvent precipitation, Flotation, Hemicelluloses, Process water, Recovery, Thermomechanical pulping
National Category
Chemical Engineering
Identifiers
urn:nbn:se:miun:diva-22315 (URN)10.1016/j.carbpol.2014.07.033 (DOI)000343613000052 ()2-s2.0-84907321202 (Scopus ID)
Available from: 2014-06-27 Created: 2014-06-27 Last updated: 2017-12-05Bibliographically approved
Zasadowski, D., Strand, A., Sundberg, A., Edlund, H. & Norgren, M. (2014). Selective purification of bleached spruce TMP process water by induced air flotation (IAF). Holzforschung, 68(2), 157-165
Open this publication in new window or tab >>Selective purification of bleached spruce TMP process water by induced air flotation (IAF)
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2014 (English)In: Holzforschung, ISSN 0018-3830, E-ISSN 1437-434X, Vol. 68, no 2, p. 157-165Article in journal (Refereed) Published
Abstract [en]

The environmentally benign closure of water systems in paper mills leads to the problem of accumulation of dissolved and colloidal wood substances (DCS) in process water. Notably, pitch affects the pulp and paper production negatively and increases the demand for additional treatment of the process water. In the present article, the purification of thermomechanical pulping process water from the alkaline peroxide bleaching stage has been investigated, with the induced air flotation (IAF) in focus. The following parameters were considered concerning the IAF efficiency to remove detrimental substances: concentration of cationic foaming agent, pH value, calcium concentration, and temperature. The amounts and characteristics of residual DCS were determined by gas chromatography and turbidity measurements. Residual concentrations of the foaming agent dodecyltrimetylammonium chloride were determined by electrospray ionization mass spectrometry. Up to 90% of pitch was removed, whereas hemicelluloses, which are important in preventing pitch problems, remained in the waters. Up to 70% of the pectic acids accounted for the high cationic demand of the process waters were removed by optimization of the IAF parameters. The presented separation process gives new opportunities to a selective purification of the process waters.

Keywords
cationic dodecyltrimetylammonium chloride (DoTAC), cationic foaming agent (DoTAC), colloidal wood pitch, induced air flotation, mechanical pulp, pectic acids, peroxide bleaching
National Category
Chemical Sciences
Identifiers
urn:nbn:se:miun:diva-19809 (URN)10.1515/hf-2013-0045 (DOI)000331947600003 ()2-s2.0-84900602252 (Scopus ID)
Note

Published online 2013-08-10.

Available from: 2013-08-29 Created: 2013-08-29 Last updated: 2017-12-06Bibliographically approved
Zasadowski, D. (2014). Selective Separation Of Wood Components In Internal Process Waters Originating From Mechanical Pulping. (Doctoral dissertation). Sundsvall: Mid Sweden University
Open this publication in new window or tab >>Selective Separation Of Wood Components In Internal Process Waters Originating From Mechanical Pulping
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Dissolved and Colloidal substances (DSC) and metals are released from woodduring thermomechanical pulp (TMP) production. These components have atendency to accumulate in process waters, as the water circulation systems inintegrated paper mills are closed. Disturbances such as pitch depositions in thepaper machine (pitch problems), specks in the paper, decreased wet and drystrength, interference with cationic process chemicals, and impaired sheetbrightness and friction properties appear when DSC are present. Transition metalions such as manganese results in higher consumption of bleaching chemicals(hydrogen peroxide) and lowers the optical quality of the final product, andaddition of complexing agents, such as EDTA or DTPA, to prevent this is needed.The never ending trends to decrease water consumption and increase processefficiency in pulp and paper production emphasizes that it is very important bothto know the effects of wood substances on pulping and papermaking and to beable to remove them in an efficient way. From a biorefinery point of view, DSCcomponents can be promising renewable raw materials for biofuels, bio‐basedchemicals and materials.In this thesis, a new approach using induced air flotation (IAF) without a cationicpolyelectrolyte addition for the removal of pitch and metal ions from mechanicalpulp mill process waters is presented. The induced air flotation of different processwaters is facilitated by the addition of a chelating surfactant and different foamingagents. The influence of the pH value, temperature and foaming agentconcentration on the flotation efficiency has been investigated. The investigations

presented show that the disturbing components can be removed from TMP presswater to a high extent. A 90% decrease in turbidity and a 91% removal of lipophilicextractives (i.e. resin and fatty acids, triglycerides, sterols and steryl esters) fromunbleached and bleached TMP process water can be obtained by addition of acationic surfactant as foaming agent during flotation. Lower amount of foamingagent is needed to purify efficiently bleached TMP process water, than unbleached.Additionally, fibres located in TMP press water are not removed with the foamfraction but purified. A retained concentration of hydrophilic extractives (i.e.hemicelluloses and lignans) in the process water indicates that the flotation isselective. Moreover, by introduction of a new recoverable surface activecomplexing agent, a chelating surfactant, manganese ions in the form of chelatescan be successfully removed from the pulp fibres and separated from the processwater in the same flotation process. Furthermore, from the purified unbleachedTMP process water a 90% recovery of dissolved hemicelluloses by anti‐solventprecipitation was obtained.The findings presented above indicate new possibilities for the internal watercleaning stage to decrease DSC emissions to recipient and for recovery of valuableraw materials from purified process water if flotation technology is applied in anintegrated mechanical pulp mill.

Place, publisher, year, edition, pages
Sundsvall: Mid Sweden University, 2014. p. 178
Series
Mid Sweden University doctoral thesis, ISSN 1652-893X ; 184
Keywords
flotation, foaming agents, chelating surfactant, TMP process water, pitch control, internal cleaning stage, hemicellulose recovery, anti‐solvents, solvents, precipitation
National Category
Polymer Chemistry
Identifiers
urn:nbn:se:miun:diva-22244 (URN)978-91-87557-45-3 (ISBN)
Public defence
2014-05-28, O102, Holmgatan 10, Sundsvall, 12:33 (English)
Opponent
Supervisors
Projects
FORE
Funder
Knowledge Foundation, 2180
Available from: 2014-06-27 Created: 2014-06-23 Last updated: 2015-03-13Bibliographically approved
Zasadowski, D., Norgren, M. & Edlund, H. (2013). Recovery of water-soluble hemicelluloses from TMP process water after selective flotation.. In: The 17th International Symposiumon on Wood, Fiber and Pulping Chemistry: . Paper presented at The 17th International Symposiumon on Wood, Fiber and Pulping Chemistry.
Open this publication in new window or tab >>Recovery of water-soluble hemicelluloses from TMP process water after selective flotation.
2013 (English)In: The 17th International Symposiumon on Wood, Fiber and Pulping Chemistry, 2013Conference paper, Oral presentation with published abstract (Refereed)
National Category
Chemical Engineering
Identifiers
urn:nbn:se:miun:diva-20746 (URN)
Conference
The 17th International Symposiumon on Wood, Fiber and Pulping Chemistry
Available from: 2013-12-17 Created: 2013-12-17 Last updated: 2014-06-27Bibliographically approved
Zasadowski, D., Norgren, M., Hedenström, E., Willför, S., Strand, A. & Sundberg, A. (2013). Selective froth flotation of pitch components from spruce TMP process water.. In: The 17th International Symposiumon on Wood, Fiber and Pulping Chemistry: . Paper presented at The 17th International Symposiumon on Wood, Fiber and Pulping Chemistry.
Open this publication in new window or tab >>Selective froth flotation of pitch components from spruce TMP process water.
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2013 (English)In: The 17th International Symposiumon on Wood, Fiber and Pulping Chemistry, 2013Conference paper, Oral presentation with published abstract (Refereed)
National Category
Chemical Engineering
Identifiers
urn:nbn:se:miun:diva-20747 (URN)
Conference
The 17th International Symposiumon on Wood, Fiber and Pulping Chemistry
Available from: 2013-12-17 Created: 2013-12-17 Last updated: 2016-09-29Bibliographically approved
Högberg, I., Zasadowski, D., Karlsson, A., Wikman, B., Andersson, F., Hedenström, E., . . . Norgren, M. (2012). Brightness development of a hydrogen peroxide bleached spruce TMP. Comparisons of pre-treatments with DTPA and a separable chelating surfactant. Nordic Pulp & Paper Research Journal, 27(1), 50-55
Open this publication in new window or tab >>Brightness development of a hydrogen peroxide bleached spruce TMP. Comparisons of pre-treatments with DTPA and a separable chelating surfactant
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2012 (English)In: Nordic Pulp & Paper Research Journal, ISSN 0283-2631, E-ISSN 2000-0669, Vol. 27, no 1, p. 50-55Article in journal (Refereed) Published
Abstract [en]

In this investigation a new type of recoverable complexing agent (chelating surfactant) has been compared with a conventional complexing agent; diethylenetriamine pentaacetic acid (DTPA), in the metal ion sequestering of thermomechanical pulps (TMP) to be hydrogen peroxide bleached. After different degrees of washing of the pulps, bleaching experiments at different total alkali charges were performed with and without sodium silicate additions, and the ISO brightness of hand-made sheets was measured. The residual hydrogen peroxide in the bleaching liquor was also determined. No significant difference in either the brightness development or the residual hydrogen peroxide content could be detected between the pulps treated with equivalent molar ratios of the different complexing agents. Furthermore, the recovery of the chelating surfactant-manganese complexes from laboratory made white water by froth flotation was also studied. Two different foaming agents; sodium dodecyl sulphonate (SDS) and dimethyldodecylamine oxide (DDAO), were tested in the froth generation. After an addition of 160 ppm of DDAO, more than 80% of the manganese chelates could be recovered in the foam, containing 3% of the initial water mass.

Keywords
Chelating surfactant; DTPA; Flotation; Hydrogen peroxide bleaching; Manganese; Thermomechanical pulp
National Category
Chemical Engineering
Identifiers
urn:nbn:se:miun:diva-16093 (URN)10.3183/NPPRJ-2012-27-01-p050-055 (DOI)000311019900006 ()2-s2.0-84860145718 (Scopus ID)
Available from: 2012-04-17 Created: 2012-04-17 Last updated: 2017-12-07Bibliographically approved
Zasadowski, D. (2012). REMOVAL OF LIPOPHILIC EXTRACTIVES AND MANGANESE IONS FROM SPRUCE TMP WATER BY FLOTATION. (Licentiate dissertation). Sundsvall: Mittuniversitet
Open this publication in new window or tab >>REMOVAL OF LIPOPHILIC EXTRACTIVES AND MANGANESE IONS FROM SPRUCE TMP WATER BY FLOTATION
2012 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

Dissolved and Colloidal substances (DisCo) and metals are released from wood during thermomechanical pulp (TMP) production. The mechanical treatment causes that these components have a tendency to accumulate in process waters, as the water circulation systems in integrated paper mills are being closed. Disturbances such as pitch depositions on the paper machine (pitch problems), specks in the paper, decreased wet and dry strength, interference with cationic process chemicals, and impaired sheet brightness and friction properties appear in the presence of DisCo substances. The presence of transition metal ions such as manganese results in higher consumption of bleaching chemicals (hydrogen peroxide) and lowers the optical quality of the final product, and addition of complexing agents, such as EDTA or DTPA, to prevent this is needed. The never ending trends to decrease water consumption and increase process efficiency in pulp and paper production stress that it is very important both to know the effects of wood substances on pulping and papermaking and to be able to remove them in an efficient way.

Carried out investigations presented in this thesis show that the lipophilic extractives can be removed from TMP press water to high extent. A 90% decrease in turbidity and a 91% removal of lipophilic extractives from TMP press water can be obtained by addition of a cationic surfactant as foaming agent during flotation. Additionally, fibres located in TMP press water are not removed with the foam fraction but purified. A retained concentration of hydrophilic extractives in the process water indicates that the flotation is selective. Moreover, by introduction of a new recoverable surface active complexing agent, a chelating surfactant, manganese ions in the form of chelates can be successfully removed from the pulp fibres and separated from the process water in the same flotation process.

iii

The findings presented above indicate new possibilities for internal water cleaning and decreased emissions to water if flotation technology is applied in an integrated mechanical pulp mill.

Place, publisher, year, edition, pages
Sundsvall: Mittuniversitet, 2012. p. 50
Series
Mid Sweden University licentiate thesis, ISSN 1652-8948 ; 74
Keywords
Flotation, Foaming agents, Chelating surfactant, TMP process water, Pitch control, Internal cleaning stage
National Category
Physical Chemistry
Identifiers
urn:nbn:se:miun:diva-16088 (URN)978-91-87103-01-8 (ISBN)
Presentation
2012-03-01, sal O102, Mid Sweden University, Sundsvall, 10:15 (English)
Opponent
Supervisors
Projects
ReGain/FORE
Available from: 2012-04-17 Created: 2012-04-17 Last updated: 2014-06-27Bibliographically approved
Zasadowski, D., Hedenström, E., Edlund, H. & Norgren, M. (2012). Removal of lipophilic extractives and manganese ions from spruce TMP waters in a customized flotation cell. BioResources, 7(2), 2376-2392
Open this publication in new window or tab >>Removal of lipophilic extractives and manganese ions from spruce TMP waters in a customized flotation cell
2012 (English)In: BioResources, ISSN 1930-2126, E-ISSN 1930-2126, Vol. 7, no 2, p. 2376-2392Article in journal (Refereed) Published
Abstract [en]

The influence of a chelating surfactant, different foaming agents, cationic polyelectrolytes, pH value, and temperature on the purification efficiency of process waters from a mechanical pulp mill has been studied by flotation in a 1 L customized unit. Turbidity measurements and gas chromatography (GC) were carried out to determine the removal and characteristics of dissolved and colloidal substances (DisCo). The manganese ion content in the process waters before flotation and the metal chelate removal capacity by flotation were determined by Inductively Coupled Plasma (ICP) and Atomic Absorption Spectrometry (AAS) measurements. It was found that a 99% removal of complex bound manganese ions and a 94% decrease in turbidity of the TMP water produced at the laboratory can be achieved in a single-stage flotation with a chelating surfactant and a foaming agent. Furthermore, a 91% decrease in turbidity, the removal of up to 96% of resin and fatty acids, and 93% of triglycerides from TMP water can be obtained after application of a foaming agent.

Keywords
Chelating surfactant; Extractives; Flotation; Foaming agents; Internal cleaning stage; Purification
National Category
Chemical Engineering
Identifiers
urn:nbn:se:miun:diva-16094 (URN)000306481700077 ()2-s2.0-84863812526 (Scopus ID)
Available from: 2012-04-17 Created: 2012-04-17 Last updated: 2017-12-07Bibliographically approved
Strand, A., Zasadowski, D., Norgren, M., Hedenström, E., Willför, S. & Sundberg, A. (2012). Selective froth flotation of pitch components from spruce TMP process water. Appita journal, 65(4), 337-346
Open this publication in new window or tab >>Selective froth flotation of pitch components from spruce TMP process water
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2012 (English)In: Appita journal, ISSN 1038-6807, Vol. 65, no 4, p. 337-346Article in journal (Refereed) Published
Abstract [en]

Selective removal of dissolved and colloidal pitch components from an unbleached thermomechanical pulp (TMP)

pressate by addition of a cationic foaming agent, dodecyltrimethylammonium chloride (DoTAC), and subsequent froth

flotation was assessed. The experiments were conducted with varying pH, temperature, and concentrations of DoTAC

and calcium. The concentrations of pitch components, lignans, and dissolved polysaccharides were determined

before and after flotation.

All pitch components were removed more efficiently by flotation at pH 5 and 3.5 than by flotation at pH 7.6. Resin

and fatty acids were removed to a higher degree than neutral pitch substances at all the tested pH levels. Most of the

water-soluble uronic acids and galactoglucomannans stayed in the TMP water after flotation.

Froth flotation with DoTAC was an effective way of selectively removing colloidal and dissolved pitch. Removal of pitch,

especially of resin acids, at an early stage should be beneficial to the overall papermaking process.

Keywords
Colloidal pitch, wood resin, mechanical pulp, flotation, anionic trash
National Category
Physical Chemistry
Identifiers
urn:nbn:se:miun:diva-17243 (URN)000309898500026 ()
Projects
Fore
Funder
EU, European Research Council
Available from: 2012-11-02 Created: 2012-10-26 Last updated: 2017-12-07Bibliographically approved
Organisations
Identifiers
ORCID iD: ORCID iD iconorcid.org/0000-0002-0770-2086

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