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- Almlöf Ambjörnsson, Heléne, 1968-
(författare)
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Mercerization and Enzymatic Pretreatment of Cellulose in Dissolving Pulps
- 2013
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- This thesis deals with the preparation of chemically and/or enzymatically modified cellulose. This modification can be either irreversible or reversible. Irreversible modification is used to prepare cellulose derivatives as end products, whereas reversible modification is used to enhance solubility in the preparation of regenerated cellulose.The irreversible modification studied here was the preparation of carboxymethyl cellulose (CMC) using extended mercerization of a spruce dissolving pulp. More specifically the parameters studied were the effect of mercerization at different proportions of cellulose I and II in the dissolving pulp, the concentration of alkali, the temperature and the reaction time. The parameters evaluated were the degree of substitution, the filterability and the amount of gel obtained when the resulting CMC was dissolved in water. Molecular structures of CMC and its gel fractions were analysed by using NIR FT Raman spectroscopy. It was found that the alkali concentration in the mercerization stage had an extensive influence on the subsequent etherification reaction. FT Raman spectra of CMC samples and their gel fractions prepared with low NaOH concentrations (9%) in the mercerization stage indicated an incomplete transformation of cellulose to Na-cellulose before carboxymethylation to CMC. Low average DS values of the CMC, i.e. between 0.42 and 0.50 were obtained. Such CMC dissolved in water resulted in very thick and semi solid gum-like gels, probably due to an uneven distribution of substituents along the cellulose backbone. FT Raman spectra of CMC samples and their gel fractions mercerized at higher alkaline concentration, i.e. 18.25 and 27.5% in the mercerization stage, indicated on the other hand a complete transformation of cellulose to Na-cellulose before carboxymethylation to CMC. Higher average DS values of the CMC, i.e. between 0.88 and 1.05 were therefore obtained. When dissolved in water such CMC caused gel formation especially when prepared from dissolving pulp with a high fraction of cellulose II.The reversible modification studied was the dissolution of cellulose in NaOH/ZnO. Here the effect of enzyme pretreatment was investigated by using two mono-component enzymes; namely xylanase and endoglucanase, used in consecutive stages. It was found that although the crystallinity and the specific surface area of the dissolving pulp sustained minimal change during the enzymatic treatment; the solubility of pulp increased in a NaOH/ZnO solution from 29% for untreated pulp up to 81% for enzymatic pretreated pulp.
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- Almlöf, Heléne, 1968-
(författare)
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Extended Mercerization Prior to Carboxymethyl Cellulose Preparation
- 2010
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Licentiatavhandling (övrigt vetenskapligt/konstnärligt)abstract
- Carboxymethyl cellulose (CMC) is produced commercially in a two-stage process consisting of a mercerization stage, where the pulp is treated with alkali in a water alcohol solution, followed by an etherification stage in which monochloroacetic acid is added to the pulp slurry. In this thesis an extended mercerization stage of a spruce ether pulp was investigated where the parameters studied were the ratio of cellulose I and II, concentration of alkali, temperature and retention time. The influence of the mercerization stage conditions on the etherification stage, were evaluated as the degree of substitution (DS) of the resulting CMC and the filterability of CMC dissolved in water at a concentration of 1%. The DS results suggested that the NaOH concentration in the mercerization stage was the most important of the parameters studied. When the NaOH concentration in the mercerization step was low (9%), a high cellulose II content in the pulp used was found to have no negative impact on the DS of the resulting CMC compared with pulps with only cellulose I. However, when the NaOH concentration was high (27.5%), pulps with high content of cellulose II showed a lower reactivity than those with only cellulose I with respect to the DS of the CMC obtained after a given charge of NaMCA. The results obtained from the filtration ability study of CMC water solutions suggested that both the amount of cellulose II in the original pulp and the temperature had a negative influence on the filtration ability whereas the NaOH concentration in the mercerization stage had a positive influence. The filtration ability was assumed to be influenced highly by the presence of poorly reacted cellulose segments. A retention time between 1-48 h in the mercerization stage had no effect on either the DS or the filtration ability of the CMC. Using NIR FT Raman spectroscopy molecular structures of CMC and its gel fraction were analyzed with respect to the conditions used in the extended mercerization stage. Here it was found that the alkaline concentration had a very strong influence on the following etherification reaction. FT Raman spectra of CMC samples and their gel fractions prepared with low NaOH concentrations (9%) in the mercerization stage indicated an incomplete transformation of cellulose to Na-cellulose before carboxymethylation to CMC. Low average DS values of the CMC, i.e. between 0.42 and 0.50, were yielded. Such CMC dissolved in water caused very thick and semi solid gum-like gels, probably due to an uneven distribution of substituting groups along the cellulose backbone. FT Raman spectra of CMC mercerized with alkaline concentrations at 18.25 and 27.5% in the mercerization stage indicated, however, that all of the cellulose molecules were totally transferred to CMC of high DS, i.e. between 0.88 and 1.05. When dissolved in water such CMC caused gels when they were prepared from ether pulp with a high fraction of cellulose II.
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- Almlöf, Heléne, 1968-, et al.
(författare)
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The influence of extended mercerization on some properties of carboxymethyl cellulose (CMC)
- 2012
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Ingår i: Holzforschung. - 0018-3830 .- 1437-434X. ; 66, s. 21-27
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Tidskriftsartikel (refereegranskat)abstract
- Carboxymethyl cellulose (CMC) is produced commercially in a two stage process consisting of a mercerization stage in which the pulp is treated with alkali in a water alcohol solution and a second etherification stage whereby monochloro-acetic acid is added to the pulp slurry. In this study, the influence of the conditions of an extended mercerization stage was evaluated on the etherification stage concerning the degree of substitution (DS) and the filterability of the resulting CMC. The parameters studied were: (1) the ratio of cellulose I and cellulose II in the original pulp, (2) the concentration of alkali, (3) the temperature and (4) the retention time in the mercerization stage. The DS results indicate that the NaOH concentration in the mercerization stage is the most important among the parameters studied. When the NaOH concentration in the mercerization stage was high (27.5%), cellulose II showed a lower reactivity than cellulose I with respect to the DS obtained in the resulting CMC. The results from the filtration ability of CMC water solutions are interpreted that the amount of cellulose II in the original pulp and the temperature has a negative influence, while the NaOH concentration in the mercerization stage has a positive influence on the filtration ability. Retention time between 1 h–48 h in the mercerization stage had no effect on the DS or the filtration value. The filtration ability was assumed to be highly influenced by the presence of poorly reacted cellulose segments. The CMC samples with the lowest filtration ability at a given DS can be assumed to have the highest degree of unevenly substituted segments.
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- Andersson, Niclas, et al.
(författare)
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A new sensor and a novel control concept for optimized fiber line operation
- 2014
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Ingår i: TAPPI Journal. - : TECH ASSOC PULP PAPER IND INC. - 0734-1415. ; 13:10, s. 39-45
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Tidskriftsartikel (refereegranskat)abstract
- Kraft and sulfite pulp mills use several consecutive process stages for pulp production. However, usually only one key pulp parameter is used for process control and that is the lignin content in the fibers, typically expressed as the kappa number. Even so, to improve process efficiency, more variables need to be monitored. To do that, a new sensor was developed, the dissolved lignin transmitter (DLT), along with a new control concept. The DLT measures the dissolved lignin content in the pulp slurry using a unique principle based on optical measurements. The device can measure the dissolved lignin inline at low consistency and at medium consistency. The sensor has two major applications: 1) improving the efficiency in washing stages and 2) optimizing chemical charges. Results from several mill trials have shown that the contribution from dissolved lignin in the filtrate portion of the pulp is up to 30% of the total bleach load, i.e., fiber and filtrate kappa number combined into the bleach plant. Hence, chemical savings can be achieved taking this component into account compared to only measuring the washed fiber kappa number. Application: The results of this study can help mills understand how to better control the pulping stages, which might lead to significant economic savings and better pollution control.
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