US20210002825A1 - Cellulose pulp and shaped lyocell article having a reduced cellulose content - Google Patents

Cellulose pulp and shaped lyocell article having a reduced cellulose content Download PDF

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US20210002825A1
US20210002825A1 US16/978,340 US201916978340A US2021002825A1 US 20210002825 A1 US20210002825 A1 US 20210002825A1 US 201916978340 A US201916978340 A US 201916978340A US 2021002825 A1 US2021002825 A1 US 2021002825A1
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lyocell
content
pulp
hemicellulose
weight
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Verena Silbermann
Martina Opietnik
Gabrielle Schild
Susanne Moderl
Magdalena Korbler
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Lenzing AG
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Lenzing AG
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Assigned to LENZING AKTIENGESELLSCHAFT reassignment LENZING AKTIENGESELLSCHAFT ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: Silbermann, Verena, MODERL, SUSANNE, KORBLER, MAGDALENA, OPIETNIK, Martina, SCHILD, GABRIELE
Publication of US20210002825A1 publication Critical patent/US20210002825A1/en
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/02—Synthetic cellulose fibres
    • D21H13/08—Synthetic cellulose fibres from regenerated cellulose
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
    • D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
    • D01F2/30—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate by the dry spinning process
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001—Modification of pulp properties
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001—Modification of pulp properties
    • D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/02—Synthetic cellulose fibres

Definitions

  • the present invention describes special cellulose compositions which allow the large-scale stable production of a lyocell fiber with a reduced cellulose content, as well as the lyocell fiber produced from it.
  • Lyocell fibers are used in a variety of applications. Purified cellulose is often used as a raw material, with a very small proportion of various end parts made of cellulose.
  • Pulp is obtained from wood consisting only of 40-44% cellulose by weight. Since a high cellulose content of over 95% by weight is generally required in pulp for the production of lyocell moldings, a large proportion of the raw material for material use is lost during cooking and bleaching. There are a number of known ways of reducing the proportion of hemicelluloses in particular, both in pulp production on the way from wood to pulp or to the lyocell end product:
  • WO 98/16682 describes a production process for a cellulose composition suitable for fiber production.
  • a starting mixture which is not considered suitable for fiber production (but only for paper production) is processed in such a way that the hemicellulose content, in particular the xylan content, is reduced.
  • the WO 99/47733 describes Lyocell fibers and the WO 2010/132151 A2 reveals a pulp with a cellulose with a low degree of polymerization.
  • the present invention provides a pulp according to claim 1 , a lyocell product according to claim 9 , and the methods according to claims 16 and 18 .
  • Preferred forms of the invention are indicated in the subclaims and the following detailed description of the invention.
  • the present invention provides the following aspects, as well as the preferred embodiments cited in the subclaims and the description.
  • FIG. 1 shows the correlation of crystallinity and water retention capacity of lyocell fibers of the present invention and of standard lyocell fibers.
  • FIG. 2 shows the ratio of xylan to mannan in sulphite pulp as a function of the H factor when beech wood is used.
  • FIG. 3 shows the ratio of xylan to mannan in sulphite pulp as a function of the H-factor when using spruce wood.
  • hemicelluloses essentially polyoses from the sugar monomers xylose, arabinose, mannose, galactose, glucose and rhamnose
  • lignin lignin
  • Cellulose It is the structural substance of the cell walls in wood and is mainly used for tensile strength. The long molecule chains of glucose units are stored together in so-called fibrils several times in a helical structure. This helical arrangement in the cell wall ensures good bending strength of the tree, e.g. in the event of wind loading or of the wood, e.g. in a roof construction. Cellulose is hydrophilic, but not water-soluble due to its high crystallinity.
  • Lignin binder for the solid bond of cellulose in the form of an amorphous matrix.
  • lignin is mainly responsible for the compressive strength, on the other hand it is less flexible and in contrast to cellulose hydrophobic. It is responsible for the stamina of the tree. Plants that do not store lignin reach only low growth heights. Lignin is biologically relatively stable and biodegradable only slowly.
  • Hemicellulose in the sense of the present invention means components present in wood in the form of short-chain polymers of C5 and/or C6 sugars. In contrast to cellulose, they have side groups and can therefore only form crystals to a much lesser extent. Their basic building blocks are mannose, xylose, glucose, rhamnose and galactose. The side groups preferably consist of arabinose groups, acetyl groups and galactose residues as well as 0-acetyl groups and 4-O-methylglucuronic acid side groups. It is known that mannans prefer to be associated with cellulose, while xylans tend to associate with lignin. The composition of hemicelluloses varies greatly depending on the type of wood used.
  • hemicelluloses includes those in their native structure as well as those which have been altered by their processing and also those which have been adjusted for their intended use by specific chemical modification. Also included are short-chain celluloses and other polyoses with a DP of up to 500.
  • Accessory constituents are organic and inorganic wood components other than lignin, cellulose and hemicellulose, and usually include salts and low molecular organic compounds of up to about 100 atoms, such as tannins, resins, fats and waxes, tannins and humins, terpenes, terpenoids and phenolic compounds, pectins, suberins, polyphenols and polyoses.
  • a reduced cellulose content in the pulp of less than 90% by weight has a hemicelluloses content of at least 7% by weight, the ratio of sugars with five carbon atoms such as xylan to sugars with six carbon atoms such as mannan (hereinafter referred to as C5/C6 ratio) being in the range from 125:1 to 1:3.
  • the cell materials used here which are preferably used in the context of the present invention, show, as already explained, a relatively high content of hemicelluloses with the composition defined here.
  • the preferred pulps used in the context of this invention also show further differences, which are listed below.
  • the cell materials preferably used in the present invention show a rather fluffy view. After grinding (during the production of starting materials for the production of spinning solutions for the Lyocell process), this results in a particle size distribution with a high proportion of larger particles. As a result, the bulk density is much lower compared to standard pulps with a low hemicellulose content. Such a low bulk density requires adaptations with regard to dosing parameters (e.g. dosing using at least two storage tanks) during the production of the spinning solutions.
  • the cell materials preferably used in the present invention show an impregnation behavior towards NMMO, which in comparison with standard cell materials shows that impregnation is more difficult here.
  • the pulp used for the manufacture of lyocell products shows a SCAN viscosity in the range 300 to 440 ml/g, in particular 320 to 420 ml/g, more preferably 320 to 400 ml/g.
  • the SCAN viscosity is determined in accordance with SCAN-CM 15:99 using a cupriethylenediamine solution, a method known to the professional and which can be performed with commercially available devices, such as the Auto PulpIVA PSLRheotek device, available from PSL-Reotek.
  • the SCAN viscosity is an important parameter which influences the processing of pulp during the production of spinning solutions.
  • lyocell process designate a direct dissolution process of wood cellulose pulp or other cellulose based starting materials in a polar solvent (e.g. N-methylmorpholine-n-oxide (NMMO, NMO) or ionic liquids).
  • a polar solvent e.g. N-methylmorpholine-n-oxide (NMMO, NMO) or ionic liquids.
  • the cellulose solution is usually extruded in a so-called dry wet spinning process using a forming tool and the formed solution is obtained e.g. after passing an air gap into a precipitation bath where the formed body is obtained by precipitating the cellulose.
  • the molded body is washed and optionally dried after further treatment steps.
  • a process for the production of lyocell fibers is described in U.S. Pat. No. 4,246,221, WO 93/19230, WO 95/02082 or WO 97/38153.
  • the fiber properties are strongly influenced by the type and composition of the polymers. It is also known that cellulosic fibers produced by the Lyocell process have a very high crystallinity of about 44 to 47%, while fibers from the viscose process have a crystallinity of about 29 to 34%.
  • the crystallinity describes the orientation of the cellulose polymers towards each other and thus, for example, their ability to absorb, swell and store water.
  • the polymer chains in the non-crystalline areas of the lyocell fibers are more ordered than in the viscose fibers. As a result, ordinary lyocell fibers swell less and are less suitable for highly absorbent products than viscose fibers.
  • cellulose with a reduced cellulose content in accordance with the invention unexpectedly enables a completely different type of aggregation of the polymers and thus a different structure of the lyocell fibers.
  • Their crystallinity is significantly lower, typically 40% or less, such as 39% or less, and for example in the range 38% to 30%, such as in the range 37% to 33%.
  • the values for WRV for fibers in accordance with the present invention, isolated or in combination with the other preferred designs described here, preferably in combination with the values for the crystallinity of the fiber described here, are preferably 70% or more, in particular 75% or more, such as 80% or more, e.g. from 70 to 85%.
  • the hemicelluloses still have side groups, since the glucuronic acid side groups of xylans are comparatively stable under the conditions of acid digestion (Sixta H (Ed.) (2006): Handbook of Pulp Vol. 1; Wiley VCH p. 418).
  • the hemicelluloses thus fulfil all the conditions required to disrupt the crystallization of the cellulose and thus form a more disordered structure than standard Lyocell fibers.
  • the expert would expect that with a higher hemicellulose content and reduced cellulose content, useless products, in particular fibers, would result.
  • the hemicelluloses content in combination with the C5/C6 ratio can be used to selectively control product properties.
  • the qualities of the new Lyocell fibers with reduced cellulose content are similar to those of conventional TENCEL® fibers. It becomes clear that the fiber strengths are slightly below those of TENCEL® fibers, measured in the examples as strength and working capacity. At the same time, the cellulose content could be significantly reduced, recorded in the examples as a glucan value. By absorbing other wood components, the crystallinity decreases by up to 21% and the absorbency increases significantly by up to 27%, measured in the examples as crystallinity index and water retention capacity.
  • the crystallinities of the new Lyocell fibers according to the invention lie between those of conventional TENCEL® fibers and nonwovens Lenzing Viscose® fibers; at the same time, the WRV is in the range of Lenzing Viscose®.
  • the WRV thus rises more strongly than it could be explained by the decreasing crystallinity of the fibers.
  • the other components such as in particular hemicelluloses, but also lignin and accessory components from the wood not only provide a significant increase in yield, i.e. improved sustainability, but also a significant improvement in product properties such as water retention capacity.
  • the pulp according to the invention is characterized by a reduced cellulose content, a minimum of hemicelluloses and a certain C5/C6 ratio with respect to the composition of the hemicellulose.
  • the pulp which may also be a mixture of different pulps (as long as the essential conditions are met), is a pulp having a hemicellulose content of from 7 to 50% by weight, preferably from 7 to 30% by weight, more preferably from 15 to 25% by weight, such as from 10 to 20% by weight.
  • the pulp to be used in accordance with the invention is also preferably a pulp containing at least 9% xylan by weight, preferably at least 10% xylan by weight.
  • the proportion of mannan can be chosen, in combination or independently, in a wide range, as long as the ratio defined in the invention is fulfilled. Suitable man contents lie in the range from 0.1 to 10 wt. %, such as from 0.1 to 9 wt. %, and in the form of 0.1 to 6 wt. %, from 0.1 to 4 wt. %, from 5 to 10 wt. %, from 6 to 10 wt. %, etc., from 0.1 to 9 wt. %.
  • the mannan content is in the range from 0.1 to 1 wt. %, preferably in combination with a xylan content of at least 9 wt. %, preferably at least 10 wt. %.
  • the manganese content is higher, preferably in the range of 6% or more by weight.
  • the cellulose content in the pulp is in a range of equal to or less than 90 wt. % to 50 wt. %, preferably in a range of 90 wt. % to 60 wt. %, such as from 85 wt. % to 70 wt. %.
  • the weight ratio of cellulose to hemicellulose may range from 1:1 to 20:1.
  • the proportion of accessory components can be more than 0.05 wt. %, preferably more than 0.2 wt. %, more preferably more than 0.5 wt. %.
  • the effect can be supported that with such proportions of accessory components in the pulp according to the invention, the effect can be supported that the C5/C6 ratio in the produced lyocell products, especially fibers, is stable and the hemicellulose content does not change significantly (i.e. the content in the lyocell product does not decrease or only decreases to a minor extent compared to the pulp).
  • the C5/C6 ratio in accordance with the invention achieves such a high retention capacity that at the same time a proportion of metal compounds, usually present as their oxides and hydroxides, of up to 25% by weight, based on the weight of the lyocell product (e.g. Mg(OH) 2 or Al(OH) 3 for flame retardant purposes) is made possible, which further substantially reduces the cellulose proportion.
  • metal compounds are in particular TiO2, Al2O 3 , MgO, SiO2, CeO2, Mg(OH) 2 , Al(OH) 3 , BN, ZnO and originate partly from the mineral components of the wood or can be added to the cellulose solution as functional additives (flame retardants, matting agents, biocides . . . ).
  • lyocell fibers with a cellulose content reduced to less than 70% can be produced, which not only meet the practical requirements compared with the known lyocell fibers (mechanical strength etc.), but are also even more suitable for some applications due to the new properties resulting from the invention.
  • the relevant studies have shown that fibers in the proposed composition show in particular an increased water retention capacity and rapid biodegradability during composting.
  • the ratio of C5/C6 sugars of non-cellulosic polymers has been shown to be an important factor in adjusting the fiber composition and its resulting properties. By adjusting this ratio, also in combination with the content of hemicelluloses, the desired product properties can be adjusted.
  • the expert knows how to control or adjust the C5/C6 ratio. This can be achieved by mixing various pulps such as softwood pulps with a higher mannan content with hardwood pulps with a higher xylan content. Trials have confirmed another very effective way to adjust the setting.
  • the ratio of C5 to C6 sugars can be controlled by setting specific cooking parameters such as the H factor. This is illustrated in FIGS. 2 and 3 .
  • the H-factor is regarded as an essential parameter for controlling sulphite cooking (Sixta (Vol. 1 2006) p. 432). It summarizes cooking temperature and cooking time as one size.
  • FIG. 2 shows the influence of the H factor in sulfite boiling on the hemicellulose ratio in hardwood using beech as an example.
  • the content of xylan in hardwoods is naturally higher.
  • Xylan is degraded more than Mannan.
  • the ratio C5/C6 decreases.
  • Another way to adjust the pulp composition according to the invention is to add C5 and/or C6 sugars previously obtained in other processes or process steps, such as an alkaline extraction, be it a cold alkaline extraction or an E step or the like.
  • an alkaline extraction be it a cold alkaline extraction or an E step or the like.
  • the addition of hemicelluloses in dissolved form to the spinning mass and the subsequent joint spinning are known (WO2014086883). This allows viscose fibers with a reduced cellulose content to be produced. This is only possible because the viscose process takes place in an aqueous medium and the hemicelluloses are correspondingly alkali-soluble, so the cellulose exanthate and the dissolved hemicelluloses can be mixed together and spun out together.
  • the pulp is dissolved in NMMO or similar solvents in the Lyocell process, which means that no alkaline or aqueous solutions can be added. They would dilute the solvent and reduce solubility or even lead to unwanted precipitation. Hemicelluloses cannot therefore be added in the form of solutions in the production of spinning solutions but must be introduced differently into the process. One possibility is the addition in the pulp production process, so that the mixture can then be dried with the pulp.
  • hemicellulose composition is a crucial point for the technical production of lyocell moldings, in particular fibers.
  • a large-scale use of hemicellulose in the fiber structure is only possible if the proportion of the C5 fraction is correlated with the proportion of the C6 fraction.
  • the ratio of xylan to mannan is preferred between 18:1 to 1:3, preferably 9:1 to 1:2. At the same time such a mixing ratio allows the incorporation of 0.5-5 wt. % lignin (and/or other accessory components) into the fiber structure without impairing the desired properties to an adverse extent.
  • the fibers provided by the invention have common fiber titers, such as 7 dtex or less, for example 2.2 dtex or less, such as 1.3 dtex, or less, or even less, such as 0.9 dtex or less, depending on the desired application.
  • titers of 1.5 to 1.8 dtex are typical, while lower titers such as 1.2 to 1.5 dtex are suitable for textile applications.
  • This invention also includes fibers with even lower titers as well as fibers with significantly higher titers, such as 10 dtex or less, such as 9 dtex or less, or even 7 dtex or less.
  • Suitable lower limits for fiber titers are values of 0.5 dtex or more, such as 0.8 dtex or more, and 1.3 dtex or more in the forms.
  • the upper and lower limits revealed here can be combined and the resulting ranges, such as from 0.5 to 9 dtex, are also included.
  • the earth discovery at hand enables the production of fibers with titers that can be used in the entire spectrum of fiber applications, including textile applications as well as nonwoven applications.
  • the crystallinity index is determined by Raman spectroscopy. This method is calibrated with data from the X-ray wide-angle method (WAX) and was published by Röder et al. (2009) (Roder T, Moosbauer J, Kliba G, Schlader S, Zucker Toor G, and Sixta H (2009): Comparative Characterizations of Man-Made Regenerated Cellulose Fibers. Lenzing Reports Vol. 87, p. 98 ff.).
  • Table 1 shows the results of the adjustment of the C5/C6 ratio, for two wood species, using the example of the variation of the H-factor in magnesium bisulphite digestion.
  • Table 3 summarizes the salaries of the sugar monomers of the starting pulps for the production of Lyocell fibers.
  • Table 4 shows mechanical properties for standard fibers (lyocell and viscose) compared to properties achieved with lyocell fibers produced with invention pulp. The results impressively demonstrate the advantages of this invention.
  • the new, inventive lyocell fibers thus combine the advantageous properties of previously commercially available lyocell and viscose fibers.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Textile Engineering (AREA)
  • Paper (AREA)
  • Artificial Filaments (AREA)
  • Nonwoven Fabrics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Knitting Of Fabric (AREA)
US16/978,340 2018-03-06 2019-03-06 Cellulose pulp and shaped lyocell article having a reduced cellulose content Pending US20210002825A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP18160123.8A EP3536850A1 (de) 2018-03-06 2018-03-06 Zellstoff und lyocellformkörper mit reduziertem cellulosegehalt
EP18160123.8 2018-03-06
PCT/EP2019/055593 WO2019170763A1 (de) 2018-03-06 2019-03-06 Zellstoff und lyocellformkörper mit reduziertem cellulosegehalt

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EP (2) EP3536850A1 (de)
CN (1) CN111788348B (de)
BR (1) BR112020017780A2 (de)
CA (1) CA3092615C (de)
CL (1) CL2020002286A1 (de)
ES (1) ES2968528T3 (de)
FI (1) FI3762537T3 (de)
TW (1) TWI746936B (de)
WO (1) WO2019170763A1 (de)
ZA (1) ZA202006048B (de)

Cited By (1)

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US20200407883A1 (en) * 2018-03-06 2020-12-31 Lenzing Aktiengesellschaft Solvent-spun cellulosic fiber

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CN113109205A (zh) * 2021-03-29 2021-07-13 杭州融凯盛科技有限公司 一种快速检测莱赛尔纤维成型状态方法

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EP3762537B1 (de) 2023-10-25
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RU2020132856A3 (de) 2022-04-12
BR112020017780A2 (pt) 2020-12-22
EP3536850A1 (de) 2019-09-11
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