WO2014152960A1 - Cellulose fonctionnalisée permettant d'améliorer l'essorage et l'efficacité énergétique - Google Patents

Cellulose fonctionnalisée permettant d'améliorer l'essorage et l'efficacité énergétique Download PDF

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WO2014152960A1
WO2014152960A1 PCT/US2014/028398 US2014028398W WO2014152960A1 WO 2014152960 A1 WO2014152960 A1 WO 2014152960A1 US 2014028398 W US2014028398 W US 2014028398W WO 2014152960 A1 WO2014152960 A1 WO 2014152960A1
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Prior art keywords
cellulose fibers
functionalized
cellulose
fibers
paper
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English (en)
Inventor
Marko HAKOVIRTA
William Robert Ashurst
Burak AKSOY
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Auburn University
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Auburn University
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Priority to US14/775,158 priority Critical patent/US20160032529A1/en
Publication of WO2014152960A1 publication Critical patent/WO2014152960A1/fr
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Classifications

    • 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/13—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02—Silicon compounds
    • C07F7/08—Compounds having one or more C—Si linkages
    • C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
    • C07F7/1804—Compounds having Si-O-C linkages
    • 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
    • D21H11/20—Chemically or biochemically modified fibres
    • 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
    • D21H17/24—Polysaccharides
    • D21H17/25—Cellulose
    • 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
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/06—Paper forming aids
    • D21H21/10—Retention agents or drainage improvers
    • 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
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/16—Sizing or water-repelling agents

Definitions

  • the invention relates to the functionalization of cellulose fibers by a process to render all or part of their surface to be hydrophobic.
  • the invention includes methods for improving the dewatering and drainage practices involved in a paper making process, improving flow properties in papermaking nano/micro-fibrillated cellulose production processes resulting in improvements in energy expenditures associated with the current process and significantly reduced plugging problems during nano/micro-fibrillated cellulose production.
  • the process of making paper requires a large amount of energy, and nearly 80% of the required energy is consumed by paper drying.
  • the sizeable proportion of energy necessary for paper drying is due to the process of drying by vaporization.
  • the paper manufacturing process is essentially a very large dewatering operation through which network formation and consolidation of fibers occur. The ease with which water is released from furnish during the papermaking process affects both the production rate and energy consumption.
  • the entire dewatering process for sheet formation is a very complex sequence utilizing various physical phenomena.
  • a low-solids cellulose fiber and water suspension (typically ⁇ 1% consistency) is distributed on a permeable fabric belt in the paper machine. This belt can move at a speed of some 2000 meters per minute and the water drains out from the cellulosic fiber mixture by gravity and inertia.
  • a hydrofoil is used on the other side of the fabric opposite to the paper web being formed. This system is used to apply a short term vacuum impulse and to move the fibers to create drainage channels in the fiber web.
  • perforated suction rolls and vacuum flat-boxes can be used to improve dewatering.
  • the paper web has a solids content of about 15-25%.
  • the next step involves a series of press nips where water is forced from the paper sheet into the voids of the continuous felts. After the press section, the solid content of the paper web is about 40-55%.
  • the paper web moves through a series of steam heated rolls in order to vaporize most of the remaining water and eventually the moisture drops to a level of 4-8% which is the equilibrium moisture content of the finished paper product. All of these process steps require a substantial amount of energy and demand very high capital equipment investments and maintenance costs.
  • the cost of removing one unit of moisture in the forming, pressing, and drying sections of the paper making process is related by the ratios 1:5:220, respectively. Therefore, removing as much water as possible during the first two stages of the dewatering process greatly reduces the steam heated dryer load and improves papermaking economics provided that water removal is balanced with achieving desired end use requirements for the product produced such as formation. If water drainage could be improved even slightly, the impact would be considerable from both a financial and environmental perspective.
  • R/D additives such as electrolytes, polymers or micro particle-polymer combinations and are commonly used to improve the first- pass retention of fines and fillers and drainage properties of furnish during the forming process.
  • Highly charged cationic polyelectrolyte polymers are also used to reduce the inter-fiber friction which enhances the rate at which fibers slide past each other in the wet-end by partially covering the surface of the fibers (patch agglomeration) thus aiding drainage.
  • Microparticle systems have also been found to significantly improve the dewatering of the papermaking stock in neutral and alkaline systems as well as high speed paper machines. Enzyme treatment of cellulosic fibers also seem to improve the freeness of the papermaking stock by reducing the hydrodynamic surface area of fibers and by reducing fines content of the papermaking furnish. However, excessive treatment of fibers with enzymes have been found to increase the fines content of furnish, thus reducing the dewatering ability.
  • the present disclosure provides improved methods for functionalizing cellulose fibers that exhibit desirable properties and provide related advantages for improvement in the paper making process and/or the nano/micro-fibrillated cellulose production process.
  • the methods comprising the functionalization of cellulose fibers according to the present disclosure provide several advantages compared to other methods known in the art.
  • First, the methods improve the freeness and dewatering of the paper making process during the paper making process, leading to an increased production rate and reduced energy consumption.
  • Second, the methods improve the suspension flow of the cellulosic fiber composition during the paper making process, leading to a lower amount of cellulosic fiber flocculation during the process.
  • the methods improve the bulk of the resultant paper made during the process.
  • the methods improve the thickness of paper produced from a paper making process utilizing the described methods.
  • the methods result in better wet web strength (runnability), ability to use of slower draining fibers, ability to increase refining without production loss, and reduced press load to maintain bulk.
  • a method of functionalizing cellulose fibers in a paper making process or a nano/micro-fibrillated cellulose production process comprising the steps of:
  • a method of using functionalized cellulose fibers in a paper making process or a nano/micro-fibrillated cellulose production process comprising the steps of:
  • a method of removing water in a paper making process or a nano/micro- fibrillated cellulose production process comprising the steps of:
  • a method of improving drainage in a paper making process or a nano/micro-fibrillated cellulose production process comprising the steps of:
  • the inclusion of the first plurality of cellulose fibers improves drainage in the paper making process or the nano/micro-fibrillated cellulose production process.
  • a method of improving dewatering of a cellulose fiber composition comprising the steps of:
  • a method of preparing a cellulose fiber composition comprising functionalized cellulose fibers, said method comprising the steps of:
  • a method of forming water channels in a cellulose fiber composition comprising the steps of:
  • step (c) results in a cellulose fiber composition comprising between 5% and 95% of functionalized cellulose fibers and between 5% and 95% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising between 10% and 90% of functionalized cellulose fibers and between 10% and 90% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising between 15% and 85% of functionalized cellulose fibers and between 15% and 85% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising between 25% and 75% of functionalized cellulose fibers and between 25% and 75% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising between 35% and 65% of functionalized cellulose fibers and between 35% and 65% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising about 1% of functionalized cellulose fibers and about 99% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising about 5% of functionalized cellulose fibers and about 95% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising about 10% of functionalized cellulose fibers and about 90% of non-functionalized cellulose fibers. 19. The method of any one of the preceding clauses, wherein the combination of step (c) results in a cellulose fiber composition comprising about 15% of functionalized cellulose fibers and about 85% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising about 25% of functionalized cellulose fibers and about 75% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising about 35% of functionalized cellulose fibers and about 65% of non-functionalized cellulose fibers.
  • step (c) results in a cellulose fiber composition comprising about 50% of functionalized cellulose fibers and about 50% of non-functionalized cellulose fibers.
  • the paper is selected from the group consisting of board, paperboard, fiberboard, cardboard, a printing paper grade, tissue paper, towel paper, a sanitary paper grade, a personal care paper grade, a superabsorbent paper grade, or any combination thereof.
  • liquid phase silanization scheme comprises treating the cellulose fibers with an organosilane.
  • liquid phase silanization scheme comprises treating the cellulose fibers with a fluorosilane.
  • liquid phase silanization scheme comprises treating the cellulose fibers with a composition comprises a silane dissolved in a solvent.
  • liquid phase silanization comprises octadecyltrichlorosilane and a hexane.
  • FIGURE 1 shows examples of the physical changes of fibers after valley beater pre-treatment.
  • FIGURE 2 shows Canadian Standard Freeness (CSF) values of bleached hardwood pulp mixtures at varying amounts of functionalized fiber addition. Pre-treatment included Valley beating until CSF value 530 ml.
  • CSF Canadian Standard Freeness
  • FIGURE 3 shows CSF values of bleached softwood pulp mixtures at varying amounts of functionalized fiber addition. Pre-treatment included Valley beating until CSF value 530 ml.
  • FIGURE 4 shows Water Retention Value (WRV) of bleached hardwood pulp mixtures at varying amounts of functionalized fiber addition. Pre-treatment included Valley beating until CSF value 530 ml.
  • WRV Water Retention Value
  • FIGURE 5 shows WRV values of bleached softwood pulp mixtures at varying amounts of functionalized fiber addition. Pre-treatment included Valley beating until CSF value 530 ml.
  • FIGURE 6 shows sedimentation properties of non-functionalized
  • functionalized hardwood fibers (a) non-functionalized hardwood, 1 minute (left 530 ml CSF, right 660 ml CSF), (b) functionalized hardwood, 1 minute (left 530 ml CSF, right 660 ml CSF).
  • FIGURE 7 shows sedimentation properties of non-functionalized and 100% functionalized hardwood fibers: (a) non-functionalized hardwood, 60 minutes (left 530 ml CSF, right 660 ml CSF), (b) 100% functionalized hardwood, 60 minutes (left 530 ml CSF, right 660 ml CSF).
  • FIGURE 8 shows sediment volumes of 100% functionalized ( ⁇ ) and non- functionalized ( ⁇ ) hardwood fibers of 530 ml CSF.
  • FIGURE 9 shows sediment volumes of 100% functionalized ( ⁇ ) and non- functionalized ( ⁇ ) hardwood fibers of 660 ml CSF (not pre-treated).
  • method of functionalizing cellulose fibers in a paper making process or a nano/micro-fibrillated cellulose production process comprises the steps of a) obtaining a first plurality of cellulose fibers; b) functionalizing the first plurality of cellulose fibers by subjecting the cellulose fibers to a process in which all or part of the surface of one or more of the first plurality of cellulose fibers is rendered hydrophobic; c) optionally combining the first plurality of cellulose fibers with a second plurality of cellulose fibers, wherein the second plurality of cellulose fibers comprises non-functionalized cellulose fibers; and d) utilizing the first plurality of cellulose fibers, and optionally the second plurality of cellulose fibers, in the paper making process or the nano/micro-fibrillated cellulose production process.
  • a method of using functionalized cellulose fibers in a paper making process or a nano/micro-fibrillated cellulose production process comprises the steps of a) obtaining a first plurality of cellulose fibers; b) functionalizing the first plurality of cellulose fibers by subjecting the cellulose fibers to a process in which all or part of the surface of one or more of the first plurality of cellulose fibers is rendered hydrophobic; c) optionally combining the first plurality of cellulose fibers with a second plurality of cellulose fibers, wherein the second plurality of cellulose fibers comprises non-functionalized cellulose fibers; and d) using the first plurality of cellulose fibers, and optionally the second plurality of cellulose fibers, in the paper making process or the nano/micro-fibrillated cellulose production process.
  • a method of removing water in a paper making process or a nano/micro-fibrillated cellulose production process comprises the steps of a) obtaining a first plurality of cellulose fibers; b) functionalizing the first plurality of cellulose fibers by subjecting the cellulose fibers to a process in which all or part of the surface of one or more of the first plurality of cellulose fibers is rendered hydrophobic; c) optionally combining the first plurality of cellulose fibers with a second plurality of cellulose fibers, wherein the second plurality of cellulose fibers comprises non- functionalized cellulose fibers; and d) utilizing the first plurality of cellulose fibers, and optionally the second plurality of cellulose fibers, in the paper making process or the nano/micro-fibrillated cellulose production process, wherein the inclusion of the first plurality of cellulose fibers removes water from the paper making process or the nano/micro-fibrillated cellulose production process.
  • a method of improving drainage in a paper making process or a nano/micro-fibrillated cellulose production process comprises the steps of a) obtaining a first plurality of cellulose fibers; b) functionalizing the first plurality of cellulose fibers by subjecting the cellulose fibers to a process in which all or part of the surface of one or more of the first plurality of cellulose fibers is rendered hydrophobic; c) optionally combining the first plurality of cellulose fibers with a second plurality of cellulose fibers, wherein the second plurality of cellulose fibers comprises non- functionalized cellulose fibers; and d) utilizing the first plurality of cellulose fibers, and optionally the second plurality of cellulose fibers, in the paper making process or the nano/micro-fibrillated cellulose production process, wherein the inclusion of the first plurality of cellulose fibers improves drainage in the paper making process or the nano/micro-fibrillated cellulose production process.
  • a method of improving dewatering of a cellulose fiber composition comprises the steps of a) obtaining a first plurality of cellulose fibers; b) functionalizing the first plurality of cellulose fibers by subjecting the cellulose fibers to a process in which all or part of the surface of one or more of the first plurality of cellulose fibers is rendered hydrophobic; and c) combining the first plurality of cellulose fibers with a second plurality of cellulose fibers to form the cellulose fiber composition, wherein the second plurality of cellulose fibers comprises non-functionalized cellulose fibers, wherein the inclusion of the first plurality of cellulose fibers improves dewatering of the cellulose fiber composition.
  • a method of preparing a cellulose fiber composition comprising functionalized cellulose fibers.
  • the method comprises the steps of a) obtaining a first plurality of cellulose fibers; b) functionalizing the first plurality of cellulose fibers by subjecting the cellulose fibers to a process in which all or part of the surface of one or more of the first plurality of cellulose fibers is rendered hydrophobic; and c) combining the first plurality of cellulose fibers with a second plurality of cellulose fibers to form the cellulose fiber composition, wherein the second plurality of cellulose fibers comprises non-functionalized cellulose fibers.
  • a method of forming water channels in a cellulose fiber composition comprises the steps of a) obtaining a first plurality of cellulose fibers; b) functionalizing the first plurality of cellulose fibers by subjecting the cellulose fibers to a process in which all or part of the surface of one or more of the first plurality of cellulose fibers is rendered hydrophobic; and c) combining the first plurality of cellulose fibers with a second plurality of cellulose fibers to form the cellulose fiber composition, wherein the second plurality of cellulose fibers comprises non-functionalized cellulose fibers, wherein the inclusion of the first plurality of cellulose fibers forms water channels in the cellulose fiber composition.
  • the method involves cellulose fibers in a paper making process or a nano/micro-fibrillated cellulose production process.
  • cellulose fibers refers to fibers from a plant or plant-based materials, including natural cellulose fibers, manufactured cellulose fibers, and the like.
  • paper making process refers to the manufacture of paper. The paper making process is well known in the art such as, for example, as described in Holik, Handbook of Paper and Board, Wiley- VCH, Second Edition (2013).
  • the term “nano/micro-fibrillated cellulose production process” is also well known in the art.
  • the term “functionalization” refers to the utilization of any process that renders all or part of the surface of at least one cellulose fiber hydrophobic.
  • hydrophobic has its general definition as known in the art, i.e. the physical property of a molecule that is repelled from, tends not to combine with, or is incapable of dissolving in water.
  • the paper making process results in the formation of paper comprising the first plurality of cellulose fibers and optionally the second plurality of cellulose fibers.
  • a first plurality of cellulose fibers is combined with a second plurality of cellulose fibers.
  • the combination results in a cellulose fiber composition comprising between 5% and 95% of functionalized cellulose fibers and between 5% and 95% of non-functionalized cellulose fibers.
  • the combination results in a cellulose fiber composition comprising between 10% and 90% of functionalized cellulose fibers and between 10% and 90% of non-functionalized cellulose fibers.
  • the combination of results in a cellulose fiber composition comprising between 15% and 85% of functionalized cellulose fibers and between 15% and 85% of non- functionalized cellulose fibers.
  • the combination results in a cellulose fiber composition comprising between 25% and 75% of functionalized cellulose fibers and between 25% and 75% of non-functionalized cellulose fibers. In other embodiments, the combination results in a cellulose fiber composition comprising between 35% and 65% of functionalized cellulose fibers and between 35% and 65% of non-functionalized cellulose fibers.
  • the combination results in a cellulose fiber composition comprising about 1% of functionalized cellulose fibers and about 99% of non-functionalized cellulose fibers. In other embodiments, the combination results in a cellulose fiber composition comprising about 5% of functionalized cellulose fibers and about 95% of non-functionalized cellulose fibers. In yet other embodiments, the combination results in a cellulose fiber composition comprising about 10% of functionalized cellulose fibers and about 90% of non- functionalized cellulose fibers. In some embodiments, the combination results in a cellulose fiber composition comprising about 15% of functionalized cellulose fibers and about 85% of non-functionalized cellulose fibers.
  • the combination results in a cellulose fiber composition comprising about 25% of functionalized cellulose fibers and about 75% of non-functionalized cellulose fibers. In yet other embodiments, the combination results in a cellulose fiber composition comprising about 35% of functionalized cellulose fibers and about 65% of non-functionalized cellulose fibers. In some embodiments, the combination results in a cellulose fiber composition comprising about 50% of functionalized cellulose fibers and about 50% of non-functionalized cellulose fibers.
  • the first plurality of cellulose fibers is pre-treated prior to functionalizing.
  • the second plurality of cellulose fibers is pre-treated.
  • pre-treatment refers to any method that reduces fiber size of the first plurality of cellulose fibers or the second plurality of cellulose fibers.
  • the pre-treatment can be performed according to any procedure or process known in the art.
  • the pre-treatment is a mechanical method that reduces fiber size of the first or second plurality of cellulose fibers.
  • the pre-treatment is an enzymatic method that reduces fiber size of the first or second plurality of cellulose fibers.
  • the pre- treatment is selected from the group consisting of beating, refining, cyrocrushing, grinding, electro spinning, and enzymatic pretreatment.
  • the pre-treatment is beating, for example via a Valley beater.
  • the pre-treatment is refining.
  • the pre-treatment is cyrocrushing.
  • the pre-treatment is grinding.
  • the pre-treatment is electro spinning.
  • the pre-treatment is enzymatic pretreatment.
  • the cellulose fibers comprise hardwood cellulose fibers. In other embodiments, the cellulose fibers comprise softwood cellulose fibers. The terms "hardwood” and “softwood” are well known in the art and are given their understood meanings. In yet other embodiments, the cellulose fibers comprise plant fibers. In some embodiments, the cellulose fibers are bamboo fibers. In other embodiments, the cellulose fibers are kenaf fibers. In yet other embodiments, the cellulose fibers are reed fibers.
  • paper of the paper making process, or the resultant paper made from the paper making process, includes all types of paper that can be made according to the processes known in the art.
  • paper is selected from the group consisting of board, paperboard, fiberboard, cardboard, a printing paper grade, tissue paper, towel paper, a sanitary paper grade, a personal care paper grade, a superabsorbent paper grade, or any combination thereof.
  • the paper is board.
  • the paper is paperboard.
  • the paper is fiberboard.
  • the paper is cardboard.
  • the paper is a printing paper grade.
  • the paper is tissue paper.
  • the paper is towel paper.
  • the paper is a sanitary paper grade. In yet other embodiments, the paper is a personal care paper grade, such as diapers, feminine hygiene products, fluff paper grades, and the like. In some embodiments, the paper is a superabsorbent paper grade.
  • cellulose fibers may be functionalized according to any process that renders all or part of the surface of at least one cellulose fiber hydrophobic.
  • the hydrophobic process is performed according to a process selected from the group consisting of a liquid phase silanization, a gas phase silanization, plasma deposition, and an aqueous phase treatment scheme. Methods of rendering cellulose fibers to be hydrophobic are well known in the art.
  • the hydrophobic process comprises a liquid phase silanization.
  • the hydrophobic process comprises a gas phase
  • the hydrophobic process comprises plasma deposition. In some embodiments, the hydrophobic process comprises an aqueous phase treatment scheme.
  • the liquid phase silanization scheme comprises treating the cellulose fibers with an organosilane.
  • the organosilane is
  • the liquid phase silanization scheme comprises treating the cellulose fibers with a fluorosilane. In yet other aspects, the liquid phase silanization scheme comprises treating the cellulose fibers with a composition comprises a silane dissolved in a solvent. In some embodiments, the solvent is a hexane. In one
  • the liquid phase silanization comprises octadecyltrichlorosilane and a hexane.
  • the paper making process or the nano/micro-fibrillated cellulose production process is associated with improved drainage.
  • the concept of drainage is well known in the art of paper making and nano/micro-fibrillated cellulose production.
  • freeness is standard measure of how quickly water is able to drain from a fiber furnish sample in the paper making process.
  • the drainage is improved compared to a paper making process or a nano/micro-fibrillated cellulose production process without functionalized cellulose fibers.
  • the paper making process or the nano/micro-fibrillated cellulose production process is associated with improved dewatering.
  • the concept of dewatering is well known in the art of paper making and is associated with any means that reduces the water used during the paper making process.
  • the dewatering is improved compared to a paper making process or a nano/micro-fibrillated cellulose production process without functionalized cellulose fibers.
  • the paper making process or the nano/micro-fibrillated cellulose production process is associated with improved freeness.
  • freeness can be measured utilizing the Canadian Standard Freeness (CSF) method.
  • CSF Canadian Standard Freeness
  • the freeness is improved compared to a paper making process or a nano/micro-fibrillated cellulose production process without functionalized cellulose fibers.
  • the paper making process or the nano/micro-fibrillated cellulose production process is associated with improved water retention value.
  • Retention Value is a useful tool in evaluating the performance of pulps relative to dewatering behavior on the paper machine.
  • the WRV method was established to provide standard values of centrifugal force, time of centrifuging, and sample preparation so that results can be compared between investigators at standard values.
  • the WRV test can be used to estimate the maximum amount of water that can be removed from a certain furnish before the wet web leaves the press section of a paper machine. Examples of WRV measurements are described herein.
  • the WRV is improved compared to a paper making process or a nano/micro-fibrillated cellulose production process without functionalized cellulose fibers.
  • the paper making process or the nano/micro-fibrillated cellulose production process is associated with improved suspension flow.
  • the concept of suspension flow is well known in the art of paper making and nano/micro-fibrillated cellulose production, for example characterized by an observation of significantly fewer process problems such as plugging of the microfluidizer channels.
  • the improved suspension flow is characterized by a lower amount of cellulosic fiber flocculation.
  • the term "flocculation" refers to a process of contact and adhesion whereby the particles of a dispersion form larger-size clusters.
  • the suspension flow properties are improved compared to a paper making process or a nano/micro-fibrillated cellulose production process without functionalized cellulose fibers.
  • the nano/micro-fibrillated cellulose production can utilize fiber samples prepared using a microfluidizer. After, the cellulose fiber composition is passed through the channels of the microfluidizer, the system can be evaluated to determine the presence or absence of plugging problems of the chambers of the microfluidizer.
  • the nano/micro-fibrillated cellulose production utilizing the methods of the present disclosure are substantially free of problems that are typically observed in the traditional production of nanofibrillated cellulose (e.g., minimal plugging of the chambers is observed using the methods of the present disclosure).
  • the paper making process or the nano/micro-fibrillated cellulose production process is associated with improved bulk.
  • Paper bulk is well known in the art and is defined as the volume occupied by a given mass of paper (i.e., the inverse of density).
  • the bulk of paper and paperboard is important because it contributes to the paper's thickness, also known as caliper. Increased paper thickness leads to higher rigidity or bending stiffness, an important measure of strength. Higher bulk also allows the papermaker to calender the paper under greater pressure, which is done by passing it through rollers.
  • the bulk is improved compared to a paper making process or a nano/micro-fibrillated cellulose production process without functionalized cellulose fibers.
  • the paper making process produces paper with increased thickness. Increased paper thickness leads to higher rigidity or bending stiffness, an important measure of strength. In various aspects, the thickness is increased compared to paper produced from a paper making process without functionalized cellulose fibers.
  • water channels refers to any channel in the formed cellulose fiber composition through which water may pass, such as a channel in a mat.
  • paper components or additives can be functionalized according to the methods described herein.
  • components such diatoms, diatomaceous earth, other forms of porous nanosilica, and the like could be added to the paper matrix. These component could be functionalized according to the described methods either before or after their addition to the paper.
  • Cellulose fibers can undergo pre-treatment prior to functionalization.
  • bleached hardwood kraft and bleached softwood kraft pulps underwent pre-treatment by beating.
  • the beating pre-treatment was performed by using a laboratory size Valley beater.
  • the fibers were beaten until a pre-determined freeness testing value (530 ml) was reached.
  • beating causes fibers to flatten, shorten and internally and externally fibrillate.
  • cellulose fibers undergo physical changes following pre-treatment.
  • fiber mats were prepared from the beaten pulps by using Buchner funnel and filter paper. They were then allowed to air dry at ambient conditions.
  • Air dried fiber mats comprising cellulose fibers can be subjected to a process in which all or part of the surface of the cellulose fibers is rendered hydrophobic.
  • the cellulose fibers can be treated using a liquid phase silanization scheme.
  • cellulose fibers were treated with octadecyltrichlorosilane (OTS) dissolved in one or more hexanes.
  • OTS octadecyltrichlorosilane
  • the functionalization process that results in the bonding of the OTS molecule to the cellulose surface can involve two reactions: 1) the hydrolysis of OTS with adventitious dissolved water to produce the reactive intermediate (a trisolanol) and 2) the condensation of the trisilanol with surface hydroxyl groups to form a grafted OTS moiety.
  • the batch process begins with the preparation and conditioning of 2 liters of an OTS-hexane solution. This solution is allowed to condition by uptake of ambient humidity for approximately 10 minutes to cause the hydrolysis step of the functionalization mechanism.
  • Cellulose fibers as well as a rigorously cleaned piece of silicon (100) wafer are added to the solution and the mixture is allowed to react for a period of time. Periodically, the silicon (100) wafer piece is removed from the solution and checked for completeness of functionalization by contact angle goniometry. Once the water contact angle on the silicon (100) piece exceeds 105°, the functionalization is deemed to be complete.
  • the functionalized fibers are separated from the spent OTS-hexane solution by Buchner funnel filtration and rinsing with neat hexane. The fibers are dried to bone-dryness in an oven at 77 °C prior to testing. The concentration of OTS in the OTS-hexane solution is determined based on an assumed specific surface area of cellulose fiber (100 m /g) and complete surface coverage by functionalization.
  • this amount was approximately 1.7 mmol OTS per air-dried gram of cellulose fiber to be treated.
  • the amount of cellulose to be treated is weighed, and the appropriate amount of neat OTS is added to the 2 liters of hexane to prepare the OTS-hexane solution.
  • a typical amount of cellulose fibers treated according to this example is 50 grams.
  • Freeness is an industry- standard measure of how quickly water is able to drain from a fiber furnish sample. In many cases, there is a direct correlation between freeness value and either 1) a target level of refining of pulp, or 2) the ease of drainage of white water from the wet web, especially in the early sections of a Fourdrinier former. Freeness of pulp (Canadian standard method) was measured according to T227 OM -09 (Tappi Stadards).
  • CSF Canadian Standard Freeness
  • Figure 2 shows CSF values observed for bleached hardwood pulp mixtures.
  • Figure 3 shows CSF values observed for bleached softwood pulp mixtures.
  • both hardwood and softwood pulps behaved similarly. However, there is a slight CSF difference in the lower functionalized percentage of fibers comparing the pre-treated hardwood and softwood pulps. Before pre-treatment, the softwood fibers were approximately 2.5 mm long and about 70 ⁇ wide and hardwood fibers before pre-treatment were
  • the hydrophobic fibers that have less surface area or less external reach due to fibrillation do appear to create less drainage improving effect in the pulp. Due to the hydrophobic nature surrounding the treated fibers reduction of the inter-fiber friction, additional fiber movement in furnish, and in general reorientation of fibers may be expected. This activity would be anticipated to aid gravity drainage of fiber suspension. Furthermore, this may be indirect evidence that the phenomenology of the drainage improvement is very similar to the highly charged cationic polyelectrolyte polymers that are used in reducing the inter-fiber friction in the wet-end.
  • Water Retention Value is a useful tool in evaluating the performance of pulps relative to dewatering behavior on the paper machine.
  • the WRV method was established to provide standard values of centrifugal force, time of centrifuging, and sample preparation so that results can be compared between investigators at standard values.
  • the WRV test can be used to estimate the maximum amount of water that can be removed from a certain furnish before the wet web leaves the press section of a paper machine.
  • the basic WRV measurement procedure was the following: the wet specimen weight (W5) is obtained by subtracting the weight of the filtering crucible or specimen holder alone (Wl) from the weight of the specimen and holder after centrifuging (W2).
  • the dry specimen weight (W3) is measured by subtracting the weight of the filtering crucible or specimen holder alone (Wl) from the weight of the specimen and holder after drying (W4).
  • W5 wet specimen weight
  • WRV testing was done also using Valley beating as the pre-treatment.
  • the starting CSF values for both hardwood and softwood were about 530 ml. Since the pulp mixtures with no pre-treatment had limited effect on freeness values WRV tests were not performed on the pulp mixtures with no pre-treatment. In both CSF and WRV testing, it was determined that reaching exactly the same CSF value from pre-treatment was difficult and therefore an error of about 2-3% was observed. However, this was not expected to create uncertainties as the overall repeatability relatively to the starting CSF value has been reported to be 3-5% with CSF of 530 ml.
  • WRV is a standardized empirical measure of the capacity of a test pad of fibers to hold and retain water. It is well known that WRV-value increases upon the increase in beating with a Valley beater because it causes flattening of fibers, partial removal of primary wall, and loosening of internal structure. This promotes fiber swelling and renders fibers soft and flexible. The swelling phenomenon occurs concurrently with the development of external fibrils that involves loosening of the fibrils and rising of the finer microfibrils on the surfaces of the fibers which results in a very large increase in surface area on the fibers. As a result, beaten fibers effectively hold water.
  • the WRV value of papermaking furnishes is known to increase with increasing refining and increasing pH. Higher pH values promote fiber swelling and water access to swollen fibers is considerably easier. Also, WRV value tends to decrease when kraft fibers are dried and re- slurried due to increased stiffness of the fibers.
  • Figures 4 and 5 show the correlation of fiber functionalization to WRV for hardwood pulp and softwood pulp, respectively. Furthermore, detailed results are presented in Tables 3 and 4 for hardwood pulp and softwood pulp, respectively. Table 3. WRV values for hardwood cellulose fibers following pre-treatment
  • the effect of water retention in fibrillation due to a loosened fiber structure and external fibrillation due to beating is greatly reduced using the disclosed methods.
  • the effect is up to 39% and reduces down to 29% with only 5% functionalized fibers in the fiber test pads for WRV testing.
  • softwood the effect ranged from 59% down to 52%.
  • test results demonstrate the effect to be related to the external fibrils that are not able to absorb water and are functioning as highly increased effective area for reduced inter-fiber friction and internal sliding movements and reorientation that effectively increases drainage.
  • Sediment volume formation behavior of the functionalized and non- functionalized fibers was investigated according to the following procedure. Three (3) grams of fibers was mixed in 997 ml water and were then disintegrated to individual fibers using disintegrator for 3 minutes. Thereafter, a 100 ml sample was taken from the slurry and poured in to a 100 ml graduated cylinder. Photographs were taken and fiber levels were recorded at specified time intervals.
  • pretreated and functionalized fibers had a faster initial settling rate than that of non-functionalized fibers of 530 ml CSF.
  • the sediment volume of functionalized fibers level off after 10 minutes at about 75 ml and give a significantly open fiber distribution (open space) in water in comparison to non-functionalized fiber.
  • open fiber distribution eases the water flow through the paper mat in the thickening process and fibers more easily sliding past each other, thus delaying the sealing of the mat for water passage.
  • non-pre-treated and non-functionalized fibers had a faster initial settling rate than that of non-functionalized fibers of 660 ml CSF.
  • non-pre-treated and non-functionalized fibers possibly form mat faster than that of pretreated, functionalized fibers reducing water drainage.
  • the sediment volume of functionalized fibers levels off after 5 minutes at about 90 ml and give significantly open fiber distribution in water in comparison to non-functionalized fiber. This observed behavior further increases the water drainage rate.
  • the fiber samples can be prepared for nano/micro-fibrillated cellulose production using a microfluidizer. Briefly, the procedure for microfluidizer application in nanofibrillated cellulose production is as follows. First, 80% pretreated (2 hour PFI refining) and TEMPO oxidized fiber is mixed with 20% functionalized (hydrophobic) fiber. Then, the mixture is passed through the channels of the microfluidizer. Subsequently, the system can be evaluated to determine the presence or absence of plugging problems of the chambers of the microfluidizer.
  • the observed results of the example demonstrate that the microfluidizer is advantageously substantially free of problems for the production of nanofibrillated cellulose (e.g., minimal plugging of the chambers).
  • Paper samples i.e., "handsheets"
  • handsheets Paper samples
  • TAPPI T-205 procedure (i.e., TAPPI Test Method No. T-205, entitled "Forming handsheets for physical tests of pulp”).
  • paper samples contained 100% non-functionalized fibers, 100% functionalized fibers, or a mixture of 5% functionalized fibers and 95% non- functionalized fibers.
  • the calipers (i.e., thickness) of the resultant paper samples can be measured according to the art-recognized TAPPI T 411 procedure (i.e., TAPPI Test Method No. T 411, entitled “Thickness (caliper) of paper, paperboard, and combined board”).
  • the observed thickness (caliper) values of the paper samples created according to a paper making process utilizing methods of the present disclosure are shown in Table 5 (hardwood) and Table 6 (softwood) below.
  • paper samples produced using functionalized hardwood cellulose fibers demonstrate an increased thickness compared to paper samples produced using non-functionalized hardwood cellulose fibers.
  • the thickness values increased with a larger percentage of functionalized cellulose fibers in the composition.
  • paper samples produced using 5% functionalized hardwood cellulose fibers show a 2.26% increase in thickness compared to paper samples produced using non-functionalized hardwood cellulose fibers.
  • paper samples produced using 100% functionalized hardwood cellulose fibers show a 29.0% increase in thickness compared to paper samples produced using non- functionalized hardwood cellulose fibers.
  • paper samples produced using functionalized softwood cellulose fibers demonstrate an increased thickness compared to paper samples produced using non-functionalized hardwood cellulose fibers.
  • paper samples produced using 5% functionalized hardwood cellulose fibers show a 5.83% increase in thickness compared to paper samples produced using non-functionalized hardwood cellulose fibers.
  • the thickness of paper samples can be increased for paper products made from both hardwood and softwood.

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Abstract

La présente invention concerne des procédés d'amélioration de l'essorage dans le processus de fabrication de papier, par incorporation de fibres de cellulose fonctionnalisées dans la composition de papier. De plus, l'invention concerne le moyen pour éliminer des problèmes de processus, principalement des problèmes d'engorgement dans un processus de production de cellulose nano/micro-fibrillée, par incorporation de fibres de cellulose fonctionnalisées dans une composition de fibres de cellulose, et des procédés de fonctionnalisation de fibres de cellulose dans un processus de fabrication de papier. Les procédés selon la présente invention fournissent plusieurs avantages, tels que l'amélioration de l'égouttage et de l'essorage pendant le processus de fabrication de papier, ce qui permet d'obtenir une amélioration de la vitesse de production et une réduction de la consommation d'énergie.
PCT/US2014/028398 2013-03-14 2014-03-14 Cellulose fonctionnalisée permettant d'améliorer l'essorage et l'efficacité énergétique Ceased WO2014152960A1 (fr)

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CZ306274B6 (cs) * 2015-11-05 2016-11-09 Technická univerzita v Liberci Způsob funkcionalizace celulózových vláken nebo textilního útvaru tvořeného alespoň částečně celulózovými vlákny, textilní útvar funkcionalizovaný tímto způsobem, a aktivní krytí pro rány a kožní defekty
WO2016207783A1 (fr) * 2015-06-26 2016-12-29 Stora Enso Oyj Procédé de fabrication pour un film ou un produit comprenant un polymère amphiphile

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US3840489A (en) * 1971-12-23 1974-10-08 American Cyanamid Co Novel vinylamide dry strength resins and paper containing the same hydrophilic-hydrophobic vinylamide polymers and manufacture of paper
US4198267A (en) * 1978-01-03 1980-04-15 Dorset Industrial Chemicals Ltd. Improved pulp sheet formation
EP1400625A2 (fr) * 2002-08-20 2004-03-24 Louis Rousseau Procédé pour le traitement en surface de substrat(s), naturel(s) ou synthétique(s)
US20040123962A1 (en) * 2002-12-31 2004-07-01 Kimberly-Clark Worldwide, Inc. Amino-functionalized pulp fibers
WO2008145519A1 (fr) * 2007-05-25 2008-12-04 Metso Paper, Inc. Procédé et appareil pour sécher une nappe de pâte chimique

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Publication number Priority date Publication date Assignee Title
US2563897A (en) * 1945-07-13 1951-08-14 American Cyanamid Co Sizing cellulosic fibers with cationic melamine resin and hydrophobic material
US3840489A (en) * 1971-12-23 1974-10-08 American Cyanamid Co Novel vinylamide dry strength resins and paper containing the same hydrophilic-hydrophobic vinylamide polymers and manufacture of paper
US4198267A (en) * 1978-01-03 1980-04-15 Dorset Industrial Chemicals Ltd. Improved pulp sheet formation
EP1400625A2 (fr) * 2002-08-20 2004-03-24 Louis Rousseau Procédé pour le traitement en surface de substrat(s), naturel(s) ou synthétique(s)
US20040123962A1 (en) * 2002-12-31 2004-07-01 Kimberly-Clark Worldwide, Inc. Amino-functionalized pulp fibers
WO2008145519A1 (fr) * 2007-05-25 2008-12-04 Metso Paper, Inc. Procédé et appareil pour sécher une nappe de pâte chimique

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016207783A1 (fr) * 2015-06-26 2016-12-29 Stora Enso Oyj Procédé de fabrication pour un film ou un produit comprenant un polymère amphiphile
US10358772B2 (en) 2015-06-26 2019-07-23 Stora Enso Oyj Manufacturing method for a film or product comprising an amphiphilic polymer
CZ306274B6 (cs) * 2015-11-05 2016-11-09 Technická univerzita v Liberci Způsob funkcionalizace celulózových vláken nebo textilního útvaru tvořeného alespoň částečně celulózovými vlákny, textilní útvar funkcionalizovaný tímto způsobem, a aktivní krytí pro rány a kožní defekty

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