EP2531643A1 - Procédé et dispositif de production de cellulose sèche microfibrillée - Google Patents

Procédé et dispositif de production de cellulose sèche microfibrillée

Info

Publication number
EP2531643A1
EP2531643A1 EP11702157A EP11702157A EP2531643A1 EP 2531643 A1 EP2531643 A1 EP 2531643A1 EP 11702157 A EP11702157 A EP 11702157A EP 11702157 A EP11702157 A EP 11702157A EP 2531643 A1 EP2531643 A1 EP 2531643A1
Authority
EP
European Patent Office
Prior art keywords
liquid
carbon dioxide
mfc
cellulose
suspension
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP11702157A
Other languages
German (de)
English (en)
Inventor
Stefan Ole Backa
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Borregaard AS
Original Assignee
Borregaard AS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Borregaard AS filed Critical Borregaard AS
Publication of EP2531643A1 publication Critical patent/EP2531643A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • D21C9/007—Modification of pulp properties by mechanical or physical means
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
    • D21D1/00—Methods of beating or refining; Beaters of the Hollander type
    • D21D1/20—Methods of refining

Definitions

  • the present invention relates to a method and a device for producing dry microfibrillated cellulose in a cost efficient and environmentally friendly way.
  • the dry microfibrillated cellulose produced can be reconstituted without significant loss of important properties, in particular without significant loss of surface area, viscosity and gel-like structure relative to microfibrillated cellulose that has not been dried.
  • Microfibrillated cellulose hereinafter denoted MFC
  • MFC Microfibrillated cellulose
  • MFC is a valuable product derived from cellulose and is commonly manufactured in a process in which cellulose fibres in water are disintegrated to form microfibrils and/or nanofibrils by passage through a geometrical constraint, such as in a homogenizer.
  • the resulting gel-like, cellulose fibril aqueous slurry is used as such, or provided in a desired solvent, or dried.
  • the common methods of drying are oven drying and freeze drying.
  • MFC has unique properties and leads to important commercial products that are utilized in a wide range of industrial applications such as specialty paper manufacturing, composites, additives in the food industry, galenics and formulations in the pharmaceutical industry and in cosmetics applications, among others.
  • the MFC should preferably be provided as a dried gel or as a dry powder.
  • MFC obtained according to US patent 4483743 (Turbak) is preferably used in un-dried form.
  • solvent exchange of aqueous MFC is exemplified in US patent 6703497 (Ladouce), where solvent exchange is a part in the production of surface modified MFC.
  • the solvents used were acetone, methanol and toluene, and the solvent exchanges were repeatedly done in a centrifuge or on a filter. No final drying of the solvent exchanged MFC is mentioned. Oven drying is the most common drying concept both in laboratory and industrial preparation of cellulosic materials.
  • aqueous MFC When aqueous MFC is dried in an oven at e.g. 105°C, the fibrils stick irreversible to each other and form e.g. paper. The fibrils are thereafter difficult to disintegrate and important properties like the high surface area, e.g. as measured according to the BET method (Brunauer-Emmet-Teller method for the determination of the surface area, usually measured as area per weight unit), of the MFC is lost.
  • BET method Brunauer-Emmet-Teller method for the determination of the surface area, usually measured as area per weight unit
  • freeze-drying encompasses the sublimation drying of a deep-frozen composition.
  • the substance is solidified e.g. by freezing in a liquid medium.
  • the liquid such as water
  • the vacuum is adjusted so that the frozen liquid turns directly into vapour in a sublimation process without first passing through the liquid stage. After the sublimation of the liquid, the solid remain, see e.g. US patent 4608764 (Leuenberger).
  • any drying process involving frozen particles be it freeze-drying or otherwise, typically a large amount of (frozen) liquid must be removed effectively.
  • a significant energy input is required to remove said liquid, for example by means of heating (evaporating the liquid) or by means of applying a vacuum (sublimating the liquid). While this may be feasible on a small scale, high costs for freezing and fine vacuum render this process prohibitive for commercial implementation in regard to effectively separating MFC from large amounts of liquid.
  • the dry microfibrillated cellulose produced by the method should be reconstituted without significant loss of properties, in particular without significant loss of surface area and properties derived from that, relative to a microfibrillated cellulose which has never been dried.
  • the present invention provides, in one aspect, a method for producing dry microfibrillated cellulose (MFC) and comprises at least the following steps:
  • the present invention also relates to a device for drying microfibrillated cellulose (MFC), said device at least comprises:
  • the cellulose fibres employed as starting material in the process can be cellulose fibres from cellulose fibre sheets. Such cellulose fibre sheets are readily available from cellulose mills.
  • the cellulose fibre sheets are dried or partially dried cellulose obtained from a cellulose pulp.
  • the fibre sheets are dissolved in a liquid containing a carbon dioxide miscible liquid, e.g. in ethanol.
  • the liquid should consist mainly of the carbon dioxide miscible liquid, however, minor amounts of water (preferably less than 10%) and other products may be acceptable.
  • the fibre sheets may be shredded, and mixing e.g. by stirring of the fibre sheets and the liquid may be performed to facilitate the dissolution of the cellulose sheets. If stirring is performed, employing a mechanical stirring device is preferred. If necessary or desirable, water may be removed from the fibre sheet as explained for the cellulose pulp
  • the cellulose fibres are provided as a cellulose pulp.
  • the cellulose pulp is usually in aqueous solution or dispersion, and can be prepared according to methods known in the art.
  • the cellulose pulp comprises a fibre material of paper, soft-wood and hardwood, fruit or vegetable origin, such as citrus, beets, orange or lemon or tomato, agricultural waste such as bagasse, and the like, or annual plants or energy crops, may be employed in step (i). These types of pulps are known in the art, and any mixture of these may also be used.
  • Sulfite pulp is preferred, preferably that of soft-wood and in particular bleached sulfite pulp.
  • the starting material for the conversion of cellulose to MFC may be any cellulose fibres from a cellulose pulp, preferably a chemical pulp, further preferably bleached, half- bleached and unbleached sulphite, sulphate, soda pulps and Kraft pulps together with unbleached, half-bleached and bleached chemical pulps, and mixtures of these.
  • Said cellulose pulp may be mechanically or chemically or enzymatically pretreated or may not be pretreated at all.
  • a particularly preferred source of cellulose fibre is regular, fibre-length cellulose fibre sheets and cellulose pulp, where the pulp is derived from either hardwood or soft-wood, or both types (in mixtures), normally available from a pulping operation, or pre-cut if desired.
  • said pulp contains pulp from soft-wood.
  • the pulp may also contain soft-wood of one kind only or a mixture of different soft-wood types.
  • said pulp may contain a mixture of pine and spruce or spruce only.
  • the water of the cellulose pulp usually will contain various other materials and chemicals from the pulping process, usually in dissolved form. Water in the context of the present invention means pure water and water comprising various other such materials and chemicals.
  • Liquid carbon dioxide miscible liquids which are feasible for the method according to the present invention should preferably be environmental friendly and non-toxic or having low toxicity, and being available in good supply and reasonably priced.
  • the liquids should also be water-soluble.
  • Preferred liquid carbon dioxide miscible liquids comprise aliphatic alcohols, acetone and amyl acetate, butyl aldehyde and isobutyraldehyde. Lower aliphatic alcohols are particularly preferred, especially methanol, ethanol, propanol and butanol and in particular ethanol. Acetone is also preferred as the liquid carbon dioxide miscible liquid. Mixtures of these liquids are also feasible. It is usually tolerable that the liquid carbon miscible liquid contains minor amounts of other compounds, in particular that it contains water, preferably in amounts of less than 10%.
  • the concentration of the cellulose fibres in the liquid suspension of fibres and the liquid containing the carbon dioxide miscible liquid of step (i) of the process may vary.
  • the concentration of cellulose fibres in the liquid suspension of fibres and the liquid carbon dioxide miscible liquid amounts to a consistency of from approximately 0.5% to
  • cellulose fibre consistency is meant the percentage of the cellulose fibres in the suspension comprising the fibres in the solvent, i.e. the solution or suspension.
  • step (0) may optionally be performed prior to step (i).
  • a major part of the water of the cellulose fibre sheet or the cellulose pulp of the starting material is to be exchanged with the liquid carbon dioxide miscible liquid.
  • the liquid carbon dioxide miscible liquid preferably, at least 80% or at least 90%, further preferably at least 95%.
  • MFC Microfibrillated cellulose
  • cellulose fibres that have been reduced in their size to result in microfibrils and/or nanofibrils.
  • a homogenizing process performed by the passing of a liquid suspension of cellulose fibres through a small-diameter orifice in which the suspension is subjected to high-velocity shearing actions is a useful method for the forming of cellulose micro and nano fibrils of the MFC.
  • MFC is known from the art, for example from US patent 4374702 (Turbak).
  • microfibrillated cellulose has properties distinguishable from celluloses known previously and is produced by passing a liquid suspension of cellulose through a small diameter orifice in which the composition is subjected to a pressure drop of at least 3000 psig and a high velocity shearing action followed by a high velocity decelerating impact. The passage of said composition through said orifice is repeated until the cellulose composition becomes a substantially stable composition. This process converts the cellulose into microfibrillated cellulose (MFC) without substantial chemical change of the cellulose starting material
  • MFC microfibrillated cellulose
  • WO 2007/091942 of STFI-Packforsk AB describes a method for treatment of chemical pulp for the manufacturing of microfibrillated cellulose comprising the following steps: a) providing a hemicellulose containing pulp, b) refining said pulp in at least one step and treating said pulp with one or more wood degrading enzymes at a relatively low enzyme dosage, and c) homogenizing said pulp thus providing said microfibrillated cellulose.
  • MFC microfibrillated cellulose
  • Weibel provides relatively simple and inexpensive means for refining fibrous cellulosic material into a dispersed tertiary level of structure and thereby achieving the desirable properties attendant with such structural change.
  • the cellulosic fibre produced in this way is referred to as "microdenominated cellulose (MDC)", a sub-group of microfibrillated cellulose.
  • Microfibrillated cellulose is therein obtained by repeatedly passing a liquid composition of fibrous cellulose through a zone of high shear, which is defined by two opposed surfaces, with one of the surfaces rotating relative to the other (rotor/stator device), under conditions and for a length of time sufficient to render the composition substantially stable, and to impart to the composition a water retention that shows consistent increase with repeated passage of the cellulose composition through the zone of high shear.
  • a liquid carbon miscible liquid according to the present invention e.g. ethanol or acetone
  • the exchange of the liquid carbon dioxide miscible liquid with liquid carbon dioxide will be facilitated.
  • lubricants may be use during the homogenization procedure.
  • An example of such a lubricant is PEG (polyethylene glycol).
  • the MFC composition is obtained from a homogenizer as a gel or as a high viscosity composition typically having a consistency of less than about 5%
  • the liquid carbon dioxide miscible liquid of the MFC liquid suspension is displaced to the desired degree by liquid carbon dioxide by methods known from the state of art such as exchanging repeatedly the liquid in the MFC suspension with liquid carbon dioxide under pressure.
  • the pressure and the temperature are in the subcritical region. When operating in the carbon dioxide liquid region, the temperature must be beyond the boiling point of carbon dioxide at the employed pressure. In the interest of optimizing the economy of the process, the ratio of the pressure and the temperature should be balanced.
  • the pressure should be relatively low and may vary between approximately 10 and 70 bar, while the temperature should be from minus 55°C to 31 °C. At ambient temperature, a pressure of about 40 bars may be employed.
  • the displacement of the liquid carbon dioxide miscible liquid by liquid carbon dioxide may take place in a number of conceivable ways.
  • the displacement is performed in a container that can be pressurized, preferably a container that can also be exerted to movements during the procedure, e.g. which can be shaken and/or rotated.
  • the movements of the container during the displacement will avoid the formation of big particles.
  • the movements of the container should be adjusted to provide dried MFC particles of the desired size. Usually, particles appearing as a powder are desired.
  • a rotating drum e.g. a washing drum
  • the MFC liquid suspension may be loaded into a perforated container which is placed in the washing drum.
  • the washing drum can be rotated around any axis, e.g. a horizontal axis or a vertical axis, preferably around a substantially horizontal axis.
  • the rotation may be in one direction only or may change direction during time, e.g. in an agitational manner as is usual for commercial available washing drums.
  • Suitable perforated containers may be of almost any form and material and may simply be a washing bag for domestic use.
  • the liquid carbon dioxide miscible liquid together with a fraction of the liquid carbon dioxide is removed to a separator vessel, continuously or batch-wise during the displacement process.
  • the carbon dioxide is decompressed and returned to a gaseous state, preferably for reuse.
  • the liquid carbon dioxide miscible liquid together with any contaminants or other additives or liquids present will remain in the liquid form and are removed from the separator vessel, e.g. through a bottom valve.
  • the liquids may preferably be refined for reuse.
  • the gaseous carbon dioxide is sent through a cooling device, pressurized and returned to the container e.g. the washing drum, optionally via a storage tank.
  • the removed liquid mixture contains increasing amounts of liquid carbon dioxide.
  • the displacement procedure is discontinued.
  • the carbon dioxide is removed, preferably by evaporation.
  • the pressure in the container e.g. the washing drum, is released to allow the carbon dioxide to evaporate in gaseous form. This may simply be done by opening the pressurized container to the atmosphere to decease the pressure to approximately atmospheric pressure. More preferred the pressure is decreased by opening a valve in a pipe leading to a holding container maintaining a lower pressure, e.g. about atmospheric pressure, to allow the carbon dioxide to be collected for reuse as explained above.
  • “dried” and “dry” microfibrillated cellulose (MFC) and “drying” microfibrillated cellulose (MFC) means removing at least some liquid from the MFC liquid suspension produced in step (ii), which is a composition comprising MFC in a liquid, often comprising a fraction of water.
  • the dry MFC as much as 50% by weight relative to the overall weight of the final product may remain as liquid.
  • not more than 20% or more that 10%, further preferably not more than 5% should remain as liquid, wherein liquid in this context mainly comprises water.
  • the MFC is present as an essentially dry powder or solid.
  • the method for producing dry MFC comprises the following steps and features:
  • (0) optionally adjusting the cellulose fibre content of a cellulose pulp to a consistency of from approximately 2% to approximately 10 % by the removal of water;
  • the present invention relates to a device for the drying of
  • MFC microfibrillated cellulose
  • (c) means for exchanging the liquid carbon dioxide miscible liquid of the liquid suspension with liquid carbon dioxide under sub-critical conditions with regard to temperature and pressure;
  • the means (a) may be a container or similar suitable for dissolving fibre sheets in the desired liquid and/or for a solvent exchange, e.g. by adding the liquid carbon dioxide miscible liquid to the cellulose pulp and draining off water and liquid usually in repeated steps.
  • the device may contain means for the removal of water from the pulp.
  • such means may be a wash press or a wash filter or similar equipment as well as similar equipment known from the state of art and used for this purpose in pulp mills.
  • the means (b) for subjecting the liquid suspension to high shear forces may be a
  • means (c) for exchanging liquid carbon dioxide miscible liquid with liquid carbon dioxide may be a moveable container or similar as is also discussed above, in particular a rotating washing drum.
  • Means (d) for the removal of the liquid carbon dioxide mixture from the MFC suspension may simply be a valve for releasing of the pressure to the environment or through a pipe to a holding container as is further described.
  • the liquid carbon dioxide miscible liquid and the liquid and gaseous carbon dioxide are preferably recovered and reused.
  • the device preferably includes means (c'), a holding container, for collecting the liquid carbon dioxide miscible liquid and liquid carbon dioxide which are released during the steps of the process.
  • Means for the collection of the liquid carbon dioxide miscible liquid may be any suitable device such as a tank.
  • the collected liquid can be separated in its different constituents and recirculated as desired.
  • the liquid carbon dioxide released during the process steps together with the liquid carbon dioxide miscible liquid should be collected and decompressed to carbon dioxide gas in a separator maintaining a lower pressure, e.g. about atmospheric pressure, to allow the carbon dioxide to be collected and processed for reuse as carbon dioxide in its liquid state as explained above.
  • the dry MFC produced by the method of the invention is found to have several desired properties which make the MFC particularly useful for the commercial purposes mentioned above, in particular for the use in composites, additives in the food industry, galenics and formulation in the pharmaceutical industry and in cosmetics applications, among others.
  • the surface area of the dried MFC is particularly high, possibly because the surface tension between the different micro and/or nano fibrils is reduced.
  • the dried MFC will also have a low bacteria number, in particular when bactericides such as ethanol are used during the process.
  • the treatment with liquid carbon dioxide under enhanced pressure also has a positive effect to reduce the bacteria load in the dried MFC.
  • none of the additives frequently used in the preparation of dried MFC is needed.
  • the dried MFC obtained by the present method has several highly desired properties sought by the industry.
  • Said dried MFC in particular if present as a powder or a solid, may be reconstituted by means of adding the same or any other liquid or liquid mixture, if necessary while employing shear forces and/or means of mixing.
  • the composition comprising MFC before drying and after reconstitution in at least one liquid, in particular water may have a dynamic viscosity that is 10 times or 100 times or 1000 times higher than the viscosity of water. Said composition may in particular be present as gel.
  • MFC preferably has non-Newtonian flow properties, for example displaying shear thinning and a gel-like consistency. Documents cited above are hereby included by reference. Examples
  • the units of measurement are metric units if not noted otherwise.
  • the resulting MFC slurry (4 I) was put in a net bag and the bag was put into a drum of a C0 2 textile dry cleaning machine.
  • the air was evacuated; the drum pressurized to 40 bars; and liquid carbon dioxide added (100 I).
  • the drum started to rotate and after 10 min., the washing liquid was drained off and a new portion of 100 I of liquid carbon dioxide was added. This was repeated two more times, after which the pressure was released and the net bag with the dry MFC (70 % weight of fibres) was taken out of the washing machine.
  • the fibre/ethanol slurry was mixed with an Ultrathurax mixer until most of the fibers were free- floating.
  • the mixed fibre/ethanol slurry was homogenized twice by passing the slurry through a 200 micron orifice at a pressure of 2000 bar. 10 volume% of the ethanol was drained off the MFC on a filter.
  • the resulting MFC slurry was put in a net bag and the bag was put into a drum of a C0 2 textile dry cleaning machine.
  • the air was evacuated; the drum pressurized to 40 bars; and liquid carbon dioxide added (70 I).
  • the drum started to rotate and after 10 min., the washing liquid was drained off and a new portion of 70 I of liquid carbon dioxide was added. This was repeated six more times, after which the pressure was released and the net bag with the dry MFC was taken out of the washing machine.
  • the dryness of the MFC was 95 % and the surface area (BET) was 20 m 2 /g. This BET value is at the same level as the water diluted reference sample, which was more extensively homogenized by passing through a 100 micron orifice and then freeze dried.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

La présente invention concerne un procédé de séchage de cellulose microfibrillée dans laquelle une suspension liquide de fibres de cellulose et un liquide miscible dans un dioxyde de carbone liquide sont formés et la suspension liquide est defibrillée. Le liquide miscible dans le dioxyde de carbone liquide est remplacé par du dioxyde de carbone liquide sous pression, et le dioxyde de carbone est éliminé par évaporation. L'invention concerne également un dispositif utilisable à cette fin.
EP11702157A 2010-02-04 2011-02-03 Procédé et dispositif de production de cellulose sèche microfibrillée Withdrawn EP2531643A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
NO20100188 2010-02-04
PCT/EP2011/000489 WO2011095335A1 (fr) 2010-02-04 2011-02-03 Procédé et dispositif de production de cellulose sèche microfibrillée

Publications (1)

Publication Number Publication Date
EP2531643A1 true EP2531643A1 (fr) 2012-12-12

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Application Number Title Priority Date Filing Date
EP11702157A Withdrawn EP2531643A1 (fr) 2010-02-04 2011-02-03 Procédé et dispositif de production de cellulose sèche microfibrillée

Country Status (2)

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EP (1) EP2531643A1 (fr)
WO (1) WO2011095335A1 (fr)

Families Citing this family (9)

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Publication number Priority date Publication date Assignee Title
SE538085C2 (sv) 2012-11-09 2016-03-01 Stora Enso Oyj Torknings- och blandningsförfarande för mikrofibrillerad cellulosa
FI126089B (en) 2012-12-20 2016-06-30 Kemira Oyj PROCEDURE FOR PREPARING DRAINED MICROFIBRILLARY CELLULOSA
CA2993900C (fr) 2015-09-25 2021-01-26 Sappi Netherlands Services B.V. Sechage par atomisation de cellulose en presence de co2 supercritique
FI130254B (en) * 2016-02-03 2023-05-11 Kemira Oyj METHOD FOR PREPARATION OF MICROFIBRILLATED CELLULOSE AND PRODUCT
US11821047B2 (en) 2017-02-16 2023-11-21 Apalta Patent OÜ High pressure zone formation for pretreatment
EP3406140A1 (fr) 2017-05-24 2018-11-28 Bayer CropScience AG Composition aqueuse adaptée à la protection de semis ou d'arbres
EP3825375A1 (fr) 2019-11-20 2021-05-26 Covestro Deutschland AG Collage humide des adhésifs de pulvérisation 1k à base de polychloroprène stables au stockage
BR112022012348A2 (pt) 2019-12-22 2022-09-13 Sweetwater Energy Inc Métodos de fazer lignina especializada e produtos de lignina da biomassa
WO2022087431A1 (fr) * 2020-10-25 2022-04-28 Sweetwater Energy, Inc. Procédé de déshydratation de cellulose

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