• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention relates to the preparation of a cellulosic suspension, in particular a premix for the preparation of a cellulose solution in organic solvents such as, for example, aqueous N-methylmorpholine-N-oxide (NMMO) solution.
    公开号:AT512601A1
    申请号:T279/2012
    申请日:2012-03-05
    公开日:2013-09-15
    发明作者:
    申请人:Chemiefaser Lenzing Ag；
    IPC主号:
    专利说明:

    ·· «« ··
    Lenzing AG, PL0526
    Process for the preparation of a cellulosic suspension
    The present invention relates to a process for the preparation of a cellulose solution in organic solvents such as aqueous NMMO solution, wherein a substantially dry cellulosic raw material is mixed in a mash aggregate with the suspending agent to obtain a cellulosic suspension, this cellulose suspension to a cellulose content of 9 - 15% is pressed, and the wet cellulose is fed to a dissolving unit. The invention further relates to a process 10 for producing cellulosic molded bodies.
    State of the art
    The production of cellulosic moldings such as fibers, filaments, films by dissolving cellulosic raw materials and subsequent precipitation has long been known. An example of such a process is the so-called amine oxide process in which a cellulosic feedstock is dissolved in a solvent consisting essentially of an amine oxide, preferably N-methylmorpholine N-oxide (NMMO), and water and then in an aqueous precipitation bath is ausgefälit in the desired shape again. US Pat. No. 4,246,221 describes an amine oxide process for the production of spinnable cellulose solutions, which is used as starting material i.a. a mixture of cellulose in liquid, aqueous N-methylmorpholine N-oxide (NMMO) is used. According to this method, a suspension of crushed cellulose in 25 of the aqueous amine oxide solution is prepared in a batch mixing apparatus and the mixture is heated simultaneously under reduced pressure, water is removed and a first solution is prepared, which after filtration and post-processing in an extruder into a formable solution is transferred. As a mixing device for the preparation of the cellulosic suspension according to Example I, a conventional double arm mixer is used. In this mixer, a suspension with a consistency of about 20 mass% cellulose is produced. FOLLOW-UP | 1
    Lenzing AG, PL0526 «9 9 999 999 9 9 9 9 9IM I 9 9999 999 99
    However, this method described above has the disadvantage that it is discontinuous and industrially difficult to carry out.
    Furthermore, it is recommended in US Pat. No. 4,246,221 to use this and the (solid) amine oxide hydrate in a ground state for the particularly gentle and rapid dissolution of the cellulose. However, this is disadvantageous because the cellulose is damaged by the grinding process when e.g. comes to a local overheating. Furthermore, it is disadvantageous to use as the starting material for the preparation of the cetlulose solution, a solid mixture of crushed cellulose and crushed amine oxide, since it is known from EP-A - 0 10 419 356 that a suspension of cellulose in an aqueous
    Amine oxide can be converted faster, gentler and better into the formable cellulose solution with the help of thin-film technology.
    It is also recommended in US Pat. No. 4,416,698 to grind the cellulose up to a particle size of less than 0.5 mm. According to DD-A-226 573, a NMMO-containing cellulose suspension with a low consistency of not more than 2.5 mass% of cellulose is used for solution preparation. The NMMO concentration in the pure suspension medium should be about 70% by weight. This cellulose suspension is homogenized in a stirred vessel. Subsequently, the pulp density is increased to 12.5 mass% by centrifuging or pressing, dried to a water content of 10-15 mass% (based on NMMO) and in an extruder with degassing zone at temperatures between 75 and 120'C in a clear solution converted. One of the disadvantages of the process according to DD-A-226 573 mentioned above is that, after homogenization, the consistency must be increased from 2.5% by mass to 12.5% by mass before it is possible to start the actual preparation of the solution. This not only requires a very large amount of suspension medium to be circulated, but also a considerable effort to separate off the excess suspension medium again. Although the DD-A - 226 573 mentions the method of pressing, but leaves completely open as this can be practically, in particular on a large scale, performed.
    REPLACED 2
    Lenzing AG, PL0526
    «· *« «I · * ··« «« «· · · ·« «· · · · · · · · · · · · ·« · · · · · · · · ································································· · * · «T« With IM ···
    For example, it is by no means disclosed to the person skilled in the art how a uniform degree of pressing, which is a prerequisite for a constant solution composition, can be achieved.
    Applicant's WO 95/11261 discloses a process according to which (1) pre-shredded oululosic materials are introduced into an aqueous solution of a tertiary amine oxide to produce a first suspension having a dry matter density of at least 10 mass% cellulose, (2) the first suspension is subjected to grinding to obtain a second suspension, and (3) the second suspension is converted to the moldable cellulose solution by applying heat under reduced pressure. The grinding serves to further break down occasionally remaining pulp particles and split them up into individual fibers. As grinding devices conventional high consistency mixers, dispersers and refiners are proposed. From WO 94/28217 a process for the preparation of a premix of comminuted cellulose and aqueous amine oxide is known, from which a moldable cellulose solution can be prepared. The starting material used is pulp in roll form, which is first shredded in a shredder. It is pointed out in WO 94/28217 20 that care should be taken when cutting the pulp that it is compressed as little as possible at the cut edges, as this complicates the subsequent mixing with the aqueous amine oxide solution. For this purpose, a special cutting machine is recommended, in which pulp pieces of a size of 25 typically 15 cm2 maximum are produced. As a by-product of the cutting process, however, considerable amounts of pulp dust are produced. After cutting in the cutting machine, the pre-shredded pulp is further comminuted in a fan with propeller blades and transported by air to a sieve in which the pre-shredded pulp is separated from the air stream. The sieve separates all pulp particles having a particle size of at least 2.54 mm. In the remaining air flow, however, there is still a significant amount of dust with a
    FOLLOW-UP 3 5 Lenzing AG, PL0526 · * ·· ♦ * ♦ * "" * * t # ····························································································································································· 15 15
    Particle size of less than 2.54 mm. In order not to lose this pulp, it is collected in a filtration device and finally reunited with the larger pulp particles. To prepare the suspension, the comminuted cellulose and the amine oxide solution are introduced into a horizontally mounted, cylindrical mixing chamber, which has a rotor with axially spaced stirring elements. The mixture is stirred in the mixing chamber by rotating the rotor at a rate of 40 to 80 revolutions per minute. On the wall of the cylindrical mixing chamber are still preferably provided rapidly rotating refiner blades, with which the pulp particles are crushed. The combined effect of the stirring blades with the rapidly rotating refiner blades finally leads to a homogeneous mixture which has up to about 13% by weight of cellulose, based on the mass of the suspension. However, this known method has the disadvantage that it is technically complicated and tedious to finally produce the homogeneous suspension from the roll pulp. In addition, the previously known process is discontinuous and takes more than 20 minutes per batch alone in mixing time.
    EP 0853642 first states that conventional pulpers or pulpers, as used in various designs in the viscose or paper industry, can not be used satisfactorily for the present task since they are alleged to produce cellulosic pulps having a pulp density of a maximum of only about 11.5%. The same document also states that the high swelling of the pulp in 60-78% aqueous NMMO at the required processing temperature of 60-90 ° C would reduce the flowability of the suspension to such an extent that the pulp pulp / NMMO / Water is no longer sufficient shear or mixing over the entire mix more subject. In Comparative Example 5 there is found when using a conventional pulper, a 74% NMMO solution at 70-80 ° C and gradual addition of leaf pulp without pre-crushing that after about 12 minutes and reaching a consistency of 11.57 stopped had to be there
    FOLLOW-UP 4
    Lenzing AG, PL0526 · ;; , It was no longer possible to increase the consistency because no mixing took place in the peripheral zones and thus no suspension was obtained.
    EP 0853642 instead proposes a process for preparing a homogeneous suspension of cellulose in an aqueous solution of a tertiary amine oxide, wherein pulp is mixed with the aqueous solution of the tertiary amine oxide in a mixing device comprising a container for holding the suspension and a mixing tool , and characterized in that a mixing device is used, whose container rotates during mixing. Thus, it should be possible to prepare a cellulosic suspension which can be passed directly to a dissolving step. The aqueous solution of the tertiary amine oxide used in this process contains the amine oxide, preferably NMMO, between 60 and 82% by weight. The process is conveniently carried out at a temperature between 60 and 90 ° C. This made it possible to produce cellulosic suspensions with a consistency of more than 13% and, in addition, to use a concentrated amine oxide solution containing 78% by weight of NMMO. However, it has also been found that these effects are significant when using a mixer with a non-moving, i. non-rotating container and rotating mixing tool, should not be achievable.
    Finally, WO 2005/113869 A1 describes a method and a device for producing a cellulose solution which is extrudable into endless molded articles, in which a cellulose suspension is first produced in a pulper of cellulose and water, which is then pressed off by a pressing means. After pressing off, the cellulose suspension is supplied as solvent with a tertiary amine oxide, in particular N-methylmorpholine-N-oxide, thus producing a cellulose solution. This method has the disadvantage that a great deal of water is introduced into the cellulose, which subsequently has to be evaporated again during the preparation of the solution with great expenditure of energy.
    task
    FOLLOW-UP 5
    Lenzing AG, PL0526 * 4 M · * · · »·· * ♦» ·· »* ··« * • · * »* · · ··· · * * * * * * * · «« «« »Ml I ·· * ·
    The object of the present invention was to provide an improved process for the preparation of the cellulase mash, which in particular requires the least possible expenditure of energy and is to be carried out with a simple system consisting of as few apparatuses as possible. Likewise, such a procedure should be as safe as possible.
    Description of the invention
    The solution of the above-described object consists in a process for the production of a cellulose solution in organic solvents, which is characterized in that a. Mixing a substantially dry cellulosic raw material in a mash aggregate with a suspending agent to obtain a cellulose suspension having a cellulose content of 4.0-9.0 15% by weight, b. The in step a. pressed cellulosic suspension is pressed to a cellulose content of 9.0 -15.0 wt .-%, c. The in step b. suspension medium-moist cellulose obtained is fed to a dissolving unit. The suspending agent is preferably a so-called ionic solvent. Suitable ionic solvents are known, for example, from WO 03/029329 and WO 06/108861. Another suitable ionic solvent is the abovementioned aqueous NMMO solution, which has been used commercially for many years in the amine oxide-25 process. In a particularly preferred embodiment of the present invention, therefore, the suspending agent is an aqueous NMMO solution. The dissolving power of such aqueous NMMO solution for cellulose depends on the water content. Therefore, in this embodiment, additional dissolution of water occurs in the dissolving unit until
    FOLLOW-UP 6
    Lenzing AG, PL0526; ··· · ··
    • I ί! · · · III III • :::. * ··: · ::: a homogeneous celulose solution is reached. Corresponding dissolution conditions are known to the person skilled in the art.
    In this embodiment, in step a. the suspending agent is a 72 to 80 wt .-% aqueous NMMO solution with which the cellulose at 60 to 85 ° C 5 is mixed and in step b. in step a. obtained
    Cellulose suspension is pressed at 65 to 75 ° C. Minor deviations from these values may be possible on a case by case basis and still comply with the present invention.
    The NMMO concentration in step a. 10 used is preferably 75 to 79 wt .-% NMMO. Important for the success of the process according to the invention is to have in the finished Ceilulosesuspension a NMMO and water content as close as possible to that of the cellulose solution, following the step c. will be produced.
    For a cellulose content in step a. less than 4.0% by weight would require very much suspending agent which would have to be recycled. Thus, all units of this cycle would be very large to dimension and correspondingly expensive. For a cellulose content in step a. more than 9.0% by weight, full mixing with a customary, commercially available mash aggregate would hardly be attainable, and furthermore, with such a composition of the contents of the container, it would not be possible to add the cellulosic raw material without further comminution in the dry state. because the shear effect would not be sufficient due to the high cellulose content.
    In step b. becomes the step a. pressed cellulose suspension to a 25% cellulose content of 9.0 -15.0 wt .-% pressed by the
    Pressing the Celluiosegehalt by at least 1 percentage point, preferably 2 percentage points or more, to be increased. A lesser degree of pressing is not economically viable and would not justify the expense of the additional press. If the cellulosic suspension is pressed to a cellulose content 30 of less than 9.0% by weight, the cellulose solution obtained in the subsequent dissolving step will have only a cellulose content,
    nachgereioht] 7
    Lenzing AG, PL0526. . **. ·· .:: * ·· * ·: ::: »: ·; · ♦ * ··· · · ** too low for common applications. Pressing off the cellulose suspension to a cellulose content of more than 15.0 wt .-% is associated with a too large and therefore usually no more economic effort. The invention also encompasses analogous modifications of the described method using other ionic solvents.
    The mash aggregate is preferably a so-called pulper known from the paper and viscose industry. Its task is to separate the fibers of the cellulosic raw material as much as possible. In particular, a conventional Dickstoffpulper from the paper industry for the inventive method is preferred. However, it must be built so that in any case all wetted parts are temperature controlled. The stirrer, often referred to as a turbine, should for the purposes of the present invention be mounted some distance from the container bottom of the pulper 15 in order to achieve optimum mixing of the entire contents and optimum separation of the cellulose fibers.
    The mashing in step a. can be done either in a continuously operated mash aggregate or batchwise. In the second case, preferably two pulpers are operated alternately. The feeding of the cellulosic raw material to the mash aggregate preferably takes place in sheet or roll form. Preferably, the cellulosic raw material - usually it is wood pulp, more rarely cotton linters - used in sheet form, since pulp is preferably supplied by many manufacturers in leaf shape. If a pulper 25 is used as the mashing aggregate, no complicated single-sheet feeder is necessary, but a simple feeder which simultaneously allocates several sheets is sufficient. The addition in flake form (so-called fluff pulp, which is also commercially available) is possible.
    The feed of the cellulosic raw material into the mash aggregate is particularly preferably carried out without further comminution in the dry state. This is one of the great advantages of this invention over that
    FOLLOW-UP 8
    Lenzing AG, PL0526; ···. ··· * · · · · · · · · · · · · · · · ·
    State of the art, since in this way dust formation, keratinization at the cutting edges and the formation of aggregates is almost completely avoided. The separation of the fibers takes place only by the shearing action in the pulper in the presence of the NMMO solution, which acts immediately as a suspension medium and prevents damage to the individual fibers. Surprisingly, it has also been shown that the quality of the solution improves, presumably by the gentler opening of the sheet, since any mechanical stress on the dry pulp sheet leads to compressions and particles in the spinning mass. This leads to advantageous longer filter-10 and nozzle service lives.
    Pressing off in step a. obtained cellulose suspension is preferably carried out by a belt filter press. This is the most suitable pressing device for the consistency range according to the invention.
    The pressing is preferably carried out between an upper and a lower 15 Siebband. Such belt presses are basically known and - commercially available, for example, from Andritz / Graz. The sieve belts can consist of a conventional fabric generally used for pressing off pulp, for example a single-layer or multi-layer fabric made of plastic or metal filaments. As 20 plastic filaments are for example polyester or polyamide filaments in question.
    The two screen belts are not arranged parallel to one another in such a press, but in such a way that the distance between them decreases from the suspension feed to the discharge of the press cake. In the wedge-shaped space lying between the sieve bands, which is constantly decreasing, the pressing effect is achieved. For the purposes of the present invention, namely the squeezing of a cellulose suspension prior to solution preparation, the screen belt press and its control must be designed so that this "wedge" is adjustable. An adjustment of the wedge 30 may be required, for example, if another cellulosic I NACHGERBCHT1 9
    Lenzing AG, PL0526
    Raw material is used with a changed swelling behavior or when the supplied amount of suspension varies.
    A likewise suitable, special embodiment of a belt press after the Siebbandabschnrtt still an additional roller press 5 on. This roller press plant contains at least one, but preferably two or more press rolls, between which the press cake is further pressed again. Also, this roller press work should be adjustable in order to control the pressing action can. This form of screen belt press is used, inter alia, in the viscose industry as so-called "AC press" 10.
    When designing such a belt filter press it is essential to ensure that the pressed NMMO solution is sucked off at any point by means of vacuum. This would evaporate water out of the NMMO solution and cause NMMO to crystallize inside the press, which would affect their performance.
    After pressing off the cellulosic suspension, cellulose fibers and other residues normally remain on the sieve belt. The sieve belts are therefore preferably cleaned during operation inside the press with aqueous NMMO solution whose composition corresponds to the NMMO solution used in step a 20. This will be the best on the one hand
    Achieved cleaning effect and on the other hand introduced in this process step, no additional water in the pulp, which would then have to be evaporated again. For the method according to the invention, it has proven to be particularly advantageous when the screen press is loaded with 1000-3000 g / m2 of suspension. At lower loads, economic operation is no longer guaranteed; at higher loads, the effect of being pressed on the highly weighed cellulosic suspension is too low.
    The pressing can alternatively be done by a screw press. In this case, the sieve geometry must be designed according to the fiber dimensions and the high pressing pressure required for pressing, but that is
    RETURNED 10
    Lenzing AG, PL0526 • * * 4 • ♦ * * * ♦ ······································································································································································································· 'the skilled person is aware of the present invention , Other possible apparatuses with which excess suspending agent can be separated from the swollen cellulose are, for example, centrifuges and decanters. For the trouble-free implementation of the method according to the invention, all parts of the press which come into contact with the product are preferably to be kept at a temperature of 60-85 ° C., when an aqueous NMMO solution is used as suspending agent. If the process is to be carried out using the belt filter press described above, all parts in contact with the product must be within one encapsulation for a uniform temperature control. The sieve belts must always be kept at the stated temperature over their entire length, even when cleaning. In other words, this means that the wire belt press must be completely enclosed. The temperature of the parts in contact with the product should preferably be equal to 15 or higher than the melting temperature of the step a. be used NMMO solution.
    Between step b. and step c. For example, comminution of the presscake with aggregates known to the person skilled in the art, such as, for example, a defibrator, can take place. This depends on the consistency of the press cake and thus on the type of cellulosic raw material, among other things.
    The in step b. Press liquor obtained can again be used to prepare the suspension in step a. be used. It is preferably returned to the mash aggregate without further purification.
    In a preferred embodiment, between step a. and step b. 25 stored the cellulase mash in a container. For this purpose, a buffer tank is installed between the mash aggregate and the press. This serves primarily as a buffer to compensate for production fluctuations in continuous operation or when switching from one mash tank to another in batch mode. The contents of the buffer tank are mixed by means of a stirrer in order to settle or demix the cellulosic suspension at longer Verweiizeiten
    REPLACED 11
    Lenzing AG, PL0526 • · «« · «« * * * * ** * * * * * * «···« * · «« ·· «* 4« * ♦ 4 • · * »·. It must also be heated to prevent cooling of the contents and thus, for example, the crystallization of NMMO.
    The invention further relates to a process for the preparation of a moldable cellulose solution, which is characterized in that a homogeneous suspension prepared according to the method according to the invention is processed with evaporation of water to form a moldable cellulose solution. The preparation of the cellulose solution is conveniently carried out in a thin-film treatment apparatus. Such a method is described, for example, in EP-A-0 356 419. An embodiment 10 of a thin-film treatment apparatus is, for example, a so-called film extruder, as manufactured by Buss AG (Switzerland). A thin-film treatment apparatus is also described in DE-A 2 011 493. Usually, a mixture of cellulose and aqueous NMMO solution is supplied to the film extruder, which for the purposes of the present invention should be referred to as a cellulose suspension. In the filmtruder itself, some of the water is evaporated from this mixture, with the cellulose going into solution. WO 94/06530, published in 1994, uses the thin-layer technique already known from EP-A-0 356 419 in order to obtain a mixture of cellulose in an aqueous solution of a tertiary amine oxide into a moldable solution.
    The present invention further relates to a process for producing cellulosic molded bodies, which consists in converting a cellulose suspension prepared according to the invention into a moldable cellulose solution, which is subsequently processed in known manner into films, fibers, membranes or other shaped articles.
    The suspension prepared according to the invention may be fed via a dosing device directly or via a suitable buffer container, e.g. in PCT / AT96 / 00059 of the applicant and in WO 94/28217, are fed into the film extruder and processed there for dissolution. The suspension prepared according to the invention can also be converted into the cellulose solution in other devices.
    POSSIBLE REVIEW 12 5 4 Lenzing AG, PL0526 • ♦ • · · · * * · · · > ·· ♦ • · 10 15
    It is clear to the person skilled in the art that mixtures of different pulps for suspension production can also be used in the process according to the invention. Also, excipients and functional additives, such as stabilizers, dispersants, spin aids, reactivity-improving reagents, inorganic or organic incorporation media (barytes, activated carbon, S1O2, CMC, BaS04l flame-retardant substances such as flames, modifiers (polyethylene glycols)) and other polymers, such as. Nylon, or even dyes can be added to the suspension already in the mash aggregate. The admixture of such auxiliaries, depending on the nature of the respective substance and based on the amount of cellulose, up to an amount between 0.1 and about 80% is possible, if the final product is to be a not formed by the action of distortion forces shaped cellulose body. If the end product is to be a shaped cellulose article molded by distortion forces, for example a cellulose fiber, a cellulose filament or a cellulose film, an admixture of such auxiliaries, also depending on the nature of the respective substance and based on the amount of cellulose, up to an amount between 0 , 1 and about 60% possible because the auxiliaries can cause problems when warping. The invention presented here requires, inter alia, a much less complex plant compared to known processes from the prior art with dry grinding of the pulp before suspension production. This advantage is particularly clear when leaf pulp is to be used, because then whole aggregates - such as a sheet splitter o. Ä. - fall away. 25 Since pulps are often offered by the manufacturer either only in sheet form or only in roll form, a more flexible supply of raw materials is possible when using the invention presented here. In addition, the energy consumption is lower than in the combination of a mill with subsequent, pneumatic transport of the ground pulp for mashing. In particular, the safety technology is much simpler than in the prior art, since no dust explosion protection is required. This also significantly reduces the annual maintenance costs. | REPLACED | 13
    Lenzing AG, PL0526 ···· ·· J * J · · · * ·· «« ·· t ·; · · · · · · · · · · · · · · · · · · ·
    Example:
    From a beech pulp having a mean fiber length of 0.61 mm and a water retention capacity (WRV) of 80% and a 78 wt .-% aqueous NMMO solution as a suspending agent in a pulper 5 suspension with 5 wt .-% cellulose was prepared , This suspension was applied to a twin-wire belt press (type TWT from Andritz / Graz). The task was carried out at a temperature of 70 ° C and at a Siebbandbeladung of 2000 g / m2. The wire speed was 10 m / min. Thus, a consistency of 14% by weight of cellulose could be achieved.
    Further tests showed that satisfactory results could not be achieved with a screen belt load of less than 1000 g / m 2 or more than 3000 g / m 2. At 1000 g / m 2, only a consistency of 11% by weight of cellulose was achievable. The layer was too thin for effective 15 squeeze. At 3000 g / m2, only a consistency of 7.5% by weight was
    Cellulose achievable. The layer was too thick for effective squeezing.
    SUBSEQUENT 14
    权利要求:
    Claims (16)
    [1]
    ♦♦ Μ I »•« · I * • φ · · · · · · · Φ • # ♦ tt ······ «· • Μ * · M ♦ · · * * * * ♦ *« f «· ··· · «φ Lenzing AG, PL0526

    Claims: 1. A process for the preparation of a cellulose solution in organic solvents, characterized in that a. a substantially dry cellulosic raw material is mixed in a mash aggregate with a suspending agent to obtain a cellulose suspension having a cellulose content of 4.0-9.0% by weight, b. in step a. pressed cellulose suspension is pressed to a cellulose content of 9.0 to 15.0 wt .-%, c. in step b. suspension medium-moist cellulose obtained is fed to a dissolving unit.
    [2]
    2. The method of claim 1, wherein the mash aggregate is a pulper.
    [3]
    3. The method of claim 1, wherein the pressing is done by a belt press.
    [4]
    4. The method of claim 3, wherein the squeezing takes place between two screen belts.
    [5]
    5. The method according to claim 3, wherein the sieve belts are cleaned with suspending agent whose composition corresponds to the suspending agent used in step a.
    [6]
    6. The method of claim 3, wherein the screen press is loaded with 1000 -3000g / m2 suspension.
    [7]
    7. The method of claim 1, wherein the pressing is carried out by a screw press.
    [8]
    The process of claim 1 wherein the suspending agent is an ionic solvent. FOLLOW-UP 15 Lenzing AG, PL0526 • · • · • • • Ψ ··································································

    [9]
    The method of claim 8, wherein the suspending agent is an aqueous NMMO solution.
    [10]
    10. The method according to claim 9, wherein in step a. the suspending agent is a 72 to 80 wt .-% aqueous NMMO solution with which the cellulose is mixed at 60 to 85 ° C and in step b. in step a. obtained cellulose suspension is pressed at 65 to 75 ° C.
    [11]
    11. The method of claim 9, wherein all product contacting parts of the press are maintained at a temperature of 60-85 ° C.
    [12]
    12. The method of claim 9, wherein the temperature of the product wetted parts equal to or higher than the melting temperature of the in step a. used NMMO solution.
    [13]
    13. The method of claim 1, wherein in step b. The resulting compressed liquor is returned to the preparation of the suspension in step a. 15
    [14]
    14. The method of claim 1, wherein between step a. and step b. the cellulase mash is stored in a container.
    [15]
    15. The method of claim 1, wherein the supply of cellulosic raw material to the mash aggregate in sheet or roll form, preferably in bale shape.
    [16]
    16. The method of claim 1, wherein the feed of the cellulosic raw material into the mash aggregate takes place without prior further comminution. l FOLLOW-UP 16
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    同族专利:
    公开号 | 公开日
    CN104145052A|2014-11-12|
    TW201348539A|2013-12-01|
    WO2013131113A1|2013-09-12|
    TWI639738B|2018-11-01|
    US20150007952A1|2015-01-08|
    US10612191B2|2020-04-07|
    AT512601B1|2014-06-15|
    IN2014DN06855A|2015-05-22|
    CN110003497A|2019-07-12|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    ATA279/2012A|AT512601B1|2012-03-05|2012-03-05|Process for the preparation of a cellulosic suspension|ATA279/2012A| AT512601B1|2012-03-05|2012-03-05|Process for the preparation of a cellulosic suspension|
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    IN6855DEN2014| IN2014DN06855A|2012-03-05|2013-02-15|
    PCT/AT2013/000027| WO2013131113A1|2012-03-05|2013-02-15|Method for producing a cellulose suspension|
    CN201380012471.8A| CN104145052A|2012-03-05|2013-02-15|Method for producing a cellulose suspension|
    US14/382,808| US10612191B2|2012-03-05|2013-02-15|Method for producing a cellulose suspension|
    TW102107274A| TWI639738B|2012-03-05|2013-03-01|Method for preparing a cellulose suspension|
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