• 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 process for producing microfibrated cellulose The present invention is correlated with a process for treating cellulosic fibers, the process of which comprises fiber pretreatment with an enzyme in a first enzymatic treatment, followed by mechanical fiber pretreatment in a first mechanical treatment, and a second enzymatic treatment followed by a second mechanical treatment of the fibers to form microfibrillated cellulose (mfc). This makes it possible to produce mfc in an improved and energy-efficient way.
    公开号:BR112012000144B1
    申请号:R112012000144-2
    申请日:2010-07-02
    公开日:2019-08-06
    发明作者:Isto Heiskanen；Kaj Backfolk；Marianna Vehviläinen；Taina Kamppuri；Pertti Nousiainen
    申请人:Stora Enso Oyj；
    IPC主号:
    专利说明:

    Field of the Invention
    The present invention relates to a process for producing microfibrillated cellulose by treating cellulosic fibers.
    Background of the Invention
    Cellulosic fibers are multi-component structures made of cellulose polymers, that is, cellulose chains. Lignin, pentosans and other components known in the art may also be present. The cellulose chains in the fibers are fixed together to form elementary fibrils. Several elementary fibrils are linked together to form microfibrils and several microfibrils form aggregates. The bonds between the cellulose chains, elementary fibrils and microfibrils are hydrogen bonds.
    Mycofibrillated cellulose (MFC) (also known as nanocellulose) is a material made of wood cellulose fibers, where the individual microfibrils have been partially or totally detached from each other. MFC is usually very thin (~ 20 nm) and the span is usually between 100 nm to 1 pm.
    MFC can be produced in a number of different ways. It is possible to mechanically treat cellulosic fibers, so that microfibrils are formed. However, this method is very energy-consuming, for example, fiber defibration or refining, and therefore is not normally used.
    The production of nanocellulose or microfibrillated cellulose with the use of bacteria is another option. Contrary to the above, this is a biosynthetic process, which starts from another raw material other than wood fibers. It is also a very expensive and time-consuming process.
    It is also possible to produce microfibrils from cellulose, with the help of different chemicals, which will break or dissolve the fibers. However, it is difficult to control the extent of the fibrils formed, and the fibrils are usually markedly short.
    An example of producing MFC is described in patent document WO 2007/091942. In the method described in this document, MFC is produced with the help of refining, in combination with the addition of an enzyme.
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    A common problem that prevails in procedures according to the state of the art is that process conditions are not favorable for scale production or for large industrial applications, which require high quantities.
    Therefore, there is still a need for an improved process for the production of microfibrillated cellulose.
    Summary of the Invention
    It is an objective of the present invention to provide a process for producing microfibrillated cellulose in an improved way and which is energy efficient.
    Another objective of the present invention is to produce microfibrillated cellulose with high consistency.
    These objectives and other advantages are achieved by the process according to claim 1. By alternating enzymatic treatments with mechanical treatments, as described in claim 1, it becomes possible to produce microfibrillated cellulose (MFC) in a very efficient way of spending energy. In addition, it is possible to increase the consistency of the MFC produced, which provides clear benefits in terms of handling, dosing, drying or delivering the MFC to another user. This is achieved as described in the independent claim and the preferred modalities of the process are defined by the dependent claims.
    The invention relates to a process for treating cellulosic fibers, the process of which involves pretreating the fibers with an enzyme in a first enzymatic treatment, followed by a mechanical pretreatment of the fibers in a first mechanical treatment. Then, the fibers are treated with an enzyme in a second enzymatic treatment, followed by a final mechanical treatment of the fibers in a second mechanical treatment, in order to form the microfibrillated cellulose. In this way, it is possible to produce MFC in an improved and energy efficient way.
    The enzyme activity during the first enzyme treatment can be between 0.01-250 nkat / g, however, the activity of the first enzyme treatment is preferably low, preferably between 0.05-50 nkat / g, and the activity of enzyme during the second enzyme treatment is preferably higher, preferably between 50-300 nkat / g.
    «
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    The first mechanical treatment and the second mechanical treatment are preferably carried out by shredding or refining the fibers. The first mechanical treatment opens the fiber structure before the next treatment with the enzyme. In this way, the second enzyme treatment will be more effective and selective, which also improves the second mechanical treatment and, thus, also the production of microfibrillated cellulose (MFC).
    The fibers are preferably mechanically treated with a consistency between 2-40% by weight, relative to the total weight. Preferably, the fibers are mechanically pretreated in the first mechanical treatment with a high consistency, between 15-40% by weight, in relation to the total weight. It has been shown that the mechanical pretreatment of fibers with high consistency reduces the amount of fines. Then, the fibers are preferably mechanically treated in the second stage of mechanical treatment, with a consistency between 15-40% by weight, relative to the total weight.
    The pH during the first and / or second mechanical treatment is preferably greater than 9. The increase in pH during the mechanical treatment has been shown to decrease the required energy.
    The enzyme used during the first and / or the second enzyme treatment is preferably an enzyme that reacts with hemicellulose, such as, xylanase or mannanase, or an enzyme that reacts with cellulose, such as cellulase. The enzyme used in the process will decompose the cellulosic fibers and increase the accessibility and activity of the fibers, and thus, also, the production of microfibrillated cellulose.
    Cellulosic fibers are preferably Kraft pulp fibers.
    Detailed Description of the Invention
    The invention relates to a process for producing mycofibrillated cellulose in an improved and energy-efficient manner. In addition, it is possible to produce MFC with a high consistency.
    It has been shown that the combination of a first enzymatic treatment followed by a first mechanical treatment and a second enzymatic treatment, activates and opens the fiber structure in an improved way. In addition, it has been shown that a second mechanical treatment of the treated fibers can be done in order to produce the microfibrillated cellulose. Through this process it is possible to produce the
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    MFC in a very controlled and cost-effective way and also to produce MFC with a high consistency.
    It has also been shown that a first enzymatic treatment of cellulosic fibers, followed by a first mechanical treatment, preferably, in a high consistency, can increase the fiber cutting procedure, at the same time that the production of fines is kept low. It is preferable to keep the amount of fines to a minimum after the first mechanical treatment, since the enzymes that will be added in the second enzymatic treatment will first decompose the fines, before decomposing the fibers. Consequently, a low amount of fines increases the efficiency of the second enzyme treatment.
    The first enzyme treatment, as well as the second enzyme treatment, are carried out in order for the enzymes to break down cellulosic fibers and improve the production of MFC. The enzyme will decompose the primary fiber layer and, thus, increase the accessibility of the fibers, being then able to penetrate the fiber structure and be disposed between the fibrils. Through enzymatic treatments it is possible to reduce the duration of mechanical treatments. A mechanical treatment of cellulosic fibers must markedly reduce the strength of the fibers, and it is therefore advantageous to reduce the duration of such treatment as much as possible. By treating the fibers with enzymes before both mechanical treatments, it is possible to avoid any unnecessary decrease in the strength of the fibers, since the duration of the mechanical treatments can be shortened and the mechanical treatments can be done in a smoother way.
    The enzyme used in the first and second enzyme treatments can be any wood-breaking enzyme that breaks down cellulosic fibers. Cellulase is preferably used, but other enzymes, for example, enzymes that break the hemicellulose chain, such as xylanase and mannanase, can also be used. A single enzyme or different enzymes can be used in the two enzyme treatments. Usually, the enzyme is an enzyme preparation that may contain small parts of other enzyme activities, different from the main enzyme of the preparation.
    The enzyme is added to the fibers that are in the form of a sludge, which has a concentration of approximately 4-5%. The enzyme is added
    5/9 under agitation, both at the beginning of the first and / or second treatments, and throughout the reaction time.
    The temperature used for treatments with the enzyme can be between 3085 ° C. However, the temperature depends on the enzyme used and the optimal working temperature for the specific enzyme, as well as other treatment parameters, such as time and pH. If cellulase is used, the temperature during treatment can be approximately 50 ° C.
    The first and second enzyme treatments can last from 30 minutes to 5 hours. The time required depends on the cellulosic fibers that are treated and the activity of the enzyme, as well as the temperature of the treatment.
    Enzymatic treatments can be terminated by raising the temperature or pH in order to denature the enzymes. The pH during treatment with the enzyme is preferably between 4-6.
    The enzyme activity during the first treatment can be between 0.01-250 nkat / g, preferably between 0.05-50 nkat / g. The purpose of the first enzyme treatment is only to weaken or decompose the upper surface of the fibers. Consequently, the activity of the enzyme is preferably low, so that the fibers are not overly decomposed. The enzyme activity during the second enzyme treatment is preferably between 50-300 nkat / g. The second enzymatic treatment is done in order to decompose the primary layer of the fibers, as previously discussed, that is, not just the upper surface. Consequently, the activity of the enzyme during the second enzyme treatment needs to be greater than during the first enzyme treatment.
    After the first enzymatic treatment, the cellulosic fibers are mechanically pretreated in a first mechanical treatment. The fibers are preferably defibrated or refined in order to increase their specific surface area, thereby facilitating and improving the effect of the second enzymatic treatment. Defibration or refining can be done at a consistency between 240% by weight, relative to the total weight. However, a high consistency, preferably between 15-40% by weight, or between 10-20% by weight, with respect to the total weight, is normally preferred. A low consistency, for example, between 2-6% by weight, with respect to the total weight, or a medium consistency, for example, 10-20% by weight, with respect to the total weight, can also be used.
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    The fines after the first mechanical treatment can be separated, for example, by fractioning the treated fibers, the longer fibers can still be treated in the second enzymatic and mechanical treatments.
    The first mechanical treatment is preferably carried out at a consistency between 15-40% by weight, with respect to the total weight. It has been shown that the treatment of cellulosic fibers with a first enzymatic treatment, with a relatively low enzymatic activity, followed by a mechanical treatment under high consistency, can increase the yield of the fiber cutting procedure, that is, fibers with a reduced extension are produced , while the amount of fines is kept to a minimum, compared to other mechanical treatments. If a large amount of fines is present during an enzyme treatment, the enzymes will first break down these fines and not the fibers, which are the target of the enzyme treatment. Consequently, the first enzymatic and mechanical treatments will increase the efficiency of the second enzyme treatment, consequently, also the efficiency of the second mechanical treatment, as well as the production of MFC. In addition, by reducing the length of the fiber, the processability during mechanical treatments under high consistency increases. In view of the possibility of increasing consistency during mechanical treatments, less fines will be produced and internal fibrillation, which makes the fiber surface more open for enzyme penetration, is then improved.
    Other mechanical pretreatments, in addition to refining and defibration, such as beating, steam blast, defibrillation, homogenization, ultrasonic treatment, dry cutting or other known mechanical treatments of fibers, to soften and make the fibers more active and reactive before treatments The following can also be used.
    After the first mechanical treatment, an enzyme is again added to the fibers, which are in the form of a sludge, which has a concentration of approximately 4-5%. The enzyme is added under stirring, at the beginning of the second enzyme treatment or during the entire reaction time. The second treatment with the enzyme increases the accessibility and activity of the fibers, in addition to improving the next mechanical treatment to form the MFC.
    Then, the fibers are mechanically treated in a second mechanical treatment in order to form the microfibrillated cellulose. The time and temperature
    7/9 during this treatment vary, depending on the treated fibers, as well as on the previous treatments, these parameters being controlled in order to receive fibers with the desired extension. The second mechanical treatment can be done by means of a refiner, defibrator, beater, friction polisher, high shear fibrillator (such as, Cavitron rotor / stator system), disperser, homogenizer (such as, micro-fluidizer) or other known mechanical fiber treatment apparatus. Normally, the fiber consistency during treatment in a microfluidizer cannot be markedly high. However, the exposure of fibers to high pressure in narrow capillarity under high consistency will also result in a high mechanical impact on the fibers, so that the fibers can be treated with high consistency in a micro-fluidizer, according to the described process in claim 1.
    The fiber consistency during mechanical treatment is preferably between 2-40% by weight, relative to the total weight. It is preferred to have a high consistency during the second mechanical treatment, preferably between 15-40% by weight, with respect to the total weight. The MFC produced will then also have a high consistency, preferably above 15% by weight, with respect to the total weight or, preferably, between 15-40% by weight, with respect to the total weight, or even more preferably, between 15- 25% by weight, relative to the total weight. In this way it is possible to transport the MFC to the place of use in a very concentrated way. If necessary, it is possible to add water or a chemical product, so that the produced MFC is expanded and, thus, it is guaranteed that all microfibrils are separated in the water or chemical. The addition of water during the second mechanical treatment should be avoided, since the MFC will expand and it will be difficult to remove this produced MFC from the refining device, defibrator device or some other mechanical treatment device.
    The pH during the first and / or the second mechanical treatment is preferably greater than 9, more preferably still greater than 10. The increase in pH during the mechanical treatment has been shown to increase the efficiency of the mechanical treatment, thereby decreasing the energy required in the process.
    Also, it is possible to add chemicals that will modify the friction of the fibers with each other or modify the expansion of the fibers during the process, according to claim 1. Friction-reducing chemicals can, for example, be
    8/9 example, carboxymethylcellulose (CMC), starch or different polymers such as polyacrylamide (PAM) or surface active agents. Friction-reducing chemicals can be fillers, such as talc, calcium carbonate, kaolin, titanium dioxide, etc. Chemicals that increase or reduce fiber expansion can be, for example, sodium hydroxide, other pH-modifying chemicals, different salts or charged polymers. These chemicals are preferably added after the second enzymatic treatment, before the second mechanical treatment. However, it is also possible to add chemicals before or during the first mechanical treatment. Another reason for the addition, for example, of polymers, is the fact that fibrils stabilize.
    The cellulosic fibers used in the process according to the invention are preferably Kraft pulp fibers, that is, they have been treated according to the Kraft process. It has been shown that the primary fiber wall in the Kraft pulp normally prevents the fibers from providing fibril formation. Thus, it is necessary to remove the primary wall. The primary fiber wall can be removed by intensifying the pretreatment of the fibers. Thus, an intense refining procedure, preferably a high consistency refining, has been shown to be quite effective. Also, enzymes that react with hemicellulose can be used, alone or in combination with a refining procedure, preferably refining under high consistency. It has been shown that the combination of enzymatic pretreatment, mechanical pretreatment, enzymatic treatment and a mechanical treatment, as described in claim 1, is quite effective when it aims to remove the primary walls of the cellulosic fibers. However, other chemical pulps, mechanical pulps, or chemical-mechanical pulps can also be used, an example being sulfite pulp. The fibers can be bleached or non-bleached. Thin-walled fibers are preferably used.
    Cellulosic fibers can be hardwood or softwood fibers. It has been shown that sulfite pulp and pine Kraft pulp disintegrate into smaller fractions, when treated according to the invention, compared to eucalyptus and birch Kraft pulps. Therefore, it is preferred to treat softwood fibers with the process according to the invention.
    The microfibrillated cellulose produced has very satisfactory binding properties, that is, it provides satisfactory connections with different materials,
    9/9 such as glass, aluminum, paper or wood. Thus, microfibrillated cellulose (MFC) can be used for film production. Another advantage of the MFC produced is that it can be used as a primer agent between different materials, such as, bio-barrier and fiber-based substrate.
    Microfibrillated cellulose (MFC) is also commonly referred to as nanocellulose. Fibers that have been fibrillated and that have microfibrils on the surface and microfibrils that are separated and located in an aqueous phase of a slurry are included in the definition of MFC.
    权利要求:
    Claims (8)
    [1]
    1. Process for treating cellulosic fibers, the process of which is characterized by comprising:
    - pretreat the fibers with an enzyme in a first enzymatic treatment, in which the enzyme during the first enzymatic treatment has an activity of 0.01-250 nkat / g;
    - mechanically pretreating the fibers in a first mechanical treatment;
    - treating the fibers with an enzyme in a second enzyme treatment, where the enzyme during the second enzyme treatment has an activity of 50-300 nkat / g and the enzyme activity in the second enzyme treatment is superior to the first enzyme treatment; and
    - mechanically treat the fibers in a second mechanical treatment, in order to form microfibrillated cellulose.
    [2]
    2. Process according to claim 1, characterized by the fact that the fibers are mechanically treated by means of defibration or refining.
    [3]
    3. Process according to any one of the preceding claims, characterized by the fact that the fibers are treated mechanically, with a consistency between 2-40% by weight, with respect to the total weight.
    [4]
    4. Process according to any one of the preceding claims, characterized by the fact that the fibers are pre-treated mechanically in the first mechanical step, with a consistency between 15-40% by weight, with respect to the total weight.
    [5]
    5. Process according to any one of the preceding claims, characterized by the fact that the fibers are mechanically treated in the second mechanical stage, with a consistency between 15-40% by weight, with respect to the total weight.
    [6]
    6. Process according to any one of the preceding claims, characterized by the fact that the pH is greater than 9 during the first and / or second mechanical stage.
    [7]
    7. Process according to any of the preceding claims, characterized by the fact that the enzyme used during the first and / or second enzymatic treatments is an enzyme that reacts with hemicellulose, such as xylanase or mannanase, or an enzyme that reacts with cellulose, such as cellulase.
    Petition 870190030486, of 03/29/2019, p. 6/7
    2/2
    [8]
    8. Process according to any one of the preceding claims, characterized by the fact that the fibers are Kraft pulp fibers.
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    法律状态:
    2018-04-10| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|
    2019-01-29| B06T| Formal requirements before examination|
    2019-07-02| B09A| Decision: intention to grant|
    2019-08-06| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 02/07/2010, OBSERVADAS AS CONDICOES LEGAIS. (CO) 20 (VINTE) ANOS CONTADOS A PARTIR DE 02/07/2010, OBSERVADAS AS CONDICOES LEGAIS |
    优先权:
    申请号 | 申请日 | 专利标题
    SE0950535-5|2009-07-07|
    SE0950535A|SE533509C2|2009-07-07|2009-07-07|Method for producing microfibrillar cellulose|
    PCT/IB2010/053044|WO2011004301A1|2009-07-07|2010-07-02|Process for producing microfibrillated cellulose|
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