• 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:
    microfibrillated cellulose production method. the present invention relates to methods of producing microfibrillated cellulose (mfc). according to the invention a fibrous pulp suspension is mechanically fibrillated to a consistency of 12.5%, dewatered to raise the consistency of the fibrillated suspension to at least 12.5%, and then subjected in the dehydrated condition to further fibrillation . alternatively, an initially fibrillated fibrous pulp suspension can be dewatered and fibrillated in the dehydrated condition, after which these dehydration and fibrillation steps are repeated one or more times, so that the pulp consistency is increased at each fibrillation step. the goals of increasing consistency between subsequent fibrillation steps are correlated with energy savings and an increase in elongation in the mfc. the invention further comprises the use of mfc products, for example, as a papermaking supply additive or additive for injection molded plastic composite materials.
    公开号:BR112015016087B1
    申请号:R112015016087-5
    申请日:2013-12-30
    公开日:2021-09-14
    发明作者:Heiskanen Isto；Kastinen Henri；Kauppi Anna；Kankkunen Jukka；Axrup Lars；Cecilia Land Hensdal；Saxell Heidi；Backfolk Kaj
    申请人:Stora Enso Oyj；
    IPC主号:
    专利说明:

    Background of the Invention
    [001] The present invention is related to a method of production of microfibrillated cellulose (MFC). The invention further comprises the use of the MFC obtained by said method. In connection with the invention, the term "microfibrillated cellulose" or "MFC" also covers what is known as nanofibrillated cellulose (NFC).
    [002] Microfibrillated cellulose (MFC) is defined herein as a fibrous material comprising very fine cellulosic fibrils, with a diameter of about 5 to 100 nm, on average of about 20 nm, and having a fibril length of about 20 nm to 200 μm, although typically 100 nm to 100 μm. Nanofibrillated cellulose (NFC) is a specific class of MFC, with fiber dimensions at the lower end of said fibril size range. In isolated MFC, the microfibrils are partially or completely detached from each other. 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. MFC has a very open active surface area, generally in the range of around 1 to 300 m2/g, and is useful for a wide range of final products used, notably, in the papermaking field.
    [003] The methods cited by the state of the art of manufacturing microfibrillated cellulose (MFC) include mechanical disintegration by refining, grinding, pressing and homogenizing, and still refining, for example, through an extruder. These mechanical procedures can be intensified through chemical or chemical-enzymatic treatments, in a preliminary step.
    [004] US Patent 4,341,807 describes the production of MFC by passing a fibrous suspension repeatedly through a small diameter orifice, subjecting the liquid suspension to a pressure drop. The starting suspension contains 0.5 to 10% by weight of cellulose. The product is a homogeneous suspension in gel form of MFC.
    [005] Patent document WO 2007/091942 Al describes a process in which a chemical pulp is first refined, then treated with one or more wood decomposition enzymes, and finally homogenized to produce MFC as a final product. The pulp consistency is thought to be preferably 0.4 to 10%. The advantage of this is to avoid any type of obstruction in the fluidizer or high pressure homogenizer.
    [006] The above two prior art references are correlated with what may be referred to as low consistency (LC) refining through the use of diluted suspensions. The patent document WO 2012/097446 A1 instead describes a NFC manufacturing process by high consistency (HC) multi-pass refining of fibers obtained chemically or mechanically. In reference, (HC) refers to a discharge consistency of more than 20% by weight. The product comprises a population of free filaments and filaments attached to the fiber core from which they were produced. Fiber diameter is reduced from about 8-45 µm of common papermaking fibers to the nanometer scale of less than 100 nm. The advantage is to obtain nanofibrillated cellulose (NFC) with high elongation, that is, the extension of the fibril in relation to its diameter, which produces an improved intrinsic resistance of the product.
    [007] Patent document WO 2012/072874 Al teaches a multi-step NFC production process, in which the cellulose is refined in a first refiner, the product is divided into an acceptance fraction and a rejection fraction, water is removed of the acceptance fraction and finally the acceptance fraction is refined in a second refiner to obtain a gel-like product with a fiber diameter of 2 to 200 nm. In the first refining step, the consistency of the material is below 10%, but it is increased by removing water to about 15%, or even 20%, to intensify the washing of the material. For the second refining, the pulp can be thinned back to a consistency below 10%.
    [008] US Patent 3,382,140 teaches the preparation of high consistency papermaking pulp, in which the pulp obtained from a Kraft pulping process is first dehydrated to obtain a non-flowing or semi-solid mass, which cannot be pumped. The dewatered mass having a consistency of 20 to 30% is then refined, diluted to a conventional papermaking consistency and formed into a tissue paper. There is no mention of MFC production, and the teaching of the direct use of dough as a supply for papermaking does not suggest the presence of MFC, it is only observed as a minimal additive in such a supply.
    [009] In patent document WO 2011/114004, a different approach to fibrillation of lignocellulosic material is described, based on treatment with ionic liquid, that is, molten salt, which preserves the fibers basically intact. Salts comprising an imidazolium-type cation are mentioned as an example of such liquids. The process is said to weaken the bond between the fibrils or tracheids and separate the fibrils or tracheids from the fiber walls. Invention Summary
    [010] A problem that occurs with the conventional low consistency refining, provided by hammer mills or ball mills, is that a large amount of energy is consumed for continuation of fibrillation after the initial phase of the process. Partial hydrolysis of semicrystalline lignocellulose using chemical agents or enzymes could help, but it has the drawbacks of breaking down cellulose fibrils, loss of yield and high costs for enzymatic treatment.
    [011] Instead of refining with hammer or ball mills, a microfluidizer or a homogenizer can be used. However, the fibrillation process requires pretreatment of the pulp suspension and a relatively low concentration in order to operate uniformly and with efficient energy consumption.
    [012] A common drawback of low consistency fibrillations (LC) is that the resulting suspension is diluted and thus expensive to transport to another location, to be used. On the other hand, high consistency fibrillation (HC), as described, for example, in US Patent 3,382,140, has relatively high energy consumption, initial refiner processability is poor, and high fibrillation methods. known consistency (HC) are therefore not economically viable.
    [013] In general, the problems that occur with the existing methods are the limitations of productivity and the difficulty of providing the process in production scale. With respect to refining, an additional problem is fiber shear, resulting in low elongation (fiber extension in relation to fiber diameter), and loss of fiber strength. For scaled production using homogenizer-based fibrillation, a multiple set of fibrillation units would be required, as well as a consistency enhancer, which makes it even more difficult to make the process for scale production.
    [014] The problem to be solved is addressed by providing a method for producing microfibrillated cellulose or lignocellulose, which can be produced in scale and which has reduced overall energy consumption. The objective is also to obtain a microfibrillated cellulose (MFC) having increased consistency, in order to reduce product transport costs, facilitate storage and packaging, as well as provide a high elongation of the product, so that it is useful as a reinforcing additive for papers or cardboards, and various composite materials.
    [015] The solution, according to the invention, is the production of microfibrillated cellulose (MFC) through the steps of: (a) mechanically fibrillating a fibrous pulp suspension with a consistency of less than 12.5%; (b) dehydrating the fibrillated pulp obtained from step (a) to a consistency of at least 12.5%; and (c) subjecting the dehydrated pulp obtained from step (b) to further fibrillation, with a consistency of 12.5 to 20%.
    [016] The main point of the invention can be said to be the gradual fibrillation of the suspension, so that a first fibrillation is carried out in the low consistency range and the next fibrillation in the high consistency range.
    [017] In correlation with the present invention, low consistency (LC) is defined to mean a suspension consistency of less than 12.5% by weight, typically 1 to 10% by weight. In a preferred embodiment, the consistency can be from 2 to 8% by weight, precisely from 3 to 5% by weight. A high consistency (HC) means a suspension consistency of 12.5 to 20% by weight, typically 15 to 20% by weight. An average consistency (MC), as sometimes referred to in the technique segment, can be interpreted as belonging to the (LC) and (HC) categories, according to said dividing line of 12.5% by weight.
    [018] As a useful modification, the invention further comprises the production of microfibrillated cellulose (MFC) through the steps of: (a) fibrillating a fibrous pulp suspension; (b) dehydrating the fibrillated pulp obtained from step (a);( c) repeating said fibrillation and dehydration steps referred to by (a) and (b) one or more times, with increased pulp consistency for each fibrillation step (a); and (d) subjecting the dehydrated pulp obtained from the final dehydration step (b) to a final fibrillation step.
    [019] In the above modification there is a progressive increase in the consistency of the pulp, and the limit of 12.5% between the category ranges (LC) and (HC) is preferably exceeded in the course of the process.
    [020] The present inventors surprisingly found that after the initial fibrillation of the thicker pulp suspension in the (LC) range, i.e. less than 12.5% and preferably less than 10%, the consistency can in one step subsequent be increased by dehydration to the range 12.5% to 20%, preferably to the range 15 to 20%. This concentrated suspension is then fibrillated through a high consistency (HC) fibrillation device, for example, a high consistency (HC) refiner or extruder. The advantage of this is that fiber-to-fiber friction occurs more intensely and causes fibrillation with greater amounts of high elongation MFC.
    [021] If refining in the low-consistency fibrillation range is done in several refiners in series, the first refiner can be loaded with greater intensity, the second refiner with less intensity, and so on until the loading can no longer Be done. This is because the fibrous material becomes thinner, and a lower refining load can be applied within the raw material. As each refiner has a so-called no-load energy demand (no load, energy demand is measured with water); for the same effect, the less energy is put into the fibers, the more energy is needed. This disadvantage will be overcome by increasing the consistency of the raw material, in accordance with the present invention (increasing the consistency, a greater amount of refining energy is applied in fibrillation).
    [022] In comparison, a sequence of refining steps with a constant low consistency would require a progressive increase in energy to obtain continuous fibrillation, thus, a very ineffective procedure. Refining in the high-consistency fibrillation (HC) range, without preliminary low-consistency (LC) fibrillation, would similarly be more energy-consuming and ineffective. However, the invention offers an optimal solution, with reduced energy consumption and an improved MFC product.
    [023] The objective is to obtain a high elongation rate of MFC, with better mechanical properties, less fiber cut, and a product that is more suitable for composite materials, as well as products where cut resistance is necessary .
    [024] Another advantage is that a smaller amount of fines is obtained, if compared to the traditional production of MFC, as disclosed in the prior art. Furthermore, a better yield and lower sugar content in the aqueous phase are still obtained. Brief Description of Drawings
    [025] Figures 1 and 2 are schematic representations of possible embodiments of the present invention.
    [026] Figures 3a and 3b show microscopic photos of the fibers obtained using the method of the present invention. The bar in the photo in figure (a) is correlated at 100 µm, and in figure (b) at 200 µm. Detailed Description of the Invention
    [027] A preferred method of producing microfibrillated cellulose (MFC), according to the invention, comprises the steps of: (a) mechanically fibrillating a fibrous pulp suspension with a low consistency (LC), less than 12.5% by weight; (b) dehydrating the fibrillated pulp from said fibrillation step to a high consistency (HC) of at least 12.5% by weight and subjecting the dehydrated pulp from the dehydrating step to further fibrillation.
    [028] The method of the invention is processed in commercially available devices and can be scaled up to production in bulk. Appropriate methods were presented and discussed, for example, in the publication "Papermaking, Part 1, Stock Preparation and Wet End"; Volume 8; Editor: Hannu Paulapuro; 2008. The method also enhances processability in the high consistency fibrillation (HC) step, whereby energy consumption is then reduced. The resulting product is homogeneous, the fibers have a high elongation index and the amount of fines is low. The product also has a high solids content and probably also a reduced water holding capacity when compared to products obtained using traditional methods.
    [029] According to an embodiment, said first fibrillation step (a) is fibrillation in low consistency, with a consistency of less than 12.5% by weight, preferably at most 10% by weight, and the said further fibrillation step (c) is high consistency fibrillation (HC) having a consistency of 12.5 to 20% by weight, preferably from 15 to 20% by weight. Low consistency in the first fibrillation step reduces fiber flocculation. The LC fibrillation step also reduces energy consumption in the HC fibrillation step. Dehydration increases the solids content of the final product and the reduced volume is a marked economic advantage in transportation.
    [030] There may be one or more low-consistency fibrillation steps before the pulp is dehydrated to a high-consistency. Preferably, consistency is increased between each soft fibrillation step so that the refining energy is applied to the fibrillation in each refining step. The fraction of water containing a low solids content can be circulated back to the low consistency fibrillation step(s).
    [031] According to an embodiment, said first fibrillation step (a) is a refining step and said additional fibrillation step (c) is a refining or extrusion step. This results in fibers having a high elongation index.
    [032] According to an embodiment, the pulp is refined to a drainage resistance (SR) of more than 45°, more preferably more than 60°, most preferably more than 80°. This step is preferably done in low or medium concentration. Refining the pulp to a higher degree of drainage resistance (SR) results in lower energy consumption and better equipment processability during high consistency fibrillation (HC).
    [033] Another preferred way of practicing the invention is the production of microfibrillated cellulose (MFC), through the steps of: (a) fibrillating a fibrous pulp suspension; (b) dehydrating the fibrillated pulp obtained from step (a); (c) repeating said fibrillation and dehydration steps referred to by (a) and (b) one or more times, with increased pulp consistency for each fibrillation step (a); and (d) subjecting the dehydrated pulp obtained from the final dehydration step (b) to a final fibrillation step.
    [034] The advantages achieved by the present method were discussed above. The increase in consistency allows the refining energy to be used in each fibrillation step.
    [035] According to an additional embodiment of the invention, the dehydrated pulp subjected to the final step of fibrillation has a consistency in the range of 15 to 20% by weight.
    [036] According to another embodiment of the invention, the pulp subjected to the final step of fibrillation has a resistance to drainage (SR) of at least 45 , preferably at least 60 , more preferably at least 80 .
    [037] According to another embodiment of the invention, the first fibrillation step is carried out for a pulp having a consistency of at most 10% by weight.
    [038] According to a further embodiment of the invention, said first fibrillation step (a) is a low consistency (LC) fibrillation step, with a consistency of less than 10% by weight, and said final fibrillation step (d) is a high-consistency (HC) fibrillation step, with a consistency of 15 to 20% by weight, or even higher. High consistency fibrillation results in a product having a high solids content, which is easier to pack and transport, is environmentally friendly, and is more cost-effective.
    [039] According to another embodiment of the invention, a conical or disc refiner is used in the first fibrillation step (a), and a refiner or an extruder is used in the final fibrillation step (d). The low consistency and conical or disc refiner equipment allow the use of bars that provide a low fiber cutting effect.
    [040] According to a further embodiment of the invention, dehydration is carried out by pressure sieving. Pressure sieving is an effective way of removing excess water, also allowing the pulp to be fractionated according to fiber length, if desired.
    [041] After dehydration, the fibrillated fraction of the separated aqueous phase, usually with a high solids content, can be circulated back to the process in order to reduce water consumption and prevent fiber loss.
    [042] According to another embodiment of the invention, a fraction retained by the sieve is subjected to an additional fibrillation. It has been found that using multiple refining steps results in more homogeneous refining and better fiber strength properties than using only a single refining step.
    [043] According to a further embodiment of the invention, dehydration is carried out by centrifugation or with a spacing washing machine.
    [044] According to another embodiment of the invention, a chemical agent such as a refining aid or an enzyme is used to enhance defibrillation. Chemical agents that lower or increase fiber-to-fiber friction and/or fiber flocculation can be used to promote equipment fibrillation and processability. Examples of such chemical agents known to those skilled in the art and commonly used as refining additives are polysaccharides such as CMC and starches, but also nanoparticles. Enzymes such as cellulases and hemicellulases can be used to enhance fibrillation by dissolving the lignocellulose or cellulose structure, or by modifying the fiber properties. Chemical agents can also be used to regulate pH when necessary. Typically, the pH is close to neutral, as an acidic pH prevents water penetration into the fibers and thus promotes cutting and fines generation, and a highly alkaline pH makes it difficult to keep the fibers at the bar edges.
    [045] According to the invention, the fibrous pulp suspension may comprise one or more of a chemical pulp, chemithermomechanical pulp (CTMP), thermomechanical pulp (TMP), ground wood pulp, nanoscale pulp, broken and recycled fiber . Pulps of a non-wood origin, such as pulps of agricultural origin (straws, stalks, etc.) can be used.
    [046] Possible non-limiting embodiments of the invention are illustrated in the form of figures 1 and 2.
    [047] In Figure 1, which illustrates a very simple modality of the invention, a pulp container (1) containing raw material is described; a low consistency refiner (2); a dehydration unit (3); and a high consistency refiner (4).
    [048] In figure 2 a pulp container (1) containing raw material is described; a first low consistency refiner (2); an optional second low-consistency refiner (2'); an optional dehydration unit (3) between the first and second low consistency refiners; a dewatering unit (3') before the high consistency refiner (4) and an optional dehydrating unit (3") before an optional second high consistency refiner (4'); an acceptance fraction (a) having a mass consistency of about 1 to 2% by weight which can be removed from the process or circulated back to the process; an excess of water (a' ) and (a') which can be removed from the process; a reject fraction (b) having a mass consistency of about 8% by weight; a fraction (c) entering a high consistency refiner having a bulk consistency of about 15% by weight; and a fraction (d) and/or (d') and/or (d') having a consistency of about 20% by weight Some alternatives are shown by means of dashed lines.
    [049] Within the scope of the present invention it is also possible to have more than one low consistency refiner in series. Dehydration between refining steps is preferred. Optionally, the fibrillated and dehydrated fiber fraction can be circulated back to the refining step one or more times. Also, there may be more than one dehydration step in series. Furthermore, a high consistency refining can be repeated using the same or different refining machinery. Adjustment of consistency, typically by dehydration or concentration, can be advantageous when carried out between refining steps. The pulp obtained using the present process can be further dehydrated, for example, for eventual transport and then, before use, diluted to a suitable consistency.
    [050] The present invention also covers the products that can be obtained by the method described here, as well as the use of these products.
    [051] The use of microfibrillated cellulose (MFC) as described herein comprises said use as part of a raw material supplied to a paper mill, in a paper or cardboard production machine. When compared to a conventional MFC, the microfibrillated cellulose (MFC) obtained according to the present invention improves pulp retention during tissue formation of a paper or cardboard production machine. This is due to the high elongation of the fibrils and the low amount of fine fines. The initial wet strength of wet fabric is quite satisfactory due to the formation of a high solids content and longer fibrils. Also, the obtained strength properties of paper and paperboard are improved.
    [052] According to a preferred embodiment, the microfibrillated cellulose (MFC) obtained as described herein forms at least 40% by weight, preferably at least 75% by weight, of dry fiber material of the raw material, due to the improved dehydration (when compared to a normal MFC), making it possible to produce tissue containing close to 100% MFC with this material.
    [053] Because of the high elongation fibrils (long and thin), this type of microfibrillated cellulose can be considered as an ideal material for different types of composite and similar products, in which the strength effect is necessary.
    [054] A clear advantage presented by the present MFC is that the amount of fine fines is quite small. Thus, the drying of this type of MFC is much simpler (since the very fine fines cause the formation of small cornified stone-like particles during drying).
    [055] The use of MFC produced as described herein also comprises use as an additive in an injection molded plastic composite material. MFC can reduce the weight of composites and improve strength properties such as crack resistance.
    [056] The invention is further illustrated by the following non-limiting example. It is to be understood that the embodiments presented in the above description and examples are for illustrative purposes only, and that various alternatives and modifications are possible within the scope of the invention. Example
    [057] A never-before-dried Kreft pine pulp having a consistency of about 4% by weight was fibrillated using a conical refiner, to obtain a drainage strength (SR) of 90 (about 0 as CSF). The resulting pulp was subjected to dehydration to a consistency of about 35% by weight. The pulp was then thinned to a consistency of 25% by weight and then refined 2-3 times with a high consistency disc refiner.
    [058] The resulting suspension was visually evaluated using an optical microscope. It was observed that the resulting suspension is substantially homogeneous and that the fibrils exhibit high elongation. The result is shown as shown in figures 3a and 3b.
    [059] Thus, the high elongation microfibrillated cellulose (MFC) obtained was used in a pilot paper production machine, and compared to a typical MFC. The raw material consisted of 70% bleached birch and 30% bleached pine, refined to a drainage strength of 23-26 SR. The amount of MFC used was 25 kg/t. It was surprisingly found that the dehydration of the high elongation index MFC was easier compared to a normal MFC. Furthermore, the samples containing high elongation MFC showed, when compared to a normal MFC, an improved tear strength, better fracture toughness and greater porosity.
    权利要求:
    Claims (11)
    [0001]
    1. Method of production of microfibrillated cellulose (MFC) characterized by comprising the steps of: (a) mechanically fibrillating a fibrous pulp suspension with a consistency of less than 12.5%; (b) dehydrating the fibrillated pulp obtained from step (a ) to a consistency of at least 12.5%; (c) subjecting the dehydrated pulp from step (b) to further fibrillation at a consistency of 12.5 to 20%.
    [0002]
    2. Method according to claim 1, characterized in that said first fibrillation step (a) is a low-consistency (LC) fibrillation step, at a consistency of at most 10%, and said step Additional fibrillation (c) is a high-consistency (HC) fibrillation step at a consistency of 15 to 20%.
    [0003]
    3. Method according to any one of claims 1 and 2, characterized in that said first fibrillation step (a) is a refining step and said additional fibrillation step (c) is a refining step or extrusion.
    [0004]
    4. Method according to any one of the preceding claims, characterized in that the pulp is fibrillated to a drainage resistance (SR) of at least 45°, preferably at least 60°, and even more preferably at least 80° .
    [0005]
    5. Method of production of microfibrillated cellulose (MFC) characterized in that it comprises the steps of: (a) fibrillating a fibrous pulp suspension; (b) dehydrating the fibrillated pulp obtained from step (a); (c) repeating said steps of fibrillation and dehydration of (a) and (b) for one or more times, with increased pulp consistency for each fibrillation step (a); and (d) subjecting the dehydrated pulp obtained from the final dehydration step (b) to a final fibrillation step.
    [0006]
    6. Method according to claim 5, characterized in that the dehydrated pulp submitted to the final stage of fibrillation has a consistency of 15 to 20%.
    [0007]
    7. Method, according to any one of claims 5 and 6, characterized in that the pulp submitted to the final fibrillation step presents a drainage resistance (SR) of at least 45°, preferably, at least preferably, at least 80°. 60th and even more
    [0008]
    8. Method according to any one of claims 5 to 7, characterized in that the first fibrillation step is carried out for a pulp having a consistency of at most 10%.
    [0009]
    9. Method according to any one of claims 5 to 8, characterized in that said first fibrillation step (a) is a low-consistency (LC) fibrillation step, with a consistency of less than 10%, and said final fibrillation step (d) is a high consistency (HC) fibrillation step with a consistency greater than 15 to 20%.
    [0010]
    10. Method according to claim 9, characterized in that a conical or disc refiner is used for the first fibrillation step (a), and a refiner or an extruder is used for the final fibrillation step (d ).
    [0011]
    11. Method according to any of the preceding claims, characterized in that the fibrous pulp suspension comprises chemical pulp, chemithermomechanical pulp (CTMP), thermomechanical pulp (TMP) or ground wood pulp.
    类似技术:
    公开号 | 公开日 | 专利标题
    BR112015016087B1|2021-09-14|METHOD OF PRODUCTION OF MICROFIBRILLATED CELLULOSE
    US9458571B2|2016-10-04|Method for producing furnish, furnish and paper
    CA2824191C|2015-12-08|High aspect ratio cellulose nanofilaments and method for their production
    AU2014353890B2|2019-11-14|Nanocellulose
    ES2560455T3|2016-02-19|Procedure for the production of nanofibrillar cellulose suspensions
    JP2018517856A|2018-07-05|Dry-mixed redispersible cellulose filament / carrier product and process for producing the same
    JP2019520490A|2019-07-18|Microfibrillated film
    Raj et al.2016|Gel point as a measure of cellulose nanofibre quality and feedstock development with mechanical energy
    PT2414435T|2017-10-20|Process for the production of nano-fibrillar cellulose gels
    Ankerfors et al.2014|The use of microfibrillated cellulose in fine paper manufacturing–Results from a pilot scale papermaking trial
    González et al.2013|Suitability of rapeseed chemithermomechanical pulp as raw material in papermaking
    Lengowski et al.2019|Nanocellulose in the paper making
    Tarrés et al.2017|Lignocellulosic micro/nanofibers from wood sawdust applied to recycled fibers for the production of paper bags
    CA3036599C|2020-12-29|Method for producing cellulose filaments with less refining energy
    FI125948B|2016-04-29|Papermaking procedure
    Kumar et al.2014|Preparation and characterization of cellulose nanofibers from bleached pulp using a mechanical treatment method
    CA3056849A1|2018-10-04|Method for producing paper, board or the like
    Kumar et al.2012|Fiber modification with enzymes for improving refining and drainage
    Wang et al.2017|Improved Bleached Chemical Reed Pulp Properties Using Atmospheric High Consistency Refining
    Park et al.2012|Effect of PFI mill and Valley beater refining on Viscosity, Alpha Cellulose, and Crystallinity of wood and cotton fibers
    BR112020017828A2|2020-12-29|METHOD FOR MANUFACTURING A COMPOSITION UNDERSTANDING MICROFIBRILLATED CELLULOSIS
    同族专利:
    公开号 | 公开日
    WO2014106684A1|2014-07-10|
    BR112015016087A2|2017-07-11|
    NO2941442T3|2018-01-27|
    EP2941442A4|2016-08-10|
    EP2941442B1|2017-08-30|
    CN105051070B|2017-07-18|
    EP2941442A1|2015-11-11|
    FI20135016A|2014-07-05|
    CN105051070A|2015-11-11|
    US20150337493A1|2015-11-26|
    FI127682B|2018-12-14|
    PL2941442T3|2018-01-31|
    US10240288B2|2019-03-26|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US3382140A|1966-12-30|1968-05-07|Crown Zellerbach Corp|Process for fibrillating cellulosic fibers and products thereof|
    US3642139A|1968-08-12|1972-02-15|Peter C Wilson|Apparatus for centrifugally removing liquid from a mixture|
    US4341807A|1980-10-31|1982-07-27|International Telephone And Telegraph Corporation|Food products containing microfibrillated cellulose|
    SE445937B|1983-08-23|1986-07-28|Billeruds Ab|COMPOSITION CARTON MATERIAL FOR LIQUID PACKAGING|
    SE513140C2|1998-11-19|2000-07-10|Valmet Fibertech Ab|Procedure for producing upgraded newsprint pulp to SC / LWC quality|
    SE528348C2|2004-09-21|2006-10-24|Noss Ab|Method and apparatus for producing cellulose pulp|
    DE07709298T1|2006-02-08|2014-01-30|Stfi-Packforsk Ab|Process for the preparation of microfibrillated cellulose|
    US7566014B2|2006-08-31|2009-07-28|Kx Technologies Llc|Process for producing fibrillated fibers|
    JP2008075214A|2006-09-21|2008-04-03|Kimura Chem Plants Co Ltd|Method for producing nanofiber and nanofiber|
    GB0908401D0|2009-05-15|2009-06-24|Imerys Minerals Ltd|Paper filler composition|
    SE533509C2|2009-07-07|2010-10-12|Stora Enso Oyj|Method for producing microfibrillar cellulose|
    FI121887B|2009-08-07|2011-05-31|Upm Kymmene Corp|Mechanical pulp as well as system and method for manufacturing the mechanical pulp|
    GB0919422D0|2009-11-05|2009-12-23|Interface Internat B V|Apparatus and method for the manufacture of paper and/or card|
    JP5638001B2|2009-12-01|2014-12-10|国立大学法人京都大学|Cellulose nanofiber|
    FI20105272A|2010-03-18|2011-09-19|Univ Helsinki|Method for fibrillation of lignocellulosic material, fibers and their use|
    US8673113B2|2010-06-09|2014-03-18|The University Of British Columbia|Process for reducing specific energy demand during refining of thermomechanical and chemi-thermomechanical pulp|
    FI122776B|2010-11-30|2012-06-29|Upm Kymmene Corp|Procedures and systems for the manufacture of nanocellulose and nanocellulose|
    AU2012208922B2|2011-01-21|2016-10-13|Fpinnovations|High aspect ratio cellulose nanofilaments and method for their production|
    FI126978B|2011-06-15|2017-09-15|Upm-Kymmene Corp|Procedure for manufacturing nanofibrillar cellulose material and nanofibrillar cellulose material|GB2502955B|2012-05-29|2016-07-27|De La Rue Int Ltd|A substrate for security documents|
    US9879361B2|2012-08-24|2018-01-30|Domtar Paper Company, Llc|Surface enhanced pulp fibers, methods of making surface enhanced pulp fibers, products incorporating surface enhanced pulp fibers, and methods of making products incorporating surface enhanced pulp fibers|
    WO2015007953A1|2013-07-16|2015-01-22|Stora Enso Oyj|A method of producing oxidized or microfibrillated cellulose|
    FI126042B|2014-03-31|2016-06-15|Upm Kymmene Corp|Process for the manufacture of nanofibrillar cellulose and nanofibrillar cellulose product|
    FI127716B|2014-03-31|2018-12-31|Upm Kymmene Corp|A method for producing fibrillated cellulose|
    GB201409047D0|2014-05-21|2014-07-02|Cellucomp Ltd|Cellulose microfibrils|
    EP3303404A4|2015-06-04|2019-01-23|GL&V Luxembourg S.à.r.l.|Method of producing cellulose nanofibrils|
    SE540016E|2015-08-27|2020-11-13|Stora Enso Oyj|Method and apparatus for producing microfibrillated cellulose fiber|
    FI128901B|2015-09-16|2021-02-26|Upm Kymmene Corp|Method for producing nanofibrillar cellulose|
    SE539950C2|2016-05-20|2018-02-06|Stora Enso Oyj|An uv blocking film comprising microfibrillated cellulose, amethod for producing said film and use of a composition hav ing uv blocking properties|
    FR3052101B1|2016-06-01|2019-05-10|Centre Technique De L'industrie Des Papiers, Cartons Et Celluloses|FIXING METHOD AND SYSTEM OBTAINED BY SUCH A METHOD|
    US10753042B2|2016-06-28|2020-08-25|GranBio Intellectual Property Holdings, LLC|Processes and systems for producing nanocellulose from old corrugated containers|
    EP3512998A4|2016-09-14|2020-04-15|FPInnovations Inc.|Method for producing cellulose filaments with less refining energy|
    US11078630B2|2016-11-03|2021-08-03|Oregon State University|Molded pomace pulp products and methods|
    US10196778B2|2017-03-20|2019-02-05|R.J. Reynolds Tobacco Company|Tobacco-derived nanocellulose material|
    WO2019055973A2|2017-09-18|2019-03-21|International Paper Company|Method and apparatus for controlling a fiber fractionation system|
    EP3456639A1|2017-09-19|2019-03-20|Borregaard AS|Compact system for packaging microfibrillated cellulose|
    SE543549C2|2018-03-02|2021-03-23|Stora Enso Oyj|Method for manufacturing a composition comprising microfibrillated cellulose|
    EP3890515A1|2018-12-06|2021-10-13|Cellucomp Limited|Method for replacing eggs in compositions|
    CA3134990A1|2019-03-26|2020-10-01|Domtar Paper Company, Llc|Paper products subjected to a surface treatment comprising enzyme-treated surface enhanced pulp fibers and methods of making the same|
    法律状态:
    2018-03-06| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2018-03-13| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2018-03-20| B06I| Publication of requirement cancelled [chapter 6.9 patent gazette]|Free format text: ANULADA A PUBLICACAO CODIGO 6.6.1 NA RPI NO 2462 DE 13/03/2018 POR TER SIDO INDEVIDA. |
    2019-12-24| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|
    2021-03-09| B06A| Patent application procedure suspended [chapter 6.1 patent gazette]|
    2021-07-06| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2021-09-14| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 30/12/2013, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    FI20135016|2013-01-04|
    FI20135016A|FI127682B|2013-01-04|2013-01-04|A method of producing microfibrillated cellulose|
    PCT/FI2013/051213|WO2014106684A1|2013-01-04|2013-12-30|A method of producing microfibrillated cellulose|
    [返回顶部]