CN118661001A - Process for producing microfibrillated cellulose from high-yield kraft pulp, microfibrillated cellulose obtainable by said process, and kraft pulp and paper products comprising said microfibrillated cellulose - Google Patents
Process for producing microfibrillated cellulose from high-yield kraft pulp, microfibrillated cellulose obtainable by said process, and kraft pulp and paper products comprising said microfibrillated cellulose Download PDFInfo
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- CN118661001A CN118661001A CN202380020990.2A CN202380020990A CN118661001A CN 118661001 A CN118661001 A CN 118661001A CN 202380020990 A CN202380020990 A CN 202380020990A CN 118661001 A CN118661001 A CN 118661001A
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- pulp
- microfibrillated cellulose
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 111
- 239000001913 cellulose Substances 0.000 title claims abstract description 111
- 239000002655 kraft paper Substances 0.000 title claims abstract description 97
- 239000000123 paper Substances 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 65
- 230000008569 process Effects 0.000 title description 39
- 229920005610 lignin Polymers 0.000 claims abstract description 42
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 244000166124 Eucalyptus globulus Species 0.000 claims description 23
- 230000014759 maintenance of location Effects 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 13
- 239000011121 hardwood Substances 0.000 claims description 4
- 239000011122 softwood Substances 0.000 claims description 4
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 3
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 3
- 238000009459 flexible packaging Methods 0.000 claims description 2
- 238000007639 printing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 34
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 230000001862 defibrillatory effect Effects 0.000 abstract 1
- 238000010411 cooking Methods 0.000 description 24
- 239000000835 fiber Substances 0.000 description 23
- 239000000126 substance Substances 0.000 description 15
- 238000011282 treatment Methods 0.000 description 12
- 239000002994 raw material Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 229920002472 Starch Polymers 0.000 description 8
- 238000004061 bleaching Methods 0.000 description 8
- 238000004537 pulping Methods 0.000 description 8
- 239000008107 starch Substances 0.000 description 8
- 235000019698 starch Nutrition 0.000 description 8
- 239000002023 wood Substances 0.000 description 8
- 229920003043 Cellulose fiber Polymers 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 125000002091 cationic group Chemical group 0.000 description 6
- 230000002255 enzymatic effect Effects 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 238000010009 beating Methods 0.000 description 4
- 206010061592 cardiac fibrillation Diseases 0.000 description 4
- 230000002600 fibrillogenic effect Effects 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 229920001131 Pulp (paper) Polymers 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229920001046 Nanocellulose Polymers 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 1
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000004155 Chlorine dioxide Substances 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000004692 Eucalyptus globulus Nutrition 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 229920000147 Styrene maleic anhydride Polymers 0.000 description 1
- YUUKIOKWOBAUSK-UHFFFAOYSA-L [OH-].[OH-].[Cu+2].NCCN Chemical compound [OH-].[OH-].[Cu+2].NCCN YUUKIOKWOBAUSK-UHFFFAOYSA-L 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- -1 alkyl ketene dimers Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004182 chemical digestion Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000019398 chlorine dioxide Nutrition 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000003842 industrial chemical process Methods 0.000 description 1
- 235000020044 madeira Nutrition 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 238000007431 microscopic evaluation Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000012764 mineral filler Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 235000015927 pasta Nutrition 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 235000012015 potatoes Nutrition 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/02—Chemical or chemomechanical or chemothermomechanical pulp
- D21H11/04—Kraft or sulfate pulp
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
- D21H11/18—Highly hydrated, swollen or fibrillatable fibres
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/005—Mechanical treatment
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/10—Packing paper
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/30—Multi-ply
- D21H27/40—Multi-ply at least one of the sheets being non-planar, e.g. crêped
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Paper (AREA)
Abstract
本发明涉及一种由高产率纸浆生产微纤化纤维素的方法，包括以下步骤：选择总木质素含量为按重量计5％至30％的牛皮纸浆，并对其进行解纤以获得最小细小纤维含量为按重量计15％的微纤化纤维素悬浮液。本发明的其他方面涉及通过所述方法可获得的微纤化纤维素，以及包括所述微纤化纤维素的牛皮纸浆和纸产品。所述的方法允许以较低的能耗生产微纤化纤维素，并且所述微纤化纤维素具有增强的造纸适用性，使得纸产品具有增强的机械强度特性。
The present invention relates to a method for producing microfibrillated cellulose from high yield pulp, comprising the steps of selecting kraft pulp having a total lignin content of 5% to 30% by weight and defibrillating it to obtain a microfibrillated cellulose suspension having a minimum fines content of 15% by weight. Other aspects of the invention relate to microfibrillated cellulose obtainable by said method, as well as kraft pulp and paper products comprising said microfibrillated cellulose. Said method allows the production of microfibrillated cellulose with lower energy consumption and said microfibrillated cellulose has enhanced suitability for papermaking, resulting in paper products having enhanced mechanical strength properties.
Description
Technical Field
The present invention relates to a process for the production of microfibrillated cellulose from high yield kraft pulp. Furthermore, the invention relates to microfibrillated cellulose obtainable by said method, as well as kraft pulp and paper products comprising the microfibrillated cellulose obtained. The invention is applied to the field of paper industry.
Background
Microfibrillated cellulose has become an increasingly interesting target for different applications, i.e. in pulp and paper production. They can be produced from different raw materials such as, for example, cellulose fibers from wood, lignocellulose plants, herbs and tubers, etc., and by processes which can involve enzymatic, chemical and mechanical operations alone or in several stages (Klem et al,Nanocelluloses:ANew Family of Nature-Based Materials,Angew.Chem.,Int.Ed.,2011,50,5438—5466).
Traditionally, microfibrillated cellulose is produced from pulp which has been delignified and preferably bleached (Osong et al.,Processing of wood-based microfibrillated cellulose and nanofibrillated cellulose,and applications relating to papermaking:A review,2016,23,93-123;Klemm et al.,Nanocellulose as a natural source for groundbreaking applications in materials science:Today's state,Materials Today,2018,7,720-748).
In fact, as shown in the documents mentioned below, the production process of microfibrillated cellulose is carried out from conventional cellulosic raw materials, i.e. cellulose pulp delignified and/or bleached by typical chemical cooking processes (such as kraft or sulfite processes), and therefore generally has a total lignin content of less than 5% by weight. Likewise, the literature reporting the use of microfibrillated cellulose in the production of paper materials considers it according to its conventional definition as to raw materials and its properties derived from it.
Patent EP3341523B1 discloses a method for producing microfibrillated cellulose requiring less passage through a refiner and therefore low energy consumption, which method involves pulping chemical pulp of cellulose fibers with blades of a certain size.
Patent EP2494107B1 relates to a method for producing microfibrillated cellulose by means of an extruder, wherein at least one chemical product (carboxymethyl cellulose, methyl cellulose, polyvinyl alcohol, calcium stearate, alcohols, surfactants and surface-active products (tensioactives) or other hydrophobic chemical products), preferably cellulose fibers, but also cotton fibers and fibers from agricultural products such as potatoes and cereals, are added to the extruder during processing of the fiber mixture.
Patent application EP2196579A1 describes a process for the production of microfibrillated cellulose with low associated energy consumption, which process involves passing a suspension of cellulose pulp in a solvent such as water, alcohol, dimethyl sulfoxide, glycerol and mixtures thereof through the pores of a homogenizer such that the suspension is subjected to a pressure drop. The diameter of the pores is 100 to 700 μm and the pressure drop has a maximum value of 100 MPa. The cellulose pulp described in this patent application refers to conventional pulp and those pulps obtained by typical production methods, such as bleached, semi-bleached and unbleached pulps by sulfite and sulfate chemistry.
Patent application WO 2014147293A1 discloses a microfibrillated cellulose production process which combines in chemical cooking physical/mechanical treatments of the impregnated cellulose fiber source (such as pressing and shearing), a treatment performed during or after fiber impregnation or during or after fiber cooking, wherein a change in the cell structure of the fiber wall is observed, thereby reducing the energy consumption involved in the production of microfibrillated pulp. The process then proceeds to typical cooking steps, such as cooking by kraft, washing and bleaching, and further pulping with enzymes or solvents, and finally milling the resulting fibrils. The invention describes the use of herbaceous and non-herbaceous fibres and combinations thereof.
Patent EP2576629B1 describes a process for producing microfibrillated cellulose, said to be more efficient and more cost-effective than the prior art, involving acid hydrolysis or acidification at elevated temperature followed by washing and hydrolysis of the cellulosic material at elevated temperature. The lignin content of the cellulosic starting material is less than 5% by weight. As a cellulosic material, chemical pulp of bleached or unbleached hard wood or softwood, such as kraft pulp, sulfite and soda pulp, is considered.
Patent EP2452014B1 describes a more efficient microfibrillated cellulose production process compared to the prior art, consisting of pulp processed cellulose fibers with enzyme and mechanical treatment, where both are performed simultaneously in a single step. Bleached fibers, such as softwood and hardwood fibers, are used because, as described in the aforementioned patent, the presence of lignin in the unbleached pulp results in greater energy consumption in the production of microfibrillated cellulose.
Patent application US20160273165A1 discloses a process for producing a paper product with improved strength and filler and good retention, which process involves adding anionically modified microfibrillated cellulose to a fiber suspension in an amount of 0.1-10% by weight.
Patent application EP3433428A4 describes a board with improved compression strength, involving the use of cellulose pulp with a drainage value of between 15 and 28 (calculated as schober-regel value), to which between 1 and 5% by weight of microfibrillated cellulose and hydrophobic additives such as alkyl ketene dimers, succinic anhydride, rosin and styrene-maleic anhydride, or emulsions, modifications and mixtures thereof are added.
EP2978894B1 describes a method for producing paper and board having strength properties from a mixture of fibers, which method involves adding microfibrillated cellulose, strength additives and particulates such as silica and bentonite in a specific order to the mixture of fibers.
One of the most common industrial chemical processes for producing pulp from wood is Kraft cooking (Kraft cooking) or sulfate cooking (sulfate cooking). Such chemical processes include the digestion of wood in a pressurized reactor at a temperature of about 140 to 180 c in a digestion liquor typically consisting of sodium hydroxide and sodium sulfide (Ek, monica; GELLERSTEDT,Henriksson,Gunnar;Pulp and Paper Chemistry and Technology Volume 2,Pulping Chemistry and Technology,2009,De Gruyter,Berlim). This chemical cooking process is typically ended when the total lignin content is below 5% by weight. It is necessary to extend the kraft cooking process to lignin levels below 5% in order to be able to treat the pulp for direct papermaking or for subsequent bleaching. Kraft cooking is one of the processes typically used to produce raw materials used in prior art microfibrillated cellulose production processes.
The low lignin content in the cellulose pulp used as starting pulp for the production of cellulose fibrils obtained by delignification of wood by chemical means and by an additional bleaching step is necessary and is thus a regulator of the cellulose fibril production process employing these low mechanical and chemical energy costs, as evidenced by Chaker and co-authors, who, when evaluating the suitability of cellulose pulp for fibrillation, select an initial pulp with a lignin content below 20% by weight and subject it after cooking to an additional bleaching step to additionally reduce the lignin content to a value significantly below 5%, typically below 1%, reducing the effect of the presence of lignin on the fibrillation of cellulose pulp (Chaker et al.,Key role of the hemicellulose content and the cell morphology on the nanofibrillation effectiveness of cellulose pulps,Cellulose,2013,20,2863—2875).
Thus, the prior art shows a process for producing microfibrillated cellulose from cellulosic material conventionally used for microfibrillated cellulose production, which is understood as pulp of delignified and/or additionally bleached cellulose by typical chemical cooking methods, such as kraft or sulfite, including modifications for increasing efficiency and reducing associated costs, which involve the use of e.g. organic solvents, chemical treatments such as hydrolysis and fibrillation equipment developed for this purpose in several stages or in combination. Cellulose pulp having a lignin content significantly below 5% is also used as raw material, for which purpose bleaching treatments are applied, for example, to the original cellulose pulp.
Thus, there is a need for a microfibrillated cellulose production process that avoids the use of complex chemical and/or mechanical treatments of the raw material in order to reduce the lignin content of the raw material to a value below 5% by weight, and also does not require such treatments during its conversion to microfibrillated cellulose. There is also a need for a microfibrillated pulp production process which provides lower energy consumption, thereby reducing the costs associated therewith, and which process can be used to produce paper materials with improved strength properties compared to microfibrillated cellulose produced by prior art production processes using conventional cellulosic raw materials, i.e. lignin content below 5%.
Disclosure of Invention
In a first aspect the invention relates to a method for producing microfibrillated cellulose, wherein the method comprises the steps of:
a) Selecting kraft pulp having a total lignin content of 5 to 30% by weight;
b) Mechanically defibrating the pulp selected in step a) until a microfibrillated cellulose suspension with a minimum fines content of 15% by weight is obtained.
A second aspect of the invention relates to microfibrillated cellulose obtained by the method according to the first aspect of the invention.
A third aspect of the invention relates to kraft pulp comprising the microfibrillated cellulose according to the second aspect.
A fourth aspect of the invention relates to a paper product comprising the microfibrillated cellulose according to the second aspect.
Drawings
Fig. 1 shows microscopic observations of microfibrillated cellulose produced from (a) high yield kraft pulp (used in the present invention) and from (b) bleached kraft pulp (used in the prior art) and from (c) commercial microfibrillated cellulose from the prior art. Bars represent a scale of 100 μm.
Fig. 2 shows the percentage of fines of microfibrillated cellulose produced from high yield pulp (squares) and unbleached pulp (diamonds) or bleached pulp (circles) with different grinding energies (measured in an L & W fiber tester 912 apparatus based on total sample, length weighted). The fiber values of the fines of the commercial microfibrillated cellulose are shown in solid lines.
Detailed Description
Described herein is a method for producing microfibrillated cellulose from high yield kraft pulp (i.e. kraft pulp with a total lignin content of 5 to 30% by weight in the context of the present invention), also referred to as MFC in the present specification for simplicity, which surprisingly shows a papermaking capacity providing increased mechanical strength properties for paper products incorporating said microfibrillated cellulose compared to conventional solutions using microfibrillated cellulose by conventional cellulose pulp (i.e. pulp delignified and/or additionally bleached by typical chemical cooking methods such as kraft pulp or sulphite method), according to the following description, compared to methods for producing microfibrillated cellulose from e.g. conventional kraft pulp (in connection with which is a low lignin content, i.e. with a total lignin content of less than 5% by weight in the context of the present invention).
In the context of the present invention kraft cooking refers to kraft cooking or sulfate cooking. This is a chemical process well known in the art and involves cooking wood in a pressurized reactor at a temperature of 140-180 ℃ in a cooking liquor typically consisting of sodium hydroxide and sodium sulfide. Conventional kraft process is understood herein to be a typical chemical digestion process which produces pulp in yields of about 45-55%.
In the context of the present invention, kraft pulp refers to pulp obtained by digestion by the kraft process.
In the context of the present invention, unbleached kraft pulp refers to pulp produced by conventional kraft process, typically having a total lignin content of less than 5% by weight.
In the context of the present invention, bleached kraft pulp refers to pulp produced by a conventional kraft process and further subjected to a bleaching step, typically having a total lignin content of less than 1% by weight. The purpose of the bleaching step is to continue delignification by the action of oxidants such as oxygen, chlorine dioxide and hydrogen peroxide.
In the context of the present invention, high yield kraft pulp refers to kraft pulp produced by chemical kraft cooking in yields exceeding 60% and thus having a total lignin content of 5 to 30% by weight. Thus, when reference is made in this specification to "high yield kraft pulp" it is meant a simplified reference to kraft pulp having a total lignin content of 5 to 30% by weight.
In the context of the present invention, the cooking yield is calculated by the following formula:
pulp weight/wood weight x 100
(Based on absolute dry weight)
In the context of the present invention, the total lignin content by weight is the content of insoluble lignin (content determined according to the Tappi 222om-02 standard) and the content of soluble lignin (content determined according to the standard Tappi UM 250, to which borohydride is added for modification for spectrophotometry-Pinto p.,da estrutura química dos componentes da madeira no seu desempenho nos processos dede pastas celulósicas.Estudo comparativo entre Eucalyptus globulus e outras folhosas,PhD Thesis,Universidade de Aveiro,2005) Is a sum of (a) and (b).
In the context of the present invention and according to standard ISO/TS20477 microfibrillated cellulose refers to cellulose fibers consisting of at least one protofibril (ELEMENTARY FIBRE) comprising crystalline, sub-crystalline and amorphous regions and having an aspect ratio (length/diameter) of more than 10, and may comprise longitudinal fibrils, cross-links between particles or network structures, e.g. produced by mechanical and/or chemical treatment of wood, such as enzymatic treatment.
Therefore, in the background of the technical field, microfibrillated cellulose produced by mechanical treatment alone is generally referred to as "mechanical microfibrillated cellulose" and when produced by a combination of these with enzymatic treatment is referred to as "enzymatic microfibrillated cellulose", because these microfibrillated cellulose are chemically composed of the same elements as the raw material pulp, the intrinsic properties of the produced microfibrillated cellulose depend directly on the process for their production, so that it is impossible to characterize them by their composition due to their heterogeneous nature. This is also contemplated by other production methods and depends on the raw materials involved.
In the context of the present invention, the percentage of fines refers to the percentage of fibrils having a length of less than or equal to 0.2mm as measured on the L & W fiber tester 901 apparatus relative to the average length of the entire sample. With mechanical defibration technology, combined with modern machinery and sufficient energy and time consumption, it is possible to obtain 100% fines. However, in prior art industrial practice, the feedstock is typically treated to a fines level of approximately 50% by weight (measured on the L & W fiber tester 912, length weighted average). The fines content to be achieved may be higher or lower depending on the intended use of the MFC.
In the context of the present invention, microfibrillated cellulose from high yield kraft pulp refers to microfibrillated cellulose produced from high yield kraft pulp.
In the context of the present invention, microfibrillated cellulose from unbleached kraft pulp refers to microfibrillated cellulose produced from unbleached kraft pulp.
In the context of the present invention, microfibrillated cellulose from bleached kraft pulp refers to microfibrillated cellulose produced from bleached kraft pulp.
In the context of the present invention, commercial microfibrillated cellulose refers to a commercially available sample, characterized in that it is produced from fully delignified wood pulp, which is pulp finally used for the production of microfibrillated cellulose by mechanical processes and enzymatic pretreatment, after conventional kraft cooking (the total lignin content in the cellulose fibers of the produced pulp is less than 5% by weight) followed by a bleaching process.
In the context of the present invention, retention aid means additives added during the paper formation process to retain fines and mineral fillers, such as but not limited to linear cationic polyacrylamide.
In the context of the present invention, cardboard refers to paper commonly used in the manufacture of corrugated board.
The top and bottom layers of corrugated board are referred to as linerboards. It is typically a two-layer product, top and bottom layers. Virgin and recycled fibers are used in the production of such papers. In the first option, when the fibers used are virgin fibers produced chemically, primarily by the kraft process, the product is referred to as kraft liner board. When recycled fibers are used primarily, the product is referred to as strong linerboard (testliner). The corrugation between two facers is called corrugation (fluting) or corrugating base paper (corrugated medium).
In the context of the present invention, tissue paper refers to paper used for hygienic and cleaning purposes in the home or public place.
Described herein is a process for producing microfibrillated cellulose from high yield kraft pulp, by definition, comprising a high lignin content, i.e. a total lignin content of 5 to 30% by weight in the context of the present invention.
Surprisingly, the process of the present invention simultaneously allows for the production of microfibrillated cellulose with lower energy consumption compared to prior art processes using conventional kraft pulp (total lignin content below 5% by weight), and wherein the obtained microfibrillated cellulose has papermaking capacity providing increased mechanical strength properties to paper products incorporating said microfibrillated cellulose compared to conventional solutions using microfibrillated cellulose produced by conventional cellulose pulp, i.e. by typical chemical cooking processes such as kraft pulp process or sulphite process delignified and/or bleached pulp.
Indeed, surprisingly, the process of the present invention makes it possible to produce microfibrillated cellulose with the above-mentioned advantages from kraft pulp having a high total lignin content (5% to 30% by weight), contrary to the established practice in the prior art where the use of such high total lignin content pulps (also commonly referred to as high yield kraft pulps) is not advocated.
The process described herein involves selecting a high yield kraft pulp, followed by mechanical defibration thereof until a microfibrillated cellulose suspension is obtained. The method may further comprise, prior to the mechanical defibration step, subjecting the selected pulp to enzymatic hydrolysis.
According to a preferred embodiment of the first aspect of the invention, the method further comprises a step of enzymatic hydrolysis of the pulp selected in step a) between the selection of step a) and the defibration of b).
According to a preferred embodiment of the first aspect of the invention, in step a) the pulp is selected from the group consisting of hardwood pulp, softwood pulp and mixtures thereof.
According to a preferred embodiment of the first aspect of the invention, in step a), the pulp selected is eucalyptus pulp.
According to a preferred embodiment of the second aspect of the invention, the microfibrillated cellulose comprises a minimum fines content of 15% by weight.
According to a preferred embodiment of the fourth aspect of the invention, the paper product is selected from the group consisting of kraft cardboard, strong cardboard, corrugated board, sack paper, shopping bag paper, flexible packaging paper, toilet paper and printing and writing paper.
Examples
Method for producing microfibrillated Cellulose (CMFHYKEP) from high yield eucalyptus kraft
Example 1
In a conical refiner, high yield eucalyptus kraft having a total lignin content of 8% was previously disintegrated and pulped with the following pulping parameters: rotation speed 1230rpm, edge length 0.574km/s, power 0.918kW, SEL (specific energy load applied by the bar edge) 1.6Ws/m and specific energy 350 kWh/ton. The resulting product is further pulped in two stages in a disc refiner. The first stage is carried out with the following beating parameters: the rotation speed is 700rpm, the edge length is 39.48km/s, the power is 5.076kW,SEL 0.15Wm/s and the specific energy is 200 kWh/ton. The second stage is performed with the following beating parameters: the rotation speed is 700rpm, the edge length is 39.48km/s, the power is 5.922kW,SEL 0.10Wm/s and the specific energy is 250 kWh/ton. Beating was performed until a minimum fines content of 15% by weight (length weighted average, based on total sample and measured on the L & W fiber tester 912 device) was reached.
Fig. 1 depicts microscopic analysis of the obtained microfibrillated cellulose suspension. The fibrillation obtained after mechanical treatment and the non-uniformity of size in the same sample can be confirmed. Samples were analyzed in an L & W fiber tester 912 device for particle size determination. Table 1 shows the length weighted average of fiber length and diameter, and the degree of polymerization calculated according to ISO 5351:2010 using the parameters and equations defined in the mark-houwink equation (Henrikson et al.,Cellulose Nanopaper Structures of High Toughness,Biomacromolecules 2008,9,1579-1585) using the intrinsic viscosity values determined on samples dissolved in ethylenediamine copper dihydroxide solution.
Table 1. Characterization of microfibrillated cellulose produced from high yield kraft pulp used in the present invention (size and degree of polymerization) and comparison with values obtained from prior art unbleached pulp produced microfibrillated cellulose, bleached pulp produced microfibrillated cellulose and commercial microfibrillated cellulose.
Fig. 2 depicts the percentage of fines of microfibrillated cellulose produced with different pulping energies (based on total sample, length weighted, measured on an L & W fiber tester 912 instrument).
It was confirmed that with the same beating energy, a higher percentage of fines was obtained with high yield kraft pulp than with kraft pulp obtained with conventional kraft process (total lignin content of 2%) and with bleached pulp commonly used in the aforementioned technique (total lignin content of less than 1%). This therefore shows that for high yield pulp, lower energy is required to produce the same amount of fines.
Example 2
High yield eucalyptus kraft having a total lignin content of 5% by weight is decomposed and pulped as described in example 1. The results obtained also show that with this high yield kraft pulp a higher percentage of fines is obtained than with bleached kraft pulp obtained by conventional kraft process, using the same pulping energy.
Example 3
In the same manner as described in example 1, high yield eucalyptus kraft having a total lignin content of 10% by weight was decomposed and pulped. For the same pulping energy, a higher percentage of fines is obtained with this high yield kraft pulp than with bleached kraft pulp obtained by conventional kraft process.
Example 4
High yield kraft pulp having a total lignin content of 7% by weight from eucalyptus and pine in a weight ratio of 85/15, respectively, was decomposed and pulped as described in example 1. It has also been found that with this high yield kraft pulp a higher percentage of fines is obtained than with bleached kraft pulp obtained by conventional kraft process, using the same pulping energy.
Example 5
High yield pine kraft pulp having a total lignin content of 30% by weight was decomposed and pulped as described in example 1. A higher percentage of fines is also obtained with this high yield kraft pulp than with bleached kraft pulp obtained by conventional kraft process, which is consistent with the previous examples.
Papermaking ability of microfibrillated cellulose from high yield kraft pulp
After production MFC HYKEP, its papermaking ability was evaluated according to the following examples. The MFC HYKEP produced was added to high yield kraft pulp (HYKEP) with a total lignin content of 7% by weight. However, the lignin content of the high yield kraft pulp added with MFC HYKEP is independent of the corresponding content of HYKEP pulp used to produce MFC HYKEP. Any HYKEP pulp with a total lignin content of 5 to 30% by weight can be used.
Example 6-papermaking Capacity of microfibrillated cellulose (MFC HYKEP) obtained from high yield eucalyptus kraft blended into high yield eucalyptus kraft (HYKEP) and microfibrillated cellulose (MFC BEKP) obtained from bleached eucalyptus kraft blended into Bleached Eucalyptus Kraft (BEKP)
Comparison of papermaking Capacity
High yield eucalyptus kraft having a consistency of 0.64% (v/w) is mixed with MFC HYKEP having a consistency of 0.5% (w/w) and 35% fines in a ratio of 5 to 10% by weight.
Bleached Eucalyptus Kraft (BEKP) having a total lignin content of less than 1% by weight and a concentration of 0.64% (v/w) is mixed with MFC BEKP having fines at a concentration of 0.5% (w/w) and 31, 45 or 54% in a ratio of 5 and 10% by weight.
Isotropic laboratory paper was prepared on a bench paper former (bench sheet former). For this purpose, the pulp is pulped in advance. The MFC suspension was added to the beaten pulp suspension in a beaker and magnetically stirred for 120s, after which the mixture was poured into a paper former, following the ISO 5269-1 paper forming standard.
O results
150G/m 2(135g Absolute drying (OD)/m2) structural and mechanical strength properties of the paper
Tables 2 and 3 show the results of comparisons of the relative increase in mechanical strength properties compared to the reference of paper produced from BEKP pulp without MFC BEKP and paper produced from HYKEP pulp without CMF HYKEP addition. Mechanical properties were measured according to the corresponding criteria: burst index (ISO 2758:2015), tear index (ISO 1974:2012), tensile index (ISO 1924-2:2008), scott Bond strength (Scott-Bond) (TAPPI 403).
Table 2. Increase (%) in strength properties obtained in paper incorporating 5% MFC relative to the reference (no MFC).
Table 3. Increase (%) in strength properties obtained in paper incorporating 10% MFC relative to the reference (no MFC).
It was confirmed that HYKEP pulp paper having MFC HYKEP had an increased burst index, tear index and tensile index relative to the reference (HYKEP pulp paper without MFC). This increase was also higher than that observed for BEKP pulp sheet with MFC BEKP relative to the corresponding reference (BEKP pulp sheet without MFC).
Thus, the effect of obtaining increased mechanical strength properties in paper made up of HYKEP pulp and MFC HYKEP was demonstrated relative to the conventional option of adding MFC BEKP to BEKP pulp.
HYKEP pulp paper with MFC HYKEP also observed an increased burst index, tear index and tensile index compared to the reference (HYKEP pulp sheet without MFC), with MFC HYKEP having 15% and 50% fines by weight.
Example 7-comparison of papermaking Capacity of microfibrillated cellulose (MFCHYKEP) obtained from high yield eucalyptus kraft or of commercial microfibrillated cellulose (MFC commercial) (white) incorporated into high yield eucalyptus kraft (HYKEP)
135G/m 2 (OD) paper was prepared from high yield eucalyptus kraft pulp having a consistency of 0.64% (v/w) mixed with MFC HYKEP% consistency of 0.5% (w/w).
The procedure for forming the paper is the same as in the previous embodiment.
O results
150G/m 2(135gOD/m2) mechanical strength properties of paper
Table 4 describes the results of the mechanical strength properties of 150g/m 2 paper made from HYKEP pulp with different CMF HYKEP ratios and 150g/m 2 paper made from HYKEP pulp without CMF HYKEP added. In addition, a comparison of the same results obtained with the addition of white commercial MFC to HYKEP pulp was also shown.
Table 4. Increase (%) in intensity properties relative to the reference (HYKEP without MFC HYKEP).
The incorporation of 5% and 10% by weight CMF HYKEP% fines improves the mechanical strength of the paper, such as burst index, tear index and tensile index. The observed increase in CMF HYKEP is always higher than the corresponding increase in commercial CMF.
Also, CMF HYKEP with 15% and 50% by weight fines observed an increase in paper mechanical strength such as burst index, tear index and tensile index.
Example 8 comparison of papermaking Capacity of microfibrillated cellulose (MFCHYKEP) obtained from high yield eucalyptus kraft incorporated into high yield eucalyptus kraft (HYKEP) in the Presence or absence of Retention agent
135G/m 2 (OD) paper was prepared from HYKEP pulp at a consistency of 0.64% (v/w) mixed with MFC HYKEP% at a consistency of 0.5% (w/w). Additional series were produced by adding retention aids according to the compositions shown in table 5.
The procedure for forming the paper is the same as in the previous embodiment.
Table 5. Composition for preparing 135g/m 2 paper.
Table 6 shows the results of a comparison of the mechanical strength properties of 150g/m 2 paper obtained from a pulp containing HYKEP pulp with different proportions of MFC HYKEP pulp and 150g/m 2 paper obtained from HYKEP pulp without MFC HYKEP addition. Two series are shown, namely the absence and presence of retention aid (linear cationic polyacrylamide).
Table 6. Increase (%) in strength properties relative to the reference (HYKEP without MFC HYKEP) in the presence and absence of retention aid.
The incorporation of MFC HYKEP% and 10% by weight of fines in the presence and absence of retention aid resulted in an increase in the mechanical strength properties relative to the reference (always positive results in table 4). Furthermore, an increase in papermaking capacity of MFC HYKEP in the presence of retention aid was observed (relative to the increase in reference without MFC, higher than that observed in the absence of retention aid).
An increase in the mechanical strength properties relative to the reference is also observed with MFC HYKEP having 15% and 50% fines by weight, with and without retention aid.
Example 9-comparison of papermaking ability of microfibrillated cellulose (MFCHYKEP) obtained from high yield eucalyptus kraft incorporated into high yield eucalyptus kraft (HYKEP) in the presence or absence of cationic starch.
According to the following composition shown in table 6: 135g/m 2 (OD) paper prepared from HYKEP pulp with cationic starch incorporated and 0.64% (v/w) mixed with MFC HYKEP at 0.5% (w/w) concentration, and with retention aid.
The procedure for forming the paper is the same as in the previous embodiment.
Table 7. Composition for preparing 135g/m 2 paper.
O results
150G/m 2(135gOD/m2) structural and mechanical strength properties of the paper
Table 8 shows the results of a comparison of the mechanical strength properties of 150g/m 2 paper obtained from HYKEP pulp containing MFC HYKEP pulp in different proportions and 150g/m 2 paper obtained from HYKEP pulp without MFC HYKEP added, in the presence or absence of starch and in the presence or absence of retention aid.
Table 8. Increase (%) in strength properties in the presence and absence of bulk starch (added to pulp suspension) relative to the reference (HYKEP without MFC) in the presence of retention aid.
The use of paper additives such as cationic starch and retention aids commonly used in the production of paper making materials maintains the competitive advantage of using MFC HYKEP to enhance mechanical properties.
A competitive advantage of the reinforcing properties was also observed with MFC HYKEP, wherein MFC HYKEP had 15% and 50% fines by weight.
Example 10-comparison of papermaking Capacity of high yield eucalyptus kraft added to high yield eucalyptus kraft (HYKEP) microfibrillated cellulose (MFCHYKEP) obtained with 35% or 41% fines
Paper 135g/m 2 (OD) was prepared from HYKEP pulp (with incorporated cationic starch and 0.64% (v/w) in the presence or absence of retention aid) mixed with MFC HYKEP (having a fines content of 35% or 41% and a concentration of 0.5% (w/w)).
The procedure for forming the paper is the same as in the previous embodiment.
O results
150G/m 2(135gOD/m2) mechanical strength properties of paper
In tables 9 and 10, the mechanical strength properties of the HYKEP pulp incorporating MFC HYKEP with different levels of fines were increased compared to the properties of the paper made up of high yield pulp without the addition MFC HYKEP.
Table 9. Increase (%) in strength properties of paper with 5% HYKEP CMF and 35% or 41% fines added relative to the reference (HYKEP without MFC) in the presence of bulk starch and in the absence of retention aid.
Table 10. Increase (%) in strength properties of paper with 5 or 10% MFC HYKEP and 35% or 41% fines added relative to the reference (HYKEP without MFC) in the presence of bulk starch and retention aid.
As expected, MFC HYKEP with higher fines content had a more significant impact on the strength properties, e.g. a 50% increase in burst index when compared to the reference without MFC HYKEP.
Claims (10)
1. A method of producing microfibrillated cellulose, wherein the method comprises the steps of:
a) Selecting kraft pulp having a total lignin content of 5 to 30% by weight;
b) Mechanically defibrating the pulp selected in step a) until a microfibrillated cellulose suspension with a minimum fines content of 15% by weight is obtained.
2. The method according to claim 1, wherein the method further comprises a step of enzymatic hydrolysis of the pulp selected in step a) between the selection of step a) and the mechanical defibration of b).
3. The method according to any of the preceding claims, wherein in step a) the pulp is selected from the group consisting of hardwood pulp, softwood pulp and mixtures thereof.
4. A method according to claim 3, wherein in step a) the pulp selected is eucalyptus pulp.
5. Microfibrillated cellulose obtainable by the method of any one of claims 1 to 4.
6. The microfibrillated cellulose of claim 5, wherein the microfibrillated cellulose comprises a minimum fines content of 15% by weight.
7. A kraft pulp comprising microfibrillated cellulose according to any one of claims 5 to 6.
8. A paper product comprising microfibrillated cellulose according to any one of claims 5 to 6.
9. The paper product of claim 8, wherein the paper product further comprises a retention aid.
10. The paper product according to any one of claims 8 and 9, wherein the paper product is selected from the group consisting of kraft cardboard, strong cardboard, corrugated board, pocket paper, shopping bag paper, flexible packaging paper, toilet paper, and printing and writing paper.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PTPT117870 | 2022-03-23 | ||
| PT117870A PT117870B (en) | 2022-03-23 | 2022-03-23 | PROCESS FOR PRODUCTION OF MICROFIBRILLED CELLULOSE FROM HIGH-YIELD KRAFT PULP, MICROFIBRILLED CELLULOSE OBTAINED FROM THE KRAFT PULP PROCESS AND PAPER PRODUCTS COMPRISING THE SAID MICROFIBRILLED CELLULOSE |
| PCT/IB2023/052806 WO2023180947A1 (en) | 2022-03-23 | 2023-03-22 | Process for the production of microfibrillated cellulose from high-yield kraft pulp, microfibrillated cellulose obtainable by said process and kraft pulp and paper products comprising said microfibrillated cellulose |
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| CN118661001A true CN118661001A (en) | 2024-09-17 |
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| CN202380020990.2A Pending CN118661001A (en) | 2022-03-23 | 2023-03-22 | Process for producing microfibrillated cellulose from high-yield kraft pulp, microfibrillated cellulose obtainable by said process, and kraft pulp and paper products comprising said microfibrillated cellulose |
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| EP (1) | EP4497869A1 (en) |
| CN (1) | CN118661001A (en) |
| CL (1) | CL2024002439A1 (en) |
| PT (1) | PT117870B (en) |
| WO (1) | WO2023180947A1 (en) |
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| PT117870B (en) | 2025-01-24 |
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