EP3607136A1

EP3607136A1 - Method for producing microscale and/or nanoscale fiber material

Info

Publication number: EP3607136A1
Application number: EP18714294.8A
Authority: EP
Inventors: Stefan TRUNIGER; Tobias WOLFINGER
Original assignee: Weidmann Holding AG
Current assignee: Weidmann Holding AG
Priority date: 2017-04-07
Filing date: 2018-04-05
Publication date: 2020-02-12
Also published as: US20210010201A1; WO2018185227A1

Abstract

The invention relates to a method for producing microscale and/or nanoscale fiber material. The method has at least the step of dispersing (5) dried pre-comminuted pulp in a liquid. The method additionally has a step of finely comminuting (6) the pulp dispersed in the liquid such that a fine comminution mixture is produced which contains the liquid and the fiber material with the microscale and/or nanoscale fibril agglomerates.

Description

TITLE

PROCESSES FOR THE PRODUCTION OF MICROSCALE AND / OR

NANOSCALE FIBER MATERIAL

TECHNICAL AREA

The present invention relates to a method for the production of micro- and / or nanoscale fiber material, the use of a mixture containing such a fiber material, and the material itself.

STATE OF THE ART

Microscale and / or nanoscale fiber material is suitable for a wide variety of applications. For example, micro-scale and / or nanoscale fiber material is used in paper and board production, for reinforcing plastics, for electrical insulation and even in cosmetics.

Microscale and nanoscale fiber material is a material made from any cellulosic material. For example, the micro-scale or nanoscale fiber material from wood, sugar beets, potatoes, hemp, flax, cotton, wheat straw or algae can be produced. Normally, however, micro-scale or nanoscale fiber material is produced from wood. The production of microscale and nanoscale fiber material is known to those skilled in principle. For the production of the microscale or nanoscale fiber material, for example, a pulp is processed based on the cellulose-containing material. According to a customary variant, a pulp is formed from the pulp by adding water in a pulper or in a dissolving drum. The pulp fibers dispersed in the pulp are then pre-shredded in a refiner. The resulting pre-shredded pulp is then re-added water if necessary. Subsequently, the pulp dispersed in the water is finely comminuted in another refiner or in a high-pressure homogenizer. In the case of energy-intensive coarse or pre-shredding, a relatively large groove volume of the refiner's grinding set must be selected so that the groove size is matched to the fiber lengths. Depending on the starting material, a different machine configuration must be selected. Since the fibers are shortened by the comminution, at most even the blades of the Refmers must be changed during the pre-shredding, whereby the material throughput is delayed.

In addition, in the pre-crushing of the pulp dispersed in the water whose fiber structure is broken, whereby the water penetrates into the amorphous areas of the pulp and leads to fiber swelling. The material obtained after the pre-shredding is therefore relatively difficult with respect to a possible transport or must still be dewatered, which takes much time and / or energy due to the high water retention.

Another problem with the production methods customary in the prior art is the metal abrasion in the refiners. In the case of coarse and, in particular, fine comminution, the metal knives of the refiner generally have a certain degree of wear, which occurs in the end product in the form of metal particles or metal particles ., a grayish discoloration uttered. While this is not relevant in some applications, metal particles are unacceptable for example in electrical engineering applications.

WO 2014/029909 A1 describes the production of microscale and nanoscale fiber material by means of a wet pre-comminuting step. The fiber material obtained by this step is dried, remoistened and then further comminuted. WO 201 1/004301 A1 describes a process for the treatment of cellulose fibers by means of an enzymatic and mechanical pretreatment step in an aqueous medium.

WO 2016/024046 describes a process for the production of nanofibrillar cellulose. The process comprises a plurality of comminution steps, wherein the fiber material has at least 20% by weight of water after the first comminuting step. Additional drainage can increase the amount of dry material.

US 4,966,651 describes the crushing of bleached and wet pulp in a grinding machine having a grinding wheel with an abrasive surface. PRESENTATION OF THE INVENTION

It is therefore an object of the present invention to provide a simple but efficient method for producing high-quality microscale and / or nanoscale fiber material. To solve this problem, a method is proposed, as indicated in claim 1. Claims 15 and 16 specify the use of a mixture which contains the fiber material resulting from said process. In addition, a material is specified in claim 18, which has such a fiber material. Preferred embodiments are given in the dependent claims.

The present invention thus provides a process for the production of microscale and / or nanoscale fiber material, the process having at least the following process steps:

- dispersing dry, pre-shredded pulp in a liquid; such as

- Finely comminuting the pulp dispersed in the liquid such that a Feinzerkleinerungsmischung formed, which contains the liquid and the fiber material with the micro-scale and / or nanoscale Fibrillenagglomeraten.

According to the invention, the starting material used is thus pre-shredded pulp in dry form. By contrast, in the case of the processes customary in the prior art, the pulp is already dispersed in a liquid before the preliminary comminution, so that it is present after the pre-comminution in an aqueous dispersion and with appropriately swollen fibers. The use of pre-shredded pulp in dry form has the advantage that it can be produced much simpler and with less expenditure of energy. For example, the pre-shredding can be carried out purely mechanically and preferably essentially without the addition of liquid, more preferably without the addition of liquid. This makes the equipment required for the pre-shredding easier and less expensive. The machine configuration also becomes less dependent on the starting material used. Nevertheless, in the dry pre-shredding with simpler means usually a narrower and thus qualitatively better fiber length distribution is achieved than is the case with the wet pre-shredding. This has the advantage that in the subsequent fine comminution, the risk of clogging of the device used for the fine comminution can be reduced. Due to the dryness of the fibers even a classification of the fibers in the starting material with respect to their length by means of a sieve is possible. In addition, the problem of fiber graying does not arise, or at least less, since any metal debris arising during dry pre-shredding can not penetrate into the interior of the fibers together with the liquid. Further advantages arise in relation to the storage and transport of the starting material. Since no liquid penetrates into the fibers during the preliminary comminution and the water content before and after the pre-comminution is thus substantially the same depth, preferably the same, the pre-comminuted pulp has a significantly lower weight and volume and is therefore easily transportable. The fact that the pre-shredded fibers have significantly less moisture also delays the formation of odors and biodegradation of the pulp, allowing it to be stored much longer. The use of dry, pre-shredded pulp, which is dispersed in a liquid and then finely comminuted, has the further advantage that the liquid content after comminution can be easily reduced, for example, thermally and / or under reduced pressure or by sedimentation and subsequent skimming. The reason for this is that the liquid in the inventive method does not or much less penetrates into the cell structure of the pulp fibers, as is the case in the conventional methods of the prior art. This is an advantage in washing processes after, for example, a chemical pretreatment in that the dewatering process can be realized without fiber losses and low specific water consumption. In the case of the method according to the invention, the pulp is thus comminuted, the pulp essentially not yet being fibrillated during the coarse comminution, preferably not fibrillated. In the subsequent comminution, the dry, pre-shredded pulp is then fibrillated. By contrast, in the prior art processes the pulp is already fibrillated during the coarse comminution.

The fiber material comprises microsized and / or nanoscale fibril agglomerates. That is, the individual fibers and in particular the microfibrils of the original pulp are partially or wholly separated from each other and comminuted, in particular the separated microfibrils form due to mutual association Fibrillenagglomerate, which are further specified below with respect to their average length in more detail. The microfibrils present within the fibril agglomerates are completely separated from the original fiber structure of the pulp and are interconnected due to mutual adhesion, so that they form a common structure, in particular a network. It is known to the person skilled in the art that microfibrils are to be understood as meaning an arrangement of a plurality of individual fibrils, as described, for example, in WO 201 1/004301. When dispersing the fibril agglomerates in a liquid, such as in particular in water or in a liquid comprising water, a mutual association, ie attraction or adhesion of the individual fibril agglomerates generally takes place, so that a gel-like material is formed. On the other hand, if the liquid is completely or at least substantially removed, which is easily possible with a liquid such as, for example, acetone or ethanol, there is generally no association of the individual fibril agglomerates with one another.

Preferably, the comminution mixture produced by means of the specified method and in particular the fiber material with the microscale and / or nanoscale fibril agglomerates is completely or at least substantially free of visible individual fibrils. The individual fibrils are then considered to be visible if, when viewed under an electron microscope, they are readily recognizable as such at an enlargement factor of 10Ό00 and a resolution of 10 nm. On the other hand, the fibrous material is completely or at least substantially free of visible individual fibrils if all or substantially all of the fibrils, as a rule in comminuted form, are bound respectively in the networks forming the fibril agglomerates. The comminution mixture or the fiber material with the microscale and / or nanoscale fibril agglomerates is considered to be substantially free of visible individual fibrils if the visible individual fibrils at most 5 percent, in particular at most 1 percent of the total number of visible particles of the comminution mixture or the fiber material make up the microscale and / or nanoscale fibril agglomerates.

The starting material used is dry pulp, which is already in a pre-shredded state. The pre-shredded pulp is considered to be dry if it has the usual moisture for pulp, that is, has no significant fluid additions. Slight additions of liquid may be present, but not those which excessively affect the total weight of the pulp, that is, more than 15% by weight, preferably more than 10% by weight, more preferably more than 5% by weight. The pulp is considered not to be dry, especially when dispersed in a liquid. Preferably, the dry, pre-shredded pulp has a water content of 15% by weight or less, more preferably at most 10% by weight, even more preferably from 1% to 9% by weight, most preferably 5% by weight. - 8 wt .-%, based on the total weight of the dry, pre-shredded pulp, wherein the water content is preferably measured according to the Nonn EN 20638, September 1993. At the stated water contents of the dry, pre-shredded pulp, a consistent, reproducible fine comminution of the dry, pre-shredded pulp be guaranteed. If the water content of the dry, pre-shredded pulp is too high, the fine comminution of the pulp results in knotting of the fibers which, for example, can lead to blockage in machine parts of the comminution device.

The pulp is precomminuted when a major proportion of the total number of fibers, that is more than 50%, more preferably even more than 75%, most preferably even more than 90% of the fibers have a length which is longer than the original fiber length the starting material used is significantly and in particular many times smaller. In the case of dry, pre-shredded pulp, at least some of the fibers are shortened. This means that the material used as the starting material for the dispersion was already pre-comminuted in a previously performed process step, so that the fiber lengths were reduced. In fine comminution, the previously pre-shredded pulp, after having been dispersed in the liquid, is further comminuted until it forms the fiber material with the micro-scale and / or nanoscale fibril agglomerates. That is to say, in the case of fine comminution, the pulp fibers are further reduced in terms of their length expansion and, in particular, again reduced by a multiple. In addition, the fibers and in particular the individual microfibrils are separated from each other during comminution so that they are preferably more than 60%, more preferably more than 70%, more preferably more than 80%, even more preferably more than 90% after the comminution step %, most preferably more than 95%, are separated from each other. These mutually separated, comminuted microfibrils attract each other and form the microscale and / or nanoscale fibril agglomerates.

The fine comminution is preferably carried out mechanically and preferably by means of a mineral material, in particular by means of comminution means, such as a comminution set, from a mineral material. In a mineral material, a certain micro-roughness is always present even with the occurrence of wear and tear. In addition, the problem of metal abrasion does not exist. The mineral material is preferably corundum, diamond or silicon carbide (SiC).

For the fine comminution, a refiner, in particular a refiner comprising comminuting means made of a mineral material, is preferably used. However, it is also possible to use a ball mill, a homogenizer or a microfluidizer. Furthermore, it is possible to comminute by means of ultrasound, jet collision or cryocrushing accomplish.

The method preferably has the additional step that the pulp is preferably pre-shredded mechanically before being dispersed and essentially without addition of a liquid, preferably without addition of a liquid. For the pre-crushing, which may also be referred to as coarse comminution, preferably pulp plates or flash-dried pulp, which may be present in particular in the form of bales, are used. Flash dried pulp is made by flash drying in which the pulp is dried unhindered in a hot air stream. The mechanical pre-shredding is advantageously carried out by means of a metal, preferably by means of a comminuting agent made of metal. Since essentially no liquid, preferably no liquid, is added and the preliminary comminution is thus carried out in the dry state of the pulp, any metal particles do not penetrate into the interior of the fibers and are also easier to remove again. The use of pulp plates or flash-dried pulp offers the advantage that the pulp has a comparatively small volume and thus the device for dry pre-shredding, in particular in a shredder, can be filled well with the pulp.

The pre-shredding can, if pulp plates are used, for example by means of a fine mill, a granulator, a hammer mill, a mixer, an impact mill or any combination thereof. The elements of these devices, which directly effect comminution, are preferably made of metal.

If flash-dried pulp is used, the pre-crushing may be carried out, for example, by means of a shredder, a granulator or a hammer mill. Again, the elements of these devices, which cause the crushing directly, preferably made of metal.

The average fiber length of the pulp used for the pre-crushing is preferably in the range of greater than or equal to 0.4 mm (millimeters), more preferably in the range of 0.4 mm - 10 mm, more preferably in the range of 0.6 - 8 mm, most preferably in the range of 0.6 mm - 6 mm, wherein the average fiber length is preferably measured according to the standard TAPPI T271 pm -91 from 1991. These areas have the advantage that the risk is reduced that the device for pre-shredding or dry comminution or coarse shredding, clogged. The pulp used for the pre-shredding is preferably dry and preferably has a water content of only at most 15 wt .-%, more preferably of at most 10 Wt .-%, more preferably from 1 wt .-% - 9 wt .-%, most preferably from 5 wt .-% - 8 wt .-%, based on the total weight of the pulp used for the pre-crushing on. The measurement of the water content is preferably based on the standard EN 20638 of September 1993.

As the original starting material for the production of the dry, pre-shredded pulp or in particular for the production of the pulp plates or the flash-dried pulp used for the pre-shredding is advantageously used a plant, such as in particular a wood or a year-old plant. The plant preferably uses the stem, the foliage or the skin of the fruit.

As the original starting material for the production of the dry, pre-shredded pulp or in particular for the preparation of the pulp plates or the flash-dried pulp used for the pre-shredding, are particularly advantageous fruits, such as citrus fruits or apples, cereals, such as wheat or corn, grass or fiber-containing vegetables, such as peas, legumes or carrots. The citrus fruits include, for example, lemons, oranges, limes or grapefruit. In the case of lemons and oranges, the shell is particularly preferably the original starting material. For apples, the apple pomace is particularly preferably the original starting material. The stated original starting materials have the advantage that they allow a particularly high pulp yield. The citrus fruits, especially the shells of lemons and oranges, as well as the apples, in particular the apple pomace, also offer the advantage that they have a particularly high pectin content. The comminution mixture or the fiber material with the microscale and / or nanoscale fibril agglomerates is preferably used for increasing the viscosity, such as, for example, a liquid. If the fiber material is made with the microscale and / or nanoscale fibril agglomerates using pectin-containing original starting materials, then a fiber material results which is more viscosity-enhanced compared to fiber material made using non-pectin-containing original starting materials.

From the original starting material, which is preferably a plant, such as in particular a wood or a year-old plant, preferably chips or wood chips are produced, preferably in the case of wood, which are then mechanically, chemically or combined mechanically and chemically processed to the Starting material for pre-shredding, in particular the mentioned pulp plates or the mentioned flash-dried pulp. As a result of the further processing, the original starting material, which is in particular a woody or an annual plant, is delignified and the fibers are separated from the wood composite, that is to say the original starting material is defiberized. In this case, in particular, the degree of whiteness can be increased. For chemical processing, sulfate, sulfite, ASAM (alkaline sulfite process with anthraquinone and methanol) or S0 ₂ / ethanol can be used. The chemical processing can also be done by means of Organocell or Steam Exposion. Furthermore, the chemical processing can also be carried out by means of an Allcell, Acetosolv, Acetocell, Formacell or Milox process.

Advantageously, the dry, pre-shredded pulp is compacted, more advantageously in the form of pellets and / or briquettes before. The dry, pre-shredded pulp is thus advantageously compacted before dispersing in the liquid, preferably pelleted or briquetted. The densification, preferably pelleting or briquetting, reduces the volume of the pulp, there is less dust and the packaging costs are reduced. In addition, the compacted pulp, especially if it is in the form of pellets or briquettes, is pumpable. In addition, the water absorption rate of the compressed pulp, in particular the pellets or briquettes, slower and the compressed pulp, in particular the pellets or briquettes, are better dosed. The compaction of the pulp, in particular the pelleting or briquetting, thus improves the storage and transportability as well as the handling of the dry, pre-shredded pulp.

The dry, pre-shredded pulp preferably has a water content of at most 15% by weight, more preferably at most 10% by weight, even more preferably from 1% by weight to 9% by weight, most preferably 5% by weight. 8 wt .-%, based on the total weight of the dry, pre-shredded pulp, on. The measurement of the water content is preferably based on the standard EN 20638 of September 1993.

Advantageously, the dry, pre-shredded pulp is in the form of a powder. The fiber length is preferably in the range of 0.025 - 6 mm, more preferably in the range of 0.4 - 1.7 mm. Such a fiber length is optimally suited for fine comminution and economic operation of the plant. Such fiber lengths offer the particular advantage that the risk of clogging of the apparatus for comminution, such as the homogenizer or the ball mill, is reduced. In addition, in a refiner no set change is necessary. Furthermore, at least two refiners are not necessary, ie a coarse refiner and a fine refiner. The water retention capacity is preferably 40-60 wt .-% based on the total weight of the dry, pre-shredded pulp. The water retention capacity is measured according to the information given in "T. Wolfinger, Three-dimensional structural analysis and modeling of the force-strain behavior of fiber structures, TU Dresden, Faculty of Environmental Sciences, Dissertation submitted in November 2016 ». The low water retention capacity compared to the coarse shredding in a refiner leads to a rapid sedimentation of the material, which in turn has an advantage in, for example, washing operations. The preferred drainage resistance of the dry, pre-shredded pulp, determined according to ISO 5267-1 of July 2000, is preferably 12-15 ° SR (Schopper-Riegler). Advantageously, at least 10% by weight, preferably at least 20% by weight, more preferably at least 40% by weight, more preferably 60% by weight, even more preferably 80%, even more preferably at least 90%, even more preferably at least, after comminuting 95%, most preferably 100% by weight of the fiber material of the comminution mixture, based on the total weight of the fiber material of the comminution mixture, in the form of microscale and / or nanoscale fibril agglomerates. With a rather small proportion of microscale and / or nanoscale fibril agglomerates in the fiber material, such as in particular in a proportion of 10 wt .-% to 30 wt .-% based on the total weight of the fiber material, the fiber material is particularly well suited for influencing the strength, for example, in applications in the paper industry. With an average proportion of from 30% by weight to 60% by weight, based on the total weight of the fiber material, it is possible in particular to utilize the texturing and structure-forming properties of the fiber material. With a high proportion of at least 60% by weight of the microscale and / or nanoscale fibril agglomerates, based on the total weight of the fiber material, the fiber material can be used for different applications, in particular for rheology and / or porosity control, due to the very large surface area formed by the fibril agglomerates become.

The mean length of the microscale fibril agglomerates is preferably in the range from 500 nm to 1000 μm, more preferably in the range from 500 nm to 600 μm, even more preferably in the range from 500 nm to 200 μm. The determination of the average length of the fibril agglomerates is carried out preferably according to the standard ISO 13322-2, 1st edition of 1.1 1.2006. The narrower the distribution of the average fiber length, the more defined properties of the fiber material can be achieved. Fiber material with such Fibrillenagglomeraten is particularly suitable for various materials, such as food, cosmetic products or pharmaceutical products to produce.

The average length of the nanoscale fibril agglomerates is preferably in the range of 10 nm. 500 nm.

The fibrous material having the microscale and / or nanoscale fibril agglomerates preferably has a surface area of 40-450 m ² / g, more preferably a surface area of 50-400 m ² / g, even more preferably a surface area of 60-400 m ² / g, most preferably a surface of 80 - 350 m ² / g. Fiber material with such surfaces is particularly suitable for producing a wide variety of materials, such as, for example, foods, cosmetic products or pharmaceutical products. For the measurement of the surface, the following method is preferably carried out with the method steps "sample preparation 1", "sample preparation II" and "carrying out the nitrogen adsorption measurement / calculation of the surface":

Sample preparation I:

Approximately 20 g of a fiber dispersion comprising water and 2% by weight of fiber material comprising micro-scale and / or nanoscale fibril agglomerates are weighed into a 50 ml Falcon tube. The volume of the Falcon tube is supplemented to 50 ml with ethanol (94%) and mixed with a vortex mixer for 30 - 60 s. The sample is centrifuged in a centrifuge (eg type Hettich Rotina 380 with 6-fold 45 ° angle rotor) at 5000 1 / min for 10 minutes. Subsequently, the filtrate is poured off, the now empty volume again with ethanol (94%) supplemented and stirred with a glass rod. Subsequently, the sample is again loosened for 30-60 s with a vortex mixer and centrifuged again at the same parameters. This process is repeated 5 times. Subsequently, the residual moisture is carried out from the material by drying in supercritical C0 ₂ such as in a Tousimis Autosamdri 931. Sample preparation II:

The sample, dewatered by the method of Sample Preparation I, is placed in a previously dried and empty glass tube and allowed to stand for a min. 24 h at min. Degassed 105 ° C. Execution of the nitrogen adsorption measurement / calculation of the surface:

The glass tube containing the degassed sample after sample preparation II is now placed in a suitable instrument for the determination of nitrogen sorption isotherms such as a Micromeritics 3Flex version 3.01. For example, the sample mass is 0.0777 g, but may differ from instrument to instrument or sample specific. The nitrogen and helium used for the measurement have a purity of 99.999%. The result of the measurement will be on one decimal place specified in m ² / g. The stated value of the result is based on the calculation basis for BET according to Brunauer, Emmett and Teller, which is known to the person skilled in the art.

Preferably, at least 1%, more preferably at least 10%, even more preferably at least 20%, even more preferably at least 40%, even more preferably at least 50%, even more preferably at least 60%, even more preferably at least 70%, even more preferably at least 80%, more preferably at least 90%, bevorzugtesten 100%, of the total particles of the fibrous material preferably have an average length in the range of 500 nm - 1000 μιη, more preferably in the range of 500 nm - 600 ^μι η, more preferably in the range of 500 nm - 200 μιη on. The particles of the fiber material comprise not only the microscale and / or nanoscale fibril agglomerates, but may also comprise any fibrils present and any other constituents of the fiber material. The stated percentages of the mean fiber lengths are preferably determined by means of the standard ISO 13322-2, 1st edition of 1.1 1.2006. Fiber material with such amounts of particles is particularly suitable for producing a wide variety of materials, such as, for example, foods, cosmetic products, pharmaceutical products.

The D90 value for the length of the particles of the fiber material with the micro-scale and / or nanoscale fibril agglomerates, the length preferably being measured according to the standard ISO 13322-2, 1st edition of 1.1 1.2006, indicates which maximum length is 90% have the particles of the fiber material, and is preferably in the range of 1 - 200 μιη, more preferably in the range of 30 - 150 μιη, more preferably in the range of 40 - 140 μιη. Fiber material comprising such particles is particularly suitable for producing a wide variety of materials, such as, for example, foods, cosmetic products, pharmaceutical products. The calculation of the D90 value is known to the person skilled in the art.

The D90 value for the thickness of the particles of the fiber material with the microscale and / or nanoscale fibril agglomerates, wherein the thickness is preferably measured according to the standard ISO 13322-2, 1st edition of 1.1 1.2006, indicates which maximum thickness is 90% have the particles of the fiber material, and is preferably in the range of 0.5 to 20 μιη, more preferably in the range of 1 to 10 μηι, more preferably in the range of 1-8 μπι. Fiber material comprising such particles is particularly suitable for producing a wide variety of materials, such as, for example, foods, cosmetic products, pharmaceutical products. The calculation of the D90 value is known to the person skilled in the art. The water retention capacity of the fiber material with the microscale and / or nanoscale fibril agglomerates is preferably in a range of 100-700 wt%, more preferably in a range of 150 wt% - 600 wt%, more preferably in a range of 170 wt% % - 500 wt .-%, wherein the water retention capacity preferably according to the information in "T. Wolfinger, three-dimensional structural analysis and modeling of the force-strain behavior of fiber structures, TU Dresden, Faculty of Environmental Sciences, Dissertation submitted in November 2016 », is measured.

Particularly preferably, the fiber material with the microscale and / or nanoscale fibril agglomerates has at least one, preferably several, particularly preferably all of the properties mentioned selected from the group comprising the average length of the microscale and / or nanoscale fibril agglomerates, the surface of the fiber material, the percentages of mean fiber lengths, the water retention capacity of the fiber material, the D90 value for the length of the particles and the D90 value for the thickness of the particles. The resulting combination options are not explicitly mentioned, but are all considered disclosed. Such a fiber material is particularly suitable for producing a wide variety of materials, such as, for example, foods, cosmetic products, pharmaceutical products.

By dispersing the dry, pre-shredded pulp in the liquid results in a dispersion, which advantageously has a liquid content of at least 60 wt .-%, more preferably of at least 80 wt .-%, more preferably from 90 wt .-% - 99 wt .-% most preferably from 94% to 98% by weight, based on the total weight of the dispersion. These liquid contents enable efficient operation of the apparatus for comminution as well as optimum feedability of the apparatus for comminution with the dispersion. The solids content of the dispersion is preferably measured according to the standard ISO 41 19: 1995.

According to an advantageous embodiment, the liquid in which the pulp is dispersed, in particular during comminution, is or comprises a polar substance, in particular water, acetone, chloroform, glycerol or an alcohol, for example isopropanol, glycol, ethanol or a mixture of at least two polar substances, such as in particular an azeotrope, such as a mixture of ethanol and water, or a mixture of water and an enzyme. The use of glycerin as a liquid offers the advantage that the risk of clogging of the device for comminution is reduced. It has been found that glycerol in fine comminution prevents agglomeration of fibers, especially microscale and nanoscale fibril agglomerates. The Liquid used for the preparation of the remoistened mixture, which will be described later, may also be a polar liquid.

According to a further preferred embodiment, the liquid in which the pulp is dispersed, in particular during comminution, is or comprises an apolar liquid, in particular a hydrocarbon, such as an alkane, or an oil, or a mixture of at least two apolar liquids , This has the advantage that the apolar liquid can be removed from the comminution mixture or the comminution mixture dried, the microsized and / or nanoscale fibril agglomerates contained in the comminution mixture agglomerating little to no longer during the drying process and thus the microscale and / or nanoscale Fibrillenagglomerate in the dry mixture substantially individually, preferably individually. The liquid used to make the remoistened mixture, which will be described later, may also be an apolar liquid.

According to another preferred embodiment, the liquid is approved for the production of foodstuffs. This offers the advantage that the fiber material produced according to the invention with the aid of such a liquid may be used in the production of foods. The liquids authorized for food processing are to be taken from the respective national food legislation. The liquid which is used for the production of the remoistened mixture, which will be described below, is preferably also such a liquid, if this remoistened mixture is to serve for the production of a foodstuff.

According to a further preferred embodiment, the liquid is a foodstuff or an intermediate product for producing a foodstuff which is present as a liquid. For example, a liquid food is a non-alcoholic beverage such as milk, fruit juice, tea, coffee, an alcoholic beverage such as wine, beer, or edible oil. This offers the advantage that the fiber material produced with the aid of such liquids may be used with the micro-scale and / or nanoscale fibril agglomerates in the production of foods. An advantage is found, for example, in the production of chocolate, in which no water may come during the production. Advantageously, therefore, the fiber material with the micro-scale and / or nanoscale fibril agglomerates, which is to be incorporated into chocolate, made using the liquid milk and thus no water as such in the chocolate on the fiber material entered. The liquid used for the preparation of the remoistened mixture, which will be described below, is preferably also a liquid food, if this remoistened mixture is to be used to produce a food.

Particularly preferably, the liquid serves as a starting material for the production of a food. Preferably, the fiber material is produced with the microscale and / or nanoscale fibril agglomerates by means of the starting material present as a liquid for the production of a food and preferably then used in the preparation of said food. This offers the advantage that the fiber material and the food are particularly compatible with each other. For example, milk is used as a raw material for the production of yoghurt. If the fiber material with the micro-scale and / or nanoscale fibril agglomerates is used for the production of a yoghurt, milk is advantageously the liquid with the aid of which the fiber material is produced. The liquid which is used for the production of the remoistened mixture, which will be described below, is preferably also such a liquid, if this remoistened mixture is to serve for the production of a foodstuff.

According to a further preferred embodiment, the liquid is authorized for the production of cosmetic products. This offers the advantage that the fiber material produced with the aid of such liquids may be used with the micro-scale and / or nanoscale fibril agglomerates in the production of cosmetic products. The liquids authorized for the manufacture of cosmetic products are to be taken from the respective national legislation. The liquid used for the preparation of the remoistened mixture, which will be described below, is preferably also such a liquid, if this remoistened mixture is to serve for the production of a cosmetic product. Preferably, the liquid used in conjunction with cosmetic products is acetone, hexane, cyclohexane, dioxane, T-butylmethyl ether, dimethoxymethane, chloroform, dichloromethane, ethyl acetate, tetrahydrofuran, 2-butanone, 1,2-dimethoxyethane, acetonitrile, or a mixture thereof, or a non-aqueous protic liquid such as ethanol or isopropanol, or an azeotropic mixture.

According to a further preferred embodiment, the liquid is approved for the production of pharmaceutical products. This offers the advantage that the fiber material produced with the aid of such liquids can be used with the micro-scale and / or nanoscale fibril agglomerates in the production of pharmaceutical products may. The liquids approved for the manufacture of pharmaceutical products are to be taken from the respective national legislation. The liquid used for the preparation of the remoistened mixture, which will be described below, is preferably also such a liquid, if this remoistened mixture is to serve for the production of a pharmaceutical product.

If the fiber material is to serve for the production of cosmetic products and / or pharmaceutical products, the wood of a deciduous tree, in particular beech wood and / or eucalyptus wood, is preferably used as the original starting material for the production of the dry, pre-shredded pulp. If eucalyptus wood is used, this comes beneficially from the eucalyptus Urograndis. Such types of wood have a high content of xylose. It has been found that a high xylose content leads to a particularly pleasant, especially supple and silky sensation of the corresponding product on the skin. The fibrous material, in particular the microscale and / or nanoscale fibril agglomerates, therefore generally has more than 10% by weight, more preferably more than 15% by weight, most preferably even more than 20% by weight of xylose based on the total weight the fiber material or based on the total weight of the micro-scale and / or nanoscale Fibrillenagglomerate. The content of xylose in the fiber material or in the microscale and / or nanoscale fibril agglomerates is preferably measured according to the information given in "T. Wolfinger, three-dimensional structural analysis and modeling of the force-strain behavior of fiber structures, TU Dresden, Faculty of Environmental Sciences, Dissertation submitted in November 2016 »are included. Advantageously, the liquid has a boiling point at atmospheric pressure (101325 Pascals) of 100 ° C or less, more preferably less than 100 ° C, more preferably less than 100 ° C to 50 ° C, most preferably 50 ° C - 90 ° C , on. If the fiber material is produced with the micro-scale and / or nanoscale fibril agglomerates with such liquids, the liquid can be removed from the fiber material particularly gently, in particular thermally and / or under reduced pressure, or the fine comminution mixture can be dried particularly gently, so that the fiber mixture is not damaged, such as by agglomerating the fibril agglomerates together. The dried mixture resulting from the drying of the comminution mixture can be re-added to liquid and the resulting remoistened mixture has the same properties or quality as the fiber material or comminution mixture before drying. Such a property is for example the Viscosity increasing effect.

Particularly advantageously, the boiling point of the liquid is less than 100 ° C, more preferably less than 90 ° C, even more preferably less than 80 ° C, as a result, the liquid can be particularly easily removed from the fiber material or from the comminution mixture. In particular, the liquid can be removed more easily than water from the fiber material or from the comminution mixture. In addition, the risk is reduced that the fiber material, in particular the micro-scale and / or nanoscale Fibrillenagglomerate be damaged.

Preferably, the lowest boiling point of the liquid is at 50 ° C, since this can reduce the risk of ignition of the liquid during the manufacturing process of the fiber material or during the production of the remoistened mixture. According to a preferred embodiment, the same liquid is used for dispersing, comminuting and producing the remoistened mixture.

According to a preferred embodiment, the same liquid is used for dispersing and comminuting, but for the production of the remoistened mixture a liquid is used which is different in comparison to the liquid for dispersing and comminuting. Two liquids are different if the composition of the liquids is different.

The dry, pre-shredded pulp is preferably dispersed in powder form and advantageously by means of a device for mixing, in particular by means of a homogenizer, in the liquid. The pre-shredded pulp in the solution or dispersion then preferably has a liquid content of at least 60 wt%, more preferably at least 80 wt%, even more preferably 90 wt% -99 wt%, most preferably from 94 wt .-% - 98 wt .-%, based on the total weight of the dispersion. While the advantage of the liquid is water, particularly in its availability and ease of handling, acetone, chloroform, ethanol or an azeotrope mixture having a boiling point of less than 100 ° C at atmospheric pressure, such as a mixture of ethanol and water, has the advantage of in that the dry, pre-shredded pulp is readily dispersible in acetone, chloroform, the azeotropic mixture comprising water and ethanol or ethanol and, after the fine comminution, again being separable from the comminution mixture, in particular in comparison with water. When using a mixture of water and an enzyme, it may be the enzyme in particular a cellulase, such as an endo-1,4-glucanase, a hemicellulase, such as a xylanase or a laccase, or a mixture of said enzymes. The weight fractions are then preferably about 30 wt .-% comminuted pulp and about 70 wt .-% water with enzyme based on the total weight of the mixture comprising the crushed pulp, the water and the enzyme. The dispersion of the dry, pre-shredded pulp in a mixture of water and an enzyme can be carried out in a continuous mixer, in particular in an extruder preferably having three sections (continuous), or in a reaction vessel (discontinuous), such as a Henschel mixer. In the case of an extruder with three sections, the first section advantageously has a starting temperature of 15-40 ° C., in the second section for activating the enzyme a temperature of 40-60 ° C. and in the third section for deactivating the enzyme a temperature of 60-90 ° C ago. When using an enzyme, a faster production of the end product, in particular the comminution mixture, can be achieved with a lower expenditure of energy.

Alternatively, a chemical treatment of the dry, pre-shredded pulp and subsequent dispersion of the treated pulp in the liquid, such as preferably water, with a device for mixing, such as a homogenizer, are performed. The chemical treatment may be, in particular, TEMPO oxidation, carboxymethylation, phosphoric acid treatment, pretreatment in a mixture of water and N-methylmorpholine N-oxide, pretreatment in alkaline solutions, e.g. Sodium hydroxide to a pretreatment in acidic solutions such. Sulfuric acid to a pretreatment with oxidizing agents such. Ozone, hydrogen peroxide, oxygen, peroxyacetic acid or hypochlorites and / or pretreatment with reducing agents, e.g. Sodium thiosulfate, sodium sulfite or sodium borohydride.

The fine comminution results in a mixture of the liquid and the fiber material with the micro-scale and / or nanoscale fibril agglomerates, ie the fine comminution mixture. In particular, if the liquid of the comminution mixture is water or comprises water, the microscale and / or nanoscale fibril agglomerates are present in the liquid in associated form. Associated form means that the micro-scale and / or nanoscale fibril agglomerates bind to each other. In particular, a fine comminution mixture comprising water and the associated micro-scale and / or nanoscale fibril agglomerates offers the advantage that this fine-particle comminution mixture, in particular the micro-scale and / or nanoscale Fibrillenagglomerate, other substances, such as substances that are used in the manufacture of cosmetic products, absorb well, store and release again. In addition, the strength of the association of the micro-scale and / or nanoscale fibril agglomerates can be influenced in a defined manner and thus the properties, in particular the viscosity of the comminution mixture, can be influenced in a defined manner.

The method preferably has the further step that the comminution mixture obtained after comminution comprising the liquid and the fiber material with the microscale and / or nanoscale Fibrillenagglomeraten, thermally, such as by spray drying, and / or under reduced pressure, or mechanically, such as by Filtration, sedimentation in the gravitational field or centrifugation is dried, so that a dried mixture results, in which preferably the solids content in a range of 70 wt .-% - 100 wt .-%, more preferably 80 wt .-% - 97 wt. %, more preferably from 85% to 95% by weight, based on the total weight of the dried mixture. The drying is preferably carried out by means of vacuum or mechanically or by spray drying, since these types of drying are particularly gentle.

The method preferably comprises the further step of re-adding the same or another liquid to the dried mixture to result in a remoistened mixture, the re-wetted mixture preferably having a solids content of at most 40% by weight based on the total weight of the remoistened mixture having. Such a mixture can be used particularly well for the production of a food, cosmetic product or a pharmaceutical product. The liquid added to the dried mixture to obtain the remoistened mixture can be water or any other liquid.

Advantageously, at least one of the substances selected from the group comprising pulp, dry, pre-shredded pulp, dispersion comprising the pre-shredded pulp, comminution mixture, dry mixture, remoistened mixture is added in an additional process step at least one dry substance, preferably blended. Advantageously, this dry substance is a component of a material which is produced using the comminution mixture, the dry mixture or the remoistened mixture. For example, such a dry substance may be a pharmaceutically active substance if the comminution mixture, dry mixture, or remoistened mixture is to be used to make a pharmaceutical product. Advantageously, at least one of the substances selected from the group comprising dry, pre-shredded pulp, dispersion comprising the pre-shredded pulp, fine comminution mixture, dry mixture, remoistened mixture, added in an additional process step, at least one functional liquid, which optionally solids, added, preferably admixed. This functional liquid advantageously exhibits an effect during the process according to the invention or advantageously in the material which is produced using the comminution mixture, the dry mixture or the remoistened mixture, an effect. A functional fluid which exhibits an effect in the material thus becomes part of this material. For example, flavoring agents in the form of liquids are used in food production. Thus, a liquid comprising flavors can be used as the functional liquid and thus added, for example, to the dry, pre-shredded pulp, the dispersion comprising the pre-shredded pulp, the comminution mixture, the dry blend, the re-wetted blend. Such a functional fluid may for example also be a dye.

The present invention also relates to a material, such as, in particular, a comminution mixture, a dried mixture or a remoistened mixture, which is prepared according to the method indicated above. The material has microscale and / or nanoscale fibril agglomerates and is preferably substantially free, more preferably completely free, of visible individual fibrils. The material which is the comminution mixture, the dried mixture or the remoistened mixture can be used, for example, each as an ideal base for the production of a food, a cosmetic product or a pharmaceutical product, since the material, in particular the micro-scale and / or nanoscale Fibrillenagglomerate, which are optionally associated with each other, well absorb substances, store and optionally return. By being substantially free, more preferably completely free, of visible individual fibrils, the material has advantageous properties for various applications, especially since the surface area of the material is very high due to the fibril agglomerates. Thus, when using the material in cosmetic products, for example, results in a particularly pleasant, especially supple and silk-like sensation on the skin. Preferably, the microscale and / or nanoscale fibril agglomerates of the fiber material, which is contained in the comminution mixture, are largely free, especially completely free of visible individual fibrils. More preferably, the fibrous material contained in the comminution mixture is substantially free, more preferably completely free, of visible individual fibrils. Most preferably, the comminution mixture is substantially free, particularly completely free, of visible individual fibrils.

Preferably, the microscale and / or nanoscale fibril agglomerates of the fiber material contained in the dried mixture are substantially free, especially completely free of visible individual fibrils. More preferably, the fiber material contained in the dried mixture is substantially free, especially completely free, of visible individual fibrils. Most preferably, the dried mixture is substantially free, especially completely free, of visible individual fibrils.

The microscale and / or nanoscale fibril agglomerates of the fiber material which is contained in the remoistened mixture are preferably substantially free, in particular completely free of visible individual fibrils. More preferably, the fiber material contained in the remoistened mixture is substantially free, especially completely free, of visible individual fibrils. Most preferably, the remoistened mixture is substantially free, especially completely free, of visible individual fibrils.

The substantial freedom or freedom of visible individual fibrils has the advantage of reducing the risk of clogging the devices for processing the comminution mixture, dried mixture and remoistened mixture.

The comminution mixture, the dried mixture and the remoistened mixture, each comprising the fiber material with the microscale and / or nanoscale fibril agglomerates, are preferably used as agents for effecting a rheology change in materials, such as, in particular, flowable materials, such as liquids for influencing the flexibility of materials, as a means for reinforcing materials, as a means for filling pores of materials, as a means for influencing the roughness of the surface of materials, as a means for absorbing and storing liquids such as a sponge, as a means for Influencing the texture of materials or as means for influencing the uptake and / or the storage and / or the dispensing of liquids and / or solids of materials, in particular as an agent contained in the material, which is used as Trä Substance for fragrances and / or flavors.

The present invention further relates to the use of the comminution mixture prepared according to the above-mentioned method, to the use of the dried mixture prepared according to the above-mentioned method and to the use of the remoistened mixture prepared according to the above-mentioned method for the production of an insulating element, which electrical insulation of an electrical component is used. It has been recognized that the blends prepared according to the above-mentioned process are optimally suited for the production of insulating elements with such an application.

Furthermore, the present invention relates to the use of the comminution mixture prepared according to the above-mentioned method, to the use of the dried mixture prepared according to the above-mentioned method and the remoistened mixture prepared according to the above-mentioned method for the production of a cosmetic product. The mixtures prepared according to the method mentioned above are particularly advantageous for the production of cosmetic products, in particular due to the resulting skin sensation. Furthermore, the present invention relates to the use of the comminution mixture prepared according to the above-mentioned method, to the use of the dried mixture prepared according to the above-mentioned method, and to the use of the remoistened mixture prepared according to the above-mentioned method for the production of a foodstuff. The mixtures prepared according to the above-mentioned method are particularly advantageous for the production of food.

Furthermore, the present invention relates to the use of the comminution mixture prepared according to the above-mentioned method, the dried mixture prepared according to the above-mentioned method and the remoistened mixture prepared according to the above-mentioned method for the production of a pharmaceutical product. The mixtures prepared according to the method mentioned above are particularly advantageous for the production of pharmaceutical products. The fine grinding mixture, the dried mixture and the remoistened mixture prepared by the above-mentioned method may further For example, in the production of the following materials are used: banknotes, paper, cardboard, concrete, cement, absorbent materials, paints, adhesives, insulating panels, composites, textiles, plastics, fillers, biotechnological products, detergents, perfume, bandages, such as paving.

The invention further relates to a material, such as the comminution mixture produced according to the invention, the dried mixture produced according to the invention or the re-bonded mixture prepared according to the invention, the material having micro-scale and / or nanoscale fibril agglomerates, in particular fiber material with micro- and / or nanoscale fibril agglomerates, and wherein the material is preferably substantially free, more preferably completely free, of visible individual fibrils. The material, which may also be an end product, such as an electrotechnical insulation element, a cosmetic product or a mid-life, is characterized in particular by the fact that in the cell structure of the pulp fibers due to the inventive manufacturing process much less metal particles or a much less pronounced greyish discoloration occurs than is the case with the usual prior art materials of the prior art.

BRIEF DESCRIPTION OF THE DRAWINGS

Preferred embodiments of the invention will be described below with reference to the drawings, which are given by way of illustration only and are not to be interpreted as limiting. In the drawings: FIG. 1 shows a flow chart for illustrating a method according to the invention;

FIG. 2a shows an electron microscope with an enlargement factor of

10Ό00 created view of a fibrillated pulp, which was prepared by a method of the prior art;

FIG. 2b shows an electron microscope with an enlargement factor of

10Ό00 created view of a part of a micro-scale Fibrillenagglomerates prepared by a method according to the invention; such as

3 shows an exemplary representation of microsized fibril agglomerates which are contained in the fiber material, which is produced by means of a method according to the invention. DESCRIPTION OF PREFERRED EMBODIMENTS

FIG. 1 shows a flowchart which illustrates the individual method steps of a method according to the invention.

As the original starting material, wood la or annual plants 1b or a combination thereof may be used. As the original starting material for the production of the dry, pre-shredded pulp or in particular for the preparation of pulp plates or the flash-dried pulp, also fruits, such as citrus fruits or apples, cereals, such as wheat or corn, grass or fiber-containing vegetables, such as For example, peas, legumes or carrots. The production of pulp from fruits, cereals, grass or fiber-containing vegetables is known to the person skilled in the art. The wood 1a or the annual plants 1b are processed into pulp 3a or 3b according to a process known to those skilled in the art. The pulp 3a or 3b are preferably pulp plates or flash-dried pulp.

When using wood l a as the starting material this is first crushed into chips 2a or wood chips. The chips 2a are then further processed into pulp 3a, wherein the pulp 3a may be, for example, pulp plates, flash-dried pulp or some other form of pulp. By further processing the chips 2a to pulp 3a, the wood is delignified and defibrated, that is, the fibers are dissolved out of the wood composite. At the same time an increase in the degree of whiteness can be effected in the further processing to the pulp 3a.

The further processing of the chips 2a to the pulp 3a can be accomplished by a purely mechanical treatment of the chips 2a. However, the mechanical treatment can also be combined with a chemical treatment of the chips 2a. Alternatively, the further processing of the chips 2a to pulp can also be based on a purely chemical treatment.

If a chemical treatment of the chips 2a is carried out, for example, sulfate, sulfite and / or S0 ₂ and ethanol can be used for this purpose. The chemical treatment may in particular be an ASAM (alkaline sulphite process with anthraquinone and methanol), an Organosolv, an AIcell, an Acetosolv, an Acetocell, a Formacell or a Milox process. It is also possible to carry out a steam explosion. If the pulp 3a or 3b are pulp plates, they are preferably substantially completely or at least predominantly made up of fibers having an average length in the range of 0.6-6 mm, the fiber length preferably being in accordance with the ISO standard 13322-2, 1st edition of 1.1 1.2006. The water content of the pulp plate is preferably at most 15% by weight, more preferably at most 10% by weight, still more preferably 1% by weight to 9% by weight, most preferably 5% by weight to 8% by weight on the total weight of the pulp board, in the case of preferred measurement of the water content in accordance with standard EN 20638 of September 1993. If the pulp 3a or 3b is flash-dried pulp, it is preferably formed essentially completely or at least predominantly from fibers, which have an average length of 0.6-6 mm, wherein the average fiber length is preferably measured according to the standard TAPPI T271 pm -91 from 1991. The water content of the flash-dried pulp is preferably at most 15% by weight, more preferably at most 10% by weight, even more preferably 1-9% by weight, most preferably 5-8% by weight, based on the total weight of the flash-dried pulp. with preferred measurement of the water content according to the standard EN 20638 of September 1993. To facilitate the handling, the flash-dried pulp is preferably in the form of bales. The pulp 3a or 3b may, for example, be a bleached softwood pulp, a bleached eucalyptus pulp or a pulp obtained from cotton. It is thus possible in particular to use softwood pulp and / or hardwood pulp. The pulp 3a or 3b obtained from wood 1 a and / or from annual plants 1 b is then fed to coarse pre-shredding 4. In the coarse pre-shredding 4, pulp 3a based on wood 1a or pulp 3b based on annual lb, or a combination thereof in the form of pulp plates, flash-dried pulp or other form of pulp or a combination thereof can be used.

For the coarse pre-shredding 4, the pulp 3a and / or 3b is used in the dry state. By the dry state it is meant that the pulp 3a or 3b has a moisture usual for pulp, which means that it has no substantial liquid additions. For example, the pulp 3a, 3b in the dry state have a water content of 7 wt .-% based on the total weight of the pulp. Slight additions of liquids may be present, but not those which overly reduce the total weight of the pulp, that is, by more than 15% by weight, preferably by more than 10% by weight, more preferably by more than 5% by weight. The pulp 3a, 3b is considered not to be dry, especially when dispersed in a liquid. Substantially no liquid, preferably no liquid, is added to the pulp 3a or 3b before the coarse pre-shredding 4, but during the pre-shredding 4 it furthermore has a water content of approximately 7% by weight, preferably 7% by weight. based on the total weight of the pulp. Advantageously, the dry pulp 3a or 3b is fed directly to the coarse pre-shredding 4 without any pretreatment. If pulp plates are used, the coarse pre-shredding 4 can be carried out, for example, by means of a fine mill (dry mill), a cutting mill, a hammer mill, a mixer and / or an impact mill. If flash-dried pulp is used, for example, a shredder, a granulator and / or a hammer mill may be used. As a rule, the apparatus used for coarse pre-shredding 4 has cutting blades or other shredding tools made of a metal.

So no pulper is used for the entire process and in particular the pre-shredding 4. In most cases, moreover, a single passage of the pulp through the apparatus required for pre-shredding 4, that is, for example, the mill, is sufficient. The process time for pre-shredding the pulp is thus relatively short.

After completion of the coarse pre-shredding 4, the pulp is preferably in the form of a powder, ie a bulk material before. The water content of the pre-shredded pulp is not greater than that of the pulp 3a or 3b prior to the pre-shredding. As a rule, the water content of the pulp before and after the pre-shredding 4 is approximately the same.

The mean fiber length of the pulp after the dry pre-shredding 4 is preferably in the range of 0.025 mm - 6 mm, more preferably in the range of 0.4 - 1.7 mm. The mean fiber length is preferably determined according to the TAPPI T271 pm-91 standard from 1991. By pre-shredding 4, the fiber length of the pulp is preferably shortened by a multiple, in particular by about three times, on average.

The pulp present after this process step, that is to say the pre-shredding 4, is particularly well suited for storage and transport. It is therefore very possible, the process steps from the original starting material 1 or lb to and with the coarse pre-shredding 4 on the one hand and the method steps described below with a Pretreatment 5 and a fine comminution 6 on the other hand temporally and / or locally separate from each other. It is thereby also possible, in particular, for example, for the rough pre-shredding to be carried out by a first company, for the dry, pre-shredded pulp obtained thereby to be stored over a period of up to six months, for example in the form of pellets, and for the pretreatment to be carried out as well as the fine comminution 6 are then carried out by a second company at a different location.

The dry, roughly pre-shredded pulp is then fed to the pretreatment 5. In this case, the pulp is dispersed in a liquid which may, for example, be water, in particular pure tap water or chemically distilled water. Alternatively, for example, dispersion in a liquid such as acetone, glycol, ethanol, chloroform, isopropanol or in water to which an enzyme (e.g., cellulase: endo-l, 4-.beta.-glucanase) has previously been incorporated is also possible. Preferably, the liquid has a boiling point of 100 ° C or less, preferably less than 100 ° C. In addition, the boiling point of the liquid is preferably at least 50 ° C. Most preferably, the boiling point of the liquid is in the range of 50 ° C - 90 ° C, at atmospheric pressure (101325 Pascals). This has the advantage that the liquid can be gently removed from the fiber material, in particular can be removed gently, without the fiber material being damaged. A chemical treatment of the pulp, for example based on a TEMPO oxidation, a carboxymethylation or a phosphoric acid treatment with subsequent dispersion in a liquid such as water, acetone, glycol, ethanol, chloroform or isopropanol is possible. The proportion by weight of the liquid in the dispersion is in all processes except those with the enzyme, preferably at least 60 wt .-%, more preferably at least 80 wt .-%, more preferably in a range of 90 wt .-% - 99 wt .-%, more preferably in a range of 94 wt .-% - 98 wt .-% based on the total weight of the dispersion. The solids content of the dispersion is preferably measured according to the standard ISO 41 19: 1995. When the pulp is dispersed in water with added enzyme, the weight fraction of the pulp in the liquid is preferably about 30% by weight, based on the total weight of the dispersion.

After the pretreatment 5, the pulp dispersed in the liquid or the dispersion of the fine comminution 6 is supplied. This takes place, for example, in a refiner, a ball mill, a homogenizer, an ultrasonic device, a microfluidizer, a jet collision device and / or a cryocrushing device instead. Particularly preferred is the use of a Refmers comprising a cutting material made of a mineral material. In principle, the use of a refiner with cutting means made of metal is possible for the fine comminution, which is disadvantageous in many cases, however, because very fine knives are required for this and often not all fibers are detected by the knives. In addition, there is the risk of metal abrasion and thus the risk that metal particles get into the fiber material to be produced with the micro-scale and / or nanoscale Fibrillenagglomeraten and thus in the material to be produced using the fiber material. In materials, such as foods, pharmaceutical products, cosmetics or insulation elements, which serve for electrical insulation of an electrical component, which are produced using the fiber material according to the invention, metal particles are undesirable.

Advantageously, the same grinding media are used for the entire comminution 6. This is possible because the pulp fibers are already very short due to the dry pre-shredding 4 and have a narrow fiber length distribution.

As the end product of the fine comminution 6, the comminution mixture comprising the fiber material with the micro-scale and / or nanoscale fibril agglomerates is present. The water content of the comminution mixture preferably corresponds substantially, more preferably exactly to the water content of the dispersion before comminution. The fibril agglomerates are each formed by a plurality of partially or wholly separate individual microfibrils. The average length of the microscale Fibrillenagglomerate is preferably in the range of 500 nm - 1000 μιη, more preferably in the range of 500 nm - 600 ^μι η, and more preferably in the range of 500 nm - 200 μιη, said lengths according to the standard ISO 13322- 2, 1st edition of 1.1 1.2006.

FIG. 3 shows by way of example several microscale fibril agglomerates which are contained in the fiber material, which is produced by a method according to the invention.

FIG. 2b shows, by way of example, a view of a part of a microscale fibril agglomerate produced by means of a method according to the invention by means of an electron microscope at an enlargement factor of 10Ό00. Good to see is the typical network structure with the interconnected, crushed fibrils within a Fibrillenagglomerats. The fibril agglomerate is largely, in the section shown in FIG. 2b, even completely free of visible individual fibrils These are present only in each shredded form and are also involved in the forming the Fibrillenagglomerate networks. By way of comparison, FIG. 2a shows, with the same magnification factor, a pulp produced by a prior art process. The individual fibrils are clearly recognizable here and do not form a common network, but are unconnected and do not form a common structure.

Subsequent to the fine comminution 6, the comminution mixture can be dried, for example, thermally or mechanically or under the action of reduced pressure, or liquid can be withdrawn, wherein the thermal drying is preferably carried out under reduced pressure. For example, the comminution mixture may be dried to result in a dried mixture in which the solids content is preferably in a range of 70% to 100% by weight, more preferably in a range of 80% to 97% by weight. %, more preferably in a range of 85 wt .-% - 95 wt .-%, based on the total weight of the dried mixture. The dried mixture is particularly suitable for storage and transport.

In a further possible step, liquid may be added to the dried mixture again to give a remoistened mixture which preferably has a solids content in the range of greater than 0% by weight to 40% by weight, based on the total weight of the remoistened mixture. For example, what is added to a liquid for rewetting the dried mixture depends on what kind of material is to be made by means of the remoistened mixture.

Both the comminution mixture, the dried mixture and the remoistened mixture may be used in the production of a material such as a food, an osmetikproduktes or even a pharmaceutical product. Of course, the comminution mixture, the dried mixture and the remoistened mixture can be used in the production of many other materials.

REFERENCE LIST l a Feedstock Wood 3b Pulp

1 b starting material annual plant 4 coarse pre-shredding

2a wood chips 5 pretreatment

3a pulp 6 fine comminution

Claims

1. A process for the production of microscale and / or nanoscale fiber material, comprising at least the following process steps:

Mechanically pre-shredding (4) pulp substantially without adding a liquid, preferably without adding a liquid, so that the mean fiber length of the pulp is in the range of 0.025 mm-6 mm, in particular 0.4 mm-1.7 mm;

- dispersing (5) the dry, mechanically pre-shredded pulp in a liquid; such as

- Finely comminuting (6) the pulp dispersed in the liquid such that a fine comminution mixture is formed, which contains the liquid and the fiber material with micro-scale and / or nanoscale Fibrillenagglomeraten.

2. The method of claim 1, wherein the fine crushing (6) is performed mechanically by means of a mineral material.

3. The method according to claim 1 or 2, wherein the average fiber length of the pulp used for the pre-crushing (4) in the range of 0.6 mm - 6 mm.

4. The method according to any one of the preceding claims, wherein the pulp is used in the form of pulp plates and / or flash-dried pulp as a raw material for the pre-crushing.

5. The method according to any one of the preceding claims, wherein the pre-shredded pulp before dispersing (5) compacted in the liquid, in particular pelleted and / or briquetted, is.

6. The method according to any one of the preceding claims, wherein the dry, pre-shredded pulp has a water content of at most 15 wt .-%, preferably of at most 10 wt .-%, more preferably 1-9 wt .-%, most preferably of 5 wt .-% - 8 wt .-%, based on the total weight of the dry, pre-shredded pulp having.

7. The method according to any one of the preceding claims, wherein the fiber material is a Forming solids content of the comminution mixture resulting from the comminution of at most 40 wt .-% based on the total weight of the comminution mixture.

8. The method according to any one of the preceding claims, wherein the average length of the microscale Fibrillenagglomerate in the range of 500 nm - 1000 μηι, preferably from 500 nm - 600 μιη, more preferably from 500 nm - 200 μιη, and / or the average length of nanoscale fibril agglomerates in the range of 10 nm to 500 nm.

9. A process according to any one of the preceding claims, wherein the dispersion resulting from dispersing the dry, pre-shredded pulp in a liquid in comminution (6) has a liquid content of at least 60% by weight, preferably at least 80% by weight, more preferably 90 wt .-% - 99 wt .-%, more preferably from 94 wt .-% - 98 wt .-%, based on the total weight of the dispersion having.

10. The method according to any one of the preceding claims, wherein the comminution mixture is substantially free, preferably completely free, of visible individual fibrils.

1 1. The method according to any one of the preceding claims, wherein the fine comminution mixture resulting from the fine crushing (6) is dried in a further process step, preferably thermally or mechanically dried or under application of negative pressure, so that a dried mixture results, in which preferably Solids content in a range of 70% by weight to 100% by weight, more preferably 80% by weight to 97% by weight, even more preferably 85% by weight to 95% by weight, based on the total weight the dried mixture is.

12. The method of claim 1 1, wherein the dried mixture is substantially free, preferably completely free, of visible individual fibrils.

13. The method of claim 1 1 or 12, wherein the dried mixture is added again in a further process step the same or another liquid, so that a remoistened mixture results, wherein the remoistened mixture preferably has a solids content of at most 40 wt .-% based on the total weight of the remoistened mixture.

14. The method of claim 13, wherein the remoistened mixture is substantially free, preferably completely free, of visible individual fibrils

15. Use of the comminution mixture according to any one of claims 1 to 10 or the dried mixture according to any one of claims 1 1 or 12 or the remoistened mixture according to any one of claims 13 or 14 for the preparation of an insulating element, which serves for electrical insulation of an electrical component.

16. Use of the comminution mixture according to any one of claims 1 to 10 or the dried mixture according to any one of claims 1 1 or 12 or the remoistened mixture according to any one of claims 13 or 14 for the preparation of a material which is a cosmetic product or a pharmaceutical product or a food is.

17. Material comprising fiber material with micro-scale and / or nanoscale Fibrillenagglomeraten, wherein the fiber material is prepared by a method according to any one of claims 1-14, wherein the material is preferably substantially free, more preferably completely free, of visible individual fibrils.

18. A material according to claim 17, wherein the material is the comminution mixture prepared according to any one of the methods set forth in claims 1 to 10, the dried mixture prepared according to one of the processes recited in claims 11 or 12 or the remoistened mixture prepared according to one of the specified in claims 13 or 14 method.