EP3599893A1 - Desintegrierte und dekompaktierte cellulose-basierte pflanzenfaserstoffe. verwendung und verfahren zur gewinnung und herstellung - Google Patents
Desintegrierte und dekompaktierte cellulose-basierte pflanzenfaserstoffe. verwendung und verfahren zur gewinnung und herstellungInfo
- Publication number
- EP3599893A1 EP3599893A1 EP18712260.1A EP18712260A EP3599893A1 EP 3599893 A1 EP3599893 A1 EP 3599893A1 EP 18712260 A EP18712260 A EP 18712260A EP 3599893 A1 EP3599893 A1 EP 3599893A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- cellulose
- based fibers
- water
- fibers
- compounds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2250/00—Food ingredients
- A23V2250/50—Polysaccharides, gums
- A23V2250/51—Polysaccharide
- A23V2250/5108—Cellulose
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N2533/00—Supports or coatings for cell culture, characterised by material
- C12N2533/70—Polysaccharides
- C12N2533/78—Cellulose
Definitions
- Disintegrated and dekompacted cellulose-based plant fiber Use and process for extraction and production.
- Fiber is a group of food components that can not or only to a small extent be digested and absorbed in the human digestive tract. This may be inorganic material, e.g. Clays or other minerals or complex-bound organic material, such. As lignin-based shells act.
- indigestible fiber in plant foods consists of polymeric carbohydrates that are not digested and absorbed by the carnivore's digestive tract. Even if a diet is chosen that largely consists of vegetables, the recommended consumption of dietary fiber is not possible or only at the expense of an increased calorie intake.
- swelling agents are offered, such as psyllium husks, which have a high water-binding capacity but have only a low calorific value.
- the supply of an amount of these swelling agents which ensures an adequate and soft stool consistency, can hardly be implemented in practice, since a swelling that accompanies the formation of slime, leads to an unpleasant mouthfeel.
- cellulose products are offered and already used for food preparation.
- Such cellulose products are obtained according to the prior art from a digestion of wood or woody convincedma- materials.
- cellulose products which have been chemically digested and / or modified and as cellulose derivatives, which are also referred to below as cellulose ethers or cellulose preparations, are offered with a defined molecular weight and geometric dimensions, of such cellulose products by grinding of Stängelmasse or Spel - have been made zen, which are called cellulose fibers in the following.
- Cellulose is the most abundant biopolymer on earth. It is synthesized by plants and essentially serves to support and stabilize the entire organism of the plants, for which purpose these polymers are combined in parallel fibrils and are cross-linked with each other and are usually present over long distances as a continuous macromolecule. In addition, these linear structural and holding filaments are subdivided by an enclosing lignin-based release layer, which on the one hand a strong hydrophobicity and thus protection against dissolution, z. As by decay, and on the other hand, the structural stability of the enclosed cellulose fiber bundles considerably increased.
- a digestion of cellulose eg., for the purpose of pulp or papermaking, dissolution and removal of the lignin by known wet-chemical digestion methods, such as the Kraft method performed. From the wood pulp fibrillar cellulose fibers are obtained, which have only a low swelling capacity.
- Cellulose is a polymer which, as a homopolysaccharide, is composed of 1-> 4- ⁇ -glucosidically linked anhydro-D-glucose units and is thus water-insoluble and has hydrophobic properties owing to its structural structure.
- derivatives of cellulose fibers are prepared by mechanically comminuting and hydrolyzing them, as well as by esterification of the hydroxy groups to water-soluble cellulose esters, cellulose acetates or cellulose nitrates. Depending on the degree of esterification, these have strongly hydrophilic to hydrophobic properties.
- Cellulose derivatives which have hydrophilic properties are completely dissolved in a water and, due to their large hydrodynamic diameter, already in small quantities cause a strong increase in the viscosity of the liquid in which they are dissolved. Only a few grams / liter in water are sufficient to produce a high-viscosity colloidal solution.
- methyl ethyl cellulose MEC
- HEMC hydroxyethylmethyl cellulose
- HPMC hydroxypropylmethyl cellulose
- MEC methyl ethyl cellulose
- HEMC hydroxyethylmethyl cellulose
- HPMC hydroxypropylmethyl cellulose
- tissue structures are also formed by plants, which are present in different compartments and functional units of plant structures and in this case bound or connect the functional or structural units.
- Such structural or functional units can, for.
- ZT are also minerals such as calcium or zinc or inorganic compounds such as sulfates or nitrogen-containing compounds and organic compounds such as free carboxylic acids, such as phytic acid, participate in complex formation / compaction responsible for the structural integrity of the various organic components.
- cellulose-based fibers differ chemically from cellulose fibers present in woody or woody plant materials and, depending on their place of origin and functionality, have different constituents or ligands with which they produce electrostatic or covalent bonds.
- cellulose-based fibers differ substantially in molecular dimensions and branching structure from cellulose fibers. It could be shown that both the spatial structures and the surface properties are of crucial importance for the resulting functional properties of such cellulose-based fibers.
- the cellulose-based fibers according to the invention thus differ structurally and chemically from cellulose fibers which can be obtained, for example, from a wood by a pulping process from the prior art.
- the cellulose-based fibers according to the invention fulfill functional tasks, for example in flowers, seeds or fruits of plants. It has been found that their proportion of the organic matter in which they are present, vary considerably can, for example, less than 5 wt%, z. B. in the pulp of a watermelon, to over 70Gew% in the stalk of some types of cabbage.
- cellulose-based fibers could not be separated in a large aqueous distribution volume, ie freed / decomposed from the other constituents of the plant, and drying or caking of the resulting mass took place, which proceeded only very slowly and allowed to hydrate for the most part incompletely again in an aqueous medium.
- the obtainable cellulose-based fibers are free or nearly free of water-soluble aroma and / or dyes which can be rinsed out into an aqueous medium. Furthermore, it surprisingly turned out that cornification of the cellulose-based fibers obtainable by one of the processes according to the invention does not take place or only to a small extent in a drying process if one of the processes according to the invention was used for the production of the cellulose-based fibers.
- a further object of the invention is to prepare and prepare cellulose-based vegetable fibers which are free of secondary substances and which do not emit any sensory-perceivable aroma substances or dyes into an aqueous medium. Furthermore, it is also the object of the invention to provide a method with which the cornification of cellulose-based fibers can be prevented or reduced or reversed.
- the object is achieved by the technical description and the examples of methods for obtaining and producing cellulose-based fibers by means of aqueous digestion solutions containing amino acids and / or peptides.
- the present invention therefore relates to digested, dekompaktiert, cellulose-based fibers obtained from a vegetable starting material, wherein the digested and dekompakt convinced cellulose-based fibers have an aspect ratio after swelling in water from longitudinal diameter to transverse diameter of 1: 1 to 1000: 1 and a water binding capacity of> 200% by weight and have a water retention capacity of> 50%.
- the present invention relates to a process for the production and preparation of digested decompactivated cellulose-based fibers, which process comprises the following steps: Providing a disintegrated or non-disintegrated plant starting material containing contacted cellulose-based fibers conjugated to at least one organic compound selected from:
- water-insoluble organic solids comprising lignin-rich shells
- step a separation of the digested, decompacted, cellulose-based fibers of step c1) of the water-insoluble organic solids
- the readily water-soluble organic compounds have a water solubility of> 100 g / L at 20 ° C., preferably> 140 g / L at 20 ° C. and the sparingly water-soluble organic compounds have a water solubility of ⁇ 100 g / L at 20 ° C, preferably of ⁇ 75 g / L at 20 ° C have.
- Polymers from non-digestible carbohydrates are the major constituent of non-absorbable fiber in the human diet. There is predominantly an insufficient intake of dietary fiber, which is due to the diet of the population of industrial nations due to modern food preparations.
- Cellulosic fibers derived from the digestion of lignocellulosic cellulose and the milling of stalks and husks of crops are also used in food preparations, but when exceeding an amount of more than 1-3% by weight, unwanted sensory sensations occur when eating such Food preparations and / or the quality of the food preparation is adversely affected. So conditionally z.
- Example 2 the interference of 2% by weight of hydroxy cellulose in a meatball preparation a strong thickening effect, which caused a disintegration of the preparation in the cooking or when used in a pudding preparation caused an unacceptable solidification of the product.
- cellulosic fibers from the grinding of stalk or husk mass with an addition of> 3 wt%, there was practically a regular perception of a farinaceous solid and a disturbed mouthfeel with a reduction in the perceptibility of aroma characteristics necessary for a qualitative evaluation of the preparation products are decisive. Due to the resulting volume and consistency, it was not possible to deliver more than 50% by weight of the daily fiber requirement of hydroxy or methyl cellulose preparations by addition to food
- the processes according to the invention for obtaining cellulose-based fibers have produced compacted and functional cellulose-based fibers which have extremely advantageous effects in the preparation of foodstuffs as well as on the human digestive system.
- digested, dekompaktator and functional cellulose-based plant fibers which are characterized by
- Absence of readily water-soluble carbohydrates and proteins Absence of the release of flavoring or coloring agents onto a water phase and obtainable from an aqueous disintegration and / or digestion and / or purification process.
- the cellulose-based fibers produced have adjustable properties, such as rapid hydrratability of dried cellulose-based fibers in water, surface properties that ensures interaction with different media or the uptake of microorganisms, which develop their biological activity therein , allows.
- the cellulose-based fibers produced according to the invention make it possible to obtain ideal conditions for inclusion / uptake of substances / compounds or microorganisms susceptible to drying out. It has been found that cellulose-based fibers produced in this way in a very advantageous manner spontaneously or without relevant technical effort substances / compounds or microorganisms attach to their surfaces or they can be attached or be included in the geometric structures / interiors. Due to the high water-binding capacity and the high water-holding capacity, the ingested compounds / substances / organisms have been protected from dehydration which inactivates or destroys such compounds / substances / organisms for considerably longer than is possible with preparations of the prior art, such as cellulose fibers.
- Nutrient media such as Gujar or Agiinaten
- the mass transfer which is necessary, for example, for the maintenance of a cell metabolism, was still possible with a binding / introduction to / in cellulose-based fibers produced according to the invention, while this was only to a significantly lesser degree or not at all for the other materials investigated Case was.
- the incorporated compounds / substances / organisms showed, even after 2 weeks of cool storage in a humid chamber, functionality or metabolic activity unchanged from the outlet, which was not possible when stored with preparations of the prior art.
- cellulose-based fibers prepared according to the invention are suitable for the attachment and / or incorporation of compounds / substances / organisms that are sensitive to desiccation in order to preserve them here and stabilize their integrity and functionality and to preserve.
- the cellulose-based fibers to / in which compounds / substances / organisms have been deposited / stored are very well suited for the preparation of foodstuffs.
- bakers' yeasts were shown to be stably placed in the interiors of the dekompacted cellulose-based fibers and had the same metabolic activity after 14 days of storage in a vessel under refrigerated conditions after reactivation as the same amount of yeasts at baseline.
- Non-digestible carbohydrates which also include the cellulosic fibers of the present invention, account for the major component of the amount of fiber in the average human diet.
- Non-digestible means that these compounds can not be cleaved by enzymes of the human gastrointestinal tract, such as amylases, and thus cleaved into C-6-sugar compounds that are absorbable.
- the cellulose-based fibers remain essentially as unchanged components in the intestinal contents and thus become part of the stool.
- their ability to bind water they gain importance as an important regulator of the consistency of the colon content.
- the water binding capacity of the intestinal contents also determines the passage time of the feces produced in the colon.
- Short-chain fatty acids or phytosterols that are produced or released from the breakdown of complex carbohydrates and can pass through the colon wall. It is therefore strongly recommended by the World Health Associations and the FDA to consume fiber at a dry matter level of 30 g per day. This goal is not achieved in the vast majority of the forms of nutrition practiced in the industrialized nations as well as in the emerging economies. There is an inverse correlation between dietary fiber consumption and the incidence and severity of obesity and diabetes mellitus, as well as with it mortality. However, a practical feasibility of the recommendations on dietary fiber content of the diet can be for different reasons, such. As a lack of employment or an implied social behavior, in spite of all known information and explanations not enforce. Also, country-policy appeals to the food industry have remained without sustainable effect in view of the low selection of fiber from the state of the art and the demands made on the sensory properties of the product by consumers.
- the cellulose-based fibers obtained and produced according to the invention are outstandingly suitable for completely covering the daily requirement of dietary fiber, which should be supplied with human food intake. It could be shown in practical application that both the daily requirement of fiber by the sole supply of cellulose-based fibers according to the invention, as well as by an additive addition of these to a normal diet, practicable and perform for the consumer in an acceptable form leaves.
- an otherwise fiber-free diet has been prepared by using the produced cellulosic-based fibers (28-36 g daily weight) together with proteins and minerals and as exclusive food in a satiety amount of subjects over a 4 week period were consumed.
- the food preparation was rated good or very good by all participants and did not lead to any unwanted by-effects. However, it was registered in all participants a weight reduction of 5.3 kg on average, despite a subjectively perceived as sufficient and satisfying food intake.
- TG 15g
- the practicability of use was of the cellulose-based fibers and the qualitative / sensory properties of the food prepared therewith have been rated as good to very good. Also in the participants of this study, an unintentional weight loss of 3.2 kg occurred on average.
- participant suffering from chronic constipation received cellulose-based fibers or cellulosic fibers prepared according to the invention over a period of 14 days in an amount between 8 and 15 g (TG) per day as an admixture to a common diet .
- Participants taking the manufactured cellulose-based fibers increased stool frequency and softening of stool consistency after 3 days, which continued over time. All participants rated the addition of the cellulose-based fibers as practicable and pleasant.
- a significant weight reduction of 900g was documented among the study participants.
- the participation of people taking cellulose supplements was prematurely stopped in 30%.
- a positive effect on the stool frequency or stool consistency was reported by 12% of the participants; 56% of the participants reported no relevant effect and 32% of the participants reported an undesired effect (in particular an increase in stool consistency). There was no weight reduction.
- cellulose-based fibers produced according to the invention By cellulose-based fibers, which are A blowing agent, such as yeast or sodium bicarbonate were coated on the inner surfaces, an increase in the baking volume and a more uniform distribution of the air chambers formed could be effected. At the same time, the dough, which was made with the cellulose-based fibers, had a higher pressure stability and compared to the reference recipe gave a better mouthfeel and a more harmonious taste impression.
- cellulose-based fibers produced according to the invention can be used as a fat substitute in food preparations.
- at least 50% by weight of the amount of fats and oils can be reduced to achieve the same preparation volume and equivalent or better sensory and qualitative characteristics, as is the case with preparations with the otherwise usual amount of fats or oils.
- polymeric carbohydrates is understood to mean cyclic C-6 compounds which are linked to polymers 1-> 4-.beta.-glucosidically and can not be cleaved by enzymes of the human organism or only in small amounts. They are therefore not split in the digestive tract of men and carnivores and thus excreted undigested again with the chair.
- aqueous solutions in which amino acids and / or peptides are dissolved are rapidly and completely disintegrated from non-woody vegetable starting materials, such as press residues of seeds and grains or ground products, such as flour from grains or cores or from the pulp or the disintegrated organic mass of vegetables or fruits or tubers in which the above-mentioned constituents are present together in a dense / compacted composite, are taken up and hydrated so that subsequently a complete separation of the various constituents is made possible.
- non-woody vegetable starting materials such as press residues of seeds and grains or ground products, such as flour from grains or cores or from the pulp or the disintegrated organic mass of vegetables or fruits or tubers in which the above-mentioned constituents are present together in a dense / compacted composite
- cellulose-based fibers have numerous side groups or functional groups and compounds whose compositions differ in specific species. For example, mass spectroscopic analysis showed that in addition to the elements carbon, oxygen and hydrogen, nitrogen, phosphorus, sulfur, sodium, chloride, calcium, magnesium, zinc, copper, iron, manganese and other elements are present in a variable proportion.
- the filigree, space-structuring, cellulosic, cellulose-based fibrous structures obtainable by the process according to the invention differ both chemically and in terms of their physical and performance properties of cellulose or of cellulose fibers or cellulose derivatives, for example from a digestion of Wood can be obtained or produced.
- the digestion solutions according to the invention preferably contain naturally occurring amino acids and / or peptides which consist of or contain these amino acids in a completely dissolved form in water.
- this is a solution of one, two or more amino acids (s) and / or peptides (s), in the individual and / or total concentration in a range of 10 ⁇ / ⁇ to 3mol / l, more preferably between 1 mmol / l and 1 mol / and more preferably between 0.1 mol / and 0.5 mol / l.
- These may be L- or D-forms or racemates. Preferred is the use of the L-form.
- the amino acids arginine, lysine, histidine and glutamine are particularly preferred. Particularly preferred are cationic amino acids and amino acid derivatives such as arginine and its derivatives.
- the peptides which can be used according to the invention may be di-, tri- and / or polypeptides.
- the peptides of the invention have at least one functional group that can bind or bind a proton.
- the preferred molecular weight is below 500 kDa, more preferably ⁇ 250 kDa, more preferably ⁇ 100 kDa and particularly preferably ⁇ 1000 dA.
- the preferred functional groups are in particular a gunanidine, amidine, amine, amide, ammonium, hydrazino, hydrazono, hydroxyimino or nitro group.
- the amino acids may have a single functional group or more of the same class of compounds or one or more functional group (s) of different classes of compounds.
- the amino acids and peptides according to the invention preferably have at least one positive charge group or have a positive total charge. Particularly preferred are peptides with cationic functional groups.
- a pH of the cationic amino acid or peptide solution ranges from 7 to 14, more preferably between 8 and 13, and more preferably between 8.5 and 12.5.
- the pH may be adjusted to any pH range between 6 and 14 by the addition of an acid or a base.
- Acids and bases known in the art may be used, such as caustic soda or HCl.
- Particularly preferred peptides contain at least one of the amino acids arginine, lysine, histidine and glutamine in any number and sequential order. Especially zugt are therefore amino acids and / or derivatives containing at least one guadinino and / or amidino group.
- the chemical radical H 2 NC (NH) -NH- and its cyclic forms is referred to as amidino and the chemical radical H 2 NC (NH) - and its cyclic forms.
- guanidino compounds which, in addition to the guanidino group, have at least one carboxylate group (-COOH). Further, it is preferable that the carboxylate group (s) is separated from the guanidino group in the molecule by at least one carbon atom.
- amidino compounds which, in addition to the amidino group, have at least one carboxylate group (-COOH). Further, it is preferable that the carboxylate group (s) is separated from the amidino group in the molecule by at least one carbon atom.
- di-, tri- or oligipeptides and polypeptides which are composed of one, two or more amino acids.
- peptides which have both hydrophobic and cationic and / or anionic side groups such as RDG, BCAA, NCR, HIS, SPR, EHP or SFA.
- Preference is given to a process in which aqueous solutions of one or more amino acid (s) and / or of one or more peptides are used for obtaining and / or producing cellulose-based fibers.
- step a1) and / or step b) has a pH of between 7 and 14.
- the aqueous solutions may contain adjuvants, such as e.g. Alcohols, antioxidants or surfactants.
- adjuvants such as e.g. Alcohols, antioxidants or surfactants.
- Preferred alcohols are methanol, ethanol, polyethylene glycol.
- Preferred surfactants are urea, thiourea, sodium lauryl sulfate and DMSO.
- Preference is given to a process for obtaining and producing cellulose-based fibers, in which a disintegration of the vegetable starting material takes place.
- poorly water-soluble organic compounds comprising complex carbohydrates; and or water-insoluble organic solids comprising lignin-rich shells.
- dekompakt cellulose-based fibers, which are obtained from a vegetable starting material containing, in addition to konnpakt striv cellulose-based fibers, at least one organic compound selected from:
- water-insoluble organic solids comprising lignin-rich shells.
- digested decompactivated cellulose-based fibers is from a disintegrated or non-disintegrated plant feedstock containing compacted cellulose based fibers compacted with at least one organic compound selected from:
- water-insoluble organic solids comprising lignin-rich shells
- a disintegration of plant starting material takes place with or together with an aqueous solution of one or more amino acid (s) and / or of one or more peptides.
- a disintegration by means of a thermal process such as. B. by heating the vegetable starting material in a water bath.
- the thermal disintegration takes place in an aqueous solution for disintegration or digestion of the starting material.
- a disintegration / digestion process can be applied, for example, to all vegetable raw materials that have a closed shell that can not be substantially penetrated by water. It is also used in vegetable starting materials, in which the cellulose-based fibers have thermolabile compounds with one another or with other structures, which can be identified by z. B. disintegrate a cooking process and thus be unlocked.
- disintegration and / or disruption of the tissue assemblies takes place following drying of the vegetable starting material.
- mechanical processes such as a denomination or a grinding, are preferred. This is advantageous because amino acid and / or peptide solutions can thereby be arranged more rapidly at the boundary layers within the vegetable starting material.
- Disintegration and / or disintegration and digestion of the vegetable starting material should preferably be provided whenever put the plant starting matehal in one of the amino acid and / or peptide solutions of the invention or applying them, a digestion and recovery of cellulose-based fibers is not or not completely possible.
- the amino acid and / or peptide solutions are preferably added in a mass ratio of between 0.3: 1 and 3: 1 to the vegetable starting material that can be penetrated by the solutions and mixed therewith, such that complete wetting / Impregnation of the organic starting material is ensured.
- it is also possible to select significantly larger volume ratios in particular if the constituents of the starting material detached from the cellulose-based fibers are to be dissolved and removed in an aqueous medium using this solution.
- a mixture is used to ensure complete penetration of the vegetable starting material.
- the temperature at which this takes place can be chosen freely, preferred are temperatures between 4 ° and 90 ° C., more preferably between 15 ° and 70 ° C.
- the duration of the penetration phase naturally depends on the type and nature of the vegetable starting material. Preferred is a duration between 5 minutes and 24 hours, more preferably between 10 minutes and 12 hours and more preferably between 20 minutes and 6 hours.
- a vegetable starting material which also contains lignin-based shell material will then have sufficient Separation of the vegetable starting material from the cellulose-based fibers when it comes to a mixing process in the water phase to rapid sedimentation of the lignin-rich shells and the macroscopically visible cellulose-based fibers have little or no tendency to sediment, with simultaneous absence of undissolved aggregates of the starting material.
- filtration of the suspension is carried out with a sieve, preferably a screen size of 0 , 2 to 0.6mm. After physical removal of unbound water, resuspension of the cellulose-based fibers in water occurs.
- aqueous digestion is carried out in step b): impregnation of the disintegrated plant starting material from step a) or saturation of the vegetable starting material from step a1) after thermal and / or mechanical and / or aqueous disintegration until reaching a Moisture content of greater than 20 wt.% And a complete hydration of the readily soluble organic compounds with an aqueous digestion solution of dissolved digestive substances containing at least one dissolved amino acid with a molar mass of less than 400 g / mol and a solubility of at least 35 g / L in water at 20 ° C and / or peptides from 2 to 50 of these amino acids to digest the konnpakt convinced cellulose-based fibers.
- the recovery of the cellulose-based fibers takes place by being freed from the other constituents of the vegetable starting material by a rinsing process.
- This rinsing process can be carried out, for example, by adding a sufficiently large volume of water to the batch.
- the addition volume ratio is more than 2: 1, more preferably> 4: 1, and most preferably> 10: 1.
- the required volume depends on whether the specification characteristics (see Methods) can be achieved for the available cellulose-based fibers, this can be easily determined by analytical methods.
- the digested, decompactivated cellulose-based fibers have a very high water-binding capacity, which is preferably> 100% by volume, more preferably> 150% by volume, more preferably> 200% by volume, even more preferably> 300% by volume and particularly preferably> 400% by volume. is.
- the volume of distribution can be increased and / or the distribution process is repeated in a further distribution process, after prior separation of the cellulose-based fibers. Therefore, the distribution process is done until the specification values are met.
- the distribution volume is preferably less than 500: 1, more preferably ⁇ 300: 1, further preferably ⁇ 150: 1, and further preferably ⁇ 20: 1. Preference is given to the use of an intensive mixer in this process step.
- step c1) is carried out:
- the rinse water is preferably removed by filtration. Particularly preferred is a filtration with a vibrating screen. Further preferred are bow screens and chamber filter presses. Also preferred is a separation of the rinse water with a decanter. Preference is given to a repetition of the rinsing process after removal of the free water phase from the cellulose-based fibers obtainable with one of the aforementioned techniques until the rinsing liquid is clear, colorless and odorless. In a further preferred embodiment, the batch is placed in a sieve or other space with porous boundaries and water is purged until the rinse water is clear and colorless. Surprisingly, it has been found that the cellulose-based fibers obtainable and / or preparable with the methods described herein are also low in taste and odor, or tasteless and odorless.
- the cellulose-based fibers according to the invention can be almost completely retained by a sieve having a sieve size which corresponds to a multiple of the mean diameter of the cellulose-based fibers. This is very likely due to a mutual entanglement of the complex spatial structures of the cellulose-based fibers obtained. This greatly simplifies the rinsing out of other components of the vegetable starting material.
- a pressing of the previously rinsed cellulose-based fibers takes place intermittently, as a result of which the amount of water required for complete rinsing of the cellulose-based fibers can be reduced.
- the rinsing process is complete and the cellulose-based fibers according to the invention are present when, after squeezing out of water, no dissolution of soluble constituents in a water phase occurs and the fibers show no or only a minimal tendency to sedimentation after suspension in water.
- the cellulose-based fibers produced according to the invention no flavoring substances or dyes are dissolved out in water which lead to a formation of taste or color.
- the decompacted cellulose-based fibers according to the invention are microscopically free of attaching others of the starting material and have three-dimensional spatial structures with empty interior spaces. These spatial structures have a coral or sponge-like shape. The size dimensions vary depending on the related plant source material.
- the cellulose-based fibers obtained according to the invention have the abovementioned specifications, especially when complete or almost complete separation of all readily water-soluble compounds has taken place.
- the preferred cellulose-based fibers have a content of slightly water-soluble carbohydrates, proteins and flavoring or coloring agents, preferably of ⁇ 3% by weight, more preferably of 2% by weight, more preferably of 1% by weight and even more preferably of 0.5% by weight. on.
- Preferred is a process in which digested, dekompaktABLE, cellulose-based fibers have a content of slightly water-soluble carbohydrates, proteins and flavoring or dyes of ⁇ 1% by weight.
- the disintegration / digestion process according to the invention allows in a very advantageous manner a very easy separability of digested, dekompacted cellulose-based fibers and other insoluble organic compounds.
- lignin-rich shells or husks or stalk materials which are not soluble by the process according to the invention and remain stable as solid solids are often present in the non-lignified starting materials.
- These solids usually have a much larger volume and / or a higher specific gravity than the cellulose-based fibers according to the invention. This allows easy separability of these insoluble organic solids with methods of the prior art.
- this filtration process for. B. by means of a vibrating or Bogensiebs or eddy current method, as is possible for example with a Hydrozyclon.
- methods based on a centrifugal acceleration may also be used.
- rieren, z. B. a Siebdekanter can be performed.
- step c2) the implementation of step c2) is preferred:
- step a separation of the digested, dekompakt striv, cellulose-based fibers of step c1) of the water-insoluble organic solids.
- step d1) the removal of the bound water fraction from the cellulose-based fibers is carried out by a physical process known from the prior art.
- the cellulose-based fibers which are obtained in a suspended form after process step c1) or c2) or c3) are made obtainable by a state-of-the-art filtration or centrifugal process. Preference is Siebdekanter or chamber filter presses. In an advantageous method embodiment, the obtainable fiber mass is also pressed out mechanically.
- the residual moisture content achievable depends on the process-specific requirements. It is preferred to remove the unbound and part of the bound water. Preferably, a residual moisture content of between 30 and 200% by weight, more preferably between 40 and 150% by weight and even more preferably between 45 and 120% by weight is achieved.
- step d1) takes place after step c1) or c2) or c3):
- the cellulose-based pulp is passed from a suspension to a porous material and thereby applied a uniform film of the cellulose-based fibers.
- the bound water can escape through the pores and, on the other hand, a gas stream, preferably of heated air, can be passed through.
- a gentle drying of the resulting cellulose-based fibers is achieved.
- the drying by heating, or the passage of a hot air is preferably carried out at a temperature between 15 ° and 1 10 ° C, more preferably between 20 ° and 90 ° C and more preferably between 35 ° and 75 ° C.
- the drying is carried out by a freeze and / or vacuum drying.
- spray drying is performed.
- prior art processes for drying the related cellulose-based fibers related Preference is given to thermal processes which involve drying at a low temperature, which is preferably ⁇ 150 ° C., more preferably ⁇ 120 ° C., more preferably ⁇ 100 ° C., even more preferably ⁇ 85 ° C. and particularly preferably ⁇ 70 ° C., enable. Also preferred are spray drying and vacuum drying. But also band / contact drying methods are preferred.
- a residual moisture content of the dried cellulose-based fibers is preferably between 8 and 35% by weight, more preferably between 10 and 30% by weight and more preferably between 12 and 25% by weight.
- step d2) Preference is given to a method in which, after step d1), step d2):
- a surface conditioning or functionalization process can be carried out in the optional process steps c3) and / or d3).
- the already digested and dekompaktiere mass cellolose-based fibers is provided in a dry, dried, damp or suspended form and mixed with one or more compounds / solutions / cultures and mixed with these.
- the appropriate process conditions must be determined specifically. Suitable compounds / microorganisms and the thereby obtainable properties of the conditioned / functionalized cellulose-based fibers are shown below.
- step c3) and / or d3) which takes place after step c1 or c2) or after step d1) and / or d2), is carried out for the conditioning / functionalization of cellulose-based fibers, comprising the steps:
- conditioning / functionalizing substances comprising amino acids and / or peptides, carboxylic acids, carbonates, alcohols, sugar compounds, cellulose ethers,
- step e) conditioned and / or functionalized, digested, dekompacted, cellulose-based fibers are obtained, the anti-static and / or have hygroscopic, hydrophilic or hydrophobic and / or conductive surface properties.
- the object of the invention the recovery of cellulose-based fibers, is accomplished by an aqueous process with which cellulose-based vegetable fibers can be obtained and produced.
- step a) disintegration of the vegetable starting material from step a) by a thermal and / or mechanical digestion process
- the aqueous digestion solution contains dissolved amino acids and / or peptides.
- step a1) disintegration of the plant of the plant starting material from step a) by a thermal and / or mechanical digestion process, b) impregnation of the disintegrated plant material from step a1) with an aqueous digestion solution containing dissolved amino acids and / or peptides,
- the object of the invention is therefore to provide digested decompacted cellulose-based fibers which, on the one hand, retain their natural physical properties and, on the other hand, are free from other readily soluble organic compounds and in particular from flavorings.
- step b) impregnation of the disintegrated plant material from step a) or a1) with an aqueous digestion solution containing dissolved amino acids and / or peptides, in which the at least one amino acid is a cationic amino acid and / or the at least a peptide contains at least one cationic amino acid.
- the at least one dissolved amino acid according to step b) has a molar mass in the range from 70 g / mol to 400 g / mol, preferably from 75 g / mol to 350 g / mol, more preferably from 100 g / mol to 320 g / mol, more preferably from 140 g / mol to 300 g / mol and / or a solubility of at least 75 g / L in water at 20 ° C, preferably of at least 100 g / L in water at 20 ° C and more preferably at least 140 g / L in water at 20 ° C and / or it is ⁇ , ß or ⁇ -amino acids and / or proteinogenic and / or non-proteinogenic amino acids.
- the water binding capacity and the water retention capacity are particularly high in a digestion process in which cationic amino acids were present in the aqueous digestion solution.
- the amino acids are arginine, lysine and histidine.
- Preference is given to a process in which cellulose-based fibers are obtained and obtained which are aroma-free. Preference is given to cellulose-based fibers which form three-dimensional spatial structures and contain no or only minimal amounts of readily soluble carbohydrates and / or proteins and / or flavorings and / or dyes.
- the method is just as applicable to starting vegetable materials in which impregnation with an aqueous solution is already possible and therefore disintegration is not required in order to make the cellulose-based fibers according to the invention obtainable.
- This can be the case, for example, with press residues of an oilseed or of fruit and vegetables or with dried fruit, peeled products or plant materials which have been mechanically or microbially altered or dried and / or comminuted.
- the production and production of cellulose-based vegetable fibers by a process consisting of the a) providing a vegetable starting material containing compacted cellulose-based fibers, which can be penetrated by aqueous solutions,
- step b) a saturation of the plant material from step a) with an aqueous digestion solution containing dissolved amino acids and / or peptides, in which the at least one amino acid is a cationic amino acid and / or the at least one peptide, at least contains a cationic amino acid.
- the cellulose-based fibers according to the invention can be produced simultaneously.
- the cellulose-based fibers according to the invention are characterized by
- a water binding capacity of> 200% by weight a proportion of chemical compounds and functional groups of> 2.5% by weight that do not correspond to a polymeric carbohydrate.
- At least two of the abovementioned characteristics are present simultaneously in the case of the cellulose-based fibers according to the invention.
- the cellulose-based fibers produced according to the invention are further distinguished by a very low fiber length weight, the coarseness, which is preferably ⁇ 70 mg / 100m, more preferably ⁇ 50 mg / 100m, more preferably ⁇ 30 mg / 100m and even more preferably ⁇ 20 mg / 100m, more preferably ⁇ 15mg / 100m, and most preferably ⁇ 10mg / 100m.
- Preference is given to a process in which cellulose-based fibers having a length weight of ⁇ 20 mg / 100 m are obtained and / or produced.
- Preference is given to a process in which cellulose-based fibers having a length weight of ⁇ 20 mg / 100 m are obtained and / or prepared which have not undergone a polymer-analogous reaction.
- nature-identical cellulose-based fibers having a very short length weight can be obtained directly from an organic starting material and without changing the polymeric structures, such as an ether reaction, directly and with excellent colloidal properties.
- cellulose-based fibers An essential property of these functional cellulose-based fibers is their high water-binding capacity. So this is largely responsible for the strength and water retention of vegetables and fruits, which are made for the most part of water, such as carrots or pumpkins. These functional properties can be obtained by the production and production of the cellulose-based fibers by the processes according to the invention without a chemical modification of the cellulose-based fibers obtained being necessary for this purpose.
- Such cellulose-based fibers are characterized in particular by a very high water-binding capacity and by their particularly high water retention capacity and their colloidal properties.
- the water-binding capacity is preferably more than 200% by weight, more preferably more than 400% by weight, more preferably more than 800% by weight and more preferably more than 1000% by weight.
- a water retention capacity of preferably> 50% by weight, more preferably of> 80% by weight and more preferably of> 120% by weight.
- water binding capacity and “water binding capacity” are used synonymously herein.
- the water retention capacity may i.a. be tested by the cellulose-based fibers in the fully hydrated state first of free-running water, with a layer thickness of 20mm on a filter cloth, freed. Next, a 10 cm diameter punch is placed on the mass with a defined mass weight (e.g., 1000 g). After 30 minutes, the residual moisture content of the compressed mass is determined. Another method is described under "Methods”.
- Pulping processes for cellulose are carried out according to the prior art by mechanical comminution of vegetable cellulosic material, ie wood or woody vegetable constituents. This includes stems and husks. As a result, it is possible to obtain high-purity cellulose fiber powders which have a defined size distribution of the fibers. It has been shown that pulping processes, such as those used for the production of cellulose according to the prior art, give fibrillar cellulose fibers which do not lead to a sensory or functionally satisfactory result. In contrast to fibrillar cellulose fibers, which are synthesized by plants for holding and structural tasks.
- the cellulose-based fibers according to the invention which occur in non-lignified or woody plant materials, just for the desired chewing and Taste experience responsible for a consumption.
- the cellulose-based fibers obtained and produced according to the invention are soft, nature-identical fiber materials derived from fibrillar cellulose fibers, which are obtained, for example, from a wood pulp, or from cellulose derivatives which, by esterification, also have a different structure from that of US Pat present, exhibit, and differ in sensory perception from skins and mucous membranes are not perceived as pointed, hard or bite-resistant / unappealable.
- a post-treatment of the separated cellulose-based fibers takes place in order to obtain further functional properties of the cellulose-based fibers.
- the optional process step c3) and / or d3) conditioning / functionalizing the cellulose-based fibers.
- the surfaces of the cellulose-based fibers are hygroscopic.
- glycerol or a sugar syrup or an amino sugar compound which are present for example dissolved in water, be used, in particular, if the cellulose-based fibers are to be supplied to a preparation of desserts or it can be an aqueous salt or acid solution, the z.
- dissolved amino acids and / or peptides are used for conditioning.
- the dekompakt faced cellulose-based fibers which are obtained in the process stage c1) or c2) and / or d1) or d2) inserted and hydrated the solution in a solution with the dissolved amino acids and / or peptides.
- Preferred amino acids are arginine, lysine and glutamate.
- micro- or nanoemulsions are used for conditioning.
- Micro- or nanoemulsions consisting of a guanidino- and / or amidine-group-bearing supporting compound and an acid are preferred have been produced.
- Arginine and a carboxylic acid are preferred.
- Preferred for a hydrophilization of the surfaces are short-chain fatty acids such. As lactate or adipic acid.
- the still moist cellulose-based fiber mass obtained from the recovery process is for this purpose by a mechanical method, such as a pressing or centrifugation with a preferred residual moisture of 5 to 100Gew%, more preferably from 10 to 80Gew% and more preferred from 25 to 60% by weight, into an acid solution having a preferred pH range between 2 and 6, more preferably between 2.5 and 4, or into a basic solution having a preferred pH range between 8 and 14, more preferably between 8 , 5 and 12.5 or in an aqueous solution with a surfactant, such as DMSO, at a concentration of 0.1 to 20%, more preferably between 0.5 and 15%, preferably by means of a stirring addition.
- a mechanical method such as a pressing or centrifugation with a preferred residual moisture of 5 to 100Gew%, more preferably from 10 to 80Gew% and more preferred from 25 to 60% by weight
- an acid solution having a preferred pH range between 2 and 6, more preferably between 2.5 and 4, or into a basic solution having a preferred pH range
- the use of cationic or anionic amino acids and / or peptides as acid-forming or base-forming compounds is preferred.
- the duration of the conditioning is subject to the individual requirements, preferred is a conditioning period of 1 minute to 3 days, more preferably from 1 hour to 24 hours.
- the temperature can in principle be chosen freely, preferably a temperature between 10 ° and 90 ° C., more preferably between 15 ° and 60 ° C.
- Micro- or nanoemulsions can be used in any concentration and in any proportion with the cellulose-based fibers in the same way as described above.
- a reduction of pathogenic agents, germs or toxins and / or bleaching takes place in process step c3) or d3).
- compounds of the prior art can be used. Preference is given to aqueous solutions containing peroxides or chlorates. Preference is given to hydrogen peroxide or sodium hypochlorite. The required concentration and the Duration of exposure depends on the deactivation / decoloration to be achieved and must be determined individually.
- the conditioned cellulose-based fibers are then rinsed copiously with water or a suitable mixed solution.
- the conditioned and rinsed cellulose-based fibers are then dried and ground.
- an acceleration of the water recovery after drying of the conditioned cellulose-based fibers is achieved by the conditioning. This can be checked by z. B. the duration for the complete absorption of a volume of water, with which a complete swelling of the dried cellulose-based fiber material is achieved, is determined.
- the conditioning achieves an increase in the water reuptake rate of> 100%, more preferably> 200% and more preferably> 300% over unconditioned cellulose-based fibers.
- the conditioning achieves an improvement in the adhesion of compounds, for example of sugar compounds or proteins.
- the attachment / incorporation of compounds to / in the cellulose-based fibers may be as described elsewhere in this disclosure.
- conditioning requires an improvement in the adhesion of compounds in a subsequent functionalization of the cellulose-based fibers. This is especially true for the use of micro- or nanoemulsions which are preferred for carrying out a conditioning.
- the change in the adhesion of compounds to the cellulose-based fibers can be reconstructed by prior art methods, for example, by dilution experiments.
- the cellulose-based fibers produced and dried according to the invention have a very rapid and complete hydratability.
- the hydratability can be recognized by a complete singleness of the fibers, which do not exceed a maximum volume of 2.000 ⁇ and in which there is an absence of a granular or spiky property in the sensory evaluation.
- the cellulose-based fibers obtained according to the invention can be functionalized very easily and effectively.
- the method according to the invention contains the optional cess step c3) and / or d3): functionalizing the surfaces of the cellulose-based fibers, following the process step c1) or c2) and / or d1) or d2)
- Suitable for this purpose are the still wet, dried or completely dried cellulose-based fibers obtained according to the invention with / without prior conditioning, as described herein.
- the cellulose-based fibers obtained and produced according to the invention are distinguished by their high absorption capacity for functionalizing components, which is very probably based on the high binding capacity for water but also for lipophilic compounds (especially when using the dried cellulose-based fibers), out. It has thus been shown that a uniform and complete coating / loading of the cellulose-based fibers with proteins, carbohydrates, microorganisms or dyes from aqueous solutions or suspensions is possible.
- oils and fats completely occupy the inner and outer surfaces, provided that they were brought into contact directly or dissolved in a suitable solvent with the dried or dried cellulose-based fibers.
- the applicability of incorporation and incorporation / picking differed considerably from that which could be achieved with cellulosic fibers.
- a larger amount of compounds / substances could be immobilized on or in the cellulose-based fibers produced according to the invention.
- the cellulase-based fibers produced according to the invention are very well suited for receiving and enclosing a large amount of compounds / substances. Nevertheless, after drying the recovered and produced cellulose-based fibers a good formability, eg. As a powder, possible.
- powders can preferably be produced by a grinding process or by an impact comminution process. Very good results could also be achieved by spray drying, milling drying or freeze drying, therefore processes for producing coated cellulose-based fibers which are obtained by means of spray drying, milling drying or freeze drying are preferred.
- sugar / saccharide compounds or organic acids such as citric acid or lactate
- surfactants such as phospholipids or glycolipids or glycoglycerolipids
- chelating agents such as EDTA
- the product properties of the cellulose-based fibers can be changed by the incorporation / application of surface modifiers.
- incorporation of the cellulose-based fibers obtained into aqueous solutions containing surface-active compounds leads, for example, to an increase in the volume of space of the cellulose-based fibers and, at the same time, a markedly reduced settling rate of such cellulose-based fibers a liquid is achieved.
- Such effects could be achieved, for example, by sodium lauryl sulfate or DMSO by suspending the cellulose-based fibers in these solutions.
- Even after subsequent rinsing with water and drying, the cellulose-based fibers produced had a significantly larger volume of space and could be hydrated faster than cellulose-based fibers that have not been surface-modified after their extraction.
- dried and powdered cellulose-based fibers are used for incorporation / attachment of surface functionalization and / or surface modifiers.
- the powdered cellulose-based fibers are suspended in a solution / suspension of an aqueous or non-aqueous phase and agitated therein by means of an agitator.
- concentration of the compounds used for the functionalization or surface modification is to be determined individually.
- the process of functionalization / surface modification preferably takes place until complete swelling of the cellulose-based fibers has been achieved. This can be assessed, for example, on the settling behavior of the agitated fiber mass.
- cellulose-based fibers are subsequently freed of free water, for example by application to a vibrating screen, and if necessary to a preferred residual moisture content of 0 to 100% by weight, more preferably 10 to 80% by weight and more preferably 20 to 60% by weight % dried by techniques of the prior art. If necessary, then carried out a mechanical fragmentation of the dried cellulose-based pulp.
- Preference is given to a process for obtaining and producing cellulose-based fibers in which a surface modification takes place.
- Preferred is a method in which the surface modification is carried out with a surface-active substance.
- a modification of the properties of the cellulose-based fibers could also be effected by other compounds.
- a sensory perceptibility of recovered cellulose-based fibers by carboxylic acids which were in the form of micro or nanoemulsions and in which the cellulose-based fibers were suspended, can be significantly reduced.
- oils and fats For example, it could be shown that cellulose-based fibers, which had been surface-modified with carboxylic acids, had a significantly increased oil absorption capacity.
- lipophilic or amphiphilic compounds are brought to / on the surfaces of the cellulose-based fibers by means of micro- or nanoemulsions.
- micro- and nanoemulsions The preparation of micro- and nanoemulsions is known in the art. Preference is given to nanoemulsions which consist of cationic amino acids and carboxylic acids. Arginine, lysine and histidine as well as oleic acid and linoleic acid are preferred.
- Concentrations of the amino acids from ⁇ ⁇ to 0.6 mol, more preferably ⁇ to 0.1 mol are dissolved in water and with a carboxylic acid in a ratio to the amino acid used of preferably from 0.01: 1 to 1 for the preparation of the preferred nanoemulsions : 1, more preferably 0.1: 1 to 0.5: 1 and stirred until a clear liquid is obtained.
- the micro- or nanoemulsions can be contacted in any proportion with wet, dried or dry cellulose-based fibers.
- Preferred compounds which can be applied with micro / nanoemulsions to / on the surfaces of the cellulose-based fibers include carboxylic acids, waxes, phospholipids, mono-di- and triglycerides, glycolipids, glycoglycerolipids, steryl glycosides or lipophilic dyes and flavorings.
- the respective concentration of the compound (s) to be dissolved in a micro / nanoemulsion is to be determined in each case in solution experiments.
- Preferred is a complete solution so that micelles or particles herein have a diameter of less than 200nm. Such a surface coating gives rise to further extremely advantageous effects.
- the oxidation stability of a lipid phase can be increased by such a surface modification of cellulose-based fibers.
- a significant reduction of secondary oxidation products could be effected in a camelina oil, when the cellulose-based fibers to which carotene or carotenoids had been incorporated / incorporated.
- Such anti-oxidative effects could then also be demonstrated for the attachment / incorporation of antioxidants to / in the cellulose-based fibers.
- Such antioxidants are, for example, ascorbic acid. Preference is given to surface-modified cellulose-based fibers for the oxidation stabilization of lipid phases.
- Preference is given to a process in which surface modification of cellulose-based fibers takes place by means of a micro / nanoemulsion.
- cellulose-based fibers also exhibited improved miscibility and stability with lipid phase emulsions. It has been shown that cellulose-based fibers are outstandingly suitable for producing lotions, creams, ointments or pastes. On the one hand, there is a very easy incorporation of cellulose-based fibers into already existing lotions / emulsions / creams or ointments without destabilizing the water-in-oil or oil-in-water mixture. Such preparations retained the same turgor and shape significantly longer in air exposition. Furthermore, the pull-in behavior on the skin was significantly increased, the skin surfaces were faster fat-free, as was the case with the original preparations.
- the lotions / creams / ointments or pastes could be admixed with aqueous solutions containing hydrophilic compounds in the first place or in substantially larger amounts without any subsequent segregation when cellulose-based fibers were mixed in.
- the stabilizations of the formulations of lotions / creams / ointments or pastes achievable with the cellulose-based fibers were significantly better than formulations with cellulose fibers.
- the cellulose-based fibers can be applied in any desired form to lotions / creams / ointments or pastes, preference is given to the use of cellulose-based fibers having a residual moisture content of from 10 to 200% by weight, more preferably from 15 to 100% by weight and more preferably from 20 to 80% by weight ..
- the preferred addition amount is cellulose-based Fibers (TG) to lotions / creams / ointments or pastes and 0.0001: 1 to 0.5: 1, more preferably 0.001: 1 to 0.2: 1, and more preferably 0.01: 1 to 0.1: 1.
- TG cellulose-based Fibers
- the mixture is carried out by methods of the prior art. If desired, water or solubilizers may be added to the formulation.
- Cellulose-based fibers are preferred for stabilizing lotions / creams / ointments or pastes. Preference is given to cellulose-based fibers for introducing and formulating compounds in lotions / creams / ointments or pastes.
- auxiliaries / active substances in lotions / creams / ointments or pastes by the attachment / incorporation of compounds onto / into the cellulose-based fibers and that these are present in stable form herein.
- auxiliaries / active substances in lotions / creams / ointments or pastes
- these are present in stable form herein.
- a very stable and homogeneous introduction and distribution of light quantum adsorbents in emulsions and lotions with the cellulose-based fibers can be achieved.
- carotenes or ascorbic acid were introduced into / into the cellulose-based fibers by placing the cellulose-based fibers in an organic solution containing carotenes or an aqueous solution containing ascorbic acid for 5 hours and then removing them from organic solvents or Completely freed of water or dried to a residual moisture content of 50% by weight.
- the loaded cellulose-based fibers were then stirred into a lotion or cream for 3 hours.
- the preparations were applied to a radiation-transparent support in a defined layer thickness and the adsorption of UV radiation transmission was determined.
- cellulose-based fibers obtained according to the invention In further studies on the functionalizability of cellulose-based fibers obtained according to the invention, it has surprisingly been found that, in contrast to cellulose fibers, a coupling / functionalizing layer is achieved by impregnation of the cellulose-based fibers with dissolved coupling / functionalizing substances alone, so that it can be assumed that that the connection to the surfaces of the cellulose-based fibers obtained largely for the most part via electrostatic exchange forces.
- the cellulose-based fibers obtained according to the present invention are suitable, due to the presence of the large number of compounds which are not polymeric carbohydrates and are functionalizable, a wide range of reactive To provide groups / connections.
- Compounds with which a surface coupling / functional layer can be made are known in the art. Preference is given to compounds which carry sulfur, phosphorus or OH groups, such as sulfonates, phosphates or alcohols.
- a surface coating of the cellulose-based fibers with a coupling / functional layer which is effected by an electrostatic and / or covalent surface bond is preferred.
- cellulose-based fibers having a surface coating as a coupling / functional layer for electrostatic and / or covalent surface bonding.
- the cellulose-based fibers according to the invention are particularly suitable for the uptake / storage and cultivation of microorganisms.
- the preferred microorganisms are preferably useful organisms which are capable of producing and / or fermenting compounds / substances.
- Typical representatives of such microorganisms are, for example, glucose-splitting yeasts, such as the baker's yeast or lactose-splitting bacteria, such as Bacillus bifidum.
- the cellulose-based fibers are used for stabilization / storage / preservation of compounds / substances / organisms.
- all cellulose-based fibers produced according to the invention can be used for this purpose. Preference is given to cellulose-based fibers of soybean, rapeseed, maize or pumpkin.
- cellulose-based fibers are preferred which have a residual moisture content of between 20 and 80% by weight.
- the attachment / introduction is preferably by suspending the cellulose-based fibers in a solution in which the compounds / substances / organisms to be introduced / introduced are dissolved or suspended.
- the preferred exposure time is between 10 seconds to 24 hours, more preferably between 1 minute and 12 hours, and more preferably between 2 minutes and 6 hours, in which the cellulose-based fibers are present in the solutions / suspensions containing compounds / substances / organisms be left.
- Preference is given to an easy agitation of the suspension with an agitator during the exposure time.
- Preference is given to a temperature between 5 and 90 ° C, more preferably between 15 and 75 ° C and more preferably between 25 and 50 ° C.
- cellulose-based fibers which have a residual moisture content of ⁇ 20% by weight are added to a solution / suspension with compounds / substances / organisms and hydrated therein, which leads to an accumulation / incorporation of the compounds / substances / Organisms in the cellulose-based fibers comes.
- cellulose-based fibers which have a residual moisture content of> 25% by weight are added to the compounds / substances / organisms to be introduced / introduced in dry or dried or agglomerated form and mixed with the cellulose-based fibers, resulting in the Compounds / substances / organisms on / in the cellulose-based fibers store / store.
- Preference is given to the introduction / introduction of organic compounds to / in the cellulose-based fibers particular preference is given, for example, to vitamins, enzymes, antioxidants, furthermore microorganisms, for example yeasts, lactic acid-producing bacterial strains or algae.
- cellulose-based fibers are used for culturing microorganisms. It has been shown that proliferation and / or product proliferation production of yeasts and algae as well as Bakthenstämmen by an attachment / on cellulose-based fibers against a culture on / in culture media from the prior art significantly improved.
- algae that have been incorporated into cellulose-based fibers produced a greater yield of triglycerides per unit volume than algae grown in a free liquid culture or attached to cellulosic fibers.
- bakers' yeasts incorporated / incorporated into cellulose-based fibers could be shown to have a higher rate of reproduction than yeasts cultured in a fiber-free medium or yeasts attached to cellulosic fibers. The same was true for the metabolism of carbohydrates and the production of CO2.
- Virtually all cellulose-based fibers according to the invention can be supplied as fiber to human or animal nutrition. It may be a substitute for other fiber and / or fiber supplements of foods and food preparations or a diet.
- the cellulose-based fibers can, in principle, be consumed in any desired amount and food preparations added / admixed. Preference is given to a consumption of cellulose-based fibers obtainable according to the invention from 0.01 g to 500 g (TG) / day, more preferably from 0.1 g to 250 g (TG) / day, more preferably from 1 g to 150 g (TG) / Day and more preferably from 5 to 80g (day).
- the cellulose-based fibers of the present invention can be consumed in any shape and consistency as a dietary fiber replacement or supplement. Preference is given to preparations with hydrogenated forms of the cellulose-based fibers, for. In liquid formulations such as beverages, soups or sauces; or in consistent formulations, such as meatballs, dumplings or casseroles; or low-water formulations, such as pies or baked goods; or in dry formulations, such as chips or pastries.
- the cellulose-based fibers according to the invention can be added / admixed to all nutrients and all foods or processed or prepared with them. The amount added to a food is not limited and results from the formulability of the individual preparation.
- the mixtures can be made with dry raw materials and / or with wet and / or dissolved in water or a lipid phase starting materials. In this case, any mixing tool can be used and any temperature and any mixing or stance period can be selected.
- the preparation result may be prepared in directly preserved and raw form, in crude stored form, in cooked or fried or baked form, in a liquid to dry state.
- ready-mixed mixtures can be produced with the cellulose-based fibers according to the invention by admixing a cellulose-based fiber mass, for example kidney beans, seasoning mixtures of the prior art homogeneously or a liquid seasoning to a dried and pulverized cellulose-based fiber mass is added until a homogeneous distribution has taken place and the mixtures are then offered for consumption in moist or dried form.
- wet or dried cellulose-based fibers are mixed with proteins.
- the proteins can be of plant or animal or microbial origin and can be present in dry or moist / hydrated form.
- the resulting mass is subjected to belt drying and comminuted to a powder.
- cellulose-based fibers prepared according to the invention are used for the regulation of intestinal transit and / or stool consistency.
- all cellulose-based fibers according to the invention are applicable for this purpose.
- the aforementioned preparations can also be used for a regulation of intestinal transit and stool consistency.
- instant forms are, for example, powders or granules.
- these are prepared with flavor / seasoning / sweeteners and / or stabilizers or soluble carbohydrates, by methods known in the art.
- the application of the cellulose-based fibers takes place in the form of a tablet or a capsule.
- the cellulose-based fibers according to the invention are particularly well suited for this purpose since they can be brought into a very compact form. It has been found that during a drying process, a moist mass of recovered cellulose-based fibers around a center of mass during drying spontaneous konnpaktiert so that a homogeneous self-contained dry matter is formed. As a result, the cellulose-based fibers can be compressed to very compact space without relevant technical effort. It is advantageous that such compacted cellulose-based fibers, which have no cornification, can be hydrated only slowly and thereby advantageously fully hydrated and isolated in the gastrointestinal passage only in the small and / or large intestine.
- the daily supply of cellulose-based fibers according to the invention for this application is preferably 1 to 50 g (TG) / day, more preferably 2 to 25 g (TG) / day and more preferably 3 to 15 g (TG) / day.
- cellulose-based fibers are used as a fiber additive or dietary fiber substituent.
- cellulose-based fibers are used as regulators to effect an acceleration of the gastrointestinal passage and / or a softening of the stool.
- cellulose-based fibers are used to treat constipation.
- cellulose-based fibers produced according to the invention can be added to a regular diet, incorporated into it or consumed together with it or separately, in a moist, dried or dry form and over any desired period of time. In this case, applications in the form of capsules or tablets are possible.
- the admixture of cellulose-based fibers produced according to the invention to the different food preparations is preferred.
- the cellulose-based fibers produced according to the invention can also be used specifically for weight-loss therapy.
- the oral intake takes place at 2 or 3 times of day.
- weight reduction therapy for the purpose of weight reduction therapy,> 15g / d, more preferably> 30g / d, more preferably> 35g / d, even more preferably> 40g / d orally, and more preferably 50g / d (the weights given herein are based on U.S. Pat dry mass). Also here Applications in the form of capsules or tablets are possible. The duration of the application is not limited and depends on the achieved and desired result of the weight reduction.
- Another example is the trunk, z. B. of cabbage, and vegetables without special aromatic qualities, such as pumpkins or celery.
- a large amount of fruits and vegetables is fed annually for qualitative deficiencies and / or insufficient freshness of destruction.
- most fruits and vegetables do not consume and dispose of their hulls and trays.
- the preparations had a pleasant mouthfeel, even in the case of a high concentration of the cellulose-based fibers produced according to the invention, in the absence of a "sliminess” or a “mealiness", which was present when such a thickening effect with, for example, a cellulose derivative or a starch had been made.
- the cellulose-based fibers obtained according to the invention can be functionalized with cellulose derivatives, preferably in process step c3) or d3). It has been shown that even small amounts of dissolved cellulose derivatives are sufficient to cause an increase in the colloidal properties of the cellulose-based fibers produced.
- a functionalization is carried out with a cellulose derivative and / or a starch.
- the invention also relates to processes for the functionalization of cellulose-based fibers. Furthermore, the invention also relates to functionalized cellulose-based fibers.
- the cellulose-based fibers produced according to the invention have a very good emulsifying power in W / O or O / W mixtures, very probably by exposed hydrophobic cellulose structures.
- Another peculiarity with which the cellulose-based fibers produced according to the invention differ very markedly from cellulose fibers which results from a grinding process of husks or Stängelmassen, is their ability to stabilize the structure of food preparations, such as a baked good in baking processes.
- Two components, which are very likely to occur in parallel, can be assumed to be causal, among others: 1. a skeleton function through the formation of multilocular contacts with other compounds of a baked good, such as proteins or carbohydrates, through the versatilen side groups and the large-volume spatial structures of the cellulose-based fibers and 2.
- the cellulose-based fibers obtained and / or produced by the processes according to the invention differ substantially in morphology, chemical constituents, physico-chemical properties and the effects which can be achieved therewith in various applications against cellulose fibers which have been produced from stalk or spelled materials but also to cellulose derivatives, such as cellulose ethers.
- cellulose derivatives such as cellulose ethers.
- flour in the preparation of baked goods such as bread rolls, bread, cakes and flour products, such as pasta (eg noodles ), Streusel, sauces wholly or partly by inventively produced cellulose-based fibers to replace.
- a replacement of flour in food preparations is preferably carried out to> 10% by weight, more preferably of> 25% by weight, more preferably of> 50% by weight, more preferably of> 75% by weight, even more preferably of> 90% by weight and most preferably of 100% by weight %.
- the cellulose-based fibers can be used in any form or consistency as a flour substitute.
- cellulose-based fibers having a residual moisture content of preferably ⁇ 30% by weight, more preferably ⁇ 20% by weight and more preferably of ⁇ 10% by weight. Preference is given to the use of powdered cellulose-based fibers. Such cellulose-based fibers may preferably have a surface modification, according to one of the methods described herein.
- cellulose-based fibers produced according to the invention were used as a flour substitute which have a residual moisture content of preferably 30 to 300% by weight, more preferably 40 to 200% by weight and more preferably 50 to 100% by weight.
- Such stirrable or spreadable cellulose-based fiber pulps can be used in particular for the production of doughs, whereby the time for a swelling, as is the case with a flour, can be saved.
- a bread roll or a pizza dough dough with cellulose-based fibers according to the invention could be produced, wherein a replacement of the otherwise used flour content amounts to 80% by weight and also completely.
- Both bakery products had a qualitatively comparable result compared to the original recipe, but the tasting showed a better rating for the preparation with the cellulose-based fibers.
- the replacement of oils or fats by cellulose-based fibers produced according to the invention, in a food or edible preparation of> 5% by weight, more preferably> 10% by weight, more preferably> 20% by weight, more preferably> 30% by weight , more preferably> 40 %
- the cellulose-based fibers, along with the oils or fats or separately therefrom, may be blended into the food or food preparation. The mixing ratios and mixing time required for the desired product specification must be determined individually.
- oils or fats which have a low melting point and / or low viscosity are subjected to thermal and / or chemical processes in order to increase the melting point / viscosity of the oils or fats. This can result in harmful reaction products.
- the oils or fats emulsifiers and / or stabilizers are admixed, which also have harmful potential or lead to a taste impairment.
- the cellulose-based fibers according to the invention can be mixed with oils and fats in virtually any desired mixing ratio, forming stable mixtures having an increased viscosity and melting point.
- dry and powdered, dried or moist cellulose-based fibers can be used.
- Particularly preferred is a residual moisture content of 10 to 100% by weight, more preferably between 15 and 70% by weight and more preferably from 20 to 50% by weight.
- Preference is given to the use of cellulose-based fibers in which surface modification and / or surface functionalization and / or surface loading, for example with antioxidants or vitamins, has occurred.
- the qualitative mixing result can be determined by methods from the prior art for determining the viscosity or the melting point.
- an increase in the melting point between 0.2 and 30 ° C, more preferably between 0.5 and 20 ° C and further preferably between 0.8 and 10 ° C.
- cellulose-based fibers produced according to the invention are mixed with oils or fats in order to produce a butter or margarine therefrom. The preparation of a readily spreadable preparation is preferred.
- the cellulose-based fibers produced are outstandingly suitable for formulating dissolved or soluble proteins.
- proteins which are present in an aqueous solution, it comes to the formation of a hard mass that can be crushed only with high energy expenditure and incomplete. A comminution is necessary because the very easily soluble proteins before drying can be brought back into solution in the dried state very poorly. Therefore, a fine grinding is preferable.
- the soluble or dissolved proteins are processed into granules or powders with a high expenditure of energy / input.
- the mixture can in principle take place in any desired mixing ratio, it is preferred to add the liquid phase until a water content of 20 to 120% by weight, more preferably from 25 to 90% by weight, more preferably between 28 and 60% by weight and more preferably between 30 and 30% 50% by weight.
- the mixture should preferably be carried out until complete hydration of the cellulose-based fibers has been achieved.
- a dough-like mass is obtained, which is very easy to process and in particular does not tend to stick or stick, as is the case with the pure protein fraction.
- This also makes it possible to carry out drying processes that are not suitable for drying the sole protein fraction, as this gives little or no soluble protein agglomerates.
- the object of the mixture of proteins and cellulose-based fibers on a bath-drying apparatus is preferred.
- the drying can then be carried out in a temperature range between 40 ° and 200 ° C, more preferably between 50 ° and 150 ° C and more preferably between 60 ° and 120 ° C. Preference is given to a simultaneous vacuum system.
- the mixture may be comminuted or agitated during the drying process. This has the advantage that already after drying a granulate or powder is present. Alternatively, a grinding of the condensates / agglomerates can be carried out after the drying process. Surprisingly, a powder obtainable from the dried mass is very readily soluble in water, with complete hydration of the proteins contained. Preference is given to obtaining a protein powder which has a proportion of cellulose-based fibers produced according to the invention of between 1 and 95% by weight, more preferably between 10 and 80% by weight, more preferably between 15 and 70% by weight and more preferably between 20 and 50% by weight %.
- the average particle size of the powder is between 1 ⁇ m and 500 ⁇ m, more preferably between 5 ⁇ m and 300 ⁇ m, and more preferably between 10 ⁇ m and 200 ⁇ m.
- the obtainable mixtures are also characterized by an odor and / or taste neutrality, due to the adsorption of odorants and flavorings by the cellulose-based fibers produced according to the invention.
- the mixtures of proteins and cellulose-based fibers produced according to the invention are distinguished by their very good solubility, which corresponds to formulation of the protein by spray-drying.
- the time to complete dissolution of proteins from the mixture of proteins and cellulose-based fibers is within 50 to 150% of the time required for the complete solution of the spray-dried proteins is required, more preferably between 70 and 130% and more preferably between 80 and 120% of the time span.
- the processes according to the invention make it possible to obtain cellulose-based fibers which are suitable as a formulation matrix for all soluble or dissolved proteins. Preference is given to dissolved proteins from seeds of, in particular, rape, sunflowers, camelina, jatropha; in addition, from the digestion of kernels, such as soya or beans, and also from nuts, such as almonds or hazelnuts; further, grains such as wheat or oats; also made from lentils and peas or lupines.
- any other protein fraction can also be formulated by the cellulose-based fibers according to the invention.
- milk protein is especially suitable.
- fish or marine proteins are formulated with the cellulose-based fibers by one of the methods described herein. This has the enormous advantage that it comes to a significantly lower expression of a fishy odor. In many formulations, in contrast to the dried protein mass, practically no fishy odor was perceptible.
- proteins from microorganisms, such as algae or yeast are bound to and / or agglomerated with the cellulose-based fibers.
- the proteins which are formulated by one of the processes with the cellulose-based fibers according to the invention are prepared by, for example, swelling a disintegrated seed of rapeseed with a digestion solution.
- a digestion solution Preferably, cationic amino acids and especially arginine are present in the digestion solution.
- a distribution of the digested constituents of the plant material in a water phase is carried out, in which the proteins are then present almost completely in dissolved form.
- an aqueous solution is obtained in which all readily water-soluble constituents of the starting material are present in dissolved form.
- Aggregation of the proteins which can be carried out for example by a change in the pH of the solution and / or a change in the salinity and / or use of complexing agents, leads to the formation of condensate of the dissolved proteins, causing them to sediment in aggregates. and condense with process of the prior art and can be separated.
- the use of such recovered and aggregated protein mixtures for formulation with the cellulose-based fibers produced according to the invention is preferred. Very particular preference is given to the use of cellulose-based fibers which have the same origin as the proteins formulated herewith.
- the cellulose-based fibers according to the invention are used as nuclei for agglomeration of soluble or dissolved proteins.
- cellulose-based fibers are used by these are filled, for example, in a rapidly rotating drum and a stripper and the protein suspension is applied by means of a spray device on the cellulose-based fibers.
- the drum is flowed through by a warm air. The process is finished when the resulting aggregates / granules have the desired dimensions.
- This method offers the advantage that a larger mass ratio can be produced between the on / off / deposited proteins and the cellulose-based fibers.
- a mass ratio between protein and the cellulose-based fibers of 2: 1 to 1 .000: 1, more preferably from 10: 1 to 500: 1, and more preferably between 20: 1 to 300: 1 of one obtainable by one of the methods agglomerates / condensates.
- Cellulose-based fibers are preferred for the formulation of dissolved or soluble proteins.
- the cellulose-based fibers produced according to the invention are distinguished by particular sensory effects which differ considerably from those of the cellulose fibers, which are obtained from husk and stem mass, and from those of the cellulose ethers.
- the spatial dimensions of the fibers according to the invention are distributed over a wide range between 10 ⁇ and> 1 .000 ⁇ and the median of the widest extent was between ⁇ ⁇ and 500 ⁇ . From studies on the perceptibility of corpuscular solids by the Oral mucosa is known that even particles with a diameter of more than 15 ⁇ are perceptible as a solid.
- the cellulose-based fibers according to the invention are in a pasty and spreadable form; solid gels are not formed. Accordingly, the sensory impressions perceived upon consumption of cellulose-based fibers made according to the present invention have been reported as soft or tender, silky, melting, greasy, full and pleasing to the testers. The sense impression "soft" was associated with the absence of the feeling of corpuscular materials that is perceptible with the tongue or during chewing.
- cellulose-based fibers produced according to the invention do not encrust in a baking, roasting, or frying process with temperatures of more than 100 ° C. and / or have no or practically no charring marks.
- Roasting experiments showed that cellulose-based fibers, which were fried with a residual moisture content of 20% by weight in a frying fat at 240 ° C., condensed to golden yellow smallest grains after evaporation of the bound water, which did not continue even after the frying process was continued for 15 minutes changed in their color and appearance.
- a coating of a food including meat, tofu, fish, flour doughs
- dried and powdered cellulose-based fibers according to the invention allows a similar good cooking behavior and neutral taste without a dark discoloration or sensory change of the food.
- cellulose-based fibers produced according to the invention are used as release agents for roasting, baking or frying goods in order to avoid searing, dehydration or other thermal damage to the baked goods. It has also been found that, in particular when using cellulose-based fibers which have a residual moisture content of more than 10% by weight, the food undergoes less water loss during the cooking process.
- the examiners found a long-lasting fruity taste. This could be reproduced in repeated investigations and was the case in particular after the tasting of cellulose-based fibers of pumpkins prepared according to the invention. Furthermore, surprisingly, the Participants of tasting attempts that it comes after the tasting of cellulose-based fibers produced according to the invention to a larger Speix- flow and mouth odors no longer occur. In a comparative study with cellulosic fibers of husk and stem mass as well as with cellulose ethers, it was found that, in contrast to the consumption of cellulose fibers or cellulose ethers, after consumption of more than 0.5 g (TM) of the cellulose-based Fibers felt a sense of increased saliva.
- TM 0.5 g
- cellulose-based fibers have very particularly advantageous effects in the formulation and application of solutions, gels, lotions or creams which are used for application to the skin and mucous membranes.
- oils or fats required for the formulation of ingredients could be reduced or eliminated altogether.
- the preservable solutions, gels, lotions or creams were stable even after 6 months, ie that, for example, no segregation of ingredients has occurred.
- a very easy to use / dissolveability of the solutions, gels, lotions or creams on the skin and mucous membranes which was better than the original formulation.
- cellulose-based fibers for the formulation of solutions, gels, lotions or creams for use on the skin and / or mucous membranes for / Reduction / replacement of oils and / or fats and / or increase of the surface moisture of skin and / or mucous membranes.
- the object of the invention the production of cellulose-based fibers, is accomplished by an aqueous process with which cellulose-based vegetable fibers can be obtained and produced in their natural form.
- step a) disintegration of the vegetable starting material from step a) by a thermal and / or mechanical digestion process
- the aqueous digestion solution contains dissolved amino acids and / or peptides.
- step a) disintegration of the vegetable starting material from step a) by a thermal and / or mechanical digestion process
- amino acids and the peptides in step b) are preferably cationic amino acids.
- a further object of the invention the use of cellulose-based fibers for the production of food and nutritional supplements, is accomplished by an aqueous process with which cellulose-based vegetable fibers can be obtained and produced in their natural form.
- cellulose-based vegetable fibers for food preparation and / or as a food supplement, produced by a method consisting of the /
- step a) disintegration of the vegetable starting material from step a) by a thermal and / or mechanical digestion process
- the aqueous digestion solution contains dissolved amino acids and / or peptides.
- step a) disintegration of the vegetable starting material from step a) by a thermal and / or mechanical digestion process
- amino acids and the peptides in step b) are preferably cationic amino acids.
- a method and process variants can be provided with which functional decompactivated cellulose-based fibers can be obtained and produced from a wide variety of vegetable starting materials.
- the method is particularly suitable for obtaining and producing functional cellulose-based fibers without the use of a further digestion process, from non-woody plant materials.
- the methods of the invention may also be applied to vegetable biomass, preferably waste consisting of vegetable foodstuffs.
- the processes according to the invention can be used to produce cellulose-based fibers, which, in particular because of their geometric structures and the physical properties chemical properties are clearly different from both cellulose fibers and cellulose ethers from woody or lignified plant material.
- This relates in particular to the functional properties of the cellulose-based fibers produced according to the invention, which leads to unexpected product properties when using the cellulose-based fibers.
- a considerable improvement in the water-binding and retention capacity of products to which cellulose-based fibers produced according to the invention were admixed or used together with these could be shown.
- foods that dry out easily such as a fruit or cheesecake or bakery products, such as bread or cakes, can be protected from dehydration for much longer than with prior art compounds.
- mixtures for example aqueous and oily systems, can be formulated more easily and more stably than is possible with cellulose fibers or cellulose ethers.
- cellulose-based fibers produced according to the invention can be taken up, transported and stored, whereby, for example, antioxidant or photoprotective compounds can be introduced into dermatological preparations and stabilized.
- the cellulose-based fibers produced according to the invention enable the incorporation and / or addition of microorganisms and algae, resulting in further advantageous effects.
- a significant increase in the proliferation and metabolic activity of microorganisms and algae can be achieved, as a result of which, for example, a fermentation of milk into a yoghurt or the formation of carbon dioxide for volume production in a baking preparation can be significantly accelerated.
- microorganisms and algae can be cultivated, transported and stored by incorporation and / or addition to / in the cellulose-based fibers produced according to the invention.
- Cellulose-based fibers prepared according to the invention also cause extremely advantageous effects in the preparation of foods or foods.
- cellulose-based fibers prepared according to the invention can be used as a substitute for both flour and starch, as well as fats and oils, without there being any undesirable impairment of the sensory product properties.
- soluble or dissolved proteins can be formulated by the cellulose-based fibers produced according to the invention and processed much more easily than with processes from the prior art.
- a reduction in weight can be achieved, as well as a regulation of bowel activity and stool consistency. definitions:
- the term "vegetable sources” as used herein includes all of the vegetable products containing cellulose
- the vegetable starting materials may contain any proportion of lignin and cellulosic fibers, among other compounds Plant materials characterized by a low content of lignin
- the non-lignified vegetable materials referred to herein more particularly have a lignin content of ⁇ 10% by weight.
- Such vegetable starting materials may include, for example, seeds, grains, kernels, beans, beet plants, vegetables, Fruits, berries, cucumbers, flowers and roots or tubers or nuts.
- the vegetable raw material may be in intact form, damaged, crushed, peeled, pressed, ground or otherwise disintegrated, including but not limited to milled or grounded flour, resulting, for example, from mechanical extraction of oils, so-called presscake.
- These also include vegetable starting materials which have previously undergone a thermal and / or liquid extraction process, eg. With an alcohol or an organic solvent such as hexane. Also included are plant starting materials in which a thermal treatment has taken place.
- plants that are obtainable from a digestion and / or fermentation process, in particular, when it comes to residues, such as brewery residues (eg in the form of grains or grain flour) or pomace in must production or olive pomace or beet pulp, in particular after extraction of the molasses.
- residues such as brewery residues (eg in the form of grains or grain flour) or pomace in must production or olive pomace or beet pulp, in particular after extraction of the molasses.
- residues of cocoa beans residues, such as brewery residues (eg in the form of grains or grain flour) or pomace in must production or olive pomace or beet pulp, in particular after extraction of the molasses.
- residues of press residues which are found, for example, in the extraction of juices (for example apple, tomato or carrot juice) or pomace, e.g. B. of grapes or apples or extracts, as in the production of jellies or liqueurs (eg., Blackberry jelly, Cassis) incurred.
- juices for example apple, tomato or carrot juice
- pomace e.g. B. of grapes or apples or extracts
- jellies or liqueurs eg., Blackberry jelly, Cassis
- peel, reveal or gut products of plant starting materials may be used.
- the lignin-rich shells of seeds, grains, fruits, vegetables or legumes include the stalk and root system; not wax and / or fiber-rich shells or foliage of this.
- the definition includes roots and ovaries, such as ginseng or beetroot; but not fibrous shells and ramifications.
- fruits such as apples, pears, quinces, plums, bananas; not including lignin-rich shells or husks of these.
- the flowers of ornamentals and useful plants are also included.
- non-woody refers to the above-defined starting materials in which a weight fraction of lignin polymer compounds of ⁇ 15% by weight, preferably ⁇ 10% by weight, and more preferably ⁇ 5% by weight and especially ⁇ 0.5% by weight ,
- cellulose-based fibers includes all of the corpuscular structures of the plant starting materials consisting of a backbone of polymeric carbohydrate / cellulose structures having at least two of the following characteristics: - an origin of a vegetable source material,
- the cellulose-based fibers according to the invention have three-dimensional spatial and surface structures. They may be in a composite structure which can be divided into spherical or corpuscular fragments by physical means such as mechanical comminution and / or thermal treatment.
- the cellulose-based fibers produced according to the invention are further distinguished by a very low fiber length weight, the coarseness, which is preferably ⁇ 70 mg / 100m, more preferably ⁇ 50 mg / 100m, more preferably ⁇ 30 mg / 100m and even more preferably ⁇ 20 mg / 100m, more preferably ⁇ 15mg / 100m and most preferably ⁇ 10mg / 100m.
- the cellulose-based fibers are water-insoluble.
- the cellulose-based fibers produced according to the invention can be hydrated by water.
- the cellulose-based fibers according to the invention are not cellulose derivatives which have been prepared by a chemical process for polymer-analogous reaction.
- compacted cellulose-based fibers may exist in a disintegrated association with other compounds or components, such as e.g. B. in a broken and broken apart by a pressing or bouncing matrix, such as. B. in the case of pressed oilseed or ground grains, or they are compacted in a stable composite structure, which prevents disinucleation of the cellulose-based fibers, such as the z. B. in vegetables or fruits is the case.
- the fibers included in the definition are characterized by structural features and physical properties that are common to them. For example, they consist predominantly of non-linear or cellulose-shaped fiber bundles. In particular, they have spatial structures in the form of free fibers, nets or spatial tissue structures.
- the cellulose-based fibers according to the invention preferably have a planar and / or corpuscular geometry. They may include or include pigments, or they are structural constituents of the fibers of the present invention. However, other organic or inorganic compounds may also be constituents of the cellulose-based fibers or not detachably connected to them by an aqueous medium.
- the cellulose-based fibers produced according to the invention are further characterized in that they have at least one of the following properties: three-dimensional spatial structures through the uptake of water, a high water binding and / or water retention capacity, an absence of readily water-soluble carbohydrates and proteins, as well as a non-delivery of flavor or dyes to a water phase.
- the cellulose-based fibers preferably consist of polymeric saccharide compounds containing side functional groups, such as SH, OH, NH or COOH groups, or covalently linked to other compounds.
- Cellulose-based fibers are u. a. functionalizable via physico-chemical interactions of the functional side groups with organic and inorganic compounds. Preference is given to fibers having a maximum volume diameter of from 10 ⁇ m to 2 000 ⁇ m, more preferably from 20 ⁇ m to 1 ⁇ m, and more preferably from 30 ⁇ m to 500 ⁇ m. Preference is given to cellulose-based fibers having a minimum volume diameter between ⁇ , ⁇ and 50 ⁇ , more preferably between 1 ⁇ and 30 ⁇ and more preferably between 3 ⁇ and 20 ⁇ .
- Preference is given to complex spatial structures which are formed by the cellulose-based fibers.
- the cellulose-based fibers have a content of slightly water-soluble carbohydrates, proteins and flavoring or coloring agents, preferably of ⁇ 3% by weight, more preferably of 2% by weight, more preferably of 1% by weight and even more preferably of 0.5% by weight ,
- the cellulose-based fibers produced according to the invention which are obtained with the process steps d) or e), have these properties, which can be checked by methods of the prior art.
- disintegration means all processes which lead to a separation of plant tissues or textures, whereby complete contacting of the structural components with one of the digestion compounds can take place in the process of stages a) to d) in the form of an aqueous Solution available.
- the definition includes all processes that result in the creation of cracks, voids, or crevices of shell or shell materials of the plant source material, to complete digestion with exposure of the surfaces of the constituents of the plant source material.
- Decisive here is that a disintegration the wetting of the surfaces of the constituents of the vegetable starting material with the compounds of the digestion solution is made possible. Disintegration by definition is thus equivalent to the production of wettability of constituents of the non-woody vegetable starting material for the aqueous digestion solutions and the compounds contained therein.
- digestion herein is meant the process of hydration, by contacting the aqueous digestion solution with the constituents of the starting material, which causes the soluble constituents among themselves and the non-soluble constituents ( If, by means of a process for disintegration, it is also possible to carry out digestion in the same process step, such as, for example, when using an aqueous solution containing digestion compounds which are used for the Disintegration and digestion can be used interchangeably With the hydration of the slightly water-soluble compounds, the digestibility or digestion of the compacted cellulose-based fibers thus also occurs closed dekompaktêtieri cellulose-based fibers.
- aqueous digestion solution means an aqueous solution of one (m) or more amino acid (s) and / or peptide (s) that are completely dissolved therein.
- Preferred are naturally occurring amino acids and / or Peptides consisting of or containing these amino acids in a completely water-soluble form, preferably a solution of one, two or more amino acid (s) and / or peptide (s) present in the individual and / or total concentration in a range from 10 ⁇ / ⁇ to 3mol / l, more preferably between 1 mmol / l and 1 mol / l and more preferably between 0.1 mol / and 0.5 mol / l L- or D-forms or racemates are preferred.
- the use of the L-form is preferred, alanine, arginine, asparagine, aspartic acid, glutamine, glutamic acid, glycine, histidine, isoleucine, leucine, lysine, phenyla
- the amino acids arginine, lysine, histidine and glutamine are particularly preferred.
- the peptides which can be used according to the invention may be Di-, tri- and / or polypeptides act.
- the peptides of the invention have at least one functional group that can bind or bind a proton.
- the preferred molecular weight is less than 500 kDa, more preferably ⁇ 250 kDa, more preferably ⁇ 100 kDa, and most preferably ⁇ 1000 dA.
- the preferred functional groups are in particular a gunanidine, amidine, amine, amide, hydrazino, hydrazono, hydroxyimino or nitro group.
- the amino acids may have a single functional group or contain several of the same class of compounds or one or more functional group (s) of different classes of compounds.
- the amino acids and peptides according to the invention preferably have at least one positive charge group or have a positive total charge.
- Particularly preferred peptides contain at least one of the amino acids arginine, lysine, histidine and glutamine in any number and sequential order.
- Particular preference is given to amino acids and / or derivatives which contain at least one guanidino and / or amidino group.
- the guanidino group is the chemical radical H 2 NC (NH) -NH- and its cyclic forms
- the amidino group is the chemical radical H 2 NC (NH) - and its cyclic forms.
- guanidino compounds and amidino compounds preferably have a distribution coefficient K 0 w between n-octanol and water of less than 6.3 (K 0 w ⁇ 6.3).
- arginine derivatives are defined as compounds having a guanidino group and a carboxylate group or an amidino group and a carboxylate group, wherein guanidino group and carboxylate group or amidino group and carboxylate group are separated by at least one carbon atom, ie at least one of the following groups between the guanidino group or the amidino group and the carboxylate group is: - CH 2 -, -CHR-, -CRR'-, wherein R and R 'independently represent any chemical radicals.
- Compounds having more than one guanidino group and more than one carboxylate group are, for example, oligoarginine and polyarginine. Other examples of compounds that fall under this definition are guanidinoacetic acid, creatine, glycocyamine.
- Preferred compounds have as a common feature the general formula (I) or (II)
- Preferred compounds have as a common feature the general formula (I) or (II)
- X represents -NH-, -NR "" -, or -CH 2 - or a substituted carbon atom
- L represents a C1 to Cs linear or branched and saturated or unsaturated carbon chain having at least one substituent selected from the group consisting of or consisting of
- hydrocarbon chain L is in the range of C1 to C7, of preferred in the range of C1 to Ce, more preferably in the range of C1 to C5, and at Rushzugtesten in the range of C1 through C 4.
- L represents -CH (NH 2) -COOH, -CH 2 -CH (NH 2) -COOH, -CH 2 -CH 2 -CH (NH 2) -COOH, -CH 2 -CH 2 -CH (NH 2) -COOH, -CH 2 -CH 2 -CH 2 -CH (NH 2 ) -COOH, or -CH 2 -CH 2 -CH 2 -CH 2 -CH (NH 2 ) -COOH.
- compounds of general formula (III) as shown below:
- radicals X and L have the meanings as disclosed herein.
- di-, tri- or oligipeptides and polypeptides which are composed of one, two or more amino acids.
- short-chain peptides for. B. RDG.
- peptides which have both hydrophobic and cationic and / or anionic side groups such as RDG, BCAA, NCR, HIS, SPR, EHP or SFA.
- Digestion solutions according to the invention may comprise further compounds which are completely dissolved herein. These may be compounds for adjusting the pH of the solution, in particular an acid or base, such as urea or triethylamine or acetic acid or uric acid, or compounds having surface-active properties, such as, for example, DMSO or SDS. Also included herein are stabilizers such as antioxidants or reducing agents. Preference is furthermore given to compounds which make possible the decomposition of constituents of the starting material; preference is given to compounds from the group of the sulfites and sulfates and also carbonates. These are preferably initially introduced in a concentration of between 0.01 and 30% by weight in the digestion solution.
- proteins refers to macromolecules consisting of amino acids linked together by peptide bonds.
- the proteins referred to herein have a number of> 100 amino acids, and in their primary structure, secondary structure In the case of the secondary structure, the spatial geometry may be in the form of an ⁇ -helix, ⁇ -sheet, ⁇ -loop, ⁇ -helix or may be randomly arranged as random-coil structures.
- carbohydrates as used herein includes all of C3 to C6 sugar molecules and compounds composed thereof, including, but not limited to, monosaccharides such as hexoses, including glucose or fructose, and pentoses, among them Ribose and ribulose and trioses: glyceraldehyde, dihydroxyacetone, disaccharides such as maltose, sucrose, lactose, and polysaccharides such as dextranes, cyclodextrins, starch or cellulose, starch can be distinguished from amylose and amylopectin.
- monosaccharides such as hexoses, including glucose or fructose, and pentoses, among them Ribose and ribulose and trioses: glyceraldehyde, dihydroxyacetone, disaccharides such as maltose, sucrose, lactose, and polysaccharides such as dextranes, cyclodextrins, starch or
- olfactory and flavor is also synonymously used herein with flavoring.
- organic compounds are present which lead to a sensory perception in the sense of a taste or an odor.
- the structural composition of these carbon-based compounds is uneven.
- Some typical classes of compounds are alkaloids, alcohols, aldehydes, amino acids, aromatic hydrocarbons, esters, lactones, cyclic ethers, furans, furanoids, free fatty acids, flavonols, glycosides, ketones, saturated and unsaturated hydrocarbons, enamine ketones, ketopiperazines, isoprenoids, Mono-terpenes, terpenes, cyclic terpenes, triterpenes, triterpenoids, tetraterpenes, sesquiterpenes, sequiterpenoids, sterols, phytosterols, purine derivatives, phenylpropanoids, phenols and / or hydroxycinnamic acid derivatives. These classes of compounds can occur either individually or in any composition.
- dyes is taken to mean, in general terms, organic compounds which coexist in starting materials of biogenic origin in different quantities and compositions.
- plant dyes "encompasses all coloring compounds herein. This applies in particular to the group of chlorophylls and their degradation products, such as pheophyline, chlorophyllide, pheophorbide, phyropheophytine, chlorin, rhodins and purpurins. But there are also connections, which are grouped under the group of carotenes or carotenoids.
- the starting materials which can be used according to the invention, these can be present in different forms and states.
- whole / intact seeds, grains, kernels, nuts, vegetables, fruits, flowers, ovaries or roots can be involved and / or wholegrain or partially disrupted, broken, crushed, crushed, crushed or pressed plant materials and / or plants Materials in which a partial or complete fermentative or desintegrative process has taken place, in particular by an autolysis / microbial degradation / chemical-physical reaction, and / or residues from agricultural production / food processing. Production or utilization.
- the broken, split, crushed, powdered or liquidated or dissolved vegetable starting materials may be in the form of coherent or discrete pieces or complexed, eg as pellets or molding compound or in a loose composite, e.g. As granules or bulk material or in isolated form, such as a flour or powder or in the form of a suspension.
- the consistency, shape and size of the vegetable starting materials is in principle irrelevant, but preferred are comminuted plant raw materials that allow easier digestion.
- Preferred maximum diameters of the dispersible particles of the vegetable starting materials between ⁇ ⁇ and 100cm, more preferably between 0.5 mm and 50cm, more preferably between 1 mm and 20cm and more preferably between 2mm and 5 cm.
- the form of the suitable vegetable starting materials is arbitrary, as well as the consistency, which may be hard or soft, or it may be in a liquefied form.
- the starting material may have any desired temperature, preferably a heated starting material, as obtained, for example, following a pressing operation. If the vegetable starting material does not fulfill the suitable properties / requirements for one of the process executions according to the invention, these conditions can be produced by methods which are available from the prior art. These include, in particular, methods with which an inventive digestion of the vegetable starting material can be facilitated and / or facilitated. These include, in particular, mechanical processes with which the vegetable raw material is decomposed. can be reduced.
- the comminuted and then dried vegetable starting material is comminuted to a certain particle size before process step a), preferably particle sizes between 10 ⁇ m and 2 cm, more preferably between 30 ⁇ m and 5 mm.
- a crushing which takes place during or after the addition of a digestion solution.
- lignin-containing components of the vegetable starting materials are first removed. These may be, for example, shell materials of the vegetable starting materials, such as. As skins, shells or trays, such as those of apple or grape seeds.
- a method for dissolving and / or dissolving lignin can be carried out before carrying out process step a) or a1).
- Such processes are known in the art, for example, as a "kraft process.”
- degradation or digestion of lignin is achieved by boiling with a caustic.
- the starting materials are filled in a suitable container, which can preferably be filled from above and has a closable outlet at the bottom.
- the digestion solutions according to the invention are prepared with the digestion compounds according to the invention as defined herein.
- one or more of the compounds is / are dissolved in water, wherein the water may be a clarified process water, a completely ion-free water and well or city water.
- the water may be a clarified process water, a completely ion-free water and well or city water.
- a pH of the cationic amino acid or peptide solution ranges from 7 to 14, more preferably between 8 and 13, and more preferably between 8.5 and 12.5.
- the pH may be adjusted to any pH range between 6 and 14 by the addition of an acid or a base. Acids and bases known in the art may be used, such as caustic soda or HCl.
- Additives can be added to the solutions which improve or accelerate the digestion and recovery of cellulose-based fibers or disintegrate and / or dissolve other constituents of the starting material.
- Such compounds include, but are not limited to, the following compounds such as: urea, NH 3 , thethylamine; ionic or nonionic surfactants, such as SDS or DMSO; Antioxidants or NaSO3, sodium bisulfite, sodium sulfite.
- the compounds are dissolved in water at a concentration of between 0.1 and 30% by weight, more preferably between 0.5 and 15% by weight, and most preferably between 1 and 5% by weight.
- the digestion solutions according to the invention can be provided with additives which in particular improve the solubility of certain compounds of the starting material, these include, inter alia. Alcohols, fatty acid esters, lactones.
- the digestion solutions can be prepared at any temperature and added to the starting material in the process stage a1), b) and c1), c2), c3), or d1), d2) and d3).
- the application can be carried out in droplets, drops or beams, continuously or discontinuously to, in and / or on the starting material. In a preferred embodiment, this is done under exclusion of air and / or inert gas conditions.
- the application is carried out by a prepared digestion solution from a reservoir via a supply line in an adjustable amount is fed to the starting material.
- the cellulose-based fibers In order to carry out the production and manufacture of disintegrated cellulose fibers based on disintegration according to the invention, it is necessary for the cellulose-based fibers to be dissolved out of the organic matrix in which they are formed and to be decomposed, for which it is necessary to use the composite the cellulose-based fibers with each other and with other organic compounds have to unlock, so that the enclosed / enclosed organic compounds or water can be released.
- the cellulose-based fibers according to the invention are present in a disintegrated form, d. H. they are dissolved or leachable out of a solid and water-insoluble composite or surrounding composite structures (eg shells) and are thus decompactable, physical and / or chemical processes must be used.
- thermal or mechanical methods are used as the physical methods by which disintegration is performed.
- electro-magnetic waves such as. B. Microwaves.
- the selection of the method depends on the water and / or oil content, the consistency and type of plant sources.
- a thermal disintegration is advantageous if the vegetable raw material has a high water content, as with fresh fruits and vegetables. sen.
- the disintegration is preferably carried out by a transfer of thermal energy by water or water vapor.
- a pressurization takes place at the same time.
- a mechanical disintegration is particularly advantageous when the plant-lye starting materials have a low water content and / or enclosed in shells / shells that are impermeable to water. Furthermore, a mechanical method is preferable when first another fraction of the vegetable starting material, such as. As oil, should be removed from this.
- disintegration takes place in the case of vegetable raw materials, in that the raw material is comminuted completely or in part, placed in a water bath and heated until the proportion of the raw material, which essentially contains the recoverable cellulose-based fibers, so soft that it is activated by a light force, e. B. by crushing with the fingers, disintegrates into a mushy or liquid phase.
- a light force e. B. by crushing with the fingers
- the different structures such as, for example, the mesosperm and the shell, can very easily be differentiated from one another as layers and mechanically separated.
- the heating takes place together with a pressure increase in an autoclave.
- vegetable shell materials are removed before and / or after disintegration of the vegetable starting material.
- disintegration of the vegetable starting material takes place by prior introduction into one of the aqueous solutions according to the invention, comprising an aqueous digestion solution according to the invention.
- the volume or weight ratio can be chosen freely, but it is advantageous if the vegetable starting material is completely wetted by the digestion solution.
- the duration of exposure to the digestion solution depends on the plant source materials used. Preferred is a duration between 1 minute and 48 hours, more preferably between 10 minutes and 14 hours and more preferably between 20 minutes and 6 hours.
- the temperature at which the exposure of the vegetable starting material is carried out with the aqueous digestion solutions is, in principle, freely selectable.
- a temperature between 5 ° and 140 ° C, more preferably between 10 ° and 120 ° C and more preferably between 15 ° and 90 ° C.
- a previous and / or simultaneous and / or subsequent treatment of the vegetable starting material with compounds which cause a disintegration or chemical reaction of lignin compounds Preference is given to the use of sulfite and Sulfate compounds. Particularly preferred is sodium bisulfite.
- This process step can be dispensed with or dispensed with if the vegetable starting material is already present in a disintegrated form which qualifies for the use of process step b) and in which the implementation of process step a1) has no advantage over a further process sequence with process step b) results.
- the wetting of the surfaces of the constituents within the vegetable starting material must be ensured. This can be done with prior art methods on intact or disintegrated plant starting materials. Preference is given to inserting the plant material to be digested into an aqueous digestion solution. For the rational use of the digestion solution, it may be sufficient to spray the digestible plant material with the digestion solution during mixing, whereby a naturaltränkung can take place without resulting in a non-permeable for the portion of a free water phase, which then before the next process step is preferably separated.
- a water volume ratio of the aqueous digestion solution to the mass of the plant material is preferably between 0.3 and 30% by weight, more preferably between 0.5 and 20% by weight, more preferably between 0.7 and 10% by weight and more preferably between 0.8 and 5% by weight.
- the impregnation of the plant material with one of the digestion solutions takes place during the application of one of the disintegration methods or immediately afterwards.
- the impregnation is carried out directly together with compounds that enable / accelerate disintegration of the vegetable starting material. This may be the case even if, for example, the aqueous digestion solution is used for disintegration in a thermal process.
- impregnation of the plant material with the compounds of the digestion solution takes place here.
- the impregnation is carried out under reduced or overpressure conditions in a container suitable for this purpose.
- the system is a pressure of 1 mbar to 50 bar, more preferably from 10mbar to 10 bar and more preferably from lOOmbar to 5 bar.
- the impregnation can take place at any temperature. Preference is given to simultaneous heating of the plant material in order to accelerate the soaking process.
- the process step it is preferable to continue the process step at a temperature between 5 ° and 150 ° C, more preferably between 8 ° and 140 ° C preferably between 10 ° and 120 ° C and more preferably between 15 ° and 90 ° C. It is preferable to carry out the process step with simultaneous increase in temperature and underpressure or overpressure.
- the preferred duration of the process step depends on the permeability and the degree of digestion of a previous disintegration. Preferred is a duration between 10 seconds and 10 days, more preferably between 1 minute and 2 days, more preferably between 10 minutes and 24 hours, even more preferably between 15 minutes and 8 hours and most preferably between 20 minutes and 4 hours.
- a moisture content of the vegetable starting material of> 20% by weight and complete hydration of the readily soluble compounds are achieved by the abovementioned processes.
- the completeness of penetration and hydration can also be checked very simply by suspending, for example, 1 ml of the sample of the dissolved plant material in 1 000 ml of water and stirring with a magnetic stirrer for 10 minutes at a rotation frequency of 300 / min. agitated.
- the duration of the soaking phase is sufficient.
- the amino acid and / or peptide solutions used for the digestion are preferably added in a mass ratio of between 0.3: 1 and 3: 1 to the vegetable starting material which can be penetrated by the solutions, and mixed with it complete wetting / impregnation of the organic starting material is ensured.
- a disintegrated starting material is provided.
- a mixture is carried out with one of the digestion solutions according to the invention, which ensures complete penetration.
- the temperature at which this takes place can be chosen freely, preferred are temperatures between 4 ° and 90 ° C., more preferably between 15 ° and 70 ° C. and more preferably between 20 ° and 45 ° C.
- the duration of the penetration phase naturally depends on the type and nature of the vegetable starting material. Preference is given to a duration of between 5 minutes and 24 hours, more preferably between 10 minutes and 12 hours and more preferably between 20 minutes and 6 hours.
- Methods for carrying out process step c1) washing out of soluble constituents of the vegetable starting material and decomposing the cellulosic fibers.
- the soluble constituents of the plant material attached to / from the surfaces of the cellulose-based hydrated are transferred into an aqueous rinse solution or suspended therein.
- aqueous rinse solution Preference is given to the use of water as a washout solution. These may be tap, well, partially deionized or distilled water.
- the rinsing liquid is additized, preferably with water-soluble compounds.
- Preferred additives are substances which cause a lowering of the water surface tension, such as DMSO.
- Particularly suitable additives for this process step are ionic and nonionic surfactants. In appropriate cases, a shift in the pH is made, for example with an acid or a base.
- alcohols are used as a rinsing liquid or as an additive. It is preferable to carry out this process step with a liquid volume which is large enough to be able to absorb the dissolved soluble constituents of the plant material and to prevent re-accumulation / incorporation of these constituents on / in the cellulose-based fibers.
- a volume ratio of the rinse solution to the volume of the plant material from process step b) is between 1: 1 and 500: 1, more preferably between 2: 1 and 300: 1, more preferably between 3: 1 and 150: 1 and more preferred between 5: 1 and 20: 1.
- the suspension is agitated, using methods known in the art.
- the suspension is pumped one or more times through nozzles or thin conduits ensuring a turbulent flow.
- This process preferably takes place under pressure.
- a shear mixture preferably with a rotor-stator shear mixing method or a colloid mill, is carried out.
- the required duration of the washout process depends on the starting material and the other process conditions. Preferred is a duration between 1 minute and 48 hours, more preferably between 2 minutes and 24 hours, more preferably between 3 minutes and 6 hours and more preferably between 4 minutes and 2 hours.
- the temperature of the suspension during the washout process can be chosen freely.
- a temperature between 5 ° and 150 ° C, more preferably between 8 ° and 140 ° C, more preferably between 10 ° and 120 ° C and more preferably between 15 ° and 90 ° C.
- the prior art provides methods and methods with which it is possible to check whether in the process a sufficient leaching of soluble constituents of the starting material is done.
- a volume of 5 ml of filter residue from the suspension taken with a 0.6 mm sieve from the agitated suspension of this step can be used, which is resuspended in 100 ml of distilled water and mixed with a high performance Shear mixer (eg Ultrathurrax) for 30 seconds at a revolution frequency of 10,000 rpm. agitated.
- a high performance Shear mixer eg Ultrathurrax
- the suspension is filtered with the same filter as before.
- the degree of turbidity of the filtrate is determined, for example with a turbimeter. At a turbidity level of ⁇ 20 FTU sufficient leaching of the plant components has been achieved in this stage of the process.
- a detachment of soluble constituents of the vegetable starting material from the cellulose-based fibers is preferably achieved to> 90% by weight, more preferably> 95% by weight, more preferably> 97% by weight and more preferably> 99% by weight whereby cellulosic-based fibers can be obtained which preferably contain or adhere to other soluble organic and / or inorganic compounds ⁇ 5% by weight, more preferably ⁇ 3% by weight, more preferably ⁇ 1% by weight.
- the digested decompacted cellulose-based fibers are present if they have a hydration volume of preferably> 100% by volume, more preferably> 150% by volume, more preferably of> 200% by volume, more preferably of 300% by volume and most preferably of> 400% by volume. and are present in isolated form.
- Methods for Carrying out Method Step c2) Separation of water-insoluble organic solids of the starting material.
- the solid constituents of the starting material which are meant herein are organic compounds which do not correspond to the cellulose-based fibers according to the invention and which do not dissolve further as a result of one of the disintegration / decomposition processes according to the invention and are present as particulate structures, for example.
- B. win by means of filtration Such organic solids include, in particular skins, shells, husks, stems or bark material.
- the recovery of these solid constituents preferably takes place by means of filtration techniques from the prior art. However, it can also be applied process techniques in which a separation of the solid solids from the liquid mixture, for example by means of a centrifugal acceleration, z. B. a Siebdekanter or an eddy current process is accomplished. Preference is given to eddy current methods, such as e.g. can be performed with a Hydrozyclon.
- the method step c3) can be: Condition of the cellulose-based fibers take place. In a process variant, this is done by the wet or dried mass of cellulose-based fibers z. Into a kettle together with a solution containing a conditioning fluid and placed therein for a period of preferably 30 seconds to 2 days, more preferably 1 minute to 1 day and more preferably 5 minutes to 3 hours with continuous mixing remains. The subsequent removal of the free and optionally bound water phase then takes place in the next process stage.
- the optional process step c3 functionalizing the surfaces of the cellulose-based fibers, take place.
- the process technology can be carried out as described above.
- any compounds may be present individually or in combination, at any pH and temperature, in the appropriate solutions. It can be done any pressure and / or negative pressure for any duration.
- the free water phase is the volume of water which is bound to the outer surfaces of the recovered and produced cellulose-based fibers, in particular by capillary forces arising from the assembly of cellulose-based fibers, and by gravity either spontaneously, e.g. , B. by a separation, flows off or by mechanical methods, such as a filtration process, can be separated from the cellulose-based fibers.
- the bound water content consists of the volume of water, which is not separated by the aforementioned measures and can only be separated from the cellulose-based fibers by means of physical / thermal processes.
- the separation of free water by filtration of the cellulose-based fibers can be done by retaining them through a sieve.
- the separation of free and / or bound water is carried out by screening the cellulose-based fibers by means of a vibrating sieve device.
- this is configured as a self-unloading swing / tumble screen.
- a screen size is used which preferably has a retention of> 90% by weight, further preferably of> 95% by weight and more preferably of> 99% by weight of the cellulose-based fibers from the rinsing liquid of process step c): washing out of soluble constituents of the vegetable starting material.
- the sieve size can be selected, for example, by applying a sample of the process liquid of process step c) to sieves with different sieve dimensions of a laboratory vibratory sieve analyzer and determining the number and size of the cellulose-based fibers found in the filtrate.
- a curved screen or a belt filter for the Abtrennaufgabe be used the appropriate sieve dimensions are determined in an analogous manner.
- Another prior art method of performing process step d1) is chamber filter presses. This process technology is particularly suitable when a separation of a free and bound water phase should take place immediately and in one operation. Hereby a high surface pressure can be exerted on the material retained by means of a filter fabric, whereby the main part of the free and bound water phase can be removed.
- the sieve size of a suitable filter cloth is carried out in an analogous manner to the selection of a sieve.
- the pressurization at a pressure of the filter residue depends on the desired residual moisture content of the cellulose-based pulp. Pressure values between 10 g / cm 2 and 500kg / cm 2 are preferred, more preferably between 100 g / cm 2 and 100kg / cm 2 and more preferably between 500 g / cm 2 to 50kg / cm 2. Preference is given to a method in which first a screening of the cellulose-based fibers from the process water of process step c1) or c2) or c3) by means of a sieve and in a further process step the filter retention in a pressing device of further free and / or freed water is released.
- Preferred press devices are also a belt filter press or a lift-stamp filter press.
- Other pressing devices that are suitable for carrying out the method are screw press devices.
- a decanter or Siebdekanter is used to remove the free and bound water phase.
- centrifugal processes such as centrifuges or decanters, can be used to carry out the process step.
- the cellulose-based fibers obtained are subjected to one or more further purification and / or conditioning and / or functionalization processes.
- a residual moisture content is is reached between 30 and 200% by weight, more preferably between 40 and 150% by weight and even more preferably between 45 and 120% by weight.
- the process step d2) is followed by the process step d1) or d3): drying of the cellulose-based fibers.
- This process step is to be used if the fiber mass obtainable from step d1) has too high a water content.
- a residual moisture content of the dried cellulose-based fibers is preferably between 8 and 35% by weight, more preferably between 10 and 30% by weight and more preferably between 12 and 25% by weight.
- Methods for carrying out process step c3) or d3) Conditioning the digested, dekompacted, cellulose-based fibers.
- This can be done for example by the moist, dried or already dried mass of cellulose-based fibers is distributed to a band filter and then sprayed with a functionalizing solution, soaked or flowed through. Preference is given to a penetration of a gas / vapor phase through the mass distributed on a filter cellulose-based fibers.
- the method step d1) or d2) can then be performed for the first time or repeatedly.
- the optional process step c3) and / or d3) is carried out by adding moist, dried or dried mass of cellulose-based fibers to a vessel together with a solution containing a conditioning liquid, and is preferred herein over a period of time 30 seconds to 2 days, more preferably 1 minute to 1 day, and more preferably 5 minutes to 3 hours, with continuous mixing, remains inserted.
- a surface conditioning and in process step d3) a surface functionalization take place.
- a surface functionalization can be carried out with the same methods and solutions as in the case of surface conditioning (see below).
- this is done by the cellulose-based fiber mass is distributed on a belt filter and then sprayed with a functionalizing solution is soaked or flowed through.
- the method step d1) and / or d2) can then be carried out for the first time or repeatedly, after any duration.
- the cellulose-based fibers of the invention may be in a moist form (ie with a proportion of free and / or bound water phase), dried form (ie absence of a free water phase in the presence of a bound water content) or in dry form (ie a residual water content of ⁇ 5 wt %). They can emerge in isolated form or as a shapeable mass from the process stages. They are manufactured if they have the specified product properties. Preferred is the use in the form of a moist, brushable and kneadable mass, with a preferred residual moisture of 20 to 100% by weight, more preferably from 30 to 85% by weight. Preference is furthermore given to a powdered or pourable consistency, with a residual moisture of from 0 to 20% by weight, more preferably from 5 to 15% by weight.
- the cellulose-based fibers according to the invention in hydrated form preferably have a maximum space length of 10 ⁇ m to 2,000 ⁇ m. Preferably, they form three-dimensional spatial structures with irregular boundaries. Preferably, a broad distribution of the dimensions of the cellulose-based fibers is obtained.
- the cellulose-based fibers have functional groups with which they can form electrostatic and / or covalent bonds with other can make connections. These are preferably OH, SH, COOH, PO 4 and / or NH groups.
- the cellulose-based fibers have cyclic and / or aliphatic organic side groups, such as a fatty acid residue, but also sugar residues are preferred. Also preferred are cellulose-based fibers which have as side groups amino acids and / or peptides, such as, for example, cysteine or arginine.
- Fiber analyzers such as B. Fiberlab FS 300 Fa. Valmet available.
- the geometric spatial structure can be represented for example by means of cryo-TEM.
- the presence of functional groups on the surfaces of the cellulose-based fibers can be determined for example by a titration, the determination of the conductivity or a mass spectroscopy (ICP-AES) of the combustion residue.
- ICP-AES mass spectroscopy
- the dimensions of the cellulose-based fibers obtained can be reduced by mechanically comminuting the cellulose-based fibers. This may be done, for example, by mechanically fractionating the cellulose-based fibers present in a water suspended and hydrated state by a high frequency shear mixer / disperser or, when in the dried state, e.g. B. be ground with a cutting or grinding mill.
- the recovery of water can be enabled or accelerated by various methods.
- the cellulose-based fibers to be hydrated are placed in an electrolyte-free and ion-free water.
- the water into which the cellulose-based fibers to be hydrated are introduced is heated, preferably to 30 ° to 99 ° C., more preferably to 45 ° to 80 ° C. and more preferably to 50 to 65 ° C. Preference is given to an alkaline pH of an aqueous solution in which a hydration of cellulose-based fibers takes place.
- the solution of cationic amino acids and / or peptides is preferred. Particularly preferred are arginine solutions.
- the preferred arginine solutions have a concentration of dissolved arginine or arginine derivatives between ⁇ ⁇ and 0.6 mol / l, more preferably between ⁇ ⁇ to 0.3 mol / l and more preferably between 1 mmol and 0.1 mol / l.
- a mechanical distribution takes place the cellulose-based fibers. Stirring devices are preferred for the distribution.
- shear force mixing devices such as rotor-stator shear mixers or colloid mills.
- the cellulose-based fibers suspended and to be hydrated in a water are preferably distributed with a shear force mixer for 2 seconds to 15 minutes, more preferably for 10 seconds to 5 minutes and more preferably between 30 seconds and 2 minutes at any temperature .
- the hydration processes can also partially or completely reverse the partial or total keratinization of cellulose-based fibers.
- the water retention capacity can be determined by methods of the prior art. In one of the methods, the water content of a 0.5 g sample is determined and this suspended in a 100ml Ehenmeyer flask in 50ml of distilled water. After agitation for 1 hour at 20 ° C, the free water phase is freed by application to a G3 glass frit, together with the glass frit, the sample material is centrifuged at 2,000 x g for 15 min. The amount of centrifuged liquid and the sample weight are determined.
- the water retention value (WRR) is calculated according to the following formula
- the hydration volume can be determined by adding the resulting dekompacted cellulose-based fibers (eg 100 g with a water content of 100% by weight) by means of an intensive mixer in a water phase having a neutral pH and a volume ratio to the solid mass of the fibers of> 1: 000: 1 for 3 Minutes are allowed and thereafter, the flow of the unbound water phase through a sieve with a sieving of 50 ⁇ is made possible. After 1 hour, a determination of the volume of space of the cellulose-based fiber mass. Thereafter, mechanical dewatering and then drying to a residual moisture content of ⁇ 10% by weight. Determination of the room volume and calculation of the volume ratio.
- the cellulose-based fibers according to the invention can be functionalized with processes from the prior art with functional compounds which are bound electrostatically and / or covalently to the cellulose-based fibers.
- the effects that can be achieved with such a functionalization include, inter alia, surface effects that can be summarized as anti-static, hydraulic hydrophilic, hydrophobic, oleophilic, amphiphilic, electrostatically with a positive and / or negative surface charge, hygroscopic and / or conductive.
- the establishment of multiple combinations of the aforementioned surface properties is possible.
- the desired surface property and the selection of the compounds which can be used for this purpose depend on the application of the functionalized cellulose-based fibers.
- alcohols or polyols polyvalent alcohols, amino alcohols, other amines, such as betaine, amides, imides, imidazoles, triazoles, melamines, creatine, creatinine, carnitine, further organic acids such as acetic acid, tartaric acid, lactic acid, malic acid , Mandelic acid, gluconic acid, nitriloacetic acid, also fatty acid esters, mono- / diglycerides, phospholipids, glycolipids, glyceroglycolipids, amino acids (especially arginine, lysine and histidine as well as glutamine and glutamic acid), mono-, di- or polypeptides such as the RDG peptide.
- sugar compounds such as dextrose or fructose
- macromolecular surface functionalizations are possible, such as with polysaccharides, such as polydextrins or starch.
- cellulose derivatives such as methyl, ethyl or hydroxycellulose, as well as combinations of these.
- a surface functionalization can also be effected by accumulation of reactive or reaction-promoting compounds in / on the cellulose-based fibers, for example with carbonates, such as, for example, sodium bicarbonate or silicates, for example sodium metasilicate.
- carbonates such as, for example, sodium bicarbonate or silicates, for example sodium metasilicate.
- attachment / incorporation of compounds to / in the cellulose-based fibers in the form of micro / nanoemulsions particularly preferred is the use of nanoemulsions of cationic amino acids or peptides, such as arginine or lysine with organic acids, such as linolenic acid or ascorbic acid.
- the compounds used for surface functionalization are to be dissolved in a suitable solvent (e.g., water, ethanol or acetone) and in an adequate concentration.
- a suitable solvent e.g., water, ethanol or acetone
- a pretreatment of the surfaces for example to increase the reactivity, can be carried out using methods from the prior art, such as, for example, an alcohol, an oxidizing or reducing agent, such as, for example, an acid, an alkali or H2O2.
- a covalent carrier layer can be applied / incorporated, for example by a silane, such as, for example, APTMS.
- moist, dried or dry cellulose-based fibers can be used for surface coating. Preference is given to dried cellulose-based fibers.
- the cellulose-based fibers to be coated can in a solution with coating compounds contained therein are placed or placed in a device where they are flowed through by a solution with coating compounds contained therein.
- the surface coating is carried out in an autoclave at an elevated temperature and pressure. If necessary, it may be necessary to apply high-energy radiation before and / or after the surface functionalization and / or to expose the cellulose-based fibers to an elevated temperature.
- the cellulose-based fibers according to the invention may be in a fresh form or after storage and in moist (ie with a proportion of free and / or bound water phase), dried (ie absence of a free water phase in the presence of a bound water content) or in dry form ( ie a residual water content of ⁇ 5% by weight), be used. They can be used in the forms described above in isolated form or as a moldable mass. Preferred is the use in the form of a moist, brushable and kneadable mass, with a preferred residual moisture of 20 to 100% by weight, more preferably from 30 to 85% by weight.
- a celulose-based pulp produced by a preferred process is preferably completely free of germs, spores or microorganisms, unless they have been introduced / introduced in one of the process steps. Therefore, moist or dried preparations of the cellulose-based fibers are preferably> 2 days, more preferably> 5 days, more preferably> 12 days and more preferably> 21 days after their preparation or after thawing from a frozen phase and under cooled conditions (eg at 6 ° C) and can be used for food.
- Cellulosic fibers can be prepared and used in any of the previously described forms in a wet or dried state as a fresh product, under refrigerated conditions (eg at 6 ° C), with or without evacuation of air, in suitable packaging for a food preparation ,
- the dried or moist cellulose-based fibers are preferably dissolved in water at any temperature, or added to an aqueous preparation or mixed / contacted with other materials for food preparation.
- Such prepared preparations of cellulose-based fibers can be stored virtually unlimited, since there is no risk of perishable in a dry storage.
- To get as fast as possible To ensure hydration / water absorption of the dried cellulose-based fibers, it is advantageous to carry out a fine grinding of the dried cellulose-based fibers.
- the dried cellulose-based fibers in the dried form e.g. B. be used for an application as bread crumbs or a pharmaceutical formulation or in a hydrated form.
- the hydration can be carried out, for example, by adding the dried cellulose-based fiber preparation in water and causing a swelling, the swollen mass can then be used for the application as it is or by collecting in a sieve of the free Liquid phase freed and then used.
- hydration occurring in the aqueous medium of use is also possible.
- Cellulose-based fibers according to the invention can be used in various food preparations. In one embodiment, finished or instant preparation mixtures are prepared herewith.
- the mixture may then be packaged or formulated in the form in which it is obtained, ie in dry, dried or moist form, or it may be converted to another form, for example by drying with warm air and subsequent mechanical comminution a defined grain size.
- the types of process according to the invention can in principle be used with all vegetable starting materials. These may be in the form of immature, ripened, mature, overripe, aged or even damaged vegetable sources. Contaminated or spoiled plant starting materials can also be used for the production and production of cellulose-based fibers according to the invention.
- the vegetable starting material may be in intact form, damaged, crushed, peeled, pressed, ground or otherwise disintegrated.
- meal or flour are suitable.
- shot which arise for example after a mechanical extraction of oils, so-called press cake, are suitable.
- vegetable starting materials which have previously been subjected to a thermal and / or liquid extraction process, eg. With an alcohol or an organic solvent have been subjected to such agents as hexane.
- herbal starting materials in which a thermal treatment has taken place, are suitable.
- This also includes plant products which are obtainable from a digestion and / or fermentation process, in particular if they are residues, such as, for example, brewery residues (for example in the form of spent grains or grain flour), or pomace of must production or olive pomace.
- residues of cocoa beans or sugar beet are residues, such as, for example, brewery residues (for example in the form of spent grains or grain flour), or pomace of must production or olive pomace.
- residues of press residues which are found, for example, in the extraction of juices (for example apple, tomato or carrot juice) or pomace, e.g. B. of grapes or apples or extracts, as in the production of jellies or liqueurs (eg., Blackberry jelly, Cassis) incurred.
- juices for example apple, tomato or carrot juice
- pomace e.g. B. of grapes or apples or extracts
- jellies or liqueurs eg., Blackberry jelly, Cassis
- peel, reveal or gut products of plant starting materials may be used.
- the vegetable starting materials which can be used for one of the processes according to the invention, or from which the cellulose-based fibers according to the invention can be obtained and produced therefore comprise all vegetable seeds, such as e.g. Linseed, poppy seeds, chia, amaranth, chilli, tomatoes, anise, berries; Grains such as oilseed rape, camelina, oats, hemp, wheat, buckwheat, rye, barley, corn, sunflowers, greens, jatropha; Cores, z.
- the cellulose-based fibers produced according to the invention can in principle be used in all areas of life as well as in industrial processes and process sequences.
- the cellulose-based fibers according to the invention are particularly suitable for applications of human nutrition.
- it is suitable as a dietary food additive for a calorie-reduced food preparation.
- the cellulose-based fibers according to the invention are suitable for dietary weight reduction.
- soluble carbohydrates such as pectins or starch
- the cellulose-based fibers according to the invention are suitable for regulating intestinal activity and for altering / softening stool consistency.
- the cellulose-based fibers can be used in animals for chair regulation and dietary weight reduction. Furthermore, cellulose-based fibers according to the invention are suitable for the thickening and stabilization of liquid or flowable foods and food preparations. Cellulose-based fibers produced according to the invention increase the water-binding and retention capacity of food preparations. As a result, these cellulose-based fibers are also suitable for keeping the water content in foods or food preparations longer or keeping them fresh and reducing the risk of dehydration. Further, the produced cellulose-based fibers can be used to introduce and / or stabilize substances / compounds or microorganisms in foods or food preparations.
- labile compounds such as vitamins or antioxidants
- this microorganisms can be introduced into foods that exhibit increased metabolic activity, such as yeasts or lactic acid-splitting bacteria.
- These properties of such cellulose-based fibers can also be used to cultivate algae or other microorganisms and use them to produce substances / compounds or gases with increased efficiency.
- Cellulose-based fibers prepared according to the invention are particularly suitable for the preparation of lotions / creams / ointments or pastes for applications on skin or mucous membranes.
- the cellulose-based fibers are very well suited as release agents for food products / foodstuffs be cooked with high temperature direct or indirect heat, such as roasting, baking, barbecue or deep-frying.
- cellulose-based fibers produced according to the invention are usable as release agents or as substitutes for breading / bread crumbs, for example in preparations of meat or fish and meat or fish products, potato or dough preparations.
- cellulose-based fibers of the present invention are useful for formulating or preserving other nutrients or nutritional ingredients. This is the case in particular in the production of protein products, such as protein concentrates or isolates.
- preparations with oils / fats and / or soluble or complexed carbohydrates or odorous and aromatic substances can also be prepared and / or formulated and / or stored with the cellulose-based fibers according to the invention.
- cellulose-based fibers according to the invention are suitable for effecting a long-lasting moisturizing feeling on mucous membranes. Therefore, cellulose-based fibers are particularly suitable for treating a dry oral mucosa.
- cellulose-based fibers prepared according to the invention are suitable for reducing odors, in particular they are applicable for the reduction or avoidance of bad breath.
- the crude protein content of the samples was determined according to LMBG ⁇ 3 5 L 03.00-27, via the determination of nitrogen by the Dumas method. To convert the nitrogen content into the crude protein content of the samples, the factor 6.25 was used. The determination of nitrogen was carried out with the Leco system FP-528.
- the fat content of the samples was determined according to Caviezel® with the DGF unit method K-1 2c (00). The fat content was carried out with a Buchi B-815 extraction unit and a Buchi B-820 fat estimator.
- Droplet or particle size determinations were made by non-invasive laser light backscatter analysis (DLS) (Zetasizer Nano S, Malvern, UK). For this purpose, 2 ml of a liquid to be analyzed were filled into a measuring cuvette and inserted into the measuring cell. The analysis on particles or phase boundaries forming droplets is automatic. It is covered a measuring range of 0.3 nm to 10 ⁇ .
- DLS non-invasive laser light backscatter analysis
- a quantification of the turbidity (turbidimetry) of the water phases (aqueous emulsions) was also carried out by means of a scattered light detection, in which the re-entry of a scattered beam at 90 ° is determined with a probe immersed in a sample volume of 10 ml (InPro 8200-measuring sensor, M800 -1 transmitter, Mettler Toledo, Germany). The measuring range is 5 to 4000 FTU. There were always duplicate determinations per sample.
- the water binding capacity (WBC) of the cellulose-based fibers was determined at room temperature.
- the implementation of the method was based essentially on the AACC method 56-20. 2 g sample was weighed to the nearest 0.01 g into a centrifuge tube and mixed with 40 ml demineralized water for one minute with a test tube shaker. After 5 min and after 10 min, the mixture was vigorously mixed with the test tube shaker for 30 seconds. It was then centrifuged at 1000 * g and 20 ° C for 15 min. The supernatant was decanted. The centrifuge tube was weighed back. The weight of the water-saturated sample was determined
- the fat-binding capacity of the cellulose-based fibers was determined at room temperature. 3 g were dispersed in a graduated 25 ml centrifuge tube in 20 ml of oil (commercial corn oil). The mixture was then centrifuged at 700 * g for 15 min. The volume of unbound oil was determined. The oil binding capacity is given in ml of oil / g protein.
- the hydrratability of dried or dried fiber fractions was determined by adding 10 g of the material, preferably in the form of a powder or granules, in 100 ml of water (30 ° C., pH 7) and leaving it for 15 minutes. Subsequently, agitation of the mixture and collection of representative samples from the suspension, which are examined for the presence of the Qualifying Characteristic (QM) as follows: 1. Microscopic smear preparation: QM: complete separation of cellulose-based fibers and the absence of adhesions, 2. Fiber analysis using a fiber analyzer (FiberLab FS300, Valmet). QM: presence of contiguous fibers with a maximum space length of ⁇ 2.000 ⁇ , 3. Sensory QM: absence of granularity. Complete hydration of cellulose-based fibers was present when the QM was met.
- QM Qualifying Characteristic
- Aqueous digestion by placing the materials A) and B) in a bath of the digestion compounds at a temperature of a) 25 ° C and b) 60 ° C respectively over 60 Minutes under a continuous stirring mixture, c) further by means of a thermal disintegration in an autoclave at 125 ° C of the materials C) and D) inserted into the digestion solutions for 15 minutes.
- digestion solutions were used: 1. Water, 2. 0.1 N sodium hydroxide, 3. aqueous solution of arginine 0.3 molar, 4. aqueous solution of lysine 0.3 and glutamine 0.2 molar, 5. 30% sulfuric acid solution, 6. 15% solution of sodium bisulfite with NaOH at a pH of 10, 7. 25% solution of SDS.
- the resulting mixtures of free liquid were freed by centrifugation, so that they were present as a solid mass.
- the masses were dissolved in 10 l of water and finely distributed with a mixer for 10 minutes.
- a separation of the water phase was carried out by a vibrating sieve with a screen size of ⁇ ⁇ . From the fractions obtained, samples were taken for analysis.
- the drip-free masses were weighed and then dried in a drying oven. The water binding capacity was calculated from the difference in weight between the wet and dried mass.
- the wet samples were analyzed microscopically for the structure of the fibers and the degree of lumping / clumping with other organic constituents.
- the dry matter obtained was analyzed for the content of readily soluble carbohydrates and proteins (see example methods).
- the number of fibers (pcs) per gram of wet mass, the maximum spatial extent and the aspect ratio were analyzed with a fiber analyzer (FiberLab FS300, Valmet).
- a digestion of the starting materials by water could not be achieved.
- a lye (2.) was a partial digestion of the starting materials A) and B) possible at room temperature, but not with the digestion solutions 5-7.
- An extensive digestion could be achieved with the digestion solution 2. at elevated temperature (A) b) and B) b)) and thermal disintegration (C) and D)).
- the degree of digestion was low to moderate when digestion solutions 5-7 were used.
- Digestion solutions 3 and 4 provided complete digestion and decompaction under all experimental conditions. Microscopically, the methods in which macroscopic complete disruption had not been achieved showed the presence of solid particles and / or fibers that were partially trapped by other organic compounds or constituents and the presence of caking with other fibers or organic compounds.
- the volume of drip-free masses obtained by digestion with digestion solutions 3 and 4 was significantly larger than the volumes of pulping masses after the other pulping processes were carried out. Accordingly, the water-binding capacity was significantly lower (80-190% by weight) in these processes than in cellulose-based fibers obtained with the digestion solutions 3 and 4 (680-850% by weight).
- the dried preparations with a residual content of slightly soluble carbohydrates and proteins of> 2% by weight were very hard and could not be ground to a fine powder.
- the solubility in water was minimal, only a small number of isolated cellulose-based fibers were detected in the dissolution liquid.
- the preparations which had been obtained after drying from a digest with digestion solutions 3 and 4 were well milled to a fine powder.
- the resulting powder was easily dissolved in water to give a soft pulp upon re-constriction.
- the analysis of the dimensions and number of cellulose-based fibers, which were carried out by a digestion process with the digestion solutions 3 and 4, showed a broad and uniform distribution of isolated fibers in a range between 20 ⁇ and ⁇ with a number of fibers from 550 to 237pcs / g and an aspect ratio of 2.5: 1 to 22: 1.
- the length weight was between 0.8 to 2.5 mg / 100m.
- V1 grinding of the starting products to a mean grain size of ⁇ ⁇ .
- air classification with a fine classifier (Netsch CFS 5); V2) grinding of the starting products to a mean grain size of ⁇ ⁇ .
- an aqueous solution in which the following compounds were in dissolved form: a) arginine 0.2 molar, b) histidine and lysine in each case 0.1 molar, c) polyarginine 0.1 molar and glutamic acid 0.1 molar , d) NH 0.2 molar, e) KOH, 0.2 molar, f) urea 0.3 molar, in a weight ratio of 1: 3, so that the starting material completely embedded in the aqueous solution for 4 hours.
- the starting materials are added in not further comminuted form to the following aqueous solutions: a) arginine 0.3 molar, b) polylysine 0.2 molar, c) polyglutamate 0.2 molar and histidine 0.4 molar, d) triethylamine 0 , 2 molar, e) NaOH, 0.2 molar, f) urea 0.3 molar.
- the addition volume of the aqueous solutions was chosen so that complete saturation of the starting material had just occurred. The batches were allowed to stand for 24 hours. Then stir the mixtures in water in a volume ratio of 1:10 and mix with a hand blender.
- the fiber fractions from digestion study V1 contained even larger amounts of on slightly soluble carbohydrates (24-36% by weight) and proteins (18-29% by weight), which were in compacted form.
- contents of easily soluble carbohydrates of 12-22% by weight and of proteins of 14-25% by weight were contained in the fiber pulps obtained.
- the fiber fraction which had been obtained from digestion study V1 could only be partially rehydrated after drying and very rapid sedimentation after filling into the measuring cylinder occurred.
- the powdered fiber fractions prepared from digestion studies V2 with the digestion compounds d) -f) were partially hydrated sufficiently, while the powdered fibers of the digestion experiment V3, which were carried out with the digestion compounds d) - f), only a small Share were hydrated.
- the determined sedimentation time at V2 was 15 - 25 minutes and at V3 4 - 10 minutes for digestion products obtained with these digestion compounds.
- complete hydration of the powdered material of digestion experiments V2 and V3 carried out with the digestion compounds a) -c) was registered.
- the dissolved cellulose-based fibers of these digestion fractions showed a very low sedimentation rate in a graduated cylinder, so that a lowering of the dissolved cellulose-based fibers below the 50 ml mark was present only after 12 to 27 hours.
- the fiber lengths were on average between 150 and 300 ⁇ , the fiber width between 1 1 and 19 ⁇ .
- the fiber length weight was between 1, 2 and 5.1 mg / 100m.
- the following digestion solutions were used: a) water, b) caustic soda 0.2 molar, c) urea 0.2 molar, d) arginine 0.2 molar, e) poly-lysine and histidine 0.2 molar, f) arginine 0, 1 molar and Natruimsulfit 1% by weight.
- the soft masses obtained after the thermal disintegration of test series 1 and 2 were, together with the residual water, mixed with water in the ratio 1: 3 and mixed with a mixer for 5 minutes.
- the hydrated homogeneous mixtures of the test series 1 and 2 were immediately and free of test series 1 .1 and 2.1 after 4 hours with a chamber filter press of free water, so that a residual moisture of 70 to 90% by weight of the condensates was present. These were dissolved in a weight ratio of 1:10 with water with the mixer over 2 minutes, so that a finely divided suspension was present. This was passed through a pass unit. The permeate was concentrated by means of a fine sieve (Siebfrequent ⁇ ⁇ ) and reduced to a residual moisture content of 70% by weight. The same was done with the filter residue. From the fractions obtained analyzes were carried out on the content of readily soluble carbohydrates and proteins (according to Example 1). Furthermore, a tasting according to Example 2 was carried out.
- both the fibers of the permeate and the solids in the filter residue contained more soluble carbohydrates and proteins using a digestion solution b) or c) (12.5 to 27.8% by weight) than was the case with the digestion solutions d) - f) (0.1-0.4% by weight).
- the tasting of the cellulose-based fibers obtained with the permeate showed that in all test series samples obtained with the digestion substances d) -f) were practically odorless and tasteless, while the other samples had a distinctly typical odor. and taste.
- the samples recovered with the NaOH digestion solution additionally had a soapy taste.
- the mean fiber diameters which were present in the permeate when using the digestion solutions b) and c) were in the range of 500 to 850 ⁇ (range 10 ⁇ to 2200 ⁇ ) and those using digestion solutions d) - f) were between 250 and 350 ⁇ in a range between 10 and 1 .800 ⁇ .
- 500g of the following starting materials were used for each study: 1) rapeseed press cake, 2) soya press cake, 3) jatropha press cakes, 4) carrots, 5) pumpkin, 6) celery.
- the digestion solutions used were: a) arginine 0.1 molar, lysine 0.1 molar, glutamic acid 0.1 molar; b) Polylysine 0.3 molar, c) arginine 0.3 molar; d) histidine 0.2 molar, lysine 0.1 molar, valine-isoleucine peptide 0.2 molar.
- the starting materials were treated according to 2 routes:
- Route A) Loading the starting materials 1) - 3) into one of the digestion solutions in a weight ratio of 1: 1.5 for 4 hours at 25 ° C. After this, the mass was distributed in tap water in a weight ratio of 1: 8 by means of a colloid mill with which an intensive mixture was carried out for 5 minutes. Subsequently, the mixture was placed on a vibrating screen with a sieve size of 200 ⁇ and the sieve residue separated and reduced with a filter press to a residual moisture content of 70 to 90Gew%. The resulting press residue was then suspended 2 times in a weight ratio of 1:10 with tap water with a hand blender for 3 minutes and distributed, followed by first dehydrating with the vibrating screen and then with the filter press as before.
- Route B Loading the starting materials 4) - 6), which had been shredded into 2 cm thick pieces, into the digestion solutions in a weight ratio of 1: 0.8 in a container, which was placed in an autoclave. This is a pressurization of 1, 8 bar and a heating to 125 ° C for 5 minutes. Then removal of shell portions at 5) and 6). A free water phase is removed by means of a vibrating screen. The sieve residue is mixed intensively in a weight ratio of 1:10 with tap water by means of a colloid mill for 5 minutes. Subsequently, the mixture was placed on a vibrating screen with a sieve size of 200 ⁇ and the sieve residue separated and reduced with a filter press to a residual moisture content of 70 to 90% by weight. The resulting press residue was then dissolved and distributed twice in a weight ratio of 1:10 with tap water with a hand blender for 3 minutes, and then first with the vibrating screen and then with the filter press, as previously dewatered.
- cellulose-based fibers By using the digestion solutions, and without any simultaneous disintegration of the starting material, cellulose-based fibers could be removed from all starting materials and freed from the other constituents of the starting materials. Thus, between 0.1 and 0.3% by weight of soluble carbohydrates and between 0 and 0.3% by weight of proteins were detected in the resulting fractions of cellulose-based fibers.
- the fiber dimensions of the cellulose-based fibers obtained from route A) tended to be slightly larger than those obtained from the process of route B) (mean maximum diameter 120 ⁇ to 360 ⁇ vs. 40 ⁇ to 290 ⁇ ; distribution of the maximum fiber diameter between 20 ⁇ and 1480 ⁇ vs. 10 ⁇ and 980 ⁇ ).
- the fiber length weight was between 0.8 and 3.1 mg / 100m.
- the materials to 1) to 3) were first placed in a disinfecting bath (DMSO 10% by weight, ethanol 20% by weight) for 2 hours and then rinsed with water.
- a disinfecting bath DMSO 10% by weight, ethanol 20% by weight
- wet grinding was carried out with a colloid mill adding one of the following digestion solutions in a volume ratio of 2: 1: a) arginine 0.1 molar, leucine-alanine 0.1 molar; b) histidine, poly-arginine; c) lysine 0.2 molar, valine 0.1 molar, glutamine 0.1 molar; d) arginine 0.1 molar, lysine 0.1 molar, leucine 0.1 molar; e) NaOH 0.1 normal; f) H 2 O.
- the suspensions were fed to a pass unit to separate uncut materials having a particle size of> 5 mm.
- the permeate was placed in an autoclave and disintegrated at 120 ° C and a pressure of 2 bar for 6 to 10 minutes.
- the resulting masses were homogenized in a ratio of 1: 3 (v / v) with water by means of a shear mixer for 2 minutes.
- the resulting viscous suspensions were filled in PP filter cloths and placed in a chamber filter press with a Pressed pressure of 400kg / m 2 over 5 minutes.
- the filter residue was homogenized twice with a dilution volume of 6 liters each with the blender and dehydrated as before with the filter press.
- the obtained cellulose-based fiber material was taken for analysis of the fiber dimensions and fiber weight (according to Example 1), the content of proteins and readily soluble carbohydrates (according to Example 1) as well as for culturing to determine a microbial colonization.
- the obtained cellulose-based fiber fractions after use of the Aufsch thoroughlyatesen a) to d) had a mean fiber diameter of 150 ⁇ to 400 ⁇ , with a distribution between 105 ⁇ and 1 .500 ⁇ .
- the fiber length weight was between 1.4 and 3.9 mg / 100m.
- Levels of protein and soluble carbohydrate contents of ⁇ 0.5% by weight were determined.
- the mean fiber diameter when using the digestion solutions e) and f) was 850 ⁇ or 1 .200 ⁇ at a distribution between 150 ⁇ and 3,400 ⁇ .
- Levels of slightly soluble carbohydrates and proteins between 12 and 35% by weight were determined.
- the microbiological tests showed that no growth of bacteria or fungi occurred in all samples obtained with the digestion solutions a) to d) in an observation period of 2 weeks.
- the starting materials 1 and 2 were formed using the digestion compounds d) and e), and the starting material 3 was found to be fouling bacteria, and further, the preparation 4 had a rancid odor. This was not the case for the cellulose-based fibers obtained with the digestion solutions a) -d).
- the starting materials were roughly cut and softened in a water bath for 30 minutes to 2 hours at 90-95 ° C, so that the fragments could be crushed with fingers. Bowls, kernels and husks were then removed and the still hot fragments minced with a shear mixer (Ultrathurrax 25T, Germany) for 2 minutes at 20,000rpm. Thereafter, the addition of tap water in a ratio of 8: 1 to 12: 1 and a new homogenization with the Schernnischer for 5 minutes. After that, a water removal by means of a chamber filter press.
- the cellulose-based fibers were dewatered and tasted by means of a Fliterpresse to a residual moisture content of 70-80%.
- the tasting included a smell and taste test by 4 experts. Through this, a sensory examination was carried out on, among other things, taste neutrality, softness, mouthfeel and a feeling of swallowing.
- the preparations prepared with Digestion Solutions 1 and 6 had very low and greatly retarded solubility as well as a faster settling rate than the dried and ground cellulose-based fibers made with Digestion Solutions 2-5. the case was.
- the cellulose-based fibers produced by digestion solutions 2-5 were completely taste neutral, had a high degree of perceived softness, a pleasant mouthfeel, and an undisturbed sense of swallowing.
- the fractions prepared with the digestion solutions 1 and 6 there was a distinctly art-like taste and smell, and there were also significantly lower ratings for softness and mouthfeel than in the evaluation of the cellulose-based fibers used with the digestion solutions. 5 was the case. With swallowing it came with these preparations (1 and 6) further to a Kratzvorfinden in the neck.
- Example 7 Investigation of the surface coatability and the establishment of a surface functionalization layer in cellulose fibers and cellulose-based fibers.
- each of the powdered fibers was returned to samples for analysis and 2 g each in 50 ml of an aqueous solution of A) polyethersulfone (10%), B) PEG 200 (15%), C) sodium lauryl sulfate (2.5%). ig), D) a nanoemulsion of arginine 0.2 molar and oleic acid 0.1 molar and E) water and stirred for 3 hours. Subsequently, the pulp masses were separated from the solutions by means of a fine sieve and redissolved twice in water for 5 minutes and then concentrated. Finally, drying took place in a vacuum drying oven at 45 ° C. for 48 hours.
- the resulting dry masses were reground and subsequently split into fractions which, like the recovery samples of the starting materials, were placed in fluorescent dye solutions having a hydrophilic (green fluorescent protein (GFP) or hydrophobic (Nile red) compound dissolved therein for 2 hours and then abundantly rinsed with water.
- the binding of the fluorescence markers was quantified by means of a suspension of the labeled fibers by means of a flow-through fluorescence analyzer and normalized to the detected particle number.
- the investigated cellulose-based fibers had a higher coverage rate for surface coating than for uncoated cellulose fibers (SK + 160%, RPK + 180%, AF + 120) for both the hydrophilic and the lipophilic fluorescent dye %).
- After surface modification there was a marked increase in the surface coverage of cellulose-based fibers, which compared to cellulose fibers by 360 ⁇ 35%, 220 ⁇ 40%, 420 ⁇ 41%, 680 ⁇ 23% for A), B), C ) and D) was greater for the lipophilic marker than for cellulose fibers and for 480 ⁇ 60%, 550 ⁇ 35%, 260 ⁇ 50% and 180 ⁇ 35% for A), B), C) and D) for the hydrophilic Marker was greater than cellulose fibers or compared to cellulose-based fibers that had not been surface-modified, with an increase of 120%, 100%, 240%, 310% for A), B), C) and D) for the lipophilic marker and by 250%, 320%, 140% and 90% for A
- Example 8 Investigation into the production of cellulose-based fibers from organic starting materials.
- the pulps were dissolved in water in a volume ratio of 1:10 and pumped through a hydrocyclone (Akavortex, AKW, Germany). The upper course was collected and filtered (Siebrete ⁇ ⁇ ) by means of a curved screen. The sieve residue was analyzed and used for the study.
- the resulting masses were suspended in a weight ratio of 1: 5 in an aqueous solution containing a) arginine 0.3 molar, b), poly-lysine, urea 10%), c) arginine 0.1 molar + NaSO3 1% and the Suspension treated in an autoclave for 8 and 16 minutes at a temperature of 120 ° C.
- the digestion result was filtered and rinsed 2 times exhaustively with water. From the final sieve residue, samples were taken for analysis.
- the suspensions were stirred in a series of experiments (T60) for 24 hours at 60 ° C and treated in another series (T120) for 8 minutes at 120 ° C in an autoclave.
- T60 series of experiments
- T120 another series
- the resulting suspensions were filtered and rinsed twice with water. From the final sieve residue, samples were taken for analysis.
- the analysis carried out included the analysis of the size distribution of the cellulose-based fibers, the content of slightly water-soluble proteins and carbohydrates (according to Example 1), investigations on the solubility of dyes (test by incorporation of the test fraction in water and aqueous surfactant solutions with 48 hours) subsequent filtration and spectroscopic analysis of the filtrate) and a sensory evaluation by 4 experts according to the criteria of Ex. 4.
- Series II The fiber analysis showed that the treatment resulted in a comminution of complexes of cellulose-based fibers, which had a clearly shifted to the left diameter spectrum, particles with a diameter of> 2.000 ⁇ were not or in a proportion of ⁇ 0.1% before.
- Series III From the obtained masses of cellulose-based fibers of both the test series T60 and T120 no dyes could be dissolved out more by aqueous solutions.
- cellulose-based fibers had a content of slightly water-soluble proteins and / or carbohydrates of ⁇ 0.1% by weight.
- Example Experiments 1-3 RF-V, KaF-V, HF-V, kuF-V
- the digestion was not carried out with an amino acid and / or peptide solution
- the viscosity of the suspension was determined 3 times with a viscometer (Krüss, Germany) and the mean was calculated. Thereafter, the water content of a 0.5 g sample was determined and this suspended in a 100 ml Erlenmeyer flask in 50 ml of distilled water.
- the free water phase is freed by application to a G3 glass frit, together with the glass frit, the sample material is centrifuged at 2,000g for 15 min. The amount of centrifuged liquid and the sample weight are determined. The water retention value (WRR) was calculated as indicated under "Methods.” The remaining mass was redissolved in tap water under agitation at 25 ° C and agitation paused every 5 minutes and viscosity was determined, which was carried out consecutively.
- the cellulose-based fibers produced according to the invention caused a higher viscosity of the suspensions than cellulose fibers and cellulose-based fibers which had not been treated with the amino acid and / or peptide solutions.
- the water retention capacity could not be determined for the cellulose preparations due to the method.
- the WRR was significantly greater in the cellulose-based fibers produced according to the invention than in the cellulosic fibers and also greater than in cellulose-based fibers which had not been produced according to the invention.
- the restoration of the colloidal properties could be achieved with the cellulose-based fibers produced according to the invention just as quickly as with hydroxy-celluloses, in the vegetable cellulose fibers and the cellulose-based fiber not according to the invention required a much greater time required for this purpose. While in cellulosic fibers and cellulose-based fibers not according to the invention, phase separation after mixing with a lipophilic phase occurred very rapidly, a stable mixture was the longest possible with the cellulose-based fibers produced according to the invention.
- Dried (TB) and a residual moisture of 50% by weight containing (NB) cellulose-based fibers of soybean (SF) and beans (BF) prepared according to the examples 1 (arginine method c)) and 4 with amino acid and / or peptide solutions were dissolved in an aqueous suspension with baker's yeast (BH), a sourdough kit (ST) containing, inter alia, Saccharomyces cerevisiae, Lactobacillus plantarum and Lactobacillus brevis, and further a solution of sodium bicarbonate (NHC) and at 25 ° C (BH + ST) or 10 ° C. (NHC) for 2 hours (coating A).
- BH baker's yeast
- ST sourdough kit
- the cellulose-based fibers were freed with a pocket-chamber filter press to a residual moisture content of between 40 and 50% by weight of free and bound liquid.
- the fiber masses were suspended in different solutions (coating B): 1) vitamin C 10 % By weight, 2) citric acid 10% by weight, 3) oat protein concentrate (60% by weight) 10% by weight suspension, 4) soy protein isolate (90% by weight) 10% by weight suspension with glucose 3% by weight for 10 minutes 10 ° C stirred. Then dewater the cellulose-based fiber fractions through a filter press.
- Experimental series 1 In each case 50 g of the individual preparations were placed for 1 hour in a mixture of 50 ml of water and 50 ml of milk with 2 g of sugar at a temperature of 25 ° C and occasionally stirred. The suspensions were each added with 200 g of wheat flour and 1, 5 g of salt and kneaded into a homogeneous dough and formed into rolls. The baking process was started after 2 hours and was carried out under the same conditions for all samples.
- Test series 2 In each case 100 g of the individual preparations were placed for 2 hours in 150 ml of water at a temperature of 25 ° C.
- the masses were each added with 250 g of a bread flour mixture and 2 g of salt and kneaded into a homogeneous dough and formed into a loaf of bread.
- the baking process was started after 24 hours and carried out for all samples under the same conditions.
- Test series 3 10 g each of the individual preparations were each mixed with 250 g corn flour, 10 g sugar, 1 g salt and then 250ml milk, 1 egg and 40 g butter incorporated, so that a viscous homogeneous dough was formed, which was filled into molds.
- the baking process was started after 10 minutes and carried out for all samples under the same conditions.
- test series were also carried out with yeast (VS1), sourdough (VS2) and NHC (VS3) instead of the preparations.
- yeast VS1
- VS2 sourdough
- NHC VS3
- OFB area
- EDS indentation stability
- the quantitative measurements were set in relation to the results of the reference baking samples and are given as a relative value in Table 2.
- the coherent aggregates are comminuted by grinding with a grinding mill to particles of ⁇ 0.3 mm.
- 1 g of the ground fibers are added to the following nutrient media: skimmed milk for the preparations loaded with A) and B) and a glucose solution for preparations loaded with C).
- the suspensions were stirred continuously at 30 ° C.
- the pH of the suspensions was monitored and the values determined after 1 and 3 hours.
- a suspension with a cell number was added to the nutrient media in a series of experiments, as it had been used to load the fibers. The course of the pH measurement result was determined as the reference value and the pH values obtained with the fiber preparations were related to this.
- the enzymatic activity of the microorganisms which had been loaded on the cellulose-based fibers developed differently over time, the activity after 1 hour between 55% and 75% of the activity of the reference experiment and was after 3 hours between 180% and 240% above the activity in the reference experiment.
- the activity of the microorganisms was between 22% and 35% compared to the reference experiment, compared to the reference experiment. Hour and between 60% and 75% after the 3rd hour.
- TM carrier materials
- SF celulose-based fibers of soybean
- SBF sunflower
- KF pumpkin
- WF methylhydroxypropylcellulose and hydroxyethylcellulose
- MC 1 and MC 2 methylhydroxypropylcellulose and hydroxyethylcellulose
- SP protein concentrates
- SP soy protein
- RP rape protein
- MP milk protein
- the protein-containing permeate was treated with an organic acid (including citric acid), resulting in an aggregation of proteins, which were obtained by filtration and free water shares up was freed to a residual moisture content of 50-70% by weight, so that a spreadable material was obtained.
- Part of the protein fraction thus obtained was spray-dried and then in a powdery consistency.
- the MP corresponded to a commercially available powdered milk protein concentrate.
- TM with the PK was carried out according to the following modalities: 1. TM with a moisture content of 70-80% by weight and PK with a residual moisture content of ⁇ 5% and 2. TM with a residual moisture content of ⁇ 5% by weight and PK with a moisture content of 80-90% by weight are kneaded together. In all approaches, dry weight ratios of 1: 5 (TM: PK) were used. The substances were mixed by means of a kneading / stirring device until a fine to coarse-grained substance mixture having a residual moisture content of ⁇ 40% by weight was obtained. This was dried at a temperature of 50 ° C until a residual moisture of ⁇ 8% by weight. This was followed by fine grinding with a grinding mill.
- preparations A) and B) were cooked under standardized conditions, preparation A) was in the heated state, preparation B) in the cooled state after 6 hours and preparation C) tasted immediately after receipt by 4 experts and including the following properties on a scale of 1 (very bad / little) to 10 (very good / much) rated: for A): product cohesion (PZ), chewability (Z); for B) product cohesion (PZ), stickiness (K); for C) Creaminess (S), Fattening (M), the sensory dexterity, such as fiberiness / graininess (FK) and mouthfeel (MG) were evaluated for all.
- the cellulose preparations and the protein preparations did not mix with any of the two modalities to a uniform mass, it formed lumpy inclusions, which could be partially resolved only by adding a large volume of dilution and a long entry time, the subsequent investigations were therefore not performed.
- the following composition of the fraction fractions could be determined: protein content 58 to 76% by weight, insoluble carbohydrates 24 to 41% by weight, soluble carbohydrates 0.2 to 2.3% by weight, fats ⁇ 0.01 to 0 , 8% by weight.
- proteins from the cellulose-based fibers were enclosed for both production modalities of the supported protein preparations and were mixed with these agglomerated proteins. were merited. There were only a few particles of proteins that were not bound to cellulose-based fibers or were contiguous. In contrast, the proteins were predominantly in condensed form when using cellulosic fibers derived from husk or stem mass as TM.
- stickiness to cellulose fibers consisted of husks or stalk material, while using cellulose-based fibers as TM was not. Patties made with cellulose-based fibers as TM exhibited the best cohesion and best chewability, while patties made with husk and stem cellulosic cellulite broke apart during cooking as well as hard aggregates, which led to a negative evaluation during the tasting.
- preparation B In the preparation of preparation B), the miscibility of protein foam was significantly better for the doughs made with cellulose-based fibers than TM, to obtain and more uniform distribution of air bubbles, this was on doughs with cellulose fibers, the Husk or stem material were made, not the case. According to Garung, preparations made with cellulose-based fibers as TM showed a significantly greater cohesion of the dough mass and a lower stickiness than was the case with preparations using cellulosic fibers from husk or stem mass had been. In the preparation of preparation C), cellulose fibers made from husks or stalk pulp did not stabilize the foam by the steam treatment, whereas in the case of preparations made with cellulose-based fibers very good stabilization came. In the sensory evaluation, the preparations using cellulose-based fibers as TM were judged to be significantly creamier with less fattening to preparations than the preparations prepared from ciliated or stem cellulosic cellulosic fibers.
- the stored samples had no change in their physical properties over 12 months. There was no microbial load on the samples.
- the solubility in water of the stored preparations and the qualitative and sensory properties of the preparation products prepared with the stored samples corresponded to the results given here, which were obtained with these preparations immediately after their preparation.
- Example 13 Investigation into the industrial production of baked goods made from / with cellulose-based fibers.
- the dough mass is pumped by means of a screw pump into a filling device, with which a defined volume of the mass is placed in the molds of a device. After filling, the mold is closed by a vapor permeable counterpart, so that the dough masses to a 3 mm thin slices (diameter 5 cm) in the form enclosed by this all around form. Subsequently, heat the entire mold plate to 140 ° C for 5 minutes.
- the chips falling out when the molds are opened are conveyed with a belt into an oven in which they are heated to 180 ° C. for 2 minutes.
- the cooled chips are then air-tight and vapor-tight packed in an anhydrous nitrogen atmosphere. It will receive 31 kg of chips.
- a visual, tactile and sensory examination takes place after a storage period of 2, 6 and 12 months.
- the appearance remained unchanged, as well as the fracture behavior and the surface texture.
- the consistency was evaluated as tasting at all times as cross and a pleasant mouthfeel stated. It came in the course of storage to no change in the taste characteristics.
- the flowable dough was filled into bakeware with a diameter of 30 cm, 2 cm high and baked at 180 ° C for 20 minutes. After cooling, the biscuit trays were dissolved out and packed in a nitrogen atmosphere in airtight and vapor-tight. A visual, tactile and sensory examination takes place after a storage period of 2, 6 and 12 months. The appearance remained unchanged, as well as the indentation resistance and the surface finish. The consistency was judged to be slightly cross at the tasting at all times and the mouthfeel was stated as soft and rounded. It came in the course of storage to no change in the taste characteristics.
- A) Original fondant recipe Swell 12 g of gelatine in 60 ml of water and then gently heat it by stirring in 10 ml of glycerine, 1 g of salt and flavorings and 90 g of melted Palminfett. 1000 g of powdered sugar are mixed into the mixture and finally kneaded into a homogeneous dough.
- the formulation is changed by exchanging 50 or 90% by weight of the original amount of powdered sugar for the preparations with a residual moisture content of 20% by weight, or 5 and 9% by weight, against cellulose ethers.
- the dough masses obtained are stored airtight over 24 hours and then processed or evaluated after renewed kneading.
- preparations were prepared and evaluated with the specified amount of sugar.
- the preparations were tested 24 times twice in alliance with 4 experts.
- the following sensory parameters were assessed according to a rating scale from 1 (very low / very poor) to 10 (very high / very good): a) sweetness intensity (Sl), mouthfeel (SG), mouthfeel (MG), spreadability / processability (V), dimensional stability (FS).
- Cellulose preparations proved to be unsuitable for the preparation of the preparations B) and C), it produced sticky, unprocessable masses.
- the test series R90 could not be completed with the cellulose preparations WF and HC, since the preparations A) and D) could not be processed.
- the sensation of sweetness was low due to the cellulose-based fibers and greatly reduced by cellulose fibers from husks and cellulose preparations.
- Cellulose-based fibers improved the processability of the preparations with increasing exchange ratio to the sugar used.
- the mouthfeel could be improved by cellulose-based fibers compared to the reference products of formulations A) to C), whereas this deteriorated when using cellulose fibers.
- the flour content (MG) (wheat flour type 405) or corn starch (SG) (corn starch) of the following food products: A) pizza dough, B) pasta dough, C) potato dumplings, D) waffles were reduced by 50% (series R50) and 90% (test series R90) exchanged with the following preparations: cellulose-based fibers (prepared according to Examples 3 V2) e) and 4) of camelina (LF) and soybean (SF), cellulose fibers of oat hulls (HF) and methylhydroxypropyl cellulose (MHC).
- Production instructions (A) 500 g of flour, 500 g of flour, 10 g of yeast, a pinch of salt and 3 tablespoons of olive oil were added to each 500 g of flour and kneaded to a homogeneous dough; B) for each 300g of flour, 1 pinch of salt, 3 eggs and 2 tablespoons of olive oil were added and kneaded to a firm dough; C) For every 100g of cornflour, 500g of pre-cooked and crushed potatoes, 1, 5g of salt, 2 egg yolks, 50 butter and spices were added and kneaded to a moldable dumpling dough; D) For each 300g of food starch, 2 g sodium bicarbonate, 50 g sugar, 100 g butter, 100 ml milk and 3 tablespoons vegetable oil were added and stirred to a homogeneous flowable dough.
- the following sensory parameters were scored according to a rating scale from 1 (very low / very bad) to 10 (very high / very good): a) Fatigue (MI), mouth stickiness (MK), mouthfeel (MG), chewability (Z ), Dimensional stability (FS).
- MI Fatigue
- MK mouth stickiness
- MG mouthfeel
- Z chewability
- FS Dimensional stability
- Preparations made with cellulose-based fibers as a substitute for flour or cornstarch showed less adherence and stickiness to molds or preparation tools than do formulations made with flour or starch or cellulose fibers made from husk material or those prepared with cellulosic preparations , Preparations with MHC were sticky.
- the preparations prepared with cellulose-based fibers exhibited greater cross-over in formulations A) and D) and less delamination of dough components of formulations B) and C). compared to the other preparations.
- the tasting revealed a better overall evaluation of the preparations made with cellulose-based fibers compared to the other preparations. In the case of the individual evaluations of features, this particularly concerned a lower fatigue sensation, a more comfortable chewability, a lower stickiness when chewing the preparations and the absence of a dry mouthfeel.
- the results of test series 1 and 2 almost coincided.
- the still warm mass is kneaded together with 100 g cocoa butter and 200 g cocoa mass to a homogeneous mass; D) 200g block chocolate are melted and then 250g soft butter, 200g melted palm fat and 250g powdered sugar, 50ml water, 0.5g salt and flavors mixed and stirred at low heat until a homogeneous viscous-flowing mass.
- Deviating from preparations with the examined preparations are prepared by replacing 50 or 90% by weight of the original amount of fats against the preparations with a residual moisture content of 10% by weight (Series 1) and with a residual moisture content of 30% by weight (Series 2).
- HC hydroxycellulose
- 10% of dry matter were used, ie 5 and 9% by weight. If necessary, water was added to the preparations or these were hydrogenated in order to achieve a comparable consistency.
- preparation A was carried out after cooling after the standardized baking process, that of the preparations B) and C) immediately after their preparation and that of the preparation D) 24 hours after application to a cake base.
- Preparation A) fragility, softness
- Preparation B), C) and D) Homogeneity, dimensional stability after extrusion from a spout with a fine star-shaped outlet, spreadability.
- Preparation B) fragility, softness
- Preparation B), C) and D) Homogeneity, dimensional stability after extrusion from a spout with a fine star-shaped outlet, spreadability.
- an allied tasting was carried out by 4 experts.
- Cellulose-based fibers caused a lower brittleness of the preparation A) compared to the original formulation or a fat substitute of cellulosic fibers from stalk mass or by methylcelluloses. There was the same softness as when using the full amount of fat and a greater softness compared to preparations in which cellulosic fibers or methylcellulose had been used.
- preparations B), C) and D the greatest homogeneity in preparations made with cellulose-based fibers was compared with the use of the other preparations. Extrusion through a spout with a narrow outlet was possible well and evenly only by preparations using cellulose-based fibers.
- the desiccation of food preparations was investigated on the following preparations: A) dumpling dough, B) pasta dough, C) noble marzipan, D) butter cream from Examples 14-16. From the doughs / preparations according to the original formulation as well as the cellulose-based fibers and cellulose fibers, which were made of glaze or stick mass, as well as cellulose preparations, spheres of 1 cm in diameter were formed and weighed. The preparations were stored for 48 hours at 25 ° C under room air conditions. They were then weighed and their surfaces examined for their appearance, consistency and properties.
- the surfaces of these preparations showed no (test series R90) or only small (test series R50) color changes, which were caused by a drying.
- the preparations which had been prepared according to the original formulation and with the comparators showed moderate to marked changes in color.
- crust formation in the sliced preparations prepared according to the original formulation or with cellulose fibers or cellulose preparations was to a moderate or pronounced degree, whereas in the case of the preparations made with cellulose-based fibers it was only minimal (R50). or nonexistent (R90).
- Diet 1 protein content 70% by weight, digestible carbohydrates 20% by weight, indigestible carbohydrates 8% by weight, fat ⁇ 1% by weight, minerals / vitamins 1% by weight.
- Diet 2 protein content 70% by weight, digestible carbohydrates 8% by weight, indigestible carbohydrates 20% by weight, fat ⁇ 1% by weight, minerals / vitamins 1% by weight.
- the indigestible carbohydrates of diet 2 consisted of the following preparations: a) fluffed shell, b) wheat husk fiber (75 ⁇ ), c) cellulose-based fibers of carrots, d) cellulose-based fibers of pumpkin, e) hydroxy-methyl cellulose ether ( HMC).
- the proteins and indigestible carbohydrates were formulated together according to the procedures described in Example 12. Between diet periods, the dietary fiber-rich standard diet, which is also used for preparation, was consumed for 5 days. Abdominal complaints (AB), painful intestinal gas production (DG), stool frequency (SF) and stool consistency (SC) were recorded.
- diet 2 a) to e) was continued for 2 subjects each for 4 weeks (long-term use).
- stool samples were analyzed for lactate, acetate and microbiome content after 14 days of preparation and after long-term use.
- a dietary supplement containing cellulose-based fibers was found in 10 people with symptoms of chronic irritable bowel syndrome (including, for example, abdominal discomfort, irregular stool frequency) over a period of 4 weeks.
- 10 g (TG) of various cellulose-based fibers (including soy, pumpkin, camelina) per day were incorporated in the individual food preparations, such as, for example, In a spread, a milk or fruit juice beverage, a sauce or in a patty, or in addition to these, taken by the participants to themselves.
- Attendees were required to document their abdominal discomfort and bowel habits during an initial 14-day documentation phase, and to eat and follow their diet, as in the subsequent 4-week take-up phase of the cellulose-based fibers, during which this documentation was continued.
- 500 kg of dried corn pellets are filled into a kettle with 800 liters of a 0.1 molar arginine solution and the kettle contents are stirred for 2 hours at 85 ° C. Subsequently, the heated slurry is conveyed by means of a screw pump through a pipeline into a colloid mill. The feed line is continuously fed in a volume ratio of 8: 1 water. The mixture is conveyed to a colloid mill at a flow rate of 500 L / h and a pressure of 1 bar. The outlet of the colloid mill is connected to a pipeline which, by means of a pump, directs the suspension into a hydrocyclone plant.
- the suspensions of the upper (OL) and lower (UL) are directed to separate Vibrationssiebvorraumen (screen size each ⁇ ⁇ ).
- the sieve residue of OL was charged to a reaction vessel and suspended with water in a weight ratio of 1:10 by means of a shear mixer apparatus at a temperature of 45 ° C for 10 minutes. Subsequently, with continuous mixing of the suspension, an line via a pipeline to a vibrating sieve (screen size 200 ⁇ ).
- the sieve residue is fed by means of a conveying device of an application device of a vacuum belt screening machine, through which an order of the cellulose-based pulp is applied to a polypropylene screen (screen size of 80 ⁇ ) with a layer height of 1, 5 cm.
- the mass has a residual moisture content of 30-40% by weight.
- the easily separable mass is distributed on sieve pallets, which are stacked on top of each other.
- the pallet stack is moved into a vacuum drying oven in which the cellulose-based fiber mass is dried to a residual moisture content of ⁇ 10% by weight.
- a fine grinding with a disc mill.
- the sieve analysis gives an average particle size of 0.2 mm on average. The particles dissolve quickly in the mouth or in water and are odorless and tasteless.
- a content of slightly soluble carbohydrates of 0.25% by weight and a content of readily soluble proteins of 0.1% by weight are determined.
- the water binding capacity (determination according to Example 1) is 660% by weight, the water retention capacity (determination according to Example 9) is 61%.
- the Siebschreibstand from the UL is washed twice with water in a volume ratio of 1: 5 and then dried on a belt filter device and sent for further use.
- the filter permeate of the process stages is combined and sent to a settling tank, from which the water clarified by settling is reused for further process operations.
- the sediment of this settling process is separated and dried by means of a belt sieve and fed to a further utilization.
- step a) disintegration of the vegetable starting material from step a) by a thermal and / or mechanical digestion process
- a method according to any one of items 1-9 wherein recovered and / or produced cellulose-based fibers containing functional groups and compounds in which at least one of the elements nitrogen, phosphorus, sulfur, sodium, chloride, calcium, magnesium , Zinc, copper, iron or manganese is included. 1 1.
- Cellulose-based fibers prepared by a process according to any one of items 1-15 for use as oil / fat replacer.
- Cellulosic fibers produced by a method according to any one of items 1-15 for the formulation of dissolved or soluble proteins.
- Cellulose-based fibers produced by a process according to any one of items 1-15, as a separating agent of cooking products intended for a roasting, baking, grilling or frying process.
- Cellulose-based fibers produced by a process according to any one of items 1-15 for the preservation and preservation of compounds and / or substances and / or organisms.
- Cellulosic fibers produced by a method according to any one of items 1-15 for the incorporation and formulation of compounds, lotions and / or creams and / or ointments and / or pastes.
- Cellulosic fibers prepared by a method according to any one of items 1-15 for the treatment of constipation and / or regulation of bowel motility and / or stool consistency.
- Cellulosic fibers prepared by a method according to any one of items 1-15 for stimulating salivation and / or reducing unpleasant halitosis.
- Cellulose-based fibers prepared by a process according to any one of items 1-15 for the binding of odorants and flavorings.
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Abstract
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DE102017003176 | 2017-03-28 | ||
EP17207166 | 2017-12-13 | ||
PCT/EP2018/057843 WO2018178121A1 (de) | 2017-03-28 | 2018-03-27 | Desintegrierte und dekompaktierte cellulose-basierte pflanzenfaserstoffe. verwendung und verfahren zur gewinnung und herstellung |
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US (1) | US11525013B2 (de) |
EP (1) | EP3599893A1 (de) |
AU (1) | AU2018241915B2 (de) |
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EP3942110B1 (de) * | 2019-03-20 | 2023-10-04 | Roberto Nusca | Verfahren und vorrichtung zur behandlung von pflanzlichem material zur verwendung als füllmaterial für synthetische und/oder natürliche rasen |
US11802838B2 (en) | 2020-03-23 | 2023-10-31 | Bay State Milling Company | Rapid high amylose wheat seed purity test |
EP4185123A1 (de) * | 2020-07-22 | 2023-05-31 | Herbstreith & Fox GmbH & Co. KG Pektin-Fabriken | Verwendung einer aktivierten karottenfaser zur herstellung von erzeugnissen |
CN112741259B (zh) * | 2021-01-13 | 2023-05-05 | 江西博君生态农业开发有限公司 | 一种蜜桔粗粮米粉制备用糅合装置 |
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JPS57206344A (en) * | 1981-06-12 | 1982-12-17 | Daicel Chem Ind Ltd | Cellulose sulfate gel composition |
US4923981A (en) | 1982-09-03 | 1990-05-08 | Sbp, Inc. | Use of parenchymal cell cellulose to improve comestibles |
FR2730252B1 (fr) * | 1995-02-08 | 1997-04-18 | Generale Sucriere Sa | Cellulose microfibrillee et son procede d'obtention a partir de pulpe de vegetaux a parois primaires, notamment a partir de pulpe de betteraves sucrieres. |
US6379446B1 (en) * | 2000-04-03 | 2002-04-30 | E. Khashoggi Industries, Llc. | Methods for dispersing fibers within aqueous compositions |
US20040009263A1 (en) * | 2001-02-02 | 2004-01-15 | Jingping Liu | Methods for extracting corn proteins from corn gluten meal |
US7094317B2 (en) * | 2002-11-06 | 2006-08-22 | Fiberstar, Inc. | Process of manufacturing and using highly refined fiber mass |
CA2803863A1 (fr) | 2013-01-25 | 2014-07-25 | 9198-4740 Quebec Inc. (D.B.A. Ventix Environnement Inc.) | Procede d'extraction de cellulose |
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US11525013B2 (en) | 2022-12-13 |
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AU2018241915B2 (en) | 2023-10-26 |
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