EP3947567A1 - Procédé de production de particules de lignine ultrafines - Google Patents

Procédé de production de particules de lignine ultrafines

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Publication number
EP3947567A1
EP3947567A1 EP19715042.8A EP19715042A EP3947567A1 EP 3947567 A1 EP3947567 A1 EP 3947567A1 EP 19715042 A EP19715042 A EP 19715042A EP 3947567 A1 EP3947567 A1 EP 3947567A1
Authority
EP
European Patent Office
Prior art keywords
lignin
suspension
nozzle
nozzle opening
particles
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
Application number
EP19715042.8A
Other languages
German (de)
English (en)
Inventor
Gilda Joana GIL-CHÁVEZ
Irina Smirnova
Stefan Heinrich
Ernst-Ulrich Hartge
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lignopure GmbH
Original Assignee
Lignopure GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Lignopure GmbH filed Critical Lignopure GmbH
Publication of EP3947567A1 publication Critical patent/EP3947567A1/fr
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00—Compositions of lignin-containing materials
    • C08L97/005—Lignin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/16—Evaporating by spraying
    • B01D1/18—Evaporating by spraying to obtain dry solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/16—Evaporating by spraying
    • B01D1/20—Sprayers

Definitions

  • the invention relates to a method for producing ultrafine lignin particles by means of
  • Biomass is becoming increasingly important as a raw material, for example for
  • Lignin basically has consumer-oriented application potential as a starting material for phenol production in the basic industry, as an adhesive additive, injection molding substrate,
  • Fuel raw material for adsorbers and insulating materials.
  • lignin is usually a by-product by
  • Lignocellulose is digested with alkalis, acids or organic solvents, more rarely with steam or aqueous solutions.
  • the lignin is in particulate form and has a particle size distribution that is as homogeneous as possible.
  • it is often necessary to mechanically comminute and grind the lignin in several steps, which is complex and expensive.
  • Gil-Cbirvez describes a spray-drying process in which lignin particles are produced in a single step (Gil-Cbirvez GJ, 2016, Development of a Lignin Recovery Process Targeting its Formulation and Application into Consumer Goods, In: Book of Abstract, ESS -HPT 2016, The European Summer School in High Pressure Technology, July 3-17, 2016, 39-41).
  • a lignin suspension is fed to a nozzle and the
  • Spray drying takes place at a drying temperature in the range of 180-200 ° C, a nozzle pressure in the range of 1-1.5 bar and a flow rate of the lignin suspension of 75-100 mL / min.
  • the present invention provides a method for producing ultrafine lignin particles by means of spray drying at a two-fluid nozzle with a first nozzle opening and a second nozzle opening, wherein a lignin-containing solution or suspension is fed to the first nozzle opening of the two-fluid nozzle and an atomizing gas is supplied to the second nozzle opening of the two-fluid nozzle, and wherein
  • the flow rate at which the lignin-containing solution or suspension is fed to the first nozzle opening (31) of the two-fluid nozzle is 60 to 65 mL / min
  • the drying temperature is 150 to 175 ° C.
  • the pressure of the atomizing gas at the second nozzle opening of the two-fluid nozzle is 3 to 6 bar.
  • Lignin powders produced according to the invention have a comparatively homogeneous composition with regard to the
  • Size range of, for example, 3-15 gm can be produced.
  • lignin particles with advantageous properties with regard to storage and transport as well as for desired applications can be obtained, e.g. for use in
  • lignin particles produced according to the invention agglomerate comparatively little, which is advantageous for many applications.
  • lignin which is insoluble in water can also advantageously be spray-dried.
  • water-insoluble lignin can be used, for example in aqueous suspension.
  • ultrastrengine lignin particles is used here to refer to lignin particles with an average particle diameter of ⁇ 100 ⁇ m, preferably ⁇ 90 ⁇ m, ⁇ 80 ⁇ m, ⁇ 70 ⁇ m, ⁇ 60 ⁇ m or ⁇ 50 ⁇ m, particularly preferably with an average particle diameter Particle diameters of ⁇ 40 pm, ⁇ 35 pm, ⁇ 30 pm, ⁇ 25 pm, ⁇ 20 pm or ⁇ 15 pm are understood.
  • Specifying a particle size distribution of, for example, D90: ⁇ 25 pm, D50: ⁇ 10 pm and D10: ⁇ 5 pm means that 90% of the particles have an average diameter of ⁇ 25 pm, 50% of the particles have an average diameter of ⁇ 10 pm and 10% have a mean diameter of ⁇ 5 pm.
  • lignin-containing substrate is used here, it is to be understood as a material or a material mixture that contains lignin.
  • lignin-containing substrates are wood, straw, bagasse, bran, grass, etc.
  • the lignin-containing substrate can also be an already pretreated substrate, for example waste from the sulphate or kraft process often used in paper production, or waste from lignin-containing substrates treated with organic-aqueous solvents (Organosolv process). In connection with this type of waste, the terms “alkali lignin”, “organosolv” lignin or hydrolysis lignin are also used.
  • lignocellulosic substrate also includes biomass containing lignocellulose.
  • alkali lignin refers to lignin that is obtained after treating wood at an elevated temperature (typically 170 ° C) with lye, for example with NaOH and / or a mixture of NaOH and sodium sulfate (Na 2 SC> 4 ) .
  • lignin refers to a complex polymer of aromatic alcohols as monomers, which are known as monolignols and are essentially connected to one another via ether groups.
  • Monolignols are, for example, phenylpropanoids such as p-coumaryl alcohol, coniferyl alcohol and sinapyl alcohol, which, for example, can be methoxylated to different degrees.
  • Lignin is a component of the secondary cell wall of plants and some algae, where it forms cross-linked macromolecules with molecular weights greater than 5000 u. Different types of wood and plants have lignins
  • lignin from coniferous wood predominantly contains coniferyl units, which have a guaiacyl radical (3-methoxy-4-hydroxyphenyl radical), while lignin from hardwood contains varying proportions of guaiacyl radicals and sinapyl units, which contain a syringyl radical (3,5-methoxy-4-hydroxyphenyl radical), having.
  • Lignin from grasses contains all three units.
  • VOC volatile organic compounds
  • VOCs are understood here to mean volatile organic compounds which already have a high vapor pressure at ambient temperature and can consequently preferably diffuse out of the substrate into the atmosphere.
  • VOC is understood to mean in particular organic components which have a boiling point of 50-260 ° C. Examples of VOC are guaiacol and reduced organic sulfur compounds such as dimethyl disulfide and dimethyl trisulfide.
  • Lignin-containing substrates is described, for example, in DE 102014108841 B3.
  • supercritical fluid or “supercritical fluid”, also abbreviated to SCF, this term refers to a fluid substance in the near or supercritical state, ie at a temperature and a pressure close to or above critical point (T c and P c ) of the substance. In this state are liquid phase and
  • Gas phase no longer distinguishable.
  • the term preferably refers to single-substance fluids, i.e. Fluids which, apart from unavoidable impurities, essentially consist of only one substance, e.g. CO2, exist. Under a "supercritical fluid mixture" or
  • Supercritical fluid mixture is understood to mean multi-component fluids, i.e. Mixtures of two or more substances, for example from CO2 and propane, or CO2 and small proportions of ethanol or water.
  • SCCO2 means supercritical carbon dioxide.
  • Carbon dioxide is at a temperature of 304.13 K (30.98 ° C) and a pressure of 7.375 MPa (73.75 bar). At temperatures and pressures above this point, supercritical carbon dioxide is produced.
  • Aquasolv-Solid-Lignin or “AS-Lignin” is understood here to mean lignin that has been subjected to hot water extraction.
  • a “hot water extraction”, possibly also referred to as “hot water hydrolysis” or “thermal hydrolysis”, means a thermal treatment using water at a temperature of> 100 ° C and a pressure above the vapor pressure of the water at the respective temperature. Examples are temperatures of 100-250 ° C. at pressures of 1-50 bar, for example a temperature of 200 ° C. at a pressure of 30 bar. If the terms “hot water hydrolysis” or “hot water pretreatment” are also used here, they are used synonymously with the above term “hot water extraction”.
  • “Feed rate” in relation to the lignin-containing solution or suspension is understood here as the volume flow of the lignin-containing solution or suspension in the direction of the nozzle.
  • drying temperature refers to the temperature of the
  • Spray drying used hot gas, which is used to dry the lignin-containing drops emerging from the nozzle.
  • the term refers to the
  • the hot gas can be a single-component gas or a gas mixture, for example air, CO2 or N2.
  • Materials are converted into dry powder form.
  • spray drying the material to be dried is atomized by means of an atomizer and introduced into a hot gas or a stream of hot gas, whereby it dries to a powder in a short time.
  • Enzymatic hydrolysis is understood to mean hydrolysis using a cellulase or a mixture of cellulases.
  • the enzymatic hydrolysis can for example be carried out at a temperature of 30-70 ° C, especially 45-60 ° C or 45-55 ° C, e.g. 50 ° C, and a pH of 4.5-5.5, preferably 4.8, can be carried out.
  • Cellulases are that
  • atomizing pressure refers to the pressure of the atomizing gas at the second nozzle opening of the two-fluid nozzle.
  • two-fluid nozzle refers to a nozzle with at least two separate nozzle openings, a first fluid being able to emerge from the first nozzle opening and a second fluid from the second nozzle opening.
  • the nozzle openings are arranged in relation to one another in such a way that, for example, a first fluid, e.g. a liquid, upon exiting the first nozzle opening with a jet of a second fluid, e.g. a preloaded gas, can be brought into contact.
  • the first nozzle opening of the two-fluid nozzle can be arranged centrally and surrounded concentrically by an annular second nozzle opening.
  • the term “two-fluid nozzle” is not to be understood here in a restrictive way as meaning that the nozzle cannot have more than two nozzle openings, for example three nozzle openings.
  • Any smaller area from the area is also intended to be disclosed, the smaller area also being understood to mean areas that do not include any of the limit values of the area.
  • An indication such as “300 gm to 5 mm” not only includes areas such as “300 gm to 4 mm” or “400 gm to 5 mm”, but
  • a lignin-containing solution or suspension is passed through a first nozzle opening of a two-fluid nozzle and, when exiting the first nozzle opening, a pressurized atomizer gas from the second nozzle opening is applied, whereby the solution or suspension is broken down into individual droplets is atomized.
  • the droplets are generated within a few seconds by means of a hot gas of suitable temperature, e.g. dried within 3-10 seconds, creating lignin particles of a desired size.
  • the drying temperature is 150 to 175 ° C, preferably 150 to 170 ° C
  • the atomization pressure i.e. the pressure of the atomizer gas at the second nozzle opening of the two-fluid nozzle is 3 to 6 bar and the flow rate of the lignin-containing solution or suspension is 60 to 65 mL / min.
  • the diameter of the first nozzle opening of the two-fluid nozzle is 1 to 2 mm, preferably 1.5 to 2 mm.
  • the pressure of the atomizer gas at the second nozzle opening of the two-fluid nozzle is preferably 3 to 5.5 bar, preferably 3 to 5 bar or 3 to 4.5 bar, particularly preferably 3 to 4 bar.
  • the lignin-containing solution or suspension is a solution or suspension of lignin which has been produced from a lignin-containing substrate which has been subjected to hot water extraction.
  • a lignin pretreated in this way is optionally also referred to here as AS lignin.
  • the hot water extraction can, for example, with pure water in one
  • the hot water extraction can be carried out in one or more stages, for example with gradually increasing temperature and increasing pressure.
  • the ratio of water to lignin-containing substrate is preferably 5-10: 1. In the case of a fixed bed process preferably used for this purpose, the hot water flows through the lignin-containing substrate under pressure, preferably in the opposite direction to the direction of gravity.
  • the lignin-containing solution or suspension is a solution or suspension of lignin that has been produced from a lignin-containing substrate that has been subjected to hot water extraction and subsequent enzymatic hydrolysis using cellulase (s).
  • a particularly suitable pretreatment process is described, for example, in DE 102014108841 B3.
  • a deodorized lignin in the method according to the invention it is also possible to use a deodorized lignin.
  • a lignin pretreated by means of hot water extraction and enzymatic hydrolysis can be subjected to an extraction with a supercritical fluid, for example with supercritical carbon dioxide, as described in DE 102014108841 B3.
  • the solids content of the lignin solution or lignin suspension is preferably 5 to 20% by weight.
  • the lignin can be dissolved, partially dissolved, or suspended in any suitable solvent. However, it is preferred that the lignin is dissolved or suspended, preferably suspended, in water.
  • the lignin-containing solution or suspension is injected through the nozzle into a drying chamber which contains a hot drying gas.
  • the droplets of the lignin-containing solution or suspension formed by the atomizer gas when exiting the nozzle reach a chamber with a hot gas, for example air or nitrogen gas.
  • the solvent for example water, evaporates in the chamber and dried lignin particles are formed.
  • the chamber can be designed so that different particle fractions, eg
  • Particle size effects can be taken separately from the chamber.
  • a removal point for coarser particles can be provided at the bottom of the chamber, while finer particles are removed from a side wall of the chamber at one or more predetermined heights.
  • the hot drying gas is preferably passed into the drying chamber in cocurrent with the lignin-containing solution or suspension.
  • the hot drying gas is fed into the drying chamber, for example, at an inlet temperature of 150 to 175 ° C. and brought into contact with the fine droplets formed at the nozzle.
  • cocurrent refers to the fact that the drying gas is fed into the drying chamber in essentially the same direction as the lignin-containing solution or suspension, so that the particle flow and the flow of the drying gas in the drying chamber run in the same direction.
  • the lignin-containing solution or suspension is passed through one nozzle opening of the two-fluid nozzle, while at the same time the atomizer gas, e.g. Nitrogen, CO2 or air.
  • the atomizer gas e.g. Nitrogen, CO2 or air.
  • Volume flows of both fluids can be controlled separately and coordinated with one another.
  • the two-fluid nozzle has a central first nozzle opening and an annular second nozzle opening concentrically surrounding the central nozzle opening.
  • Suspension is fed to the central first nozzle opening of the two-fluid nozzle, while the second nozzle opening with the pressurized atomizer gas, preferably air, CO2 or nitrogen, is applied.
  • the lignin-containing solution or suspension which is preferably an aqueous solution or suspension of AS lignin, is fed to the central nozzle opening of the two-fluid nozzle, while at the same time a stream of atomizing gas is emitted from the second nozzle opening concentrically surrounding the first nozzle opening , e.g. nitrogen gas, CO2, air or another suitable input or
  • the droplets of lignin-containing solution or suspension that form on exit from the first nozzle opening of the nozzle are preferably flowing in cocurrent to the lignin-containing solution or suspension by means of the
  • Hot gas stream within a short time e.g. within 3-10 seconds, dried, i.e. the solvent, preferably water, is evaporated by means of the hot gas.
  • the lignin particles that form often have an advantageous hollow structure, i.e. are hollow on the inside with an outer wall made of lignin.
  • an advantageous hollow structure i.e. are hollow on the inside with an outer wall made of lignin.
  • the solvent initially evaporates in the surface areas of the droplets formed, as a result of which a comparatively solid lignin wall initially forms there. Subsequently, further solvent evaporates from the interior of the droplets over this lignin wall, as a result of which further lignin is transported to the lignin wall and deposited.
  • Such hollow lignin particles can be used particularly advantageously, for example, as additives in adhesives and in pharmaceutical or cosmetic products.
  • the invention also relates to lignin-containing microbeads
  • Merobeads that contain ultrafine lignin-containing particles produced according to the invention and at least one binder.
  • the lignin-containing microbeads preferably comprise ultra-fine lignin-containing particles which are produced from Aquasolv lignin (AS lignin).
  • AS lignin particles are produced by the method according to the invention from AS-lignin, ie lignin obtained from a lignin-containing substrate, for example straw, by means of a thermal treatment with hot (for example 200 ° C.), pressurized liquid water and preferably a subsequent enzymatic hydrolysis by cellulase (s).
  • Suitable binders are known to the person skilled in the art.
  • the binder is preferably a gel-forming biopolymer.
  • AS-Lignin can for example be used in combination with one or more gel-forming biopolymers, for example alginate, cellulose, pectin, chitosan, starch, polylactide (PLA) or silicates as well as proteins such as zein, whey protein and others.
  • the gelation of lignin in combination with another biopolymer takes place preferably in the presence of a cross-linking molecule.
  • gel formation can take place at low temperature (e.g. -6 ° C, 0 ° C), high temperature (80-140 ° C), in acidic (pH ⁇ 6) or basic ( pH> 7) environment.
  • the mass fraction of lignin in the formulation can be 10 to 90% by weight
  • the indication of the mass fraction relates to the formulation of AS lignin and binding agent before cross-linking.
  • Microbeads made from lignin formulations such as lignin alginate, lignin pectin, lignin chitosan, lignin cellulose, lignin starch and lignin protein can be used in food, pharmaceutical and cosmetic products.
  • Microbeads made from lignin formulations such as lignin starch, lignin cellulose, lignin silicate can be used in building materials.
  • Microbeads from the lignin formulation lignin silicate can also be used in cosmetic applications.
  • Microbeads from formulations such as lignin-poly lactide, lignin-poly lactide silicate can be used for building materials, packaging materials or biocomposites.
  • Cosmetic applications are, for example, peeling products for body care, face masks, soap,
  • Microbeads can, for example, be used as active ingredients in functional foods, as carriers of antioxidants, flavorings, vitamins, etc.
  • the mean particle diameter of the microbeads can be, for example, 300 ⁇ m to 5 mm.
  • the mean particle diameter is preferably 300 ⁇ m to 1.5 mm.
  • the mean particle diameter of the microbeads is 300 to 800 ⁇ m.
  • the mean particle diameter of the microbeads is, for example, 400 ⁇ m to 1.5 mm.
  • Figure 1 Schematic diagram of a portion of a device with which a preferred
  • Embodiment of the method according to the invention can be carried out.
  • FIG. 5 IC50 values of various fignins for the inhibition of ⁇ -glucosidase and ⁇ -amylase.
  • Fine fraction SDF fine;
  • Coarse fraction SDF coarse
  • FIG. 7 Free radical scavenging capacity (% inhibition) of spray-dried fignin according to the invention and fignins obtained by other biorefining processes.
  • EtOH ethanol;
  • Organosolv-Fignin fignin extracted with ethanol (manufactured by Fraunhofer CBP Feuna);
  • EtOH CO2 fignin particles that have undergone a solvent exchange (change from water to ethanol), the ethanol then being extracted with supercritical CO2.
  • FIG. 9 Composition of nine different batches of lignin with different excipient concentrations.
  • Particle size distribution homogeneous lignin powder with desired properties can be produced in one step. It was possible to dispense with the multiple comminution and grinding steps previously required.
  • FIG. 1 shows schematically the spray drying process by means of a two-fluid nozzle 2 as part of the system 100 used for the experiments.
  • FIG. 2 shows a simplified flow diagram of the production of the system 100 used for the AS lignin particles.
  • the spray drying process according to the invention involves the production of a lignin powder by drying a liquid solution or suspension with a hot one
  • the liquid lignin-containing material (solution or suspension) is atomized and brought into contact with a hot gas stream.
  • two-fluid nozzle 2 was used, which is shown in longitudinal section.
  • the two-fluid nozzle 2 comprises a central bore 3 with a central first nozzle opening 31 to a drying chamber 1 and a bore 4 concentrically surrounding the central bore 3 with a second nozzle opening 41 concentrically surrounding the first nozzle opening 31 to the drying chamber 1.
  • the liquid AS -Lignin-containing material was fed via a first inlet opening 32 through the central bore 3 to the central first nozzle opening 31 (arrows with continuous Line), the atomizer gas, here N2, via a second inlet opening 42 through the concentric bore 4 to the second nozzle opening 41 (arrows with dotted line).
  • the hot gas, here also N2 was passed into the drying chamber 1 in such a way that the hot gas flow 7 ran in cocurrent with the particle flow formed.
  • the hot gas was introduced into the drying chamber 1 in the immediate vicinity of the two-fluid nozzle 2. Hot gas flow 7 and particle flow ran essentially in the direction of gravity.
  • the contact between the material to be dried and the hot gas in the drying chamber 1 is short, but sufficient to cause water to evaporate within the atomized droplets 5.
  • the atomization is pneumatic by a high velocity of the compressed atomizing gas in contact with the liquid lignin material
  • the morphology and particle size of the final product can be varied by varying the
  • Ratio of the flow rates between the feed material (lignin suspension or solution) and the pressurized atomization gas at the respective nozzle openings 31, 41 and the inlet and outlet temperature in the drying chamber 1 can be controlled.
  • the extraction of the dried lignin particles 6 can vary depending on the configuration of the spray dryer system 100. In the experiments described here, a
  • Spray dryer system used with a drying chamber 1, which was equipped with two extraction points 11, 12 (see Figure 2). Coarse (larger and heavier) particles 6 (coarse fraction) could be collected through a first removal point 12 at the bottom, and finer particles 6 (fine fraction) could be collected through the second removal point 11 arranged on the side. A fraction with finer lignin particles 6 can be transferred via the lateral removal point 11 into a cyclone 101 for further separation.
  • the AS lignin suspension was kept in a storage container 104 and fed to the first (central) bore 3 of the two-fluid nozzle 2 by means of a pump 105.
  • the atomizer gas, here N2 was held in a tank 102 and fed to the nozzle 2 by means of a compressor unit 103.
  • the hot gas, here also N2 was set to the desired level by means of a heater 106
  • the inlet temperature of the hot gas which, due to the introduction of the hot gas in the immediate vicinity of the two-fluid nozzle 2, corresponds to the temperature of the hot gas (N2) at the two-fluid nozzle 2.
  • the pressure of the atomizing gas at the second nozzle opening 31 of the two-fluid nozzle 2 (also referred to as “atomizing pressure).
  • AS fignin suspension with a solids content of 5 to 20% by weight was used.
  • the AS-fignin was produced by means of thermal hydrolysis and subsequent enzymatic hydrolysis by pressing liquid water under pressure at about 200 ° C through straw and adding cellulases to the resulting suspension.
  • the diameter of the nozzle opening 31 was 1-2 mm. In this configuration, the inlet temperature of the hot gas controls the temperature in drying chamber 1.
  • the reason could be the arrangement of hydrophobic fignin sites on the outer particle layer that prevent the binding or interaction of
  • Hollow particles can, for example, be used for the controlled release of drugs, chemical reagents and cosmetics from the interior of the hollow particles via the surface be used.
  • the low density of hollow lignin particles is advantageous for many pharmaceutical applications.
  • a D50 value of ⁇ 10 ⁇ m and a D10 value of ⁇ 5 ⁇ m were achieved with nozzle openings of 1.5-2 mm (see FIG. 3). It is particularly noteworthy that, in addition, a D90 value of ⁇ 25 ⁇ m (see FIG. 3) could be achieved, as a result of which all the particles that were added to adhesive compositions had sizes below 30 ⁇ m.
  • the water content of the lignin powder obtained was 1.5 to 5% by weight.
  • Lignin concentrations were investigated. These enzymes are responsible for breaking down complex high molecular weight carbohydrates and producing sugar monomers that are readily available for absorption in the human body. It is believed that
  • Lignin particles produced according to the invention show a comparatively high antidiabetic effect.
  • lignin can be used as an alternative to activated carbon.
  • the behavior of the pharmaceutical Lormen strongly depends on the particle properties and the compression behavior.
  • the direct compression of the lignin particles obtained by the method according to the invention was therefore compared with known pharmaceutical excipients.
  • the tested formulations are listed in Ligur 9, alginate, starch, microcrystalline cellulose (MCC), lactose and a direct compression excipient (DCE) were listed in
  • the AS lignin spray-dried according to the invention was compared with a medicinal lignin (“softwood lignin”) that was used to produce a lignin-based medicinal tablet.
  • a medicinal lignin (“softwood lignin”) that was used to produce a lignin-based medicinal tablet.
  • Ligur 6 shows the hardness of the various compositions based on AS lignin specified in Ligur 9.
  • the hardness of the tablets increases with the addition of excipients. Nevertheless, the desired hardness depends on the release behavior of the tablet.
  • tablet dosage forms should have a friability
  • the antioxidant potential of the spray-dried lignin was measured by the DPPH radical method.
  • DPPH 2,2-diphenyl-l-picrylhydrazyl
  • lignin spray-dried according to the invention various lignins were used (see Pig. 7). Generally is a
  • Spray-dried fine lignin produced according to the invention was incorporated into adhesives. The appearance of kneaded samples was evaluated. The samples contained lignin obtained by various methods and lignin from various biomass sources. The adhesive films, the ultrafine produced according to the invention
  • Calcium carbonate a commonly used standard filler.
  • microbeads Production of AS-lignin-based microbeads
  • Lignin-based microbeads according to the invention were produced using lignin-containing particles produced by means of the method according to the invention.
  • stock solutions or stock suspensions were produced which contain AS lignin particles in combination with gel-forming biopolymers (alginate, cellulose, pectin, chitosan, starch, polylactide).
  • the gel-forming biopolymers were in a mass fraction of 1 wt .-%, 2 wt .-%, 3 wt .-%, 4 wt .-% and 5 wt .-% in water (deionized or distilled, optionally heated), acidic or mixed alkaline media.
  • the mixture of biopolymer solution and AS lignin particles can have a proportion of 10-90 Contain wt .-% lignin. The mixture was mixed thoroughly until a homogeneous solution / suspension was obtained.
  • Microparticles were produced from the stock solutions / suspensions using a jet cutter ("jet cutter", Type S, geniaLab GmbH, Braunschweig, Germany).
  • jet cutter Type S, geniaLab GmbH, Braunschweig, Germany.
  • particles are generated from a fluid jet which exits a nozzle under pressure by cutting the full jet emerging from the nozzle into uniform cylindrical segments using a rotating cutting tool from radially arranged cutting wires. Due to the surface tension, spherical drops of uniform size form from the fluid segments as they fall.
  • the size of the droplets can, for example, via the rotational speed of the cutting tool, the diameter and
  • volume flow of the liquid jet can be adjusted.
  • the drops created in this way fall into a crosslinking / hardening solution.
  • the nozzle was opened using compressed air (1-3 bar)
  • microparticles The production of microparticles (“microbeads) was carried out, for example, using the following parameters: flow rate of the stock solution / suspension in the range from 0.5 to 10 g / s, nozzle diameter from 200 ⁇ m to 5 mm.
  • the cutting disks can contain, for example, 16 to 180 wires with a wire thickness of 100 ⁇ m to 500 ⁇ m.
  • the crosslinking solution can include, for example, calcium chloride, ethanol, acetic acid, aqueous acidic solutions or aqueous basic solutions.
  • the distance between the nozzle and the gelling bath was kept in the range of about 50 to 100 cm.
  • the volume of the crosslinking bath was at least four times the total volume of the processed biopolymer solution / suspension in order to avoid agglomeration of microbeads.
  • the contents of the collecting baths are stirred until the particles are removed. Gelled particles are separated from the gelling-adding bath by sieving and / or filtering. The separated microparticles can be dried, oven dried or supercritical dried at ambient temperature.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Medicinal Chemistry (AREA)
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  • Organic Chemistry (AREA)
  • Compounds Of Unknown Constitution (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)
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  • Medicines Containing Plant Substances (AREA)

Abstract

La présente invention concerne un procédé de production de particules de lignine ultrafines par séchage par pulvérisation sur une buse bi-fluides (2) présentant une première ouverture de buse (31) et une seconde ouverture de buse (41), une solution ou suspension contenant de la lignine étant introduite dans le premier orifice (31) de la buse bi-fluides (2) et un gaz de pulvérisation étant introduit dans le second orifice (41) de la buse bi-fluides (2), et a) le débit auquel la solution ou suspension contenant de la lignine est acheminée jusqu'à la première ouverture (31) de la buse bi-fluides (2) s'élevant à 60-65 ml/min, b) la température de séchage s'élevant à 150-175 °C et c) la pression du gaz de pulvérisation au niveau de la seconde ouverture (41) de la buse bi-fluides (2) étant de 3 à 6 bars.
EP19715042.8A 2019-03-28 2019-03-28 Procédé de production de particules de lignine ultrafines Pending EP3947567A1 (fr)

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US3808192A (en) 1973-04-11 1974-04-30 Westvaco Corp Production of high surface area lignins by spray drying
DE19503157B4 (de) * 1994-02-01 2004-07-01 Bend Research, Inc., Bend Instabile Insektizid-Zusammensetzungen
US5939089A (en) * 1998-04-09 1999-08-17 Lignotech Usa, Inc. Method for providing a stable protective coating for UV sensitive pesticides
KR101088520B1 (ko) * 2003-01-10 2011-12-06 디에스엠 아이피 어셋츠 비.브이. 지용성 물질의 분말 제제의 제조방법
DE102013112499A1 (de) * 2013-11-13 2015-05-13 Brandenburgische Technische Universität Cottbus-Senftenberg Vorrichtung und Verfahren zur Agglomeration der Ablauge eines Cellulosegewinnungsprozesses
DE102014108841B3 (de) 2014-06-24 2015-05-28 Technische Universität Hamburg-Harburg Verfahren zur Desodorierung von Lignin

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JP2022532294A (ja) 2022-07-14
WO2020192929A1 (fr) 2020-10-01

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