WO2025171299A1 - Procédés et systèmes de séchage et de concentration à cisaillement élevé - Google Patents

Procédés et systèmes de séchage et de concentration à cisaillement élevé

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Publication number
WO2025171299A1
WO2025171299A1 PCT/US2025/015064 US2025015064W WO2025171299A1 WO 2025171299 A1 WO2025171299 A1 WO 2025171299A1 US 2025015064 W US2025015064 W US 2025015064W WO 2025171299 A1 WO2025171299 A1 WO 2025171299A1
Authority
WO
WIPO (PCT)
Prior art keywords
feedstock
vortex
drying
heated
high shear
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
PCT/US2025/015064
Other languages
English (en)
Inventor
Amos CLINE
David J. Neivandt
Charles EME
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.)
University of Maine System
Original Assignee
University of Maine System
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 University of Maine System filed Critical University of Maine System
Publication of WO2025171299A1 publication Critical patent/WO2025171299A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001—Modification of pulp properties
    • D21C9/007—Modification of pulp properties by mechanical or physical means

Definitions

  • CNFs cellulose nanofibrils
  • cellulose-based nanomaterials among others such as cellulose nanocrystals and bacterial nanocellulose, and are typically produced via mechanical refining of lignocellulosic materials in a liquid feedstock.
  • CNFs have a hierarchical structure ranging from the micron scale down to nanometer dimensions with desirable characteristics including biodegradability, low density, high surface area, high aspect ratio and superior mechanical properties.
  • CNFs include biomedical and health care, electronics and sensors, construction, food and packaging, consumer products, and as a reinforcing agent in thermoplastic feedstocks for large scale additive manufacturing.
  • substances that are suspended and/or dissolved in liquid and can be dried or concentrated to form products include proteins, nucleic acids, polysaccharides, milk, viruses, black liquor, lignin, maple sap, salts, and pharmaceuticals.
  • the present embodiments are directed to a method for producing dried cellulose nanofibril (CNF) material, including: providing a cellulosic feedstock; heating the cellulosic feedstock; exposing the cellulosic feedstock to a high shear environment to form treated material; and collecting the treated material, wherein the treated material includes a plurality of cellulose nanofibrils, and wherein the cellulose nanofibrils are substantially not aggregated.
  • CNF dried cellulose nanofibril
  • the high shear environment includes a heated, turbulent air flow or gas flow. In some embodiments, the heating and exposing happen substantially simultaneously.
  • the method additionally includes filtering the treated material to form filtered material. In some embodiments, filtering includes passing at least a portion of the treated material through meshes, filter papers, or combinations thereof.
  • the cellulosic feedstock includes at least 50% fines (e.g., at least 60% fines, 70% fines, 80% fines, 85% fines, 90% fines, 95% fines, 99% fines, 100% fines).
  • FIG. 2 is a schematic diagram of acid hydrolysis of cellulose microfibrils to release cellulose nanocrystals (CNC) (Mishra R. K., Sabu A., & Tiwari, S. K. (2016). Materials chemistry and the futurist eco-friendly applications of nanocellulose: status and prospect. Journal of Saudi Chemical Society 22:949- 978.).
  • CNC cellulose nanocrystals
  • the present disclosure provides, inter alia, methods to thermally dry cellulosic feedstock without the structures undergoing significant aggregation or degradation to form nanostructured CNFs, while being scalable, cost-effective, and energy efficient.
  • the present disclosure features new methods and systems for drying and/or concentrating CNFs using high shear forces and heating that result in CNF materials with a significant yield of nanofibrillar structure.
  • the drying and/or concentrating system 100, 200 includes a turbulence module 141 that includes one or more vortex generators.
  • FIGS. 7-14 show schematic diagrams and photographs of an exemplary turbulence module 141.
  • an injection nozzle is used for generating a primary vortex (or vortex 1) while a plenum chamber with circumferential holes generates a secondary vortex (or vortex 2) which may rotate in opposite directions and generate the high shear needed to separate dispersed materials in the liquid feedstock (e.g., cellulosic fibers) and to evaporate solvent.
  • Hot air 404 enters the input end of an injection nozzle 408 (e.g., a fuel injection nozzle), which is held by a flange 406.
  • a vortex i.e., primary vortex or vortex 1
  • the injection nozzle 408 fits coaxially inside the inner cylinder 412.
  • Hot air 420 enters the space between the inner cylinder 412 and outer cylinder via another inlet connector (not shown here, but shown in FIGS. 9-14) and passes through plurality of circumferential holes drilled in the inner cylinder 412 to form another vortex (i.e., secondary vortex or vortex 2), which rotates in the opposite direction to vortex 1.
  • FIG. 14A is a photograph of an assembled turb turbulence module 141, with injection nozzle 512 and second vortex generator comprising the inner cylinder 516 and outer cylinder 518 visible, according to aspects of the present embodiments. Holes 517 drilled in the wall of the inner cylinder 516 are also visible. In the opening tip of the injection nozzle 512, the air-liquid diverter 508 is visible.
  • FIG. 14B is a photograph of the inner wall 516 (or inner cylinder 516) of the plenum chamber of the turbulence module 141, which helps to form the secondary vortex in combination with the outer cylinder 518, according to aspects of the present embodiments.
  • Radial circumferential holes 517 are visible in the wall of the inner cylinder 516.
  • a drill bit is inserted to indicate the direction of the holes 517.
  • the radial circumferential holes are tapered (e.g., using a 7 degree tapered ream) so that the diameters of the holes at the inner surface of inner cylinder 516 may be smaller than the diameters of the holes at the outer surface of inner cylinder 516 (e.g., diameter at inner surface about 1/16”), each hole forming a small nozzle.
  • the inner cylinder 516 may be made of stainless steel, and have a base for attaching to other components of the feed nozzle.
  • hole sizes, positions, angle with respect to cylinder, taper angles, shapes, and numbers drilled in inner cylinder 516 may be varied in order to tune the behavior of a secondary vortex. In some embodiments, another means of generating a secondary vortex may be used.
  • FIG. 14C is a photograph of an assembled turbulence module 141, with injection nozzle 512 and secondary vortex generator formed by the inner cylinder 516 and outer cylinder 518 visible, and with the primary vortex and secondary vortex indicated by the small and large curved arrows, respectively, according to aspects of the present embodiments.
  • the primary vortex and secondary vortex are rotating in opposite directions in the embodiment shown in FIG. 14C.
  • the plenum chamber 519 is formed by the gap between the inner cylinder 516 and the outer cylinder 518.
  • Operation parameters of the high shear drying and/or concentrating system may affect the yield of dried material collected at the end of processing, and may also affect the morphology of the resulting material.
  • FIGS. 26 and 27 show broad and detailed exemplary methods 600, 700 for the operation of a high shear drying and/or concentrating system to produce dried materials (e.g., CNF materials) and/or concentrated substances.
  • the detailed method 700 in FIG. 27 show where various parameters may be set. These parameters may include the feed rate of the liquid feedstock, heater temperature for the compressed air or gas flows entering vortex 1 and vortex 2, the flow rates of compressed air or gas flows entering vortex 1 and vortex 2.
  • Additional parameters include the set temperature of the liquid feedstock heater, the characteristics of the liquid feedstock such as the solvent, type of dispersed material, distribution of sizes of dispersed material, and concentration of dispersed material.
  • the relevant parameters may also include percent fines of cellulosic material in the feedstock, and the original source of the cellulosic material (e.g., the type of plant, method of processing to produce cellulosic material).
  • FIG. 26 is a flow chart diagram for a method 600 of high shear drying and/or concentrating to form dried materials and/or concentrated substances from materials dispersed and/or dissolved in a liquid feedstock, according to aspects of the present embodiments.
  • the method 600 is a general method, and may include the following steps: step 602, providing a liquid feedstock; step 604, heating the liquid feedstock; step 606, exposing the liquid feedstock to a high shear environment to form treated material; and step 608, collecting the treated material.
  • the liquid feedstock may be a cellulosic feedstock.
  • a high shear environment may be a heated, turbulent airflow.
  • treated material may include a plurality of cellulose nanofibrils that are substantially not aggregated.
  • FIG. 27 is a flow chart diagram for an exemplary method 700 of high shear drying and/or concentrating to form dried and/or concentrated materials from a dispersion and/or solution in a liquid feedstock, according to aspects of the present embodiments.
  • the method 700 is a detailed method, and may include the following steps: step 702, assemble parts of collection system; step 704, wash injection nozzle to remove residues from previous run; step 706, load liquid feedstock into feed reservoirs; step 708, pressurize feed reservoirs with gas; step 710, turn on syringe pumps and set flow rates; step 712, charge syringe pumps with feedstock; step 714, turn on feedstock heater and set temperature; step 716, turn on humidity data recording; step 718, turn on regenerative blower by turning on variable frequency drive (VFD); step 720, open valves to introduce compressed air into injection nozzle to create vortex 1, and into plenum chamber to generate vortex 2; step 722, turn on inline heaters to heat compressed air entering vortices; step 724, run syringe pumps to start the flow of feedstock; step 726, monitor pressure of system, where end of run is determined by increase in differential pressure across filter assembly (e.g., 70 inch water pressure); step 728, turn off heaters and
  • Feed rate of cellulosic feedstock 10 ml/min, 20 ml/min, and 30 ml/min were used, with the 10 ml/min feed rate producing the highest nanofibrous product yield with the most non-aggregated morphology
  • Compressed air or gas flow rate for vortex generation two truncated cone valves control the flow of air into the injection nozzle for vortex 1 generation, and into the plenum chamber for vortex 2 generation were opened by varying numbers of turns. Valve openings of 1, 1.5, 2, and 2.5 turns were used, resulting in the optimal nanofibrous yield at 2 turns open on each of the compressed air control valves.
  • An example of valve openings and flow rates are summarized in the table below.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Wood Science & Technology (AREA)
  • Mechanical Engineering (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

Des substances qui sont en suspension, dispersées et/ou dissoutes dans un liquide peuvent être séchées ou concentrées pour obtenir un matériau séché ou concentré. Par exemple, des nanofibrilles de cellulose (CNF) sont des matériaux à base de cellulose ayant des dimensions nanométriques et des propriétés souhaitables formées par traitement de fibres de cellulose macroscopiques pour les défibriller en une suspension ou une charge d'alimentation, suivi du séchage de la charge d'alimentation pour former un matériau CNF sec. Des procédés de séchage tels que le séchage par pulvérisation et le séchage au four provoquent une agrégation excessive des matériaux séchés, tandis que la lyophilisation et le séchage par CO2 supercritique sont coûteux et difficiles à mettre en œuvre à grande échelle. Les présents modes de réalisation comprennent des procédés et des systèmes utilisant un cisaillement élevé pour sécher ou concentrer des charges d'alimentation liquides contenant des substances en suspension et/ou dissoutes afin de produire des substances séchées ou concentrées d'une manière évolutive avec un rendement élevé.
PCT/US2025/015064 2024-02-09 2025-02-07 Procédés et systèmes de séchage et de concentration à cisaillement élevé Pending WO2025171299A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US202463551895P 2024-02-09 2024-02-09
US63/551,895 2024-02-09

Publications (1)

Publication Number Publication Date
WO2025171299A1 true WO2025171299A1 (fr) 2025-08-14

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Country Status (1)

Country Link
WO (1) WO2025171299A1 (fr)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5324751A (en) * 1989-01-24 1994-06-28 Ici Americas Inc. Cryoprotectant sorbitol crystal spherules
US20030136707A1 (en) * 2000-09-22 2003-07-24 Engelhard Corporation FCC catalysts for feeds containing nickel and vanadium
US20110260348A1 (en) * 2010-04-27 2011-10-27 University Of Maine System Board Of Trustees Method for drying cellulose nanofibrils
US20160152811A1 (en) * 2013-07-18 2016-06-02 University Of Maine System Board Of Trustees Nanofibril-polymer composites
US20170210826A1 (en) * 2015-09-30 2017-07-27 Api Intellectual Property Holdings, Llc Processes for producing nanocellulose, and nanocellulose compositions produced therefrom
US20170266693A1 (en) * 2014-11-28 2017-09-21 Teknologian Tutkimuskeskus Vtt Oy Method for improving the water tolerance of bio-based CNF-films
US10066028B1 (en) * 2017-05-11 2018-09-04 King Saud University Method of fabricating biocompatible cellulose nanofibrils
US20200094272A1 (en) * 2017-08-04 2020-03-26 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
US20230303896A1 (en) * 2022-03-23 2023-09-28 Fiberlean Technologies Limited Resin reinforced with nanocellulose for wood-based panel products

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5324751A (en) * 1989-01-24 1994-06-28 Ici Americas Inc. Cryoprotectant sorbitol crystal spherules
US20030136707A1 (en) * 2000-09-22 2003-07-24 Engelhard Corporation FCC catalysts for feeds containing nickel and vanadium
US20110260348A1 (en) * 2010-04-27 2011-10-27 University Of Maine System Board Of Trustees Method for drying cellulose nanofibrils
US20160152811A1 (en) * 2013-07-18 2016-06-02 University Of Maine System Board Of Trustees Nanofibril-polymer composites
US20170266693A1 (en) * 2014-11-28 2017-09-21 Teknologian Tutkimuskeskus Vtt Oy Method for improving the water tolerance of bio-based CNF-films
US20170210826A1 (en) * 2015-09-30 2017-07-27 Api Intellectual Property Holdings, Llc Processes for producing nanocellulose, and nanocellulose compositions produced therefrom
US10066028B1 (en) * 2017-05-11 2018-09-04 King Saud University Method of fabricating biocompatible cellulose nanofibrils
US20200094272A1 (en) * 2017-08-04 2020-03-26 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
US20230303896A1 (en) * 2022-03-23 2023-09-28 Fiberlean Technologies Limited Resin reinforced with nanocellulose for wood-based panel products

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