WO2015085168A1 - Finely ground biomass - Google Patents
Finely ground biomass Download PDFInfo
- Publication number
- WO2015085168A1 WO2015085168A1 PCT/US2014/068784 US2014068784W WO2015085168A1 WO 2015085168 A1 WO2015085168 A1 WO 2015085168A1 US 2014068784 W US2014068784 W US 2014068784W WO 2015085168 A1 WO2015085168 A1 WO 2015085168A1
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- WO
- WIPO (PCT)
- Prior art keywords
- particles
- biomass material
- finely ground
- particle size
- microns
- Prior art date
Links
- 239000002028 Biomass Substances 0.000 title claims abstract description 72
- 239000002245 particle Substances 0.000 claims abstract description 105
- 239000000463 material Substances 0.000 claims abstract description 73
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000009837 dry grinding Methods 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002985 plastic film Substances 0.000 claims description 20
- 229920006255 plastic film Polymers 0.000 claims description 20
- 239000011347 resin Substances 0.000 claims description 18
- 229920005989 resin Polymers 0.000 claims description 18
- 238000013329 compounding Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 9
- 239000000088 plastic resin Substances 0.000 claims description 9
- 241000209140 Triticum Species 0.000 claims description 6
- 235000021307 Triticum Nutrition 0.000 claims description 6
- 239000004631 polybutylene succinate Substances 0.000 claims description 6
- 229920002961 polybutylene succinate Polymers 0.000 claims description 6
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 4
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 4
- 239000004571 lime Substances 0.000 claims description 4
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 4
- -1 polybutylene succinate Polymers 0.000 claims description 4
- 239000004626 polylactic acid Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 244000075850 Avena orientalis Species 0.000 description 31
- 235000007319 Avena orientalis Nutrition 0.000 description 31
- 239000004033 plastic Substances 0.000 description 9
- 229920003023 plastic Polymers 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 5
- 240000007594 Oryza sativa Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000010903 husk Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 238000010951 particle size reduction Methods 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 235000000346 sugar Nutrition 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000283690 Bos taurus Species 0.000 description 1
- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 description 1
- HMFHBZSHGGEWLO-SOOFDHNKSA-N D-ribofuranose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H]1O HMFHBZSHGGEWLO-SOOFDHNKSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 240000004658 Medicago sativa Species 0.000 description 1
- 235000017587 Medicago sativa ssp. sativa Nutrition 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 101000972349 Phytolacca americana Lectin-A Proteins 0.000 description 1
- PYMYPHUHKUWMLA-LMVFSUKVSA-N Ribose Natural products OC[C@@H](O)[C@@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-LMVFSUKVSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- HMFHBZSHGGEWLO-UHFFFAOYSA-N alpha-D-Furanose-Ribose Natural products OCC1OC(O)C(O)C1O HMFHBZSHGGEWLO-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229920000704 biodegradable plastic Polymers 0.000 description 1
- 229920006025 bioresin Polymers 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000000378 dietary effect Effects 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 235000019621 digestibility Nutrition 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000003621 hammer milling Methods 0.000 description 1
- 239000002029 lignocellulosic biomass Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000019895 oat fiber Nutrition 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 235000021309 simple sugar Nutrition 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/20—Methods of refining
- D21D1/32—Hammer mills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C21/00—Disintegrating plant with or without drying of the material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C9/00—Other milling methods or mills specially adapted for grain
- B02C9/04—Systems or sequences of operations; Plant
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/20—Agglomeration, binding or encapsulation of solid waste
- B09B3/21—Agglomeration, binding or encapsulation of solid waste using organic binders or matrix
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/09—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
- B29C48/10—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels flexible, e.g. blown foils
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/12—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by wet methods, by the use of steam
- D21B1/30—Defibrating by other means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2867/00—Use of polyesters or derivatives thereof as mould material
- B29K2867/04—Polyesters derived from hydroxycarboxylic acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2867/00—Use of polyesters or derivatives thereof as mould material
- B29K2867/04—Polyesters derived from hydroxycarboxylic acids
- B29K2867/046—PLA, i.e., polyactic acid or polyactide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2911/00—Use of natural products or their composites, not provided for in groups B29K2801/00 - B29K2809/00, as mould material
- B29K2911/10—Natural fibres, e.g. wool or cotton
Definitions
- the present invention relates generally to finely ground plant matter, and more particularly to finely ground seed hulls or husks such as oat hulls, ground to a maximum particle size of 10 microns or less.
- Hard hulls, or husks, of seeds such as oat hulls, are waste products that are typically discarded or sold very cheaply, where producers of those hulls generally have to pay to discard the hulls.
- the outermost layer of the oat grain is the oat hull fiber which contains high amounts of cellulose, insoluble non-cellulosic polysaccharides, and lignin.
- the most common varieties of oats grown today have approximately 20 - 35% of their weight from the hulls. In the unprocessed state, these hulls contain approximately 85% insoluble dietary fiber and, with further processing to bleached oat fiber, the insoluble dietary content can be more than 90%.
- Oat hulls contain cellulose, hemicellulose and lignin in a framework comprising the cell walls.
- Hemicellulose is a polysaccharide containing a number of simple sugars in addition to glucose. Others have reported the presence of mannose and ribose in addition to sugars.
- By-products from an agricultural milling process include hulls or mill feeds, which are very inexpensive.
- Oat hulls are typically managed by oat processors as a waste stream, or as a very low value stream. Values to the processor can be from a negative value up to its value as an energy source for boiler steam. Uses by downstream parties include animal bedding, burning as a fuel source, and emergency low digestibility winter cattle feed filler. No broad use of oat hulls with a value comparable to other types of biomass, such as alfalfa, is enjoyed by bulk purchasers of oat hulls. Oat hulls and rice hulls are known for their abrasiveness and difficulty to grind, although oat hulls are known to be less abrasive than rice hulls.
- bio-based plastics are produced by fermenting biochemicals from sugar sources such as grain and cellulose. From the core biochemicals, bioresins are produced. A lower-cost additive/filling is desired by industry to produce foam used in auto interiors, bio-strings which can be woven into ultra thin, yet strong fabrics, or extruded as thin film used in a wide range of food and other packaging, as examples. Opportunity exists to employ biomass based resins in 3D printers.
- the invention provides a finely ground biomass material made from biomass material, which is hard or dried biomass, where at least 98% of the dried biomass particles have a particle size of 20 microns or less.
- At least 98% of the particles have a particle size of 15 microns or less.
- at least 99% of the particles have a particle size of 20 microns or less.
- At least 99% of the particles have a particle size of 15 microns or less.
- At least 98% of the particles have a particle size of 10 microns or less.
- At least 75% of the particles have a particle size of 7 microns or less, and at least 25% of the particles have a particle size of 4.2 microns or less.
- At least 99% of the particles have a particle size of 10 microns or less.
- least 85% of the particles have a particle size of 7 microns or less, and at least 50% of the particles have a particle size of 4.2 microns or less.
- the finely ground biomass material may be seed hulls.
- the finely ground biomass material may oat hulls or wheat hulls.
- the invention also provides a method for producing finely ground biomass material from biomass material.
- the biomass material is first ground using a hammermill equipped with a screen having a screen with a 0.5 millimeter or smaller hole pattern until all the ground biomass particles have passed through the screen.
- the hammermilled biomass particles are then ground with a dry grinding attritor until less than 2% of the particles have a particle size greater than 20 microns.
- the hammermilled biomass particles are ground with a dry grinding attritor until less than 2% of the particles have a particle size greater than 15 microns.
- the hammermilled biomass particles are ground with a dry grinding attritor until less than 2% of the particles have a particle size greater than 10 microns.
- the method may also include forming a slurry by adding water to the ground material after the step of grinding the hammermilled biomass particles with a dry grinding ball mill.
- the slurry may then be processed using a high shear and cavitation device.
- the slurry may then be dried, and the dried material processed with an attrition mill to disagglomerate agglomerated material in the dried material.
- the biomass material may be seed hulls, which may be oat hulls or wheat hulls or rice hulls, or any other type of hull biomass.
- These methods may further include the step of compounding the ground biomass particles with plastic resin to form a plastic film.
- the invention also provides the use of the finely ground biomass material described above to form a plastic film by compounding the finely ground biomass material with resin.
- the invention also provides a plastic film formed by compounding a plastic resin with the finely ground biomass material described above.
- the plastic resin may be, for example, polylactic acid or polybutylene succinate, A filler, such as lime may also be included.
- At least 10% of the material forming the plastic film may be the finely ground biomass material.
- Preferably at least 25% or 50% of the material forming the plastic film is the finely ground biomass material
- This invention provides powdered seed hull material with very small particle sizes, such as 99% or more of the material being less than 10 microns, or less than 1 micron, and a process for creating the powdered seed hulls.
- the process creates unique fine fibers by ball milling particles in combinations of dry milling, wet milling in water- followed by drying, both followed by compounding with bio-based plastic resins such as PL A (polylactic acid or polylactide) or PBS (polybutylene succinate) to compound the resin and particles while dis-agglomerating the final fiber products to achieve a controlled upper target particle size mostly no greater than individual particle sizes created before agglomeration.
- bio-based plastic resins such as PL A (polylactic acid or polylactide) or PBS (polybutylene succinate)
- the powdered material may be used in thin dimension products such as plastic films, or particles, in the presence of plastic resins and optional fillers, above 10% of biomass-to-plastic-resin ratios, including percentages up to 80%, such as 25%, 50% or 60%.
- extremely thin films of resins containing or not containing processed fibers as described herein can be used in single or multiple layers to create the outer layers of a thin sheet in which fine fibers, or fine fibers in a compound of resins and optional fillers such as calcium carbonate is filled in between the outer layers described above, to produce a smooth surface, effectively sandwiching powdered oat hull fibers with veneers on each side of the final film to minimize or virtually eliminate, or completely eliminate measurable surface irregularities.
- the first step is to grind lignocellulosic biomass, specifically oat hulls, using a mechanical mill such as a Prater Mega Mill.TM A Fitzmill,TM which combines hammers and sharp cutting blades, may alternatively be used. Both types of machines may be configured with screens as small as 120 mesh. Other types of mechanical grinding mills can alternately be used.
- a mechanical mill such as a Prater Mega Mill.TM A Fitzmill,TM which combines hammers and sharp cutting blades, may alternatively be used. Both types of machines may be configured with screens as small as 120 mesh. Other types of mechanical grinding mills can alternately be used.
- Oat hulls acquired from an oat processing operation were hammermilled through a 0.3 millimeter screen with delta shaped holes.
- the Prater Mega Mill grinds oat hulls by contact with a set of steel hammers which swing on a central shaft driven by an electric motor.
- the hammers shatter, cut and grind and crush oat hulls into ever smaller particles until they can pass through the chosen size screen.
- Alternatives to the Prater Mega Mill include burr mills, double disk attrition mills, a new custom, and a large impact mill such as Prater's Classifier Mills (CLM).
- the CLM is a grinder/classifier mill with a screen hammermill function which recycles oversize particles back through the machine until target particle size is reached.
- a newly designed CLM type of grinder could be used within the present process with utility.
- Other systems referenced above are not designed for high percentage biomass grinding below 10 micron, but could potentially be redesigned for the process described herein.
- a Prater Mega Mill hammermill may be equipped with a screen having a 0.5 millimeter or smaller hole pattern, such as 0.3 mm as in the above described run, although screens with a 0.2 millimeter or smaller may also be employed. Larger screen hole sizes may be optionally employed to shift work to downstream processing, such as ball mills.
- the oat hulls are ground in the hammermill until all material has passed the through the screen.
- hammermilled oat hulls with a moisture content of about 7.3% may be processed with a dry grinding attritor, such as a Union ProcessTM SD- 50 attritor for a period such as about 150 minutes.
- the attritor is a vertical shaft ball mill with a 75 hp engine and a ball mill tank that can hold 81 gallons.
- the ball mill grinding tank was filled with stainless steel grinding media balls weighing 1520 pounds representing about 38/81 of the volume of the stainless steel tank.
- Horizontal arms attached to a vertical shaft move the stainless steel balls around the shaft at about 150 RPM. 34.2 pounds of oat hulls were added to the steel media balls in the process tank.
- the final processed powdered oat hull yield was about 33.1 pounds due to system losses.
- the temperature of powder during processing was about 150-175°F .
- the powdered oat hulls were processed in the attritor for about 2.5 hours and the processed oat hulls were separated by opening an exit valve while the mixing arms continued rotating, causing the fine powders to fall off the balls through the exit port.
- the attritor was operated with an open port on the bottom to allow powder to systematically exit the tank, and to separate from the media balls. The powder is recovered and tested.
- 99.35% of the particles were recorded by Micro Distribuo be less than 10 micron mesh, while 90% were recorded by Micro Distribuo be less than 7.02 micron mesh and 50% were recorded by Micro Distribuo be less than 4.16 micron mesh.
- the generally ⁇ 10 micron particles are blended with a choice of plastic resins, such as polylactic acid (PLA) or polybutylene succinate (PBS) resins, both biomass derived "bioplastic resins", at a temperature suitable for pumping with a progressive cavity pump, such as a Moyno or other similar brand.
- plastic resins such as polylactic acid (PLA) or polybutylene succinate (PBS) resins, both biomass derived "bioplastic resins”
- PBS polybutylene succinate
- the resin based slurry which can consist of 10% particles to 90% resin, up to 80% biomass and 20% resin, or 60% biomass, 20% lime filler, or other combinations of the above, is flowed into an attritor or other type of ball mill such as a Netsch horizontal ball mill to blend the fiber, resin and optional lime filler to
- the above described ball mill based disagglomeration is combined in sequence, repeated as necessary, with traditional compounding systems.
- the embodiments described above generally refer to oat hulls by way of example, the invention is not limited to finely ground oat hull material.
- the above-described methods can be used to produce finely ground versions of various dried or relatively hard biomass materials, such as hulls of wheat, corn, wheat, rice, beans and various seeds.
- a "hull” (or husk) in general is the outer shell or coating of a seed.
- particle size of a particle means the length of the largest dimension of the particle. For example, if a particle is generally spherical, then the particle size is the diameter of the particle. Although it is preferred that, for example, 99% or more of the material has a particle size of less than 10 microns,
- embodiments where, for example, 98% or 99% of the material has a particle size of less than 20 microns are also within the scope of the invention, as are embodiments where 98% or 99% of the material has a particle size of less than 15 microns.
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Food Science & Technology (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention is a finely ground biomass material made from biomass material, where at least 98% of the biomass particles have a particle size of 20 microns or less. The invention also provides a method for producing finely ground biomass material from biomass material. The biomass material is first ground using a hammermill equipped with a screen having a screen with a 0.5 millimeter or smaller hole pattern until all the ground biomass particles have passed through the screen. The hammermilled biomass particles are then ground with a dry grinding attritor until less than 2% of the particles have a particle size greater than 20 microns. The method may also include forming a slurry by adding water to the ground material. The slurry may then be processed using a high shear and cavitation device, dried, and processed with an attrition mill to disagglomerate agglomerated material in the dried material.
Description
FINELY GROUND BIOMASS
CROSS-REFERENCE TO RELATED APPLICATIONS
[01] This application claims priority to U.S. Provisional Patent Application No. 61/912,233, filed December 5, 2013 the entire contents of which are incorporated herein by reference in its entirely.
FIELD OF THE INVENTION
[02] The present invention relates generally to finely ground plant matter, and more particularly to finely ground seed hulls or husks such as oat hulls, ground to a maximum particle size of 10 microns or less.
BACKGROUND OF THE INVENTION
[03] Hard hulls, or husks, of seeds such as oat hulls, are waste products that are typically discarded or sold very cheaply, where producers of those hulls generally have to pay to discard the hulls.
[04] The outermost layer of the oat grain is the oat hull fiber which contains high amounts of cellulose, insoluble non-cellulosic polysaccharides, and lignin. The most common varieties of oats grown today have approximately 20 - 35% of their weight from the hulls. In the unprocessed state, these hulls contain approximately 85% insoluble dietary fiber and, with further processing to bleached oat fiber, the insoluble dietary content can be more than 90%.
[05] Oat hulls contain cellulose, hemicellulose and lignin in a framework comprising the cell walls. Hemicellulose is a polysaccharide containing a number of simple sugars in addition to glucose. Others have reported the presence of mannose and ribose in addition to sugars.
[06] By-products from an agricultural milling process include hulls or mill feeds, which are very inexpensive.
[07] Oat hulls are typically managed by oat processors as a waste stream, or as a very low value stream. Values to the processor can be from a negative value up to its value as an energy source for boiler steam. Uses by downstream parties include
animal bedding, burning as a fuel source, and emergency low digestibility winter cattle feed filler. No broad use of oat hulls with a value comparable to other types of biomass, such as alfalfa, is enjoyed by bulk purchasers of oat hulls. Oat hulls and rice hulls are known for their abrasiveness and difficulty to grind, although oat hulls are known to be less abrasive than rice hulls.
[08] While the potential utility of such finely ground seed hulls is clear, nobody has produced a finely ground material, suitable for high value, small dimension plastics manufacturing. Ground agricultural by-products having particle sizes of about 25 to 50 microns have been reported, such as ground corn hominy as fine as 40 microns. The use of such material to form containers has been disclosed, although generally the finer materials are formed from by-products other than oat hulls, largely starch with minimal cellulose. Oat hulls may be more difficult to grid very finely to reach a marketable value in direct plastic compounding.
[09] Presently, "green" bio-based plastics are produced by fermenting biochemicals from sugar sources such as grain and cellulose. From the core biochemicals, bioresins are produced. A lower-cost additive/filling is desired by industry to produce foam used in auto interiors, bio-strings which can be woven into ultra thin, yet strong fabrics, or extruded as thin film used in a wide range of food and other packaging, as examples. Opportunity exists to employ biomass based resins in 3D printers.
[10] The cost for foam resins is about 70 cents per pound, and thin film plastics resins cost between 90 cents and $1.00 per pound. Manufacturing biomass fillers which can create small dimension particles or films at a cost below those described above holds market potential in the billions of dollars per annum
SUMMARY OF THE INVENTION
[11] The invention provides a finely ground biomass material made from biomass material, which is hard or dried biomass, where at least 98% of the dried biomass particles have a particle size of 20 microns or less.
[12] Preferably, at least 98% of the particles have a particle size of 15 microns or less.
[13] Preferably, at least 99% of the particles have a particle size of 20 microns or less.
[14] Preferably, at least 99% of the particles have a particle size of 15 microns or less.
[15] Preferably, at least 98% of the particles have a particle size of 10 microns or less.
[16] Preferably, at least 75% of the particles have a particle size of 7 microns or less, and at least 25% of the particles have a particle size of 4.2 microns or less.
[17] Preferably, at least 99% of the particles have a particle size of 10 microns or less.
[18] In some embodiments, least 85% of the particles have a particle size of 7 microns or less, and at least 50% of the particles have a particle size of 4.2 microns or less.
[19] The finely ground biomass material may be seed hulls. The finely ground biomass material may oat hulls or wheat hulls.
[20] The invention also provides a method for producing finely ground biomass material from biomass material. The biomass material is first ground using a hammermill equipped with a screen having a screen with a 0.5 millimeter or smaller hole pattern until all the ground biomass particles have passed through the screen. The hammermilled biomass particles are then ground with a dry grinding attritor until less than 2% of the particles have a particle size greater than 20 microns.
[21] Preferably, the hammermilled biomass particles are ground with a dry grinding attritor until less than 2% of the particles have a particle size greater than 15 microns.
[22] Preferably, the hammermilled biomass particles are ground with a dry grinding attritor until less than 2% of the particles have a particle size greater than 10 microns.
[23] The method may also include forming a slurry by adding water to the ground material after the step of grinding the hammermilled biomass particles with a dry
grinding ball mill. The slurry may then be processed using a high shear and cavitation device. The slurry may then be dried, and the dried material processed with an attrition mill to disagglomerate agglomerated material in the dried material.
[24] In these methods, the biomass material may be seed hulls, which may be oat hulls or wheat hulls or rice hulls, or any other type of hull biomass.
[25] These methods may further include the step of compounding the ground biomass particles with plastic resin to form a plastic film.
[26] The invention also provides the use of the finely ground biomass material described above to form a plastic film by compounding the finely ground biomass material with resin.
[27] The invention also provides a plastic film formed by compounding a plastic resin with the finely ground biomass material described above. The plastic resin may be, for example, polylactic acid or polybutylene succinate, A filler, such as lime may also be included. At least 10% of the material forming the plastic film may be the finely ground biomass material. Preferably at least 25% or 50% of the material forming the plastic film is the finely ground biomass material
DETAILED DESCRD?TION OF THE INVENTION
[28] This invention provides powdered seed hull material with very small particle sizes, such as 99% or more of the material being less than 10 microns, or less than 1 micron, and a process for creating the powdered seed hulls. The process creates unique fine fibers by ball milling particles in combinations of dry milling, wet milling in water- followed by drying, both followed by compounding with bio-based plastic resins such as PL A (polylactic acid or polylactide) or PBS (polybutylene succinate) to compound the resin and particles while dis-agglomerating the final fiber products to achieve a controlled upper target particle size mostly no greater than individual particle sizes created before agglomeration. Additional particle size reduction, or major particle size reduction to ultimate target upper particle size in combination with disagglomeration is employed to achieve resins which can be converted into thin film with small particles, or thin string surfaces with smooth appearance and/or function.
[29] The powdered material may be used in thin dimension products such as plastic films, or particles, in the presence of plastic resins and optional fillers, above 10% of biomass-to-plastic-resin ratios, including percentages up to 80%, such as 25%, 50% or 60%. In one embodiment, extremely thin films of resins containing or not containing processed fibers as described herein can be used in single or multiple layers to create the outer layers of a thin sheet in which fine fibers, or fine fibers in a compound of resins and optional fillers such as calcium carbonate is filled in between the outer layers described above, to produce a smooth surface, effectively sandwiching powdered oat hull fibers with veneers on each side of the final film to minimize or virtually eliminate, or completely eliminate measurable surface irregularities.
[30] In a preferred embodiment of the method, the first step is to grind lignocellulosic biomass, specifically oat hulls, using a mechanical mill such as a Prater Mega Mill.™ A Fitzmill,™ which combines hammers and sharp cutting blades, may alternatively be used. Both types of machines may be configured with screens as small as 120 mesh. Other types of mechanical grinding mills can alternately be used.
[31] Hammermilling with a Prater Mega Mill was performed with the following configuration.
[32] Oat hulls acquired from an oat processing operation were hammermilled through a 0.3 millimeter screen with delta shaped holes. The Prater Mega Mill grinds oat hulls by contact with a set of steel hammers which swing on a central shaft driven by an electric motor. The hammers shatter, cut and grind and crush oat hulls into ever smaller particles until they can pass through the chosen size screen.
[33] This resulted in the following distribution of particle sizes. The powder was passed through meshes of varying sizes to assess the particle size distribution.
[34] Thus, 66% of the powdered oat hull material had a particle size of 150 microns or less and 17% had a particle size of 45 microns or less.
[35] Alternatives to the Prater Mega Mill include burr mills, double disk attrition mills, a new custom, and a large impact mill such as Prater's Classifier Mills (CLM). The CLM is a grinder/classifier mill with a screen hammermill function which recycles oversize particles back through the machine until target particle size is reached. However, testing has shown that, while the CLM is capable of producing a substantial number of particles below 10 micron, it was not feasible to get everything below 10 micron and available equipment is more suitable for very small volume processing, but not volumes which can practically address the market potential. A newly designed CLM type of grinder could be used within the present process with utility. Other systems referenced above are not designed for high percentage biomass grinding below 10 micron, but could potentially be redesigned for the process described herein.
[36] A Prater Mega Mill hammermill may be equipped with a screen having a 0.5 millimeter or smaller hole pattern, such as 0.3 mm as in the above described run, although screens with a 0.2 millimeter or smaller may also be employed. Larger screen hole sizes may be optionally employed to shift work to downstream processing, such as ball mills. The oat hulls are ground in the hammermill until all material has passed the through the screen.
[37] In a second step, hammermilled oat hulls with a moisture content of about 7.3%, may be processed with a dry grinding attritor, such as a Union Process™ SD-
50 attritor for a period such as about 150 minutes. The attritor is a vertical shaft ball mill with a 75 hp engine and a ball mill tank that can hold 81 gallons. In one run, the ball mill grinding tank was filled with stainless steel grinding media balls weighing 1520 pounds representing about 38/81 of the volume of the stainless steel tank. Horizontal arms attached to a vertical shaft move the stainless steel balls around the shaft at about 150 RPM. 34.2 pounds of oat hulls were added to the steel media balls in the process tank. The final processed powdered oat hull yield was about 33.1 pounds due to system losses. The temperature of powder during processing was about 150-175°F .The powdered oat hulls were processed in the attritor for about 2.5 hours and the processed oat hulls were separated by opening an exit valve while the mixing arms continued rotating, causing the fine powders to fall off the balls through the exit port. Upon completion of grinding, the attritor was operated with an open port on the bottom to allow powder to systematically exit the tank, and to separate from the media balls. The powder is recovered and tested. Upon completion of grinding, 99.35% of the particles were recorded by Microtrakto be less than 10 micron mesh, while 90% were recorded by Microtrakto be less than 7.02 micron mesh and 50% were recorded by Microtrakto be less than 4.16 micron mesh.
[38] In one embodiment, the generally <10 micron particles are blended with a choice of plastic resins, such as polylactic acid (PLA) or polybutylene succinate (PBS) resins, both biomass derived "bioplastic resins", at a temperature suitable for pumping with a progressive cavity pump, such as a Moyno or other similar brand. The resin based slurry which can consist of 10% particles to 90% resin, up to 80% biomass and 20% resin, or 60% biomass, 20% lime filler, or other combinations of the above, is flowed into an attritor or other type of ball mill such as a Netsch horizontal ball mill to blend the fiber, resin and optional lime filler to
disagglomerate the mainly <10 micron particles from each other until the target maximum particle size is achieved before the final plastic is cooled and formed into pellets, thin sheets, strings or small individual plastic compound particles.
Optionally, the above described ball mill based disagglomeration is combined in sequence, repeated as necessary, with traditional compounding systems.
[39] While the embodiments described above generally refer to oat hulls by way of example, the invention is not limited to finely ground oat hull material. As will be appreciated by skilled persons, the above-described methods can be used to produce finely ground versions of various dried or relatively hard biomass materials, such as hulls of wheat, corn, wheat, rice, beans and various seeds. A "hull" (or husk) in general is the outer shell or coating of a seed.
[40] As used herein "particle size" of a particle means the length of the largest dimension of the particle. For example, if a particle is generally spherical, then the particle size is the diameter of the particle. Although it is preferred that, for example, 99% or more of the material has a particle size of less than 10 microns,
embodiments where, for example, 98% or 99% of the material has a particle size of less than 20 microns are also within the scope of the invention, as are embodiments where 98% or 99% of the material has a particle size of less than 15 microns.
[41] It should be understood that the above-described embodiments of the present invention, particularly, any "preferred" embodiments, are only examples of implementations; merely set forth for a clear understanding of the principles of the invention. Many variations and modifications may be made to the above-described embodiments) of the invention as will be evident to those skilled in the art.
[42] Where, in this document, a list of one or more items is prefaced by the expression "such as" or "including", is followed by the abbreviation "etc.", or is prefaced or followed by the expression "for example", or "e.g.", this is done to expressly convey and emphasize that the list is not exhaustive, irrespective of the length of the list. The absence of such an expression, or another similar expression, is in no way intended to imply that a list is exhaustive. Unless otherwise expressly stated or clearly implied, such lists shall be read to include all comparable or equivalent variations of the listed item(s), and alternatives to the item(s), in the list that a skilled person would understand would be suitable for the purpose that the one or more items are listed.
[43] Where, in this document, including the claims, the conjunction "or" is used in a list, such as in "w is done by performing x, performing y or by performing z", unless otherwise clearly implied, the "or" is non-exclusive. In this example, w may
therefore be done by performing all of x, y and z, performing any two of x, y and z, or performing any one of x, y and z, unless the simultaneous performance is not possible or does not make sense.
[44] The words "comprises" and "comprising", when used in this specification and the claims, are to used to specify the presence of stated features, elements, integers, steps or components, and do not preclude, nor imply the necessity for, the presence or addition of one or more other features, elements, integers, steps, components or groups thereof.
[45] The scope of the claims that follow is not limited by the embodiments set forth in the description. The claims should be given the broadest purposive construction consistent with the description as a whole.
Claims
What is claimed is:
1. A finely ground biomass material comprising biomass material comprising particles where at least 98% of the particles have a particle size of 20 microns or less.
2. The finely ground biomass material of claim 1, wherein at least 98% of the particles have a particle size of 15 microns or less.
3. The finely ground biomass material of claim 1, wherein at least 99% of the particles have a particle size of 20 microns or less.
4. The finely ground biomass material of claim 1, wherein at least 99% of the particles have a particle size of 15 microns or less.
5. The finely ground biomass material of claim 1, wherein at least 98% of the particles have a particle size of 10 microns or less.
6. The finely ground biomass material of claim 5, wherein at least 75% of the particles have a particle size of 7 microns or less, and at least 25% of the particles have a particle size of 4.2 microns or less.
7. The finely ground biomass material of claim 1, wherein at least 99% of the particles have a particle size of 10 microns or less.
8. The finely ground biomass material of claim 7, wherein at least 85% of the particles have a particle size of 7 microns or less, and at least 50% of the particles have a particle size of 4.2 microns or less.
9. The finely ground biomass material of any one of claims 1 to 8, wherein the biomass material is seed hulls.
10. The finely ground biomass material of claim 9, wherein the biomass material is oat hulls.
11. The finely ground biomass material of claim 9, wherein the biomass material is wheat hulls.
plastic film by compounding the finely ground biomass material with resin.
13. A method for producing finely ground biomass material, the method comprising the steps of:
(a) providing biomass material;
(b) grinding the biomass material using a hammermill equipped with a
screen having a screen with a 0.5 millimeter or smaller hole pattern until all the ground biomass particles have passed through the screen; and
(c) grinding the hammermilled biomass particles with a dry grinding attritor until less than 2% of the particles have a particle size greater than 20 microns.
14. The method of claim 13, wherein the hammermilled biomass particles are
ground with a dry grinding attritor until less than 2% of the particles have a particle size greater than 15 microns.
15. The method of claim 14, wherein the hammermilled biomass particles are
ground with a dry grinding attritor until less than 2% of the particles have a particle size greater than 10 microns.
16. The method of claim 13, further comprising the step of compounding the ground biomass particles with plastic resin to form a plastic film.
17. The method of claim 13, further comprising the steps of:
(d) after the step of grinding the hammermilled biomass particles with a dry grinding attritor, forming a slurry by adding water to the ground material;
(e) processing the slurry using a high shear and cavitation device;
(f) drying the slurry after processing the slurry using a high shear and
cavitation device; and
(g) processing the dried material with an attrition mill to disagglomerate agglomerated material in the dried material.
18. The method of claim 17, further comprising the step of compounding the dried material with plastic resin to form a plastic film.
19. The method of and one of claims 13 to 18, wherein the biomass material is seed hulls.
20. The method of and one of claims 13 to 18, wherein the biomass material is oat hulls.
21. The method of and one of claims 13 to 18, wherein the biomass material is wheat hulls.
22. A plastic film formed by compounding a plastic resin with the finely ground biomass material of any one of claims 1 to 8.
23. The plastic film of claim 22, wherein the plastic resin is polylactic acid.
24. The plastic film of claim 22, wherein the plastic resin is polybutylene succinate.
25. The plastic film of claim 22 further comprising a filler.
26. The plastic film of claim 22, wherein the filler is lime.
27. The plastic film of claim 22, wherein at least 10% of the material forming the plastic film is the finely ground biomass material.
28. The plastic film of claim 27, wherein at least 25% of the material forming the plastic film is the finely ground biomass material.
29. The plastic film of claim 28, wherein at least 50% of the material forming the plastic film is the finely ground biomass material.
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