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Sommaire du brevet 2780589 

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Disponibilité de l'Abrégé et des Revendications

L'apparition de différences dans le texte et l'image des Revendications et de l'Abrégé dépend du moment auquel le document est publié. Les textes des Revendications et de l'Abrégé sont affichés :

  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Brevet: (11) CA 2780589
(54) Titre français: SYSTEMES ET PROCEDES DE SEPARATION DE SOLIDES EN SUSPENSION
(54) Titre anglais: SUSPENDED SOLIDS SEPARATION SYSTEMS AND METHODS
Statut: Réputé périmé
Données bibliographiques
(51) Classification internationale des brevets (CIB):
  • C12F 3/10 (2006.01)
  • C13B 20/16 (2011.01)
  • B01D 21/00 (2006.01)
(72) Inventeurs :
  • KOHL, SCOTT (Etats-Unis d'Amérique)
  • GALLOP, CHARLES C. (Etats-Unis d'Amérique)
  • DIEKER, KURT A. (Etats-Unis d'Amérique)
(73) Titulaires :
  • ICM, INC. (Etats-Unis d'Amérique)
(71) Demandeurs :
  • ICM, INC. (Etats-Unis d'Amérique)
(74) Agent: RIDOUT & MAYBEE LLP
(74) Co-agent:
(45) Délivré: 2013-09-24
(22) Date de dépôt: 2012-06-21
(41) Mise à la disponibilité du public: 2012-08-31
Requête d'examen: 2012-06-21
Licence disponible: S.O.
(25) Langue des documents déposés: Anglais

Traité de coopération en matière de brevets (PCT): Non

(30) Données de priorité de la demande:
Numéro de la demande Pays / territoire Date
61/501,030 Etats-Unis d'Amérique 2011-06-24

Abrégés

Abrégé français

Un procédé qui consiste à clarifier une vinasse dans un processeur mécanique pour produire un flux de solides fins en suspension et une vinasse clarifiée. Le procédé consiste en plus à amener la vinasse et la vinasse clarifiée, séparément ou dans un flux combiné, à un ou plusieurs évaporateurs afin de produire un ou plusieurs flux à teneur réduite de solides en suspension, chaque flux ayant une quantité réduite de solides en suspension et une viscosité inférieure à celle de flux de procédés ayant une teneur en solides totale comparable, mais une plus grande quantité de solides en suspension. Le procédé peut de plus consister à effectuer un traitement supplémentaire d'un ou de plusieurs des flux à teneur réduite de solides en suspension afin de produire de la biohuile.


Abrégé anglais

A method that includes clarifying a thin stillage product in a mechanical processor to produce a fine suspended solids stream and a clarified thin stillage is provided. The method further includes providing the thin stillage product and the clarified thin stillage, separately or in a combined stream, to one or more evaporators to produce one or more reduced suspended solids streams, each stream having a reduced amount of suspended solids and a lower viscosity as compared to process streams having a comparable total solids content but containing a higher amount of suspended solids. The method can further included further processing of one or more of the reduced suspended solids streams to produce a bio-oil product.

Revendications

Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.



WHAT IS CLAIMED IS:

1. A method comprising:
clarifying a thin stillage product in a mechanical processor to produce a fine

suspended solids stream and a clarified thin stillage; and
providing the thin stillage product and the clarified thin stillage,
separately or in a
combined stream, to one or more evaporators to produce one or more reduced
suspended
solids streams, each stream having a reduced amount of suspended solids and a
lower
viscosity as compared to process streams having a comparable total solids
content and
which contains a higher amount of suspended solids.
2. The method of claim 1, wherein asuspended solids stream comprises less
than about 10% by weight of the total solids content and the total solids
content is
between about 68% and about 72% by weight.
3. The method of claim 1, wherein at least one of the one or more reduced
suspended solids stream has a total solids content comprising suspended solids
and
dissolved solids in an amount between about 30% and about 90% by weight,
wherein the
suspended solids comprise less than 25% by weight of the total solids content.
4. The method of claim 1, wherein at least one of the one or more reduced
suspended solids stream is a clarified concentrated thin stillage, which
contains an
amount of bio-oil which is greater, by volume, than an amount of bio-oil
present in a
concentrated thin stillage which has not been clarified.
5. The method of claim 4, wherein the clarified concentrated thin stillage
is
subject to mechanical processing to produce a bio-oil product.
6. The method of claim 5, wherein the mechanical processing produces an
emulsion concentrate which is broken in an emulsion breaking reaction to
produce a bio-
oil phase.



7. The method of claim 5, wherein the mechanical processing also produces
a solids stream and a de-oiled clarified concentrated thin stillage product,
and further
comprises providing the de-oiled clarified concentrated thin stillage product
to the one or
more evaporators.
8. The method of claim 1, wherein at least one of the one or more reduced
suspended solids stream is a molasses product having a total solids content no
less than
about 45% by weight, wherein the suspended solids comprise less than 25% by
weight
down to 0% of the total solids content.
9. The method of claim 1, wherein substantially all of the clarified thin
stillage is provided to the thin stillage product.
10. The method of claim 1, further comprising:
combining at least a portion of the one or more reduced suspended solids
streams
with wet cake to produce a wet cake product containing reduced suspended
solids; and
drying the wet cake product to produce a distillers dried grain.
11. The method of claim 1, further comprising:
providing at least a portion of the one or more reduced suspended solids
streams to
a dryer to produce distiller's dried grain solubles.
12. The method of claim 1, further comprising drying the fine suspended
solids stream to produce dry distiller's solubles containing single cell
proteins.
13. The method of claim 1, wherein the thin stillage product is produced
from
low water extractable non-starch polysaccharide-containing plant biomass.
14. The method of claim 1, producing a product comprising a concentrated
thin stillage, a clarified thin stillage or a fine suspended solids stream.

41


15. The method of claim 1, producing a product comprising a fine suspended
solids stream, a molasses product, dry distiller's solubles, wet cake product,
distiller's
dry grain, distiller's dry grain solubles, or combinations thereof.
16. A method comprising:
clarifying a thin stillage product in a mechanical processor to produce a fine

suspended solids stream and a clarified thin stillage;
providing the thin stillage product and the clarified thin stillage,
separately or in a
combined stream, to one or more evaporators to produce at least two reduced
suspended
solids streams, each of the at least two streams having a reduced amount of
suspended
solids and a lower viscosity as compared to process streams having a
comparable total
solids content but containing a higher amount of suspended solids; and
subjecting at least one of the at least two reduced suspended solids streams
to
mechanical processing to produce a bio-oil product.
17. The method of claim 16, wherein the at least two reduced suspended
solids streams comprise a stream containing a clarified concentrated thin
stillage and a
stream containing a molasses product, wherein the clarified concentrated thin
stillage is
subjected to the mechanical processing.
18. The method of claim 16, wherein the mechanical processing produces an
emulsion concentrate which is broken in an emulsion breaking reaction to
produce the
bio-oil phase.
19. The method of claim 17, wherein the molasses product contains two to
three times the amount of bio-oil per volume as compared to concentrated thin
stillage.
20. The method of claim 17, wherein the molasses product has between about
65% and about 75% total solids, by weight, and contains between about 8% and
about
12% bio-oil, by volume.
21. The method of claim 17, wherein the molasses product is to be sold,
combined with wet cake, and/or dried.

42


22. A method comprising:
clarifying a thin stillage product to produce one or more reduced suspended
solids
streams, each having a total solids content between about 30% and about 90% by
weight,
wherein the total solids content comprises suspended solids and dissolved
solids, and the
suspended solids comprise less than 25% by weight of the total solids content.
23. The method of claim 22, wherein at least one of the reduced suspended
solids product is subject to mechanical processing to produce a bio-oil
product.
24. The method of claim 23, wherein the mechanical processing produces an
emulsion concentrate which is broken in an emulsion breaking reaction to
produce the
bio-oil product.
25. A system comprising:
a clarifier for clarifying a thin stillage product to produce a fine suspended
solids
stream and clarified thin stillage; and
one or more evaporators for evaporating the thin stillage product and the
clarified
thin stillage to produce one or more reduced suspended solids streams, each
having a
reduced amount of suspended solids and a lower viscosity as compared to a
process
stream having a comparable total solids content but containing a higher amount
of
suspended solids.
26. The system of claim 25, further comprising a system control device
adapted to provide a quantity of thin stillage product for use downstream.
27. The system of claim 26, wherein the system control device is a holding
tank which is optionally connected with a heat source.
28. The system of claim 25, further comprising:
a dewatering system for dewatering a bio-oil containing process stream to
produce an emulsion concentrate containing entrapped bio-oil; and

43


an emulsion breaking system configured to at least partially break the
emulsion
concentrate with an emulsion breaking additive so that the entrapped bio-oil
is
released.
29. The system of claim 28, further comprising an alcohol production
facility.
30. The system of claim 29, wherein the alcohol production facility is an
ethanol production facility.
31. The system of claim 30, wherein the bio-oil is com oil.
32. A method for reducing a dryer load in a bio-product production facility

comprising:
clarifying a thin stillage product in a mechanical processor to produce a fine

suspended solids stream and a clarified thin stillage; and
providing the thin stillage product and the clarified thin stillage,
separately or in a
combined stream, to one or more evaporators to produce one or more reduced
suspended
solids streams, each stream having a reduced amount of suspended solids and a
lower
viscosity as compared to process streams having a comparable total solids
content and
which contains a higher amount of suspended solids, wherein the dryer load is
reduced as
compared to a method performed without a clarifying step.
33. A method for improving bio-product production yield comprising:
clarifying a thin stillage product in a mechanical processor to produce a fine

suspended solids stream and a clarified thin stillage; and
providing the thin stillage product and the clarified thin stillage,
separately or in a
combined stream, to one or more evaporators to produce one or more reduced
suspended
solids streams, each stream having a reduced amount of suspended solids and a
lower
viscosity as compared to process streams having a comparable total solids
content and
which contains a higher amount of suspended solids, wherein bio-product
production
yield is increased as compared to a method performed without a clarifying
step.

44


34. The method of claim 33 wherein the bio-product is a biofuel or
biochemical.
35. A method of reducing emissions in a bio-product production facility
comprising:
clarifying a thin stillage product in a mechanical processor to produce a fine

suspended solids stream and a clarified thin stillage; and
providing the thin stillage product and the clarified thin stillage,
separately or in a
combined stream, to one or more evaporators to produce one or more reduced
suspended
solids streams, each stream having a reduced amount of suspended solids and a
lower
viscosity as compared to process streams having a comparable total solids
content and
which contains a higher amount of suspended solids, wherein emissions from the
bio-
product production facility are reduced as compared to a method performed
without a
clarifying step.


Description

Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.


CA 02780589 2013-02-04
SUSPENDED SOLIDS SEPARATION SYSTEMS AND METHODS
This application claims the benefit of U.S. Provisional Application Serial No.
61/501,030 filed June 24, 2011, U.S. Patent Application Serial No. 13/292,266
filed
November 9, 2011, U.S. Patent Application Serial No. 13/105,789 filed May 11,
2011,
now issued as U.S. Patent No. 8,192,627, U.S. Patent Application Serial No.
61/371,568
filed August 6, 2010, U.S. Patent Application Serial No. 61/420,674 filed
December 7,
2010, and U.S. Patent Application Serial No. 61/472,549, filed April 6, 2011.
Background
The methods for producing various types of alcohol from grain generally follow

similar procedures, depending on whether the grain milling process is operated
wet or
dry. One alcohol of great interest today is ethanol, which can be produced
from virtually
any type of grain, but is most often made from corn. Ethanol can also be made
from
various cellulosic sources. Ethanol production generates co-products which can
be used
as is or which can be further processed.
Summary
There is a need for improving production processes for various bio-products,
such as alcohol production co-products. By removing suspended solids in a thin
stillage
stream as described herein, not only are the total solids reduced in
downstream process
streams, the viscosity of these streams is also reduced, allowing for more
efficient
dewatering. Additionally and surprisingly, with the suspended solids removed,
soluble
solids are now easier to concentrate. As a result, water can be removed in a
more
efficient manner, thus reducing operating costs, such as natural gas costs for
dryers.
The various embodiments described herein not only allow various reduced
suspended solids streams, such as a molasses product, to be produced, but also

provide for enhanced recovery of bio-oil from alcohol production co-products.
A
solids product with enhanced amounts of fermentation aids can also be
produced.

CA 02780589 2013-02-04
Brief Description of the Drawings
Some embodiments are illustrated by way of example and not limitation in the
figures of the accompanying drawings in which:
FIG. lA is a schematic illustration of a conventional stillage processing
system;
FIG. 1B is a schematic illustration of a bio-oil recovery system;
FIG. 2 is a schematic illustration of a suspended solids separation system in
combination with a bio-oil recovery system capable of producing an emulsion
concentrate according to various embodiments;
FIG. 3 is a schematic illustration of a mechanical processor for separating
suspended solids according to various embodiments;
FIG. 4 is a schematic illustration of a suspended solids separation system in
combination with a bio-oil recovery system according to various embodiments;
FIG. 5 is a schematic illustration of a suspended solids separation system
without
a bio-oil recovery system according to various embodiments;
FIG. 6 is an image of test vials showing suspended solids capture efficiency
for a
high-speed centrifuge according to various embodiments;
FIG. 7 is an image of spin vials showing suspended capture efficiency for a
high-
speed centrifuge according to various embodiments;
FIG. 8 is a graph showing fraction emulsion versus degree Brix (i.e., sugar
content) concentration in clarified concentrated thin stillage according to
various
embodiments; and
FIG. 9 is an image of spin vials containing a molasses product according to
various embodiments.
Detailed Description of the Embodiments
In the following detailed description, embodiments are described in sufficient

detail to enable those skilled in the art to practice them, and it is to be
understood that
other embodiments may be utilized and that chemical and procedural changes may
be
made without departing from the scope of the present subject matter. The
following
detailed description is, therefore, not to be taken in a limiting sense, and
the scope of
embodiments of the present invention is defined only by the appended claims.
The various embodiments provide suspended solids separation systems and
methods related thereto. Although the systems and methods described herein
focus
2

CA 02780589 2012-06-21
primarily on separating suspended solids from thin stillage resulting from
ethanol
production, any of the systems and methods described herein can be used to
separate
suspended solids from other types of bio-product process streams, including,
for
example, various other alcohol streams, such as butanol (e.g., isobutanol),
biochemical
streams, and the like.
The term "biomass" as used herein, refers generally to organic matter
harvested
(in particular seeds such as corn kernels or wheat kernels) or collected from
a renewable
biological resource as a source of energy. The renewable biological resource
can include
plant materials (e.g., plant biomass), animal materials, and/or materials
produced
biologically. The term "biomass" is not considered to include non-renewable
fossil
fuels, such as coal, petroleum and natural gas_ These types of fossil fuels
are formed by
natural processes (such as anaerobic decomposition of long dead, buried
organisms) and
contain hydrocarbons such as alkanes, cycloalkanes, and various aromatic
hydrocarbons,
but do not normally include glycerides (e.g., tri-, di-, mono-).
The terms "plant biomass" or "ligno-cellulosic biomass" as used herein, are
intended to refer to virtually any plant-derived organic matter (woody or non-
woody)
available to produce energy on a sustainable basis. Plant biomass can include,
but is not
limited to, agricultural crop wastes and residues such as corn stover, wheat
straw, rice
straw, sugar cane, bagasse, and the like. Plant biomass can further include
byproducts of
plant biomass, such as molasses_ Plant biomass further includes, but is not
limited to,
woody energy crops, wood wastes and residues such as trees, which can include
fruit
trees, such as fruit-bearing trees, (e.g., apple trees, orange trees, and the
like), softwood
forest thinnings, barky wastes, sawdust, paper and pulp industry waste
streams, wood
fiber, and the like. The skins and/or rinds of the various fruits can also be
used as plant
biomass. Holo-cellulosic materials (hemicellulose and cellulose polymers)
found in grain
seeds, particularly those concentrated in the pericarp or hull of the seed,
but often found
in lower concentrations throughout the seed can also be used as plant biomass_
Additionally grass crops, such as various prairie grasses, including prairie
cord
grass, switchgrass, big bluestern, little bluestem, side oats grama, energy
sorghum and
the like, have the potential to be produced large-scale as additional plant
biomass
sources. For urban areas, potential plant biomass includes yard waste (e.g.,
grass
clippings, leaves, tree clippings, brush, etc.) and vegetable processing
waste. Plant
biomass is known to be the most prevalent form of carbohydrate available in
nature.
3

CA 02780589 2012-06-21
The term "low water extractable non-starch polysaccharide-containing plant
biomass" or "low NSP plant biomass," as used herein, refers to plant biomass
containing
less than about 0.5%, by weight, down to 0% NSP. Corn, in particular the corn
kernel, is
one example of a low NSP plant biomass.
The term "biofuel" as used herein, refers to any renewable solid, liquid or
gaseous fuel produced biologically, such as bin-oils, including for example,
bio-oils
derived from biomass. Most biofuels are originally derived from biological
processes
such as the photosynthesis process and can therefore be considered a solar or
chemical
energy source. Biofuels can be derived from biomass synthesized during
photosynthesis,
such as with agricultural biofuels (defined below). Other biofuels include
algaculture
biofuels (from algae), municipal waste biofuels (residential and light
commercial
garbage or refuse, with most of the recyclable materials such as glass and
metal
removed) and forestry biofuels (e.g., trees, waste or byproduct streams from
wood
products, wood fiber, pulp and paper industries). Biofuels also include, but
are not
limited to, biodiesels, bioethanol (i.e., ethanol), biogasoline, biomethanol,
biobutanol,
biogas, and the like.
The term "bio-oil" as used herein, refers to food-grade and non-food grade
oils
and fats that are derived from plants and/or animals (e.g., vegetable oils and
animal fats,
which contain primarily triglycerides, but can also contain fatty acids,
diglycerides, and
monoglycerides. (As used herein, the term "fat" is understood to include
"lipids").
Examples of bio-oils derived from plants include, but are not limited to, corn
oil,
flaxseed oil, canola oil, and the like. See also the listing of biofuel
sources noted in the
definition for "agricultural biofuel" below, which are also useful as sources
for bio-oil.
The term "agricultural biofuel" as used herein refers to a biofuel derived
from
agricultural crop (e.g., grains, such as corn and soybeans) plant biomass,
crop residues,
grain processing facility wastes (e_g., wheat/oat hulls, corn/bean fines, out-
of-
specification agricultural or biomass materials, etc.), livestock production
facility waste
(e.g., manure, carcasses, etc.), livestock processing facility waste (e.g.,
undesirable parts,
cleansing streams, contaminated materials, etc.), food processing facility
waste (e.g.,
separated waste streams such as grease, fat, stems, shells, intermediate
process residue,
rinsing/cleansing streams, etc.), value-added agricultural facility co-
products (e.g.,
distiller's grain of any moisture content and/or syrup from ethanol production
facilities,
etc.), and the like. Examples of livestock include, but are not limited to,
cattle, hogs,
4

CA 02780589 2012-06-21
turkey, fish or chicken. Examples of agricultural crops include, but are not
limited to,
any type of non-woody plant (e.g., cotton), grains, including any type of
cereal grains
such as corn, wheat, soybeans, sorghum, barley, oats, rye, milo, rape seeds,
canola,
sunflower, pennycress, and the like, herbs (e.g., peanuts), herbaceous crops
such as
switchgrass, alfalfa, other starch containing crops such as bagasse,
sugarcane, and other
bio-oil-bearing starch or sugar based materials, and so forth. Ethanol and
biodiesel are
examples of agricultural biofuels.
The term "stillage" as used herein refers to a co-product produced during
production of a biofuel, and is sometimes referred to as "slop." When used
without
qualification, the term "stillage" can refer to whole stillage, thin stillage,
or concentrated
stillage (such as condensed distillers soluble, i.e., syrup, which can be
produced from
biofuel process streams, e.g., ethanol production process streams). Such
streams contain
soluble organic and inorganic compounds, suspended materials containing
protein,
carbohydrate, and bio-oil fractions and may have a free bio-oil component and
an
emulsified bio-oil component, or all of the bio-oil may be emulsified.
The term "free oil" or "free bio-oil" as used herein, refers to a bio-oil that
is not
emulsified, physically or chemically bound or trapped by components in the
process
stream and can be phase separated from the process stream, i.e., recovered
from the
process stream via mechanical processing and/or non-mechanical processing as
defined
herein.
The terms "emulsion" or "emulsified layer" as used herein refer to a mixture
of
two or more immiscible (unblendable) liquids, i.e., liquids that are sparingly
soluble
within each other. Emulsions are part of a more genera] class of two-phase
systems of
matter called colloids. Although the terms colloid and emulsion are sometimes
used
interchangeably, emulsion tends to imply that both the dispersed and the
continuous
phase are liquid. In an emulsion, one liquid (the dispersed phase) is
dispersed in the other
(the continuous phase) (Wikipedia http://en.wikipedia.org/wilci/Emulsion).
Whether an
emulsion becomes a water-in-oil emulsion or an oil-in-water emulsion depends
on the
volume fraction of both phases and on the type of emulsifier.
Generally, the Bancroft rule applies, which suggests that emulsifiers and
emulsifying particles tend to promote dispersion of the phase into which they
are not
well dissolved; for example, proteins dissolve better in water than in oil. As
a result,
5

CA 02780589 2012-06-21
proteins tend to form oil-in-water emulsions, i.e., proteins promote the
dispersion of oil
droplets throughout a continuous phase of water.
An emulsion can contain entrapped components, such as bio-oil, as well as
other
components, including, but not limited to, starches, free fatty acids (FFA)
(e.g., arachidic
acid, stearic acid, palmitic acid, erucic acid, oleic acid, arachidonic acid,
linoleic acid
and/or linolenic acid), fatty acid lower(alkyl) esters, phospholipids, grain
germ fractions,
yeast, protein, fiber, glycerol, residual sugars, other organic compounds
and/or other
inorganic compounds such as anion and cation salts of organic acids (e.g.,
metallic salts
such as sodium sulfate, sodium sulfite, magnesium sulfate and potassium
phytate,
magnesium phytate, magnesium phosphate, sodium carbonate, magnesium oxalate,
calcium oxalate, caratenoids, and/or antioxidants).
The term "emulsion concentrate" as used herein refers to a stable emulsion
(water-in-bio-oil or bio-oil-in-water) containing minor amounts of other
components
from a processing stream, such as from the processing streams described
herein.
The term "mechanical processing" or "mechanical process" as used herein refers
to interaction of a machine or device with any portion of a process stream
sufficient to
cause or alter motion of the process stream. Mechanical processing is
accomplished with
mechanical force and/or addition and/or reduction of kinetic energy.
The term "mechanical processor" OT device as used herein refers to a machine
or
device (with or without moving parts) capable of carrying out mechanical
processing and
can further include a device capable of carrying out mechanical processing in
combination with non-mechanical processing (such as the use of a centrifuge to
add
centripetal force to aid phase separation caused by gravity).
The term "non-mechanical processing" or "non-mechanical process" as used
herein refers to a non-mechanical process that causes change in a process
stream other
than by imparting and/or altering motion of the processing stream. A non-
mechanical
process includes any type of chemical process such as gravity separation.
The term "non-mechanical processor" as used herein refers to a machine or
device capable of carrying out non-mechanical processing on a process stream.
One
example of a non-mechanical processor is a gravity-settling tank.
The term "chemical processing" or "chemical process" as used herein refers to
a
process that changes the composition of the process stream in one or more
steps with or
without the use of added components and with or without added (or reduced)
heat and/or
6

CA 02780589 2012-06-21
added or reduced pressure. A chemical reaction is one type of chemical
process. One
example of such a reaction is the emulsion breaking reaction as described in
the '627
Patent. Other examples of a chemical process include catalysis, coagulation,
and
flocculation. A chemical process can also refer to a passive chemical process.
The term "passive chemical processing" or "passive chemical process" as used
herein refers to a process that allows a chemical change to occur naturally in
a process
stream over time without adding additional components to the process stream
and/or
heating and/or pressurizing the process stream. Gravity separation of phases
in a process
stream is one example of a passive chemical process as it uses only the force
of gravity
to allow separation to occur.
The term "aqueous phase" as used herein refers to a process stream containing
primarily water and solids,-and which can further contain glycerin, acetic
acid, sulfuric
acid, residual soluble sugars, soluble proteins, and trace minerals, such as
Mg, Fe, and
Ca. In the system described in the'789 Application, the aqueous phase further
includes
an amount of emulsion breaking additive (as defined therein).
The term "bio-oil phase" as used herein refers to a process stream containing
primarily bio-oil, and which can further contain an amount of emulsion
breaking additive
and other minor components.
The term "evaporation" as used herein refers to removal or vaporization of a
solvent. Use of increased temperature and/or decreased pressure is one type of
evaporation that is often referred to as "flashing" or "flash evaporation."
The term "total solids" as used herein refers to all components in a process
stream other than water. When used without qualification, the term "solids" is
intended
to refer to total solids, by weight.
The term "dissolved solids" or "solubles" as used herein refers to solid
particles
that are mixed sufficiently with the fluid in a process steam such that they
do not
separate from the process stream during mechanical processing.
The term "fine suspended solids stream" as used herein refers to a process
stream
containing suspended solid particles, i.e., "insolubles," which can be
separated from the
process stream. The particles in the fine suspended solids stream are
primarily less than
about 20 micrometers in diameter, but can also include larger solid particles.
The term "thin stillage" as used herein refers to a conventional process
stream
produced as a co-product of alcohol production (e.g., ethanol production)
which contains
7

CA 02780589 2012-06-21
between about 3% and about 15%, by weight, of total solids, of which about 25%
to 75%
are suspended solid particles.
The term "concentrated thin stillage" or "syrup" as used herein refers to a
conventional process stream produced as a co-product of alcohol production
(e.g.,
ethanol production) which contains between more than about 20% up to about
45%, by
weight, of solids, of which about 25% to 75% are suspended solid particles.
The term "clarified thin stillage" as used herein refers to a process stream
containing between about 3% and about 15%, by weight, of total solids, of
which less
than 25% are suspended solid particles. A clarified thin stillage stream
typically has a
cloudy appearance.
The term "thin stillage product" as used herein refers to a process steam
containing various ratios of thin stillage and clarified thin stillage. At
start-up, the thin
stillage product can comprise only thin stillage.
The term "clarified concentrated thin stillage" as used herein refers to a
process
stream containing between about 15% and 40%, by weight, of total solids, of
which less
than about 25% are suspended solid particles. A clarified concentrated thin
stillage
stream typically has a cloudy appearance.
The term "molasses product" as used herein refers to a process stream
containing
at least 45% by weight of total solids, of which less than 25% are suspended
solid
particles. As such, the "molasses product" described herein can be used as a
substitute
for conventional "molasses", which is a viscous by-product from the processing
of sugar
cane, grapes or sugar beets into sugar.
The term "reduced suspended solids stream" as used herein refers to a process
stream having any total solids content between about 2% up to substantially or
about
100%, by weight, but which has a reduced amount of suspended solids particles
as
compared to conventional process streams with comparable total solids content,
and can
further include a stream containing no suspended solid particles. Process
streams
comprised of clarified thin stillage, thin stillage product (after start-up),
clarified
concentrated thin stillage, and molasses products are examples of reduced
suspended
solids streams. Such process streams have a lower viscosity as compared to
conventional process streams with comparable total solids content as these
conventional
streams contain more suspended solid particles.
8

CA 02780589 2013-02-04
Grain-based ethanol can be produced from a wet mill process, a dry grind
ethanol
process, or a "modified" dry grind ethanol process as is understood in the
art. See, for
example, Kohl, S., Ethanol 101: Overview of Ethanol Production, Ethanol Today,
July
2003, pp. 36-37 for a detailed description of a typical dry grind ethanol
process. See also
Patent '627 and the various Kohl references cited herein for additional
details on dry
grind and modified dry grind processes as on typical wet milling processes.
Regardless of the specific process used (wet mill, dry grind or modified dry
grind), conventional ethanol production results in useful co-products which,
after
mechanical processing, or heating and mechanical processing, are designed to
recover
free bio-oil and/or bio-oil present in an unstable emulsion. (See also the
'627 Patent in
which bio-oil is recovered from a stable emulsion).
Co-products produced as a result of distillation and dehydration include whole

stillage, which is typically subject to a centrifugation or decanter step to
separate
insoluble solids ("wet cake") from the liquid (which is oftentimes referred to
as
"centrate" until it enters a stillage tank, if present, at which point it is
sometimes referred
to as "thin stillage"). In a dry grind ethanol process, stillage enters
evaporators in order
to boil away moisture, producing a concentrated syrup containing the soluble
(dissolved)
solids from the fermentation. See, for example, Kohl, S., Ethanol 101-9:
Evaporation,
Ethanol Today, May 2004, pp 36-39.
This concentrated syrup can be mixed with the centrifuged wet cake, and the
mixture sold to beef and dairy feedlots as Distillers Wet Grain with Solubles
(DWGS).
Alternatively, the wet cake and concentrated syrup mixture may be dried and
sold as
Distillers Dried Grain with Solubles (DDGS) to dairy and beef feedlots. See,
for
example, Kohl, S., Ethanol 101-10: Drying-Production of DDGS, Ethanol Today,
June
2004, pp. 34-36.
Adding syrup to wet cake has limited economic value. Additionally, using syrup

to produce DDGS is expensive, since the dryers utilize a large amount of
energy to
evaporate water from the syrup. Additionally, syrup can contain sulfur and
salts, both of
which can lower the quality, and thus the selling price, of the DDGS. With its
lower
protein content, syrup can also dilute the protein content of the DDGS. The
appearance
9

CA 02780589 2012-06-21
of the DDGS can also be affected by addition of syrup, giving it an
undesirable brown
color.
Selling syrup as a liquid feed supplement can be about 3 to 6 times less cost
effective than selling DDGS. Syrup has a low value for a number of reasons,
such as
wide variability of composition, poor handling characteristics, high water
content
(greater than 60% by weight) and high viscosity (semi-solid) upon cooling such
that it
requires heating in order to be pumped.
In contrast, in the various embodiments described herein, at least a portion
of a
thin stillage product is provided to a mechanical processor to separate
suspended solids
(primarily fme suspended solids having a diameter less than about 20
micrometers)
present in the process stream from the dissolved solids also present in the
process stream
to produce a fine suspended solids stream
In some embodiments, the fine suspended solids stream can then be added to the

wet cake product fraction, resulting in DDGS having increased value due to the
presence
of high value components, such as single cell proteins, e.g., yeast (See, for
example, FIG_
5). As a result, the dryer load (e.g., 119) can be reduced, which not only
reduces costs
for the dryer operation, but can also allow the entire facility to run more
efficiently_ It is
also likely that the DDGS provided is of higher quality due to use of lower
dryer
temperatures.
In the various embodiments described herein, a thin stillage product from an
alcohol production facility is provided to a mechanical processor to separate
it into a fine
suspended solids stream and clarified thin stillage. Some or all of the
clarified thin
stillage is then returned to the thin stillage product. By clarifying at least
a portion of the
thin stillage and then providing the two products, either separately or in a
combined
stream, to one or more evaporators, it is now possible to produce a stream
having a
reduced suspended solids content, i.e., a reduced suspended solids stream.
Examples of
a reduced suspended solids stream include, for example, a molasses product
having a
total solids content no less than about 45% by weight, with a suspended solids
content of
less than 25% down to substantially or about 0%. In one embodiment, the fine
suspended solids stream contains fermentation aids (e.g., single cell proteins
such as
yeast), which can be dried and sold. In one embodiment, use of the solids
separation
technology in combination with bio-oil recovery systems improves bin-oil
yield.

CA 02780589 2012-06-21
Conventional attempts to remove suspended solids from process streams include
operations that separate whole stillage to produce an insoluble solids portion
containing
non-single celled high protein wain products such as corn meal. In contrast to
thin
stillage, whole stillage is known to contain large fiber and protein particles
with a
substantial portion, i.e., at least 30 up to 80% of these particles greatcr
than 20
micrometers in diameter.
Other attempts to separate stillage include various non-mechanical and/or
chemical separation techniques. Such techniques are known to result in limited

suspended solids recovery.
Other attempts to remove fine suspended particles have included electrostatic
or
ionic precipitation, which are known to achieve less than satisfactory
results. Yet other
attempts include pH adjustment to cause precipitation. However, costs of
adjusting pH
can be quite high. Additionally, higher products can become discolored,
thus
reducing their value. Additional problems with pH adjustment include the
production of
soap, and reduced palatability for animals consuming animal feed made from
these
products.
FIG. 1A shows a prior art system 100A for processing stillage from an ethanol
production process. Stillage can be subjected to dewatering by a variety of
means, such
as by evaporation or pressing before or instead of providing to a drying zone.
In FIG. 1,
whole stillage 124 (from ethanol production) is provided to a decanter 126
where it is
separated into wet cake 128 and centrate 127. A portion of the centrate 127
can be
recycled as "backset" in the ethanol production facility and the remaining
portion,
although also having the identical content as centrate 127, is commonly
referred to as
"thin stillage" at this point in the process. The thin stillage 102 is then
provided to
evaporators 104 for concentration.
As shown in FIG_ IA, the resulting concentrated thin stillage (i.e., syrup)
106
exiting the evaporators 104 is provided to a syrup tank 118. The concentrated
thin
stillage 106 can be dried in a dryer 119 (often referred to as a "Distiller's
Grain Dryer")
to produce DDGS as discussed above and/or sold as is and/or further processed.
Alternatively or additionally, a portion of the concentrated thin stillage 106
can be
combined with the wet cake 128 and the mixture sold as DWGS and/or the mixture
can
be provided to the dryer 119 to produce DDGS. The wet cake 128 exiting the
decanter
126 can alternatively be provided as is to the dryer 119.
11

CA 02780589 2012-06-21
FIG. 1B shows a bio-oil recovery system 10013 for processing stillage from an
ethanol production process, as described in the '627 Patent, which includes
all of the
steps as described in FIG. 1A, together with steps directed to producing free
bio-oil. As
shown in FIG. 1B, concentrated thin stillage 106 is provided to a centrifuge
112 for
further separation into free bio-oil 113, de-oiled concentrated thin stillage
114, and solids
115. The free bin-oil 113 is provided to bio-oil storage 116. The de-oiled
concentrated
thin stillage 114 can then be returned to the evaporators 104 as shown, and/or
can be
provided to the process stream exiting the evaporators 104 which contains
concentrated
thin stillage (i.e., syrup) 106 and/or directly to the syrup tank 118.
In contrast, the novel embodiments described herein do not provide all of the
thin
stillage 102 directly to the evaporators 104 as shown in FIGS IA and 1B.
Instead, a thin
stillage product 260 containing a reduced amount of suspended solids is
provided to an
evaporator 204 as shown in the suspended solids separating system 200 in FIG.
2. The
thin stillage product 260 (comprised at start-up of thin stillage 202 and,
during operation,
of thin stillage 202 in combination with clarified thin stillage 242) can be
provided to a
mechanical processor 240.
= In the embodiment shown in FIG. 2, the thin stillage product 260 is
optionally
held in a thin stillage product tank 203 for a suitable period of time prior
to being
provided to the mechanical processor 240. Use of a holding tank such as the
thin stillage
product tank 203 in this manner can serve as a system control device by
providing a
quantity of thin stillage product 260 for use in this portion of the system,
whether or not
the processes upstream are operating or down for repair. The thin stillage
product tank
203 can, optionally, utilize a heat source, such as steam from an in-house
source, to
increase the temperature of the thin stillage product 260 if desired. In other
embodiments, there is no thin stillage product tank 203 and the thin stillage
product 260
is provided directly to the mechanical processor 240. In one embodiment, only
a portion
of the thin stillage product 260 is provided to the mechanical processor 240,
with the
remainder provided directly to the evaporator 204.
In the embodiment shown in FIG. 2, the suspended solids separating system 200
includes a bio-oil recovery system 250 (as described in, for example, Patent
'627). in
this embodiment, whole stillage 124 is derived from an ethanol production
facility. In
other embodiments, the whole stillage 124 can be derived from any type of
alcohol
production facility, such as an ethanol or butanol production facility. The
system 200
12

CA 02780589 2012-06-21
shown in FIG. 2 includes separating whole stillage 124 in a decanter 126 to
produce
centrate 227 and a wet cake product 228, which, at start-up comprises
conventional wet
cake, and thereafter, can comprise a molasses product-containing wet cake,
and, in some
embodiments, can additionally or alternatively include fine suspended solids
from a fine
suspended solids stream (e.g., 529, FIG. 5).
In the embodiment shown in FIG. 2, the wet cake product 228 is provided to a
first dryer 219 to produce DDG 220. A portion of the centrate 227 is provided
as
"backset," a portion or all of which can be provided to the mechanical
processor 240 as
shown in FIG. 2. The other portion of the centrate 227, although
compositionally the
same, is referred to in this point of the process as thin stillage 202.
In one embodiment (not shown), all of the centrate 227 is instead provided to
the
mechanical processor 240. In this embodiment, the clarified thin stillage 242
can be split
into more than one stream, such that a portion of it becomes backset and a
portion is
provided to the evaporator 204.
As noted above, the thin stillage product 260 enters the mechanical processor
240
where it is separated into a fine suspended solids stream 229 and clarified
thin stillage
242. The clarified thin stillage 242 (now depleted in protein and enriched in
bio-oil and
soluble as compared to the thin stillage product 260) can be returned to the
thin stillage
product tank 203. Thereafter, the thin stillage product 260 is provided to the
evaporator
204 for dewatering.
At this point in the process, the thin stillage product 260 is comprised of a
mixture of thin stillage 202 and clarified thin stillage 242, with the ratios
of each varying
throughout the operation. The thin stillage product 260 has a reduced
suspended solids
content as compared to the thin stillage 202. In one embodiment, a portion of
the
clarified thin stillage 242 is provided directly to the evaporator 204.
The fine suspended solids stream 229 can be processed in any suitable manner.
In the embodiment shown in FIG_ 2, the fine suspended solids stream 229 is
provided to
a second dryer 244 to produce Dry Distiller's So1ubles (DDS) 246. The second
dryer
244 is, in one embodiment, any dryer capable of handling a highly viscous
material (i.e.,
having a viscosity greater than about 5000 eentipoise), such as a non-rotary
dryer, (e.g.,
steam tube dryer, flash dryer, ring dryer, spray dryer, tunnel dryer and the
like). In other
embodiments, as shown in FIG. 5, for example, a portion or all of the fme
suspended
solids stream 229 can be provided to the decanter 126 to produce the wet cake
product
13

CA 02780589 2012-06-21
228. In yet another embodiment, prior to entering the second dryer 244, the
fine
suspended solids stream 229 is subjected to a dewatering step to remove
additional water
prior to drying. The dewateiing can include any suitable means, including, but
not
limited to, centrifuging (e.g., high-G compactor centrifuge, e.g., 370 in FIG.
3), filtering,
decanting, and the like.
The DDS 246 contains an increased amount of single cell proteins, e.g., yeast,
as
well as a reduced amount of grain protein, fiber, and bio-oil. In one
embodiment, the
DDS 246 is a high protein, low fiber feed product (e.g., at least about 30%
protein and no
more than about 10% fiber, by weight). In one embodiment, single cell proteins
are
present in the fine suspended solids stream 229 at a level below 40 %, by
weight. In one
embodiment single cell proteins are present at a level greater than 40%, by
weight, such
as up to greater than 70% or 90%, including any values there between.
Referring again to FIG. 2, the evaporator 204 can represent multiple effect
evaporators, such as any number of evaporators, such as one, two, three or
more,
such as four, five, six, or seven evaporators, further including, for example,
eight (8)
evaporators. In some embodiments, more than eight evaporators may be used. In
such embodiments, forward feeding can take place when the thin stillage
product 260
enters the evaporator 204 through a first effect evaporator that is run at the
highest
temperature. The thin stillage product 260 is then partially concentrated, as
some of
the water has vaporized and can be used downstream. This clarified and
partially
concentrated product (not shown) are then fed into a second effect evaporator
that is
slightly lower in temperature than the first effect evaporator. The second
effect
evaporator uses the heated vapor created from the first stage as its source of
heating.
In one embodiment, the evaporator 204 comprises first effect and second effect
evaporators that utilize recycled steam.
In one embodiment, the first effect evaporators use steam from a boiler (not
shown) in the alcohol production facility (e.g., ethanol production facility)
to generate
process steam. This steam becomes cooled and can be re-used in a distillation
step (not
shown). In one embodiment, the second effect evaporators also use recycled
steam. In
one embodiment, direct steam from the boiler is used in the distillation step
and the
evaporator 204 comprises multiple evaporators which are run "post
distillation."
In one embodiment, the evaporator is a multiple effect evaporator as described

above, such as a three effect evaporator. In one embodiment, the evaporator is
a four
14

CA 02780589 2012-06-21
effect evaporator. In one embodiment, the evaporator is a five effect
evaporator. In one
embodiment, the evaporator is a Mechanical Vapor Recompression (MVR)-type
energy
cascade system.
In embodiments having eight (8) evaporators, the first evaporator can be run
at
temperatures as high as about 210 F (99 C), with the fourth evaporator run
at
temperatures between about 200 F (93 C) and about 205 F (96 C). In other
embodiments with fewer evaporators or with one evaporator, the temperatures
can vary
between about 22 C and about 121 C, such as between about 130 F (54.4 C)
and
about 210 F (99 C), including any ranges there between.
As the thin stillage product 260 progresses through the evaporator 204, it
becomes increasingly concentrated to the point it eventually becomes a
molasses product
206, which, in one embodiment, can have a water concentration between about 5%
and
about 55%.
It is possible to withdraw the reduced suspended solids product at any point
or
points during evaporation, depending on the desired final product or products.
In one
embodiment, a reduced suspended solids product, such as clarified concentrated
thin
stillage 205 having a water concentration of between about 65% and about 75%
by
weight, such as about 70%, is withdrawn from the evaporator 204 and provided
to a
centrifuge 212 to produce solids 215 and a clarified emulsion concentrate 222.
The
clarified emulsion concentrate 222 is provided to the bio-oil recovery system
250, which
produces a bio-oil phase 236 and an aqueous phase 234. The bio-oil phase 236
is then
provided to bio-oil storage 216 where it can be sold into various markets,
such as the
feed, chemical and/or biofuel oil markets at a higher selling price than
conventional
syrup or Distiller's Dry Grain Solubles (DDGS).
The resulting de-oiled reduced suspended solids product, i.e., the de-oiled
clarified concentrated thin stillage 214, can be returned to the evaporator
204 where the
evaporation process continues until the molasses product 206 is produced In
one
embodiment, the molasses product 206 is a cooled molasses product, which is a
solid
product that is congealed. However, in order to move the molasses product 206
through
the system 200, in most embodiments, the molasses product 206 is heated
sufficiently to
allow it to be pumped. In one embodiment, the molasses product 206 is heated
to a
temperature of at least about 100 F (38 C). In this way, although highly
concentrated,

CA 02780589 2012-06-21
the molasses product 216 is a ptunpable liquid product due to the reduced
amount of
suspended solids.
In one embodiment, a reduced suspended solids stream, which is more
concentrated than the thin stillage product 260, but less concentrated than
the molasses
product 206 can be withdrawn from the evaporator (not shown in FIG.2). Such a
product
can have a total solids content between about 30% and 90%, by weight, with the

suspended solids comprising less than about 25%, by weight, of the total
solids content,
is produced.
In one embodiment, the reduced suspended solids stream is the molasses product
206 having a total solids content greater than about 45%, by weight, such as
greater than
about 60% or 70% or 80% or 90% or 95% or higher up to substantially 100%, as
long as
the molasses product 206 is still pumpable at elevated temperatures, including
any range
there between.
In one embodiment, the suspended solids in the molasses product 206 comprise
less than 25%, by weight of the total solids, such as about 20% or about 0% or
lower,
down to about 5% or lower, down to about 1% or lower, such as about 0.001%, by

weight, down to substantially or about zero%, including any range there
between. In one
embodiment, the molasses product 206 has a total solids content between about
65% and
75%, by weight, such as about 70%, with a suspended solids content comprising
less
than 3.5%, by weight, of the total solids content.
It is possible to withdraw the clarified concentrated thin stillage 205 and/or
the
molasses product 206 from the evaporator 204 at temperatures lower than their
boiling
points. In one embodiment, the clarified concentrated thin stillage 205 and/or
another
reduced suspended solids stream (not shown) and/or the molasses product 206 is
withdrawn at a temperature of about 205 F (96.1 C) or below. In embodiments
having
eight evaporators, the clarified concentrated thin stillage 205 and/or another
reduced
suspended solids stream (not shown) and/or molasses product 206 may be
withdrawn
from any of the evaporators, such as from the fourth, fifth, sixth, seventh,
and/or eighth
evaporators at temperatures of between about 170 OF (76.7 C) and about 205 F
(96.1
C). The decision as to which evaporator 204 the clarified concentrated thin
stillage 205
and/or any other reduced suspended solids process stream (not shown) and/or
molasses
product 206 should be removed from depends on several factors, including, but
not
limited to, the volume % of unstable emulsion present, viscosity of the
clarified
16

CA 02780589 2012-06-21
concentrated thin stillage 205 and/or other reduced suspended solids process
stream
and/or molasses product 206, and the like, which can vary depending on
upstream
processing conditions.
Referring again to FIG. 2, the molasses product 206 exiting the evaporator 204
can be at any suitable pH. In one embodiment, the molasses product 206 is at a
pH of
between about 2 and about 5.8. In one embodiment, the pH may be closer to
p117. In
one embodiment, the pH may be higher, such as about 8.3.
By separating out the suspended solids in the fine suspended solids stream
229,
the thin stillage product 260 entering the evaporator 204 now contains a
reduced amount
of suspended solids. As a result, it is now possible to efficiently and
economically
produce clarified concentrated thin stillage 205 and/or any other reduced
suspended
solids process stream, including a molasses product 206 as a co-product of
alcohol
production, e.g., ethanol production. These reduced suspended solids products,
such as
the molasses product 206 shown in FIG. 2, can then be provided to a molasses
product
tank 218 and sold and/or combined with the wet cake product 228 and dried in
the first
dryer 219 to produce DDGS 221. In one embodiment, the molasses product 206 is
additionally or alternatively combined with the wet cake product 228 and-can
optionally
also be provided as DWGS.
The molasses product 206 further contains an amount of bio-oil that is greater
than the amount, per volume, of bio-oil present in conventional concentrated
thin
stillage. In one embodiment, the molasses product 206 contains two to three
times the
amount of bio-oil, per volume, as compared to conventional concentrated thin
stillage.
As a comparison and for example purposes only, a given volume of concentrated
thin stillage having about 35% total solids, by weight, can contain about 4 to
about 6%
No-oil, by volume, whereas the same volume of molasses product 206 can have
about
70% total solids, by weight, and contain about 8 to about 12% bio-oil, by
volume. As
such, mechanical processing, such as centrifugation, can run more efficiently
as
compared with mechanical processing performed in conventional operations. In
one
embodiment, the number of centrifuges used in the system can be reduced, such
as by
one-half, such as from two to one.
In the embodiment shown in FIG. 2 the system further includes a bio-oil
recovery
system 250, such as is described in the '627 Patent. In this embodiment, the
operation of
the centrifuge 212 is adjusted to dewater or concentrate the clarified
concentrated thin
17

CA 02780589 2012-06-21
stillage 205 to produce an emulsion concentrate, which, since there is a
reduced amount
of suspended solids contained therein, is referred to in FIG. 2 as a clarified
emulsion
concentrate 222. The clarified emulsion concentrate 222 is thereafter provided
to an
emulsion breaking/phase separating process 250, which produces an aqueous
phase 234
and a bin-oil phase 236.
The mechanical processor 240 is capable of changing the nature of the solid
particles, i.e., neutralizing the electrostatic charge of fme suspended solids
from
dissolved solids in the process stream, thus allowing the fme suspended solids
to bind
together. In this way, the fine suspended solids can be separated from the
thin stillage
product 260. The mechanical processor 240 can comprise any suitable device
capable of
separating the line suspended solids mixture 229 as described.
Separation efficiency of the mechanical processor 240, i.e., the ability of
the
mechanical processor 240 to separate suspended solids from the process stream,
is also a
consideration. In one embodiment, the separation efficiency is at least 50%,
up to about
60%, 70%, 80%, 90% or higher, including any ranges there between. In one
embodiment, the separation efficiency is at least 80%. In one embodiment, the
separation efficiency is between about 80% and about 90% or between about 85%
and
about 95%. In one embodiment, the separation efficiency is at least 96%, such
as about
96.7%. Higher separation efficiencies may also be possible.
In one embodiment, the mechanical processor 240 is a centrifuge, such as a
disc
stack centrifuge. A disc stack centrifuge is a vertically-oriented centrifuge
with the
capability to separate fine suspended particles from solution more effectively
than a
standard centrifuge. 'The enhanced separation efficiency is due to the higher
0-force
produced by the disc stack unit as well as the large surface area provided by
the discs
inside the centrifuge. The discs are stacked closely together to provide
additional surface
area for more effmtive separation. As the centrifuge spins, centrifugal force
sends the
denser solids outward against the wall of the bowl, and the less dense liquid
is forced to
the center. The fine suspended solids stream 229 is discharged through a fixed
port or by
rapidly opening and closing space in the wall of the centrifuge, and the
clarified thin
stillage 242 is discharged through a pipe at the top (not shown). In one
embodiment, any
suitable filtration system comprising one or more filters, is additionally or
alternatively
used as a mechanical processor 240. In one embodiment, the system includes a
bio-oil
recovery system 250 and the mechanical processor 204 comprises a filtration
system.
18 =

CA 02780589 2012-06-21
In one embodiment, as shown in FIG. 3, the mechanical processor 240 comprises
both a disc stack centrifuge 360 and a high "G" compacting centrifuge 370_ The
high
"G" compacting centrifuge 370 is capable of operating in excess of 3000 G
forces. In
the embodiment shown in FIG. 3, the thin stillage product 260 enters the disc
stack
centrifuge 360, which separates the thin stillage product 260 into clarified
thin stillage
242 and an intermediate fine suspended solids stream 365. The intermediate
fine
suspended solids stream 365 is provided to the high "G" compacting centrifuge
370
which produces the fine suspended solids stream 229 which is provided to the
decanter
(226, FIG. 2) or to the second dryer (244, FIG. 2). In one embodiment, the
fine suspended
solids stream 229 has a water concentration of about 75% to about 80%, though
lower water
contents may be possible.
In the embodiment shown in FIG. 3, wash water 372 can be provided to the disc
stack centrifuge 360 to wash dissolved solids away from the suspended solids
material.
In one embodiment, the wash water 372 is provided within an internal loop. In
one
embodiment, the wash water 372 is provided within an external washing loop.
FIG. 4 shows an embodiment of a suspended solids separation system 400 in
which clarified free bio-oil 413 is recovered via conventional means from
clarified
concentrated thin stillage 405, such as with any suitable type of centrifuge
412, i.e.,
without a bio-oil recovery system (250) as shown in FIG. 2. In one embodiment,
the
centrifuge 412 is any type of tricanter or decanter. As discussed herein, in
addition to
producing the clarified free bin-oil 413, the other streams exiting the
centrifuge 412
include solids 415 and a de-oiled clarified concentrated thin stillage 414,
which can be
provided to the evaporator 204, to a molasses product 406 and/or to the
molasses product
tank 218.
As such, in the embodiment shown in FIG. 4, the suspended solids separating
system 400 do not include a bio-oil recovery system (250) as shown in FIG. 2.
Otherwise, the process can begin, in one embodiment, by separating whole
stillage 124
from any suitable source, such as from ethanol production, in a decanter 126
to produce
centrate 427 and a wet cake product 428. At start-up, the wet cake product
comprises
conventional wet cake, and thereafter, can comprise a molasses product-
containing wet
cake, and, in some embodiments, can additionally or alternatively include fine
suspended
solids from a fine suspended solids stream (e.g., 529, FIG. 5).
19

CA 02780589 2012-06-21
In the embodiment shown in FIG. 4, the wet cake product 428 is provided to a
first dryer 219 to produce DDG 420. A portion of the centrate 427 is provided
as
"backset," a portion or all of which can be provided to the mechanical
processor 240 as
shown in FIG. 4. The other portion of the centrate 427, although
compositionally the
same, is referred to in this point of the process as thin stillage.
The thin stillage product 460 (comprised at start-up of thin stillage (not
shown)
and, during operation, of thin stillage in combination with clarified thin
stillage 442 in
varying ratios), can be provided to the mechanical processor 240. As with the
above
described embodiments, the thin stillage product 460 enters the mechanical
processor
240 where it is separated into a fine suspended solids stream 429 and
clarified thin
stillage 442. In contrast to the embodiment shown in FIG. 2, however, the
embodiment
in FIG. 4 does not include a thin stillage product tank (203), although such a
tank can be
provided if desired. As such, the clarified thin stillage 442 (now depleted in
protein and
enriched in bio-oil and soluble as compared to the thin stillage product 460)
is provided
directly to the evaporator 204 for dewatering to produce clarified
concentrated thin
stillage 405.
The clarified concentrated thin stillage 405 is further processed in a
centrifuge
412 to produce the clarified free bio-oil 413, solids 415 and de-oiled
clarified
concentrated thin stillage 414. The de-oiled clarified concentrated thin
stillage 414 can,
in turn be provided to the evaporator 204, and/or a reduced suspended solids
stream,
such as the molasses product 406 shown in FIG. 4 and/or a reduced suspended
solids
stream tank, such as the molasses product tank 218 shown in FIG. 4.
Other reduced suspended solids streams, such as the molasses product 406 shown
in FIG. 4, can then be provided to the molasses product tank 218 as shown and
sold
and/or combined with the wet cake product 428 and provided to the first dryer
219 to
produce DDGS 421. Optionally, the molasses product 406 can then be provided to
the
wet cake product 428 and can optionally also be provided as DWGS. Optionally,
the
molasses product 406 can be sold and the wet cake product 428 provided to the
first
dryer 219 to produce DDG 420.
Otherwise, the process proceeds as described in FIG. 2, with the fine
suspended
solids stream 429 being processed in any suitable manner. In the embodiment
shown in
FIG. 4, the fine suspended solids stream 429 is provided to a second dryer 244
to
produce Dry Distiller's Solubles (DDS) 446.

CA 02780589 2012-06-21
In the embodiment shown in FIG. 5, the suspended solids separating system 500
does not include any type of bio-oil recovery, i.e., no recovery of a bio-oil
phase 236, as
in P10.2 and no recovery of clarified free bio-oil 413 as in FIG. 4. However,
as in other
embodiments, whole stillage 124 can be derived from any suitable source. The
system
500 shown in FIG. 5, can begin with, in one embodiment, separating whole
stillage 124
in a decanter 126 to produce centrate 527 and a wet cake product 528, which,
at start-up
comprises conventional wet cake, and thereafter, can comprise a molasses
product-
containing wet cake, and, as shown in FIG. 5, can additionally or
alternatively include
fine suspended solids from a fine suspended solids stream 529.
In the embodiment shown in FIG. 5, the wet cake produCt 528 is provided to a
dryer 119 to produce DDG 520. A portion of the centrate 527 is provided as
"backset," a
portion or all of which can be provided to the mechanical processor 240 as
shown in
FIG. 5. The other portion of the centrate 527, although compositionally the
same, is
referred to in this point of the process as thin stillage.
The thin stillage product 560 (comprised at start-up of thin stillage (not
shown)
and, during operation, of thin stillage in combination with clarified thin
stillage 542 in
varying ratios), can be provided to the mechanical processor 240 where it is
separated
into a fine suspended solids stream 529 and clarified thin stillage 542.
As with the embodiment shown in FIG. 4, the embodiment in FIG. 5 does not
include a thin stillage product tank (203), although such a tank can be
provided if
desired_ As such, the clarified thin stillage 542 (now depleted in protein and
enriched in
bio-oil and soluble as compared to the thin stillage product 560) is provided
directly to
the evaporator 204 for dewatering to produce a reduced suspended solids
stream, such as
the molasses product 506 shown in FIG. 5.
In contrast to the embodiments shown in FIGS. 2 and 4, however, in the
embodiment shown in FIG. 5, the fine suspended solids stream 529 is not dried,
but, as
noted above, is instead provided to the decanter 126 where it can be processed
and/or
dried as described above. When the fine suspended solids stream 529 is
provided to the
decanter 126, it can be combined with the wet cake product 528 where it can be
dried in
a dryer 119, such as a distiller's rotary grain dryer, thus increasing the
volume and
protein content of the resulting DDG 520.
The various reduced suspended solids streams produced in the evaporator 204,
such as the molasses product 506 shown in FIG. 5, can be provided to a
molasses
21

CA 02780589 2012-06-21
product tank 218 and sold and/or combined with the wet cake product 528 and
provided
to the dryer 119 to produce DDGS 521. Optionally, the wet cake product 528
containing
varying amounts of the fine suspended solids stream 529 can additionally or
alternatively
also be provided as DWG.
The various embodiments described herein further produce a de-oiled water
phase, which can be further concentrated to lower moisture contents (i.e.,
down to about
20% moisture content on a dry weight basis, while remaining a purnpable
liquid. This is
due to the presence of components, such as glycerol, lactic acid, and acetic
acid present
in liquid form and thus able to dissolve residual sugars present in the de-
oiled liquid
phase.
The specific materials and designs of additional minor components necessary to

perform the process, e.g., valves, pumps, lines, and the like, are understood
in the art and
are not all described in detail herein. The apparatus and method can further
be
implemented using a variety of specific equipment available to and understood
by those
skilled in process control art For example, means for sensing temperature,
pressure and
flow rates in all of the flow lines may be accomplished by any suitable means.
It will
also be appreciated by those skilled in the art that the various embodiments
can include a
system controller.
Specifically, the system controller can be coupled to various sensing devices
to
monitor certain variables or physical phenomena, process the variables, and
output
control signals to control devices to take necessary actions when the variable
levels
exceed or drop below selected or predetermined values. Such amounts are
dependent on
other variables, and may be varied as desired by using the input device of the
controller.
Such sensing devices may include, but are not limited to, devices for sensing
temperatures, pressures, density and flow rates, and transducing the same into
proportional electrical signals for transmission to readout or control devices
may be
provided for in all of the principal fluid flow lines. Such a controller may
be a local or
remote receiver only, or a computer, such as a laptop or personal computer as
is well-
known in the art. In one embodiment, the controller is a personal computer
having all
necessary components for processing input signals and generating appropriate
output
signals as is understood in the art. These components can include a processor,
a utility, a
driver, an event queue, an application, and so forth, although the embodiments
are not so
limited. In one embodiment, the controller has a non-volatile memory comprised
of a
22

CA 02780589 2012-06-21
disk drive or read only memory device that stores a program to implement the
above
control and store appropriate values for comparison with the process variables
as is well
known in the art. In other embodiments, the information is stored remotely.
In one embodiment, these components are all computer programs executed by a
processor of the computer, which operates under the control of computer
instructions,
typically stored in a computer-readable media such as a memory. In this way,
useful
operations on data and other input signals can be provided by the computer's
processor.
The controller also desirably includes an operating system for running the
computer
programs, as can be appreciated by those within the art. The system controller
may also
comprise a machine coupled to a control panel. Buttons and dials can be
provided on the
control panel to allow modification of the values and to control the
agricultural biofuel
energy generating system to take the desired steps described herein.
The system controller can also be programmed to ignore data from the various
sensors when the operator activates certain other buttons and dials on the
control panel as
he deems necessary, such as fill override or emergency stop buttons.
Alternatively, or in
addition to the foregoing, the control panel can include indicator lights or
digital displays
to signal an operator as to the status of the operation_ Indicator lights can
also be used to
signal that a certain variable level is outside the desired range, therefore
alerting the
operator to the need for corrective action. In such an embodiment, the
corrective action
is not automatic, but requires the operator to initiate corrective action by
either pushing a
specific button or turning a specific dial on the control panel, or by
manually adjusting
the appropriate valve or device_
Additionally, as is known in the art, in implementing the system described
herein, general chemical engineering principles are adhered to, including
accounting for
the various types of energy and materials being input to and output from the
system, in
order to properly size the system. This includes not only the energy
associated with
mass flow, but also energy transferred by heat and work. In some embodiments,
the
system is optimized for maximum performance utilizing any known optimization
methods known in the art. The present subject matter is further described by
reference to
the following examples, which are offered to further illustrate various
embodiments. It
should be understood, however, that many variations and modifications may be
made
while remaining within the scope of the embodiments described herein.
23

CA 02780589 2012-06-21
EXAMPLE I
Thin stillage starting material (e.g., 202, FIG. 2) was obtained from a
commercial
corn-to-ethanol production facility (hereinafter "ethanol production
facility") and
analyzed for content. The thin stillage 202 was thereafter further processed
and analyzed
as described below.
Thin Stillage Content
Thin stillage total % solids and thin stillage dissolved % solids were
determined
using a calibrated Mettler Toledo analytical balance and a Binder forced draft
laboratory '
oven set at a temperature of approximately 105 C. The procedure involved
calibrating
the analytical balance and validating with standardized weights.
Determination of thin stillage total % solids and dissolved solids, included
taking
the fresh, hot sample and putting immediately into a herrnitically sealed
bottle to allow
cooling of each sample for about 45 minutes to minimize moisture loss while
the sample
was being handled. For the dissolved % solids, samples were centrifuged at a
maximum
revolutions per minute (RPM) for approximately I 0 minutes in a laboratory
style
centrifuge. Using the calibrated analytic balance, the initial weight of the
aluminum
weigh pan was recorded and the balance tared with the weigh pan.
For total % solids determination, approximately 10 to approximately 12
grams(g)
of the cooled sample were added. For dissolved % solids determination, the
sample was
thereafter pipetted into a syringe with a 0.2 micrometer (j.un) High Pressure
Liquid
Chromatography (FIPLC) syringe filter. Thereafter, about 10 to about 12 grams
(g) of
the sample were added to the drying pan by passing the liquid through the
filter, thereby
removing suspended solids from the material, the total grams were recorded.
For both types of solids, the samples were heated for about 3 hours to a
temperature of approximately 105 C in a forced draft drying oven. Most
samples were
then placed in a desiccator to further cool under controlled conditions.
However,
samples, which were weighed within about 5 minutes of being removed from the
oven,
were not placed in the desiccator, but were instead allowed to cool for about
I to about 2
min prior to weighing. The final thy weight of the dried sample and weigh pan
were
then recorded.
The various % solids were calculated as follows:
Total % Solids = ((Final Weight ¨ Initial Pan Weight)/Grams of Sample) x 100
24

CA 02780589 2012-06-21
% Dissolved Solids = ((Final Weight - Initial Pan Weight)/Grams of Sample) x
100
% Suspended Solids = Total % Solids - Dissolved % Solids
% Suspended Ratio % Suspended Solidi% Total Solids
% Dissolved Ratio = Dissolved Solids 1% Total Solids
% Suspended to % Dissolved Ratio = Suspended Solids/% Dissolved Solids
Compositional analysis of the thin stillage was performed using a Shimadzu
IIPLC system configured with SIL-20AC HT refrigerated autosampler, LC-20AT
pump,
CTO-20A oven, and RID-10A detector. The method used was Phenomenex Rezex ROA
Organic Acid H+ 150 x 7.8 ram column with 0.6raL/min flow rate, temperature in
autosampler at about 4 C, and at about 65 C column temperature_ The results
are
shown in Table 1, which also includes the Degree or Polymerization (DP) for
dextrin
molecules.
Table 1. Soluble com sition of thin stillase as C
weight/volume %
Lactic Acetic
DP4+ DP3 Maltose Glucose Acid _
Glycerol _ Acid Ethanol
average 0.62 0.07 0.57 0.17 0.12 1.64
0.07 _ 0.01
stdeva 0.19 0.02 0.21 0.08 0.04 0.53
0.03 0.01
max 1.18 0.08 0.73 0.31 0.15 2.08 0.1
0.03
min 0.27 0 0.08 0.04 0112 0.32 0.01 0

samples 53 , 53 53 53 53 53 53 53
DP4+ (Dextrin and 4 or more additional sugars)
DP3 (Dextrin plus 3 additional sugars)
The resulting % solids contents calculated as described above, are shown in
Table
2.
Table 2. Compositional analysis of thin stillage
pH %TS %Soluble %TSS % Pat DMB
average 4.02 4.14 2_90 1.25 19.63
stdeva 0.15 0.67 0.33 0.41 4.35
max 4.25 5.69 4.10 3.00 26.18
min 3.64 3.26 _ 2.15 0.02 9.53
# samples 53 5353 53 _ 53
%Total Solids (TS) weight/weight perc-entage of sample which is not water

CA 02780589 2012-06-21
% soluble 7 weight/weight percentage of which is soluble in water
% Total Suspended Solids (TSS) = weight/weight percentage of sample which is
not soluble in water
% Fat Dry Matter Basis (DMB) = weight percentage of a sample that is soluble
in petroleum ether/weight
percentage
of sample which is not water
Processing and Analysis of Thin Stillage
Analysis of the process streams was performed according to the methods
described herein and/or known to those skilled in the art using a Shitnadzu
HPLC system
configured with SIL-20AC HT refrigerated autosampler, LC-20AT pump, CTO-20A
oven, arid RID-10A detector. The method used was Phenomenex Rezex ROA Organic
Acid H+ 150 x 7.8 mm column with 0.6mL/min flow rate, temperature in
atrtosampler 4
C, and a 65 C column temperature.
After the initial compositional determinations were made, as described above,
the
thin stillage was provided to a shot style disc stack centrifuge Flottweg
model AC1000.
The temperature of the thin stillage feed to the centrifuge was kept at a
constant 180 F
(82 C) during all centrifugation testing. The underflow (i.e., fine suspended
solids
stream, i.e., 229, FIG. 2) from the centrifuge was transferred to a holding
tank where the
elevated temperature was maintained. Overflow (i.e., clarified thin stillage,
i.e., 242,
FIG. 2) was collected for compositional analysis and dryer testing using an
Anhydro
spray dryer. The dried product retained color and appeared suitable for
further
processing. Samples of the overflow and underflow were simultaneously taken
every
two to four hours during the processing and individually analyzed to determine
the split
and efficiency of the system. The fraction of suspended solids captured by the
centrifuge
averaged 93.6% as shown in Table 3.
Table 3. Volumetric ratios of suspended solids versus total volume in vin
test
feed overflow
underflow suspended
"shot suspended suspended suspended solids
cycle" volume volume volume recovery
seconds ratio ratio ratio ratio
Average 80 0_082 0.005 0.794 0.936
Std dev 0 0.014 0.003 0.115 0.044
¨ -
Max 80 0.107 0.018 0.971 0.967
Min _____________________ 80 0.036 0.004 0.286 _ 0.75
# samples 48 _ 40 40 40 40
(A "shot cycle" refers to the opening and closing of the gate or door against
which solids build up when
closed and are released when open).
26

CA 02780589 2012-06-21
FIGS. 6 and 7 are images of spin vials showing suspended capture efficiency
from the AC1000. FIG. 6 comprises a set of four spin vials 602, 604, 606 and
608. Spin
vial 602 is empty but is included to show the volume delineations. Black lines
drawn on
spin vials 604, 606 and 608 are labeled as 610, 612 and 614, respectively.
These
markings denote an intersection line between the suspended solids and
supernatant
layers. Spin vial 608 is a sample containing the feed material with
approximately 1.5 mL
solids in a 14 mL sample. Spin vials 604 and 606 are overflow samples produced
from
the starting material in spin vial 608 according to the process described
above with the
high speed centrifuge. As FIG. 6 shows, spin vials 604 and 606 each have
approximately
0.08 mL of solids in a 14 mL sample. This represents 94.7% suspended solids
capture
efficiency.
The feed rate was adjusted during the operation starting at about 2 gallons
per
minute and ramping to about 4 gallons per minute over a 4 day test period. A
second 5
day test period used an approximately 4.4 gallon per minute feed rate was
conducted at a
later time. Compositional analysis of the overflow and underflow obtained in
the
manner described above during the 9 days of operation is shown in Tables 4 and
5.
Table 4, Compositional analysis of 53 overflow samples taken over the 9 days
of
centrifuge operation
Centrifuge Overflow
% Fat
%TS Soluble %TSS DMB
Avg 3.5 3.45 0.30 20.28
Stileva 0.44 0.49 1.80 6.05
Max 5.80 5.80 12.85 38.51
Min 2.93 2.74 -0_57 7.4
# samples 53 51 53 53
Table 5. Compositional analysis of 53 overflow samples taken over 9 days of
centrifuge
,operation
____________________ centrifuge Underflow
% Fat % Prot
%TS % Soluble %TSS DMB DMB
Avg 13.86 1_33 12.64 7.55 40.57
Stdeva 2.31 0_71 2.64 2.97 3_34
Max 20.21 4.28 21.08 15.27 49.01
Min 8.39 0.22 6.46 2.47 31.19.
# samples , 53 46 53 53 53
27

CA 02780589 2012-06-21
% Prot DM I3 = (weight percentage of Nitrogen of a sample X 6_25)/weight
percent of a sample which is
not Water
A mass balance split between the two fractions was calculated by using the
ratios
of suspended-to-dissolved solids in feed and comparing to the overflow and
underflow.
This analysis showed that about 70% of the non-water mass splits into the
overflow and
about 30% splits into the underflow. Multiplying this mass split times the
fraction of
bio-oil in each material (20.3% concentration fat in overflow and 7.6%
concentration fat
in underflow), it was determined that approximately 86% of the bio-oil in the
thin
stillage product was captured in the overflow and 14% of the bio-oil was
captured in the
underflow.
Overflow from the centrifuge separation was concentrated under vacuum at
approximately 200 F (93 C) from an initial Brix concentration of 5.3 to a
final Brix
concentration of 39.1 degrees Brix (hereinafter "Brix"). ("Degrees Brix"
refers to sugar
content of an aqueous solution. One degree Brix corresponds to 1 gram of
sucrose in 100
grams of solution, thus representing the strength of the solution as a
percentage by
weight (% w/w)). Concentrated material was drawn out of the evaporator as the
Brix
approached 35 in order to build a stock of 35 Brix to test for bio-oil
extraction via
centrifugation. Brix measurements were made with a handheld Brix refractometer
during the concentration process_ .As Brix measurements were made, the samples
were
also tested for bio-oil via laboratory spin testing. There was a fair amount
of emulsion in
the bio-oil layer. As the total solids concentration increased, the bio-
oil/emulsion
concentration increased, as observed by the spin testing (which determined
solids by
volume).
See, for example FIG. 8 which shows a volume/volume ernulsion/bio-oil with
increasing Brix concentration. As can be seen, the samples exhibited
increasing bio-oil
emulsion as the amount of solids increased.
The 35 Brix concentrate was centrifuged with a FlottwegTM Z23 tricanter for
bio-
oil recovery. The feed was delivered hot to the tricanter and an emulsified
bio-oil layer
was recovered from the centrifuge. This emulsified bio-oil was broken into
free bio-oil
and water phases by adding ethanol at elevated temperature to the emulsion and
then
flashing the ethanol back out of the emulsified mixture. (See Patent '627).
Using this
technique, it was observed that recoveries over 80% of theoretical are
achievable_
28

CA 02780589 2012-06-21
EXAMPLE 2
In this testing, the thin stillage from the same commercial source as
described in
Example 1 was subjected to further processing and compositional data on
overflow (i.e.,
fine suspended solids stream, i.e., 229, FIG. 2) and underflow (i.e.,
clarified thin stillage,
i.e., 242, FIG. 2) was obtained.
A 600 gallon tank and tube-and-shell heat exchanger (constructed in-house)
were
used as an evaporator in the pilot plant. A Flottweg AC1000 (disc stack) was
used to
remove suspended solids from The thin stillage. The AC 1000 was operated at a
rate of
about 2 to 4 gpm. The evaporative rate on the evaporator was about 1.1 gpm. A
Flottweg Z23 (tricanter) was also used to separate the emulsion concentrate. A
modified
commercial spray dryer was used to spray dry the centrifuged solids.
Suspended solids recovery was about 95%, while DDS recovery was between
about 55 up to 80 v/v% concentration. Protein levels in the DDS were measured
at about
40%, with bio-oil content about 5%.
Table 6 shows compositional data from this testing determined according to the
methods described in Example 1 and other methods known to those skilled in the
art:
Table 6. Compositional Data (% of dry matter)
Centrifuge Feed Overflow Underflow
pH Fat Total Fat Total Protein Fat Total
solids solids solids
avg 4.0 20 4.3 21. 3.7 42 5.3 14
std 0.36 2.5 0.37 3.1 0.50 3.1 1.9 1.9
max 4.3 24. 5.7 27 5.8 49 9.4 18
_
min 3.6 14 3.8 16 3.1 34 2.5 12
The fine suspended solids stream (i.e., 229 in FIG. 2) had the composition as
shown in Table 7:
Table 7. Fine Suspended Solids Stream Analysis (% of dry matter unless noted
otherwise)
Dry Basis As Received
Moisture 5j5 %
Dry Matter 94.85 %
Protein, Crude 29.39 27.88 %
Acid Detergent Insoluble Protein 0.62 0.59 %
Neutral Detergent Insoluble Protein 2.12 2.01 %
Soluble Protein (% of Crude Protein) 18 %
29

CA 02780589 2012-06-21
ADF-Acid Detergent Fiber 1.35 1,28 %
NDF-Neutral Detergent Fiber 5.13 4.87 %
NFC- Non Fibrous Carbohydrates 38.46
Lignin-Acid Insoluble Less than 0.2
NEL: Net Energy-Lactation 1.33 1.26 Meal/lb
NEG: Net Energy-Gain 1.06 1.01 Mcal/lb
NEM: Net Energy-Maintenance 1.46 1.38 Mcal/lb
TDN: Total Digestible Nutrients 124_90 118.47 %
Digestible Energy - DE 2.50 2.37 Mcal/lb
Metabolizable Energy - ME 2.05 1.95 Mcal/lb
Fat (EE) 23.96 22.73 %
Ash 5.18 4.91 %
Calcium 0.14 0.13 %
Phosphorus 0.89 0.84 %
Potassium 1.11 1.05 %
Magnesium 0_34 0.32 %
Sodium 0.49 0,46 %
Chloride 0.08 0.08 %
Sulfur 1.28 1.21 %
Cobalt Less than 0.2 ppm
Copper 17.30 16.41 ppm
Iron 258.00 244.71 ppm
Manganese 46.20 43.82 ppm
Molybdenum Less than 0.3 ppm
Zinc 5170 50.93 ppm
Total Starch 12.3 11.7 %
RFV-Relative Feed Value 1593 s.u.
The molasses product (e.g., 206) had a composition in a first test as shown in
Table
8:
Table 8. Molasses Product Analysis (Run 1) (% of dry matter unless noted
otherwise)
Dry As Received
_________________________________________ Basis
Moisture, Karl-Fischer 36.2 %
Dry Matter 63_8 %
Protein, Crude 14.091 8.99 %
Acid Detergent Insoluble Protein 0 %
Neutral Detergent Insoluble Protein 0 %
Soluble Protein (% of Crude Protein) 98 %
ADF-Acid Detergent Fiber 1.254 0.8 %
NDF-Neutral Detergent Fiber 1.881 1.2 %
NFC- Non Fibrous Carbohydrates 60_94 38.88 %
Lignin-Acid Insoluble 0
NEL: Net Energy-Lactation 0.91 0.581
Mcal/lb
NEG: Net Energy-Gain 0.67 0427 Mcal/lb
NEM: Net Energy-Maintenance 0.98 0.625 McaUlb

CA 02780589 2012-06-21
TDN: Total Digestible Nutrients 87.13 55.589 %
Digestible Energy - DE 1.746 1.114 Mcal/lb
Metabolizable Energy -ME 1.432 0.914 Mcalllb
Fat By Acid-Hydrolysis 7.853 5.01 %
Ash 15.251 9_73 %
Calcium 0.094 0.06 %
Phosphorus 2.006 1.28 %
Potassium 2.9 1.85 %
Magnesium 0_956 0.61 %
Sodium 1.254 0.8 %
Chloride 0.627 0.4 %
Sulfur 2.006 1_28 %
Cobalt 0 ppm
Copper 4.561 2.91 ppm
Iron 133.072 84.9 ppm
Manganese 102.351 65.3 ppm
Molybdenum 0 ppm
Zinc 115.831 73.9 ppm
Total Starch 5.799 3.7 %
The HPLC profile ( /0 w/v) for the molasses product of Table 8 is shown in
Table 9.
Table 9. DMB - HPLC p_rofile (% W/V)
Molasses DP4+ 0P3 'Maltose Glucose Lactic Glycerol Acetic Ethanol
Product
1 12.-6-4 1.71 8.09 3.33 2.66 36.52 0.27 0.00
The molasses product (e.g., 206) had a composition in a second test as shown
in
Table 10:
Table 10. MI lasseso&thict Analysis (Run 2) (% of dry matter unless ted
otherwise)
Dry Basis As Received _
Moisture, Karl-Fischer 17.3 %
Dry Matter 82.7 %
Protein, Crude 8.767 7.25 %
Acid Detergent Insoluble Protein 0 %
Neutral Detergent Insoluble Protein 0 %
Soluble Protein (% of Crude Protein) 100 %
ADP-Acid Detergent Fiber 0.931 0_77 %
NDF-Neutral Detergent Fiber 1.282 1.06 %
NFC- Non Fibrous Carbohydrates 67.13 55.517 %
Lignin-Acid Insoluble 0 %
Fat By Acid-Hydrolysis 12.201 10.09 %
Ash 10.629 8.79 %
Calcium 0.085 0.07 %
Phosphorus 1.79 1.48 %
31

CA 02780589 2012-06-21
Potassium 2.963 2.45 %
Magnesium 0.762 0.63 %
Sodium 0.568 0.47 %
Chloride 1.112 0.92 %
Sulfur 0.653 0.54 %
Cobalt 0 ppm
Copper 3.458 2.86 ppm
Iron 73.156 60.5 ppm
Manganese 23.216 19.2 ppm
Molybdenum 0 ppm
Zinc 73.156 60.5 ppm
Total Starch 2.539 2.1 %
The HPLC profile (% w/v) for the molasses product of Table 10 is shown in
Table 11.
Table 11. DMB ¨ HPLC profile (% W/V)
Syrup DP4+ DP3 Maltose Glucose Lactic Glycerol Acetic Ethanol
2 10.84 1.38 6.57 6.62 2.74 36.02 0.26 0.00
See also FIG. 9 showing spin vials containing the molasses product obtained
in this testing at 30%, 40% and 50% total solids, which contains varying
amounts of
emulsion concentrate.
It was observed that overflow held for more than 14 days allowed Maillard
products to form, which likely resulted in a lower quality molasses product.
Possible
solutions to this issue are discussed in Example 4 (Prophetic).
Additionally, the Regenerative Thermal Oxidizer (RTO) did not function
properly during the evaporation run, causing loss of the vacuum source. As a
result, the
temperature of the molasses product in the evaporator increased from 170 F to
215 F,
thus overcooking the molasses product, causing an off-odor in the molasses
product and
producing additional Maillard reaction products. Possible solutions to this
issue are
discussed in Example 5 (Prophetic).
EXAMPLE 3
Centrate (e.g., 227, FIG. 2) from a decanter (e.g., 126, FIG. 2) was taken
from the
same. Commercial ethanol production facility described in Example I during
real-time
operations.
An FQ950 (Fluid Quip) stack nozzle centrifuge (size 40 nozzle) was used to
recover suspended solids (comprising primarily fine suspended solids as
defined herein)
32

CA 02780589 2012-06-21
from the centrate. Samples were drawn off directly from the centrate into the
centrifuge
at a temperature of approximately 180 F (82 C).
The centrifuge was flushed twice per day during testing. In-place cleaning was

performed every 7 days using 5% caustic soda concentration.
The centrifuge was operated at a full-rated rotation rate. Feed rate to the
centrifuge is shown below in Table 12. Overflow from the centrifuge was
transferred
back into the evaporation system in the facility. Underflow from the
centrifuge was
transferred to the decanter system in the facility. The fraction of suspended
solids
captured by the centrifuge averaged 86.3% as shown in Table 13.
Overflow and underflow rates are also shown in Table 12. The centrifuge tended
to entrain air into the overflow and underflow process streams, which likely
introduced a
minor error (less than 15%) in the flow rate meter readings for these streams.
As such,
the values given in Table 12 are approximate
Table 12. Volumetric ratios of suspended solids versus total volume in-spin
test
feed
overflow underflow suspended
feed rate overflow underflow suspended suspended suspended solids
(Lpm) (Lpm) (Lpm) volume volume volume recovery
= ratio ratio ratio
ratio
Average 1500 1150 425 , 0.13 0.02 0.3
0.9
st. d.ev, 120 200 140 0.02 0.01 0.05
0.1
Max 1800 1830 540 0.2 0.07 0.47 1
Min 1025 800 0 0.07 0 0.17
0.4
165 165 165 165 165 165 165
s amples
EXAMPLE 4 (PROPHETIC)
Improved results as compared to those discussed in Example 2 may be obtained
by matching evaporator performance rate with overflow production rate. In this
way,
overflow material at 190 F (88 C) is kept for a number of hours versus weeks
before
going to the evaporator.
Improved results may additionally or alternatively be obtained by using an
additional heat exchanger may be used to increase heat input into the
evaporator to
increase the throughput of the system. The new heat exchanger may be put in
parallel
with the existing heat exchanger to increase the evaporative rate by
approximately 2.5
times. This is expected to create a 2.5 gpm (9.5 Lpm) condensate production
rate.
33

CA 02780589 2012-06-21
Improved results may additionally or alternatively be obtained by using an
additional vacuum line to reduce pressure in the evaporator, thus keeping the
temperature
down and/or increasing the flux rate through the exchanger.
These processing steps may be tested alone or in combination, with improved
results
possible, as compared to the results in Example 2.
EXAMPLE 5 (PROPHETIC)
Improved results as compared to those discussed in Example 2 may be obtained
by monitoring evaporator temperatures.
Improved results may additionally or alternatively be obtained by selecting 35
Brix as a target concentration for the molasses product prior to bio-oil
recovery. Products
above this concentration can be de-oiled with Z23.
Improved results may additionally or alternatively be obtained by selecting 70-
75
Brix as a target concentration for the final molasses product concentration
based on
tlowability. This concentration can be accomplished through evaporation.
These processing steps may be tested alone or in combination, with improved
results
possible, as compared to the results in Example 2.
EXAMPLE 6 (PROPHETIC)
DDS material has a high variability in fat content, likely due to the shot
cycle
frequency being used on the unit combined with feed rate. The working
hypothesis is
that after centrifugation, the DDS material has a full open shot cycle, with
the next cycle
having very low bio-oil content because the system is getting maximum
recovery. Each
successive shot cycle will produce a higher bio-oil content because the system
is getting
maximum recovery. Each successive shot cycle will produce a higher bio-oil
content
DDS recovery_ It is desired to have low bio-oil content in the DDS material,
as well as a
consistent product so the bio-oil concentration will be determined with an
increased
degree of accuracy.
The shot cycle hypothesis will be tested by taking a series of samples
throughout
the full cycle to determine the compositional make-up of the bio-oil.
Depending on the
results, the shot cycle will be altered in order to produce DDS material that
contains no
more than 5% fat.
34

CA 02780589 2012-06-21
In one embodiment, a method is provided, comprising clarifying a thin
stillage product in a mechanical processor (e.g,, centrifuge and/or one or
more filters,
and the like) to produce a fine suspended solids stream and clarified thin
stillage; and
providing the thin stillage product and the clarified thin stillage,
separately or in a
combined stream, to one or more evaporators to produce one or more reduced
suspended solids streams, each stream having a reduced amount of suspended
solids
and a lower viscosity as compared to process streams having a comparable total

solids content and which contains a higher amount of suspended solids. The
suspended solids can comprise, in one embodiment, less than about 10% by
weight
of the total solids content and the total solids content can be between about
68% and
about 72% by weight. In one embodiment, substantially all or a majority of the

clarified thin stillage can be provided to the thin stillage product.
In one embodiment, at least one of thc one or more reduced suspended solids
stream has a total solids content comprising suspended solids and dissolved
solids in
an amount between about 30% and about 90% by weight, wherein the suspended
solids comprise less than 25% by weight of the total solids content.
At least one of the one or more reduced suspended solids stream can be, for
example, clarified concentrated thin stillage, which contains an amount of bio-
oil that
is greater, by volume, than an amount of bio-oil present in a concentrated
thin stillage
that has not been clarified. In some embodiments, the clarified concentrated
thin
stillage can be subject to mechanical processing to produce a bio-oil product,
such as
a bio-oil phase or free bio-oil.
In one embodiment, the mechanical processing produces an emulsion
concentrate that is broken in an emulsion breaking reaction to produce the bio-
oil
phase. In one embodiment, the mechanical processing also produces a solids
stream
and a de-oiled clarified concentrated thin stillage product, and the method
further
comprises providing the de-oiled clarified concentrated thin stillage product
to the
one or more evaporators.
In one embodiment, at least one of the one or more reduced suspended solids
stream is a molasses product having a total solids content no less than about
45% by
weight, wherein the suspended solids comprise less than 25% by weight down to
about 0% of the total solids content.

CA 02780589 2012-06-21
The method can further comprise, for example, combining at least a portion
of the one or more reduced suspended solids streams with wet cake to produce a
wet
cake product containing reduced suspended solids, and drying the wet cake
product
to produce a distillers dried grain.
In one embodiment, the method further comprises providing at least a portion
of the one or more reduced suspended solids streams to a dryer to produce
distiller's
dried grain solubles and/or drying the fine suspended solids stream to produce
dry
distiller's solubles containing single cell proteins.
In one embodiment, the thin stillage product may be produced from low water
extractable non-starch polysaccharide (NSP)-containing plant biomass. Use of
NSP-
containing biomass provides reduced protein dilution in the resulting process
stream.
As such, an improved feed product from the underflow (e.g., fine suspended
solids
stream, e.g., 229, FIG. 2) may be provided.
Various bin-products can be produced according to the methods described
herein,
including, but not limited to, clarified concentrated thin stillage, clarified
thin stillage,
fme suspended solids stream, a molasses product, dry distiller's solubles, wet
cake
product, distiller's dry grain, distiller's dry grain solubles, and
combinations thereof.
In one embodiment, a method is provided comprising clarifying a thin stillage
product in a mechanical processor to produce a fine suspended solids stream
arid
clarified thin stillage; providing the thin stillage product and the clarified
thin stillage,
separately or in a combined stream, to one or more evaporators to produce at
least two
reduced suspended solids streams, each of the at least two streams having a
reduced
amount of suspended solids and a lower viscosity as compared to process
streams having
a comparable total solids content but containing a higher amount of suspended
solids;
and subjecting at least one of the at least two reduced suspended solids
streams to
mechanical processing to produce a bio-oil product. The at least two reduced
suspended
solids streams may comprise, for example, a stream containing clarified
concentrated
thin stillage and a stream containing a molasses product, wherein the
clarified
concentrated thin stillage is subjected to the mechanical processing. The
molasses
product may contain, for example, two to three times the amount of bio-oil per
volume as
compared to concentrated thin stillage. In one embodiment, the molasses
product has
between about 65% and 75% total solids, by weight, and contains between about
8% and
36

CA 02780589 2012-06-21
about 12% bio-oil, by volume. The molasses product may be sold, combined with
wet
cake, and/or dried.
In one embodiment, a method is provided, comprising clarifying a thin stillage

product to produce one Or more reduced suspended solids streams, each having a
total
solids content between about 30% and about 90% by weight, wherein the total
solids
Content comprises suspended solids and dissolved solids, and the suspended
solids
comprise less than 25% by weight of the total solids content.
In one embodiment, a system is provided, comprising a clarifier for clarifying
a
thin stillage product to produce a fine suspended solids stream and clarified
thin stillage;
and one or more evaporators for evaporating the thin stillage product and the
clarified
thin stillage to produce one or more reduced suspended solids streams, each
having a
reduced amount of suspended solids and a lower viscosity as compared to a
process
stream having a comparable total solids content but containing a higher amount
of
suspended solids. A system control device (e.g., a holding tank that is
optionally
connected to a heat source) that is adapted to provide a quantity of thin
stillage product
for use downstream may also be used.
In one embodiment, the system further comprises a biomass processing facility
having one or more process streams and configured to produce a biofuel and a
containing process stream, wherein the biomass processing facility includes a
dewatering
system for dewatering the bio-oil containing process stream to produce an
emulsion
concentrate containing entrapped bio-oil; and an emulsion breaking system
configured to
at least partially break the emulsion concentrate with an emulsion breaking
additive so
that the entrapped bio-oil (e.g., corn oil) is released. The system can
further comprise, for
example, a bin-product production facility capable of producing bin-products,
such as
biofuels, biochemical, and the like. In one embodiment, the biofuel is alcohol
(e.g.,
ethanol, butanol, etc.).
In one embodiment, a method for reducing a dryer load in a bio-product
production facility is provided comprising clarifying a thin stillage product
in a
mechanical processor to produce a fine suspended solids stream and clarified
thin
stillage; and providing the thin stillage product and the clarified thin
stillage, separately
or in a combined stream, to one or more evaporators to produce one or more
reduced
suspended solids streams, each stream having a reduced amount of suspended
solids and
a lower viscosity as compared to process streams having a comparable total
solids
37

CA 02780589 2012-06-21
= content and which contains a higher amount of suspended solids, wherein
the dryer load
is reduced as compared to a method performed without a clarifying step.
In one embodiment, a method for improving bio-product production yield is
provided comprising clarifying a thin stillage product in a mechanical
processor to
produce a fine suspended solids stream and clarified thin stillage; and
providing the thin
stillage product and the clarified thin stillage, separately or in a combined
stream, to one
or more evaporators to produce one or more reduced suspended solids streams,
each
stream having a reduced amount of suspended solids and a lower viscosity as
compared
to process streams having a comparable total solids content and which contains
a higher
amount of suspended solids, wherein bio-products production yield is increase
as
compared to a method performed without a clarifying step.
In one embodiment, a method of reducing emissions in a bio-product production
facility comprising clarifying a thin stillage product in a mechanical
processor to produce
a fme suspended solids stream and clarified thin stillage; and providing the
thin stillage
product and the clarified thin stillage, separately or in a combined stream,
to one or more
evaporators to produce one or more reduced suspended solids streams, each
stream
having a reduced amount of suspended solids and a lower viscosity as compared
to
process streams having a comparable total solids content and which contains a
higher
amount of suspended solids, wherein emissions from the bio-product production
facility
are reduced as compared to a method performed without a clarifying step.
In one embodiment, energy costs in the alcohol production facility are
reduced as compared with conventional methods, since more moisture can be
removed with evaporators rather than expensive dryers. In one embodiment, the
reduced dryer load allows for an increased rate of production of alcohol and
co-
products at the alcohol production facility. In one embodiment, dryer load is
reduced
by at least 10%.
In one embodiment, production rate is also improved by operating one or
more evaporators (e.g., first effect evaporators) at a higher temperature,
thus reducing
the energy required for evaporation. In one embodiment, the energy
requirements for
evaporation are reduced by at least 33%.
DDGS produced according to the embodiments described herein not only
meets current minimum market levels of 8% bio-oil content by volume, but in
some
38

CA 02780589 2012-06-21
embodiments contain an increased amount of protein, as well as a reduced
sulfur and
ash content.
The various embodiments also reduce production facility emissions overall,
including emission of volatile organic contaminants (VOCs) since dryer loads
are
reduced.
Although specific embodiments have been illustrated and described herein, it
will be appreciated by those of ordinary skill in the art that any procedure
that is
calculated to achieve the same purpose may be substituted for the specific
embodiments shown. This application is intended to cover any adaptations or
variations of the present subject matter. Therefore, it is manifestly intended
that
embodiments of this invention be limited only by the claims and the
equivalents
thereof,
39

Dessin représentatif
Une figure unique qui représente un dessin illustrant l'invention.
États administratifs

Pour une meilleure compréhension de l'état de la demande ou brevet qui figure sur cette page, la rubrique Mise en garde , et les descriptions de Brevet , États administratifs , Taxes périodiques et Historique des paiements devraient être consultées.

États administratifs

Titre Date
Date de délivrance prévu 2013-09-24
(22) Dépôt 2012-06-21
Requête d'examen 2012-06-21
(41) Mise à la disponibilité du public 2012-08-31
(45) Délivré 2013-09-24
Réputé périmé 2021-06-21

Historique d'abandonnement

Il n'y a pas d'historique d'abandonnement

Historique des paiements

Type de taxes Anniversaire Échéance Montant payé Date payée
Requête d'examen 800,00 $ 2012-06-21
Le dépôt d'une demande de brevet 400,00 $ 2012-06-21
Taxe finale 300,00 $ 2013-07-08
Taxe de maintien en état - brevet - nouvelle loi 2 2014-06-23 100,00 $ 2014-05-22
Taxe de maintien en état - brevet - nouvelle loi 3 2015-06-22 100,00 $ 2015-04-01
Taxe de maintien en état - brevet - nouvelle loi 4 2016-06-21 100,00 $ 2016-01-11
Taxe de maintien en état - brevet - nouvelle loi 5 2017-06-21 200,00 $ 2016-12-28
Taxe de maintien en état - brevet - nouvelle loi 6 2018-06-21 200,00 $ 2018-06-12
Taxe de maintien en état - brevet - nouvelle loi 7 2019-06-21 200,00 $ 2019-06-12
Taxe de maintien en état - brevet - nouvelle loi 8 2020-06-22 200,00 $ 2020-04-01
Titulaires au dossier

Les titulaires actuels et antérieures au dossier sont affichés en ordre alphabétique.

Titulaires actuels au dossier
ICM, INC.
Titulaires antérieures au dossier
S.O.
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Abrégé 2012-06-21 1 17
Description 2012-06-21 39 1 899
Revendications 2012-06-21 6 194
Dessins représentatifs 2012-08-06 1 23
Page couverture 2012-09-07 1 56
Revendications 2013-02-04 6 214
Description 2013-02-04 39 1 904
Dessins représentatifs 2013-09-04 1 22
Page couverture 2013-09-04 2 60
Dessins 2013-02-04 8 190
Correspondance de la poursuite 2013-02-04 24 874
Cession 2012-06-21 6 138
Poursuite-Amendment 2012-09-11 1 18
Poursuite-Amendment 2012-11-06 3 102
Correspondance 2013-07-08 1 50