U.S. patent application number 10/942548 was filed with the patent office on 2005-02-10 for use of fermentation residues as flow-enhancing agents in cementitious materials.
This patent application is currently assigned to A. E. Staley Manufacturing Co.. Invention is credited to Harrison, Michael D., Hoffman, Andrew J..
Application Number | 20050031719 10/942548 |
Document ID | / |
Family ID | 30443565 |
Filed Date | 2005-02-10 |
United States Patent
Application |
20050031719 |
Kind Code |
A1 |
Hoffman, Andrew J. ; et
al. |
February 10, 2005 |
Use of fermentation residues as flow-enhancing agents in
cementitious materials
Abstract
Herein is disclosed an admixture, for concrete, gypsum panels,
and other cementitious products, derived from fermentation still
bottoms. The admixture typically comprises protein, glycerol, and
lactate, as well as smaller amounts of other alcohols, sugars, and
other organic acids. The admixture may be present as a solution
(typically comprising about 30-50 wt % solids) or as a dry mixture.
The admixture allows increased flow and reduced water use in
concrete and gypsum slurries used in gypsum panel production.
Concrete, cement, and gypsum premixes, ready-mixes, and poured
structures are disclosed.
Inventors: |
Hoffman, Andrew J.; (Mt.
Zion, IL) ; Harrison, Michael D.; (Decatur,
IL) |
Correspondence
Address: |
Raymund F. Eich, Ph.D.
WILLIAMS, MORGAN & AMERSON, P.C.
Suite 1100
10333 Richmond
Houston
TX
77042
US
|
Assignee: |
A. E. Staley Manufacturing
Co.
|
Family ID: |
30443565 |
Appl. No.: |
10/942548 |
Filed: |
September 16, 2004 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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10942548 |
Sep 16, 2004 |
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10200813 |
Jul 22, 2002 |
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6797050 |
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Current U.S.
Class: |
424/780 ;
106/645 |
Current CPC
Class: |
C04B 24/001 20130101;
C05G 5/40 20200201; C04B 28/02 20130101; C04B 28/02 20130101; C04B
28/14 20130101; C04B 28/02 20130101; C04B 24/14 20130101; C04B
24/10 20130101; C04B 24/001 20130101 |
Class at
Publication: |
424/780 ;
106/645 |
International
Class: |
C04B 024/14 |
Claims
What is claimed is:
1. A composition, comprising: a cementitious material, and a
fermentation residue.
2. The composition of claim 1, wherein the cementitious material is
selected from the group consisting of cements and gypsum.
3. The composition of claim 2, wherein the cementitious material is
Type I Portland cement.
4. The composition of claim 1, wherein the fermentation residue is
a yeast ethanol fermentation residue or a Corynebacterium lysine
fermentation residue.
5. The composition of claim 1, wherein the fermentation residue is
prepared by growing a microorganism on a medium, to form at least a
microorganism biomass and the fermentation residue, and separating
the fermentation residue from the microorganism biomass.
6. The composition of claim 5, wherein the separating is performed
by microfiltration with at least one membrane having a pore size
from about 50 nm to about 1500 nm.
7. The composition of claim 1, wherein the fermentation residue
comprises from about 20 wt % to about 100 wt % water-soluble
compounds.
8. The composition of claim 1, wherein the fermentation residue is
dry.
9. The composition of claim 1, wherein the fermentation residue
comprises protein, glycerol, and at least one organic acid.
10. The composition of claim 1, wherein the composition comprises
from about 0.1 oz. fermentation residue water-soluble compounds per
100 pounds cementitious material to about 50 oz. fermentation
residue water-soluble compounds per 100 pounds cementitious
material.
11. The composition of claim 10, wherein the composition comprises
from about 1 oz. fermentation residue water-soluble compounds per
100 pounds cementitious material to about 20 oz. fermentation
residue water-soluble compounds per 100 pounds cementitious
material.
12. The composition of claim 1, further comprising water other than
any water present in the fermentation residue.
13. The composition of claim 12, wherein the water-cement weight
ratio is from about 0.25 to about 0.75.
14. The composition of claim 1, further comprising an additive
selected from the group consisting of flow improvers, plasticity
improvers, water reducers, strengtheners, set retarders, set
accelerators, air entrainers, corrosion inhibitors, and shrink
compensation agents.
15. The composition of claim 14, wherein the additive is present at
from about 5 wt % to about 50 wt % relative to fermentation residue
water-soluble compounds.
16. The composition of claim 1, further comprising aggregate.
17. The composition of claim 16, wherein the aggregate is present
at from about 0.1 lbs/lb cementitious material to about 10 lbs/lb
cementitious material.
18. The composition of claim 17, wherein the aggregate is present
at from about 4 lbs/lb cementitious material to about 6 lbs/lb
cementitious material.
19. The composition of claim 1, wherein the fermentation residue
comprises, by weight, from about 8 parts to about 11 parts protein,
from about 0.01 parts to about 0.04 parts fat, from about 6 parts
to about 10 parts glycerol, from about 0.1 parts to about 0.4 parts
arabitol, from about 0.1 parts to about 0.8 parts sorbitol, from
about 0.5 parts to about 1.2 parts trehalose, from about 0.9 parts
to about 1.2 parts glucose, from about 0.05 parts to about 0.10
parts fructose, from about 1.1 parts to about 1.3 parts isomaltose,
from about 0.1 parts to about 0.3 parts maltose, from about 0.01
parts to about 0.05 parts maltotriose, from about 0.07 parts to
about 0.30 parts panose, from about 0.01 parts to about 0.06 parts
linear 4-24 unit dextrose oligomers, from about 2 parts to about 4
parts nonlinear 4-24 unit dextrose oligomers, from about 3 parts to
about 6 parts lactate, from about 0.1 parts to about 0.2 parts
acetate, from about 0 parts to about 0.03 parts formate, from about
0.1 parts to about 0.2 parts pyruvate, from about 0.4 parts to
about 0.6 parts chloride, from about 0.9 parts to about 1.1 parts
succinate, from about 0.5 parts to about 0.7 parts sulfate, from
about 0.2 parts to about 0.3 parts oxalate, and from about 2 parts
to about 4 parts phosphate.
20. A method of preparing a composition comprising a cementitious
material and a fermentation residue, the method comprising: growing
a microorganism on a medium, to form at least a microorganism
biomass and a fermentation residue; separating the fermentation
residue from the microorganism biomass; and combining the
fermentation residue with the cementitious material, to form the
composition.
21. The method of claim 20, further comprising concentrating the
fermentation residue water-soluble compounds prior to combining the
fermentation residue with the cementitious material.
22. The method of claim 20, wherein the cementitious material is
selected from the group consisting of cements and gypsum.
23. The method of claim 20, wherein the microorganism is selected
from the group consisting of yeast and Corynebacterium.
24. The method of claim 20, wherein the separating is performed by
microfiltration with at least one membrane having a pore size from
about 50 nm to about 1500 nm.
25. The method of claim 20, wherein the growing step further
comprises producing at least one target product, and the method
further comprises removing the at least one target product from the
medium, to retain the microorganism biomass and the fermentation
residue.
26. The method of claim 25, wherein the at least one target product
is selected from the group consisting of ethanol and lysine.
27. The method of claim 20, further comprising removing one or more
compounds from the fermentation residue prior to the combining
step.
28. The method of claim 20, further comprising combining the
fermentation residue and the cementitious material with at least
one additional material selected from group consisting of water,
aggregate, and additives selected from the group consisting of flow
improvers, plasticity improvers, water reducers, strengtheners, set
retarders, set accelerators, air entrainers, corrosion inhibitors,
and shrink compensation agents.
29. A method of producing a cementitious structure, comprising:
combining at least a fermentation residue, a cementitious material,
and water, to yield a slurry; forming the slurry into an unset
cementitious structure; and setting the unset cementitious
structure, to yield the cementitious structure.
30. The method of claim 29, wherein the fermentation residue is a
yeast ethanol fermentation residue or a Corynebacterium lysine
fermentation residue.
31. The method of claim 29, wherein the cementitious material is
selected from the group consisting of cements and gypsum.
32. The method of claim 29, wherein the combining step further
comprises combining aggregate with the fermentation residue, the
cementitious material, and water.
33. The method of claim 29, wherein the cementitious structure is
selected from the group consisting of foundations, floors, walls,
slabs, construction panels, roads, mortar, grout, terrazo, and
adhesive.
34. A composition, comprising: a fermentation residue, water, and
an inorganic material dispersed in the water.
35. The composition of claim 34, wherein the fermentation residue
is prepared by growing a microorganism on a medium, to form at
least a microorganism biomass and the fermentation residue, and
separating the fermentation residue from the microorganism
biomass.
36. The composition of claim 35, wherein the separating is
performed by microfiltration with at least one membrane having a
pore size from about 50 nm to about 1500 nm.
37. The composition of claim 34, wherein the inorganic material is
selected from the group consisting of paper fillers and paper
pigments.
38. A method of preparing a composition comprising a fermentation
residue, water, and an inorganic material dispersed in the water,
the method comprising: growing a microorganism on a medium, to form
at least a microorganism biomass and the fermentation residue;
separating the fermentation residue from the microorganism biomass;
and combining the fermentation residue with the water and the
inorganic material, to form the composition.
39. A method of producing a paper structure containing an inorganic
material, comprising: combining a fermentation residue with water
and an inorganic material, to yield a solution; treating the paper
structure with the solution, to yield a treated paper structure;
and removing water from the treated paper structure, to yield the
paper structure containing the inorganic material.
Description
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates generally to the fields of
microbial fermentation and cementitious admixtures. More
particularly, it concerns the use of fermentation residues to
improve the properties of concretes and similar products.
[0003] 2. Description of Related Art
[0004] Fermentation is a well-known technique for producing a
number of commercially relevant organic compounds, including, but
not limited to, ethanol and organic acids. In fermentation, a
microorganism, in many cases yeast, is grown in a fermentation
vessel on a medium suitable for the microorganism's growth. A
commonly-used medium for yeast comprises dextrose and corn steep
liquor. During the course of fermentation, the microorganism
biomass increases and a commercially relevant target product is
generated. After microorganism growth is complete, the target
product is isolated, typically by one or more of distillation,
crystallization, solvent extraction, and chromatographic
separation. After recovery of the target product the microorganism
biomass, non-fermentable components of the medium, and
water-soluble compounds generated by the microorganism remain in
the fermentation vessel. These components together may be referred
to as "beer still bottoms" or "fermentation still bottoms."
[0005] To dispose of beer still bottoms, producers frequently pass
this material to the animal feeds industry. This does capture some
economic value from the material; however, this value is typically
very low. Therefore, producers would prefer to capture more
economic value from beer still bottoms than is possible from animal
feeds uses.
[0006] Concrete is a ubiquitous construction material, both in the
United States and in most countries of the world. In the United
States during the year 2000, roughly 440 million cubic yards of
ready-mix concrete were produced. In order to save on the amount of
water used, enhance the properties of the concrete prepared
therefrom, or both, about 90% of all ready-mix concrete in the
United States is treated with an admixture. Low range water
reducing admixtures are often used at about 0.25 gal per cubic
yard. High range water reducing admixtures are often used at about
1 gal per cubic yard. Assuming that these admixtures are produced
as solutions comprising 50 wt % solids, annual admixture demand in
the United States alone would be in the range of 50 million pounds
to 100 million pounds.
[0007] Therefore, it would be desirable to have a new and valuable
use for beer still bottoms or one or more components thereof It
would also be desirable to have cementitious compositions with
improved flow and related properties without a concomitant increase
in the amount of water required in the cementitious composition. It
is well known in the art that increased water in the cementitious
slurry will decrease the ultimate strength of the hardened
material.
[0008] Yoshizawa et al., U.S. Pat. No. 4,311,721, reports the
extracting of water-soluble compounds from fermentation still
bottoms and the use of the water-soluble compounds in a
fermentation medium or an animal feed.
[0009] Willgohs, U.S. Pat. No. 5,662,810, discloses the use of
dewatered beer still bottoms as an animal feed.
[0010] Hamstra et al., U.S. Pat. No. 5,760,078, teaches the
extraction of potassium salts from the water-soluble compounds of
fermentation still bottoms, and the use of such potassium salts as
a fertilizer.
[0011] Sapienza, U.S. Pat. No. 6,315,919, reports the use of
water-soluble compounds from beer still bottoms as a deicing
agent.
SUMMARY OF THE INVENTION
[0012] In one embodiment, the present invention relates to a
composition comprising a cementitious material and a fermentation
residue.
[0013] In another embodiment, the present invention relates to a
method of preparing a composition comprising a cementitious
material and a fermentation residue, the method comprising (i)
growing a microorganism on a medium, to form at least a
microorganism biomass and fermentation residue; (ii) separating the
fermentation residue from the microorganism biomass; and (iii)
combining the fermentation residue with the cementitious material,
to form the composition.
[0014] In still another embodiment, the present invention relates
to a method of producing a cementitious structure, comprising (i)
combining at least a fermentation residue, a cementitious material,
and water, to yield a slurry; (ii) forming the slurry into an unset
cementitious structure; and (iii) setting the unset cementitious
structure, to yield the cementitious structure.
[0015] In a further embodiment, the present invention relates to a
composition, comprising a fermentation residue, water, and an
inorganic material dispersed in the water.
[0016] In yet a further embodiment, the present invention relates
to a method of preparing a composition comprising a fermentation
residue, water, and an inorganic material dispersed in the water,
the method comprising: (i) growing a microorganism on a medium, to
form at least a microorganism biomass and fermentation residue;
(ii) separating the fermentation residue from the microorganism
biomass; and (iii) combining the fermentation residue with the
water and the inorganic material, to form the composition.
[0017] In still a further embodiment, the present invention relates
to a method of producing a paper structure containing an inorganic
material, comprising: (i) combining a fermentation residue with
water and an inorganic material, to yield a solution; (ii) treating
the paper structure with the solution, to yield a treated paper
structure; and (iii) removing water from the treated paper
structure, to yield the paper structure containing the organic
material.
[0018] The various embodiments of the present invention provide a
new and valuable use for fermentation residues. The present
invention also provides for cementitious compositions with improved
flow and related properties without a concomitant increase in the
amount of water required in the cementitious composition.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The following drawings form part of the present
specification and are included to further demonstrate certain
aspects of the present invention. The invention may be better
understood by reference to one or more of these drawings in
combination with the detailed description of specific embodiments
presented herein.
[0020] FIG. 1 shows a process flow diagram for the isolation of a
fermentation residue from a fermentation process.
DESCRIPTION OF ILLUSTRATIVE EMBODIMENTS
[0021] The various embodiments of the present invention relate to a
fermentation residue and methods for its production and use.
[0022] Fermentation involves growing a microorganism on a medium,
to form at least a microorganism biomass and fermentation still
bottoms comprising water-soluble compounds and insoluble compounds.
A typical fermentation yields a target product, water,
microorganism biomass, and water-soluble compounds. The
microorganism biomass and water-soluble compounds may together be
referred to as "corn stillage." The remaining contents of the
fermentation medium, after removal of the target product and the
microorganism biomass, may be referred to as a "fermentation
residue" or "distillers solubles."
[0023] The growing step can involve any microorganism and any
medium known to one of ordinary skill in the art to be suitable for
growing the microorganism. Typical microorganisms useful in the
method include, but are not limited to, yeast, other fungi, and
bacteria, among others. Media appropriate for the growing of any
particular microorganism will generally be well known in the art.
The growing step will typically take place in a fermentor at a
temperature, pressure, pH, duration, and other parameters which
allow the microorganism to grow to a desired concentration,
typically a static concentration at the upper range of a sigmoidal
growth curve. During the growing step, a microorganism biomass and
fermentation residue will form.
[0024] Also during the growing step, the microorganism biomass may
produce at least one target product, i.e. a desirable compound
readily produced by and extractable from a microorganism biomass.
Typically, the microorganism is grown on the medium with the
primary objective of producing a target product or compounds.
However, this is not necessary. The target product or compounds
produced will depend on the microorganism and the medium. The
microorganism can, but need not, be a recombinant organism capable
of producing target products other than target products producible
by the wild-type or nonrecombinant microorganism. In one
embodiment, the microorganism is yeast. In one embodiment, the
target product is ethanol. In another embodiment, the microorganism
is a Corynebacterium (i.e., a bacterium of the genus
Corynebacterium). In another embodiment, the target product is
lysine. In one embodiment, the microorganism is a yeast and the at
least one target product is ethanol. In another embodiment, the
microorganism is a Corynebacterium and the at least one target
product is lysine.
[0025] If at least one target product is produced by the
fermentation, it is desirable to remove the at least one target
product, to retain the microorganism biomass and the fermentation
residue. If no target product is produced by the fermentation, then
such a removal step will not be necessary. Removal of any target
product can be performed by any appropriate technique; most
commonly, removal of any target product from the microorganism
biomass and fermentation still bottoms can be performed by one or
more of distillation, crystallization, solvent extraction, and
chromatographic separation.
[0026] A subsequent step in the process is separating the
fermentation residue from the microorganism biomass. In the
separating step, after the target product, if any, has been
isolated, the fermentation residue is separated from the
microorganism biomass by one or more appropriate techniques, such
as filtration, evaporation (including evaporation assisted by the
application of vacuum, heat, or both), centrifugation, and solvent
extraction, among others. Typically, the microorganism biomass and
the fermentation residue are subjected to microfiltration. One or
more membranes with pore sizes in the range of from about 50 nm to
about 1500 nm are generally suitable. Upon microfiltration, the
fermentation residue will generally be present in the permeate, and
the microorganism biomass will be present in the retentate. The
fermentation residue will generally comprise water-soluble
compounds.
[0027] The steps described to this point, as exemplified in a
typical but non-limiting yeast ethanol fermentation, are shown in
FIG. 1. A medium is added from a medium source 100 to a fermentor
102. A yeast culture (not shown) is also added to the fermentor
102, and growth of the yeast is allowed. During this process,
ethanol is produced. The medium, yeast biomass, ethanol, and other
components are then passed to a distillation tower 104, from which
ethanol is extracted in fraction 106. In the conventional process
known in the art, the yeast biomass 110 and fermentation residue
112 (collectively known as "beer still bottoms" or "BSB" 114) was
processed to animal feed 108. In the present invention, beer still
bottoms 114 are fed to a separating apparatus, such as one or more
microfiltration membranes 116, wherein the yeast biomass 110
remains in the retentate 118, and the fermentation residue 112
passes to the permeate 120. Alternative process flows and
techniques and apparatus usable therein are possible, as will be
apparent to one of ordinary skill in the art.
[0028] The fermentation residue can be used as-is. The
concentration of water-soluble compounds in the fermentation
residue will typically only be in the range of about 2% to about
10%. In many applications, it may be suitable to prepare a more
highly concentrated solution of the fermentation residue.
Therefore, the method may further comprise concentrating the
fermentation residue prior to subsequent use thereof. Such
concentration can be performed by evaporation, spray drying, or any
other appropriate technique known to one of ordinary skill in the
art.
[0029] The method may further comprise the partial or complete
removal of one or more compounds from the fermentation residue.
[0030] The composition of the fermentation residue is complex and
will depend on the microorganism, the medium, and the properties of
the fermentation process (including, but not limited to, duration,
medium temperature, medium pH, and medium oxygenation, among
others). Also, one or more compounds can be removed from the
fermentation residues as a matter of routine experimentation by one
of ordinary skill in the art. In various embodiments, the
fermentation residue comprises one or more compounds selected from
protein; glycerol; at least one organic acid; protein and glycerol;
protein and at least one organic acid; glycerol and at least one
organic acid; or protein, glycerol, and at least one organic
acid.
[0031] The fermentation residue can further comprise additional
compounds, depending on the microorganism, the medium, and the
properties of the fermentation process as described above. In the
case of a yeast ethanol fermentation, the fermentation residue can
further comprise any one or more of fat, arabitol, sorbitol,
trehalose, glucose, fructose, isomaltose, maltose, maltotriose,
panose, chloride, sulfate, and phosphate, among other compounds. In
the case of a yeast ethanol fermentation, the at least one organic
acid can be any one or more of lactate, acetate, formate, pyruvate,
succinate, and oxalate, among other compounds.
[0032] In one embodiment, the fermentation residue comprises, by
weight, from about 8 parts to about 11 parts protein, from about
0.01 parts to about 0.04 parts fat, from about 6 parts to about 10
parts glycerol, from about 0.1 parts to about 0.4 parts arabitol,
from about 0.1 parts to about 0.8 parts sorbitol, from about 0.5
parts to about 1.2 parts trehalose, from about 0.9 parts to about
1.2 parts glucose, from about 0.05 parts to about 0.10 parts
fructose, from about 1.1 parts to about 1.3 parts isomaltose, from
about 0.1 parts to about 0.3 parts maltose, from about 0.01 parts
to about 0.05 parts maltotriose, from about 0.07 parts to about
0.30 parts panose, from about 0.01 parts to about 0.06 parts linear
4-24 unit dextrose oligomers, from about 2 parts to about 4 parts
nonlinear 4-24 unit dextrose oligomers, from about 3 parts to about
6 parts lactate, from about 0.1 parts to about 0.2 parts acetate,
from about 0 parts to about 0.03 parts formate, from about 0.1
parts to about 0.2 parts pyruvate, from about 0.4 parts to about
0.6 parts chloride, from about 0.9 parts to about 1.1 parts
succinate, from about 0.5 parts to about 0.7 parts sulfate, from
about 0.2 parts to about 0.3 parts oxalate, and from about 2 parts
to about 4 parts phosphate.
[0033] A typical fermentation residue comprises water-soluble
compounds in aqueous solution. For such a composition, there is no
particular lower limit on the concentration of water-soluble
compounds in the solution. However, some minimal concentration of
water-soluble compounds will be produced in any typical
fermentation. A typical minimum concentration produced by a typical
fermentation, but one not to be construed as limiting, is about 2
wt % water-soluble compounds. Also, one of ordinary skill in the
art will recognize that a particular fermentation residue intended
for a particular application will have a certain minimum
economically- and fimctionally-desirable concentration of
water-soluble compounds. In one embodiment, the minimum
concentration of water-soluble compounds in the fermentation
residue is about 20 wt %. In another embodiment, the minimum
concentration of water-soluble compounds in the fermentation
residue is about 30 wt %. In still another embodiment, the minimum
concentration of water-soluble compounds in the fermentation
residue is about 40 wt %.
[0034] Also, there is no particular upper limit on the
concentration of water-soluble compounds in the fermentation
residue. One of ordinary skill in the art will recognize that a
particular fermentation residue intended for a particular
application will have a certain maximum concentration of
water-soluble compounds beyond which higher concentrations may pose
little, if any, economic or functional benefit. In one embodiment,
the maximum concentration of water-soluble compounds in the
fermentation residue is about 60 wt %. In another embodiment, the
maximum concentration of water-soluble compounds in the
fermentation residue is about 70 wt %. In still another embodiment,
the maximum concentration of water-soluble compounds in the
fermentation residue is about 80 wt %. In yet another embodiment,
the maximum concentration of water-soluble compounds in the
fermentation residue is about 90 wt %. In a further embodiment, the
maximum concentration of water-soluble compounds in the
fermentation residue is about 100 wt %.
[0035] In any embodiment wherein the fermentation residue comprises
at least about 90 wt % water-soluble compounds, the fermentation
residue may be referred to as a "dry" fermentation residue.
[0036] Depending on the particular fermentation residue and
intended application, any range of concentrations of the
water-soluble compounds is possible. Preferred ranges include all
possible ranges defined by any of the minimum concentrations and
any of the maximum concentrations described above. In one
embodiment, the fermentation residue comprises from about 20 wt %
to about 100 wt % water-soluble compounds. In another embodiment,
the fermentation residue is dry.
[0037] Fermentation residues, as described above, possess utility
as a concrete admixture, either alone or with other admixtures.
Admixtures are used routinely to improve the flow and setting
properties in concrete.
[0038] Fermentation residues also possess utility in improving the
flow properties or dispersion of any inorganic material that is
mixed in water. One such material is gypsum mixed in water, the
flow of which is improved, which property would be useful to
improve the production process of wallboard (also known as drywall
or gypsum panels, and commercially available under the tradename
Sheetrock.RTM., USG Corporation, Chicago, Ill.).
[0039] Fermentation residues also possess utility in dispersing
filler, pigment, or both in water for applications in paper
manufacture and paper coating operations.
[0040] Many of the embodiments of this invention, as described
below, provide superior flow properties in mixed concrete with a
low cost additive. Better flow is beneficial to make concrete fill
the gaps between rebar in roadways and is helpful when pumping
concrete into forms. Additionally, improved flow allows less water
to be used during mixing concrete, thus typically resulting in
stronger cured strength.
[0041] Similarly, in the production of wallboard, better flow
allows less water to be used during mixing, thus typically allowing
reduced drying costs in the wallboard manufacturing process.
[0042] After the fermentation residue has been separated and, if
desired, concentrated, the fermentation residue is combined with a
cementitious material, to form a composition comprising a
cementitious material and a fermentation residue.
[0043] A "cementitious material," as the term is used herein, is
any material which, when a dry powdered form thereof is wetted and
allowed to set, will yield a rigid unitary solid. In one
embodiment, the cementitious material is a cement. In another
embodiment, the cementitious material is gypsum. In a further
embodiment, the cementitious material is selected from the group
consisting of cements and gypsum.
[0044] In one preferred embodiment, the cementitious material is
Type I Portland cement.
[0045] The composition comprising the fermentation residue and the
cementitious material can be in any form. Typical forms include,
but are not limited to, a dry composition wherein the cementitious
material, the fermentation residue, and other components are
present in a homogeneous mixture of powdered ingredients (commonly
termed a "premix"), such as is commonly commercially available as a
ready-mix cement, concrete, mortar, or grout, among others; a
slurry wherein the cementitious material, the fermentation residue,
and other components are mixed with water, such as is commonly
prepared prior to pouring a cement, concrete, mortar, grout,
drywall panel, among others; and a set composition, such as is
formed after a poured slurry is allowed to set. Any composition
described herein can be in any form described above or known to one
of ordinary skill in the art.
[0046] The composition can comprise fermentation residue
water-soluble compounds and cementitious material in any weight
ratio. However, certain weight ratios will provide compositions
that are more economical, have more desirable functional
properties, or both. In one embodiment, the minimum weight ratio of
fermentation residue water-soluble compounds to cementitious
material is about 0.1 oz. fermentation residue water-soluble
compounds per 100 pounds cementitious material. In another
embodiment, the minimum weight ratio of fermentation residue
water-soluble compounds to cementitious material is about 0.5 oz.
fermentation residue water-soluble compounds per 100 pounds
cementitious material. In yet another embodiment, the minimum
weight ratio of fermentation residue water-soluble compounds to
cementitious material is about 1.0 oz. fermentation residue
water-soluble compounds per 100 pounds cementitious material.
[0047] In one embodiment, the maximum weight ratio of fermentation
residue water-soluble compounds to cementitious material is about
2.5 oz. fermentation residue water-soluble compounds per 100 pounds
cementitious material. In another embodiment, the maximum weight
ratio of fermentation residue water-soluble compounds to
cementitious material is about 5.0 oz. fermentation residue
water-soluble compounds per 100 pounds cementitious material. In
yet another embodiment, the maximum weight ratio of fermentation
residue water-soluble compounds to cementitious material is about
10 oz. fermentation residue water-soluble compounds per 100 pounds
cementitious material. In a further embodiment, the maximum weight
ratio of fermentation residue water-soluble compounds to
cementitious material is about 20 oz. fermentation residue
water-soluble compounds per 100 pounds cementitious material. In
yet a further embodiment, the maximum weight ratio of fermentation
residue water-soluble compounds to cementitious material is about
50 oz. fermentation residue water-soluble compounds per 100 pounds
cementitious material.
[0048] Depending on the particular fermentation residue,
cementitious material, and intended application, among other
parameters, any weight ratio of fermentation residue water-soluble
compounds to cementitious material is possible. Preferred ranges
include all possible ranges defined by any of the minimum weight
ratios and any of the maximum weight ratios described above. In one
preferred embodiment, the composition comprises from about 0.1 oz.
fermentation residue water-soluble compounds per 100 pounds
cementitious material to about 50 oz. fermentation residue
water-soluble compounds per 100 pounds cementitious material. In
another embodiment, the composition comprises from about 1 oz.
fermentation residue water-soluble compounds per 100 pounds
cementitious material to about 20 oz. fermentation residue
water-soluble compounds per 100 pounds cementitious material.
[0049] In one embodiment, a weight ratio of from about 1.0 oz.
fermentation residue water-soluble compounds per 100 pounds cement
to about 7.0 oz. fermentation residue water-soluble compounds per
100 pounds cement is suitable for use in a Type "A" or Type "D"
concrete admixture (American Society for Testing and Materials
(ASTM) Standard C494 (West Conshohocken, Pa.)). In one embodiment,
a weight ratio of from about 8.0 oz. fermentation residue
water-soluble compounds per 100 pounds cement to about 25.0 oz.
fermentation residue water-soluble compounds per 100 pounds cement
is suitable for use in a Type "F" or Type "G" concrete admixture
(ASTM C494). Such concrete admixtures, as well as others that will
be known to one of ordinary skill in the art, typically require
additional components, such as water, aggregate, and in some cases,
various additives. These additional components will be discussed
below.
[0050] In addition to the fermentation residue and the cementitious
material, at least one additional material can be added to the
composition.
[0051] The composition may further comprise water in addition to
any water present in the fermentation residue. The composition can
comprise water when the composition is in a slurry (unset) form or
in a set form. When the composition is in a slurry form, the
concentration of water, including both water present in the
fermentation residue and water added separately to the composition
(which may be referred to herein as "total water"), is typically
reported as a water-cement ratio, defined as the weight of total
water divided by the weight of the cementitious material. In one
embodiment of a slurry form, particularly suitable for concrete
applications, the composition has a lower limit to the water-cement
ratio of about 0.25. In another embodiment of the slurry form, the
composition has a lower limit to the water-cement ratio of about
0.3. In a further embodiment of the slurry form, the composition
has a lower limit to the water-cement ratio of about 0.35.
[0052] In one embodiment of the slurry form, the composition has an
upper limit to the water-cement ratio of about 0.75. In another
embodiment of the slurry form, the composition has an upper limit
to the water-cement ratio of about 0.7. In a further embodiment of
the slurry form, the composition has an upper limit to the
water-cement ratio of about 0.65.
[0053] Depending on the particular fermentation residue,
cementitious material, and intended application, among other
parameters, any economically- and functionally-desirable
water-cement ratio is possible for a slurry form of the
composition. Preferred ranges for concrete applications include all
possible ranges defined by any of the minimum water-cement ratio
and any of the maximum water-cement ratio described above. In one
preferred embodiment of the slurry form, the composition has a
water-cement ratio from about 0.25 to about 0.75.
[0054] The composition may further comprise an additive which
imparts one or more desirable properties to the composition, either
in a dry form, a slurry, a set form, or two or more of the above.
The additive can comprise one active ingredient or a plurality of
active ingredients, as well as fillers, carriers, and other
ingredients. In various preferred embodiments, the additive is
selected from one of several groups wherein each group
independently comprises one or more of flow improvers, plasticity
improvers, water reducers, strengtheners, set retarders, set
accelerators, air entrainers, corrosion inhibitors, or shrink
compensation agents. In one preferred embodiment, the additive is
selected from the group consisting of a flow improver, a plasticity
improver, a water reducer, a strengthener, a set retarder, a set
accelerator, an air entrainer, and a shrink compensation agent.
[0055] The composition may comprise more than one additive.
Desirably, each additive will be selected so as to not interfere
with the functional properties of the fermentation residue, the
cementitious material, and the other additive or additives, if
any.
[0056] Specific examples of additives useful in the composition
include various maltodextrins containing from 1-100 dextrose
equivalents (DE), such as Star-Dri 200 (a 20 DE maltodextrin made
from normal corn starch) (A.E. Staley, Decatur, Ill.), setting
accelerators such as triethanolamine (Sigma Chemical, St. Louis,
Mo.), and RM35C and RM1000C (International Admixtures Inc., Boca
Raton, Fla.). For such additives, as well as many others, the
additive can be present at a wide range of concentrations. In one
embodiment, the additive is present at at least about 5 wt %
relative to fermentation residue water-soluble compounds. In
another embodiment, the additive is present at at least about 10 wt
% relative to fermentation residue water-soluble compounds. In a
further embodiment, the additive is present at at least about 15 wt
% relative to fermentation residue water-soluble compounds.
[0057] In one embodiment, the additive is present at no more than
about 50 wt % relative to fermentation residue water-soluble
compounds. In another embodiment, the additive is present at no
more than about 40 wt % relative to fermentation residue
water-soluble compounds. In a further embodiment, the additive is
present at no more than about 30 wt % relative to fermentation
residue water-soluble compounds.
[0058] In one preferred embodiment, the additive is present at from
about 5 wt % to about 50 wt % relative to fermentation residue
water-soluble compounds.
[0059] The composition may further comprise aggregate. Aggregate
can be any material suitable for bulking and strengthening. The
inclusion of aggregate distinguishes concrete from cement. Commonly
used aggregates include sand, gravel, crushed rock, and mixtures
thereof, although any aggregate known to one of ordinary skill in
the art can be used. Sand is commonly referred to as "fine
aggregate," and gravel, crushed rock, or a mixture thereof is
commonly referred to as "coarse aggregate." Aggregate may be a
component of the composition when the composition is in a dry
(premix) form, a slurry form, or a set form.
[0060] Any amount of aggregate suitable for the intended type of
concrete to be prepared from a composition comprising the aggregate
can be used. In one embodiment, the aggregate is present at at
least about 0.1 lbs/lb cementitious material. In another
embodiment, the aggregate is present at at least about 1 lb/lb
cementitious material. In a further embodiment, the aggregate is
present at at least about 4 lbs/lb cementitious material.
[0061] In one embodiment, the aggregate is present at no more than
about 10 lbs/lb cementitious material. In another embodiment, the
aggregate is present at no more than about 8 lbs/lb cementitious
material. In a further embodiment, the aggregate is present at no
more than about 6 lbs/lb cementitious material.
[0062] In one preferred embodiment, the aggregate is present at
from about 0.1 lbs/lb cementitious material to about 10 lbs/lb
cementitious material. In another preferred embodiment, the
aggregate is present at from about 4 lbs/lb cementitious material
to about 6 lbs/lb cementitious material.
[0063] In various embodiments, the composition comprises one or
more of at least one additional material selected from water;
aggregate; at least one additive selected from the group consisting
of flow improvers, plasticity improvers, water reducers,
strengtheners, set retarders, set accelerators, air entrainers,
corrosion inhibitors, and shrink compensation agents; water and
aggregate; water and at least one additive listed above; aggregate
and at least one additive listed above; or water, aggregate, and at
least one additive listed above. Alternatively or in addition to
the above, further materials known to one of ordinary skill in the
art may be added to the composition.
[0064] The order of addition of the various components of the
composition is generally not crucial. However, water is generally
only added as part of the process of forming a cementitious
structure.
[0065] Upon the preparation of the composition comprising the
fermentation residue and the cementitious material, a slurry can be
prepared, formed, and set to yield a cementitious structure.
[0066] By "cementitious structure" is meant any structure or
structural element which can be produced by the pouring and setting
of a slurry comprising water and a cementitious material. After
pouring and before setting, the structure may be referred to as an
"unset cementitious structure." After setting, the structure may be
referred to as a "set cementitious structure." Cementitious
structures include foundations, floors, walls, slabs, construction
panels, roads, bridges, mortar, grout, terrazo, and adhesive, among
many others.
[0067] First, the water is added to the fermentation residue and
the cementitious material, to yield a slurry. Further components
which can be combined with the fermentation residue, the
cementitious material, and water include aggregate. Any aggregate
as described above can be used. An additive, such as the additives
described above, can also or alternatively be combined with the
fermentation residue, the cementitious material, and water. The
components, and any others that may be present, can be combined in
any apparatus useful in containing, mixing, or allowing both to be
performed on the components. Typically, the slurry is agitated to
provide a homogeneous mixture and retard setting until after an
unset cementitious structure is formed.
[0068] Forming the slurry into an unset cementitious structure can
be performed by any appropriate technique known in the art. As is
well known in the art, forming typically involves pouring,
spraying, or otherwise introducing the slurry into a mold, form, or
other structure. Within the space defined by the mold or form may
be placed, prior to forming, an object or material such as rebar
for the purpose of enhancing the strength or other structural
properties of the set cementitious structure to be produced by the
method.
[0069] Thereafter, the unset cementitious structure undergoes
setting, to yield the cementitious structure. Setting proceeds by
processes known in the art, and can be accelerated or retarded by
the inclusion of various additives in the composition or by other
processing techniques, as is known in the art.
[0070] In another embodiment, the present invention relates to a
composition, comprising:
[0071] a fermentation residue, water, and
[0072] an inorganic material dispersed in the water.
[0073] The fermentation residue and the water are as described
above. The fermentation residue may be prepared by separation from
a microorganism biomass and concentrating the water-soluble
compounds of the fermentation residue, as described above.
[0074] By "inorganic material" is meant a material not comprising
carbon. In one embodiment, the inorganic material is a filler for
paper manufacture or coating. In another embodiment, the inorganic
material is a pigment for paper manufacture or coating. In a
further embodiment, the inorganic material is selected from the
group consisting of paper fillers and paper pigments.
[0075] Dispersal of the inorganic material in the water can be
affected by any technique known in the art, such as dissolution,
suspension, and emulsification, among others. Various of these
techniques may call for further compounds, such as surfactants or
emulsifiers, as will be apparent to one of ordinary skill in the
art.
[0076] In another embodiment, the present invention relates to a
method of preparing a composition comprising a fermentation
residue, water, and an inorganic material dispersed in the water,
the method comprising:
[0077] growing a microorganism on a medium, to form at least a
microorganism biomass and a fermentation residue;
[0078] separating the fermentation residue from the microorganism
biomass; and
[0079] combining the fermentation residue with the water and the
inorganic material, to form the composition.
[0080] The growing and separating steps, and the compositions acted
on or yielded by these steps, are essentially the same as those
described in the context of fermentation, above. The fermentation
may result in the formation of one or more target products, and
those compounds may be removed prior to the separating step, as
described above in the context of fermentation. Also as described
above, one or more compounds may be partially or completely removed
from the fermentation residue prior to the combining step. In the
combining step, the inorganic material is as described above, and
combining can be performed according to any appropriate technique
known in the art.
[0081] In another embodiment, the present invention relates to a
method of producing a paper structure containing an inorganic
material, comprising:
[0082] combining a fermentation residue with water and an inorganic
material, to yield a solution;
[0083] treating the paper structure with the solution, to yield a
treated paper structure; and
[0084] removing water from the treated paper structure, to yield
the paper structure containing the inorganic material.
[0085] The solution comprising the fermentation residue, water, and
the inorganic material is as described above, and combining can be
performed by any appropriate technique.
[0086] The paper structure can be any structure comprising paper,
paperboard, cardstock, cardboard, or any other material in any
known form, including, but not limited to, printing paper, cartons,
and carton blanks, among others. The paper structure may contain
materials other than the inorganic material, and these materials
may be added before, after, or contemporaneously with the inorganic
material added during the performance of the method.
[0087] In the treating step, the paper structure is contacted with
the solution by any appropriate technique. Such techniques include,
but are not limited to, immersion of the paper structure in the
solution, spraying the solution onto the paper structure or a
surface thereof, and applying the solution via a brush or roller to
the paper structure or a surface thereof, among others. The
duration of the treating step, as well as the temperature of the
solution and other relevant process parameters, can readily be
determined for a given application by one of ordinary skill in the
art.
[0088] The treating step yields a paper structure comprising water,
the inorganic material, and the fermentation residue. Thereafter,
the water is removed from the paper structure during the removing
step. Removing water can be performed by any appropriate technique
that does not impair the structure and physical properties of the
paper structure. Such techniques include, but are not limited to,
evaporation, including evaporation assisted by heat, vacuum, or
both, among others. By "removing," in this context, is meant that
at least about 90 wt % of all water present in the portion of the
solution present in the paper structure after the treating step is
eliminated from the paper structure.
[0089] After removal of water, the paper structure comprises the
inorganic material and is suitable for further processing and
use.
[0090] The following examples are included to demonstrate preferred
embodiments of the invention. It should be appreciated by those of
skill in the art that the techniques disclosed in the examples
which follow represent techniques discovered by the inventor to
function well in the practice of the invention, and thus can be
considered to constitute preferred modes for its practice. However,
those of skill in the art should, in light of the present
disclosure, appreciate that many changes can be made in the
specific embodiments which are disclosed and still obtain a like or
similar result without departing from the spirit and scope of the
invention.
EXAMPLES
[0091] The beneficial flow properties of beer still bottoms (BSB)
filtrate concentrate (a "fermentation residue" as defined above)
are reported below as observed in concrete mixing studies, mortar
mixing studies, and in gypsum (wallboard) mixing studies.
Example 1
Pilot Scale Fractionation
[0092] Three 55-gallon drums of "raw" BSB were subjected to
microfiltration. The configuration of the microfiltration apparatus
was as follows:
[0093] Feed pump--Waukesha Model 60 with a VFD.
[0094] Circulation pump--Waukesha Model 220 (165 gpm)
[0095] Elements: 3 housings, in series, with 3 ceramic elements in
each housing
[0096] #1 housing--1400 nm pore--Membralox
[0097] #2 housing--800 nm pore--Membra Flow
[0098] #3 housing--200 nm pore--Membra Flow
[0099] All elements had 6 mil lumen.
[0100] Each Element Area=0.36 m.sup.2
[0101] It took about 30 minutes to collect approximately 90 gallons
of filtrate (.about.210 L/m.sup.2/hr (LMH)). The yeast retentate
was discarded. The filtrate was then processed on a drum scale
evaporator in a pilot plant to bring the dry solids level up to
about 50%. It took 5 hours of evaporation to give 8 gallons of
Concentrated BSB filtrate product.
[0102] The following evaporation conditions were found to work
well:
1 Steam 12 psig Feed Pump 56-57% Extraction Pump 58-59% Vacuum 23
inches Hg Product Temperature 140.degree. F.
[0103] The following analytical results for Concentrated BSB
filtrate were obtained (Table 1):
2 TABLE 1 Ash 8.56 % as is Moisture 54.57 % as is Protein 10.96 %
as is Fat 0.03 % as is Glycerol 9.33 % as is Arabitol 0.31 % as is
Sorbitol 0.70 % as is Trehalose 1.14 % as is Glucose 0.93 % as is
Fructose 0.09 % as is Iso-Maltose 1.21 % as is Maltose 0.25 % as is
Maltotriose 0.02 % as is Panose 0.29 % as is Linear Highers
(dp4-dp24) 0.01 % as is Non Linear Highers (dp4-dp24) 3.91 % as is
Lactate 5.21 % as is Acetate 0.19 % as is Formate 0.00 % as is
Pyruvate 0.12 % as is Chloride 0.52 % as is Succinate 0.99 % as is
Sulfate 0.59 % as is Oxalate 0.28 % as is Phosphate 2.89 % as
is
[0104] "Highers," as the term is used herein, refers to dextrose
oligomers comprising from 4 to 24 dextrose units. "Linear highers"
are dextrose oligomers that do not comprise branched or cyclic
structures. "Nonlinear highers" are dextrose oligomers comprising
branched or cyclic structures.
Example 2
Truckload Scale Fractionation
[0105] Microfiltration of 5,100 gallons of BSB (to remove the yeast
bodies) was accomplished in about 4 hours at 150.degree. F. The
microfiltration apparatus housed ceramic membranes with an average
pore size of 50 nm. The microfiltration was performed at a pressure
of 38 psig, a feed flow rate of about 31 gpm, and a recirculation
flow rate of about 11 gpm. This process produced 4,600 gallons of
permeate at an average rate of 20 gpm (.about.285 LMH).
[0106] Evaporation of the filtrate was completed in about 48 hours.
At an early stage of the evaporation, we applied 550 lb/hr of steam
at a vacuum of 18 inches of mercury. This resulted in an
evaporation rate of about 400 lb/hr of water at a temperature of
150.degree. F. At a later stage of the evaporation, we increased
the steam to 1,050 lb/hr at a vacuum of 22 inches of mercury. This
resulted in an evaporation rate of about 800 lb/hr of water at a
temperature of 134.degree. F.
[0107] Heating for the evaporator was discontinued when the product
refractive index (RI; measured at 40.degree. C. on an Atago RX-500
refractometer, with distilled water RI measured as 1.3307) reached
1.3907 to yield 280 gallons of Concentrated BSB filtrate product at
approximately 40% dry solids. The product was collected in five
55-gallon drums and one 5-gallon pail.
[0108] The following analytical results for Concentrated BSB
filtrate were obtained (Table 2):
3 TABLE 2 Ash 7.74 % as is Moisture 65.08 % as is Protein 8.36 % as
is Fat 0.02 % as is Glycerol 6.52 % as is Arabitol 0.18 % as is
Sorbitol 0.18 % as is Trehalose 0.51 % as is Glucose 1.13 % as is
Fructose 0.06 % as is Iso-Maltose 1.17 % as is Maltose 0.17 % as is
Maltotriose 0.04 % as is Panose 0.08 % as is Linear Highers
(dp4-dp24) 0.05 % as is Non Linear Highers (dp4-dp24) 2.88 % as is
Lactate 3.53 % as is Acetate 0.12 % as is Formate 0.02 % as is
Pyruvate 0.11 % as is Chloride 0.44 % as is Succinate 1.04 % as is
Sulfate 0.59 % as is Oxalate 0.23 % as is Phosphate 3.01 % as
is
[0109] It should be noted that chloride, sulfate, and phosphate
from this analysis are double counted both under "ash" and in their
own right. After taking this observation into account, greater than
99% of the mass of the material is accounted for.
[0110] The majority of the Concentrated BSB Filtrate used in the
following examples was taken from the batch whose analysis is shown
above in Table 2. The fermentation residue of Table 2 may be
referred to herein as "O2-002." Substantially all of the remaining
Concentrated BSB Filtrate used in the examples was taken from a
second batch, whose analysis was given in Table 1.
[0111] Although a number of components of BSB differ in their
levels between the two batches, no significant difference in
functional properties between the two batches was seen.
Example 3
Pilot Scale Study of Concentrated BSB Filtrate as a Mortar
Admixture
[0112] A pre-weighed 1.0 kg portion of Portland cement (Type I,
LaFarge Corp., Hemdon, Va.) was placed in the bowl of a 5-quart
mixer (Kitchen Aid, U.S.A., St. Joseph, Mich.). A 1.0 kg portion of
sand was likewise added to the mixer. Then 380 grams of water (or
water including test agent) was added to the mixing bowl. The mixer
was then switched on and allowed to mix at the lowest setting for
60 seconds. The water-cement ratio, defined as the weight of water
divided by the weight of cement in the mixture, was equal to 0.38
in this case (W/C=0.38).
[0113] Immediately after mixing was complete, a portion of the
mortar was placed into a flow table cone. The cone was filled
carefully to ensure that voids were not introduced during filling
and that the cone was completely filled and level at the top.
[0114] Next, the cone was carefully removed, and the diameter of
the mortar pile was measured at three places around the
circumference of the pile with a caliper. The results were recorded
and the average was reported as the initial, or "0 drop," flow in
inches. Then one end of the drop table was lifted 1 inch above its
resting position and allowed to drop freely. This dropping action
caused the mortar to flow out radially from its initial position
and the diameter of the mortar pile tended to increase as a
function of this vibration. A total of 5 drops were performed in
succession, and the mortar pile was once again measured at three
places around the circumference of the pile with a caliper. The
results were recorded and the average was reported as the "5 drop"
flow in inches. Five more drops were then applied to the sample to
give the "10 drop" flow in a similar manner. A greater diameter
indicates greater flow of the mortar pile.
[0115] After the flow test was complete, the remainder of the
mortar mix was transferred to a plastic container for a set-time
assay. The material was "worked" a bit in the plastic container to
ensure that no voids were present and that the material was evenly
distributed in the container. The container was then transferred to
a forced air oven set to 100.degree. F. for the duration of the
set-time assay. During this test, the sample was periodically
removed from the oven and tested with a hand penetrometer for its
compressive strength. The set-time for this assay was defined as
the time it took for the mortar to reach a compressive strength of
500 psi as determined with the penetrometer. Triplicate
measurements were taken and the average recorded about every 30
minutes until the endpoint was reached. More frequent measurements
were taken near the endpoint so that an accurate set-time could be
determined. The final measurements just below and above the 500 psi
target were used to interpolate the time where a compressive
strength of 500 psi was reached and this time was recorded as the
set-time for the experiment.
[0116] Typically, products were tested at a few levels of addition
to evaluate the "dose-response" relationship. Admixture
preparations for mortar and concrete are typically liquids with a
dry solids content in the range of 30 to 50% solids. The industry
also tends to report admixture dosages based on fluid ounces per
100 pounds of cement in the formula. Both the concentration of the
admixture and the amount of admixture used relative to the weight
of cement in the mix must be defined to quantify the effects of the
active ingredients on the functional properties.
[0117] Usually a "no admix" control mortar sample was run for a
baseline comparison. Results from a recent test using O2-002 with
quantities given as fl. oz. per 100 pounds cement are shown below
(Table 3):
4 TABLE 3 0 drop 5 drop 10 drop set-time Admixture inches inches
inches hours no admix control 4.0 5.9 6.8 2.3 O2-002 @ 5 oz 5.1 6.7
7.7 3.3 O2-002 @ 10 oz 5.2 6.8 7.8 4.2 O2-002 @ 15 oz 5.9 7.2 8.3
5.0
[0118] In this test, a dose dependent increase in flow was caused
by the O2-002 relative to the no admix control. A dose dependent
retardation of set-time due to the O2-002 was also seen in this
study.
Example 4
Pilot Scale Study of Concentrated BSB Filtrate as a Mortar
Admixture in Conjunction with Further Additives
[0119] In the next test, we investigated the effect of adding
RM1000C (IAI, Boca Raton) to O2-002 on the flow properties of
mortar. Two parts of RM1000C were added to seven parts O2-002 in
the test admixture. The results are shown in Table 4. An additional
increase in flow was seen with the addition of RM1000C to the
O2-002.
5TABLE 4 dosage 0 drop 5 drop 10 drop Admixture oz/100# inches
inches inches no admix control 0 3.9 5.3 6.2 O2-002 10 5.3 6.6 7.5
15 6.0 7.5 8.1 20 6.1 7.8 8.7 O2-002 (with RM1000C) 10 6.6 8.1 9.1
15 6.7 8.4 9.5 20 6.6 8.4 9.5
Example 5
Pilot Scale Study of Concentrated BSB Filtrate as a Mortar
Admixture in Conjunction with Further Additives
[0120] Another mortar study was performed to measure flow and
set-time on a wider range of doses for the O2-002/RM1000C (7:2)
combination, and results shown in Table 5, below. In this test, a
dose dependent increase in flow was seen for the admixture. A dose
dependent increase in set-time was seen up to a dose of 15 oz, then
the trend reversed giving shorter set-times at higher doses.
6TABLE 5 dosage 0 drop 5 drop 10 drop set-time Admixture oz/100#
inches inches inches hours no admix control 0 4.3 5.3 6.2 2.3
O2-002 5 5.9 6.9 7.6 3.6 (with RM1000C) 10 6.4 8.1 9.1 3.0 15 6.5
8.3 9.3 4.2 20 6.6 8.4 9.5 4.1 25 6.8 8.7 9.5 3.0
Example 6
Pilot Scale Study of Concentrated Molasses Solubles (CMS) as a
Mortar Admixture
[0121] A mortar study was performed on a different fermentation
residue to show the general utility of the present invention.
Concentrated Molasses Solubles (CMS) is obtained from fermentation
of Corynebacterium where lysine is produced as the target product.
After the target product is removed by ion exchange chromatography,
and the biomass is filtered off, the fermentation residue is
evaporated to provide CMS. The CMS had the following analysis:
7 Total Nitrogen 6-7% Ammonia Nitrogen 5% Phosphorous
(P.sub.2O.sub.5) 0.2% Potassium (K.sub.2O) 0.2-0.4% Sulfates 15-20%
Chlorides 2% pH 4 to 5 Total Solids 42-46%
[0122] In this example a mortar test was conducted to measure flow
and set-time on a range of admixture doses for the CMS (used "as
is" at about 44% solids). Results are shown in Table 6, below. In
this test, a significant dose dependent increase in flow was seen
for the CMS admixture up to the 10 oz dose. A slight reduction in
flow was seen at 15 oz when compared to the 10 oz results. A dose
dependent increase in set-time was seen up to a dose of 15 oz for
the CMS.
8TABLE 6 dosage 0 drop 5 drop 10 drop set-time Admixture oz/100#
inches inches inches hours no admix control 0 4.1 5.8 6.8 2.4 Conc.
Molasses 5 5.5 7.1 8.1 2.8 Solubles 10 5.7 7.6 8.6 3.2 15 4.7 7.2
8.4 3.8
Example 7
Pilot Scale Study of Concentrated BSB Filtrate as a Concrete
Admixture in Conjunction with Further Additives
[0123] The concrete formula used in this test included 10.0 kg of
Portland cement (Type 1, LaFarge), 29.5 kg of coarse aggregate
(3/4" stone), 24.3 kg of fine aggregate (sand) and 5.5 kg of water
(or water+admixture). This formula resulted in a water-cement
ratio. of 0.55 (W/C=0.55).
[0124] The inside of a mixer was lightly moistened with water
before initiating mixing. The mixer was turned on, then 5.0 kg of
water was added, followed by about half of the coarse aggregate and
about half of the fine aggregate. Next, all of the cement was added
a scoopful at a time. After the cement was mixed in over a few
minutes, the remaining coarse and fine aggregate was added to the
mixer. Finally, the last 0.5 kg of water (or water+admixture) was
added and mixing was allowed to proceed another 2.5 minutes.
[0125] Immediately after the concrete mixing was complete, a
portion of the concrete was transferred into a slump cone. The
bottom third of the slump cone was filled, then subjected to twenty
up and down strokes with an iron rod to ensure that voids were not
introduced during filling. The "rodding" procedure was repeated
after the cone was two-thirds full and also when the cone was
completely filled and level at the top.
[0126] Next, the slump cone was carefully removed, and the distance
that the concrete pile "slumped down" from its original height in
the cone was measured with a ruler and is reported as inches of
slump.
[0127] After the slump test was complete, a portion of the concrete
was passed through a #4 screen and transferred to a plastic
container for the set-time assay. The material was "worked" a bit
in the plastic container to ensure that no voids were present and
that the material was evenly distributed in the container. The
container was covered and allowed to sit at room temperature for
the duration of the set-time assay. During this test, the sample
was periodically uncovered and tested with a hand penetrometer for
its compressive strength. The set-time for this assay was defined
as the time it took for the mortar to reach a compressive strength
of 500 psi as determined with the penetrometer. Triplicate
measurements were taken, and the average recorded, about every 30
minutes until the endpoint was reached. More frequent measurements
were taken near the endpoint so that an accurate set-time could be
determined. The final measurements just below and above the 500 psi
target were used to interpolate the time where a compressive
strength of 500 psi was reached and this time is recorded as the
set-time for the experiment.
[0128] The remainder of the concrete is transferred to plastic
molds to make concrete cylinders for compressive strength testing.
Twenty up and down strokes with an iron rod were delivered to the
concrete in the mold after the mold was one-third, two-thirds, and
completely filled. The molds were capped with a plastic lid, then
sent off to a concrete testing lab. The samples were typically
tested for compressive strength on 1, 3, 7, and 28 days after
mixing. The average of duplicate (or triplicate) tests are reported
in units of psi.
[0129] Typically, products were tested at a few levels of addition
to evaluate the "dose-response" relationship. Admixture
preparations for mortar and concrete are typically liquids with a
dry solids content in the range of 30 to 50% solids. The industry
also tends to report admixture dosages based on fluid ounces per
100 pounds of cement in the formula. Both the concentration of the
admixture and the amount of admixture used relative to the weight
of cement in the mix must be defined to quantify the effects of the
active ingredients on the functional properties. Usually a "no
admix" control concrete mix was run for a baseline comparison.
Results from a test using O2-002 are shown below (Table 7):
9TABLE 7 7 day 28 day slump set-time strength strength Admixture
inches hours psi psi no admix control 1.9 3.5 5,527 7,039 O2-002 @
7.5 oz 2.9 4.7 5,200 6,367 O2-002 @ 15 oz 8.8 5.9 2,795 3,511
O2-002 (with RM1000C) @ 15 oz 9.3 6.5 3,528 4,563
[0130] In this test, a dose dependent increase in slump was caused
by the O2-002 relative to the no admix control. A dose dependent
retardation of set-time due to the O2-002 was also seen in this
study. A dose dependent decrease in strength was noted at 7 days
and 28 days. Also in this test an additional ingredient, RM1000C
(IAI, Boca Raton), was added to the O2-002. Blending RM1000C into
the O2-002 admix gave improved results in the slump and strength
tests when compared to the results seen with O2-002 alone.
Example 8
Study of Concentrated BSB Filtrate as a Concrete Admixture in
Conjunction with Further Additives
[0131] A series of slump, set-time and strength measurements were
performed on concrete that had been treated with O2-002. Concrete
was made with the test admixtures at a W/C=0.53 and an ambient
temperature of approximately 70.degree. F.
[0132] Concrete made in this test had the following material usage
per cubic yard:
10 Cement (Type I Portland) 564 lbs. Coarse Aggregate (#57
Limerock) 1656 lbs. Fine Aggregate (FDOT Concrete Sand) 1316 lbs.
Water 298 lbs.
[0133] The test admixtures in this study were:
[0134] WRDA-64, a commercially available low range water reducing
admixture manufactured by the W. R. Grace Co.
[0135] O2-002 blended with RM35C (IAI, Boca Raton, 7:1 ratio), a
low range water reducing admixture.
[0136] O2-002 with RM1000C (IAI, Boca Raton, 7:2 ratio), a high
range water reducing admixture.
[0137] Slump and set-time results from the independent testing are
shown below (Table 8):
11TABLE 8 Dosage initial 30 min 45 min initial final oz/100# slump
slump slump set time set time Admixture cement inches inches inches
hours hours WRDA-64 4 5.75 3 2.5 5.5 6.75 O2-002 5 8 5 3.5 4.75
6.25 (with RM35C) O2-002 8 5.75 4.5 3.75 5.25 6.5 (with RM35C)
O2-002 10 6 2 1.75 7 9 (with RM35C) O2-002 10 8 5.75 4 8 9 (with
RM1000C) O2-002 15 10.25 8.25 5.5 10 12.5 (with RM1000C)
[0138] In this study, a dose dependent increase in slump was caused
by the O2-002. A dose dependent retardation of set-time due to the
O2-002 was also seen in this study. The low range water reducing
admixture containing O2-002 at 5 oz compared favorably with the
commercially available material WRDA-64 at 4 oz.
[0139] Compressive strength results from the independent testing
are shown below (Table 9):
12TABLE 9 Dosage 3 day 7 day 28 day oz/100# strength strength
strength Admixture cement psi psi psi WRDA-64 4 4,230 5,370 6,573
O2-002 (with RM35C) 5 3,540 5,090 6,295 O2-002 (with RM35C) 8 n.t
n.t n.t O2-002 (with RM35C) 10 n.t n.t n.t O2-002 (with RM1000C) 10
4,650 6,630 7,960 O2-002 (with RM1000C) 15 3,250 5,680 6,780
[0140] The strength table shows that the treatments gave quite
similar results with a possible indication of improved strength for
the O2-002 (with RM1000C) at a dose of 10 oz.
Example 9
Field Trial of Concentrated BSB Filtrate as a Concrete Admixture in
Conjunction with Further Additives
[0141] A field trial was conducted at a ready-mix plant in order to
assess the performance of O2-002 as a concrete admixture under
"real-life" conditions. The trial was conducted at a W/C=0.54 and
an ambient temperature of approximately 105.degree. F.
[0142] Concrete made in this test had the following material usage
per cubic yard:
13 Cement (Type I Portland) 540 lbs. Coarse Aggregate (3/8" River
Granite) 1040 lbs. Fine Aggregate (River Sand) 1964 lbs. (contains
3% water) Water 233 lbs.
[0143] The only test admixture used in this study was O2-002 with
RM1000C (IAI, Boca Raton, 7:2 ratio) as a high range water reducing
admixture.
[0144] The admixture was used at a dosage of 10 oz/100 lb of cement
(4.2 gallons per 10 cubic yards). The initial slump was 8.5 inches,
measured 10 minutes after mixing. At the job site, the slump was
measured at 7.5 inches at 80 minutes after mixing. The batch
continued to maintain a good plasticity even at 200 minutes after
mixing, as it was pumped up to fill a second story beam loaded with
rebar and completed the job without problems. Even though the
material showed remarkable plasticity, especially considering the
high temperature at the job site, it had built enough strength to
enable a crew to finish a floor poured from the batch, with no
difficulty, just 2 hours after pouring.
Example 10
Pilot Scale Study of Concentrated BSB Filtrate as an Admixture in
Gypsum Panel Production
[0145] For each sample, 75 grams of room temperature water (or
water with admixture) was added to a 600-mL stainless steel beaker.
Then, 100 g dry gypsum powder (National Gypsum Corporation,
Charlotte, N.C.) was gently poured onto the water in the cup and a
timer was started. A six-inch, stainless steel spatula was then
used to gently push the gypsum under the surface of the water
(without stirring) over 10-20 seconds.
[0146] After allowing the gypsum to wet until 70 seconds had
elapsed on the timer, the slurry was vigorously mixed with the
spatula for twenty seconds. When the timer showed 90 seconds had
elapsed, the slurry was poured through a glass funnel positioned in
a ring stand. The lower, small mouth of the funnel was positioned
three inches above a glass plate. The diameter of the poured gypsum
patty was measured using large calipers. The average of four
measurements taken across the diameter of the patty was
recorded.
[0147] After the gypsum patty had been poured onto the glass plate,
the plate was moved under a 1/4 lb. Gilmore needle. Elapsed time
from the pouring of the patty was continuously monitored. The 1/4
lb. Gilmore needle was lowered until the needle point just touched
the gypsum patty, and then the needle was released. The force
produced by the mass of the weight alone pushed the needle into the
patty. When the 1/4 lb. Gilmore needle only penetrated the patty to
a depth of 1 mm, the elapsed time from pouring was recorded as the
set-time.
[0148] Results from a recent test using O2-002 are shown below
(Table 10):
14 TABLE 10 patty diameter set-time Admixture inches minutes no
admix control 3.5 4.58 O2-002 @ 0.3% 4.3 4.83 O2-002 @ 0.6% 4.6
6.58 O2-002 @ 1.2% 4.8 >10.00
[0149] In this test, a dose dependent increase in flow was caused
by the O2-002 relative to the no admix control. A dose dependent
retardation of set-time due to the O2-002 was also seen in this
study.
[0150] Summary statistics for all runs of O2-002 in gypsum can be
found below (Table 11):
15TABLE 11 patty diameter set-time inches minutes Admixture mean
+/- SD mean +/- SD no admix control 3.77 +/- 0.17 4.48 +/- 0.14 (n
= 5) O2-002 @ 0.3% 4.27 +/- 0.03 4.88 +/- 0.21 (n = 5) O2-002 @
0.6% 4.48 +/- 0.11 6.44 +/- 0.80 (n = 7) O2-002 @ 1.2% 4.63 +/-
0.12 >10.00 (n = 7)
Example 11
Study of Particular Components of Concentrated BSB Filtrate as
Mortar Admixture
[0151] In order to determine if a few of the high concentration
ingredients found in O2-002 were mostly responsible for the
activity seen in our applications testing, we tested both glycerol
and lactic acid individually for activity in our mortar and gypsum
assays. In the mortar assay, we matched the concentration of
glycerol and lactic acid (9.3% and 5.2%) respectively to that found
in O2-002. Results are shown in Table 12.
16TABLE 12 Dosage 0 drop 5 drop 10 drop set-time Admixture oz/100#
inches inches inches hours no admix control 0 4.0 5.9 6.8 2.3
glycerol 5 4.1 6.0 7.1 2.3 10 4.2 6.1 7.1 2.3 15 4.3 5.8 6.8 2.3
lactic acid 5 3.9 6.0 7.0 2.3 10 4.1 6.0 6.9 2.3 15 4.0 6.1 7.0 2.3
O2-002 5 5.1 6.7 7.7 3.3 10 5.2 6.8 7.8 4.2 15 5.9 7.2 8.3 5.0
[0152] The results show that individually, the glycerol and the
lactic acid have virtually no response difference from the "no
admix" control. The effect of the O2-002 in this study was
pronounced, and as expected.
Example 12
Pilot Scale Study of Concentrated BSB Filtrate and Particular
Components Thereof as an Admixture in Gypsum Panel Production
[0153] A separate study in our gypsum assay is shown below,
following procedures and using materials described below (Table
13):
17TABLE 13 inclusion patty diameter set-time Admixture % inches
minutes no admix control 0.0 3.8 4.48 BSB "as is" 0.6 3.6 4.33 1.2
3.7 4.58 BSB retentate 0.6 3.3 4.33 1.2 3.1 4.83 O2-002 (BSB
permeate) 0.3 4.3 4.88 0.6 4.5 6.44 1.2 4.6 >10.00 glycerol 0.3
4.3 4.83 0.6 4.2 4.58 1.2 4.1 4.33 lactic acid (50%) 0.3 4.3 4.83
0.6 4.2 5.58 1.2 4.4 7.3
[0154] In this study, we tested 50% stock solutions of BSB
retentate (yeast fraction), glycerol, and lactic acid, in addition
to BSB "as is" directly from the fermentor. We also used our O2-002
preparation (35% solids). The BSB "as is" results were not
significantly different from control, while the BSB retentate
results showed a decrease in flow. Glycerol showed an increase in
flow compared to control but may have shown an accelerated set at
higher dose. Lactic acid paralleled the results seen with O2-002
fairly closely, but it was tested at ten times the level at which
it was found in O2-002 (50% vs. 5%).
[0155] All of the compositions and methods disclosed and claimed
herein can be made and executed without undue experimentation in
light of the present disclosure. While the compositions and methods
of this invention have been described in terms of preferred
embodiments, it will be apparent to those of skill in the art that
variations may be applied to the compositions and methods and in
the steps or in the sequence of steps of the methods described
herein without departing from the concept, spirit and scope of the
invention as defined by the appended claims.
* * * * *