Note: Descriptions are shown in the official language in which they were submitted.
POTASSIUM HUMATE SULFUR COMPOUND GRANULE
FIELD OF THE INVENTION
100011 A process such as is described in various embodiments herein
relates to
making a humic acid sulfur compound granule. Such a compound granule is useful
as an
organic aid to crop growth as well as useful for overcoming a plethora of soil
problems.
BACKGROUND OF THE INVENTION
[0002] Extraction of humic acid and related materials from
carbonaceous raw
materials such as humalite, leonardite, sub-bituminous coal, menefee, peat,
and the like has
been practiced for years and is accordingly known in the art. Process steps
vary, but the
process output is generally a particulate material with suboptimal solubility
in water.
[0003] It is known that humic substances (HS) include fulvic acid,
humic acid,
and/or humin. Of these, fulvic acid has the lowest molecular weight and least
resistance to
decomposition by microorganisms; humin has the highest molecular weight and
greatest
resistance to decomposition, because it has a large number of negative charges
per unit
mass, humin also has a very high CEC. The large molecules of humus bind to
clay particles
and greatly increase aggregate formation and stability therefore improving
soil properties.
Humin is the alkali (and acid) insoluble portion of HS that many manufacturers
dispose of,
although it is known that there are individuals who may extract and use it.
[0004] Since it takes longer for dry lignite to be broken down, and
thus be functional
in the soil, it is necessary to convert the lignite into forms that provide a
more timely overall
benefit (e.g. transformation into a water-soluble form). Such a conversion
"unrolls" the
tight molecular ball of lignite and creates water-soluble humic acids, either
as a liquid or in
the form of sodium, potassium, or ammonium salts (known as humates). Such a
water-
soluble form is desirable, as in their soluble form, humic acids can readily
chelate nutrients,
preserve nitrates from leaching, enhance root development, and improve overall
crop vigor
and yields.
-1-
CA 3070820 2020-02-04
[0005] In addition to the desirability of a fully water-soluble humic
acid composition
various soil and tissue analyses have indicated a lack of ample sulfur exists
in many
agricultural soils. This lack of available sulfur combined with nitrogen to
sulfur ratios
influence crop yield and quality. Sulfur plays a distinctive and visible role
in protein
synthesis, producing amino acids, enzymes, and vitamins. Sulfur also helps
soils fortify
plant resistance to disease. Therefore, it may be desirable to combine fully-
water soluble
humic acid (i.e. humates) and sulfur into a granule for application to soil.
The combinatorial
chemistry of the fully soluble humic acid (i.e. humate) and sulfur may serve
as a catalyst for
the production of sulfates and sulfuric acids and construct a sulfur reserve
within the soil.
SUMMARY OF EMBODIMENTS
[0006] The present embodiments provide one or more of the features
recited in the
appended claims and/or the following features which alone or in combination,
may comprise
patentable subject matter.
[0007] In a first aspect, a process for making a potassium humate
sulfur compound
granule is described. The process including: obtaining a sample of a
carbonaceous
substance comprising humic acid and one or more other substances; contacting
the sample
with an amount of an alkaline mixture, forming an extraction mixture, the
extraction mixture
consisting essentially of a sludge component, the sludge component including,
predominantly, the sample, and an extraction component, the extraction
component
including, predominantly, the alkaline mixture; maintaining the sludge
component in contact
with the extraction component for a period of time sufficient for the
extraction component to
become relatively enriched in humic acid and the sludge component to become
relatively
depleted of humic acid; separating the sludge component from the extraction
component;
spray drying the extraction component, forming a plurality of potassium humate
powder
particles; adding the plurality of potassium humate particles to elemental
sulfur, forming a
homogenized mixture; and solidifying at least a portion of the homogenized
mixture under
conditions where the at least a portion of the homogenized mixture is made
into a form of a
granule; thereby making a potassium humate sulfur compound granule.
-2-
CA 3070820 2020-02-04
[0008] In some embodiments, the elemental sulfur is a molten sulfur.
In some
embodiments, the homogenized mixture includes about 1 pound to about 200
pounds of the
plurality of potassium humate powder particles per one ton (2000 pounds) of
elemental
sulfur. In other embodiments, the homogenized mixture includes about 100
pounds of the
plurality of potassium humate powder particles per one ton of elemental
sulfur. In still other
embodiments, the plurality of potassium humate powder particles comprises
about 5% of the
homogenous mixture.
[0009] In some embodiments, the potassium humate sulfur compound
granule has a
pH of at least 7.5. In other embodiments, the potassium humate sulfur compound
granule
has a pH of 7.5 to about 12. In still other embodiments, the potassium humate
sulfur
compound granule has a pH of about 9.
[0010] In some embodiments, the homogenized mixture further includes
bentonite
clay as a binder. In such instances, the bentonite clay may comprise about 10%
of the
homogenized mixture.
[0011] In some embodiments, the solidifying step further includes
pumping the
homogenized mixture through a rotoformer or drop former and onto a flat
surface (e.g. a
conveyor belt, or the like) and cooling the homogenized mixture on the flat
surface.
[0012] In another aspect a process for making a potassium humate
sulfur compound
granule is disclosed, where the process includes: obtaining a sample of a
carbonaceous
substance comprising humic acid and one or more other substances; contacting
the sample
with an amount of an alkaline mixture, forming an extraction mixture, the
extraction mixture
consisting essentially of a sludge component, the sludge component comprising,
predominantly, the sample, and an extraction component, the extraction
component
comprising, predominantly, the alkaline mixture; maintaining the sludge
component in
contact with the extraction component for a period of time sufficient for the
extraction
component to become relatively enriched in humic acid and the sludge component
to
become relatively depleted of humic acid; separating the sludge component from
the
extraction component; spray drying the extraction component, forming a
plurality of powder
potassium humate particles; adding the plurality of potassium humate particles
to elemental
sulfur, forming a homogenized mixture, where the plurality of potassium humate
powder
-3-
CA 3070820 2020-02-04
particles comprises about 5% of the homogenized mixture; and solidifying at
least a portion
of the homogenized mixture under conditions where the at least a portion of
the
homogenized mixture is made into a form of a granule; thereby making a
potassium humate
sulfur compound granule with a potassium humate component and a sulfur
component,
where the potassium humate sulfur compound granule has a pH of 7.5 to about
12, and
where the potassium humate component of the granule solubilizes upon
application to a
desired site and enhances conversion of the sulfur component into sulfate.
[0013] In some embodiments, the potassium humate sulfur compound
granule has a
pH of about 9. In some embodiments, the homogenized mixture further includes
bentonite
clay as a binder. In such embodiments, the bentonite clay may comprise about
10% of the
homogenized mixture.
[0014] In some embodiments, the solidifying step further includes
pumping the
homogenized mixture through a rotoformer and onto a flat surface and cooling
the
homogenized mixture on the flat surface.
[0015] In another aspect, a potassium humate sulfur compound granule
is disclosed,
where the granule includes: a potassium humate component and an elemental
sulfur
component at a ratio of about 1:20; where the potassium humate sulfur compound
granule is
semi-soluble, where the potassium humate component of the granule fully
solubilizes upon
application to a desired site and enhances conversion of the sulfur component
into sulfate by
at least about 15% as compared to elemental sulfur alone; and where the
potassium humate
sulfur compound granule has a pH of 7.5 to about 12.
[0016] In some embodiments, the granule has a pH of about 9. In some
embodiments, the granule enhances conversion of the sulfur component into
sulfate by at
least 50% as compared to elemental sulfur alone. In some embodiments, the
granule further
includes bentonite clay component as a binder.
DETAILED DESCRIPTION
[0017] A process and composition such as is described in various
embodiments
herein now will be described more fully hereinafter. A process such as is
described in
various embodiments herein may, however, be embodied in many different forms
and
-4-
CA 3070820 2020-02-04
should not be construed as limited to the embodiments set forth herein;
rather, these
embodiments are provided so that this disclosure will be thorough and
complete, and will
fully convey the scope of a process such as is described in various
embodiments herein to
those skilled in the art. As used in this specification and the claims, the
singular forms "a,"
"an," and "the" include plural referents unless the context clearly dictates
otherwise. When
used in this specification and the claims as an adverb rather than a
preposition, "about"
means "approximately" and comprises the stated value and every value within
10% of that
value; in other words, "about 100%" includes 90% and 110% and every value in
between.
[00181 When used in this specification and the claims, a product is
"enriched in
humic acid" if the product possesses a higher concentration of humic acid than
a raw
material from which the product is made. A component becomes "enriched in
humic acid"
as the concentration of humic acid in the component increases. A component
becomes
"depleted of humic acid" as the concentration of humic acid in the component
decreases.
100191 When used in this specification and the claims, a "carbonaceous
substance
comprising humic acid and one or more other substances" refers to a
carbonaceous
substance that contains humic acid and that also contains one or more other
substances other
than humic acid. An example is Humalite. An example is lignite. An example is
Leonardite.
100201 When used in this specification and the claims, "humate" refers
to a fully-
water soluble humic acid composition in the form of a salt. For example
"potassium
humate" is a fully-water soluble potassium salt of humic acid, "ammonium
humate" is a
fully-water soluble ammonium salt of humic acid, and so on.
100211 Aspects of a process such as is described in various
embodiments herein are
further illustrated by the following examples, which are set forth to
illustrate certain aspects
of a process such as is described in various embodiments herein and are not to
be construed
as limiting thereof.
100221 In an example, production of a potassium humate sulfur compound
granule
was undertaken as a multi-step process. This process includes blending of raw
material and
an alkaline mixture in a blend tank; screening of the blended mixture that was
made in the
blend tank; drying of the liquid derived from screening of the blended
mixture, thereby
-5-
CA 3070820 2020-02-04
forming a fine potassium humate powder; adding the fine powder to molten
sulfur, forming
a homogenized mixture; and solidifying of the homogenized mixture to form
potassium
humate sulfur compound granules.
[0023] In an example, a blending of raw material with an alkaline
mixture in a blend
tank resulted in extraction of humic acid and other humic substances from the
raw material.
Hot water and caustic potash solution and Humalite were added to a thermally
insulated tank
in that order and blended. The hot water was at 160-180 degrees Fahrenheit.
The caustic
potash solution was 45% membrane grade. The mass ratio of hot water to caustic
potash
solution to Humalite was 73.7:5.8:20.5.
[0024] In an example, water, caustic potash solution and Humalite were
placed into
a thermally insulated tank to form a 42,000 lb mixture, which was then
blended. The liquid
phase was sampled, and a colorimetric assay for humic acid was performed on
each sample,
in which the amount of light absorbed was proportional to the concentration of
humic acid.
[0025] In an example, a blended mixture prepared according to the
paragraph
immediately above consisted of liquid and sludge. This blended mixture was
then pumped
by a 3 HP motor to two 200 mesh screeners at a rate of ¨40 gal/min (-350
lbs/min). It took
¨120 minutes to screen 42000 lbs. The screener allowed liquids and very small
particles to
be passed through, but not the insoluble sand, clay, and humin fraction, also
known as
sludge. The amount of sludge varied, but typically the sludge was about 5-7%
of the total
weight of the blended mixture.
[0026] In an example, the screened humic acid enriched liquid, which
had a density
of 8.35-9 lb/gallon, was collected in an insulation tank, which had a capacity
of 12500 gal.
The humic acid enriched liquid was pumped from the insulation tank to a spray
dryer firing
tank from which it was transferred to a spray dryer.
[0027] In an example, a spray dryer system comprised a burner, a
dryer, two cyclone
separators, a baghouse and a powder hopper. Humic acid enriched liquid was
processed at a
rate of 14-16 gal/min. Hydraulic pressure-nozzle atomization was used in which
liquid was
passed through a filter and then through a hydraulic pressure pump. The
pressure of the
liquid was directly proportional to the force delivered by the hydraulic
pressure pump and
was generally 1500 psi but ranged from 1300-1700 psi depending on the moisture
of the fine
-6-
CA 3070820 2020-02-04
powder. The humic acid enriched liquid was then forced through 8 nozzles to
break the
liquid into fine droplets. Filtered air was passed through a burner where it
was heated to
600-650 degrees Fahrenheit. The temperature of the inlet air never exceeded
800 degrees
Fahrenheit. The hot air met the liquid droplets in a co-current manner for a
time of about 2
seconds. This time was enough to remove more than 85% of the moisture from the
dryer to
form a humic acid enriched powder, which was collected in a common line. The
air
emerging out of the dryer still had some particles and was generally at 190-
205 degrees
Fahrenheit and never exceeded 250 degrees Fahrenheit. Heavier particles were
collected
using two cyclone separators in series and the lighter particles were
collected using a
baghouse filter. The hot gas, also called flue gas, was then emitted from the
bag house; the
hot gas consisted mostly of air and steam at 150-180 degrees Fahrenheit. The
temperature
of the exhaust never exceeded 250 degrees Fahrenheit. The potassium humate or
humic acid
enriched powder from the common line was then transferred to a powder hopper.
Moisture
content of the powder was measured and kept between 11%-13%. When the moisture
was
below 11%, moisture content was increased in either of two ways, by reducing
the
temperature of the burner or by operating the hydraulic pressure pump at a
higher capacity
which in turn increased the flow rate of the liquid. When the moisture was
above 13%,
moisture content was decreased in either of two ways, by increasing the
temperature of the
burner or by operating the hydraulic pressure pump at a lower capacity which
in turn
decreased the flow rate of the liquid. The loose bulk density of the potassium
humate
powder ranged from about 35 to about 42 pounds per cubic foot. The feed
particle size
distribution of a typical powder sample was as follows: 1.5% of the particles
by weight
were less than 100 microns; 15% of the particles by weight were less than 200
microns; 35%
of the particles by weight were less than 270 microns; 55% of the particles by
weight were
less than 400 microns.
[0028] The fine 100% soluble potassium humate powder may be combined
with
elemental sulfur to form the potassium humate sulfur compound granule. In an
example, the
potassium humate sulfur compound granule may be manufactured using a batch or
a
continuous flow method depending on the manufacturing set up and/or product
demand
needs. The elemental sulfur, may in some instances, be in a molten form. In
some
-7-
CA 3070820 2020-02-04
instances, a non-molten sulfur may desired be heated until in a molten state.
The molten
sulfur is transported into a mixing tank, for example, by pumping and
metering. Inside the
mixing tank the potassium humate powder is added to the molten sulfur. In some
embodiments, a bentonite clay may also be added as a binder. The mixture is
continuously
mixed, for example by stirring or blending, until the molten sulfur, potassium
humate, and
bentonite clay (if present) form one substantially homogenous mixture. The
mixing tank
and/or sulfur contained therein may be heated in order to maintain the sulfur
in a molten
state (e.g. above the melting temperature of sulfur ¨ 270 degrees Fahrenheit).
Once
homogenized, the molten mixture is moved from the mixing tank through a filter
and
pumped through a rotoformer and onto flat surface (e.g. a conveyor belt or the
like), where
the mixture may be generally pea-shaped and/or be in shape of a granule. Once
on the flat
surface, the mixture is cooled, forming solid potassium humate granules.
100291 Resulting granules have been found to aid plant growth in both
agricultural
and horticultural applications. Various soil bacteria may convert the inert
and insoluble
elemental sulfur present in the granule to sulfate, and in turn sulfuric acid.
For example, in
calcareous soils, this sulfuric acid may cause fixed calcium carbonates and
free lime to
release calcium in soil solution, while the potassium humate (soluble humic
acid) may alter
the rhizodeposition and plant roots. This may result in a metamorphosis of
overall root
architecture, provide more root hair, and translocate the exchangeable calcium
to the plant
roots and plant tissues. The potassium humate also may simultaneously buffer,
chelate, and
complex macro-micronutrients, making them more readily available to roots and
plants.
Furthermore, due to its nanoparticle size the potassium humate (soluble humic
acid) may
create micropores for roots, water, and nutrients to reside, which may become
oxygenated as
a result of the dynamics of soil physics. Traditionally, about 70% to about
90% of sulfur
present in soil is in the form of organic matter, which must be converted to
sulfate by soil
bacteria in order to be usable by plants. The combination of the potassium
humate (soluble
= humic and) sulfur may enhance the conversion of sulfur to sulfate,
resulting in a conversion
rate from about 15% to about 70%. The conversation rate may be contingent upon
dynamics such as soil temperature, moisture, and/or presence of autotropic
bacteria. In
another example, where the soil is sandy, irrigated, or has high rainfall
amounts, the slow
-8-
CA 3070820 2020-02-04
release of sulfur may create sulfate for immediate plant use (approximately
30%), while the
remainder of the sulfur is activated to create sulfates and sulfuric acids in
a long lasting
manner with minimal leaching, which may ensure further sulfate formation at
various stages
of plant growth.
[0030] In an example, the application of postasium humate sulfur
compound
granules in conjunction with the nitrogen may enhance nitrogen to sulfur
ratios in crops
where the protein requirements are high. Such enhancement may be attributable
to the
creation of desirable soil texture and structure by the organosulfur complexes
created by the
application of the postasium humate sulfur compound granules to the soil. For
example, the
organosulfur complexes may loosen soil in tied clay soils creating adequate
drainage,
suitable aeration, and buffering properties. The creation of these
organosulfur complexes
may also result in, through various chemical pathways and the labyrinthine
network of
microorganisms, the decomposition of high molecular weight of organic
materials, which
may create up to 5,000 calories per gram of energy available for plant use.
[0031] Aspects of a process such as is described in various
embodiments herein are
further illustrated by the following further examples, which are set forth to
illustrate certain
aspects of a process such as is described in various embodiments herein and
are not to be
construed as limiting thereof.
[0032] Further example 1. A process for making a potassium humate
sulfur
compound granule, the process comprising:
obtaining a sample of a carbonaceous substance comprising humic acid and one
or more other substances;
contacting the sample with an amount of an alkaline mixture, thereby forming
an
extraction mixture, the extraction mixture consisting essentially of a sludge
component, the sludge component comprising, predominantly, the sample, and an
extraction component, the extraction component comprising, predominantly, the
alkaline mixture;
maintaining the sludge component in contact with the extraction component for
a
period of time sufficient for the extraction component to become relatively
enriched
-9-
CA 3070820 2020-02-04
in humic acid and the sludge component to become relatively depleted of humic
acid;
separating the sludge component from the extraction component;
spray drying the extraction component, thereby forming a plurality of powder
particles;
adding the plurality of potassium humate particles to elemental sulfur,
thereby
forming a homogenized mixture; and
solidifying at least a portion of the homogenized mixture under conditions
wherein the at least a portion of the homogenized mixture is made into a form
of a
granule;
[0033] thereby making a potassium humate sulfur compound granule.
[0034] Further example 2. A process according to further example 1,
wherein the
carbonaceous substance comprises a coal and/or a claystone and/or a mudstone
and/or a
shale.
[0035] Further example 3. A process according to further example 1,
wherein the
carbonaceous substance comprises a lignite and/or a Leonardite and/or a
Humalite.
[0036] Further example 4. A process according to further example 1,
wherein the
carbonaceous substance comprises a Humalite.
[0037] Further example 5. A process according to further example 1,
wherein the
alkaline mixture comprises water.
[0038] Further example 6. A process according to further example 1,
wherein the
alkaline mixture comprises a base.
[0039] Further example 7. A process according to further example 1,
wherein the
alkaline mixture comprises sodium hydroxide or potassium hydroxide.
[0040] Further example 8. A process according to further example 1,
wherein the
alkaline mixture comprises caustic potash solution.
[0041] Further example 9. A process according to further example 1,
wherein the
alkaline mixture comprises, by mass, between about 10 and about 15 parts
water, and about
1 part caustic potash solution, wherein the caustic potash solution is 45%
membrane grade.
-10-
CA 3070820 2020-02-04
[0042] Further example 10. A process according to further example 1,
wherein the
alkaline mixture comprises, by mass, about 73.7 parts water and about 5.8
parts caustic
potash solution, wherein the caustic potash solution is 45% membrane grade.
[0043] Further example 11. A process according to further example 1,
wherein the
mass ratio of the alkaline mixture to the sample is between about 75:25 and
about 84:16.
[0044] Further example 12. A process according to further example 1,
wherein the
mass ratio of the alkaline mixture to the sample is between about 78:22 and
about 81:13.
[0045] Further example 13. A process according to further example 1,
wherein the
mass ratio of the alkaline mixture to the sample is about 79.5:20.5.
[0046] Further example 14. A process according to further example 1,
wherein the
sludge component is maintained in contact with the extraction component for
between about
4 hours and about 12 hours.
[0047] Further example 15. A process according to further example 1,
wherein the
sludge component is maintained in contact with the extraction component for
between about
6 hours and about 10 hours.
[0048] Further example 16. A process according to further example 1,
wherein the
sludge component is maintained in contact with the extraction component for
about 8 hours.
[0049] Further example 17. A process according to further example 1,
wherein the
sludge component is maintained in contact with the extraction component for a
period of
time sufficient for the extraction component to possess a humic acid content
of at least about
6%.
[0050] Further example 18. A process according to further example 1,
wherein the
sludge component is maintained in contact with the extraction component for a
period of
time sufficient for the extraction component to possess a humic acid content
of at least about
14%.
[0051] Further example 19. A process according to further example 1,
wherein the
sludge component is maintained in contact with the extraction component for a
period of
time sufficient for the extraction component to possess a humic acid content
of at least about
17%.
-11-
CA 3070820 2020-02-04
[0052] Further example 20. A process according to further example 1,
wherein the
sludge component is maintained in contact with the extraction component for a
period of
time sufficient for the extraction component to possess a humic acid content
of at least about
18%.
[0053] Further example 21. A process according to further example 1,
wherein the
separating is effected by filtration.
[0054] Further example 22. A process according to further example 1,
wherein the
separating is effected by sedimentation.
[0055] Further example 23. A process according to further example 1,
wherein the
drying is effected by spray drying.
[0056] Further example 24. A process according to further example 1,
wherein the
drying is effected by spray drying, and wherein the spray drying is
characterized by an inlet
temperature and an outlet temperature, and wherein the inlet temperature
passing through a
burner heats to between about 400 degrees Fahrenheit and about 800 degrees
Fahrenheit,
and wherein the outlet temperature is between bout 150 degrees Fahrenheit and
about 250
degrees Fahrenheit.
[0057] Further example 25. A process according to further example 1,
wherein the
drying is effected by spray drying, and wherein the spray drying is
characterized by an inlet
temperature and an outlet temperature, and wherein the inlet temperature is
between about
600 degrees Fahrenheit and about 650 degrees Fahrenheit, and wherein the
outlet
temperature is between about 150 degrees Fahrenheit and about 180 degrees
Fahrenheit.
[0058] Further example 26. A process according to further example 1,
wherein the
plurality of powder particles is characterized by a moisture content, and
wherein the
moisture content is between about 9% and about 15%.
[0059] Further example 27. A process according to further example 1,
wherein the
plurality of powder particles is characterized by a moisture content, and
wherein the
moisture content is between about 10% and about 14%.
[0060] Further example 28. A process according to further example 1,
wherein the
plurality of powder particles is characterized by a moisture content, and
wherein the
moisture content is between about 11% and about 13%.
-12-
CA 3070820 2020-02-04
[0061] Further example 29. A process according to further example 1,
wherein the
plurality of powder particles is characterized by a loose bulk density, and
wherein the loose
bulk density is between about 28 and about 49 pounds per cubic foot.
[0062] Further example 30. A process according to further example 1,
wherein the
plurality of powder particles is characterized by a loose bulk density, and
wherein the loose
bulk density is between about 31.5 and about 45.5 pounds per cubic foot.
[0063] Further example 31. A process according to further example 1,
wherein the
plurality of powder particles is characterized by a loose bulk density, and
wherein the loose
bulk density is between about 35 and about 42 pounds per cubic foot.
[0064] Further example 32. A process according to further example 1,
wherein the
plurality of powder particles is characterized by a particle size
distribution, and wherein, in
the particle size distribution, about 1.5% of the particles by weight are less
than about 100
microns, about 15% of the particles by weight are less than about 200 microns,
about 35%
of the particles by weight are less than 270 microns, and about 55% of the
particles by
weight are less than about 400 microns.
[0065] Further example 33. A process according to further example 1,
wherein the
sulfur is a molten state ranging from about 230 degrees Fahrenheit to about
280 degrees
Fahrenheit.
[0066] Further example 34. A process according to further example 1,
wherein the
sulfur is in a solid state and heated to a range of about 230 degrees
Fahrenheit to about 280
degrees Fahrenheit prior to the addition of the plurality of potassium humate
particles.
[0067] Further example 35. A process according to further example 1,
wherein the
homogenized mixture includes about 1 pound to about 200 pounds of the
plurality of
potassium humate powder particles per one ton (2000 pounds) of elemental
sulfur.
[0068] Further example 36. A process according to further example 1,
wherein the
homogenized mixture includes about 100 pounds of the plurality of potassium
humate
powder particles per one ton (2000 pounds) of elemental sulfur.
[0069] Further example 37. A process according to further example 1,
wherein the
homogenized mixture includes about 5% potassium humate.
-13-
CA 3070820 2020-02-04
[0070] Further example 38. A process according to further example 1,
wherein the
homogenized mixture further includes a binder, such as bentonite clay.
[0071] Further example 39. A process according to further example 39,
wherein the
bentonite clay may be about 5% to about 15% of the homogenized mixture.
[0072] Further example 40. A process according to further example 39,
wherein the
bentonite clay comprises about 10% of the homogenous mixture.
[0073] Further example 41. A process according to further example 1,
wherein the
homogenized mixture is mixed for up to 10 hours.
[0074] Further example 42. A process according to further example 1,
wherein the
homogenized mixture is mixed for up to five hours.
[0075] Further example 43. A process according to further example 1,
wherein the
homogenized mixture is mixed for up to one hour.
[0076] Further example 44. A process according to further example 1,
wherein the
solidifying is effected by an apparatus comprising a filter, rotoformer or
drop former, and
flat surface (e.g. conveyor belt).
[0077] Further example 45. A process according to further example 44,
wherein the
filter size may be a 140 mesh filter, a 230 mesh filter, a 270 mesh filter, a
325 mesh filter, or
a 400 mesh filter.
[0078] Further example 46. A process according to further example 44,
wherein the
flat surface is a steel belt.
[0079] Further example 47. A process according to further example 44,
wherein the
solidifying further includes cooling the mixture on the flat surface.
[0080] Further example 48. A process according to further example 47,
wherein the
cooling is effectuated by spraying a cooled liquid solution (e.g., 40 to 50
degrees
Fahrenheit), for example water, on the underside of the steel belt, resulting
in the cooling of
the belt and subsequently the homogenized mixture deposited thereon.
[0081] Further example 49. A process according to further example 47,
wherein the
cooling is effectuated by moving the belt into, or through, a chiller. In some
instances, such
a chiller may be set to about 40 to 50 degrees Fahrenheit, although this is
not to be
understood as limiting.
-14-
CA 3070820 2020-02-04
[0082] Further example 50. A process according to further example 47,
wherein the
cooling may be any other active means of cooling known in the art, such as
other forms of
refrigeration.
[0083] Further example 51. A process according to further example 47,
wherein the
cooling may be a passive means of cooling; for example the cooling may be
simply allowing
the mixture to cool to room temperature without any further intervention.
[0084] Further example 52. A process according to further example 1,
wherein the
potassium humate sulfur compound granule is between about 0.5 mm and about 4.5
mm.
[0085] Further example 53. A process according to further example 1,
wherein the
potassium humate sulfur compound granule is between about 0.8 mm and about 4.0
mm.
[0086] Further example 54. A process according to further example 1,
wherein the
potassium humate sulfur compound granule is between about 0.8 mm and about 2.0
mm.
[0087] Further example 55. A process according to further example 1,
wherein the
potassium humate sulfur compound granule is between about 2.1 mm and about 4.0
mm.
[0088] Further example 56. A process according to further example 1,
wherein the
potassium humate sulfur compound granule has a pH of at least 7.5.
[0089] Further example 57. A process according to further example 1,
wherein the
potassium humate sulfur compound granule has a pH of 7.5 to about 12.
[0090] Further example 58. A process according to further example 1,
wherein the
potassium humate sulfur compound granule has a pH of about 9.
[0091] Further example 59. A process according to further example 1,
wherein the
process further includes applying the potassium humate sulfur compound granule
to a
desired site, such as an agriculture setting.
[0092] Further example 60. A process according to further example 1,
wherein the
potassium humate sulfur compound granule has a potassium humate component and
a sulfur
component, and the potassium humate component of the granule solubilizes upon
application to a desired site and enhances conversion of the sulfur component
into sulfate.
[0093] Further example 61. A process according to further example 1,
wherein the
potassium humate sulfur compound granule enhances the conversion of sulfur to
sulfate by
about 15% to about 70% as compared to elemental sulfur alone.
-15-
CA 3070820 2020-02-04
[0094] Aspects of a potassium humate sulfur compound granule such as
is described
in various embodiments herein are further illustrated by the following further
examples,
which are set forth to illustrate certain aspects of a process such as is
described in various
embodiments herein and are not to be construed as limiting thereof.
[0095] Further example 62. A potassium humate sulfur compound granule,
the
granule made by a process comprising:
obtaining a sample of a carbonaceous substance comprising humic acid and one
or more other substances;
contacting the sample with an amount of an alkaline mixture, thereby forming
an
extraction mixture, the extraction mixture consisting essentially of a sludge
component, the sludge component comprising, predominantly, the sample, and an
extraction component, the extraction component comprising, predominantly, the
alkaline mixture;
maintaining the sludge component in contact with the extraction component for
a
period of time sufficient for the extraction component to become relatively
enriched
in humic acid and the sludge component to become relatively depleted of humic
acid;
separating the sludge component from the extraction component;
spray drying the extraction component, thereby forming a plurality of powder
potassium humate particles;
adding the plurality of potassium humate particles to elemental sulfur,
thereby
forming a homogenized mixture, wherein the plurality of potassium humate
powder
particles comprises about 5% of the homogenized mixture; and
solidifying at least a portion of the homogenized mixture under conditions
wherein the at least a portion of the homogenized mixture is made into a form
of a
granule;
thereby making a potassium humate sulfur compound granule with a potassium
humate component and a sulfur component,
wherein the potassium humate sulfur compound granule has a pH of 7.5 to
about 12, and
-16-
CA 3070820 2020-02-04
wherein the potassium humate component of the granule solubilizes upon
application to a desired site and enhances conversion of the sulfur component
into sulfate.
[0096] Further example 63. A potassium humate sulfur compound granule
according to further example 62, wherein the carbonaceous substance comprises
a coal
and/or a claystone and/or a mudstone and/or a shale.
[0097] Further example 64. A potassium humate sulfur compound granule
according to further example 62, wherein the carbonaceous substance comprises
a lignite
and/or a Leonardite and/or a Humalite.
[0098] Further example 65. A potassium humate sulfur compound granule
according to further example 62 wherein the carbonaceous substance comprises a
Humalite.
[0099] Further example 66. A potassium humate sulfur compound granule
according to further example 62, wherein the alkaline mixture comprises water.
[0100] Further example 67. A potassium humate sulfur compound granule
according to further example 62, wherein the alkaline mixture comprises a
base.
[0101] Further example 68. A potassium humate sulfur compound granule
according to further example 62, wherein the alkaline mixture comprises sodium
hydroxide
or potassium hydroxide.
[0102] Further example 69. A potassium humate sulfur compound granule
according to further example 62, wherein the alkaline mixture comprises
caustic potash
solution.
[0103] Further example 70. A potassium humate sulfur compound granule
according to further example 62, wherein the alkaline mixture comprises, by
mass, between
about 10 and about 15 parts water, and about 1 part caustic potash solution,
wherein the
caustic potash solution is 45% membrane grade.
[0104] Further example 71. A potassium humate sulfur compound granule
according to further example 62, wherein the alkaline mixture comprises, by
mass, about
73.7 parts water and about 5.8 parts caustic potash solution, wherein the
caustic potash
solution is 45% membrane grade.
-17-
CA 3070820 2020-02-04
[0105] Further example 72. A potassium humate sulfur compound granule
according to further example 62, wherein the mass ratio of the alkaline
mixture to the
sample is between about 75:25 and about 84:16.
[0106] Further example 73. A potassium humate sulfur compound granule
according to further example 62, wherein the mass ratio of the alkaline
mixture to the
sample is between about 78:22 and about 81:13.
[0107] Further example 74. A potassium humate sulfur compound granule
according to further example 62, wherein the mass ratio of the alkaline
mixture to the
sample is about 79.5:20.5.
[0108] Further example 75. A potassium humate sulfur compound granule
according to further example 62, wherein the sludge component is maintained in
contact
with the extraction component for between about 4 hours and about 12 hours.
[0109] Further example 76. A potassium humate sulfur compound granule
according to further example 62, wherein the sludge component is maintained in
contact
with the extraction component for between about 6 hours and about 10 hours.
[0110] Further example 77. A potassium humate sulfur compound granule
according to further example 62, wherein the sludge component is maintained in
contact
with the extraction component for about 8 hours.
[0111] Further example 78. A potassium humate sulfur compound granule
according to further example 62, wherein the sludge component is maintained in
contact
with the extraction component for a period of time sufficient for the
extraction component to
possess a humic acid content of at least about 6%.
[0112] Further example 79. A potassium humate sulfur compound granule
according to further example 62, wherein the sludge component is maintained in
contact
with the extraction component for a period of time sufficient for the
extraction component to
possess a humic acid content of at least about 14%.
[0113] Further example 80. A potassium humate sulfur compound granule
according to further example 62, wherein the sludge component is maintained in
contact
with the extraction component for a period of time sufficient for the
extraction component to
possess a humic acid content of at least about 17%.
-18-
CA 3070820 2020-02-04
[0114] Further example 81. A potassium humate sulfur compound granule
according to further example 62, wherein the sludge component is maintained in
contact
with the extraction component for a period of time sufficient for the
extraction component to
possess a humic acid content of at least about 18%.
[0115] Further example 82. A potassium humate sulfur compound granule
according to further example 62, wherein the separating is effected by
filtration.
[0116] Further example 83. A potassium humate sulfur compound granule
according to further example 62, wherein the separating is effected by
sedimentation.
[0117] Further example 84. A potassium humate sulfur compound granule
according to further example 62, wherein the drying is effected by spray
drying.
[0118] Further example 85. A potassium humate sulfur compound granule
according to further example 62, wherein the drying is effected by spray
drying, and
wherein the spray drying is characterized by an inlet temperature and an
outlet temperature,
and wherein the inlet temperature passing through a burner heats to between
about 400
degrees Fahrenheit and about 800 degrees Fahrenheit, and wherein the outlet
temperature is
between about 150 degrees Fahrenheit and about 250 degrees Fahrenheit.
[0119] Further example 86. A potassium humate sulfur compound granule
according to further example 62, wherein the drying is effected by spray
drying, and
wherein the spray drying is characterized by an inlet temperature and an
outlet temperature,
and wherein the inlet temperature is between about 600 degrees Fahrenheit and
about 650
degrees Fahrenheit, and wherein the outlet temperature is between about 150
degrees
Fahrenheit and about 180 degrees Fahrenheit.
[0120] Further example 87. A potassium humate sulfur compound granule
according to further example 62, wherein the plurality of powder particles is
characterized
by a moisture content, and wherein the moisture content is between about 9%
and about
15%.
[0121] Further example 88. A potassium humate sulfur compound granule
according to further example 62, wherein the plurality of powder particles is
characterized
by a moisture content, and wherein the moisture content is between about 10%
and about
14%.
-19-
CA 3070820 2020-02-04
[0122] Further example 89. A potassium humate sulfur compound granule
according to further example 62, wherein the plurality of powder particles is
characterized
by a moisture content, and wherein the moisture content is between about 11%
and about
13%.
[0123] Further example 90. A potassium humate sulfur compound granule
according to further example 62, wherein the plurality of powder particles is
characterized
by a loose bulk density, and wherein the loose bulk density is between about
28 and about
49 pounds per cubic foot.
[0124] Further example 91. A potassium humate sulfur compound granule
according to further example 62, wherein the plurality of powder particles is
characterized
by a loose bulk density, and wherein the loose bulk density is between about
31.5 and about
45.5 pounds per cubic foot.
[0125] Further example 92. A potassium humate sulfur compound granule
according to further example 62, wherein the plurality of powder particles is
characterized
by a loose bulk density, and wherein the loose bulk density is between about
35 and about
42 pounds per cubic foot.
[0126] Further example 93. A potassium humate sulfur compound granule
according to further example 62, wherein the plurality of humic acid enriched
powder
particles is characterized by a particle size distribution, and wherein, in
the particle size
distribution, about 1.5% of the particles by weight are less than about 100
microns, about
15% of the particles by weight are less than about 200 microns, about 35% of
the particles
by weight are less than 270 microns, and about 55% of the particles by weight
are less than
about 400 microns.
[0127] Further example 94. A potassium humate sulfur compound granule
according to further example 62, wherein the sulfur is a molten state ranging
from about 230
degrees Fahrenheit to about 280 degrees Fahrenheit.
[0128] Further example 95. A potassium humate sulfur compound granule
according to further example 62, wherein the sulfur is in a solid state and
heated to a range
of about 230 degrees Fahrenheit to about 280 degrees Fahrenheit prior to the
addition of the
plurality of potassium humate particles.
-20-
CA 3070820 2020-02-04
[0129] Further example 96. A potassium humate sulfur compound granule
according to further example 62, wherein the homogenized mixture includes
about 1 pound
to about 200 pounds of the plurality of potassium humate powder particles per
one ton (2000
pounds) of elemental sulfur.
[0130] Further example 97. A potassium humate sulfur compound granule
according to further example 62, wherein the homogenized mixture includes
about 100
pounds of the plurality of potassium humate powder particles per one ton (2000
pounds) of
elemental sulfur.
[0131] Further example 98. A potassium humate sulfur compound granule
according to further example 62, wherein the homogenized mixture further
includes a
binder, such as bentonite clay.
[0132] Further example 99. A potassium humate sulfur compound granule
according to further example 98, wherein the bentonite clay comprises about 5%
to about
15% of the homogenized mixture.
[0133] Further example 100. A potassium humate sulfur compound granule
according to further example 98, wherein the bentonite clay is about 10% of
the
homogenized mixture.
[0134] Further example 101. A potassium humate sulfur compound granule
according to further example 62, wherein the homogenized mixture is mixed for
up to 10
hours.
[0135] Further example 102. A potassium humate sulfur compound granule
according to further example 62, wherein the homogenized mixture is mixed for
up to five
hours.
[0136] Further example 103. A potassium humate sulfur compound granule
according to further example 62, wherein the homogenized mixture is mixed for
up to one
hour.
[0137] Further example 104. A potassium humate sulfur compound granule
according to further example 62, wherein the solidifying is effected by an
apparatus
comprising a filter, rotoformer or drop former, and flat surface (e.g.
conveyor belt).
-21-
CA 3070820 2020-02-04
[0138] Further example 105. A potassium humate sulfur compound granule
according to further example 104, wherein the filter size may be a 140 mesh
filter, a 230
mesh filter, a 270 mesh filter, a 325 mesh filter, or a 400 mesh filter.
[0139] Further example 106. A potassium humate sulfur compound granule
according to further example 104, wherein the flat surface is a steel belt.
[0140] Further example 107. A potassium humate sulfur compound granule
according to further example 62, wherein the solidifying further includes
cooling the
mixture on the flat surface.
[0141] Further example 108. A potassium humate sulfur compound granule
according to further example 107, wherein the cooling is effectuated by
spraying a cooled
liquid solution, for example water, on the underside of the steel belt,
resulting in the cooling
of the belt and subsequently the homogenized mixture deposited thereon.
[0142] Further example 109. A potassium humate sulfur compound granule
according to further example 107, wherein the cooling is effectuated by moving
the belt
into, or through, a chiller.
[0143] Further example 110. A potassium humate sulfur compound granule
according to further example 107, wherein the cooling may be any other active
means of
cooling known in the art, such as other types of refrigeration.
[0144] Further example 111. A potassium humate sulfur compound granule
according to further example 107, wherein the cooling may be a passive means
of cooling;
for example the cooling may be simply allowing the mixture to cool to room
temperature
without any further intervention.
[0145] Further example 112. A potassium humate sulfur compound granule
according to further example 62, wherein the granule is between about 0.5 mm
and about
4.5 mm.
[0146] Further example 113. A potassium humate sulfur compound granule
according to further example 62, wherein the granule is between about 0.8 mm
and about
4.0 mm.
-22-
CA 3070820 2020-02-04
[0147] Further example 114. A potassium humate sulfur compound granule
according to further example 62, wherein the granule is between about 0.8 mm
and about
2.0 mm.
[0148] Further example 115. A potassium humate sulfur compound granule
according to further example 62, wherein the granule is between about 2.1 mm
and about
4.0 mm.
[0149] Further example 116. A potassium humate sulfur compound granule
according to further example 62, wherein the potassium humate sulfur compound
granule
has a pH of about 9.
[0150] Further example 117. A potassium humate sulfur compound granule
according to further example 62, wherein the potassium humate sulfur compound
granule is
applied to a desired site, such as agricultural soil.
[0151] Further example 118. A potassium humate sulfur compound granule
according to further example 62, wherein the potassium humate sulfur compound
granule
enhances the conversion of sulfur to sulfate by about 15% to about 70% as
compared to
elemental sulfur alone.
[0152] Aspects of a potassium humate sulfur compound granule such as
is described
in various embodiments herein are further illustrated by the following further
examples,
which are set forth to illustrate certain aspects of the granule such as is
described in various
embodiments herein and are not to be construed as limiting thereof
[0153] Further example 119. A potassium humate sulfur compound granule
comprising:
a potassium humate component and an elemental sulfur component at a ratio of
about 1:20;
where the potassium humate sulfur compound granule is semi-soluble,
wherein the potassium humate component of the granule fully solubilizes upon
application to a desired location and enhances conversion of the sulfur
component
into sulfate by at least about 15% as compared to elemental sulfur alone; and
wherein the potassium humate sulfur compound granule has a p1-1 of 7.5 to
about
12.
-23-
CA 3070820 2020-02-04
[0154] Further example 120. A potassium humate sulfur compound granule
according to further example 119, wherein the potassium humate sulfur compound
granule
has a pH of about 9.
[0155] Further example 121. A potassium humate sulfur compound granule
according to further example 119, wherein the potassium humate sulfur compound
granule
enhances conversion of the sulfur component into sulfate by at least 50% as
compared to
elemental sulfur alone.
[0156] Further example 122. A potassium humate sulfur compound granule
according to further example 119, wherein the potassium humate sulfur compound
granule
further includes a binding component.
[0157] Further example 123. A potassium humate sulfur compound granule
according to further example 119, wherein the binding component is bentonite
clay.
[0158] Further example 124. A potassium humate sulfur compound granule
according to further example 119, wherein the compound granule ranges from
about 0.5 mm
to 4.5 mm in diameter.
[0159] Further example 125. A potassium humate sulfur compound granule
according to further example 119, wherein the granule is between about 0.8 mm
and about
2.0 mm in diameter.
[0160] Further example 126. A potassium humate sulfur compound granule
according to further example 119, wherein the granule is between about 2.1 mm
and about
4.0 mm in diameter.
[0161] Further example 127. A potassium humate sulfur compound granule
according to further example 119, wherein the desired location is an
agricultural soil.
[0162] Many modifications and other embodiments of a process such as
is described
in various embodiments herein will come to mind to one skilled in the art to
which this
disclosed process pertains having the benefit of the teachings presented in
the foregoing
description. Therefore, it is to be understood that a process such as is
described in various
embodiments herein is not to be limited to the specific embodiments disclosed
and that
modifications and other embodiments are intended to be included within the
scope of the
-24-
CA 3070820 2020-02-04
appended claims. Although specific terms are employed herein, they are used in
a generic
and descriptive sense only and not for purposes of limitation.
-25-
CA 3070820 2020-02-04
