Title of Invention

PROCESS FOR MANUFACTURING ULTRA LOW CONSISTENCY α- AND ß- BLEND STUCCO

Abstract A process is disclosed for making a blend of alpha- and beta-stucco including a slurry calcination step to produce alpha calcium sulfate hemihydrate followed by a fluidized bed calcination step to produce beta calcium sulfate hemihydrate. The process starts with 50-75% gypsum-containing solids slurry, and then steam calcines the slurry in a first reactor to form partially calcined gypsum slurry which contains calcium sulfate dihydrate and alpha calcium sulfate hemihydrate. The partially calcined slurry is then dewatered. Then the filter cake is fed into a kettle to complete the calcination process by converting the calcium sulfate dihydrate of the filter cake material into beta calcium sulfate hemihydrate.
Full Text PROCESS FOR MANUFACTURING ULTRA LOW CONSISTENCY α-AND
β- BLEND STUCCO
FIELD OF THE INVENTION
[001 ] This invention relates to an improved method of making calcined gypsum
which results in an ultra-low consistency alpha- and beta- blend stucco. In
particular, the present invention provides a process which comprises a slurry
calcination step in a first reactor to produce alpha calcium sulfate hemihydrate
followed by a calcination step, for example a fluidized bed calcination step, in a
second reactor to produce beta calcium sulfate hemihydrate.
BACKGROUND OF THE INVENTION
[002] Gypsum calcium sulfate dihydrate, CaSO4-2H2O comes from a variety of
sources. Land plaster is a term for natural gypsum which is any mixture
containing more than 50% calcium sulfate dihydrate, CaS04.2H2O (by weight).
[003] Generally, gypsum-containing products are prepared by forming a mixture
of calcined gypsum phase (i.e., calcium sulfate hemihydrate and/or calcium
sulfate soluble anhydrite) and water, and, optionally, other components, as
desired. The mixture typically is cast into a pre-determined shape or onto the
surface of a substrate. The calcined gypsum reacts with the water to form a
matrix of crystalline hydrated gypsum, i.e., calcium sulfate dihydrate. It is the
desired hydration of calcined gypsum that enables the formation of an
interlocking matrix of set gypsum, thereby imparting strength to the gypsum
structure in the gypsum-containing product.
[004] Stucco is defined as chemically calcium sulfate hemihydrate and is a well-
known building material used to make building plasters and gypsum wallboard.
Stucco is typically made by crushing the gypsum rock with and then heating the
gypsum at atmospheric pressure to calcine (dehydrate) the calcium sulfate
dihydrate into calcium sulfate hemihydrate. In addition to natural gypsum rock
the use of Flue Gas Desulphurization gypsum or gypsum from chemical
processes can be used as well. Traditionally, the calcining of gypsum has

occurred in a large atmospheric pressure kettle containing a mixture of the
various phases of the gypsum
[005] US Patent No. 5,927,968 to Rowland et al., incorporated herein by
reference in its entirety, discloses its own method and apparatus for continuous
calcining of gypsum in a refractoryless atmospheric kettle. However, US Patent
No. 5,927,968 to Rowland et al. also discloses a variety of kettles for calcining
stucco. One such kettle has a thickened dome-shaped bottom, against which a
gas-fired flame is directed, with the kettle and burner flame being enclosed in a
suitable refractory structure. There is usually an associated hot pit into which the
calcined material is fed. The kettle must withstand temperatures in the 2,000 -
2,400 °F (1093 - 1314 °C) range. US Patent No. 5,927,968 to Rowland et al.
states US Patent No. 3,236,509 to Blair typifies this type construction.
[006] U.S. Pat. No. 3,236,509 to Blair, incorporated herein by reference,
discloses continuous fluidized kettle calcination in which dried mineral gypsum
powder is fed to a covered, but air vented and lightly vacuum exhausted,
calcination vessel. After a steady state of operation is attained in the vessel, a
substantially continuous stream of cold gypsum that has been pre-dried and
ground to a finely divided state and with a wide distribution of fragmented particle
sizes, is added on top of the fluidized, boiling mass in the kettle. Under such
conditions, the thermal shock upon the cold, dry mineral being dropped into the
already boiling mass radically fractures the ground gypsum rock fragments, and
the resultant stucco (beta hemihydrate) is highly fractured and fissured, as well
as being widely distributed in particle size. This causes the stucco to disperse
very rapidly in water, and requires high amounts of gauging water to be mixed
with the stucco for rehydration to gypsum at customary use consistencies.
[007] This "dispersed consistency", also known in the art as "consistency" or
"water demand", is an important property of stucco. Stuccos of lower
consistency generally result in stronger casts.
[008] The normal consistency of stucco (gypsum plaster) is a term of art and is
determinable according to ASTM Procedure C472, or its substantial equivalents.
It is defined as the amount of water in grams per 100 grams of stucco.

[009] US Patent No. 4,533,528 to Zaskalicky, incorporated herein by reference
in its entirety, discloses directly feeding wet chemical gypsum cake to a
continuous kettle calciner to produce beta hemihydrate of lower consistency. As
explained in Zaskalicky, and also for purposes of the present description,
"dispersed consistency" may be defined as the water volume required to give a
standard viscosity or flow when a standard amount by weight of stucco is
dispersed by mechanical mixing in a laboratory mixer at high shear intensity and
for a standard time to equal mixing encountered in the gypsum board forming
line, e.g., 7 seconds, or in an industrial plaster formulation casting mixer, e.g. 60
seconds.
[0010] For example, as explained in US Patent No. 4,201,595 to O'Neill,
incorporated herein by reference in its entirety, calcined gypsum made by
continuous calcination may have a dispersed consistency of about 100-150 cc.
"Dispersed consistency" for purposes of gypsum board manufacture may be
defined as the water volume required to give a standard viscosity or flow when
100 grams of stucco is dispersed by mechanical mixing in a laboratory high
speed blender at high shear intensity and for 7 seconds which is equivalent to
the mixing encountered in the board forming line. While the dispersed
consistency may be expressed in a particular numerical figure, it will be
appreciated that any particular number is variable from one process to the next
depending on the particular stucco and the rate of production.
[0011] Low consistency stucco is particularly advantageous in automated
gypsum board manufacture, in which a large portion of the processing time and
processing energy is devoted to removing excess water from the wet board.
Considerable excess water is required in gypsum board manufacture to properly
fluidize the calcined gypsum and obtain proper flow of the gypsum slurry.
[0012] A dispersed consistency value of 100-150 cc. indicates a water
requirement of about 85-100 parts of water per 100 parts of the calcined
gypsum for a typical slurry in a gypsum wallboard plant. The theoretical water
required to convert the calcined gypsum (calcium sulfate hemihydrate or stucco)

to set gypsum dihydrate is only 18.7% by weight on a pure basis. This leaves
about 67 to about 82% of the water present in the gypsum slurry to be removed
in drying the board. Ordinarily, gypsum board dryers in a gypsum board
manufacturing line will remove this water, for example, by maintaining the air
temperature at about 400 °F (204 °C) and requiring a drying time of about 40
minutes.
[0013] US Patent Nos. 4,201,595 (also mentioned above), 4,117,070 and
4,153,373 to O'Neill, all incorporated herein by reference in their entirety, teach
to lower the dispersed consistencies of continuously calcined kettle stuccos by
an after calcination treatment of the stucco with small amounts of water or
various aqueous solutions, resulting in a damp but dry appearing material and
allowing the small amounts of free water to remain on the calcined gypsum
particle surface for a short period of time, about 1-10 minutes for the treated
stucco to "heal".
[0014] U.S. Patent No. 3,410,655 to Ruter et al., incorporated herein by
reference in its entirety, teaches producing alpha calcium sulfate hemihydrate.
Ruter et al. states the alpha-hemihydrate forms non-needle like crystals, as
opposed to the beta calcium sulfate hemihydrate which forms needle-like
crystals. Ruter et al. also states the usual plaster of Paris (calcium sulfate
hemihydrate) is the beta calcium sulfate hemihydrate. However, depending on
the manner of preparation, the plaster of Paris still contains more or less
anhydrous calcium sulfate, and/or alpha calcium sulfate hemihydrate. Moreover,
plasters with definite alpha-hemihydrate content exhibit higher strengths. Ruter
et al. teaches to make alpha calcium sulfate hemihydrate in the form of non-
needle-like crystals by elutriating the dihydrate with water to remove organic
impurities and fine and slimy crystal portions, forming an aqueous suspension of
the dihydrate at a pH about 1.5-6, and subsequently heating under closely
controlled conditions.
[0015] US Patent No. 2,907,667 to Johnson, incorporated herein by reference in
its entirety, states alpha-hemihydrate is prepared by heating the dihydrate under

controlled vapor pressure conditions in the presence of steam or in an aqueous
solution.
US Patent No. 4,234345 to Fassle discloses fast-setting alpha calcium sulfate
hemihydrate made from calcium sulfate dihydrate by hydrothermally
recrystallizing calcium sulfate dihydrate to form a mixture containing 95%-99%
by weight alpha calcium sulfate hemihydrate and 5 to 1% calcium sulfate
dihydrate. The dihydrate in this mixture is then converted to beta calcium sulfate
hemihydrate by calcining, except for a remainder of up to 0.5 percent of
dihydrate, which remains in the mixture.
[0016] There is a need for stuccos having low consistency and good strength
characteristics.
SUMMARY OF THE INVENTION
[0017] It is an object of the invention to provide a process for making a stucco
composition comprising alpha calcium sulfate hemihydrate and beta calcium
sulfate hemihydrate.
[0018] The present process starts with 50-75 % gypsum-containing solids by
weight in aqueous slurry.
[0019] Direct injection of steam of a quality between 100 to 200 psig, into the
slurry in or prior to the first continuous stirred tank reactor, at 60 psig, converts
50 to 95% wt. % of the gypsum solids to alpha calcium sulfate hemihydrate.
This forms partially calcined gypsum slurry which contains calcium sulfate
dihydrate and alpha calcium sulfate hemihydrate. In particular, about 80-90% wt.
% or 70-85 wt. % of the gypsum is calcined to alpha calcium sulfate
hemihydrate. The partially calcined gypsum slurry is then dewatered, for
example in a Miter press to produce a filter cake of dewatered solids of 95 to 98
% solids. The filter cakes temperature is maintained above 170 °F (77 °C)
during the separation. Then the dewatered hot sotids are fed to an atmospheric
kettle to complete the calcination process by converting the calcium sulfate
dihydrate of the dewatered solids into beta calcium sulfate hemihydrate. The hot

water (recovered without significant cooling) is returned to the feed of the
process to minimize the energy used in the process. Alternately, the heat from
the water can be used along with the waste heat from the kettle process to
preheat the feed slurry of gypsum at the start of the process.
[0020] The present process for making a blend of alpha- and beta-stucco results
in near theoretical water demand for use in a board manufacturing process. The
theoretical amount of water to hydrate 100 % pure CSH (calcium sulfate
hemihydrate) to the gypsum form would be 21 parts of water to 100 parts of
CSH. This process results in a water demand down to 21 parts with a minimum
amount of dispersants or fluidizers required. Beta stucco alone has a water
demand up to 140 parts of water and requires a large amount of dispersant to
reach the flow characteristic of the alpha-beta blend stucco. Alternately a blend
of alpha and beta hemihydrate can be made using powders. The resulting
material requires more total energy if made by stand alone processes. Also, the
resulting material requires a higher percentage of alpha to beta to achieve the
same results. Therefore, the present invention provides a more economical
calcining method to produce the alpha-beta stucco.
[0021] The alpha hemihydrate aids in fluidity while the beta-hemihydrate aids in
reactivity. The process can also be energy efficient because it can recycle hot
water recovered from dewatering. Also, the solids are kept hot during
dewatering to ensure the material does not hydrate back to gypsum.
BRIEF DESCRIPTION OF THE DRAWING
[0022] FIG. 1 is a process flow diagram of an embodiment of the process of the
present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0023] FIG. 1 shows an embodiment of an apparatus for performing the process
of the present invention. Gypsum (calcium sulfate dihydrate) and water are
mixed in a mixer (not shown) to form a 50-75% solids gypsum slurry 10.
Gypsum slurry 10 is fed to a jacketed reactor 12 (autoclave). Steam 13 is also

fed to the reactor 12 to provide heat. Other forms of heat may also be provided
to the reactor 12 as appropriate. The feed gypsum may be any form of gypsum,
such as land plaster, gypsum mineral from ground or unground sources,
synthetic gypsum from flue gas desulfurization processes in power plants, or
other chemical gypsum as by-products of the titanium dioxide industry.
Traditionally the feed gypsum is land plaster manufactured by grinding gypsum
rock to a fine particle size in a roller mill. The fineness of the land plaster is 95 to
98 % less than 100 ASTM mesh. Land plaster gypsum purity can range from 80
to 99 wt. % calcium sulfate dihydrate.
[0024] A crystal modifier 14 may also be fed to the reactor 12 if desired. The
crystal modifier 14 controls the crystal morphology of the calcium sulfate alpha
hemihydrate to achieve a desired particle size, e.g., 50 to 20 microns (d50)
average particle size. Prior to the dewatering of the alpha hemihydrate slurry
additives may be added that will aid in the filtration, act as a hydration
accelerator, and/or provide added fluidity to the final material.
[0025] The slurry 10 is held in the reactor 12 at conditions for calcining the
gypsum to partially convert it to alpha calcium sulfate hemihydrate, for example
55 psig at 300 °F (149 °C). Typically, 50 to 95%, or 80 to 95 %, or 80 to 90% of
the gypsum is converted by calcination to alpha calcium sulfate hemihydrate,
alpha-CaSO4.0.5 H2O with a residence time of 5 minutes. The conversion can be
controlled by changing the residence time or temperature of the reactor
discharge. The higher the temperature the faster the conversion takes place.
The longer the residence time the higher the conversion rate is achieved.
[0026] Typically, the reactor 12 is a continuous stirred tank reactor (CSTR)
operating at a pressure of 15 to 100 psig (29.7 to 114.7 psia, 2.0 to 7.9 bar),
preferably 25 to 75 psig (39.7 to 89.7 psia, 2.7 to 6.2 bar) or 35 to 55 psig (49.7
to 69.7 psia, 3.4 to 4.8 bar). The temperature of the reactor 12 corresponds to
the temperature of saturated steam at the operating pressure. For example, a
pressure of about 52 psig (66.7 psia, 4.6 bar) corresponds to a temperature of

about 300 °F (149 °C). The residence time of the slurry in the reactor 12
generally ranges from 2 to 30 minutes, preferably 5 to 15 minutes.
[0027] For example, in a typical embodiment, after the reactor 12 is closed, hot
steam 13 is delivered to the jacket around the reactor 12 to heat the reactor 12
for about 5 minutes. The change in temperature and pressure inside the reactor
are monitored as a function of time. Then after about 10 minutes, the delivery
pressure of the steam 13 was increased to bring the reaction to completion in
about 5 additional minutes. The crystal modifiers 14 could, for example, be
added to the slurry 10 before heating begins or while the slurry 10 is being
heated or maintained at a desired temperature in the reactor 12.
[0028] The partially calcined gypsum product 16 discharges from the reactor 12
as a slurry comprising calcium sulfate dihydrate and alpha calcium sulfate
hemihydrate and feeds an accumulator tank 20. Accumulator tank 20 acts as a
holding tank and permits release of the steam as the slurry's pressure drops to
atmospheric pressure. If desired the accumulator tank 20 may be omitted if the
separation stage (dewatering unit 30) is direct coupled.
[0029] The slurry 24 discharges from the accumulator tank 20 and feeds a
dewatering unit 30 which removes water to produce a dewatered solids-
containing product 32 and a removed water stream 34.
[0030] All or a portion of the removed water 34 may be recycled as a stream 38
to be part of the slurry 10 to assist in recycling water, heat and chemicals (such
as the crystal modifiers or other additives) used in the process. Typically the
stream 38 is recycled at an elevated temperature, such as 100 to 200 °F (38 to
93 °C). The partially calcined gypsum product 16, the accumulator tank 20, the
stream 24, the dewatering unit 30 and the dewatered product 32 are kept at a
temperature sufficiently high to prevent the alpha hemihydrate from rehydrating,
e.g., kept at elevated temperature of 160-212 °F (71-100°C).
[0031] Typically the dewatering unit 30 is a filter press and/or centrifuge and the
dewatered product 32 has a 2 to 6 wt. %, typically 4 %, free water moisture
content. A typical filter press employs steam to press down on a plate over the
partially calcined gypsum product slurry to drive out the water. If desired the

process of Baehr US patent number 4,435,183 may be employed for dewatering
and drying calcium sulfate hemihydrate in a centrifuging and flash drying
operation by ejecting the wet solids from the centrifuge bowl directly into the
flash dryer's high velocity, high volume, heated air stream. Baehr US patent
number 4,435,183 is incorporated herein by reference.
[0032] The dewatered product 32 is fed to a board stucco kettle calciner 40 at
conditions to convert the majority or all of the gypsum in the dewatered product
32 to beta calcium sulfate hemihydrate. The kettle calciner 40 typically is
indirectly heated at atmospheric pressure by use of natural gas heating on the
bottom and direct fired heated air 42. The material behaves as a fluidization bed
due to the free water vapor leaving the solids fed to the kettle reactor 40 as well
as the bound water released as the gypsum (calcium sulfate dihydrate) converts
to calcined beta gypsum (beta calcium sulfate hemihydrate). Fluidization gas
may also be provided by the indirect fired gas heated air or use of direct fired
heated air 42. The kettle 40 typically operates at atmospheric pressure, and a
temperature of from 150 to 1000 °F (66 to 538 °C), preferably 250 to 650 °F (121
to 343 °C) or 400 to 500 °F (204 to 260 °C) or 285 to 300 °F (140 to 149 °C).
[0033] The kettle 40 discharges a dry product 44 comprising alpha calcium
sulfate hemihydrate and beta calcium sulfate hemihydrate (also known as an
alpha and beta stucco blend). Optionally, the dry product 44 is sent to grinding
50 to reduce the particle size of the material.
[0034] Typically the dry product 44 has less than 5 wt. %, preferably less than 2
wt. %, calcium sulfate anhydrite and less than 5 wt. %, preferably less than 2 wt.
. %, calcium sulfate dihydrate.
[0035] Typically the calcium sulfate of the final product is 50-95 wt. % alpha
hemihydrates and 50 to 5 wt. % beta hemihydrate; for example, 70-85 wt %
alpha hemihydrates and 30-15 wt % beta hemihydrate; or 80-90 wt. % alpha
hemihydrates and 20-10 wt. % beta hemihydrates.
[0036] The crystal modifier 14, if employed, is in the solution during the period of
calcination to alpha hemihydrate. The pH of the solution is in the neutral range
between 6 and 8. The crystal modifiers 14 act in reducing the number of nuclei

that form in the solution and also restrain the growth of the crystal in one of its
axis. The result is control of the particle size through control of the number of
crystals forming and growing. The other result is that the shape of the crystal is
cubic like in aspect ratio. With no modifiers in the solution the shape of the
alpha hemihydrate would be a long acicular needle shaped crystal of aspect ratio
up to 100:1 in length to diameter.
[0037] The resulting alpha- beta-stucco blend typically has a number of
desirable properties of consistency, compressive strength and density.
[0038] For example, the typical dry product has a normal consistency of about
30 to 36 as measured by a handmix drop consistency determination.
[0039] In contrast to normal consistency measured according to ASTM
Procedure C472, normal consistency as measured by a handmix drop
consistency method is not ASTM Procedure C472 test. The test method for
measuring normal consistency by a handmix drop consistency method is as
follows.
[0040] Weigh a 50 gram sample of the plaster to be tested at 70-80 °F (21-27
°C) to 0.1 gram accuracy. Drained the mixing cup and spatula before using
such that the mixing cup and spatula contain a maximum of 1/4 cc of
adhering droplets of water or are wiped dry. Add water to the mixing cup from
a burette (deionized or distilled at 70-80 °F (21-27 °C) unless otherwise
specified) in the estimated quantity to produce the proper flow. Sift the plaster
into the water and allow the sample to soak undisturbed for 60 seconds. Mix
thoroughly for 30 seconds, stirring 90 to 100 complete revolutions with the
spatula. Pour the slurry immediately after mixing on to a clean, dry,
unscratched PLEXIGLASS sheet from a height of 1½ inch. At the correct con-
sistency, the mix will flow out of the cup without the aid of the spatula.
[0041] The mix should form a round patty of reasonably uniform thickness.
The patty diameters for each specific consistency range are as follows in
TABLE 1 (when measured in at least two directions and averaged):


CRYSTAL MODIFIERS
[0042] TABLE 2 presents typical crystal modifiers. Also, US Patent No.
2,907,667 to Johnson, incorporated herein by reference, discloses a number of
chemicals which impact reactions in reactors for making alpha calcium sulfate
hemihydrate.

[0043] The stucco composition of the invention can be used in both the
manufacture of gypsum wallboard and stucco for production of a plaster for
interior and exterior applications. One or more additives can be added to the
stucco composition to facilitate the desired viscosity, and other optional
additives may be added to achieve desired physical characteristics in the final

set product, such as, for example, flexural strength, abuse resistance (e.g.,
chip resistance), water resistance, flame resistance, and the like, or
combinations thereof.
EXAMPLES
[0044] A plant control and three plant trial examples of the present invention
were conducted. In the Control and Examples, 75% solids slurry was fed to one
continuous stirred tank reactor (CSTR) of 275 gallons (1041 liters) in size used
for the Alpha-portion of the calcinations. A high temperature Tube mill was used
for the Beta-portion of the calcinations of the Examples. The Tube mill was a
heated ball mill.
CONTROL
[0045] At a reactor temperature of 298 °F (148 °C), 99% of the gypsum of the
feed slurry was calcined to Alpha calcium sulfate hemihydrate, which had a
normal consistency of 32 to 34 cc. Normal consistencies in the Control and the
following Examples were measured by the above-described hand drop test.
EXAMPLE 1
[0046] At a reactor temperature of 285 "F (141 "C), 90% of the gypsum fed to the
first reactor was calcined to Alpha calcium sulfate hemihydrate. The resulting
slurry was filtered and the filtered solids were further calcined in the Tube mill at
300 °F (149 °C). The filtered product before being fed to the Tube mill was kept
at elevated temperature of 160-212 °F (71-100°C). The Tube mill converted at
least a portion of the calcium sulfate dihydrate of the dewatered solids into beta
calcium sulfate hemihydrate. Thus, the resulting product had 90% alpha calcium
sulfate hemihydrate and 8.5%-9% beta calcium sulfate hemihydrate for a total
hemihydrate yield of 98.5% or higher relative to the amount of gypsum of the
feed slurry. In other words, 90% of the gypsum of the feed slurry converted to
alpha calcium sulfate hemihydrate and 8.5%-9% converted to beta calcium
sulfate hemihydrate. The normal consistency of the resulting product was 32 cc.

EXAMPLE 2
[0047] At a reactor temperature of 280 °F (138 °C), 85% of the gypsum fed to the
first reactor was calcined to alpha calcium sulfate hemihydrate. The resulting
slurry was filtered and the filtered solids were further calcined in the tube mill at
300 °F (149 °C). The filtered product before being fed to the Tube mill was kept
at elevated temperature of 160-212 °F (71-100°C). The Tube mill converted at
least a portion of the calcium sulfate dihydrate of the dewatered solids into beta
calcium sulfate hemihydrate. The resulting product had 85% alpha calcium
sulfate hemihydrate and 13.5%-14% beta calcium sulfate hemihydrate for a total
hemihydrate yield of 98.5% or higher relative to the amount of gypsum of the
feed slurry. The normal consistency of the resulting product was 34 cc.
EXAMPLE 3
[0048] At a reactor temperature of 275 °F (135 °C), 80% of the gypsum fed to the
first reactor was calcined to alpha calcium sulfate hemihydrate. The resulting
slurry was filtered and the filtered solids were further calcined in the tube mill at
300 °F (149 °C). The filtered product before being fed to the Tube mill was kept
at elevated temperature of 160-212 °F (71-100°C). The Tube mill converted at
least a portion of the calcium sulfate dihydrate of the dewatered solids into beta
calcium sulfate hemihydrate. The resulting product had 80% alpha calcium
sulfate hemihydrate and 18.5%-19% beta calcium sulfate hemihydrate for a total
hemihydrate yield of 98.5% or higher relative to the gypsum of the feed slurry.
The normal consistency of the resulting product was 32 cc.
[0049] The data shows the present inventive process has the advantage that it
results in a combined alpha calcium sulfate hemihydrate and beta calcium
sulfate hemihydrate product that has a normal consistency similar to that of an
alpha calcium sulfate hemihydrate product.

[0050] Although we have described the preferred embodiments for implementing
our invention, it will be understood by those skilled in the art to which this
disclosure is directed that modifications and additions may be made to the
invention without departing from the spirit and scope thereof.

We claim:
1. A process of manufacturing a product comprising alpha calcium
sulfate hemihydrate and beta calcium sulfate hemihydrate comprising the steps
of:
feeding a 50-75 wt. % gypsum slurry to a first reactor, the slurry
comprising calcium sulfate dihydrate and water;
calcining the slurry in the reactor at conditions sufficient to form a partially
calcined slurry comprising water, calcium sulfate dihydrate and alpha calcium
sulfate hemihydrate, wherein the slurry is held in the first reactor at conditions for
calcining the gypsum to convert 50 to 95% of the gypsum to alpha calcium
sulfate hemihydrate;
dewatering the partially calcined slurry to form a water stream and
dewatered solids comprising the calcium sulfate dihydrate and alpha calcium
sulfate hemihydrate;
feeding the dewatered solids to a second reactor; and
calcining the dewatered solids in the second reactor to convert at least a
portion of the calcium sulfate dihydrate of the dewatered solids into beta calcium
sulfate hemihydrate.
2. The process of claim 1, wherein the slurry is held in the first reactor
at conditions for calcining the gypsum to convert 80 to 95% of the gypsum to
alpha calcium sulfate hemihydrate.
3. The process of claim 1, wherein the slurry is held in the first reactor
at conditions for calcining the gypsum to convert 70 to 85% of the gypsum to
alpha calcium sulfate hemihydrate.
4. The process of claim 1, wherein at least one crystal modifier is
added to the calcium sulfate dihydrate and water before said calcining in the first
reactor.

5. The process of claim 1, wherein the first reactor is a continuous
stirred tank reactor (CSTR).
6. The process of claim 1, wherein the first reactor is operating at a
pressure of 15 to 100 psig during the calcining in the first reactor.
7. The process of claim 1, wherein the first reactor is operating at a
pressure of 25 to 75 psig during the calcining in the first reactor.
8. The process of claim 1, wherein the first reactor is operating at a
pressure of 35 to 55 psig during the calcining in the first reactor.
9. The process of claim 1, wherein the residence time of the slurry in
the first reactor ranges from 2 to 30 minutes during the calcining in the first
reactor.
10. The process of claim 1, wherein the residence time of the slurry in
the first reactor ranges from 5 to 15 minutes during the calcining in the first
reactor.
11. The process of claim 1, wherein the second reactor comprises a
kettle.
12. The process of claim 11, wherein the calcining of the dewatered
solids occurs in the kettle containing a fluidized bed comprising the dewatered
solids.
13. The process of claim 12, wherein the calcining of the dewatered
solids occurs in the kettle operated at atmospheric pressure and a temperature
o ffrom 150 to 1000°F.

14. The process of claim 12, wherein the calcining of the dewatered
solids occurs in the kettle operated at atmospheric pressure, and a temperature
of from 250 to 650 oF.
15. The process of claim 12, wherein the calcining of the dewatered
solids occurs in the kettle operated at atmospheric pressure, and a temperature
of from 400 to 500 °F.
16. The process of claim 13, wherein the calcining of the dewatered
solids occurs in the kettle operated at atmospheric pressure, and a temperature
of from or 285 to 300 °F.
17. The process of claim 12, wherein the dewatered solids fed to the
kettle comprise 2 to 6 wt. % free water.
18. The process of claim 1, wherein the dewatered solids have a
temperature between 150 and 300 °F upon dewatering and when fed to the
second reactor.
19. The process of claim 1, further comprising mixing water and
gypsum to form the 50 - 75 wt. % gypsum slurry, wherein the water stream from
dewatering is recycled to the mixing step.
20. The process of claim 19, wherein the water stream from dewatering
is recycled at elevated temperature to the mixing step to recover heat, water and
chemicals used in the process.

A process is disclosed for making a blend of alpha- and beta-stucco including a slurry calcination step to produce alpha calcium sulfate hemihydrate followed by a fluidized bed calcination step to produce beta calcium sulfate hemihydrate. The process starts with 50-75% gypsum-containing solids slurry, and then steam calcines the slurry in a first reactor to form partially calcined gypsum slurry which contains calcium sulfate dihydrate and alpha calcium sulfate hemihydrate. The partially calcined
slurry is then dewatered. Then the filter cake is fed into a kettle to complete the calcination process by converting the calcium sulfate
dihydrate of the filter cake material into beta calcium sulfate hemihydrate.

Documents:

1463-KOLNP-2009-(06-09-2011)-CORRESPONDENCE.pdf

1463-KOLNP-2009-(06-09-2011)-PA.pdf

1463-KOLNP-2009-(07-07-2009)-ASSIGNMENT.pdf

1463-KOLNP-2009-(07-07-2009)-CORRESPONDENCE.pdf

1463-KOLNP-2009-(08-10-2013)-CORRESPONDENCE.pdf

1463-KOLNP-2009-(08-10-2013)-FORM-3.pdf

1463-KOLNP-2009-(25-05-2012)-CORRESPONDENCE.pdf

1463-KOLNP-2009-(25-05-2012)-FORM-1.pdf

1463-KOLNP-2009-(25-05-2012)-FORM-13.pdf

1463-KOLNP-2009-(25-05-2012)-PA-CERTIFIED COPIES.pdf

1463-KOLNP-2009-(30-05-2014)-ABSTRACT.pdf

1463-KOLNP-2009-(30-05-2014)-CLAIMS.pdf

1463-KOLNP-2009-(30-05-2014)-CORRESPONDENCE.pdf

1463-KOLNP-2009-(30-05-2014)-DRAWINGS.pdf

1463-KOLNP-2009-(30-05-2014)-FORM-1.pdf

1463-KOLNP-2009-(30-05-2014)-FORM-2.pdf

1463-KOLNP-2009-(30-05-2014)-FORM-3.pdf

1463-KOLNP-2009-(30-05-2014)-FORM-5.pdf

1463-KOLNP-2009-(30-05-2014)-OTHERS.pdf

1463-kolnp-2009-abstract.pdf

1463-kolnp-2009-claims.pdf

1463-kolnp-2009-correspondence.pdf

1463-kolnp-2009-description (complete).pdf

1463-kolnp-2009-drawings.pdf

1463-kolnp-2009-form 1.pdf

1463-KOLNP-2009-FORM 18.pdf

1463-kolnp-2009-form 3.pdf

1463-kolnp-2009-form 5.pdf

1463-kolnp-2009-gpa.pdf

1463-kolnp-2009-pct priority document notification.pdf

1463-kolnp-2009-pct request form.pdf

1463-kolnp-2009-specification.pdf

abstract-1463-kolnp-2009.jpg

PETITION 1463-KOLNP-20090001.pdf


Patent Number 265287
Indian Patent Application Number 1463/KOLNP/2009
PG Journal Number 08/2015
Publication Date 20-Feb-2015
Grant Date 17-Feb-2015
Date of Filing 20-Apr-2009
Name of Patentee UNITED STATES GYPSUM COMPANY
Applicant Address 550 WEST ADAMS STREET, CHICAGO, IL
Inventors:
# Inventor's Name Inventor's Address
1 SONG, WEIXIN DAVID 1785 W. NEWPORT, LAKE FOREST, ILLINOIS 60045
2 LYNN, MICHAEL R. 2640 N. PRINDLE AVE., ARLINGTON HEIGHTS, ILLINOIS 60004
3 YU, QIANG 1252 SANDPIPER COURT, GRAYSLAKE, ILLINOIS 60030
4 CLOUD, MICHAEL LEE 411 W. WALNUT, CANTON, OKLAHOMA 73724
5 LIU, QINGXIA 108 N. FIORE PARKWAY, VERNON HILLS, ILLINOIS 60061
PCT International Classification Number C01F 11/46
PCT International Application Number PCT/US2007/018558
PCT International Filing date 2007-08-22
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 11/533,604 2006-09-20 U.S.A.