Title of Invention

ORGANIC-INORGANIC COMPOSITE

Abstract An inorganic-organic composite comprises an inorganic phase, such as gypsum crystals, and a film forming organic phase. The film forming organic phase is selected from substituted starches having a degree of polymerization; degree of substitution and viscosity such that the substituted starches are insoluble in water during mixing but dissolve at a higher processing temperature during forming, setting or drying of the composite. Thus, excessive migration of the substitute starch is prevented and the composite is substantially strengthened.
Full Text ORGANIC-INORGANIC COMPOSITE
CROSS-REFERENCE TO RELATED APPLICATION
[0001] The present application claims the benefit of previously filed, co-
pending U.S. Provisional Patent Applications, Serial No. 60/603,491, filed August 20,
2004; and Serial No. 60/528,536; filed December 10, 2003; and Serial No.
60/553,423, filed March 15, 2004, and incorporates by reference the contents therein.
FIELD OF THE INVENTION
[0002] The field of the invention relates to organic-inorganic composites for
low-cost, fire-retardant building materials and the like.

BACKGROUND
[0003] Substituted starches are starch derivatives that have been chemically
reacted to replace one or more of the hydroxyl functional groups. Typically, the
process involves etherification or esterification of a starch or modified starch which
append ether or ester linkages along the starch polymer backbone. This process differs
from more traditional modifications made to starches such as oxidization, acid-
thinning, cross-linking, and pre-gelatinization. The starch may come from one of
many natural sources, such as potato, tapioca, or com. In fact, any of numerous
starches are well known and commercially available in a variety of forms, including
liquids, particles and fine powders. A substituted starch may also be modified in
another way, such as acid-thinning, prior to or after substitution with one or more
types of functionalities. For example, substituent groups may be alkyl as in methyl or
ethyl substitution, hydroxyalkyl as in hydroxyethyl, hydroxymethyl, or hydroxypropyl
substitution, hydrophobic, cationic, anionic, or combinations of these. Regardless,
methods of preparing substituted starches is well known.
[0004] Acid-thinned or pre-gelatinized starches are sometimes added to
wallboard core formulations to improve the bonding of the wallboard core to the
paper facing. These starches typically migrate to the surface or .are applied directly to
the surface of the wallboard core. In conventional wallboard, the paper facing resists
most of the stress,'and a reliable bond between the paper facing and the wallboard
core is essential to obtain strength and durability of a wallboard. Also, it is well
known and accepted that such starches do little or nothing to significantly strengthen
the wallboard core.


[0005] Indeed, most starches either do not dissolve and disperse in the
inorganic matrix or migrate efficiently to the surfaces during drying. Thus, such
starches serve no known role in strengthening the wallboard core. Even starches that
remain predominantly dispersed throughout the composite do not adequately bind the
discrete inorganic phase, which may be of any morphology, including needle-like
crystals, particulates, or fibers. Many attempts have been made to find an inexpensive
and useful additive for strengthening the wallboard core, but such attempts have failed
to provide properties that are substantially better than conventional wallboard.
SUMMARY
[0006] A substituted starch reinforced composite comprises a discrete
inorganic phase and a polymeric phase which includes a substituted starch. It is
believed that the microstructure of the composite is controlled to produce an inorganic
phase reinforced by a percolating, polymeric film including a substituted starch
without limiting the claims in any way. For example, a substituted starch, such as
hydroxyethylated, hydroxypropylated, or acetylated starch, is selected having a degree
of substitution that makes the substituted starch insoluble in cold water. The starch is
dispersed by mixing. For example, the substituted starch may be mixed as a dry
powder with powdered calcium sulfate hemihydrate prior to mixing with excess water
to form a flowable slurry. Subsequently, during drying, the.temperature of the slurry
increases and the substituted starch, which is mostly undissolved, begins to dissolve in
the excess water. The substituted starch remains in the gypsum core and deposits on
the hydrated inorganic phase during drying. A substituted starch, such as a starch-
ether or starch-ester, acts as an efficient binder for the discrete inorganic phase, such
as gypsum crystals that form during hydration of calcium sulfate hemihydrate with
small additions of the substituted starch.
[0007] It is an object to provide a composite with an intimate dispersion and
interaction of inorganic and organic components. An advantage is that low additive
levels of organic components significantly increases the strength and nail pull
resistance of the composite while keeping the costs of the composition of matter in a
range that is commercially advantageous. Another advantage is that the weight of the
composite can be reduced without sacrificing strength, allowing for decreased
production costs.
[0008] In one example, substituted starches are selected that possess good
film-forming properties and hydrophilic properties which result in intimate interaction
between the organic and inorganic phases. The substituted starch composition


thoroughly penetrates the inorganic matrix and strongly adheres to and binds the
inorganic phase.
[0009] It is another object is to provide an enhanced stucco slurry that has
low viscosity during mixing and forming. For example, by delaying dissolution of a
starch additive until the temperature of the slurry is increased to the dissolution point,
the viscosity of the slurry remains low until setting and drying of the wallboard. In
one example, a starch-based polymer with a low degree of substitution is used to
delay dissolution until the temperature is raised during the setting and drying portion
of the process used to form the article made of the composition of matter. An
advantage is that the delayed dissolution prevents the slurry from clogging or sticking
to manufacturing equipment. Another advantage is that the composition of matter has
a molecular dispersion of the polymer, which remains throughout the inorganic matrix
of the article upon drying of the composite. Yet another advantage is that the polymer
is less likely to migrate to the surface of the composite, where it is unavailable for
improving the strength of the core.
[00010] Other features and advantages will become apparent from the
following description which refers to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] Figure 1 shows a graph of the board weight (BDWT) in pounds (lbs)
per million square feet (MSF) versus the weight percent of starch ether addition that
achieves a desired strength requirement, which is superimposed on a graph of the
relative cost of the board in dollars versus the weight percent of starch ether (SE)
addition.
[0012] Figure 2A compares the relative increase in nail pull resistance at a
specific board weight versus weight percent additive (Additive Level) for an acid-
modified starch (Acid-mod), an hydroxyethyl starch ether (HE Starch), a hydrophobic
starch ether (Hydrophobic SE), and a hydroxypropylmethyl cellulose (HPMC).
[0013] Figure 2B compares the relative percent increase in nail pull
resistance at a specific board weight versus additional cost per million square feet
(Cost/MSF) for the same additives as compared in Figure 2A.
DETAILED DESCRIPTION
[0014] The following examples do not exclude other solutions that are based
on the teachings in the Summary. Instead, the following merely provide some of the
examples of specific embodiments.


[0015] Certain substituted starches can greatly enhance the strength of a
gypsum wallboard core. Most starches, including traditional wallboard starches and
many substituted starches, do not substantially increase the strength of a gypsum-
based construction material. Herein, substantially increasing the strength by including
any additive means that a flat, one-half inch thick sample of a paperless core has at
least a 10% increase in nail pull resistance or flexural strength with addition of an
additive compared to the same density of paperless core made without the additive.
[0016] For example, starches may be selected that have a particular
molecular weight and type and degree of substitution which result in efficient
distribution throughout and intimate interaction with the inorganic composite. The
resulting substituted starch reinforced composite has improved hardness and strength,
which is an excellent combination for improving nail pull resistance. In addition, the
toughness of the sample does not diminish with increasing additive in the sample.
Thus, wallboard with such a substituted starch reinforced core has improved nail pull
resistance and hardness.
[0017] In some examples, substituted starches used in the composite have
solubility characteristics that allow full dissolution in the inorganic core without
migration to surfaces during the production process. For example, the substituted
starch may be of an hydroxyethyl starch with a low degree of substitution, e.g. less
than 0.3 DS, which is insoluble in cold water. Cold water is the expression used to
relate to the processing temperature of the water during mixing, which is less than the
temperature of the composite material during setting and/or drying. In one wallboard
manufacturing process, the starch is added as a dried powder, preferably with the
other dry ingredients, prior to mixing with water and wet components. The starch
remains undissolved during mixing, forming, and setting, and therefore does not
significantly affect slurry viscosity or stucco hydration, which allow all of the various
wallboard manufacturing processes to be used with little or no modification. The
substituted starch dissolves, forms an aqueous molecular dispersion, and evenly
deposits throughout the gypsum matrix during setting and drying phases of the
process, as the temperature of the wallboard increases above the dissolution point,
allowing the starch additive to reinforce the composite by forming a molecular
network.
[0018] Polysaccharides other than starch may be used, so long as the
distribution in the core material, the interaction of the polysaccharides with the
inorganic composite and the migration of the polysaccharides in the core material are


similarly controlled. However, as show in Figure 2B, substituted starches cost less,
which provides a significant commercial advantage.
[0019] The control of the degree of substitution and dissolution temperature
is important in selecting reinforcing additives. The additives should readily dissolve at
some point during the process of forming an article of manufacture, but the amount of
migration, after dissolution of the additive, should be limited. Thus, the additive is
substantially retained within the core of the article of manufacture, where it can
strengthen the composite.
[0020] For example, wallboard drying typically involves passing wet boards
through a multi-stage drying lain, resulting in heat and mass transfer through board.
As heat from the kiln enters the board, the excess water increases in temperature and
evaporates. Water vapor, or steam, escapes predominantly through the faces of the
board, usuaDy through heavy wallboard paper. Therefore, throughout the drying
process, the particular temperature and moisture profile through the thickness of the
board varies. In one example, a substituted starch is selected that responds to changes
in temperature and moisture to form a continuous, fine film throughout the wallboard
core during the drying process. Most of the additive is retained in the wallboard core.
[0021] A substituted starch may come from any native starch source,
initially. Starches from various sources have different granule sizes, degrees of
polymerization (DP), and ratios of amylose (linear starch) to amylopectin (branched
starch). DP refers to the average number of anhydroglucose units per starch molecule.
Dent corn, waxy maize, or potato starch are preferred due to cost considerations. Dent
com and potato starch are predominantly amylopectin with native potato starch
having more amylose and a higher DP. Waxy maize corn is 100% amylopectin.
Special hybrid corn species produce high amylose starch which may also be
substituted. Starches of high DP are preferably acid-thinned prior to substitution in
order to obtain the proper viscosity characteristics.
[0022] Substituted starches may be cold water insoluble, meaning that they
do not increase solution viscosity until heated past their gel temperatures. The
response in viscosity of a particular starch to cooking is often characterized by visco-
anslysis: a starch dispersion under shear is heated to and held at 90 - 95 C for a given
period of time and is then cooled to 35 - 50 C while measuring viscosity throughout
the process. Different types of modified and substituted starches have a wide range of
viscosity profiles measured by visco-analysis (RVA). Typical response to cooking
involves granule swelling as the starch is heated, granular burst and molecular
dispersion during heating or cooking, and viscosity increase and starch re-association


upon cooling. Several points on the viscosity profile can be used to characterize the
starch. These are gel temperature, peak viscosity, trough viscosity (holding strength),
and final viscosity (see figure). Starch viscosity profiles are also influenced by shear
rate, pH, salts, and particulates.
[0023] Different types of starch modification and substitution may be used
to adjust the viscosity characteristics for particular applications. In one composition,
the hydroxyl groups of the starch are substituted with another group connected by an
ester or ether linkage. Some preferred substituents due to availability, cost, and
performance are hydroxypropyl, hydroxyethyl, acetyl, hydrophobic, anionic, and
cationic. While these substitutions result in starches with different molecular
compositions, they share some characteristics. In general, substitution accomplishes:
decrease in gel temperature; decrease in the time and temperature range over which
the starch granules swell and burst, releasing starch molecules into solution; altered
ratio between peak, trough, and final viscosity; and reduced tendency to retrograde
(set-back). All of these effects tend to improve film forming ability. Starches used in
the inventive compositions have improved film flexibility and strength compared to
modified and unmodified starches. It is believed that substituted starches may have an
altered balance of hydrophobicity and hydrophilicity, improving affinity and adhesion
to inorganic phases in the matrix of the article of manufacture.
' [0024] For example, starch may be substituted with particular substituent
groups to various degrees by altering reaction conditions. The degree of substitution is
usually expressed as either DS, the number of hydroxyl groups replaced per
anhydroglucose unit, or weight percent, the total weight of the substituent units
divided by the total weight of the polymer. Both refer to the average amount of
substitution, as the actual substitution may vary among hydroxyl location as well as
along the starch chain and between starch molecules. The DS of the starch in the
inventive compositions is critical to strength enhancement. Starches with a low DS do
not have the lower gel point and trough viscosity that leads to proper dissolution and
dispersion. Also, starches with a high DS become cold water soluble and affect slurry
viscosity and stucco hydration. Starches with the optimum DS have viscosity
characteristics and hydrophobic/hydrophilic balance that give the most favorable
interaction with the inorganic matrix of the composite. In one embodiment, the
substituted starch has a degree of substitution no greater than 6 weight percent, which
substantially strengthens the composite when added as described herein. In one
preferred embodiment, the degree of substitution is selected in a range from 1-3


weight percent. In another preferred embodiment, the degree of subsititution is
selected in a range from 1.5-2.5 percent
[0025] The strength enhancing ability of particular type of substituted
starch is dependent upon the viscosity of the starch as well as the degree of
substitution. The effect of viscosity on the strength enhancement of substituted
starches was explored using commercially available starches as well as starches
prepared in the laboratory. Starches with various viscosities due to different degrees
of acid-thinning were substituted to the same degree in order to determine the
optimum viscosity for strength enhancement. Acid-modified starches from Grain
Processing Corp designated as C68F, C165, C150, C140, C124, and C110 were each
substituted with approximately 2.3 wt% hydroxypropyl (HP) groups using a standard
substitution reaction scheme. The substitution level of the starches was analyzed by
digestion and gas chromatography. The starch samples were added at 2 wt% of stucco
to a standard wallboard formulation which were then tested for nail pull resistance
and normalized to control samples to determine the amount of strength improvement.
The results can be found in Table 1. Viscosity is presented as the solids content of the
starting material required to achieve a cooked viscosity of 1000 cps at 150F. Starches
with higher "wt% solids at 1000 cps" have lower viscosity.

[0026] Commercially available hydroxyethylated (HE) starches of different
viscosities were added at 2 wt% of stucco to wallboard samples to evaluate their
strength enhancing properties. Tested samples included a series of Ethylex starches
from AE Staley Co and a series of Coatmaster starches from Grain Processing Corp.
Again, the substitution level was determined for each sample. The results can be
found in Tables 2 and 3. Viscosity data is taken from the literature as the solids
content required to achieve a cooked viscosity of 1000 cps at 150F for Coatmaster and
at 95F for Ethylex.


[0027] Table 2 shows that a range of weight percent solids of from 17-30
for 1000 cps at 150 °F is preferred. More preferably, the range is 17-21 weight
percent solids.
[0028]. The data collected from laboratory land commercial HE and HP
starches with similar DS and varying viscosity, or degree of acid-modification,
indicates that peak performance comes at an intermediate viscosity. For dent com
starch ethers, strength enhancement is greatest at a degree of acid-thinning that gives
1000 cps viscosity for around 20 wt% solids at 150F. (Note: Ethylex viscosity is
represented at a lower temperature, therefore viscosity at 150F would be lower and
wt% solids for 1000 cps would be higher, resulting in a correspondence between peak
viscosities.) It is believed that this intermediate viscosity allows dissolution and
diffusion throughout the inorganic matrix without causing excessive migration to the
surface of the composite material. Optimum viscosity may vary depending on stucco
type and quality as well as processing conditions such as water-to-stucco ratio and
drying rate and temperature.
[0029] Iodine solution staining was used to identify the location of the
substituted starch polymer in the gypsum core. An iodine solution was prepared by
dissolving iodine (12) chips in isopropyl alcohol and water at room temperature.
Wallboard samples to be analyzed were cross-sectioned using a technique similar to
"score-and-snap," in which one paper facing was partially cut, with care not penetrate
the core, and the samples broken evenly. The iodine solution was then applied
liberally to the broken faces of the samples. The solution was given several minutes to

hydrate and complex with the starch in the sample. The stained samples were then
examined under a stereo microscope and the tint, hue, and location of the stained
starch was noted.
[0030] Starch staining results were related to molecular composition in
order to further explain trends in performance. Several key attributes were identified
to characterize starch behavior in samples after drying. Wallboard samples were
primarily characterized by the tint of stain in the bulk of the gypsum matrix, the size
and tint of granular particles within the matrix, and the thickness of darker tint at the
drying faces of the sample.
[0031] Wallboard samples that were not heated to above the gel
temperature of the incorporated starches were found to have no stain in the core or at
the faces and finely delineated particles within the core. In this case, the board core
and starch throughout never reach a high enough temperature to dissolve the starch.
The starch remains as granules that neither swell nor disperse.
[0032] Samples containing substituted starches with high viscosity had a
light tint in the core, very little stain at the faces, and larger, more diffuse particles
within the core. Here, the starches reached their gel temperature and began to
dissolve. The starch granules then either remained in the swollen state or burst but
diffused slowly due to high starch viscosity.
[0033] Samples with substituted starches of low viscosity had light tint in
the core with thick, dark staining along the faces. These starches became fully
dissolved and formed a molecular dispersion but then migrated toward the faces
during drying. The degree of migration was indicated by the thickness of the stain
along the paper facing.
[0034] Samples with substituted starches of the proper viscosity had dark
staining throughout the core. In these samples, the starch granules dissolved and
diffused through the gypsum matrix but did not migrate significantly to the faces
during drying. Although these samples may have had some stains indicating remnants
of granules and/or thin, concentrated layers at the faces, the starch was substantially
dispersed throughout the gypsum composite.
[0035] Viscosity was also found to be critical to performance in other types
of substituted starches such as starch-esters. For example, a commercially available
hydrophobically modified acid-thinned waxy maize starch, Filmkote 54 from National
Starch and Chemical Co, imparted excellent nail pull performance at low levels of
addition in a wallboard samples. However, its high viscosity counterpart, Filmkote
550, gave little or no improvement. likewise, an unmodified starch, B20F from Grain


Processing Corp, which was substituted with a low degree of hydroxypropyl groups
and added to a wallboand sample did not dissolve or increase strength. When the same
substituted starch was acid-thinned, however, and added to a wallboard sample, it
greatly improved the nail pull resistance.
[0036] Optimum viscosity is necessary but not sufficient for substituted
starch strength-enhancing performance. The starch must also have the proper degree
of substitution. If the substitution is too low, gel temperature; viscosity characteristics,
and film-forming ability are not altered enough to improve composite strength. When
substituted to too high a degree, the starch becomes cold water soluble, in which case
it affects slurry viscosity and stucco hydration and does not significantly improve
strength. These effects were demonstrated by substituting acid-thinned dent corn
starch, Wallboard Binder from AE Staley, with various amounts of HE substitution.
The samples were added to wallboard formulations which were tested for nail pull
resistance in order to determine the amount of strength enhancement, which is
outlined in Table 4.

[0037] Even when the amount of substitution is within the range to make a
starch cold water soluble with lowered gel temperature, degree of substitution can
affect strength enhancement It is believed that the DS affects the starch film
properties and affinity to the inorganic matrix, which is, in this case, gypsum crystals.
Starcheswere produced with increasing amounts of HP substitution. Again, wallboard
samples were made with 2 wt% additive of these starches and mechanically tested. A
peak in nail pull performance was found between 1.5 and 2.5 wt% HP. A similar trend
was found for starch-esters. Acetylated and butyrylated samples were made with
increasing amounts of substitution, below the limit of cold water solubility. Maximum
strength-enhancing ability was achieved with samples of intermediate substitution.
[0038] The type of starch that is substituted can also affect dissolution and
performance. Waxy maize corn, which is composed of the branched form of starch,
amylopectin, generally provides superior strength enhancement when modified or
substituted with a variety of groups. This is believed to be due to the strong affinity of
amylopectin to inorganics, such as gypsum crystals. The interaction was demonstrated

by adding pre-dissolved, acid-thinned waxy maize corn to a slurry of stucco. The
solution, which was not high viscosity, prevented the stucco from setting into
gypsum. This was probably due to amylopectin coordinating to surface of the growing
gypsum crystals, preventing their growth. When modified or substituted amylopectin
starch is not pre-dissolved or cold water soluble, this is not a problem because stucco
set occurs before starch dissolution.
[0039] Potato starch can also be substituted to produce a strength
enhancing additive for inorganic composites. It was found that substituted potato
starches of the preferred viscosity and substitution impart good strength enhancement
but with different dissolution characteristics. Many of the granules remain intact after
drying of the composite. This could be due to the larger granules and higher amylose
in potato starches. It is believed that a fraction of the substituted starch leaches out of
the granules into the matrix and is responsible for the majority of the strength
enhancement. Tapioca starch, and conceivably any other native starch source, can also
become strength-enhancing when adjusted to the proper viscosity and substituted
within a given DS. Selection of the type of strength-enhancing starch to use in a given
composition depends largely on their performance to addition and performance to cost
ratio.
[0040] The substituted starches of the inventive compositions are
particularly attractive due to their effective strength enhancement and low cost They
can be used at low levels to improve the strength of gypsum wallboard at current
board weights or to reduce the weight of wallboard without sacrificing strength. In
either of these cases, the cost effectiveness of strength-enhancing starches is of
primary importance. The increased cost of substituting a starch is offset by the
improvement in strength enhancing characteristics. Significantly less of a substituted
starch can be added to a composite to achieve the same effect as a less effective starch
or additive. The overall performance to cost ratio is therefore greater with substituted
starches than with other strength enhancing additives.
[0041] A desired additive level for reducing the weight and cost of gypsum
wallboard can be found using simple cost analysis. Increase in the strength to weight
ratio of the gypsum core and composite sandwich structure allow the production of
lighter weight boards with the same nail pull resistance. The lighter weight boards
contain less material in the core which results in more cost savings than cost added by
the starch. However, the benefits of adding a strength-enhancing starch generally
level off at higher additive levels. At some point, the added cost of the starch begins
to outweigh the weight reducing ability and resulting cost savings. For example, an


HE starch can be used to reduce the minimum board weight to pass ASTM nail pull
standards from 1550 Ibs/MSF to 1400 Ibs/MSF at 1.5 wt% stucco addition with a 3%
manufacturing cost savings.
[0042] In other cases, the performance per additive is more important, such
as in the case of high performance construction boards. These boards typically contain
a higher percentage of strength enhancing additives. When higher levels of organic
additives are added to a composite, other factors such as fire and mold resistance
become important Fire resistance is a key benefit of inorganic compositions,
particularly gypsum wallboard, which should not be compromised by additives. Fire-
resistant additives, such as phosphates, may be included in me composition but are
often expensive. Mold susceptibility is a more recent concern that must be addressed
in construction materials. The use of a high level of organic components often
significantly decreases the mold resistance of a composite and requires the addition of
anti-microbial agents. Therefore, it may be an advantage to keep the organic strength
enhancing additive at as low a level as possible that achieves the desired mechanical
properties. In this case, the strength performance to additive ratio is of importance
when selecting a strength enhancing agent,
[0043] Strength enhancing starches may also be combined with other
additives to improve performance. Starches, when added as the sole enhancing
additive in wallboard, increase the hardness and nail pull resistance of the board, but
may also make the gypsum more brittle. Other additives can be added to complement
the effect of the substituted starch. For example, substituted starches may be
combined with strength enhancing cellulose ethers in inorganic composites. Certain
cellulose ethers are known to improve the toughness and flexural strengtti of inorganic
composites and can be used to counter the brittle nature imparted by the starch. When
used in combination in wallboard, the result is improved nail pull resistance, flexural
strength, hardness, and toughness of the board. In some cases, the combined
mechanical performance of the cellulose ether and substituted starch is greater than
the sum of the individual performances.
[0044] Fibers may also be included in the composite to improve flexural
strength, toughness, and abuse-resistance. It is known that fibers reduce damage
caused by handling, installation, and use of brittle, inorganic composites. It is believed
that small additions of cellulose ethers in the composite helps to bind the fibers to the
inorganic matrix and increases their pull-out strength. This results in much better
performance than when ether fibers or cellulose ether alone are added to the


composite. In one preferred embodiment, glass fibers are added due to their high
strength, low cost, and fire-resistance.
[0045] In one embodiment, substituted starch, cellulose ether, and glass
fibers are added at 10 wt%, 2 wt%, and 2 wt% stucco respectively. The resulting
slurry was cast into a 1/4 inch sheet with no facing material and dried in a two-stage
procedure. The resulting board had good nail pull resistance and flexural strength at
low board weight and excellent abrasion resistance. Similar formulations may include
a water resistant additive, such as a paraffin wax emulsion. An anti-fungal agent may
also be added to reduce mold susceptibility. Finally, the dried boards may be coated
with a priming material such as an acrylic or vinyl acetate ethylene copolymer
emulsion to facilitate later painting or finishing.
EXAMPLES
Control Sample 1: Acid-modified Dent Com Starch (Hi Bond)
[0046] Dry ingredients including 1000 g stucco, 10 g Hi Bond acid-
modified dent corn starch from Bunge Milling, and 10 g ground gypsum accelerator
were thoroughly mixed together. This mixture was then added to 1200 g warm (102
F) tap water with two drops of set retarder in a 4L Waring blender. The combination
was blended for 10 seconds on "low" setting. The resulting slurry was poured into a
paper envelope within a 12" x 12" x 1/2" horizontal mold and the surface was
compressed to ½" with a glass plate. The sample fully set within ten minutes and was
removed from the mold and placed in a 250 C convection oven. The sample was dried
to 75% of its original weight and then placed in a 50 C convection oven until
completely dry.
Control Sample 2: Acid-modified Dent Corn Starch (Wallboard Binder)
[0047] Dry ingredients including 1000 g stucco, 10 g Wallboard Binder
acid-modified dent corn starch from AE Staley, and 10 g ground gypsum accelerator
were thoroughly mixed together. This mixture was then added to 1200 g warm (102
F) tap water with two drops of set retarder in a 4L Waring blender. The combination
was blended for 10 seconds on "low" setting. The resulting slurry was poured into a
paper envelope within a 12" x 12" x 1/2" horizontal mold and the surface was
compressed to ½" with a glass plate. The sample fully set within ten minutes and was
removed from the mold and placed in a 200 C convection oven. The sample was dried


to 75% of its original weight and then placed in a 50 C convection oven until
completely dry.
Control Sample 3: Acid-modified Dent Com Starch (C165)
[0048] Dry ingredients including 1000 g stucco, 10 g C165 acid-modified
dent corn starch from Grain Processing Corp., and 10 g ground gypsum accelerator
were thoroughly mixed together. This mixture was then added to 1200 g warm (102
F) tap water with two drops of set retarder in a 4L Waring blender. The combination
was blended for 10 seconds on "low" setting. The resulting slurry was poured into a
paper envelope within a 12" x 12" x 1/2" horizontal mold and the surface was
compressed to ½" with a glass plate. The sample fully set within ten minutes and was
removed from the mold and placed in a 200 C convection oven. The sample was dried
to 75% of its original weight and then placed in a 50 C convection oven until
completely dry.
Control Sample 4: Acid-modified Dent Corn Starch (20g)
• [0049] Dry ingredients including 1000 g stucco, 20 g C165 acid-modified
dent com starch from Grain Processing Corp., and 10 g ground gypsum accelerator
were thoroughly mixed together. This mixture was then added to 1200 g warm (102
F) tap water with two drops of set retarder in a 4L Waring blender. The combination
was blended for 10 seconds on "low" setting. The resulting slurry was poured into a
paper envelope within a 12" x 12" x 1/2" horizontal mold and the surface was
compressed to ½" with a glass plate. The sample fully set within ten minutes and was
removed from the mold and placed in a 200 C convection oven. The sample was dried
to 75% of its original weight and then placed in a 50 C convection oven until
completely dry.
Hvdroxyethyl Starches
[0050] Dry ingredients including 1000 g stucco, 20 g Coatmaster K55F
hyrdoxyethylated, acid-modified dent com starch from Grain Processing Corporation,
and 10 g ground gypsum accelerator were thoroughly mixed together. This mixture
was then added to 1200 g warm (102 F) tap water with two drops of set retarder in a
4L Waring blender. The combination was blended for 10 seconds on "low" setting.
The resulting slurry was poured into a paper envelope within a 12" x 12" x 1/2"


horizontal mold and the surface was compressed to ½" with a glass plate. The sample
fully set within ten minutes and was removed from the mold and placed in a 250 C
convection oven. The sample was dried to 75% of its original weight and then placed
in a 50 C convection oven until completely dry.
[0051] Dry ingredients including 1000 g stucco, 20 g Coatmaster K54F
hyrdoxyethylated, acid-modified dent corn starch from Grain Processing Corporation,
and 10 g ground gypsum accelerator were thoroughly mixed together. This mixture
was then added to 1200 g warm (102 F) tap water with two drops of set retarder in a
4L Waring blender. The combination was blended for 10 seconds on "low" setting.
The resulting slurry was poured into a paper envelope within a 12" x 12" x 1/2"
horizontal mold and the surface was compressed to ½" with a glass plate. The sample
fully set within ten minutes and was removed from the mold and placed in a 250 C
convection oven. The sample was dried to 75% of its original weight and then placed
in a 50 C convection oven until completely dry.
[0052] Dry ingredients including 1000 g stucco, 20 g Coatmaster K56F
hyrdoxyethylated, acid-modified dent corn starch from Grain Processing Corporation,
and 10 g ground gypsum accelerator were thoroughly mixed together. This mixture
was then added to 1200 g warm (102 F) tap water with two drops of set retarder in a
4L Waring blender. The combination was blended for 10 seconds on "low" setting.
The resulting slurry was poured into a paper envelope within a 12" x 12" x 1/2"
horizontal mold and the surface was compressed to ½" with a glass plate. The sample
fully set within ten minutes and was removed from the mold and placed in a 250 C
convection oven. The sample was dried to 75% of its original weight and then placed
in a 50 C convection oven until completely dry.
[0053] Dry ingredients including 1000 g stucco, 20 g Coatmaster K57F
hyrdoxyethylated, acid-modified dent corn starch from Grain Processing Corporation,
and 10 g ground gypsum accelerator were thoroughly mixed together. This mixture
was then added to 1200 g warm (102 F) tap water with two drops of set retarder in a
4L Waring blender. The combination was blended for 10 seconds on "low" setting.
The resulting slurry was poured into a paper envelope within a 12" x 12" x 1/2"
horizontal mold and the surface was compressed to ½" with a glass plate. The sample
fully set within ten minutes and was removed from the mold and placed in a 250 C


convection oven. The sample was dried to 75% of its original weight and then placed
in a 50 C convection oven until completely dry.
[0054] Dry ingredients including 1000 g stucco, 20 g Coatmaster K58F
hyrdoxyethylated, acid-modified dent com starch from Grain Processing Corporation,
and 10 g ground gypsum accelerator were thoroughly mixed together. This mixture
was then added to 1200 g warm (102 F) tap water with two drops of set retarder in a
4L Waring blender. The combination was blended for 10 seconds on "low" setting.
The resulting slurry was poured into a paper envelope within a 12" x 12" x 1/2"
horizontal mold and the surface was compressed to ½" with a glass plate. The sample
fully set within ten minutes and was removed from the mold and placed in a 250 C
convection oven. The sample was dried to 75% of its original weight and then placed
in a 50 C convection oven until completely dry.
[0055J Dry ingredients including 1000 g stucco, 20 g Coatmaster K500
hyrdoxyethylated, unmodified dent com starch from Grain Processing Corporation,
and 10 g ground gypsum accelerator were thoroughly mixed together. This mixture
was then added to 1200 g warm (102 F) tap water with two drops of set retarder in a
4L Waring blender. The combination was blended for 10 seconds on 'low" setting.
The resulting slurry was poured into a paper envelope within a 12" x 12" x 1/2"
horizontal mold and the surface was compressed to ½" with a glass plate. The sample
fully set within ten minutes and was removed from the mold and placed in a 250 C
convection oven. The sample was dried to 75% of its original weight and then placed
in a 50 C convection oven until completely dry.
[0056] Dry ingredients including 1000 g stucco, 20 g Ethylex 2065
hyrdoxyethylated, acid-modified dent com starch from AE Staley, and 10 g ground
gypsum accelerator were thoroughly mixed together. This mixture was then added to
1200 g warm (102 F) tap water with two drops of set retarder in a 4L Waring blender.
The combination was blended for 10 seconds on "low" setting. The resulting slurry
was poured into a paper envelope within a 12" x 12" x 1/2" horizontal mold and the
surface was compressed to ½" with a glass plate. The sample fully set within ten
minutes and was removed from the mold and placed in a 250 C convection oven. The
sample was dried to 75% of its original weight and then placed in a 50 C convection
oven until completely dry.


[0057] Dry ingredients including 1000 g stucco, 10 g Ethylex 2065
hyrdoxyethylated, acid-modified dent corn starch from AE Staley, and 10 g ground
gypsum accelerator were thoroughly mixed together.. This mixture was then added to
1200 g warm (102 F) tap water with two drops of set retarder in a 4L Waring blender.
The combination was blended for 10 seconds on "low" setting. The resulting slurry
was poured into a paper envelope within a 12" x 12" x 1/2" horizontal mold and the
surface was compressed to ½" with a glass plate. The sample fully set within ten
minutes and was removed from the mold and placed in a 250 C convection oven. The
sample was dried to 75% of its original weight and then placed in a 50 C convection
oven until completely dry.
[0058] Dry ingredients including 1000 g stucco, 30 g Ethylex 2065
hyrdoxyethylated, acid-modified dent corn starch from AE Staley, and 10 g ground
gypsum accelerator were thoroughly mixed together. This mixture was then added to
1200 g warm (102 F) tap water with two drops of set retarder in a 4L Waring blender.
The combination was blended for 10 seconds on "low" setting. The resulting slurry
was poured into a paper envelope within a 12" x 12" x 1/2" horizontal mold and the
surface was compressed to ½" with a glass plate. The sample fully set within ten
minutes and was removed from the mold and placed in a 250 C convection oven. The
sample was dried to 75% of its original weight and then placed in a 50 C convection
oven until completely dry.
[0059] Dry ingredients including 1000 g stucco, 20 g Kollotex
hyrdoxyethylated, acid-modified potato starch from Avebe, and 10 g ground gypsum
accelerator were thoroughly mixed together. This mixture was then added to 1200 g
warm (102 F) tap water with two drops of set retarder in a 4L Waring blender. The
combination was blended for 10 seconds on "low" setting. The resulting slurry was
poured into a paper envelope within a 12" x 12" x 1/2" horizontal mold and the
surface was compressed to ½" with a glass plate. The sample fully set within ten
minutes and was removed from the mold and placed in a 250 C convection oven. The
sample was dried to 75% of its original weight and then placed in a 50 C convection
oven until completely dry.


[0060] Dry ingredients including 1000 g stucco, 20 g acetylated, acid-
modified tapioca starch from Avebe, and 10 g ground gypsum accelerator were
thoroughly mixed together. This mixture was then added to 1200 g warm (102 F) tap
water with two drops of set retarder in a 4L Waring blender. The combination was
blended for 10 seconds on 'low" setting. The resulting slurry was poured into a paper
envelope within a 12" x 12" x 1/2" horizontal mold and the surface was compressed
to ½" with a glass plate. The sample folly set within ten minutes and was removed
from the mold and placed in a 250 C convection oven. The sample was dried to 75%
of its original weight and then placed in a 50 C convection oven until completely dry.
Hydroxypropyl Starches
[0061] Dry ingredients including 1000 g stucco, 20 g PureCote B760
hydroxypropylated, acid-modified dent com starch from Grain Processing
Corporation, and 10 g ground gypsum accelerator were thoroughly mixed together.
This mixture was then added to 1200 g warm (102 F) tap water with two drops of set
retarder in a 4L Waring blender. The combination was blended for 10 seconds on
"low" setting. The resulting slurry was poured into a paper envelope within a 12" x
12" x 1/2" horizontal mold and the surface was compressed to ½" with a glass plate.
The sample fully set within ten minutes and was removed from the mold and placed
in a 250 C convection oven. The sample was dried to 75% of its original weight and
then placed in a 50 C convection oven until completely dry.
[0062] Dry ingredients including 1000 g stucco, 20 g ICBM SE-24
hydroxypropylated, acid-modified dent com starch having 2.34% hydroxypropylation,
and 10 g ground gypsum accelerator were thoroughly mixed together. This mixture
was then added to 1200 g warm (102 F) tap water with two drops of set retarder in a
4L Waring blender. The combination was blended for 10 seconds on "low" setting.
The resulting slurry was poured into a paper envelope within a 12" x 12" x 1/2"
horizontal mold and the surface was compressed to ½" with a glass plate. The sample
fully set within ten minutes and was removed from the mold and placed in a 250 C
convection oven. The sample was dried to 75% of its original weight and then placed
in a 50 C convection oven until completely dry.

Hydrophobically Substituted Starch
[0063] Dry ingredients including 1000 g stucco, 20 g Filmkote
hyrdoxyethylated, acid-modified waxy maize starch from National Starch, and 10 g
ground gypsum accelerator were thoroughly mixed together. This mixture was then
added to 1200 g warm (102 F) tap water with two drops of set retarder in a 4L Waring
blender. The combination was blended for 10 seconds on "low" setting. The resulting
slurry was poured into a paper envelope within a 12" x 12" x 1/2" horizontal mold
and the surface was compressed to ½" with a glass plate. The sample fully set within
ten minutes and was removed from the mold and placed in a 250 C convection oven.
The sample was dried to 75% of its original weight and men placed in a 50 C
convection oven until completely dry.
Hydroxyethyl Control Sample / uniroc example 1
[0064] Uniroc Example 1. Dry ingredients including 1000 g stucco, 200 g
Coatmaster K57F hyrdoxy-ethylated starch from Grain Processing Corporation, 10 g
ground gypsum accelerator, and 5 g sulfonated melamme-formaldehyde dispersant
were thoroughly mixed together. This mixture was then added to 1200 g cold (60 F)
tap water with two drops of set retarder in a 4L Waring blender. The combination was
blended for 10 seconds on "low" setting. The resulting slurry was poured into a 10" x
12" x 1/4" mold and the surface was leveled with a doctor blade. The sample fully set
within ten minutes and was removed from the mold and placed in a 200 C convection
oven. The sample was dried to 75% of its original weight and then placed in a 50 C
convection oven until completely dry.
Glass Fiber
[0065] Uniroc Example 2. Dry ingredients including 1000 g stucco, 200 g
Coatmaster K57F hyrdoxy-ethylated starch from Grain Processing Corporation, 20 g
½" chopped glass strand, 5 g sulfonated melamine-formaldehyde dispersant, and 2 g
ground gypsum accelerator were thoroughly mixed together. This dry mixture was
then added to 1300 g cold (60 F) tap water with two drops of set retarder in a 4L
Waring blender. The combination was blended for 10 seconds on "low" setting. The
resulting slurry was poured into a 10" x 12" x1/4" mold and the surface was leveled


with a doctor blade and covered with a glass plate. The sample fully set within ten
minutes and was removed from the mold and placed in a 200 C convection oven. The
sample was dried to 75% of its original weight and then placed in a 50 C convection
oven until completely dry.
[0066] Uniroc Example 3. Dry ingredients including 1000 g stucco, 100 g
Coatmaster K57F hyrdoxy-ethylated starch from Grain Processing Corporation, 15 g
½" chopped glass strand, 5 g sulfonated melamine-formaldehyde dispersant, and 2 g
ground gypsum accelerator were thoroughly mixed together. This dry mixture was
then added to 1300 g cold (60 F) tap water with two drops of set retardcr in a 4L
Waring blender. The combination was blended for 10 seconds on "low" setting. The
resulting slurry was poured into a 10" x 12" x 1/4" mold and the surface was leveled
with a doctor blade. The sample fully set within ten minutes and was removed from
the mold and placed in a 200 C convection oven. The sample was dried to 75% of its
original weight and then placed in a 50 C convection oven until completely dry.
[0067] Uniroc Example 4 (with cellulose ether). Dry ingredients including
1000 g stucco, 100 g Coatmaster K57F hyrdoxy-ethylated starch from Grain
Processing Corporation, 20 g ½" chopped glass strand, 20 g surface-treated
hydroxylethyl methylcellulose with delayed solubility (HEMC 15kPFR) from
Culminal, 5 g sulfonated melarfline-formaldehyde dispersant, and 2 g ground gypsum
accelerator were thoroughly mixed together. This dry mixture was then added to 1300
g cold (60 F) tap water with two drops of set retarder in a 4L Waring blender. The
combination was blended for 10 seconds on "low" setting. The resulting slurry was
poured into a 10" x 12" x 1/4" mold and the surface was leveled with a doctor blade
and covered with a glass plate. The sample fully set within ten minutes and was
removed from the mold and placed in a 200 C convection oven. The sample was dried
to 75% of its original weight and then placed in a 50 C convection oven until
completely dry.
[0068] Uniroc Example 5 (Wood Fibers). Dry ingredients including 1000 g
stucco, 200 g Coatmaster K57F hyrdoxy-ethylated starch from Grain Processing
Corporation, 60 g wet recycled paper pulp (20 g dry fiber), 5 g sulfonated melamine-
formaldehyde dispersant, and 5 g ground gypsum accelerator were thoroughly mixed
together. This dry mixture was then added to 1300 g cold (60 F) tap water with two


drops of set retarder in a 4L Waring blender. The combination was blended for 10
seconds on "low" setting. The resulting slurry was poured into a 10" x 12" x 1/4" mold
and the surface was leveled with a doctor blade. The sample fully set within ten
minutes and was removed from the mold and placed in a 200 C convection oven. The
sample was dried to 75% of its original weight and then placed in a 50 C convection
oven until completely dry.
[0069] Uniroc Example 6 (Glass & Wood Fibers with cellulose ether). Dry
ingredients including 1000 g stucco, 100 g Coatmaster K57F hyrdoxy-ethylated starch
from Grain Processing Corporation, 30 g wet recycled paper pulp (10 g dry fiber), 20
g surface-treated hydroxylethyl methylcellulose with delayed solubility (HEMC
15kPFR) from Culminal, 10 g ½" chopped glass strand, 5 g sulfonated melamine-
formaldehyde dispersant, and 2 g ground gypsum accelerator were thoroughly mixed
together. This dry mixture was then added to 1300 g cold (60 F) tap water with two
drops of set retarder in a 4L Waring blender. The combination was blended for 10
seconds on "low" setting. The resulting slurry was poured into a 10" x 12" x VA" mold
and the surface was leveled with a doctor blade and covered with a glass plate. The
sample fully set within ten minutes and was removed from me mold and placed in a
200 C convection oven. The sample was dried to 75% of its original weight and then
placed in a 50 C convection oven until completely dry.

WE CLAIM:
1. An organic-inorganic composite comprises:
a substituted starch, such as herein described, having a degree of substitution of at
least one substituent group, such as herein described;
an inorganic phase, such as herein described; and
water, wherein the inorganic phase, the substituted starch and the water
are mixed together to form a mixture, the inorganic phase, is at least partially hydrated
by the water, and the degree of substitution, such as herein described and the at least one
substituent group, such as herein described, are selected such that, the substituted starch
is not soluble during mixing at a mixing temperature, such as herein described, but at
least partially dissolves as the temperature increases during processing of the mixture and
forms a film substantially dispersed throughout the organic-inorganic composite wherein
the organic-inorganic composite is substantially strengthened.
2. The organic-inorganic composite as claimed in claim 1, wherein the at least one
substituent group is selected from substituent groups consisting of an ether substituent
group and an ester substituent group.
3. The organic-inorganic composite as claimed in claim 2, wherein the at least one
substituent group is selected from substituent groups consisting of an ester substituent
group.
4. The organic-inorganic composite as claimed in claim 2, wherein the at least one
substituent group is selected from substituent groups consisting of an ether substituent
group.
5. The organic-inorganic composite as claimed in claim 1, wherein the at least one
substituent group is selected from substituent groups consisting of an alkyl substituent
group, an ethyl succinate substituent group, a cationic substituent group, an anionic
substituent group, and combinations thereof, such as herein described .
6. The organic-inorganic composite as claimed in claim 1, wherein the substituted
starch is hydroxyethylated, hydroxypropylated, or acetylated.
7. The organic-inorganic composite as claimed in claim 1 , wherein the at least one
substituent group is selected such that the substituted starch is film-forming and
hydrophilic such that the substituted starch forms a film on the hydrated inorganic phase.
8. The organic-inorganic composite as claimed in claim 1, wherein the substituted
starch forms a percolating, polymeric film.
9. The organic-inorganic composite as claimed in claim 1 , wherein the at least one
substituent group and the degree of substitution is selected such that a weight percent
solids at a viscosity of 1000 cps is at least 4 percent.
10. The organic-inorganic composite as claimed in claim 9, wherein the at least one


substituent group and tbe degree of substitution is selected such that a weight percent
solids at a viscosity of 1000 cps and a temperature of 150 degrees Fahrenheit is in a range
from 9 percent to 43 percent.
11. The organic-inorganic composite as claimed in claim 9, wherein the at least one
substituent group is a hydoxypropyl group and the degree of substitution is selected such
that a weight percent solids at a viscosity of 1000 cps an a temperature of 150 degrees
Fahrenheit is in a range from 14 percent to 20 percent.
12. The organic-inorganic composite as claimed in claim 9. wherein the at least one
substituent group is a hydroxyethyl group and the degree of substitution is selected such
that a weight percent solids at a viscosity of 1000 cps and a temperature of 150 degrees
Fahrenheit is in a range from 17 percent to 30 percent.
13. The organic-inorganic composite as claimed in claim 12, wherein the degree of
substitution of the hydroxyethyl group is selected such that a weight percent solids at a
viscosity of 1000 cps and a temperature of 150 degrees Fahrenheit is in a range from 17
percent to 21 percent
14. The organic-inorganic composite as claimed in claim 12, wherein the degree of
substitution is less than 0.3.
15. The organic-inorganic composite as claimed in claim 12, wherein the degree of
substitution is less than 6 weight percent.
16. The organic-inorganic composite as claimed in claim 12, wherein the degree of
substitution is selected in a range from 1 to 3 weight percent.
17. The organic-inorganic composite as claimed in claim 1, wherein the substituted
starch is at least partially comprised of amylopectin.
18. The organic-inorganic composite as claimed in claim 17, wherein the substituted
starch is substantially amylopectin.
19. The organic-inorganic composite as claimed in claim 1, wherein substantially all
of the substituted starch is dissolved and forms a polymeric film.
20. The organic-inorganic composite as claimed in claim 1, wherein the substituted
starch is of a hydrophobically-modified. acid-thinned waxy maize starch.
21. The organic-inorganic composite as claimed in claim 1, wherein the substituted
starch is of an acid-thinned starch and the at least one substituent group is of an
hydroxypropyl group.
22. The organic-inorganic composite as claimed in claim 21, wherein the degree of
substitution is selected in a range from 1.5 to 2.5 weight percent hydroxypropyl.
23. The organic-inorganic composite as claimed in claim 1, wherein the substituted

starch is of an acetylized, acid-thinned waxy maize starch.
24. The organic-inorganic composite as claimed in claim 1, wherein the amount of
substituted starch is no greater than 2 weight percent of the weight of the substituted
starch and inorganic phase.
25. The organic-inorganic composite as claimed in claim 1, comprising fibers
dispersed substantially throughout the organic-inorganic composite.
26. The organic-inorganic composite as claimed in claim 25, wherein the fibers are
glass fibers.
27. The organic-inorganic composite as claimed in claim 1, comprising a cellulose
ether additive selected such that a synergistic improvement in flexural strength is
achieved.
28. The organic-inorganic composite as claimed in claim 27, wherein the cellulose
ether is selected from the group of cellulose ethers consisting of hydroxypropylmethyl
cellulose, methyl cellulose, hydroxyethylmethyl cellulose, hydroxyethyl cellulose,
hydroxypropyl cellulose, cationic cellulose, carboxymethyl cellulose and combinations
thereof.
29. The organic-inorganic composite as claimed in claim 28, wherein the cellulose
ether is of hydroxpropylmethyl cellulose.
30. A method of preparing an organic-inorganic composite article using a process
having a mixing temperature range, the method comprising:
selecting a substituted starch, such as herein described, having a degree of
substitution, a degree of polymerization, and at least one substituent group, such as herein
described, such that the substituted starch is insoluble in water in the mixing temperature
range;
mixing the substituted starch, an inorganic phase, such as herein described, and
water in a continuous process at a temperature within the mixing temperature range:
forming the composite article;
hydrating at least a portion of the inorganic phase;
raising the temperature above the mixing temperature range, wherein the
substituted starch at least partially dissolves in the water; and
setting and drying the composite article such that the substituted starch forms a
continuous polymeric film within the composite article.


An inorganic-organic composite comprises an inorganic phase, such as gypsum crystals, and a film forming organic
phase. The film forming organic phase is selected from substituted starches having a degree of polymerization; degree of substitution
and viscosity such that the substituted starches are insoluble in water during mixing but dissolve at a higher processing temperature
during forming, setting or drying of the composite. Thus, excessive migration of the substitute starch is prevented and the composite
is substantially strengthened.

Documents:

01652-kolnp-2006 assignment.pdf

01652-kolnp-2006 correspondence others-1.1.pdf

01652-kolnp-2006 form-3-1.1.pdf

01652-kolnp-2006 generalpower of authority.pdf

01652-kolnp-2006-abstract.pdf

01652-kolnp-2006-claims.pdf

01652-kolnp-2006-correspondence other.pdf

01652-kolnp-2006-description (complete).pdf

01652-kolnp-2006-drawings.pdf

01652-kolnp-2006-form-1.pdf

01652-kolnp-2006-form-3.pdf

01652-kolnp-2006-form-5.pdf

01652-kolnp-2006-international publication.pdf

01652-kolnp-2006-international search authority report.pdf

01652-kolnp-2006-pct form.pdf

01652-kolnp-2006-priority document.pdf

1652-KOLNP-2006-(21-12-2011)-ASSIGNMENT.pdf

1652-KOLNP-2006-(21-12-2011)-CORRESPONDENCE.pdf

1652-KOLNP-2006-(21-12-2011)-FORM-16.pdf

1652-KOLNP-2006-(21-12-2011)-FORM-3.pdf

1652-KOLNP-2006-(21-12-2011)-PA-CERTIFIED COPIES.pdf

1652-KOLNP-2006-AMENDED PAGES.pdf

1652-kolnp-2006-assignment.pdf

1652-KOLNP-2006-CANCELLED PAGES.pdf

1652-KOLNP-2006-CORRESPONDENCE-1.1.pdf

1652-KOLNP-2006-CORRESPONDENCE-1.2.pdf

1652-kolnp-2006-correspondence-1.3.pdf

1652-kolnp-2006-examination report.pdf

1652-KOLNP-2006-FORM 1.1.1.pdf

1652-kolnp-2006-form 18.pdf

1652-kolnp-2006-form 3.pdf

1652-kolnp-2006-form 5.pdf

1652-KOLNP-2006-FORM-27.pdf

1652-kolnp-2006-gpa.pdf

1652-kolnp-2006-granted-abstract.pdf

1652-kolnp-2006-granted-claims.pdf

1652-kolnp-2006-granted-description (complete).pdf

1652-kolnp-2006-granted-drawings.pdf

1652-kolnp-2006-granted-form 1.pdf

1652-kolnp-2006-granted-specification.pdf

1652-kolnp-2006-others-1.1.pdf

1652-KOLNP-2006-OTHERS.pdf

1652-KOLNP-2006-PCT REQUEST FORM.pdf

1652-kolnp-2006-reply to examination report-1.1.pdf

1652-KOLNP-2006-REPLY TO EXAMINATION REPORT.pdf

1652-KOLNP-2006-SCHEDUAL-ANNEXURE FORM 3.pdf

1652-KOLNP-2006PETITION UNDER RULE 137.pdf


Patent Number 246020
Indian Patent Application Number 1652/KOLNP/2006
PG Journal Number 06/2011
Publication Date 11-Feb-2011
Grant Date 09-Feb-2011
Date of Filing 14-Jun-2006
Name of Patentee INNOVATIVE CONSTRUCTION AND BUILDING MATERIALS, LLC.
Applicant Address 626, BANCROFT WAY, SUITE 3B, BERKELEY, CA
Inventors:
# Inventor's Name Inventor's Address
1 POLLOCK, JACOB FREAS 1622, WOOLSEY STREET, BERKELEY, CA 94703
2 SAITO, KEN 2612, HILLEGASS AVENUE, #3, BERKELEY, CA 94704
3 TAGGE, CHRISTOPHER D. 1124, CEDAR STREET, SAN CARLOS, CA 94070
PCT International Classification Number C04B 24/10
PCT International Application Number PCT/US2004/041514
PCT International Filing date 2004-12-10
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 60/553,423 2004-03-15 U.S.A.
2 60/528,595 2003-12-10 U.S.A.
3 60/603,491 2004-08-20 U.S.A.
4 10/952,122 2004-09-27 U.S.A.