Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
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DESCRIPTION TITLE: CLOSED CELL GEOPOLYMER FOAM
[00011The invention belongs to the field of geopolymers and more particularly
to that of mineral
foams.
[0002]The invention relates to an incombustible and thermally insulating
mineral foam.
[0003 ]The invention also relates to the method for manufacturing said foam,
as well as the
intermediate composition designed to form the foam.
[00041The invention also relates to insulated or sealed doors or pipes and
other supports upon
which is applied, or upon which is comprised, said foam.
[0005]Finally, the invention relates to a kit comprising said intermediate
composition as well as a
pozzolanic material.
Prior art
[0006]Geopolymer foams are known from the prior art. Geopolymer foams have
many advantages,
the main one being that instead of the carbon chain of conventional polymers,
mineral material
composed of silica and alumina is used. They are therefore inorganic polymers
composed of
mineral matter such as silica and alumina.
[0007]In the context of this invention, by geopolymer is meant an inorganic
polymer essentially
composed of units, silico-oxide (-Si-O-Si-0-), silico-aluminate (-Si-O-A1-0-),
ferro-silico-
aluminate (-Fe-O-Si-O-A1-0-) or aluminum-phosphate (-A1-0-P-0-), created by a
process called
g eopo lymeri zati on.
[0008]Geopolymers, by their nature, find applications in the field of
construction, in particular for
the manufacture of cements and concrete or even fire protection. These mineral
foams are of
particular interest due to their low density and their insulating and fire-
resistant properties which
make them suitable for use in the construction of walls, doors, insulation
panels and may also be
used to insulate, seal or repair pipes, furnaces and other systems subjected
to high temperatures.
These latter uses imply that the foam forms and hardens quickly (in a few
minutes to a few tens of
minutes) so that it may be applied directly to the area to be isolated or
sealed.
[0009]The incombustible mineral foams of the invention can in particular be
prepared from an
inorganic binder such as metakaolin, a natural pozzolanic material. The term -
metakaolin" is
understood to mean a thermally dehydroxylated kaolinite clay. In other words,
it is a
dehydroxylated alumina silicate of general composition Al2O3, 2Si02.
[000101It is known that one can prepare a geopolymer in the form of a mineral
foam by mixing an
inorganic binder with a so-called activation solution, most often comprising
alkali metal
hydroxides, then adding thereto an expanding agent which will form a gas in
situ. The generation
of gas will create gas bubbles in the liquid phase and form a foam, while the
reaction of the
inorganic binder with the activating solution most often accelerated by the
addition of a hardener
Date Recue/Date Received 2021-03-30
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(for example a Ca2+ donor) causes rapid hardening, the result of
polymerization, which then freezes
the network of bubbles or the porosity. The product obtained is a rigid and
porous foam.
[000111Geopolymer foams can also be made with an external gas supply unlike
foams made by in
situ gas generation. Generally speaking, foams with an external gas supply are
made in two stages.
On the one hand, an aqueous foam is made from water and surfactants, on the
other hand, a slurry
of the inorganic binder is made. A foam is thus obtained resulting from the
mixture of the slurry
with the aqueous foam, which will gradually solidify over a relatively long
period depending on
the inorganic binder used. It is also possible to manufacture a geopolymer
foam in a single step by
mixing an inorganic binder with an activating solution to which foaming agents
are added. Using
different tools, a gas (for example air), is then introduced to the suspension
obtained. The
manufacture of foam using an external gas supply requires obtaining a very
stable foam not only
over time but also vis-à-vis the phenomena of coalescence or disappearance of
bubbles or
microbubbles of gas after injection and dispersion of the latter.
[000121FR3027023 discloses foams prepared from metakaolin, one or more natural
or synthetic
foaming agents of animal or plant origin. In particular, this application
targets foaming agents of
the protein type.
[000131W02015062860 discloses foams based on metakaolin and further comprising
a surfactant.
The authors recommend the use of nonionic surfactants, such as alkyl
polyglucosides for
stabilization of the foam. A supply of gas is preferred over gas generation in
situ. Fibers acting as
fillers may be used in order to improve the mechanical stability of the
hardened foam, these fibers
preferably having a millimetric length of a maximum of 120 mm, particularly a
maximum of 6
mm.
[0001410E102004006563 discloses organic/inorganic hybrid foams comprising
surfactants. In
particular, the surfactants are amine oxides and alkyl sulfates.
[000151US2015060720 or W02015062819 disclose methods of preparing a fast
curing (less than
minutes) inorganic foam. The blowing agent has the distinction of being scrap
aluminum
powder, which is a mixture of aluminum powder, aluminum nitride and aluminum
oxide.
[000161W02018091482 discloses a metakaolin-based foam comprising the
combination of 2
types of anionic and nonionic surfactants. The foam is formed by generating
gas in situ. Fibers
acting as fillers may be used, their lengths being less than 5 mm.
[000171W02017138913 discloses a composition of cement foam comprising a
hydraulic cement,
water, a foam-generating surfactant, a gas and stabilizing cellulose
nanofibers (CNF) of a size
between 35 and 10,000 nm. The CNFs are obtained by high-energy complex
grinding methods
and/or chemical or enzymatic pretreatments, as opposed to cellulose fibers of
micrometric sizes
Date Recue/Date Received 2021-03-30
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obtained generally through wet grinding and selection that possess a simple
morphology without
crystallinity or ramification.
[000181The Prud'homme et al. Eur. Phys. J. Special Topics 224, 1725-1735
(2015) publication
discusses the control of the porosity and thermal properties of geopolymer
material either by
modification of the formula or by adding additives, the second option being
considered as the most
promising. The influence of the additives on the mass of the samples is
debated, figure 7 shows
that the increase of the mass of the foam increases the thermal conductivity
up until a certain point,
and that the use of additives such as carbo fibers, cellulose fibers or starch
increases the mass of
the foam and also increases the thermal conductivity.
[000191W02017174560A1 discloses a geopolymer foam comprising cellulose
nanofibers used for
sound-absorbing applications. The disclosed foam possesses a majority of open
cells due to the
precise quantity of cellulose nanofibers.
The disadvantage of the mineral foams of the prior art is their open-cell
nature resulting in high
thermal conductivity. Open cells or pores are cells that are interconnected or
have open binding
channels. These open channels more or less connect the cells. The thermal
conductivity of a foam
is dependent on the porosity of the system and is therefore determined by the
path of the air through
the composition. The air path through an open cell foam is facilitated
resulting in an increase in
thermal conductivity.
[00020]The Applicant has surprisingly demonstrated that the use of micrometric
lengths of fibers
combined with the use of a specific amount of surfactants, gives mineral foam
a perfectly stable
closed-cell nature, and consequently a relatively low thermal conductivity.
[000211None of the abovementioned documents address the relationship between
the size of the
fibers and the foam cellularity, nor the means of obtaining the closed-cell
mineral foams having
a low thermal conductivity.
[00022]The properties of the foams according to the invention are as follows:
- incombustible foams;
- better control of foam mass;
- better control of cell density and size;
- better surface appearance (skin);
- reduced risk of cracks.
The incombustible mineral foams according to the invention may be used as fire
barriers and
comply with Al according to the "reaction to fire" and "resistance to fire"
standards, NF EN ISO
1182 and 1716 respectively. They have a thermal resistance up to at least 1200
C.
Date Recue/Date Received 2021-03-30
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Description of the Figures
[00023]Figure 1: Surface appearance of 3 samples of geopolymer foams
respectively comprising
from A to C no fibers, micrometric lengths of fibers, and millimetric lengths
of fibers used as
fillers.
Detailed Description of the Invention
[00024]The invention consists of a geopolymer foam comprising:
- from 50% to 90% by mass of pozzolanic material polymerized relative to
the total mass of
said foam;
- from 0.01% to 2%, by mass of at least one surfactant relative to the
total mass of said foam;
- from 1% to 20% by mass of fibers with lengths of between 5 and 1500 pm
relative to the
total mass of said foam.
[00025]The term -fibers" is understood to mean an element of elongated or
extended shape. In the
present application, the length of a fiber is considered to be of an average
length.
[00026]"Polymerized pozzolanic material" is understood to be a geopolymer
formed by the
reaction of a pozzolanic material with an activating solution (e.g., a basic
solution).
[000271In one embodiment, the geopolymer foam according to the invention is
characterized in
that the pozzolanic material is metakaolin.
[000281In one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises from 55% to 85% by mass of polymerized pozzolanic material
relative to the
total mass of said foam.
[000291In one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises from 60% to 80% by mass of polymerized pozzolanic material
relative to the
total mass of said foam.
[000301In one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises from 65% to 75% by mass of polymerized pozzolanic material
relative to the
total mass of said foam.
[000311In one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises from 0.01% to 1.5% by mass of at least one surfactant
relative to the total mass
of said foam.
[000321In one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises from 0.01% to 1% by mass of at least one surfactant relative
to the total mass of
said foam.
[00033]Preferably, the geopolymer foam according to the invention is
characterized in that it
comprises from 0.01 to 0.5% by mass of at least one surfactant relative to the
total mass of said
foam.
Date Recue/Date Received 2021-03-30
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[000341In one embodiment, the geopolymer foam according to the invention is
characterized in
that the at least one surfactant is selected from the group consisting of
anionic surfactants, nonionic
surfactants, and mixtures thereof.
[00035]The term -anionic surfactant" is intended to mean a surfactant which
releases a negative
charge in aqueous solution. The class of anionic surfactants is widely
described in the literature.
[000361In one embodiment, the geopolymer foam according to the invention is
characterized in
that the at least one surfactant is selected from the group consisting of
anionic surfactants, nonionic
surfactants, and mixtures thereof.
[00037]The term ``nonionic surfactant" is understood to mean a surfactant
whose molecules have
no net charge. The class of nonionic surfactants is widely described in the
literature.
[0003 811n one embodiment, the geopolymer foam according to the invention is
characterized in
that the nonionic surfactants are selected from alkyl polyglucosides (D-
glucopyranose, oligomers,
alkyl glucosides).
[000391In one embodiment, the geopolymer foam according to the invention is
characterized in
that the nonionic surfactants are selected from alkyl polyglucosides (D-
glucopyranose, oligomers,
alkyl glucosides).
[00040]The term -alkyl-poly-glucoside" is understood to mean a nonionic
surfactant having the
formula: H-(C6H1005) m-O-R1, in which (C6H1005) is a glucose unit and R1 is a
C6-C22 alkyl
group, preferably C8-C16 and C8-C10, and m is a positive integer between 1 and
10, l< m < 10.
[000411In one embodiment, the alkyl polyglucosides are those marketed by the
company SEPPIC,
such as SIMULSOL SL8 (D-glucopyranose, oligomers, decyl octyl glycosides, 01-
2119488530-
36, CE: 500-200-1), or SIMULSOL SL 826 (D-glucopyranose, oligomers, decyl
octyl glycosides,
01-2119488530-36, CE: 500-200-1, D-Glucopyranose, oligomeric, C10-16 (even
numbered)-
alkyl glycosides,
01-2119489418-23, CE: 600-975-8, (2-methoxymethylethoxy) propanol,
012119450011-60, CE:
252-104-2, dodecan-l-ol, 01-2119485976-15, EC: 203-982-0) or SIMULSOL SL26 (D-
Glucopyranose, oligomeric, C10-16 (even numbered) alkyl glycosides, 01-
2119489418-23, CE:
600-975-8) or mixtures thereof.
[000421In one embodiment, the alkyl polyglucosides SIMULSOL SL 8, SL 826 and
SL26 are in
preferential ratios of 50: 50 for the couple SL8: SL826 and 50: 2.5: 47.5 for
that of SL8: SL26:
SL826.
[000431In one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises from 1% to 17% by mass of fibers with lengths of between 5
and 1500 gm relative
to the total mass of said foam.
Date Recue/Date Received 2021-03-30
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[000441In one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises from 1% to 15% by mass of fibers with lengths of between 5
and 1500 gm relative
to the total mass of said foam.
[00045] In one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises from 1% to 12% by mass of fibers with lengths of between 5
and 1500 gm relative
to the total mass of said foam.
[000461In one embodiment, the geopolymer foam according to the invention is
characterized in
that the fibers have lengths between 5 and 1000 pm.
[000471In one embodiment, the geopolymer foam according to the invention is
characterized in
that the fibers have lengths between 10 and 800 pm.
[000481In one embodiment, the geopolymer foam according to the invention is
characterized in
that the fibers have lengths between 5 and 50 pm.
[000491In one embodiment, the geopolymer foam according to the invention is
characterized in
that the fibers have lengths between 10 and 40 pm.
[000501In one embodiment, the geopolymer foam according to the invention is
characterized in
that the fibers have lengths between 15 and 30 pm.
[0005 liln one embodiment, the geopolymer foam according to the invention is
characterized in
that the fibers are selected from the group consisting of plant fibers, animal
fibers, mineral fibers,
semi-synthetic fibers, polymeric fibers.
[000521In one embodiment, the geopolymer foam according to the invention is
characterized in
that the fibers are not cellulose nanofibers (CNF).
[00053] In one embodiment, the geopolymer foam according to the invention is
characterized in
that the fibers do not have dimensions in the nanometer range. This is
understood to mean that no
fiber has an average length of less than 1 gm.
[000541In one embodiment, the geopolymer foam according to the invention is
characterized in
that the fibers are cellulose fibers.
[00055]Preferably, the cellulose fibers possess at least one of the following
characteristics:
- They are made from paper pulp, made from wood from renewable resources.
- They have an average diameter of approximately 25 pm.
- They have an apparent mass between 20 and 250 g/L.
- They are resistant to temperatures of up to 150 C, briefly up to
approximately 200 C.
- They have a high absorption and retention of liquid media.
- They have a high traction resistance.
- They are insoluble in water and oil and are not comparable to cellulose
derivatives soluble in
water such as carboxymethyl cellulose (CMC).
Date Recue/Date Received 2021-03-30
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- They are inert to acids and alkalis in a range of pH values from 4 to 12.
[00056] The use of micrometric lengths of fibers contributes significantly to
increasing the density
of the cells or pores, as well as the stability of the foam in its liquid
phase before curing.
[000571In one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises at least one hydrophobic agent.
[000581In one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 1% to 20% by mass of at least one hydrophobic
agent relative to the
total mass of said foam.
[000591In one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 1% to 15% by mass of at least one hydrophobic
agent relative to the
total mass of said foam.
[00060]In one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 1% to 10% by mass of at least one hydrophobic
agent relative to the
total mass of said foam.
[00061]In one embodiment, the geopolymer foam according to the invention is
characterized in
that the at least one hydrophobic agent is selected from the group consisting
of siliconates, silanes,
siloxanes and mixtures thereof.
[000621In one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises at least one thickener.
[00063]The term "thickener" is understood to mean a substance intended to
modulate/increase the
viscosity of a composition.
[000641In one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 1 to 25% by mass of at least one thickener
relative to the total mass
of said foam.
[000651In one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 1 to 20% by mass of at least one thickener
relative to the total mass
of said foam.
[000661In one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 1 to 15% by mass of at least one thickener
relative to the total mass
of said foam.
[000671In one embodiment, the foam is characterized in that the at least one
thickener is selected
from the group consisting of chemically modified water-soluble starches such
as pre-frozen starch,
salts of carboxymethylated starches and adipates of acetylated distarch,
galactomannans such as
guar gum, xanthan gum, mineral fillers such as kaolinite clays, cellulose
derivatives such as methyl
ethyl cellulose, and mixtures thereof.
Date Recue/Date Received 2021-03-30
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[00068]The term -kaolinite" is understood to be a hydrated alumina silicate
constituting one of the
main clay minerals and forming the essential element of kaolin.
[0006911n one embodiment the at least one thickener is a mineral filler.
[00070]Mineral fillers are used to improve the mechanical characteristics, the
refractory
properties, as well as the material price of mineral foams. Preferably the
inorganic filler is kaolinite
clay as it is used to produce metakaolin and it does not react under the
action of the activating
solution under the conditions of foam manufacturing procedures.
[0007 liln one embodiment the at least one thickener is a chemically modified
starch.
[00072]Preferably the chemically modified starch is a pre-frozen starch.
[0007311n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises at least one protein or a mixture of animal or plant
proteins selected from
the group consisting of albumin, keratin hydrolysates such as extracts of
keratin from animal
hooves and/or horns, and mixtures thereof.
[0007411n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 0.1% to 10% by mass of the at least one protein
or a mixture of
animal or plant proteins selected from the group consisting of albumin,
keratin hydrolysates such
as extracts of keratin from animal hooves and/or horns, and mixtures thereof,
relative to the total
mass of said foam.
[0007511n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 0.1% to 7% by mass of the at least one protein
or a mixture of animal
or plant proteins selected from the group consisting of albumin, keratin
hydrolysates such as
extracts of keratin from animal hooves and/or horns, and mixtures thereof,
relative to the total
mass of said foam.
[0007611n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 0.1% to 5% by mass of the at least one protein
or a mixture of animal
or plant proteins selected from the group consisting of albumin, keratin
hydrolysates such as
extracts of keratin from animal hooves and/or horns, and mixtures thereof,
relative to the total
mass of said foam.
[00077]Preferably the at least one protein or mixture of animal or vegetable
proteins are keratin
hydrolysates.
[00078]The use of keratin hydrolysates facilitates the entrainment of air
during the manufacture
of the foam and provides a lubricating effect which allows better flow of the
foam at densities less
than or equal to 200 Kg/m3.
[0007911n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises at least one pH buffer.
Date Recue/Date Received 2021-03-30
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[0008011n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 0,1% to 15% by mass of at least one pH buffer
relative to the total
mass of said foam.
[000811In one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 0,1% to 10% by mass of at least one pH buffer
relative to the total
mass of said foam.
[0008211n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 0.1% to 7% by mass of at least one pH buffer
relative to the total
mass of said foam.
[0008311n one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises at least one pH buffer, selected from the group consisting
of monocalcium
phosphate, bicalcium phosphate, citric acid, citrate, gamma butyrolactone
esters, glyceryl
triacetate, glycerol and mixtures thereof.
[0008411n one embodiment, the geopolymer foam according to the invention is
characterized in
that the at least one pH buffer is bi-calcium phosphate.
[0008511n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises at least one set-accelerator.
[0008611n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 0.1% to 8% by mass of at least one set-
accelerator relative to the
total mass of said foam.
[0008711n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 0.1% to 6% by mass of at least set-accelerator
relative to the total
mass of said foam.
[0008811n one embodiment, the geopolymer foam according to the invention is
characterized in
that it further comprises from 0.1% to 4% by mass of at least one set-
accelerator relative to the
total mass of said foam.
[0008911n one embodiment, the geopolymer foam according to the invention is
characterized in
that it comprises at least one set-accelerator selected from the group
consisting of Portland cement,
plaster of Paris, calcium hydroxide, hydrated lime, and mixtures thereof.
[0009011n one embodiment, the geopolymer foam according to the invention is
characterized in
that the at least one set-accelerator is hydrated lime.
[00091]The addition of a set-accelerator allows the foam produced at the exit
of the machine to
solidify in less than an hour to half an hour, thus freezing the distribution
of gas microbubbles, i.e.,
cells or pores, this being a determining factor for obtaining good thermal
insulation properties.
Date Recue/Date Received 2021-03-30
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[000921In one embodiment, the geopolymer foam according to the invention is
characterized in
that the thermal conductivity is between 0.025 and 0.05 W.m-2.K.
[000931In one embodiment, the geopolymer foam according to the invention is
characterized in
that its density is between 80 and 300 Kg/m3.
[000941In one embodiment, the geopolymer foam according to the invention is
characterized in
that its density is between 100 and 150 Kg/m3.
[000951In one embodiment, the foam according to the invention is characterized
in that it has a
thermal resistance greater than 900 C, preferably greater than 1000 C and even
more preferably
up to at least 1200 C.
[00096]The invention also relates to any support such as for example a fire
door, an insulating
panel, a furnace, a pipe, which comprises or upon which is affixed an
incombustible inorganic
foam as defined above. The support on which is affixed a non-combustible
inorganic foam as
defined above can be made of any material selected from organic, inorganic or
metallic materials,
such as for example a wooden board, a brick or a metal beam.
[00097]The invention also relates to a process for preparing a geopolymer foam
comprising the
following steps:
a) Place in contact within an aqueous solution,
O at least one pozzolanic material,
O an activation solution comprising at least one soluble metal hydroxide,
O at least one silicate,
O at least one surfactant,
O fibers with lengths of between 5 and 1500 gm.
b) Mix by stirring and obtaining a suspension,
c) Introduction of a gas,
d) Hardening.
[000981In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the at least one soluble metal hydroxide is an alkali metal hydroxide.
[00099]Preferably, the at least one alkali metal hydroxide is selected from
the group consisting of
sodium hydroxide and potassium hydroxide, alone or in combination.
[0001001In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of the at least one surfactant relative to the total mass of the
suspension obtained in
step b) is between 0.03% and 0.6%.
[0001011In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of the at least one surfactant relative to the total mass of the
suspension obtained in
step b) is between 0.03% and 0.45%.
Date Recue/Date Received 2021-03-30
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[0001021In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of the at least one surfactant relative to the total mass of the
suspension obtained in
step b) is between 0.03% and 0.3%.
[0001031Preferably, in one embodiment, the process for preparing a geopolymer
foam is
characterized in that the amount of the at least one surfactant relative to
the total mass of the
suspension obtained in step b) is between 0.03 and 0.15%.
[0001041In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of fibers with lengths of between 5 and 1500 gm relative to the
total mass of the
suspension obtained in step b) is between 1% and 10%.
[0001051In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of fibers with lengths of between 5 and 1500 gm relative to the
total mass of the
suspension obtained in step b) is between 1% and 8%.
[0001061In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of fibers with lengths of between 5 and 1500 gm relative to the
total mass of the
suspension obtained in step b) is between 2% and 7%.
[0001071In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of fibers with lengths of between 5 and 1500 gm relative to the
total mass of the
suspension obtained in step b) is between 3% and 6%.
[0001081In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the fibers have lengths between 5 and 1000 gm.
[0001091In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the fibers have lengths between 10 and 800 gm.
[00011011n one embodiment, the process for preparing a geopolymer foam is
characterized in that
the fibers have a diameter of between 5 and 50 gm.
[00011111n one embodiment, the process for preparing a geopolymer foam is
characterized in that
the fibers have a diameter of between 10 and 40 gm.
[0001121In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the fibers have a diameter of between 15 and 30 gm.
[0001131In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the fibers are cellulose fibers.
[0001141In one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of the pozzolanic material relative to the total mass of the
suspension obtained in step
b) is between 20% and 60%.
Date Recue/Date Received 2021-03-30
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[00011511n one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of the pozzolanic material relative to the total mass of the
suspension obtained in step
b) is between 25% and 55%.
[00011611n one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of the pozzolanic material relative to the total mass of the
suspension obtained in step
b) is between 30% and 50%.
[00011711n one embodiment, the process for preparing a geopolymer foam is
characterized in that
the amount of the pozzolanic material relative to the total mass of the
suspension obtained in step
b) is between 35% and 45%.
[00011811n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step a), the pozzolanic material is metakaolin.
[00011911n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step a) at least one hydrophobic agent is added.
[00012011n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step a) at least one hydrophobic agent from 2% to 10% by mass relative to
the total mass of the
suspension obtained in step b) is added.
[00012111n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step a) at least one hydrophobic agent from 2% to 8% by mass relative to
the total mass of the
suspension obtained in step b) is added.
[00012211n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step a) at least one hydrophobic agent from 2% to 6% by mass relative to
the total mass of the
suspension obtained in step b) is added.
[0001231In one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step a) at least one thickener from 1% to 10% by mass relative to the total
mass of the suspension
obtained in step b) is added.
[00012411n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step a) at least one thickener is added.
[00012511n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step a) at least one thickener from 1% to 8% by mass relative to the total
mass of the suspension
obtained in step b) is added.
[00012611n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step a) at least one thickener from 3 to 7% by mass relative to the total
mass of the suspension
obtained in step b) is added.
[00012711n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step b) the stirring is carried out using a deflocculating disc dispenser.
Date Recue/Date Received 2021-03-30
13
[0001281The stirring speed is adapted based on the dimensions of the disc and
the tank.
[00012911n one embodiment, the process for preparing a geopolymer foam is
characterized in that
between step b) and c) at least one protein or a mixture of animal or plant
proteins selected from
the group consisting of albumin, keratin hydrolysates such as extracts of
keratin from animal
hooves and/or horns, and mixtures thereof is added.
[00013011n one embodiment, the process for preparing a geopolymer foam is
characterized in that
between step b) and c) between 0.1% to 4% by mass of at least one protein or
one mixture of
animal or vegetable proteins selected from the group consisting of albumin,
keratin hydrolysates
such as extracts of keratin from animal hooves and/or horns, and mixtures
thereof, relative to the
total mass of the suspension obtained in step b) is added.
[00013 On one embodiment, the process for preparing a geopolymer foam is
characterized in that
between step b) and c) between 0.1% to 3% by mass of at least one protein or
one mixture of
animal or vegetable proteins selected from the group consisting of albumin,
keratin hydrolysates
such as extracts of keratin from animal hooves and/or horns, and mixtures
thereof, relative to the
total mass of the suspension obtained in step b) is added.
[00013211n one embodiment, the process for preparing a geopolymer foam is
characterized in that
between step b) and c) between 0.1% to 2% by mass of at least one protein or
one mixture of
animal or vegetable proteins selected from the group consisting of albumin,
keratin hydrolysates
such as extracts of keratin from animal hooves and/or horns, and mixtures
thereof, relative to the
total mass of the suspension obtained in step b) is added.
[0001331In one embodiment, the process for preparing a geopolymer foam is
characterized in that
between step b) and c) at least one set-accelerator is added.
[00013411n one embodiment, the process for preparing a geopolymer foam is
characterized in that
between step b) and c) at least one set-accelerator from 0.1% to 4% by mass
relative to the total
mass of the suspension obtained in step b) is added.
[00013511n one embodiment, the process for preparing a geopolymer foam is
characterized in that
between step b) and c) at least one set-accelerator from 0.1% to 3% by mass
relative to the total
mass of the suspension obtained in step b) is added.
[00013611n one embodiment, the process for preparing a geopolymer foam is
characterized in that
between step b) and c) at least one set-accelerator from 0.1% to 2% by mass
relative to the total
mass of the suspension obtained in step b) is added.
[00013711n one embodiment, the process for preparing a geopolymer foam is
characterized in that
between step b) and c) the at least one set-accelerator is hydrated lime.
[0001381The term -gas" is understood to mean any body which is in the state of
an expandable
and compressible fluid (gaseous state) under normal temperature and pressure
conditions.
Date Recue/Date Received 2021-03-30
14
[00013911n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step c), the gas is air.
[00014011n one embodiment, the process for preparing a geopolymer foam is
characterized in that
in step c) the introduction of gas is carried out using an expansion machine.
[0001411The use of an expansion machine, also called an aerator/mixer, with a
dynamic or static
expansion unit, preferably dynamic, ensures control over the definition of the
densities of the foam,
the density and the size of the cells present in it through flow controls,
which are desirable
characteristics for non-combustible foams according to industrial
applications.
[0001421The invention also relates to a composition for the preparation of a
geopolymer foam
comprising:
- an alkaline activation solution comprising at least one soluble metal
hydroxide,
- at least one silicate;
- at least one surfactant,
- fibers with lengths of between 5 and 1500 gm.
[00014311n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that the at least one soluble metal hydroxide is an alkali metal hydroxide.
[000144]Preferably, the at least one alkali metal hydroxide is selected from
the group consisting
of sodium hydroxide and potassium hydroxide, alone or in combination.
[00014511n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it comprises at least one surfactant from 0.03% to 0.6% by mass
relative to the total mass
of said composition.
[00014611n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it comprises at least one surfactant from 0.03% to 0.45% by mass
relative to the total mass
of said composition.
[00014711n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it comprises at least one surfactant from 0.03% to 0.3% by mass
relative to the total mass
of said composition.
[00014811n one embodiment, the composition for the preparation of a geopolymer
foam is
characterized in that the at least one surfactant is selected from the group
consisting of nonionic
alkyl polyglucoside surfactants.
[00014911n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it comprises fibers with lengths of between 5 and 1500 pm from 1% to
10% by mass relative
to the total mass of said composition.
Date Recue/Date Received 2021-03-30
15
[00015011n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it comprises fibers with lengths of between 5 and 1500 pm from 1% to
8% by mass relative
to the total mass of said composition.
[00015111n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it comprises fibers with lengths of between 5 and 1500 pm from 2% to
7% by mass relative
to the total mass of said composition.
[0001521In one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it comprises fibers with lengths of between 5 and 1500 pm from 3% to
6% by mass relative
to the total mass of said composition.
[00015311n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that the fibers have lengths between 5 and 1000 gm.
[00015411n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that the fibers have lengths between 10 and 800 gm.
[00015511n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that the fibers have a diameter of between 5 and 50 gm.
[00015611n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that the fibers have a diameter of between 10 and 40 gm.
[0001571In one embodiment, the composition for preparing a geopolymer foam is
characterized
in that the fibers have a diameter of between 15 and 30 gm.
[00015811n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that the fibers are cellulose fibers.
[00015911n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it further comprises at least one hydrophobic agent.
[00016011n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it further comprises at least one hydrophobic agent from 2% to 10% by
mass relative to the
total mass of said composition.
[00016111n one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it comprises at least one hydrophobic agent from 2% to 8% by mass
relative to the total
mass of said composition.
[0001621In one embodiment, the composition for preparing a geopolymer foam is
characterized
in that it further comprises at least one hydrophobic agent from 2% to 6% by
mass relative to the
total mass of said composition.
[00016311n one embodiment, the geopolymer foam according to the invention is
characterized in
that the at least one hydrophobic agent is selected from the group consisting
of siliconates, silanes,
siloxanes and mixtures thereof.
Date Recue/Date Received 2021-03-30
16
[0001641The invention also relates to the use of a composition for the
preparation of a geopolymer
foam as described above.
[000165] The invention also relates to a kit comprising:
- a composition for the preparation of a geopolymer foam as described
above;
- a pozzolanic material.
[00016611n one embodiment, the kit according to the invention is characterized
in that the
pozzolanic material is metakaolin.
The different elements of the kit are not in contact with each other for an
extemporaneous
preparation of geopolymer mineral foam.
Date Recue/Date Received 2021-03-30
17
Examples
[000167]Example 1: Composition for the preparation of a geopolymer foam
according to the
invention:
% of dry
material
Components s
Pozzolanic 1 Metakaolin 26.05
Material
2A Sodium Hydroxide 4.66
Activation ___________________________________________
Solution 2B Sodium Silicate 10.98
Hydrophobic Agent
Potassium Methyl
3 Silicone 4.02
Nonionic Surfactant
Alkyl Polyglucoside
4 SFT 5L8 0.034
Nonionic Surfactant
Alkyl Polyglucoside
5L826 0.034
Powdered Egg
6 Albumin Fraction 0.74
7 Kaolinitic Clays 5.21
pH Buffer
8 CaHPO4 2.61
Cellulose fibers of a
length of 18 or 40 gm
TECHNOCEL 10 or
9 40 1.49
Cellulose fibers of a
Other length of 150gm
Components 10 TECHNOCEL 90-2 1.49
Date Recue/Date Received 2021-03-30
18
Cellulose fibers of a
length of 500 and 700
Ilm
TECHNOCEL 300
11 and 1000 0.74
12 Keratin Hy drolysate 1.19
Hydrated Lime
13 Ca(OH)2 1.12
EAU Total 39.63%
[000168]Table 1: Composition for the preparation of a geopolymer foam
according to the
invention with a 100% basic Na activating solution.
[000169] Example 2: Composition for the preparation of a geopolymer foam
according to the
invention:
% of dry
Components materials
Pozzolanic 1 Metakaolin 25.69
Material ____________________________________________
2A Potassium Hydroxide 6.17
Activation __________________________________________
Solution 2B Sodium Silicate 4.46
2C Potassium Silicate .. 6.31
Other 3 Hydrophobic Agent
Components Potassium Methyl
Silicone 4.08
4 Nonionic Surfactant
Alkyl Polyglucoside
SFT 5L8 0.034
Nonionic Surfactant
Alkyl Polyglucoside
5L826 0.034
6 Powdered Egg Albumin
Fraction 0.76
7 Kaolinitic Clays 6.04
8 pH Buffer CaHPO4 1.13
Date Recue/Date Received 2021-03-30
19
9 Cellulose fibers of a
length of 18 or 40 gm
TECHNOCEL 10 or 40 1.51
Cellulose fibers of a
length of 150 gm
TECHNOCEL 90-2 1.51
11 Cellulose fibers of a
length of 500 and 700
gm
TECHNOCEL 300 and
1000 0.76
12 Keratin hydrolysate 1.21
13 Hydrated Lime
Ca(OH)2 1.13
EAU Total 39.17%
[000170]Table 2: Composition for the preparation of a geopolymer foam
according to the
invention with a K based basic activating solution.
[000171]Example 3: Manufacture of a geopolymer foam according to the
invention.
[0001721Manufacturing the cream:
[0001731Liquid components (2A, 2B, 2C, 3, 4, 5) are mixed, solid components
(1, 6, 7) and fibers
(9, 10, 11) are added and stirred with a deflocculating disc dispenser at 1000-
1500 rpm for
approximately 25 minutes. The temperature of the mixture is maintained at 18-
20 C.
[0001741Manufacturing the foam:
[0001751The component 8 is added and mixed for 1 min under the same
conditions, then
components 12, 13, as well as water QSP are mixed for one minute. The cream
may then be aerated
using an expansion machine. The air and cream flow rates and the speed of the
expansion unit are
adjusted to obtain the final foam upon leaving the machine.
[000176]Example 4: Comparative test between a geopolymer foam according to the
invention with
and without fibers, as well as with a geopolymer foam disclosed in
W02018091482.
[0001771A simplified geopolymer foam composition was carried out to
demonstrate the effect of
the presence or absence of micrometric sized fibers on the texture of the
geopolymer foam.
[0001781The composition of the 3 samples tested is summarized in the following
Table 3:
Date Recue/Date Received 2021-03-30
20
Components % of dry materials
Metakaolin 26.72
K based activating solution 17.61
Hydrophobic Agent 4.25
Surfactants 0.07
EAU Total 51.35%
[000179] Table 3: composition of samples tested.
[000180]Three portions of the above composition weighing 200 g or 230 ml are
poured into 3
separate 1L beakers.
[0001811No addition is made to a first beaker A.
[0001821In a second beaker B, 4.33% by mass of fibers having a length of 18 pm
relative to the
total mass of the composition is added. 99.5% of these fibers are less than 32
gm in length.
[0001831In a third beaker C, 4.33% of millimetric fibers is added. In
particular, these millimetric
fibers are used as fillers in the composition of the geopolymer foam disclosed
in W02018091482.
80% of the millimetric fibers added have a length of between 800 pm and 2.5
mm.
[0001841The various fibers added to beakers B and C are mixed by stirring for
3 minutes and then
the mixture is left to stand for 10 minutes before being stirred again for one
minute at low speed.
[0001851The foams are then produced using a kitchen mixer with 5 speeds, in
the following
sequence:
- 30 seconds at speed 1 (the lowest speed);
- 2 minutes and 30 seconds at speed 4.
The same operating mode is applied to the 3 mixtures, A, B and C.
[0001861The 3 samples are then left to stand for solidification.
[0001871Results:
[0001881At T = 2 hours, a change in surface appearance is observed in sample A
as well as in
sample C. No change is observed in sample B.
[0001891At T = 5 hours, the samples are completely solidified. A marked and
clear porosity is
observed in samples A and C, while sample B has a homogeneous appearance with
fine porosity.
[000190]The appearance of the 3 different samples is illustrated in Figure 1.
[000191]These observations demonstrate that the use of fibers of micrometric
sizes in a
geopolymer foam composition confers upon it the nature of a closed cell or
pore after
solidification.
Date Recue/Date Received 2021-03-30
21
[0001921Example 5: Comparative test between a foam according to the invention
and a foam
disclosed in W02018091482
[00019210ne sample of each foam is available in the form of cylindrical
stoppers of approximately
800 ml. The samples have similar densities (approximately 250 Kg/m3).
[000194] Each of the 2 samples was placed in a large container filled with
water. Each container
are sized to allow free movement of the sample and its complete immersion. The
samples are
placed on water and left for 5 min. The immersion height of each sample in
water is measured and
expressed as a percentage of the total height of the latter.
[0001951The samples are then removed from the water and placed on an inclined
plane so as to
drain out the water trapped in their porosities for a period of 2 hours.
[0001961The samples are weighed before testing and after draining, the
increase in weight as
compared to the initial weight is expressed as a percentage.
[000197] Case of the foam sample disclosed in W02018091482:
= Immersion height after 5 min. = 75 to 80%, the sample gradually sinks.
= Weight increase after draining = 81%
[000198] Case of the foam sample according to the invention
= Immersion height after 5 min = 10-15%, the immersion depth remains
unchanged, the sample floats.
= Weight increase after draining = 0.9%
[000199] These observations demonstrate that the foam according to the
invention has a
majority of closed cells unlike the foam disclosed in W02018091482, the
porosity of which is open.
Date Recue/Date Received 2021-03-30
