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    • 专利摘要:
    The invention thus consists of an incombustible mineral foam comprising: from 30 to 90% by weight of pozzolanic inorganic binder comprising polymerized metakaolin, from 0.08 to 2% by weight of thickener, of from 0.003 to 0.07 % by weight of at least one anionic surfactant selected from the group consisting of Cs-Cis-alkyl sulfates, C8-C18-alkyl ether sulfates, C8-C18-alkyl aryl sulfonic acids, C8 fatty acids -C18 and mixtures thereof, - from 0.002 to 0.03% by weight of at least one nonionic surfactant selected from the group consisting of alkylpolyglucosides, - a gaseous phase. The invention also relates to the method of manufacturing said foam, as well as the intermediate composition for forming the foam before it comes into contact with an expansion agent. The invention further relates to doors, clogged conduits and other supports on which is applied, or which include, said foam.
    公开号:FR3058719A1
    申请号:FR1661126
    申请日:2016-11-17
    公开日:2018-05-18
    发明作者:Philippe TOUSSAINT
    申请人:Hubert Barth Agissant Pour Le Compte De Isolfeu Creation Soc En Cours De Formation；
    IPC主号:
    专利说明:

    GEOPOLYMER FOAM WITH IMPROVED PROPERTIES [0001] The invention belongs to the field of geopolymers and more particularly to that of mineral foams.
    The invention relates to an incombustible, hydrophobic and thermally insulating mineral foam. The invention also relates to the method of manufacturing said foam, as well as the intermediate composition intended to form the foam before it is brought into contact with an expanding agent. Finally, the invention relates to doors, clogged pipes and other supports on which is applied, or which comprise, said foam.
    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.
    In the context of the present invention, the term “geopolymer” means an inorganic polymer essentially composed of units, silico-oxide (-Si-O-Si-O-), siico-aluminate (-Si-O-AI- O-), ferro-silico-aiuminate (-Fe-O-Si-O-AI-O-) or aiumino-phosphate (-AI-OPO-), created by a process called geopolymerization. Geopolymers, by their nature, find applications in the field of construction, in particular for the manufacture of cements and concretes or even fire protection. These mineral foams are particularly interesting because of their low density and their insulating and fireproofing properties, which means that they can be used in the construction of walls, doors, insulating panels and can also be used to seal or repair pipes, ovens. and other systems subject to high temperatures. These latter uses imply that the foam forms and hardens quickly (in a few minutes) so that it can be applied directly to the area to be sealed.
    The noncombustible mineral foams of the invention can in particular be prepared from an inorganic binder such as metakaolin, a natural pozzolanic material. Metakaolin is understood to mean a thermally dehydroxy kaolinitic clay. In other words, i! it is a dehydroxylated alumina silicate of general composition AI2O3, 2SiO2.
    Mineral foams are known from the prior art. It is known that a geopolymer can be prepared in the form of mineral foam by mixing an inorganic binder with a so-called activation solution, most often comprising hydroxides of alkali metals, and then adding a blowing agent which will form a gas in situ. The generation of gas will make it possible to disperse gas bubbles in the liquid phase and form a foam, while the reaction of the inorganic binder with the activation solution results in hardening, the result of the polymerization. The product obtained is a rigid and porous foam.
    FR 3,027,023 discloses foams prepared from metakaolin, from one or more natural or synthetic foaming agents of animal or vegetable origin. In particular, this request relates to foaming agents of the protein type (example 1).
    WO 2015/062860 discloses foams based on metakaolin and further comprising a surfactant. The authors recommend the use of nonionic surfactants, such as alkylpolyglucosides which are ideal for stabilizing the foam. In addition, a gas supply is preferred to a generation of gas in situ. DE 10 2004 006 563 discloses organic / inorganic hybrid foams comprising surfactants. In particular, the surfactants are amine oxides and alkyl sulfates.
    US 2015/0060720 or WO 2015/052819 disclose methods of preparing an inorganic foam with rapid hardening (less than 10 minutes). The blowing agent has the particularity of being aluminum scrap powder, which is a mixture of aluminum powder, aluminum nitride and aluminum oxide.
    Expansion (sometimes called swelling) and rapid hardening of the foam induce a number of constraints.
    In fact, expansion is a phenomenon that occurs quickly (after 1 minute). Then the top of the liquid takes shape. The expansion stops and the foam plug tightens. The Applicant has found that the use of a single ionic or non-ionic surfactant as recommended in the prior art had the effect of obtaining a foam capable of exhibiting defects in cohesion. In particular, the use of surfactants as demonstrated in the counterexamples leads to premature collapse of the foam or to problems of retention in mixture.
    The term “collapse” is understood to mean a sudden or progressive, total or partial collapse, of the expanded foam on itself.
    The defects observed are:
    - a collapse of the foam on itself a few minutes after the start of the expansion;
    - at the start of the expansion, the gas produced is not retained, there is loss of gas without gaining in volume of foam. Thus, there is either a collapse of the foam before complete expansion and hardening, or a loss of gas which induces a partial expansion with hardening.
    This leads to foams whose quality is insufficient for the recommended uses. In particular, it is important that the foam swells quickly and still does not have any defects such as collapses, partial retraction of the edges, microcracks.
    The Applicant has surprisingly demonstrated that the use of a specific combination, according to the invention, of at least one anionic surfactant and at least one nonionic surfactant provides a uniform expansion without shrinkage on the edges and without blistering (or blister). In addition, the combined use of these surfactants with a thickener, surprisingly contributes to improving the surface condition by eliminating its microcracks. The product of the invention is thus able to meet the expectations of the user, both in terms of speed of expansion / hardening and of quality and homogeneity of the foam. The product of the invention can be used in construction but also in conditions of emergency clogging of surfaces.
    In particular, the incombustible mineral foams according to the invention can be used as fire barriers and conform to Al according to the standards "reaction to fire" and "fire resistance", NF EN ISO 1182 and 1716 respectively. They have a thermal resistance up to at least 1200 ° C. In addition, the foams can be hydrophobic and constitute an additional barrier to its fire-fighting properties. The product of the invention can be molded, poured and even injected from a distance to make blockages and caulking on any type of surface under normal or extreme conditions.
    The foams of the invention have:
    - improved mechanical properties, durability over time, properties that change with drying, cohesion, rapid expansion and hardening compatible with use under harsh conditions.
    The invention thus consists of a non-combustible mineral foam comprising:
    from 30 to 90% by mass of inorganic pozzolanic binder comprising polymerized metakaolin,
    - from 0.08 to 2% by mass of thickener, from 0.003 to 0.07% by mass of at least one anionic surfactant chosen from the group consisting of Cs-Cis-alkyl sulfates, Cs-Cis -alkyl ether sulfates, Cs-Cis-alkyl aryl sulfonic acids, Its Cs-Cis fatty acids and their mixtures, from 0.002 to 0.03% by mass of at least one nonionic surfactant chosen from the group consisting of Its alkylpolyglucosides, a gas phase.
    The term “polymerized metakaolin” is understood to mean a geopolymer gei formed by the reaction of metakaolin with an activation solution (for example a basic solution).
    In one embodiment, the foam is characterized in that it comprises 45 to 90% by mass of inorganic pozzolanic binder.
    The term “thickener” is intended to mean a substance intended to modify / increase the viscosity of a composition.
    In one embodiment, the foam is characterized in that the thickener is chosen from the group consisting of its water-soluble starches te! as pregel starch, galactomannans such as guar gum, xanthan gum, clays such as bentonite or montmorillonite and cellulose derivatives such as methyl ethyl cellulose.
    In one embodiment, the foam according to the invention comprises from 0.1 to 2% by mass of thickener.
    In one embodiment, the foam according to the invention comprises from 0.1 to 1% by mass of thickener.
    In one embodiment, the foam according to the invention comprises from 0.2 to 1% by mass of thickener.
    In one embodiment, the foam according to the invention comprises from 0.2 to 0.5% by mass of thickener.
    The term "anionic surfactant" means a surfactant which releases a negative charge in aqueous solution. The class of anionic surfactants is extensively described in the literature.
    In one embodiment, the foam according to the invention is characterized in that the at least one anionic surfactant is chosen from the group consisting of Cs-Cis-alkyl sulfates, Cs-Cis-alkyl ether sulfates, Cs-Cis-alkyl aryl sulfonic acids, Cs-Cis fatty acids and mixtures thereof.
    In the present application, the abbreviations of type "C x -C y " indicate intervals ranging from x to y carbon atoms. For example, "Cs-Cis-alkyl sulfates" represents the group of alkyl sulfates comprising between 8 and 18 carbon atoms, "Cs-Cis-alkyl ether sulfates" represents the group of alkyl ether sulfates whose alkyl chain has between 8 and 18 carbon atoms and "Cs-Cis-alkyl aryl sulfonic acids" represents the group of alkyl aryl sulfonic acids in which the alkyl chain has between 8 and 18 carbon atoms. In one embodiment, the carbon chains contain an even number of carbon atoms.
    In one embodiment, the foam according to the invention is characterized in that the at least one anionic surfactant is a mixture of Cs-Cis-alkyl aryl sulfonate, Cs-Cis-alkyl ether sulfate and d fatty acid in Cs-Cie.
    In one embodiment, the foam according to the invention is characterized in that the anionic surfactant comprises sodium dodecylbenzene sulfonate, sodium pareth sulfate and potassium cocoate.
    In the context of the invention, one can use surfactants whose CAS number is 68411-31-4, 58131-39-5 or 61789-30-8. One can for example use EMPICOL XHL 300, marketed by the company HUNTSMAN PERFORMANCE PRODUCTS (mixture of sodium dodecylbenzene sulfonate, sodium pareth sulfate, potassium cocoate, cocamide DEA, C12-15 Pareth-7).
    In one embodiment, the foam according to the invention is characterized in that it comprises from 0.005 to 0.05% by mass of at least one anionic surfactant. Preferably, the foam comprises from 0.005 to 0.025% by mass of at least one anionic surfactant.
    The term "nonionic surfactant" means a surfactant whose molecules have no net charge. The class of nonionic surfactants is extensively described in His literature.
    In the context of the invention, the nonionic surfactants are chosen from among its alkyipolygiucosides (D-glucopyranose, oligomers, aikyl glucosides). In a preferred embodiment, the nonionic surfactant is a specific mixture of several types of alkylpolyglucosides.
    By alkylpolyglucoside is meant a nonionic surfactant having the formula: H-iCeHioOsjm-OR 1 , in which (CôHioOs) is a glucose unit and R 1 is a C6-C22 alkyl group, preferably Ca -Ci6 and Cs-Cio, and m is a positive integer between 1 and 10, 1 <m <10.
    In one embodiment, the foam according to the invention is characterized in that the nonionic surfactant is a mixture, having a ratio of between 60:40 and 90:10, of alkylpolyglucosides in which R 1 is a C1-C10 alkyl group and alkylpolyglucosides in which R 1 is a C1-C6 alkyl group. Preferably the ratio of alkylpolyglucosides is equal to 80:20.
    In one embodiment, the alkylpolyglucosides are those marketed by the company SEPPIC, such as SIMULSOL SL8 (D-glucopyranose, oligomers, decyî octy! Glycosides, 01-2119488530-36, CE: 500-200-1) or SIMULSOL SL 826 (D-glucopyranose, oligomers, decyl octy! glycosides, 01-2119488530-36, CE: 500-200-1, D-Glucopyranose, oiigomeric, C10-16 (even numbered) -alkyl glycosides, 01- 2119489418-23, CE: 600-975-8, (2-methoxymethylethoxy) propanol, 012119450011-60, CE: 252-104-2, dodecane-l-ol, 01-2119485976-15, CE: 203-982-0 ).
    In one embodiment, the foam according to the invention is characterized in that it further comprises other surfactants such as Ce-Cie-ethoxylated alcohols and Cs-Cw dialcoolamides.
    In one embodiment, the foam according to the invention is characterized in that it comprises from 0.002 to 0.02% by mass of at least one nonionic surfactant chosen from the group consisting of alkylpolyglucosides. Preferably, the foam comprises from 0.004 to 0.01% by mass of at least one nonionic surfactant chosen from the group consisting of alkylpolyglucosides.
    In one embodiment, the foam according to the invention is characterized in that it further comprises from 0.5 to 4% of a plasticizer, said plasticizer preferably being a polycarboxylate, Preferably, the foam includes 0.5 to 2% plasticizer.
    In one embodiment, the foam according to the invention is characterized in that it also comprises 1.5 to 8% by mass of a hydrophobic agent, preferably chosen from siliconates, silanes and siloxanes and their mixtures. Preferably, the foam comprises from 3.5 to 7% of a hydrophobic agent.
    In one embodiment, the foam according to the invention is characterized in that it further comprises from 0.3 to 8.3% by mass of an animal or vegetable protein, preferably ovalbumin or a soy protein isolate. Preferably, the foam comprises from 2 to 5% protein.
    In one embodiment, the foam according to the invention is characterized in that it also comprises from 0.01 to 7% by mass of stabilizing agent, preferably triethylcitrate. Preferably, the foam comprises from 0.16 to 3% of stabilizing agent.
    In one embodiment, the foam according to the invention is characterized in that it further comprises from 1.6 to 13% of a hydraulic binder or mixture of hydraulic binder, preferably chosen from donors of CaO, such as Portîand cement, plaster of Paris, calcium hydroxide or slaked lime. CaO donors have the particularity of accelerating the hardening of the foam. Preferably, the foam comprises from 4 to 9% of hydraulic binder.
    In one embodiment, the foam according to the invention is characterized in that it further comprises fibers or fillers, in particular chosen from textile microfibers, cellulose microfibers and grain grain lint.
    In one embodiment, the foam according to the invention is characterized in that it has a thermal conductivity between 0.04 and 0.08 W.nr 2 .K. In 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.
    In one embodiment, the foam according to the invention is characterized in that it has a density of between 140 and 180 kg / m 3 .
    In one embodiment, the foam according to the invention is characterized in that it has a hydrophobic character. A foam without hydrophobic agent will absorb water, while a hydrophobic foam will see water droplets remaining on the surface.
    The invention also relates to any support such as for example a fire door, an insulating panel, an oven, a pipe, which comprises or on which is affixed an incombustible inorganic foam as defined above.
    The invention also consists of a composition for the preparation of an incombustible mineral foam.
    In one embodiment, the composition intended for the preparation of an incombustible mineral foam according to the invention comprises:
    from 20 to 60% by mass of at least one inorganic pozzolanic binder comprising metakaolin, from 0.05 to 1.3% by mass of thickener, from 0.002 to 0.04% of at least one anionic surfactant chosen from the group consisting of Cs-Cis-alkyl sulfates, Cs-Cis-alkyl ether sulfates, Ce-Cie-alkyl aryl sulfonic acids, Cs-Cis fatty acids and their mixtures, from 0.001 to 0.02 % of at least one nonionic surfactant chosen from the group consisting of alkyipolyglucosides, at least one alkaline activator chosen from the group of alkali metal hydroxides and alkali metal silicates and their mixtures, water qs.
    "Qs" = sufficient quantity for.
    In one embodiment, the pH of the composition is between 12 and 14.
    In one embodiment, the composition is characterized in that the thickener is chosen from the group consisting of water-soluble starches such as pregel starch, galactomannans such as guar gum, ia gum xanthan, clays such as bentonite or montmorillonite and its cellulose derivatives te! than methyl ethyl cellulose.
    In one embodiment, the composition according to the invention is characterized in that it comprises from 0.06 to 1.3% by mass of thickener.
    In one embodiment, the composition according to the invention is characterized in that it comprises from 0.06 to 0.6% by mass of thickener.
    In one embodiment, the composition according to the invention is characterized in that it comprises from 0.1 to 0.6% by mass of thickener.
    In one embodiment, the composition according to the invention is characterized in that it comprises from 0.1 to 0.3% by mass of thickener.
    In one embodiment, the composition according to the invention is characterized in that the at least one nonionic surfactant is an alkylpolyglucoside or a mixture of alkylipolyglucosides of formula H- (C6Hio05) m-0- R 1 , in which (C6H10O5) is a glucose unit and R 1 is a C6-C22 alkyl group, preferably CsC16 or Ce-Cio, and m is a positive integer between 1 and 10.
    In one embodiment, the composition according to the invention is characterized in that the at least one non-nionic surfactant is a mixture of alkylipolyglucosides in which R 1 is a Cs-Cio alkyl group and d alkyipolyglucosides in which R 1 is a Cs-C16 alkyl group, the ratio of said mixture being between 60:40 and 90:10. Preferably, the ratio is 80:20.
    In one embodiment, the composition according to the invention is characterized in that it comprises from 0.002 to 0.02% by mass of at least one nonionic surfactant chosen from the group consisting of alkylpolyglucosides. Preferably, the composition comprises from 0.004 to 0.01% by mass of at least one nonionic surfactant chosen from the group consisting of alkylpolyglucosides.
    In one embodiment, the composition according to the invention is characterized in that Se at least one anionic surfactant is a mixture of Ce-Ciealkyle aryl sulfonate, Cs-Cis-alkyl ether sulfate and acid bold in Cs-Cis.
    In one embodiment, the composition according to the invention is characterized in that the anionic surfactant comprises sodium dodecylbenzene sulfonate, sodium pareth sulfate and potassium cocoate.
    In one embodiment, the composition according to the invention is characterized in that it comprises from 0.005 to 0.03% by mass of at least one anionic surfactant. Preferably, the composition comprises from 0.005 to 0.02% by mass of at least one anionic surfactant.
    In one embodiment, the composition according to the invention is characterized in that it further comprises other surfactants such as ethoxylated Cs-Cisalcohols and Cs-Cis dialcoolamides.
    In one embodiment, the alkaline activator is a mixture of potash (KOH) and / or soda (NaOH) and sodium and potassium silicates, said mixture comprising, in mass percentages: H2O from 60 to 70%, K2O from 10 to 16%, Na2O from 1 to 4% and S1O2 from 10 to 20%.
    In one embodiment, its composition according to the invention is characterized in that it also comprises from 0.5 to 3% by mass of a plasticizer, said plasticizer preferably being a polycarboxylate. Preferably, the composition comprises from 0.5 to 2% of plasticizer.
    In one embodiment, the composition according to the invention is characterized in that it also comprises from 1 to 5% by mass of a hydrophobic agent, preferably chosen from siliconates, silanes, siloxanes and their mixtures. Preferably, the composition comprises between 2 and 4.5% of hydrophobic agent.
    In one embodiment, an emulsion of silicone resin and of polydimethylsiloxane is used. The foam can also be surface treated after expansion and hardening with an emulsion, mixture of silane and siloxane, in an amount less than or equal to 1% by mass.
    In one embodiment, the composition according to the invention is characterized in that it further comprises from 0.2 to 5% by mass of an animal or vegetable protein, preferably ovalbumin or an isolate of soy protein. Preferably, the composition comprises between 1 and 4% protein.
    In one embodiment, the composition according to the invention is characterized in that it also comprises from 0.1 to 4% by mass of stabilizing agent, preferably triethyl citrate. Preferably, the composition comprises between 0.5 and
    1.5% stabilizing agent.
    ίο [00076] In one embodiment, the composition according to the invention is characterized in that it also comprises from 1 to 9% of a hydraulic binder or mixture of hydraulic binder, preferably chosen from CaO donors , such as Portland cement, plaster of Paris, calcium hydroxide or slaked lime. Preferably, the composition comprises from 3 to 7% of hydraulic binder. In one embodiment, the composition according to the invention is characterized in that it also comprises fibers or fillers, in particular chosen from textile microfibers, microfibers of cellulose and lump of cereal grains.
    The invention also relates to the use of a composition according to the invention for the preparation of an incombustible mineral foam.
    In what follows, reference will be made to these compositions under the name "composition A" or "part A".
    In one embodiment, the invention also relates to a kit comprising:
    (1) a composition A according to the invention and (2) a composition B comprising a blowing agent.
    [00081] A kit according to the invention can in particular be used in emergency situations. The mixing is carried out on site at the time of spraying or application on the surface to be covered or the cavity to be sealed.
    In one embodiment, the blowing agent comprises aluminum powder, free of aluminum nitride and aluminum oxide.
    In one embodiment, the blowing agent is ground aluminum, the particle size of which is continuous or spread out. An average statistical diameter is used to characterize the powder and the maximum grain diameter (here strictly less than 250 μm). The mean statistical diameter corresponds to 50% of the grains or particles which are higher or lower.
    In one embodiment, the blowing agent is aluminum powder, free from aluminum nitride or aluminum oxide, the grains of which have a diameter between 25 and 90 μm, preferably between 45 and 90 μm, or even between 45 and 75 μm, said aluminum grains being covered with a layer of high molecular weight glycols.
    In one embodiment, the aluminum powder represents from 0.2 to% by mass of the composition comprising the blowing agent.
    In one embodiment, the composition comprising the blowing agent further comprises powdered calcium carbonate.
    In one embodiment, ie calcium carbonate represents from 25 to 90% by mass of the composition comprising the blowing agent.
    In one embodiment, the composition comprising the blowing agent comprises from 0.2 to 20% aluminum and from 80 to 90% calcium carbonate.
    In one embodiment, its composition comprising the expansion agent further comprises a hydraulic binder. The hydraulic binder may be identical to or different from the hydraulic binder of composition A.
    In one embodiment, the blowing agent comprises hydrogen peroxide or a source of hydrogen peroxide.
    In one embodiment, the blowing agent is an aqueous solution of hydrogen peroxide.
    In one embodiment, the source of hydrogen peroxide is a perborate or a percarbonate. In one embodiment, the blowing agent is sodium perborate (Na2B2O4 (OH) 4) or sodium percarbonate (2Na2CO3-3H2O2). In one embodiment, traces of MnCh or aluminum powder are also used to catalyze the formation of peroxide and the release of oxygen.
    In one embodiment, the invention relates to a process for the preparation of non-combustible mineral foam.
    The method according to the invention consists in bringing a part A (or composition A) into contact with a part B (or composition B). This contacting is followed by expansion and hardening which lead to the formation of a foam according to the invention.
    Advantageously, the expansion is rapid and takes place in a few minutes. The hardening is simultaneous, or after the expansion stage and also takes place in a few minutes. In one embodiment, the properties of the foam continue to evolve with the drying of said foam. In particular, properties can continue to evolve over a period of up to 40 days.
    [00096] Complete hardening is generally observed after a period of at least 100 hours, preferably 72 hours. This period is considerably shortened in the case of accelerated hardening by adding heat.
    In one embodiment, the process for preparing an incombustible mineral foam comprises the steps of:
    a) bringing into contact, in aqueous solution, o at least one inorganic pozzolanic binder comprising metakaolin, o at least one alkaline activator chosen from the group of alkali metal hydroxides and alkali metal silicates and their mixtures, o at least one thickener, o at least one anionic surfactant chosen from the group consisting of Cs-Cis-alkyl sulfates, Cs-Cis-alkyl ether sulfates, CsCis-alkyl aryl sulfonic acids, acids fatty Cs-Cis and their mixture, and o at least one nonionic surfactant chosen from the group consisting of alkylpolyglucosides,
    b) mixing and obtaining a composition A,
    c) bringing composition A of step b) into contact with composition B comprising a blowing agent,
    d) expansion by generation of gas in situ using the blowing agent and
    e) hardening, characterized in that the amount of thickener relative to the total mass of the composition obtained in step b) is between 0.05 and 1.3%, the amount of anionic surfactant relative to the total mass of the composition obtained in step b) is between 0.002 and 0.04%, the amount of nonionic surfactant chosen from the group consisting of alkylpolyglucosides relative to the total mass of the composition obtained at step b) is between 0.001 and 0.02%, the blowing agent is chosen from the group consisting of aluminum powder, free of aluminum nitride and aluminum oxide, and peroxide hydrogen.
    In one embodiment, the method is characterized in that an inorganic pozzolanic binder comprising metakaolin is metakaolin and represents between 20 and 60% of the mass of the composition obtained in step b), preferably between 30 and 40%.
    In one embodiment, the method is characterized in that the hardening of step e) is accelerated by means of a supply of heat.
    In one embodiment, the method is characterized in that it further comprises a step f) of drying.
    In one embodiment, the method is characterized in that the accelerated hardening of step e) and the drying of step f) are carried out simultaneously by adding heat.
    In one embodiment, the method is characterized in that the pH of the composition obtained in step b) is between 12 and 14.
    In one embodiment, the method is characterized in that the thickener is chosen from the group consisting of water-soluble starches such as pregel starch, galactomannans such as guar gum, gum xanthan, clays such as ia bentonite or montmorillonite and its cellulose derivatives such as methyl ethyl cellulose.
    In one embodiment, the method is characterized in that the composition obtained in step b) comprises from 0.06 to 1.3% by mass of thickener. In one embodiment, the method is characterized in that the composition obtained in step b) comprises from 0.06 to 0.6% by mass of thickener. In one embodiment, the method is characterized in that the composition obtained in step b) comprises from 0.1 to 0.6% by mass of thickener.
    In one embodiment, the method is characterized in that the composition obtained in step b) comprises from 0.1 to 0.3% by mass of thickener.
    In one embodiment, the method is characterized in that the at least one nonionic surfactant is an alkylpolyglucoside or a mixture of alkylpolyglucosides of formula H-CCeHloOsjm-OR 1 , in which (CôHiqOs) is a glucose unit and R 1 is a C6-C22 alkyl group, preferably Cs-Ci6 or Cs-Cio, and m is a positive integer between 1 and 10.
    In one embodiment, the method is characterized in that the at least one non-nionic surfactant is a mixture, having a ratio between 60:40 and 90:10, of alkylpolyglucosides in which R 1 is a Cs-C10 alkyl group and alkylpolyglucosides in which R 1 is a Cs-C6 alkyl group. Preferably, the ratio is 80:20.
    In one embodiment, the method is characterized in that the composition obtained in step b) comprises from 0.002 to 0.02% by mass of at least one nonionic surfactant chosen from the group made up of ankylpoyglucosides. Preferably, the composition obtained in step b) comprises from 0.004 to 0.01% by mass of at least one nonionic surfactant chosen from the group consisting of ankylpoylucosides.
    In one embodiment, the method is characterized in that the anionic surfactant is a mixture of Cs-Cis-alkyl aryl sulfonate, Cs-Cis-alkyl ether sulfate and fatty acid Cs-Cis.
    In one embodiment, the method is characterized in that the anionic surfactant comprises sodium dodecyibenzene sulfonate, sodium pareth sulfate and potassium cocoate.
    In one embodiment, the method is characterized in that the composition obtained in step b) comprises from 0.005 to 0.03% by mass of at least one anionic surfactant. Preferably, the composition obtained in step b) comprises from 0.005 to 0.025% by mass of at least one anionic surfactant.
    In one embodiment, the method is characterized in that the composition obtained in step b) further comprises other surfactants such as Cs-Cis-ethoxylated alcohols and Cs-Cis dialcoolamides.
    In one embodiment, the method is characterized in that the alkaline activator is a mixture of potash (KOH) and / or soda (NaOH) and sodium and potassium silicates, said mixture comprising, in mass percentages: H2O from 60 to 70%, K2O from 10 to 16%, Na2O from 1 to 4% and S1O2 from 10 to 20%.
    In one embodiment, the method is characterized in that the composition obtained in step b) further comprises from 0.5 to 3% by mass of a plasticizer, said plasticizer preferably being a poiycarboxylate. Preferably, the composition obtained in step b) comprises from 0.5 to 2% of plasticizer.
    In one embodiment, the method is characterized in that the composition obtained in step b) further comprises from 1 to 5% by mass of a hydrophobic agent, preferably chosen from siliconates, silanes, siioxanes and their mixtures. Preferably, the composition obtained in step b) comprises from 2 to 4.5% of hydrophobic agent.
    In one embodiment, the method is characterized in that the composition obtained in step b) further comprises from 0.2 to 5% by mass of an animal or vegetable protein, preferably ovalbumin. Preferably, the composition obtained in step b) comprises from 1 to 4% of protein.
    In one embodiment, the method is characterized in that the composition obtained in step b) further comprises from 0.1 to 4% by mass of stabilizing agent, preferably triethylcitrate. Preferably, the composition obtained in step b) comprises from 0.5 to 1.5% of stabilizing agent.
    In one embodiment, the method is characterized in that the composition obtained in step b) further comprises from 1 to 9% of a hydraulic binder or mixture of hydraulic binder, preferably chosen from donors CaO, such as Portland cement, plaster of Paris, calcium hydroxide or slaked lime. Preferably, the composition obtained in step b) comprises from 3 to 7% of hydraulic binder.
    In one embodiment, the method is characterized in that the gas generated in situ in step d) is dihydrogen (H2) or dioxygen (O2).
    In one embodiment, the method is characterized in that the blowing agent is aluminum powder, free of aluminum nitride or aluminum oxide, the grains of which have a diameter between 25 and 90 pm, preferably between 45 and 90 pm, or between 45 and 75 pm, said aluminum grains being covered with a layer of high molecular weight glycols.
    In one embodiment, the method is characterized in that the amount of aluminum powder represents from 0.2 to 20% by mass of the composition comprising the blowing agent.
    In one embodiment, the method is characterized in that the composition comprising the blowing agent further comprises powdered carbonate of silicon.
    In one embodiment, the method is characterized in that the amount of calcium carbonate represents from 20 to 90% by mass of the composition comprising the blowing agent.
    In one embodiment, the method is characterized in that the composition comprising the blowing agent comprises from 0.2 to 20% aluminum and from 80 to 90% calcium carbonate.
    In one embodiment, the method is characterized in that the composition comprising the blowing agent also comprises a hydraulic binder, said hydraulic binder being identical to or different from that possibly present in the composition obtained at î ' step b).
    In one embodiment, the process is characterized in that the blowing agent is an aqueous solution of hydrogen peroxide or a source of hydrogen peroxide.
    In one embodiment, the source of hydrogen peroxide is a perborate or a percarbonate. In one embodiment, the blowing agent is sodium perborate (Na2B2O4 (OH) 4) or sodium percarbonate (2Na2CC> 3-3H2C> 2). In one embodiment, traces of MnC> 2 or aluminum powder are also used to catalyze the formation of peroxide and its release of oxygen. In one embodiment, the method is characterized in that the hardening of step e) is consecutive to the expansion.
    In one embodiment, the method is characterized in that the duration of the step d) of expansion is between 1 and 10 minutes, preferably between 1 and minutes.
    In one embodiment, the method is characterized in that the duration of the curing step e) is between 4 and 10 minutes, preferably 5 and 8 minutes.
    Examples
    Example 1:
    Component Detai! Amount % PART A g 100 metakaolin 37.4 30.16 Solutionactivation Mixture of KOH and Na and K silicates (H 2 O: 66.3; K 2 0: 13.9; Na 2 O: 2; SiO 2 (Total) 15.2: SiO 2 : K 2 O: 8.56; SiO 2 : NaO: 6.62; OH (Total) 14.4) Note: i.e. 23.3 g of mat. dry 23.3 19.18 Agenthydrophobic 0 0 Water 50.4 41.2 Surfactant I Dilution of Empicol XHL300 in water Note -1: 11 (g / g) x 67% or 0.011 g of mat. active 0,011 0,009 Surfactant II Dilution of a mixture of simulsol SL8 / SL826 (80:20) in waterNote = l: ll (g / g) x 60% - i.e. 0.005 g of mat. active 0.005 0,004 Thickening Corn starch pregel 0.2 0.16 plasticizer polycarboxylates (30% dry matter) 0.8 0.64 Surfactant III (stabilizing agent) triethyl citrate or 1,2,3-propane tricarboxylic acid, 2-hydroxy, triethyl ester (couple with albumin) 1 0.82 Cpj32 cement 5 4.09 CaSO4.1 / 2H 2 O Non-delayed plaster 1.5 1.23 Egg albumin powder Fraction of 2.5 2.04 PART B g 100 Aluminum Aluminum powder treated with high molecular weight glycols (PM), average static diameter <75 pm (here 52 or 48 pm) 0.48 10 Micronized calcium carbonate 90% <at 75 - 90 pm 4.32 90
    Table 1: composition of parts A and B [000133] All the quantities indicated in table 1 are quantities of dry matter. All of the water, all origins combined, is shown on the "water" line.
    [000134] Operating mode:
    Part A is prepared as follows:
    (1) the powdered metakaolin is added in rain and dispersed with stirring in the aqueous and alkaline activation solution for 3 to 5 min max. ;
    (2) the stirring of the suspension obtained in (1) is continued at 800 rpm for 30 to 35 min. (slight increase in suspension temperature, around 8 ° C). The suspension may be cooled to between 18 and 25 ° C if the ambient temperature is high (> 25 ° C);
    (3) are then added successively and with vigorous stirring, the hydrophobic agent (optional), the starch powder, the dispersant (polycarboxylate).
    (4) after 2 minutes the cement powders, plaster and albumin then the surfactants are added successively to the mixture and dispersed with the same stirring for 5 minutes; the final mixture obtained has the consistency of a thick cream.
    Part B is added at the end of the previous operation and mixed with intensive stirring for 20 to 30 sec.
    The expansion of the mixture occurs from one minute and ends at 5 minutes. The consistency of the foam strengthens and hardens between 5 and 8 min.
    For its complete hardening, the mineral foam obtained is kept in a closed enclosure or in a plastic film (or tarpaulin) for a period of at least 72 hours, either at room temperature or at a temperature below 100 ° C. but always under plastic film (hardening is then accelerated). The foam is then stored at room temperature to ensure its drying and the development of its hydrophobic property (which is achieved by a reaction with carbon dioxide (CO2) from the air.
    We measure a coefficient of thermal conductivity of 0.06 W / m 2 K. We observe an open porosity for breathing. The thermal resistance of the foam is recognized up to 1200 ° C. It can be used as a fire barrier and complies with the above classifications “fire resistance” and “reaction to fire”.
    Example 2:
    The foam of Example 2 was prepared according to the method of Example 1
    with quantities and proc following: Component Detail Amount PART A g metakaolin 37.4 Solutionactivation Mixture of KOH and Na and K silicates (H 2 O: 66.3; K 2 O: 13.9; Na 2 O: 2; SiO 2 (Total) 15.2: SiO 2 : K 2 O: 8.56; SiO 2 : NaO: 6.62; OH (Total) 14.4) 69.1 Hydrophobic agent Aqueous solution of methyl K-siliconate (54% dry matter) 7 Water 0 Surfactant I Dilution of Empicol XHL300 in water = 1:11 (g / g) 0/2 Surfactant II Dilution of a mixture of simulsol SL8 / SL826 (80:20) in water = 1:11 (g / g) 0.1 Thickening Corn starch pregel 0.2 plasticizer polycarboxylates (30% dry matter) 2.6 Surfactant III (stabilizing agent) triethyl citrate or 1,2,3-propane tricarboxylicacid, 2-hydroxy, triethyl ester (couple with albumin) 1 Cpj32 cement 5 CaSO4.1 / 2H 2 O Non-delayed plaster 1.5 Egg albumin powder Fraction of 2.5 PART B Aluminum Aluminum powder treated with glycoïsat high PM, average static diameter <75 pm (here 52 or 48 pm) 0.48 Micronized calcium carbonate 90% <at 75 - 90 pm 4.32
    Table 2: Composition of Parts A and B The mineral foam obtained according to Example 2 retains the properties and the advantages of the foam obtained in Example 1. It is also made hydrophobic: it can constitute a barrier of additional protection.
    Example 3 The foam of Example 3 was prepared according to the method of Example 1
    Component detail amount PART A 9 metakaolin 37.4 Activation solution Mixture of KOH and Na and K silicates (H 2 O: 66.3; K 2 0: 13.9; Na 2 O: 2; SiO 2 (Total) 15.2: SiO 2 : K 2 O: 8.56; SiO 2 : NaO: 6.62; OH (Total) 14.4) 69.1 Hydrophobic agent Aqueous solution of methyl K-siliconate (54% dry matter) 7 Surfactant I Dilution of Empicol XHL300 in water = 1:11 (g / g) 0.2 Surfactant II Dilution of a mixture of simulsol SL8 / SL826 (80:20) in water = 1:11 (g / g) 0.1 Thickening Corn starch pregel 0.2 plasticizer Polycarboxylates (30% dry matter) 2.6 Surfactant III (stabilizing agent) triethyl citrate or 1,2,3-propanetricarboxylicacid, 2-hydroxy, triethyl ester (couple with albumin) 1 Cpj32 cement 5 CaSO4.1 / 2H 2 O Non-delayed plaster 1.5 Egg albumin powder Fraction of 2.5 microfiber Textiles, plants, paper, lemons (length <5mm) 4 PART B Aluminum Aluminum powder treated with glycols at high PM, average static diameter <75 pm (here 52 or 48 pm) 0.48 Micronized calcium carbonate 90% <at 75 - 90 pm 4.32
    Table 3: Composition of Foam No. 3 Before Expansion / Curing [000141] The mineral foam No. 3 obtained according to Example 3 retains the properties and the advantages of the foam obtained in Example 2.
    Counterexamples:
    The following counterexamples were prepared according to the protocol of Example 1, unlike the specific combination of surfactants.
    Foams # 4, 5 and 6 are counter-examples.
    See example # 1: te n s i o a ctif EMPICOL HXL-300 only.
    Component Detail Amount PART A g metakaolin 37.4 Solutionactivation Mixture of KOH and Na and K silicates (H 2 O: 66.3; K 2 O: 13.9; Na 2 O: 2; SiO 2 (Total) 15.2: SiO 2 : K 2 O: 8.56; SiO 2 : NaO: 6.62; OH (Total) 14.4) 69.1 Hydrophobic agent Aqueous solution of methyl K-siliconate (54% dry matter) 7 Surfactant I Dilution of Empicol XHL300 in water = 1:11 (g / g) 0.26 Thickening Corn starch pregel 0.2 plasticizer Polycarboxylates (30% dry matter) 1.2 Cpj32 cement 5.5 CaSO 4 .l / 2H2O Non-delayed plaster 3.4 PART B Aluminum Aluminum powder treated with high PM glycols, average static diameter <75 pm (here 52 or 48 pm) 0.47 Micronized calcium carbonate 90% <at 75 - 90 pm 4.23
    Table 4: composition of foam No. 4 before expansion / hardening The expansion of its foam reaches 600 ml then is followed by a relaxation (collapse) of this volume which ends at 500 ml despite a higher rate in cement and plaster (source of CaO). (The objective being to ensure a hardening at the end of the maximum expansion without shrinkage or relaxation).
    Counterexample # 2: SIMULSOL surfactants alone.
    Component Detail Amount PART A g metakaolin 37.4 Activation solution Mixture of KOH and Na and K silicates (H 2 O: 66.3; K 2 0: 13.9; Na 2 O: 2; SiO 2 (Totai) 15.2: SiO 2 : K 2 O: 8.56; SiO 2 : NaO: 6.62; OH (Total) 14.4) 69.1 Hydrophobic agent Aqueous solution of methyl K-siliconate (54% dry matter) 7 Surfactant II Dilution of a mixture of simulsol SL8 / SL826 (80:20) in water = 1:11 (g / g) 0.22 Thickening Corn starch pregel 0.2 plasticizer Polycarboxylates (30% dry matter) 1.2 Cpj32 cement 5.5 CaSO 4 .l / 2H 2 O Non-delayed plaster 3.4 PART B Aluminum Aluminum powder treated with glycols toHigh PM, average static diameter <75 pm (here 52 or 48 pm) 0.47 Micronized silicon carbonate 90% <at 75 - 90 pm 4.23
    Table 5: composition of foam no. 5 before expansion / hardening [000144] The expansion of the foam is limited to 460 ml followed by a loss of volume 5 which ends at 400 ml. there is no reduction in gas losses and therefore an improvement in volume fina! foam. The stabilization of the latter by hardening is also not improved.
    Counterexample No. 3: triethyl citrate and albumin powder without surfactants I and II
    Component Detai! Amount PART A g metakaolin 37.4 Activation solution Mixture of KOH and Na and K silicates (H 2 O: 66.3; K 2 0: 13.9; Na 2 O: 2; SiO 2 (Total) 15.2: SiO 2 : K 2 O: 8.56; SiO 2 : NaO: 6.62; OH (Total) 14.4) 69.1 Hydrophobic agent Aqueous solution of methyl K-siliconate (54% dry matter) 7 Thickening Corn starch pregel 0.2 plasticizer Polycarboxylates (30% dry matter) 2.1 Surfactant III (stabilizing agent) triethyl citrate or 1,2,3-propane tricarboxylicacid, 2-hydroxy, triethyi ester (cut with albumin) 1.5 Cpj32 cement 5 CaSO 4 .l / 2H 2 O Non-delayed plaster 1.8 Egg albumin powder Fraction of 2.5 PART B Aluminum Aluminum powder treated with high PM glycols, average static diameter <75 pm (here 52 or 48 pm) 0.48 Micronized calcium carbonate 90% <at 75 - 90 pm 4.32
    Table 6: composition of foam No. 6 before expansion / hardening [000145] The foam expansion reaches 500 ml and stabilizes. There is a regular expansion but also a significant loss of gas. Finally after hardening, a section of the foam reveals a very heterogeneous porosity (mixture of large and fine pores), which underlines the complementary role of the other surfactants.
    权利要求:
    Claims (12)
    [1" id="c-fr-0001]
    1. Non-combustible mineral foam comprising:
    - from 45 to 90% by mass of inorganic pozzolanic binder comprising polymerized metakaolin,
    - from 0.08 to 2% by mass of thickener, from 0.003 to 0.07% by mass of at least one anionic surfactant chosen from the group consisting of Cs-Cis-alkyl sulfates, Cs-Cie -alkyl ether sulfates, Cs-Cis-alkyl aryl sulfonic acids, Cs-Cis fatty acids and their mixture, from 0.002 to 0.03% by mass of at least one nonionic surfactant chosen from the group consisting of alkylpolyglucosides, a gas phase.
    [2" id="c-fr-0002]
    2. Foam according to the preceding claim, characterized in that the thickener is chosen from the group consisting of water-soluble starches such as pregel starch and galactomannans such as guar gum, xanthan gum, clays such as bentonite or montmorillonite or cellulose derivatives such as methyl ethyl cellulose.
    [3" id="c-fr-0003]
    3. Foam according to any one of the preceding claims, characterized in that the at least one nonionic surfactant is an alkylpolyglucoside or a mixture of alkylpolyglucosides of formula H-CCâHioOsjm-OR 1 , in which (C6H10O5) is a glucose unit and R 1 is a C6-C22 alkyl group, preferably Cs-Ci6 or Cs-Cio, and m is a positive integer between 1 and 10, 1 <m <10.
    [4" id="c-fr-0004]
    4. Foam according to any one of the preceding claims, characterized in that the at least one anionic surfactant is a mixture of Cs-Cis-alkyl aryl sulfonate, Cs-Cis-alkyl ether sulfate and fatty acid Cs cis.
    [5" id="c-fr-0005]
    5. Support comprising a foam according to any one of claims 1 to 4.
    [6" id="c-fr-0006]
    6. Composition for the preparation of an incombustible mineral foam according to any one of claims 1 to 4:
    from 20 to 60% by mass of at least one inorganic pozzolanic binder comprising metakaolin, from 0.05 to 1.3% by mass of thickener, from 0.002 to 0.04% of at least one anionic surfactant chosen from the group consisting of Cs-Cis-alkyl sulfates, Cs-Cis-alkyl ether sulfates, Cs-Cis-alkyl aryl sulfonic acids, Ce-Cis fatty acids and mixtures thereof,
    from 0.001 to 0.02% of at least one nonionic surfactant chosen from the group consisting of alkylpolyglucosides, at least one alkaline activator chosen from the group of alkali metal hydroxides and alkali metal silicates and mixtures thereof,
    - water qs.
    [7" id="c-fr-0007]
    7. Use of a composition according to the preceding claim for the preparation of an incombustible mineral foam.
    [8" id="c-fr-0008]
    8. Kit including:
    (1) a composition according to any one of claims 1 to 4, (2) a composition comprising a blowing agent.
    [9" id="c-fr-0009]
    9. A method of preparing a foam comprising the steps of;
    a) bringing into contact, in aqueous solution, o at least one inorganic pozzolanic binder comprising metakaolin, o at least one alkaline activator chosen from the group of alkali metal hydroxides and alkali metal silicates and their mixtures, o at least one thickener, o at least one anionic surfactant selected from the group consisting of Cs-Cis-alkyl sulfates, Cs-Cis-alkyl ether sulfates, Its CeCie-alkyl aryl sulfonic acids and ies fatty acids in Ce-Cis, and o of at least one nonionic surfactant chosen from the group consisting of Ses alkylpolyglucosides,
    b) mixing and obtaining a composition,
    c) bringing the composition of step b) into contact with a composition comprising a blowing agent,
    d) expansion by generation of gas in situ using the blowing agent and
    e) hardening, characterized in that the amount of thickener relative to the total mass of the composition obtained in step b) is between 0.05 and 0.4%, the amount of anionic surfactant relative to the total mass of the composition obtained in step b) is between 0.002 and 0.02%, the amount of nonionic surfactant chosen from the group consisting of alkylpolyglucosides relative to the total mass of the composition obtained at step b) is between 0.001 and 0.02%, the blowing agent is chosen from the group consisting of aluminum powder, free of aluminum nitride and aluminum oxide, and of peroxide hydrogen.
    [10" id="c-fr-0010]
    10. Method according to the preceding claim characterized in that i! further includes a drying step f).
    [11" id="c-fr-0011]
    11. Method according to the preceding claim characterized in that the hardening of step e) is consecutive to the expansion of step d).
    [12" id="c-fr-0012]
    12. Method according to the preceding claim, characterized in that the duration of the expansion step is between 1 and 10 minutes, preferably between 1 and 5
    5 minutes and in that the duration of the hardening stage d) is between 4 and 10 minutes, preferably 5 and 8 minutes.
    FRENCH REPUBLIC
    National registration number
    FA 835348 FR 1661126 irai - I NATIONAL INSTITUTE
    INDUSTRIAL PROPERTY
    RESEARCH REPORT
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    引用文献:
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    法律状态:
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    2018-05-18| PLSC| Publication of the preliminary search report|Effective date: 20180518 |
    2018-10-17| PLFP| Fee payment|Year of fee payment: 3 |
    2019-10-18| IM| Registration of a company|Owner name: ISOLFEU-CREATION, FR Effective date: 20190909 |
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    优先权:
    申请号 | 申请日 | 专利标题
    FR1661126A|FR3058719B1|2016-11-17|2016-11-17|GEOPOLYMER FOAM WITH IMPROVED PROPERTIES|
    FR1661126|2016-11-17|FR1661126A| FR3058719B1|2016-11-17|2016-11-17|GEOPOLYMER FOAM WITH IMPROVED PROPERTIES|
    PCT/EP2017/079238| WO2018091482A1|2016-11-17|2017-11-14|Geopolymer foam with improved properties|
    EP17801431.2A| EP3541767B1|2016-11-17|2017-11-14|Geopolymer foam with improved properties|
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