EP2531553A1 - Materiaux d'isolation thermique hautes performances - Google Patents

Materiaux d'isolation thermique hautes performances

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Publication number
EP2531553A1
EP2531553A1 EP11707455A EP11707455A EP2531553A1 EP 2531553 A1 EP2531553 A1 EP 2531553A1 EP 11707455 A EP11707455 A EP 11707455A EP 11707455 A EP11707455 A EP 11707455A EP 2531553 A1 EP2531553 A1 EP 2531553A1
Authority
EP
European Patent Office
Prior art keywords
insulating material
thermal insulating
material according
binder
less
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP11707455A
Other languages
German (de)
English (en)
French (fr)
Inventor
Daniela Pasquero
Claude Da Silva
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Saint Gobain Isover SA France
Original Assignee
Saint Gobain Isover SA France
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Saint Gobain Isover SA France filed Critical Saint Gobain Isover SA France
Publication of EP2531553A1 publication Critical patent/EP2531553A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066Use of inorganic compounding ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/30Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by mixing gases into liquid compositions or plastisols, e.g. frothing with air
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04BGENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62Insulation or other protection; Elements or use of specified material therefor
    • E04B1/74Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
    • E04B1/76Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only
    • E04B1/7604Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only fillings for cavity walls
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00Foams characterised by their properties
    • C08J2205/02Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
    • C08J2205/026Aerogel, i.e. a supercritically dried gel
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2321/00Characterised by the use of unspecified rubbers
    • C08J2321/02Latex
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2425/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2425/02Homopolymers or copolymers of hydrocarbons
    • C08J2425/04Homopolymers or copolymers of styrene
    • C08J2425/08Copolymers of styrene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2433/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2433/06Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C08J2433/08Homopolymers or copolymers of acrylic acid esters
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04BGENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62Insulation or other protection; Elements or use of specified material therefor
    • E04B1/74Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
    • E04B2001/742Use of special materials; Materials having special structures or shape

Definitions

  • the present invention relates to a high performance thermal insulation material, its manufacturing method, and its use in the field of construction to isolate the walls (exterior or interior) of buildings, or to fill gaps in the materials of construction.
  • fibrous insulators based on natural or synthetic fibers such as glass or rock wool
  • cellular insulators of the expanded or foamed polymer type such as expanded polystyrene
  • extruded or polyurethane and airgel mats, ie layered aerogels in the form of a web of mechanically strong entangled fibers, but for which it is difficult to print a particular shape.
  • Silica aerogels are the most efficient insulation products. However, their poor mechanical properties make it necessary to use them in combination with a reinforcing agent. Their use has remained very little developed until today, because their use in association with the usual insulation products (polystyrene ...) did not make it possible to obtain exploitable products, as underlined later in the text. Silica aerogels that can achieve thermal conductivities down to 12 mW / mK are produced from silica gel dried in special conditions. They may be in the form of either translucent granules which must be protected from handling, with application to insulating glass, or from fine powder and can not be used as such to constitute conventional insulating products such as insulating panels (thermal, acoustic ...) for the insulation of building walls.
  • composite foam comprising 27-47% by volume of supercritical silica airgel in the form of 2-5 mm particles and between 53 and 73% by volume of styrene polymer foam are found in EP489319.
  • the products are advertised with a thermal conductivity of 20 to 27 mW / m.K at 10 ° C.
  • WO03097227 the direct incorporation of a polymeric binder to airgel particles.
  • the application US20080287561 relates more particularly to silica airgel composites such as composite materials made from aerogels associated with syntactic foams without hollow microspheres (glass or thermoplastic). These syntactic foams are obtained in particular through the use of an aqueous polymer ("water-based polymer”) in the mixture.
  • water-based polymer aqueous polymer
  • the thermal performances obtained by this technique are limited, the samples obtained by the protocol described in US20080287561 not making it possible to obtain thermal conductivities of less than 60 mW / m.K.
  • the application WO03097227 also relates to syntactic foams obtained in particular by virtue of the use of an aqueous polymeric binder ("aqueous binder ”) in the form of foam.
  • the foams are syntactic foams generated by the use of hollow microspheres (glass or thermoplastic).
  • Such syntactic foams including the aforementioned microspheres are particularly expensive.
  • the thermal performance obtained by this technique is limited, since the microspheres used degrade the high thermal performance provided by the airgel.
  • the present invention aims to provide a new type of insulating material demonstrating excellent thermal performance, while maintaining good mechanical strength and low densities for relief of the load.
  • the present invention also aims at providing an innovative material that remains easy to spread during curing and to which it is possible to impart all desirable shapes, including molding.
  • the present invention relates to a thermal insulating material capable of being obtained from the mixture of at least the following elements: an aqueous foam, particles silica airgel, an organic binder and / or a mineral binder.
  • thermal insulating materials comprising silica aerogels prepared from aqueous foams make it possible to achieve thermal performances close to those of aerogels as such, with densities compatible for use as lightweight material.
  • thermal insulating material also demonstrates very good mechanical performance, especially in terms of compressive strength and deformability.
  • the insulating material of the invention is therefore compatible both for use as a filler material, and for use on the surface, especially on the facade.
  • Silica aerogels used in the context of the present invention are prepared from commercial airgel granules, for example aerogels marketed by Cabot (Nanogel® TLD 302, etc.). They can be used after grinding and sieving or alternatively be used directly without any transformation. Aerogels are usually obtained from of a gel manufactured, for example by hydrolysis in the presence of a solvent and then gelling with catalysis, from an organic or inorganic precursor, and then by evaporation or extraction of the gel-forming liquid (for example at high temperature and / or or under pressure) to replace this liquid with a gas (in particular air). Aerogels can be produced especially in the form of foam, granules, blocks that are divided if necessary.
  • the mixture for the preparation of the thermal insulating material comprises an organic and / or inorganic binder. It is used, for example, to allow the binding of the particles together and / or the binding of the particles to the rest of the material structure at the final product.
  • binder used alone will refer indifferently to a mineral binder, an organic binder or a binder system belonging to at least one of these two families.
  • the thermally insulating material described above is capable of being prepared from at least the following elements, taken in quantities expressed as a percentage by weight relative to the total mass of the mixture (overall mixture used for the preparation of the material insulation), varying from 25 to 75% for the aqueous foam, from 5 to 35% for the silica airgel particles and from 5 to 35% for the binder.
  • the amount of aqueous foam varies from 35 to 65%, preferably from 45 to 55%, and even up to 50%.
  • the amount of silica airgel particles advantageously varies from 17 to 25%, preferably from 21 to 23%, and even is 22%.
  • the amount of binder advantageously varies from 17 to
  • aqueous foam in the meaning of the invention defines any type of foam obtained by a disordered stack of gas bubbles in an aqueous phase, in particular in a soapy liquid.
  • a soap-like liquid comprises water and at least one surfactant compound.
  • the aqueous foam used to obtain the insulating material of the invention is preferably prepared from a mixture comprising:
  • At least one cationic surfactant salt selected from one of the following compounds of general formula:
  • R is an aliphatic chain of 8 to 24 carbon atoms
  • R 1 is a group selected from alkyls containing 1 to 16 carbon atoms, hydroxyalkyls containing 1 to 16 carbon atoms, a benzyl group, a group which, taken together with the nitrogen of formula (I), gives a heterocycle optionally substituted with at least one fluorine atom
  • R 2 and R 3 are selected from groups consisting of an alkyl group having 1 to 6 carbon atoms, hydroxyalkyls containing 1 to 6 carbon atoms, a hydrogen atom, a benzyl group, a group which, taken together with the nitrogen of the formula (I), gives a heterocycle optionally substituted by at least one fluorine atom
  • X " is a counter-anion
  • At least one anionic surfactant salt selected from one of the following compounds of general formula (II):
  • R is an aliphatic chain of 10 to 24 carbon atoms
  • X " is a group bearing a negative charge selected from carboxylate, sulphate and phosphate groups
  • Y + is a counter cation selected from ammonium, sodium and potassium groups.
  • the ratio of the weight content of the cationic surfactant salt to the weight content of the anionic surfactant salt varies from 0.05: 1 to 15: 1, preferably from 0.2: 1 to 5: 1, or even 0.4: 1 at 2.5: 1.
  • the cationic surfactant salt is selected from alkyltrimethylammonium salts containing an alkyl group having 10 to 22 carbon atoms, and is preferably selected from at least one of the following compounds: the bromide (or chloride) of dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide (or chloride), hexadecyltrimethylammonium bromide (or chloride), octadecyltrimethylammonium bromide (or chloride), cetyltrimethylammonium bromide (or chloride), cetylbenzyldimethylammonium chloride, cetyltriethylammonium bromide, and tallowtri
  • the anionic surfactant salt is tallowtrimethylammonium chloride.
  • the anionic surfactant salt (s) mentioned above is (are) selected from at least one of the following compounds: ammonium stearate, potassium stearate and sodium stearate.
  • anionic surfactants consisting of an alkali metal salt of an organic acid carrying an aliphatic chain containing 12 to 24 carbon atoms, advantageously a sodium, potassium or ammonium salt (optionly substituted).
  • the group X " of the general formula (II) can be a carboxylate, sulphate or sulphonate group, and salts of carboxylates containing from 12 to 24 carbon atoms, selected for example from the salts of: myristate, palmitate, stearate, of oleate, or of the conjugated base of behenic acid, and in particular the selected anions derived from soap by hydrolysis of triglyceride (saponification), and other carboxylates such as those resulting from the treatment of acids.
  • tallow fat including palmitate, stearate and oleate
  • Other conjugated fatty acid bases may also be used, such as soaps / shower gels comprising fatty acids from natural sources such as tallow , coconut oil or even palm oil.
  • the cationic and anionic surfactants are comprised in two distinct aqueous phases and are mixed in the contents indicated above to form the foam.
  • the aqueous foam can also be prepared from the two-component kits marketed by the company Allied Foam (referenced 425A and 510B). Such kits consist of a first aqueous mixture containing an anionic surfactant and a second aqueous mixture comprising a cationic surfactant and a latex.
  • aqueous foams comprising a cationic surfactant and anionic surfactant have the advantage of remaining particularly stable during the incorporation of silica airgel particles. It becomes easy enough to control the amount of silica airgel to be introduced into the mixture for the preparation of the insulating material of the invention. This aspect is particularly interesting because it allows access to a wide range of different products. Indeed, silica aerogels being quite expensive, it is preferable to be able to control their content to be able to prepare more affordable products in terms of cost, without degrading too much the thermal properties and mechanical strength.
  • Increasing the foam / airgel ratio also makes it possible to prepare ventilated advantage systems, thus more compressible when this is associated with an intrinsic flexibility of the material, which is sought for certain uses, such as, for example, soil insulation (particularly the sound insulation) or the filling of honeycomb structures.
  • the use of stable foams also makes it possible to obtain a material which remains of low density, even with lower concentrations of silica airgel.
  • aqueous foams may be used in the context of the present invention, for example, Gillette Foam Regular Foam.
  • aqueous foams comprising a water / glycerol mixture, one or more surfactants (as previously defined) and one or more zwitterions.
  • zwitterions there may be mentioned amino acids or derivatives, or molecules synthesized from acids amines.
  • Betaines may also be mentioned, such as phosphorus betaines and / or ammonium betaines.
  • such aqueous foams comprise a mixture of 25 to 55% glycerol (expressed in percentages by weight relative to the total mass of foam).
  • these aqueous foams comprise less than 5%, advantageously less than 2%, or even less than 1% of preferably anionic surfactant.
  • these aqueous foams comprise less than 5%, preferably less than 2%, or even less than 1% of zwitterion, preferably selected from ammonium betaines.
  • such an aqueous foam comprises 35 to 45% of glycerol, ideally 40%, mixed with less than 0.5% of dodecylpolyoxyethylene-3-sulfate, less than 0.5% of cocoamidopropyl betaine and less than 0.05% of myristic acid.
  • the binder used in the composition used to obtain the thermally insulating material according to the invention is an organic binder, preferably a latex.
  • the thermal insulating material according to the invention is obtained from a mixture comprising at least one organic binder and at least one inorganic binder.
  • the weight of organic binder represents a content of less than 25% relative to the total weight of binder (organic and inorganic), preferably this level is less than 15%, more preferably it is less than 10%, or even less than 10%. 8%.
  • the binder (s) can (s) consist solely of inorganic material (s), which ensures the fireproof properties of the insulating material.
  • latex in the sense of the present invention refers in particular latex polymers usually used in building materials.
  • polymers that may be included in the composition of such a powder, mention may be made, for example, of elastomeric latices, thermoplastic latices and thermosetting latices.
  • the term "latex" means an aqueous emulsion or dispersion of one or more natural or synthetic, generally thermoplastic, polymeric substances.
  • the polymer (s) may be self-emulsifiable, or else the emulsion or dispersion is stabilized by suitable surfactants.
  • a latex useful in the context of the present invention advantageously has a glass transition temperature Tg of less than 50 ° C. Ideally the Tg should be between -50 ° C and 25 ° C, preferably between -20 ° C and 10 ° C, preferably between -10 ° C and 0 ° C, or be substantially -5 ° C. Such ranges of Tg make it possible to obtain a desired rigidity for the insulating materials to be applied to a support in the field of building construction, since the product obtained is flexible and deformable.
  • polymers with a Tg at most slightly less than room temperature are also preferred.
  • the latex contains a polymer, copolymer or terpolymer (or more) of vinyl type, acrylic type and / or carboxylic acid derivative.
  • Vinyl-type latices in particular with pendant ester functional groups, or based on copolymers of vinyl chloride and of olefin, whether or not silanized, are particularly preferred.
  • Mention may in particular be made of vinyl acetate-based latexes, in particular based on polyvinyl acetate homopolymer, or vinyl acetate copolymer, and especially acid and / or ester copolymer. (meth) acrylic, maleic ester, olefin and / or vinyl chloride, or based on vinyl chloride / ethylene copolymer.
  • Other useful latexes may be chosen from those containing a polymer of acrylic and / or methacrylic type, especially an acrylonitrile / acrylic ester copolymer, or styrene / acid or silanized acrylic ester (that is to say copolymerized with a monomer with ethylenic unsaturation carrying at least one silane or silanol function).
  • the latex may advantageously be a styrene-acrylic copolymer, or an all-acrylic copolymer (derived from different acrylic monomers) obtained by radical polymerization in emulsion or dispersion. These latices are stabilized with acrylic acid and / or acrylonitrile.
  • Such polymers marketed by BASF are found in the range referenced by the name Acronal®, in particular Acronal® S 400. It is also possible to use alternatively or in combination any latex (one or more) of this Acronal range. ®.
  • the powders marketed by the company Hexion TM and the Axilat TM UP range such as the Axilat TM UP 620 E.
  • the Axilat TM UP 620 E, as well as the Axilat TM UP 600 B and the Axilat TM UP 820 A, are terpolymers of vinyl acetate, vinyl versatate and maleic ester.
  • the thermal conductivity of the material according to the invention is generally less than or equal to 27 mW / m.K.
  • the thermal conductivity of the material according to the invention is less than or equal to 25 mW / m ⁇ K, and is advantageously less than or equal to 23 mW / m ⁇ K; particularly preferably it is less than or equal to 20 mW / m.K, or even less than or equal to 19 mW / m.K.
  • the densities of thermal insulating materials obtained according to the invention described above are generally less than 250 kg / m 3 .
  • the densities of thermal insulation materials obtained according to the invention described above are typically less than or equal to 150 kg / m 3 (for comparison the density of an airgel block is of the order of 150 kg / m 3 ).
  • the density of the insulating material according to the invention is less than or equal to 130 kg / m 3 and advantageously preferred 120 kg / m 3 , advantageously the density is less than or equal to 100 kg / m 3 , or even less than or equal to 85 kg / m 3 , and even less than or equal to 70 kg / m 3 , or even less than or equal to at 55 kg / m 3 .
  • the invention also relates to a method of manufacturing the thermal insulation material described above, comprising the steps of: a) preparing an aqueous foam;
  • step a) it is possible to add the binder directly to step a) during the preparation of the aqueous foam.
  • This aspect is dependent on the binder used: when latexes in the form of powder are used, the binder can be added after the preparation of the stable aqueous foam, that is to say in step b), whereas uses a latex in the form of a dispersion / suspension in a liquid (preferably aqueous) it will be added preferably in step a).
  • the shaping and drying step may comprise casting operations or molding of said preparation in cavities of appropriate shape or section.
  • molding is to be taken in the broadest sense and covers any form of conformation, such as open mold casting, extrusion through a die and cutting the extrudate, etc.
  • the shaping can be achieved by co-extruding the preparation with a polymeric organic phase, and / or with gypsum, to make a surface layer.
  • thermal insulating material within the meaning of the invention described above can be used in the form of at least one layer applied for example on a plasterboard.
  • a particularly elastic and deformable insulating material may be impregnated or spread over a web (for example non-woven ).
  • the aqueous foam is prepared as follows: a) stir-foaming a mixture comprising the cationic surfactant; b) then adding an aqueous solution comprising the anionic surfactant.
  • the inventors have demonstrated that an aqueous foam prepared and remained stable throughout the manufacturing process, even after incorporating the other ingredients (airgel, fillers, adjuvants ).
  • the conductivity measurement is carried out according to the principle of the Flash method (BALAGEAS D. - Measurement of thermal diffusivity by the flash method, R 2955, Engineering Technique, Measurement and Control Treaty -1986), where the thermal excitation is obtained by a plane heating resistor, in accordance with the protocol described in the document "A new method for measuring the thermophysical properties of super-insulators", Yves Jannot & Alain Degiovanni, Infrared thermography conference for building and public works, Mesurexpo (Villepinte ), October 2, 2008.
  • the characterization temperature ranges from 34 to 37 ° C, and measurements are made at atmospheric pressure.
  • the accuracy of the measurements is estimated at 5%.
  • Thermal conductivities were also measured with a NETZSCH TM HFM 436 series flowmeter following the protocols established by ASTM C518 and ISO 8301. The measured samples have dimensions of 15x15x5 cm 3 .
  • the density is determined by the ratio of the mass of the sample by its volume.
  • a kit provided by the company Allied Foam is used (the percentages are weight contents calculated with respect to the total mass of the compositions):
  • Component 2 of commercial reference 510B is Component 2 of commercial reference 510B:
  • Anionic surfactant mixture belonging to the class of fatty acids 15-30%
  • the foam is generated by a foam generator marketed by the company Allied Foam.
  • Component 1 is diluted to 136 g for 1 L of water.
  • Component 2 is introduced directly into the tank provided for this purpose.
  • aqueous foam prepared as follows may be used:
  • Two aqueous solutions (1 and 2) are prepared as follows (the percentages are weight contents calculated with respect to the total mass of the solutions after dilution):
  • Solution 1 (supplemented to 200 g with distilled water) is prepared by adding 3.2% by weight of Arquad® T50 marketed by BASF (49% of propylene glycol, 51% of tallowtrimethylammonium chloride (64% of C18 alkyl, 31% of C16 alkyl, 4% of C14 alkyl and 1% of C12 alkyl, suspended in propylene glycol) in suspension in water) and 0.65% mass of Triton® X-405 sold by Dow Chemical (70% octylphenol ethoxylate).
  • Arquad® T50 marketed by BASF
  • Triton® X-405 sold by Dow Chemical (70% octylphenol ethoxylate
  • Solution 2 (supplemented to 40 g with distilled water) is prepared by adding 5% potassium stearate.
  • Solution 1 is introduced into a high speed mixer (Kenwood Major 1800 Watts). To the foam obtained by this first mixture, the solution 2 is added and mixed.
  • aqueous foam 250 g of freshly obtained aqueous foam are weighed to which 100 g of styrene-acrylic ester copolymer (latex) in aqueous solution (Acronal® S 400, BASF, whose latex content is 57%) are added.
  • latex styrene-acrylic ester copolymer
  • the silica aerogels used for the realization of the invention are produced by the company Cabot: they are in the form of millimetric granules, it was necessary to grind and sieve in order to obtain the desired particle size for the test .
  • the sieving is carried out by grinding the aerogels above a sieve whose mesh width is 250 ⁇ .
  • the powder recovered after sieving thus has a smaller particle size equal to 250 ⁇ .
  • the airgel powder is introduced into the foam during kneading; this operation has a duration of about 5 minutes.
  • the pulp which has undergone a mass loss of about 50%, has hardened and is in the form of a solid having a certain flexibility, this also depending on the amount of aerogels present in the mixed.
  • the aerogels are present in the final product at a content of approximately 50% of the total volume.
  • the protocol is identical to that of Example 1, but the silica aerogels (Nanogel® TLD 302) are not sieved. Thus the aerogels were not subjected to sieving, but inserted into the mixture in the form of millimetric granules.
  • the change in the size of the aerogels makes it possible to introduce a larger quantity into the latex-reinforced foam: 140 g. This is because the foam does not undergo settlement and / or collapse, a phenomenon which is observed during the manufacture of the sample during the introduction of aerogels of smaller particle size equal to 250 ⁇ .
  • Sample 5 the sample, referred to as Sample 5, was subjected to a thermal conductivity measurement.
  • the product is particularly flexible and aerated, it was necessary to squeeze the sample between the plates of the measuring apparatus in order to obtain a thermal conductivity value for a determined corresponding density.
  • Two aqueous solutions (1 and 2) are prepared as follows (the percentages are weight contents calculated with respect to the total mass of the solutions after dilution):
  • Solution 1 is prepared by adding 3.2% by weight of Arquad® T50 marketed by BASF (49% of propylene glycol, 51% of tallowtrimethylammonium chloride (64% of C18 alkyl, 31% of alkyl). C16, 4% C14 alkyl and 1% C12 alkyl, suspended in propylene glycol) in suspension in water) and 0.65% by weight of Triton® X-405 marketed by Dow Chemical (70% octylphenol ethoxylate), the whole is added to a solution of distilled water to obtain an aqueous solution of 200 g.
  • Solution 2 is prepared by adding 5% by weight of potassium stearate to a solution of distilled water to obtain an aqueous solution of 40 g.
  • Solution 1 is introduced into a high speed mixer (Kenwood Major 1800 Watts) and foamed by stirring at maximum speed for two minutes. To this first foam, solution 2 is added. The mixture is stirred at maximum speed for two minutes to obtain the stable aqueous foam. 3.2 Transformation of the aqueous foam into finished product:
  • 230 g of the stable aqueous foam freshly prepared are weighed according to the protocol described in 3.1, to which is added an inorganic binder formed from a plaster batch formed from powdered plaster, optionally sodium silicate (NaO / SiO 2 .3H 2 O) powder, and an organic latex of the vinyl terpolymer powder type (Axilat® UP 620 E, Hexion Company, with a latex content of 90-95%) with a solid / water in the mix of 10: 9 by weight. Stirring continues in the mixer: it is now a mixing because the foam becomes more and more pasty.
  • an inorganic binder formed from a plaster batch formed from powdered plaster, optionally sodium silicate (NaO / SiO 2 .3H 2 O) powder
  • an organic latex of the vinyl terpolymer powder type (Axilat® UP 620 E, Hexion Company, with a latex content of 90-95%) with a solid / water in the mix
  • the silica aerogels sold by Cabot (Nanogel® TLD 302), a fraction of which is sieved to a particle size of less than or equal to 250 ⁇ , are incorporated into the foamed mixture.
  • the silica aerogels sold by Cabot Nagel® TLD 302
  • one more dough is obtained in addition compact, depending on the amount of aerogels introduced, which remains however easy enough to spread and manipulate to give it different forms.
  • the paste which has undergone a weight loss of about 50%, has hardened and is in the form of a solid having a certain flexibility, this also depending on the amount of aerogels present in the mixture.
  • Two aqueous solutions (1 and 2) are prepared as follows (the percentages are weight contents calculated with respect to the total mass of the solutions after dilution):
  • Solution 1 is prepared by adding 3.2% by weight of Arquad® T50 marketed by BASF (49% of propylene glycol, 51% of tallowtrimethylammonium chloride (64% of C18 alkyl, 31% of alkyl). C16, 4% C14 alkyl and 1% C12 alkyl, suspended in propylene glycol) in suspension in water) and 0.65% by weight of Triton® X-405 marketed by Dow Chemical ( 70% octylphenol ethoxylate), the whole is added to a solution of distilled water to obtain an aqueous solution of 200 g.
  • Arquad® T50 marketed by BASF (49% of propylene glycol, 51% of tallowtrimethylammonium chloride (64% of C18 alkyl, 31% of alkyl). C16, 4% C14 alkyl and 1% C12 alkyl, suspended in propylene glycol) in suspension in water
  • Triton® X-405 marketed by Dow Chemical ( 70% oct
  • Solution 2 is prepared by preparing an aqueous solution (distilled water) of 40 g containing 5% by weight of potassium stearate, to which 25-38% by weight of spraying is added with stirring by the operator.
  • an organic binder of the styrene-acrylic ester copolymer (latex) type in aqueous solution (Acronal® S 400, BASF, the latex content of which is 57%).
  • Solution 1 is introduced into a high speed mixer (Kenwood Major 1800 Watts) and foamed by stirring at maximum speed for two minutes. To this first foam, solution 2 is added. The mixture is stirred at maximum speed for two minutes to obtain the stable aqueous foam.
  • the silica aerogels sold by Cabot (Nanogel® TLD 302), a fraction of which is sieved to a particle size of less than or equal to 250 ⁇ , are incorporated into the foamed mixture.
  • an increasingly compact paste is obtained, depending on the amount of aerogels introduced, which remains fairly easy to spread and handle to give it different shapes.
  • the paste which has undergone a weight loss of about 50%, has hardened and is in the form of a solid having a certain flexibility, this also depending on the amount of aerogels present in the mixture.
  • the amounts of reagents used and the experimental results are reported in Table 3.
  • aqueous foam Two aqueous solutions (1 and 2) are prepared as follows (the percentages are weight contents calculated with respect to the total mass of the solutions after dilution):
  • Solution 1 is prepared by adding 3.2% by weight of Arquad® T50 marketed by BASF (49% of propylene glycol, 51% of tallowtrimethylammonium chloride (64% of C18 alkyl, 31% of alkyl). C16, 4% C14 alkyl and 1% C12 alkyl, suspended in propylene glycol) in suspension in water) and 0.65% by weight of Triton® X-405 marketed by Dow Chemical ( 70% octylphenol ethoxylate), the whole is added to a solution of distilled water to obtain an aqueous solution of 200 g.
  • Arquad® T50 marketed by BASF (49% of propylene glycol, 51% of tallowtrimethylammonium chloride (64% of C18 alkyl, 31% of alkyl). C16, 4% C14 alkyl and 1% C12 alkyl, suspended in propylene glycol) in suspension in water
  • Triton® X-405 marketed by Dow Chemical ( 70% oct
  • Solution 2 is prepared by adding 5% by weight of potassium stearate to a solution of distilled water to obtain an aqueous solution of 40 g.
  • Solution 1 is introduced into a high speed mixer (Kenwood Major 1800 Watts) and foamed by stirring at maximum speed for two minutes. To this first foam, solution 2 is added. The mixture is stirred at maximum speed for two minutes to obtain the stable aqueous foam.
  • the silica aerogels sold by Cabot (Nanogel® TLD 302), a fraction of which is sieved to a particle size of less than or equal to 250 ⁇ , are incorporated into the foamed mixture.
  • an increasingly compact paste is obtained, depending on the amount of aerogels introduced, which remains fairly easy to spread and handle to give it different shapes.
  • the paste which has undergone a weight loss of about 50%, has hardened and is in the form of a solid having a certain flexibility, this also depending on the amount of aerogels present in the mixture.

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EP11707455A 2010-02-03 2011-02-03 Materiaux d'isolation thermique hautes performances Withdrawn EP2531553A1 (fr)

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FR1050744A FR2955863B1 (fr) 2010-02-03 2010-02-03 Materiaux d'isolation thermique hautes performances
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FR2977888B1 (fr) 2011-07-13 2014-01-10 Saint Gobain Isover Materiaux d'isolation thermique hautes performances.
FR2977889B1 (fr) * 2011-07-13 2014-01-10 Saint Gobain Isover Materiaux d'isolation thermique hautes performances
FR2991315B1 (fr) * 2012-06-05 2014-05-16 Saint Gobain Isover Produits d'isolation thermique hautes performances
FR2991316B1 (fr) * 2012-06-05 2014-05-16 Saint Gobain Isover Produits d'isolation thermique hautes performances
CN104603344B (zh) * 2012-06-26 2020-03-31 卡博特公司 柔性绝缘结构及其制造和使用方法
KR101804345B1 (ko) * 2013-07-04 2017-12-06 알이엠텍 주식회사 단열 조성물, 이의 제조방법 및 이를 이용한 단열 소재
US9764301B2 (en) * 2013-11-14 2017-09-19 Nanyang Technological University Silica aerogel composite
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US9045609B2 (en) 2015-06-02
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ZA201206096B (en) 2013-04-24
WO2011095745A1 (fr) 2011-08-11
FR2955863A1 (fr) 2011-08-05
US20150183947A1 (en) 2015-07-02
JP2013518961A (ja) 2013-05-23
BR112012019417B1 (pt) 2020-03-10
RU2585645C2 (ru) 2016-05-27
RU2012137251A (ru) 2014-03-10
FR2955863B1 (fr) 2012-03-09
BR112012019417A2 (pt) 2018-03-20
US20120326071A1 (en) 2012-12-27

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