WO2009093002A2 - Liquid formulation of microporous thermal insulation material, method of manufacture, and use thereof - Google Patents

Liquid formulation of microporous thermal insulation material, method of manufacture, and use thereof Download PDF

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Publication number
WO2009093002A2
WO2009093002A2 PCT/GB2009/000084 GB2009000084W WO2009093002A2 WO 2009093002 A2 WO2009093002 A2 WO 2009093002A2 GB 2009000084 W GB2009000084 W GB 2009000084W WO 2009093002 A2 WO2009093002 A2 WO 2009093002A2
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emulsion
percent
formulation
opacifier
weight
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PCT/GB2009/000084
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French (fr)
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WO2009093002A3 (en
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Oras Khalid Abdul-Kader
Luc Heymans
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Microtherm N.V.
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Publication of WO2009093002A2 publication Critical patent/WO2009093002A2/en
Publication of WO2009093002A3 publication Critical patent/WO2009093002A3/en

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    • 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
    • E04B1/7654Heat, 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 comprising an insulating layer, disposed between two longitudinal supporting elements, e.g. to insulate ceilings
    • E04B1/7658Heat, 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 comprising an insulating layer, disposed between two longitudinal supporting elements, e.g. to insulate ceilings comprising fiber insulation, e.g. as panels or loose filled fibres
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/06Aluminous cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • C04B28/26Silicates of the alkali metals
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/34Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B30/00Compositions for artificial stone, not containing binders
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/45Anti-settling agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres
    • 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
    • E04B1/78Heat insulating elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

Definitions

  • This invention relates to a liquid formulation of a microporous thermal insulation material and to a method of manufacturing the liquid formulation and to the use thereof.
  • the liquid formulation may be used for manufacturing a microporous thermal insulation material, for example comprising a microporous material supported by a flexible mat.
  • microporous' is used herein to identify dry porous or cellular materials in which the ultimate size of the cells or voids is less than the mean free path of an air molecule at NTP, i.e. of the order of 100 nm or smaller.
  • a material which is microporous in this sense will exhibit very low transfer of heat by air conduction (that is collisions between air molecules).
  • microporous materials include aerogel, which is a gel in which the liquid phase has been replaced by a gaseous phase in such a way as to avoid the shrinkage which would occur if the gel were dried directly from a liquid.
  • aerogel which is a gel in which the liquid phase has been replaced by a gaseous phase in such a way as to avoid the shrinkage which would occur if the gel were dried directly from a liquid.
  • a substantially identical structure can be obtained by controlled precipitation from solution, the temperature and pH being controlled during precipitation to obtain an open lattice precipitate.
  • Microporous thermal insulation materials have a particularly low thermal conductivity, but tend to be weak and brittle and cannot readily be formed into a variety of shapes. For example, it is not possible to supply a microporous thermal insulation material as a roll of material which can be unrolled and cut to size and shape to be positioned around irregular shapes. Microporous thermal insulation materials are also generally sensitive to water and excessive moisture, which tend to break down the microporous structure and significantly degrade the thermal insulation characteristics of the materials. Consequently, microporous thermal insulation materials are generally formulated as dry materials by mixing the components of the insulation material in a dry manner and compressing the resulting mixture into a solid block, often within a protective envelope. However, such formulations do not allow the insulation material to be readily transported and cut to size and shape to be positioned around irregular shapes.
  • a liquid formulation of a microporous thermal insulation material comprising an emulsion including:
  • microporous thermal insulating material in a proportion ranging from 10 to 90 percent by weight of the combination of opacifier and microporous thermal insulating material;
  • a binder a binder
  • a dispersion agent a dispersion agent
  • a microporous thermal insulation material comprising the steps of:
  • the impregnated mat may be dried at a temperature less than 200 degrees Celsius for several hours.
  • the fibrous mat may be impregnated with the emulsion by dipping the mat in the emulsion.
  • the emulsion may be injected into a fibrous mat.
  • the fibrous mat may comprise, for example, two layers which have been joined by a needling operation prior to injection of the emulsion.
  • the proportion of microporous material in the combination of opacifier and microporous material may be from 20 to 80 percent by weight, more preferably from 20 to 60 percent by weight.
  • the emulsion may have a solids content in the range from substantially 5 to substantially 15 percent by weight.
  • the binder may be incorporated into the emulsion in an amount from 1 to 10, preferably substantially 5, percent by weight of the combination of opacifier and microporous material (the dry mixture).
  • the dispersion agent may be incorporated into the emulsion in an amount from 0.1 to 0.5, preferably substantially 0.3, percent by weight of the combination of opacifier and microporous material (the dry mixture).
  • the microporous material may be selected from pyrogenic metal oxides, such as of silicon, aluminium and/or titanium, precipitated silica and volatilised silica.
  • the opacifier may be selected from: an oxide such as titanium dioxide, for example in the form of rutile; a carbide, such as silicon carbide; a silicate, such as zircon (zirconium silicate); and ilmenite.
  • the binder may be an inorganic binder or an organic binder.
  • Suitable inorganic binders include; colloidal silicas; silicates, such as potassium silicate; phosphates; aluminas; and cements.
  • Suitable organic binders include: silicones; polyacrylics; polyvinylalcohols; polyoxyethylenes; polyelectrolytes; and polysaccharides.
  • the dispersion agent may be selected from alkali-free deflocculating agents, and
  • Example 1 Initially, a dry fibre-free mixture was produced consisting of 60 percent by weight of microporous material in the form of pyrogenic (fumed) silica in the form of Aerosil 200 available from Degussa AG, Germany and 40 percent by weight of an opacifier in the form of rutile (titanium dioxide) having a particle size less that 9 ⁇ m available from Eggerding, Netherlands. Aerosil 200 is a conventional, non- hydrophobic form of pyrogenic silica.
  • the dry mixture was then converted into an emulsion by mixing with water together with a binder in the form of a colloidal silica binder sold under the name Ludox HS40 available from W R Grace Davison, Germany, the binder having a solids content of 40 percent by weight.
  • the binder plays a dual role in the liquid formulation, namely as a stabilising agent in the liquid and as an aid to reduce the presence of dust once the final product has been dried.
  • the emulsion was completed by the addition of a dispersion agent in the form of Duramax D-3005 available from Rohm and Haas, France.
  • the emulsion was formulated at different solids content levels in different examples, the constituents being mixed together using a conventional paint mixer.
  • 600 g of the dry mixture described above was formulated with 3 litres of water, to which were added 30 g Ludox HS40 binder (that is, 12 g colloidal silica in water) and 1.8 g Duramax D-3005 dispersion agent and the constituents were mixed together.
  • the resulting emulsion contained substantially 20 percent by weight solids.
  • the resulting emulsion was found to be too viscous to dip a mat of glass fibre material.
  • 450 g of the dry mixture described above was formulated with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together.
  • the resulting emulsion contained substantially 15 percent by weight solids.
  • a non-woven mat of glass fibre material available from Hiltex Technische Weefsels, Netherlands, having a weight of 400 g/m 2 , a thickness of 6 mm and an initial thermal conductivity of 119 mW/m.K at a mean temperature of 200 degrees Celsius was hand-dipped in the emulsion and then dried at a temperature less than 200 degrees Celsius for several hours. The dried mat was found to have a thermal conductivity of 73 mW/m.K at a mean temperature of 200 degrees Celsius. This value represents an improvement (reduction) over the thermal conductivity of the glass fibre mat alone of some 39 percent. The dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
  • 300 g of the dry mixture described above was formulated with 3 litres of water, to which were added 15 g Ludox HS40 binder (that is, 6 g colloidal silica in water) and 0.9 g Duramax D-3005 dispersion agent and the constituents were mixed together.
  • the resulting emulsion contained substantially 10 percent by weight solids.
  • Example 2 A mat of glass fibre material as described above in Example 2 was hand-dipped in the emulsion and then dried as described above in Example 2. The dried mat was found to have a thermal conductivity of 75 mW/m.K at a mean temperature of 200 degrees Celsius. This value represents an improvement (reduction) over the thermal conductivity of the glass fibre mat alone of some 37 percent. The dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
  • Example 4 15O g of the dry mixture described above was formulated with 3 litres of water, to which were added 7.5 g Ludox HS40 binder (that is, 3 g colloidal silica in water) and 0.45 g Duramax D-3005 dispersion agent and the constituents were mixed together.
  • the resulting emulsion contained substantially 5 percent by weight solids.
  • Example 2 A mat of glass fibre material as described above in Example 2 was hand-dipped in the emulsion and then dried as described above in Example 2. The dried mat was found to have a thermal conductivity of 77 mW/m.K at a mean temperature of 200 degrees Celsius. This value represents an improvement (reduction) over the thermal conductivity of the glass fibre mat alone of some 35 percent. The dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
  • An emulsion was prepared having a 15 percent by weight solids content as explained above in Example 3 and was injected into a glass fibre mat of material as described above in Example 2 and which had previously been formed from two separate layers joined together by a needling procedure using a machine available from Larocha SA, France, and described, for example, in US-A-5475 904.
  • the resulting mat was dried as explained above and was found to have a thermal conductivity of 79 mW/m.K at a mean temperature of 200 degrees Celsius. This value represents an improvement (reduction) over the thermal conductivity of the glass fibre mat alone of some 34 percent.
  • the dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
  • a dry fibre-free mixture was produced consisting of 80 percent by weight of microporous material in the form of pyrogenic (fumed) silica in the form of Aerosil 200 available from Degussa AG, Germany and 20 percent by weight of an opacifier in the form of rutile (titanium dioxide) having a particle size less that 9 ⁇ m available from Eggerding, Netherlands.
  • 450 g of the dry mixture described above was formulated with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together.
  • the resulting emulsion contained substantially 15 percent by weight solids.
  • a mat of glass fibre material as described above in Example 2 was hand-dipped in the emulsion and then dried as described above in Example 2.
  • the dried mat was found to have a thermal conductivity of 52 mW/m.K at a mean temperature of 200 degrees Celsius, representing an improvement (reduction) of about 56 percent compared with the original mat.
  • the dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
  • Example 6 The use of the emulsion of Example 6 is not ideal. The proportion of fumed silica is high and the resulting product is corresponding expensive to produce. Moreover, the emulsion has relatively high viscosity and is not ideal for dipping a mat of glass fibre material. When the emulsion was injected between two layers of glass fibre mat and subjected to the needling procedure of Example 5 the emulsion did not infiltrate the mat and the resulting product was unacceptable.
  • a dry fibre-free mixture was produced consisting of 20 percent by weight of microporous material in the form of pyrogenic (fumed) silica in the form of Aerosil 200 available from Degussa AG, Germany and 80 percent by weight of an opacifier in the form of rutile (titanium dioxide) having a particle size less that 9 ⁇ m available from Eggerding, Netherlands.
  • 450 g of the dry mixture described above was formulated with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together.
  • the resulting emulsion contained substantially 15 percent by weight solids.
  • Example 2 A mat of glass fibre material as described above in Example 2 was hand-dipped in the emulsion, which was less viscous than the emulsion of Example 6, and then dried as described above in Example 2. The dried mat was found to have a thermal conductivity of 49 mW/m.K at a mean temperature of 200 degrees
  • the dipped mat remained flexible after drying and was found to be suitable for applications up to about 600 degrees Celsius.
  • Example 7 450 g of rutile opacifier as described above in Example 7 was formulated into an emulsion with 3 litres of water, to which were added 22.5 g Ludox HS40 binder
  • Example 7 450 g of pyrogenic silica as described above in Example 7 was formulated into an emulsion with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together.
  • the resulting emulsion contained substantially 15 percent by weight solids.
  • the emulsion was found to be too viscous for dipping and no trials were conducted.
  • a dry fibre-free mixture was produced consisting of 60 percent by weight of microporous material in the form of pyrogenic (fumed) silica in the form of Aerosil
  • rutile titanium dioxide
  • 450 g of the dry mixture described above was formulated with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together.
  • the resulting emulsion contained substantially 15 percent by weight solids.
  • a non-woven mat of silica fibre material available from belChem, Germany, having a weight of 480 g/m 2 , a thickness of 6 mm and an initial thermal conductivity of 110 mW/m.K at a mean temperature of 200 degrees Celsius was hand-dipped in the emulsion, which was less viscous than the emulsion of Example 6, and then dried as described above in Example 2.
  • the dried mat was found to have a thermal conductivity of 75 mW/m.K at a mean temperature of 200 degrees Celsius, representing an improvement (reduction) of about 32 percent compared with the original mat.
  • the dipped mat remained flexible after drying and was found to be suitable for applications up to about 1000 degrees Celsius.
  • the liquid formulation can be used as a coating, for example being applied by spraying or brushing, in a gel or paste form, or can be employed in injection moulding or extrusion.
  • the present invention provides a liquid formulation of microporous material which can be used for a number of different purposes. When used to impregnate a mat, it produces a microporous thermal insulation material which is flexible and can be supplied as a roll of material which can be cut to size and positioned around irregular shapes.
  • the liquid formulation, or emulsion, of microporous material is fibre-free, the reinforcing effect normally provided by fibres incorporated into the microporous material being provided by the fibrous mat.
  • pyrogenic silica can be replaced totally or partially by other microporous materials. These include other pyrogenic metal oxides and other forms of silica, such as precipitated and volatilised silicas.
  • Suitable precipitated silicas include some of those from the Sipernat range available from Degussa in Germany, while a suitable volatilised silica is RW-Fuller silica available from RW Silicium, Germany.
  • the rutile opacifier can be replaced by other opacifiers such as silicon carbide, zircon (zirconium silicate), ilmenite and other carbide, silicate or oxide type opacifiers.
  • Alternative binders can be employed. These include both inorganic and organic binders.
  • Suitable inorganic binders include colloidal silica, silicate (such as potassium silicate type K66 available from lneos Silicas in the United Kingdom), phosphate, alumina and cement binders.
  • Suitable organic binders include silicone, polyacrylic (such as Duramax B 1000 available from Rohm & Haas, France), polyvinylalcohol (such as Optapix AC 112 available from Zschimmer & Schwarz, Germany), polyoxyethylene, polyelectrolyte and polysaccharide (cellulose/starch) binders.
  • Alternative dispersing agents include KV5068 and KV5166 available from Zschimmer & Schwarz, Germany, which are both alkali-free deflocculating agents, and Dispex A40 available from Ciba Speciality Chemicals, Switzerland, which is an acrylic dispersing agent widely used for dispersing inorganic minerals.

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Abstract

A liquid formulation of a microporous thermal insulation material comprises an emulsion including an opacifier, a microporous thermal insulating material in a proportion ranging from 10 to 90 percent by weight of the combination of opacifier and microporous thermal insulating material, water, a binder, and a dispersion agent. The formulation may be made by preparing a dry, fibre-free mixture of a microporous thermal insulating material and an opacifier in a proportion ranging from 10 to 90 percent by weight microporous material, and mixing together the dry mixture with water, a binder and a dispersion agent to form an emulsion. A microporous thermal insulation material may be made by impregnating a fibrous mat with the emulsion, and drying the impregnated mat.

Description

LIQUID FORMULATION OF MICROPOROUS THERMAL
INSULATION MATERIAL, METHOD OF MANUFACTURE,
AND USE THEREOF
This invention relates to a liquid formulation of a microporous thermal insulation material and to a method of manufacturing the liquid formulation and to the use thereof. For example, the liquid formulation may be used for manufacturing a microporous thermal insulation material, for example comprising a microporous material supported by a flexible mat.
The term 'microporous' is used herein to identify dry porous or cellular materials in which the ultimate size of the cells or voids is less than the mean free path of an air molecule at NTP, i.e. of the order of 100 nm or smaller. A material which is microporous in this sense will exhibit very low transfer of heat by air conduction (that is collisions between air molecules). Such microporous materials include aerogel, which is a gel in which the liquid phase has been replaced by a gaseous phase in such a way as to avoid the shrinkage which would occur if the gel were dried directly from a liquid. A substantially identical structure can be obtained by controlled precipitation from solution, the temperature and pH being controlled during precipitation to obtain an open lattice precipitate. Other equivalent open lattice structures include pyrogenic (fumed) and electro-thermal types in which a substantial proportion of the particles have an ultimate particle size less than 100 nm. Any of these materials, based for example on silica, alumina or other metal oxides, may be used to prepare a dry composition which is microporous as defined above.
Microporous thermal insulation materials have a particularly low thermal conductivity, but tend to be weak and brittle and cannot readily be formed into a variety of shapes. For example, it is not possible to supply a microporous thermal insulation material as a roll of material which can be unrolled and cut to size and shape to be positioned around irregular shapes. Microporous thermal insulation materials are also generally sensitive to water and excessive moisture, which tend to break down the microporous structure and significantly degrade the thermal insulation characteristics of the materials. Consequently, microporous thermal insulation materials are generally formulated as dry materials by mixing the components of the insulation material in a dry manner and compressing the resulting mixture into a solid block, often within a protective envelope. However, such formulations do not allow the insulation material to be readily transported and cut to size and shape to be positioned around irregular shapes.
It is therefore an object of the present invention to provide a liquid formulation of a microporous material, and a method of manufacturing the same, which overcomes or at least ameliorates at least some of the above-mentioned disadvantages. It is a further object of the present invention to provide such a liquid formulation which can be used for manufacturing a microporous thermal insulation material which overcomes or at least ameliorates at least some of the above-mentioned disadvantages.
According to one aspect of the present invention there is provided a liquid formulation of a microporous thermal insulation material comprising an emulsion including:
an opacifier;
a microporous thermal insulating material in a proportion ranging from 10 to 90 percent by weight of the combination of opacifier and microporous thermal insulating material;
water;
a binder; and a dispersion agent.
According to another aspect of the present invention there is provided a method of manufacturing a liquid microporous material comprising the steps of:
preparing a dry, fibre-free mixture of a microporous thermal insulating material and an opacifier in a proportion ranging from 10 to 90 percent by weight microporous material; and
mixing together the dry mixture with water, a binder and a dispersion agent to form an emulsion.
According to a further aspect of the present invention there is provided a method of manufacturing a microporous thermal insulation material comprising the steps of:
impregnating a fibrous mat with the emulsion as defined above; and
drying the impregnated mat.
The impregnated mat may be dried at a temperature less than 200 degrees Celsius for several hours.
The fibrous mat may be impregnated with the emulsion by dipping the mat in the emulsion. Alternatively, the emulsion may be injected into a fibrous mat. The fibrous mat may comprise, for example, two layers which have been joined by a needling operation prior to injection of the emulsion.
The proportion of microporous material in the combination of opacifier and microporous material (the dry mixture) may be from 20 to 80 percent by weight, more preferably from 20 to 60 percent by weight. - A -
The emulsion may have a solids content in the range from substantially 5 to substantially 15 percent by weight.
The binder may be incorporated into the emulsion in an amount from 1 to 10, preferably substantially 5, percent by weight of the combination of opacifier and microporous material (the dry mixture).
The dispersion agent may be incorporated into the emulsion in an amount from 0.1 to 0.5, preferably substantially 0.3, percent by weight of the combination of opacifier and microporous material (the dry mixture).
The microporous material may be selected from pyrogenic metal oxides, such as of silicon, aluminium and/or titanium, precipitated silica and volatilised silica.
The opacifier may be selected from: an oxide such as titanium dioxide, for example in the form of rutile; a carbide, such as silicon carbide; a silicate, such as zircon (zirconium silicate); and ilmenite.
The binder may be an inorganic binder or an organic binder. Suitable inorganic binders include; colloidal silicas; silicates, such as potassium silicate; phosphates; aluminas; and cements. Suitable organic binders include: silicones; polyacrylics; polyvinylalcohols; polyoxyethylenes; polyelectrolytes; and polysaccharides.
The dispersion agent may be selected from alkali-free deflocculating agents, and
(poly)acrylics.
Aspects of the invention are illustrated by the following examples.
Example 1 Initially, a dry fibre-free mixture was produced consisting of 60 percent by weight of microporous material in the form of pyrogenic (fumed) silica in the form of Aerosil 200 available from Degussa AG, Germany and 40 percent by weight of an opacifier in the form of rutile (titanium dioxide) having a particle size less that 9 μm available from Eggerding, Netherlands. Aerosil 200 is a conventional, non- hydrophobic form of pyrogenic silica. The dry mixture was then converted into an emulsion by mixing with water together with a binder in the form of a colloidal silica binder sold under the name Ludox HS40 available from W R Grace Davison, Germany, the binder having a solids content of 40 percent by weight. The binder plays a dual role in the liquid formulation, namely as a stabilising agent in the liquid and as an aid to reduce the presence of dust once the final product has been dried. The emulsion was completed by the addition of a dispersion agent in the form of Duramax D-3005 available from Rohm and Haas, France. The emulsion was formulated at different solids content levels in different examples, the constituents being mixed together using a conventional paint mixer.
600 g of the dry mixture described above was formulated with 3 litres of water, to which were added 30 g Ludox HS40 binder (that is, 12 g colloidal silica in water) and 1.8 g Duramax D-3005 dispersion agent and the constituents were mixed together. The resulting emulsion contained substantially 20 percent by weight solids.
The resulting emulsion was found to be too viscous to dip a mat of glass fibre material.
Example 2
450 g of the dry mixture described above was formulated with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together. The resulting emulsion contained substantially 15 percent by weight solids.
A non-woven mat of glass fibre material, available from Hiltex Technische Weefsels, Netherlands, having a weight of 400 g/m2, a thickness of 6 mm and an initial thermal conductivity of 119 mW/m.K at a mean temperature of 200 degrees Celsius was hand-dipped in the emulsion and then dried at a temperature less than 200 degrees Celsius for several hours. The dried mat was found to have a thermal conductivity of 73 mW/m.K at a mean temperature of 200 degrees Celsius. This value represents an improvement (reduction) over the thermal conductivity of the glass fibre mat alone of some 39 percent. The dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
Example 3
300 g of the dry mixture described above was formulated with 3 litres of water, to which were added 15 g Ludox HS40 binder (that is, 6 g colloidal silica in water) and 0.9 g Duramax D-3005 dispersion agent and the constituents were mixed together. The resulting emulsion contained substantially 10 percent by weight solids.
A mat of glass fibre material as described above in Example 2 was hand-dipped in the emulsion and then dried as described above in Example 2. The dried mat was found to have a thermal conductivity of 75 mW/m.K at a mean temperature of 200 degrees Celsius. This value represents an improvement (reduction) over the thermal conductivity of the glass fibre mat alone of some 37 percent. The dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
Example 4 15O g of the dry mixture described above was formulated with 3 litres of water, to which were added 7.5 g Ludox HS40 binder (that is, 3 g colloidal silica in water) and 0.45 g Duramax D-3005 dispersion agent and the constituents were mixed together. The resulting emulsion contained substantially 5 percent by weight solids.
A mat of glass fibre material as described above in Example 2 was hand-dipped in the emulsion and then dried as described above in Example 2. The dried mat was found to have a thermal conductivity of 77 mW/m.K at a mean temperature of 200 degrees Celsius. This value represents an improvement (reduction) over the thermal conductivity of the glass fibre mat alone of some 35 percent. The dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
Example 5
An emulsion was prepared having a 15 percent by weight solids content as explained above in Example 3 and was injected into a glass fibre mat of material as described above in Example 2 and which had previously been formed from two separate layers joined together by a needling procedure using a machine available from Larocha SA, France, and described, for example, in US-A-5475 904. The resulting mat was dried as explained above and was found to have a thermal conductivity of 79 mW/m.K at a mean temperature of 200 degrees Celsius. This value represents an improvement (reduction) over the thermal conductivity of the glass fibre mat alone of some 34 percent. The dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
Example 6
A dry fibre-free mixture was produced consisting of 80 percent by weight of microporous material in the form of pyrogenic (fumed) silica in the form of Aerosil 200 available from Degussa AG, Germany and 20 percent by weight of an opacifier in the form of rutile (titanium dioxide) having a particle size less that 9 μm available from Eggerding, Netherlands.
450 g of the dry mixture described above was formulated with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together. The resulting emulsion contained substantially 15 percent by weight solids.
A mat of glass fibre material as described above in Example 2 was hand-dipped in the emulsion and then dried as described above in Example 2. The dried mat was found to have a thermal conductivity of 52 mW/m.K at a mean temperature of 200 degrees Celsius, representing an improvement (reduction) of about 56 percent compared with the original mat. The dried mat remained flexible and was suitable for use in applications up to about 600 degrees Celsius.
The use of the emulsion of Example 6 is not ideal. The proportion of fumed silica is high and the resulting product is corresponding expensive to produce. Moreover, the emulsion has relatively high viscosity and is not ideal for dipping a mat of glass fibre material. When the emulsion was injected between two layers of glass fibre mat and subjected to the needling procedure of Example 5 the emulsion did not infiltrate the mat and the resulting product was unacceptable.
Example 7
A dry fibre-free mixture was produced consisting of 20 percent by weight of microporous material in the form of pyrogenic (fumed) silica in the form of Aerosil 200 available from Degussa AG, Germany and 80 percent by weight of an opacifier in the form of rutile (titanium dioxide) having a particle size less that 9 μm available from Eggerding, Netherlands. 450 g of the dry mixture described above was formulated with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together. The resulting emulsion contained substantially 15 percent by weight solids.
A mat of glass fibre material as described above in Example 2 was hand-dipped in the emulsion, which was less viscous than the emulsion of Example 6, and then dried as described above in Example 2. The dried mat was found to have a thermal conductivity of 49 mW/m.K at a mean temperature of 200 degrees
Celsius, representing an improvement (reduction) of almost 60 percent compared with the original mat.
The dipped mat remained flexible after drying and was found to be suitable for applications up to about 600 degrees Celsius.
Example 8
450 g of rutile opacifier as described above in Example 7 was formulated into an emulsion with 3 litres of water, to which were added 22.5 g Ludox HS40 binder
(that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together. The resulting emulsion contained substantially 15 percent by weight solids.
The emulsion was found to be unsuitable for dipping because the materials tended to make a sluggish dip. Example 9
450 g of pyrogenic silica as described above in Example 7 was formulated into an emulsion with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together. The resulting emulsion contained substantially 15 percent by weight solids.
The emulsion was found to be too viscous for dipping and no trials were conducted.
Example 10
A dry fibre-free mixture was produced consisting of 60 percent by weight of microporous material in the form of pyrogenic (fumed) silica in the form of Aerosil
200 available from Degussa AG, Germany and 40 percent by weight of an opacifier in the form of rutile (titanium dioxide) having a particle size less that 9 μm available from Eggerding, Netherlands.
450 g of the dry mixture described above was formulated with 3 litres of water, to which were added 22.5 g Ludox HS40 binder (that is, 9 g colloidal silica in water) and 1.35 g Duramax D-3005 dispersion agent and the constituents were mixed together. The resulting emulsion contained substantially 15 percent by weight solids.
A non-woven mat of silica fibre material, available from belChem, Germany, having a weight of 480 g/m2, a thickness of 6 mm and an initial thermal conductivity of 110 mW/m.K at a mean temperature of 200 degrees Celsius was hand-dipped in the emulsion, which was less viscous than the emulsion of Example 6, and then dried as described above in Example 2. The dried mat was found to have a thermal conductivity of 75 mW/m.K at a mean temperature of 200 degrees Celsius, representing an improvement (reduction) of about 32 percent compared with the original mat.
The dipped mat remained flexible after drying and was found to be suitable for applications up to about 1000 degrees Celsius.
As an alternative to impregnation into a mat of fibrous material, the liquid formulation can be used as a coating, for example being applied by spraying or brushing, in a gel or paste form, or can be employed in injection moulding or extrusion.
Thus, the present invention provides a liquid formulation of microporous material which can be used for a number of different purposes. When used to impregnate a mat, it produces a microporous thermal insulation material which is flexible and can be supplied as a roll of material which can be cut to size and positioned around irregular shapes. The liquid formulation, or emulsion, of microporous material is fibre-free, the reinforcing effect normally provided by fibres incorporated into the microporous material being provided by the fibrous mat.
It has been found that the pyrogenic silica can be replaced totally or partially by other microporous materials. These include other pyrogenic metal oxides and other forms of silica, such as precipitated and volatilised silicas. Suitable precipitated silicas include some of those from the Sipernat range available from Degussa in Germany, while a suitable volatilised silica is RW-Fuller silica available from RW Silicium, Germany.
The rutile opacifier can be replaced by other opacifiers such as silicon carbide, zircon (zirconium silicate), ilmenite and other carbide, silicate or oxide type opacifiers. Alternative binders can be employed. These include both inorganic and organic binders.
Suitable inorganic binders include colloidal silica, silicate (such as potassium silicate type K66 available from lneos Silicas in the United Kingdom), phosphate, alumina and cement binders.
Suitable organic binders include silicone, polyacrylic (such as Duramax B 1000 available from Rohm & Haas, France), polyvinylalcohol (such as Optapix AC 112 available from Zschimmer & Schwarz, Germany), polyoxyethylene, polyelectrolyte and polysaccharide (cellulose/starch) binders.
Alternative dispersing agents include KV5068 and KV5166 available from Zschimmer & Schwarz, Germany, which are both alkali-free deflocculating agents, and Dispex A40 available from Ciba Speciality Chemicals, Switzerland, which is an acrylic dispersing agent widely used for dispersing inorganic minerals.

Claims

1. A liquid formulation of a microporous thermal insulation material comprising an emulsion including:
an opacifier;
a microporous thermal insulating material in a proportion ranging from 10 to 90 percent by weight of the combination of opacifier and microporous thermal insulating material;
water;
a binder; and
a dispersion agent.
2. A formulation as claimed in claim 1 , characterised in that the proportion of microporous material in the combination of opacifier and microporous material (the dry mixture) is from 20 to 80 percent by weight.
3. A formulation as claimed in claim 2, characterised in that the proportion of microporous material is from 20 to 60 percent by weight.
4. Aformulation as claimed in any preceding claim, characterised in thatthe emulsion has a solids content in the range from substantially 5 to substantially 15 percent by weight.
5. " A formulation as claimed in any preceding claim, characterised in that the binder is incorporated into the emulsion in an amount from 1 to 10 percent by weight of the combination of opacifier and microporous material (the dry mixture).
6. A formulation as claimed in claim 5, characterised in that the binder is incorporated into the emulsion in an amount of substantially 5 percent by weight.
7. A formulation as claimed in any preceding claim, characterised in that the dispersion agent is incorporated into the emulsion in an amount from 0.1 to 0.5 percent by weight of the combination of opacifier and microporous material (the dry mixture).
8. A formulation as claimed in claim 7, characterised in that the dispersion agent is incorporated into the emulsion in an amount of substantially 0.3 percent by weight.
9. A formulation as claimed in any preceding claim, characterised in that the microporous material is selected from pyrogenic metal oxides, precipitated silica and volatilised silica.
10. A formulation as claimed in claim 9, characterised in that the microporous material is selected from pyrogenic metal oxides of silicon, aluminium and/or titanium.
11. A formulation as claimed in any preceding claim, characterised in that the opacifier is selected from: an oxide; a carbide; a silicate; and ilmenite.
12. A formulation as claimed in claim 11 , characterised in that the opacifier comprises titanium dioxide.
13. A formulation as claimed in claim 12, characterised in that the titanium dioxide is in the form of rutile.
14. A formulation as claimed in claim 11 , characterised in that the opacifier comprises silicon carbide.
15. A formulation as claimed in claim 11 , characterised in that the opacifier comprises zircon (zirconium silicate).
16. A formulation as claimed in any preceding claim, characterised in that the binder comprises an inorganic binder.
17. A formulation as claimed in claim 16, characterised in that the inorganic binder is selected from colloidal silicas; silicates; phosphates; aluminas; and cements.
18. A formulation as claimed in claim 17, characterised in that the inorganic binder comprises potassium silicate.
19. A formulation as claimed in any one of claims 1 to 15, characterised in that the binder comprises an organic binder.
20. A formulation as claimed in claim 19, characterised in that the organic binder is selected from silicones; polyacrylics; polyvinylalcohols; polyoxyethylenes; polyelectrolytes; and polysaccharides.
21. A formulation as claimed in any preceding claim, characterised in that the dispersion agent is selected from alkali-free deflocculating agents, and (poly)acrylics.
22. A method of manufacturing a liquid microporous material comprising the steps of:
preparing a dry, fibre-free mixture of a microporous thermal insulating material and an opacifier in a proportion ranging from 10 to 90 percent by weight microporous material; and mixing together the dry mixture with water, a binder and a dispersion agent to form an emulsion.
23. A method according to claim 22, characterised in that the proportion of microporous material in the combination of opacifier and microporous material
(the dry mixture) is from 20 to 80 percent by weight.
24. A method according to claim 23, characterised in that the proportion of microporous material is from 20 to 60 percent by weight.
25. A method according to any one of claims 22 to 24, characterised in that the emulsion has a solids content in the range from substantially 5 to substantially 15 percent by weight.
26. A method according to any one of claims 22 to 25, characterised in that the binder is incorporated into the emulsion in an amount from 1 to 10 percent by weight of the combination of opacifier and microporous material (the dry mixture).
27. A method according to claim 26, characterised in that the binder is incorporated into the emulsion in an amount of substantially 5 percent by weight.
28. A method according to any one of claims 22 to 27, characterised in that the dispersion agent is incorporated into the emulsion in an amount from 0.1 to 0.5 percent by weight of the combination of opacifier and microporous material
(the dry mixture).
29. . A method according to claim 28, characterised in that the dispersion agent is incorporated into the emulsion in an amount of substantially 0.3 percent by weight.
30. A method according to any one of claims 22 to 29, characterised in that the microporous material is selected from pyrogenic metal oxides, precipitated silica and volatilised silica.
31. A method according to claim 30, characterised in that the microporous material is selected from pyrogenic metal oxides of silicon, aluminium and/or titanium.
32. A method according to any one of claims 22 to 31 , characterised in that the opacifier is selected from: an oxide; a carbide; a silicate; and ilmenite.
33. A method according to claim 32, characterised in that the opacifier comprises titanium dioxide.
34. A method according to claim 33, characterised in that the titanium dioxide is in the form of rutile.
35. A method according to claim 32, characterised in that the opacifier comprises silicon carbide.
36. A method according to claim 32, characterised in that the opacifier comprises zircon (zirconium silicate).
37. A method according to any one of claims 22 to 36, characterised in that the binder comprises an inorganic binder.
38. A method according to claim 37, characterised in that the inorganic binder is selected from colloidal silicas; silicates; phosphates; aluminas; and cements.
39. A method according to claim 38, characterised in that the inorganic binder comprises potassium silicate.
40. A method according to any one of claims 22 to 36, characterised in that the binder comprises an organic binder.
41. A method according to claim 40, characterised in that the organic binder is selected from silicones; polyacrylics; polyvinylalcohols; polyoxyethylenes; polyelectrolytes; and polysaccharides.
42. A method according to any one of claims 22 to 41 , characterised in that the dispersion agent is selected from alkali-free deflocculating agents, and (poly)acrylics.
43. A method of manufacturing a microporous thermal insulation material comprising the steps of:
impregnating a fibrous mat with the emulsion as claimed in any one of claims 1 to 21 ; and
drying the impregnated mat.
44. A method according to claim 43, characterised in that the impregnated mat is dried at a temperature less than 200 degrees Celsius for several hours.
45. A method according to claim 43 or 44, characterised in that the fibrous mat is impregnated with the emulsion by dipping the mat in the emulsion.
46. A method according to claim 43 or 44, characterised in that the emulsion is injected into the fibrous mat.
47. A method according to claim 46, characterised in that the fibrous mat comprises two layers which have been joined by a needling operation prior to injection of the emulsion.
PCT/GB2009/000084 2008-01-25 2009-01-14 Liquid formulation of microporous thermal insulation material, method of manufacture, and use thereof WO2009093002A2 (en)

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