US20070181845A1 - Thermal and/or acoustic insulation materials shaped from silica (as amended) - Google Patents
Thermal and/or acoustic insulation materials shaped from silica (as amended) Download PDFInfo
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- US20070181845A1 US20070181845A1 US10/562,908 US56290804A US2007181845A1 US 20070181845 A1 US20070181845 A1 US 20070181845A1 US 56290804 A US56290804 A US 56290804A US 2007181845 A1 US2007181845 A1 US 2007181845A1
- Authority
- US
- United States
- Prior art keywords
- insulation material
- thermal
- silica
- fibers
- pore volume
- 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.)
- Abandoned
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 55
- 239000012774 insulation material Substances 0.000 title claims abstract description 32
- 239000011148 porous material Substances 0.000 claims abstract description 56
- 239000006185 dispersion Substances 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 239000012065 filter cake Substances 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims description 71
- 238000000034 method Methods 0.000 claims description 52
- 238000009413 insulation Methods 0.000 claims description 31
- 239000007787 solid Substances 0.000 claims description 17
- 239000000835 fiber Substances 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000470 constituent Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000004888 barrier function Effects 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- 230000005855 radiation Effects 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 3
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 claims description 3
- 229920005594 polymer fiber Polymers 0.000 claims description 3
- 230000000750 progressive effect Effects 0.000 claims description 3
- 239000012783 reinforcing fiber Substances 0.000 claims description 3
- 229910052580 B4C Inorganic materials 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229920003043 Cellulose fiber Polymers 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011490 mineral wool Substances 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 229910003468 tantalcarbide Inorganic materials 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 239000003063 flame retardant Substances 0.000 claims 2
- 239000000203 mixture Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 14
- 239000002245 particle Substances 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000005259 measurement Methods 0.000 description 7
- 239000000725 suspension Substances 0.000 description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 6
- 229910052753 mercury Inorganic materials 0.000 description 6
- 238000010981 drying operation Methods 0.000 description 5
- 238000002459 porosimetry Methods 0.000 description 5
- 238000011085 pressure filtration Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- 239000012066 reaction slurry Substances 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000006082 mold release agent Substances 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- -1 polyoxyethylene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
-
- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
- E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
- E04B1/62—Insulation or other protection; Elements or use of specified material therefor
- E04B1/74—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
Definitions
- the present invention relates to porous materials based on dried silica, generally in the form of panels, which are particularly suitable as thermal and/or acoustic insulation materials.
- the invention also relates to a method of obtaining these insulation materials.
- these panels exhibiting a thermal-insulation and/or soundproofing effect are materials based on a porous agglomerate of finely divided particles, essentially containing particles having a low thermal conductivity, such as, for example carbon black, calcium sulfate, calcium carbonate, pyrogenic silica and/or precipitated silica particles in powder form.
- reinforcing fillers such as fibrous materials
- thermally insulating panels are for the thermal insulation of enclosures heated to high temperature, such as industrial thermal enclosures (furnaces or ovens for example) or thermal enclosures of the household type (such as pyrolitic ovens in particular).
- enclosures heated to high temperature such as industrial thermal enclosures (furnaces or ovens for example) or thermal enclosures of the household type (such as pyrolitic ovens in particular).
- thermal insulation panels within this context is the manufacture of fire doors or site walls intended in particular for limiting the propagation of the onset of fires or for bringing fires under control.
- the material is in general subjected to temperatures that can vary widely, such as for example to temperature cycles in which the temperature rises and falls within a furnace or oven.
- temperatures that can vary widely, such as for example to temperature cycles in which the temperature rises and falls within a furnace or oven.
- These thermal variations have a tendency to induce expansion and contraction phenomena within the material, which may be unacceptable in certain applications and also usually result in high mechanical stresses liable to weaken the structure of the material over the relatively long term.
- incorporating reinforcing fillers limits these phenomena, but this does not always prove to be sufficient for inhibiting them and for ensuring satisfactory mechanical integrity of the material.
- opacifying agents such as for example titanium dioxide particles. These opacifying agents reflect, absorb and/or disperse at least part of the infrared radiation and thus consolidate the thermal barrier effect of the material. Even so, it turns out that the mere presence of these opacifying agents does not always make it possible to obtain optimum thermal insulation properties.
- a conventional method for preparing the aforementioned thermal and/or acoustic insulation panels consists in carrying out a dry compacting operation of their constituents, namely by applying pressure to the particles of low thermal conductivity, generally in combination with reinforcing fillers, and optionally opacifying agents.
- This method is in general carried out by introducing these constituents in the form of a blend of finely divided particles and/or powders in a porous envelope, for example a bag or a cushion made of glass fabric and then applying a high pressure (typically of about 10 bar or more) to said envelope, in order to bond the particles together, so as to obtain a compressed material having a certain mechanical integrity.
- the panels obtained according to this dry compacting method usually have insufficient physical and/or mechanical properties.
- the thermal and acoustic insulation properties of the materials often prove to be bad, in particular when the low thermal conductivity particles involved in their structure are carbon black, calcium sulfate or calcium carbonate particles.
- More acceptable insulation properties may be obtained by using silica particles.
- materials having insufficient mechanical properties are obtained, said materials being in particular friable and inclined to cracking.
- Patent EP 0 594 469 describes a method of preparing insulating panels based on dried silica, which consists in drying an aqueous composition obtained by blending a pulverized cake of precipitated silica to which at least one reinforcing filler, and optionally an opacifying agent, have been added.
- the materials obtained according to the method of EP 0 594 469 exhibit satisfactory mechanical integrity, combined with thermal and acoustic properties at least similar to those of the materials obtained by dry compacting, and usually superior to them. In this regard, it seems reasonable to suppose that the operation of drying an aqueous slurry instead of a dry compacting operation makes it especially possible to increase the pore volume of the material obtained in fine.
- the method of EP 0 594 469 also proves to be economically more advantageous than dry compacting, especially insofar as it obviates the expensive and burdensome phases of blending powders and compacting them at high pressure.
- the aqueous composition which undergoes the drying operation is in general a slurry with a solids content of at least 10%, which is fluidized (disintegrated) before being introduced into a mold, and then dried.
- the inventors have discovered that it is possible to further improve the properties of the insulation materials which are obtained by drying aqueous compositions based on precipitated silica particles, by carrying out the drying operation on a precompacted aqueous composition, e.g. a cake obtained by filtering a precipitated silica dispersion in a filter press.
- a precompacted aqueous composition e.g. a cake obtained by filtering a precipitated silica dispersion in a filter press.
- the inventors have surprisingly discovered that it is possible to improve the method of EP 0 594 469, especially by avoiding one of the steps of this method, thereby making it possible to produce more advantageous materials by means of a less expensive method.
- the use of a mold is no longer necessary for the drying step insofar as the compacted cake is already formed in the filter press. This further reduces the production costs of the material.
- the materials obtained by the inventors are moreover particularly suitable for use in a vacuum, in which they especially exhibit good mechanical integrity and useful thermal insulation properties.
- the present invention aims to provide a method of preparing insulating materials of the dried-silica panel type having mechanical integrity and thermal and/or acoustic insulation properties at least similar, and preferably superior, to those of currently known silica panels, and to attend this aim with a lower production cost than with the methods of the prior art.
- An object of the invention is further to provide novel materials based on dried silica that are suitable for thermal and/or acoustic insulation, and preferably suitable for thermal insulation at high temperature.
- the aim of the invention is in particular to provide such materials in the form of dried-silica panels having in particular sufficient mechanical integrity to allow them to be handled.
- the aim of the invention is also specifically to provide such materials that are suitable for vacuum processing, especially in order to produce vacuum thermal insulation.
- the subject of the present invention is a method of preparing a thermal and/or acoustic insulation material based on dried precipitated silica, comprising the steps consisting in:
- thermo and/or acoustic insulation material is understood to mean, within the context of the present invention, a porous solid having sufficient mechanical strength for it to be able to be handled, and possessing absorption, reflection and/or dispersion properties for thermal radiation and/or acoustic waves.
- the thermal and/or acoustic insulation material prepared according to the invention takes the form of a particulate panel, preferably of rectangular or square shape.
- the drying of step (B) consists in substantially removing the water contained in the compacted cake obtained from step (A), optionally after demolding the compacted cake obtained in the filter press.
- step (B) generally results essentially in the formation of a one-piece solid, the shape of which is determined by the filter press used in step (A), which acts as a mold for the compacted cake produced.
- step (A) when it is desired to obtain an insulation panel of given shape, it is usually advantageous to carry out step (A) within a filter press having said shape, for example in a filter press having a rectangular or square shape.
- the compacted cake obtained in step (A) may, in certain cases, be demolded from the filter press and then cut up into the desired shape, prior to the drying of step (B).
- the cutting-up operation should in particular be carried out with the least possible vibration.
- step (A) whose purpose is to form a compacted filter cake.
- the work carried out by the inventors seems to indicate that, the greater the compacting of the cake produced in step (A), the greater the reduction observed in the size of the pores present in the material obtained after the drying of step (B), thereby improving the insulation properties.
- excessive compacting results, on the contrary, in a material having a low pore volume, which is prejudicial to the insulation properties. Therefore, in the general case, it is necessary to carry out the compacting of the cake from step (A) under moderate pressure.
- the filtration in the filter press of step (A) preferably includes a compacting operation with a pressure of between 2 and 10 bar (that is to say between 2 ⁇ 10 5 Pa and 10 ⁇ 10 5 Pa).
- the pressure employed is 3 bar or higher, and more preferably 4 bar or higher.
- this pressure in particular to minimize the reduction in pore volume of the material obtained in fine, it often proves advantageous for this pressure to be 8 bar or less, preferably 7 bar or less, and more preferably less than 6 bar.
- the pressure at which the compacting of step (A) is carried out is thus between 2 and 7 bar and preferably between 4.5 and 5.5 bar (typically around 5 bar).
- the compacted filter cake obtained after step (A) has a solids content of at least 10% by weight and preferably at least 15% by weight, this content generally remaining less than 35% by weight. Usually, it is preferred for this solids content to be between 20 and 30% (typically around 25%).
- the pressure filtration of step (A) is generally carried out for a time of at least 10 minutes, typically between 10 and 40 minutes, and preferably for at least 20 minutes, especially so as to establish the optimum porosity within the material.
- step (A) comprises two successive steps, namely:
- this step is in general carried out at room temperature (typically at a temperature between 10 and 30° C.) However, according to certain methods of implementation, higher temperatures may be envisaged, (especially temperatures between 30 and 80° C.), for example in order to increase the filtration rate.
- the aqueous precipitated-silica-based dispersion D subjected to the filtration of step (A) in a filter press may in general be any dispersion based on precipitated silica particles.
- the term “precipitated silica” denotes, within the context of the present description, any silica obtained by the reaction of a silicate with an acid, according to any method of preparation, especially by the addition of an acid to a silicate stock, or else by simultaneous, total or partial, addition of acid and silicate to a water or silicate stock.
- the suspension D is a silica slurry such as that obtained after such reactions, to which various additives may optionally be added.
- the precipitated silica present in the aqueous dispersion D is a precipitated silica which, once dried, has a BET specific surface area of between 80 and 400 m 2 /g, and preferably between 100 and 350 m 2 /g and a CETAB specific surface area of between 80 and 350 m 2 /g, and preferably between 100 and 250 m 2 /g.
- precipitated silicas that are particularly suitable for implementing the method of the invention, mention may particularly be made of the precipitated silicas obtained by the methods described for example in EP 0 520 862, WO 95/09127, WO 95/09128, or WO 03/016215.
- the initial solids content of the suspension D that is subjected to the pressure filtration of step (A) may vary quite widely. However, it is preferable for this initial solids content before filtration to be between 5 and 30%, and preferably between 15 and 25% by weight.
- the precipitated silica in the aqueous dispersion D is the predominant solid compound. Thus, it is preferable for the precipitated silica in the dispersion D to be present in an amount of at least 50% by weight, preferably at least 75% by weight relative to the total mass of solids of the dispersion D.
- the aqueous dispersion D used in step (A) contains, in addition to the precipitated silica, a reinforcing filler.
- this filler is intended to increase the mechanical integrity of the insulation panel obtained by the method.
- this reinforcing filler preferably contains reinforcing fibers chosen from the group formed by aluminum silicate fibers, alumina fibers, mineral wool fibers, glass fibers, quartz fibers, ceramic fibers, polymer fibers and cellulose fibers, said reinforcing fibers preferably being glass fibers or polymer fibers, such as polyamide fibers.
- the (silica/reinforcing filler) mass ratio in the aqueous dispersion D of step (A) is between 75/25 and 99/1, and preferably between 85/15 and 98/2.
- the aqueous dispersion D used in step (A) may contain, in addition to precipitated silica and an optional reinforcing filler, an opacifying agent, namely a compound capable of reflecting absorbing and/or dispersing at least part of the infrared radiation.
- an opacifying agent acting as an infrared barrier is advantageously chosen from the group consisting of chromium oxide, zirconium oxide, iron oxide, titanium dioxide, manganese dioxide, ilmenite, quartz powder, silicon carbide, boron carbide, tantalum carbide, carbon black and graphite, in general in particulate form.
- the titanium dioxide and ore particles that it comprises, in particular the ilmenite particles, constitute particularly suitable opacifying agents within the context of the present invention.
- the (silica/opacifying agent) mass ratio within the aqueous dispersion D is between 50/50 and 99/1, and preferably between 70/30 and 90/10.
- step (A) consists in carrying out a pressure filtration operation on this dispersion, so as to obtain a compacted cake whose solid phase has substantially the same composition as the solid phase of the suspension D.
- step (A) may prove beneficial for step (A) to include one or more washing operations (using water or solvents).
- the washing operation(s) must however be carried out taking care not to obtain a pulverized cake after step (A).
- step (B) of the method of the invention must be carried out on a filter cake in the compacted state.
- washing steps it is in general preferable that they be carried out in the filter press, and advantageously under pressure, so as to obtain a properly compacted cake prior to drying.
- the drying step (B) of the method of the present invention generally consists in substantially removing the water present in the compacted cake obtained from step (A), in general so as to obtain a water content in the material of 15% or less, and typically between 1 and 10% by weight. In general, this drying is carried out slowly, especially so as to optimize the cohesion of the various particles and to avoid the formation of cracks, which would be liable to affect the insulating properties of the material, or even its mechanical strength.
- step (B) may be carried out by leaving the compacted cake obtained after step (A) in the filter press used for the filtration.
- the compacted cake obtained after step (A) is in general sufficiently compacted for it to be possible to demold it from the filter press without appreciably affecting its compacted character.
- step (B) When it is desired to demold the compacted cake from step (A) prior to the drying of step (B), it is in general advantageous to coat the internal surface of the filter press with a mold-release agent such as, for example, an organic oil or a silicone oil, prior to the pressure filtration of step (A).
- a mold-release agent such as, for example, an organic oil or a silicone oil
- step (B) of the method of the invention is carried out by leaving the compacted filter cake obtained after step (A) to dry at room temperature, namely at a temperature between 10 and 30° C., preferably between 15 and 25° C.
- room temperature namely at a temperature between 10 and 30° C., preferably between 15 and 25° C.
- the evaporation time may vary widely according to this first embodiment. However, usually a drying operation lasts around 10 to 20 days, or even a shorter time.
- step (B) is carried out by subjecting the compacted filter cake as obtained after step (A) to a progressive temperature rise, generally from room temperature (typically 20° C.) up to a temperature of at least 100° C., or even up to a temperature of at least 200° C., with the slowest possible rate of temperature rise, preferably less than 2° per minute, and typically not exceeding 0.5° C. per minute.
- a progressive temperature rise it proves to be advantageous to hold the temperature at one, two or three intermediate temperature levels.
- step (B) may be carried out under the drying conditions described in Patent EP 0 594 469.
- the subject of the present invention is porous thermal and/or acoustic insulation materials based on dried precipitated silica, which can be obtained by the method described above. These materials usually take the form of panels, generally of rectangular or square shape.
- the materials according to the present invention have a porous structure with a small pore size.
- the “pore size” referred to here is the pore size as determined using the mercury porosimetry method, for example by means of a porosimeter of the Micromeritics Autopore III 9420 type.
- the porous specimens tested are prepared as follows: the specimen is dried for two hours in an oven at 200° C.
- the pore diameters are calculated by the Washburn equation with a contact angle ⁇ of 140° and a surface tension ⁇ of 484 N/m (or dynes/cm).
- the pore volume of the pores smaller in size than 1000 nm represents at least 40%, and usually at least 50%, of the total pore volume of the material.
- the pore volume of the pores smaller in size than 1000 nm represents at least 60%, or even at least 70%, of the total pore volume.
- the pores smaller in size than 100 nm are predominant.
- mercury porosimetry shows that the pore volume of the pores smaller in size than 100 nm represents at least 50%, in general at least 60%, and advantageously at least 70% of the pore volume of pores smaller in size than 1000 nm.
- this proportion of pores smaller in size than 100 nm is higher the greater the pressure at which the filtration of step (A) is carried out.
- a material according to the present invention generally possesses a relatively high total pore volume.
- the term “pore volume” is understood here to mean the volume of the accessible pores of the material, as determined by the aforementioned mercury porosimetry method. This total pore volume is generally between 1 and 5 cm 3 /g (between 1 and 5 ml/g), and usually between 1.2 and 4 cm 3 /g, this total pore volume preferably being greater than 1.5 cm 3 /g, advantageously at least 2 cm 3 /g and even at least 2.5 cm 3 /g.
- the pore volume of the pores smaller in size than 100 nm is itself at least 1 cm 3 /g, usually at least 1.1 cm 3 /g and preferably at least 1 cm 3 /g.
- Materials having large pore volumes are in general obtained when the pressure at which the filtration of step (A) is carried out is relatively low, typically when this pressure is around 5 bar or less (for example between 2 and 5.5 bar).
- step (A) it is usually necessary to carry out step (A) at a high pressure, advantageously at least equal to 3 bar, preferably 4 bar, especially so as to obtain the highest possible mechanical strength of the material.
- an insulation material according to the invention generally has a composition extremely similar, and usually identical, to that of the solid phase of the aqueous dispersion D.
- a material according to the invention consists predominantly of dried precipitated silica, that is to say with a content of at least 50% by weight, preferably at least 75% by weight and advantageously at least 80% by weight relative to the total weight of the material.
- a material according to the invention may also include other elements than dried silica, and in particular additives such as a reinforcing filler and/or an opacifying agent.
- a material according to the invention is a material obtained from a dispersion D comprising, in addition to precipitated silica, a reinforcing filler.
- a material comprises:
- a material according to this embodiment is particularly suitable as a thermal and acoustic insulation material for walls or ceilings of buildings or dwellings. Its thermal insulation properties also make it suitable as a fire-stop material.
- a material according to the invention is a material obtained from a dispersion D comprising, in addition to precipitated silica, an opacifying agent, and optionally a reinforcing filler.
- such a material comprises:
- a material according to this specific embodiment is particularly intended for producing a high-temperature thermal insulation, in particular for the insulation of enclosures heated to high temperatures, or as constituent materials of fire-stop barriers. These materials are also suitable for the more usual uses of thermal and acoustic insulation, such as the insulation of walls and ceilings.
- the materials obtained according to the method of the invention prove to be useful as thermal and/or acoustic insulation material, and in particular for thermal insulation under reduced pressure.
- a silica cake was produced according to the method described in example 1 of EP 520 862.
- the cake as obtained after the filtration step in a filter press, which had a solids content of 21%, was diluted with water so as to obtain a silica suspension or slurry having a solids content of 13.5% by weight, and the pH of this silica suspension was increased to 5 by the addition of sulfuric acid (80 g/l aqueous solution).
- the mixture obtained was then filtered in the filter press used in Example 1 above (filter press with an inside diameter of 7 cm). A compacting pressure of 5 bar was applied, after which a compacted cake having a solids content of 27% by weight was obtained. The formed cake thus obtained was demolded and left to dry at room temperature as in the previous example. After 10 days, a dried cake with a solids content of 95% was obtained. Thus, a silica panel having a good mechanical strength and a density of 0.4 was obtained.
- the silica panel obtained had a total pore volume of 3.3 ml/g, with a pore volume of pores smaller in size than 100 nm of 1.2 ml/g.
- Thermal conductivity measurements were carried out using a TC-meter on the two silica panels of Examples 1 and 2.
- the principle used was that called the “thermal shock probe”, which is similar to the method used according to the ISO 8814-1 standard.
- thermal conductivity coefficient of the silica panels of Examples 1 and 2 was measured at various pressures in the following manner: a thermal probe was placed within the material to be characterized.
- the thermal equilibrium of the material was disturbed by generating a heat flux by means of the heating element of the probe.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Architecture (AREA)
- Physics & Mathematics (AREA)
- Civil Engineering (AREA)
- Acoustics & Sound (AREA)
- Electromagnetism (AREA)
- Silicon Compounds (AREA)
- Building Environments (AREA)
- Filtering Materials (AREA)
- Laminated Bodies (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US14/834,044 US9903109B2 (en) | 2003-06-30 | 2015-08-24 | Thermal and/or acoustic insulation materials shaped from silica |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0307903A FR2856680B1 (fr) | 2003-06-30 | 2003-06-30 | Materiaux d'isolation thermique et/ou acoustique a base de silice et procedes pour leur obtention |
FR0307903 | 2003-06-30 | ||
PCT/FR2004/001669 WO2005003057A2 (fr) | 2003-06-30 | 2004-06-29 | Materiaux d'isolation thermique et/ou acoustique a base de silice et procedes pour leur obtention |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FR2004/001669 A-371-Of-International WO2005003057A2 (fr) | 2003-06-30 | 2004-06-29 | Materiaux d'isolation thermique et/ou acoustique a base de silice et procedes pour leur obtention |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US14/834,044 Continuation US9903109B2 (en) | 2003-06-30 | 2015-08-24 | Thermal and/or acoustic insulation materials shaped from silica |
Publications (1)
Publication Number | Publication Date |
---|---|
US20070181845A1 true US20070181845A1 (en) | 2007-08-09 |
Family
ID=33515528
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US10/562,908 Abandoned US20070181845A1 (en) | 2003-06-30 | 2004-06-29 | Thermal and/or acoustic insulation materials shaped from silica (as amended) |
US14/834,044 Expired - Fee Related US9903109B2 (en) | 2003-06-30 | 2015-08-24 | Thermal and/or acoustic insulation materials shaped from silica |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US14/834,044 Expired - Fee Related US9903109B2 (en) | 2003-06-30 | 2015-08-24 | Thermal and/or acoustic insulation materials shaped from silica |
Country Status (8)
Country | Link |
---|---|
US (2) | US20070181845A1 (fr) |
EP (1) | EP1641726B1 (fr) |
JP (1) | JP4435160B2 (fr) |
AT (1) | ATE395311T1 (fr) |
DE (1) | DE602004013780D1 (fr) |
ES (1) | ES2307049T3 (fr) |
FR (1) | FR2856680B1 (fr) |
WO (1) | WO2005003057A2 (fr) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110034608A1 (en) * | 2008-04-22 | 2011-02-10 | Lafarge Gypsum International | Finishing compound suitable for an acoustic support |
RU2495853C2 (ru) * | 2009-02-13 | 2013-10-20 | Эвоник Дегусса Гмбх | Теплоизоляционный материал, содержащий осажденный диоксид кремния |
US20140287170A1 (en) * | 2013-03-22 | 2014-09-25 | Applied Materials, Inc. | Reflective liners |
CN108822420A (zh) * | 2018-07-16 | 2018-11-16 | 杨程飞扬 | 一种低密度发泡保温材料的制备方法 |
US11400688B1 (en) * | 2016-02-10 | 2022-08-02 | Consolidated Nuclear Security, LLC | Thermal protection barrier |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5700548B2 (ja) * | 2011-06-03 | 2015-04-15 | 旭化成ケミカルズ株式会社 | 成形体、被包体及び成形体の製造方法 |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3500444A (en) * | 1968-01-16 | 1970-03-10 | Johns Manville | Electrical heating unit with an insulating refractory support |
US3753751A (en) * | 1967-05-17 | 1973-08-21 | Owens Corning Fiberglass Corp | Light weight bodies of cotton fiber reinforced hydrous alkaline earth metal silicate thermal insulation material |
US4495167A (en) * | 1981-11-07 | 1985-01-22 | Degussa Aktiengesellschaft | Precipitated silicas having high structure and process for their preparation |
US4590052A (en) * | 1984-04-06 | 1986-05-20 | Rhone-Poulenc Chimie De Base | Precipitated silica having improved morphological characteristics and process for the production thereof |
US4636415A (en) * | 1985-02-08 | 1987-01-13 | General Electric Company | Precipitated silica insulation |
US4719336A (en) * | 1986-05-30 | 1988-01-12 | General Signal Corporation | Method of making thermal insulating blocks and electrical heating units and the products thereof |
US5403570A (en) * | 1991-06-26 | 1995-04-04 | Rhone-Poulenc Chimie | Dispersible silica particulates |
US6468493B1 (en) * | 1997-05-26 | 2002-10-22 | Rhodia Chimie | Precipitated silica used as reinforcing filler for elastomers |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2695981B1 (fr) | 1992-09-18 | 1994-12-09 | Rhone Poulenc Chimie | Panneau d'isolation thermique et/ou acoustique et ses procédés d'obtention. |
JP2799773B2 (ja) | 1993-09-29 | 1998-09-21 | ローヌ−プーラン シミ | 沈降シリカ |
FR2710630B1 (fr) | 1993-09-29 | 1995-12-29 | Rhone Poulenc Chimie | Nouvelles silices précipitées, leur procédé de préparation et leur utilisation au renforcement des élastomères. |
DE10102893C2 (de) * | 2000-11-13 | 2003-11-27 | Asfil Isolations & Filtermater | Flächiger Hochtemperatur-Isolierkörper sowie Verfahren zur Herstellung eines solchen Isolierkörpers auf Langsiebanlagen |
BR0211703B1 (pt) | 2001-08-13 | 2012-02-22 | processo de preparação de sìlica, sìlica, e, utilização de uma sìlica. |
-
2003
- 2003-06-30 FR FR0307903A patent/FR2856680B1/fr not_active Expired - Fee Related
-
2004
- 2004-06-29 EP EP04767513A patent/EP1641726B1/fr not_active Expired - Lifetime
- 2004-06-29 ES ES04767513T patent/ES2307049T3/es not_active Expired - Lifetime
- 2004-06-29 DE DE602004013780T patent/DE602004013780D1/de not_active Expired - Lifetime
- 2004-06-29 AT AT04767513T patent/ATE395311T1/de not_active IP Right Cessation
- 2004-06-29 WO PCT/FR2004/001669 patent/WO2005003057A2/fr active IP Right Grant
- 2004-06-29 US US10/562,908 patent/US20070181845A1/en not_active Abandoned
- 2004-06-29 JP JP2006516338A patent/JP4435160B2/ja not_active Expired - Fee Related
-
2015
- 2015-08-24 US US14/834,044 patent/US9903109B2/en not_active Expired - Fee Related
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3753751A (en) * | 1967-05-17 | 1973-08-21 | Owens Corning Fiberglass Corp | Light weight bodies of cotton fiber reinforced hydrous alkaline earth metal silicate thermal insulation material |
US3500444A (en) * | 1968-01-16 | 1970-03-10 | Johns Manville | Electrical heating unit with an insulating refractory support |
US4495167A (en) * | 1981-11-07 | 1985-01-22 | Degussa Aktiengesellschaft | Precipitated silicas having high structure and process for their preparation |
US4590052A (en) * | 1984-04-06 | 1986-05-20 | Rhone-Poulenc Chimie De Base | Precipitated silica having improved morphological characteristics and process for the production thereof |
US4636415A (en) * | 1985-02-08 | 1987-01-13 | General Electric Company | Precipitated silica insulation |
US4719336A (en) * | 1986-05-30 | 1988-01-12 | General Signal Corporation | Method of making thermal insulating blocks and electrical heating units and the products thereof |
US5403570A (en) * | 1991-06-26 | 1995-04-04 | Rhone-Poulenc Chimie | Dispersible silica particulates |
US5547502A (en) * | 1991-06-26 | 1996-08-20 | Rhone-Poulenc Chimie | Dispersible silica particulates and reinforcement of elastomer/rubber matrices therewith |
US5587416A (en) * | 1991-06-26 | 1996-12-24 | Rhone-Poulenc Chimie | Dispersible silica particulates and reinforcement of elastomer/rubber matrices therewith |
US6468493B1 (en) * | 1997-05-26 | 2002-10-22 | Rhodia Chimie | Precipitated silica used as reinforcing filler for elastomers |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110034608A1 (en) * | 2008-04-22 | 2011-02-10 | Lafarge Gypsum International | Finishing compound suitable for an acoustic support |
US8227537B2 (en) * | 2008-04-22 | 2012-07-24 | Lafarge Gypsum International | Finishing compound suitable for an acoustic support |
RU2495853C2 (ru) * | 2009-02-13 | 2013-10-20 | Эвоник Дегусса Гмбх | Теплоизоляционный материал, содержащий осажденный диоксид кремния |
US20140287170A1 (en) * | 2013-03-22 | 2014-09-25 | Applied Materials, Inc. | Reflective liners |
US11400688B1 (en) * | 2016-02-10 | 2022-08-02 | Consolidated Nuclear Security, LLC | Thermal protection barrier |
CN108822420A (zh) * | 2018-07-16 | 2018-11-16 | 杨程飞扬 | 一种低密度发泡保温材料的制备方法 |
Also Published As
Publication number | Publication date |
---|---|
WO2005003057A3 (fr) | 2005-09-22 |
DE602004013780D1 (de) | 2008-06-26 |
WO2005003057A2 (fr) | 2005-01-13 |
JP2007527349A (ja) | 2007-09-27 |
US20150361652A1 (en) | 2015-12-17 |
ATE395311T1 (de) | 2008-05-15 |
US9903109B2 (en) | 2018-02-27 |
JP4435160B2 (ja) | 2010-03-17 |
ES2307049T3 (es) | 2008-11-16 |
FR2856680A1 (fr) | 2004-12-31 |
FR2856680B1 (fr) | 2005-09-09 |
EP1641726B1 (fr) | 2008-05-14 |
EP1641726A2 (fr) | 2006-04-05 |
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