WO2014110892A1 - Matériau d'isolation thermique inorganique et son procédé de préparation - Google Patents

Matériau d'isolation thermique inorganique et son procédé de préparation Download PDF

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Publication number
WO2014110892A1
WO2014110892A1 PCT/CN2013/078744 CN2013078744W WO2014110892A1 WO 2014110892 A1 WO2014110892 A1 WO 2014110892A1 CN 2013078744 W CN2013078744 W CN 2013078744W WO 2014110892 A1 WO2014110892 A1 WO 2014110892A1
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thermal insulation
silica aerogel
insulation material
inorganic
preparation
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PCT/CN2013/078744
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Chinese (zh)
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赵峰
唐智勇
徐天宇
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Zhao Feng
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Publication of WO2014110892A1 publication Critical patent/WO2014110892A1/fr

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    • 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
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24—Compositions 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
    • C04B28/26—Silicates of the alkali metals
    • 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
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures

Definitions

  • the invention belongs to the technical field of chemical materials, and in particular relates to an inorganic thermal insulation material and a preparation method thereof.
  • Insulation materials can be divided into organic insulation materials and inorganic insulation materials.
  • Organic insulation materials include expanded polystyrene board (EPS), extruded polystyrene board (XPS), sprayed polyurethane (SPU), and polyphenylene granules.
  • EPS expanded polystyrene board
  • XPS extruded polystyrene board
  • SPU sprayed polyurethane
  • Polyphenylene granules include polyphenylene granules.
  • Organic insulation materials have the advantages of light weight, good processability, high compactness, good thermal insulation effect, etc., but they also have aging resistance, large deformation coefficient, poor stability, poor safety, easy combustion, and environmental protection.
  • the disadvantages are poor performance, difficult construction, high engineering cost, limited resources and difficult to recycle. It is necessary to add some flame retardants to meet the standard of use.
  • Inorganic insulation materials include hollow vitrified beads, expanded perlite, closed-cell perlite, rock wool and the like. Such materials are non-combustible materials and do not present fire safety issues. However, problems such as low strength, poor integrity, high water absorption, and poor freeze-thaw properties are common, and the preparation process is complicated and the production cost is high. Therefore, in order to utilize the excellent fireproof performance of inorganic insulating materials, it is necessary to further explore and research them.
  • the aerogel material is the material with the lowest thermal conductivity in the field of inorganic insulation, and is a product obtained by drying the internal solvent while keeping its gel skeleton unchanged. Aerogel is a structure-controlled nanoporous lightweight material. 99% of the composition is composed of gas. It is the lightest solid material known at present. The lightest silicone aerogel weighs only 3 mg/ Cm 3 .
  • silica aerogel is a new type of nanoporous super insulation material with powder and block shape, and its porosity is as high as 80% ⁇ 99.8%. Because silica aerogel contains nano-scale particles and pore structure (l ⁇ 100 nm), it has a large specific surface area (200 ⁇ 1000 m 2 /g), high porosity, low density (1-500 kg). /m 3 ) and low thermal conductivity (0.012 W/(mk)) have been used as thermal insulation materials, catalysts and carriers, acoustic impedance coupling materials, Cherenkov detectors, etc. However, due to the disadvantages of low inherent strength, brittleness and easy cracking of the silica aerogel material, its practical use is limited.
  • the Chinese patent publication CN1749214 A discloses an aerogel insulation composite material and a preparation method thereof, the aerogel insulation material comprising a silica aerogel, an infrared sunscreen titanium dioxide, Reinforcement material.
  • the reinforcing materials used are quartz fibers, high silica fibers, aluminum silicate fibers, aluminum carbonate fibers, carbon fibers or glass fibers.
  • the method firstly prepares a raw material such as a silicon source into a sol according to a certain ratio, and then infiltrates into a fiber mat or a fiber preform by an infiltration process, and finally obtains a supercritical fluid drying.
  • the composite has good thermal insulation performance and good hydrophobic properties, but the cost of using supercritical technology is high.
  • the technical problem to be solved by the present invention is to provide an inorganic thermal insulating material and a preparation method thereof, and the method for preparing the inorganic thermal insulating material is low in cost.
  • the invention provides an inorganic thermal insulation material which is obtained by modifying the following components by a coupling agent and then infiltrating onto a glass fiber mat to obtain:
  • the soluble silicate is potassium silicate or sodium silicate.
  • the compound of the formula (I) is dodecyltridecyl ammonium chloride.
  • the coupling agent is a silane coupling agent.
  • the invention also provides a preparation method of an inorganic thermal insulation material, comprising the following steps:
  • the silica aerogel is prepared as follows:
  • drying control chemical additive being N, N-dimercaptoamide, N, N-II Mercaptoacetamide, oxime amide or acetamide.
  • the ratio of the mixture to water is 0.8 to 2 kg: 1 L.
  • the infiltration is a pressurized spray infiltration.
  • the ratio of the slurry to the glass fiber mat is 1 L: 0.36 to 1.4 m 2 .
  • the hot pressing pressure is 80 MPa to 300 MPa
  • the hot pressing temperature is 60 ° C to 90 ° C
  • the hot pressing time is 2 to 4 h.
  • the invention provides an inorganic thermal insulation material and a preparation method thereof, the inorganic thermal insulation material comprises 15 ⁇ 60 wt% silica aerogel, 15 ⁇ 60 wt% soluble silicate, 15 ⁇ 40 wt%
  • the compound of (I) structure, 5 ⁇ 15 wt% of antimony tin oxide and 5 ⁇ 15 wt% of hollow glass microbeads are mixed, modified by coupling agent, mixed with water and infiltrated onto glass fiber mat, hot press forming After getting it.
  • the sol is impregnated into the fiber mat or the fiber preform by supercritical fluid drying.
  • the present invention is subjected to hydrophobic treatment by modification, and the nano-porous network structure of the material is due to the action of the coupling agent.
  • the water group is exposed, so that the inorganic thermal insulation material has good water resistance, does not need to be dried by the supercritical fluid, reduces the production cost, and the preparation method is simple;
  • the inorganic nano material and the inorganic fiber are used to make the inorganic thermal insulation material compressive strength , tensile strength and flexural strength are high, and the bond strength with the base layer is also high, the structure is stable; again, the silica aerogel makes the inorganic thermal insulation material have a nano-scale micro-closed-hole network structure, thereby The thermal conductivity of the inorganic thermal insulation material is lowered to improve the thermal insulation performance.
  • FIG. 1 is a 100 nm transmission electron micrograph of a silica aerogel prepared in Example 1 of the present invention
  • FIG. 2 is a 50 nm transmission electron micrograph of a silica aerogel prepared in Example 1 of the present invention
  • 3 is a scanning electron micrograph of a silica aerogel prepared in Example 1 of the present invention
  • FIG. 4 is an X-ray diffraction diagram of a silica aerogel prepared in Example 1 of the present invention; X-ray diffraction pattern of the silica aerogel prepared in Example 1 after treatment at 500 ° C;
  • Figure 6 is a X-ray diffraction pattern of the silica aerogel prepared in Example 1 of the present invention after being treated at 900 °C;
  • Figure 7 is a X-ray diffraction pattern of the silica aerogel prepared in Example 1 of the present invention after being treated at 1100 °C;
  • Figure 8 is a bar graph showing the pore size distribution of the silica aerogel prepared in Example 1 of the present invention and Comparative Example 1.
  • the invention provides a preparation method of an inorganic thermal insulation material, comprising the following steps: A) 15 ⁇ 60 wt% silica aerogel, 15 ⁇ 60 wt% soluble silicate, 15 ⁇ 40 wt% a compound of the formula (I), 5 to 15 wt% of antimony tin oxide and 5 to 15 wt% of hollow glass microbeads are mixed with a coupling agent to obtain a mixture; B) the mixture is mixed with water to obtain The slurry is infiltrated onto the glass fiber mat and hot pressed to obtain an inorganic heat insulating material;
  • l ⁇ n ⁇ 24, preferably 6 ⁇ n ⁇ 18, and X is F, Br or CI, preferably Br or Cl.
  • the silica aerogel may be a silica aerogel well known to those skilled in the art, and is not particularly limited.
  • the surface tension of the solvent can be reduced by the supercritical drying method and the solvent replacement method to obtain a gas condensation.
  • the gel product differs in that the product obtained by the supercritical drying method is a bulk aerogel and the solvent replacement method is a powder aerogel.
  • the silica aerogel described in the present invention is preferably a silica aerogel obtained by drying under normal pressure by a solvent replacement method, which may be commercially available or homemade. There are no restrictions on the source.
  • the silica aerogel of the present invention is preferably prepared according to the following method: a) adjusting the pH of the silica sol to 4 to 10 with a reducing acid, adding ethanol, heating and maintaining the wet gel; b) The wet gel, ethyl orthosilicate and ethanol are mixed and aged to obtain an alcohol gel; C) mixing the alcohol gel with a drying control chemical additive, drying under normal pressure to obtain a silica aerogel, the drying control chemical additive being N, N-dimercaptoamide, N, N-II Mercaptoacetamide, oxime amide or acetamide.
  • the silica sol is a silica sol well known to those skilled in the art, and the source thereof is not limited.
  • the silica sol is alkaline, and its pH is adjusted by adding a reducing acid to obtain a wet gel.
  • the reducing acid is not particularly limited as long as it is a reducing acid well known to those skilled in the art.
  • hydrochloric acid is preferred, and 1 mol/L hydrochloric acid is more preferred. Adjusting the pH of the silica sol to 4 ⁇ 10, preferably 5-8
  • the addition of ethanol is slowly added, and the slow addition speed is such that the silica sol does not condense into a block.
  • the ratio of the addition of ethanol to silica sol has a certain influence on the formation of the wet gel.
  • the volume ratio of the ethanol to the silica sol in the present invention is preferably from 1:2 to 5, more preferably from 1:3 to 4.
  • the ethanol may be an industrial grade alcohol without any particular limitation.
  • the temperature of the heat preservation is 40 ° C to 60 ° C, preferably 45 ° C to 55 ° C.
  • the wet gel is continuously placed in ethanol to be heated and immersed, more preferably soaked for this purpose. The procedure is repeated twice.
  • the volume ratio of the wet gel to ethanol is from 1:2 to 3, preferably from 1 to 2 to 2.5.
  • the heat preservation temperature is 40 ° C to 60 ° C, preferably 45 ° C to 55 ° C, and the heat preservation time is 20 to 30 h, preferably 20 to 25 h.
  • the gel needs to be aged to strengthen its network structure and minimize shrinkage during drying.
  • the wet gel is aged using a mixed solution of tetraethyl orthosilicate and ethanol.
  • the volume ratio of the tetraethyl orthosilicate to the ethanol is 1:3 to 5, preferably 1:3.5 to 4.5.
  • the weight ratio of the weight of the mixture of the orthosilicate and the ethanol to the wet gel is from 1 to 1.5:1, preferably from 1 to 1.3:1.
  • the aging time is 40 to 60 h, preferably 45 to 55 h.
  • the reactive hydroxyl groups on the surface of the wet gel and the weak network skeleton structure react with the tetraethyl orthosilicate, which enhances the silicon-oxygen bridge (-O-Si-O), thereby improving the network of the gel skeleton.
  • Degree and strength which can reduce the shrinkage and cracking of the gel during the drying process.
  • the step b preferably further comprises: immersing the obtained alcohol gel in ethanol to remove unreacted orthosilicate, preferably the soaking step is repeated twice, and the soaking time is preferably 20-30. h, more preferably 20 to 25 h.
  • the drying control chemical additive in the present invention is preferably N,N-dimercaptoamide, N,N-dimercaptoacetamide, decylamide or acetamide, more preferably decylamide or acetamide, and even more preferably hydrazine. Amide.
  • the molar ratio of the drying control chemical additive to the silica in the alcohol gel is from 0.15 to 0.4:1, preferably from 0.2 to 0.3:1.
  • the small radius atoms with large electronegativity in the dry control chemical additive tend to give electrons, forming hydrogen bonds with the ⁇ SiOH on the surface of the colloidal particles, thereby creating a wide shielding network around them.
  • the hydrogen bonding also causes the incomplete condensed SiO-chain in the system to slow down the polycondensation rate, and many branches are added during the formation of the skeleton network structure, which promotes the formation of large and uniform nanopores.
  • the drying temperature is 60 ° C ⁇ 80 ° C, preferably 65 ° C ⁇ 75 ° C, the drying time is
  • the silica aerogel prepared by the invention adopts an atmospheric pressure drying method, and the raw material cost is low, and the preparation process is convenient.
  • the mass fraction of the silica aerogel is preferably from 20 to 60%, more preferably from 30 to 55%, still more preferably from 40 to 55%.
  • the soluble silicon salt is not particularly limited as long as it is a soluble silicon salt well known to those skilled in the art.
  • potassium silicate or sodium silicate is preferred, and the mass fraction thereof is preferably 15 to 50%, more preferably 20 ⁇ 40%.
  • the function of the soluble silicon salt is to improve the strength of the inorganic insulating material.
  • the compound of the formula (I) is a polyalkyltrimethylammonium halide wherein n is preferably 6 ⁇ n ⁇ 18, X is preferably Br or C1, and more preferably dodecyltrimethylammonium chloride.
  • the mass fraction is preferably from 15 to 30%, more preferably from 18 to 25%.
  • the compound of the formula (I) is used as a dispersing agent in the present invention, and its function is to change the hydrophobicity of silica and to fabricate nanopores.
  • the mass fraction of the tin oxide is preferably 8 to 12%, which absorbs infrared rays and ultraviolet rays and has a certain heat insulating effect.
  • the hollow glass bead preferably has a mass fraction of 8 to 12%, and is a hollow nano-silicon-based material having a strong reflection effect, especially for infrared rays, which can effectively prevent heat radiation.
  • hollow glass beads coated with nitrogen gas are preferred, which have waterproof and moisture-proof effects.
  • each of the above substances is mixed and modified with a coupling agent, which is a coupling agent well known to those skilled in the art, and is not particularly limited.
  • a silane coupling agent is preferred.
  • the silica aerogel is subjected to a hydrophobic treatment.
  • the coupling agent and the quality of the silica aerogel The ratio is preferably 1:1 to 3, more preferably 1:1.5 to 2.5.
  • the addition time of the coupling agent is not particularly limited, and may be added after the silica aerogel, the soluble silicate, the compound of the formula (I) structure, the antimony tin oxide and the hollow glass microbeads are added, the order of addition There is no particular limitation.
  • the time of the modification is not limited to the time known to those skilled in the art, and is preferably 20-40 min in the present invention.
  • the silica aerogel, the soluble silicate, the compound of the formula (I), the antimony tin oxide and the hollow glass microbead are mixed and modified, and then mixed with water to form a slurry, which is then impregnated onto the glass fiber mat. Further, an inorganic heat insulating material is obtained.
  • the mixture obtained after the modification is mixed with water in a ratio of 0.8 to 2 kg: 1 L to form a slurry.
  • the slurry and the glass fiber mat were infiltrated at a ratio of 1 L: 0.36 to 1.4 m 2 .
  • the slurry is impregnated onto the glass fiber mat by pressurization, and the spraying pressure is 80 MPa to 300 MPa, preferably 100 MPa to 200 MPa.
  • the glass fiber mat not only has the advantages of high temperature resistance, corrosion resistance, dimensional stability, extremely small elongation and contraction rate and high strength, and the felt fiber has a single fiber, a three-dimensional microporous structure and a high porosity. A certain thermal insulation effect.
  • the present invention preferably sprays a coupling agent on the fiber mat after the slurry is wetted onto the glass fiber mat.
  • the hot pressing temperature is 60 ° C to 100 ° C, preferably 70 ° C to 90 ° C, and the pressure is 80 to 300 MPa, preferably 100 to 200 MPa.
  • the hot pressing time is 2 to 4 h, preferably 2.5 to 3.5 h.
  • the invention is subjected to hydrophobic treatment by modification, and the water-repellent group is exposed due to the action of the coupling agent in the nano-microporous network structure of the material, so that the inorganic heat insulating material has good water resistance, does not need to be dried by the supercritical fluid, and reduces the production cost.
  • the preparation method is simple; the inorganic nano material and the inorganic fiber are used to make the inorganic thermal insulation material have high compressive strength, tensile strength and flexural strength, and the bonding strength with the base layer is high, and the structure is stable;
  • the silicon aerogel makes the inorganic thermal insulation material have a nano-scale micro-closed-cell network structure, thereby lowering the thermal conductivity of the inorganic thermal insulation material and improving the thermal insulation performance.
  • the invention also provides an inorganic thermal insulation material which is obtained by modifying the following components by a coupling agent and then infiltrating onto the glass fiber mat: Silica aerogel 15-60 wt%;
  • the silica aerogel, the soluble silicate, the compound of the formula (I), the antimony tin oxide and the hollow glass microbead are all the same as described above, and will not be described herein.
  • the silica aerogel obtained in 1.3 was ground and ultrasonically dispersed, it was analyzed by transmission electron microscopy to obtain a transmission electron microscope photograph, as shown in Fig. 1 and Fig. 2, and Fig. 1 is a 100 nm transmission electron microscope.
  • Photo, Figure 2 is a 50 nm transmission electron micrograph.
  • the silica aerogel prepared in Example 1 has a spatial network structure interpenetrating with each other, and the primary particle diameter of the gel is 10 to 25 nm; the silica particles have a regular spherical shape. Structure, after the particles are bonded by chemical bonds, they are connected to each other to form a porous structure with a pore diameter of 5 to 50 nm.
  • the silica aerogel obtained in 1.3 was analyzed by a scanning electron microscope to obtain a scanning electron micrograph thereof as shown in FIG. It can be seen from Fig. 3 that the primary particles of the aerogel have a slight agglomeration, and the aggregate size is 50-100 nm.
  • the agglomeration is mainly caused by the skeleton collapse caused by the capillary tension during the atmospheric drying process.
  • the hydroxy coupling reaction between the basic nanoparticles also causes the agglomeration to occur, and finally the gel particles form a sparse nanometer by depositing in chemical bonds. Porous network structure.
  • the silica aerogel obtained in 1.3 was subjected to heat treatment, and analyzed by X-ray to obtain an X-ray diffraction pattern thereof, as shown in Figs. 4 to 7.
  • Figure 4 shows the X-ray diffraction pattern of the silica aerogel after drying at room temperature
  • Figure 5 shows the X-ray diffraction pattern of the silica aerogel after treatment at 500 °C
  • Figure 6 shows the X-ray diffraction pattern of the silica aerogel after treatment at 900 °C.
  • Figure 7 is an X-ray diffraction pattern of silica aerogel treated at 1100 °C.
  • the silica aerogel exhibits an amorphous structure when heat-treated at 900 ° C or lower. As can be seen from Fig. 7, when the treatment temperature reached 1100 ° C, the amorphous silica was converted to cristobalite.
  • the specific surface area and average pore diameter of the silica aerogel obtained in 1.3 were tested, and the results are shown in Table 2. It can be seen from Table 2 that the silica aerogel obtained in 1.3 has a relatively large average pore diameter and specific surface area.
  • the pore size of the silica aerogel obtained in 1.3 was analyzed to obtain a pore size distribution histogram, as shown in Fig. 8, wherein the pore size distribution of the silica aerogel obtained in 1.3 was obtained. It can be seen from Fig. 8 that the ratio of the smaller pore size between 1.78-3.33 nm and the larger pore size between 22.17-39.41 nm in the silica aerogel obtained in 1.3 is reduced, and the size is 3.33 ⁇ 22.17. The proportion of the intermediate pores between nm has increased, forming a relatively uniform nano-network pore skeleton.
  • 500 g of the silica aerogel obtained in Example 1 was uniformly mixed with 250 g of a silane coupling agent, stirred for 30 min, and 150 g of potassium silicate, 150 g of dodecyltridecyl ammonium chloride, 50 g tin antimony oxide and 50 g hollow glass microspheres were mixed uniformly, and stirred with 5 L of water for 30 min to obtain a slurry.
  • the slurry was sprayed evenly onto 8 pieces of 30 cm x 30 cm, 0.4 cm thick glass fiber mat, and then hot pressed at a pressure of 100 MPa and a temperature of 80 ° C to obtain an inorganic heat insulating material.
  • Example 2 The inorganic insulating material obtained in Example 2 was tested for combustion performance according to GB/T 8624-2006, and the results are shown in Table 1.
  • Example 2 According to GB/T 20473, the inorganic insulating materials obtained in Example 2 were tested for compressive strength, compressive shear bond strength and dry apparent density, and the results are shown in Table 1.
  • the dimensional stability test of the inorganic thermal insulation material obtained in Example 2 was carried out according to GB/T 8811-2008, and the results are shown in Table 1.
  • Example 2 The thermal conductivity performance test of the inorganic thermal insulation material obtained in Example 2 was carried out according to GB/T 10294-2008, and the results are shown in Table 1.
  • Example 2 The inorganic heat insulating material obtained in Example 2 was tested for freeze-thaw resistance according to GB/T 50082, and the results are shown in Table 1.
  • Example 1 The weather resistance test was carried out on the inorganic heat insulating material obtained in Example 1 according to JGJ 144-2004, and the results are shown in Table 1.
  • Example 2 The water absorption test of the inorganic heat insulating material obtained in Example 2 was carried out according to GB/T 5486-2008, and the results are shown in Table 1.
  • silica aerogel purchased from Beijing Dekedao Gold Technology Co., Ltd. was mixed with 250 g of silane coupling agent, stirred for 30 min, and 200 g of potassium silicate and 200 g of dodecyltriazine were added.
  • the ammonium chloride, 100 g of antimony tin oxide and 100 g of hollow glass microspheres were uniformly mixed, and stirred with 5 L of water for 30 min to obtain a slurry.
  • the slurry was sprayed evenly onto 8 pieces of 30 cm x 30 cm, 0.4 cm thick glass fiber mat, and then hot pressed at a pressure of 150 MPa and a temperature of 80 ° C to obtain an inorganic insulation material.
  • Example 3 The inorganic insulating material obtained in Example 3 was tested for combustion performance according to GB/T 8624-2006, and the results are shown in Table 1.
  • Example 3 According to GB/T 20473, the inorganic insulating materials obtained in Example 3 were tested for compressive strength, compressive shear bond strength and dry apparent density, and the results are shown in Table 1.
  • Example 3 The dimensional stability test of the inorganic thermal insulation material obtained in Example 3 was carried out according to GB/T 8811-2008, and the results are shown in Table 1.
  • Example 3 The thermal conductivity performance test of the inorganic thermal insulation material obtained in Example 3 was carried out according to GB/T 10294-2008, and the results are shown in Table 1.
  • Example 3 The inorganic heat insulating material obtained in Example 3 was tested for freeze-thaw resistance according to GB/T 50082, and the results are shown in Table 1.
  • Example 3 The weather resistance test was carried out on the inorganic heat insulating material obtained in Example 3 according to JGJ 144-2004, and the results are shown in Table 1.
  • Example 3 The water absorption rate test of the inorganic thermal insulation material obtained in Example 3 was carried out according to GB/T 5486-2008. The results are shown in Table 1.
  • silica aerogel purchased from Beijing Dekedao Gold Technology Co., Ltd. was mixed with 250 g of silane coupling agent, stirred for 30 min, and 180 g of potassium silicate and 180 g of dodecyltridecyl group were added.
  • Ammonium chloride, 120 g of antimony tin oxide and 120 g of hollow glass microspheres were uniformly mixed, and stirred with 5 L of water for 30 min to obtain a slurry.
  • the slurry was sprayed evenly onto 8 pieces of 30 cm x 30 cm, 0.4 cm thick glass fiber mat, and then hot pressed at a pressure of 200 MPa and a temperature of 80 °C to obtain an inorganic insulation material.
  • Example 4 The inorganic insulating material obtained in Example 4 was tested for combustion performance according to GB/T 8624-2006, and the results are shown in Table 1.
  • Example 4 According to GB/T 20473, the inorganic insulating materials obtained in Example 4 were tested for compressive strength, compressive shear bond strength and dry apparent density, and the results are shown in Table 1.
  • Example 4 The dimensional stability test of the inorganic thermal insulation material obtained in Example 4 was carried out according to GB/T 8811-2008, and the results are shown in Table 1.
  • Example 4 The thermal conductivity test of the inorganic thermal insulation material obtained in Example 4 was carried out according to GB/T 10294-2008, and the results are shown in Table 1.
  • Example 4 The inorganic heat insulating material obtained in Example 4 was tested for freeze-thaw resistance according to GB/T 50082, and the results are shown in Table 1.
  • Example 4 The weather resistance test was carried out on the inorganic heat insulating material obtained in Example 4 according to JGJ 144-2004, and the results are shown in Table 1.
  • Example 4 The water absorption test of the inorganic thermal insulation material obtained in Example 4 was carried out according to GB/T 5486-2008, and the results are shown in Table 1.
  • Embodiment 2 Embodiment 3 Embodiment 4
  • Kpa Compressive strength
  • Combustion performance A1 A1 A1 Thermal conductivity (W/(mk) ) 0.027 0.026 0.025 Weather-resistant samples after 80 cold rain samples, 80 cold rain samples, 80 cold rains
  • the pore size of the silica aerogel obtained in Comparative Example 1 was analyzed to obtain a pore shape distribution histogram as shown in Fig. 8, wherein A.

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Abstract

L'invention concerne un matériau d'isolation thermique inorganique et un procédé pour le préparer. Le matériau inorganique de conservation de la chaleur est obtenu par mélange d'un aérogel de silice, de silicate soluble, d'un composé ayant une structure de formule (I), d'oxyde d'étain et d'antimoine et de billes de verre creuses, addition d'un agent de couplage pour modification, mélange avec de l'eau et infiltration dans un feutre de fibres de verre, et mise en œuvre d'un formage à la presse à chaud. l≤n≤24 et X représente F, Br ou Cl.
PCT/CN2013/078744 2013-01-15 2013-07-03 Matériau d'isolation thermique inorganique et son procédé de préparation WO2014110892A1 (fr)

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CN201310014752.9 2013-01-15

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