WO2020009226A1 - Charge d'isolation thermique, matériau d'isolation thermique et structure d'isolation thermique - Google Patents

Charge d'isolation thermique, matériau d'isolation thermique et structure d'isolation thermique Download PDF

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Publication number
WO2020009226A1
WO2020009226A1 PCT/JP2019/026834 JP2019026834W WO2020009226A1 WO 2020009226 A1 WO2020009226 A1 WO 2020009226A1 JP 2019026834 W JP2019026834 W JP 2019026834W WO 2020009226 A1 WO2020009226 A1 WO 2020009226A1
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WO
WIPO (PCT)
Prior art keywords
mass
silica
heat
heat insulating
insulating filler
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Ceased
Application number
PCT/JP2019/026834
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English (en)
Japanese (ja)
Inventor
航平 水田
浩徳 長崎
和人 田原
内藤　牧男
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Denka Co Ltd
University of Osaka NUC
Original Assignee
Denka Co Ltd
Osaka University NUC
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Priority to JP2020529066A priority Critical patent/JP7377498B2/ja
Publication of WO2020009226A1 publication Critical patent/WO2020009226A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
    • F16L59/00—Thermal insulation in general

Definitions

  • the present invention relates to a heat insulating filler, a heat insulating material, and a heat insulating structure.
  • heat insulation materials are also attracting attention from the viewpoint of, for example, keeping the heat of internal combustion engines and fuel cells, and can be applied to various shapes not limited to molded bodies. Insulating materials are required.
  • porous body containing fine pores of 100 nm or less exhibits excellent heat insulating properties.
  • porous heat insulating materials include inorganic porous heat insulating materials using silica fine particles manufactured by a dry method as shown in Patent Documents 1 to 5. This exhibits excellent heat insulating properties because fluid heat transfer is suppressed by forming a fine porous structure by dry silica containing micropores.
  • the use form as a heat insulating material in the above-mentioned conventional technology is often based on a molded body formed by a mechanical press, and as described in the above-mentioned patent document, many studies have been made to improve dust generation and strength after molding. ing.
  • the powder to be used is required to have good fluidity that can be uniformly filled in a mold.
  • dry silica fine particles have a problem of handling properties during the manufacturing process because they exhibit a small bulk density and strong adhesiveness and squirt property derived from Coulomb force.
  • the heat insulating layer is formed by filling the space with the powder by the flow of the powder.
  • a heat insulating powder having an excellent filling property is required.
  • air in the target space is replaced with powder, so that dry silica fine particles having a very small bulk density are not suitable.
  • Patent Document 8 describes a method for producing a heat insulating material in which a mixture containing 1) silica fine particles as a main component, 2) reinforcing fibers, and 3) a liquid storage material impregnated with water is wet-formed and dried. are doing.
  • Patent Documents 9 and 10 describe heat insulating boards filled with two or more kinds of fine particles having different primary particle diameters. However, Patent Documents 8 to 10 do not describe the water content.
  • the present invention has been made in view of the above problems and background, and has an object to provide a heat-insulating filler that has good heat-insulating properties and can exhibit excellent filling properties.
  • the present inventors have conducted intensive studies, and as a result, the problem was solved by a heat insulating filler containing mixed silica powder obtained by mixing dry silica fine particles and wet silica fine particles at a predetermined ratio. We found that we could solve it. That is, the present invention is as follows.
  • An insulating filler comprising a mixed silica powder comprising 10% by mass to 80% by mass of dry silica and 20% by mass to 90% by mass of wet silica having a water content of 2% by mass or more.
  • the heat-insulating filler according to [1] containing 1 to 10 parts by mass of the inorganic fiber based on 100 parts by mass of the mixed silica powder.
  • [5] The heat-insulating filler according to any one of [1] to [4], wherein the average particle size of the dry silica is 0.8 ⁇ m or less, and the average particle size of the wet silica is 1 ⁇ m or more.
  • a heat insulating material comprising the heat insulating filler according to any one of [1] to [6].
  • [8] A heat insulating structure including the heat insulating material according to [7].
  • a heat insulating filler which has good heat insulating properties and can exhibit excellent filling properties.
  • an excellent heat insulating effect and a heat retaining effect can be provided for various shapes.
  • the heat-insulating filler according to one embodiment (the present embodiment) of the present invention is a mixture comprising 10% by mass to 80% by mass of dry silica and 20% by mass to 90% by mass of wet silica having a water content of 2% by mass or more. Contains silica powder.
  • a low thermal conductivity can be maintained by the fine pore structure formed by the fumed silica, and the charge on the surface is diffused by the moisture in the fumed silica, so that the adhesion is improved.
  • the fluidity is improved and excellent filling properties are exhibited.
  • the fluidity was further improved by the aggregation of the mixed silica powder obtained by mixing these and the addition of the mixed silica fine particles to the inorganic fibers.
  • Dry silica "used in the present invention is a general term for amorphous silica materials produced by a dry method, and those produced by any method such as a combustion method or an arc method can be used.
  • the combustion method refers to, for example, a method in which silicon tetrachloride is reacted in a high-temperature flame.
  • Dry silica (preferably dry silica fine particles) is a particle containing fine pores and gives a fine porous structure in the mixed silica powder. Therefore, from the viewpoint of reducing the thermal conductivity, the content is preferably 10% by mass to 80% by mass, and more preferably 30% by mass to 70% by mass. If the amount is less than 10% by mass, sufficient heat insulating properties may not be exhibited. If the amount exceeds 80% by mass, the fluidity of the powder cannot be sufficiently secured, and the filling property may be reduced.
  • wet silica "used in the present invention is a general term for amorphous silica substances produced by a wet method, and those produced by any method such as a precipitation method and a gel method can be used.
  • the sedimentation method refers to, for example, a method of neutralizing an aqueous solution of sodium silicate to precipitate silica, filtering and drying.
  • the wet silica preferably wet silica fine particles
  • the content is preferably from 20% by mass to 90% by mass, and more preferably from 30% by mass to 70% by mass from the viewpoint of fluidity and adhesion when the mixed silica powder is used. If the amount is less than 20% by mass, good handling properties may not be exhibited, and even if the amount exceeds 90% by mass, further enhancement of the effect cannot be expected.
  • the mixed silica powder is a powder containing dry silica and wet silica and obtained by mixing arbitrary inorganic fibers (and, if necessary, radiation scattering particles).
  • Water contained when mixing dry silica and wet silica has a role of suppressing van der Waals force acting on particles.
  • the water content is not particularly limited as long as it is 2% by mass or more based on the mass of the wet silica. If the amount is less than 2% by mass, the adhesion may increase due to static electricity acting on the particles, so that good handling properties may not be exhibited.
  • the water content of the wet silica is preferably from 3 to 15% by mass, more preferably from 5 to 10% by mass.
  • the water content of the mixed silica powder obtained by mixing the dry silica and the wet silica is preferably from 2 to 8% by mass, more preferably from 3 to 7% by mass from the viewpoint of good handling properties. preferable.
  • the average particle diameter of each of the dry silica and the wet silica (more specifically, the 50% integrated particle diameter D 50 measured by a laser diffraction type particle size analyzer (Model LS-230 manufactured by Coulter)) is 0.
  • the average particle diameter of the dry silica is preferably 10 ⁇ m or less from the viewpoint of suppressing the heat transfer of the fluid. Further, in order to improve the fluidity of the mixed silica powder and suppress the jetting property, it is preferable that the average particle diameter of wet silica is larger than that of dry silica.
  • the average particle size of the fumed silica is preferably 1 ⁇ m or less, more preferably 0.8 ⁇ m or less, and most preferably 0.5 ⁇ m or less.
  • the average particle size of the fumed silica is preferably 0.01 ⁇ m or more, more preferably 0.03 ⁇ m or more, and most preferably 0.05 ⁇ m or more.
  • the average particle size of the wet silica is preferably 0.5 ⁇ m or more, more preferably 1 ⁇ m or more, and most preferably 5 ⁇ m or more.
  • the average particle diameter of the wet silica is preferably 50 ⁇ m or less, more preferably 30 ⁇ m or less, and most preferably 20 ⁇ m or less.
  • inorganic fibers it is preferable to further mix inorganic fibers with the mixed silica powder.
  • the inorganic fiber used in the present invention is not particularly limited as long as the filling property is improved by impregnating the mixed silica powder with the fiber, and any inorganic fiber can be used. Further, at the time of molding, it has a role of giving moldability to the heat insulating filler. Typical examples are artificial fibers with excellent heat resistance, such as silica fiber, alumina silica fiber, glass fiber, zirconia fiber, silicon carbide fiber, rock wool manufactured from minerals, natural mineral wollastonite, sepiolite, etc. And one or more of these can be used as necessary.
  • the average fiber diameter of the inorganic fibers is an average value of the diameters of 100 fibers confirmed by scanning electron microscope (SEM) observation.
  • the average fiber diameter is preferably from 0.1 ⁇ m to 50 ⁇ m, and more preferably 1 ⁇ m or more, most preferably 5 ⁇ m or more, since the probability of silica fine particles being attached is increased and the ejectability of the powder is suppressed.
  • the average fiber length of the inorganic fibers is not particularly limited, but is preferably 10 ⁇ m or more, more preferably 15 to 35 ⁇ m, in consideration of the filling property of the mixed silica powder.
  • the average fiber length of the inorganic fibers can be determined as the average value of the fiber lengths of 100 fibers confirmed by scanning electron microscope (SEM) observation.
  • the content of the inorganic fiber is preferably from 1 to 10 parts by mass, more preferably from 3 to 7 parts by mass, per 100 parts by mass of the mixed silica powder.
  • the amount is 1 part by mass or more, sufficient moldability is easily exhibited, and when the amount is 10 parts by mass or less, contact between fibers is suppressed, material heat conduction is reduced, and thermal conductivity can be reduced.
  • the heat-insulating filler of the present invention may further contain radiation scattering particles in order to improve heat insulating properties at high temperatures (200 ° C. or higher).
  • the radiation scattering particles are not particularly limited as long as they can effectively scatter or absorb infrared rays.For example, silicon carbide, zirconium oxide, titanium oxide, copper oxide, and the like can be used, and one or more of these particles can be used. Seeds may be used.
  • the amount of the radiation scattering particles to be used is preferably 0.5% by mass to 35% by mass, more preferably 1.0% by mass to 20% by mass based on 100% by mass of the insulating filler.
  • the thermal conductivity of the heat-insulating filler obtained by the present invention is preferably 0.05 W / (m ⁇ K) or less at 25 ° C., and 0.029 W / (m ⁇ K) or less. Is more preferred.
  • the loose filling bulk density is a density obtained when powder is dropped and filled from a certain height into a ground container and then ground.
  • the heat-insulating filler obtained in the present invention preferably has a loose packing bulk density of 40 kg / m 3 or more, and more preferably 50 to 80 kg / m 3 , in a mixed silica powder state, from the viewpoint of approaching the designed packing density. More preferred. When it is 40 kg / m 3 or more, sufficient filling properties are exhibited, voids do not increase too much, and sufficient heat insulating properties are easily obtained.
  • the method for producing the heat-insulating filler is not particularly limited. For example, 10% to 80% by mass of dry silica and 20% to 90% by mass of wet silica having a water content of 2% by mass or more are several mm And a method of mixing them with a grinding mill having a clearance, and a method of mixing them with a metal blade while winding them up with an air current to obtain them by biaxial mixing.
  • the heat-insulating filler of the present embodiment as described above can be used as a solid. Further, among solids, it can be used as a powder.
  • Heat insulation material The heat insulation material according to the present embodiment is obtained by blending the above-mentioned heat insulation filler. Specifically, it refers to a heat insulating layer or a heat insulating material obtained by filling the above-described heat insulating filler as a raw material, for example, a heat insulating layer obtained by filling a space using the flow of powder. And a heat insulating material obtained by filling a mold with pressure.
  • the detailed method of obtaining by pressure filling is not particularly limited, but for example, it may be formed into a plate by a dry uniaxial press using a mold.
  • dry molding is preferred from the viewpoint of molding defects due to generation of voids and cracks during drying.
  • the heat insulating material according to the present embodiment may be formed by covering the whole of the above-mentioned heat insulating filler with a skin material.
  • the outer shell material is desirably in the form of sheet such as glass fiber, inorganic fiber woven fabric such as alumina fiber or inorganic fiber non-woven fabric, resin film, organic fiber woven fabric, organic fiber non-woven fabric, aluminum, metal foil such as copper foil, etc. There is no particular limitation.
  • the coating method is not particularly limited, and the filling rate of the heat-insulating filler can be appropriately set according to the intended use.
  • a heat-insulating filler formed by pressure molding may be covered with the above-described sheet, or a sheet-like processed sheet may be filled with the heat-insulating filler.
  • the heat insulation structure according to the present embodiment includes the above-described heat insulating material.
  • the heat-insulating filler according to the present embodiment may be used as it is as a heat insulating material, or may be combined with another heat insulating material to form a heat insulating structure.
  • a heat insulating structure configured by a laminated structure filled and laminated on another heat insulating material having different heat resistance
  • the heat insulating material to the heat insulating filler according to the present embodiment It can be said that this is a combined layered heat insulating structure.
  • a heat insulating structure in which a hollow box is filled with the heat insulating filler according to the present embodiment as a heat insulating material may be employed.
  • Example 1 Dry insulating silica and wet silica were mixed at a mixing ratio shown in Table 1, and 4.5 parts by mass of the inorganic fiber was mixed with 100 parts by mass of the mixture (mixed silica powder) to prepare an insulating filler.
  • Dry silica 1 (F1): CAB-O-SIL M-5 powder (trade name, manufactured by Cabot Specialty Chemicals), average particle size 0.20 ⁇ m, bulk density 70 g / L, water content 0.9 mass% Dry silica 2 (F2): AEROSIL 380 (trade name, manufactured by Nippon Aerosil Co., Ltd.), average particle size less than 0.05 ⁇ m, bulk density 50 g / L, water content 1.0 mass% Dry silica 3 (F3): NDK-N20 (trade name, manufactured by Asahi Kasei Wacker Silicone Co., Ltd.), average particle size 0.15 ⁇ m, bulk density 40 g / L, water content 1.2 mass%
  • Wet silica 1 CARPLEX # 80 powder (trade name, manufactured by Evonik Japan KK) Average particle size 15 ⁇ m, bulk density 145 g / L, water content 8.0 mass%
  • Wet silica 2 (W2): Toksil NP (trade name, manufactured by Oriental Silicas Corporation), average particle diameter 10 ⁇ m, bulk density 63 g / L, water content 6.2 mass%
  • Wet silica 3 (W3): Mizukasil P-527 (trade name, manufactured by Mizusawa Chemical Industry Co., Ltd.), average particle size 1.8 ⁇ m, bulk density 190 g / L, water content 5.2 mass%
  • Inorganic fiber 1 silica fiber sheet AS-300 (trade name, manufactured by Asahi Sangyo Co., Ltd.) Average fiber diameter 10 ⁇ m, 25 mm cutting and defibration processing (average fiber length: 25 mm)
  • the bulk density of the above-mentioned materials is a densely packed bulk density, which is measured by “Powder Tester PT-S” manufactured by Hosokawa Micron Corporation.
  • Water content The water content of dry silica, wet silica, and mixed silica powder was determined as the weight loss rate at 200 ° C. using a differential thermogravimetric analyzer TG-DTA 2000SR (trade name, Bruker AXS).
  • the loose filling bulk density was a density calculated by dropping the heat-insulating filler from the funnel into a stainless beaker having an inner diameter of 63 mm and a capacity of 200 mL at an interval of 150 mm, and performing abrasion filling.
  • a molded body (200 mm ⁇ 200 mm ⁇ 20 mm, density: about 230 kg / m 3 ) is produced from the produced heat-insulating filler by die molding using a uniaxial press, and a thermal conductivity measuring apparatus ( (Manufactured by Eiko Seiki Co., Ltd.) at 23 ° C.
  • a molded body (dimensions and the like were the same as above) was produced by die molding using a uniaxial press, and the moldability was visually evaluated. The case where no crack was observed in the molded body was evaluated as “O”, and the case where cracks or damage was observed was evaluated as “X”.
  • Example 2 Dry silica F1 was mixed at a ratio of 50% by mass and wet silica W1 was mixed at a ratio of 50% by mass, and inorganic fibers shown in Table 2 were used for the obtained mixture (mixed silica powder: Experiment No. 1-4), The procedure was performed in the same manner as in Experimental Example 1, except that the amount of the insulating filler was changed as shown in Table 2 to prepare the heat insulating filler. Table 2 shows the results.
  • Inorganic fiber 2 (Material used) Inorganic fiber 2 (IF2): glass fiber (manufactured by NEC Corporation), average fiber diameter 50 ⁇ m, average fiber length 25 mm
  • Inorganic fiber 3 (IF3): Alumina silica fiber (trade name: Denka-Alsen, manufactured by Denka) Average fiber diameter 5.0 ⁇ m, average fiber length 25 mm
  • Example 3 Experiment No. Except that the thermal conductivity (high-temperature thermal conductivity) at a high temperature (600 ° C.) was measured using the radiation-scattering particles shown in Table 3 using the formulation 1-4 and changing the blending amount as shown in Table 3. Was performed in the same manner as in Experimental Example 1.
  • a molded body (the dimensions and the like are the same as above) is produced from the produced heat-insulating filler by die molding using a uniaxial press, and a protective thermal plate method thermal conductivity measuring apparatus in accordance with JIS A 1412-1. It measured at 600 degreeC using (made by Eikoseiki).
  • the heat-insulating filler of the present invention configured as described above has excellent operability and filling properties, and has more heat resistance and heat insulating properties than before, so it can be applied to complicated shapes, It can contribute to energy saving of vehicles, airplanes, other internal combustion engines, and piping.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Thermal Insulation (AREA)
  • Silicon Compounds (AREA)

Abstract

La présente invention concerne une charge d'isolation thermique qui contient une poudre de silice mélangée qui est composée de 10 % en masse à 80 % en masse de silice sèche et de 20 % en masse à 90 % en masse de silice humide ayant une teneur en humidité supérieure ou égale à 2 % en masse. La poudre de silice mélangée contient de préférence de 1 partie en masse à 10 parties en masse de fibres inorganiques pour 100 parties en masse ; et les fibres inorganiques ont de préférence un diamètre moyen de fibre de 0,1 µm à 50 µm.
PCT/JP2019/026834 2018-07-06 2019-07-05 Charge d'isolation thermique, matériau d'isolation thermique et structure d'isolation thermique Ceased WO2020009226A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2021102998A (ja) * 2019-12-26 2021-07-15 デンカ株式会社 断熱充填材、断熱材、断熱構造
CN114576471A (zh) * 2022-03-01 2022-06-03 四川零零昊科技有限公司 一种柔性毡、隔热方法、柔性毡的填料、制备方法及用途

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JP2003026759A (ja) * 2001-07-23 2003-01-29 Nippon Polyurethane Ind Co Ltd バッキング層形成用の樹脂組成物およびマットの製造方法
JP2013199421A (ja) * 2012-02-21 2013-10-03 Japan Insulation Co Ltd 断熱材及びその製造方法

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JPS61291466A (ja) * 1985-06-18 1986-12-22 松下電器産業株式会社 真空断熱構造体
JPH07144955A (ja) * 1993-11-17 1995-06-06 Nippon Silica Ind Co Ltd 断熱板用シリカ成形体及び真空断熱板
JP5568346B2 (ja) * 2010-03-23 2014-08-06 アキレス株式会社 真空断熱材
JP5824272B2 (ja) * 2011-07-28 2015-11-25 旭化成ケミカルズ株式会社 粉体、成形体、被包体及び粉体の製造方法
JP5854642B2 (ja) * 2011-05-27 2016-02-09 旭化成ケミカルズ株式会社 粉体の製造方法

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Publication number Priority date Publication date Assignee Title
JP2003026759A (ja) * 2001-07-23 2003-01-29 Nippon Polyurethane Ind Co Ltd バッキング層形成用の樹脂組成物およびマットの製造方法
JP2013199421A (ja) * 2012-02-21 2013-10-03 Japan Insulation Co Ltd 断熱材及びその製造方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2021102998A (ja) * 2019-12-26 2021-07-15 デンカ株式会社 断熱充填材、断熱材、断熱構造
JP7466856B2 (ja) 2019-12-26 2024-04-15 デンカ株式会社 断熱充填材、断熱材、断熱構造
CN114576471A (zh) * 2022-03-01 2022-06-03 四川零零昊科技有限公司 一种柔性毡、隔热方法、柔性毡的填料、制备方法及用途

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