JP6603894B2 - 断熱シートとその製造方法 - Google Patents
断熱シートとその製造方法 Download PDFInfo
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- 238000009413 insulation Methods 0.000 title claims description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 239000000835 fiber Substances 0.000 claims description 74
- 239000000463 material Substances 0.000 claims description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 43
- 239000000377 silicon dioxide Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 8
- 239000003929 acidic solution Substances 0.000 claims description 7
- 239000004745 nonwoven fabric Substances 0.000 claims description 7
- 229920001778 nylon Polymers 0.000 claims description 6
- 239000004677 Nylon Substances 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 5
- 239000004965 Silica aerogel Substances 0.000 claims description 4
- 239000000443 aerosol Substances 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229920000742 Cotton Polymers 0.000 claims description 2
- 229920000297 Rayon Polymers 0.000 claims description 2
- 229920002978 Vinylon Polymers 0.000 claims description 2
- 239000002964 rayon Substances 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 48
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 20
- 239000003795 chemical substances by application Substances 0.000 description 15
- 238000011282 treatment Methods 0.000 description 13
- 239000002253 acid Substances 0.000 description 9
- 239000004743 Polypropylene Substances 0.000 description 8
- 238000007654 immersion Methods 0.000 description 8
- 239000011810 insulating material Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 6
- 229910002028 silica xerogel Inorganic materials 0.000 description 6
- 238000001879 gelation Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000006884 silylation reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 3
- 239000002121 nanofiber Substances 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002994 raw material 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
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
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- 230000010365 information processing Effects 0.000 description 2
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- 230000035515 penetration Effects 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 101150096839 Fcmr gene Proteins 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011490 mineral wool Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
- F16L59/04—Arrangements using dry fillers, e.g. using slag wool which is added to the object to be insulated by pouring, spreading, spraying or the like
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- 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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
- B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
- B05D3/065—After-treatment
- B05D3/067—Curing or cross-linking the coating
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- 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
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- C01B33/16—Preparation of silica xerogels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- 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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
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- 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
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/503—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms without bond between a carbon atom and a metal or a boron, silicon, selenium or tellurium atom
- D06M13/507—Organic silicon compounds without carbon-silicon bond
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- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- D06M2101/04—Vegetal fibres
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Description
まず、下敷きPPフィルム24(ポリプロピレンフィルム)をセットし、その上に図2Aで示す基材21を載せる。
まず、下敷きPPフィルム24を敷く。その上に、基材21をセットする。図2Aは、基材21である。基材21は、2種類の繊維を含有している。図2Bは、基材21の拡大断面図である。
シリカゾルのシリカ材料として、高モル珪酸水溶液(東曹産業株式会社製、SiO2濃度14%)使用する。これに触媒として濃塩酸を1.4%添加してシリカゾル溶液を調製する。
使用するシリカゾルの量は、基材21の嵩密度から求めた理論空間体積以上とし、基材21中の空隙がすべてシリカゾルで満たされるように含浸する。含浸が終了したら、シリカゾルに含まれる水分が容易に蒸発しないように、乾燥防止のPPフィルム26を含浸済み基材21の上から被せて、シリカゾルの乾燥を防止する。基材21中の空隙は、後の工程を経てエアロゲルになる。そのエアロゲルの含有率は、基材21の嵩密度にもよるが、20〜80重量%が好ましく、より好ましくは40〜70重量%である。含有率が40重量%未満では、所望の断熱性が得られない場合がある。含有率が70重量%を超えると、生産性や経済性を損なう場合がある。
含浸された基材21を20分放置し、ゲル化するのを待つ。ゲル化が確認できたら、プレスをして厚みを整える。厚みの整え方は、ロールプレスなどの方法を用いても良い。
厚みを整えた基材21を容器に入れ、温度85℃、85%設定の恒温恒湿槽に3時間保管し、シリカ二次粒子を成長させて、ゲル骨格の構造を強化する。保管温度は100℃未満が好ましい。湿度については、基材に含まれるゲルから水分が容易に蒸発しないよう、80%以上が好ましい。保管時間は0.5時間から6時間以内が好ましい。
養生の処理が終了したら、恒温恒湿槽から基材21を取り出し、図2CのPPフィルム24、26を剥がし、疎水化処理(塩酸浸漬)を行う。
前記の処理が終了したら、疎水化処理の第二段階として、シリル化剤とアルコールの混合溶液(オクタトリメチルトリシロキサンと2−プロパノール)に浸漬させた後、55℃の恒温槽にて2時間保管する。
前記疎水化処理の2つの処理が終了したら、150℃の恒温槽にて2時間の乾燥処理を行う。この際も基材21中に形成された空洞30の作用により、基材21の厚みが厚くなっても、基材21の内部まで確実に乾燥が完了する。
断熱シート27の評価は、厚みと熱伝導率を測定した。
無機の第1繊維22の不織布と、無機の第1繊維22の重量の1.5%で直径0.1mm長さが直径の2倍以上のナイロンである第2繊維23と、を含む基材21を用意した。処理手順は本実施の形態どおり行った。完成した断熱シート27の厚みは、4.15mmであった。また、熱伝導率は21.7mW/m・Kであり、所望の断熱シート27を得ることができた。
無機の第1繊維22の不織布と、無機の第1繊維22の6.4重量%で直径0.2mm長さが直径の2倍以上のナイロンの第2繊維23と、を含有させた基材21を用意した。処理手順は本実施の形態どおり行った。完成した断熱シート27は、4.09mmであった。また、熱伝導率は21.8mW/m・Kであり、所望の断熱シート27を得ることができた。
無機の第1繊維22のみで構成される不織布を使用し、処理手順は本実施の形態どおり行った。製品の完成厚みは、4.23mmであった。熱伝導率を測定しようとしたが、内部から塩酸およびシリル化剤の混合物と見られる液体が染み出しているのを確認したため、測定することができなかった。この条件では正常な断熱シートを得ることができなかった。
無機の第1繊維22の不織布と、無機の第1繊維22の25.6重量%で直径0.4mm長さが直径の2倍以上のナイロンの第2繊維23と、を含有させた基材21を用意した。処理手順は本実施の形態どおりに行なった。その結果、直径0.4mm以上の第2繊維23を使用すると、疎水化(塩酸浸漬)時に可溶繊維である第2繊維23の溶け残りが発生し、酸性溶液に溶かされて造られる空洞内に、第2繊維23の溶け残りが残留した。
表1記載の疎水化(シリル化剤処理)での塩酸排出量(g)を見ると、実施例1および2と比較例1とでは、塩酸排出量にそれぞれ12g、11gの差が見られる。
酸として塩酸を使用したが、塩酸以外の酸でもよい。養生の工程を必須でなく、あればよりよい断熱シート27を作製できる。
22 第1繊維
23 第2繊維
24 PPフィルム
25 シリカゾル溶液
26 PPフィルム
27 断熱シート
30 空洞
31 シリカエアロゲル
Claims (11)
- 第1繊維と、
前記第1繊維に含まれるシリカエアロゲルと、
繊維状の空洞と、を含む断熱シート。 - 前記断熱シートは、積層体でなく、1層であり、厚さ1.5mm以上である請求項1記載の断熱シート。
- 前記繊維状の空洞は、直径0.2mm以下、長さが直径の2倍以上である請求項1記載の断熱シート。
- 前記繊維状の空洞は、直径0.01mm以上である請求項1に記載の断熱シート。
- 前記繊維状の空洞は、前記断熱シートの少なくとも2面に存在する、請求項1に記載の断熱シート。
- 前記繊維状の空洞の体積割合は、0.02〜2vol%である、請求項1に記載の断熱シート。
- 前記シリカエアロゲルの断熱シートに占める重量割合は、40〜70重量%である、請求項1に記載の断熱シート。
- 酸性溶液に不可溶な第1繊維と前記酸性溶液に可溶な第2繊維とを含む不織布基材にシリカエアロゾル溶液を含浸させる含浸工程と、
前記シリカエアロゾル溶液をゲル化させるゲル化工程と、
前記ゲルを疎水化する疎水化工程と、
前記ゲルを乾燥させる乾燥工程と、を備え、
前記第2繊維が前記疎水化工程で溶解する断熱シートの製造方法。 - 前記第2繊維は、ナイロン、レーヨン、キュプラ、アセテート、ビニロン、綿のうち、少なくとも1つ以上である請求項8に記載の断熱シートの製造方法。
- 前記第2繊維は、直径0.2mm以下、長さが直径の2倍以上である請求項8に記載の断熱シートの製造方法。
- 前記第2繊維は、直径0.01mm以上である請求項8に記載の断熱シートの製造方法。
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