JPWO2019069405A1 - 分散液及びエアロゲル粒子 - Google Patents
分散液及びエアロゲル粒子 Download PDFInfo
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- JPWO2019069405A1 JPWO2019069405A1 JP2019546468A JP2019546468A JPWO2019069405A1 JP WO2019069405 A1 JPWO2019069405 A1 JP WO2019069405A1 JP 2019546468 A JP2019546468 A JP 2019546468A JP 2019546468 A JP2019546468 A JP 2019546468A JP WO2019069405 A1 JPWO2019069405 A1 JP WO2019069405A1
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- airgel
- mass
- wet gel
- solvent
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 229940086066 potassium hydrogencarbonate Drugs 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 description 1
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 1
- 229940100890 silver compound Drugs 0.000 description 1
- 150000003379 silver compounds Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 235000019983 sodium metaphosphate Nutrition 0.000 description 1
- 235000019830 sodium polyphosphate Nutrition 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 238000009283 thermal hydrolysis Methods 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- VPYJNCGUESNPMV-UHFFFAOYSA-N triallylamine Chemical compound C=CCN(CC=C)CC=C VPYJNCGUESNPMV-UHFFFAOYSA-N 0.000 description 1
- ADGSJBYMQJVZIJ-UHFFFAOYSA-N trihydroxy(3,3,3-trifluoropropyl)silane Chemical compound O[Si](O)(O)CCC(F)(F)F ADGSJBYMQJVZIJ-UHFFFAOYSA-N 0.000 description 1
- YLZZRAHVHXTKGO-UHFFFAOYSA-N trihydroxy(octyl)silane Chemical compound CCCCCCCC[Si](O)(O)O YLZZRAHVHXTKGO-UHFFFAOYSA-N 0.000 description 1
- FCVNATXRSJMIDT-UHFFFAOYSA-N trihydroxy(phenyl)silane Chemical compound O[Si](O)(O)C1=CC=CC=C1 FCVNATXRSJMIDT-UHFFFAOYSA-N 0.000 description 1
- VYAMDNCPNLFEFT-UHFFFAOYSA-N trihydroxy(propyl)silane Chemical compound CCC[Si](O)(O)O VYAMDNCPNLFEFT-UHFFFAOYSA-N 0.000 description 1
- QTSIIQWGUWMBTD-UHFFFAOYSA-N trihydroxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound O[Si](O)(O)CCCOCC1CO1 QTSIIQWGUWMBTD-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical class [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
Classifications
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- 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
- C01B33/16—Preparation of silica xerogels
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D201/00—Coating compositions based on unspecified macromolecular compounds
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
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Abstract
Description
狭義には、湿潤ゲルに対して超臨界乾燥法を用いて得られた乾燥ゲルをエアロゲル、大気圧下での乾燥により得られた乾燥ゲルをキセロゲル、凍結乾燥により得られた乾燥ゲルをクライオゲルと称するが、本実施形態においては、湿潤ゲルのこれらの乾燥手法によらず、得られた低密度の乾燥ゲルを「エアロゲル」と称する。すなわち、本実施形態において、「エアロゲル」とは、広義のエアロゲルである「Gel comprised of a microporous solid in which the dispersed phase is a gas(分散相が気体である微多孔性固体から構成されるゲル)」を意味する。一般的に、エアロゲルの内部は、網目状の微細構造を有しており、2〜20nm程度の粒子状のエアロゲル成分が結合したクラスター構造を有している。このクラスターにより形成される骨格間には、100nmに満たない細孔がある。これにより、エアロゲルは、三次元的に微細な多孔性の構造が形成されている。なお、本実施形態に係るエアロゲルは、例えば、シリカを主成分とするシリカエアロゲルである。シリカエアロゲルとしては、例えば、有機基(メチル基等)又は有機鎖を導入した、いわゆる有機−無機ハイブリッド化されたシリカエアロゲルが挙げられる。
本実施形態に係るエアロゲルは、下記一般式(1)で表される構造を有することができる。本実施形態に係るエアロゲルは、式(1)で表される構造を含む構造として、下記一般式(1a)で表される構造を有することができる。
本実施形態に係るエアロゲルは、支柱部及び橋かけ部を備えるラダー型構造を有し、かつ橋かけ部が下記一般式(2)で表される構造を有することができる。このようなラダー型構造をエアロゲル成分としてエアロゲルの骨格中に導入することにより、耐熱性と機械的強度を向上させることができる。なお、本実施形態において「ラダー型構造」とは、2本の支柱部(struts)と支柱部同士を連結する橋かけ部(bridges)とを有するもの(いわゆる「梯子」の形態を有するもの)である。本態様において、エアロゲルの骨格がラダー型構造からなっていてもよいが、エアロゲルが部分的にラダー型構造を有していてもよい。
本実施形態に係るエアロゲルは、加水分解性の官能基又は縮合性の官能基を有するケイ素化合物、及び、加水分解性の官能基を有するケイ素化合物の加水分解生成物からなる群より選択される少なくとも一種、を含有するゾルの縮合物である湿潤ゲルの乾燥物(ゾルから生成された湿潤ゲルを乾燥して得られるもの:ゾル由来の湿潤ゲルの乾燥物)であってもよい。なお、これまで述べてきたエアロゲルも、このように、ケイ素化合物等を含有するゾルから生成された湿潤ゲルを乾燥することで得られるものであってもよい。
本実施形態に係るエアロゲルは、さらに強靱化する観点並びにさらに優れた断熱性及び柔軟性を達成する観点から、エアロゲル成分に加え、さらにシリカ粒子を含有していてもよい。エアロゲル成分及びシリカ粒子を含有するエアロゲルを、エアロゲル複合体ということもできる。エアロゲル複合体は、エアロゲル成分とシリカ粒子とが複合化されていながらも、エアロゲルの特徴であるクラスター構造を有しており、三次元的に微細な多孔性の構造を有していると考えられる。
本実施形態におけるエアロゲル粒子は、後述のとおりバルクのエアロゲルを粉砕することにより得ることができる。
エアロゲル粒子の製造方法は、特に限定されないが、例えば以下の方法により製造することができる。
ゾル生成工程は、ケイ素化合物と、場合によりシリカ粒子(シリカ粒子を含む溶媒であってもよい)と、を混合して加水分解反応を行った後、ゾルを生成する工程である。本工程においては、加水分解反応を促進させるため、溶媒中にさらに酸触媒を添加してもよい。また、特許第5250900号公報に示されるように、溶媒中に界面活性剤、熱加水分解性化合物等を添加することもできる。さらに、熱線輻射抑制等を目的として、溶媒中にカーボングラファイト、アルミニウム化合物、マグネシウム化合物、銀化合物、チタン化合物等の成分を添加してもよい。
湿潤ゲル生成工程は、ゾル生成工程で得られたゾルをゲル化し、その後熟成して湿潤ゲルを得る工程である。本工程では、ゲル化を促進させるため塩基触媒を用いることができる。
湿潤ゲル粉砕工程を行う場合、湿潤ゲル生成工程で得られた湿潤ゲルを粉砕する。粉砕は、例えば、ヘンシャル型ミキサーに湿潤ゲルを入れるか、又はミキサー内で湿潤ゲル生成工程を行い、ミキサーを適度な条件(回転数及び時間)で運転することにより行うことができる。また、より簡易的には密閉可能な容器に湿潤ゲルを入れるか、又は密閉可能な容器内で湿潤ゲル生成工程を行い、シェイカー等の振盪装置を用いて、適度な時間振盪することにより行うことができる。なお、必要に応じて、ジェットミル、ローラーミル、ビーズミル等を用いて、湿潤ゲルの粒子径を調整することもできる。
洗浄及び溶媒置換工程は、湿潤ゲル生成工程又は湿潤ゲル粉砕工程により得られた湿潤ゲルを洗浄する工程(洗浄工程)と、湿潤ゲル中の洗浄液を乾燥条件(後述の乾燥工程)に適した溶媒に置換する工程(溶媒置換工程)を有する工程である。洗浄及び溶媒置換工程は、湿潤ゲルを洗浄する工程を行わず、溶媒置換工程のみを行う形態でも実施可能であるが、湿潤ゲル中の未反応物、副生成物等の不純物を低減し、より純度の高いエアロゲル粒子の製造を可能にする観点からは、湿潤ゲルを洗浄してもよい。
乾燥工程では、上記のとおり洗浄及び(必要に応じ)溶媒置換した湿潤ゲルを乾燥させる。これにより、エアロゲル(エアロゲルブロック又はエアロゲル粒子)を得ることができる。すなわち、上記ゾルから生成された湿潤ゲルを乾燥してなるエアロゲルを得ることができる。
湿潤ゲル粉砕工程を行わない場合は、乾燥により得られたエアロゲル(エアロゲルブロック)を粉砕することによりエアロゲル粒子を得る。例えば、ジェットミル、ローラーミル、ビーズミル、ハンマーミル等にエアロゲルを入れ、適度な回転数と時間で運転することにより行うことができる。
分散液は、上述の比表面積が350m2/g以下であるエアロゲル粒子と分散媒とを含む。分散液は、上述のエアロゲル粒子を分散媒中に分散させてなるものであるということもできる。分散液中のエアロゲル粒子は、細孔内が分散媒で満たされていてもよい。
シリカ粒子含有原料としてPL−2L(扶桑化学工業株式会社製、製品名)を100.0質量部、水を80.0質量部、酸触媒として酢酸を0.5質量部、カチオン性界面活性剤として臭化セチルトリメチルアンモニウム(和光純薬工業株式会社製)を1.0質量部、及び熱加水分解性化合物として尿素を150.0質量部混合し、これにケイ素化合物としてメチルトリメトキシシラン(信越化学工業株式会社製、製品名:KBM−13)を60.0質量部、ジメチルジメトキシシラン(信越化学工業株式会社製、製品名:KBM−22)を20.0質量部、上記一般式(B)で表される構造を有する両末端2官能アルコキシ変性ポリシロキサン化合物(以下、「ポリシロキサン化合物A」という)を20.0質量部加え、25℃で2時間反応させてゾルを得た。得られたゾルを60℃でゲル化した後、60℃で48時間熟成して湿潤ゲル1を得た。
PL−2Lを100.0質量部、水を60.0質量部、酢酸を0.10質量部、臭化セチルトリメチルアンモニウムを20.0質量部、メチルトリメトキシシランを60.0質量部、ジメチルジメトキシシランを20.0質量部、及びポリシロキサン化合物Aを20.0質量部加え、25℃で2時間反応させてゾルを得た。得られたゾルに、塩基触媒として5%濃度の炭酸ナトリウム水溶液を40.0質量部加え、60℃でゲル化した後、80℃で24時間熟成して湿潤ゲル2を得た。その後、得られた湿潤ゲル2を用いて、実施例1と同様にして上記一般式(3)、(4)及び(5)で表される構造を有するエアロゲル粒子2を得た。エアロゲル粒子2の平均粒子径D50は14.2μmであった。
ポリシロキサン化合物であるXR31−B1410(モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社製)を30.0質量部、ジメチルジメトキシシランを15.0質量部、2−プロパノールを100.0質量部、水を20.0質量部、酢酸を0.05質量部加え、25℃で4時間反応させてゾルを得た。得られたゾルに、塩基触媒として5%濃度の炭酸アンモニア水溶液を40.0質量部加え、60℃でゲル化した後、60℃で72時間熟成して湿潤ゲル3を得た。その後、得られた湿潤ゲル3を用いて、実施例1と同様にして上記一般式(4)及び(5)で表される構造を少なくとも有するエアロゲル粒子3を得た。エアロゲル粒子3の平均粒子径D50は19.7μmであった。
水ガラス(富士化学株式会社製:SiO2;8.0wt%、2Na2O・3SiO2・mH2O)10質量部に、H型イオン交換樹脂(住化ケムテックス株式会社、Duolite C20)20質量部を添加し、液のpHが1.5になるまで攪拌した。次に、イオン交換樹脂をろ別した後、アンモニア水(関東化学株式会社製、特級、1mol/L)400質量部加えてpHを4.0に調整した。これを、室温で20分間かけてゲル化し、次に50℃で24時間熟成させ、湿潤ゲルを得た。
3号ケイ酸ソーダの溶液を希釈し、SiO2:80g/L、Na2O:27g/Lの濃度に調整した。この希釈したケイ酸ソーダの溶液を、強酸性陽イオン交換樹脂IR120B(ローム・アンド・ハース社製、製品名)に通過させ、100質量部のシリカゾルを得た。このシリカゾルのpHは、2.8であった。
エアロゲル粒子6としてJIOS AeroVa(登録商標、JIOS AEROGEL CORPORATION社製、製品名)を準備した。エアロゲル粒子6の平均粒子径D50は8.7μmであった。
エアロゲル粒子のBET比表面積を、ガス吸着量測定装置(カンタクローム・インスツルメンツ・ジャパン合同会社製、Autosorb−iQ(Autosorbは登録商標))を用いて測定した。
9mLのスクリュー管に分散媒として2−プロパノールを4gを入れ、そこにエアロゲル粒子を1g投入して、ボルテックスミキサーを用いて30秒撹拌を行い、分散液を調製した。撹拌後の分散液を目視にて観察し、エアロゲル粒子の分散性を評価した。エアロゲル粒子が良好に分散し、分散液に流動性がある場合をA評価、エアロゲル粒子が分散せずに凝集し、分散液に流動性がない場合をB評価とした。
実施例1のエアロゲル粒子を用いて塗液を調製し、得られた塗膜の成膜性、付着性及び断熱性評価を行った。まず、イソプロピルアルコール50gに、エアロゲル粒子10g、チョップドストランドガラスCS 3DE−256(日東紡績株式会社製、製品名)1g、及びカルボキシメチルセルロースアンモニウム(和光純薬製、製品名)1gを加え、スリーワンモータを用いて300rpmで10分間攪拌した。続いて、水50gを加えてさらに300rpmで10分間攪拌して塗液を調製した。この塗液を、金属ヘラを用いて、厚みが1mmとなるように12μmのアルミ箔上に塗布し、120℃で1時間乾燥して塗膜を得た。
Claims (4)
- 比表面積が350m2/g以下であるエアロゲル粒子と、分散媒と、を含む分散液。
- 前記分散媒が有機溶媒を含む、請求項1に記載の分散液。
- 比表面積が350m2/g以下であるエアロゲル粒子。
- 分散液調製用である、請求項3に記載のエアロゲル粒子。
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JP2019546468A Active JP7107321B2 (ja) | 2017-10-04 | 2017-10-04 | 分散液及びエアロゲル粒子 |
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TW (1) | TW201922930A (ja) |
WO (1) | WO2019069405A1 (ja) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB805102A (en) * | 1955-05-06 | 1958-11-26 | Monsanto Chemicals | Modified silica aerogels and silicone rubbers containing the same |
US3367742A (en) * | 1963-10-18 | 1968-02-06 | Monsanto Co | Chemical compositions and processes |
JP2006515556A (ja) * | 2002-12-18 | 2006-06-01 | デグサ アクチエンゲゼルシャフト | 表面改質された、エアロゲル型ストラクチャードシリカ |
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2017
- 2017-10-04 JP JP2019546468A patent/JP7107321B2/ja active Active
- 2017-10-04 WO PCT/JP2017/036164 patent/WO2019069405A1/ja active Application Filing
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2018
- 2018-09-27 TW TW107133948A patent/TW201922930A/zh unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB805102A (en) * | 1955-05-06 | 1958-11-26 | Monsanto Chemicals | Modified silica aerogels and silicone rubbers containing the same |
US3367742A (en) * | 1963-10-18 | 1968-02-06 | Monsanto Co | Chemical compositions and processes |
JP2006515556A (ja) * | 2002-12-18 | 2006-06-01 | デグサ アクチエンゲゼルシャフト | 表面改質された、エアロゲル型ストラクチャードシリカ |
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JP7107321B2 (ja) | 2022-07-27 |
TW201922930A (zh) | 2019-06-16 |
WO2019069405A1 (ja) | 2019-04-11 |
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