JP7078104B2 - エアロゲルの製造方法、エアロゲル、エアロゲルブロック及びポリシロキサン化合物 - Google Patents
エアロゲルの製造方法、エアロゲル、エアロゲルブロック及びポリシロキサン化合物 Download PDFInfo
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- JP7078104B2 JP7078104B2 JP2020504596A JP2020504596A JP7078104B2 JP 7078104 B2 JP7078104 B2 JP 7078104B2 JP 2020504596 A JP2020504596 A JP 2020504596A JP 2020504596 A JP2020504596 A JP 2020504596A JP 7078104 B2 JP7078104 B2 JP 7078104B2
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- 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
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000019983 sodium metaphosphate Nutrition 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 235000019830 sodium polyphosphate Nutrition 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
- 239000000758 substrate Substances 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 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
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-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
- 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
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-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
- 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
-
- 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
- C01B33/16—Preparation of silica xerogels
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Silicon Polymers (AREA)
Description
本実施形態に係るエアロゲルの製造方法は、ケイ素化合物又はケイ素化合物の加水分解生成物(ケイ素化合物及び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)を含有するゾルを生成するゾル生成工程と、ゾルをゲル化して、湿潤ゲルを得る湿潤ゲル生成工程と、湿潤ゲルを乾燥してエアロゲルを得る乾燥工程と、を備える。なお、より具体的には、本実施形態に係るエアロゲルの製造方法は、乾燥工程の前工程として湿潤ゲルを洗浄する洗浄工程を更に備えることができる。
ゾル生成工程は、具体的には下記一般式(S)で表される構造を有するポリシロキサン化合物を含むゾル、あるいは当該ポリシロキサン化合物を加水分解してポリシロキサン化合物の加水分解生成物を含むゾル、を生成する工程である。このような製造方法では、特定のポリシロキサン化合物を用いることで良好な可視光透過率と強度とを両立するエアロゲルを得ることができる。なお、このような優れた効果が得られる理由を、発明者らは次のように推察する。すなわち、可視光透過率については、一般式(S)における両端の多官能ケイ素ユニットにより可視光の波長以下の径の微細孔構造が得られ易いことにより、可視光透過率を低下する要因となるミー散乱が生じ難いエアロゲルが得られているものと考えられる。また、強度については、一般式(S)における中央のジオルガノシロキサンユニットにより可撓性が担保され、また当該ユニットの両端の多官能ケイ素ユニットにより剛性が発現され、結果的に高強度のエアロゲル骨格が得られているものと考えられる。なお、一般式(S)で表される構造を有するポリシロキサン化合物を使用することにより、後述する一般式(S1)で表される構造をエアロゲルの骨格中に導入することができる。
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て、湿潤ゲルを得る工程である。より詳しくは、ケイ素化合物の加水分解生成物を得つつゾルをゲル化する、あるいはケイ素化合物の加水分解生成物を含むゾルをゲル化することで、湿潤ゲルを得る工程である。本工程は、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ってもよい。本工程では、加水分解反応及び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。
洗浄工程は、湿潤ゲル生成工程で得られた湿潤ゲルを洗浄する工程である。洗浄工程では、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溶媒置換を更に行ってもよい。
乾燥工程では、(洗浄工程を経た)湿潤ゲルを乾燥させることにより、エアロゲル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。
上記一般式(S)で表される構造を有するポリシロキサン化合物は、良好な可視光透過率と強度とを両立するエアロゲルを得るために特に有用であり、このようなポリシロキサン化合物がエアロゲル形成用の材料として従来使用された例は確認されていない。したがって、本実施形態に係るポリシロキサン化合物は、上記一般式(S)で表される構造を有する、エアロゲル形成用ポリシロキサン化合物ということができる。
本実施形態に係るエアロゲルは、上記一般式(S)で表される構造を有するポリシロキサン化合物を含有するゾルの縮合物である湿潤ゲルの乾燥物である。本実施形態に係るエアロゲルは、例えば、上記の製造方法によって得られたものであってよい。すなわち、本実施形態に係るエアロゲルは、ケイ素化合物又はケイ素化合物の加水分解生成物を含有するゾルを生成するゾル生成工程と、ゾルをゲル化して、湿潤ゲルを得る湿潤ゲル生成工程と、湿潤ゲルを乾燥してエアロゲルを得る乾燥工程と、を備え、ケイ素化合物が上記一般式(S)で表される構造を有するポリシロキサン化合物を含む、製造方法により得られるエアロゲルであってもよい。
エアロゲルブロックは、上記のエアロゲルを含むことができる。そのため、本実施形態に係るエアロゲルブロックは、非常に高い水準で可視光透過率と強度とを共に有する。
両末端9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S-1」という)を12mL、シランオリゴマー「KC-89S」(信越化学工業株式会社製、製品名)を20mL、N,N-ジメチルホルムアミドを140mL混合し、10分間撹拌した後、0.75Mに調整した水酸化テトラエチルアンモニウム水溶液6mLを加え、さらに1分間攪拌してゾルを得た。得られたゾルを80℃でゲル化し、120時間熟成して湿潤ゲルを得た。
シランオリゴマーとして、「KC-89S」に代えて「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、製品名)を用いたこと以外は、実施例1と同様にして、エアロゲルを得た。
ポリシロキサン化合物S-1を20mL、シランモノマー(メチルトリメトキシシラン)「KBM-13」(信越化学工業株式会社製、製品名)を12mL、N,N-ジメチルホルムアミドを140mL混合し、10分間撹拌した後、0.75Mに調整した水酸化テトラエチルアンモニウム水溶液6mLを加え、さらに1分間攪拌してゾルを得た。得られたゾルを80℃でゲル化し、24時間熟成して湿潤ゲルを得た。その後は実施例1と同様にして、エアロゲルを得た。
ポリシロキサン化合物S-1を16mL、シランオリゴマー「KR-500」(信越化学工業株式会社製、製品名)を16mL、N,N-ジメチルホルムアミドを140mL混合し、10分間撹拌した後、0.75Mに調整した水酸化ナトリウム水溶液6mLを加え、さらに1分間攪拌してゾルを得た。得られたゾルを80℃でゲル化し、120時間熟成して湿潤ゲルを得た。その後は実施例1と同様にして、エアロゲルを得た。
ポリシロキサン化合物S-1に代えて、両末端11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S-2」という)を用いたこと以外は、実施例1と同様にして、エアロゲルを得た。
「メチルシリケート51」、エタノール、水、及び15Nアンモニア水を、混合比が「メチルシリケート51」:エタノール:水:アンモニア水=49.56:67.06:52.97:0.25(質量比)となるように混合した。20秒程度攪拌後静置し、ゲル化させた。その後、エタノールを加え、50℃で72時間熟成し、湿潤ゲルを得た。
「メチルシリケート51」に代えて「エチルシリケート40」(コルコート株式会社製、製品名)を用いた上で、混合比を「エチルシリケート40」:エタノール:水:アンモニア水=120.18:67.06:52.97:0.25(質量比)としたこと以外は、比較例1と同様にして、エアロゲルを得た。
「XR31-B1410」を32mL、N,N-ジメチルホルムアミドを140mL混合し、10分間攪拌した後、0.75Mに調整した水酸化テトラエチルアンモニウム水溶液を6mL加え、さらに1分間攪拌してゾルを得た。得られたゾルを80℃でゲル化し、120時間熟成して湿潤ゲルを得た。その後は実施例1と同様にして、エアロゲルを得た。
各実施例及び各比較例で得られたエアロゲルについて、以下の条件に従って評価をした。結果を表1に示す。
エアロゲルの密度を、JIS K7112に記載の方法に準じてアルキメデス法により測定した。測定装置としては、電子比重計SD-200L(アルファーミラージュ株式会社製、製品名)を用いた。
エアロゲルを150mm×150mm×10mmのサイズとなるようにカットしてブロック状のエアロゲル(エアロゲルブロック)とした。面の平行を確保するために、必要に応じて#1500以上の紙やすりで整形した。整形したエアロゲルブロックを、定温乾燥機「DVS402」(ヤマト科学株式会社製、製品名)を用いて、大気圧下、100℃で30分間乾燥した後、デシケータ中に移し、25℃まで冷却して、熱伝導率測定用の測定サンプルを得た。
熱伝導率の測定は、定常法熱伝導率測定装置「HFM436Lambda」(NETZSCH社製、製品名)を用いて行った。測定条件は、大気圧下、平均温度25℃とした。測定サンプルを0.3MPaの荷重にて上部及び下部ヒーター間に挟み、温度差ΔTを20℃とし、ガードヒーターによって一次元の熱流になるように調整しながら、測定サンプルの上面温度、下面温度等を測定した。そして、測定サンプルの熱抵抗RSを次式より求めた。
RS=N((TU-TL)/Q)-RO
式中、TUは測定サンプル上面温度を示し、TLは測定サンプル下面温度を示し、ROは上下界面の接触熱抵抗を示し、Qは熱流束計出力を示す。なお、Nは比例係数であり、較正試料を用いて予め求めておいた。
得られた熱抵抗RS及び測定サンプルの厚さdより、測定サンプルの熱伝導率λを次式より求めた。
λ=d/RS
熱伝導率の測定と同様にして測定サンプルを作製した。これを3点曲げ測定用の測定サンプルとした。
測定装置としては、テンシロン万能材料試験機(引張・圧縮試験機)「RTC―1350A」(株式会社オリエンテック製、製品名)を用いた。測定モードは3点曲げとし、支点間距離を20mmとした。支点間の中央に、サンプル上面から荷重を加え、測定サンプルが破壊した点(破断点)で終了した。荷重を加える時の治具の移動速度は、0.3mm/minとし、測定温度は25℃とした。ここで、ひずみεは次式より求めた。
ε=6×s×h/L2
式中、sは破断点での変位(mm)、hは負荷をかける前の測定サンプルの厚み(mm)、Lは支点間距離(mm)を示す。
また、破断曲げ応力σ(MPa)は、次式より求めた。
σ=3×F×L/2×b×h2
式中、Fは破断点での荷重(N)を示し、bは負荷をかける前の測定サンプルの幅(mm)を示す。
そして、縦軸を応力、横軸をひずみで表した応力-ひずみ曲線において、破断点までの曲線の下側の面積を算出することにより、単位体積当りの曲げ破断エネルギー(mJ/cm3)を求めた。
サイズを20mm×25mm×10mmとしたこと以外は、熱伝導率の測定と同様にして測定サンプルを作製した。これを透過率測定用の測定サンプルとした。測定装置としては、ダブルビーム分光光度計「U-2900」(株式会社日立ハイテクノロジーズ製、商品名)を用い、20mm×25mmの面に波長550nmの光を当てて、光が10mmの距離(光路長)を透過するときの透過率(平行光線透過率)を測定した。
Claims (4)
- 前記ケイ素化合物がさらに3官能シランモノマー及びシランオリゴマーの少なくとも一種を含み、
前記3官能シランモノマーは、加水分解性の官能基又は縮合性の官能基が3個結合したケイ素原子を有し、
前記シランオリゴマーは、ケイ素原子の総数に対し、3個の酸素原子と結合したケイ素原子を50%以上有する、請求項1に記載の製造方法。
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NOGAMI Masayuki, et al.,Synthesis and characterization of transparent silica-based aerogels using methyltrimethoxysilane pre,J Sol-Gel Sci Technol,2010年07月17日,(2010)56,107-113 |
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