JP5980629B2 - 多孔質シリカ粒子の製造方法及び真空断熱材用多孔質シリカ粒子 - Google Patents
多孔質シリカ粒子の製造方法及び真空断熱材用多孔質シリカ粒子 Download PDFInfo
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- JP5980629B2 JP5980629B2 JP2012199531A JP2012199531A JP5980629B2 JP 5980629 B2 JP5980629 B2 JP 5980629B2 JP 2012199531 A JP2012199531 A JP 2012199531A JP 2012199531 A JP2012199531 A JP 2012199531A JP 5980629 B2 JP5980629 B2 JP 5980629B2
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- Prior art keywords
- porous silica
- silica particles
- aqueous solution
- alkali metal
- precipitant
- Prior art date
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- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 239000011810 insulating material Substances 0.000 title description 26
- 239000007864 aqueous solution Substances 0.000 claims description 44
- 239000002245 particle Substances 0.000 claims description 40
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims description 32
- 239000000839 emulsion Substances 0.000 claims description 23
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- 239000004094 surface-active agent Substances 0.000 claims description 17
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- 230000001376 precipitating effect Effects 0.000 claims description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 235000019353 potassium silicate Nutrition 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical group [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 5
- 239000001099 ammonium carbonate Substances 0.000 claims description 5
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
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- -1 carboxylate salt Chemical class 0.000 description 28
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- 239000011162 core material Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
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- 238000009826 distribution Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
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- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 description 2
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- 239000000499 gel Substances 0.000 description 2
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- 150000007522 mineralic acids Chemical class 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
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- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
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- 239000011734 sodium Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000005720 sucrose Substances 0.000 description 2
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- FFJCNSLCJOQHKM-CLFAGFIQSA-N (z)-1-[(z)-octadec-9-enoxy]octadec-9-ene Chemical compound CCCCCCCC\C=C/CCCCCCCCOCCCCCCCC\C=C/CCCCCCCC FFJCNSLCJOQHKM-CLFAGFIQSA-N 0.000 description 1
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- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 1
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- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
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- MUHFRORXWCGZGE-KTKRTIGZSA-N 2-hydroxyethyl (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCCO MUHFRORXWCGZGE-KTKRTIGZSA-N 0.000 description 1
- RFVNOJDQRGSOEL-UHFFFAOYSA-N 2-hydroxyethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCO RFVNOJDQRGSOEL-UHFFFAOYSA-N 0.000 description 1
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 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 1
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- 229910021529 ammonia Inorganic materials 0.000 description 1
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- Silicon Compounds (AREA)
Description
(1)ケイ酸アルカリ金属塩水溶液を、界面活性剤を含む有機溶媒中に投入して油中水滴型(W/O型)のエマルションとし、該エマルションを沈殿剤含有水溶液に投入することで、多孔質シリカ粒子を沈殿させて得る多孔質シリカ粒子の製造方法であって、前記ケイ酸アルカリ金属塩水溶液は、予め一次沈殿剤が添加されて部分ゾル化していることを特徴とする、多孔質シリカ粒子の製造方法。
(2) 前記一次沈殿剤の添加量が0.2〜0.4mol/lであり、前記沈殿剤含有水溶液の沈殿剤濃度が1.0〜2.0mol/lである、(1)に記載の多孔質シリカ粒子の製造方法。
(3)前記ケイ酸アルカリ金属塩水溶液のケイ酸濃度が0.5〜1.5mol/lである、(1)または(2)に記載の多孔質シリカ粒子の製造方法。
(4)前記ケイ酸アルカリ金属塩水溶液が水ガラスであり、前記沈殿剤が炭酸水素アンモニウムである、(1)ないし(3)のいずれかに記載の多孔質シリカ粒子の製造方法。
(5)前記エマルションを沈殿剤含有水溶液に投入した際に沈殿する沈殿物を洗浄及び乾燥して得られる、(1)ないし(4)のいずれかに記載の多孔質シリカ粒子の製造方法。
(6)(1)〜(5)のいずれかに記載の製造方法によって製造された多孔質シリカ粒子であって、真密度が0.4g/cm3以下である、真空断熱材用多孔質シリカ粒子。
(7)粒径が0.5〜30μmの範囲にある、(6)に記載の真空断熱材用多孔質シリカ粒子。
(8)非通気性の包装フィルムによって真空パックした際のパック密度が0.1〜0.25g/cm3であり、熱伝導率が4.5〜6.0mW/mKである、(6)または(7)に記載の真空断熱材用多孔質シリカ粒子。
ケイ酸アルカリ水溶液:水ガラス(SiO2/Na2Oモル比;2.1)
有機溶媒:n−ヘキサン
界面活性剤:トリオレイン酸ポリオキシエチレンソルビタン
一次・二次沈殿剤:炭酸水素アンモニウム
走査電子顕微鏡観察を行い、視野90×60μで測定した。
JIS R 1628に基づき求めた。具体的には、パウダーテスターを用い、600回タップを行い、100ml容器に入る試料の重さの変化が0.3%以下となったときの密度。
JIS R 1626に基づき、窒素の吸着等温線から求めた。具体的には、相対圧力0.1〜0.3における窒素の吸着量の傾きから求めた。
JIS Z 1831−2に基づき求めた。具体的には、窒素吸着法により相対圧力4×10−6から1まで変化させて細孔分布曲線を得たうえで、当該細孔分布から平均細孔径を求めた。
窒素吸着法により相対圧力4×10−6から1まで変化させて細孔分布曲線を得たうえで、当該細孔分布曲線から細孔容積を得る。そして、当該細孔容積の逆数を真密度とした。
粒子をラミネートフィルム中に真空パックした際の、フィルム分を除いた重量と体積から求めた。
ISO8302とJIS A 1412−1に基づき、保護熱板法により25℃における熱伝導率を測定した。
Claims (5)
- ケイ酸アルカリ金属塩水溶液を、界面活性剤を含む有機溶媒中に投入して油中水滴型のエマルションとし、該エマルションを沈殿剤含有水溶液に投入することで、多孔質シリカ粒子を沈殿させて得る多孔質シリカ粒子の製造方法であって、
前記ケイ酸アルカリ金属塩水溶液は、予め一次沈殿剤が添加されて部分ゾル化していることを特徴とする、多孔質シリカ粒子の製造方法。 - 前記一次沈殿剤の添加量が0.2〜0.4mol/lであり、
前記沈殿剤含有水溶液の沈殿剤濃度が1.0〜2.0mol/lである、請求項1に記載の多孔質シリカ粒子の製造方法。 - 前記ケイ酸アルカリ金属塩水溶液のケイ酸濃度が0.5〜1.5mol/lである、請求項1または請求項2に記載の多孔質シリカ粒子の製造方法。
- 前記ケイ酸アルカリ金属塩水溶液が水ガラスであり、
前記沈殿剤が炭酸水素アンモニウムである、請求項1ないし請求項3のいずれかに記載の多孔質シリカ粒子の製造方法。 - 前記エマルションを沈殿剤含有水溶液に投入した際に沈殿する沈殿物を洗浄及び乾燥して得られる、請求項1ないし請求項4のいずれかに記載の多孔質シリカ粒子の製造方法。
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