JP5275156B2 - 複合化粒子の製造方法 - Google Patents
複合化粒子の製造方法 Download PDFInfo
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- JP5275156B2 JP5275156B2 JP2009155156A JP2009155156A JP5275156B2 JP 5275156 B2 JP5275156 B2 JP 5275156B2 JP 2009155156 A JP2009155156 A JP 2009155156A JP 2009155156 A JP2009155156 A JP 2009155156A JP 5275156 B2 JP5275156 B2 JP 5275156B2
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- carbon dioxide
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- 239000010456 wollastonite Substances 0.000 description 2
- 229910052882 wollastonite Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 239000011667 zinc carbonate Substances 0.000 description 2
- 229910000010 zinc carbonate Inorganic materials 0.000 description 2
- 235000004416 zinc carbonate Nutrition 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- UGGQKDBXXFIWJD-UHFFFAOYSA-N calcium;dihydroxy(oxo)silane;hydrate Chemical compound O.[Ca].O[Si](O)=O UGGQKDBXXFIWJD-UHFFFAOYSA-N 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 150000001923 cyclic compounds Chemical class 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
Classifications
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Cosmetics (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Description
工程(1):被覆用微粒子、有機溶剤及び母粒子を乾式混合して混合物を得る工程、
工程(2):当該混合物が入った耐圧容器内に二酸化炭素を注入し、超臨界又は亜臨界条件において被覆用微粒子と母粒子とを複合化する工程、及び
工程(3):当該耐圧容器から有機溶剤と二酸化炭素を除去する工程、を含む複合化粒子の製造方法、に関するものである。
(1)ケトン類、例えば、アセトン、メチルエチルケトン等。
(2)エステル類、例えば、酢酸エチル等。
(3)アルコール類、例えば、エタノール、メタノール、イソプロパノール等。
(4)飽和脂肪族類、例えば、ヘキサン、ヘプタン等。
(5)環状化合物類、例えば、シクロヘキサン等。
(6)芳香族類、例えば、ベンゼン、トルエン等。
パウダテスタPT−R(ホソカワミクロン)により常温(25℃)、常圧(1013.25hPa)の条件下で、粒子の見掛け比重(固め)HK(g/mL)を測定する。また、乾式密度計「アキュピック1330」(島津製作所製)により粒子の真密度H0(g/mL)を測定する。使用した粒子の重量W(g)から、W/HK−W/H0により粒子充填層の空隙体積(mL)を算出することができる。
試料をSEMで観察し、使用した母粒子、被覆用微粒子及び複合化粒子の算術平均での平均粒径を求める。また処理後のサンプルを観察し、複合化粒子における被覆用微粒子の被覆状態、及び被覆用微粒子単独の凝集体の有無、及び母粒子又は複合化粒子の凝集体の有無を評価する。
図1に示される装置を用いて複合化粒子を以下の手順にて製造した。
被覆用微粒子としての球状のシリカ微粒子〔日本触媒(株)製、商品名:シーホスターKE−P30、平均粒径:0.3μm〕1.8gと、有機溶剤としてのエタノール9.0mLを混合して、シリカ微粒子含有液(以下、シリカ/エタノール含有液と略す)を作製した。
シリカ微粒子1.8gとエタノール12mLを使用してシリカ/エタノール含有液を作製し、該シリカ/エタノール含有液8.0mLと、PMMA粒子20.0gを用いてスーパーミキサーにより乾式混合した以外は実施例1と同様にして混合を行った。
シリカ微粒子2.7gとエタノール45mLを使用してシリカ/エタノール分散液を作製し、該シリカ/エタノール分散液20mLと、PMMA粒子20.0gを用いてスーパーミキサーにより混合した以外は、実施例1と同様にして混合を行った。
エタノールの排出を行う保持時間を5分間から20分間に変更した以外は、比較例1と同様にして複合化粒子を得た。複合化に用いた二酸化炭素量は100mLであると求められた。
被覆用微粒子としての球状のシリカ微粒子〔日本触媒(株)製、商品名:シーホスターKE−P30、平均粒径:0.3μm〕1.8gと、有機溶剤としてのエタノール9.0mLを混合して、シリカ/エタノール含有液を作製した。
2 フィルター
3 コンデンサー
4 昇圧ポンプ
5 クーラー
6a 圧力計
6b 圧力計
7 安全弁
8 安全弁
9 攪拌子
10 オートクレーブ
11 温度計
12 カートリッジヒーター
13 温度調節器
14 マグネチックスターラー
15 排気ライン
16 バグフィルター
17 複合化粒子
18 有機溶剤
19 ノズル
20 回収容器
21 排気ライン
V−1 保圧弁
V−2 バルブ
V−3 排気バルブ
V−4 排気バルブ
Claims (3)
- 工程(1):被覆用微粒子、有機溶剤及び母粒子を乾式混合して混合物を得る工程、
工程(2):該混合物が入った耐圧容器内に二酸化炭素を注入し、超臨界又は亜臨界条件において被覆用微粒子と母粒子とを複合化する工程、及び
工程(3):該耐圧容器から有機溶剤と二酸化炭素を除去する工程、
を含む複合化粒子の製造方法であって、該被覆用微粒子が無機微粒子である、複合化粒子の製造方法。 - 被覆用微粒子を含有する有機溶剤の室温(25℃)、常圧(1013.25hPa)における体積が、室温、常圧における母粒子充填層の空隙体積未満である、請求項1に記載の製造方法。
- 工程(3)を工程(2)と並行して行う、請求項1又は2に記載の製造方法。
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JP5275156B2 true JP5275156B2 (ja) | 2013-08-28 |
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JPH11197494A (ja) * | 1998-01-13 | 1999-07-27 | Kenji Mishima | 超臨界流体を用いた微小粒子コーティング |
JP3457655B2 (ja) * | 2000-10-10 | 2003-10-20 | 花王株式会社 | 複合化粒子の製造法 |
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