JP5498377B2 - シリカ粒子及びその製造方法並びにその使用方法 - Google Patents

シリカ粒子及びその製造方法並びにその使用方法 Download PDF

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JP5498377B2
JP5498377B2 JP2010511186A JP2010511186A JP5498377B2 JP 5498377 B2 JP5498377 B2 JP 5498377B2 JP 2010511186 A JP2010511186 A JP 2010511186A JP 2010511186 A JP2010511186 A JP 2010511186A JP 5498377 B2 JP5498377 B2 JP 5498377B2
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particles
silica particles
silica
particle
porous silica
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JP2010531798A (ja
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プライア，ジェームズ・ニール
キンツ，ロレンス
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オールテック・アソシエイツ・インコーポレーテッド
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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
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/124—Preparation of adsorbing porous silica not in gel form and not finely divided, i.e. silicon skeletons, by acidic treatment of siliceous materials
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • B01J20/28019—Spherical, ellipsoidal or cylindrical
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/282—Porous sorbents
    • B01J20/283—Porous sorbents based on silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3291—Characterised by the shape of the carrier, the coating or the obtained coated product
    • B01J20/3293—Coatings on a core, the core being particle or fiber shaped, e.g. encapsulated particles, coated fibers
    • 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
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/145—Preparation of hydroorganosols, organosols or dispersions in an organic medium
    • 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
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/146—After-treatment of sols
    • C01B33/148—Concentration; Drying; Dehydration; Stabilisation; Purification
    • 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
    • C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Silicon Compounds (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Cosmetics (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
JP2010511186A 2007-06-04 2008-06-04 シリカ粒子及びその製造方法並びにその使用方法 Expired - Fee Related JP5498377B2 (ja)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US93306907P 2007-06-04 2007-06-04
US60/933,069 2007-06-04
PCT/US2008/007034 WO2008150537A2 (en) 2007-06-04 2008-06-04 Silica particles and methods of making and using the same

Publications (2)

Publication Number Publication Date
JP2010531798A JP2010531798A (ja) 2010-09-30
JP5498377B2 true JP5498377B2 (ja) 2014-05-21

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JP2010511186A Expired - Fee Related JP5498377B2 (ja) 2007-06-04 2008-06-04 シリカ粒子及びその製造方法並びにその使用方法

Country Status (12)

Country Link
US (1) US20100116743A1 (enExample)
EP (1) EP2167425A2 (enExample)
JP (1) JP5498377B2 (enExample)
KR (1) KR20100022499A (enExample)
CN (1) CN101918312A (enExample)
AR (1) AR066853A1 (enExample)
AU (1) AU2008260452A1 (enExample)
CA (1) CA2690537A1 (enExample)
IN (1) IN2009DN08217A (enExample)
MX (1) MX2009013170A (enExample)
TW (1) TW200914372A (enExample)
WO (1) WO2008150537A2 (enExample)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101411007B1 (ko) * 2010-12-31 2014-06-23 제일모직주식회사 방현 필름용 조성물 및 이를 포함하는 방현 필름
CN102380345B (zh) * 2011-08-03 2013-01-16 济南大学 孔呈梯度分布的中空二氧化硅微球及其制备方法和应用
GB2497105B (en) * 2011-12-01 2014-07-23 Thermo Electron Mfg Ltd Process for the preparation of porous silica particles
CA2885263C (en) 2012-09-17 2021-11-16 W. R. Grace & Co.-Conn. Chromatography media and devices
CN107847907A (zh) 2014-05-02 2018-03-27 格雷斯公司 官能化载体材料以及制备和使用官能化载体材料的方法
BR112017026193B1 (pt) 2015-06-05 2021-09-14 W.R. Grace & Co-Conn Adsorventes, método de produção dos adsorventes e uso dos adsorventes
US20180238842A1 (en) * 2015-08-25 2018-08-23 Showa Denko K.K. Liquid chromatographic column and liquid chromatographic apparatus including the same
AU2018262708B2 (en) 2017-05-04 2021-06-03 Nanologica Ab A process for manufacturing porous silica particles loaded with at least one bioactive compound adapted for lung, nasal, sublingual and/or pharyngeal delivery
US10661250B2 (en) * 2018-04-13 2020-05-26 Agilent Technologies, Inc. Synthetic silica as packing material in supported liquid extraction
KR102427987B1 (ko) * 2018-11-27 2022-08-02 주식회사 엘지화학 전가수분해된 폴리실리케이트의 합성방법
GB201916122D0 (en) 2019-11-06 2019-12-18 Nanologica Ab New compositions
JP2025508226A (ja) * 2022-03-16 2025-03-21 ダブリュー・アール・グレース・アンド・カンパニー－コーン 多孔質の球状シリカゲル粒子を生産する方法
US20240018006A1 (en) * 2022-07-13 2024-01-18 Uchicago Argonne, Llc Method For Producing Porous Nanocrystalline Silicon

Family Cites Families (29)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1473239A (enExample) * 1966-01-31 1967-05-29
US3591518A (en) * 1968-12-31 1971-07-06 Du Pont Silica aquasols and powders
SE417431B (sv) * 1975-12-12 1981-03-16 Pharmacia Fine Chemicals Ab Dextranderivatgel for elektroforetisk separation
US4160728A (en) * 1976-12-08 1979-07-10 E. I. Du Pont De Nemours And Company Bimodal chromatographic resolving zone
US4301034A (en) * 1980-05-21 1981-11-17 Phillips Petroleum Company Silica from single phase controlled hydrolysis of silicate ester
DE3616133A1 (de) * 1985-09-25 1987-11-19 Merck Patent Gmbh Kugelfoermige sio(pfeil abwaerts)2(pfeil abwaerts)-partikel
US4943425A (en) * 1988-04-01 1990-07-24 Gte Laboratories Incorporated Method of making high purity dense silica of large particle size
US5023208A (en) * 1989-12-19 1991-06-11 Orion Laboratories, Inc. Sol-gel process for glass and ceramic articles
IT1240673B (it) * 1990-04-24 1993-12-17 Tenav Microsfere di aerogels di ossidi inorganici a stretta distribuzione dei diametri dei pori e metodo per la loro preparazione
US5409683A (en) * 1990-08-23 1995-04-25 Regents Of The University Of California Method for producing metal oxide aerogels
WO1992003378A1 (en) * 1990-08-23 1992-03-05 United States Department Of Energy A METHOD FOR PRODUCING METAL OXIDE AEROGELS HAVING DENSITIES LESS THAN 0.02 g/cm?3¿
US5425930A (en) * 1993-09-17 1995-06-20 Alliedsignal Inc. Process for forming large silica spheres by low temperature nucleation
IT1266660B1 (it) * 1993-11-04 1997-01-09 Eniricerche Spa Procedimento per la preparazione di xerogels di silice porosi in forma sferica
JP2580537B2 (ja) * 1994-06-27 1997-02-12 工業技術院長 シリカ球状粒子からなる三次元網状構造体
US5728457A (en) * 1994-09-30 1998-03-17 Cornell Research Foundation, Inc. Porous polymeric material with gradients
US6290735B1 (en) * 1997-10-31 2001-09-18 Nanogram Corporation Abrasive particles for surface polishing
GB2355711B (en) * 1999-10-27 2003-12-24 Agilent Technologies Inc Porous silica microsphere scavengers
US6569908B2 (en) * 2000-01-19 2003-05-27 Oji Paper Co., Ltd. Dispersion of silica particle agglomerates and process for producing the same
US7250214B2 (en) * 2001-08-09 2007-07-31 Waters Investments Limited Porous inorganic/organic hybrid monolith materials for chromatographic separations and process for their preparation
ES2610590T3 (es) * 2001-08-13 2017-04-28 Rhodia Chimie Procedimiento de preparación de sílices con distribución granulométrica y/o reparto de poros particulares
CN1227157C (zh) * 2001-09-25 2005-11-16 三菱化学株式会社 硅石
US20040091411A1 (en) * 2002-11-08 2004-05-13 Bijan Modrek-Najafabadi High surface area, high porosity silica packing with narrow particle and pore diameter distribution and methods of making same
JP2005154195A (ja) * 2003-11-25 2005-06-16 Matsushita Electric Works Ltd エアロゲル材、及びこのエアロゲル材にて形成される物品
US20060169640A1 (en) * 2005-02-01 2006-08-03 Hubert Quinn High throughput screening, purification and recovery system for large and small molecules
US7468130B2 (en) * 2005-02-15 2008-12-23 Dionex Corporation Organosilanes and substrates covalently bonded with same and methods for synthesis and use same
PT103257B (pt) * 2005-04-05 2007-05-31 Inst Superior Tecnico Método de produção subcrítica de xerogéis e aerogéis monolíticos híbridos de sílica e látex modificado com grupos alcoxissilano
SG131016A1 (en) * 2005-09-19 2007-04-26 Millipore Corp Asymmetric porous adsorptive bead
WO2007095158A2 (en) * 2006-02-13 2007-08-23 Advanced Materials Technology, Inc. Process for preparing substrates with porous surface
CN100396612C (zh) * 2006-09-15 2008-06-25 南开大学 纳米球形介孔二氧化硅材料和制备方法

Also Published As

Publication number Publication date
WO2008150537A3 (en) 2010-08-12
CN101918312A (zh) 2010-12-15
EP2167425A2 (en) 2010-03-31
JP2010531798A (ja) 2010-09-30
CA2690537A1 (en) 2008-12-11
AU2008260452A1 (en) 2008-12-11
TW200914372A (en) 2009-04-01
MX2009013170A (es) 2010-03-01
WO2008150537A2 (en) 2008-12-11
US20100116743A1 (en) 2010-05-13
IN2009DN08217A (enExample) 2015-07-24
KR20100022499A (ko) 2010-03-02
AR066853A1 (es) 2009-09-16

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