KR960701693A - 화학적인 표면변형에 의한 고 다공성 크세로겔의 제조방법(preparation of high porosity xerogels by chemical surface modification) - Google Patents

화학적인 표면변형에 의한 고 다공성 크세로겔의 제조방법(preparation of high porosity xerogels by chemical surface modification)

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KR960701693A
KR960701693A KR1019950704773A KR19950704773A KR960701693A KR 960701693 A KR960701693 A KR 960701693A KR 1019950704773 A KR1019950704773 A KR 1019950704773A KR 19950704773 A KR19950704773 A KR 19950704773A KR 960701693 A KR960701693 A KR 960701693A
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gel
wet gel
wet
solvent
group
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KR1019950704773A
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KR0158053B1 (ko
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데쉬판데 라빈드라
엠 스미스 더글라스
씨 브링커 제프리
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아나벨 퀸타나
유니버시티 오브 뉴 멕시코
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    • 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
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091—Preparation of aerogels, e.g. xerogels
    • 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
    • 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
    • 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.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
    • Y10T428/2995—Silane, siloxane or silicone coating

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicon Compounds (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

본 발명은 진공 내 하부-임계 압력에서 건조되었으나 초임계 압력에서 통상 건조된 에어로겔의 특성을 갖는 매우 다공성인 세로겔에 관한 것으로서, 상기 습윤 겔(예를들면 알콕시드 유래의 실리카겔)의 내부 기공 표면을 유기 표면 변형제(예를들면 벤젠내 트리메틸클로로-실란)와 반응시켜서 건조중에 기공의 유체 메니스커스의 접촉각을 변화시키고, 진공 또는 주위 압력에서 겔의 수축(통상 높은 오토클레이브 압력을 사용함으로써 피해져서 기공 유체가 임계값 이상의 온도 및 압력에서 존재함)을 피하게 하며, 제4도는 본 발명에 따라 변형되고 주위 압력 겔 처리된 것의 건조 중 시료 증량 및 시료 길이의 변화를 나타낸 것으로서, 건조의첫번째 단계중에 겔의 팽창에 의하여 최초의 수축이 발생하는 것을 묘사하고 있고, 상당히 낮은 밀도의 미세한 기공 겔 생성물은 유용한 절연성 및 기타 다른 특성을 가지고 있음을 특징으로 한다.

Description

화학적인 표면변형에 의한 고 다공성 크세로겔의 제조방법 (PREPARATION OF HIGH POROSITY XEROGELS BY CHEMICAL SURFACE MODIFICATION)
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
제4도는 본 발명에 따라 처리된 표면 변형되고 주위 압력하 겔의 건조중에 시료 중량과 시료 길이의 변화를 나타내는 그래프로서 최종 건조 단계중에 겔의 팽창에 의한 최초의 수축을 나타낸다.

Claims (13)

  1. 하기 단계로 구성된 것을 특징으로 하는 대략 0.6 이상의 기공도를 갖는 건조 크세로겔의 제조방법.
    a)기공 유체 접촉각이 O이며 표면종이 실질적인 수의 원자를 갖는 습윤 상태의 겔의 제조, b)습윤 겔을 표면 변형제와 반응시켜서 실질적인 수의 표면종을 기공 유체 접촉각 0을 실질적으로 증가시키는 다른 종과 교환, c)진공 내지 하부 임계점 범위내에서 선택되는 적어도 하나의 압력에서 습윤겔의 건조.
  2. 제1항에 있어서, 상기 습윤겔이 물을 함유하며 상기 단계 a)가 습윤겔로부터 실질적으로 모든 물을 제거하는 추가의 단계를 포함해서 습윤생태의 습윤겔이 물을 거의 포함하지 않게 하는 것을 특징으로 하는 방법.
  3. 제1항에 있어서, 상기 단계 a)가 소정기간동안 상승 온도에서 습윤겔을 경화시키는 것을 추가로 포함하는 것을 특징으로 하는 방법.
  4. 제3항에 있어서, 상기 상승된 온도가 주위온도 내지 습윤겔내 유체의 대략 끓는점 까지의 범위내인 것을 특징으로 하는 방법.
  5. 제3항에 있어서, 상기 단계 a)가 또한 경화 후, 양성지성 용매와 비양성자성 용매의 군으로부터 선택된 용매로 습윤겔을 세척하는 것을 포함하는 것을 특징으로 하는 방법.
  6. 제1항에 있어서, 상기 단계 a)가습윤겔내 유체의 끓는점까지 올린 온도에서 습윤겔을 경화시키고 양성자성 용매 및 비양성자성 용매의 군으로부터 선택된 용매내에서 상기 습윤겔을 세척하여 습윤겔로부터 실질적으로 모든 물을 제거하는 것을 특징으로 하는 방법.
  7. 제1항에 있어서, 상기 단계 b)가 또한 선택된 용매내에서 습윤겔을 오르가노실릴화시키는 것을 포함하는 것을 특징으로 하는 방법.
  8. 제7항에 있어서. 상기 선택된 용매가 유기 용매인 것을 특징으로 하는 방법.
  9. 제1항에 있어서, 상기 반응 단계가 또한 비반응의 표면 변형제를 양성자성 용매 및 비양성자성 용매의 군으로부터 선택된 용매로 제거시키는 것을 특징으로 하는 방법.
  10. 제1항에 있어서, 상기 겔이 테트라에틸오르토실리케이트(TEOS) 용액으로부터 제조된 금속 산화 겔인 것을 특징으로 하는 방법.
  11. 제1항에 있어서, 상기 겔이 콜로이드성 실리카 및 미립자 실리카의 군으로부터 선택된 실리카로 제조된 금속 산화 겔인 것을 특징으로 하는 방법.
  12. 제1항에 있어서, 상기 겔이 알콕시드와 미립자겔 및 알콕시드와 미립자겔의 배합에서 상기 군으로부터 선택된 물질로부터 제조된 금속 산화 겔인 것을 특징으로 하는 방법.
  13. 제1항에 있어서, 상기 겔의 추가 중량 손실이 없을때까지 진공 내지 하부-임계 압력 범위 및 주위 온도 내지 습윤 겔내 유체의 끓는점의 온도 범위에서 건조단계가 수행되는 것을 특징으로 하는 방법.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019950704773A 1993-04-28 1994-04-28 화학적인 표면변형에 의한 고 다공성 크세로겔의 제조방법 KR0158053B1 (ko)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US08/055,069 US5565142A (en) 1992-04-01 1993-04-28 Preparation of high porosity xerogels by chemical surface modification.
US08/055,069 1993-04-28
US8/055069 1993-04-28
PCT/US1994/005105 WO1994025149A1 (en) 1993-04-28 1994-04-28 Preparation of high porosity xerogels by chemical surface modification

Publications (2)

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KR960701693A true KR960701693A (ko) 1996-03-28
KR0158053B1 KR0158053B1 (ko) 1998-11-16

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US (1) US5565142A (ko)
EP (1) EP0707518B1 (ko)
JP (1) JP2840881B2 (ko)
KR (1) KR0158053B1 (ko)
AT (1) ATE193980T1 (ko)
BR (1) BR9406431A (ko)
CA (1) CA2160993A1 (ko)
DE (1) DE69424995T2 (ko)
NO (1) NO954274L (ko)
WO (1) WO1994025149A1 (ko)

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US5565142A (en) 1996-10-15
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EP0707518B1 (en) 2000-06-21
DE69424995D1 (de) 2000-07-27
KR0158053B1 (ko) 1998-11-16
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