KR950023442A - Airgel manufacturing method and high pressure extraction tank used in the manufacturing method - Google Patents

Airgel manufacturing method and high pressure extraction tank used in the manufacturing method Download PDF

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KR950023442A
KR950023442A KR1019940000388A KR19940000388A KR950023442A KR 950023442 A KR950023442 A KR 950023442A KR 1019940000388 A KR1019940000388 A KR 1019940000388A KR 19940000388 A KR19940000388 A KR 19940000388A KR 950023442 A KR950023442 A KR 950023442A
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airgel
producing
extraction tank
high pressure
pressure extraction
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KR1019940000388A
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KR0130181B1 (en
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유기풍
이건흥
김선영
남기동
김보찬
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남석우
대흥상공 주식회사
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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
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/08—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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

본 발명은 소수성 에어로젤의 제조방법 및 이 제조방법에 사용되는 고압추출조에 관한 것으로 보다 상세하게는 금속알콕사이드를 원료로 사용하고 솔-젤법과 초임계 건조법에 의하여 광투광성이 우수한 에어로젤을 제조하는 방법 및 이 제조방법에 사용되는 고압 추출조와 표면 처리법에 의하여 친수성을 소수성으로 바꾸는 방법에 관한 것이다.The present invention relates to a method for preparing a hydrophobic airgel and a high pressure extraction tank used in the method, and more particularly, a method for producing an airgel having excellent light transmittance by using a metal alkoxide as a raw material, and a sol-gel method and a supercritical drying method. It relates to a method of changing the hydrophilicity to hydrophobic by the high pressure extraction tank and the surface treatment method used in this manufacturing method.

Description

에어로젤의 제조방법 및 이 제조방법에 사용되는 고압추출조Airgel manufacturing method and high pressure extraction tank used in the manufacturing method

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

제1도는 종래의 에어로젤의 제조방법을 나타낸 공정도.1 is a process chart showing a conventional method for manufacturing an airgel.

제2도는 본 발명의 에어로젤의 제조방법을 나타낸 공정도.2 is a process chart showing a method for manufacturing an airgel of the present invention.

제3도는 본 발명의 고압 추출조를 보인 구조도.3 is a structural diagram showing a high pressure extraction tank of the present invention.

제4도는 본 발명의 표면처리 장치를 보인 개략도.4 is a schematic view showing a surface treatment apparatus of the present invention.

Claims (18)

단열재, 흡착제 또는 촉매의 담체로 이용되는 에어로젤의 제조방법에 있어서, 금속알콜사이드류 또는 이것의 혼합물을 증류수와 혼합시키고 산촉매를 첨가하여 가수분해 반응 및 축합반응을 수행함으로써 올리고머를 합성하는 단계 ; 상기 올리고머에 증류수와 비알코올계 희석제를 혼합하고 촉매로서 알카리를 첨가한 다음 주형에 붓고 밀봉시켜서 습윤젤을 제조하는 단계 ; 상기 습윤젤을 고압추출조에 넣고 밀봉시킨다음, 추출용매를 사용하여 희석제 및 반응에 의해 생성된 알코올을 추출하는 단계; 고압 추출조의 온도와 압력을 증가시켜서 추출용매의 임계점을 우회한후 온도를 유지시키며 상압으로 감암시킴으로써 에어로젤을 제조하는 초임계 건조단계 ; 고압추출조를 개방시키고 친수성 에어로젤을 표면처리장치에 넣은 다음, 알코올 증기과 반응시켜서 에어로젤의 표면을 소수성으로 변화시키는 기상 표면 처리단계 ; 로 이루어지는 에어로젤의 제조방법.A method for producing an airgel used as a carrier of a heat insulating material, an adsorbent or a catalyst, the method comprising: synthesizing an oligomer by mixing metal alcohols or a mixture thereof with distilled water and adding an acid catalyst to carry out a hydrolysis reaction and a condensation reaction; Preparing a wet gel by mixing distilled water and a non-alcoholic diluent to the oligomer, adding alkali as a catalyst, and then pouring and sealing the mold; Putting the wet gel into a high pressure extraction tank and sealing the same, extracting a diluent and an alcohol produced by the reaction using an extraction solvent; A supercritical drying step of manufacturing an airgel by increasing the temperature and pressure of the high pressure extraction tank to bypass the critical point of the extraction solvent and maintaining the temperature and reducing the pressure to atmospheric pressure; A gas phase surface treatment step of opening the high pressure extraction tank and placing a hydrophilic airgel into the surface treatment apparatus and reacting with alcohol vapor to change the surface of the airgel into hydrophobic; Method for producing an airgel consisting of. 제1항에 있어서, 증류시키지 않은 저순도의 원료를 직접 사요아는 에어로젤의 제조방법.The method for producing an airgel according to claim 1, wherein the raw material of low purity that is not distilled is directly used. 제1항에 있어서, 알코올을 첨가하지 않은 상태로 올리고머를 제조하는 에어로젤의 제조방법.The method for producing an airgel according to claim 1, wherein the oligomer is prepared without adding alcohol. 제1항에 있어서, 금속 알콕사이드로 실리콘 알콕사이드를 사용하는 에어로젤의 제조방법.The method for producing an airgel according to claim 1, wherein silicon alkoxide is used as the metal alkoxide. 제1항에 있어서, 신촉매로 염산, 황산, 질산 및 초산을 사용하는 에어로젤의 제조방법.The method of producing an airgel according to claim 1, wherein hydrochloric acid, sulfuric acid, nitric acid and acetic acid are used as the new catalyst. 제1항에 있어서, 희석제로 아세토니트릴, 아세톤, 에테르 및 톨루엔을 사용하는 에어로젤의 제조방법.2. The process of claim 1 wherein acetonitrile, acetone, ether and toluene are used as diluents. 제1항에 있어서, 알카리 촉매로 암모니아 및 수산화암모늄, 수산화 나트륨 및 수산화 칼륨을 사용하는 에어로젤의 제조방법.The method for producing an airgel according to claim 1, wherein ammonia and ammonium hydroxide, sodium hydroxide and potassium hydroxide are used as the alkali catalyst. 제1항에 있어서, 저온 초임계 건조 공정에 의한 친수성 에어로젤의 제조방법.The method of claim 1, wherein the hydrophilic airgel is prepared by a low temperature supercritical drying process. 제8항에 있어서, 추출제로서 액체 이산화탄소를 사용하는 에어로젤의 제조방법.The method for producing an airgel according to claim 8, wherein liquid carbon dioxide is used as an extractant. 제8항에 있어서, 습윤젤내의 용매를 다른 용매로 치환하지 않고 직접 액체 이산화탄소로 추출하는 에어로젤의 제조방법.The method of claim 8, wherein the solvent in the wet gel is directly extracted with liquid carbon dioxide without substitution with another solvent. 제8항에 있어서, 고압추출조를 알코올, 희석제 및 질소등으로 채우지 않고 직접 액체 이산화탄소를 투입하는 에어로젤의 제조방법.The method of claim 8, wherein the liquid carbon dioxide is directly added without filling the high pressure extraction tank with alcohol, diluent, nitrogen, or the like. 제8항에 있어서, 순수한 이산화탄소가 희석제, 알코올 그리고 이산화탄소의 혼합물과 완전히 섞이지 않는 상태에서 추출되는 에어로젤의 제조방법.The method of claim 8, wherein the pure carbon dioxide is extracted in a state where it is not completely mixed with a mixture of diluent, alcohol and carbon dioxide. 제1항에 있어서, 기상표면처리단계에서 캐리어 가스를 사용하지 않고 미반응물을 응축 재순환 시키며 표면처리한 소수성 에어로젤의 제조방법.The method for preparing a hydrophobic airgel according to claim 1, wherein the unreacted material is condensed and recycled without using a carrier gas in the gas phase surface treatment step. 제13항에 있어서, 환류장치를 이용하며 장치의 중간부분을 나선형으로 감아올리고, 기체를 이곳으로 통과시키며 기체의 온도조절을 하는 에어로젤의 제조방법.15. The method of claim 13, wherein the reflux device is used to spirally wind the middle portion of the device, the gas is passed therethrough, and the temperature of the gas is controlled. 제1항에 있어서, 기상표면처리 기체로 메탄올 및 에탄올을 사용하는 에어로젤의 제조방법.The method for producing an airgel according to claim 1, wherein methanol and ethanol are used as the gaseous surface treatment gas. 양쪽에 투시창이 달리고, 추출제의 투입구는 상부에, 방출구는 하부에 구비되어 에어로젤의 제조방법에 사용되는 고압추출조.High-pressure extraction tank used in the manufacturing method of the airgel is provided with a viewing window on both sides, the inlet of the extractant is provided at the top, the outlet is at the bottom. 제16항에 있어서, 상부로 순수한 이산화탄소가 유입되고 하부로 희석제 및 알콜과 섞인 이산화탄소가 추출되는 고압추출조.The high pressure extraction tank according to claim 16, wherein pure carbon dioxide is introduced into the upper portion and carbon dioxide mixed with the diluent and the alcohol is extracted into the lower portion. 제16항에 있어서, 투시창으로 강화유리, 유정유리 및 사파이어 유리를 사용한 고압추출조.The high pressure extraction tank according to claim 16, wherein tempered glass, oil glass, and sapphire glass are used as the sight glass. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019940000388A 1994-01-10 1994-01-10 Manufacturing mehtod of aerogel KR0130181B1 (en)

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