KR20130139461A - Pure Graphene Mass Production Method II - Google Patents
Pure Graphene Mass Production Method II Download PDFInfo
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- KR20130139461A KR20130139461A KR1020120062463A KR20120062463A KR20130139461A KR 20130139461 A KR20130139461 A KR 20130139461A KR 1020120062463 A KR1020120062463 A KR 1020120062463A KR 20120062463 A KR20120062463 A KR 20120062463A KR 20130139461 A KR20130139461 A KR 20130139461A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/06—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a liquid medium
- B01J2/08—Gelation of a colloidal solution
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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Abstract
Description
본 발명은 1. 금속성분 및 황.회분.수소.질소.산소와 습도 등을 제거하여 구성한 96%∼99.9% 탄소로 구성된 천연흑연 알갱이나 합성흑연 알갱이를 볼 밀에 넣고 미세분쇄하여 구성한 96%∼99.9% 탄소로 구성된 흑연분말(천연.합성)이나 흑연입자(천연.합성)에 2. 요오드(I2) 또는 이산화탄소(CO2) 수소(H2) 산소(O2). 일산화탄소(CO). 질소(N2) 헬륨(He) 네온(Ne). 아르곤(Ar) 크립톤(Kr) 제논(Xe) 플로린(F) 클로린(cl) 기체중에서 1가지 이상의 기체를 선택한 기체(A)를 250℃∼400℃로 열처리하여 (A)기체를 도핑한 흑연분말 및 흑연입자로 구성한 후 3. 용매인 NMP나 DMF 또는 알코올 물 중에서 선택한 용매에 넣고 막대로 젓거나 또는 초음파 처리하면 (A)기체를 도핑한 흑연분말 및 흑연입자는 기체에 의해 그래핀이 층간격이 생기면서 그래핀이 개별시트로 분리 분산하여서 그래핀 겔로 구성되는데 4. 그래핀 겔을 원심분리기를 이용하거나 120℃∼180℃로 열처리하여 용매를 제거하여서 순수 그래핀을 다량 얻을수 있도록 구성한 순수 그래핀 다량 제조 방법(A)에 관한 것이다The present invention is a 96% composition consisting of finely pulverized natural graphite grains or synthetic graphite grains composed of 96% to 99.9% carbon formed by removing metal components, sulfur, ash, hydrogen, nitrogen, oxygen and humidity, etc., into a ball mill. 2. Graphite powder (natural or synthetic) or graphite particles (natural or synthetic) composed of -99.9% carbon. 2. Iodine (I 2 ) or carbon dioxide (CO 2 ) hydrogen (H 2 ) oxygen (O 2 ). Carbon monoxide (CO). Nitrogen (N 2 ) Helium (He) Neon (Ne). Argon (Ar) Krypton (Kr) Xenon (Xe) Florin (F) Graphene powder doped with gas (A) by heat-treating the gas (A) selected from one or more gases from 250 to 400 ° C And graphite particles. 3. After stirring in a solvent selected from NMP, DMF or alcohol water, which is a solvent, or stirring with a stick or sonicating (A) the graphite powder and graphite particles doped with gas, the graphene layer is separated by gas. This graphene is composed of graphene gel by separating and dispersing the graphene into individual sheets. 4. Graphene gel is obtained by centrifugal separation or by heat treatment at 120 ° C. It is related with a fin quantity manufacturing method (A)
기존에는 흑연을 강한 산에 넣고 산화된 흑연 조각을 초음파 처리한 후 환원제를 사용하여 그래핀을 얻는데 있어서 발생되는 문제점은 ① 강한산. 환원제에 의한 환경오염 ② 산화된 흑연 조각을 초음파 처리하는 시간에 의해 그래핀이 파괴되는점 ③ 산화된 흑연조각이 소량이므로 소량의 그래핀을 얻는 문제점 ④ 흑연은 금속성분 및 여러 성분이 함유되어 있어 순수 그래핀을 얻기가 힘든점이 있는바 이러한 문제점을 해결하고자 본 발명은 1. 분쇄된 흑연 알갱이를 산처리후 물로 세척하거나 자석으로 금속성분을 제거한 천연흑연 알갱이나 합성흑연 알갱이를 2500℃로 가열하여 황.회분 수소.질소.산소와 습도 등을 제거하여 구성한 96%∼99.9% 탄소로 구성된 천연흑연 알갱이나 합성흑연 알갱이를 볼 밀에 넣어 미세분쇄하여 구성한 96%∼99.9% 탄소로 구성된 흑연분말(천연.합성)이나 흑연입자(천연.합성)에 2. 요오드. 이산화탄소. 수소. 산소. 일산화탄소 질소. 헬륨. 네온. 아르곤. 크립톤. 제논. 플로린. 클로린 기체 중에서 1가지 이상의 기체를 선택한 기체(A)를 열처리하여 (A)기체를 도핑한 흑연분말 및 흑연입자로 구성하면 평면층으로 켭켭이 결합되어 있는 그래핀이 기체에 의해 층간격이 생기게 되는데 (A)기체를 도핑한 흑연분말 및 흑연입자를 용매에 넣고 막대로 젓거나 초음파 처리하면 초음파 처리시간이 단축하게 되어 그래핀의 손상을 줄일수 있으며 강한산 및 환원제를 사용하지 않아 환경오염을 발생시키지 않고 96%∼99.9% 탄소로 구성된 흑연분말이나 흑연입자에서 그래핀을 개별시트로 분리하게 되므로 96%∼99.9% 탄소로 구성된 순수 그래핀을 다량 얻을수 있어 기존 흑연에서 그래핀을 얻고자하여 발생되는 문제점을 해결하면서 순수 그래핀을 다량 얻을수 있어 순수 그래핀 다량 제조 방법(A)를 발 명하게 되었다Conventionally, the problem of obtaining graphene by using a reducing agent after sonicating oxidized graphite pieces by putting graphite in a strong acid is ① strong acid. Environmental pollution by reducing agent ② Point where graphene is destroyed by the time of ultrasonic treatment of oxidized graphite fragments ③ Problem of obtaining a small amount of graphene due to the small amount of oxidized graphite fragments ④ Graphite contains metal and various components It is difficult to obtain pure graphene bar to solve these problems 1. The present invention is to wash the pulverized graphite grains after acid treatment or by heating the natural graphite grains or synthetic graphite grains to remove the metal components with magnet to 2500 ℃ Graphite powder composed of 96% to 99.9% carbon composed of 96% to 99.9% carbon by removing sulfur, ash, hydrogen, nitrogen, oxygen, humidity, etc. Natural or synthetic) or graphite particles (natural or synthetic). carbon dioxide. Hydrogen. Oxygen. Carbon monoxide and nitrogen. helium. neon. argon. krypton. Xenon. Florin. When one or more of the chlorine gas is selected, the gas (A) is heat-treated and composed of graphite powder and graphite particles doped with the gas (A). (A) If the graphite powder and graphite particles doped with gas are put in a solvent and stirred with a stick or sonicated, the ultrasonic treatment time can be shortened, thereby reducing the damage of graphene and generating environmental pollution by not using strong acid and reducing agent. Since graphene is separated into individual sheets from graphite powder or graphite particles composed of 96% to 99.9% carbon, a large amount of pure graphene composed of 96% to 99.9% carbon can be obtained, resulting in obtaining graphene from existing graphite. While solving the problem, a large amount of pure graphene can be obtained, and thus a method of preparing pure graphene large amount (A) has been developed.
본 발명은 금속성분 및 황.회분.수소.질소.산소와 습도 등을 제거하여 구성한 96%∼99.9% 탄소로 구성된 흑연분말(천연.합성)이나 흑연입자(천연.합성)에서 순수 그래핀을 다량 얻는 제조 방법을 구성하여 기존에 흑연에서 그래핀을 얻고자 하여서 발생되는 문제점을 해결하는것이 과제이다.The present invention provides pure graphene from graphite powder (natural or synthetic) or graphite particles (natural or synthetic) composed of 96% to 99.9% carbon formed by removing metal, sulfur, ash, hydrogen, nitrogen, oxygen and humidity. It is a problem to solve a problem caused by obtaining a graphene from graphite by constructing a large amount of manufacturing method.
따라서 본 발명은 1. 금속성분 및 황.회분.수소.질소.산소와 습도 등을 제거하여 구성한 96%∼99.9% 탄소로 구성된 흑연분말(천연.합성)이나 흑연입자(천연.합성)에 2. 요오드. 이산화탄소. 수소. 산소. 일산화탄소. 질소. 헬륨. 네온. 아르곤. 크립톤. 제논. 플로린. 클로린 기체 중에서 1가지 이상의 기체를 선택한 기체(A)를 250℃∼400℃로 열처리하여 (A)기체를 도핑한 흑연분말이나 흑연입자로 구성하면 평면층으로 켭켭이 결합되어 있는 그래핀이 기체에 의해 층간격이 생겨서 (A)기체를 도핑한 흑연분말 및 흑연입자를 용매에 넣고 막대로 젓거나 초음파 처리하면 초음파 시간이 단축되어 그래핀의 손상을 줄이면서. 강한산. 환원제를 사용하지 않아 환경오염을 발생시키지 않으며 96%∼99.9% 탄소로 구성된 흑연분말이나 흑연입자에서 그래핀을 개별시트로 분리하여 얻게 되므로 96%∼99.9% 탄소로 구성된 순수 그래핀을 다량 얻을수 있어 순수 그래핀 다량 제조 방법(A)는 기존 흑연에서 그래핀을 얻고자 흑연을 강한 산에 넣고 산화되어 분리된 흑연조각을 초음파 처 리한 후 환원제를 사용하여서 그래핀을 얻으면서 발생되는 문제점을 해결함으로써 과제를 해결하였다.Accordingly, the present invention is directed to graphite powder (natural and synthetic) or graphite particles (natural and synthetic) composed of 96% to 99.9% carbon formed by removing metal components, sulfur, ash, hydrogen, nitrogen, oxygen and humidity. Iodine. carbon dioxide. Hydrogen. Oxygen. carbon monoxide. nitrogen. helium. neon. argon. krypton. Xenon. Florin. When one or more gases selected from among chlorine gas are heat treated at 250 ° C. to 400 ° C. and composed of graphite powder or graphite particles doped with gas (A), the graphene, which is bound on the plane layer, is bound to the gas. (A) When the graphite powder and graphite particles doped with gas are put in a solvent and stirred with a stick or sonicated, the ultrasonic time is shortened, reducing the damage of graphene. Strong acid. Since no reducing agent is used, it does not cause environmental pollution. It is obtained by separating graphene into individual sheets from graphite powder or graphite particles composed of 96% to 99.9% carbon, and thus a large amount of pure graphene composed of 96% to 99.9% carbon can be obtained. The method for preparing a large amount of pure graphene (A) solves the problem of obtaining graphene by using a reducing agent after ultrasonically treating graphite fragments separated by oxidation by putting graphite in a strong acid to obtain graphene from existing graphite. The problem was solved.
본 발명인 순수 그래핀 다량 제조 방법(A)는 기존에 흑연에서 그래핀을 얻고자 하여 발생되는 문제점을 해결하면서 순수 그래핀을 다량 얻을수 있어 효과적이다.The method for preparing a large amount of pure graphene of the present invention (A) is effective because it is possible to obtain a large amount of pure graphene while solving the problems caused by conventionally obtaining graphene from graphite.
본 발명은 기존에 흑연에서 그래핀을 얻고자 하여 발생되는 문제점을 해결하면서 보다 순수한 다량의 그래핀을 얻고자 금속성분 및 황.회분.수소.질소.산소와 습도 등을 제거하여 구성한 96%∼99.9% 탄소로 구성된 흑연분말(천연.합성)이나 흑연입자(천연.합성)에서 순수 그래핀을 다량 얻을수 있는 제조방법을 구성하고자 하는것이 목적으로 본 발명은 1. 금속성분 및 황.회분.수소.질소.산소와 습도 등을 제거하여 구성한 96%∼99.9% 탄소로 구성된 천연흑연 알갱이나 합성흑연 알갱이를 볼 밀에 넣고 미세분쇄하여 구성한 96%∼99.9% 탄소로 구성된 흑연분말(천연.합성)이나 흑연입자(천연.합성)에 2. 요오드. 이산화탄소. 수소. 산소. 일산화탄소. 질소. 헬륨. 네온. 아르곤. 크립톤. 제논. 플로린. 클로린 기체 중에서 1가지 이상의 기체를 선택한 기체(A)를 250℃∼400℃로 열처리하여 (A)기체를 도핑한 흑연분말 및 흑연입자로 구성한 후 3. 용매인 NMP나 DMF 또는 알코올. 물 중에서 선택한 용매에 넣고 막대로 젓거나 초음파 처리하면 (A)기체를 도핑한 흑연분말 및 흑연입자는 도핑된 기체에 의해 그래핀이 층간격이 생기면서 그래핀이 개별시트로 분리 분산하여서 그래핀 겔로 구성되는데 4. 그래핀 겔을 원심분리기를 이용하거나 120℃∼180℃로 열처리하여 용매를 제거하여서 순수 그래핀을 다량 얻을수 있도록 구성한 순수 그래핀 다량 제조 방법(A)은 ①도핑된 기체(A)에 의해 그래핀이 층간격이 생겨 초음파 처리하는 시간을 단축하여 그래핀의 손상을 줄일수 있으며 ②강한산. 환원제를 사용하지 않아 환경오염을 발생시키지 않고 ③ 96%∼99.9% 탄소로 구성된 흑연분말이나 흑연입자에서 그래핀을 얻게 되므로 순수 그래핀을 다량 얻을수 있어 기존 흑연에서 그래핀을 얻고자 하여 발생되는 문제점을 해결하면서 순수 그래핀을 다량 얻을수 있어 발명하게 되었다.The present invention solves the problems caused by obtaining graphene from graphite, while removing metal components, sulfur, ash, hydrogen, nitrogen, oxygen, humidity, etc. to obtain a higher amount of graphene. The object of the present invention is to provide a method for obtaining a large amount of pure graphene from graphite powder (natural and synthetic) or graphite particles (natural and synthetic) composed of 99.9% carbon. Graphite powder consisting of 96% to 99.9% carbon (natural and synthetic) composed of 96% to 99.9% carbon by removing nitrogen, oxygen, humidity, etc. Or iodine to graphite particles (natural and synthetic). carbon dioxide. Hydrogen. Oxygen. carbon monoxide. nitrogen. helium. neon. argon. krypton. Xenon. Florin. A gas (A) selected from at least one gas among chlorine gas is heat-treated at 250 ° C. to 400 ° C. and composed of graphite powder and graphite particles doped with gas (A). 3. NMP, DMF or alcohol as a solvent. In a solvent selected from water, stirring with a stick or sonicating (A) Graphene powder and graphite particles doped with gas, graphene is separated and dispersed into individual sheets by graphene being separated by a doped gas. 4. The graphene gel is composed of a gel. The method of preparing a large amount of pure graphene (A) is configured to obtain a large amount of pure graphene by removing the solvent by heat-treating the graphene gel using a centrifuge or at 120 ° C to 180 ° C. ) Shortens the time of sonication due to the graphene's interlayer spacing, which can reduce the damage of graphene. It does not generate environmental pollution without using reducing agent ③ Because graphene is obtained from graphite powder or graphite particles composed of 96% ∼99.9% carbon, it is possible to obtain a large amount of pure graphene. While solving the problem can be obtained a large amount of pure graphene was invented.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105366662A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Preparing method for sulfur-doped graphene |
KR20180040755A (en) * | 2016-10-12 | 2018-04-23 | 주식회사 덕양 | Making method for graphite |
CN109422259A (en) * | 2017-08-24 | 2019-03-05 | 陕西燕园众欣石墨烯科技有限公司 | A kind of preparation method of nitrogen-doped graphene |
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CN105366662A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Preparing method for sulfur-doped graphene |
CN105366662B (en) * | 2014-08-27 | 2017-11-21 | 中国石油化工股份有限公司 | The preparation method of sulfur doping graphene |
KR20180040755A (en) * | 2016-10-12 | 2018-04-23 | 주식회사 덕양 | Making method for graphite |
CN109422259A (en) * | 2017-08-24 | 2019-03-05 | 陕西燕园众欣石墨烯科技有限公司 | A kind of preparation method of nitrogen-doped graphene |
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